WorldWideScience

Sample records for analytical atomic spectrometry

  1. Prospects in Analytical Atomic Spectrometry

    CERN Document Server

    Bolshakov, A A; Nemets, V M

    2006-01-01

    Tendencies in five main branches of atomic spectrometry (absorption, emission, mass, fluorescence and ionization spectrometry) are considered. The first three techniques are the most widespread and universal, with the best sensitivity attributed to atomic mass spectrometry. In the direct elemental analysis of solid samples, the leading roles are now conquered by laser-induced breakdown and laser ablation mass spectrometry, and the related techniques with transfer of the laser ablation products into inductively-coupled plasma. Advances in design of diode lasers and optical parametric oscillators promote developments in fluorescence and ionization spectrometry and also in absorption techniques where uses of optical cavities for increased effective absorption pathlength are expected to expand. Prospects for analytical instrumentation are seen in higher productivity, portability, miniaturization, incorporation of advanced software, automated sample preparation and transition to the multifunctional modular archite...

  2. A Thermo-Chemical Reactor for analytical atomic spectrometry

    Science.gov (United States)

    Gilmutdinov, A. Kh.; Nagulin, K. Yu.

    2009-01-01

    A novel atomization/vaporization system for analytical atomic spectrometry is developed. It consists of two electrically and thermally separated parts that can be heated separately. Unlike conventional electrothermal atomizers in which atomization occurs immediately above the vaporization site and at the same instant of time, the proposed system allows analyte atomization via an intermediate stage of fractional condensation as a two stage process: Vaporization → Condensation → Atomization. The condensation step is selective since vaporized matrix constituents are mainly non-condensable gases and leave the system by diffusion while analyte species are trapped on the cold surface of a condenser. This kind of sample distillation keeps all the advantages of traditional electrothermal atomization and allows significant reduction of matrix interferences. Integration into one design a vaporizer, condenser and atomizer gives much more flexibility for in situ sample treatment and thus the system is called a Thermo-Chemical Reactor (TCR). Details of the design, temperature measurements, vaporization-condensation-atomization mechanisms of various elements in variety of matrices are investigated in the TCR with spectral, temporal and spatial resolution. The ability of the TCR to significantly reduce interferences and to conduct sample pyrolysis at much higher temperatures as compared to conventional electrothermal atomizers is demonstrated. The analytical potential of the system is shown when atomic absorption determination of Cd and Pb in citrus leaves and milk powder without the use of any chemical modification.

  3. Theory of analytical curves in atomic fluorescence flame spectrometry

    NARCIS (Netherlands)

    Hooymayers, H.P.

    1968-01-01

    An explicit expression for the intensity of atomic resonance fluorescence as a function of atomic concentration in a flame is derived under certain idealized conditions. The expression is generally valid for a pure Doppler absorption line profile as well as for a combined Doppler and collisional bro

  4. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry

    Science.gov (United States)

    Montaser, A.

    In this project, new high temperature plasmas and new sample introduction systems are developed for rapid elemental and isotopic analysis of gases, solutions, and solids using atomic emission spectrometry (AES) and mass spectrometry (MS). These devices offer promise of solving singularly difficult analytical problems that either exist now or are likely to arise in the future in the various fields of energy generation, environmental pollution, nutrition, and biomedicine. Emphasis is being placed on: (1) generation of annular, helium inductively coupled plasmas (He ICPs) that are suitable for atomization, excitation, and ionization of elements possessing high excitation and ionization energies, with the intent of enhancing the detecting powers of a number of elements; (2) computer modelings of ICP discharges to predict the behavior of new and existing plasmas; (3) diagnostic studies of high temperature plasmas and sample introduction systems to quantify their fundamental properties, with the ultimate aim to improve analytical performance of atomic spectrometry; (4) development and characterization of new, low cost sample introduction systems that consume microliter or microgram quantities of samples; and (5) investigation of new membrane separators for stripping solvent from sample aerosol to reduce various interferences and to enhance sensitivity and selectivity in plasma spectrometry.

  5. Expressing self-absorption in the analytical function of inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Kántor, Tibor; Bartha, András

    2015-11-01

    The self-absorption of spectral lines was studied with up to date multi-element inductively coupled plasma atomic emission spectrometry (ICP-AES) instrumentation using radial and axial viewing of the plasma, as well, performing line peak height and line peak area measurements. Two resonance atomic and ionic lines of Cd and Mg were studied, the concentration range was extended up to 2000 mg/L. At the varying analyte concentration, constant matrix concentration of 10,000 mg/L Ca was ensured in the pneumatically nebulized solutions. The physical and the phenomenological formulation of the emission analytical function is overviewed and as the continuity of the earlier results the following equation is offered:

  6. Investigations on Freon-assisted atomization of refractory analytes (Cr, Mo, Ti, V) in multielement electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Heinrich, Hans-Joachim; Matschat, Ralf

    2007-08-01

    Premixed 1% Freon in argon inner gas of various composition (CCl 2F 2, CHClF 2, CHF 3) was applied to graphite furnace atomizer to minimize unfavorable effects of carbide formation, such as signal tailing and memory effects in the simultaneous determination of Cr, Mo, Ti and V refractory analytes by electrothermal atomic absorption spectrometry using a multielement atomic absorption spectrometer. The effect of these gaseous additives was investigated when applied separately in atomization, pyrolysis and clean-out steps. The halogenation effects were analytically useful only under the precondition of using Ar-H 2 outer gas to the furnace to all heating steps, and also using this gas in the pre-atomization (drying, pyrolysis) steps. Optimum analytical performance was obtained when mixtures of 1% Freon in argon were applied just before and during the atomization step at a flow rate of 50 mL min - 1 and 2% hydrogen was used as purge gas. Using optimum conditions, signal tailings and carry-over contamination were reduced effectively and good precision (relative standard deviation below 1%) could be attained. Applying 1% CHClF 2 and an atomization temperature of 2550 °C, the characteristic masses obtained for simple aqueous solutions were 8.8 pg for Cr, 17 pg for Mo, 160 pg for Ti, and 74 pg for V. The limits of detection were 0.05, 0.2, 2.3 and 0.5 μg L - 1 for Cr, Mo, Ti and V, respectively. The developed method was applied to the analysis of digests of advanced ceramics. The accuracy of the procedure was confirmed by analyzing the certified reference material ERM-ED 102 (Boron Carbide Powder) and a silicon nitride powder distributed in the inter-laboratory comparison CCQM-P74.

  7. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Montaser, A.

    1992-01-01

    New high temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. Emphasis was placed on atmospheric pressure He inductively coupled plasmas (ICP) suitable for atomization, excitation, and ionization of elements; simulation and computer modeling of plasma sources with potential for use in spectrochemical analysis; spectroscopic imaging and diagnostic studies of high temperature plasmas, particularly He ICP discharges; and development of new, low-cost sample introduction systems, and examination of techniques for probing the aerosols over a wide range. Refs., 14 figs. (DLC)

  8. Atomic spectrometry update : environmental analysis

    OpenAIRE

    Butler, Owen T.; Cairns, Warren R. L.; Cook, Jennifer M.; Davidson, Christine M.

    2012-01-01

    This is the 27th annual review published in Journal of Analytical Atomic Spectrometry of the application of atomic spectrometry to the chemical analysis of environmental samples. This Update refers to papers published approximately between September 2010 and August 2011 and continues the series of Atomic Spectrometry Updates (ASUs) in Environmental Analysis1 that should be read in conjunction with other related ASU reviews in the series, namely: clinical and biological materials, foods and be...

  9. Towards broadening thermospray flame furnace atomic absorption spectrometry: Influence of organic solvents on the analytical signal of magnesium

    OpenAIRE

    Ezequiel Morzan; Jorge Stripeikis; Mabel Tudino

    2015-01-01

    This study demonstrates the influence of the solvent when thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) is employed for the determination of elements of low volatility, taking magnesium (Mg) as leading case. Several organic solvents/water solutions of different characteristics (density, surface tension, viscosity, etc.) and proportions were employed for the TS-FF-AAS analytical determination. To this end, solutions containing methanol, ethanol and isopropanol in water w...

  10. Three-dimensional time-dependent computer modeling of the electrothermal atomizers for analytical spectrometry

    Science.gov (United States)

    Tsivilskiy, I. V.; Nagulin, K. Yu.; Gilmutdinov, A. Kh.

    2016-02-01

    A full three-dimensional nonstationary numerical model of graphite electrothermal atomizers of various types is developed. The model is based on solution of a heat equation within solid walls of the atomizer with a radiative heat transfer and numerical solution of a full set of Navier-Stokes equations with an energy equation for a gas. Governing equations for the behavior of a discrete phase, i.e., atomic particles suspended in a gas (including gas-phase processes of evaporation and condensation), are derived from the formal equations molecular kinetics by numerical solution of the Hertz-Langmuir equation. The following atomizers test the model: a Varian standard heated electrothermal vaporizer (ETV), a Perkin Elmer standard THGA transversely heated graphite tube with integrated platform (THGA), and the original double-stage tube-helix atomizer (DSTHA). The experimental verification of computer calculations is carried out by a method of shadow spectral visualization of the spatial distributions of atomic and molecular vapors in an analytical space of an atomizer.

  11. Arsenic speciation by hydride generation-quartz furnace atomic absorption spectrometry. Optimization of analytical parameters and application to environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Molenat, N.; Astruc, A.; Holeman, M.; Pinel, R. [Laboratoire de Chimie Analytique Bioinorganique et Environnement, Dept. de Chimie, Faculte des Sciences et Techniques, 64 - Pau (France); Maury, G. [Montpellier-2 Univ., 34 (France). Dept. de Chimie Organique Fine

    1999-11-01

    Analytical parameters of hydride generation, trapping, gas chromatography and atomic absorption spectrometry detection in a quartz cell furnace (HG/GC/QFAAS) device have been optimized in order to develop an efficient and sensitive method for arsenic compounds speciation. Good performances were obtained with absolute detection limits in the range of 0.1 - 0.5 ng for arsenite, arsenate, mono-methyl-arsonic acid (MMAA), dimethyl-arsinic acid (DMAA) and trimethyl-arsine oxide (TMAO). A pH selective reduction for inorganic arsenic speciation was successfully reported. Application to the accurate determination of arsenic compounds in different environmental samples was performed. (authors)

  12. Analytical mass spectrometry. Abstracts

    Energy Technology Data Exchange (ETDEWEB)

    1990-12-31

    This 43rd Annual Summer Symposium on Analytical Chemistry was held July 24--27, 1990 at Oak Ridge, TN and contained sessions on the following topics: Fundamentals of Analytical Mass Spectrometry (MS), MS in the National Laboratories, Lasers and Fourier Transform Methods, Future of MS, New Ionization and LC/MS Methods, and an extra session. (WET)

  13. Analytical mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    1990-01-01

    This 43rd Annual Summer Symposium on Analytical Chemistry was held July 24--27, 1990 at Oak Ridge, TN and contained sessions on the following topics: Fundamentals of Analytical Mass Spectrometry (MS), MS in the National Laboratories, Lasers and Fourier Transform Methods, Future of MS, New Ionization and LC/MS Methods, and an extra session. (WET)

  14. Flow Injection and Atomic Absorption Spectrometry - An Effective and Attractive Analytical Chemical Combination

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Nielsen, Steffen

    1998-01-01

    One of the advantages of the flow injection (FI) concept is that it is compatible with virtually all detection techniques. Being a versatile vehicle for enhancing the performance of the individual detection devices, the most spectacular results have possibly been obtained in conjunction with atomic...

  15. Development of an analytical method for antimony speciation in vegetables by HPLC-hydride generation-atomic fluorescence spectrometry.

    Science.gov (United States)

    Olivares, David; Bravo, Manuel; Feldmann, Jorg; Raab, Andrea; Neaman, Alexander; Quiroz, Waldo

    2012-01-01

    A new method for antimony speciation in terrestrial edible vegetables (spinach, onions, and carrots) was developed using HPLC with hydride generation-atomic fluorescence spectrometry. Mechanical agitation and ultrasound were tested as extraction techniques. Different extraction reagents were evaluated and optimal conditions were determined using experimental design methodology, where EDTA (10 mmol/L, pH 2.5) was selected because this chelate solution produced the highest extraction yield and exhibited the best compatibility with the mobile phase. The results demonstrated that EDTA prevents oxidation of Sb(III) to Sb(V) and maintains the stability of antimony species during the entire analytical process. The LOD and precision (RSD values obtained) for Sb(V), Sb(III), and trimethyl Sb(V) were 0.08, 0.07, and 0.9 microg/L and 5.0, 5.2, and 4.7%, respectively, for a 100 microL sample volume. The application of this method to real samples allowed extraction of 50% of total antimony content from spinach, while antimony extracted from carrots and onion samples ranged between 50 and 60 and 54 and 70%, respectively. Only Sb(V) was detected in three roots (onion and spinach) that represented 60-70% of the total antimony in the extracts. PMID:22970588

  16. Development of an analytical method for antimony speciation in vegetables by HPLC-hydride generation-atomic fluorescence spectrometry.

    Science.gov (United States)

    Olivares, David; Bravo, Manuel; Feldmann, Jorg; Raab, Andrea; Neaman, Alexander; Quiroz, Waldo

    2012-01-01

    A new method for antimony speciation in terrestrial edible vegetables (spinach, onions, and carrots) was developed using HPLC with hydride generation-atomic fluorescence spectrometry. Mechanical agitation and ultrasound were tested as extraction techniques. Different extraction reagents were evaluated and optimal conditions were determined using experimental design methodology, where EDTA (10 mmol/L, pH 2.5) was selected because this chelate solution produced the highest extraction yield and exhibited the best compatibility with the mobile phase. The results demonstrated that EDTA prevents oxidation of Sb(III) to Sb(V) and maintains the stability of antimony species during the entire analytical process. The LOD and precision (RSD values obtained) for Sb(V), Sb(III), and trimethyl Sb(V) were 0.08, 0.07, and 0.9 microg/L and 5.0, 5.2, and 4.7%, respectively, for a 100 microL sample volume. The application of this method to real samples allowed extraction of 50% of total antimony content from spinach, while antimony extracted from carrots and onion samples ranged between 50 and 60 and 54 and 70%, respectively. Only Sb(V) was detected in three roots (onion and spinach) that represented 60-70% of the total antimony in the extracts.

  17. Noise-immune cavity-enhanced analytical atomic spectrometry — NICE-AAS — A technique for detection of elements down to zeptogram amounts

    International Nuclear Information System (INIS)

    Noise-immune cavity-enhanced optical heterodyne molecular spectroscopy (NICE-OHMS) is a powerful technique for detection of molecular compounds in gas phase that is based on a combination of two important concepts: frequency modulation spectroscopy (FMS) for reduction of noise, and cavity enhancement, for prolongation of the interaction length between the light and the sample. Due to its unique properties, it has demonstrated unparalleled detection sensitivity when it comes to detection of molecular constituents in the gas phase. However, despite these, it has so far not been used for detection of atoms, i.e. for elemental analysis. The present work presents an assessment of the expected performance of Doppler-broadened (Db) NICE-OHMS for analytical atomic spectrometry, then referred to as noise-immune cavity-enhanced analytical atomic spectrometry (NICE-AAS). After a description of the basic principles of Db-NICE-OHMS, the modulation and detection conditions for optimum performance are identified. Based on a previous demonstrated detection sensitivity of Db-NICE-OHMS of 5 × 10−12 cm−1 Hz−1∕2 (corresponding to a single-pass absorbance of 7 × 10−11 over 10 s), the expected limits of detection (LODs) of Hg and Na by NICE-AAS are estimated. Hg is assumed to be detected in gas phase directly while Na is considered to be atomized in a graphite furnace (GF) prior to detection. It is shown that in the absence of spectral interferences, contaminated sample compartments, and optical saturation, it should be feasible to detect Hg down to 10 zg/cm3 (10 fg/m3 or 10−5 ng/m3), which corresponds to 25 atoms/cm3, and Na down to 0.5 zg (zg = zeptogram = 10−21 g), representing 50 zg/mL (parts-per-sextillion, pps, 1:1021) in liquid solution (assuming a sample of 10 μL) or solely 15 atoms injected into the GF, respectively. These LODs are several orders of magnitude lower (better) than any previous laser-based absorption technique previously demonstrated under

  18. Noise-immune cavity-enhanced analytical atomic spectrometry - NICE-AAS - A technique for detection of elements down to zeptogram amounts

    Science.gov (United States)

    Axner, Ove; Ehlers, Patrick; Hausmaninger, Thomas; Silander, Isak; Ma, Weiguang

    2014-10-01

    Noise-immune cavity-enhanced optical heterodyne molecular spectroscopy (NICE-OHMS) is a powerful technique for detection of molecular compounds in gas phase that is based on a combination of two important concepts: frequency modulation spectroscopy (FMS) for reduction of noise, and cavity enhancement, for prolongation of the interaction length between the light and the sample. Due to its unique properties, it has demonstrated unparalleled detection sensitivity when it comes to detection of molecular constituents in the gas phase. However, despite these, it has so far not been used for detection of atoms, i.e. for elemental analysis. The present work presents an assessment of the expected performance of Doppler-broadened (Db) NICE-OHMS for analytical atomic spectrometry, then referred to as noise-immune cavity-enhanced analytical atomic spectrometry (NICE-AAS). After a description of the basic principles of Db-NICE-OHMS, the modulation and detection conditions for optimum performance are identified. Based on a previous demonstrated detection sensitivity of Db-NICE-OHMS of 5 × 10- 12 cm- 1 Hz- 1/2 (corresponding to a single-pass absorbance of 7 × 10- 11 over 10 s), the expected limits of detection (LODs) of Hg and Na by NICE-AAS are estimated. Hg is assumed to be detected in gas phase directly while Na is considered to be atomized in a graphite furnace (GF) prior to detection. It is shown that in the absence of spectral interferences, contaminated sample compartments, and optical saturation, it should be feasible to detect Hg down to 10 zg/cm3 (10 fg/m3 or 10- 5 ng/m3), which corresponds to 25 atoms/cm3, and Na down to 0.5 zg (zg = zeptogram = 10- 21 g), representing 50 zg/mL (parts-per-sextillion, pps, 1:1021) in liquid solution (assuming a sample of 10 μL) or solely 15 atoms injected into the GF, respectively. These LODs are several orders of magnitude lower (better) than any previous laser-based absorption technique previously demonstrated under atmospheric

  19. Heavy metal adsorptivity of calcium-alginate-modified diethylenetriamine-silica gel and its application to a flow analytical system using flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Highlights: • Calcium-alginate-modified dien-silica gel adsorbed multivalent metal ions. • Metal ions adsorbed on CaAD were eluted using low acidic concentrations. • Flow system with CaAD-packed column enriched metal concentrations up to 50-fold. - Abstract: This study aimed to evaluate the heavy metal adsorptivity of calcium-alginate-modified diethylenetriamine-silica gel (CaAD) and incorporate this biosorbent into a flow analytical system for heavy metal ions using flame atomic absorption spectrometry (FAAS). The biosorbent was synthesized by electrostatically coating calcium alginate onto diethylenetriamine (dien)-silica gel. Copper ion adsorption tests by a batch method showed that CaAD exhibited a higher adsorption rate compared with other biosorbents despite its low maximum adsorption capacity. Next, CaAD was packed into a 1 mL microcolumn, which was connected to a flow analytical system equipped with an FAAS instrument. The flow system quantitatively adsorbed heavy metals and enriched their concentrations. This quantitative adsorption was achieved for pH 3–4 solutions containing 1.0 × 10−6 M of heavy metal ions at a flow rate of 5.0 mL min−1. Furthermore, the metal ions were successfully desorbed from CaAD at low nitric acid concentrations (0.05–0.15 M) than from the polyaminecarboxylic acid chelating resin (Chelex 100). Therefore, CaAD may be considered as a biosorbent that quickly adsorbs and easily desorbs analyte metal ions. In addition, the flow system enhanced the concentrations of heavy metals such as Cu2+, Zn2+, and Pb2+ by 50-fold. This new enrichment system successfully performed the separation and determination of Cu2+ (5.0 × 10−8 M) and Zn2+ (5.7 × 10−8 M) in a river water sample and Pb2+ (3.8 × 10−9 M) in a ground water sample

  20. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry. Progress report, January 1, 1990--December 31, 1992

    Energy Technology Data Exchange (ETDEWEB)

    Montaser, A.

    1992-09-01

    New high temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. Emphasis was placed on atmospheric pressure He inductively coupled plasmas (ICP) suitable for atomization, excitation, and ionization of elements; simulation and computer modeling of plasma sources with potential for use in spectrochemical analysis; spectroscopic imaging and diagnostic studies of high temperature plasmas, particularly He ICP discharges; and development of new, low-cost sample introduction systems, and examination of techniques for probing the aerosols over a wide range. Refs., 14 figs. (DLC)

  1. Development of an analytical method for the determination of arsenic in gasoline samples by hydride generation-graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Becker, Emilene M. [Universidade Federal do Pampa, Bage, RS (Brazil); Universidade Federal de Pelotas, Pelotas, RS (Brazil); Dessuy, Morgana B.; Boschetti, Wiliam [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R., E-mail: mgrvale@ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Ferreira, Sergio L.C. [Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Instituto de Quimica, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil)

    2012-05-15

    The purpose of the present work was to optimize the conditions for the determination of arsenic in gasoline with hydride generation-graphite furnace atomic absorption spectrometry after acid digestion using a full two-level factorial design with center point. The arsine was generated in a batch system and collected in a graphite tube coated with 150 {mu}g Ir as a permanent modifier. The sample volume, the pre-reduction conditions, the temperature program and modifier mass were kept fixed for all experiments. The estimated main effects were: reducing agent concentration (negative effect), acid concentration (negative effect) and trapping temperature (positive effect). It was observed that there were interactions between the variables. Moreover, the curvature was significant, indicating that the best conditions were at the center point. The optimized parameters for arsine generation were 2.7 mol L{sup -1} hydrochloric acid and 1.6% (w/v) sodium tetrahydroborate. The optimized conditions to collect arsine in the graphite furnace were a trapping temperature of 250 Degree-Sign C and a collection time of 30 s. The limit of detection was 6.4 ng L{sup -1} and the characteristic mass was 24 pg. Two different systems for acid digestion were used: a digester block with cold finger and a microwave oven. The concentration of arsenic found with the proposed method was compared with that obtained using a detergentless microemulsion and direct graphite furnace determination. The results showed that the factorial design is a simple tool that allowed establishing the appropriate conditions for sample preparation and also helped in evaluating the interaction between the factors investigated. - Highlights: Black-Right-Pointing-Pointer We determined As in gasoline using hydride generation-graphite furnace AAS. Black-Right-Pointing-Pointer We compared three sample preparation procedures. Black-Right-Pointing-Pointer A multivariate approach was used to optimize the conditions. Black

  2. Antimony in drinking water, red blood cells, and serum: development of analytical methodology using transversely heated graphite furnace atomization-atomic absorption spectrometry.

    Science.gov (United States)

    Subramanian, K S; Poon, R; Chu, I; Connor, J W

    1997-05-01

    An atomic absorption spectrometric (AAS) method has been developed for determining microg/L levels of Sb in samples of water and blood. The AAS method is based on the concept of stabilized temperature platform furnace atomization (STPF) realized through the use of a transversely heated graphite atomizer (THGA) furnace, longitudinal Zeeman-effect background correction, and matrix modification with palladium nitrate-magnesium nitrate-nitric acid. The method of standard additions is not mandatory. The detection limit (3 standard deviations of the blank) is 2.6 microg Sb/L for the water, red blood cells (RBCs), and serum samples. Data are presented on the degree of accuracy and precision. The THGA-AAS method is simple, fast, and contamination-free because the entire operation from sampling to AAS measurement is carried out in the same tube. The method has been applied to the determination of Sb in some leachate tap water samples derived from a static copper plumbing system containing Sn/Sb solders, and in small samples (0.5 ml) of RBCs and serum derived from rats given Sb-supplemented drinking water. PMID:9175512

  3. Ultratrace determination of lead by hydride generation in-atomizer trapping atomic absorption spectrometry: Optimization of plumbane generation and analyte preconcentration in a quartz trap-and-atomizer device

    Energy Technology Data Exchange (ETDEWEB)

    Kratzer, Jan, E-mail: jkratzer@biomed.cas.cz

    2012-05-15

    A compact trap-and-atomizer device and a preconcentration procedure based on hydride trapping in excess of oxygen over hydrogen in the collection step, both constructed and developed previously in our laboratory, were employed to optimize plumbane trapping in this device and to develop a routine method for ultratrace lead determination subsequently. The inherent advantage of this preconcentration approach is that 100% preconcentration efficiency for lead is reached in this device which has never been reported before using quartz or metal traps. Plumbane is completely retained in the trap-and-atomizer device at 290 Degree-Sign C in oxygen-rich atmosphere and trapped species are subsequently volatilized at 830 Degree-Sign C in hydrogen-rich atmosphere. Effect of relevant experimental parameters on plumbane trapping and lead volatilization are discussed, and possible trapping mechanisms are hypothesized. Plumbane trapping in the trap-and-atomizer device can be routinely used for lead determination at ultratrace levels reaching a detection limit of 0.21 ng ml{sup -1} Pb (30 s preconcentration, sample volume 2 ml). Further improvement of the detection limit is feasible by reducing the blank signal and increasing the trapping time. - Highlights: Black-Right-Pointing-Pointer In-atomizer trapping HG-AAS was optimized for Pb. Black-Right-Pointing-Pointer A compact quartz trap-and-atomizer device was employed. Black-Right-Pointing-Pointer Generation, preconcentration and atomization steps were investigated in detail. Black-Right-Pointing-Pointer 100% preconcentration efficiency for lead was reached. Black-Right-Pointing-Pointer Routine analytical method was developed for Pb determination (LOD of 0.2 ng ml{sup -1} Pb).

  4. Analytical aspects of hydrogen exchange mass spectrometry

    Science.gov (United States)

    Engen, John R.; Wales, Thomas E.

    2016-01-01

    The analytical aspects of measuring hydrogen exchange by mass spectrometry are reviewed. The nature of analytical selectivity in hydrogen exchange is described followed by review of the analytical tools required to accomplish fragmentation, separation, and the mass spectrometry measurements under restrictive exchange quench conditions. In contrast to analytical quantitation that relies on measurements of peak intensity or area, quantitation in hydrogen exchange mass spectrometry depends on measuring a mass change with respect to an undeuterated or deuterated control, resulting in a value between zero and the maximum amount of deuterium that could be incorporated. Reliable quantitation is a function of experimental fidelity and to achieve high measurement reproducibility, a large number of experimental variables must be controlled during sample preparation and analysis. The method also reports on important qualitative aspects of the sample, including conformational heterogeneity and population dynamics. PMID:26048552

  5. Evaluation of analyte additions method for sodium determination in fuel ethanol by flame atomic emission spectrometry; Avaliacao do metodo das adicoes de analito para a determinacao de sodio em alcool combustivel por espectrometria de emissao atomica em chama

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Adriana Paiva de; Okumura, Leonardo Luiz; Gomes Neto, Jose Anchieta [UNESP, Araraquara, SP (Brazil). Inst. de Quimica. Dept. de Quimica Analitica

    2002-07-01

    The analyte additions method was applied for sodium determination in fuel ethanol by atomic emission spectrometry. Graphics involving emission intensity versus analyte concentration in the 0 - 0.300 mg Na L{sup -1} interval concentration range containing 2.1 g K L{sup -1} as an ionisation buffer. Twenty samples of commercial fuel ethanol were collected in different gas stations located in Araraquara city, analyzed and results obtained varied from 0.0072 to 1.55 mg Na L{sup -1}. The limits of detection (L.O.D.) varied from 0.0026 to 0.0239 mg Na L{sup -1}. Recoveries varied in the 95 - 104 % interval. The relative standard deviations (n=12) for three analyte additions in all samples were {<=}4,1 %. (author)

  6. Economical Alternatives for High Sensitivity in Atomic Spectrometry Laboratory

    Directory of Open Access Journals (Sweden)

    O. Yavuz Ataman

    2007-12-01

    Full Text Available The most commonly used analytical tools for determination of elements at trace levels are atomic absorption spectrometry (AAS, inductively coupled plasma, optical emission and mass spectrometry (ICP-OES and ICP-MS and atomic fluorescence spectrometry (AFS. Although sensitive plasma techniques are becoming predominant in most of the western laboratories, AAS keeps its importance in developing countries. Simple and inexpensive ways of enhancing sensitivity will be described for laboratories equipped with only a flame AA spectrometer. Although there are many chemical preconcentration procedures to improve sensitivity of flame AAS, only some atom trapping techniques will be included here. One kind of atom trapping device is a slotted quartz tube (SQT used for in situ preconcentration of analyte species followed by a rapid revolatilization cycle to obtain an enhanced signal. These devices provide limits of detection at a level of µg L-1. Another kind of atom trapping involves use of vapor generation technique and quartz or tungsten atom trapping surfaces. The analytical steps consist of the generation of volatile species, usually by hydride formation using NaBH4, trapping these species at the surface of an atom trap held at an optimized temperature and finally re-volatilizing analyte species by rapid heating of trap. These species are transported using a carrier gas to an externally heated quartz tube as commonly used in hydride generation AAS systems; a transient signal is formed and measured. These traps have limits of detection in the order of ng L-1.

  7. An effective analytical system based on a pulsed direct current microplasma source for ultra-trace mercury determination using gold amalgamation cold vapor atomic emission spectrometry

    International Nuclear Information System (INIS)

    A novel analysis system based on a low power atmospheric pressure pulsed direct current (Pdc) microplasma is described for the determination of ultra-trace mercury in natural water by cold vapor generation atomic emission spectrometry (CV-AES). The plasma was generated with a miniaturized home-built high-voltage Pdc power supply which decreased the volume and weight of the whole experiment setup. The CV-Pdc-AES system is based on the preconcentration of mercury vapor on a gold filament trapping micro-column prior to detection that provides fast, reproducible absorption and desorption of mercury. The micro-column is produced by winding 30 μm diameter 100 m long gold filament to a small ball and then insert it into a quartz tube of 6 mm i.d, 8 mm o.d. Under the optimized experimental conditions, the new system provides high sensitivity (detection limit: 0.08 pg mL−1) and good reproducibility (RSD 3.0%, [Hg] = 20 pg mL−1, n = 11). The calibration curve is linear at levels near the detection limit up to at least 200 pg mL−1 and the accuracy is on the order of 1–4%. The proposed method was applied to 5 real water samples for mercury ultra-trace analysis. The advantages and features of the newly developed system include high sensitivity, simple structure, low cost, and compact volume with field portable potential. - Highlights: • A novel system based on a low power pulsed dc microplasma for mercury detection. • A small home-built pulsed dc power supply was used to ignite the microplasma. • A gold filament preconcentrator followed by thermal desorption was used. • A detection limit of 0.08 pg mL−1 was achieved for sensitive mercury detection. • The system is compact, low power, and has potential for field portable application

  8. An effective analytical system based on a pulsed direct current microplasma source for ultra-trace mercury determination using gold amalgamation cold vapor atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yuan, Xin [Research Center of Analytical Instrumentation, Analytical Testing Center, College of Chemistry, Sichuan University, Chengdu (China); Yang, Guang; Ding, Yu [College of Instrumentation and Electrical Engineering, Jilin University, Changchun (China); Li, Xuemei; Zhan, Xuefang; Zhao, Zhongjun [Research Center of Analytical Instrumentation, Analytical Testing Center, College of Chemistry, Sichuan University, Chengdu (China); Duan, Yixiang, E-mail: yduan@scu.edu.cn [Research Center of Analytical Instrumentation, Analytical Testing Center, College of Chemistry, Sichuan University, Chengdu (China)

    2014-03-01

    A novel analysis system based on a low power atmospheric pressure pulsed direct current (Pdc) microplasma is described for the determination of ultra-trace mercury in natural water by cold vapor generation atomic emission spectrometry (CV-AES). The plasma was generated with a miniaturized home-built high-voltage Pdc power supply which decreased the volume and weight of the whole experiment setup. The CV-Pdc-AES system is based on the preconcentration of mercury vapor on a gold filament trapping micro-column prior to detection that provides fast, reproducible absorption and desorption of mercury. The micro-column is produced by winding 30 μm diameter 100 m long gold filament to a small ball and then insert it into a quartz tube of 6 mm i.d, 8 mm o.d. Under the optimized experimental conditions, the new system provides high sensitivity (detection limit: 0.08 pg mL{sup −1}) and good reproducibility (RSD 3.0%, [Hg] = 20 pg mL{sup −1}, n = 11). The calibration curve is linear at levels near the detection limit up to at least 200 pg mL{sup −1} and the accuracy is on the order of 1–4%. The proposed method was applied to 5 real water samples for mercury ultra-trace analysis. The advantages and features of the newly developed system include high sensitivity, simple structure, low cost, and compact volume with field portable potential. - Highlights: • A novel system based on a low power pulsed dc microplasma for mercury detection. • A small home-built pulsed dc power supply was used to ignite the microplasma. • A gold filament preconcentrator followed by thermal desorption was used. • A detection limit of 0.08 pg mL{sup −1} was achieved for sensitive mercury detection. • The system is compact, low power, and has potential for field portable application.

  9. Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS)

    International Nuclear Information System (INIS)

    Mercury (Hg) is a toxic metal applied to a variety of products and processes, representing a risk to the health of occupationally or accidentally exposed subjects. Dental amalgam is a restorative material composed of metallic mercury, which use has been widely debated in the last decades. Due to the dubiety of the studies concerning dental amalgam, many efforts concerning this issue have been conducted. The Tropical Medicine Foundation (Tocantins, Brazil) has recently initiated a study to evaluate the environmental and occupational levels of exposure to mercury in dentistry attendants at public consulting rooms in the city of Araguaina (TO). In collaboration with this study, the laboratory of analysis at IPEN's Chemistry and Environment Center is undertaking the analysis of mercury levels in exposed subjects' urine samples using cold vapor atomic absorption spectrometry. This analysis requires the definition of a methodology capable of generating reliable results. Such methodology can only be implemented after a rigorous validation procedure. As part of this work, a series of tests were conducted in order to confirm the suitability of the selected methodology and to assert that the laboratory addresses all requirements needed for a successful implementation of the methodology. The following parameters were considered in order to test the method's performance: detection and quantitation limits, selectivity, sensitivity, linearity, accuracy and precision. The assays were carried out with certified reference material, which assures the traceability of the results. Taking into account the estimated parameters, the method can be considered suitable for the afore mentioned purpose. The mercury concentration found for the reference material was of (95,12 +- 11,70)mug.L-1 with a recovery rate of 97%. The method was also applied to 39 urine samples, six of which (15%) showing urinary mercury levels above the normal limit of 10μg.L-1. The obtained results fall into a range

  10. Study on Atomic Fluorescence Spectrometry Excited by Synchrotron Radiation

    Institute of Scientific and Technical Information of China (English)

    Jia-jia Guo; Wu-er Gan; Guo-bin Zhang; Qing-de Su

    2008-01-01

    A novel analysis approach using atomic fluorescence excited by synchrotron radiation is presented. A system for synchrotron radiation-atomic fluorescence spectrometry is developed, and experimental conditions such as flow rate, analyte acidity, concentration of pre-reducing and hydrogenation system are optimized. The proposed method is successfully applied to get an excitation spectrum of arsenic. Seven of ten primary spectral lines, four of which have never been reported by means of atomic fluorescence spectrometry, agree well with the existing reports. The other three are proposed for the first time. Excitation potentials and possible transitions are investigated. Especially for the prominent line at 234.99 nm, the mechanism of generation is discussed and a model of energy transition processes is proposed.

  11. CANAS '01 - Colloquium analytical atomic spectroscopy; CANAS '01 - Colloquium Analytische Atomspektroskopie. Programm. Kurzfassungen der Vortraege und Poster

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2001-07-01

    The main topics of the meeting on analytical atom spectroscopy were: optical atom spectrometry, x-ray fluorescence analysis, absorption spectroscopy, icp mass spectroscopy, trace analysis, sampling, sample preparation and quality assurance.

  12. Principle and analytical applications of resonance ionization mass spectrometry

    International Nuclear Information System (INIS)

    Resonance ionization mass spectrometry (RIMS) is a very sensitive analytical technique for the detection of trace elements. This method is based on the excitation and ionization of atoms with resonant laser light followed by mass analysis. It allows element and, in some cases, isotope selective ionization and is applicable to most of the elements of the periodic table. A high selectivity can be achieved by applying three step photoionization of the elements under investigation and an additional mass separation for an unambiguous isotope assignment. An effective facility for resonance ionization mass spectrometry consists of three dye lasers which are pumped by two copper vapor lasers and of a linear time-of-flight spectrometer with a resolution better than 2500. Each copper vapor laser has a pulse repetition rate of 6,5 kHz and an average output power of 30 W. With such an apparatus measurements with lanthanide-, actinide-, and technetium-samples have been performed. By saturating the excitation steps and by using autoionizing states for ionization step a detection efficiency of 4 x 10-6 and 2,5 x 10-6 has been reached for plutonium and technetium, respectively, leading to a detection limit of less than 107 atoms in the sample. Measurements of isotope ratios of plutonium samples were in good agreement with mass-spectrometric data. The high elemental selectivity of the resonance ionization spectrometry could be demonstrated. (Authors)

  13. Comparison of electrothermal atomization diode laser Zeeman- and wavelength-modulated atomic absorption and coherent forward scattering spectrometry

    International Nuclear Information System (INIS)

    Atomic absorption and coherent forward scattering spectrometry by using a near-infrared diode laser with and without Zeeman and wavelength modulation were carried out with graphite furnace electrothermal atomization. Analytical curves and limits of detection were compared. The magnetic field was modulated with 50 Hz, and the wavelength of the diode laser with 10 kHz. Coherent forward scattering was measured with crossed and slightly uncrossed polarizers. The results show that the detection limits of atomic absorption spectrometry are roughly the same as those of coherent forward scattering spectrometry with crossed polarizers. According to the theory with bright flicker noise limited laser sources the detection limits and linear ranges obtained with coherent forward scattering spectrometry with slightly uncrossed polarizers are significantly better than those obtained with crossed polarizers and with atomic absorption spectrometry. This is due to the fact that employing approaches of polarization spectroscopy reduce laser intensity fluctuations to their signal carried fractions

  14. The Rewards of Fundamental Atomic Spectrometry Research

    Institute of Scientific and Technical Information of China (English)

    Walter Slavin

    2000-01-01

    Atomic spectrometry research is the life-blood of the atomic spectrometry instrument industry.The instrument designer can be expected to innovate in the execution of instrumentation and should be expected to be the expert in optical,electronic and software engineering.Fundamentally new technology has required too long a period of gestation to be compatible with commercial time scales and budgets.But in the past decade,the pressure from stockholders for increased return on investments has put increasingly strong pressure on management to reduce expenses and focus increasingly on projects that guarantee a fast payback.This pressure falls particularly heavily on the larger companies;the same companies that a decade or more ago were the ones that brought the more far-reaching and expensive new concepts to market. Fundamental research in atomic spectrometry has been accomplished in the past several decades mostly in the academic environment and in research institutions that are Federally funded.All of the Federally funded research institutions have been forced to alter their missions to more tangible and immediate goals,and many have also seen severe financial reductions.

  15. Flame-in-gas-shield and miniature diffusion flame hydride atomizers for atomic fluorescence spectrometry: optimization and comparison

    International Nuclear Information System (INIS)

    A detailed optimization of relevant experimental parameters of two hydride atomizers for atomic fluorescence spectrometry: flame-in-gas-shield atomizer with a two-channel shielding unit and a standard atomizer for atomic fluorescence spectrometry, miniature diffusion flame, was performed. Arsine, generated by the reaction with NaBH4 in a flow injection arrangement, was chosen as the model hydride. Analytical characteristics of both the atomizers (sensitivity, noise, limits of detection) were compared. Under optimum conditions sensitivity obtained with flame-in-gas-shield atomizer was approximately twice higher than with miniature diffusion flame. The additional advantage of flame-in-gas-shield atomizer is significantly lower flame emission resulting in a better signal to noise ratio. The resulting arsenic limits of detection for miniature diffusion flame and flame-in-gas-shield atomizer were 3.8 ng l−1 and 1.0 ng l−1, respectively. - Highlights: • We optimized and compared two hydride atomizers for atomic fluorescence spectrometry. • Miniature diffusion flame and flame-in-gas-shield atomizer were optimized. • The limit of detection for arsenic was 1.0 ng l−1

  16. Flame-in-gas-shield and miniature diffusion flame hydride atomizers for atomic fluorescence spectrometry: optimization and comparison

    Energy Technology Data Exchange (ETDEWEB)

    Marschner, Karel, E-mail: karel.marschner@biomed.cas.cz [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Charles University in Prague, Faculty of Science, Department of Analytical Chemistry, Albertov 8, 128 43 Prague (Czech Republic); Musil, Stanislav; Dědina, Jiří [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic)

    2015-07-01

    A detailed optimization of relevant experimental parameters of two hydride atomizers for atomic fluorescence spectrometry: flame-in-gas-shield atomizer with a two-channel shielding unit and a standard atomizer for atomic fluorescence spectrometry, miniature diffusion flame, was performed. Arsine, generated by the reaction with NaBH{sub 4} in a flow injection arrangement, was chosen as the model hydride. Analytical characteristics of both the atomizers (sensitivity, noise, limits of detection) were compared. Under optimum conditions sensitivity obtained with flame-in-gas-shield atomizer was approximately twice higher than with miniature diffusion flame. The additional advantage of flame-in-gas-shield atomizer is significantly lower flame emission resulting in a better signal to noise ratio. The resulting arsenic limits of detection for miniature diffusion flame and flame-in-gas-shield atomizer were 3.8 ng l{sup −1} and 1.0 ng l{sup −1}, respectively. - Highlights: • We optimized and compared two hydride atomizers for atomic fluorescence spectrometry. • Miniature diffusion flame and flame-in-gas-shield atomizer were optimized. • The limit of detection for arsenic was 1.0 ng l{sup −1}.

  17. Preconcentration and Atomization of Arsane in a Dielectric Barrier Discharge with Detection by Atomic Absorption Spectrometry.

    Science.gov (United States)

    Novák, Petr; Dědina, Jiří; Kratzer, Jan

    2016-06-01

    Atomization of arsane in a 17 W planar quartz dielectric barrier discharge (DBD) atomizer was optimized, and its performance was compared to that of a multiple microflame quartz tube atomizer (MMQTA) for atomic absorption spectrometry (AAS). Argon, at a flow rate of 60 mL min(-1), was the best DBD discharge gas. Free As atoms were also observed in the DBD with nitrogen, hydrogen, and helium discharge gases but not in air. A dryer tube filled with NaOH beads placed downstream from the gas-liquid separator to prevent residual aerosol and moisture transport to the atomizer was found to improve the response by 25%. Analytical figures of merit were comparable, reaching an identical sensitivity of 0.48 s ng (-1) As in both atomizers and limits of detection (LOD) of 0.15 ng mL(-1) As in MMQTA and 0.16 ng mL(-1) As in DBD, respectively. Compared to MMQTA, DBD provided 1 order of magnitude better resistance to interference from other hydride-forming elements (Sb, Se, and Bi). Atomization efficiency in DBD was estimated to be 100% of that reached in the MMQTA. A simple procedure of lossless in situ preconcentration of arsane was developed. Addition of 7 mL min(-1) O2 to the Ar plasma discharge resulted in a quantitative retention of arsane in the optical arm of the DBD atomizer. Complete analyte release and atomization was reached as soon as oxygen was switched off. Preconcentration efficiency of 100% was observed, allowing a decrease of the LOD to 0.01 ng mL(-1) As employing a 300 s preconcentration period. PMID:27159266

  18. Method of trivalent chromium concentration determination by atomic spectrometry

    Science.gov (United States)

    Reheulishvili, Aleksandre N.; Tsibakhashvili, Neli Ya.

    2006-12-12

    A method is disclosed for determining the concentration of trivalent chromium Cr(III) in a sample. The addition of perchloric acid has been found to increase the atomic chromium spectrometric signal due to Cr(III), while leaving the signal due to hexavalent chromium Cr(VI) unchanged. This enables determination of the Cr(III) concentration without pre-concentration or pre-separation from chromium of other valences. The Cr(III) concentration may be measured using atomic absorption spectrometry, atomic emission spectrometry or atomic fluorescence spectrometry.

  19. New Directions and Capabilities in Analytical Spectrometry

    Institute of Scientific and Technical Information of China (English)

    Gary M. HIEFTJE; Timothy L. DANIELSON; Andrew M. LEACH; Denise M. MCCLENATHAN; Radislav A. POTYRAILO; Steven J. RAY; Andrew W. SZUMLAS; Michael R. WEBB; William C. WETZEL

    2003-01-01

    In this presentation, a number of recent activities in our research group will be highlighted. The studies represent a broad range in the general field of spectrochemical analysis, sometimes take entirely new directions, usually employ novel instrumentation, and all provide important new capabilities in analytical measurements.

  20. Analytical evaluation of atomic form factors: application to Rayleigh scattering

    CERN Document Server

    Safari, L; Amaro, P; Jänkälä, K; Fratini, F

    2014-01-01

    Atomic form factors are widely used for the characterization of targets and specimens, from crystallography to biology. By using recent mathematical results, here we derive an analytical expression for the atomic form factor within the independent particle model constructed from nonrelativistic screened hydrogenic wavefunctions. The range of validity of this analytical expression is checked by comparing the analytically obtained form factors with the ones obtained within the Hartee-Fock method. As an example, we apply our analytical expression for the atomic form factor to evaluate the differential cross section for Rayleigh scattering off neutral atoms.

  1. Analytical evaluation of atomic form factors: Application to Rayleigh scattering

    Energy Technology Data Exchange (ETDEWEB)

    Safari, L., E-mail: laleh.safari@ist.ac.at [IST Austria (Institute of Science and Technology Austria), Am Campus 1, 3400 Klosterneuburg (Austria); Department of Physics, University of Oulu, Box 3000, FI-90014 Oulu (Finland); Santos, J. P. [Laboratório de Instrumentação, Engenharia Biomédica e Física da Radiação (LIBPhys-UNL), Departamento de Física, Faculdade de Ciências e Tecnologia, FCT, Universidade Nova de Lisboa, 2829-516 Caparica (Portugal); Amaro, P. [Laboratório de Instrumentação, Engenharia Biomédica e Física da Radiação (LIBPhys-UNL), Departamento de Física, Faculdade de Ciências e Tecnologia, FCT, Universidade Nova de Lisboa, 2829-516 Caparica (Portugal); Physikalisches Institut, Universität Heidelberg, D-69120 Heidelberg (Germany); Jänkälä, K. [Department of Physics, University of Oulu, Box 3000, FI-90014 Oulu (Finland); Fratini, F. [Department of Physics, University of Oulu, Box 3000, FI-90014 Oulu (Finland); Institute of Atomic and Subatomic Physics, TU Wien, Stadionallee 2, 1020 Wien (Austria); Departamento de Física, Instituto de Ciências Exatas, Universidade Federal de Minas Gerais, 31270-901 Belo Horizonte, MG (Brazil)

    2015-05-15

    Atomic form factors are widely used for the characterization of targets and specimens, from crystallography to biology. By using recent mathematical results, here we derive an analytical expression for the atomic form factor within the independent particle model constructed from nonrelativistic screened hydrogenic wave functions. The range of validity of this analytical expression is checked by comparing the analytically obtained form factors with the ones obtained within the Hartee-Fock method. As an example, we apply our analytical expression for the atomic form factor to evaluate the differential cross section for Rayleigh scattering off neutral atoms.

  2. Miniaturized analytical systems for mass spectrometry-based protein studies

    OpenAIRE

    Abonnenc, Mélanie

    2009-01-01

    Current proteomic strategies depend strongly on the development of analytical methodologies and instrumentation. In parallel to the development of mass spectrometry (MS) - based proteomic workflows, microfluidic devices emerged in this field as a flexible tool for rapid and sensitive protein studies. In this context, the present work focuses on the development of miniaturized analytical systems for protein studies, especially by electrospray ionization mass spectrometric detection. Several ap...

  3. Analytical relativistic self-consistent-field calculations for atoms

    International Nuclear Information System (INIS)

    A new second-order representation of the Dirac equation is presented. This representation which is exact for a hydrogen atom is applied to approximate analytical self-consistent-field calculations for atoms. Results are given for the rare-gas atoms from helium to radon and for lead. The results compare favorably with numerical Dirac-Hartree-Fock solutions

  4. Determination of metal content in valerian root phytopharmaceutical derivatives by atomic spectrometry.

    Science.gov (United States)

    Arce, Silvia; Cerutti, Soledad; Olsina, Roberto; Gomez, María R; Martínez, Luis D

    2005-01-01

    Phytopharmaceuticals containing Valerian are used as mild sleep-inducing agents. The elemental composition of 3 different marks of Valeriana officinalis roots commercially available in the Argentinian market, their teas, and a commercial tincture have been studied. The content of Al, Ca, Cd, Co, Cr, Cu, Fe, Li, Mn, Ni, Pb, V, and Zn was determined in phytopharmaceuticals by flame atomic emission/absorption spectrometry, electrothermal atomic absorption spectrometry, and ultrasonic nebulization coupled to inductively coupled plasma-optical emission spectrometry. Prior to analyses of the samples, a digestion procedure was optimized. The analytical results obtained for Fe, Al, Ca, and V in the solid sample study were within the range 100-1000 mg/kg, and for Mn, Zn, and Pb within the range 10-100 mg/kg. Cadmium was found at levels up to 0.0125 mg/kg. PMID:15759744

  5. Atomic spectrometry methods for wine analysis: A critical evaluation and discussion of recent applications

    International Nuclear Information System (INIS)

    The analysis of wine is of great importance since wine components strongly determine its stability, organoleptic or nutrition characteristics. In addition, wine analysis is also important to prevent fraud and to assess toxicological issues. Among the different analytical techniques described in the literature, atomic spectrometry has been traditionally employed for elemental wine analysis due to its simplicity and good analytical figures of merit. The scope of this review is to summarize the main advantages and drawbacks of various atomic spectrometry techniques for elemental wine analysis. Special attention is paid to interferences (i.e. matrix effects) affecting the analysis as well as the strategies available to mitigate them. Finally, latest studies about wine speciation are briefly discussed.

  6. Atomic spectrometry methods for wine analysis: A critical evaluation and discussion of recent applications

    Energy Technology Data Exchange (ETDEWEB)

    Grindlay, Guillermo, E-mail: guillermo.grindlay@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences, University of Alicante, PO Box 99, 03080 Alicante (Spain); Mora, Juan; Gras, Luis [Department of Analytical Chemistry, Nutrition and Food Sciences, University of Alicante, PO Box 99, 03080 Alicante (Spain); Loos-Vollebregt, Margaretha T.C. de [Delft University of Technology, Faculty of Applied Sciences, Analytical Biotechnology, Julianalaan 67, 2628 BC Delft (Netherlands)

    2011-04-08

    The analysis of wine is of great importance since wine components strongly determine its stability, organoleptic or nutrition characteristics. In addition, wine analysis is also important to prevent fraud and to assess toxicological issues. Among the different analytical techniques described in the literature, atomic spectrometry has been traditionally employed for elemental wine analysis due to its simplicity and good analytical figures of merit. The scope of this review is to summarize the main advantages and drawbacks of various atomic spectrometry techniques for elemental wine analysis. Special attention is paid to interferences (i.e. matrix effects) affecting the analysis as well as the strategies available to mitigate them. Finally, latest studies about wine speciation are briefly discussed.

  7. Neutron activation spectrometry and neutron activation analysis in analytical geochemistry

    International Nuclear Information System (INIS)

    The present report is to show the geochemists who are interested in neutron activation spectrometry (NAS) and neutron activation analysis (NAA) which analytical possibilities these methods offer him. As a review of these analytical possibilities, a lieterature compolation is given which is subdivided into two groups: 1) rock (basic, intermediary, acid, sediments, soils and nuds, diverse minerals, tectites, meteorites and lunar material). 2) ore (Al, Au, Be, Cr, Cu, Mn, Mo, Fe, Pb, Pt, Sn, Ti, W, Zn, Zr, U and phosphate ore, polymetallic ores, fluorite, monazite and diverse ores). The applied methods as well as the determinable elements in the given materials can be got from the tables. On the whole, the literature evaluation carried out makes it clear that neutron activation spectrometry is a very useful multi-element method for the analysis of rocks. The analysis of ores, however, is subjected to great limitations. As rock analysis is very frequently of importance in prospecting for ore deposits, the NAS proves to be extremely useful for this very field of application. (orig./LH)

  8. Glass frit nebulizer for atomic spectrometry

    Science.gov (United States)

    Layman, L.R.

    1982-01-01

    The nebuilizatlon of sample solutions Is a critical step In most flame or plasma atomic spectrometrlc methods. A novel nebulzatlon technique, based on a porous glass frit, has been Investigated. Basic operating parameters and characteristics have been studied to determine how thte new nebulizer may be applied to atomic spectrometrlc methods. The results of preliminary comparisons with pneumatic nebulizers Indicate several notable differences. The frit nebulizer produces a smaller droplet size distribution and has a higher sample transport efficiency. The mean droplet size te approximately 0.1 ??m, and up to 94% of the sample te converted to usable aerosol. The most significant limitations In the performance of the frit nebulizer are the stow sample equMbratton time and the requirement for wash cycles between samples. Loss of solute by surface adsorption and contamination of samples by leaching from the glass were both found to be limitations only In unusual cases. This nebulizer shows great promise where sample volume te limited or where measurements require long nebullzatlon times.

  9. Analytic Solutions of Three-Level Dressed-Atom Model

    Institute of Scientific and Technical Information of China (English)

    WANG Zheng-Ling; YIN Jian-Ping

    2004-01-01

    On the basis of the dressed-atom model, the general analytic expressions for the eigenenergies, eigenstates and their optical potentials of the A-configuration three-level atom system are derived and analysed. From the calculation of dipole matrix element of different dressed states, we obtain the spontaneous-emission rates in the dressed-atom picture. We find that our general expressions of optical potentials for the three-level dressed atom can be reduced to the same as ones in previous references under the approximation of a small saturation parameter. We also analyse the dependences of the optical potentials of a three-level 85Rb atom on the laser detuning and the dependences of spontaneous-emission rates on the radial position in the dark hollow beam, and discuss the probability (population) evolutions of dressed-atomic eigenstates in three levels in the hollow beam.

  10. Development of an analytical model for the determination of {sup 60}Co in aqueous samples by atomic absorption and gamma spectrometry techniques; Elaboracion de un modelo analitico para la determinacion de {sup 60}Co en muestras acuosas mediante tecnicas de absorcion atomica y espectrometria gamma

    Energy Technology Data Exchange (ETDEWEB)

    Solis A, N. A.

    2015-07-01

    The applications of the nuclear energy in industry and medicine generate radioactive wastes that must be isolated and confined in order to limit its spread in the biosphere. These types of wastes are generated in hospitals, industry, research centers and nuclear power plants (during de fuel cycle). The radioactive elements (radionuclides) cannot be destroyed by any known method, either chemical or mechanical. Its final destruction is produced by radioactive decay, which makes them stable isotopes, or nuclear transmutation being bombarded with atomic particles. Consequently, the radioactive waste management is to control the radioactive discharges and reduce to tolerable limits, eliminating of effluents and wastes the radionuclides of interest, concentrating them so they can be stored or evacuated so that later not appear in dangerous concentration in the biosphere. In Mexico, the main generators of radioactive wastes are the nuclear power plant of Laguna Verde in Veracruz, Hospitals of the public and private sector, in addition Instituto Nacional de Investigaciones Nucleares (ININ) some institutes and facilities of the UNAM and Instituto Politecnico Nacional (IPN) and industries among others. The aqueous radioactive wastes, particularly those from the nuclear power plants contain traces of cobalt-60. Currently there is no model or analytical technique for the separation of this radionuclide, so it became necessary to develop an analytical model for separation and facilitate their disposal. In this paper was shown that atomic absorption and gamma spectrometry techniques can separate the active concentration of the inactive, which is important because the total concentration can be associated through direct relationships with the wear of metal parts of the nuclear reactor, since the metal alloys of the same reactor containing a fraction of cobalt. Also this analytical and mathematical model that can be reproducible and applicable to full sets of samples and that this

  11. Speciation of four selenium compounds using high performance liquid chromatography with on-line detection by inductively coupled plasma mass spectrometry or flame atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Pedersen, Gitte Alsing; Larsen, Erik Huusfeldt

    1997-01-01

    An analytical method for the speciation of selenomethionine, selenocystine, selenite and selenate by high performance liquid chromatography (HPLC) with atomic spectrometric detection is presented. An organic polymeric strong anion exchange column was used as the stationary phase in combination...... with an aqueous solution of 6 mmol L-1 of salicylate ion at pH 8.5 as the mobile phase which allowed the isocratic separation of the four selenium analytes within 8 minutes. The separated selenium species were detected on-line by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma mass...

  12. COMPARISON OF SECONDARY ION MASS SPECTROMETRY (SIMS) WITH ELECTRON MICROPROBE ANALYSIS (EPMA) AND OTHER THIN FILM ANALYTICAL METHODS

    OpenAIRE

    Werner, H.; Von Rosenstiel, A.

    1984-01-01

    Different modes of SIMS for thin film analysis and the principle of SIMS will be discussed; this will be followed by a discussion of some features related to instrumentation: types of ion sources and their characteristics ; ion microprobe versus ion microscope ; special modes of SIMS : sputter neutral mass spectrometry (SNMS) and fast atom bombardment. (FAB). The discussion of analytical features will include : element range, quantitative analysis, depth profiling, two-dimensional and three-d...

  13. Evaluation of quartz tubes as atomization cells for gold determination by thermospray flame furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    This work describes the development of a new analytical procedure able to determine gold by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) using nickel tubes (NiT) and quartz tubes (QT) as atomization cells. Experiments involving changes in the flow injection operational parameters, reagent concentrations and sizes of the QT were performed in order to optimize sensitivity. Under the same operational conditions, it was observed that the employment of QT increases the sensitivity of gold determination when compared to the nickel tube. Since solutions of highly concentrated hydrochloric acid showed the best performance as carriers, quartz tubes were also preferred due to its greater tolerance to corrosion by mineral acids in comparison to NiT. In addition, changes in the internal diameter of the QT revealed an important improvement in sensitivity for smaller tubes. Under optimized conditions the main figures of merit showed values close to that of graphite furnace atomic absorption spectrometry with the addition of an excellent improvement of the sample throughput. They are: LOD (3 s): 0.004 μg mL−1, sensitivity: 0.306 (μg mL−1)−1, RSD% (n = 10, 1 μg mL−1): 2.5, linear range: 0.01–4 μg mL−1 and sample throughput: 72 h−1. This new method was employed for the determination of gold in homeopathic medicines with no need of sample digestion. Validation of the analytical results will be shown. A full discussion of the most relevant findings regarding the role of the atomization cell as a strategic key for improving sensitivity will be also provided. - Highlights: ► Quartz tubes as furnaces in TS-FFAAS. ► Small tubes for controlling radial dispersion. ► Improved figures of merit for gold determination. ► Analysis of homeopathic medicines.

  14. Gas Atomization of Aluminium Melts: Comparison of Analytical Models

    Directory of Open Access Journals (Sweden)

    Georgios Antipas

    2012-06-01

    Full Text Available A number of analytical models predicting the size distribution of particles during atomization of Al-based alloys by N2, He and Ar gases were compared. Simulations of liquid break up in a close coupled atomizer revealed that the finer particles are located near the center of the spray cone. Increasing gas injection pressures led to an overall reduction of particle diameters and caused a migration of the larger powder particles towards the outer boundary of the flow. At sufficiently high gas pressures the spray became monodisperse. The models also indicated that there is a minimum achievable mean diameter for any melt/gas system.

  15. Ultratrace determination of tin by hydride generation in-atomizer trapping atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Průša, Libor [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Charles University in Prague, Faculty of Science, Department of Analytical Chemistry, Hlavova 8, Prague 2, CZ 128 43 Czech Republic (Czech Republic); Dědina, Jiří [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Kratzer, Jan, E-mail: jkratzer@biomed.cas.cz [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic)

    2013-12-04

    Graphical abstract: -- Highlights: •In-atomizer trapping HG-AAS was optimized for Sn. •A compact quartz trap-and-atomizer device was employed. •Generation, preconcentration and atomization steps were investigated in detail. •Hundred percent preconcentration efficiency for tin was reached. •Routine analytical method was developed for Sn determination (LOD of 0.03 ng mL{sup −1} Sn). -- Abstract: A quartz multiatomizer with its inlet arm modified to serve as a trap (trap-and-atomizer device) was employed to trap tin hydride and subsequently to volatilize collected analyte species with atomic absorption spectrometric detection. Generation, atomization and preconcentration conditions were optimized and analytical figures of merit of both on-line atomization as well as preconcentration modes were quantified. Preconcentration efficiency of 95 ± 5% was found. The detection limits reached were 0.029 and 0.14 ng mL{sup −1} Sn, respectively, for 120 s preconcentration period and on-line atomization mode without any preconcentration. The interference extent of other hydride forming elements (As, Se, Sb and Bi) on tin determination was found negligible in both modes of operation. The applicability of the developed preconcentration method was verified by Sn determination in a certified reference material as well as by analysis of real samples.

  16. Gold volatile species atomization and preconcentration in quartz devices for atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The on-line atomization of gold volatile species was studied and the results were compared with thermodynamic calculations in several quartz atomizers, namely: diffusion flame, flame-in-gas-shield, flame-in-plain-tube, externally heated T-tube and externally heated flame-in-T-tube. Atomization mechanism in the explored devices is proposed, where volatile species are converted to thermodynamically stable AuH at elevated temperature over 500 °C and then atomized by an interaction with a cloud of hydrogen radicals. Because of its inherent simplicity and robustness, diffusion flame was employed as a reference atomizer. It yielded atomization efficiency of 70 to 100% and a very good long time reproducibility of peak area sensitivity: 1.6 to 1.8 s μg−1. Six and eleven times higher sensitivity, respectively, was provided by atomizers with longer light paths in the observation volume, i.e. externally heated T-tube and externally heated flame-in-T-tube. The latter one, offering limit of detection below 0.01 μg ml−1, appeared as the most prospective for on-line atomization. Insight into the mechanism of atomization of gold volatile species, into the fate of free atoms and into subsequent analyte transfer allowed to assess possibilities of in-atomizer preconcentration of gold volatile species: it is unfeasible with quartz atomizers but a sapphire tube atomizer could be useful in this respect. - Highlights: • On-line atomization of gold volatile species for AAS in quartz devices was studied. • Atomization mechanism was proposed and atomization efficiency was estimated. • Possibilities of in-atomizer preconcentration of gold volatile species were assessed

  17. Gold volatile species atomization and preconcentration in quartz devices for atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Arslan, Yasin [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Mehmet Akif Ersoy University, Faculty of Arts & Sciences, Chemistry Department, 15030 Burdur (Turkey); Musil, Stanislav; Matoušek, Tomáš; Kratzer, Jan [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Dědina, Jiří, E-mail: dedina@biomed.cas.cz [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic)

    2015-01-01

    The on-line atomization of gold volatile species was studied and the results were compared with thermodynamic calculations in several quartz atomizers, namely: diffusion flame, flame-in-gas-shield, flame-in-plain-tube, externally heated T-tube and externally heated flame-in-T-tube. Atomization mechanism in the explored devices is proposed, where volatile species are converted to thermodynamically stable AuH at elevated temperature over 500 °C and then atomized by an interaction with a cloud of hydrogen radicals. Because of its inherent simplicity and robustness, diffusion flame was employed as a reference atomizer. It yielded atomization efficiency of 70 to 100% and a very good long time reproducibility of peak area sensitivity: 1.6 to 1.8 s μg{sup −1}. Six and eleven times higher sensitivity, respectively, was provided by atomizers with longer light paths in the observation volume, i.e. externally heated T-tube and externally heated flame-in-T-tube. The latter one, offering limit of detection below 0.01 μg ml{sup −1}, appeared as the most prospective for on-line atomization. Insight into the mechanism of atomization of gold volatile species, into the fate of free atoms and into subsequent analyte transfer allowed to assess possibilities of in-atomizer preconcentration of gold volatile species: it is unfeasible with quartz atomizers but a sapphire tube atomizer could be useful in this respect. - Highlights: • On-line atomization of gold volatile species for AAS in quartz devices was studied. • Atomization mechanism was proposed and atomization efficiency was estimated. • Possibilities of in-atomizer preconcentration of gold volatile species were assessed.

  18. Determination of cadmium in rice and water by tungsten coil electrothermal vaporization-atomic fluorescence spectrometry and tungsten coil electrothermal atomic absorption spectrometry after cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Wen Xiaodong [College of Chemistry, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Wu Peng [Analytical and Testing Center, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Chen Li [College of Chemistry, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Hou Xiandeng, E-mail: houxd@scu.edu.cn [College of Chemistry, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Analytical and Testing Center, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China)

    2009-09-14

    In this work, the microsampling nature of tungsten coil electrothermal vaporization Ar/H{sub 2} flame atomic fluorescence spectrometry (W-coil ETV-AFS) as well as tungsten coil electrothermal atomic absorption spectrometry (W-coil ET-AAS) was used with cloud point extraction (CPE) for the ultrasensitive determination of cadmium in rice and water samples. When the temperature of the extraction system is higher than the cloud point temperature of the selected surfactant Triton X-114, the complex of cadmium with dithizone can be quantitatively extracted into the surfactant-rich phase and subsequently separated from the bulk aqueous phase by centrifugation. The main factors affecting the CPE, such as concentration of Triton X-114 and dithizone, pH, equilibration temperature and incubation time, were optimized for the best extract efficiency. Under the optimal conditions, the limits of detection for cadmium by W-coil ETV-AFS and W-coil ET-AAS were 0.01 and 0.03 {mu}g L{sup -1}, with sensitivity enhancement factors of 152 and 93, respectively. The proposed methods were applied to the determination of cadmium in certified reference rice and water samples with analytical results in good agreement with certified values.

  19. Simultaneous Atomic Absorption Spectrometry for Cadmium and Lead Determination in Wastewater: A Laboratory Exercise

    Science.gov (United States)

    Correia, Paulo R. M.; Oliveira, Pedro V.

    2004-01-01

    The simultaneous determination of cadmium and lead by multi-element atomic absorption spectrometry with electrochemical atomization is proposed by employing a problem-based approach. The reports indicate that the students assimilated the principles of the simultaneous atomic absorption spectrometry (SIMAAS), the role of the chemical modifier, the…

  20. Determination of tellurium by hydride generation with in situ trapping flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Matusiewicz, H.; Krawczyk, M. [Politechn Poznanska, Poznan (Poland)

    2007-03-15

    The analytical performance of coupled hydride generation - integrated atom trap (HG-IAT) atomizer flame atomic absorption spectrometry (FAAS) system was evaluated for determination of Te in reference material (GBW 07302 Stream Sediment), coal fly ash and garlic. Tellurium, using formation of H{sub 2}Te vapors, is atomized in air-acetylene flame-heated IAT. A new design HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangernents (a water-cooled single silica tube, double-slotted quartz tube or an 'integrated trap') was investigated. An improvement in detection limit was achieved compared with using either of the above atom trapping techniques separately. The concentration detection limit, defined as 3 times the blank standard deviation (3{sigma}), was 0.9 ng mL{sup -1} for Te. For a 2 min in situ preconcentration time (sample volume of 2 mL), sensitivity enhancement compared to flame AAS, was 222 fold, using the hydride generation atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed as RSD, was 7.0% (n = 6) for Te. The accuracy of the method was verified using a certified reference material (GBW 07302 Stream Sediment) by aqueous standard calibration curves. The measured Te contents of the reference material was in agreement with the information value. The method was successfully applied to the determination of tellurium in coal fly ash and garlic.

  1. Cadmium, copper, lead, and zinc determination in precipitation: A comparison of inductively coupled plasma atomic emission spectrometry and graphite furnace atomization atomic absorption spectrometry

    Science.gov (United States)

    Reddy, M.M.; Benefiel, M.A.; Claassen, H.C.

    1987-01-01

    Selected trace element analysis for cadmium, copper, lead, and zinc in precipitation samples by inductively coupled plasma atomic emission Spectrometry (ICP) and by atomic absorption spectrometry with graphite furnace atomization (AAGF) have been evaluated. This task was conducted in conjunction with a longterm study of precipitation chemistry at high altitude sites located in remote areas of the southwestern United States. Coefficients of variation and recovery values were determined for a standard reference water sample for all metals examined for both techniques. At concentration levels less than 10 micrograms per liter AAGF analyses exhibited better precision and accuracy than ICP. Both methods appear to offer the potential for cost-effective analysis of trace metal ions in precipitation. ?? 1987 Springer-Verlag.

  2. Organic solvents as interferents in arsenic determination by hydride generation atomic absorption spectrometry with flame atomization

    Science.gov (United States)

    Karadjova, Irina B.; Lampugnani, Leonardo; Dědina, Jiri; D'Ulivo, Alessandro; Onor, Massimo; Tsalev, Dimiter L.

    2006-05-01

    Interference effects of various organic solvents miscible with water on arsenic determination by hydride generation atomic absorption spectrometry have been studied. Arsine was chemically generated in continuous flow hydride generation system and atomized by using a flame atomizer able to operate in two modes: miniature diffusion flame and flame-in-flame. The effects of experimental variables and atomization mode were investigated: tetrahydroborate and hydrochloric acid concentrations, argon, hydrogen and oxygen supply rates for the microflame, and the distance from the atomization region to the observation zone. The nature of the species formed in the flame due to the pyrolysis of organic solvent vapors entering the flame volume together with arsine is discussed. The observed signal depression in the presence of organic solvents has been mainly attributed to the atomization interference due to heterogeneous gas-solid reaction between the free arsenic atoms and finely dispersed carbon particles formed by carbon radicals recombination. The best tolerance to interferences was obtained by using flame-in-flame atomization (5-10 ml min - 1 of oxygen flow rate), together with higher argon and hydrogen supply rates and elevated observation heights.

  3. The Kalman filter approach to inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Van Veen, E. H.; Bosch, S.; De Loos-Vollebregt, M. T. C.

    1994-07-01

    This article is an electronic publication in Spectrochimica Acta Electronica (SAE), the electronic section of Spectrochimica Acta Part B (SAB). The hardcopy text, comprising the main article and two appendices, is accompanied by a disk containing the compiled program, a reference manual and data files. The work deals with data handling in inductively coupled plasma atomic emission spectrometry (ICP-AES). With this technique, the analyte signal is superimposed on a background signal. When separating the signals by manual or automated three-point background correction, there are many instances in which the data reduction fails. Based on scans recorded in a fast-scanning mode and on a library of pure-component scans, the Kaiman filter approach models the emission in the spectral window (about 100 pm) of the analyte and mathematically solves the problem of background correction. By using a criterion-based algorithm to correct for optical instability, the uncertainty in the determination of the interferent line signal is eliminated. Therefore, the present filter implementation yields more accurate and precise results, especially in the case of line overlap. The Kalman filter Approach to Atomic Spectrometry (KAAS) software automatically processes Perkin-Elmer Plasma 1000/2000 text files, but can also handle ASCII data files. Practical and comprehensive examples are given to evoke the "Kalman filter feeling" in the crucial step of creating the emission model.

  4. The direct determination of HgS by thermal desorption coupled with atomic absorption spectrometry

    Science.gov (United States)

    Coufalík, Pavel; Zvěřina, Ondřej; Komárek, Josef

    2016-04-01

    This research was aimed at the direct determination of HgS in environmental samples by means of thermal desorption coupled with atomic absorption spectrometry. Operating parameters of the apparatus used for thermal desorption (including a prototype desorption unit) are described in this work, as well as the procedure for measuring mercury release curves together with an evaluation of the analytical signal including two methods of peak integration. The results of thermal desorption were compared with HgS contents obtained by sequential extraction. The limits of quantification of the proposed method for the selective determination of the black and red forms of HgS were 4 μg kg- 1 and 5 μg kg- 1, respectively. The limit of quantification of red HgS in soils was 35 μg kg- 1. The developed analytical procedure was applied to soil and sediment samples from historical mining areas.

  5. Determination of Arsenic in Palm Kernel Expeller using Microwave Digestion and Graphite Furnace Atomic Absorption Spectrometry Method

    OpenAIRE

    Abdul Niefaizal Abdul Hammid; Ainie Kuntom; RazaIi Ismail; Norazilah Pardi

    2013-01-01

    A study on the method to determine arsenic in palm kernel expeller wascarried out. Microwave digestion technique is widely applied in the analytical chemistry field. In comparison to conventional sample digestion method, the microwave technique is simple, reduced contamination, usage of safe reagent and matrix completely digested. A graphite furnace atomic absorption spectrometry method was used for the total determination of arsenic in palm kernel expeller. Arsenic was extracted from palm ke...

  6. Development of an automated sequential injection on-line solvent extraction-back extraction procedure as demonstrated for the determination of cadmium with detection by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2002-01-01

    An automated sequential injection (SI) on-line solvent extraction-back extraction separation/preconcentration procedure is described. Demonstrated for the assay of cadmium by electrothermal atomic absorption spectrometry (ETAAS), the analyte is initially complexed with ammonium...

  7. Bibliometric mapping: eight decades of analytical chemistry, with special focus on the use of mass spectrometry.

    Science.gov (United States)

    Waaijer, Cathelijn J F; Palmblad, Magnus

    2015-01-01

    In this Feature we use automatic bibliometric mapping tools to visualize the history of analytical chemistry from the 1920s until the present. In particular, we have focused on the application of mass spectrometry in different fields. The analysis shows major shifts in research focus and use of mass spectrometry. We conclude by discussing the application of bibliometric mapping and visualization tools in analytical chemists' research.

  8. A comparative study of inductively coupled plasma optical emission spectrometry and microwave plasma atomic emission spectrometry for the direct determination of lanthanides in water and environmental samples

    International Nuclear Information System (INIS)

    A new instrumental technique – Microwave Plasma Atomic Emission Spectrometry (MP - AES) is compared to conventional Inductively Coupled Plasma Optical Emission Spectrometry (ICP - OES) for direct determination of lanthanides. Estimation of both methods is done using standard measurement conditions. The present study includes spectral and non- spectral matrix effect evaluation. Tested analytical wavelengths of lanthanides are divided into three groups: 1) relatively free, 2) interfered by other lanthanides and 3) interfered by concomitant elements. Non spectral effect on analytes is examined in two typical real matrices – acidic plant digests and saline water. The capabilities of both plasma methods for quantitative determination of La, Ce, Sm, Eu, Gd and Er are compared. The interference - free emission lines are selected; appropriate background correction is proposed and the corresponding instrumental detection limits are calculated. Key words: lanthanides, ICP -OES, MP -AES, spectral and non-spectral interference

  9. Cloud point extraction thermospray flame quartz furnace atomic absorption spectrometry for determination of ultratrace cadmium in water and urine

    Science.gov (United States)

    Wu, Peng; Zhang, Yunchang; Lv, Yi; Hou, Xiandeng

    2006-12-01

    A simple, low cost and highly sensitive method based on cloud point extraction (CPE) for separation/preconcentration and thermospray flame quartz furnace atomic absorption spectrometry was proposed for the determination of ultratrace cadmium in water and urine samples. The analytical procedure involved the formation of analyte-entrapped surfactant micelles by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution and a Triton X-114 solution. When the temperature of the system was higher than the cloud point of Triton X-114, the complex of cadmium-PDC entered the surfactant-rich phase and thus separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, the limit of detection was 0.04 μg/L for cadmium with a sample volume of 10 mL. The analytical results of cadmium in water and urine samples agreed well with those by ICP-MS.

  10. Cloud point extraction-thermospray flame quartz furnace atomic absorption spectrometry for determination of ultratrace cadmium in water and urine

    Energy Technology Data Exchange (ETDEWEB)

    Wu Peng [Analytical and Testing Center, Sichuan University, Chengdu, Sichuan 610064 (China); Zhang Yunchang [College of Chemistry, Sichuan University, Chengdu, Sichuan 610064 (China); Lv Yi [College of Chemistry, Sichuan University, Chengdu, Sichuan 610064 (China); Hou Xiandeng [Analytical and Testing Center, Sichuan University, Chengdu, Sichuan 610064 (China) and College of Chemistry, Sichuan University, Chengdu, Sichuan 610064 (China)]. E-mail: houxd@scu.edu.cn

    2006-12-15

    A simple, low cost and highly sensitive method based on cloud point extraction (CPE) for separation/preconcentration and thermospray flame quartz furnace atomic absorption spectrometry was proposed for the determination of ultratrace cadmium in water and urine samples. The analytical procedure involved the formation of analyte-entrapped surfactant micelles by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution and a Triton X-114 solution. When the temperature of the system was higher than the cloud point of Triton X-114, the complex of cadmium-PDC entered the surfactant-rich phase and thus separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, the limit of detection was 0.04 {mu}g/L for cadmium with a sample volume of 10 mL. The analytical results of cadmium in water and urine samples agreed well with those by ICP-MS.

  11. Evaluation of quartz tubes as atomization cells for gold determination by thermospray flame furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Morzan, Ezequiel; Piano, Ornela; Stripeikis, Jorge; Tudino, Mabel, E-mail: tudino@qi.fcen.uba.ar

    2012-11-15

    This work describes the development of a new analytical procedure able to determine gold by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) using nickel tubes (NiT) and quartz tubes (QT) as atomization cells. Experiments involving changes in the flow injection operational parameters, reagent concentrations and sizes of the QT were performed in order to optimize sensitivity. Under the same operational conditions, it was observed that the employment of QT increases the sensitivity of gold determination when compared to the nickel tube. Since solutions of highly concentrated hydrochloric acid showed the best performance as carriers, quartz tubes were also preferred due to its greater tolerance to corrosion by mineral acids in comparison to NiT. In addition, changes in the internal diameter of the QT revealed an important improvement in sensitivity for smaller tubes. Under optimized conditions the main figures of merit showed values close to that of graphite furnace atomic absorption spectrometry with the addition of an excellent improvement of the sample throughput. They are: LOD (3 s): 0.004 {mu}g mL{sup -1}, sensitivity: 0.306 ({mu}g mL{sup -1}){sup -1}, RSD% (n = 10, 1 {mu}g mL{sup -1}): 2.5, linear range: 0.01-4 {mu}g mL{sup -1} and sample throughput: 72 h{sup -1}. This new method was employed for the determination of gold in homeopathic medicines with no need of sample digestion. Validation of the analytical results will be shown. A full discussion of the most relevant findings regarding the role of the atomization cell as a strategic key for improving sensitivity will be also provided. - Highlights: Black-Right-Pointing-Pointer Quartz tubes as furnaces in TS-FFAAS. Black-Right-Pointing-Pointer Small tubes for controlling radial dispersion. Black-Right-Pointing-Pointer Improved figures of merit for gold determination. Black-Right-Pointing-Pointer Analysis of homeopathic medicines.

  12. Quantitative determination of impurities in nuclear grade aluminum by Flame-Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    The paper deals with quantitative determination of impurity elements in nuclear grade aluminum, used as fin tubes in research reactors, by Flame-Atomic Absorption Spectrometry (F-AAS). The results have been compared with those obtained by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) method. Experimental conditions used in both the methods are given in the paper. (author)

  13. Study on the application of cold vapor atomic absorption spectrometry and hydride generation atomic absorption spectrometry for the determination of Hg and As traces in sea water samples

    International Nuclear Information System (INIS)

    The trace amount of total mercury (Hg) and arsenic (As) in sea water samples were quantitatively determined by using the Atomic Absorption Spectrometry connected with the hydride generation technique (HG-AAS) for As, and with the cold vapour technique (CV-AAS) for Hg. The experiments were carried out at room temperature on a Hydride System Module (HS55) combined with an Atomic Absorption Spectrometer (VARIO 6, Analytik Jena AG). The effect of reductants concentration, and that of matrix on the absorption intensity of each analyzed element was studied in details. The sea water sample after fitrating through a membrane with 0.45(μm-hole size was pre-treated with an oxidant or an reductant to obtain the identical medium. The absorption intensity of each element was then measured on the VARIO-6 under the optimum parameters for spectrometer such as: maximum wavelength, current of hollow cathode lamp, and that for hydride system such as cell temperature, speed of peristaltic pump, pump time, reaction time and rewash time, ect. The analytical procedures were set-up and applied for the determination of these above mentioned elements in the synthesized sea water sample and in the real sea water samples with high precision and accuracy. (author)

  14. Advances in metallomics by atomic and molecular spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. The scope of research in the field of elemental speciation has considerably evolved during the last decade. The analysis of specific metal-containing contaminants reached the maturity and has given way to the development of analytical methods to describe interactions of metals with biomolecules which are constituents of the genome, proteome, metabolome and other -omes in a cell, tissue or organism. The entirety of metal-biomolecule species has been termed the 'metallome' which gave rise to an emerging discipline: metallomics. Advances of trace element analysis in life sciences resulted in the proliferation of new terms related to the description of metal-interactions with biomolecules, such as, e.g. ionome, metalloproteome, metallogenome, metallometabolome, heteroatom-tagged proteome, single element proteomes (e.g., selenoproteome) and the corresponding -omics. The analytical chemistry challenges in the area metallomics include the detection, quantification, identification and characterization of complexes of metals (metalloids) at trace levels in an environment rich in biomolecules often having similar physicochemical properties. In the past, the only way to access to this information was modelling using stability constants. Today, hyphenated techniques based on the coupling of a high resolution separation technique with sensitive elemental (ICP MS) and molecular (ES MS/MS) mass spectrometry offer the possibility of high-throughput acquisition of metallomics information in many biological systems. The lecture discusses advances in analytical techniques in the field of metallomics. Particular attention will be to developments in multidimensional nanoHPLC with the parallel ICP MS and ESI MS detection and the sensitive spotting of heteroelement-containing proteins in 2D gels, accompanied by advances in MALDI TOF MS. Potential for medical research (e.g., characterization for selenoproteins as new biomarkers of clinical utility

  15. Atomic force microscopy fishing and mass spectrometry identification of gp120 on immobilized aptamers

    Directory of Open Access Journals (Sweden)

    Ivanov YD

    2014-10-01

    Full Text Available Yuri D Ivanov,1 Natalia S Bukharina,1 Tatyana O Pleshakova,1 Pavel A Frantsuzov,1 Elena Yu Andreeva,1 Anna L Kaysheva,1,2 Victor G Zgoda,1 Alexander A Izotov,1 Tatyana I Pavlova,1 Vadim S Ziborov,1 Sergey P Radko,1 Sergei A Moshkovskii,1 Alexander I Archakov1 1Department of Personalized Medicine, Orekhovich Institute of Biomedical Chemistry of the Russian Academy of Medical Sciences, Moscow, Russia; 2PostgenTech Ltd., Moscow, Russia Abstract: Atomic force microscopy (AFM was applied to carry out direct and label-free detection of gp120 human immunodeficiency virus type 1 envelope glycoprotein as a target protein. This approach was based on the AFM fishing of gp120 from the analyte solution using anti-gp120 aptamers immobilized on the AFM chip to count gp120/aptamer complexes that were formed on the chip surface. The comparison of image contrasts of fished gp120 against the background of immobilized aptamers and anti-gp120 antibodies on the AFM images was conducted. It was shown that an image contrast of the protein/aptamer complexes was two-fold higher than the contrast of the protein/antibody complexes. Mass spectrometry identification provided an additional confirmation of the target protein presence on the AFM chips after biospecific fishing to avoid any artifacts. Keywords: gp120 HIV-1 envelope glycoprotein, aptamer, atomic force microscopy, mass spectrometry

  16. Study on the GaAs(110) surface using emitted atom spectrometry

    International Nuclear Information System (INIS)

    The facilities implemented at Bariloche for the ion scattering spectrometry is described, and recent examples of the technique application to determine the atomic structure and the composition of metallic and semiconductor surfaces, pure and with different adsorbates. The surface analysis technique using emitted atom spectrometry is discussed. The sensitivity to the GaAs(110) surface atomic relaxation is presented, and the kinetic of hydrogen adsorption by the mentioned surface is studied

  17. Cloud point extraction for the determination of copper in environmental samples by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Ardeshir Shokrollahi

    2008-01-01

    Full Text Available A simple cloud point extraction procedure is presented for the preconcentration of copper in various samples. After complexation by 4-hydroxy-2-mercapto-6-propylpyrimidine (PTU, copper ions are quantitatively extracted into the phase rich in Triton X-114 after centrifugation. Methanol acidified with 0.5 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS. Analytical parameters including concentrations for PTU, Triton X-114 and HNO3, bath temperature, centrifugation rate and time were optimized. The influences of the matrix ions on the recoveries of copper ions were investigated. The detection limits (3SDb/m, n=4 of 1.6 ng mL-1 along with enrichment factors of 30 for Cu were achieved. The proposed procedure was applied to the analysis of environmental samples.

  18. Preconcentration of Vanadium(Ⅴ) on Crosslinked Chitosan and Determination by Graphite Furnace Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by CCTS was 97% at pH 4.0, and vanadium(Ⅴ) was eluted from crosslinked chitosan with 2 mL 2.0 mol*L-1 chlorhydric acid and determined by GFAAS. The detection limit (3σ,n=7) for vanadium(Ⅴ) was 4.8×1 0-12g and the relative standard deviation (R.S.D) at concentration level of 2.6 μg*L-1 is less than 3.6%. The method shows a good selectivity and high sensitivity, and it was applied to determination of vanadium(Ⅴ) in oyster and water samples. The analytic recoveries are (97±5)%.

  19. Determination of molybdenum in silicates through atomic absorption spectrometry using pre-concentration by active carbon

    International Nuclear Information System (INIS)

    An analytical procedure for molybdenum determination in geological materials through Atomic Absorption Spectrometry, after pre-concentration of the Mo-APDC complex in activated carbon, has been developed, which is needed in order to reduce the dilution effect in the sample decomposition. During the development of this method the influence of pH, the amount of APDC for complexation of Mo and the interference of Fe, Ca, Mn, Al, K, Na, Mg and Ti were tested. It was shown that none of these causes any significant effect on the Mo determination proposed. The results of the analysis at the international geochemical reference samples JB-1 (basalt) and GH (granite) were very accurate and showed that the detection limit in rocks (1,00g) is 0,6 ppm, when using sample dilution of 1 ml and microinjection techniques. (author)

  20. Speciation of arsenic(III)/arsenic(V) and selenium(IV)/ selenium(VI) using coupled ion chromatography - hydride generation atomic absorption spectrometry

    Science.gov (United States)

    Simple analytical methods have been developed to speciate inorganic arsenic and selenium in the ppb range using coupled ion chromatography-hydride generation atomic absorption spectrometry. Because of the differences in toxicity and adsorption behavior, determinations of the redox states arsenite A...

  1. Low-resolution continuum source simultaneous multi-element electrothermal atomic absorption spectrometry: steps into practice

    International Nuclear Information System (INIS)

    The theory and practical problems of continuum source simultaneous multi-element electrothermal atomic absorption spectrometry (SMET AAS) are discussed by the example of direct analysis of underground water. The experimental methodology is based on pulse vaporization of the sample in a fast heated graphite tube and measurement of transient absorption of continuum spectrum radiation from D2 and Xe lamps within 200–400 nm wavelengths range with a low resolution spectral instrument and linear charge-coupled device. The setup permits the acquisition of 200 spectra during 1 s atomization pulse. Respective data matrix absorbance vs wavelength/time is employed for the quantification of elements in the sample. The calculation algorithm developed includes broad band and continuum background correction, linearization of function absorbance vs. concentration of atomic vapor and integration of thus modified absorbance at the resonance lines of the elements to be determined. Practical application shows that the method can be employed for the direct simultaneous determination of about 20 elements above microgram per liter level within 3–5 orders of the magnitude concentration range. The investigated sources of measurement errors are mainly associated with the atomization and vapor transportation problems, which are aggravated for the simultaneous release of major and minor sample constituents. Respective corrections concerning the selection of analytical lines, optimal sampling volume, matrix modification and cleaning of the atomizer have been introduced in the SMET AAS analytical technology. Under the optimized experimental conditions the calibration curves in Log-Log coordinates for all the investigated analytes in the single or multi-element reference solutions are approximated by the first order equations. The use of these equations as permanent characteristics of the setup enables instant quantification of Al, Ca, Co, Cr, Cu, Fe, Mg, Mn and Ni in the underground water

  2. Low-resolution continuum source simultaneous multi-element electrothermal atomic absorption spectrometry: steps into practice

    Energy Technology Data Exchange (ETDEWEB)

    Katskov, Dmitri, E-mail: katskovda@tut.ac.za

    2015-03-01

    The theory and practical problems of continuum source simultaneous multi-element electrothermal atomic absorption spectrometry (SMET AAS) are discussed by the example of direct analysis of underground water. The experimental methodology is based on pulse vaporization of the sample in a fast heated graphite tube and measurement of transient absorption of continuum spectrum radiation from D{sub 2} and Xe lamps within 200–400 nm wavelengths range with a low resolution spectral instrument and linear charge-coupled device. The setup permits the acquisition of 200 spectra during 1 s atomization pulse. Respective data matrix absorbance vs wavelength/time is employed for the quantification of elements in the sample. The calculation algorithm developed includes broad band and continuum background correction, linearization of function absorbance vs. concentration of atomic vapor and integration of thus modified absorbance at the resonance lines of the elements to be determined. Practical application shows that the method can be employed for the direct simultaneous determination of about 20 elements above microgram per liter level within 3–5 orders of the magnitude concentration range. The investigated sources of measurement errors are mainly associated with the atomization and vapor transportation problems, which are aggravated for the simultaneous release of major and minor sample constituents. Respective corrections concerning the selection of analytical lines, optimal sampling volume, matrix modification and cleaning of the atomizer have been introduced in the SMET AAS analytical technology. Under the optimized experimental conditions the calibration curves in Log-Log coordinates for all the investigated analytes in the single or multi-element reference solutions are approximated by the first order equations. The use of these equations as permanent characteristics of the setup enables instant quantification of Al, Ca, Co, Cr, Cu, Fe, Mg, Mn and Ni in the underground

  3. In situ atom trapping of Bi on W-coated slotted quartz tube flame atomic absorption spectrometry and interference studies

    Energy Technology Data Exchange (ETDEWEB)

    Kılınç, Ersin, E-mail: kilincersin@gmail.com [Medical Laboratory Techniques, Vocational Higher School of Healthcare Studies, Mardin Artuklu University, 47200 Mardin (Turkey); Bakırdere, Sezgin [Yıldız Technical University, Art and Science Faculy, Department of Chemistry, Esenler, TR 34220 İstanbul (Turkey); Aydın, Fırat [Dicle University, Faculty of Science, Department of Chemistry, Laboratory of Chemical Analysis, TR 21280 Diyarbakır (Turkey); Ataman, O. Yavuz [Middle East Technical University, Faculty of Arts and Sciences, Department of Chemistry, 06800 Ankara (Turkey)

    2013-11-01

    Analytical performances of metal coated slotted quartz tube flame atomic absorption spectrometry (SQT-FAAS) and slotted quartz tube in situ atom trapping flame atomic absorption spectrometry (SQT-AT-FAAS) systems were evaluated for determination of Bi. Non-volatile elements such as Mo, Zr, W and Ta were tried as coating materials. It was observed that W-coated SQT gave the best sensitivity for the determination of Bi for SQT-FAAS and SQT-AT-FAAS. The parameters for W-coated SQT-FAAS and W-coated SQT-AT-FAAS were optimized. Sensitivity of FAAS for Bi was improved as 4.0 fold by W-coated SQT-FAAS while 613 fold enhancement in sensitivity was achieved by W-coated SQT-AT-FAAS using 5.0 min trapping with respect to conventional FAAS. MIBK was selected as organic solvent for the re-atomization of Bi from the trapping surface. Limit of detection values for W-coated SQT-FAAS and W-coated SQT-AT-FAAS was obtained as 0.14 μg mL{sup −1} and 0.51 ng mL{sup −1}, respectively. Linear calibration plot was obtained in the range of 2.5–25.0 ng mL{sup −1} for W-coated SQT-AT-FAAS. Accuracy of the W-coated SQT-AT-FAAS system was checked by analyzing a standard reference material, NIST 1643e. - Highlights: • Further increasing in sensitivity of SQT-AT-FAAS was obtained by using a W coated SQT. • 613 fold sensitivity enhancement was achieved by W coated SQT-AT-FAAS versus FAAS. • A sensitive, rapid and simple technique for Bi was developed with an LOD of 0.51 ng mL{sup −1}. • The technique is suggested for laboratories equipped with only a flame AA spectrometer.

  4. Chlorine Analysis by Diode Laser Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    Joachim Koch; Aleksandr Zybin; Kay Niemax

    2000-01-01

    The general characteristics of Diode Laser Absorption Spectrometry (DLAAS) in low pressure plasmas particulary with respect to the detection of non-metals are comprehensively recapitulated and discussed. Furthermore, a detector, which is based on DLAAS in a microwave-induced low pressure plasma as an alternative technique for halogene-specific analysis of volatile compounds and polymeric matrices is described. The analytical capability of the technique is demonstrated on the chlorine-specific analysis of ablated polymer fragments as well as gas chromatographically separated hydrocarbons. Since the measurements were carried out by means of a balanced-heterodyne detection scheme, different technical noise contributions, such as laser excess and RAM noise could efficiently be suppressed and the registered absorption was limited only by the principal shot noise. Thus, in the case of the polymer analysis a chlorine-specific absolute detection limit of 10 pg could be achieved. Furthermore, fundamental investigations concerning the influence of hydrocarbons on the dissociation capability of the microwave induced plasma were performed. For this purpose, the carbon-, chlorine-and hydrogen-specific stoichiometry of the compounds were empirically determined. Deviations from the exspected proportions were found to be insignificant, implying the possibility of internal standardization relative to the response of a reference sample.

  5. Methods for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry

    Science.gov (United States)

    Chan, George C. Y.; Hieftje, Gary M.

    2010-08-03

    A method for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry (ICP-AES). ICP-AES analysis is performed across a plurality of selected locations in the plasma on an unknown sample, collecting the light intensity at one or more selected wavelengths of one or more sought-for analytes, creating a first dataset. The first dataset is then calibrated with a calibration dataset creating a calibrated first dataset curve. If the calibrated first dataset curve has a variability along the location within the plasma for a selected wavelength, errors are present. Plasma-related errors are then corrected by diluting the unknown sample and performing the same ICP-AES analysis on the diluted unknown sample creating a calibrated second dataset curve (accounting for the dilution) for the one or more sought-for analytes. The cross-over point of the calibrated dataset curves yields the corrected value (free from plasma related errors) for each sought-for analyte.

  6. Inductively coupled plasma--atomic emission spectrometry: trace elements in oil matrices

    Energy Technology Data Exchange (ETDEWEB)

    Peterson, C. A.

    1977-12-01

    The simultaneous determination of up to 20 trace elements in various oil matrices by inductively coupled plasma-atomic emission spectrometry is reported. The oil matrices investigated were lubricating oils (for wear metals), fuel oil, centrifuged coal liquefaction product, crude soybean oil, and commercial edible oils. The samples were diluted with appropriate organic solvents and injected into the plasma as an aerosol generated by a pneumatic nebulization technique. Detection limits of the 28 elements studied ranged from 0.0006 to 9 ..mu..g/g with the majority falling in the 0.01 to 0.1 ..mu..g/g range. Analytical calibration curves were linear over at least two orders of magnitude and for some elements this linearity extended over 4.5 orders of magnitude. Relevant data on precision and accuracy are included. Because metals often occur as particles in lubricating oil and coal liquefaction products, the effect of particles on the analytical results was examined. Wear metal particles in used oil did not appear to affect the analytical results. However, incomplete recovery relative to organometallic reference solutions was obtained for iron particles with a nominal mean diameter of 3.0 ..mu..m suspended in oil. It was shown that the following factors contributed to incomplete recovery for the particles: settling of the suspended particles in the flask, a difference in nebulization efficiency between particle suspensions and organometallic solutions, and indications of incomplete vaporization of the larger particles in the plasma.

  7. Temperature-controlled electrothermal atomization-atomic absorption spectrometry using a pyrometric feedback system in conjunction with a background monitoring device

    Science.gov (United States)

    Van Deijck, W.; Roelofsen, A. M.; Pieters, H. J.; Herber, R. F. M.

    The construction of a temperature-controlled feedback system for electrothermal atomization-atomic absorption spectrometry (ETA-AAS) using an optical pyrometer applied to the atomization stage is described. The system was used in conjunction with a fast-response background monitoring device. The heating rate of the furnace amounted to 1400° s -1 with a reproducibility better than 1%. The precision of the temperature control at a steady state temperature of 2000°C was 0.1%. The analytical improvements offered by the present system have been demonstrated by the determination of cadmium and lead in blood and finally by the determination of lead in serum. Both the sensitivity and the precision of the method have been improved. The accuracy of the method was checked by determining the lead content for a number of scrum samples both by ETA-AAS and differential pulse anodic stripping voltametry (DPASV) and proved to be satisfactory.

  8. Advances with tungsten coil atomizers: Continuum source atomic absorption and emission spectrometry

    International Nuclear Information System (INIS)

    Two new tungsten coil spectrometers are described: a continuum source tungsten coil atomic absorption spectrometer and a tungsten coil atomic emission spectrometer. Both devices use a 150 W tungsten coil extracted from a slide projector bulb. The power is provided by a computer-controlled, solid state, constant current 0-10 A supply. The heart of the optical system is a high-resolution spectrometer with a multi-channel detector. The continuum source system employs xenon or deuterium lamps, and is capable of multi-element analyses of complex samples like engine oil, urine, and polluted water. Spiked engine oil samples give mean percent recoveries of 98 ± 9, 104 ± 9, and 93 ± 0.8 for Al, V, and Ni, respectively. Copper, Zn, and Cd are determined in urine samples; while Cd, Co, Yb, and Sr are determined in water samples. Detection limits for Cd, Zn, Cu, Yb, Sr, and Co are: 8, 40, 1, 4, 1, and 4 μg l-1. The technique of tungsten coil atomic emission spectrometry using a 150 W commercial projector bulb is reported for the first time. Calcium, Ba, and Sr are determined with detection limits of 0.01, 0.5, and 0.1 μg l-1. Relative standard deviations are lower than 10% in each case, and Sr is determined in two water standard reference materials

  9. New analytical tools combining gel electrophoresis and mass spectrometry

    OpenAIRE

    Tobolkina, Elena

    2014-01-01

    Proteomics has been one of the main projects challenging biological and analytical chemists for many years. The separation, identification and quantification of all the proteins expressed within biological systems remain the main objectives of proteomics. Due to sample complexity, the development of fractionation, separation, purification and detection techniques that possess appropriate resolution to separate a large number of proteins, as well as being sensitive and fast enough for high thr...

  10. Mass spectrometry-based hepcidin measurements in serum and urine: analytical aspects and clinical implications.

    OpenAIRE

    Kemna, E.; Tjalsma, H.; Podust, V N; Swinkels, D. W.

    2007-01-01

    BACKGROUND: Discovery of the central role of hepcidin in body iron regulation has shed new light on the pathophysiology of iron disorders. Information is lacking on newer analytical approaches to measure hepcidin in serum and urine. Recent reports on the measurement of urine and serum hepcidin by surface-enhanced laser-desorption/ionization time-of-flight mass spectrometry (SELDI-TOF MS) necessitate analytical and clinical evaluation of MS-based methodologies. METHODS: We used SELDI-TOF MS, i...

  11. Determination of daily intake of elements from Philippine total diet samples using inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Total diet samples were analyzed for major elements (Na, K, Ca, Mg, P) and some minor trace elements (Fe, Zn, Mn, Al, Sr, Cu, Ba, Yt) using inductively coupled plasma-atomic emission spectrometry (ICP-AES). Samples analyzed were classified into sex and age groups. Results for some elements (Na, K, Mg, Zn, Cu, Mn) were compared with values from Bataan dietary survey calculated using the Philippine composition table. Exceot for Na, analytical results were similar to calculated values. Analytical results for Ca and Fe were also compared with the values from Food and Nutrition Research Institute. In general, values obtained in the study were lower than the FNRI values. Comparison of the analytical and calculated results with the Japanese and ICRP data showed that Philippine values were lower than foreign values. (Auth.). 22 refs., 9 tabs

  12. Direct determination of cadmium in Orujo spirit samples by electrothermal atomic absorption spectrometry: Comparative study of different chemical modifiers

    Energy Technology Data Exchange (ETDEWEB)

    Vilar Farinas, M. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Barciela Garcia, J. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Garcia Martin, S. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Pena Crecente, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Herrero Latorre, C. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain)]. E-mail: cherrero@lugo.usc.es

    2007-05-22

    In this work, several analytical methods are proposed for cadmium determination in Orujo spirit samples using electrothermal atomic absorption spectrometry (ETAAS). Permanent chemical modifiers thermally coated on the platforms inserted in pyrolytic graphite tubes (such as W, Ir, Ru, W-Ir and W-Ru) were comparatively studied in relation to common chemical modifier mixtures [Pd-Mg(NO{sub 3}){sub 2} and (NH{sub 4})H{sub 2}PO{sub 4}-Mg(NO{sub 3}){sub 2}] for cadmium stabilization. Different ETAAS Cd determination methods based on the indicated modifiers have been developed. In each case, pyrolysis and atomization temperatures, atomization shapes, characteristic masses and detection limits as well as other analytical characteristics have been determined. All the assayed modifiers (permanent and conventional) were capable of achieving the appropriate stabilization of the analyte, with the exception of Ru and W-Ru. Moreover, for all developed methods, recoveries (99-102%) and precision (R.S.D. lower than 10%) were acceptable. Taking into account the analytical performance (best detection limit LOD = 0.01 {mu}g L{sup -1}), the ETAAS method based on the use of W as a permanent modifier was selected for further direct Cd determinations in Orujo samples from Galicia (NW Spain). The chosen method was applied in the determination of the Cd content in 38 representative Galician samples. The cadmium concentrations ranged

  13. Atomic and Nuclear Analytical Methods XRF, Mössbauer, XPS, NAA and Ion-Beam Spectroscopic Techniques

    CERN Document Server

    Verma, H R

    2007-01-01

    This book is a blend of analytical methods based on the phenomenon of atomic and nuclear physics. It comprises comprehensive presentations about X-ray Fluorescence (XRF), Mössbauer Spectroscopy (MS), X-ray Photoelectron Spectroscopy (XPS), Neutron- Activation Analysis (NAA), Particle Induced X-ray Emission Analysis (PIXE), Rutherford Backscattering Analysis (RBS), Elastic Recoil Detection (ERD), Nuclear Reaction Analysis (NRA), Particle Induced Gamma-ray Emission Analysis (PIGE), and Accelerator Mass Spectrometry (AMS). These techniques are commonly applied in the fields of medicine, biology, environmental studies, archaeology or geology et al. and pursued in major international research laboratories.

  14. Identification of Synthetic Polymers and Copolymers by Analytical Pyrolysis-Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Kusch, Peter

    2014-01-01

    An experiment for the identification of synthetic polymers and copolymers by analytical pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) was developed and performed in the polymer analysis courses for third-year undergraduate students of chemistry with material sciences, and for first-year postgraduate students of polymer sciences. In…

  15. Methylmercury determination in biological samples using electrothermal atomic absorption spectrometry after acid leaching extraction

    Energy Technology Data Exchange (ETDEWEB)

    Saber-Tehrani, Mohammad; Hashemi-Moghaddam, Hamid; Givianrad, Mohammad Hadi; Abroomand-Azar, Parviz [Islamic Azad University, Department of Chemistry, Science and Research Branch, Tehran (Iran)

    2006-11-15

    An efficient and sensitive method for the determination of methylmercury in biological samples was developed based on acid leaching extraction of methylmercury into toluene. Methylmercury in the organic phase was determined by electrothermal atomic absorption spectrometry (ETAAS). The methylmercury signal was enhanced and the reproducibility increased by formation of certain complexes and addition of Pd-DDC modifier. The complex of methylmercury with DDC produced the optimum analytical signal in terms of sensitivity and reproducibility compared to complexes with dithizone, cysteine, 1,10-phenanthroline, and diethyldithiocarbamate. Method performance was optimized by modifying parameters such as temperature of mineralization, atomization, and gas flow rate. The limit of detection for methylmercury determination was 0.015 {mu}g g{sup -1} and the RSD of the whole procedure was 12% for human teeth samples (n=5) and 15.8% for hair samples (n=5). The method's accuracy was investigated by using NIES-13 and by spiking the samples with different amounts of methylmercury. The results were in good agreement with the certified values and the recoveries were 88-95%. (orig.)

  16. Determination of cadmium in biodiesel using microemulsion and electrothermal atomization atomic absorption spectrometry.

    Science.gov (United States)

    Lima, Adriana S; Silva, Deise G; Teixeira, Leonardo S G

    2015-01-01

    This work aimed to prepare biodiesel microemulsions for the subsequent quantification of cadmium via graphite furnace atomic absorption spectrometry (GFAAS). The biodiesel samples were prepared using n-propanol as an emulsifier, 10% (v/v) nitric acid as the aqueous phase, and biodiesel. Pseudoternary phase diagrams were constructed to determine the microemulsion region with the specified components. The optimized conditions for microemulsion formation were 57.6% (v/v) n-propanol, 21.2% (v/v) biodiesel, and 21.2% (v/v) nitric acid solution. The stability of the microemulsified system was investigated using aqueous and organic standards, and the system was found to be stable for at least 240 min. The applied pyrolysis and atomization temperatures were 800 and 2000 °C, respectively, and 5 μg of aluminum was used as the chemical modifier. The obtained limits of detection and quantification were 0.2 and 0.5 μg kg(-1), respectively, and the characteristic mass was 1.6 pg. The precision, expressed as the relative standard deviation (% R.S.D., n = 10), was 2.5% for a sample with a cadmium concentration of 6.5 μg kg(-1). The accuracy was determined from addition and recovery experiments, with results varying from 93 to 108% recovery. This study demonstrates that the proposed method based on the use of a microemulsion formation in sample preparation can be applied as an efficient alternative for the determination of cadmium in biodiesel by GFAAS. Cadmium determination in biodiesel samples of different origins (soybean, corn, cotton, and sunflower) was evaluated after acid digestion using the inductively coupled plasma-mass spectrometry (ICP-MS) technique, and the obtained results were compared to the results obtained using the proposed method. The paired t test (95% confidence level) did not show significant differences. The concentrations of cadmium found ranged from 5.3 to 8.0 μg kg(-1). PMID:25381584

  17. Determination of arsenic and cadmium in crude oil by direct sampling graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Jesus, Alexandre de; Zmozinski, Ariane Vanessa [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Damin, Isabel Cristina Ferreira [Faculdade Dom Bosco de Porto Alegre, 90520-280, Porto Alegre, RS (Brazil); Silva, Marcia Messias, E-mail: mmsilva@iq.ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Vale, Maria Goreti Rodrigues [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

    2012-05-15

    In this work, a direct sampling graphite furnace atomic absorption spectrometry method has been developed for the determination of arsenic and cadmium in crude oil samples. The samples were weighed directly on the solid sampling platforms and introduced into the graphite tube for analysis. The chemical modifier used for both analytes was a mixture of 0.1% Pd + 0.06% Mg + 0.06% Triton X-100. Pyrolysis and atomization curves were obtained for both analytes using standards and samples. Calibration curves with aqueous standards could be used for both analytes. The limits of detection obtained were 5.1 {mu}g kg{sup -1} for arsenic and 0.2 {mu}g kg{sup -1} for cadmium, calculated for the maximum amount of sample that can be analyzed (8 mg and 10 mg) for arsenic and cadmium, respectively. Relative standard deviations lower than 20% were obtained. For validation purposes, a calibration curve was constructed with the SRM 1634c and aqueous standards for arsenic and the results obtained for several crude oil samples were in agreement according to paired t-test. The result obtained for the determination of arsenic in the SRM against aqueous standards was also in agreement with the certificate value. As there is no crude oil or similar reference material available with a certified value for cadmium, a digestion in an open vessel under reflux using a 'cold finger' was adopted for validation purposes. The use of paired t-test showed that the results obtained by direct sampling and digestion were in agreement at a 95% confidence level. Recovery tests were carried out with inorganic and organic standards and the results were between 88% and 109%. The proposed method is simple, fast and reliable, being appropriated for routine analysis. - Highlights: Black-Right-Pointing-Pointer A direct sampling GF AAS method to determine As and Cd in crude oil was proposed. Black-Right-Pointing-Pointer The conventional chemical modifier Pd/Mg has been used to stabilize As and Cd. Black

  18. Determination of As, Cd, Cu, Hg and Pb in biological samples by modern electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sardans, Jordi, E-mail: j.sardans@creaf.uab.ca [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain); Montes, Fernando [Departamento de Ciencias Analiticas, Facultad de Ciencias, Universidad Nacional de Educacion a Distancia (UNED), C/ Senda del Rey 9. 28040 Madrid (Spain); Penuelas, Josep [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain)

    2010-02-15

    Pollution from heavy metals has increased in recent decades and has become an important concern for environmental agencies. Arsenic, cadmium, copper, mercury and lead are among the trace elements that have the greatest impact and carry the highest risk to human health. Electrothermal atomic absorption spectrometry (ETAAS) has long been used for trace element analyses and over the past few years, the main constraints of atomic absorption spectrometry (AAS) methods, namely matrix interferences that provoked high background absorption and interferences, have been reduced. The use of new, more efficient modifiers and in situ trapping methods for stabilization and pre-concentration of these analytes, progress in control of atomization temperatures, new designs of atomizers and advances in methods to correct background spectral interferences have permitted an improvement in sensitivity, an increase in detection power, reduction in sample manipulation, and increase in the reproducibility of the results. These advances have enhanced the utility of Electrothermal atomic absorption spectrometry (ETAAS) for trace element determination at mug L{sup -1} levels, especially in difficult matrices, giving rise to greater reproducibility, lower economic cost and ease of sample pre-treatment compared to other methods. Moreover, the recent introduction of high resolution continuum source Electrothermal atomic absorption spectrometry (HR-CS-ETAAS) has facilitated direct solid sampling, reducing background noise and opening the possibility of achieving even more rapid quantitation of some elements. The incorporation of flow injection analysis (FIA) systems for automation of sample pre-treatment, as well as chemical vapor generation renders (ETAAS) into a feasible option for detection of As and Hg in environmental and food control studies wherein large numbers of samples can be rapidly analyzed. A relatively inexpensive approach with low sample consumption provide additional advantages

  19. Padronização interna em espectrometria de absorção atômica Internal standardization in atomic absorption spectrometry

    OpenAIRE

    Kelly G. Fernandes; Mercedes de Moraes; José A. Gomes Neto; Joaquim A. Nóbrega; Pedro V. Oliveira

    2003-01-01

    This paper describes a review on internal standardization in atomic absorption spectrometry with emphasis to the systematic and random errors in atomic absorption spectrometry and applications of internal standardization in flame atomic absorption spectrometry and electrothermal atomic absorption spectrometry. The rules for selecting an element as internal standard, limitations of the method, and some comments about the application of internal standardization in atomic absorption spectrometry...

  20. Simultaneous determination of cadmium and lead in wine by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Freschi, Gian P. G.; Dakuzaku, Carolina S.; de Moraes, Mercedes; Nóbrega, Joaquim A.; Gomes Neto, José A.

    2001-10-01

    A method has been developed for the direct simultaneous determination of Cd and Pb in white and red wine by electrothermal atomic absorption spectrometry (ET-AAS) using a transversely heated graphite tube atomizer (THGA) with longitudinal Zeeman-effect background correction. The thermal behavior of both analytes during pyrolysis and atomization stages were investigated in 0.028 mol l -1 HNO 3 and in 1+1 v/v diluted wine using mixtures of Pd(NO 3) 2+Mg(NO 3) 2 and NH 4H 2PO 4+Mg(NO 3) 2 as chemical modifiers. With 5 μg Pd+3 μg Mg as the modifiers and a two-step pyrolysis (10 s at 400°C and 10 s at 600°C), the formation of carbonaceous residues inside the atomizer was avoided. For 20 μl of sample (wine+0.056 mol l -1 HNO 3, 1+1, v/v) dispensed into the graphite tube, analytical curves in the 0.10-1.0 μg l -1 Cd and 5.0-50 μg l -1 Pb ranges were established. The characteristic mass was approximately 0.6 pg for Cd and 33 pg for Pb, and the lifetime of the tube was approximately 400 firings. The limits of detection (LOD) based on integrated absorbance (0.03 μg l -1 for Cd, 0.8 μg l -1 for Pb) exceeded the requirements of Brazilian Food Regulations (decree #55871 from Health Department), which establish the maximum permissible level for Cd at 200 μg l -1 and for Pb at 500 μg l -1. The relative standard deviations ( n=12) were typically <8% for Cd and <6% for Pb. The recoveries of Cd and Pb added to wine samples varied from 88 to 107% and 93 to 103%, respectively. The accuracy of the direct determination of Cd and Pb was checked for 10 table wines by comparing the results with those obtained for digested wine using single-element ET-AAS, which were in agreement at the 95% confidence level.

  1. Column system using diaion HP-2MG for determination of some metal ions by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tuzen, Mustafa; Soylak, Mustafa

    2004-02-23

    A column solid-phase extraction method for the preconcentration and determination of cadmium(II), copper(II), cobalt(II), iron(III), lead(II), nickel(II) and zinc(II) dithizone chelates by atomic absorption spectrometry has been described. Diaion HP-2MG was used as adsorbent for column studies. The influences of the various analytical parameters including pH of the aqueous solutions, amounts of ligand and resin were investigated for the retentions of the analyte ions. The recovery values are ranged from 95 to 102%. The influences of alkaline and earth alkaline ions were also discussed. The preconcentration factor was 375, when the sample volume and final volume are 750 and 2 ml, respectively. The detection limits of the analyte ions (k=3, N=21) were varying 0.08 {mu}g/l for cadmium to 0.25 {mu}g/l for lead. The relative standard deviations of the determinations at the concentration range of 1.8x10{sup -4} to 4.5x10{sup -5} mmol for the investigated elements were found to be lower than 9%. The proposed solid-phase extraction procedure were applied to the flame atomic absorption spectrometric determinations of analyte ions in natural waters (sea, tap, river), microwave digested samples (milk, red wine and rice) and two different reference standard materials (SRM1515 apple leaves and NRCC-SLRS-4 riverine water)

  2. Liquid sample introduction in inductively coupled plasma atomic emission and mass spectrometry — Critical review

    International Nuclear Information System (INIS)

    Inductively coupled plasma optical emission spectroscopy (ICP-OES) and mass spectrometry (ICP-MS) can be considered as the most important tools in inorganic analytical chemistry. Huge progress has been made since the first analytical applications of the ICP. More stable RF generators, improved spectrometers and detection systems were designed along with the achievements gained from advanced microelectronics, leading to overall greatly improved analytical performance of such instruments. In contrast, for the vast majority of cases liquid sample introduction is still based on the pneumatic principle as described in the late 19th century. High flow pneumatic nebulizers typically demand the use of spray chambers as “aerosol filters” in order to match the prerequisites of an ICP. By this, only a small fraction of the nebulized sample actually contributes to the measured signal. Hence, the development of micronebulizers was brought forward. Those systems produce fine aerosols at low sample uptake rates, but they are even more prone for blocking or clogging than conventional systems in the case of solutions containing a significant amount of total dissolved solids (TDS). Despite the high number of publications devoted to liquid sample introduction, it is still considered the Achilles' heel of atomic spectrometry and it is well accepted, that the technology used for liquid sample introduction is still far from ideal, even when applying state-of-the-art systems. Therefore, this review is devoted to offer an update on developments in the field liquid sample introduction that had been reported until the year 2013. The most recent and noteworthy contributions to this field are discussed, trends are highlighted and future directions are outlined. The first part of this review provides a brief overview on theoretical considerations regarding conventional pneumatic nebulization, the fundamentals on aerosol generation and discusses characteristics of aerosols ideally

  3. Analytical theory for the nuclear level shift of hadronic atoms

    International Nuclear Information System (INIS)

    The spectrum problem in the Coulomb potential distorted at small distances is considered. Nuclear shifts of 3-levels in p anti p and Σ-p atoms are calculated. The probabilities of radiative transitions from p-states to the shifted s-states in hadronic atom are also given. It is shown that the reconstruction of atomic levels switches to oscillation regime when absorption increases. The limits of applicability of the perturbation theory in terms of the scattering length for different values of absorption is discussed. An exactly solvable model, Coulomb plus Yamaguchi potential, is considered

  4. Pre-concentration of trace metals from sea-water for determination by graphite-furnace atomic-absorption spectrometry.

    Science.gov (United States)

    Sturgeon, R E; Berman, S S; Desaulniers, A; Russell, D S

    1980-02-01

    Determination of Cd, Zn, Pb, Cu, Fe, Mn, Co, Cr and Ni in coastal sea-water by graphite-furnace atomic-absorption spectrometry after preconcentration by solvent extraction and use of a chelating ion-exchange resin is described. Following the extraction of the pyrrolidine-N-carbodithioate and oxinate complexes into methyl isobutyl ketone, the trace metals are further preconcentrated by back-extraction into 1.5M nitric acid. Preconcentration on the chelating resin is effected by a combined column and batch technique, allowing greater preconcentration factors to be obtained. Provided samples are appropriately treated to release non-labile metal species prior to preconcentration, both methods yield comparable analytical results with respect to the mean concentrations determined as well as to mean relative standard deviations. Control and treatment of the analytical blank is also described. PMID:18962623

  5. Application of multiwalled carbon nanotubes treated by potassium permanganate for determination of trace cadmium prior to flame atomic absorption spectrometry

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes (MWCNTs) and established a new method for the determination of trace cadmium in environment with flame atomic absorption spectrometry. The MWCNTs were oxidized by potassium permanganate under appropriate conditions before use as preconcentration packing. Parameters influencing the recoveries of target analytes were optimized. Under optimal conditions, the target analyte exhibited a good linearity (R2=0.9992)over the concentration range 0.5-50 ng/ml. The detection limit and precision of the proposed method were 0.15 ng/ml and 2.06%,respectively. The proposed method was applied to the determination of cadmium in real-world environmental samples and the recoveries were in the range of 91.3%-108.0%. All these experimental results indicated that this new procedure could be applied to the determination of trace cadmium in environmental waters.

  6. Development of analytical methods for multiplex bio-assay with inductively coupled plasma mass spectrometry

    OpenAIRE

    Ornatsky, Olga I.; Kinach, Robert; Bandura, Dmitry R.; Lou, Xudong; Tanner, Scott D; Baranov, Vladimir I.; Nitz, Mark; Mitchell A. Winnik

    2008-01-01

    Advances in the development of highly multiplexed bio-analytical assays with inductively coupled plasma mass spectrometry (ICP-MS) detection are discussed. Use of novel reagents specifically designed for immunological methods utilizing elemental analysis is presented. The major steps of method development, including selection of elements for tags, validation of tagged reagents, and examples of multiplexed assays, are considered in detail. The paper further describes experimental protocols for...

  7. Chemical vapor generation of silver for atomic absorption spectrometry with the multiatomizer: Radiotracer efficiency study and characterization of silver species

    International Nuclear Information System (INIS)

    Volatile Ag species were generated in flow injection arrangement from nitric acid environment in the presence of surfactants (Triton X-100 and Antifoam B) and permanent Pd deposits as the reaction modifiers. Atomic absorption spectrometry (AAS) with multiple microflame quartz tube atomizer heated to 900 deg. C was used for atomization; evidence was found for thermal mechanism of atomization. Relative and absolute limits of detection (3σ, 250 μl sample loop) measured under optimized conditions were: 1.4 μg l-1 and 0.35 ng, respectively. The efficiency of chemical vapor generation (CVG) as well as spatial distribution of residual analyte in the apparatus was studied by 111Ag radioactive indicator (half-life 7.45 days) of high specific activity. It was found out that 23% of analyte was released into the gaseous phase. However, only 8% was found on filters placed at the entrance to the atomizer due to transport losses. About 40% of analyte remained in waste liquid, whereas the rest was found deposited over the CVG system. Presented study follows the hypothesis that the 'volatile' Ag species are actually metallic nanoparticles formed upon reduction in liquid phase and then released with good efficiency to the gaseous phase. Number/charge size distributions of dry aerosol were determined by Scanning Mobility Particle Sizer. Ag was detected in 40-45 nm particles holding 10 times more charge if compared to Boltzmann equilibrium. At the same time, Ag was also present on 150 nm particles, the main size mode of the CVG generator. The increase of Ag in standards was reflected by proportional increase in particle number/charge for 40-45 nm size particles only. Transmission electron microscopy revealed particles of 8 ± 2 nm sampled from the gaseous phase, which were associated in isolated clusters of few to few tens of nanometres. Ag presence in those particles was confirmed by Energy Dispersive X-ray Spectroscopy (EDS) analysis.

  8. Lead determination at ng/mL level by flame atomic absorption spectrometry using a tantalum coated slotted quartz tube atom trap.

    Science.gov (United States)

    Demirtaş, İlknur; Bakırdere, Sezgin; Ataman, O Yavuz

    2015-06-01

    Flame atomic absorption spectrometry (FAAS) still keeps its importance despite the relatively low sensitivity; because it is a simple and economical technique for determination of metals. In recent years, atom traps have been developed to increase the sensitivity of FAAS. Although the detection limit of FAAS is only at the level of µg/mL, with the use of atom traps it can reach to ng/mL. Slotted quartz tube (SQT) is one of the atom traps used to improve sensitivity. In atom trapping mode of SQT, analyte is trapped on-line in SQT for few minutes using ordinary sample aspiration, followed by the introduction of a small volume of organic solvent to effect the revolatilization and atomization of analyte species resulting in a transient signal. This system is economical, commercially available and easy to use. In this study, a sensitive analytical method was developed for the determination of lead with the help of SQT atom trapping flame atomization (SQT-AT-FAAS). 574 Fold sensitivity enhancement was obtained at a sample suction rate of 3.9 mL/min for 5.0 min trapping period with respect to FAAS. Organic solvent was selected as 40 µL of methyl isobutyl ketone (MIBK). To obtain a further sensitivity enhancement inner surface of SQT was coated with several transition metals. The best sensitivity enhancement, 1650 fold enhancement, was obtained by the Ta-coated SQT-AT-FAAS. In addition, chemical nature of Pb species trapped on quartz and Ta surface, and the chemical nature of Ta on quartz surface were investigated by X-ray photoelectron spectroscopy (XPS) and Raman Spectroscopy. Raman spectrometric results indicate that tantalum is coated on SQT surface in the form of Ta2O5. XPS studies revealed that the oxidation state of Pb in species trapped on both bare and Ta coated SQT surfaces is +2. For the accuracy check, the analyses of standard reference material were performed by use of SCP SCIENCE EnviroMAT Low (EU-L-2) and results for Pb were to be in good agreement with

  9. Determination of myo-inositol hexakisphosphate (phytate) in urine by inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grases, F.; Perello, J.; Isern, B.; Prieto, R.M

    2004-05-10

    Myo-inositol hexakisphosphate (phytate) is a substance present in urine with an important role in preventing calcium renal calculi development. In spite of this, the use of urinary phytate levels on stone-formers' evaluation and treatment is still notably restricted as a consequence of the enormous difficulty to analyze this substance in urine. In this paper, a simple procedure for routinary urinary phytate determination based on phosphorus determination through inductively coupled plasma atomic emission spectrometry is described. The method only requires a previous separation of phytate from other components by column anion exchange chromatography. The working linear range used was 0-2 mg l{sup -1} phosphorus (0-7 mg l{sup -1} phytate). The limit of detection was 64 {mu}g l{sup -1} of phytate and the limit of quantification was 213 {mu}g l{sup -1}. The relative standard deviation (R.S.D.) for 1.35 mg l{sup -1} phytate was 2.4%. Different urine samples were analyzed using an alternative analytical methodology based on gas chromatography (GC)/mass detection used for inositol determination (phytate was previously hydrolyzed), resulting both methods comparable using as criterion to assess statistical significance P<0.05.

  10. Bismuth determination in environmental samples by hydride generation-electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Moscoso-Perez, Carmen; Moreda-Pineiro, Jorge; Lopez-Mahia, Purificacion; Muniategui-Lorenzo, Soledad; Fernandez-Fernandez, Esther; Prada-Rodriguez, Dario [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, E-15071, A Coruna (Spain)

    2003-12-04

    A hydride generation procedure, via flow injection, coupled to electrothermal atomic absorption spectrometry was optimised for Bi determination in sea water and hot-spring water and acid extracts from coal, coal fly ash and slag samples. The effects of several variables such as hydrochloric acid and sodium tetrahydroborate concentrations, hydrochloric acid and sodium tetrahydroborate flow rates, reaction coil length, trapping and atomisation temperatures, trapping time and the Ar flow rate have been investigated by using a 2{sup 9}*3/128 Plackett-Burman design. From these studies, certain variables (sodium tetrahydroborate concentration and trapping time) showed up as significant, and they were optimised by a 2{sup 2}+star central composite design. In addition, a study of the bismuthine trapping and atomisation efficiency from graphite tubes (GTs) permanently treated with uranium, tantalum, lanthanum oxide, niobium, beryllium oxide, chromium oxide and tantalum carbide were investigated. The results obtained were compared with those achieved by iridium and zirconium-treated GTs. The best analytical performances, with characteristic mass of 35 pg and detection limit of 70 ng l{sup -1}, were achieved by using U-treated GTs. Accuracy were checked using several reference materials: 1643d (Trace Elements in Water), TM-24 (Reference Water), GBW-07401 (Soil) and 1632c (Trace Elements in Coal)

  11. A NEW GENERATION OF INSTRUMENTATION AND CAPABILITIES FOR ATOMIC MASS SPECTROMETRY

    Institute of Scientific and Technical Information of China (English)

    1999-01-01

    @@ Atomic mass spectrometry,embodied usually as inductively coupled plasma mass spectrometry (ICPMS) or glow-discharge mass spectrometry (GDMS),has become a widely accepted tool for trace and ultra-trace elemental analysis.ICPMS offers detection limits below 1 ppt in solution,a dynamic concentration levels,isotope-analysis and isotope-dilution capabilities,modest matrix interferences,understandable spectral interferences (isobaric overlaps),precision in range of 2—5%,and rapid measurements (typically 10 seconds per isotope).

  12. A geração química de vapor em espectrometria atômica Chemical vapor generation in atomic spectrometry

    OpenAIRE

    Iracema Takase; Hugo Borges Pereira; Aderval S. Luna; Patrícia Grinberg; Reinaldo Calixto de Campos

    2002-01-01

    The historical development of atomic spectrometry techniques based on chemical vapor generation by both batch and flow injection sampling formats is presented. Detection via atomic absorption spectrometry (AAS), microwave induced plasma optical emission spectrometry (MIP-OES), inductively coupled plasma optical emission spectrometry (ICP-OES) , inductively coupled plasma mass spectrometry (ICP-MS) and furnace atomic nonthermal excitation spectrometry (FANES) are considered. Hydride generation...

  13. Gas chromatography coupled with atomic absorption spectrometry — a sensitive instrumentation for mercury speciation

    Science.gov (United States)

    Emteborg, Håkan; Sinemus, Hans-Werner; Radziuk, Bernard; Baxter, Douglas C.; Frech, Wolfgang

    1996-07-01

    New instrumentation for the speciation of mercury is described, and is applied to the analysis of natural water samples. The separation of mercury species is effected using gas chromatography of derivatized mercury species on a widebore capillary column. The solvent is vented using a bypass valve and the separated mercury species are pyrolysed on-line at 800°C for production of mercury atoms. These are then detected by atomic absorption spectrometry (AAS) at the 253.7 and 184.9 nm lines simultaneously in a quartz cuvette. The use of the 184.9 nm line provides a more than five-fold increase in sensitivity compared with the conventional 253.7 nm line and an absolute detection limit of 0.5 pg of mercury. The dynamic range of the combined analytical lines provides a linear response over more than three orders of magnitude. A number of organic compounds not containing mercury are also detected following pyrolysis, especially at the 184.9 nm line. These background species must not co-elute at the retention times for methyl- and inorganic mercury, as otherwise a positive interference would result. By maximizing the chromatographic resolution and minimizing the band broadening in the cuvette by use of a make-up gas, the retention times of interest are freed from co-eluting background peaks. The instrumentation has been applied to the determination of ng l -1 concentrations of methyl- and inorganic mercury in Lake Constance, Germany and within the Lake Constance drinking water supply organization, Bodenseewasserversorgung (BWV). The accuracy for the sum of methyl- and inorganic mercury has been assessed by comparison with an independent method for total mercury based on AAS detection implemented at BWV. Relative detection limits using 1 litre water samples and 15 ml injections of the final hexane extract were 0.03 ng l -1 for methylmercury and 0.4 ng l -1 for inorganic mercury based on the 3j criterion.

  14. Analytical model for relativistic corrections to the nuclear magnetic shielding constant in atoms

    Energy Technology Data Exchange (ETDEWEB)

    Romero, Rodolfo H. [Facultad de Ciencias Exactas, Universidad Nacional del Nordeste, Avenida Libertad 5500 (3400), Corrientes (Argentina)]. E-mail: rhromero@exa.unne.edu.ar; Gomez, Sergio S. [Facultad de Ciencias Exactas, Universidad Nacional del Nordeste, Avenida Libertad 5500 (3400), Corrientes (Argentina)

    2006-04-24

    We present a simple analytical model for calculating and rationalizing the main relativistic corrections to the nuclear magnetic shielding constant in atoms. It provides good estimates for those corrections and their trends, in reasonable agreement with accurate four-component calculations and perturbation methods. The origin of the effects in deep core atomic orbitals is manifestly shown.

  15. Considerations of particle vaporization and analyte diffusion in single-particle inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    The intensity of individual gold nanoparticles with nominal diameters of 80, 100, 150, and 200 nm was measured using single-particle inductively coupled plasma-mass spectrometry (ICP-MS). Since the particles are not perfectly monodisperse, a distribution of ICP-MS intensity was obtained for each nominal diameter. The distribution of particle mass was determined from the transmission electron microscopy (TEM) image of the particles. The distribution of ICP-MS intensity and the distribution of particle mass for each nominal diameter were correlated to give a calibration curve. The calibration curves are linear, but the slope decreases as the nominal diameter increases. The reduced slope is probably due to a smaller degree of vaporization of the large particles. In addition to the degree of particle vaporization, the rate of analyte diffusion in the ICP is an important factor that determines the measured ICP-MS intensity. Simulated ICP-MS intensity versus particle size was calculated using a simple computer program that accounts for the vaporization rate of the gold nanoparticles and the diffusion rate and degree of ionization of the gold atoms. The curvature of the simulated calibration curves changes with sampling depth because the effects of particle vaporization and analyte diffusion on the ICP-MS intensity are dependent on the residence time of the particle in the ICP. Calibration curves of four hypothetical particles representing the four combinations of high and low boiling points (2000 and 4000 K) and high and low analyte diffusion rates (atomic masses of 10 and 200 Da) were calculated to further illustrate the relative effects of particle vaporization and analyte diffusion. The simulated calibration curves show that the sensitivity of single-particle ICP-MS is smaller than that of the ICP-MS measurement of continuous flow of standard solutions by a factor of 2 or more. Calibration using continuous flow of standard solution is semi-quantitative at best. An

  16. Electrospray ionization and matrix assisted laser desorption/ionization mass spectrometry: powerful analytical tools in recombinant protein chemistry

    DEFF Research Database (Denmark)

    Andersen, Jens S.; Svensson, B; Roepstorff, P

    1996-01-01

    Electrospray ionization and matrix assisted laser desorption/ionization are effective ionization methods for mass spectrometry of biomolecules. Here we describe the capabilities of these methods for peptide and protein characterization in biotechnology. An integrated analytical strategy is presen......Electrospray ionization and matrix assisted laser desorption/ionization are effective ionization methods for mass spectrometry of biomolecules. Here we describe the capabilities of these methods for peptide and protein characterization in biotechnology. An integrated analytical strategy...

  17. Model calculation of the characteristic mass for convective and diffusive vapor transport in graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Bencs, László; Laczai, Nikoletta; Ajtony, Zsolt

    2015-07-01

    A combination of former convective-diffusive vapor-transport models is described to extend the calculation scheme for sensitivity (characteristic mass - m0) in graphite furnace atomic absorption spectrometry (GFAAS). This approach encompasses the influence of forced convection of the internal furnace gas (mini-flow) combined with concentration diffusion of the analyte atoms on the residence time in a spatially isothermal furnace, i.e., the standard design of the transversely heated graphite atomizer (THGA). A couple of relationships for the diffusional and convectional residence times were studied and compared, including in factors accounting for the effects of the sample/platform dimension and the dosing hole. These model approaches were subsequently applied for the particular cases of Ag, As, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Ni, Pb, Sb, Se, Sn, V and Zn analytes. For the verification of the accuracy of the calculations, the experimental m0 values were determined with the application of a standard THGA furnace, operating either under stopped, or mini-flow (50 cm3 min- 1) of the internal sheath gas during atomization. The theoretical and experimental ratios of m0(mini-flow)-to-m0(stop-flow) were closely similar for each study analyte. Likewise, the calculated m0 data gave a fairly good agreement with the corresponding experimental m0 values for stopped and mini-flow conditions, i.e., it ranged between 0.62 and 1.8 with an average of 1.05 ± 0.27. This indicates the usability of the current model calculations for checking the operation of a given GFAAS instrument and the applied methodology.

  18. Rapid accurate analysis of metal (oxide)-on-silica catalysts by atomic absorption spectrometry

    NARCIS (Netherlands)

    Jütte, B.A.H.G.; Heikamp, A.; Agterdenbos, J.

    1979-01-01

    The catalysts, which contain 10–60% copper, chromium, nickel and silicon, are decomposed in sealed Teflon-lined vessels and analyzed by atomic absorption spectrometry. Matrix matching and bracketing standards are applied. The RSD of a single determination is about 1% for all components.

  19. Direct microcomputer controlled determination of zinc in human serum by flow injection atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Simonsen, Kirsten Wiese; Nielsen, Bent; Jensen, Arne;

    1986-01-01

    A procedure is described for the direct determination of zinc in human serum by fully automated, microcomputer controlled flow injection atomic absorption spectrometry (Fl-AAS). The Fl system is pumpless, using the negative pressure created by the nebuliser. It only consists of a three-way valve...

  20. Evaluation of the effect of wavelength poisitioning errors on Kalman filtering results in inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    This work evaluates the effect of wavelength positioning errors in spectral scans on analytical results when the Kalman filtering technique is used for the correction of line interferences in inductively coupled plasma atomic emission spectrometry (ICP-AES). The results show that a positioning accuracy of 0.1 pm is required in order to obtain accurate and precise estimates for analyte concentrations. The positioning error in sample scans is more crucial than that in model scans. The relative bias in measured analyte concentration originating from a positioning error in a sample scan increases linearly with an increase in the magnitude of the error and the peak distance of the overlapping lines, but is inversely proportional to the signal-to-background ratio. By the use of an optimization procedure for the positions of scans with the innovations number as the criterion, the wavelength positioning error can be reduced and, correspondingly, the accuracy and precision of analytical results improved. 19 refs., 4 figs., 2 tabs

  1. MERCURY QUANTIFICATION IN SOILS USING THERMAL DESORPTION AND ATOMIC ABSORPTION SPECTROMETRY: PROPOSAL FOR AN ALTERNATIVE METHOD OF ANALYSIS

    Directory of Open Access Journals (Sweden)

    Liliane Catone Soares

    2015-08-01

    Full Text Available Despite the considerable environmental importance of mercury (Hg, given its high toxicity and ability to contaminate large areas via atmospheric deposition, little is known about its activity in soils, especially tropical soils, in comparison with other heavy metals. This lack of information about Hg arises because analytical methods for determination of Hg are more laborious and expensive compared to methods for other heavy metals. The situation is even more precarious regarding speciation of Hg in soils since sequential extraction methods are also inefficient for this metal. The aim of this paper is to present a technique of thermal desorption associated with atomic absorption spectrometry, TDAAS, as an efficient tool for quantitative determination of Hg in soils. The method consists of the release of Hg by heating, followed by its quantification by atomic absorption spectrometry. It was developed by constructing calibration curves in different soil samples based on increasing volumes of standard Hg2+ solutions. Performance, accuracy, precision, and quantification and detection limit parameters were evaluated. No matrix interference was detected. Certified reference samples and comparison with a Direct Mercury Analyzer, DMA (another highly recognized technique, were used in validation of the method, which proved to be accurate and precise.

  2. High-resolution continuum source electrothermal atomic absorption spectrometry: Linearization of the calibration curves within a broad concentration range

    Energy Technology Data Exchange (ETDEWEB)

    Katskov, Dmitri, E-mail: katskovda@tut.ac.za [Tshwane University of Technology, Chemistry Department, Pretoria 0001 (South Africa); Hlongwane, Miranda [Tshwane University of Technology, Chemistry Department, Pretoria 0001 (South Africa); Heitmann, Uwe [German Aerospace Center, Rose-Luxemburg Str. 2, 10178 Berlin (Germany); Florek, Stefan [ISAS-Leibniz-Institut fuer Analytische Wissenschaften e.V., Albert-Einstein-Str. 9,12489 Berlin (Germany)

    2012-05-15

    The calculation algorithm suggested provides linearization of the calibration curves in high-resolution continuum source electrothermal atomic absorption spectrometry. The algorithm is based on the modification of the function wavelength-integrated absorbance vs. concentration of analyte vapor in the absorption volume. According to the suggested approach, the absorption line is represented by a triangle for low and trapezium for high analyte vapor concentration in the absorption volume. The respective semi-empirical formulas include two linearization parameters, which depend on properties of the absorption line and characteristics of the atomizer and spectrometer. The parameters can be approximately evaluated from the theory and determined in practice from the original broad-range calibration curve. The parameters were found and the proposed calculation algorithm verified in the experiments on direct determination of Ag, Cd, Cu, Fe, Mn and Pb in the solutions within a concentration ranges from 0.15 to 625 {mu}g{center_dot}L{sup -1} using tube, platform tube and filter furnace atomizers. The use of various atomizers, lines, elements and atomization temperatures made possible the simulation of various practical analytical conditions. It was found that the algorithm and optimal linearization parameters made it possible to obtain for each line and atomizer linear approximations of the calibration curves within 3-4 orders of magnitude with correlation coefficients close to 0.999. The algorithm makes possible to employ a single line for the direct element determination over a broad concentration range. The sources of errors and the possibility of a priori theoretical evaluation of the linearization parameters are discussed. - Highlights: Black-Right-Pointing-Pointer New calculation algorithm for HR-CS ET AAS measurements was proposed and applied. Black-Right-Pointing-Pointer The suggested formulas include two parameters to be determined experimentally. Black

  3. A geração química de vapor em espectrometria atômica Chemical vapor generation in atomic spectrometry

    Directory of Open Access Journals (Sweden)

    Iracema Takase

    2002-12-01

    Full Text Available The historical development of atomic spectrometry techniques based on chemical vapor generation by both batch and flow injection sampling formats is presented. Detection via atomic absorption spectrometry (AAS, microwave induced plasma optical emission spectrometry (MIP-OES, inductively coupled plasma optical emission spectrometry (ICP-OES , inductively coupled plasma mass spectrometry (ICP-MS and furnace atomic nonthermal excitation spectrometry (FANES are considered. Hydride generation is separately considered in contrast to other methods of generation of volatile derivatives. Hg ¾ CVAAS (cold vapor atomic absorption spectrometry is not considered here. The current state-of-the-art, including extension, advantages and limitations of this approach is discussed.

  4. Micro-determination of ytterbium with electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    This communication reports the use of a pyrolytic graphite coated tube, lined with tantalum-tungsten, and a local made atomic absorption spectrometer (Model WFD-Y3) for the determination of small amount Yb in pure Y2O3 and mixed rare earth oxides. It is found that the method proposed is sensitive, reproducible and simple in manipulation. Even as low as 0.2 μg Yb in one gram sample (n x 10-7) can be determined directly without pre-concentration. It is found experimentally that the optimum condition for drying is at 150 deg C. for 20 sec, ashing at 1000 deg C. for 20 sec and atomization at 2770 deg C. for 12 sec. Within the range 1.0-18ng Yb/ml the calibration curve of Yb is linear. Before injecting into the tube, the acidity of the sample solution should be ajusted to 0.1 to 2 M with nitric or hydrochloric acid. For 5ng Yb/ml, Al(III), Ca(II) and La(III) interference, when their amount present is 50 μg/ml or more. On the other hand, Cu(II), Fe(III), Mg(II), K(I) and Y(III) in amount up to 1 mg/ml do not interfere

  5. Cinchocaine hydrochloride determination by atomic absorption spectrometry and spectrophotometry.

    Science.gov (United States)

    Abdel-Ghani, Nour T; Youssef, Ahmed F A; Awady, Mohamed A

    2005-05-01

    Two sensitive spectrophotometric and atomic absorption spectrometric procedures have been developed for determination of cinchocaine hydrochloride (Cin.Cl) in pure form and in pharmaceutical formulation. The spectrophotometric method was based on formation of an insoluble colored ion-associate between the cited drug and tetrathiocyanatocobaltate (CoTC) or hexathiocyanatochromate (CrTC) which dissolved and extracted in an organic solvent. The optimal experimental conditions for quantitative extraction such as pH, concentration of the reagents and solvent were studied. Toluene and iso-butyl alcohol proved to be the most suitable solvents for quantitative extraction of Cin-CoTC and Cin-CrTC ion-associates with maximum absorbance at 620 and 555 nm, respectively. The optimum concentration ranges, molar absorptivities, Ringbom ranges and Sandell sensitivities were also evaluated. The atomic absorption spectrometric method is based on measuring of the excess cobalt or chromium in the aqueous solution, after precipitation of the drug, at 240.7 and 357.9 nm, respectively. Linear application ranges, characteristic masses and detection limits were 57.99-361.9, 50.40 and 4.22 microg ml(-1) of Cin.Cl, in case of CoTC, while 37.99-379.9, 18.94 and 0.81 microg ml(-1) in case of CrTC. PMID:15910814

  6. Cinchocaine hydrochloride determination by atomic absorption spectrometry and spectrophotometry.

    Science.gov (United States)

    Abdel-Ghani, Nour T; Youssef, Ahmed F A; Awady, Mohamed A

    2005-05-01

    Two sensitive spectrophotometric and atomic absorption spectrometric procedures have been developed for determination of cinchocaine hydrochloride (Cin.Cl) in pure form and in pharmaceutical formulation. The spectrophotometric method was based on formation of an insoluble colored ion-associate between the cited drug and tetrathiocyanatocobaltate (CoTC) or hexathiocyanatochromate (CrTC) which dissolved and extracted in an organic solvent. The optimal experimental conditions for quantitative extraction such as pH, concentration of the reagents and solvent were studied. Toluene and iso-butyl alcohol proved to be the most suitable solvents for quantitative extraction of Cin-CoTC and Cin-CrTC ion-associates with maximum absorbance at 620 and 555 nm, respectively. The optimum concentration ranges, molar absorptivities, Ringbom ranges and Sandell sensitivities were also evaluated. The atomic absorption spectrometric method is based on measuring of the excess cobalt or chromium in the aqueous solution, after precipitation of the drug, at 240.7 and 357.9 nm, respectively. Linear application ranges, characteristic masses and detection limits were 57.99-361.9, 50.40 and 4.22 microg ml(-1) of Cin.Cl, in case of CoTC, while 37.99-379.9, 18.94 and 0.81 microg ml(-1) in case of CrTC.

  7. Behaviour of the thermospray nebulizer as a system for the introduction of organic solutions in flame atomic absorption spectrometry

    Science.gov (United States)

    Mora, Juan; Canals, Antonio; Hernandis, Vicente

    1996-10-01

    The results obtained in the evaluation of the thermospray nebulizer for the introduction of organic solutions in atomic spectrometry are described. To this end, the influence of the nebulization variables (i.e., liquid flow, control temperature and inner diameter of the capillary) and of the nature of the solvent on the fraction of solvent vaporized, on the drop size distribution of the primary aerosol, on the rates of analyte and solvent transport to the atomization cell and on the analytical signal has been studied. Experimental fraction of solvent vaporized values obtained under different nebulization conditions are reported for the first time. The results show that the characteristics of the aerosol generated strongly depend on the nebulization variables since they determine the amount of energy available for surface generation. The median of the volume drop size distribution of the primary aerosol decreases when the control temperature or the liquid flow is increased or when the inner diameter of the capillary is decreased. As regards the physical properties of the solvent, the so-called expansion factor (i.e., the volume of vapour produced per unit volume of liquid solvent) is the most influential. Surface tension and viscosity are much less significant here than in ordinary pneumatic nebulization. The volatility of the solvent and the characteristics of the primary aerosol determine the solvent transport efficiency which reaches values close to 100% in many cases. The analytical signal is mainly determined by the analyte transport rate, although a severe negative effect appears which is related to the high solvent load to the flame. Due to this fact, the use of organic solvents instead of water in thermospray nebulization for Flame Atomic Absorption Spectrometry does not provide clear advantages, at least without desolvation. A new modified Nukiyama-Tanasawa equation has been presented and evaluated in order to predict the Sauter mean diameter of the thermal

  8. Laser resonance ionization mass spectrometry as a sensitive analytical method for actinides and technetium

    International Nuclear Information System (INIS)

    Laser resonance ionization mass spectrometry has been investigated as a method for the determination of trace amounts of actinides and technetium. A high sensitivity and selectivity have been achieved by three-step photoionization of the elements in the atomic state followed by time-of-flight measurement for mass analysis. The system for photoionization consists of three dye lasers which are pumped simultaneously by a copper vapour laser of 30 W average power at a pulse repetition rate of 6.5 KHz. The time-of-flight spectrometer has a mass resolution better than 2500. By ionization via autoionization states and by saturation in each excitation step a detection limit of less than 108 atoms of actinides or of technetium in the sample can be reached. (author)

  9. Cloud point extraction for the determination of cadmium and lead in biological samples by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Maranhão, Tatiane De A.; Borges, Daniel L. G.; da Veiga, Márcia A. M. S.; Curtius, Adilson J.

    2005-06-01

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of Cd and Pb from digested biological samples. After complexation with O,O-diethyldithiophosphate (DDTP) in hydrochloric acid medium, the analytes are quantitatively extracted to the phase rich in the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 0.1 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by electrothermal atomic absorption spectrometry (ET AAS). The adopted concentrations for DDTP, Triton X-114 and hydrochloric acid were all optimized. Pyrolysis and atomization temperatures were optimized using the extracts and pyrolysis temperatures of 700 °C for both elements and atomization temperatures of 1400 and 1600 °C for cadmium and lead, respectively, were used without adding any modifier, which shows that considerable analyte stabilization is provided by the medium itself. A more detailed investigation was carried out to determine which components of the extract were responsible for the high thermal stability achieved and it revealed that the amount of DDTP added and the phosphorus content of the digested samples contributed significantly to this phenomenon. Detection limits (3σB) of 6 and 40 ng g-1, along with enrichment factors of 129 and 18 for Cd and Pb, respectively, were achieved. The proposed procedure was applied to the analysis of five certified biological reference materials after microwave-assisted acid digestion in a mixture of H2O2 and HNO3. Comparison with certified values was performed for accuracy evaluation, resulting in good agreement according to the t-test for a 95% confidence level. The high efficiency of cloud point extraction to carry out the determination of the studied analytes in complex matrices was, therefore, demonstrated.

  10. Cloud point extraction for the determination of cadmium and lead in biological samples by graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Maranhao, Tatiane de A. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Borges, Daniel L.G. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil)]. E-mail: daniel@qmc.ufsc.br; Veiga, Marcia A.M.S. da [Instituto de Quimica, Universidade de Sao Paulo, 05513-970, CP 26077, Sao Paulo, SP (Brazil); Curtius, Adilson J. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil)

    2005-06-30

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of Cd and Pb from digested biological samples. After complexation with O,O-diethyldithiophosphate (DDTP) in hydrochloric acid medium, the analytes are quantitatively extracted to the phase rich in the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 0.1 mol L{sup -1} HNO{sub 3} was added to the surfactant-rich phase prior to its analysis by electrothermal atomic absorption spectrometry (ET AAS). The adopted concentrations for DDTP, Triton X-114 and hydrochloric acid were all optimized. Pyrolysis and atomization temperatures were optimized using the extracts and pyrolysis temperatures of 700 deg. C for both elements and atomization temperatures of 1400 and 1600 deg. C for cadmium and lead, respectively, were used without adding any modifier, which shows that considerable analyte stabilization is provided by the medium itself. A more detailed investigation was carried out to determine which components of the extract were responsible for the high thermal stability achieved and it revealed that the amount of DDTP added and the phosphorus content of the digested samples contributed significantly to this phenomenon. Detection limits (3{sigma} {sub B}) of 6 and 40 ng g{sup -1}, along with enrichment factors of 129 and 18 for Cd and Pb, respectively, were achieved. The proposed procedure was applied to the analysis of five certified biological reference materials after microwave-assisted acid digestion in a mixture of H{sub 2}O{sub 2} and HNO{sub 3}. Comparison with certified values was performed for accuracy evaluation, resulting in good agreement according to the t-test for a 95% confidence level. The high efficiency of cloud point extraction to carry out the determination of the studied analytes in complex matrices was, therefore, demonstrated.

  11. Ionic liquid ultrasound assisted dispersive liquid-liquid microextraction method for preconcentration of trace amounts of rhodium prior to flame atomic absorption spectrometry determination

    International Nuclear Information System (INIS)

    In this article, we consider ionic liquid based ultrasound-assisted dispersive liquid-liquid microextraction of trace amounts of rhodium from aqueous samples and show that this is a fast and reliable sample pre-treatment for the determination of rhodium ions by flame atomic absorption spectrometry. The Rh(III) was transferred into its complex with 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol as a chelating agent, and an ultrasonic bath with the ionic liquid, 1-octyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide at room temperature was used to extract the analyte. The centrifuged rhodium complex was then enriched in the form of ionic liquid droplets and prior to its analysis by flame atomic absorption spectrometry, 300 μL ethanol was added to the ionic liquid-rich phase. Finally, the influence of various parameters on the recovery of Rh(III) was optimized. Under optimum conditions, the calibration graph was linear in the range of 4.0-500.0 ng mL-1, the detection limit was 0.37 ng mL-1 (3Sb/m, n = 7) and the relative standard deviation was ±1.63% (n = 7, C = 200 ng mL-1). The results show that ionic liquid based ultrasound assisted dispersive liquid-liquid microextraction, combined with flame atomic absorption spectrometry, is a rapid, simple, sensitive and efficient analytical method for the separation and determination of trace amounts of Rh(III) ions with minimum organic solvent consumption.

  12. Simple analysis of total mercury and methylmercury in seafood using heating vaporization atomic absorption spectrometry.

    Science.gov (United States)

    Yoshimoto, Keisuke; Anh, Hoang Thi Van; Yamamoto, Atsushi; Koriyama, Chihaya; Ishibashi, Yasuhiro; Tabata, Masaaki; Nakano, Atsuhiro; Yamamoto, Megumi

    2016-01-01

    This study aimed to develop a simpler method for determining total mercury (T-Hg) and methylmercury (MeHg) in biological samples by using methyl isobutyl ketone (MIBK) in the degreasing step. The fat in the samples was extracted by MIBK to the upper phase. T-Hg transferred into the water phase. This was followed by the extraction of MeHg from the water phase using HBr, CuCl2 and toluene. The MeHg fraction was reverse-extracted into L-cysteine-sodium acetate solution from toluene. The concentrations of T-Hg and MeHg were determined by heating vaporization atomic absorption spectrometry. Certified reference materials for T-Hg and MeHg in hair and fish were accurately measured using this method. This method was then applied to determine T-Hg and MeHg concentrations in the muscle, liver and gonads of seafood for the risk assessment of MeHg exposure. The mean T-Hg and MeHg concentrations in squid eggs were 0.023 and 0.022 µg/g, and in squid nidamental glands 0.052 and 0.049 µg/g, respectively. The MeHg/T-Hg ratios in the eggs and nidamental glands of squid were 94.4% and 96.5%, respectively. The mean T-Hg and MeHg concentrations in the gonads of sea urchins were 0.043 and 0.001 µg/g, respectively, with a MeHg/T-Hg ratio of 3.5%. We developed an efficient analytical method for T-Hg and MeHg using MIBK in the degreasing step. The new information on MeHg concentration and MeHg/T-Hg ratios in the egg or nidamental glands of squid and gonads of sea urchin will also be useful for risk assessment of mercury in seafood. PMID:27432235

  13. Simple analysis of total mercury and methylmercury in seafood using heating vaporization atomic absorption spectrometry.

    Science.gov (United States)

    Yoshimoto, Keisuke; Anh, Hoang Thi Van; Yamamoto, Atsushi; Koriyama, Chihaya; Ishibashi, Yasuhiro; Tabata, Masaaki; Nakano, Atsuhiro; Yamamoto, Megumi

    2016-01-01

    This study aimed to develop a simpler method for determining total mercury (T-Hg) and methylmercury (MeHg) in biological samples by using methyl isobutyl ketone (MIBK) in the degreasing step. The fat in the samples was extracted by MIBK to the upper phase. T-Hg transferred into the water phase. This was followed by the extraction of MeHg from the water phase using HBr, CuCl2 and toluene. The MeHg fraction was reverse-extracted into L-cysteine-sodium acetate solution from toluene. The concentrations of T-Hg and MeHg were determined by heating vaporization atomic absorption spectrometry. Certified reference materials for T-Hg and MeHg in hair and fish were accurately measured using this method. This method was then applied to determine T-Hg and MeHg concentrations in the muscle, liver and gonads of seafood for the risk assessment of MeHg exposure. The mean T-Hg and MeHg concentrations in squid eggs were 0.023 and 0.022 µg/g, and in squid nidamental glands 0.052 and 0.049 µg/g, respectively. The MeHg/T-Hg ratios in the eggs and nidamental glands of squid were 94.4% and 96.5%, respectively. The mean T-Hg and MeHg concentrations in the gonads of sea urchins were 0.043 and 0.001 µg/g, respectively, with a MeHg/T-Hg ratio of 3.5%. We developed an efficient analytical method for T-Hg and MeHg using MIBK in the degreasing step. The new information on MeHg concentration and MeHg/T-Hg ratios in the egg or nidamental glands of squid and gonads of sea urchin will also be useful for risk assessment of mercury in seafood.

  14. Speciation determination of chromium(III) and (VI) using preconcentration cloud point extraction with flame atomic absorption spectrometry (FAAS)

    Energy Technology Data Exchange (ETDEWEB)

    Kiran, K. [Department of Environmental Sciences, S.V. University, Tirupati, 517502 A.P. (India); Kumar, K. Suresh; Prasad, B.; Suvardhan, K. [Department of Chemistry, S. V. University, Tirupati, 517502 A.P. (India); Lekkala, Ramesh Babu [Department of Environmental Sciences, S.V. University, Tirupati, 517502 A.P. (India); Janardhanam, K. [Department of Environmental Sciences, S.V. University, Tirupati, 517502 A.P. (India)], E-mail: Kandukurijanardhanam@gmail.com

    2008-02-11

    bis-[2-Hydroxy-1-naphthaldehyde] thiourea was synthesized and preconcentration cloud point extraction (CPE) for speciation determination of chromium(III) and (VI) in various environmental samples with flame atomic absorption spectrometry (FAAS) has been developed. Chromium(III) complexes with bis-[2-hydroxynaphthaldehyde] thiourea is subsequently entrapped in the surfactant micelles. After complexation of chromium(III) with reagent, the analyte was quantitatively extracted to the surfactant-rich phase in the non-ionic surfactant Triton X-100 after centrifugation. The effect of pH, concentration of chelating agent, surfactant, equilibration temperature and time on CPE was studied. The relative standard deviation was 2.13% and the limits of detection were around 0.18 {mu}g L{sup -1}.

  15. Solid phase microextraction capillary gas chromatography combined with furnace atomization plasma emission spectrometry for speciation of mercury in fish tissues

    International Nuclear Information System (INIS)

    The use of solid phase microextraction in conjunction with tandem gas chromatography-furnace atomization plasma emission spectrometry (SPME-GC-FAPES) was evaluated for the determination of methylmercury and inorganic mercury in fish tissue. Samples were digested with methanolic potassium hydroxide, derivatized with sodium tetraethylborate and extracted by SPME. After the SPME extraction, species were separated by GC and detected by FAPES. All experimental parameters were optimized for best separation and analytical response. A repeatability precision of typically 2% can be achieved with long-term (3 months) reproducibility precision of 4.3%. Certified Reference Materials DORM-2, DOLT-2 and TORT-2 from the National Research Council of Canada were analyzed to verify the accuracy of this technique. Detection limits of 1.5 ng g-1 for methylmercury and 0.7 ng g-1 for inorganic mercury in biological tissues were obtained

  16. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bentlin, Fabrina R.S. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil); Pozebon, Dirce [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil)], E-mail: dircepoz@iq.ufrgs.br; Mello, Paola A.; Flores, Erico M.M. [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900 Santa Maria, RS (Brazil)

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO{sub 3}){sub 2} was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 {mu}g g{sup -1} of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES)

  17. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Bentlin, Fabrina R S; Pozebon, Dirce; Mello, Paola A; Flores, Erico M M

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO3)2 was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 microg g(-1) of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES).

  18. Bromine and bromide content in soils: Analytical approach from total reflection X-ray fluorescence spectrometry.

    Science.gov (United States)

    Gallardo, Helena; Queralt, Ignasi; Tapias, Josefina; Candela, Lucila; Margui, Eva

    2016-08-01

    Monitoring total bromine and bromide concentrations in soils is significant in many environmental studies. Thus fast analytical methodologies that entail simple sample preparation and low-cost analyses are desired. In the present work, the possibilities and drawbacks of low-power total reflection X-ray fluorescence spectrometry (TXRF) for the determination of total bromine and bromide contents in soils were evaluated. The direct analysis of a solid suspension using 20 mg of fine ground soil (soils (Br content range in soils = 5-40 mg kg(-1)). Information about bromide determination in soils is also possible by analyzing the Br content in water soil extracts. In this case, the TXRF analysis can be directly performed by depositing 10 μL of the internal standardized soil extract sample on a quartz glass reflector in a measuring time of 1500 s. The bromide limit of detection by this approach was 10 μg L(-1). Good agreement was obtained between the TXRF results for the total bromine and bromide determinations in soils and those obtained by other popular analytical techniques, e.g. energy dispersive X-ray fluorescence spectrometry (total bromine) and ionic chromatography (bromide). As a study case, the TXRF method was applied to study bromine accumulation in two agricultural soils fumigated with a methyl bromide pesticide and irrigated with regenerated waste water. PMID:27179429

  19. Speciation analysis of arsenic in biological matrices by automated hydride generation-cryotrapping-atomic absorption spectrometry with multiple microflame quartz tube atomizer (multiatomizer).

    Science.gov (United States)

    This paper describes an automated system for the oxidation state specific speciation of inorganic and methylated arsenicals by selective hydride generation - cryotrapping- gas chromatography - atomic absorption spectrometry with the multiatomizer. The corresponding arsines are ge...

  20. Dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zeini Jahromi, Elham [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Bidari, Araz [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Assadi, Yaghoub [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of) and Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of)]. E-mail: y_assadi@iust.ac.ir; Milani Hosseini, Mohammad Reza [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Jamali, Mohammad Reza [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of)

    2007-03-07

    Dispersive liquid-liquid microextraction (DLLME) technique was successfully used as a sample preparation method for graphite furnace atomic absorption spectrometry (GF AAS). In this extraction method, 500 {mu}L methanol (disperser solvent) containing 34 {mu}L carbon tetrachloride (extraction solvent) and 0.00010 g ammonium pyrrolidine dithiocarbamate (chelating agent) was rapidly injected by syringe into the water sample containing cadmium ions (interest analyte). Thereby, a cloudy solution formed. The cloudy state resulted from the formation of fine droplets of carbon tetrachloride, which have been dispersed, in bulk aqueous sample. At this stage, cadmium reacts with ammonium pyrrolidine dithiocarbamate, and therefore, hydrophobic complex forms which is extracted into the fine droplets of carbon tetrachloride. After centrifugation (2 min at 5000 rpm), these droplets were sedimented at the bottom of the conical test tube (25 {+-} 1 {mu}L). Then a 20 {mu}L of sedimented phase containing enriched analyte was determined by GF AAS. Some effective parameters on extraction and complex formation, such as extraction and disperser solvent type and their volume, extraction time, salt effect, pH and concentration of the chelating agent have been optimized. Under the optimum conditions, the enrichment factor 125 was obtained from only 5.00 mL of water sample. The calibration graph was linear in the rage of 2-20 ng L{sup -1} with detection limit of 0.6 ng L{sup -1}. The relative standard deviation (R.S.D.s) for ten replicate measurements of 20 ng L{sup -1} of cadmium was 3.5%. The relative recoveries of cadmium in tap, sea and rivers water samples at spiking level of 5 and 10 ng L{sup -1} are 108, 95, 87 and 98%, respectively. The characteristics of the proposed method have been compared with cloud point extraction (CPE), on-line liquid-liquid extraction, single drop microextraction (SDME), on-line solid phase extraction (SPE) and co-precipitation based on bibliographic data

  1. Optimized determination of calcium in grape juice, wines, and other alcoholic beverages by atomic absorption spectrometry.

    Science.gov (United States)

    Olalla, Manuel; González, Maria Cruz; Cabrera, Carmen; Gimenez, Rafael; López, Maria Carmen

    2002-01-01

    This paper describes a study of the different methods of sample preparation for the determination of calcium in grape juice, wines, and other alcoholic beverages by flame atomic absorption spectrometry; results are also reported for the practical application of these methods to the analysis of commercial samples produced in Spain. The methods tested included dealcoholization, dry mineralization, and wet mineralization with heating by using different acids and/or mixtures of acids. The sensitivity, detection limit, accuracy, precision, and selectiviy of each method were established. Such research is necessary because of the better analytical indexes obtained after acid digestion of the sample, as recommended by the European Union, which advocates the direct method. In addition, although high-temperature mineralization with an HNO3-HCIO4 mixture gave the best analytical results, mineralization with nitric acid at 80 degrees C for 15 min gave the most satisfactory results in all cases, including those for wines with high levels of sugar and beverages with high alcoholic content. The results for table wines subjected to the latter treatment had an accuracy of 98.70-99.90%, a relative standard deviation of 2.46%, a detection limit of 19.0 microg/L, and a determination limit of 31.7 microg/L. The method was found to be sufficiently sensitive and selective. It was applied to the determination of Ca in grape juice, different types of wines, and beverages with high alcoholic content, all of which are produced and widely consumed in Spain. The values obtained for Ca were 90.00 +/- 20.40 mg/L in the grape juices, 82.30 +/- 23.80 mg/L in the white wines, 85.00 +/- 30.25 mg/L in the sweet wines, 84.92 +/- 23.11 mg/L in the red wines, 85.75 +/- 27.65 mg/L in the rosé wines, 9.51 +/- 6.65 mg/L in the brandies, 11.53 +/- 6.55 mg/L in the gin, 7.3 +/- 6.32 mg/L in the pacharán, and 8.41 +/- 4.85 mg/L in the anisettes. The method is therefore useful for routine analysis in the

  2. Direct determination of mercury in white vinegar by matrix assisted photochemical vapor generation atomic fluorescence spectrometry detection

    Energy Technology Data Exchange (ETDEWEB)

    Liu Qingyang, E-mail: liuqingyang0807@yahoo.com.c [Beijing Center for Physical and Chemical Analysis, Beijing 100089 (China)

    2010-07-15

    This paper proposes the use of photochemical vapor generation with acetic acid as sample introduction for the direct determination of ultra-trace mercury in white vinegars by atomic fluorescence spectrometry. Under ultraviolet irradiation, the sample matrix (acetic acid) can reduce mercury ion to atomic mercury Hg{sup 0}, which is swept by argon gas into an atomic fluorescence spectrometer for subsequent analytical measurements. The effects of several factors such as the concentration of acetic acid, irradiation time, the flow rate of the carrier gas and matrix effects were discussed and optimized to give detection limits of 0.08 ng mL{sup -1} for mercury. Using the experimental conditions established during the optimization (3% v/v acetic acid, 30 s irradiation time and 20 W mercury lamp), the precision levels, expressed as relative standard deviation, were 4.6% (one day) and 7.8% (inter-day) for mercury (n = 9). Addition/recovery tests for evaluation of the accuracy were in the range of 92-98% for mercury. The method was also validated by analysis of vinegar samples without detectable amount of Hg spiked with aqueous standard reference materials (GBW(E) 080392 and GBW(E) 080393). The results were also compared with those obtained by acid digestion procedure and determination of mercury by ICP-MS. There was no significant difference between the results obtained by the two methods based on a t-test (at 95% confidence level).

  3. Analytical Solutions of Temporal Evolution of Populations in Optically-Pumped Atoms with Circularly Polarized Light

    Directory of Open Access Journals (Sweden)

    Heung-Ryoul Noh

    2016-03-01

    Full Text Available We present an analytical calculation of temporal evolution of populations for optically pumped atoms under the influence of weak, circularly polarized light. The differential equations for the populations of magnetic sublevels in the excited state, derived from rate equations, are expressed in the form of inhomogeneous second-order differential equations with constant coefficients. We present a general method of analytically solving these differential equations, and obtain explicit analytical forms of the populations of the ground state at the lowest order in the saturation parameter. The obtained populations can be used to calculate lineshapes in various laser spectroscopies, considering transit time relaxation.

  4. Chemometric extraction of analyte-specific chromatograms in on-line gradient LC-infrared spectrometry.

    Science.gov (United States)

    Kuligowski, Julia; Quintás, Guillermo; Garrigues, Salvador; de la Guardia, Miguel

    2009-12-01

    This work exploits the possibilities offered by the recently developed multivariate method named Science-Based Calibration (SBC), for the extraction of 'analyte-specific' chromatograms in on-line gradient reversed phase LC-infrared spectrometry (IR) in the presence of a high spectral and chromatographic overlapping between the analyte of interest, co-eluting sample matrix constituents and the mobile phase components. The SBC method uses an experimentally measured single response spectrum of the analyte of interest and representative noise to calculate an optimum regression vector (b(opt(1))). Then, the b(opt(1)) vector is used to predict the concentration of the analyte of interest in the spectra of the LC-IR sample chromatograms. To evaluate the advantages and pitfalls of the proposed approach, two different situations were analysed on real LC-IR data sets obtained from the injection of a series of standard solutions of four nitrophenols (p-nitrophenol, 3-methyl-4-nitrophenol, 2,4-dinitrophenol and 4-nitrophenol) in a reversed phase system under gradient conditions. In the first situation, the extraction of the 'analyte-specific' chromatogram was carried out without previous knowledge of the spectral features of other interferents present in the sample matrix. In a second situation evaluated, data obtained from the LC injection of a sample blank is available. Results show the potential applicability of this technique in a variety of situations and evidenced that the proposed chemometric approach improves the selectivity and sensitivity of the LC-IR hyphenation. PMID:19877149

  5. Direct determination of selenoproteins in polyvinylidene difluoride membranes by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Sidenius, U; Gammelgaard, Bente

    2000-01-01

    were excised and chemical modifier was added on top of the excised membrane prior to atomic absorption measurement. Acceptable linearity was achieved in the range 2-10 ng Se, corresponding to selenium concentrations close to 1 mg/L, when aqueous solutions of selenomethionine standard as well......A method for the direct determination of selenoproteins in plastic membranes after protein separation by gel electrophoresis was developed. Quantification was based on the determination of the selenium content of the proteins by electrothermal atomic absorption spectrometry (ET-AAS) after manual...

  6. Determination of serum lithium: comparison between atomic emission and absorption spectrometry methods

    Directory of Open Access Journals (Sweden)

    Carlos Elielton do Espírito Santo

    2014-02-01

    Full Text Available Introduction: The therapeutic monitoring of lithium, through concentration measurements, is important for individual dose adjustment, as a marker of treatment adherence and to prevent poisoning and side effects. Objectives: Validate and compare two methods - atomic emission and atomic absorption - for the determination of lithium in serum samples. Methodology: Parameters such as specificity, precision, accuracy, limit of detection (LOD and linearity were considered. The atomic absorption spectrometer was used, operating in either emission or absorption mode. For the quantitative comparison of 30 serum samples from patients with mood disorder treated with lithium, the results were submitted to Student's t-test, F-test and Pearson's correlation. Results: The limit of quantification (LOQ was established as 0.05 mEq/l of lithium, and calibration curves were constructed in the range of 0.05-2 mEq/l of lithium, using aqueous standards. Sample preparation time was reduced, what is important in medical laboratory. Conclusion: Both methods were considered satisfactory, precise and accurate and can be adopted for lithium quantification. In the comparison of quantitative results in lithium-treated patients through statistical tests, no significant differences were observed. Therefore the methods for lithium quantification by flame atomic absorption spectrometry (FAAS and flame atomic emission spectrometry (FAES may be considered similar.

  7. Model calculation of the characteristic mass for convective and diffusive vapor transport in graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A combination of former convective–diffusive vapor-transport models is described to extend the calculation scheme for sensitivity (characteristic mass — m0) in graphite furnace atomic absorption spectrometry (GFAAS). This approach encompasses the influence of forced convection of the internal furnace gas (mini-flow) combined with concentration diffusion of the analyte atoms on the residence time in a spatially isothermal furnace, i.e., the standard design of the transversely heated graphite atomizer (THGA). A couple of relationships for the diffusional and convectional residence times were studied and compared, including in factors accounting for the effects of the sample/platform dimension and the dosing hole. These model approaches were subsequently applied for the particular cases of Ag, As, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Ni, Pb, Sb, Se, Sn, V and Zn analytes. For the verification of the accuracy of the calculations, the experimental m0 values were determined with the application of a standard THGA furnace, operating either under stopped, or mini-flow (50 cm3 min−1) of the internal sheath gas during atomization. The theoretical and experimental ratios of m0(mini-flow)-to-m0(stop-flow) were closely similar for each study analyte. Likewise, the calculated m0 data gave a fairly good agreement with the corresponding experimental m0 values for stopped and mini-flow conditions, i.e., it ranged between 0.62 and 1.8 with an average of 1.05 ± 0.27. This indicates the usability of the current model calculations for checking the operation of a given GFAAS instrument and the applied methodology. - Highlights: • A calculation scheme for convective–diffusive vapor loss in GFAAS is described. • Residence time (τ) formulas were compared for sensitivity (m0) in a THGA furnace. • Effects of the sample/platform dimension and dosing hole on τ were assessed. • Theoretical m0 of 18 analytes were calculated for stopped & mini furnace gas flows. • Experimental

  8. Model calculation of the characteristic mass for convective and diffusive vapor transport in graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bencs, László, E-mail: bencs.laszlo@wigner.mta.hu [Institute for Solid State Physics and Optics, Wigner Research Centre for Physics, Hungarian Academy of Sciences, P.O. Box 49, H-1525 Budapest (Hungary); Laczai, Nikoletta [Institute for Solid State Physics and Optics, Wigner Research Centre for Physics, Hungarian Academy of Sciences, P.O. Box 49, H-1525 Budapest (Hungary); Ajtony, Zsolt [Institute of Food Science, University of West Hungary, H-9200 Mosonmagyaróvár, Lucsony utca 15–17 (Hungary)

    2015-07-01

    A combination of former convective–diffusive vapor-transport models is described to extend the calculation scheme for sensitivity (characteristic mass — m{sub 0}) in graphite furnace atomic absorption spectrometry (GFAAS). This approach encompasses the influence of forced convection of the internal furnace gas (mini-flow) combined with concentration diffusion of the analyte atoms on the residence time in a spatially isothermal furnace, i.e., the standard design of the transversely heated graphite atomizer (THGA). A couple of relationships for the diffusional and convectional residence times were studied and compared, including in factors accounting for the effects of the sample/platform dimension and the dosing hole. These model approaches were subsequently applied for the particular cases of Ag, As, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Ni, Pb, Sb, Se, Sn, V and Zn analytes. For the verification of the accuracy of the calculations, the experimental m{sub 0} values were determined with the application of a standard THGA furnace, operating either under stopped, or mini-flow (50 cm{sup 3} min{sup −1}) of the internal sheath gas during atomization. The theoretical and experimental ratios of m{sub 0}(mini-flow)-to-m{sub 0}(stop-flow) were closely similar for each study analyte. Likewise, the calculated m{sub 0} data gave a fairly good agreement with the corresponding experimental m{sub 0} values for stopped and mini-flow conditions, i.e., it ranged between 0.62 and 1.8 with an average of 1.05 ± 0.27. This indicates the usability of the current model calculations for checking the operation of a given GFAAS instrument and the applied methodology. - Highlights: • A calculation scheme for convective–diffusive vapor loss in GFAAS is described. • Residence time (τ) formulas were compared for sensitivity (m{sub 0}) in a THGA furnace. • Effects of the sample/platform dimension and dosing hole on τ were assessed. • Theoretical m{sub 0} of 18 analytes were

  9. Hydride generation – in-atomizer collection of Pb in a quartz trap-and-atomizer device for atomic absorption spectrometry – an interference study

    Energy Technology Data Exchange (ETDEWEB)

    Novotný, Pavel [Institute of Analytical Chemistry of the ASCR, v.v.i., Veveří 97, 602 00 Brno (Czech Republic); High School in Hořice, Husova 1414, 508 01 Hořice (Czech Republic); Kratzer, Jan, E-mail: jkratzer@biomed.cas.cz [Institute of Analytical Chemistry of the ASCR, v.v.i., Veveří 97, 602 00 Brno (Czech Republic)

    2013-01-01

    Interferences of selected hydride forming elements (As, Sb, Bi, Se and Sn) on lead determination by hydride generation atomic absorption spectrometry were extensively studied in both on-line atomization and preconcentration (collection) modes. The commonly used on-line atomization mode was found free of significant interferences, whereas strong interference from Bi was observed when employing the preconcentration mode with plumbane collection in a quartz trap-and-atomizer device. Interference of Bi seems to take place in the preconcentration step. Interference of Bi in the collection mode cannot be reduced by increased hydrogen radical amount in the trap and/or the atomizer. - Highlights: ► Interference study on Pb determination by in-atomizer trapping was performed for the first time. ► Bi was found as a severe interferent in the preconcentration mode (Pb:Bi ratio 1:100). ► No interference was found in the on-line atomization (no preconcentration). ► Bi interference occurs during preconcentration.

  10. Determination of Trace Iron in High Purity Sodium Fluoride by Graphite Furnace Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    A method is described for the direct determination of iron in high purity sodium fluoride using graphite furnace atomic absorption spectrometry. Interferences caused by the matrix are investigated. It is shown that the ashing temperature can be increased to 1 400°C and matrix interferences eliminated, the sensi tivity of iron increased in 1.27 fold by the addition of nickel nitrate. The method is applied to the determina tion of iron in sodium fluoride and satisfactory results are obtained.

  11. Mineral Analysis the Infusion of Black Tea Samples by Atomic Absorption Spectrometry

    OpenAIRE

    Lahiji N.; Tadayon F.; Tamiji F.; Lahiji A. H.

    2013-01-01

    Tea infusion is one of the most popular drinks around the world. Since tea infusion is known to contain several essential nutrients, it is considered a healthy beverage. In this study eight different Iranian brands of tea infusion and eleven brands imported tea infusion samples from another country for Cu, Zn, Mn and Al were determined by flame atomic absorption spectrometry after wet digestion. The results of analysis showed that the extraction rates of minerals from dry black tea to infusio...

  12. Determination of noble metals by Inductively Coupled Plasma Atomic Emission Spectrometry

    International Nuclear Information System (INIS)

    Full text: It is well known that significant quantities of soluble fission products such as La, Ce, Pr, Eu, Gd, Sm and noble metals such as Ag, Pt, Au, Ru, Rh, Pd are produced in the spent fuel dissolver solutions, in nuclear reactors. The recovery of noble metals from generated high level waste assumes importance in view of their usage in chemical and electronic industries. In the present work, Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) technique has been explored to determine six noble metals in aqueous solutions. Synthetic solution standards containing individually Ag, Au, Pt, Pd, Rh and Ru in the range of 1-500 μg/mL were prepared. Individual elemental solutions at 100μg/mL were fed in to the plasma. The instrumental parameters were obtained for positioning of the analytical line with appropriate sensitivity on the photomultiplier tube. The prominent ICP lines reported in literature in decreasing order of sensitivities for Au are 242.745, 267.895, 197.819, 208.219 nm; Ru are 240.272, 245.657, 267.876 nm; for Rh are 233.477, 249.077, 343.419, 252.053 nm and for Pt are 214.423, 203.646, 214.937 nm respectively. Of these the lines shown in bold are only accessible with the axial ICP unit used in these studies. In addition less sensitive lines in the polyscan mode were chosen, where one can access an elemental line 2.2 nm on either side of the analytical channel provided in polychromator of the instrument. The lines chosen in the polyscan are: Pt 306.471, Ru 249.877 and Rh at 343.489 nm. For Ag and Pd the lines at 328.068 nm and 340.458 nm available with the polychromator of the ICP unit were used. A three point standardization containing the analytes in the concentration range of 0.1 to 200 μg/mL was used. The detection limits determined as per the IUPAC convention for these elements are given. The analytical range for Ag and Pd were 0.05-200 μg/mL while for other elements viz: Au, Pt, Rh and Ru it was 0.5-500 μg/mL . Synthetic samples

  13. An Analytical Model for Adsorption and Diffusion of Atoms/Ions on Graphene Surface

    Directory of Open Access Journals (Sweden)

    Yan-Zi Yu

    2015-01-01

    Full Text Available Theoretical investigations are made on adsorption and diffusion of atoms/ions on graphene surface based on an analytical continuous model. An atom/ion interacts with every carbon atom of graphene through a pairwise potential which can be approximated by the Lennard-Jones (L-J potential. Using the Fourier expansion of the interaction potential, the total interaction energy between the adsorption atom/ion and a monolayer graphene is derived. The energy-distance relationships in the normal and lateral directions for varied atoms/ions, including gold atom (Au, platinum atom (Pt, manganese ion (Mn2+, sodium ion (Na1+, and lithium-ion (Li1+, on monolayer graphene surface are analyzed. The equilibrium position and binding energy of the atoms/ions at three particular adsorption sites (hollow, bridge, and top are calculated, and the adsorption stability is discussed. The results show that H-site is the most stable adsorption site, which is in agreement with the results of other literatures. What is more, the periodic interaction energy and interaction forces of lithium-ion diffusing along specific paths on graphene surface are also obtained and analyzed. The minimum energy barrier for diffusion is calculated. The possible applications of present study include drug delivery system (DDS, atomic scale friction, rechargeable lithium-ion graphene battery, and energy storage in carbon materials.

  14. Direct determination of sodium, potassium, chromium and vanadium in biodiesel fuel by tungsten coil atomic emission spectrometry

    International Nuclear Information System (INIS)

    Graphical abstract: -- Highlights: •Direct analysis of biodiesel on a tungsten coil atomizer. •Determination of Na, K, Cr and V by tungsten coil atomic emission spectrometry. •Sample dilution with methanol or ethanol. •Ten-microliter sample aliquots and limits of detection between 20 and 90 μg kg−1. •Low consumption of reagents, samples and gases in a 140 s per run procedure. -- Abstract: High levels of sodium and potassium can be present in biodiesel fuel and contribute to corrosion, reduced performance and shorter engine lifetime. On the other hand, trace amounts of chromium and vanadium can increase the emission of pollutants during biodiesel combustion. Sample viscosity, immiscibility with aqueous solutions and high carbon content can compromise biodiesel analyzes. In this work, tungsten filaments extracted from microscope light bulbs are used to successively decompose biodiesel's organic matrix, and atomize and excite the analytes to determine sodium, potassium, chromium and vanadium by tungsten coil atomic emission spectrometry (WCAES). No sample preparation other than simple dilution in methanol or ethanol is required. Direct analysis of 10-μL sample aliquots using heating cycles with less than 150 s results in limits of detection (LOD) as low as 20, 70, 70 and 90 μg kg−1 for Na, K, Cr and V, respectively. The procedure's accuracy is checked by determining Na and K in a biodiesel reference sample and carrying out spike experiments for Cr and V. No statistically significant differences were observed between reference and determined values for all analytes at a 95% confidence level. The procedure was applied to three different biodiesel samples and concentrations between 6.08 and 95.6 mg kg−1 for Na and K, and between 0.22 and 0.43 mg kg−1 for V were obtained. The procedure is simple, fast and environmentally friendly. Small volumes of reagents, samples and gases are used and no residues are generated. Powers of detection are comparable to

  15. Direct determination of sodium, potassium, chromium and vanadium in biodiesel fuel by tungsten coil atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dancsak, Stacia E. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Silva, Sidnei G.; Nóbrega, Joaquim A. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, São Carlos, SP (Brazil); Jones, Bradley T. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Donati, George L., E-mail: georgedonati@yahoo.com.br [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States)

    2014-01-02

    Graphical abstract: -- Highlights: •Direct analysis of biodiesel on a tungsten coil atomizer. •Determination of Na, K, Cr and V by tungsten coil atomic emission spectrometry. •Sample dilution with methanol or ethanol. •Ten-microliter sample aliquots and limits of detection between 20 and 90 μg kg{sup −1}. •Low consumption of reagents, samples and gases in a 140 s per run procedure. -- Abstract: High levels of sodium and potassium can be present in biodiesel fuel and contribute to corrosion, reduced performance and shorter engine lifetime. On the other hand, trace amounts of chromium and vanadium can increase the emission of pollutants during biodiesel combustion. Sample viscosity, immiscibility with aqueous solutions and high carbon content can compromise biodiesel analyzes. In this work, tungsten filaments extracted from microscope light bulbs are used to successively decompose biodiesel's organic matrix, and atomize and excite the analytes to determine sodium, potassium, chromium and vanadium by tungsten coil atomic emission spectrometry (WCAES). No sample preparation other than simple dilution in methanol or ethanol is required. Direct analysis of 10-μL sample aliquots using heating cycles with less than 150 s results in limits of detection (LOD) as low as 20, 70, 70 and 90 μg kg{sup −1} for Na, K, Cr and V, respectively. The procedure's accuracy is checked by determining Na and K in a biodiesel reference sample and carrying out spike experiments for Cr and V. No statistically significant differences were observed between reference and determined values for all analytes at a 95% confidence level. The procedure was applied to three different biodiesel samples and concentrations between 6.08 and 95.6 mg kg{sup −1} for Na and K, and between 0.22 and 0.43 mg kg{sup −1} for V were obtained. The procedure is simple, fast and environmentally friendly. Small volumes of reagents, samples and gases are used and no residues are generated

  16. Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS); Validacao de metodologia analitica para determinacao de mercurio total em amostras de urina por espectrometria de absorcao atomica com geracao de vapor frio (CV-AAS)

    Energy Technology Data Exchange (ETDEWEB)

    Guilhen, Sabine Neusatz

    2009-07-01

    Mercury (Hg) is a toxic metal applied to a variety of products and processes, representing a risk to the health of occupationally or accidentally exposed subjects. Dental amalgam is a restorative material composed of metallic mercury, which use has been widely debated in the last decades. Due to the dubiety of the studies concerning dental amalgam, many efforts concerning this issue have been conducted. The Tropical Medicine Foundation (Tocantins, Brazil) has recently initiated a study to evaluate the environmental and occupational levels of exposure to mercury in dentistry attendants at public consulting rooms in the city of Araguaina (TO). In collaboration with this study, the laboratory of analysis at IPEN's Chemistry and Environment Center is undertaking the analysis of mercury levels in exposed subjects' urine samples using cold vapor atomic absorption spectrometry. This analysis requires the definition of a methodology capable of generating reliable results. Such methodology can only be implemented after a rigorous validation procedure. As part of this work, a series of tests were conducted in order to confirm the suitability of the selected methodology and to assert that the laboratory addresses all requirements needed for a successful implementation of the methodology. The following parameters were considered in order to test the method’s performance: detection and quantitation limits, selectivity, sensitivity, linearity, accuracy and precision. The assays were carried out with certified reference material, which assures the traceability of the results. Taking into account the estimated parameters, the method can be considered suitable for the afore mentioned purpose. The mercury concentration found for the reference material was of (95,12 ± 11,70)μg.L{sup -1} with a recovery rate of 97%. The method was also applied to 39 urine samples, six of which (15%) showing urinary mercury levels above the normal limit of 10μg.L{sup −1}. The obtained

  17. Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS); Validacao de metodologia analitica para determinacao de mercurio total em amostras de urina para espectrometria de absorcao atomica com geracao de vapor frio (CV-AAS)

    Energy Technology Data Exchange (ETDEWEB)

    Guilhen, Sabine Neusatz

    2009-07-01

    Mercury (Hg) is a toxic metal applied to a variety of products and processes, representing a risk to the health of occupationally or accidentally exposed subjects. Dental amalgam is a restorative material composed of metallic mercury, which use has been widely debated in the last decades. Due to the dubiety of the studies concerning dental amalgam, many efforts concerning this issue have been conducted. The Tropical Medicine Foundation (Tocantins, Brazil) has recently initiated a study to evaluate the environmental and occupational levels of exposure to mercury in dentistry attendants at public consulting rooms in the city of Araguaina (TO). In collaboration with this study, the laboratory of analysis at IPEN's Chemistry and Environment Center is undertaking the analysis of mercury levels in exposed subjects' urine samples using cold vapor atomic absorption spectrometry. This analysis requires the definition of a methodology capable of generating reliable results. Such methodology can only be implemented after a rigorous validation procedure. As part of this work, a series of tests were conducted in order to confirm the suitability of the selected methodology and to assert that the laboratory addresses all requirements needed for a successful implementation of the methodology. The following parameters were considered in order to test the method's performance: detection and quantitation limits, selectivity, sensitivity, linearity, accuracy and precision. The assays were carried out with certified reference material, which assures the traceability of the results. Taking into account the estimated parameters, the method can be considered suitable for the afore mentioned purpose. The mercury concentration found for the reference material was of (95,12 +- 11,70)mug.L{sup -1} with a recovery rate of 97%. The method was also applied to 39 urine samples, six of which (15%) showing urinary mercury levels above the normal limit of 10{mu}g.L{sup -1}. The

  18. Assessment of resonance ionization mass spectrometry for analytical chemistry and spectroscopy

    International Nuclear Information System (INIS)

    Resonance ionization mass spectrometry (RIMS) is a natural outgrowth of RIS. The result of an RIS process is an ion pair. The electron can be used to detect the process, and single atom detection has been demonstrated by this method. The cation resulting from the RIS process actually carries more easily accessible and useful information (i.e. the mass of the ion). RIMS is useful in mass analysis. The development of RIMS has proceeded along several different directions, using CW or pulsed lasers, narrow or wide band laser energies, different kinds of sample generation, and different kinds of mass separations. RIMS in various forms can be used to obtain either element or isotope selectivity. Even though the RIMS technique has developed along several lines, several things are common to all approaches. Ultimately RIMS requires gaseous, free, atoms. RIMS makes use of the photoionization of these atoms by absorption of photons through allowed transitions involving real energy levels. The ion once formed is detected by standard mass spectrometric techniques

  19. Dielectric barrier discharge plasma atomizer for hydride generation atomic absorption spectrometry-Performance evaluation for selenium

    Science.gov (United States)

    Duben, Ondřej; Boušek, Jaroslav; Dědina, Jiří; Kratzer, Jan

    2015-09-01

    Atomization of selenium hydride in a quartz dielectric barrier discharge (DBD) atomizer was optimized and its performance was compared to that of the externally heated quartz multiatomizer. Argon was found as the best DBD discharge gas employing a flow rate of 75 ml min- 1 Ar while the DBD power was optimized at 14 W. The detection limits reached 0.24 ng ml- 1 Se in the DBD and 0.15 ng ml- 1 Se in the multiatomizer. The tolerance of DBD to interferences is even better than with the multiatomizer.

  20. Pure-rotational spectrometry: a vintage analytical method applied to modern breath analysis.

    Science.gov (United States)

    Hrubesh, Lawrence W; Droege, Michael W

    2013-09-01

    Pure-rotational spectrometry (PRS) is an established method, typically used to study structures and properties of polar gas-phase molecules, including isotopic and isomeric varieties. PRS has also been used as an analytical tool where it is particularly well suited for detecting or monitoring low-molecular-weight species that are found in exhaled breath. PRS is principally notable for its ultra-high spectral resolution which leads to exceptional specificity to identify molecular compounds in complex mixtures. Recent developments using carbon aerogel for pre-concentrating polar molecules from air samples have extended the sensitivity of PRS into the part-per-billion range. In this paper we describe the principles of PRS and show how it may be configured in several different modes for breath analysis. We discuss the pre-concentration concept and demonstrate its use with the PRS analyzer for alcohols and ammonia sampled directly from the breath.

  1. Two low-level gamma spectrometry systems of the IAEA Safeguards Analytical Laboratory

    Energy Technology Data Exchange (ETDEWEB)

    Parus, J.L. [IAEA, SAL, Vienna (Austria); Raab, W. [IAEA, SAL, Vienna (Austria); Donohue, D. [IAEA, SAL, Vienna (Austria); Jansta, V. [IAEA, SAL, Vienna (Austria); Kierzek, J. [IAEA, SAL, Vienna (Austria)

    1997-03-01

    A gamma spectrometry system designed for the measurement of samples with low and medium radioactivity (activity from a few to about 10{sup 4} Bq in the energy range from 25 to 2700 keV) has been installed at the IAEA Safeguards Analytical Laboratory in Seibersdorf. The system consists of 3 low level detectors: (1) n-type coaxial Ge with 42.4% relative efficiency, 1.85 keV FWHM at 1.33 MeV (2) planar Ge with 2000 mm{sup 2} area and 20 mm thickness, 562 eV FWHM at 122 keV (3) NaI(Tl) annulus of 25.4 cm diameter and 25.4 cm height, hole diameter 90 mm. (orig./DG)

  2. Analytical developments in thermal ionization mass spectrometry for the isotopic analysis of very small amounts

    International Nuclear Information System (INIS)

    In the framework of the French transmutation project of nuclear wastes, experiments consisted in the irradiation in a fast neutron reactor of few milligrams of isotopically enriched powders. Hence, the isotopic analysis of very small amount of irradiation products is one of the main issues. The aim of this study was to achieve analytical developments in thermal ionization mass spectrometry in order to accurately analyze these samples. Several axes were studied including the new total evaporation method, deposition techniques, electron multiplier potentialities and comparison between different isotope measurement techniques. Results showed that it was possible to drastically decrease the amounts needed for analysis, especially with Eu and Nd, while maintaining an uncertainty level in agreement with the project requirements. (author)

  3. Analytical Validation of Accelerator Mass Spectrometry for Pharmaceutical Development: the Measurement of Carbon-14 Isotope Ratio.

    Energy Technology Data Exchange (ETDEWEB)

    Keck, B D; Ognibene, T; Vogel, J S

    2010-02-05

    Accelerator mass spectrometry (AMS) is an isotope based measurement technology that utilizes carbon-14 labeled compounds in the pharmaceutical development process to measure compounds at very low concentrations, empowers microdosing as an investigational tool, and extends the utility of {sup 14}C labeled compounds to dramatically lower levels. It is a form of isotope ratio mass spectrometry that can provide either measurements of total compound equivalents or, when coupled to separation technology such as chromatography, quantitation of specific compounds. The properties of AMS as a measurement technique are investigated here, and the parameters of method validation are shown. AMS, independent of any separation technique to which it may be coupled, is shown to be accurate, linear, precise, and robust. As the sensitivity and universality of AMS is constantly being explored and expanded, this work underpins many areas of pharmaceutical development including drug metabolism as well as absorption, distribution and excretion of pharmaceutical compounds as a fundamental step in drug development. The validation parameters for pharmaceutical analyses were examined for the accelerator mass spectrometry measurement of {sup 14}C/C ratio, independent of chemical separation procedures. The isotope ratio measurement was specific (owing to the {sup 14}C label), stable across samples storage conditions for at least one year, linear over 4 orders of magnitude with an analytical range from one tenth Modern to at least 2000 Modern (instrument specific). Further, accuracy was excellent between 1 and 3 percent while precision expressed as coefficient of variation is between 1 and 6% determined primarily by radiocarbon content and the time spent analyzing a sample. Sensitivity, expressed as LOD and LLOQ was 1 and 10 attomoles of carbon-14 (which can be expressed as compound equivalents) and for a typical small molecule labeled at 10% incorporated with {sup 14}C corresponds to 30 fg

  4. Speciation analysis of thallium using solid phase extraction and electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. Thallium is a heavy, very toxic metallic element, which occurs in earth's crust in an estimated abundance from 0.1 to 0.8 mg.kg-1. In the environment, it is mainly combined with other elements (primarily oxygen, sulfur, halogens, potassium and rubidium) in inorganic compounds. During the weathering processes it can be mobilized by aqueous media and accumulated in sediments and soils. The main sources of pollution nowadays come from anthropogenic emissions from refineries, coal-fired power stations, mining activities, metal smelters and the cement industry. Thallium exists in natural waters as either Tl(I) (thallous) or Tl(III) (thallic) species. The oxidation state of Tl affects its complexation and subsequent bioavailability and toxicity in the environment. Thallium content in surface waters is within the range 1-82 ng l-1. Due to this low contents of Tl in water samples, it is necessary to combine the laboratory separation, preconcentration and determination techniques for the purpose of Tl speciation analysis. The scope of the presented work was to use an solid phase extraction (SPE) for the separation and preconcentration of Tl species in water samples followed by the determination using electrothermal atomic absorption spectrometry (ET AAS). In this method, Tl(III) was stabilized by formation of a Tl(III)-DTPA complex. Tl(I) species remained in its original form. These two species were then separated by using a cation exchange resin Amberlite IR120 and nitric acid as the eluent in a batch SPE protocol. The potential interferences of Fe (III), Al, Ca, Mg and other metals were investigated. The optimized experimental conditions for separation/preconcentration step (pH 2-3, time 15 min, temperature 60 deg C) and Zeeman ET AAS determination (chemical modifier Pd + ascorbic acid, atomization temperature 2100 deg C) were used for the speciation analysis of thallium in filtered acid water samples from open quartzite mine in the

  5. Analytic method development to quantify by in-situ gamma spectrometry radionuclides in the ground

    International Nuclear Information System (INIS)

    This research thesis reports the development of an analytic method based on a Monte Carlo simulation to quantify radionuclides present in soils by means of in-situ gamma spectrometry, to understand physical phenomena involved before and after detection, and to improve and complement results after spectrum analysis. The first part describes the evolution of in-situ gamma spectrometry: sensor development, in-situ measurement principle, evolution of the analysis principle. The second part introduces the Monte Carlo simulation and describes the used models (sensor model using the stripping method, development of a new simulation model for the incident flow). The third part discusses the understanding of an in-situ spectrum with the localization of the origin of incident photons and the identification of measurement parameters. Modelling results are then presented, as well as the development of spectrum de-convolution method, and the calculation of dose factors. Finally, the use of the 'Peak-to-Valley' method completed by the Monte Carlo simulation results is explained and used to localize a source depth and to define the exponential distribution of Cs-137 in Orsay

  6. Solvent microextraction-flame atomic absorption spectrometry (SME-FAAS) for determination of ultratrace amounts of cadmium in meat and fish samples.

    Science.gov (United States)

    Goudarzi, Nasser

    2009-02-11

    A simple, low cost and highly sensitive method based on solvent microextraction (SME) for separation/preconcentration and flame atomic absorption spectrometry (FAAS) was proposed for the determination of ultratrace amounts of cadmium in meat and fish samples. The analytical procedure involved the formation of a hydrophobic complex by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution. In suitable conditions, the complex of cadmium-APDC entered the micro organic phase, and thus, separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, a detection limit (3 sigma) of 0.8 ng L(-1) and an enrichment factor of 93 were achieved. The relative standard deviation for the method was found to be 2.2% for Cd. The interference effects of some anions and cations were also investigated. The developed method has been applied to the determination of trace Cd in meat and fish samples. PMID:19138082

  7. Electrochemical preconcentration and hydride generation methods for trace determination of selenium by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The use of atomic absorption spectrometry in combination with two different preconcentration/separation techniques for the determination of trace concentrations of selenium is described. Electrochemical preconcentration onto a platinum electrode with a subsequent atomization of selenium is discussed briefly. Several parameters are considered such as the presence of depolarizers, and the temperature of the electrolyzed solutions. Special attention is payed to the efficiency of the atomization step, and a method to improve this is proposed. Applications of the technique to real samples are also reported. Secondly, the separation of the selenium as the volatile selenium hydride from the sample solution is considered. Several papers in this thesis deal with commonly occurring interferants as nickel and copper and with ways of minimizing or avoiding the interferring effects, whereas other papers relate to more theoretical aspects of the hydride generation process. New methods for the determination of selenium in technical samples with high contents of nickel and copper are also presented

  8. Alternative approaches to correct interferences in the determination of boron in shrimps by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The aim of this study is to propose alternative techniques and methods in combination with the classical chemical modification to correct the major matrix interferences in the determination of boron in shrimps. The performance of an internal standard (Ge) for the determination of boron by the simultaneous multi-element atomic absorption spectrometry was tested. The use of internal standardization increased the recovery from 85.9% to 101% and allowed a simple correction of errors during sampling preparation and heating process. Furthermore, a new preparation procedure based on the use of citric acid during digestion and dilution steps improved the sensitivity of the method and decreased the limit of detection. Finally, a comparative study between the simultaneous multi-element atomic absorption spectrometry with a longitudinal Zeeman-effect background correction system, equipped with a transversely-heated graphite atomizer and the single element atomic absorption spectrometry with a D2 background correction system, equipped with an end-heated graphite atomizer was undertaken to investigate the different behavior of boron in both techniques. Different chemical modifiers for the determination of boron were tested with both techniques. Ni-citric acid and Ca were the optimal chemical modifiers when simultaneous multi-element atomic absorption spectrometry and single-element atomic absorption spectrometry were used, respectively. By using the single-element atomic absorption spectrometry, the calculated characteristic mass was 220 pg and the calculated limit of detection was 370 μg/kg. On the contrary, with simultaneous multi-element atomic absorption spectrometry, the characteristic mass was 2200 pg and the limit of detection was 5.5 mg/kg. - Highlights: • New approaches were developed to cope with interferences of B determination by ETAAS • Ge was used as internal standard for the determination of B by simultaneous ETAAS • Citric acid was used during digestion

  9. Alternative approaches to correct interferences in the determination of boron in shrimps by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Pasias, I.N.; Pappa, Ch.; Katsarou, V.; Thomaidis, N.S., E-mail: ntho@chem.uoa.gr; Piperaki, E.A.

    2014-02-01

    The aim of this study is to propose alternative techniques and methods in combination with the classical chemical modification to correct the major matrix interferences in the determination of boron in shrimps. The performance of an internal standard (Ge) for the determination of boron by the simultaneous multi-element atomic absorption spectrometry was tested. The use of internal standardization increased the recovery from 85.9% to 101% and allowed a simple correction of errors during sampling preparation and heating process. Furthermore, a new preparation procedure based on the use of citric acid during digestion and dilution steps improved the sensitivity of the method and decreased the limit of detection. Finally, a comparative study between the simultaneous multi-element atomic absorption spectrometry with a longitudinal Zeeman-effect background correction system, equipped with a transversely-heated graphite atomizer and the single element atomic absorption spectrometry with a D{sub 2} background correction system, equipped with an end-heated graphite atomizer was undertaken to investigate the different behavior of boron in both techniques. Different chemical modifiers for the determination of boron were tested with both techniques. Ni-citric acid and Ca were the optimal chemical modifiers when simultaneous multi-element atomic absorption spectrometry and single-element atomic absorption spectrometry were used, respectively. By using the single-element atomic absorption spectrometry, the calculated characteristic mass was 220 pg and the calculated limit of detection was 370 μg/kg. On the contrary, with simultaneous multi-element atomic absorption spectrometry, the characteristic mass was 2200 pg and the limit of detection was 5.5 mg/kg. - Highlights: • New approaches were developed to cope with interferences of B determination by ETAAS • Ge was used as internal standard for the determination of B by simultaneous ETAAS • Citric acid was used during

  10. Arsenic in marine tissues — The challenging problems to electrothermal and hydride generation atomic absorption spectrometry

    Science.gov (United States)

    Karadjova, Irina B.; Petrov, Panayot K.; Serafimovski, Ivan; Stafilov, Trajče; Tsalev, Dimiter L.

    2007-03-01

    Analytical problems in determination of arsenic in marine tissues are addressed. Procedures for the determination of total As in solubilized or extracted tissues with tetramethylammonium hydroxide and methanol have been elaborated. Several typical lyophilized tissues were used: NIST SRM 1566a 'Oyster Tissue', BCR-60 CRM 'Trace Elements in an Aquatic Plant ( Lagarosiphon major)', BCR-627 'Forms of As in Tuna Fish Tissue', IAEA-140/TM 'Sea Plant Homogenate', NRCC DOLT-1 'Dogfish Liver' and two representatives of the Black Sea biota, Mediterranean mussel ( Mytilus galloprovincialis) and Brown algae ( Cystoseira barbata). Tissues (nominal 0.3 g) were extracted in tetramethylammonium hydroxide (TMAH) 1 ml of 25% m/v TMAH and 2 ml of water) or 5 ml of aqueous 80% v/v methanol (MeOH) in closed vessels in a microwave oven at 50 °C for 30 min. Arsenic in solubilized or extracted tissues was determined by electrothermal atomic absorption spectrometry (ETAAS) after appropriate dilution (nominally to 25 ml, with further dilution as required) under optimal instrumental parameters (pyrolysis temperature 900 °C and atomization temperature 2100 °C) with 1.5 μg Pd as modifier on Zr-Ir treated platform. Platforms have been pre-treated with 2.7 μmol of zirconium and then with 0.10 μmol of iridium which served as a permanent chemical modifier in direct ETAAS measurements and as an efficient hydride sequestration medium in flow injection hydride generation (FI-HG)-ETAAS. TMAH and methanol extract 96-108% and 51-100% of As from CRMs. Various calibration approaches have been considered and critically evaluated. The effect of species-dependent slope of calibration graph or standard additions plot for total As determination in a sample comprising of several individual As species with different ETAAS behavior has been considered as a kind of 'intrinsic element speciation interference' that cannot be completely overcome by standard additions technique. Calibration by means of CRMs has

  11. Arsenic in marine tissues - The challenging problems to electrothermal and hydride generation atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Karadjova, Irina B.; Petrov, Panayot K. [Faculty of Chemistry, University of Sofia, 1 James Bourchier Blvd., Sofia 1164 (Bulgaria); Serafimovski, Ivan [Food Institute, Faculty of Veterinary Medicine, Sts. Cyril and Methodius University, P.O. Box 95, MK-1000, Skopje (Macedonia, The Former Yugoslav Republic of); Stafilov, Trajce [Institute of Chemistry, Faculty of Science, Sts. Cyril and Methodius University, P.O. Box 162, MK-1000, Skopje (Macedonia, The Former Yugoslav Republic of); Tsalev, Dimiter L. [Faculty of Chemistry, University of Sofia, 1 James Bourchier Blvd., Sofia 1164 (Bulgaria)], E-mail: tsalev@chem.uni-sofia.bg

    2007-03-15

    Analytical problems in determination of arsenic in marine tissues are addressed. Procedures for the determination of total As in solubilized or extracted tissues with tetramethylammonium hydroxide and methanol have been elaborated. Several typical lyophilized tissues were used: NIST SRM 1566a 'Oyster Tissue', BCR-60 CRM 'Trace Elements in an Aquatic Plant (Lagarosiphon major)', BCR-627 'Forms of As in Tuna Fish Tissue', IAEA-140/TM 'Sea Plant Homogenate', NRCC DOLT-1 'Dogfish Liver' and two representatives of the Black Sea biota, Mediterranean mussel (Mytilus galloprovincialis) and Brown algae (Cystoseira barbata). Tissues (nominal 0.3 g) were extracted in tetramethylammonium hydroxide (TMAH) 1 ml of 25% m/v TMAH and 2 ml of water) or 5 ml of aqueous 80% v/v methanol (MeOH) in closed vessels in a microwave oven at 50 deg. C for 30 min. Arsenic in solubilized or extracted tissues was determined by electrothermal atomic absorption spectrometry (ETAAS) after appropriate dilution (nominally to 25 ml, with further dilution as required) under optimal instrumental parameters (pyrolysis temperature 900 deg. C and atomization temperature 2100 deg. C) with 1.5 {mu}g Pd as modifier on Zr-Ir treated platform. Platforms have been pre-treated with 2.7 {mu}mol of zirconium and then with 0.10 {mu}mol of iridium which served as a permanent chemical modifier in direct ETAAS measurements and as an efficient hydride sequestration medium in flow injection hydride generation (FI-HG)-ETAAS. TMAH and methanol extract 96-108% and 51-100% of As from CRMs. Various calibration approaches have been considered and critically evaluated. The effect of species-dependent slope of calibration graph or standard additions plot for total As determination in a sample comprising of several individual As species with different ETAAS behavior has been considered as a kind of 'intrinsic element speciation interference' that cannot be completely

  12. Simultaneous flow injection preconcentration of lead and cadmium using cloud point extraction and determination by atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Edson Luiz [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, Av. Centenario, 303, CP 96, 13416-000 Piracicaba, SP (Brazil)], E-mail: edsonqmc@hotmail.com; Santos Roldan, Paulo dos [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, Av. Centenario, 303, CP 96, 13416-000 Piracicaba, SP (Brazil)

    2009-01-15

    A flow injection (FI) micelle-mediated separation/preconcentration procedure for the determination of lead and cadmium by flame atomic absorption spectrometry (FAAS) has been proposed. The analytes reacted with 1-(2-thiazolylazo)-2-naphthol (TAN) to form hydrophobic chelates, which were extracted into the micelles of 0.05% (w/v) Triton X-114 in a solution buffered at pH 8.4. In the preconcentration stage, the micellar solution was continuously injected into a flow system with four mini-columns packed with cotton, glass wool, or TNT compresses for phase separation. The analytes-containing micelles were eluted from the mini-columns by a stream of 3 mol L{sup -1} HCl solution and the analytes were determined by FAAS. Chemical and flow variables affecting the preconcentration of the analytes were studied. For 15 mL of preconcentrated solution, the enhancement factors varied between 15.1 and 20.3, the limits of detection were approximately 4.5 and 0.75 {mu}g L{sup -1} for lead and cadmium, respectively. For a solution containing 100 and 10 {mu}g L{sup -1} of lead and cadmium, respectively, the R.S.D. values varied from 1.6 to 3.2% (n = 7). The accuracy of the preconcentration system was evaluated by recovery measurements on spiked water samples. The method was susceptible to matrix effects, but these interferences were minimized by adding barium ions as masking agent in the sample solutions, and recoveries from spiked sample varied in the range of 95.1-107.3%.

  13. Simultaneous flow injection preconcentration of lead and cadmium using cloud point extraction and determination by atomic absorption spectrometry.

    Science.gov (United States)

    Silva, Edson Luiz; Roldan, Paulo Dos Santos

    2009-01-15

    A flow injection (FI) micelle-mediated separation/preconcentration procedure for the determination of lead and cadmium by flame atomic absorption spectrometry (FAAS) has been proposed. The analytes reacted with 1-(2-thiazolylazo)-2-naphthol (TAN) to form hydrophobic chelates, which were extracted into the micelles of 0.05% (w/v) Triton X-114 in a solution buffered at pH 8.4. In the preconcentration stage, the micellar solution was continuously injected into a flow system with four mini-columns packed with cotton, glass wool, or TNT compresses for phase separation. The analytes-containing micelles were eluted from the mini-columns by a stream of 3molL(-1) HCl solution and the analytes were determined by FAAS. Chemical and flow variables affecting the preconcentration of the analytes were studied. For 15mL of preconcentrated solution, the enhancement factors varied between 15.1 and 20.3, the limits of detection were approximately 4.5 and 0.75microgL(-1) for lead and cadmium, respectively. For a solution containing 100 and 10microgL(-1) of lead and cadmium, respectively, the R.S.D. values varied from 1.6 to 3.2% (n=7). The accuracy of the preconcentration system was evaluated by recovery measurements on spiked water samples. The method was susceptible to matrix effects, but these interferences were minimized by adding barium ions as masking agent in the sample solutions, and recoveries from spiked sample varied in the range of 95.1-107.3%. PMID:18456398

  14. Application of methane as a gaseous modifier for the determination of silicon using electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Heinrich, Hans-Joachim, E-mail: hans-joachim.heinrich@bam.de; Kipphardt, Heinrich

    2012-04-15

    For determination of silicon in aqueous solutions by electrothermal atomic absorption spectrometry methane/argon mixtures as a gaseous modifier were applied during the pyrolysis step to improve the analytical performance. The beneficial effects observed on thermal stabilization, signal enhancement and shape of absorbance signals were attributed to the thermal decomposition products of methane, which were hydrogen and carbon black (soot). Using a 5% CH{sub 4} mixture with argon, the optimized pyrolysis and atomization temperatures were 1350 Degree-Sign C and 2450 Degree-Sign C, respectively. A flushing step following the pyrolysis was mandatory to avoid background absorption and accelerated deposition of pyrolytic graphite. Characteristic masses of 50 and 30 pg were obtained for standard transversely heated graphite atomizer (THGA) tubes and end-capped THGA tubes, respectively, which were lower than with other previously applied modifiers. A limit of detection of 0.2 {mu}g L{sup -1} (3 s, n = 10) has been obtained. In addition, this gaseous modifier did not contribute to contamination which often was significant when a liquid modifier solution was co-injected. The proposed method has been applied to the determination of silicon in ultrapure water, nitric and hydrochloric acids. - Highlights: Black-Right-Pointing-Pointer CH{sub 4}/Ar gas mixtures act as new modifier in the determination of Si using ET AAS. Black-Right-Pointing-Pointer CH{sub 4} improved thermal stabilization, atomization efficiency and signal shape of Si. Black-Right-Pointing-Pointer Optimum performance by addition of 5% CH{sub 4} during pyrolysis at 1350 Degree-Sign C. Black-Right-Pointing-Pointer Gaseous modifier does not contribute to blank values. Black-Right-Pointing-Pointer Optimized method suitable for determination of Si in ultrapure reagents.

  15. Determination of silicon and aluminum in silicon carbide nanocrystals by high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Dravecz, Gabriella; Bencs, László; Beke, Dávid; Gali, Adam

    2016-01-15

    The determination of Al contaminant and the main component Si in silicon carbide (SiC) nanocrystals with the size-distribution of 1-8nm dispersed in an aqueous solution was developed using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS). The vaporization/atomization processes were investigated in a transversally heated graphite atomizer by evaporating solution samples of Al and Si preserved in various media (HCl, HNO3). For Si, the best results were obtained by applying a mixture of 5µg Pd plus 5µg Mg, whereas for Al, 10µg Mg (each as nitrate solution) was dispensed with the samples, but the results obtained without modifier were found to be better. This way a maximum pyrolysis temperature of 1200°C for Si and 1300°C for Al could be used, and the optimum (compromise) atomization temperature was 2400°C for both analytes. The Si and Al contents of different sized SiC nanocrystals, dispersed in aqueous solutions, were determined against aqueous (external) calibration standards. The correlation coefficients (R values) of the calibrations were found to be 0.9963 for Si and 0.9991 for Al. The upper limit of the linear calibration range was 2mg/l Si and 0.25mg/l Al. The limit of detection was 3µg/l for Si and 0.5µg/l for Al. The characteristic mass (m0) was calculated to be 389pg Si and 6.4pg Al. The Si and Al content in the solution samples were found to be in the range of 1.0-1.7mg/l and 0.1-0.25mg/l, respectively.

  16. In-situ vaporization and matrix removal for the determination of rare earth impurities in zirconium dioxide by electrothermal vaporization inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    A novel method for the determination of trace rare earth impurities in ZrO2 powder has been developed based on electrothermal vaporization inductively coupled plasma atomic emission spectrometry. A polytetrafluoroethylene slurry was used as a fluorinating reagent to convert both the matrix (Zr) and the analytes (rare earth elements) into fluorides with different volatilities at a high temperature in a graphite furnace. The more volatile ZrF4 was removed in-situ by selective vaporization prior to the determination of the analytes, removing matrix spectral interferences. Under optimum operating conditions, the absolute detection limits of the analytes varied from 0.04 ng (Yb) to 0.50 ng (Pr) with relative standard deviations less than 5%. The recommended approach has been successfully applied to the determination of trace rare earth impurities (La, Pr, Eu, Gd, Ho and Yb) in ZrO2 powder and the results were in good agreement with those obtained by pneumatic nebulization inductively coupled plasma atomic emission spectrometry after the separation of the matrix using a solvent extraction procedure

  17. Plasma jet desorption atomization-atomic fluorescence spectrometry and its application to mercury speciation by coupling with thin layer chromatography.

    Science.gov (United States)

    Liu, Zhifu; Zhu, Zhenli; Zheng, Hongtao; Hu, Shenghong

    2012-12-01

    A novel plasma jet desorption atomization (PJDA) source was developed for atomic fluorescence spectrometry (AFS) and coupled on line with thin layer chromatography (TLC) for mercury speciation. An argon dielectric barrier discharge plasma jet, which is generated inside a 300 μm quartz capillary, interacts directly with the sample being analyzed and is found to desorb and atomize surface mercury species rapidly. The effectiveness of this PJDA surface sampling technique was demonstrated by measuring AFS signals of inorganic Hg(2+), methylmercury (MeHg), and phenylmercury (PhHg) deposited directly on TLC plate. The detection limits of the proposed PJDA-AFS method for inorganic Hg(2+), MeHg, and PhHg were 0.51, 0.29, and 0.34 pg, respectively, and repeatability was 4.7%, 2.2%, and 4.3% for 10 pg Hg(2+), MeHg, and PhHg. The proposed PJDA-AFS was also successfully coupled to TLC for mercury speciation. Under optimized conditions, the measurements of mercury dithizonate (Hg-D), methylmercury dithizonate (MeHg-D), and phenylmercury dithizonate (PhHg-D) could be achieved within 3 min with detection limits as low as 8.7 pg. The combination of TLC with PJDA-AFS provides a simple, cost-effective, relatively high-throughput way for mercury speciation. PMID:23153091

  18. Analytical chemistry

    International Nuclear Information System (INIS)

    This book is comprised of nineteen chapters, which describes introduction of analytical chemistry, experimental error and statistics, chemistry equilibrium and solubility, gravimetric analysis with mechanism of precipitation, range and calculation of the result, volume analysis on general principle, sedimentation method on types and titration curve, acid base balance, acid base titration curve, complex and firing reaction, introduction of chemical electro analysis, acid-base titration curve, electrode and potentiometry, electrolysis and conductometry, voltammetry and polarographic spectrophotometry, atomic spectrometry, solvent extraction, chromatograph and experiments.

  19. Determination of platinum and palladium in road dust after their separation on immobilized fungus by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Woinska, Sylwia; Godlewska-Zylkiewicz, Beata, E-mail: bgodlew@uwb.edu.pl

    2011-07-15

    A flow solid phase extraction procedure based on biosorption of Pt(IV) and Pd(II) on Aspergillus sp. immobilized on cellulose resin Cellex-T was proposed for the separation and preconcentration of Pt and Pd before their determination by electrothermal atomic absorption spectrometry (ETAAS). The analytical conditions including sample pH, eluent type, flow rates of sample and eluent solutions were examined. The analytes were selectively retained on the biosorbent in acidic medium (pH 1) and subsequently eluted from the column with 1 mL of thiourea solution (0.25 mol L{sup -1} thiourea in 0.3 mol L{sup -1} HCl). The reproducibility of the procedure was below 5%. The limit of detection of the method was 0.020 ng mL{sup -1} for Pt and 0.012 ng mL{sup -1} for Pd. The method validation was performed by analysis of certified reference materials BCR-723 (tunnel dust) and SARM-76 (platinum ore). The developed separation procedure was applied to the determination of Pt and Pd in road dust samples by ETAAS. The applied biosorbent is characterized by high sorption capacity: 0.47 mg g{sup -1} for Pt and 1.24 mg g{sup -1} for Pd.

  20. Cloud point extraction for the determination of copper, nickel and cobalt ions in environmental samples by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ghaedi, M. [Chemistry Department, University of Yasouj, Yasouj 75914-353 (Iran, Islamic Republic of)], E-mail: m_ghaedi@mail.yu.ac.ir; Shokrollahi, A.; Ahmadi, F.; Rajabi, H.R. [Chemistry Department, University of Yasouj, Yasouj 75914-353 (Iran, Islamic Republic of); Soylak, M. [Chemistry Department, University of Erciyes, 38039 Kayseri (Turkey)

    2008-02-11

    A cloud point extraction procedure was presented for the preconcentration of copper, nickel and cobalt ions in various samples. After complexation with methyl-2-pyridylketone oxime (MPKO) in basic medium, analyte ions are quantitatively extracted to the phase rich in Triton X-114 following centrifugation. 1.0 mol L{sup -1} HNO{sub 3} nitric acid in methanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The adopted concentrations for MPKO, Triton X-114 and HNO{sub 3}, bath temperature, centrifuge rate and time were optimized. Detection limits (3 SDb/m) of 1.6, 2.1 and 1.9 ng mL{sup -1} for Cu{sup 2+}, Co{sup 2+} and Ni{sup 2+} along with preconcentration factors of 30 and for these ions and enrichment factor of 65, 58 and 67 for Cu{sup 2+}, Ni{sup 2+} and Co{sup 2+}, respectively. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed procedure was applied to the analysis of biological, natural and wastewater, soil and blood samples.

  1. Observations on the quantitation of the phosphate content of peptides by fast-atom bombardment mass spectrometry.

    Science.gov (United States)

    Poulter, L; Ang, S G; Williams, D H; Cohen, P

    1987-07-29

    Equimolar mixtures of the phosphorylated and dephosphorylated forms of several peptides have been subjected to fast-atom bombardment mass spectrometry (FABMS), to investigate whether the stoichiometry of phosphorylation can be determined from the relative molecular-ion abundances of the phospho and dephospho derivatives. It is concluded that quantitation can be achieved for peptides with large positive or negative hydrophobicity/hydrophilicity indices (delta F values) where addition of a phosphate group does not alter the distribution of the peptide within the matrix significantly. For peptides with small positive or negative delta F values, phosphopeptides tend to be partially suppressed by their dephosphorylated counterparts. Suppression can be partially or totally overcome by conversion of the peptide to a hydrophobic derivative, and by the selection of an appropriate matrix. Alternatively, addition of a very strong acid, perchloric acid, can even reverse the original suppression effect. This last effect is believed to be due to the increased ionic strength in the matrix, which forces a relatively hydrophilic analyte to the matrix surface; and the ability of such a phosphorylated analyte to form a more stable gas-phase cation. PMID:3038197

  2. Dispersive Liquid-Liquid Microextraction of Bismuth in Various Samples and Determination by Flame Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    Teslima Daşbaşı

    2016-01-01

    Full Text Available A dispersive liquid-liquid microextraction method for the determination of bismuth in various samples by flame atomic absorption spectrometry is described. In this method, crystal violet was used as counter positive ion for BiCl4- complex ion, chloroform as extraction solvent, and ethanol as disperser solvent. The analytical parameters that may affect the extraction efficiency like acidity of sample, type and amount of extraction and disperser solvents, amount of ligand, and extraction time were studied in detail. The effect of interfering ions on the analyte recovery was also investigated. The calibration graph was linear in the range of 0.040–1.00 mg L−1 with detection limit of 4.0 μg L−1 (n=13. The precision as relative standard deviation was 3% (n=11, 0.20 mg L−1 and the enrichment factor was 74. The developed method was applied successfully for the determination of bismuth in various water, pharmaceutical, and cosmetic samples and the certified reference material (TMDA-64 lake water.

  3. Trapping and diffusion of noble gas atoms in some off-stoichiometric ceramics studied by thermal desorption spectrometry. Doctoral thesis

    Energy Technology Data Exchange (ETDEWEB)

    Hoondert, W.H.B.

    1993-01-01

    The thesis deals with the mobility of small noble gas atoms, mainly helium, in ceramic materials with high defect concentrations. Hence, two subjects are covered: diffusion and defect physics. The experimental technique employed is Thermal Desorption Spectrometry (TDS). An introductory outline of TDS is given. The present study was initiated for various reasons. First of all, research on helium retention and mobility behavior, such as bubble nucleation and subsequent bubble migration, in potential fusion reactor wall materials (which some of the ceramics are) is of practical interest. Secondly, because the ceramic materials investigated in the present work have defect concentrations on the order of percents, and because they are binary compounds where in principle more defect types can be present than in pure materials, the defect physics is more complicated and diverse than e.g., in simple metals. Finally, high defective materials can serve as a model system for thin films produced by Ion Beam Assisted Deposition (IBAD). TDS as an analytical tool is of key importance to be able to control the IBAD process, and for the understanding of the atomic-scale phenomena involved.

  4. Self-interstitial configuration in molybdenum studied by modified analytical embedded atom method

    Indian Academy of Sciences (India)

    Jian-Min Zhang; Zhang Fang Wang; Ke-Wei Xu

    2009-05-01

    The stability of various atomic configurations containing a self-interstitial atom (SIA) in a model representing Mo has been investigated using the modified analytical embedded atom method (MAEAM). The lattice relaxations are treated with the molecular dynamics (MD) simulation at absolute zero of temperature. Six relatively stable self-interstitial configurations and formation energies have been described and calculated. The results indicate that the [1 1 1] dumbbell interstitial S111 has the lowest formation energy, and in ascending order, the sequence of the configurations is predicted to be S111, C, S110, T, S001 and O. From relaxed displacement field up to the fifth-NN atoms of six configurations, we know that the relaxed displacements depend not only on separation distances of the NN atoms from the defect centre but also strongly on the direction of the connected line between the NN atoms and the defect centre. The equilibrium distances between two nearest atoms in the core of the S111, C, S110, T, S001 and O configurations are 0.72a, 0.72a, 0.71a, 0.72a, 0.70a and 0.70a, respectively.

  5. Analytic solution and pulse area theorem for three-level atoms

    Science.gov (United States)

    Shchedrin, Gavriil; O'Brien, Chris; Rostovtsev, Yuri; Scully, Marlan O.

    2015-12-01

    We report an analytic solution for a three-level atom driven by arbitrary time-dependent electromagnetic pulses. In particular, we consider far-detuned driving pulses and show an excellent match between our analytic result and the numerical simulations. We use our solution to derive a pulse area theorem for three-level V and Λ systems without making the rotating wave approximation. Formulated as an energy conservation law, this pulse area theorem can be used to understand pulse propagation through three-level media.

  6. Calculation of phonon spectrum for noble metals by modified analytic embedded atom method (MAEAM)

    Institute of Scientific and Technical Information of China (English)

    Zhang Xiao-Jun; Zhang Jian-Min; Xu Ke-Wei

    2006-01-01

    In the harmonic approximation, the atomic force constants are derived and the phonon dispersion curves along four major symmetry directions [00ζ], [0ζζ], [ζζζ] and [0ζ1] (or △, ∑, A and Z in group-theory notation) are calculated for four noble metals Cu, Ag, Au and Pt by combining the modified analytic embedded atom method (MAEAM) with the theory of lattice dynamics. A good agreement between calculations and measurements, especially for lower frequencies,shows that the MAEAM provides a reasonable description of lattice dynamics in noble metals.

  7. Inductively Coupled Plasma(ICP) Mass Spectrometry(MS) Hyphenated with Atomic Emission Spectrometry(AES) for Simultaneous Determination of Major, Minor and Micro Amounts of Elements in Geochemical Samples

    Institute of Scientific and Technical Information of China (English)

    HUANG Zhen-yu; ZHANG Qin; HU Ke; WU Jian-ling; YANG Peng-yuan

    2005-01-01

    @@ Introduction Geological resource survey demands for determining various constituents including major, minor, micro, trace and ultra-trace levels of elements for preparing the map of resource distribution of our country. As a powerful and popularly used technique for multi-element analysis, inductively coupled plasma(ICP) atomic emission spectrometry (AES) has been applied to this field for a period of time[1-3]. However, ICP spectrometric determination of those micro, trace and ultratrace elements needs enrichment procedures for improving the detection limit, which is unacceptable in case a great mass of samples should be analyzed as that in the task of geological resource survey. On the other hand, although ICP mass spectrometry(MS) is considered the most powerful method for trace elements determination[4,5], it is difficult for ICP-MS to be used to determine the trace and major analytes simultaneously in a spectrum.

  8. Determination of the elemental composition of cyanobacteria cells and cell fractions by atomic emission and atomic absorption spectrometry

    International Nuclear Information System (INIS)

    An approach to studying the elemental composition of cyanobacteria Spirulina platensis and Nostoc commune using a set of complementary analytical methods (ICP-AES, PAAS, and ETAAS) was proposed . The procedures were adapted for the determination of macro- and microelements (Na, K, Mg, Ca, Fe, Mn, Cu, Mo, Zn, B, and Se) in the biomass of cyanobacteria and separated cell fractions (chloroform and water-methanol extracts and precipitates). The conditions for the mineralization of biological materials were optimized for autoclave and microwave sample preparation procedures. The evaporation and atomization of Se and Mo in a graphite furnace in the presence of chloroform and methanol were studied

  9. Analytical and processing methodologies for non-target screening by coupling passive sampling and high resolution mass spectrometry

    OpenAIRE

    Coralie, Soulier; Anne, Togola

    2015-01-01

    International audience Nowadays with technological advances, the use of environmental forensic approaches could help to characterize the various sources of groundwater contamination. This implies the need of specific analytical methodology to identify micropollutants, emerging substances or transformation products present at low concentrations. The high resolution mass spectrometry (HRMS) has gained increasingly in importance for monitoring organic compounds. Its high resolving power, mass...

  10. Analytical and processing methodologies for non-target screening by coupling passive sampling and high resolution mass spectrometry

    OpenAIRE

    Coralie, Soulier; Anne, Togola

    2015-01-01

    Nowadays with technological advances, the use of environmental forensic approaches could help to characterize the various sources of groundwater contamination. This implies the need of specific analytical methodology to identify micropollutants, emerging substances or transformation products present at low concentrations. The high resolution mass spectrometry (HRMS) has gained increasingly in importance for monitoring organic compounds. Its high resolving power, mass accuracy and the sensitiv...

  11. An Advanced Analytical Chemistry Experiment Using Gas Chromatography-Mass Spectrometry, MATLAB, and Chemometrics to Predict Biodiesel Blend Percent Composition

    Science.gov (United States)

    Pierce, Karisa M.; Schale, Stephen P.; Le, Trang M.; Larson, Joel C.

    2011-01-01

    We present a laboratory experiment for an advanced analytical chemistry course where we first focus on the chemometric technique partial least-squares (PLS) analysis applied to one-dimensional (1D) total-ion-current gas chromatography-mass spectrometry (GC-TIC) separations of biodiesel blends. Then, we focus on n-way PLS (n-PLS) applied to…

  12. Determination of lead in blood by chelation with ammonium pyrrolidine dithio-carbamate followed by tungsten-coil atomic absorption spectrometry

    Science.gov (United States)

    Salido, Arthur; Sanford, Caryn L.; Jones, Bradley T.

    1999-08-01

    An inexpensive, bench-top blood Pb analyzer has been developed. The system is based on tungsten-coil atomic absorption spectrometry. Pb atomization occurs on W-coils extracted from commercially available slide projector bulbs. The system has minimal power requirements: 120 ACV and 15 A. A small, computer-controlled CCD spectrometer is used as the detector. A Pb hollow cathode lamp is used as the source. Blood Pb is chelated with ammonium pyrrolidine dithio-carbamate and extracted into methyl iso-butyl ketone (4-methyl 2-pentanone). Twenty-microliter volumes of the organic phase are deposited on the W-coil, dried at 1.4 A, charred at 2.3 A and atomized at 6.0 A. Graphite furnace atomic absorption spectrometry is used as a comparison for W-coil results. Levels 1-4 of a NIST standard reference material 955b ‘lead in bovine blood’ are used to test accuracy and precision. The analytical figures of merit for the system are: 12-pg instrument detection limit, 24-pg blood detection limit and a characteristic mass of 28 pg.

  13. A double cell for X-ray absorption spectrometry of atomic Zn

    CERN Document Server

    Mihelic, A; Arcon, I; Padeznik-Gomilsek, J; Borowski, M

    2002-01-01

    A high-temperature cell with a double wall design has been constructed for X-ray absorption spectrometry of metal vapors. The inner cell, assembled from a corundum tube and thin plates without welding or reshaping, serves as a container of the vapor sample. It is not vacuum tight: instead, the outer tube provides inert atmosphere. Several spectra of K-edge atomic absorption of Zn were obtained in the stationary working regime below the Zn boiling point. The K-edge profile shows an extremely strong resonance and, above the continuum threshold, coexcitations of the outer electrons.

  14. Analysis of atmospheric aerosols by atomic emission spectrometry with electrical discharge sampling

    International Nuclear Information System (INIS)

    A procedure is developed for the determination of the concentration of heavy metals (Pb, Mn, Cu, Ni, Zn, and Cd) in atmospheric air by atomic emission spectrometry with gas-discharge sampling onto the end of a standard carbon electrode. A design of a two-section sampler is proposed; the sampler provides the rapid determination of deposition factors for the deposition of heavy metals contained in aerosol particles onto the end of a carbon electrode. Examples of determining metal concentrations in a model sample of air and in atmospheric air and determination limits of metals deposited onto the end of a carbon electrode are given

  15. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia, E-mail: e.vasileva-veleva@iaea.org

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6–4.3%), repeatability (4–9%), reproducibility (9–11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as

  16. Deriving Coarse-Grained Charges from All-Atom Systems: An Analytic Solution.

    Science.gov (United States)

    McCullagh, Peter; Lake, Peter T; McCullagh, Martin

    2016-09-13

    An analytic method to assign optimal coarse-grained charges based on electrostatic potential matching is presented. This solution is the infinite size and density limit of grid-integration charge-fitting and is computationally more efficient by several orders of magnitude. The solution is also minimized with respect to coarse-grained positions which proves to be an extremely important step in reproducing the all-atom electrostatic potential. The joint optimal-charge optimal-position coarse-graining procedure is applied to a number of aggregating proteins using single-site per amino acid resolution. These models provide a good estimate of both the vacuum and Debye-Hückel screened all-atom electrostatic potentials in the vicinity and in the far-field of the protein. Additionally, these coarse-grained models are shown to approximate the all-atom dimerization electrostatic potential energy of 10 aggregating proteins with good accuracy.

  17. Cobalt as chemical modifier to improve chromium sensitivity and minimize matrix effects in tungsten coil atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Sidnei G. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, P.O. Box 676, São Carlos, SP 13560-970 (Brazil); Donati, George L., E-mail: georgedonati@yahoo.com.br [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Santos, Luana N. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, P.O. Box 676, São Carlos, SP 13560-970 (Brazil); Jones, Bradley T. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Nóbrega, Joaquim A. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, P.O. Box 676, São Carlos, SP 13560-970 (Brazil)

    2013-05-30

    Graphical abstract: -- Highlights: •Charge transfer reactions increase the population of Cr{sup +}. •Chromium ions and electrons recombine to form excited-state Cr atoms. •A 10-fold improvement in LOD is observed for Cr emission measurements. •The two-step ionization/excitation mechanism improves sensitivity and accuracy. •High concentrations of Co also minimize matrix effects. -- Abstract: Cobalt is used as chemical modifier to improve sensitivity and minimize matrix effects in Cr determinations by tungsten coil atomic emission spectrometry (WCAES). The atomizer is a tungsten filament extracted from microscope light bulbs. A solid-state power supply and a handheld CCD-based spectrometer are also used in the instrumental setup. In the presence of 1000 mg L{sup −1} Co, WCAES limit of detection for Cr (λ = 425.4 nm) is calculated as 0.070 mg L{sup −1}; a 10-fold improvement compared to determinations without Co modifier. The mechanism involved in such signal enhancement is similar to the one observed in ICP OES and ICP-MS determinations of As and Se in the presence of C. Cobalt increases the population of Cr{sup +} by charge transfer reactions. In a second step, Cr{sup +}/e{sup −} recombination takes place, which results in a larger population of excited-state Cr atoms. This alternative excitation route is energetically more efficient than heat transfer from atomizer and gas phase to analyte atoms. A linear dynamic range of 0.25–10 mg L{sup −1} and repeatability of 3.8% (RSD, n = 10) for a 2.0 mg L{sup −1} Cr solution are obtained with this strategy. The modifier high concentration also contributes to improving accuracy due to a matrix-matching effect. The method was applied to a certified reference material of Dogfish Muscle (DORM-2) and no statistically significant difference was observed between determined and certified Cr values at a 95% confidence level. Spike experiments with bottled water samples resulted in recoveries between 93% and

  18. Enhancement effect of alkaline earth metal on the determination of aluminium by atomic absorption spectrometry with a graphite furnace

    OpenAIRE

    Matsusaki, Koji

    1987-01-01

    In the determination of aluminium by atomic absorption spectrometry with a graphite furnace, coexisting oxyanion salts of alkaline earth metal enhanced the aluminium atomic absorption. The relative absorbance was increased with decreasing of the ramp atomization rate and with decreasing of the sheathing gas flow rate less than 51 min^. These results show that the enhancement effect is caused by the reductivity of the carbide of alkaline earth metal which is formed in the furnace at ashing and...

  19. Determination of vanadium in mussels by electrothermal atomic absorption spectrometry without chemical modifiers

    Energy Technology Data Exchange (ETDEWEB)

    Saavedra, Y.; Fernandez, P. [Centro de Control do Medio Marino, Peirao de Vilaxoan s/n, Vilagarcia de Arousa, 36611 Pontevedra (Spain); Gonzalez, A. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Quimica, 15706, Santiago de Compostela (Spain)

    2004-05-01

    A method was developed for the quantitative determination of total vanadium concentration in mussels via electrothermal atomic absorption spectrometry (ETAAS). After the microwave digestion of the samples, a program using temperatures of 1600 C and 2600 C for ashing and atomization respectively, without any matrix modifiers, allowed us to obtain results that were satisfactory since they agreed closely with certified reference material values. The detection limit was 0.03 mg kg{sup -1} (dry weight), indicating that the method is suitable for the analysis of mussel samples. This determination was compared with matrix modifiers that have been reported previously. The method was applied to various cultivated and wild mussels from the Galician coast, yielding levels below 1 mg kg{sup -1} (wet weight). (orig.)

  20. Ionic liquid ultrasound assisted dispersive liquid-liquid microextraction method for preconcentration of trace amounts of rhodium prior to flame atomic absorption spectrometry determination

    Energy Technology Data Exchange (ETDEWEB)

    Molaakbari, Elaheh [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Young Research Society, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Mostafavi, Ali, E-mail: mostafavi.ali@gmail.com [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Afzali, Daryoush [Environment and Nanochemistry Department, Research Institute of Environmental Science, International Center for Science, High Technology and Environmental Science, Kerman (Iran, Islamic Republic of); Mineral Industries Research Center, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

    2011-01-30

    In this article, we consider ionic liquid based ultrasound-assisted dispersive liquid-liquid microextraction of trace amounts of rhodium from aqueous samples and show that this is a fast and reliable sample pre-treatment for the determination of rhodium ions by flame atomic absorption spectrometry. The Rh(III) was transferred into its complex with 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol as a chelating agent, and an ultrasonic bath with the ionic liquid, 1-octyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide at room temperature was used to extract the analyte. The centrifuged rhodium complex was then enriched in the form of ionic liquid droplets and prior to its analysis by flame atomic absorption spectrometry, 300 {mu}L ethanol was added to the ionic liquid-rich phase. Finally, the influence of various parameters on the recovery of Rh(III) was optimized. Under optimum conditions, the calibration graph was linear in the range of 4.0-500.0 ng mL{sup -1}, the detection limit was 0.37 ng mL{sup -1} (3S{sub b}/m, n = 7) and the relative standard deviation was {+-}1.63% (n = 7, C = 200 ng mL{sup -1}). The results show that ionic liquid based ultrasound assisted dispersive liquid-liquid microextraction, combined with flame atomic absorption spectrometry, is a rapid, simple, sensitive and efficient analytical method for the separation and determination of trace amounts of Rh(III) ions with minimum organic solvent consumption.

  1. Fourier transform ion cyclotron resonance mass spectrometry: the analytical tool for heavy oil and bitumen characterization

    Energy Technology Data Exchange (ETDEWEB)

    Oldenburg, Thomas B.P; Brown, Melisa; Hsieh, Ben; Larter, Steve [Petroleum Reservoir Group (prg), Department of Geoscience, University of Calgary, Alberta (Canada)

    2011-07-01

    The Fourier Transform Ion Cyclotron Resonance Mass Spectrometry (FTICRMS), developed in the 1970's by Marshall and Comisarow at the University of British Columbia, has become a commercially available tool capable of analyzing several hundred thousand components in a petroleum mixture at once. This analytical technology will probably usher a dramatic revolution in geochemical capability, equal to or greater than the molecular revolution that occurred when GCMS technologies became cheaply available. The molecular resolution and information content given by the FTICRMS petroleum analysis can be compared to the information in the human genome. With current GCMS-based petroleum geochemical protocols perhaps a few hundred components can be quantitatively determined, but with FTICRMS, 1000 times this number of components could possibly be resolved. However, fluid and other properties depend on interaction of this multitude of hydrocarbon and non-hydrocarbon components, not the components themselves, and access to the full potential of this new petroleomics will depend on the definition of this interactome.

  2. [The application of atomic absorption spectrometry in automatic transmission fault detection].

    Science.gov (United States)

    Chen, Li-dan; Chen, Kai-kao

    2012-01-01

    The authors studied the innovative applications of atomic absorption spectrometry in the automatic transmission fault detection. After the authors have determined Fe, Cu and Cr contents in the five groups of Audi A6 main metal in automatic transmission fluid whose travel course is respectively 10-15 thousand kilometers, 20-26 thousand kilometers, 32-38 thousand kilometers, 43-49 thousand kilometers, and 52-58 thousand kilometers by atomic absorption spectrometry, the authors founded the database of primary metal content in the Audi A6 different mileage automatic transmission fluid (ATF). The research discovered that the main metal content in the automatic transmission fluid increased with the vehicles mileage and its normal metal content level in the automatic transmission fluid is between the two trend lines. The authors determined the main metal content of automatic transmission fluid which had faulty symptoms and compared it with its database value. Those can not only judge the wear condition of the automatic transmission which had faulty symptoms but also help the automobile detection and maintenance personnel to diagnose automatic transmission failure reasons without disintegration. This reduced automobile maintenance costs, and improved the quality of automobile maintenance.

  3. Determination of trace elements in ground water by two preconcentration methods using atomic absorption spectrometry

    International Nuclear Information System (INIS)

    This is a comparative study between two different methods of preconcentration done to separate the trace elements cadmium, nickel. chromium, manganese, copper, zinc, and lead in drinking (ground) water samples taken from different locations in Gezira State, central Sudan (the map); these methods are (coprecipitation) with aluminium hydroxide and by Ammonium Pyrrolidine Dithiocarbamate (APDC) using Methyl Isobutyl Ketone (MIBK) as an organic solvent; and subsequent analysis by Atomic Absorption Spectrometry (AAS) for both methods. The result of comparison showed the superiority of the (APDC) coprecipitation method over the aluminium hydroxide coprecipitation method in the total percentage recoveries of the studied trace elements in drinking (ground) water samples, such results confirm previous studies. This study also involves direct analysis of these water samples by atomic absorption spectrometry to determine the concentrations of trace elements Cadmium, Nickel, Chromium, Manganese, Copper, Zinc and Lead and compare it to the corresponding guide line values described by the World Health Organization and the maximum concentrations of trace elements in drinking water permitted by the Sudanese Standards and Metrology Organizations (SSMO), where the concentrations of some elements in some samples were found to be different than the described values by both of the organizations. The study includes a trial to throw light on the effect of the proximity of the water samples sources to the Blue Nile river on its trace elements concentrations; no relation was proved to exist in that respect.(Author)

  4. Determination of Elements by Atomic Absorption Spectrometry in Medicinal Plants Employed to Alleviate Common Cold Symptoms

    Institute of Scientific and Technical Information of China (English)

    F Zehra Küçükbay; Ebru Kuyumcu

    2014-01-01

    Eleven important medicinal plants generally used by the people of Turkey for the treatment of com-mon cold have been studied for their mineral contents .Eleven minor and major elements (essential ,non-essen-tial and toxic) were identified in the Asplenium adiantum-nigrum L .,Althaea of ficinalis L .,Verbascum phlomoides L .,Euphorbiachamaesyce L .,Zizyphus jujube Miller ,Peganum harmala L .,Arum dioscori-dis Sm .,Sambucus nigra L .,Piper longum L .,Tussilago farfara L .and Elettariacardamomum Maton by employing flame atomic absorption and emission spectrometry and electro-thermal atomic absorption spectrom-etry .Microwave digestion procedure for total concentration was applied under optimized conditions for dissolu-tion of medicinal plants .Plant based biological certified reference materials (CRMs) served as standards for quantification .These elements are found to be present in varying concentrations in the studied plants .The baseline data presented in this work can be used in understanding the role of essential ,non-essential and toxic elements in nutritive ,preventive and therapeutic properties of medicinal plants .

  5. Slurry sampling techniques for the determination of lead in Bangladeshi fish samples by electrothermal atomic absorption spectrometry with a metal tube atomizer.

    Science.gov (United States)

    Rahman, Mohammad Arifur; Kaneco, Satoshi; Suzuki, Tohru; Katsumata, Hideyuki; Ohta, Kiyohisa

    2005-05-01

    Ultrasonic slurry sampling electrothermal atomic absorption spectrometry with a metal tube atomizer has been applied to the determination of lead in Bangladeshi fish samples. The slurry sampling conditions, such as slurry stabilizing agent, slurry concentration, pyrolysis temperature for the slurried fish samples, particle size and ultrasonic agitation time, were optimized for electrothermal atomic absorption spectrometry with the Mo tube atomizer. Thiourea was used as the chemical modifier for the interference of matrix elements. The detection limit was 53 fg (3S/N). The determined amount of lead in Bangladeshi fish samples was consistent with those measured in the dissolved acid-digested samples. The advantages of the proposed methods are easy calibration, simplicity, low cost and rapid analysis.

  6. Phonon dispersion on Ag (100) surface: A modified analytic embedded atom method study

    Science.gov (United States)

    Xiao-Jun, Zhang; Chang-Le, Chen

    2016-01-01

    Within the harmonic approximation, the analytic expression of the dynamical matrix is derived based on the modified analytic embedded atom method (MAEAM) and the dynamics theory of surface lattice. The surface phonon dispersions along three major symmetry directions , and X¯M¯ are calculated for the clean Ag (100) surface by using our derived formulas. We then discuss the polarization and localization of surface modes at points X¯ and M¯ by plotting the squared polarization vectors as a function of the layer index. The phonon frequencies of the surface modes calculated by MAEAM are compared with the available experimental and other theoretical data. It is found that the present results are generally in agreement with the referenced experimental or theoretical results, with a maximum deviation of 10.4%. The agreement shows that the modified analytic embedded atom method is a reasonable many-body potential model to quickly describe the surface lattice vibration. It also lays a significant foundation for studying the surface lattice vibration in other metals. Project supported by the National Natural Science Foundation of China (Grant Nos. 61471301 and 61078057), the Scientific Research Program Funded by Shaanxi Provincial Education Department, China (Grant No. 14JK1301), and the Specialized Research Fund for the Doctoral Program of Higher Education, China (Grant No. 20126102110045).

  7. Direct determination of Cr and Cu in urine samples by electrothermal atomic absorption spectrometry using ruthenium as permanent modifier (R1)

    Energy Technology Data Exchange (ETDEWEB)

    Lelis, Katia Linces Alves; Rocha, Clelia Aparecida [Instituto de Patologia Clinica Hermes Pardini, 30140-070 Belo Horizonte, MG (Brazil); Magalhaes, Cristina Goncalves; Silva, Jose Bento Borba of [Departamento de Quimica, Universidade Federal de Minas Gerais, 31270-901 Belo Horizonte, MG (Brazil)

    2002-12-01

    In this study Ru, deposited thermally on an integrated platform pyrolytic graphite tube, is proposed as a permanent modifier for the determination of Cu and Cr in urine samples by electrothermal atomic absorption spectrometry. The samples were diluted 1:1 with nitric acid (1% v/v). Pyrolysis and atomization temperatures for spiked urine samples were 1,100 C and 1,900 C respectively for Cu, and 1,400 C and 2,500 C respectively for Cr. For comparison purposes, the conventional modification with Pd+Mg was also studied. The sensitivity for Ru as permanent modifier was higher for the two analytes. The characteristic masses were 7.3 and 17.7 for Cr and Cu. The detection limits (3{sigma}) were 0.22 and 0.32 {mu}g/L, for Cr and Cu, respectively. Good agreement was obtained with certified urine samples for the two elements. (orig.)

  8. Simultaneous determination of iron and nickel in fluoropolymers by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Soares, Bruno M; Santos, Rafael F; Bolzan, Rodrigo C; Muller, Edson I; Primel, Ednei G; Duarte, Fabio A

    2016-11-01

    This paper reports the development of a method of simultaneous determination of iron and nickel in fluoropolymers by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) with direct solid sampling. In order to carry out simultaneous measurements, both the main resonance line of nickel (232.003nm) and the adjacent secondary line of iron (232.036nm) were monitored in the same spectral window. The proposed method was optimized with a perfluoroalkoxy (PFA) sample and was applied to the determination of iron and nickel in fluorinated ethylene propylene (FEP) and modified polytetrafluoroethylene (PTFE-TFM) samples. Pyrolysis and atomization temperatures, as well as the use of Pd and H2 (during pyrolysis) as chemical modifiers, were carefully investigated. Compromise temperatures for pyrolysis and atomization of both analytes were achieved at 800 and 2300°C, respectively, using only 0.5Lmin(-1) H2 as chemical modifier during pyrolysis. Calibration curves were performed with aqueous standards by using a single solution which contained both analytes. Limits of detection were 221 and 9.6ngg(-1) for iron and nickel, respectively. Analyte concentrations in all samples ranged from 3.53 to 12.4µgg(-1) for iron and from 37 to 78ngg(-1) for nickel, with relative standard deviation less than 19%. Accuracy was evaluated by comparing these results with those obtained by inductively coupled plasma mass spectrometry after sample digestion by microwave-induced combustion and no significant statistical difference was observed. PMID:27591638

  9. Evaluation of the temporal profiles and the analytical features of a laser ablation - Pulsed glow discharge coupling for optical emission spectrometry

    Science.gov (United States)

    González de Vega, Claudia; Bordel, Nerea; Pereiro, Rosario; Sanz-Medel, Alfredo

    2016-07-01

    The coupling of a glow discharge (GD) in pulsed mode (PGD) as secondary source for excitation/ionization of the material provided by laser ablation (LA) has been investigated using optical emission spectrometry (OES). The variation of the laser pulse delay with respect to the GD pulse allows to producing the ablation process during prepeak, plateau or afterglow GD regions. Emission properties of the LA-PGD plasma in each temporal region of the GD pulse have been evaluated for analytical lines of different elements. Resonant atomic lines have shown higher emission intensity in the prepeak region compared to non-resonant lines. Non-resonant lines showed higher enhancement of the emission intensity in the afterglow region. Moreover, the coupled LA-PGD system offered better linear correlation coefficients using a set of glass standards for calibration as well as lower detection limits (by at least a factor of two) when compared to laser induced breakdown spectroscopy.

  10. Permanent modification in electrothermal atomic absorption spectrometry — advances, anticipations and reality

    Science.gov (United States)

    Tsalev, Dimiter L.; Slaveykova, Vera I.; Lampugnani, Leonardo; D'Ulivo, Alessandro; Georgieva, Rositsa

    2000-05-01

    Permanent modification is an important recent development in chemical modification techniques which is promising in view of increasing sample throughput with 'fast' programs, reducing reagent blanks, preliminary elimination of unwanted modifier components, compatibility with on-line and in situ enrichment, etc. An overview of this approach based on the authors' recent research and scarce literature data is given, revealing both success and failure in studies with permanently modified surfaces (carbides, non-volatile noble metals, noble metals on carbide coatings, etc.), as demonstrated in examples of direct electrothermal atomic absorption spectrometric (ETAAS) applications to biological and environmental matrices and vapor generation (VG)-ETAAS coupling with in-atomizer trapping of hydrides and other analyte vapors. Permanent modifiers exhibit certain drawbacks and limitations such as: poorly reproducible treatment technologies — eventually resulting in poor tube-to-tube repeatability and double or multiple peaks; impaired efficiency compared with modifier addition to each sample aliquot; relatively short lifetimes; limitations imposed on temperature programs, the pyrolysis, atomization and cleaning temperatures being set somewhat lower to avoid excessive loss of modifier; applicability to relatively simple sample solutions rather than to high-salt matrices and acidic digests; side effects of overstabilization, etc. The most important niches of application appear to be the utilization of permanently modified surfaces in coupled VG-ETAAS techniques, analysis of organic solvents and extracts, concentrates and fractions obtained after enrichment and/or speciation separations and direct ETAAS determinations of highly volatile analytes in relatively simple sample matrices.

  11. Evaluation of vapor generation for the determination of nickel by inductively coupled plasma-atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Marrero, Julieta [Comision Nacional de Energia Atomica, Unidad de Actividad Quimica, Centro Atomico Constituyentes, Av. Gral. Paz 1499, 1650-San Martin, Pcia. de Buenos Aires (Argentina); Smichowski, Patricia [Comision Nacional de Energia Atomica, Unidad Proyectos Especiales de Suministros Nucleares, Av. Libertador 8250, 1429-Buenos Aires (Argentina)

    2002-09-01

    Volatile species of Ni were generated by merging acidified aqueous samples and sodium tetrahydroborate(III) in a continuous flow system. The gaseous analyte was subsequently introduced via a stream of Ar carrier into the inlet tube of the plasma torch. Inductively coupled plasma atomic emission spectrometry (ICP-AES) was used for detection. The operating conditions (chemical and physical parameters) and the concentrations of different acids were evaluated for the efficient generation of Ni vapor. The detection limit (3 {sigma}{sub blank}) was 1.8 ng mL{sup -1}. The precision (RSD) of the determination was 4.2% at a level of 500 ng mL{sup -1} and 7.3% for 20 ng mL{sup -1} (n=10). The efficiency of the generation process was estimated to be 51%. The possible interfering effect of transition metals (Cd, Co, Cu, Cr, Fe, Mn, Zn), hydride forming elements (As, Ge, Pb, Sb, Se, Sn, Te), and Hg on Ni signal was examined. This study has demonstrated that Ni vapor generation is markedly free of interferences. (orig.)

  12. Unusual calibration curves observed for iron using high-resolution continuum source graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Welz, Bernhard, E-mail: w.bernardo@terra.com.b [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis-SC (Brazil); Instituto Nacional de Ciencia e Tecnologia do CMPq-INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador-BA (Brazil); Santos, Lisia M.G. dos [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis-SC (Brazil); Instituto Nacional de Controle de Qualidade em Saude-INCQS-Fiocruz, 21040-900 Rio de Janeiro-RJ (Brazil); Araujo, Rennan G.O. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis-SC (Brazil); Departamento de Quimica, Universidade Federal de Sergipe, 49100-000 Sao Cristovao-SE (Brazil); Jacob, Silvana do C. [Instituto Nacional de Controle de Qualidade em Saude-INCQS-Fiocruz, 21040-900 Rio de Janeiro-RJ (Brazil); Vale, Maria Goreti R. [Instituto Nacional de Ciencia e Tecnologia do CMPq-INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador-BA (Brazil); Instituto de Quimica, Universidade Federal do Rio Grande do Sul, 91501-970 Porto Alegre-RS (Brazil); Okruss, Michael; Becker-Ross, Helmut [Leibniz-Institut fuer Analytische Wissenschaften-ISAS-Department Berlin, 12489 Berlin (Germany)

    2010-03-15

    The simultaneous determination of cadmium and iron in plant and soil samples has been investigated using high-resolution continuum source graphite furnace atomic absorption spectrometry. The primary cadmium resonance line at 228.802 nm and an adjacent secondary iron line at 228.726 nm, which is within the spectral interval covered by the charge-coupled device (CCD) array detector, have been used for the investigations. Due to the very high iron content in most of the soil samples the possibility has been investigated to reduce the sensitivity and extend the working range by using side pixels for measurement at the line wings instead of the line core. It has been found that the calibration curves measured at all the analytically useful pixels of this line consisted of two linear parts with distinctly different slopes. This effect has been independent of the positioning of the wavelength, i.e., if the Cd line or the Fe line was in the center of the CCD array. The most likely explanation for this unusual behavior is a significant difference between the instrument width DELTAlambda{sub Instr} and the absorption line width DELTAlambda{sub Abs}, which is quite pronounced in the case of Fe. Using both parts of the calibration curves and simultaneous measurement at the line center and at the wings made it possible to extend the working range for the iron determination to more than three orders of magnitude.

  13. Cloud point extraction for the preconcentration of silver and palladium in real samples and determination by atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tavallali, Hossein; Yazdandoust, Saeed; Yazdandoust, Mozhdeh [Department of Chemistry, Payame Noor University (PNU), Shiraz (Iran)

    2010-03-15

    A cloud point extraction procedure is presented for the preconcentration and simultaneous determination of Ag{sup +} and Pd{sup 2+} in various samples. After complexation with 2-((2-((1H-benzo[d]imidazole-2-yl)methoxy)phenoxy)methyl)-1H-benzo[d]imidazol (BIMPI), which was used as a new chelating agent, analyte ions were quantitatively extracted to a phase rich in Triton X-114 following centrifugation, and determination was carried out by flame atomic absorption spectrometry (FAAS). Under the optimum experimental conditions (i. e., pH = 7.0, 15.0.10{sup -5} mol/L BIMPI and 0.036% (w/v) Triton X-114), calibration graphs were linear in the range of 28.0-430.0 {mu}g/L and 57.0-720.0 {mu}g/L with detection limits of 10.0 and 25.0 {mu}g/L for Ag{sup +} and Pd{sup 2+}, respectively. The enrichment factors were 35.0 and 28.0 for Ag{sup +} and Pd{sup 2+}, respectively. The method has been successfully applied to evaluate these metals in some real samples, including waste water, soil and hydrogenation catalyst samples. (Abstract Copyright [2010], Wiley Periodicals, Inc.)

  14. Cloud point extraction and flame atomic absorption spectrometry combination for copper(II) ion in environmental and biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Shokrollahi, Ardeshir [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of)], E-mail: ashokrollahi@mail.yu.ac.ir; Ghaedi, Mehrorang [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of)], E-mail: m_ghaedi@mail.yu.ac.ir; Hossaini, Omid; Khanjari, Narges [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Soylak, Mustafa [Chemistry Department, University of Erciyes, 38039 Kayseri (Turkey)

    2008-12-30

    A cloud point extraction procedure was presented for the preconcentration of copper(II) ion in various samples. After complexation by 4-(phenyl diazenyl) benzene-1,3-diamine (PDBDM) (chrysoidine), copper(II) ions were quantitatively recovered in Triton X-114 after centrifugation. 0.5 ml of methanol acidified with 1.0 mol L{sup -1} HNO{sub 3} was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The influence of analytical parameters including ligand, Triton X-114 and HNO{sub 3} concentrations, bath temperature, heating time, centrifuge rate and time were optimized. The effect of the matrix ions on the recovery of copper(II) ions was investigated. The detection limit (3S.D.{sub b}/m, n = 10) of 0.6 ng mL{sup -1} along with preconcentration factor of 30 and enrichment factor of 41.1 with R.S.D. of 1.0% for Cu was achieved. The proposed procedure was applied to the analysis of various environmental and biological samples.

  15. Preconcentration and determination of zinc and lead ions by a combination of cloud point extraction and flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tavallali, H. [Chemistry Department, Payamenore University, Shiraz (Iran); Shokrollahi, A.; Zahedi, M. [Chemistry Department, Yasouj University, Yasouj (Iran); Niknam, K. [Chemistry Department, Persian Gulf University, Bushehr (Iran); Soylak, M. [Chemistry Department, University of Erciyes, Kayseri (Turkey); Ghaedi, M.

    2009-04-15

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of lead(II) and zinc(II). After complexation with 3-[(4-bromophenyl) (1-H-inden-3-yl)methyl]-1 H-indene (BPIMI), the analytes were quantitatively extracted to a phase rich in Triton X-114 after centrifugation. Methanol acidified with 1 mol/L HNO{sub 3} was added to the surfactant rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The concentration of bis((1H-benzo [d] imidazol-2yl)ethyl)sulfane, Triton X-114, pH and amount of surfactant were all optimized. Detection limits (3 SDb/m) of 2.5 and 1.6 ng/mL for Pb{sup 2+} and Zn{sup 2+} along with preconcentration factors of 30 and an enrichment factor of 32 and 48 for Pb{sup 2+}and Zn {sup 2+} ions were obtained, respectively. The proposed cloud point extraction was been successfully applied for the determination of these ions in real samples with complicated matrices such as food and soil samples, with high efficiency. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  16. Analytical study of four-wave mixing with large atomic coherence

    CERN Document Server

    Korsunsky, E A; Marangos, J P; Bergmann, K

    2002-01-01

    Four-wave mixing in resonant atomic vapors based on maximum coherence induced by Stark-chirped rapid adiabatic passage (SCRAP) is investigated theoretically. We show the advantages of a coupling scheme involving maximum coherence and demonstrate how a large atomic coherence between a ground and an highly excited state can be prepared by SCRAP. Full analytic solutions of the field propagation problem taking into account pump field depletion are derived. The solutions are obtained with the help of an Hamiltonian approach which in the adiabatic limit permits to reduce the full set of Maxwell-Bloch equations to simple canonical equations of Hamiltonian mechanics for the field variables. It is found that the conversion efficiency reached is largely enhanced if the phase mismatch induced by linear refraction is compensated. A detailed analysis of the phase matching conditions shows, however, that the phase mismatch contribution from the Kerr effect cannot be compensated simultaneously with linear refraction contrib...

  17. Analytical estimation of the gravitational constant with atomic and nuclear physical constants

    International Nuclear Information System (INIS)

    If NA represents the Avogadro's number, gravitational constant associated with atomic electromagnetic interaction can be expressed as GE ≅ N2AG. With GE and with the assumed two new pseudo numbers x ≈ 38.725 and y ≈ 47.415, value of G can be fixed for 10 digits in a verifiable approach. (x, y) can be called as the back ground analytical numbers using by which micro-macro physical constants can be interlinked qualitatively and quantitatively

  18. Comparative oxidation state specific analysis of arsenic species by high-performance liquid chromatography- inductively coupled plasma-mass spectrometry and hydride generation-cryotrapping-atomic absorption spectrometry

    OpenAIRE

    Currier, J. M.; Saunders, R J; Ding, L.; Bodnar, W.; Cable, P.; Matoušek, T. (Tomáš); Creed, J. T.; Stýblo, M.

    2013-01-01

    The formation of methylarsonous acid (MAsIII) and dimethylarsinous acid (DMAsIII) in the course of inorganic arsenic (iAs) metabolism plays an important role in the adverse effects of chronic exposure to iAs. High-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) and hydride generation-cryotrapping-atomic absorption spectrometry (HG-CT-AAS) have been frequently used for the analysis of MAsIII and DMAsIII in biological samples. While HG-CT-AAS has con...

  19. Determination of Cd, Pb and As in sediments of the Sava River by electrothermal atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    SIMONA MURKO

    2010-01-01

    Full Text Available The applicability of nitric acid, palladium nitrate and a mixture of palladium and magnesium nitrate as matrix modifiers were estimated for the accurate and reproducible determination of cadmium (Cd, lead (Pb and arsenic (As in sediments of the Sava River by electrothermal atomic absorption spectrometry, ETAAS. Decomposition of the samples was done in a closed vessel microwave-assisted digestion system using nitric, hydrochloric and hydrofluoric acids, followed by the addition of boric acid to convert the fluorides into soluble complexes. The parameters for the determination of Cd, Pb and As in sediments were optimised for each individual element and for each matrix modifier. In addition, two sediment reference materials were also analysed. In determination of Cd and Pb, nitric acid was found to be the most appropriate matrix modifier. The accurate and reliable determination of Cd and Pb in sediments was possible also in the presence of boric acid. The use of a mixture of palladium and magnesium nitrate efficiently compensated for matrix effects and enabled the accurate and reliable determination of As in the sediments. Quantification of Cd and As was performed by calibration using acid matched standard solutions, while the standard addition method was applied for the quantification of Pb. The repeatability of the analytical procedure for the determination of Cd, Pb and As in sediments was ±5 % for Cd, ±4 % for Pb and ±2 % for As. The LOD values of the analytical procedure were found to be 0.05 mg/kg for Cd and 0.25 mg/kg for Pb and As, while the LOQ values were 0.16 mg/kg for Cd and 0.83 mg/kg for Pb and As. Finally, Cd, Pb and As were successfully determined in sediments of the Sava River in Slovenia.

  20. The determination of trace metals in lubricating oils by atomic spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Aucelio, Ricardo Q. [Departamento de Quimica, Pontificia Universidade Catolica do Rio de Janeiro, Rua Marques de Sao Vicente 225, 22451-900 Rio de Janeiro (Brazil)], E-mail: aucelior@rdc.puc-rio.br; Martins de Souza, Roseli; Calixto de Campos, Reinaldo; Miekeley, Norbert; Porto da Silveira, Carmem L. [Departamento de Quimica, Pontificia Universidade Catolica do Rio de Janeiro, Rua Marques de Sao Vicente 225, 22451-900 Rio de Janeiro (Brazil)

    2007-09-15

    The determination of trace metals in lubricating oils using atomic spectrometric methods is reviewed. The importance of such analyses for technical diagnostics as well as the specific sample characteristics related to the analyte form (metallo-organic and metal particles) is discussed. Problems related to sample pre-treatment for appropriate sample introduction and calibration are addressed as well as the strategies to overcome them. Recent trends aimed at simplifying sample manipulation are presented. The applications and scope of AAS, ICP OES and ICP MS techniques for the determination of trace metals in lubricating oil is individually discussed, as well as some present instrumental trends.

  1. Determination of serum aluminum by electrothermal atomic absorption spectrometry: A comparison between Zeeman and continuum background correction systems

    Science.gov (United States)

    Kruger, Pamela C.; Parsons, Patrick J.

    2007-03-01

    Excessive exposure to aluminum (Al) can produce serious health consequences in people with impaired renal function, especially those undergoing hemodialysis. Al can accumulate in the brain and in bone, causing dialysis-related encephalopathy and renal osteodystrophy. Thus, dialysis patients are routinely monitored for Al overload, through measurement of their serum Al. Electrothermal atomic absorption spectrometry (ETAAS) is widely used for serum Al determination. Here, we assess the analytical performances of three ETAAS instruments, equipped with different background correction systems and heating arrangements, for the determination of serum Al. Specifically, we compare (1) a Perkin Elmer (PE) Model 3110 AAS, equipped with a longitudinally (end) heated graphite atomizer (HGA) and continuum-source (deuterium) background correction, with (2) a PE Model 4100ZL AAS equipped with a transversely heated graphite atomizer (THGA) and longitudinal Zeeman background correction, and (3) a PE Model Z5100 AAS equipped with a HGA and transverse Zeeman background correction. We were able to transfer the method for serum Al previously established for the Z5100 and 4100ZL instruments to the 3110, with only minor modifications. As with the Zeeman instruments, matrix-matched calibration was not required for the 3110 and, thus, aqueous calibration standards were used. However, the 309.3-nm line was chosen for analysis on the 3110 due to failure of the continuum background correction system at the 396.2-nm line. A small, seemingly insignificant overcorrection error was observed in the background channel on the 3110 instrument at the 309.3-nm line. On the 4100ZL, signal oscillation was observed in the atomization profile. The sensitivity, or characteristic mass ( m0), for Al at the 309.3-nm line on the 3110 AAS was found to be 12.1 ± 0.6 pg, compared to 16.1 ± 0.7 pg for the Z5100, and 23.3 ± 1.3 pg for the 4100ZL at the 396.2-nm line. However, the instrumental detection limits (3

  2. Determination of serum aluminum by electrothermal atomic absorption spectrometry: A comparison between Zeeman and continuum background correction systems

    Energy Technology Data Exchange (ETDEWEB)

    Kruger, Pamela C. [Department of Environmental Health Sciences, School of Public Health, University at Albany, State University of New York, P.O. Box 509, Albany, NY 12201-0509 (United States); Parsons, Patrick J. [Department of Environmental Health Sciences, School of Public Health, University at Albany, State University of New York, P.O. Box 509, Albany, NY 12201-0509 (United States); Lead Poisoning/Trace Elements Laboratory, Wadsworth Center, New York State Department of Health, P.O. Box 509, Albany, NY 12201-0509 (United States)], E-mail: patrick.parsons@wadsworth.org

    2007-03-15

    Excessive exposure to aluminum (Al) can produce serious health consequences in people with impaired renal function, especially those undergoing hemodialysis. Al can accumulate in the brain and in bone, causing dialysis-related encephalopathy and renal osteodystrophy. Thus, dialysis patients are routinely monitored for Al overload, through measurement of their serum Al. Electrothermal atomic absorption spectrometry (ETAAS) is widely used for serum Al determination. Here, we assess the analytical performances of three ETAAS instruments, equipped with different background correction systems and heating arrangements, for the determination of serum Al. Specifically, we compare (1) a Perkin Elmer (PE) Model 3110 AAS, equipped with a longitudinally (end) heated graphite atomizer (HGA) and continuum-source (deuterium) background correction, with (2) a PE Model 4100ZL AAS equipped with a transversely heated graphite atomizer (THGA) and longitudinal Zeeman background correction, and (3) a PE Model Z5100 AAS equipped with a HGA and transverse Zeeman background correction. We were able to transfer the method for serum Al previously established for the Z5100 and 4100ZL instruments to the 3110, with only minor modifications. As with the Zeeman instruments, matrix-matched calibration was not required for the 3110 and, thus, aqueous calibration standards were used. However, the 309.3-nm line was chosen for analysis on the 3110 due to failure of the continuum background correction system at the 396.2-nm line. A small, seemingly insignificant overcorrection error was observed in the background channel on the 3110 instrument at the 309.3-nm line. On the 4100ZL, signal oscillation was observed in the atomization profile. The sensitivity, or characteristic mass (m{sub 0}), for Al at the 309.3-nm line on the 3110 AAS was found to be 12.1 {+-} 0.6 pg, compared to 16.1 {+-} 0.7 pg for the Z5100, and 23.3 {+-} 1.3 pg for the 4100ZL at the 396.2-nm line. However, the instrumental detection

  3. Determination of ultra trace amounts of bismuth in biological and water samples by electrothermal atomic absorption spectrometry (ET-AAS) after cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Shemirani, Farzaneh; Baghdadi, Majid; Ramezani, Majid; Jamali, Mohammad Reza

    2005-04-04

    A new approach for a cloud point extraction electrothermal atomic absorption spectrometric method was used for determining bismuth. The aqueous analyte was acidified with sulfuric acid (pH 3.0-3.5). Triton X-114 was added as a surfactant and dithizone was used as a complexing agent. After phase separation at 50 deg. C based on the cloud point separation of the mixture, the surfactant-rich phase was diluted using tetrahydrofuran (THF). Twenty microliters of the enriched solution and 10 {mu}l of 0.1% (w/v) Pd(NO{sub 3}){sub 2} as chemical modifier were dispersed into the graphite tube and the analyte determined by electrothermal atomic absorption spectrometry. After optimizing extraction conditions and instrumental parameters, a preconcentration factor of 196 was obtained for a sample of only 10 ml. The detection limit was 0.02 ng ml{sup -1} and the analytical curve was linear for the concentration range of 0.04-0.60 ng ml{sup -1}. Relative standard deviations were <5%. The method was successfully applied for the extraction and determination of bismuth in tap water and biological samples (urine and hair)

  4. Some metals determination in beers by atomic emission spectrometry of induced argon plasma

    International Nuclear Information System (INIS)

    It was made the identification and determination of metals in brazilian bottled and canned beer, using atomic emission spectrometry with d.c. are and argon coupled plasma excitation sources. The elements Co, Cr, Cu, Fe, Pb and Zn were determined in beer samples, after treatment with HNO sub(3) conc. /H sub(2) O sub(2) (30%). In the determination of Co, Cr, Cu, Pb and Zn and alternative method using HNO sub(3) conc. /O sub(3) was proved be useful. The results obtained for Co, Cr, Cu, Fe, Pb and Zn were below the limits established by brazilian legislation, showing the good quality of the beer concerning the metals. The results of this work were requested by the previous Ministerio do Meio Ambiente e Urbanismo in order to contribute to review the brazilian legislation in foods and beverages about metals contents. (author)

  5. Analysis of soil reference materials for vanadium(+5) species by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Solid Certified Reference Materials (CRMs) with known vanadium(+5) content are currently not commercially available. Because of this, vanadium species have been determined in solid CRMs of soil, viz. CRM023-50, CRM024-50, CRM049-50, SQC001 and SQC0012. These CRMs are certified with only total vanadium content. Vanadium(+5) was extracted from soil reference materials with 0.1 M Na2CO3. The quantification of V(+5) was carried out by electrothermal atomic absorption spectrometry (ET-AAS). The concentration of V(+5) in the analyzed CRMs was found to be ranging between 3.60 and 86.0 μg g-1. It was also found that SQC001 contains approximately 88% of vanadium as V(+5) species. Statistical evaluation of the results of the two methods by paired t-test was in good agreement at 95% level of confidence.

  6. The coupling of rapidly synergistic cloud point extraction with thermospray flame furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Rapidly synergistic cloud point extraction (RS-CPE) was coupled with thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) to result in new CPE patterns and accelerated (1 min) protocols. It is demonstrated, for the case of copper (II) ion, that TS-FF-AAS improves the sampling efficiency and the sensitivity of FAAS determinations. Problems of nebulization associated with previous methods based on the coupling of FAAS and RS-CPE are overcome. TS-FF-AAS also improves sensitivity and gives a limit of detection for copper of 0.20 μg L-1, which is better by a factor of 32. Compared to direct FAAS, the factor is 114. (author)

  7. Determination of Trace Selenium in Electrolytic Manganese by Graphite Furnace Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    YAO Jun; ZHOU Fang-qin; MA Cheng-jin; TUO Yong; LIU Jian-ben; WU Zhu-qin; TAN Zhu-zhong

    2003-01-01

    The effects of four types of graphite tube and five matrix modifiers on the determination of selenium by graphite furnace atomic absorption spectrometry were compared.The results show that platform thermolysis coat graphite tube and magnesium nitrate and cobaltco as matrix modifer can get a high sensitivity and a good recovery.The optimized working conditions and interference in the determination were invesigated.This result is consistent with that of XRF.The recovery is from 100.8 % to102.2 %,the relative standard deviation is from 3.47% to 5.56 % (n=9),and the detection limit of selenium is 378 pg (C=44.5μg/g to 97.3μg/g.).The proposed method can be applied to the rapid determination of selenium in electrolytic manganese.

  8. Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review.

    Science.gov (United States)

    de la Calle, Inmaculada; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

    2016-09-14

    An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. PMID:27566338

  9. Multi-element analysis of manganese nodules by atomic absorption spectrometry without chemical separation

    Science.gov (United States)

    Kane, J.S.; Harnly, J.M.

    1982-01-01

    Five manganese nodules, including the USGS reference nodules A-1 and P-1, were analyzed for Co, Cu, Fe, K, Mg, Mn, Na, Ni and Zn without prior chemical separation by using a simultaneous multi-element atomic absorption spectrometer with an air-cetylene flame. The nodules were prepared in three digestion matrices. One of these solutions was measured using sixteen different combinations of burner height and air/acetylene ratios. Results for A-1 and P-1 are compared to recommended values and results for all nodules are compared to those obtained with an inductively coupled plasma. The elements Co, Cu, Fe, K, Mg, Mn, Na, Ni, and Zn are simultaneously determined with a composite recovery for all elements of 100 ?? 7%, independent of the digestion matrices, heights in the flame, or flame stoichiometries examined. Individual recoveries for Co, K, and Ni are considerably poorer in two digests than this composite figure, however. The optimum individual recoveries of 100 ?? 5% and imprecisions of 1-4%, except for zinc, are obtained when Co, K, Mn, Na and Ni are determined simultaneously in a concentrated digest, and in another analytical sequence, when Cu, Fe, Mg, Mn and Zn are measured simultaneously after dilution. Determination of manganese is equally accurate in the two sequences; its measurement in both assures internal consistency between the two measurement sequences. This approach improves analytical efficiency over that for conventional atomic absorption methods, while minimizing loss of accuracy or precision for individual elements. ?? 1982.

  10. Extraction and preconcentration of trace levels of cobalt using functionalized magnetic nanoparticles in a sequential injection lab-on-valve system with detection by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Graphical abstract: An approach to performing extraction and preconcentration employing functionalized magnetic particles for the determination of cobalt in the sequential injection lab-on-valve system using detection by electrothermal atomic absorption spectrometry. Highlights: ► New SPE method for cobalt separation/preconcentration was reported. ► Functionalized magnetic nanoparticles were used as adsorbent. ► Extraction, elution, and detection procedures were performed in the LOV system. ► This automatic extraction technique provided a good platform for metal analysis. - Abstract: A new approach to performing extraction and preconcentration employing functionalized magnetic nanoparticles for the determination of trace metals is presented. Alumina-coated iron oxide nanoparticles were synthesized and used as the solid support. The nanoparticles were functionalized with sodium dodecyl sulfate and used as adsorbents for solid phase extraction of the analyte. Extraction, elution, and detection procedures were performed sequentially in the sequential injection lab-on-valve (SI-LOV) system followed by electrothermal atomic absorption spectrometry (ETAAS). Mixtures of hydrophobic analytes were successfully extracted from solution using the synthesized magnetic adsorbents. The potential use of the established scheme was demonstrated by taking cobalt as a model analyte. Under the optimal conditions, the calibration curve showed an excellent linearity in the concentration range of 0.01–5 μg L−1, and the relative standard deviation was 2.8% at the 0.5 μg L−1 level (n = 11). The limit of detection was 6 ng L−1 with a sampling frequency of 18 h−1. The present method has been successfully applied to cobalt determination in water samples and two certified reference materials.

  11. Mercury in Environmental and Biological Samples Using Online Combustion with Sequential Atomic Absorption and Fluorescence Measurements: A Direct Comparison of Two Fundamental Techniques in Spectrometry

    Science.gov (United States)

    Cizdziel, James V.

    2011-01-01

    In this laboratory experiment, students quantitatively determine the concentration of an element (mercury) in an environmental or biological sample while comparing and contrasting the fundamental techniques of atomic absorption spectrometry (AAS) and atomic fluorescence spectrometry (AFS). A mercury analyzer based on sample combustion,…

  12. Application of FTIR spectrometry to determine the atomic composition of submicron silicon nitride layers HxSirNzHy

    International Nuclear Information System (INIS)

    Authors presents the developed software that allows to use the data from Fourier transform infrared spectrometry to calculate atomic composition in the silicon nitride HxSirNzHy layers of the submicron thickness. Autonomous and rapid method for the quantitative analysis of the IR spectra does not require prior measurement of thickness and density of the layers

  13. SPECIATION OF SELENIUM(IV) AND SELENIUM(VI) USING COUPLED ION CHROMATOGRAPHY: HYDRIDE GENERATION ATOMIC ABSORPTION SPECTROMETRY

    Science.gov (United States)

    A simple method was developed to speciate inorganic selenium in the microgram per liter range using coupled ion chromatography-hydride generation atomic absorption spectrometry. Because of the differences in toxicity and adsorption behavior, determination of the redox states selenite, Se(IV), and s...

  14. The Use of Gas Chromatography and Mass Spectrometry to Introduce General Chemistry Students to Percent Mass and Atomic Mass Calculations

    Science.gov (United States)

    Pfennig, Brian W.; Schaefer, Amy K.

    2011-01-01

    A general chemistry laboratory experiment is described that introduces students to instrumental analysis using gas chromatography-mass spectrometry (GC-MS), while simultaneously reinforcing the concepts of mass percent and the calculation of atomic mass. Working in small groups, students use the GC to separate and quantify the percent composition…

  15. Nondestructive atomic compositional analysis of BeMgZnO quaternary alloys using ion beam analytical techniques

    Energy Technology Data Exchange (ETDEWEB)

    Zolnai, Z., E-mail: zolnai.zsolt@ttk.mta.hu [Research Centre for Natural Sciences, Institute of Technical Physics and Materials Science (MFA), Konkoly-Thege M. út 29-33, H-1121 Budapest (Hungary); Toporkov, M. [Department of Electrical and Computer Engineering, Virginia Commonwealth University, 601W Main St, Richmond, VA 23284 (United States); Volk, J. [Research Centre for Natural Sciences, Institute of Technical Physics and Materials Science (MFA), Konkoly-Thege M. út 29-33, H-1121 Budapest (Hungary); Department of Electrical and Computer Engineering, Virginia Commonwealth University, 601W Main St, Richmond, VA 23284 (United States); Demchenko, D.O. [Department of Physics, Virginia Commonwealth University, 701W. Grace St., Richmond, VA 23284 (United States); Okur, S. [Department of Electrical and Computer Engineering, Virginia Commonwealth University, 601W Main St, Richmond, VA 23284 (United States); Szabó, Z. [Research Centre for Natural Sciences, Institute of Technical Physics and Materials Science (MFA), Konkoly-Thege M. út 29-33, H-1121 Budapest (Hungary); Özgür, Ü.; Morkoç, H.; Avrutin, V. [Department of Electrical and Computer Engineering, Virginia Commonwealth University, 601W Main St, Richmond, VA 23284 (United States); Kótai, E. [Wigner Research Centre for Physics, Institute for Particle and Nuclear Physics, Konkoly-Thege M. út 29-33, H-1121 Budapest (Hungary)

    2015-02-01

    Highlights: • BeMgZnO thin layers were grown with plasma-assisted molecular beam epitaxy (MBE). • The Be contents were accurately measured with RBS and proton elastic backscattering. • The Tauc bandgap was measured from optical transmittance experiments. • The bandgap has been varied between 3.26 eV and 4.62 eV via the Be and Mg content. • Experimental and density functional theory calculated bandgaps were in good agreement. - Abstract: The atomic composition with less than 1–2 atom% uncertainty was measured in ternary BeZnO and quaternary BeMgZnO alloys using a combination of nondestructive Rutherford backscattering spectrometry with 1 MeV He{sup +} analyzing ion beam and non-Rutherford elastic backscattering experiments with 2.53 MeV energy protons. An enhancement factor of 60 in the cross-section of Be for protons has been achieved to monitor Be atomic concentrations. Usually the quantitative analysis of BeZnO and BeMgZnO systems is challenging due to difficulties with appropriate experimental tools for the detection of the light Be element with satisfactory accuracy. As it is shown, our applied ion beam technique, supported with the detailed simulation of ion stopping, backscattering, and detection processes allows of quantitative depth profiling and compositional analysis of wurtzite BeZnO/ZnO/sapphire and BeMgZnO/ZnO/sapphire layer structures with low uncertainty for both Be and Mg. In addition, the excitonic bandgaps of the layers were deduced from optical transmittance measurements. To augment the measured compositions and bandgaps of BeO and MgO co-alloyed ZnO layers, hybrid density functional bandgap calculations were performed with varying the Be and Mg contents. The theoretical vs. experimental bandgaps show linear correlation in the entire bandgap range studied from 3.26 eV to 4.62 eV. The analytical method employed should help facilitate bandgap engineering for potential applications, such as solar blind UV photodetectors and

  16. A espectrometria atômica e a determinação de elementos metálicos em material polimérico Atomic spectrometry and the determination of metals in polymeric materials

    Directory of Open Access Journals (Sweden)

    Solange Cadore

    2008-01-01

    Full Text Available Polymeric materials are widely used in the chemical industry and are part of our daily lives. Inorganic species may be added to them as additives, anti-oxidizing agents, stabilizers, plasticizers, colorants and catalysts and may be present in a wide range of concentrations. Their determination demands the development of analytical methods considering different kinds of polymeric materials, their composition and the final use of the material. Although many different analytical techniques may be used, this review emphasizes those based on atomic absorption and emission spectrometry. Solid sampling techniques and digestion methods are described and discussed and compared considering published results.

  17. Electrochemical hydride generation atomic fluorescence spectrometry for detection of tin in canned foods using polyaniline-modified lead cathode

    International Nuclear Information System (INIS)

    An electrochemical hydride generation system with polyaniline-modified lead cathode was developed for tin determination by coupling with atomic fluorescence spectrometry. The tin fluorescence signal intensity was improved evidently as the polyaniline membrane could facilitate the transformation process from atomic tin to the SnH4 and prevent the aggradation of Sn atom on Pb electrode surface. The effects of experimental parameters and interferences have been studied. The limit of detection (LOD) was 1.5 ng mL-1 (3σ) and the relative standard deviation (RSD) was 3.3% for 11 consecutive measurements of 50 ng mL-1 Sn(IV) standard solution.

  18. Analytic Evaluation of some 2-, 3- and 4- Electron Atomic Integrals Containing Exponentially Correlated Functions of $r_{ij}$

    CERN Document Server

    Padhy, Bholanath

    2016-01-01

    A simple method is outlined for analytic evaluation of the basic 2-electron atomic integral with integrand containing products of atomic s-type Slater orbitals and exponentially correlated function of the form $r_{ij} exp(-\\lambda_{ij}r_{ij})$, by employing the Fourier representation of $exp(-\\lambda_{ij}r_{ij})/r_{ij}$ without the use of either the spherical harmonic addition theorem or the Feynman technique. This method is applied to obtain closed-form expressions, in a simple manner, for certain other 2-,3- and 4-electron atomic integrals with integrands which are products of exponentially correlated functions and atomic s-type Slater orbitals.

  19. Validação de metodologia analítica para determinação de mercúrio total em amostras de urina por espectrometria de absorção atômica com geração de vapor frio (CV-AAS: estudo de caso Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS: case study

    Directory of Open Access Journals (Sweden)

    Sabine Neusatz Guilhen

    2010-01-01

    Full Text Available Mercury is a toxic metal used in a variety of substances over the course history. One of its more dubious uses is in dental amalgam restorations. It is possible to measure very small concentrations of this metal in the urine of exposed subjects by the cold vapor atomic absorption technique. The present work features the validation as an essential tool to confirm the suitability of the analytical method chosen to accomplish such determination. An initial analysis will be carried out in order to evaluate the environmental and occupational levels of exposure to mercury in 39 members of the auxiliary dental staff at public consulting rooms in the city of Araguaína (TO.

  20. Mesoporous Silica Nanoparticles as an Adsorbent for Preconcentration and Determination of Trace Amount of Nickel in Environmental Samples by Atom Trap Flame Atomic Absorption Spectrometry

    Science.gov (United States)

    Shirkhanloo, H.; Falahnejad, M.; Zavvar Mousavi, H.

    2016-01-01

    A rapid enrichment method based on solid-phase extraction (SPE) has been established for preconcentration and separation of trace Ni(II) ions in water samples prior to their determination by atom trap flame atomic absorption spectrometry. A column filled with bulky NH2-UVM7 was used as the novel adsorbent. Under optimal conditions, the linear range, limit of detection (LOD), and preconcentration factor (PF) were 3-92 μg/L, 0.8 μg/L, and 100, respectively. The validity of the method was checked by the standard reference material.

  1. Mass Spectrometry as a Powerful Analytical Technique for the Structural Characterization of Synthesized and Natural Products

    Science.gov (United States)

    Es-Safi, Nour-Eddine; Essassi, El Mokhtar; Massoui, Mohamed; Banoub, Joseph

    Mass spectrometry is an important tool for the identification and structural elucidation of natural and synthesized compounds. Its high sensitivity and the possibility of coupling liquid chromatography with mass spectrometry detection make it a technique of choice for the investigation of complex mixtures like raw natural extracts. The mass spectrometer is a universal detector that can achieve very high sensitivity and provide information on the molecular mass. More detailed information can be subsequently obtained by resorting to collision-induced dissociation tandem mass spectrometry (CID-MS/MS). In this review, the application of mass spectrometric techniques for the identification of natural and synthetic compounds is presented. The gas-phase fragmentation patterns of a series of four natural flavonoid glycosides, three synthesized benzodiazepines and two synthesized quinoxalinone derivatives were investigated using electrospray ionization mass spectrometry (ESI-MS) and tandem mass spectrometry techniques. Exact accurate masses were measured using a modorate resolution quadrupole orthogonal time-of-flight QqTOF-MS/MS hybrid mass spectrometer instrument. Confirmation of the molecular masses and the chemical structures of the studied compounds were achieved by exploring the gas-phase breakdown routes of the ionized molecules. This was rationalized by conducting low-energy collision CID-MS/MS analyses (product ion- and precursor ion scans) using a conventional quadrupole hexapole-quadrupole (QhQ) tandem mass spectrometer.

  2. Arsenic species analysis in porewaters and sediments using hydride generation atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    LIAO Meng-xia; DENG Tian-long

    2006-01-01

    It was observed that the atomic fluorescence emission due to As(Ⅴ) could has a 10% to 40% of fluorescence emission signal during the determination of As(Ⅲ) in the mixture of As(Ⅲ) and As(Ⅴ). Besides, interferes from heavy metals such as Pb(Ⅱ),Cu(Ⅱ) can cause severe increase of the signals as compared to the insignificant effects caused by Cd(Ⅱ), Zn(Ⅱ), Mn(Ⅱ) and Fe(Ⅲ). On the basis of further studies, the masking agent of 8-hydroxyquinoline was used as an efficient agent to eliminate interference of As(Ⅴ)emission and the heavy metal of Cu2+ and Pb2+ in the measurements of arsenic species. After a series standard additions and CRM researches, a sensitive and interference-free analytical procedure was developed for the speciation of arsenic in samples ofporewaters and sediments in Poyang Lake, China.

  3. Coacervative extraction of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hagarová, Ingrid, E-mail: hagarova@fns.uniba.sk; Bujdoš, Marek; Matúš, Peter; Kubová, Jana

    2013-10-01

    In this work, a relatively simple and sensitive method for separation/preconcentration of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry has been proposed. The method is based on the extraction of Pb–dithizone chelate with coacervates made up of lauric acid in the presence of potassium ions and methanol. Several important factors affecting extraction efficiency such as pH, concentration of lauric acid and dithizone, ionic strength, incubation and centrifugation time were investigated and optimized. After separation of aqueous bulk solution from surfactant-rich phase, the final extract was redissolved by using 500 μl of methanol acidified with 0.2 mol l{sup −1} HNO{sub 3}. Under the optimized conditions (using initial sample volume of 10 ml), enrichment factor of 17.0, detection limit of 0.12 μg l{sup −1}, quantification limit of 0.38 μg l{sup −1}, relative standard deviation of 4.2% (for 2 μg l{sup −1} of Pb; n = 26), linearity of the calibration graph in the range of 0.5–4.0 μg l{sup −1} (with correlation coefficient better than 0.995) were achieved. The method was validated by the analysis of certified reference material (TMDA-61). Extraction recoveries for the CRM, spiked model solutions and spiked natural water samples were in the range of 91–96%. Finally, the method was applied to the separation/preconcentration and determination of trace lead in natural waters. - Highlights: • The potential of coacervates for the extraction of metal ions is examined. • No difficulties in coupling of ETAAS with the proposed CAE are observed. • Achieved preconcentration factor results in enhanced sensitivity. • Analytical performance is confirmed by the reliable determination of trace Pb. • The proposed CAE is ecofriendly and efficient.

  4. Determination of calcium, magnesium and zinc in lubricating oils by flame atomic absorption spectrometry using a three-component solution.

    Science.gov (United States)

    Zmozinski, Ariane V; de Jesus, Alexandre; Vale, Maria G R; Silva, Márcia M

    2010-12-15

    Lubricating oils are used to decrease wear and friction of movable parts of engines and turbines, being in that way essential for the performance and the increase of that equipment lifespan. The presence of some metals shows the addition of specific additives such as detergents, dispersals and antioxidants that improve the performance of these lubricants. In this work, a method for determination of calcium, magnesium and zinc in lubricating oil by flame atomic absorption spectrometry (F AAS) was developed. The samples were diluted with a small quantity of aviation kerosene (AVK), n-propanol and water to form a three-component solution before its introduction in the F AAS. Aqueous inorganic standards diluted in the same way have been used for calibration. To assess the accuracy of the new method, it was compared with ABNT NBR 14066 standard method, which consists in diluting the sample with AVK and in quantification by F AAS. Two other validating methods have also been used: the acid digestion and the certified reference material NIST (SRM 1084a). The proposed method provides the following advantages in relation to the standard method: significant reduction of the use of AVK, higher stability of the analytes in the medium and application of aqueous inorganic standards for calibration. The limits of detection for calcium, magnesium and zinc were 1.3 μg g(-1), 0.052 μg g(-1) and 0.41 μg g(-1), respectively. Concentrations of calcium, magnesium and zinc in six different samples obtained by the developed method did not differ significantly from the results obtained by the reference methods at the 95% confidence level (Student's t-test and ANOVA). Therefore, the proposed method becomes an efficient alternative for determination of metals in lubricating oil.

  5. Determination of manganese in diesel, gasoline and naphtha by graphite furnace atomic absorption spectrometry using microemulsion medium for sample stabilization

    Science.gov (United States)

    Brandão, Geisamanda Pedrini; de Campos, Reinaldo Calixto; de Castro, Eustáquio Vinicius Ribeiro; de Jesus, Honério Coutinho

    2008-08-01

    The determination of Mn in diesel, gasoline and naphtha samples at µg L - 1 level by graphite furnace atomic absorption spectrometry, after sample stabilization in a three-component medium (microemulsion) was investigated. Microemulsions were prepared by mixing appropriate volumes of sample, propan-1-ol and nitric acid aqueous solution, and a stable system was immediately and spontaneously formed. After multivariate optimization by central composite design the optimum microemulsion composition as well as the temperature program was defined. In this way, calibration using aqueous analytical solution was possible, since the same sensitivity was observed in the optimized microemulsion media and 0.2% v/v HNO 3. The use of modifier was not necessary. Recoveries at the 3 µg L - 1 level using both inorganic and organic Mn standards spiked solutions ranged from 98 to 107% and the limits of detection were 0.6, 0.5 and 0.3 µg L - 1 in the original diesel, gasoline and naphtha samples, respectively. The Mn characteristic mass 3.4 pg. Typical relative standard deviation ( n = 5) of 8, 6 and 7% were found for the samples prepared as microemulsions at concentration levels of 1.3, 0.8, and 1.5 µg L - 1 , respectively. The total determination cycle lasted 4 min for diesel and 3 min for gasoline and naphtha, equivalent to a sample throughput of 7 h - 1 for duplicate determinations in diesel and 10 h - 1 for duplicate determinations in gasoline and naphtha. Accuracy was also assessed by using other method of analysis (ASTM D 3831-90). No statistically significant differences were found between the results obtained with the proposed method and the reference method in the analysis of real samples.

  6. Combination of cloud point extraction and flame atomic absorption spectrometry for preconcentration and determination of nickel and manganese ions in water and food samples

    International Nuclear Information System (INIS)

    A simple, rapid, inexpensive, and nonpolluting cloud point extraction (CPE) technique has been improved for the preconcentration and determination of nickel and manganese. After complexation with p-nitrophenylazoresorcinol (Magneson I), the analytes could be competitively extracted in a surfactant octylphenoxy polyethoxyethanol (Triton X-114), prior to determination by flame atomic absorption spectrometry (FAAS). The effects of experimental conditions such as pH, concentration of chelating agent and surfactant, equilibration temperature and time on CPE were studied. Under the optimum conditions, preconcentration of a 25 mL sample solution permitted the detection of 2.7 ng mL-1 Ni2+ and 2.9 ng mL-1 Mn2+ with enrichment factors of 17 and 19 for Ni2+ and Mn2+, respectively. The developed method was applied to the determination of trace nickel and manganese in water and food samples with satisfactory results.

  7. Flow injection analysis-flame atomic absorption spectrometry system for indirect determination of cyanide using cadmium carbonate as a new solid-phase reactor

    Energy Technology Data Exchange (ETDEWEB)

    Noroozifar, M. [Analytical Research Laboratory, Department of Chemistry, Sistan and Baluchestan University, P.O. Box 98165-181, Zahedan (Iran, Islamic Republic of)]. E-mail: mnoroozifar@hamoon.usb.ac.ir; Khorasani-Motlagh, M. [Inorganic Research Laboratory, Department of Chemistry, Sistan and Baluchestan University, Zahedan (Iran, Islamic Republic of); Hosseini, S.-N. [Analytical Research Laboratory, Department of Chemistry, Sistan and Baluchestan University, P.O. Box 98165-181, Zahedan (Iran, Islamic Republic of)

    2005-01-10

    A new and simple flow injection system procedure has been developed for the indirect determination of cyanide. The method is based on insertion of aqueous cyanide solutions into an on-line cadmium carbonate packed column (25% m/m suspended on silica gel beads) and a sodium hydroxide with pH 10 is used as the carrier stream. The eluent containing the analyte as cadmiumcyanide complexes, produced from reaction between cadmium carbonate and cyanide, measured by flame atomic absorption spectrometry. The absorbance is proportional to the concentration of cyanide in the sample. The linear range of the system is up to 15 mg L{sup -1} with a detection limit 0.2 mg L{sup -1} and sampling rate 72 h{sup -1}. The method is suitable for determination of cyanide in industrial waste waters with a relative standard deviation better than 1.22%.

  8. Combination of cloud point extraction and flame atomic absorption spectrometry for preconcentration and determination of nickel and manganese ions in water and food samples

    Energy Technology Data Exchange (ETDEWEB)

    Arpa Sahin, Cigdem, E-mail: carpa@hacettepe.edu.tr [Hacettepe University, Chemistry Department, 06800, Beytepe, Ankara (Turkey); Efecinar, Melis; Satiroglu, Nuray [Hacettepe University, Chemistry Department, 06800, Beytepe, Ankara (Turkey)

    2010-04-15

    A simple, rapid, inexpensive, and nonpolluting cloud point extraction (CPE) technique has been improved for the preconcentration and determination of nickel and manganese. After complexation with p-nitrophenylazoresorcinol (Magneson I), the analytes could be competitively extracted in a surfactant octylphenoxy polyethoxyethanol (Triton X-114), prior to determination by flame atomic absorption spectrometry (FAAS). The effects of experimental conditions such as pH, concentration of chelating agent and surfactant, equilibration temperature and time on CPE were studied. Under the optimum conditions, preconcentration of a 25 mL sample solution permitted the detection of 2.7 ng mL{sup -1} Ni{sup 2+} and 2.9 ng mL{sup -1} Mn{sup 2+} with enrichment factors of 17 and 19 for Ni{sup 2+} and Mn{sup 2+}, respectively. The developed method was applied to the determination of trace nickel and manganese in water and food samples with satisfactory results.

  9. Functionalization of cross linked chitosan with 2-aminopyridine-3-carboxylic acid for solid phase extraction of cadmium and zinc ions and their determination by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    We have developed a new method for solid phase extraction (SPE) and preconcentration of trace amounts of cadmium and zinc using cross linked chitosan that was functionalized with 2-aminopyridine-3-carboxy acid. Analytical parameters, sample pH, effect of flow rate, sample volume, and concentration of eluent on column SPE were investigated. The effect of matrix ions on the recovery of cadmium and zinc has been investigated and were found not to interfere with preconcentration. Under the optimum experimental conditions, the preconcentration factors for Cd(II) and Zn(II) were found to be 90. The two elements were quantified via atomic absorption spectrometry. The detection limits for cadmium and zinc are 21 and 65 ng L -1, respectively. The method was evaluated by analyzing a certified reference material (NIST 1643e; water) and has been successfully applied to the analysis of cadmium and zinc in environmental water samples. (author)

  10. Solid sampling determination of lithium and sodium additives in microsamples of yttrium oxyorthosilicate by high-resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Laczai, Nikoletta; Kovács, László; Péter, Ágnes; Bencs, László

    2016-03-01

    Solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (SS-HR-CS-GFAAS) methods were developed and studied for the fast and sensitive quantitation of Li and Na additives in microsamples of cerium-doped yttrium oxyorthosilicate (Y2SiO5:Ce) scintillator materials. The methods were optimized for solid samples by studying a set of GFAAS conditions (i.e., the sample mass, sensitivity of the analytical lines, and graphite furnace heating programs). Powdered samples in the mass range of 0.099-0.422 mg were dispensed onto graphite sample insertion boats, weighed and analyzed. Pyrolysis and atomization temperatures were optimized by the use of single-element standard solutions of Li and Na (acidified with 0.144 mol/L HNO3) at the Li I 610.353 nm and Na I 285.3013 nm analytical lines. For calibration purposes, the method of standard addition with Li and Na solutions was applied. The correlation coefficients (R values) of the calibration graphs were not worse than 0.9678. The limit of detection for oxyorthosilicate samples was 20 μg/g and 80 μg/g for Li and Na, respectively. The alkaline content of the solid samples were found to be in the range of 0.89 and 8.4 mg/g, respectively. The accuracy of the results was verified by means of analyzing certified reference samples, using methods of standard (solution) addition calibration.

  11. An automated flow injection system for metal determination by flame atomic absorption spectrometry involving on-line fabric disk sorptive extraction technique.

    Science.gov (United States)

    Anthemidis, A; Kazantzi, V; Samanidou, V; Kabir, A; Furton, K G

    2016-08-15

    A novel flow injection-fabric disk sorptive extraction (FI-FDSE) system was developed for automated determination of trace metals. The platform was based on a minicolumn packed with sol-gel coated fabric media in the form of disks, incorporated into an on-line solid-phase extraction system, coupled with flame atomic absorption spectrometry (FAAS). This configuration provides minor backpressure, resulting in high loading flow rates and shorter analytical cycles. The potentials of this technique were demonstrated for trace lead and cadmium determination in environmental water samples. The applicability of different sol-gel coated FPSE media was investigated. The on-line formed complex of metal with ammonium pyrrolidine dithiocarbamate (APDC) was retained onto the fabric surface and methyl isobutyl ketone (MIBK) was used to elute the analytes prior to atomization. For 90s preconcentration time, enrichment factors of 140 and 38 and detection limits (3σ) of 1.8 and 0.4μgL(-1) were achieved for lead and cadmium determination, respectively, with a sampling frequency of 30h(-1). The accuracy of the proposed method was estimated by analyzing standard reference materials and spiked water samples. PMID:27260436

  12. Optimized determination of iron in grape juice, wines, and other alcoholic beverages by atomic absorption spectrometry.

    Science.gov (United States)

    Olalla, M; Cruz González, M; Cabrera, C; López, M C

    2000-01-01

    This paper describes a study of the different methods of sample preparation for the determination of iron in grape juice, wines, and other alcoholic beverages by atomic absorption spectrometry with electrothermal atomization; results are also reported for the practical application of these methods to the analysis of commercial samples produced in Spain. The methods examined include dealcoholization and dry and wet mineralization treatment using different acids and/or mixtures of them, both with and without heating. The sensitivity, detection limit, accuracy, precision, and selectivity of each method were established. The best results were obtained for wet mineralization with heated acid (HNO3-H2SO4); the results for table wines had an accuracy of 97.5-101.6%, a relative standard deviation of 3.51%, a detection limit of 19.2 micrograms/L, and a determination limit of 32.0 micrograms/L. The method was also sufficiently sensitive and selective. It was applied to the determination of iron in grape juice, different types of wines, and beverages with high alcoholic content, all of which are produced and widely consumed in Spain. The values obtained ranged from 3.394 +/- 2.15 mg/L for the juice, 2.938 +/- 1.47 mg/L for the white wines, 19.470 +/- 5.43 mg/L for the sweet wines, 0.311 +/- 0.07 mg/L for the brandies, and 0.564 +/- 0.12 mg/L for the anisettes. Thus, the method is useful for routine analysis in the quality control of these beverages. PMID:10693020

  13. Hooke's Atom in an Arbitrary External Electric Field: Analytical Solutions of Two-Electron Problem by Path Integral Approach

    Institute of Scientific and Technical Information of China (English)

    CAI Liang; ZHANG Ping; YANG Tao; PAN Xiao-Yin

    2011-01-01

    By using the path integral approach, we investigate the problem of Hooke's atom (two electrons interacting with Coulomb potential in an external harmonic-oscillator potential) in an arbitrary time-dependent electric field. For a certain infinite set of discrete oscillator frequencies, we obtain the analytical solutions. The ground state polarization of the atom is then calculated. The same result is also obtained through linear response theory.

  14. Determination of selenium and tellurium in the gas phase using specific columns and atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Muangnoicharoen, S.; Chiou, K.Y.; Manuel, O.K.

    1986-11-01

    Total selenium and tellurium in the gas phase were analyzed after adsorption on gold-coated beads and charcoal. The thermally eluting gas was trapped on columns filled with quartz beads that were cooled in an ice bath. The beads were boiled in dilute HCl, and the resulting solution was analyzed for Se and Te by graphite furnace atomic absorption spectrometry. Their results demonstrate that gold-coated beads efficiently trap gaseous Se and Te at a low gas flow rate, but at higher flow rates charcoal traps are more expedient. With charcoal traps, it was found that local air samples contain Se in the range of 0.92-3.05 ng m/sup -3/ and Te in the range of 0.10-0.34 ng m/sup -3/. Detection limits down to about 0.1 ng m/sup -3/ allow the ready detection of Se and Te in rural air with a precision of about +/- 6% at the nanogram level of Te and about +/- 4% at the nanogram level of Se.

  15. Determination of inorganic species of Sb and Te in cereals by hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Reyes, Mariela N.M.; Cervera, Maria L.; Guardia, Miguel de la, E-mail: m.luisa.cervera@uv.e [University of Valencia, Valencia (Spain). Dept. of Analytical Chemistry

    2011-07-01

    A non-chromatographic fast, sensitive and easy method has been developed for the determination of Sb(III), Sb(V), Te(IV) and Te(VI) in cereal samples. The procedure is based on ultrasound assisted extraction and determination by hydride generation atomic fluorescence spectrometry (HG AFS). Preliminary studies were made in order to get the best extraction efficiency using 1 mol L{sup -1} phosphoric acid, 1 mol L{sup -1} nitric acid, aqua regia, 1 mol L{sup -1} sulfuric acid and 6 mol L{sup -1} hydrochloric acid. The extraction with aqua regia showed a clear interconversion of the species during the process, being H{sub 2}SO{sub 4} the best extractant with efficiencies greater than 90% from the total content of Sb and Te quantified previously and without species interconversion. This point was checked by recovery experiments at different spiked levels. The method provided limits of detection values from 0.1 to 0.5 ng g{sup -1} with relative standard deviation values from 5.4 to 9.2% of 10 independent analysis of samples containing few ng g-1 of Sb and Te species. (author)

  16. Determination of inorganic species of Sb and Te in cereals by hydride generation atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    A non-chromatographic fast, sensitive and easy method has been developed for the determination of Sb(III), Sb(V), Te(IV) and Te(VI) in cereal samples. The procedure is based on ultrasound assisted extraction and determination by hydride generation atomic fluorescence spectrometry (HG AFS). Preliminary studies were made in order to get the best extraction efficiency using 1 mol L-1 phosphoric acid, 1 mol L-1 nitric acid, aqua regia, 1 mol L-1 sulfuric acid and 6 mol L-1 hydrochloric acid. The extraction with aqua regia showed a clear interconversion of the species during the process, being H2SO4 the best extractant with efficiencies greater than 90% from the total content of Sb and Te quantified previously and without species interconversion. This point was checked by recovery experiments at different spiked levels. The method provided limits of detection values from 0.1 to 0.5 ng g-1 with relative standard deviation values from 5.4 to 9.2% of 10 independent analysis of samples containing few ng g-1 of Sb and Te species. (author)

  17. Determination of manganese in thermoluminescent materials by inductively coupled plasma atomic emission spectrometry and spectrophotometry

    International Nuclear Information System (INIS)

    The content of manganese in the mixed fluorides CaF2: MnF2 and CaF2: Mn thermoluminophors was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and spectrophotometry. The various Mn emission lines were compared and the manganese emission line at 257.610 nm was used for ICP-AES analysis. For the spectrophotometric determination the manganese(II) ions were oxidized to intensively coloured permanganate ions using potassium periodate. No statistically significant differences were found between the results of ICP-AES and spectrophotometric methods of analysis. The thermoluminophors were synthesized by coprecipitation of manganese with CaF2, varying the concentration of manganese in the initial solutions in the range of 0.01 - 2.0 % (m/m). The coprecipitated mixed fluorides CaF2: MnF2 were heated at 1423 K. The glow curves of synthesized CaF2: Mn thermoluminophors were measured. (author)

  18. Speciation Analysis of Serum Copper by Ultrafiltration Com-bined with Graphite Furnace Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    WANG Zhi-Hua; MA Hui-Min; MA Quan-Li; LIANG Shu-Chuan

    2001-01-01

    UItrafiltration combined with graphite furnace atomic absorp-tion spectrometry(GFAAS)was used to study protein binding and speciation of copper in human serum..UItrafiltration was carried out using a cell unit ultrafiltration membraoes having a nominal cut-off of 10,000Dalton.The effects of var-ious experimental factors including the kind and concentration of electrolyte,sample storge,pH,pressure and the precon-ditioning of the membranes on the speciation analysis of serum copper by ultrafiltration were examined.It was observed that 4.5±2.3% of the total copper in serum was ultrafiltrable and this value did not seem to be influenced by the total serum ele-mental concentration,the PH (6.5——10) adn the pressure(≤1.5kg/cm2).the preconditioning of the ultrafiltration system with 0.1mol/L calcium nitrate can overcome the adsorption loss of copper effectively,and the addition of tris-HCI sohtion (pH 7.4)to serum accelerates the ultrafiltration.The present method was proved to be suitable for speciation analysis for its simplicity,rapidity,small sample reuqirement and easy con-trol.The results obtained with the method are accurate and reliable.

  19. Determination of lead in croatian wines by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A method has been developed for direct determination of lead in wine by graphite furnace atomic absorption spectrometry (GFAAS) with Zeeman-effect background correction. The thermal behaviour of Pb during pyrolysis and atomisation stages was investigated without matrix modifier and in the presence of Pd(NO3)2, Pd(NO3)2 + Mg(NO3)2 x 6H2O, and NH4H2PO4 + Mg(NO3)2 x 6H2O as matrix modifiers. A simple 1:1 dilution of wine samples with Pd(NO3)2 as a matrix modifier proved optimal for accurate determination of Pb in wine. Mean recoveries were 106 % for red and 114 % for white wine, and the detection limit was 3 μg L-1. Within-run precision of measurements for red and white wine was 2.1 % and 1.8 %, respectively. The proposed method was applied for analysis of 23 Croatian wines. Median Pb concentrations were 33 μg L-1, range (16 to 49) μg L-1 in commercially available wines and 46 μg L-1, range (14 to 559) μg L-1 in home-made wines. There were no statistically significant differences (P<0.05) in Pb concentration between commercial and home-made wines or between red and white wines. (authors)

  20. EVALUATION OF HEAVY METALS CONTENT IN EDIBLE MUSHROOMS BY MICROWAVE DIGESTION AND FLAME ATOMIC ABSORPTION SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Cristiana Radulescu

    2011-05-01

    Full Text Available The aim of this work was to determine the heavy metal (Cd, Cr, Ni, Pb, Mn, Zn, Fe and Cu content of the fruiting bodies (cap and stipe of four species (Amanita caesarea, Pleurotus ostreatus, Fistulina hepatica and Armillariella mellea and their substrate, collected from forest sites in Dâmboviţa County, Romania. The elements were determined by Flame Atomic Absorption Spectrometry (FAAS after microwave assisted digestion. From the same collecting point were taken n = 5 samples of young and mature fruiting bodies of mushrooms and their substrate. The high concentrations of lead, chrome and cadmium (Pb: 0.25 – 1.89 mg.kg-1, Cr: 0.36 – 1.94 mg.kg-1, Cd: 0.23 – 1.13 mg.kg-1 for all collected wild edible mushrooms, were determined. These data were compared with maximum level for certain contaminants in foodstuffs established by the commission of the European Committees (EC No 466/2001. A quantitative evaluation of the relationship of element uptake by mushrooms from substrate was made by calculating the accumulation coefficient (Ka. The moderately acid pH value of soil influenced the accumulation of Zn and Cd inside of the studied species. The variation of heavy metals content between edible mushrooms species is dependent upon the ability of the species to extract elements from the substrate and on the selective uptake and deposition of metals in tissue.

  1. Determination of iron in natural and mineral waters by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    ROLANDAS KAZLAUSKAS

    2004-05-01

    Full Text Available Simple methods for the determination of Fe in natural and mineral waters by flame atomic absorption spectrometry (AAS are suggested. The results of the investigation of selectivity of the proposed AAS method proved that this procedure is not affected by high concentrations of other metals. The calibration graph for iron was linear at levels near the detection limit up to at least 0.10 mg ml-1. For the determination of microamounts of iron in mineral waters, an extraction AAS technique was developed. Iron was retained as Fe-8-oxyquinoline complex and extracted into chloroform. The optimal conditions for the extraction of the iron complex were determined. The AAS method was applied to the determination of Fe in mineral waters and natural waters from different areas of Lithuania. The accuracy of the developed method was sufficient and evaluated in comparison with a photometric method. The obtained results demonstrated that the procedure could be successfully applied for the analysis of water samples with satisfactory accuracy.

  2. Determination of cadmium in water samples by fast pyrolysis-chemical vapor generation atomic fluorescence spectrometry

    Science.gov (United States)

    Zhang, Jingya; Fang, Jinliang; Duan, Xuchuan

    2016-08-01

    A pyrolysis-vapor generation procedure to determine cadmium by atomic fluorescence spectrometry has been established. Under fast pyrolysis, cadmium ion can be reduced to volatile cadmium species by sodium formate. The presence of thiourea enhanced the efficiency of cadmium vapor generation and eliminated the interference of copper. The possible mechanism of vapor generation of cadmium was discussed. The optimization of the parameters for pyrolysis-chemical vapor generation, including pyrolysis temperature, amount of sodium formate, concentration of hydrochloric acid, and carrier argon flow rate were carried out. Under the optimized conditions, the absolute and concentration detection limits were 0.38 ng and 2.2 ng ml- 1, respectively, assuming that 0.17 ml of sample was injected. The generation efficiency of was 28-37%. The method was successfully applied to determine trace amounts of cadmium in two certified reference materials of Environmental Water (GSB07-1185-2000 and GSBZ 50009-88). The results were in good agreement with the certified reference values.

  3. Stabilizing Agents for Calibration in the Determination of Mercury Using Solid Sampling Electrothermal Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    Hana Zelinková

    2012-01-01

    Full Text Available Tetramethylene dithiocarbamate (TMDTC, diethyldithiocarbamate (DEDTC, and thiourea were investigated as stabilizing agents for calibration purposes in the determination of mercury using solid sampling electrothermal atomic absorption spectrometry (SS-ETAAS. These agents were used for complexation of mercury in calibration solutions and its thermal stabilization in a solid sampling platform. The calibration solutions had the form of methyl isobutyl ketone (MIBK extracts or MIBK-methanol solutions with the TMDTC and DEDTC chelates and aqueous solutions with thiourea complexes. The best results were obtained for MIBK-methanol solutions in the presence of 2.5 g L-1 TMDTC. The surface of graphite platforms for solid sampling was modified with palladium or rhenium by using electrodeposition from a drop of solutions. The Re modifier is preferable due to a higher lifetime of platform coating. A new SS-ETAAS procedure using the direct sampling of solid samples into a platform with an Re modified graphite surface and the calibration against MIBK-methanol solutions in the presence of TMDTC is proposed for the determination of mercury content in solid environmental samples, such as soil and plants.

  4. Use of Atomic Absorption Spectrometry in Assessment of Biomonitor Plants for Lead, Cadmium and Copper Pollution

    Institute of Scientific and Technical Information of China (English)

    Gokce Kaya; Mehmet Yaman

    2012-01-01

    Eleven plant species were collected from the vicinity of lead-battery plant in the city of Gaziantep,Turkey.Lead,cadmium and copper concentrations in the soil and leaves of plants were determined by atomic absorption spectrometry.Lead,Cd and Cu concentrations in the soil samples taken from battery area were found to be in the ranges of 304~602,0.4~0.44 and 31~37 mg · kg-1,respectively.Significantly increased lead concentration up to 2 750 mg · kg-1 was found in the leaves of Eleagnus angustifolia L.plant.The lead concentrations in the other plant leaves taken from 50 m around battery factory followed the order Ailanthus altissima >Morus sp.> Juglans regia L.> Ficus carica L.>Cydonia oblonga Miller> Prunus x domestica L.The plants,Populus nigra L.,Eleagnus angustifolia L.and Salix sp.were found useful for Cd,and the plant,Eleagnus angustifolia L.for Pb,to be considered as potential biomonitor.Especially,leaves of trees and plants taken from the distance of 50 m from battery plant have relatively higher Pb concentrations.Therefore,people who and animals which live in this area and benefit from these soil and plants have vital risks.

  5. Speciation of iron (II) and (III) by using solvent extraction and flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yaman, Mehmet [Department of Chemistry, Science and Arts Faculty, Firat University, Elazig (Turkey)]. E-mail: myaman@firat.edu.tr; Kaya, Gokce [Department of Chemistry, Science and Arts Faculty, Firat University, Elazig (Turkey)

    2005-05-17

    A method for speciation, preconcentration and separation of Fe{sup 2+} and Fe{sup 3+} in different matrices was developed using solvent extraction and flame atomic absorption spectrometry. PAN as complexing reagent for Fe{sup 2+} and chloroform as organic solvent were used. The complex of Fe{sup 2+}-PAN was extracted into chloroform phase in the pH range of 0.75-4.0 and Fe{sup 3+} remains in water phase in the pH range 0.75-1.25. The optimum conditions for maximum recovery of Fe{sup 2+} and minimum recovery of Fe{sup 3+} were determined as pH = 1, the stirring time of 20 min, the PAN amount of 0.5 mg and chloroform volume of 8 mL. The developed method was applied to the determination of Fe{sup 2+} and Fe{sup 3+} in tea infusion, fruit juice, cola and pekmez. It is seen that there is high bioavailable iron (Fe{sup 2+}) in pekmez. The developed method is sensitive, simple and need the shorter time in comparison with other similar studies.

  6. Wet sample digestion for quantification of vanadium(V) in serum by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Three types of pressure digestion systems used prior to the determination of the ultratrace element vanadium by electrothermal atomic absorption spectrometry were evaluated: The high-pressure ashing (HPA) system, the DAB III pressure digestion system and the pressurized microwave digestion (PMD) system. Complete sample digestion and no loss of graphite tube sensitivity as well as reliable vanadium values could only be achieved with HPA digests of freeze-dried serum. The mean recovery rate was 98% and no loss of tube sensitivity could be observed. Using non-lyophilized serum the mean recovery rate was 70%. The DAB III digestion system, vicarious for closed pressure digestion in steel bombs with an allowable temperature up to about 200C, cannot be recommended to mineralize human biological material for vanadium determinations, because the remaining not completely decomposed organic compounds extracted together with the vanadium-cupferron complex caused a marked carbon-buildup and formation of carbides in the graphite tube were found to change the shape of the absorption signals distinctly, and to decline the tube sensitivity strongly (about 25%) so that reliable results cannot be achieved. The recovery rate was too low in general (about 50%). In addition, a subsequent treatment of the DAB III digests with perchloric acid was unsuccessful. The PMD system proved to be not suited, because the samples became highly contaminated by vanadium possibly from the titan seal. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  7. Novel Method for Indirect Determination of Iodine in Marine Products by Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    LU Jian-ping; TAN Fang-wei; TANG Qiong; JIANG Tian-cheng

    2013-01-01

    A method for the determination of iodine based upon compound H2HgI4,formed between I-and Hg2+ in nitric acid and extracted in methyl isobutyl ketone(MIBK),was developed via atomic fluorescence spectrometry(AFS).After the compound is reduced with potassium borohydrid(KBH4),the resultant mercury vapor was injected into the instrument and iodine was,therefore,indirectly determined.Experimental parameters such as the conditions of extraction reagents,aqueous phase acidity,elemental mercury diffusion temperature in a vial and other factors were investigated and optimized.Under the optimum experimental conditions,this method shows a detection limit of 0.038 μg/L iodine and a linear relationship between 0.04-20 μg/L.The method was applied to determining the iodine content in marine duck eggs,kelps,laver and Ganoderma lucidum spirulina,showing a relative standard deviation(RSD) of 2.15% and the recoveries in the range of 98.1%-102.5%.

  8. Use of atomic absorption spectrometry in assessment of biomonitor plants for lead, cadmium and copper pollution.

    Science.gov (United States)

    Gokce, Kaya; Mehmet, Yaman

    2012-01-01

    Eleven plant species were collected from the vicinity of lead-battery plant in the city of Gaziantep, Turkey. Lead, cadmium and copper concentrations in the soil and leaves of plants were determined by atomic absorption spectrometry. Lead, Cd and Cu concentrations in the soil samples taken from battery area were found to be in the ranges of 304-602, 0.4-0.44 and 31-37 mg x kg(-1), respectively. Significantly increased lead concentration up to 2 750 mg x kg(-1) was found in the leaves of Eleagnus angustifolia L. plant. The lead concentrations in the other plant leaves taken from 50 m around battery factory followed the order Ailanthus altissima > Morus sp. > Juglans regia L. > Ficus carica L. > Cydonia oblonga Miller > Prunus x domestica L. The plants, Populus nigra L. , Eleagnus angustifolia L. and Salix sp. were found useful for Cd, and the plant, Eleagnus angusti folia L. for Pb, to be considered as potential biomonitor. Especially, leaves of trees and plants taken from the distance of 50 m from battery plant have relatively higher Pb concentrations. Therefore, people who and animals which live in this area and benefit from these soil and plants have vital risks.

  9. Determination of eight trace elements in doped crystal ALN by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. In this paper, an accurate and simple method has been developed for the determination of trace Cr, Co, Cu, Fe, Mg, Mn ,Ni and Zn in doped AlN crystal using inductively coupled plasma atomic emission spectrometry (ICP-AES). AlN crystal becomes ideal substrate for the epitaxial growth of GaN, AlGaN with high Al ingredient and AlN which are used to fabricate ultraviolet LEDs, blue- ultraviolet solid state LDs, lasers, ultraviolet detectors. At present, It is a very important aspect for scientific workers to promote in the transition metals elements doped AlN showing ferromagne. Owing its low detection limits and multi-element capability, ICP-AES has been used in many fields.The optimum instrument working conditions are selected .AlN crystal was fused with KOH and the fusion product was dissolved in dilute aqua regia. Matrix effect from KOH and interference to the spectral lines of the elements to be determined were investigated and corrected by matrix matching and background correction method. Detection limits of elements were 0.01% to 0.0002% The recoveries for elements were 98% to 104%. The relative standard deviation was 0.5% to 4.0%.

  10. Direct solid soil analysis by laser ablation inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Determination of heavy metals in soils by inductively coupled plasma atomic emission spectrometry (ICP-AES) usually involves the time-consuming step of preparing a solution of the solid that is then nebulized into the plasma. According to regulations, digestion by aqua regia(hydrochloric acid + nitric acid, 3 + 1) should be carried out although it is known that this method is incomplete for silicate soils. The problem can be eliminated by introducing the solid directly into the plasma using the laser ablation technique for sampling. Results are described for a study of laser ablation using a Q-switched Nd: YAG laser coupled with a new échelle spectrometer which has a multichannel solid-state detector. The laser pulses were focused onto the solid surface of pressed soil samples to generate an aerosol which is entrained in a flowing Ar stream, transported through a tube and then introduced directly into the inductively coupled plasma. Some characteristics of the preparation technique, the selection of an internal standard and homogeneity tests of the elemental distribution are reported along with a comparison and evaluation of three methods of calibration. The criteria used to measure the performance of laser ablation ICP-AES are the relative standard deviations obtained of 4.9–12.7% and the accuracy, 0.3–12.4% for Fe, Mn, Cu, Pb, Cr, Zn and Ni

  11. Analytical Approaches Based on Gas Chromatography Mass Spectrometry (GC/MS) to Study Organic Materials in Artworks and Archaeological Objects.

    Science.gov (United States)

    Bonaduce, Ilaria; Ribechini, Erika; Modugno, Francesca; Colombini, Maria Perla

    2016-02-01

    Gas chromatography/mass spectrometry (GC/MS), after appropriate wet chemical sample pre-treatments or pyrolysis, is one of the most commonly adopted analytical techniques in the study of organic materials from cultural heritage objects. Organic materials in archaeological contexts, in classical art objects, or in modern and contemporary works of art may be the same or belong to the same classes, but can also vary considerably, often presenting different ageing pathways and chemical environments. This paper provides an overview of the literature published in the last 10 years on the research based on the use of GC/MS for the analysis of organic materials in artworks and archaeological objects. The latest progresses in advancing analytical approaches, characterising materials and understanding their degradation, and developing methods for monitoring their stability are discussed. Case studies from the literature are presented to examine how the choice of the working conditions and the analytical approaches is driven by the analytical and technical question to be answered, as well as the nature of the object from which the samples are collected. PMID:27572989

  12. Analytical Approaches Based on Gas Chromatography Mass Spectrometry (GC/MS) to Study Organic Materials in Artworks and Archaeological Objects.

    Science.gov (United States)

    Bonaduce, Ilaria; Ribechini, Erika; Modugno, Francesca; Colombini, Maria Perla

    2016-02-01

    Gas chromatography/mass spectrometry (GC/MS), after appropriate wet chemical sample pre-treatments or pyrolysis, is one of the most commonly adopted analytical techniques in the study of organic materials from cultural heritage objects. Organic materials in archaeological contexts, in classical art objects, or in modern and contemporary works of art may be the same or belong to the same classes, but can also vary considerably, often presenting different ageing pathways and chemical environments. This paper provides an overview of the literature published in the last 10 years on the research based on the use of GC/MS for the analysis of organic materials in artworks and archaeological objects. The latest progresses in advancing analytical approaches, characterising materials and understanding their degradation, and developing methods for monitoring their stability are discussed. Case studies from the literature are presented to examine how the choice of the working conditions and the analytical approaches is driven by the analytical and technical question to be answered, as well as the nature of the object from which the samples are collected.

  13. Synthesis, characterization and application of a new chelating resin for solid phase extraction, preconcentration and determination of trace metals in some dairy samples by flame atomic absorption spectrometry.

    Science.gov (United States)

    Daşbaşı, Teslima; Saçmacı, Şerife; Çankaya, Nevin; Soykan, Cengiz

    2016-11-15

    In this study, a simple and rapid solid phase extraction/preconcentration procedure was developed for determination of Cd(II), Co(II), Cr(III), Cu(II), Fe(III), Mn(II), Pb(II), and Zn(II) trace metals by flame atomic absorption spectrometry (FAAS). A new chelating resin, poly(N-cyclohexylacrylamide-co-divinylbenzene-co-2-acrylamido-2-methyl-1-propanesulfonic acid) (NCA-co-DVB-co-AMPS) (hereafter CDAP) was synthesized and characterized. The influences of the analytical parameters such as pH of the sample solution, type and concentration of eluent, flow rates of the sample and eluent, volume of the sample and eluent, amount of chelating resin, and interference of ions were examined. The limit of detection (LOD) of analytes were found (3s) to be in the range of 0.65-1.90μgL(-1). Preconcentration factor (PF) of 200 and the relative standard deviation (RSD) of ⩽2% were achieved (n=11). The developed method was applied for determination of analytes in some dairy samples and certified reference materials. PMID:27283608

  14. Validation, using a chemometric approach, of gas chromatography-inductively coupled plasma-atomic emission spectrometry (GC-ICP-AES) for organotin determination

    Energy Technology Data Exchange (ETDEWEB)

    Aguerre, Sandrine; Pecheyran, Christophe; Lespes, Gaetane [Laboratoire de Chimie Analytique Bio-Inorganique et Environnement (L.C.A.B.I.E.), UMR 5034 CNRS Universite de Pau et des Pays de l' Adour, Avenue de l' Universite, 64012, Pau Cedex (France)

    2003-05-01

    The coupling between gas chromatography (GC) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) has been optimised using experimental designs. Four factors were considered in order to assist the crucial part of the coupling which is the analytes passing through the transfer line. The methodological approach based on the planning of fractional designs is described and justified according to an optimal experimentation. Then, the GC-ICP-AES-based method has been validated by means of statistical tests performed on calibration curves and evaluation of accuracy, precision and limits of detection (LOD), according to ISO standards and IUPAC recommendations. The absolute LOD are found to be quite similar to those obtained using flame photometer. Relative LOD ranged between 20 and 80 ng (Sn) L{sup -1} after liquid-liquid extraction of the analytes. When solid phase micro-extraction (SPME) is used, LOD are sub 10 ng (Sn) L{sup -1}. The repeatability is 3-10%, according to the extraction used. Analyses of reference sediment, fresh and waste waters confirm the suitability and capabilities of GC-ICP-AES for organotin determination in the environment. The statistical approach has been demonstrated to be a powerful methodological tool, enhancing the experimental part by providing reliable analytical results. (orig.)

  15. Automatic microemulsion preparation for metals determination in fuel samples using a flow-batch analyzer and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Cunha, Francisco Antônio S; Sousa, Rafael A; Harding, David P; Cadore, Solange; Almeida, Luciano F; Araújo, Mário César U

    2012-05-21

    The principal thermodynamic advantages of using microemulsions over standard emulsions for flow metal analysis are the greatly increased analyte stability and emulsive homogeneity that improve both the ease of sample preparation, and the analytical result. In this study a piston propelled flow-batch analyzer (PFBA) for the determination of Cu, Cr and Pb in gasoline and naphtha by graphite furnace atomic absorption spectrometry (GF AAS) was explored. Investigative phase modeling for low dilution was conducted both for gasoline and naphtha microemulsions. Rheological considerations were also explored including a mathematical flow derivation to fine tune the system's operational parameters, and the GF AAS coupling. Both manual and automated procedures for microemulsion preparation were compared. The results of the paired t test at a 95% confidence level showed no significant differences between them. Further recovery test results confirmed a negligible matrix effect of the sample on the analyte absorption signals and an efficient stabilization of the samples (with metals) submitted to microemulsion treatment. The accuracy of the developed procedure was attested by good recovery percentages in the ranges of 100.0±3.5% for Pb in the naphtha samples, and 100.2±3.4% and 100.7±4.6% for Cu and Cr, respectively in gasoline samples. PMID:22541820

  16. Sapphire: a better material for atomization and in situ collection of silver volatile species for atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Musil, Stanislav, E-mail: stanomusil@biomed.cas.cz; Matoušek, Tomáš; Dědina, Jiří

    2015-06-01

    Sapphire is presented as a high temperature and corrosion resistant material of an optical tube of an atomizer for volatile species of Ag generated by the reaction with NaBH{sub 4}. The modular atomizer design was employed which allowed to carry out the measurements in two modes: (i) on-line atomization and (ii) in situ collection (directly in the optical tube) by means of excess of O{sub 2} over H{sub 2} in the carrier gas during the trapping step and vice versa in the volatilization step. In comparison with quartz atomizers, the sapphire tube atomizer provides a significantly increased atomizer lifetime as well as substantially improved repeatability of the Ag in situ collection signals shapes. In situ collection of Ag in the sapphire tube atomizer was highly efficient (> 90%). Limit of detection in the on-line atomization mode and in situ collection mode, respectively, was 1.2 ng ml{sup −1} and 0.15 ng ml{sup −1}. - Highlights: • Sapphire was tested as a new material of an atomizer tube for Ag volatile species. • Two measurement modes were investigated: on-line atomization and in situ collection. • In situ collection of Ag was highly efficient (> 90%) with LOD of 0.15 ng ml{sup −1}. • No devitrification of the sapphire tube observed in the course of several months.

  17. Chemometric evaluation of Cd, Co, Cr, Cu, Ni (inductively coupled plasma optical emission spectrometry) and Pb (graphite furnace atomic absorption spectrometry) concentrations in lipstick samples intended to be used by adults and children.

    Science.gov (United States)

    Batista, Érica Ferreira; Augusto, Amanda dos Santos; Pereira-Filho, Edenir Rodrigues

    2016-04-01

    A method was developed for determining the concentrations of Cd, Co, Cr, Cu, Ni and Pb in lipstick samples intended to be used by adults and children using inductively coupled plasma optical emission spectrometry (ICP OES) and graphite furnace atomic absorption spectrometry (GF AAS) after treatment with dilute HNO3 and hot block. The combination of fractional factorial design and Desirability function was used to evaluate the ICP OES operational parameters and the regression models using Central Composite and Doehlert designs were calculated to stablish the best working condition for all analytes. Seventeen lipstick samples manufactured in different countries with different colors and brands were analyzed. Some samples contained high concentrations of toxic elements, such as Cr and Pb, which are carcinogenic and cause allergic and eczematous dermatitis. The maximum concentration detected was higher than the permissible safe limits for human use, and the samples containing these high metal concentrations were intended for use by children. Principal component analysis (PCA) was used as a chemometrics tool for exploratory analysis to observe the similarities between samples relative to the metal concentrations (a correlation between Cd and Pb was observed). PMID:26838401

  18. Studies of ion-imprinted polymers for solid-phase extraction of ruthenium from environmental samples before its determination by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zambrzycka, Elzbieta; Roszko, Dorota; Lesniewska, Barbara; Wilczewska, Agnieszka Z.; Godlewska-Zylkiewicz, Beata, E-mail: bgodlew@uwb.edu.pl

    2011-07-15

    The examination of the effect of interfering ions on the analytical signal of ruthenium measured by electrothermal atomic absorption spectrometry was initially performed in this work. The complexes of ruthenium(III) with thiosemicarbazide (TSd) and acetaldehyde thiosemicarbazone (AcTSn) were prepared and imprinted in polymeric network. The ion-imprinted polymers were synthesized by copolymerization of methacrylic acid, as functional monomer and ethylene glycol dimethacrylate, as crosslinking agent in the presence of 2,2-azobisisobutyronitrile as initiator. The effects of sample volume, pH, and flow rate on the extraction of analyte were studied in dynamic mode. The optimum pH for quantitative retention of ruthenium on each of the studied sorbents was 7.5 {+-} 0.5. The elution of analyte was completed with 0.2 mol L{sup -1} thiourea in 0.2 mol L{sup -1} HCl. The effect of matrix ions on ruthenium(III) separation process was studied. The analytical performance of the Ru-TSd polymer in the presence of competing ions was better than Ru-AcTSn polymer, considering recovery of analyte, reproducibility of results, selectivity coefficients, and sorbent capacity. The detection limit of the proposed method (0.16 ng mL{sup -1} on Ru-TSd and 0.25 ng mL{sup -1} on Ru-AcTSn) is lower in comparison with the previously published methods. The developed separation method was successfully applied to the determination of trace amounts of ruthenium in spiked water samples, sludge, grass, and human hair.

  19. Studies of ion-imprinted polymers for solid-phase extraction of ruthenium from environmental samples before its determination by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Zambrzycka, Elżbieta; Roszko, Dorota; Leśniewska, Barbara; Wilczewska, Agnieszka Z.; Godlewska-Żyłkiewicz, Beata

    2011-07-01

    The examination of the effect of interfering ions on the analytical signal of ruthenium measured by electrothermal atomic absorption spectrometry was initially performed in this work. The complexes of ruthenium(III) with thiosemicarbazide (TSd) and acetaldehyde thiosemicarbazone (AcTSn) were prepared and imprinted in polymeric network. The ion-imprinted polymers were synthesized by copolymerization of methacrylic acid, as functional monomer and ethylene glycol dimethacrylate, as crosslinking agent in the presence of 2,2-azobisisobutyronitrile as initiator. The effects of sample volume, pH, and flow rate on the extraction of analyte were studied in dynamic mode. The optimum pH for quantitative retention of ruthenium on each of the studied sorbents was 7.5 ± 0.5. The elution of analyte was completed with 0.2 mol L -1 thiourea in 0.2 mol L -1 HCl. The effect of matrix ions on ruthenium(III) separation process was studied. The analytical performance of the Ru-TSd polymer in the presence of competing ions was better than Ru-AcTSn polymer, considering recovery of analyte, reproducibility of results, selectivity coefficients, and sorbent capacity. The detection limit of the proposed method (0.16 ng mL -1 on Ru-TSd and 0.25 ng mL -1 on Ru-AcTSn) is lower in comparison with the previously published methods. The developed separation method was successfully applied to the determination of trace amounts of ruthenium in spiked water samples, sludge, grass, and human hair.

  20. Elemental analysis using instrumental neutron activation analysis and inductively coupled plasma atomic emission spectrometry: a comparative study

    Energy Technology Data Exchange (ETDEWEB)

    Chung, Yong Sam; Choi, Kwang Soon; Moon, Jong Hwa; Kim, Sun Ha; Lim, Jong Myoung; Kim, Young Jin [KAERI, Taejon (Korea, Republic of); Quraishi, Shamshad Begum [Bangladesh Atomic Energy Commission, Dhaka (Bangladesh)

    2003-05-01

    Elemental analyses for certified reference materials were carried out using instrumental neutron activation analysis and inductively coupled plasma-atomic emission spectrometry. Five Certified Reference Materials (CRM) were selected for the study on comparative analysis of environmental samples. The CRM are Soil (NIST SRM 2709), Coal fly ash (NIST SRM 1633a), urban dust (NIST SRM 1649a) and air particulate on filter media (NIST SRM 2783 and human hair (GBW 09101)

  1. Elemental analysis using instrumental neutron activation analysis and inductively coupled plasma atomic emission spectrometry: a comparative study

    International Nuclear Information System (INIS)

    Elemental analyses for certified reference materials were carried out using instrumental neutron activation analysis and inductively coupled plasma-atomic emission spectrometry. Five Certified Reference Materials (CRM) were selected for the study on comparative analysis of environmental samples. The CRM are Soil (NIST SRM 2709), Coal fly ash (NIST SRM 1633a), urban dust (NIST SRM 1649a) and air particulate on filter media (NIST SRM 2783 and human hair (GBW 09101)

  2. Determination of Copper-Based Fungicides by Flame Atomic Absorption Spectrometry Using Digestion Procedure with Sulfuric and Nitric Acid

    OpenAIRE

    Jelena Milinović; Rada Đurović

    2007-01-01

    Copper-based fungicides can be effectively digested by treatment with a mixture of concentrated sulfuric and nitric acid in exactly 15 minutes for the rapid determination via copper using flame atomic absorption spectrometry (AAS). Under optimum conditions, the results of copper fungicide analysis were consistent to those obtained by the AOAC’s recommended method. Recovery values ranged from 98.63 to 103.40%. Relative standard deviation values are lower than 2%. The proposed digestion procedu...

  3. Determination of Trace Silver in Water Samples by Online Column Preconcentration Flame Atomic Absorption Spectrometry Using Termite Digestion Product

    OpenAIRE

    Joyce Nunes Bianchin; Eduardo Carasek; Edmar Martendal

    2011-01-01

    A new method for Ag determination in water samples using solid phase extraction (SPE) coupled to a flow injection system and flame atomic absorption spectrometry was developed. The sorbent used for Ag preconcentration and extraction was the termite digestion product. Flow and chemical variables of the system were optimized through a multivariate procedure. The factors selected were adsorbent mass, buffer type and concentration, sample pH, and sample flow rate. The detection limit and precisio...

  4. Analytical procedure for characterization of medieval wall-paintings by X-ray fluorescence spectrometry, laser ablation inductively coupled plasma mass spectrometry and Raman spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Syta, Olga; Rozum, Karol; Choińska, Marta [Faculty of Chemistry, University of Warsaw, Pasteura 1, 02-093 Warsaw (Poland); Zielińska, Dobrochna [Institute of Archaeology, University of Warsaw, Krakowskie Przedmieście 26/28, 00-927 Warsaw (Poland); Żukowska, Grażyna Zofia [Chemical Faculty, Warsaw University of Technology, Noakowskiego 3, 00-664 Warsaw (Poland); Kijowska, Agnieszka [National Museum in Warsaw, Aleje Jerozolimskie 3, 00-495 Warsaw (Poland); Wagner, Barbara, E-mail: barbog@chem.uw.edu.pl [Faculty of Chemistry, University of Warsaw, Pasteura 1, 02-093 Warsaw (Poland)

    2014-11-01

    Analytical procedure for the comprehensive chemical characterization of samples from medieval Nubian wall-paintings by means of portable X-ray fluorescence (pXRF), laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) and Raman spectroscopy (RS) was proposed in this work. The procedure was used for elemental and molecular investigations of samples from archeological excavations in Nubia (modern southern Egypt and northern Sudan). Numerous remains of churches with painted decorations dated back to the 7th–14th century were excavated in the region of medieval kingdoms of Nubia but many aspects of this art and its technology are still unknown. Samples from the selected archeological sites (Faras, Old Dongola and Banganarti) were analyzed in the form of transfers (n = 26), small fragments collected during the excavations (n = 35) and cross sections (n = 15). XRF was used to collect data about elemental composition, LA-ICPMS allowed mapping of selected elements, while RS was used to get the molecular information about the samples. The preliminary results indicated the usefulness of the proposed analytical procedure for distinguishing the substances, from both the surface and sub-surface domains of the wall-paintings. The possibility to identify raw materials from the wall-paintings will be used in the further systematic, archeometric studies devoted to the detailed comparison of various historic Nubian centers. - Highlights: • The analytical procedure for examination of unique wall paintings was proposed. • Identification of pigments and supporting layers of wall-paintings was obtained. • Heterogeneous samples were mapped with the use of LA-ICPMS. • Anatase in the sub-surface regions of samples was detected by Raman spectroscopy.

  5. Analytical procedure for characterization of medieval wall-paintings by X-ray fluorescence spectrometry, laser ablation inductively coupled plasma mass spectrometry and Raman spectroscopy

    International Nuclear Information System (INIS)

    Analytical procedure for the comprehensive chemical characterization of samples from medieval Nubian wall-paintings by means of portable X-ray fluorescence (pXRF), laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) and Raman spectroscopy (RS) was proposed in this work. The procedure was used for elemental and molecular investigations of samples from archeological excavations in Nubia (modern southern Egypt and northern Sudan). Numerous remains of churches with painted decorations dated back to the 7th–14th century were excavated in the region of medieval kingdoms of Nubia but many aspects of this art and its technology are still unknown. Samples from the selected archeological sites (Faras, Old Dongola and Banganarti) were analyzed in the form of transfers (n = 26), small fragments collected during the excavations (n = 35) and cross sections (n = 15). XRF was used to collect data about elemental composition, LA-ICPMS allowed mapping of selected elements, while RS was used to get the molecular information about the samples. The preliminary results indicated the usefulness of the proposed analytical procedure for distinguishing the substances, from both the surface and sub-surface domains of the wall-paintings. The possibility to identify raw materials from the wall-paintings will be used in the further systematic, archeometric studies devoted to the detailed comparison of various historic Nubian centers. - Highlights: • The analytical procedure for examination of unique wall paintings was proposed. • Identification of pigments and supporting layers of wall-paintings was obtained. • Heterogeneous samples were mapped with the use of LA-ICPMS. • Anatase in the sub-surface regions of samples was detected by Raman spectroscopy

  6. Effect of Atomic Coherence on Absorption in Four-level Systems: an Analytical study

    CERN Document Server

    Sandhya, S N

    2006-01-01

    Absorption profile of a four-level ladder atomic system interacting with three driving fields is studied perturbatively and analytical results are presented. Numerical results where the driving field strengths are treated upto all orders are presented. The absorption features is studied in two regimes, i) the weak middle transition coupling, i.e. $\\Omega_2 \\Omega_{1,3}$ and ii) the strong middle transition coupling $\\Omega_2 \\Omega_{1,3}$. In case i), it is shown that the ground state absorption and the saturation characteristics of the population of level 2 reveal deviation due to the presence of upper level couplings. In particular, the saturation curve for the population of level 2 shows a dip for $\\Omega_1 = \\Omega_3$. While the populations of levels 3 and 4 show a maxima when this resonance condition is satisfied. Thus the resonance condition provides a criterion for maximally populating the upper levels. A second order perturbation calculation reveals the nature of this minima (maxima). In the second ca...

  7. Determination of Inorganic Arsenic Species by Electrochemical Hydride Generation Atomic Absorption Spectrometry with Selective Electrochemical Reduction

    Institute of Scientific and Technical Information of China (English)

    LI Xun; WANG Zheng-Hao

    2007-01-01

    A new direct procedure for the determination of inorganic arsenic species was developed by electrochemical hydride generation atomic absorption spectrometry (EcHG-AAS) with selective electrochemical reduction. The determination of inorganic arsenic species is based on the fact that As(Ⅲ) shows significantly higher absorbance at low electrolytic currents than As(Ⅴ) in 0.3 mol·L-1 H2SO4.The electrolytic current used for the determination of As(Ⅲ) without considerable interferences of As(V) was 0.4 A, whereas the current for the determination of As(Ⅲ)and As(V) was 1.2 A. For equal concentrations of As(Ⅲ) and As(V) in a sample, the interferences of As(V) during the As(Ⅲ) determination were smaller than 5%. The absorbance for As(V) could be calculated by subtracting that for As(Ⅲ) measured at 0.4 A from the total absorbance for As(Ⅲ) and As(V) measured at 1.2 A, and then the concentration of As(V) can be obtained by its calibration curve at 1.2 A. The methodology developed provided the detection limits of 0.3 and 0.6 ng·ml-1 for As(Ⅲ) and As(V) respectively.The relative standrad deviations were of 3.5% for 20 ng·ml-1 As(Ⅲ) and 302% for 20 ng·ml-1 As(V).The method was successfully applied to determination of soluble inorganic arsenic species in Chinese medicine.

  8. Gunshot residue testing in suicides: Part II: Analysis by inductive coupled plasma-atomic emission spectrometry.

    Science.gov (United States)

    Molina, D Kimberley; Castorena, Joe L; Martinez, Michael; Garcia, James; DiMaio, Vincent J M

    2007-09-01

    Several different methods can be employed to test for gunshot residue (GSR) on a decedent's hands, including scanning electron microscopy with energy dispersive x-ray (SEM/EDX) and inductive coupled plasma-atomic emission spectrometry (ICP-AES). In part I of this 2-part series, GSR results performed by SEM/EDX in undisputed cases of suicidal handgun wounds were studied. In part II, the same population was studied, deceased persons with undisputed suicidal handgun wounds, but GSR testing was performed using ICP-AES. A total of 102 cases were studied and analyzed for caliber of weapon, proximity of wound, and the results of the GSR testing. This study found that 50% of cases where the deceased was known to have fired a handgun immediately prior to death had positive GSR results by ICP/AES, which did not differ from the results of GSR testing by SEM/EDX. Since only 50% of cases where the person is known to have fired a weapon were positive for GSR by either method, this test should not be relied upon to determine whether someone has discharged a firearm and is not useful as a determining factor of whether or not a wound is self-inflicted or non-self-inflicted. While a positive GSR result may be of use, a negative result is not helpful in the medical examiner setting as a negative result indicates that either a person fired a weapon prior to death or a person did not fire a weapon prior to death. PMID:17721164

  9. Determination of Lead in Human Teeth by Hydride Generation Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    Hassan T. Abdulsahib

    2011-01-01

    Full Text Available Problem statement: The determination of lead in human teeth at concentration levels of ìg/ml is proposed using Hydride Generation Atomic Absorption Spectrometry (HG-AAS. To do this, 2% (wv lanthanum chloride solution is employed as matrix modifying reagent to increase sensitivity and remove matrix interferences. Approach: About 100 µL of sample and 100 µL of 3.0% (m/v NaBH4 are simultaneously injected into carrier streams. The detection of limit of 0.46 µg L-1 for Pb was achieved and the relative standard deviation of 3.0% for 10 µg L-1 lead was obtained. The recovery percentage of the method has been found to be (92.8-100.5% for known quantities of lead added to teeth sample which were completely recovered. A comparison of the proposed method with standard addition method showed nearly results in the same samples of teeth and the results compared with other studies in the world. Results: The method was shown to be satisfactory for determination of traces of lead in teeth samples with excellent accuracy. Teeth analysis reveals that intact teeth contained the highest amounts of lead which provide an evidence that lead may reduce the prevalence of dantal caries. Statistically significant differences (pConclusion: Statistically significant difference between age groups were seen in the mean value of lead concentrations in human teeth, the concentration of lead increased with age. The differences may be due to the exposure of lead and others factors such as differences in diet and drinking water.

  10. Investigation of aging processes of graphite tubes modified with iridium and rhodium used for atomic spectrometry

    Science.gov (United States)

    Bulska, Ewa; Piaścik, Marek; Katskov, Dmitri; Darangwa, Nicholas; Grotti, Marco

    2007-11-01

    UV spectrometry (187-380 nm) with charge coupled device (CCD) detection was used to study the evolution of absorption spectra during the vaporization of various species in the pyrocoated graphite furnace, with electrodeposited Ir and Rh as modifiers. In order to mimic a typical matrix composition, various salts of aluminum, manganese, copper, magnesium, sodium, and lead were used in microgram amounts. Changes in spectra and vapor release rate, along with aging of the tubes in the repetitive temperature cycles, were observed. Compared to the unmodified pyrocoated tubes, the presence of Ir or Rh causes a significant reduction in the vaporization efficiency, especially for microgram amounts of copper and aluminum introduced as nitrates, and manganese introduced as a sulfate. The vaporization efficiency, for magnesium and sodium as chlorides, and for lead as a sulfate, remained unchanged. Interestingly, the aging of the tubes was accompanied by partial restoration of the spectral characteristics for unmodified tubes. For example, with unmodified pyrocoated tubes, the vaporization spectrum, appearing as a consequence of the decomposition of aluminum nitrate, consisted of Al2O bands overlapped by Al atomic lines. In the freshly modified tubes, intensities of those lines and bands were substantially reduced, and in this case, the dominance of AlO molecules was observed. The efficiency of vaporization of aluminum species increased in the aged modified tubes. The scanning electron microscopy (SEM) images of the modified surfaces for the new and aged tubes indicated that aging of the tubes is accompanied by the destruction of the pyrocoating, formation of pyrographite shells around the areas where the modifier was electrodeposited, and finally, complete substitution of the metal on the graphite surface by pyrographite debris.

  11. On-line characterization of gaseous and particulate organic analytes using atmospheric pressure chemical ionization mass spectrometry

    International Nuclear Information System (INIS)

    A modified atmospheric pressure chemical ionization ion source is applied for direct analysis of volatile or low volatile organic compounds in air. The method is based on the direct introduction of the analytes in the gas phase and/or particle phase into the ion source of a commercial ion-trap mass spectrometer. Two methods are employed for the production of primary ions at atmospheric pressure, photoionization and corona discharge. It is shown that in the presence of a dopant, photoionization can be a highly efficient ionization method also for real-time analysis with detection limits for selected analytes in the lower ppt-range. Using corona discharge for the production of primary ions, which is instrumentally easier since no additional chemicals have to be added to the sample flow, we demonstrate the analytical potential of on-line atmospheric pressure chemical ionization mass spectrometry for reaction monitoring experiments. To do so, an atmospherically relevant gas phase reaction is carried out in a 500 l reaction chamber and gaseous and particulate compounds are monitored in the positive and negative ion mode of the mass spectrometer

  12. Determination of natural isotopic variation in antimony using inductively coupled plasma mass spectrometry for an uncertainty estimation of the standard atomic weight of antimony

    International Nuclear Information System (INIS)

    The isotopic variation of industrially produced antimony was estimated using multiple-collector inductively coupled plasma mass spectrometry. A reproducible 123Sb/121Sb ratio of ±0.004% (2 standard deviations) was routinely obtained using a Sn doping mass discrimination correction technique. Only a small isotopic variation of about 0.05% was observed among industrially important Sb materials (five commercially available reagents and two ore minerals). The degree of Sb isotopic variation to determine the uncertainty in Sb atomic weight can be reduced by this new analytical technique to 0.00025 compared to the currently accepted IUPAC isotopic variation determined by conventional mass spectrometry of ±0.001. Heavy isotope enrichment of Sb in a drainage water sample from a stibnite mining area was found. This heavy isotope enrichment tendency in an aqueous environment may be useful in detecting anthropogenic Sb input from industrial emission by the smelting process via air because Sb of anthropogenic origin will have lighter isotope enrichment features. (author)

  13. The use of nanomaterials for mass spectrometry can be uplifting for analyte detection

    Science.gov (United States)

    Li, J.; Lipson, R. H.

    2014-03-01

    Surface-Assisted Laser Desorption Ionization (SALDI) involves desorbing and ionizing analyte molecules from a nanoporous substrate by laser irradiation for detection in a mass spectrometer. In this work experiments were designed to better understand the mechanisms governing desorption and ionization for Desorption Ionization On Silicon (DIOS), a variant of SALDI which uses porous silicon (pSi) as a substrate. Experiments are also reported for other nanoporous semiconducting materials (WO3, TiO2) which exhibit very similar behaviors; specifically, that both protonated analyte ions and analyte radical cations can be generated with relative intensities that depend on the position of the incident laser focus relative to substrate surface. While thermal desorption appears to be important, preliminary evidence suggests that the ionization mechanism leading to protonated analytes involves in part electrons and holes formed when photoexciting the substrate above its electronic band gap, and the presence of defect states within the band gap. Radical cation formation appears to be driven in part by electron transfer due to the large electron affinity of each substrate used in this work.

  14. The use of nanomaterials for mass spectrometry can be uplifting for analyte detection

    Energy Technology Data Exchange (ETDEWEB)

    Li, J.; Lipson, R. H. [University of Victoria Department of Chemistry, P.O. Box 3065, STN CSC Victoria, BC V8W 3V6 (Canada)

    2014-03-31

    Surface-Assisted Laser Desorption Ionization (SALDI) involves desorbing and ionizing analyte molecules from a nanoporous substrate by laser irradiation for detection in a mass spectrometer. In this work experiments were designed to better understand the mechanisms governing desorption and ionization for Desorption Ionization On Silicon (DIOS), a variant of SALDI which uses porous silicon (pSi) as a substrate. Experiments are also reported for other nanoporous semiconducting materials (WO{sub 3}, TiO{sub 2}) which exhibit very similar behaviors; specifically, that both protonated analyte ions and analyte radical cations can be generated with relative intensities that depend on the position of the incident laser focus relative to substrate surface. While thermal desorption appears to be important, preliminary evidence suggests that the ionization mechanism leading to protonated analytes involves in part electrons and holes formed when photoexciting the substrate above its electronic band gap, and the presence of defect states within the band gap. Radical cation formation appears to be driven in part by electron transfer due to the large electron affinity of each substrate used in this work.

  15. Application of analytical pyrolysis-mass spectrometry in characterization of animal manures

    Science.gov (United States)

    Different analytical pyrolysis techniques have been used in characterizing natural organic matter and synthesized organic polymers. Most common ones are pyrolysis followed by direct detection using MS such as in Py-FIMS technique or pyrolysis followed by GC separation of pyrosates then detected by M...

  16. Advanced analytical techniques for the extraction and characterization of plant-derived essential oils by gas chromatography with mass spectrometry.

    Science.gov (United States)

    Waseem, Rabia; Low, Kah Hin

    2015-02-01

    In recent years, essential oils have received a growing interest because of the positive health effects of their novel characteristics such as antibacterial, antifungal, and antioxidant activities. For the extraction of plant-derived essential oils, there is the need of advanced analytical techniques and innovative methodologies. An exhaustive study of hydrodistillation, supercritical fluid extraction, ultrasound- and microwave-assisted extraction, solid-phase microextraction, pressurized liquid extraction, pressurized hot water extraction, liquid-liquid extraction, liquid-phase microextraction, matrix solid-phase dispersion, and gas chromatography (one- and two-dimensional) hyphenated with mass spectrometry for the extraction through various plant species and analysis of essential oils has been provided in this review. Essential oils are composed of mainly terpenes and terpenoids with low-molecular-weight aromatic and aliphatic constituents that are particularly important for public health.

  17. An analytical method for determination of mercury by cold vapor atomic absorption spectroscopy; Determinazione di mercurio. Metodo per spettrometria di assorbimento atomico a vapori freddi (CV-AAS)

    Energy Technology Data Exchange (ETDEWEB)

    Campanella, L. [Rome Univ. La Sapienza, Rome (Italy); Mastroianni, D.; Capri, S.; Pettine, M. [CNR, Rome (Italy). Ist. di Ricerca sulle Acque; Spezia, S.; Bettinelli, M. [ENEL, Unified Modelling Language, Piacenza (Italy)

    1999-09-01

    An analytical procedure for the determination of total mercury in wastewaters and natural waters is described. Aqueous samples are fast digested with nitric acid by using the microwave-oven technique; the analysis of mercury is then performed by cold vapor atomic absorption spectrometry (CV-AAS) using two possible instrumental apparatus (batch system or flow injection). Sodium borohydride is used as the reducing agent for mercury in solution (Method A). The use of amalgamation traps on gold for the preconcentration of mercury lowers the detection limit of the analyte (Method B). [Italian] Viene descritta una procedura analitica per la determinazione del mercurio totale in acque di scarico e naturali. Il campione acquoso viene sottoposto a mineralizzazione con acido nitrico in forno a microonde e analizzato mediante spettroscopia di assorbimento atomico a vapori freddi (CV-AAS) in due possibili configurazioni strumentali (sistema batch oppure flow injection), utilizzando sodio boro idruro come agente riducente del mercurio (metodo A). L'impiego della trappola di oro per la preconcentrazione del mercurio mediante amalgama consente di determinare l'analita a livelli di pochi ng/L (metodo B).

  18. Investigation of spectral interferences in the determination of lead in fertilizers and limestone samples using high-resolution continuum source graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Borges, Aline R. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Becker, Emilene M.; François, Luciane L.; Jesus, Alexandre de [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Dessuy, Morgana B., E-mail: mbdessuy@ufrgs.br [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil)

    2014-11-01

    In the present work, spectral interferences on the determination of lead in fertilizer and limestone samples were investigated using high-resolution continuum source graphite furnace atomic absorption spectrometry at the main analytical lines: 217.001 and 283.306 nm. For these investigations, samples were introduced into the furnace as slurry together with a mixture of Pd and Mg as chemical modifier. Spectral interferences were observed for some samples at both analytical lines. In order to verify whether a wet digestion procedure would avoid these interferences, a reference method for wet digestion of fertilizers was employed as an alternative sample preparation procedure. However, the same interferences were also observed in the digested samples. In order to identify and eliminate the fine-structured background using a least-squares background correction, reference spectra were generated using the combination of different species. The use of the latter technique allowed the elimination of spectral interferences for most of the investigated samples, making possible the determination of lead in fertilizer and limestone samples free of interferences. The best results were found using a reference spectrum of NH{sub 4}H{sub 2}PO{sub 4} at 217.001 nm, and a mixture of H{sub 2}SO{sub 4} + Ca and HNO{sub 3} + Ca at the 283.306 nm line. The accuracy of the method was evaluated using a certified reference material “Trace Elements in Multi-Nutrient Fertilizer”. Similar results were obtained using line source graphite furnace atomic absorption spectrometry with Zeeman-effect background correction, indicating that the latter technique was also capable to correct the spectral interferences, at least in part. - Highlights: • Spectral interferences on the determination of lead in fertilizers and limestone. • The analytical lines at 217.001 nm and 283.306 nm using HR-CS GF AAS. • Various combinations of compounds were used to create reference spectra. • LSBC

  19. Investigation of spectral interferences in the determination of lead in fertilizers and limestone samples using high-resolution continuum source graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    In the present work, spectral interferences on the determination of lead in fertilizer and limestone samples were investigated using high-resolution continuum source graphite furnace atomic absorption spectrometry at the main analytical lines: 217.001 and 283.306 nm. For these investigations, samples were introduced into the furnace as slurry together with a mixture of Pd and Mg as chemical modifier. Spectral interferences were observed for some samples at both analytical lines. In order to verify whether a wet digestion procedure would avoid these interferences, a reference method for wet digestion of fertilizers was employed as an alternative sample preparation procedure. However, the same interferences were also observed in the digested samples. In order to identify and eliminate the fine-structured background using a least-squares background correction, reference spectra were generated using the combination of different species. The use of the latter technique allowed the elimination of spectral interferences for most of the investigated samples, making possible the determination of lead in fertilizer and limestone samples free of interferences. The best results were found using a reference spectrum of NH4H2PO4 at 217.001 nm, and a mixture of H2SO4 + Ca and HNO3 + Ca at the 283.306 nm line. The accuracy of the method was evaluated using a certified reference material “Trace Elements in Multi-Nutrient Fertilizer”. Similar results were obtained using line source graphite furnace atomic absorption spectrometry with Zeeman-effect background correction, indicating that the latter technique was also capable to correct the spectral interferences, at least in part. - Highlights: • Spectral interferences on the determination of lead in fertilizers and limestone. • The analytical lines at 217.001 nm and 283.306 nm using HR-CS GF AAS. • Various combinations of compounds were used to create reference spectra. • LSBC eliminated spectral interferences for most of

  20. Major constituent quantitative determination in uranium alloys by coupled plasma atomic emission spectrometry and X ray fluorescence wavelength dispersive spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Luis Claudio de; Silva, Adriana Mascarenhas Martins da; Gomide, Ricardo Goncalves; Silva, Ieda de Souza, E-mail: luis.claudio@ctmsp.mar.mil.br, E-mail: adriana@ctmsp.mar.mil.br, E-mail: gomide@ctmsp.mar.mil.br, E-mail: ieda@ctmsp.mar.mil.br [Centro Tecnologico da Marinha em Sao Paulo (CEA/CTMSP), Ipero, SP (Brazil). Centro Experimental Aramar

    2013-07-01

    A wavelength-dispersive X-ray fluorescence (WD-XRF) spectrometric method for determination of major constituents elements (Zr, Nb, Mo) in Uranium/Zirconium/Niobium and Uranium/Molybdenum alloy samples were developed. The methods use samples taken in the form of chips that were dissolved in hot nitric acid and precipitate particles melted with lithium tetraborate and dissolved in hot nitric acid and finally analyzed as a solution. Studies on the determination by inductively coupled plasma optic emission spectrometry (ICP OES) using matched matrix in calibration curve were developed. The same samples solution were analyzed in both methods. The limits of detection (LOD), linearity of the calibrations curves, recovery study, accuracy and precision of the both techniques were carried out. The results were compared. (author)

  1. Determination of Ultra-trace Amounts of Arsenic(III) by Flow Injection Hydride Generation Atomic Absorption Spectrometry with On-line Preconcentration by Coprecipitation with Lanthanum Hydroxide or Hafnium Hydroxide

    DEFF Research Database (Denmark)

    Nielsen, Steffen; Sloth, Jens Jørgen; Hansen, Elo Harald

    1996-01-01

    A time-based flow-injection (FI) procedure for the determination of ultra-trace amounts of inorganic arsenic(III) is described, which combines hydride generation atomic absorption spectrometry (HG-AAS) with on-line preconcentration of the analyte by inorganic coprecipitation-dissolution in a filt......A time-based flow-injection (FI) procedure for the determination of ultra-trace amounts of inorganic arsenic(III) is described, which combines hydride generation atomic absorption spectrometry (HG-AAS) with on-line preconcentration of the analyte by inorganic coprecipitation......-dissolution in a filterless knotted Microline reactor. The sample and coprecipitating agent are mixed on-line and merged with an ammonium buffer solution, which promotes a controllable and quantitative collection of the generated hydroxide on the inner walls of the knotted reactor incorporated into the FI-HG-AAS system....... Subsequently the precipitate is eluted with 1 mol/l hydrochloric acid, allowing ensuing determination of the analyte via hydride generation. The preconcentration of As(III) was tested by coprecipitation with two different inorganic coprecipitating agents namely La(III) and Hf(IV). It was shown that As...

  2. Feasibility of dispersive liquid–liquid microextraction for extraction and preconcentration of Cu and Fe in red and white wine and determination by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A method for extraction and preconcentration of Cu and Fe in red and white wines using dispersive liquid–liquid microextraction (DLLME) and determination by flame atomic absorption spectrometry (F AAS) was developed. Extraction was performed using sodium diethyldithiocarbamate as chelating agent and a mixture of 40 μL of 1,2-dichlorobenzene (extraction solvent) and 900 μL of methanol (dispersive solvent). Some parameters that influencing the extraction efficiency such as pH (2 to 5), concentration of chelating agent (0 to 2%), effect of salt addition (0 to 10%), number of washing steps (1 to 4) and centrifugation time (0 to 15 min) were studied. Accuracy was evaluated after microwave-assisted digestion in closed vessels and analytes were determined by inductively coupled plasma optical emission spectrometry. Agreement with the proposed method ranged from 91 to 110 and from 89 to 113% for Cu and Fe, respectively. Calibration of F AAS instrument was performed using analyte addition method and limits of detection were 6.3 and 2.4 μg L−1 for Cu and Fe, respectively. The proposed method was applied for the determination of Cu and Fe in five samples of red wine and three samples of white wine, with concentration ranging from 21 to 178 μg L−1 and from 1.38 to 3.74 mg L−1, respectively. - Highlights: • Determination of Cu and Fe in wine using DLLME and F AAS • High preconcentration factors and low LODs were achieved. • Alternative method for the determination of Cu and Fe in wine for routine analysis

  3. Feasibility of dispersive liquid–liquid microextraction for extraction and preconcentration of Cu and Fe in red and white wine and determination by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Seeger, Tassia S.; Rosa, Francisco C.; Bizzi, Cezar A.; Dressler, Valderi L.; Flores, Erico M.M.; Duarte, Fabio A., E-mail: fabioand@gmail.com

    2015-03-01

    A method for extraction and preconcentration of Cu and Fe in red and white wines using dispersive liquid–liquid microextraction (DLLME) and determination by flame atomic absorption spectrometry (F AAS) was developed. Extraction was performed using sodium diethyldithiocarbamate as chelating agent and a mixture of 40 μL of 1,2-dichlorobenzene (extraction solvent) and 900 μL of methanol (dispersive solvent). Some parameters that influencing the extraction efficiency such as pH (2 to 5), concentration of chelating agent (0 to 2%), effect of salt addition (0 to 10%), number of washing steps (1 to 4) and centrifugation time (0 to 15 min) were studied. Accuracy was evaluated after microwave-assisted digestion in closed vessels and analytes were determined by inductively coupled plasma optical emission spectrometry. Agreement with the proposed method ranged from 91 to 110 and from 89 to 113% for Cu and Fe, respectively. Calibration of F AAS instrument was performed using analyte addition method and limits of detection were 6.3 and 2.4 μg L{sup −1} for Cu and Fe, respectively. The proposed method was applied for the determination of Cu and Fe in five samples of red wine and three samples of white wine, with concentration ranging from 21 to 178 μg L{sup −1} and from 1.38 to 3.74 mg L{sup −1}, respectively. - Highlights: • Determination of Cu and Fe in wine using DLLME and F AAS • High preconcentration factors and low LODs were achieved. • Alternative method for the determination of Cu and Fe in wine for routine analysis.

  4. A simple and fast method for assessment of the nitrogen–phosphorus–potassium rating of fertilizers using high-resolution continuum source atomic and molecular absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bechlin, Marcos André; Fortunato, Felipe Manfroi; Moutinho da Silva, Ricardo; Ferreira, Edilene Cristina; Gomes Neto, José Anchieta, E-mail: anchieta@iq.unesp.br

    2014-11-01

    The determination of N, P, and K in fertilizers by high-resolution continuum source flame atomic and molecular absorption spectrometry is proposed. Under optimized conditions, measurements of the diatomic molecules NO and PO at 215.360 and 247.620 nm, respectively, and K using the wing of the alternative line at 404.722 nm allowed calibration curves to be constructed in the ranges 500–5000 mg L{sup −1} N (r = 0.9994), 100–2000 mg L{sup −1} P (r = 0.9946), and 100–2500 mg L{sup −1} K (r = 0.9995). Commercial fertilizers were analyzed by the proposed method and the concentrations of N, P, and K were found to be in agreement with those obtained by Kjeldahl, spectrophotometric, and flame atomic emission spectrometry methods, respectively, at a 95% confidence level (paired t-test). A phosphate rock certified reference material (CRM) was analyzed and the results for P and K were in agreement with the reference values. Recoveries from spiked CRM were in the ranges 97–105% (NO{sub 3}{sup −}-N), 95–103% (NH{sub 4}{sup +}-N), 93–103% (urea-N), 99–108% (P), and 99–102% (K). The relative standard deviations (n = 12) for N, P, and K were 6, 4, and 2%, respectively. - Highlights: • A single technique is proposed to analyze NPK fertilizer. • HR-CS FAAS is proposed for the first time for N, P and K determination in fertilizers. • The method employs the same sample preparation and dilution for the three analytes. • Addition of H{sub 2}O{sub 2} allows analysis of fertilizers with different nitrogen species. • Proposal provides advantages over traditional methods in terms of cost and time.

  5. Multivariate optimization of ultrasound-assisted extraction for determination of Cu, Fe, Ni and Zn in vegetable oils by high-resolution continuum source atomic absorption spectrometry.

    Science.gov (United States)

    Trindade, Alex S N; Dantas, Alailson F; Lima, Daniel C; Ferreira, Sérgio L C; Teixeira, Leonardo S G

    2015-10-15

    An assisted liquid-liquid extraction of copper, iron, nickel and zinc from vegetable oil samples with subsequent determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) was optimized by applying a full factorial design in two levels and the response surface methodology, Box-Behnken. The effects of the acid concentration and the amplitude, cycle and time of sonication on the extraction of the analytes, as well as their interactions, were assessed. In the selected condition (sonication amplitude = 66%, sonication time = 79 s, sonication cycle = 74%), using 0.5 mol L(-1) HCl as the extractant, the limits of quantification were 0.14, 0.20, 0.21 and 0.04 μg g(-1) for Cu, Fe, Ni and Zn, respectively, with R.S.D. ranging from 1.4% to 3.6%. The proposed method was applied for the determination of the analytes in soybean, canola and sunflower oils. PMID:25952852

  6. Use of High-Resolution Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS) for Sequential Multi-Element Determination of Metals in Seawater and Wastewater Samples

    Science.gov (United States)

    Peña-Vázquez, E.; Barciela-Alonso, M. C.; Pita-Calvo, C.; Domínguez-González, R.; Bermejo-Barrera, P.

    2015-09-01

    The objective of this work is to develop a method for the determination of metals in saline matrices using high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Module SFS 6 for sample injection was used in the manual mode, and flame operating conditions were selected. The main absorption lines were used for all the elements, and the number of selected analytical pixels were 5 (CP±2) for Cd, Cu, Fe, Ni, Pb and Zn, and 3 pixels for Mn (CP±1). Samples were acidified (0.5% (v/v) nitric acid), and the standard addition method was used for the sequential determination of the analytes in diluted samples (1:2). The method showed good precision (RSD(%) < 4%, except for Pb (6.5%)) and good recoveries. Accuracy was checked after the analysis of an SPS-WW2 wastewater reference material diluted with synthetic seawater (dilution 1:2), showing a good agreement between certified and experimental results.

  7. A dispersive liquid--liquid microextraction methodology for copper (II) in environmental samples prior to determination using microsample injection flame atomic absorption spectrometry.

    Science.gov (United States)

    Alothman, Zeid A; Habila, Mohamed; Yilmaz, Erkan; Soylak, Mustafa

    2013-01-01

    A simple, environmentally friendly, and efficient dispersive liquid-liquid microextraction method combined with microsample injection flame atomic absorption spectrometry was developed for the separation and preconcentration of Cu(II). 2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol (5-Br-PADAP) was used to form a hydrophobic complex of Cu(II) ions in the aqueous phase before extraction. To extract the Cu(II)-5-Br-PADAP complex from the aqueous phase to the organic phase, 2.0 mL of acetone as a disperser solvent and 200 microL of chloroform as an extraction solvent were used. The influences of important analytical parameters, such as the pH, types and volumes of the extraction and disperser solvents, amount of chelating agent, sample volume, and matrix effects, on the microextraction procedure were evaluated and optimized. Using the optimal conditions, the LOD, LOQ, preconcentration factor, and RSD were determined to be 1.4 microg/L, 4.7 microg/L, 120, and 6.5%, respectively. The accuracy of the proposed method was investigated using standard addition/recovery tests. The analysis of certified reference materials produced satisfactory analytical results. The developed method was applied for the determination of Cu in real samples. PMID:24645524

  8. Preconcentration of uranium, thorium, zirconium, titanium, molybdenum and vanadium with oxine supported on microcrystalline naphthalene and their determinations by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    A sensitive and rapid method for the determination of uranium, thorium, zirconium, titanium, molybdenum and vanadium by inductively coupled plasma atomic emission spectrometry (ICP-AES) after solid-liquid extraction with microcrystalline naphthalene is developed. Analytes were quantitatively adsorbed as their oxinate complexes on naphthalene and determined by ICP-AES after stripping with 2 M HCl. The effect of various experimental parameters such as pH, reagent amounts, naphthalene amount and stripping conditions on the determination of these elements was investigated in detail. Under the optimized experimental conditions, the detection limits of this method for U (VI), Th (IV), Zr (IV), Ti (IV), Mo (VI) and V (V) were 20.0 ng mL-1 and the relative standard deviations obtained for three replicate determinations at a concentration of 1.0 µg mL-1 were 1.5-3.0%. The proposed method has been applied in the analysis of SY-2, SY-3 and pre-analysed samples for U, Th, Zr, Ti, Mo and V the analytical results are in good agreement with recommended values. (author)

  9. Flagging and correcting non-spectral matrix interferences with spatial emission profiles and gradient dilution in inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Matrix interference remains one of the most daunting challenges commonly encountered in inductively coupled plasma-atomic emission spectrometry (ICP-AES). In the present study, a method is described that enables identification and correction of matrix interferences in axial-viewed ICP-AES through a combination of spatial mapping and on-line gradient dilution. Cross-sectional emission maps of the plasma are used to indicate the presence of non-spectral (plasma-related and sample-introduction-related) matrix interferences. In particular, apparent concentrations of an analyte species determined at various radial locations in the plasma differ in the presence of a matrix interference, which allows the interference to be flagged. To correct for the interference, progressive, on-line dilution of the sample, performed by a gradient high-performance liquid-chromatograph pump, is utilized. The spatially dependent intensities of analyte emission are monitored at different levels of sample dilution. As the dilution proceeds, the matrix-induced signal variation is reduced. At a dilution where the determined concentrations become independent of location in the plasma, the matrix interference is minimized. - Highlights: • Non-spectral matrix interference in ICP-AES is flagged and minimized. • Emission from different locations of the plasma are collected simultaneously. • Spatially dependent determined concentrations indicate the presence of interference. • Gradient dilution is performed on both calibration standards and sample. • Optimal dilution factor to minimize interference is found as dilution increases

  10. Novel extraction induced by emulsion breaking as a tool for the determination of trace concentrations of Cu, Mn and Ni in biodiesel by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Pereira, Fernanda M; Zimpeck, Renata C; Brum, Daniel M; Cassella, Ricardo J

    2013-12-15

    This work proposes a novel method for the determination of trace concentrations of Cu, Mn and Ni in biodiesel samples by electrothermal atomic absorption spectrometry. In order to overcome problems related to the organic matrix in the direct introduction of the samples, a new extraction approach was investigated. The method was based on the extraction induced by emulsion breaking, in which metals were transferred from the biodiesel to an acid aqueous phase after formation and breaking of a water-in-oil emulsion prepared by mixing the biodiesel sample with an aqueous solution containing surfactant and nitric acid. Several parameters that could influence the performance of the system were evaluated. Quantitative extractions of the analytes were obtained when the extraction was performed using an emulsifier solution containing 2.1 mol L(-1) of HNO3 and 7% m/v of Triton X-100. The extraction time had remarkable influence on the efficiency of the process, being necessary an agitation time of 60 min to achieve maximum extraction. The limits of quantification were below 1 µg L(-1) for the three analytes under study. The accuracy of the method was tested by application of a recovery test (recovery percentages between 89% and 109% were observed) and by comparison with a well-established method, taken as reference. PMID:24209306

  11. Methylmercury in water samples at the pg/L level by online preconcentration liquid chromatography cold vapor-atomic fluorescence spectrometry

    Science.gov (United States)

    Brombach, Christoph-Cornelius; Chen, Bin; Corns, Warren T.; Feldmann, Jörg; Krupp, Eva M.

    2015-03-01

    Ultra-traces of methylmercury at the sub-ppt level can be magnified in the foodweb and is of concern. In environmental monitoring a routine robust analytical method is needed to determine methylmercury in water. The development of an analytical method for ultra-trace speciation analysis of methylmercury (MeHg) in water samples is described. The approach is based on HPLC-CV-AFS with on-line preconcentration of water samples up to 200 mL, resulting in a detection limit of 40 pg/L (ppq) for MeHg, expressed as Hg. The unit consists of an optimized preconcentration column filled with a sulfur-based sorption material, on which mercury species are preconcentrated and subsequently eluted, separated and detected via HPLC-CV-AFS (high performance liquid chromatography-cold vapor atomic fluorescence spectrometry). During the method development a type of adsorbate material, the pH dependence, the sample load rate and the carry-over were investigated using breakthrough experiments. The method shows broad pH stability in the range of pH 0 to 7, without the need for buffer addition and shows limited matrix effects so that MeHg is quantitatively recovered from sewage, river and seawater directly in the acidified samples without sample preparation.

  12. Mercury(II) and methyl mercury determinations in water and fish samples by using solid phase extraction and cold vapour atomic absorption spectrometry combination.

    Science.gov (United States)

    Tuzen, Mustafa; Karaman, Isa; Citak, Demirhan; Soylak, Mustafa

    2009-07-01

    A method has been developed for mercury(II) and methyl mercury speciation on Staphylococcus aureus loaded Dowex Optipore V-493 micro-column in the presented work, by using cold vapour atomic absorption spectrometry. Selective and sequential elution with 0.1 molL(-1) HCl for methyl mercury and 2 molL(-1) HCl for mercury(II) were performed at the pH range of 2-6. Optimal analytical conditions including pH, amounts of biosorbent, sample volumes were investigated. The detection limits of the analytes were 2.5 ngL(-1) for Hg(II) and 1.7 ngL(-1) for methyl mercury. The capacity of biosorbent for mercury(II) and methyl mercury was 6.5 and 5.4 mgg(-1), respectively. The validation of the presented procedure is performed by the analysis of standard reference material. The speciation procedure established was successfully applied to the speciation of mercury(II) and methyl mercury in natural water and microwave digested fish samples.

  13. Speciation analysis of arsenic by selective hydride generation-cryotrapping-atomic fluorescence spectrometry with flame-in-gas-shield atomizer: achieving extremely low detection limits with inexpensive instrumentation.

    Science.gov (United States)

    Musil, Stanislav; Matoušek, Tomáš; Currier, Jenna M; Stýblo, Miroslav; Dědina, Jiří

    2014-10-21

    This work describes the method of a selective hydride generation-cryotrapping (HG-CT) coupled to an extremely sensitive but simple in-house assembled and designed atomic fluorescence spectrometry (AFS) instrument for determination of toxicologically important As species. Here, an advanced flame-in-gas-shield atomizer (FIGS) was interfaced to HG-CT and its performance was compared to a standard miniature diffusion flame (MDF) atomizer. A significant improvement both in sensitivity and baseline noise was found that was reflected in improved (4 times) limits of detection (LODs). The yielded LODs with the FIGS atomizer were 0.44, 0.74, 0.15, 0.17 and 0.67 ng L(-1) for arsenite, total inorganic, mono-, dimethylated As and trimethylarsine oxide, respectively. Moreover, the sensitivities with FIGS and MDF were equal for all As species, allowing for the possibility of single species standardization with arsenate standard for accurate quantification of all other As species. The accuracy of HG-CT-AFS with FIGS was verified by speciation analysis in two samples of bottled drinking water and certified reference materials, NRC CASS-5 (nearshore seawater) and SLRS-5 (river water) that contain traces of methylated As species. As speciation was in agreement with results previously reported and sums of all quantified species corresponded with the certified total As. The feasibility of HG-CT-AFS with FIGS was also demonstrated by the speciation analysis in microsamples of exfoliated bladder epithelial cells isolated from human urine. The results for the sums of trivalent and pentavalent As species corresponded well with the reference results obtained by HG-CT-ICPMS (inductively coupled plasma mass spectrometry).

  14. Selective Flow-Injection Quantification of Ultra-trace Amounts of Cr(VI) via On-line Complexation and Preconcentration with APDC Followed by Determination by Electrothermal Atomic Absorption Spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Steffen; Hansen, Elo Harald

    1998-01-01

    A rapid, sensitive and selective time-based flow injection (FI) preconcentration procedure is described for the determination of ultra-trace amounts of Cr(VI) via on-line reaction with ammonium pyrrolidine dithiocarbamate (APDC) and formation of the Cr(VI)-PDC complex. The preconcentration...... is effected by adsorption on the inner wall of a knotted reactor made from PTFE tubing. The complex is subsequently eluted with a monosegmented discrete zone of ethanol (55 mu l), and the analyte is quantified by electrothermal atomic absorption spectrometry (ETAAS). The operations of the FI...

  15. Elemental determination of microsamples by liquid film dielectric barrier discharge atomic emission spectrometry.

    Science.gov (United States)

    He, Qian; Zhu, Zhenli; Hu, Shenghong; Zheng, Hongtao; Jin, Lanlan

    2012-05-01

    In this study, a new liquid-film dielectric barrier discharge (LFDBD) atomic emission source was developed for microsample elemental determination. It consists of a copper electrode, a tungsten wire electrode, and a piece of glass slide between them, which serves as the dielectric barrier as well as the sample plate. The sample solution with 1 mol L(-1) nitric acid, when deposited onto the surface of the glass slide, forms a thin liquid film. The plasma is generated between the tip of the tungsten wire electrode and the liquid film surface when alternating-current (ac) high voltage (peak voltage ~3.7 kV, frequency ~30 kHz) is applied on the electrodes. Qualitative and quantitative determinations of metal ions in the sample solution were achieved by atomic emission measurements in the plasma and were demonstrated in this study with elements Na, K, Cu, Zn, and Cd. Detection limits were in the range from 0.6 ng (7 μg L(-1)) for Na to 6 ng (79 μg L(-1)) for Zn. Repeatability, expressed as relative standard deviation from seven repetitive analyses of samples with analyte concentrations at 1 mg L(-1), varied from 2.1% to 4.4%. Compared with other liquid discharge systems that operate at atmospheric pressure, the current system offers several advantages: First, it eliminates the use of a sample flow system (e.g., syringe or peristaltic pump); instead, a small aliquot of sample is directly pipetted onto the glass slide for analysis. Second, it is a microanalysis system and requires sample volume ≤80 μL, a benefit when a limited amount of sample is available. Third, because the sample is applied in aliquot, there is no washout time, and the analysis can be easily extended to sample array for high-throughput analysis. The proposed LFDBD is promising for in-field elemental determination because of its simplicity, cost effectiveness, low power supply, and no inert gas requirement. PMID:22486234

  16. Study of the roles of chemical modifiers in determining boron using graphite furnace atomic absorption spectrometry and optimization of the temperature profile during atomization

    International Nuclear Information System (INIS)

    The measurement conditions for determining boron using graphite furnace–atomic absorption spectrometry (GF-AAS) were investigated. Differences in the boron absorbance profiles were found using three different commercially available GF-AAS instruments when the graphite atomizers in them were not tuned. The boron absorbances found with and without adjusting the graphite atomizers suggested that achieving an adequate absorbance for the determination of boron requires a sharp temperature profile that overshoots the target temperature during the atomization process. Chemical modifiers that could improve the boron absorbance without the need for using coating agents were tested. Calcium carbonate improved the boron absorbance but did not suppress variability in the peak height. Improvement of boron absorbance was comparatively less using iron nitrate or copper nitrate than using calcium carbonate, but variability in the peak height was clearly suppressed using iron nitrate or copper nitrate. The limit of detection was 0.0026 mg L−1 when iron nitrate was used. It appears that iron nitrate is a useful new chemical modifier for the quick and simple determination of boron using GF-AAS. (author)

  17. Chemical modifiers in arsenic determination in biological materials by tungsten coil electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bruhn, C.G.; Huerta, V.N.; Neira, J.Y. [Departamento de Analisis Instrumental, Facultad de Farmacia, Universidad de Concepcion, P.O. Box 237, Concepcion (Chile)

    2004-01-01

    Palladium, iridium, and rhodium are evaluated as possible chemical modifiers in the determination of As in digest solutions of biological materials (human hair and clam) by tungsten coil electrothermal atomic absorption spectrophotometry (TCA-AAS). The modifier in solution was applied onto the coil and thermally pre-reduced; the pre-reduction conditions, the amount of modifier, and the thermal program were optimized. Palladium was not satisfactory, whereas Ir and Rh were effective modifiers and rendered better relative sensitivity for As by a factor of 1.4 and 1.9, respectively compared to the case without modifier. Upon optimization of thermal conditions for As in pre-reduced Ir (2.0 {mu}g) and Rh (2.0 {mu}g) modifiers and in the digest solutions of the study matrices, Rh (2.0 {mu}g) was more effective modifier and was selected as such. The mean within-day repeatability was 2.8% in consecutive measurements (25-100 {mu}g L{sup -1}) (3 cycles, each of n=6) and confirmed good short-term stability of the absorbance measurements. The mean reproducibility was 4.4% (n=20 in a 3-day period) and the detection limit (3{sigma}{sub blank}/slope) was 29 pg (n=15). The useful coil lifetime in Rh modifier was extended to 300-400 firings. Validation was by determination of As in the certified reference material (CRM) of ''Oyster tissue'' solution with a percentage relative error (E{sub rel}%) of 2% and percentage relative standard deviation (RSD%) of 3% (n=4), and by analytical recovery of As spiked in CRM of human hair [94{+-}8% (n=4)]. The methodology is simple, fast (sample readout frequency 21 h{sup -1}), reliable, of low cost, and was applied to the determination of As in hair samples of exposed and unexposed workers. (orig.)

  18. Determination of copper and mercury in phosphate fertilizers employing direct solid sampling analysis and high resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    de Oliveira Souza, Sidnei; François, Luciane Luiza; Borges, Aline Rocha; Vale, Maria Goreti Rodrigues; Araujo, Rennan Geovanny Oliveira

    2015-12-01

    The present study proposes the determination of copper and mercury in phosphate fertilizers by direct solid sampling analysis (SS) employing high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). For Cu determination, two analytical lines were used: 327.3960 nm and 249.2146 nm. Hg determination was carried out on the line 253.6521 nm and 100 μg KMnO4 was used as chemical modifier. The optimal pyrolysis temperature for Cu determination was 1300 °C. Atomization temperatures for Cu and Hg were 2400 and 1100 °C, respectively. External calibration with aqueous standard solutions was adopted for both elements. The limits of quantification (LoQs) and characteristic mass (m0) obtained for Cu determination were 0.4 μg g- 1 and 1.12 ng, respectively, on line 249.2146 nm, and 64 μg g- 1 and 25 pg on 327.3960 nm. For mercury, LoQ and m0 were 4.8 ng g- 1 and 39 pg, respectively. The accuracy of the proposed methods was confirmed by the analysis of standard reference material (SRM) of Trace Elements in Multi-Nutrient Fertilizer (SRM NIST 695). The precision expressed as relative standard deviation (RSD), was better than 8.2% for Hg and 7.7% for the Cu (n = 5), considered satisfactory for microanalysis in solid sample. Four fertilizer samples acquired in commercial establishments in the city of Salvador, Bahia, Brazil, were analyzed. The optimized analytical methods were simple, fast, accurate, precise and free of spectral interferences for the determination of Cu and Hg in phosphate fertilizer samples by SS-HR-CS GF AAS, avoiding the dissolution of the sample, the use of harmful reagents and the generation of residues.

  19. ANALYSES OF QUINOLONE ANTIMICROBIALS IN HUMAN PLASMA BY CAPILLARY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY/FAST ATOM BOMBARDMENT MASS SPECTROMETRY

    OpenAIRE

    Hattori, Hideki; Suzuki, Osamu; Seno, Hiroshi; Ishii, Akira; Yamada, Takamichi

    1993-01-01

    Capillary high-performance liquid chromatography (HPLC) was combined with frit fast atom bombardment (FAB)-mass spectrometry (MS) , and a detailed procedure has been established for on-line analysis of ten quinolone antimicrobials in human plasma by the HPLC/FAB-MS. A special column switching device for concentration enabled injection of as large as a 500 μl sample; and the capillary column (0.5 mm i. d.) enabled introduction of its entire effluent to the frit interface of FAB-MS. These condi...

  20. Determination of Heavy Metals in Meat, Intestine, Liver, Eggs, and Chicken Using Neutron Activation Analysis and Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    The elements As, Cd, Co, Cr, Fe, Hg, Ni, Pb, Sb, se and Zn in meat, intestine, and liver of cow and goat, as well as in broiler, local breed chicken and eggs have been determined using Neutron Activation Analysis and Atomic Absorption Spectrometry. Mercury was determined after being separated radiochemically. The results showed that concentration of the essential elements studied i.e. Cr, Cu, Fe, Zn, Co, and Ni were higher in liver and intestine than in the meat, but still in the normal range, while toxic elements As, Cd, and Pb were undetectable in all samples. (author). 8 refs., 6 tabs

  1. Analytical Model of the Nonlinear Dynamics of Cantilever Tip-Sample Surface Interactions for Various Acoustic-Atomic Force Microscopies

    Science.gov (United States)

    Cantrell, John H., Jr.; Cantrell, Sean A.

    2008-01-01

    A comprehensive analytical model of the interaction of the cantilever tip of the atomic force microscope (AFM) with the sample surface is developed that accounts for the nonlinearity of the tip-surface interaction force. The interaction is modeled as a nonlinear spring coupled at opposite ends to linear springs representing cantilever and sample surface oscillators. The model leads to a pair of coupled nonlinear differential equations that are solved analytically using a standard iteration procedure. Solutions are obtained for the phase and amplitude signals generated by various acoustic-atomic force microscope (A-AFM) techniques including force modulation microscopy, atomic force acoustic microscopy, ultrasonic force microscopy, heterodyne force microscopy, resonant difference-frequency atomic force ultrasonic microscopy (RDF-AFUM), and the commonly used intermittent contact mode (TappingMode) generally available on AFMs. The solutions are used to obtain a quantitative measure of image contrast resulting from variations in the Young modulus of the sample for the amplitude and phase images generated by the A-AFM techniques. Application of the model to RDF-AFUM and intermittent soft contact phase images of LaRC-cp2 polyimide polymer is discussed. The model predicts variations in the Young modulus of the material of 24 percent from the RDF-AFUM image and 18 percent from the intermittent soft contact image. Both predictions are in good agreement with the literature value of 21 percent obtained from independent, macroscopic measurements of sheet polymer material.

  2. Multiple response optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry with sample injection as detergent emulsion

    Energy Technology Data Exchange (ETDEWEB)

    Brum, Daniel M.; Lima, Claudio F. [Departamento de Quimica, Universidade Federal de Vicosa, A. Peter Henry Rolfs s/n, Vicosa/MG, 36570-000 (Brazil); Robaina, Nicolle F. [Departamento de Quimica Analitica, Universidade Federal Fluminense, Outeiro de S.J. Batista s/n, Centro, Niteroi/RJ, 24020-141 (Brazil); Fonseca, Teresa Cristina O. [Petrobras, Cenpes/PDEDS/QM, Av. Horacio Macedo 950, Ilha do Fundao, Rio de Janeiro/RJ, 21941-915 (Brazil); Cassella, Ricardo J., E-mail: cassella@vm.uff.br [Departamento de Quimica Analitica, Universidade Federal Fluminense, Outeiro de S.J. Batista s/n, Centro, Niteroi/RJ, 24020-141 (Brazil)

    2011-05-15

    The present paper reports the optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry (GF AAS) employing a strategy based on the injection of the samples as detergent emulsions. The method was optimized in relation to the experimental conditions for the emulsion formation and taking into account that the three analytes (Cu, Fe and Pb) should be measured in the same emulsion. The optimization was performed in a multivariate way by employing a three-variable Doehlert design and a multiple response strategy. For this purpose, the individual responses of the three analytes were combined, yielding a global response that was employed as a dependent variable. The three factors related to the optimization process were: the concentration of HNO{sub 3}, the concentration of the emulsifier agent (Triton X-100 or Triton X-114) in aqueous solution used to emulsify the sample and the volume of solution. At optimum conditions, it was possible to obtain satisfactory results with an emulsion formed by mixing 4 mL of the samples with 1 mL of a 4.7% w/v Triton X-100 solution prepared in 10% v/v HNO{sub 3} medium. The resulting emulsion was stable for 250 min, at least, and provided enough sensitivity to determine the three analytes in the five samples tested. A recovery test was performed to evaluate the accuracy of the optimized procedure and recovery rates, in the range of 88-105%; 94-118% and 95-120%, were verified for Cu, Fe and Pb, respectively.

  3. Automatic microemulsion preparation for metals determination in fuel samples using a flow-batch analyzer and graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Cunha, Francisco Antonio S. [Universidade Federal da Paraiba, CCEN, Departamento de Quimica, P. Box 5093, 58051-970, Joao Pessoa, PB (Brazil); Sousa, Rafael A. [Institute of Chemistry-University of Campinas, P.O. Box 6154, 13083-970, Campinas, SP (Brazil); Harding, David P. [Universidade Federal da Paraiba, CCEN, Departamento de Quimica, P. Box 5093, 58051-970, Joao Pessoa, PB (Brazil); Cadore, Solange [Institute of Chemistry-University of Campinas, P.O. Box 6154, 13083-970, Campinas, SP (Brazil); Almeida, Luciano F. [Universidade Federal da Paraiba, CCEN, Departamento de Quimica, P. Box 5093, 58051-970, Joao Pessoa, PB (Brazil); Araujo, Mario Cesar U., E-mail: laqa@quimica.ufpb.br [Universidade Federal da Paraiba, CCEN, Departamento de Quimica, P. Box 5093, 58051-970, Joao Pessoa, PB (Brazil)

    2012-05-21

    Highlights: Black-Right-Pointing-Pointer Micro-emulsion composition phase study to obtain low fuel dilutions. Black-Right-Pointing-Pointer Automated and instantaneous in-line preparation of micro-emulsions for metals determinations. Black-Right-Pointing-Pointer A versatile piston-driven form of 'Flow-batch Analysis'. Black-Right-Pointing-Pointer Rheological considerations explored including a mathematical derivation of flow parameters. - Abstract: The principal thermodynamic advantages of using microemulsions over standard emulsions for flow metal analysis are the greatly increased analyte stability and emulsive homogeneity that improve both the ease of sample preparation, and the analytical result. In this study a piston propelled flow-batch analyzer (PFBA) for the determination of Cu, Cr and Pb in gasoline and naphtha by graphite furnace atomic absorption spectrometry (GF AAS) was explored. Investigative phase modeling for low dilution was conducted both for gasoline and naphtha microemulsions. Rheological considerations were also explored including a mathematical flow derivation to fine tune the system's operational parameters, and the GF AAS coupling. Both manual and automated procedures for microemulsion preparation were compared. The results of the paired t test at a 95% confidence level showed no significant differences between them. Further recovery test results confirmed a negligible matrix effect of the sample on the analyte absorption signals and an efficient stabilization of the samples (with metals) submitted to microemulsion treatment. The accuracy of the developed procedure was attested by good recovery percentages in the ranges of 100.0 {+-} 3.5% for Pb in the naphtha samples, and 100.2 {+-} 3.4% and 100.7 {+-} 4.6% for Cu and Cr, respectively in gasoline samples.

  4. Direct determination of arsenic in petroleum derivatives by graphite furnace atomic absorption spectrometry: A comparison between filter and platform atomizers

    Energy Technology Data Exchange (ETDEWEB)

    Becker, Emilene; Rampazzo, Roger T.; Dessuy, Morgana B. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R., E-mail: mgrvale@ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq - INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Silva, Marcia M. da [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Welz, Bernhard [Instituto Nacional de Ciencia e Tecnologia do CNPq - INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Katskov, Dmitri A. [Tshwane University of Technology (TUT), Faculty of Science, Chemistry Department, Pretoria 0001 (South Africa)

    2011-05-15

    In the present work a direct method for the determination of arsenic in petroleum derivatives has been developed, comparing the performance of a commercial transversely heated platform atomizer (THPA) with that of a transversely heated filter atomizer (THFA). The THFA results in a reduction of background absorption and an improved sensitivity as has been reported earlier for this atomizer. The mixture of 0.1% (m/v) Pd + 0.03% (m/v) Mg + 0.05% (v/v) Triton X-100 was used as the chemical modifier for both atomizers. The samples (naphtha, gasoline and petroleum condensate) were stabilized in the form of a three-component solution (detergentless microemulsion) with the sample, propan-1-ol and 0.1% (v/v) HNO{sub 3} in a ratio of 3.0:6.4:0.6. The characteristic mass of 13 pg found in the THFA was about a factor of two better than that of 28 pg obtained with the THPA; however, the limits of detection (LOD) and quantification (LOQ) were essentially the same for both atomizers (1.9 and 6.2 {mu}g L{sup -1}, respectively, for THPA, and 1.8 and 5.9 {mu}g L{sup -1}, respectively, for THFA) due to the increased noise observed with the THFA. A possible explanation for that is a partial blockage of the radiation from the hollow cathode lamp by the narrow inner diameter of this tube and the associated loss of radiation energy. Due to the lack of an appropriate certified reference material, recovery tests were carried out with inorganic and organic arsenic standards and the results were between 89% and 111%. The only advantage of the THFA found in this work was a reduction of the total analysis time by about 20% due to the 'hot injection' that could be realized with this furnace. The arsenic concentrations varied from < LOQ to 43.3 {mu}g L{sup -1} in the samples analyzed in this work.

  5. LASER-ENHANCED IONIZATION SPECTROMETRY WITH A TOTAL CONSUMPTION BURNER

    OpenAIRE

    Green, R; Hall, Janet

    1983-01-01

    This paper describes the use of a total consumption burner as an analytical atom reservoir for laser-enhanced ionization spectrometry. A total consumption burner and premixed burner are compared for limits of detection and matrix interferences. These results demonstrate that high sensitivity laser-enhanced ionization measurements are possible in adverse sample environments where traditional methods of optical spectrometry have proven inadequate.

  6. Analytical approaches for determination of bromine in sediment core samples by X-ray fluorescence spectrometry.

    Science.gov (United States)

    Pashkova, Galina V; Aisueva, Tatyana S; Finkelshtein, Alexander L; Ivanov, Egor V; Shchetnikov, Alexander A

    2016-11-01

    Bromine has been recognized as a valuable indicator for paleoclimatic studies. Wavelength dispersive X-ray fluorescence (WDXRF) and total reflection X-ray fluorescence (TXRF) methods were applied to study the bromine distributions in lake sediment cores. Conventional WDXRF technique usually requires relatively large mass of a sediment sample and a set of calibration samples. Some analytical approaches were developed to apply WDXRF to small sediment core samples in the absence of adequate calibration samples with a known Br content. The mass of a sample to be analyzed was reduced up to 200-300mg and the internal standard method with correction using fundamental parameters was developed for Br quantification. TXRF technique based on the direct analysis of a solid suspension using 20mg of sediment sample by internal standard method was additionally tested. The accuracy of the WDXRF and TXRF techniques was assessed by the comparative analysis of reference materials of sediments, soil and biological samples. In general, good agreement was achieved between the reference values and the measured values. The detection limits of Br were 1mg/kg and 0.4mg/kg for WDXRF and TXRF respectively. The results of the Br determination obtained with different XRF techniques were comparable to each other and used for paleoclimatic reconstructions. PMID:27591627

  7. Analytical Absorption Cross-Section for Photon by a Hydrogen 2s Atom

    Institute of Scientific and Technical Information of China (English)

    Boniface Otieno Ndinya; Stephen Onyango Okeyo

    2011-01-01

    We calculate the absorption cross-section for photon by a hydrogen 2s atom using the quantum-classical approximation for the total photo cross-section of many electron atoms.With the application of the first-order term of the Baker-Hausdorf expansion, the absorption cross-section for the hydrogen 2s atom decreases to a minimum, the Cooper pair minimum, at low photon energy.Such a minimum is absent in the exact absorption cross-section for photon by a hydrogen 2s atom.We have extended the calculation for the absorption cross-section of the hydrogen 2s atom using the quantum-classical approximation for the total photo cross-section of many electron to include the second-order term of the Baker-Hausdorf expansion and observed a great reduction in the dip associated with the Cooper pair minimum at the zero crossing.

  8. Characterization of Arsenic Biotransformation Products from an Open Anaerobic Degradation of Fucus distichus by Hydride Generation Gas Chromatography Atomic Absorption Spectrometry and High Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry

    OpenAIRE

    Abiodun A. Ojo; Onasanya, Amos

    2013-01-01

    This work reports on the isolation and determination of biotransformation products obtained from the organoarsenic compounds that are present in Fucus distichus when it was subjected to an open anaerobic decomposition by using the Hydride Generation Gas Chromatography Atomic Absorption Spectrometry (HG-GC-AAS) and High Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS). The seaweed and filtrate residues obtained from the open anaerobic degradation pro...

  9. Contents of cadmium, mercury and lead in fish from the Atlantic sea (Morocco) determined by atomic absorption spectrometry.

    Science.gov (United States)

    Chahid, Adil; Hilali, Mustapha; Benlhachimi, Abdeljalil; Bouzid, Taoufiq

    2014-03-15

    As a part of a specific monitoring program, lead (Pb) cadmium (Cd) and mercury (Hg) concentrations in important species of fish from various fishing ports of the southern Kingdom of Morocco (Sardina pilchardus, Scomber scombrus, Plectorhinchus mediterraneus, Trachurus trachurus, Octopus vulgaris, Boops boops, Sarda sarda, Trisopterus capelanus, and Conger conger) were investigated by the Moroccan Reference Laboratory (NRL) for trace elements in foodstuffs of animal origin. The samples were analysed for lead and cadmium by a graphite furnace atomic absorption spectrometry (GFAAS); and for mercury by cold vapour atomic absorption spectrometry (CVAAS). The results were expressed as μg/g of wet weight (w/w). The levels of Cd, Pb and Hg in muscles of fish were 0.009-0.036, 0.013-0.114 and 0.049-0.194 μg/g, respectively. The present study showed that different metals were present in the sample at different levels but within the maximum residual levels prescribed by the EU for the fish and shellfish from these areas, in general, should cause no health problems for consumers.

  10. Determination of gaseous semi-and low-volatile organic halogen compounds by barrier-discharge atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    Yifei Sun; Nobuhisa Watanabe; Wei Wang; Tianle Zhu

    2013-01-01

    A group parameter approach using "total organic halogen" is effective for monitoring gaseous organic halogen compounds,including fluorine,chlorine,and bromine compounds,generated from combustion.We described the use of barrier-discharge radiofrequencyhelium-plasma/atomic emission spectrometry,for the detection of semi-and low-volatile organic halogen compounds (SLVOXs),which can be collected by CarbotrapTM adsorbents and analyzed using thermal desorption.The optimal carrier gas flow rates at the injection and desorption lines were established to be 100 mL/min.The detection range for SLVOXs in the gaseous samples was from 10 ng to tens of micrograms.Measuring F was more diflicult than measuring Cl or Br,because the wavelength ofF is dose to that of air.The barrierdischarge radiofrequency-helium-plasma/atomic emission spectrometry measured from 85% to 103% of the SLVOXs in the gas sample.It has been found that Carbotrap B is appropriate for high-boiling-point compounds,and Carbotrap C is suitable for the determination of organic halogen compounds with lower boiling points,in the range 200-230℃.Under optimal analysis conditions,a chlorinecontaining plastic was destroyed using different oxygen concentrations.Lower oxygen concentrations resulted in the production of lower amounts of organic halogen compounds.

  11. Determination of Mercury in Aqueous and Geologic Materials by Continuous Flow-Cold Vapor-Atomic Fluorescence Spectrometry (CVAFS)

    Science.gov (United States)

    Hageman, Philip L.

    2007-01-01

    New methods for the determination of total mercury in geologic materials and dissolved mercury in aqueous samples have been developed that will replace the methods currently (2006) in use. The new methods eliminate the use of sodium dichromate (Na2Cr2O7 ?2H2O) as an oxidizer and preservative and significantly lower the detection limit for geologic and aqueous samples. The new methods also update instrumentation from the traditional use of cold vapor-atomic absorption spectrometry to cold vapor-atomic fluorescence spectrometry. At the same time, the new digestion procedures for geologic materials use the same size test tubes, and the same aluminum heating block and hot plate as required by the current methods. New procedures for collecting and processing of aqueous samples use the same procedures that are currently (2006) in use except that the samples are now preserved with concentrated hydrochloric acid/bromine monochloride instead of sodium dichromate/nitric acid. Both the 'old' and new methods have the same analyst productivity rates. These similarities should permit easy migration to the new methods. Analysis of geologic and aqueous reference standards using the new methods show that these procedures provide mercury recoveries that are as good as or better than the previously used methods.

  12. Determination of total selenium in pharmaceutical and herbal supplements by hydride generation and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Kazi, Tasneem G; Kolachi, Nida F; Afridi, Hassan I; Brahman, Kapil Dev; Shah, Faheem

    2014-01-01

    The total selenium (Se) was determined in herbal and pharmaceutical supplements used for liver diseases. The total Se contents were determined in different pharmaceutical and herbal supplements by hydride generation atomic absorption spectrometry (HGAAS) and graphite furnace atomic absorption spectrometry (GFAAS) after microwave-assisted acid digestion. The accuracy of the techniques was evaluated by using certified reference material and the standard addition method. The recoveries of total Se were 99.4 and 99.0% for HGAAS and GFAAS, respectively. The precision of the techniques expressed as RSD were 2.34 and 4.54% for HGAAS and GFAAS measurements, respectively. The LOD values for HGAAS and GFAAS were 0.025 and 0.052 pglg, respectively. The concentrations of Se in pharmaceutical and herbal supplements were found in the range of 19.2-53.8 and 25.0-42.5 pg/g, respectively, corresponding to 35-76% and 45-76% of the total recommended dose of Se for adults. PMID:25632445

  13. Determination of gold in geologic materials by solvent extraction and atomic-absorption spectrometry

    Science.gov (United States)

    Huffman, Claude; Mensik, J.D.; Riley, L.B.

    1967-01-01

    The two methods presented for the determination of traces of gold in geologic materials are the cyanide atomic-absorption method and the fire-assay atomic-absorption method. In the cyanide method gold is leached with a sodium-cyanide solution. The monovalent gold is then oxidized to the trivalent state and concentrated by extracting into methyl isobutyl ketone prior to estimation by atomic absorption. In the fire-assay atomic-absorption method, the gold-silver bead obtained from fire assay is dissolved in nitric and hydrochloric acids. Gold is then concentrated by extracting into methyl isobutyl ketone prior to determination by atomic absorption. By either method concentrations as low as 50 parts per billion of gold can be determined in a 15-gram sample.

  14. Comprehensive analytical strategy for biomarker identification based on liquid chromatography coupled to mass spectrometry and new candidate confirmation tools.

    Science.gov (United States)

    Mohamed, Rayane; Varesio, Emmanuel; Ivosev, Gordana; Burton, Lyle; Bonner, Ron; Hopfgartner, Gérard

    2009-09-15

    A comprehensive analytical LC-MS(/MS) platform for low weight biomarkers molecule in biological fluids is described. Two complementary retention mechanisms were used in HPLC by optimizing the chromatographic conditions for a reversed-phase column and a hydrophilic interaction chromatography column. LC separation was coupled to mass spectrometry by using an electrospray ionization operating in positive polarity mode. This strategy enables us to correctly retain and separate hydrophobic as well as polar analytes. For that purpose artificial model study samples were generated with a mixture of 38 well characterized compounds likely to be present in biofluids. The set of compounds was used as a standard aqueous mixture or was spiked into urine at different concentration levels to investigate the capability of the LC-MS(/MS) platform to detect variations across biological samples. Unsupervised data analysis by principal component analysis was performed and followed by principal component variable grouping to find correlated variables. This tool allows us to distinguish three main groups whose variables belong to (a) background ions (found in all type of samples), (b) ions distinguishing urine samples from aqueous standard and blank samples, (c) ions related to the spiked compounds. Interpretation of these groups allows us to identify and eliminate isotopes, adducts, fragments, etc. and to generate a reduced list of m/z candidates. This list is then submitted to the prototype MZSearcher software tool which simultaneously searches several lists of potential metabolites extracted from metabolomics databases (e.g., KEGG, HMDB, etc) to propose biomarker candidates. Structural confirmation of these candidates was done off-line by fraction collection followed by nanoelectrospray infusion to provide high quality MS/MS data for spectral database queries. PMID:19702294

  15. Nonstationary structure of atomic and molecular layers in electrothermal. Atomic absorption spectrometry: formation of atomic and molecular absorbing layers of gallium and indium

    International Nuclear Information System (INIS)

    The dynamics of the formation of absorbing layers of gallium and indium atoms and their compounds in a graphite tubular atomizer was investigated by the shadow spectral filming method. These compounds are localozed in the central part of the furnace over the platform and dissapear ay the hotter walls. It the case of gallium and indium atomization, the effects of chemical reactions between the vapor and the walls of the furnace on the formation of absorbing layers are stronger than that of diffusion and convective mass-transfer processes, which are common to all of the elements. Atom propagation from the center to the stomizer ends proceeds through the cascade mechanism because of its relatively low rate of warming up and strong longitudinal anisothermicity

  16. Ultrasensitive determination of cadmium in seawater by hollow fiber supported liquid membrane extraction coupled with graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Peng, Jin-feng; Liu, Rui; Liu, Jing-fu; He, Bin; Hu, Xia-lin; Jiang, Gui-bin

    2007-05-01

    A new procedure, based on hollow fiber supported liquid membrane preconcentration coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection, was developed for the determination of trace Cd in seawater samples. With 1-octanol that contained a mixture of dithizone (carrier) and oleic acid immobilized in the pores of the polypropylene hollow fiber as a liquid membrane, Cd was selectively extracted from water samples into 0.05 M HNO 3 that filled the lumen of the hollow fiber as a stripping solution. The main extraction related parameters were optimized, and the effects of salinity and some coexisting interferants were also evaluated. Under the optimum extraction conditions, an enrichment factor of 387 was obtained for a 100-mL sample solution. In combination with graphite furnace atomic absorption spectrometry, a very low detection limit (0.8 ng L - 1 ) and a relative standard deviation (2.5% at 50 ng L - 1 level) were achieved. Five seawater samples were analyzed by the proposed method without dilution, with detected Cd concentration in the range of 56.4-264.8 ng L - 1 and the relative spiked recoveries over 89%. For comparison, these samples were also analyzed by the Inductively Coupled Plasma Mass Spectrometry (ICP-MS) method after a 10-fold dilution for matrix effect elimination. Statistical analysis with a one-way ANOVA shows no significant differences (at 0.05 level) between the results obtained by the proposed and ICP-MS methods. Additionally, analysis of certified reference materials (GBW (E) 080040) shows good agreement with the certified value. These results indicate that this present method is very sensitive and reliable, and can effectively eliminate complex matrix interferences in seawater samples.

  17. Ultrasensitive determination of cadmium in seawater by hollow fiber supported liquid membrane extraction coupled with graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Peng Jinfeng; Liu Rui [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P. O. Box 2871, Beijing 100085 (China); Liu Jingfu [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P. O. Box 2871, Beijing 100085 (China)], E-mail: jfliu@rcees.ac.cn; He Bin; Hu Xialin; Jiang Guibin [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P. O. Box 2871, Beijing 100085 (China)

    2007-05-15

    A new procedure, based on hollow fiber supported liquid membrane preconcentration coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection, was developed for the determination of trace Cd in seawater samples. With 1-octanol that contained a mixture of dithizone (carrier) and oleic acid immobilized in the pores of the polypropylene hollow fiber as a liquid membrane, Cd was selectively extracted from water samples into 0.05 M HNO{sub 3} that filled the lumen of the hollow fiber as a stripping solution. The main extraction related parameters were optimized, and the effects of salinity and some coexisting interferants were also evaluated. Under the optimum extraction conditions, an enrichment factor of 387 was obtained for a 100-mL sample solution. In combination with graphite furnace atomic absorption spectrometry, a very low detection limit (0.8 ng L{sup -1}) and a relative standard deviation (2.5% at 50 ng L{sup -1} level) were achieved. Five seawater samples were analyzed by the proposed method without dilution, with detected Cd concentration in the range of 56.4-264.8 ng L{sup -1} and the relative spiked recoveries over 89%. For comparison, these samples were also analyzed by the Inductively Coupled Plasma Mass Spectrometry (ICP-MS) method after a 10-fold dilution for matrix effect elimination. Statistical analysis with a one-way ANOVA shows no significant differences (at 0.05 level) between the results obtained by the proposed and ICP-MS methods. Additionally, analysis of certified reference materials (GBW (E) 080040) shows good agreement with the certified value. These results indicate that this present method is very sensitive and reliable, and can effectively eliminate complex matrix interferences in seawater samples.

  18. Green method for ultrasensitive determination of Hg in natural waters by electrothermal-atomic absorption spectrometry following sono-induced cold vapor generation and 'in-atomizer trapping'

    International Nuclear Information System (INIS)

    Sono-induced cold vapor generation (SI-CVG) has been used for the first time in combination with a graphite furnace atomizer for determination of Hg in natural waters by electrothermal-atomic absorption spectrometry after in situ trapping onto a noble metal-pretreated platform (Pd, Pt or Rh) inserted into a graphite tube. The system allows 'in-atomizer trapping' of Hg without the use of conventional reduction reactions based on sodium borohydride or tin chloride in acid medium for cold vapor generation. The sono-induced reaction is accomplished by applying ultrasound irradiation to the sample solution containing Hg(II) in the presence of an organic compound such as formic acid. As this organic acid is partly degraded upon ultrasound irradiation to yield CO, CO2, H2 and H2O, the amount of lab wastes is minimized and a green methodology is achieved. For this purpose, experimental variables influencing the generation/trapping process are fully investigated. The limit of detection for a 10 min trapping time and 10 mL sample volume was 0.03 μg L-1 (Integrated absorbance) and the repeatability expressed as relative standard deviation was about 3%. Carbonates and chlorides at 100 mg L-1 level caused a signal depression by 20-30%. The enhanced trapping efficiency observed with the sono-induced cold vapor generation as compared with 'in-atomizer trapping' methods employing chemical vapor generation is discussed. A reaction pathway for SI-CVG is proposed on the basis of the current knowledge for synthesis of noble metal nanoparticles by ultrasound

  19. An analytical platform for mass spectrometry-based identification and chemical analysis of RNA in ribonucleoprotein complexes.

    Science.gov (United States)

    Taoka, Masato; Yamauchi, Yoshio; Nobe, Yuko; Masaki, Shunpei; Nakayama, Hiroshi; Ishikawa, Hideaki; Takahashi, Nobuhiro; Isobe, Toshiaki

    2009-11-01

    We describe here a mass spectrometry (MS)-based analytical platform of RNA, which combines direct nano-flow reversed-phase liquid chromatography (RPLC) on a spray tip column and a high-resolution LTQ-Orbitrap mass spectrometer. Operating RPLC under a very low flow rate with volatile solvents and MS in the negative mode, we could estimate highly accurate mass values sufficient to predict the nucleotide composition of a approximately 21-nucleotide small interfering RNA, detect post-transcriptional modifications in yeast tRNA, and perform collision-induced dissociation/tandem MS-based structural analysis of nucleolytic fragments of RNA at a sub-femtomole level. Importantly, the method allowed the identification and chemical analysis of small RNAs in ribonucleoprotein (RNP) complex, such as the pre-spliceosomal RNP complex, which was pulled down from cultured cells with a tagged protein cofactor as bait. We have recently developed a unique genome-oriented database search engine, Ariadne, which allows tandem MS-based identification of RNAs in biological samples. Thus, the method presented here has broad potential for automated analysis of RNA; it complements conventional molecular biology-based techniques and is particularly suited for simultaneous analysis of the composition, structure, interaction, and dynamics of RNA and protein components in various cellular RNP complexes.

  20. Effects of Tailored Surface Chemistry on Desorption Electrospray Ionization Mass Spectrometry: a Surface-Analytical Study by XPS and AFM

    Science.gov (United States)

    Penna, Andrea; Careri, Maria; Spencer, Nicholas D.; Rossi, Antonella

    2015-08-01

    Since it was proposed for the first time, desorption electrospray ionization-mass spectrometry (DESI-MS) has been evaluated for applicability in numerous areas. Elucidations of the ionization mechanisms and the subsequent formation of isolated gas-phase ions have been proposed so far. In this context, the role of both surface and pneumatic effects on ion-formation yield has recently been investigated. Nevertheless, the effect of the surface chemistry has not yet been completely understood. Functionalized glass surfaces have been prepared, in order to tailor surface performance for ion formation. Three substrates were functionalized by depositing three different silanes [3-mercaptopropyltriethoxysilane (MTES), octyltriethoxysilane (OTES), and 1H,1H,2H,2H-perfluorooctyltriethoxy-silane (FOTES)] from toluene solution onto standard glass slides. Surface characterization was carried out by contact-angle measurements, tapping-mode atomic force microscopy, and X-ray photoelectron spectroscopy. Morphologically homogeneous and thickness-controlled films in the nm range were obtained, with surface free energies lying between 15 and 70 mJ/m2. These results are discussed, together with those of DESI-MS on low-molecular-weight compounds such as melamine, tetracycline, and lincomycin, also taking into account the effects of the sprayer potential and its correlation with surface wettability. The results demonstrate that ion-formation efficiency is affected by surface wettability, and this was demonstrated operating above and below the onset of the electrospray.

  1. Investigation of an alternating current plasma as an element selective atomic emission detector for high-resolution capillary gas chromatography and as a source for atomic absorption and atomic emission spectrometry

    Science.gov (United States)

    Ombaba, Jackson M.

    This thesis deals with the construction and evaluation of an alternating current plasma (ACP) as an element-selective detector for high resolution capillary gas chromatography (GC) and as an excitation source for atomic absorption spectrometry (AAS) and atomic emission spectrometry (AES). The plasma, constrained in a quartz discharge tube at atmospheric pressure, is generated between two copper electrodes and utilizes helium as the plasma supporting gas. The alternating current plasma power source consists of a step-up transformer with a secondary output voltage of 14,000 V at a current of 23 mA. The device exhibits a stable signal because the plasma is self-seeding and reignites itself every half cycle. A tesla coil is not required to commence generation of the plasma if the ac voltage applied is greater than the breakdown voltage of the plasma-supporting gas. The chromatographic applications studied included the following: (1) the separation and selective detection of the organotin species, tributyltin chloride (TBT) and tetrabutyltin (TEBT), in environmental matrices including mussels (Mvutilus edullus) and sediment from Boston Harbor, industrial waste water and industrial sludge, and (2) the detection of methylcyclopentadienyl manganesetricarbonyl (MMT) and similar compounds used as gasoline additives. An ultrasonic nebulizer (common room humidifier) was utilized as a sample introduction device for aqueous solutions when the ACP was employed as an atomization source for atomic absorption spectrometry and as an excitation source for atomic emission spectrometry. Plasma diagnostic parameters studied include spatial electron number density across the discharge tube, electronic, excitation and ionization temperatures. Interference studies both in absorption and emission modes were also considered. Figures of merits of selected elements both in absorption and emission modes are reported. The evaluation of a computer-aided optimization program, Drylab GC, using

  2. Photoassisted vapor generation in the presence of organic acids for ultrasensitive determination of Se by electrothermal-atomic absorption spectrometry following headspace single-drop microextraction

    International Nuclear Information System (INIS)

    A method is described for the determination of selenium at the pg/mL level by electrothermal-atomic absorption spectrometry using in situ photogeneration of Se vapors, headspace sequestration onto an aqueous microdrop containing Pd(II) and subsequent injection in a graphite tube. Several organic acids (formic, oxalic, acetic, citric and ethylenediaminetetraacetic) have been tried for photoreduction of Se(IV) into volatile Se compounds under UV irradiation. Experimental variables such as UV irradiation time, organic acid concentration, Pd(II) concentration in the drop, sample and drop volumes, extraction time and pH were fully optimized. Low-molecular weight acids such as formic and acetic provided optimal photogeneration of volatile Se species at a 0.6 mol/L concentration. Citric and ethylenediaminetetraacetic acid allowed to use a concentration as low as 1 mmol/L, but extraction times were longer than for formic and acetic acids. Photogeneration of (CH3)2Se from Se(IV) in the presence of acetic acid provided a detection limit of 20 pg/mL, a preconcentration factor of nearly 285 and a precision, expressed as relative standard deviation, of 4%. Analytical performance seemed to depend not only on the photogeneration efficiency obtained with each acid but also on the stability of the vapors in the headspace. The method showed a high freedom from interferences caused by saline matrices, but interferences were observed for transition metals at a relatively low concentration

  3. Use of gradient dilution to flag and overcome matrix interferences in axial-viewing inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Despite the undisputed power of inductively coupled plasma-atomic emission spectrometry (ICP-AES), its users still face serious challenges in obtaining accurate analytical results. Matrix interference is perhaps the most important challenge. Dilution of a matrix-containing sample is a common practice to reduce matrix interference. However, determining the optimal dilution factor requires tedious and time-consuming offline sample preparation, since emission lines and the effect of matrix interferences are affected differently by the dilution. The current study exploits this difference by employing a high-performance liquid chromatography gradient pump prior to the nebulizer to perform on-line mixing of a sample solution and diluent. Linear gradient dilution is performed on both the calibration standard and the matrix-containing sample. By ratioing the signals from two emission lines (from the same or different elements) as a function of dilution factor, the analyst can not only identify the presence of a matrix interference, but also determine the optimal dilution factor needed to overcome the interference. A ratio that does not change with dilution signals the absence of a matrix interference, whereas a changing ratio indicates the presence of an interference. The point on the dilution profile where the ratio stabilizes indicates the optimal dilution factor to correct the interference. The current study was performed on axial-viewing ICP-AES with o-xylene as the solvent

  4. Separation and preconcentration of trace quantities of copper ion using modified alumina nanoparticles, and its determination by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    We report on a sensitive, reliable and relatively fast method for separation, preconcentration and determination of trace quantities of copper(II) ion. It is making use of nanometer-sized γ-alumina nanoparticles modified with sodium dodecyl sulfate (SDS). The adsorptive potential was assessed via a Langmuir isotherm and the maximal sorption capacity was found to be 138 mg g-1. The effects of pH values, amount of ligand, flow rate, type of eluting agent, volume of eluent, and the volume of sample were examined. The effects of interfering ions on the recovery of the analyte were also investigated. Copper ion was then determined by flame atomic absorption spectrometry. The relative standard deviation for five replicate determinations (at 50 μg L-1 of copper) is 3.3%. The detection limit (at 3 s) is 2.5 μg L-1. This method was validated with a certified reference material of oyster tissue (NIST SRM 1566b) and the results coincided well with the certified values. The procedure was successfully applied to the determination of Cu in water and food samples. (author)

  5. Graphene-based solid-phase extraction combined with flame atomic absorption spectrometry for a sensitive determination of trace amounts of lead in environmental water and vegetable samples.

    Science.gov (United States)

    Wang, Yukun; Gao, Shutao; Zang, Xiaohuan; Li, Jingci; Ma, Jingjun

    2012-02-24

    Graphene, a novel class of carbon nanostructures, has great promise for use as sorbent materials because of its ultrahigh specific surface area. A new method using a column packed with graphene as sorbent was developed for the preconcentration of trace amounts of lead (Pb) using dithizone as chelating reagent prior to its determination by flame atomic absorption spectrometry. Some effective parameters on the extraction and complex formation were selected and optimized. Under optimum conditions, the calibration graph was linear in the concentration range of 10.0-600.0 μg L(-1) with a detection limit of 0.61 μg L(-1). The relative standard deviation for ten replicate measurements of 20.0 and 400.0 μg L(-1) of Pb were 3.56 and 3.25%, respectively. Comparative studies showed that graphene is superior to other adsorbents including C18 silica, graphitic carbon, and single- and multi-walled carbon nanotubes for the extraction of Pb. The proposed method was successfully applied in the analysis of environmental water and vegetable samples. Good spiked recoveries over the range of 95.3-100.4% were obtained. This work not only proposes a useful method for sample preconcentration, but also reveals the great potential of graphene as an excellent sorbent material in analytical processes. PMID:22284885

  6. Ultrasound-assisted extraction technique for establishing selenium contents in breast cancer biopsies by Zeeman-electrothermal atomic absorption spectrometry using multi-injection

    International Nuclear Information System (INIS)

    A solid-liquid extraction method is developed to establish the contents of selenium in breast cancer biopsies. The method is based on the ultrasound-assisted extraction of selenium from pretreated biopsies prior to Se determination by atomic absorption spectrometry with longitudinal-Zeeman background correction. Fifty-one breast biopsies were collected from the Cies Hospital (Vigo, Spain), 32 of which correspond to tumor tissue and 19 to normal tissue (parenchyma). Difficulties arising from the samples analyzed, i.e. small samples mass (50-100 mg), extremely low Se contents and sample texture modification including tissue hardening due to formaldehyde preservation are addressed and overcome. High intensity sonication using a probe together with addition of hydrogen peroxide succeeded in completely extracting Se from biopsies. The multiple injection technique was useful to tackle the low Se contents present in some biopsies. The detection limit was 25 ng g-1 of Se and the precision, expressed as relative standard deviation, was less than 10%. Se contents ranged from 0.08 to 0.4 μg g-1 for parenchyma samples and from 0.09 to 0.8 μg g-1 for tumor samples. In general, Se levels in tumor biopsies were higher as compared with the adjacent normal tissue in 19 patients by a factor of up to 6. Analytical data confirmed Se accumulation in the breast tumors

  7. Ultrasound-assisted extraction technique for establishing selenium contents in breast cancer biopsies by Zeeman-electrothermal atomic absorption spectrometry using multi-injection

    Energy Technology Data Exchange (ETDEWEB)

    Lavilla, I. [Departamento de Quimica Analitica y Alimentaria, Facultad de Quimica, Universidad de Vigo, As Lagoas-Marcosende s/n, 36310 Vigo (Spain); Mosquera, A. [Departamento de Quimica Analitica y Alimentaria, Facultad de Quimica, Universidad de Vigo, As Lagoas-Marcosende s/n, 36310 Vigo (Spain); Millos, J. [Centro de Apoyo Cientifico y Tecnologico a la Investigacion, Universidad de Vigo (Spain); Cameselle, J. [Complejo Hospitalario Xeral-Cies, Pizarro 22, 36311 Vigo (Spain); Bendicho, C. [Departamento de Quimica Analitica y Alimentaria, Facultad de Quimica, Universidad de Vigo, As Lagoas-Marcosende s/n, 36310 Vigo (Spain)]. E-mail: bendicho@uviqo.es

    2006-04-27

    A solid-liquid extraction method is developed to establish the contents of selenium in breast cancer biopsies. The method is based on the ultrasound-assisted extraction of selenium from pretreated biopsies prior to Se determination by atomic absorption spectrometry with longitudinal-Zeeman background correction. Fifty-one breast biopsies were collected from the Cies Hospital (Vigo, Spain), 32 of which correspond to tumor tissue and 19 to normal tissue (parenchyma). Difficulties arising from the samples analyzed, i.e. small samples mass (50-100 mg), extremely low Se contents and sample texture modification including tissue hardening due to formaldehyde preservation are addressed and overcome. High intensity sonication using a probe together with addition of hydrogen peroxide succeeded in completely extracting Se from biopsies. The multiple injection technique was useful to tackle the low Se contents present in some biopsies. The detection limit was 25 ng g{sup -1} of Se and the precision, expressed as relative standard deviation, was less than 10%. Se contents ranged from 0.08 to 0.4 {mu}g g{sup -1} for parenchyma samples and from 0.09 to 0.8 {mu}g g{sup -1} for tumor samples. In general, Se levels in tumor biopsies were higher as compared with the adjacent normal tissue in 19 patients by a factor of up to 6. Analytical data confirmed Se accumulation in the breast tumors.

  8. A Green Preconcentration Method for Determination of Cobalt and Lead in Fresh Surface and Waste Water Samples Prior to Flame Atomic Absorption Spectrometry

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem Gul; Shah, Faheem; Afridi, Hassan Imran; Khan, Sumaira; Arian, Sadaf Sadia; Brahman, Kapil Dev

    2012-01-01

    Cloud point extraction (CPE) has been used for the preconcentration and simultaneous determination of cobalt (Co) and lead (Pb) in fresh and wastewater samples. The extraction of analytes from aqueous samples was performed in the presence of 8-hydroxyquinoline (oxine) as a chelating agent and Triton X-114 as a nonionic surfactant. Experiments were conducted to assess the effect of different chemical variables such as pH, amounts of reagents (oxine and Triton X-114), temperature, incubation time, and sample volume. After phase separation, based on the cloud point, the surfactant-rich phase was diluted with acidic ethanol prior to its analysis by the flame atomic absorption spectrometry (FAAS). The enhancement factors 70 and 50 with detection limits of 0.26 μg L−1 and 0.44 μg L−1 were obtained for Co and Pb, respectively. In order to validate the developed method, a certified reference material (SRM 1643e) was analyzed and the determined values obtained were in a good agreement with the certified values. The proposed method was applied successfully to the determination of Co and Pb in a fresh surface and waste water sample. PMID:23227429

  9. Investigation of novel rapidly synergistic cloud point extraction pattern for bismuth in water and geological samples coupling with flame atomic absorption spectrometry determination

    Science.gov (United States)

    Wen, Xiaodong; Zhao, Yu; Deng, Qingwen; Ji, Shoulian; Zhao, Xia; Guo, Jie

    2012-04-01

    Rapidly synergistic cloud point extraction (RS-CPE) greatly simplified and accelerated the procedure of traditional cloud point extraction (CPE). In order to expand the application of RS-CPE, this work was carried out after the establishment of the improved extraction technique. The new established extraction method was firstly applied for bismuth extraction and determination coupled with flame atomic absorption spectrometry (FAAS) in this work. The improved RS-CPE was accomplished in the room temperature in 1 min. Non-ionic surfactant Triton X-100 (TX-100) was used as extractant. Octanol worked as cloud point revulsant and synergic reagent. TX-100 has a relatively high cloud point temperature (CPT), which limited its application in CPE. In this work, TX-100 accomplished the RS-CPE procedure in room temperature successfully. The factors influencing RS-CPE, such as concentrations of reagents, pH, conditions of phase separation, effect of environmental temperatures, salt effect and instrumental conditions, were studied systematically. Under the optimal conditions, the limit of detection (LOD) for bismuth was 4.0 μg L-1, with sensitivity enhancement factor (EF) of 43. The proposed method greatly improved the sensitivity of FAAS for the determination of bismuth and was applied to the determination of trace bismuth in real and certified samples with satisfactory analytical results. The proposed method was rapid, simple, and sensitive.

  10. Cloud point extraction for the determination of lead and cadmium in urine by graphite furnace atomic absorption spectrometry with multivariate optimization using Box-Behnken design

    Energy Technology Data Exchange (ETDEWEB)

    Maranhao, Tatiane de A; Martendal, Edmar; Borges, Daniel L.G.; Carasek, Eduardo [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Welz, Bernhard [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Grupo de Pesquisa em Quimica Analitica, Instituto de Quimica, Universidade Federal da Bahia, 40170-290, Salvador, BA (Brazil); Curtius, Adilson J. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil)], E-mail: curtius@qmc.ufsc.br

    2007-09-15

    Cloud point extraction (CPE) is proposed as a pre-concentration procedure for the determination of Pb and Cd in undigested urine by graphite furnace atomic absorption spectrometry (GF AAS). Aliquots of 0.5 mL urine were acidified with HCl and the chelating agent ammonium O,O-diethyl dithiophosphate (DDTP) was added along with the non-ionic surfactant Triton X-114 at the optimized concentrations. Phase separation was achieved by heating the mixture to 50 deg. C for 15 min. The surfactant-rich phase was analyzed by GF AAS, employing the optimized pyrolysis temperatures of 900 deg. C for Pb and 800 deg. C for Cd, using a graphite tube with a platform treated with 500 {mu}g Ru as permanent modifier. The reagent concentrations for CPE (HCl, DDTP and Triton X-114) were optimized using a Box-Behnken design. The response surfaces and the optimum values were very similar for aqueous solutions and for the urine samples, demonstrating that aqueous standards submitted to CPE could be used for calibration. Detection limits of 40 and 2 ng L{sup -1} for Pb and Cd, respectively, were obtained along with an enhancement factor of 16 for both analytes. Three control urine samples were analyzed using this approach, and good agreement was obtained at a 95% statistical confidence level between the certified and determined values. Five real samples have also been analyzed before and after spiking with Pb and Cd, resulting in recoveries ranging from 97 to 118%.

  11. Cloud point extraction for the determination of lead and cadmium in urine by graphite furnace atomic absorption spectrometry with multivariate optimization using Box Behnken design

    Science.gov (United States)

    Maranhão, Tatiane De A.; Martendal, Edmar; Borges, Daniel L. G.; Carasek, Eduardo; Welz, Bernhard; Curtius, Adilson J.

    2007-09-01

    Cloud point extraction (CPE) is proposed as a pre-concentration procedure for the determination of Pb and Cd in undigested urine by graphite furnace atomic absorption spectrometry (GF AAS). Aliquots of 0.5 mL urine were acidified with HCl and the chelating agent ammonium O,O-diethyl dithiophosphate (DDTP) was added along with the non-ionic surfactant Triton X-114 at the optimized concentrations. Phase separation was achieved by heating the mixture to 50 °C for 15 min. The surfactant-rich phase was analyzed by GF AAS, employing the optimized pyrolysis temperatures of 900 °C for Pb and 800 °C for Cd, using a graphite tube with a platform treated with 500 μg Ru as permanent modifier. The reagent concentrations for CPE (HCl, DDTP and Triton X-114) were optimized using a Box Behnken design. The response surfaces and the optimum values were very similar for aqueous solutions and for the urine samples, demonstrating that aqueous standards submitted to CPE could be used for calibration. Detection limits of 40 and 2 ng L- 1 for Pb and Cd, respectively, were obtained along with an enhancement factor of 16 for both analytes. Three control urine samples were analyzed using this approach, and good agreement was obtained at a 95% statistical confidence level between the certified and determined values. Five real samples have also been analyzed before and after spiking with Pb and Cd, resulting in recoveries ranging from 97 to 118%.

  12. Determination of total Sb,Se Te, and Bi and evaluation of their inorganic species in garlic by hydride-generation-atomic-fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Matos Reyes, M.N.; Cervera, M.L.; Guardia, M. de la [University of Valencia, Department of Analytical Chemistry, Burjassot, Valencia (Spain)

    2009-07-15

    A sensitive and simple analytical method has been developed for determination of Sb(III), Sb(V), Se(IV), Se(VI), Te(IV), Te(VI), and Bi(III) in garlic samples by using hydride-generation-atomic-fluorescence spectrometry (HG-AFS). The method is based on a single extraction of the inorganic species by sonication at room temperature with 1 mol L{sup -1} H{sub 2}SO{sub 4} and washing of the solid phase with 0.1% (w/v) EDTA, followed by measurement of the corresponding hydrides generated under two different experimental conditions directly and after a pre-reduction step. The limit of detection of the method was 0.7 ng g{sup -1} for Sb(III), 1.0 ng g{sup -1} for Sb(V), 1.3 ng g{sup -1} for Se(IV), 1.0 ng g{sup -1} for Se(VI), 1.1 ng g{sup -1} for Te(IV), 0.5 ng g{sup -1} for Te(VI), and 0.9 ng g{sup -1} for Bi(III), in all cases expressed in terms of sample dry weight. (orig.)

  13. Accuracy of a method based on atomic absorption spectrometry to determine inorganic arsenic in food: Outcome of the collaborative trial IMEP-41.

    Science.gov (United States)

    Fiamegkos, I; Cordeiro, F; Robouch, P; Vélez, D; Devesa, V; Raber, G; Sloth, J J; Rasmussen, R R; Llorente-Mirandes, T; Lopez-Sanchez, J F; Rubio, R; Cubadda, F; D'Amato, M; Feldmann, J; Raab, A; Emteborg, H; de la Calle, M B

    2016-12-15

    A collaborative trial was conducted to determine the performance characteristics of an analytical method for the quantification of inorganic arsenic (iAs) in food. The method is based on (i) solubilisation of the protein matrix with concentrated hydrochloric acid to denature proteins and allow the release of all arsenic species into solution, and (ii) subsequent extraction of the inorganic arsenic present in the acid medium using chloroform followed by back-extraction to acidic medium. The final detection and quantification is done by flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS). The seven test items used in this exercise were reference materials covering a broad range of matrices: mussels, cabbage, seaweed (hijiki), fish protein, rice, wheat, mushrooms, with concentrations ranging from 0.074 to 7.55mgkg(-1). The relative standard deviation for repeatability (RSDr) ranged from 4.1 to 10.3%, while the relative standard deviation for reproducibility (RSDR) ranged from 6.1 to 22.8%. PMID:27451169

  14. A Green Preconcentration Method for Determination of Cobalt and Lead in Fresh Surface and Waste Water Samples Prior to Flame Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    Naeemullah

    2012-01-01

    Full Text Available Cloud point extraction (CPE has been used for the preconcentration and simultaneous determination of cobalt (Co and lead (Pb in fresh and wastewater samples. The extraction of analytes from aqueous samples was performed in the presence of 8-hydroxyquinoline (oxine as a chelating agent and Triton X-114 as a nonionic surfactant. Experiments were conducted to assess the effect of different chemical variables such as pH, amounts of reagents (oxine and Triton X-114, temperature, incubation time, and sample volume. After phase separation, based on the cloud point, the surfactant-rich phase was diluted with acidic ethanol prior to its analysis by the flame atomic absorption spectrometry (FAAS. The enhancement factors 70 and 50 with detection limits of 0.26 μg L−1 and 0.44 μg L−1 were obtained for Co and Pb, respectively. In order to validate the developed method, a certified reference material (SRM 1643e was analyzed and the determined values obtained were in a good agreement with the certified values. The proposed method was applied successfully to the determination of Co and Pb in a fresh surface and waste water sample.

  15. Preconcentration of lead, cadmium and zinc on silica gel loaded with diethyldithiocarbamate prior to their determination by flame-atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Rio-Segade, S. [Dept. de Quimica Analitica y Alimentaria, Univ. de Vigo, Orense (Spain); Perez-Cid, B. [Dept. de Quimica Analitica y Alimentaria, Univ. de Vigo, Orense (Spain); Bendicho, C. [Dept. de Quimica Analitica y Alimentaria, Univ. de Vigo, Orense (Spain)

    1995-04-01

    A silica gel sorbent loaded with sodium diethyldithiocarbamate has been developed for the preconcentration of lead, cadmium and zinc prior to their determination by flame-atomic absorption spectrometry (FAAS). The sorption and desorption of the metal ions was studied under both static and dynamic conditions. The metal ions were quantitatively retained on the silica gel sorbent based on an equilibrium time of less than 1 min. In case of the batch method, the effects of pH, shaking time, amount of sorbent, and desorption time were investigated. Among the desorption agents studied, only EDTA in ammonium chloride/ammonia buffer yielded quantitative recoveries. Freundlich`s sorption isotherms determined for each metal show that sufficient sorption ability is obtained. The column method allows the preconcentration of metal ions from large sample volumes (e.g. 200 mL) using a flow rate of 5 mL min{sup -1}. The influence of foreign ions present in natural waters and saline solutions was examined. The reproducibility of the total analytical method, expressed as relative standard deviation (RSD) is 1.8, 0.5 and 0.6%, for lead, cadmium and zinc, respectively. (orig.)

  16. Investigation of novel rapidly synergistic cloud point extraction pattern for bismuth in water and geological samples coupling with flame atomic absorption spectrometry determination.

    Science.gov (United States)

    Wen, Xiaodong; Zhao, Yu; Deng, Qingwen; Ji, Shoulian; Zhao, Xia; Guo, Jie

    2012-04-01

    Rapidly synergistic cloud point extraction (RS-CPE) greatly simplified and accelerated the procedure of traditional cloud point extraction (CPE). In order to expand the application of RS-CPE, this work was carried out after the establishment of the improved extraction technique. The new established extraction method was firstly applied for bismuth extraction and determination coupled with flame atomic absorption spectrometry (FAAS) in this work. The improved RS-CPE was accomplished in the room temperature in 1 min. Non-ionic surfactant Triton X-100 (TX-100) was used as extractant. Octanol worked as cloud point revulsant and synergic reagent. TX-100 has a relatively high cloud point temperature (CPT), which limited its application in CPE. In this work, TX-100 accomplished the RS-CPE procedure in room temperature successfully. The factors influencing RS-CPE, such as concentrations of reagents, pH, conditions of phase separation, effect of environmental temperatures, salt effect and instrumental conditions, were studied systematically. Under the optimal conditions, the limit of detection (LOD) for bismuth was 4.0 μg L(-1), with sensitivity enhancement factor (EF) of 43. The proposed method greatly improved the sensitivity of FAAS for the determination of bismuth and was applied to the determination of trace bismuth in real and certified samples with satisfactory analytical results. The proposed method was rapid, simple, and sensitive.

  17. Magnetic stirrer induced dispersive ionic-liquid microextraction for the determination of vanadium in water and food samples prior to graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem Gul; Tuzen, Mustafa

    2015-04-01

    A new dispersive liquid-liquid microextraction, magnetic stirrer induced dispersive ionic-liquid microextraction (MS-IL-DLLME) was developed to quantify the trace level of vanadium in real water and food samples by graphite furnace atomic absorption spectrometry (GFAAS). In this extraction method magnetic stirrer was applied to obtained a dispersive medium of 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM][PF6] in aqueous solution of (real water samples and digested food samples) to increase phase transfer ratio, which significantly enhance the recovery of vanadium - 4-(2-pyridylazo) resorcinol (PAR) chelate. Variables having vital role on desired microextraction methods were optimised to obtain the maximum recovery of study analyte. Under the optimised experimental variables, enhancement factor (EF) and limit of detection (LOD) were achieved to be 125 and 18 ng L(-1), respectively. Validity and accuracy of the desired method was checked by analysis of certified reference materials (SLRS-4 Riverine water and NIST SRM 1515 Apple leaves). The relative standard deviation (RSD) for 10 replicate determinations at 0.5 μg L(-1) of vanadium level was found to be food samples.

  18. Atomic Mineral Characteristics of Indonesian Osteoporosis by High-Resolution Inductively Coupled Plasma Mass Spectrometry

    OpenAIRE

    Zairin Noor; Sutiman Bambang Sumitro; Mohammad Hidayat; Agus Hadian Rahim; Akhmad Sabarudin; Tomonari Umemura

    2012-01-01

    Clinical research indicates that negative calcium balance is associated with low bone mass, rapid bone loss, and high fracture rates. However, some studies revealed that not only calcium is involved in bone strengthening as risk factor of fracture osteoporosis. Thus, in this report, the difference of metallic and nonmetallic elements in osteoporosis and normal bones was studied by high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). The influence of these elements on bone...

  19. Determination of Ultratrace Amounts of Copper(Ⅱ) in Water Samples by Electrothermal Atomic Absorption Spectrometry After Cloud Point Extraction

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    A novel approach was developed for the determination of ultratrace amounts of copper in water samples by using electrothermal atomic absorption spectrometry (ETAAS) after cloud point extraction (CPE). 1-( 2-Pyridylazo)-2-naphthol was used as the chelating reagent and Triton X-114 as the micellar-forming surfactant. CPE was conducted in a pH 8.0 medium at 40 ℃ for 10 min. After the separation of the phases by centrifugation, the surfactant-rich phase was diluted with 1 mL of a methanol solution of 0. 1 mol/L HNO3. Then 20 μL of the diluted surfactant-rich phase was injected into the graphite furnace for atomization in the absence of any matrix modifier. Various experimental conditions that affect the extraction and atomization processes were optimized. A detection limit of 5 ng/L was obtained after preconcentration. The linear dynamic range of the copper mass concentration was found to be 0-2.0ng/mL, and the relative standard deviation was found to be less than 3.1% for a sample containing 1.0 ng/mL Cu(Ⅱ). This developed method was successfully applied to the determination of ultratrace amounts of Cu in drinking water, tap water, and seawater samples.

  20. 原子荧光光谱法测定土壤中的砷含量%Determination of Arsenic in Soil by Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    刘燕芬

    2015-01-01

    通过结合具体的试验对运用原子荧光光谱法测定土壤中的砷含量进行了探讨,以期能为有关方面的需要提供有益的参考和借鉴。%In order to provide a useful reference for the relevant aspects of the arsenic content in soil by atomic fluorescence spectrometry, the method of atomic fluorescence spectrometry was used to determine the arsenic content in soil.

  1. Separation and preconcentration of ultra trace amounts of beryllium in water samples using mixed micelle-mediated extraction and determination by inductively coupled plasma-atomic emission spectrometry.

    Science.gov (United States)

    Beiraghi, Assadollah; Babaee, Saeed

    2008-01-28

    In the present study a cloud point extraction process using mixed micelle of the cationic surfactant cetyl-pyridinium chloride (CPC) and non-ionic surfactant Triton X-114 for extraction of beryllium from aqueous solutions is developed. The extraction of analyte from aqueous samples was performed in the presence of 1,8-dihydroxyanthrone as chelating agent in buffer media of pH 9.5. After phase separation, the surfactant-rich phase was diluted with 0.4mL of a 60:40 methanol-water mixture containing 0.03 mL HNO(3). Then, the enriched analyte in the surfactant-rich phase was determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The different variables affecting the complexation and extraction conditions were optimized. Under the optimum conditions (i.e. 1.6 x 10(-4) molL(-1) 1,8-dihydroxyanthrone, 1.2 x 10(-4) molL(-1) CPC, 0.15% (v/v) Triton X-114, 50 degrees C equilibrium temperature) the calibration graph was linear in the range of 0.006-80 ngmL(-1) with detection limit of 0.001 ngmL(-1) and the precision (R.S.D.%) for five replicate determinations at 18 ngmL(-1) of Be(II) was better than 2.9%. In this manner the preconcentration and enrichment factors were 16.7 and 24.8, respectively. Under the presence of foreign ions no significant interference was observed. Finally, the proposed method was successfully utilized for the determination of this cation in water samples.

  2. Separation and preconcentration of ultra trace amounts of beryllium in water samples using mixed micelle-mediated extraction and determination by inductively coupled plasma-atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Beiraghi, Assadollah [Faculty of Chemistry, Tarbiat Moallem University, Mofatteh Avenue, No. 49, P.O. Box 15614, Tehran (Iran, Islamic Republic of)], E-mail: Beiraghi@Saba.tmu.ac.ir; Babaee, Saeed [Faculty of Chemistry, Tarbiat Moallem University, Mofatteh Avenue, No. 49, P.O. Box 15614, Tehran (Iran, Islamic Republic of)

    2008-01-28

    In the present study a cloud point extraction process using mixed micelle of the cationic surfactant cetyl-pyridinium chloride (CPC) and non-ionic surfactant Triton X-114 for extraction of beryllium from aqueous solutions is developed. The extraction of analyte from aqueous samples was performed in the presence of 1,8-dihydroxyanthrone as chelating agent in buffer media of pH 9.5. After phase separation, the surfactant-rich phase was diluted with 0.4 mL of a 60:40 methanol-water mixture containing 0.03 mL HNO{sub 3}. Then, the enriched analyte in the surfactant-rich phase was determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The different variables affecting the complexation and extraction conditions were optimized. Under the optimum conditions (i.e. 1.6 x 10{sup -4} mol L{sup -1} 1,8-dihydroxyanthrone, 1.2 x 10{sup -4} mol L{sup -1} CPC, 0.15% (v/v) Triton X-114, 50 deg. C equilibrium temperature) the calibration graph was linear in the range of 0.006-80 ng mL{sup -1} with detection limit of 0.001 ng mL{sup -1} and the precision (R.S.D.%) for five replicate determinations at 18 ng mL{sup -1} of Be(II) was better than 2.9%. In this manner the preconcentration and enrichment factors were 16.7 and 24.8, respectively. Under the presence of foreign ions no significant interference was observed. Finally, the proposed method was successfully utilized for the determination of this cation in water samples.

  3. Activated carbon-modified knotted reactor coupled to electrothermal atomic absorption spectrometry for sensitive determination of arsenic species in medicinal herbs and tea infusions

    Energy Technology Data Exchange (ETDEWEB)

    Grijalba, Alexander Castro; Martinis, Estefanía M. [Laboratory of Analytical Chemistry for Research and Development (QUIANID), Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Cuyo, Padre J. Contreras 1300, (5500) Mendoza (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Buenos Aires (Argentina); Lascalea, Gustavo E. [Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Buenos Aires (Argentina); Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar [Laboratory of Analytical Chemistry for Research and Development (QUIANID), Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Cuyo, Padre J. Contreras 1300, (5500) Mendoza (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Buenos Aires (Argentina)

    2015-01-01

    A flow injection system based on a modified polytetrafluoroethylene (PTFE) knotted reactor (KR) was developed for arsenite [As(III)] and arsenate [As(V)] species preconcentration and determination by electrothermal atomic absorption spectrometry (ETAAS). Activated carbon (AC) was immobilized on the inner walls of a PTFE KR by a thermal treatment. A significant increase in analyte retention was obtained with the AC-modified KR (100%) as compared to the regular PTFE KR (25%). The preconcentration method involved the on-line formation of As(III)-ammonium pyrrolidinedithiocarbamate (As-APDC) complex, followed by its adsorption onto the inner walls of the AC-modified KR. After analyte retention, the complex was eluted with acetone directly into the graphite furnace of ETAAS. The parameters affecting the flow injection system were evaluated with a full central composite face centered design with three center points. Under optimum conditions, a preconcentration factor of 200 was obtained with 10 ml of sample. The detection limit was 4 ng L{sup −1} and the relative standard deviation (RSD) for six replicate measurements at 0.2 μg L{sup −1} of As were 4.3% and 4.7% for As(III) and As(V), respectively. The developed methodology was highly selective towards As(III), while As(V), monomethylarsonic acid [MMA(V)] and dimethylarsinic [DMA(V)] were not retained in the AC-modified KR. The proposed method was successfully applied for As speciation analysis in infusions originated from medicinal herbs and tea. - Highlights: • We report an efficient method for As speciation. • We have modified a knotted reactor with activated carbon for high sorption capacity. • We provide a simple procedure for surface modification of a PTFE knotted reactor. • We have selectively separated inorganic As species from complex matrix samples. • We have implemented a modified KR in a flow injection system coupled to ETAAS.

  4. Methylmercury in water samples at the pg/L level by online preconcentration liquid chromatography cold vapor-atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Brombach, Christoph-Cornelius [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom); Chen, Bin; Corns, Warren T. [PS Analytical, Arthur House, Crayfields Industrial Estate, Main Road, Orpington, Kent BR5 3HP (United Kingdom); Feldmann, Jörg [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom); Krupp, Eva M., E-mail: e.krupp@abdn.ac.uk [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom)

    2015-03-01

    Ultra-traces of methylmercury at the sub-ppt level can be magnified in the foodweb and is of concern. In environmental monitoring a routine robust analytical method is needed to determine methylmercury in water. The development of an analytical method for ultra-trace speciation analysis of methylmercury (MeHg) in water samples is described. The approach is based on HPLC-CV-AFS with on-line preconcentration of water samples up to 200 mL, resulting in a detection limit of 40 pg/L (ppq) for MeHg, expressed as Hg. The unit consists of an optimized preconcentration column filled with a sulfur-based sorption material, on which mercury species are preconcentrated and subsequently eluted, separated and detected via HPLC-CV-AFS (high performance liquid chromatography–cold vapor atomic fluorescence spectrometry). During the method development a type of adsorbate material, the pH dependence, the sample load rate and the carry-over were investigated using breakthrough experiments. The method shows broad pH stability in the range of pH 0 to 7, without the need for buffer addition and shows limited matrix effects so that MeHg is quantitatively recovered from sewage, river and seawater directly in the acidified samples without sample preparation. - Highlights: • We demonstrate that a novel mixture of thiourea-thiolsilica shows an excellent trapping of MeHg between a broad pH range 1–6. • We develop the method so that it can potentially be automated for inorganic and methyl-mercury. • The method is matrix independent with highly accurate results for MeHg in hair CRM extracts and spiked water samples • The limit of detection is around 40 pg/L when just 200 mL sample is used, without any intensive preparation.

  5. Simple hollow fiber renewal liquid membrane extraction method for pre-concentration of Cd(II) in environmental samples and detection by Flame Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    A hollow fiber renewal liquid membrane (HFRLM) extraction method to determine cadmium (II) in water samples using Flame Atomic Absorption Spectrometry (FAAS) was developed. Ammonium O,O-diethyl dithiophosphate (DDTP) was used to complex cadmium (II) in an acid medium to obtain a neutral hydrophobic complex (ML2). The organic solvent introduced to the sample extracts this complex from the aqueous solution and carries it over the poly(dimethylsiloxane) (PDMS) membrane, that had their walls previously filled with the same organic solvent. The organic solvent is solubilized inside the PDMS membrane, leading to a homogeneous phase. The complex strips the lumen of the membrane where, at higher pH, the complex Cd-DDTP is broken down and cadmium (II) is released into the stripping phase. EDTA was used to complex the cadmium (II), helping to trap the analyte in the stripping phase. A multivariate procedure was used to optimize the studied variables. The optimized variables were: sample (donor phase) pH 3.25, DDTP concentration 0.05% (m/v), stripping (acceptor phase) pH 8.75, EDTA concentration 1.5 x 10-2 mol L-1, extraction temperature 40 deg. C, extraction time 40 min, a solvent mixture N-butyl acetate and hexane (60/40%, v/v) with a volume of 100 μL, and addition of ammonium sulfate to saturate the sample. The sample volume used was 20 mL and the stripping volume was 165 μL. The analyte enrichment factor was 120, limit of detection (LOD) 1.3 μg L-1, relative standard deviation (RSD) 5.5% and the working linear range 2-30 μg L-1.

  6. Ambient-Temperature Trap/Release of Arsenic by Dielectric Barrier Discharge and Its Application to Ultratrace Arsenic Determination in Surface Water Followed by Atomic Fluorescence Spectrometry.

    Science.gov (United States)

    Mao, Xuefei; Qi, Yuehan; Huang, Junwei; Liu, Jixin; Chen, Guoying; Na, Xing; Wang, Min; Qian, Yongzhong

    2016-04-01

    A novel dielectric barrier discharge reactor (DBDR) was utilized to trap/release arsenic coupled to hydride generation atomic fluorescence spectrometry (HG-AFS). On the DBD principle, the precise and accurate control of trap/release procedures was fulfilled at ambient temperature, and an analytical method was established for ultratrace arsenic in real samples. Moreover, the effects of voltage, oxygen, hydrogen, and water vapor on trapping and releasing arsenic by DBDR were investigated. For trapping, arsenic could be completely trapped in DBDR at 40 mL/min of O2 input mixed with 600 mL/min Ar carrier gas and 9.2 kV discharge potential; prior to release, the Ar carrier gas input should be changed from the upstream gas liquid separator (GLS) to the downstream GLS and kept for 180 s to eliminate possible water vapor interference; for arsenic release, O2 was replaced by 200 mL/min H2 and discharge potential was adjusted to 9.5 kV. Under optimized conditions, arsenic could be detected as low as 1.0 ng/L with an 8-fold enrichment factor; the linearity of calibration reached R(2) > 0.995 in the 0.05 μg/L-5 μg/L range. The mean spiked recoveries for tap, river, lake, and seawater samples were 98% to 103%; and the measured values of the CRMs including GSB-Z50004-200431, GBW08605, and GBW(E)080390 were in good agreement with the certified values. These findings proved the feasibility of DBDR as an arsenic preconcentration tool for atomic spectrometric instrumentation and arsenic recycling in industrial waste gas discharge. PMID:26976077

  7. Direct determination of chromium in infant formulas employing high-resolution continuum source electrothermal atomic absorption spectrometry and solid sample analysis.

    Science.gov (United States)

    Silva, Arlene S; Brandao, Geovani C; Matos, Geraldo D; Ferreira, Sergio L C

    2015-11-01

    The present work proposed an analytical method for the direct determination of chromium in infant formulas employing the high-resolution continuum source electrothermal atomic absorption spectrometry combined with the solid sample analysis (SS-HR-CS ET AAS). Sample masses up to 2.0mg were directly weighted on a solid sampling platform and introduced into the graphite tube. In order to minimize the formation of carbonaceous residues and to improve the contact of the modifier solution with the solid sample, a volume of 10 µL of a solution containing 6% (v/v) H2O2, 20% (v/v) ethanol and 1% (v/v) HNO3 was added. The pyrolysis and atomization temperatures established were 1600 and 2400 °C, respectively, using magnesium as chemical modifier. The calibration technique was evaluated by comparing the slopes of calibration curves established using aqueous and solid standards. This test revealed that chromium can be determined employing the external calibration technique using aqueous standards. Under these conditions, the method developed allows the direct determination of chromium with limit of quantification of 11.5 ng g(-1), precision expressed as relative standard deviation (RSD) in the range of 4.0-17.9% (n=3) and a characteristic mass of 1.2 pg of chromium. The accuracy was confirmed by analysis of a certified reference material of tomato leaves furnished by National Institute of Standards and Technology. The method proposed was applied for the determination of chromium in five different infant formula samples. The chromium content found varied in the range of 33.9-58.1 ng g(-1) (n=3). These samples were also analyzed employing ICP-MS. A statistical test demonstrated that there is no significant difference between the results found by two methods. The chromium concentrations achieved are lower than the maximum limit permissible for chromium in foods by Brazilian Legislation.

  8. Peat as a natural solid-phase for copper preconcentration and determination in a multicommuted flow system coupled to flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Gonzales, A.P.S. [Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adelia, 166, 09210-170 Santo Andre (Brazil); Firmino, M.A. [Departamento de Engenharia de Materiais, Escola de Engenharia, Universidade Presbiteriana Mackenzie, Rua da Consolacao, 930, 01302-970 Sao Paulo (Brazil); Nomura, C.S. [Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adelia, 166, 09210-170 Santo Andre (Brazil); Rocha, F.R.P.; Oliveira, P.V. [Departamento de Quimica Fundamental, Instituto de Quimica, Universidade de Sao Paulo, Av. Prof. Lineu Prestes, 748, 05508-000 Sao Paulo (Brazil); Gaubeur, I. [Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adelia, 166, 09210-170 Santo Andre (Brazil)], E-mail: ivanise.gaubeur@ufabc.edu.br

    2009-03-23

    The physical and chemical characteristics of peat were assessed through measurement of pH, percentage of organic matter, cationic exchange capacity (CEC), elemental analysis, infrared spectroscopy and quantitative analysis of metals by ICP OES. Despite the material showed to be very acid in view of the percentage of organic matter, its CEC was significant, showing potential for retention of metal ions. This characteristic was exploited by coupling a peat mini-column to a flow system based on the multicommutation approach for the in-line copper concentration prior to flame atomic absorption spectrometric determination. Cu(II) ions were adsorbed at pH 4.5 and eluted with 0.50 mol L{sup -1} HNO{sub 3}. The influence of chemical and hydrodynamic parameters, such as sample pH, buffer concentration, eluent type and concentration, sample flow-rate and preconcentration time were investigated. Under the optimized conditions, a linear response was observed between 16 and 100 {mu}g L{sup -1}, with a detection limit estimated as 3 {mu}g L{sup -1} at the 99.7% confidence level and an enrichment factor of 16. The relative standard deviation was estimated as 3.3% (n = 20). The mini-column was used for at least 100 sampling cycles without significant variation in the analytical response. Recoveries from copper spiked to lake water or groundwater as well as concentrates used in hemodialysis were in the 97.3-111% range. The results obtained for copper determination in these samples agreed with those achieved by graphite furnace atomic absorption spectrometry (GFAAS) at the 95% confidence level.

  9. Coprecipitation of trace amounts of silicon with aluminum hydroxide and the determination by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Ardeshir Shokrollahi

    2014-01-01

    Full Text Available A simple preconcentration method of silicon based on coprecipitation with aluminum hydroxide prior to its flame atomic absorption (FAAS determination was established. The recovery values of analyte ion was higher than 95%. The parameters including types of hydroxide ion source for precipitation, acid type for dissolution step, amount of aluminum ion as collector, pH, temperature, standing and centrifuge time, and sample volume were optimized for the quantitative recovery of the analyte. The influences of matrix ions were also examined. The relative standard deviation was found to be 3.2%. The limit of detection was calculated as (0.1 mg L-1. The preconcentration factor is 100 for (200 mL solution. The proposed method was successfully applied for the determination of silicon in some water and alloy samples.

  10. Determination of Mercury in Milk by Cold Vapor Atomic Fluorescence: A Green Analytical Chemistry Laboratory Experiment

    Science.gov (United States)

    Armenta, Sergio; de la Guardia, Miguel

    2011-01-01

    Green analytical chemistry principles were introduced to undergraduate students in a laboratory experiment focused on determining the mercury concentration in cow and goat milk. In addition to traditional goals, such as accuracy, precision, sensitivity, and limits of detection in method selection and development, attention was paid to the…

  11. Atoms

    Institute of Scientific and Technical Information of China (English)

    刘洪毓

    2007-01-01

    Atoms(原子)are all around us.They are something like the bricks (砖块)of which everything is made. The size of an atom is very,very small.In just one grain of salt are held millions of atoms. Atoms are very important.The way one object acts depends on what

  12. Electron impact ionization and excitation of laser-excited atoms: investigation by means of electron spectrometry

    International Nuclear Information System (INIS)

    We have measured the electron spectra following the excitation and ionization of laser-excited atoms by impact of 1.5 keV electrons: 2p excitation and 2s ionization of Na(3p3/2), 1s excitation of Li(2p3/2) and 5p ionization of Ba(6s5d 1,3D). Except for Ba the intensities of ejected electrons are directly proportional to the cross sections of Auger and autoionizing states. Theoretical excitation cross sections (Na 2p, Li 1s) are obtained in first Born approximation including the full relaxation of the atomic electrons. Relative ionization cross sections (Na 2s, Ba 5p) are evaluated in sudden approximation as a two-step process: pure 2s(5p) ionization plus relaxation of the rest of the atomic electrons. The experimental spectra are compared to theoretical spectra

  13. Feasibility guidelines for kaonic-atom experiments with ultra-high-resolution X-ray spectrometry

    CERN Document Server

    Friedman, E

    2013-01-01

    Recent studies of strong interaction effects in kaonic atoms suggest that analysing so-called `lower' and `upper' levels in the same atom could separate one-nucleon absorption from multinucleon processes. The present work examines the feasibility of direct measurements of upper level widths in addition to lower level widths in future experiments, using superconducting microcalorimeter detectors. About ten elements are identified as possible candidates for such experiments, all of medium-weight and heavy nuclei. New experiments focused on achieving good accuracy for widths of such pairs of levels could contribute significantly to our knowledge of the $K^-$-nucleon interaction in the nuclear medium.

  14. New analytical LC-mass spectrometry methodologies for the quali-quantitative determination of natural substances and drugs in complex matrices

    OpenAIRE

    Spinozzi, Silvia

    2015-01-01

    This thesis reports an integrated analytical and physicochemical approach for the study of natural substances and new drugs based on mass spectrometry techniques combined with liquid chromatography. In particular, Chapter 1 concerns the study of Berberine a natural substance with pharmacological activity for the treatment of hepatobiliary and intestinal diseases. The first part focused on the relationships between physicochemical properties, pharmacokinetics and metabolism of Berberine and...

  15. Analytical Method for Pu-239, Pu-240, Np-237 and Tc-99 using Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    An efficient analytical method for Pu isotopes (Pu-239 and Pu-240), Np-237 and Tc-99 in environmental samples has been developed using sector field inductively coupled plasma mass spectrometry (SF-ICPMS) detection. The chemical separation of Pu in terrestrial samples, soil, and sediment was carried out on two extraction resins, Sr-Spec and TEVA, which were sequentially combined in PrepLab, an integrated liquid handing device. By reducing the final eluent volume to 2.4 mL, directly injecting it to SF-ICPMS, and employing MCN-6000, a membrane desolvating sample introduction system, the analysis of Pu isotopes was found to be feasible in 1 g of soil. The detection limits of Pu-239, Pu-240, and Pu-242 were approximately 4 fg mL-1 (9.2 Bq mL-1), 3 fg mL-1 (25 Bq mL-1), and 6 fg mL-1 (0.87 Bq mL-1), which represent total amounts of 9.6, 7.2, and 14 fg, respectively, in the final eluent. Chemical separation and measurement were fully automated by a sequential injection (SI) program in an on-line system, and the analysis could thereby be completed within roughly 5 hours. The reliability of this method was confirmed by a validity test with several certified standard reference materials (NIST-4350b, IAEA-6, IAEA-300, IAEA-367, IAEA-368, IAEA-375). The analytical method for Pu in environmental seawater is different from that of terrestrial samples owing to the strong interference effect of U as well as ultra-low level Pu. Although the principle of chemical separation is nearly the same as in soil, seawater was co-precipitated with Fe(OH)2 in the pre-treatment step and a micro TEVA column (50 L) was used in the on-line system to improve precision and the lower detection limit. With this method, it was possible to analyze ultra-trace level Pu isotopes in only 5 L of surface seawater within 1 day, and the precision for Pu-239 and Pu-240 was less than 3.4% (n=7) and 5% (n=7), respectively. The accuracy of this method was verified by analysis of reference seawater (IAEA-381) as

  16. Analytical Method for Pu-239, Pu-240, Np-237 and Tc-99 using Inductively Coupled Plasma Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Cheol Su

    2007-02-15

    An efficient analytical method for Pu isotopes (Pu-239 and Pu-240), Np-237 and Tc-99 in environmental samples has been developed using sector field inductively coupled plasma mass spectrometry (SF-ICPMS) detection. The chemical separation of Pu in terrestrial samples, soil, and sediment was carried out on two extraction resins, Sr-Spec and TEVA, which were sequentially combined in PrepLab, an integrated liquid handing device. By reducing the final eluent volume to 2.4 mL, directly injecting it to SF-ICPMS, and employing MCN-6000, a membrane desolvating sample introduction system, the analysis of Pu isotopes was found to be feasible in 1 g of soil. The detection limits of Pu-239, Pu-240, and Pu-242 were approximately 4 fg mL-1 (9.2 Bq mL-1), 3 fg mL-1 (25 Bq mL-1), and 6 fg mL-1 (0.87 Bq mL-1), which represent total amounts of 9.6, 7.2, and 14 fg, respectively, in the final eluent. Chemical separation and measurement were fully automated by a sequential injection (SI) program in an on-line system, and the analysis could thereby be completed within roughly 5 hours. The reliability of this method was confirmed by a validity test with several certified standard reference materials (NIST-4350b, IAEA-6, IAEA-300, IAEA-367, IAEA-368, IAEA-375). The analytical method for Pu in environmental seawater is different from that of terrestrial samples owing to the strong interference effect of U as well as ultra-low level Pu. Although the principle of chemical separation is nearly the same as in soil, seawater was co-precipitated with Fe(OH)2 in the pre-treatment step and a micro TEVA column (50 L) was used in the on-line system to improve precision and the lower detection limit. With this method, it was possible to analyze ultra-trace level Pu isotopes in only 5 L of surface seawater within 1 day, and the precision for Pu-239 and Pu-240 was less than 3.4% (n=7) and 5% (n=7), respectively. The accuracy of this method was verified by analysis of reference seawater (IAEA-381) as

  17. Atmospheric deposition of heavy metals studied by analysis of moss samples using neutron activation analysis and atomic absorption spectrometry

    International Nuclear Information System (INIS)

    In a study of the atmospheric deposition of trace elements in different parts of Norway samples of the moss Hylocomium splendens were analyzed with respect to 26 elements. The determination of Cu, Zn, Pb, Cd and Ni was carried out by flame atomic absorption spectrometry, while an additional 21 elements were determined by instrumental neutron activation analysis. Several elements showed a substantially higher deposition in the southernmost parts of Norway than in places located farther north. As regards Pb, As and Sb, the difference amounted to a factor of ten or more. A similar but less pronounced trend was evident for elements such as V, Zn, Cd, Se and Ag. In some cases local pollution sources or marine aerosols had a significant effect on the results. For several heavy metals however long-distance transport from areas to the south and the south west of Norway was responsible for a major part of the air pollution

  18. Acid dissolution of soils and rocks for the determination of boron by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    The boron concentration in rocks, soils and standard reference materials was determined using hydrofluoric acid-aqua regia dissolution followed by inductively coupled plasma atomic emission spectrometry (ICP-AES) using the B 1 249.773 -nm line, corrected for spectral interference by iron. An excess of fluoride was complexed with aluminium to release boron from the stable fluoroborate ion and to protect the borosilicate and quartz components of the instrument. Boron was not lost by volatilisation during volume reduction. Soil and rock boron values determined using the recommended dissolution procedures were comparable to those obtained using the accepted sodium carbonate fusion procedure and by d.c. arc emission spectrophotometry, and those for standard reference materials showed good agreement and precision with the literature values. (author)

  19. Rapid determination of major and minor elements in rare earth-cobalt magnets by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Major and minor constituents, Sm, Ce, Y, Co, Fe, Mn, Cu, Zr and Hf, in typical rare earth-cobalt magnets were determined sequentially by inductively coupled plasma atomic emission spectrometry. Sample solutions were prepared by dissolving the magnets with aqua regia followed by dilution with 1.2 M HCl to suitable concentration. Beryllium was added as an internal standard in order to improved experimental accuracy and precision, and the emission intensity of Be was measured by using an additional small monochromator attached to the original instrument system. Cobalt, Fe, Cu and Zr in the magnets were also determined by conventional spectrophotometry. The results obtained by both methods were in good agreement with each other. (author)

  20. Nonthermal Optical Emission Spectrometry: Direct Atomization and Excitation of Cadmium for Highly Sensitive Determination.

    Science.gov (United States)

    Cai, Yi; Zhang, Ya-Jie; Wu, De-Fu; Yu, Yong-Liang; Wang, Jian-Hua

    2016-04-19

    The low atomization and excitation capability of nonthermal microplasma, e.g., dielectric barrier discharge (DBD), has greatly hampered its potential applications for the determination of metals in solution. In the present work, an inspiring development is reported for direct atomization and excitation of cadmium in aqueous solution by DBD and facilitates highly sensitive determination. A DBD microplasma is generated on the nozzle of a pneumatic micronebulizer to focus the DBD energy on a confined space and atomize/excite metals in the spray. Meanwhile, an appropriate sample matrix and nebulization in helium further improves the atomization and excitation capability of DBD. With cadmium as a model, its emission is recorded by a CCD spectrometer at 228.8 nm. By using an 80 μL sample solution nebulized at 3 μL s(-1), a linear range of 5-1000 μg L(-1) along with a detection limit of 1.5 μg L(-1) is achieved, which is comparable to those obtained by commercial bulky inductively coupled plasma (ICP)-based instrumentations. PMID:27030025

  1. Sputtering of copper atoms by keV atomic and molecular ions A comparison of experiment with analytical and computer based models

    CERN Document Server

    Gillen, D R; Goelich,

    2002-01-01

    Non-resonant multiphoton ionisation combined with quadrupole and time-of-flight analysis has been used to measure energy distributions of sputtered copper atoms. The sputtering of a polycrystalline copper target by 3.6 keV Ar sup + , N sup + and CF sub 2 sup + and 1.8 keV N sup + and CF sub 2 sup + ion bombardment at 45 deg. has been investigated. The linear collision model in the isotropic limit fails to describe the high energy tail of the energy distributions. However the TRIM.SP computer simulation has been shown to provide a good description. The results indicate that an accurate description of sputtering by low energy, molecular ions requires the use of computer simulation rather than analytical approaches. This is particularly important when considering plasma-surface interactions in plasma etching and deposition systems.

  2. Analytic variationally optimized internally orthogonalized modified Laguerre orbitals in accurate atomic configuration interaction calculation

    Institute of Scientific and Technical Information of China (English)

    Xiong Zhuang; Bacalis N C

    2006-01-01

    An analytic configuration interaction method based on variationally optimized internally orthogonalized modified Laguerre orbitals is presented. We have developed the corresponding computer code. For application, we study the ls2s 1S isoelectronic sequence from helium to neon, and compare with other methods. By taking into account the Eckart upper-bound theorem, we obtained more accurate and more intuitively understandable results than Hartree-Fock and multi-configuration Hartree-Fock reported results.

  3. Analytical investigation of the feasibility of sacrificial microchannel sealing for Chip-Scale Atomic Magnetometers

    OpenAIRE

    Tsujimoto, Kazuya; Hirai, Yoshikazu; Sugano, Koji; Tsuchiya, Toshiyuki; TABATA, Osamu

    2014-01-01

    An alkali metal vapor cell is a crucial component of the highly sensitive Chip Scale Atomic Magnetometers (CSAMs) that are increasingly deployed in a variety of electronic devices. Herein, we propose a novel microfabrication technique utilizing an array of microchannels at a bonded interface, to enable gas feedthrough for evacuation of unwanted gases from a vapor cell and subsequent introduction of an inert gas, followed by permanent sealing of the microchannels by reflow of a glass frit. The...

  4. Analytical framework of 'atoms for sustainable development'

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Tae Joon [Nuclear Policy Division, Korea Atomic Energy Research Institute, 150 Deokjin-dong, Yuseong-gu, Daejeon, 305-353 (Korea, Republic of)

    2010-07-01

    The term of 'Atoms for Sustainable Development' constantly pursues the increasing contribution of nuclear energy to the sustainable development which is providing an external kindling to the so-called nuclear renaissance. This paper explores a conceptual framework and a set of its elemental proxies to analyse the sustainable competitiveness of the nuclear energy system with a classification of the economic, environmental and social dimensions. (authors)

  5. Use of atomic absorption spectrometry to determine metallic impurities in coal

    International Nuclear Information System (INIS)

    The Brazilian Energetic Alternative Program expects the reduction of our dependence on foreign energy sources, by replacing fuel oil by mineral coal. Its gasification by means of nuclear energy must be also considered. However, the intensive burning of coal leads to serious environmental problems. During its combustion the release to atmosphere of toxic elements such as As, Hg, Pb, Zn and others is of great concern. Hence, it is important to have reliable analytical methods which can monitor inorganic constituents at various stages of coal production and utilization. The AAS is a suitable analytical technique to determine pollutants in coal because it is sensitive, simple, economic and cover a large range of concentration. The need of a previous treatment of sample is overcome by using an acid attack (HNO3 + HClO4 + HF) which has been proved to be rapid and efficient. (Author)

  6. International comparison of Cd content in a quality control material of Navajuelas (Tagelus dombeii) determined by anodic stripping voltammetry, atomic absorption spectrometry and neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Queirolo, F. (Universidad Catolica del Norte, Antofagasta (Chile). Dept. of Chemistry Forschungszentrum Juelich GmbH (Germany, F.R.). Inst. fuer Angewandte Physikalische Chemie Universidad de Extremadura, Badajoz (Spain). Dept. of Analytical Chemistry and Electrochemistry); Ostapczuk, P. (Forschungszentrum Juelich GmbH (Germany, F.R.). Inst. fuer Angewandte Physikalische Chemie); Valenta, P.; Stegen, S. (Forschungszentrum Juelich GmbH (Germany, F.R.). Inst. fuer Angewandte Physikalische Chemie Universidad de Extremadura, Badajoz (Spain). Dept. of Analytical Chemistry and Electrochemistry); Marin, C.; Vinagre, F.; Sanchez, A. (Universidad de Extremadura, Badajoz (Spain). Dept. of Analytical Chemistry and Electrochemistry)

    1991-05-01

    The determination of Cd was performed by neutron activation analysis (NAA), atomic absorption spectrometry (AAS) with flame or in the electrothermal mode and anodic stripping voltammetry in the differential pulse mode (DPASV) and the square wave mode (SWASV). (orig./EF).

  7. Investigations into the Role of Modifiers for Entrapment of Hydrides in Flow Injection Hydride Generation Electrothermal Atomic Absorption Spectrometry as Exemplified for the Determination of Germanium

    DEFF Research Database (Denmark)

    Hilligsøe, Bo; Andersen, Jens Enevold Thaulov; Hansen, Elo Harald

    1997-01-01

    Pd-conditioned graphite tubes, placed in the furnace of an atomic absorption spectrometry instrument, are used for entrapment of germane as generated in an associated flow injection system. Two different approaches are tested with the ultimate aim to allow multiple determinations, that is...

  8. Determination of Vanadium, Tin and Mercury in Atmospheric Particulate Matter and Cement Dust Samples by Direct Current Plasma Atomic Emission Spectrometry.

    Science.gov (United States)

    Hindy, Kamal T.; And Others

    1992-01-01

    An atmospheric pollution study applies direct current plasma atomic emission spectrometry (DCP-AES) to samples of total suspended particulate matter collected in two industrial areas and one residential area, and cement dust collected near major cement factories. These samples were analyzed for vanadium, tin, and mercury. The results indicate the…

  9. Determination of trace copper in food samples by flame atomic absorption spectrometry after solid phase extraction on modified soybean hull

    International Nuclear Information System (INIS)

    Soybean hull was chemically modified with citric acid and used as a solid phase extraction adsorbent for the determination of trace amounts of Cu2+ in food samples by flame absorption spectrometry (FAAS). The effect of pH, sample flow rate and volume, elution flow rate and volume and co-existing ions on the recovery of the analyte were investigated. The results showed that Cu2+ could be adsorbed on the modified soybean hull at pH 8.0 and eluted by 2.0 mL of 1.0 mol L-1 HCl. Under the optimized conditions, the adsorption capacity of modified soybean hull was found to be 18.0 mg g-1 for Cu2+. The detection limit of the proposed method was 0.8 ng mL-1 for Cu2+ with an enrichment factor of 18. The analytical result for the certified reference tea sample (GBW07605) was in a good agreement with the certified value. The proposed method has also been successfully applied to the determination of trace Cu2+ in dried sweet potato, lake water and milk powder, the recovery of Cu2+ for spiked samples was between 91% and 109.6%.

  10. Analytical approach for the determination of steroid profile of humans by gas chromatography isotope ratio mass spectrometry aimed at distinguishing between endogenous and exogenous steroids.

    Science.gov (United States)

    Bulska, Ewa; Gorczyca, Damian; Zalewska, Izabela; Pokrywka, Andrzej; Kwiatkowska, Dorota

    2015-03-15

    The contamination of commonly used supplements by unknown steroids as well as their metabolites (parent compounds) become a challenge for the analytical laboratories. Although the determination of steroids profile is not trivial because of the complex matrix and low concentration of single compound, one of the most difficult current problem is to distinguish, during analytical procedure, endogenous androgens such as testosterone, dehydrotestosterone or dehydroepiandrosterone from their synthetic equivalents. The aim of this work was to develop and validate an analytical procedure for determination of the steroid profile in human urine by gas chromatography-combustion-isotope ratio mass spectrometry (GC/C/IRMS) toward distinguishing between endogenous and exogenous steroids. Beside the optimization of the experimental parameters for gas chromatography separation and mass spectrometry, attention was focused on urine sample preparation. Using an optimized sample preparation protocol it was possible to achieve better chromatographic resolutions and better sensitivity enabling the determination of 5 steroids, androsterone, etiocholanolone, testosterone, 5-androstandiol, 11-hydroxyandrdostane, pregnandiol, with the expanded uncertainty (k=2) below 1‰. This enable to evaluate the significant shift of the δ(13)C/(12)C [‰] values for each of examined steroids (excluding ERC). The analytical protocol described in this work was successfully used for the confirmation of positive founding urine by evaluation T/E ratio after GC/C/IRMS analysis. PMID:25498150

  11. Analysis of slurries by inductively coupled plasma mass spectrometry using desolvation to improve transport efficiency and atomization efficiency

    Science.gov (United States)

    Hartley, James H. D.; Hill, Steve J.; Ebdon, Les

    1993-09-01

    A slurry sample introduction system incorporating a heated spray chamber and a condenser, cooled using Peltier coolers, has been designed to desolvate the slurry before entry into the plasma. Drying the slurry increased the transport efficiency (2.2-4.9%) and the atomization efficiency. This enhanced both sensitivities and recoveries. The increase in the recovery enabled larger particles to be fully atomized (≈8μm c.f.3˜μm) principally because of the desolvation that decreases the droplet size of the particles that enter the plasma. Fractionation of the samples before analysis by inductively coupled plasma mass spectrometry, using a cascade impactor, enabled information about the transport efficiency and recoveries to be obtained and also effects of inhomogeneity in the sample to be observed. The desolvation of the slurry also caused a decrease in the ionization temperature (from ≈6400°C to ≈5500°C). Local thermal equilibrium is supposed to be obtained and the ionization temperature here is obtained from the Saha equation. The reason for the increase in the recoveries is therefore considered to be due to the removal of the jacket of aqueous solvent around the particle. The ionization temperature of the plasma can be increased by increasing the forward power or by the addition of molecular gases to the nebulizer gas, particularly hydrogen. The addition of 1.5% v/v hydrogen can raise the ionization temperature from about 5500 to 8400°C.

  12. Determination of cadmium, aluminium, and copper in beer and products used in its manufacture by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Viñas, Pilar; Aguinaga, Nerea; López-García, Ignacio; Hernandez-Córdoba, Manuel

    2002-01-01

    Procedures were developed for determining cadmium, aluminium, and copper in beer and the products used in its manufacture by electrothermal atomic absorption spectrometry. Beer samples were injected into the furnace and solid samples were introduced as suspensions after preparation in a medium containing hydrogen peroxide, nitric acid, and ammonium dihydrogen phosphate for cadmium atomization. Calibration was performed with aqueous standards, and characteristic masses and detection limits were, respectively, 1 and 0.3 pg for cadmium, 18 and 5.4 pg for aluminium, and 5.6 and 6.8 pg for copper. Different samples of beer, wort, brewer's yeast, malt, raw grain, and hops were analyzed by the proposed procedures. Cadmium was found in low concentrations (0.001-0.08 microg/g and 0-1.3 ng/mL); copper (3-13 microg/g and 25-137 ng/mL) and aluminium (0.6-9 microg/g and 0.1-2 microg/mL) were found at higher levels. The reliability of the procedure was confirmed by comparing the results obtained with others based on microwave oven sample digestion, and by analyzing several certified reference materials. PMID:12083268

  13. Investigation of lead contents in lipsticks by solid sampling high resolution continuum source electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Gunduz, Sema; Akman, Suleyman

    2013-02-01

    In this study, the lead contents of different kinds of lipsticks were determined by solid sampling high resolution continuum source electrothermal atomic absorption spectrometry (SS-HR-CS ET AAS) and the results were compared with those obtained after microwave-assisted acid digestion of the samples. The experimental parameters for solid sampling such as the maximum amount of sample on the platforms of solid autosampler, graphite furnace program were optimized. Samples were directly loaded on the platforms of solid autosampler between 0.25 and 2.0mg and lead was determined applying 800 °C for pyrolysis and 2100 °C for atomization. Under optimized conditions, interference-free determination could be performed using aqueous standards. The LOD and the characteristic mass were 21.3 and 12.6 pg, respectively. The lead in the same lipstick samples was determined after microwave-assisted acid digestion and compared with those found by solid sampling. Mostly, there was no significant difference between the lead concentrations found by the two techniques. The lead in 25 lipstick samples with different properties were 0.11-4.48 ng mg(-1) which were not significantly different from those (<0.026-7.19 ng mg(-1)) reported by FDA for around 400 samples. PMID:23099440

  14. Analytical procedure for mapping the distribution of 10B and 99Tc markers in cryo-sections of animal tissue samples by secondary ion mass spectrometry

    Science.gov (United States)

    Marchetti, Ilaria; Menichetti, Luca; Kusmic, Claudia; de las Heras, Laura Aldave; Salvadori, Piero; Fuoco, Roger; Belloni, Fabio; L'Abbate, Antonio; Betti, Maria

    2009-09-01

    The development of a complete, standard analytical procedure for a quantitative use of secondary ion mass spectrometry to map the distribution in animal tissues of exogenous isotopes presents difficulties inherently related to sample preparation and preservation, as well as to the specific application being considered. We have tested in two very different cases a procedure based on the cryo-preparation of samples and calibration standards. The applications under investigation were the mapping of 10B in mouse brain tissue, with relevance to the boron neutron capture therapy, and of the perfusion tracer 99Tc in mouse heart tissue, with relevance to the study of microcirculation and cardiovascular pathologies. Scanning electron microscopy and inductively coupled mass spectrometry analysis were used as reference techniques for secondary ion mass spectrometry images and analyte measurements, respectively. Cryo-preparation of tissue sections for ion microscopy proved to be simple and efficient (in terms of structural and chemical integrity) for both brain and heart samples derived from fresh organs. This technique, however, turned out to be reliable only on the brain tissue when applied to the preparation of standards, which required chemical fixation of portions of organs. Brain and heart tissues showed a totally different response to chemical fixation, from both a structural and an analytical point of view. On the one hand, we were able to estimate a relative sensitivity factor for 10B in the cryo-sectioned brain matrix; on the other hand, even without the possibility of an absolute quantification of the 99Tc signal and notwithstanding the presence of an isobaric interference, secondary ion mass spectrometry mapping however proved to be capable to resolve the specific response of the cardiac tissue to the perfusion mechanism.

  15. Analytical procedure for mapping the distribution of {sup 10}B and {sup 99}Tc markers in cryo-sections of animal tissue samples by secondary ion mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Marchetti, Ilaria [European Commission, Joint Research Centre, Institute for Transuranium Elements, P.O. Box 2340, D-76125 Karlsruhe (Germany); Menichetti, Luca [National Research Council, Institute of Clinical Physiology, via G. Moruzzi, 1, 56124 Pisa (Italy)], E-mail: luca.m@ifc.cnr.it; Kusmic, Claudia [National Research Council, Institute of Clinical Physiology, via G. Moruzzi, 1, 56124 Pisa (Italy); Aldave de las Heras, Laura [European Commission, Joint Research Centre, Institute for Transuranium Elements, P.O. Box 2340, D-76125 Karlsruhe (Germany); Salvadori, Piero [National Research Council, Institute of Clinical Physiology, via G. Moruzzi, 1, 56124 Pisa (Italy); Fuoco, Roger [University of Pisa, Department of Chemistry and Industrial Chemistry, via Risorgimento, 35, 56126 Pisa (Italy); Belloni, Fabio [European Commission, Joint Research Centre, Institute for Transuranium Elements, P.O. Box 2340, D-76125 Karlsruhe (Germany)], E-mail: fabio.belloni@ec.europa.eu; L' Abbate, Antonio [Scuola Superiore Sant' Anna, P.zza Martiri della Liberta, 33, 56127 Pisa (Italy); Betti, Maria [European Commission, Joint Research Centre, Institute for Transuranium Elements, P.O. Box 2340, D-76125 Karlsruhe (Germany); International Atomic Energy Agency, IAEA-MEL Laboratories, MC 98000 Montecarlo, Principality of Monaco (Monaco)

    2009-09-15

    The development of a complete, standard analytical procedure for a quantitative use of secondary ion mass spectrometry to map the distribution in animal tissues of exogenous isotopes presents difficulties inherently related to sample preparation and preservation, as well as to the specific application being considered. We have tested in two very different cases a procedure based on the cryo-preparation of samples and calibration standards. The applications under investigation were the mapping of {sup 10}B in mouse brain tissue, with relevance to the boron neutron capture therapy, and of the perfusion tracer {sup 99}Tc in mouse heart tissue, with relevance to the study of microcirculation and cardiovascular pathologies. Scanning electron microscopy and inductively coupled mass spectrometry analysis were used as reference techniques for secondary ion mass spectrometry images and analyte measurements, respectively. Cryo-preparation of tissue sections for ion microscopy proved to be simple and efficient (in terms of structural and chemical integrity) for both brain and heart samples derived from fresh organs. This technique, however, turned out to be reliable only on the brain tissue when applied to the preparation of standards, which required chemical fixation of portions of organs. Brain and heart tissues showed a totally different response to chemical fixation, from both a structural and an analytical point of view. On the one hand, we were able to estimate a relative sensitivity factor for {sup 10}B in the cryo-sectioned brain matrix; on the other hand, even without the possibility of an absolute quantification of the {sup 99}Tc signal and notwithstanding the presence of an isobaric interference, secondary ion mass spectrometry mapping however proved to be capable to resolve the specific response of the cardiac tissue to the perfusion mechanism.

  16. Analytical procedure for mapping the distribution of 10B and 99Tc markers in cryo-sections of animal tissue samples by secondary ion mass spectrometry

    International Nuclear Information System (INIS)

    The development of a complete, standard analytical procedure for a quantitative use of secondary ion mass spectrometry to map the distribution in animal tissues of exogenous isotopes presents difficulties inherently related to sample preparation and preservation, as well as to the specific application being considered. We have tested in two very different cases a procedure based on the cryo-preparation of samples and calibration standards. The applications under investigation were the mapping of 10B in mouse brain tissue, with relevance to the boron neutron capture therapy, and of the perfusion tracer 99Tc in mouse heart tissue, with relevance to the study of microcirculation and cardiovascular pathologies. Scanning electron microscopy and inductively coupled mass spectrometry analysis were used as reference techniques for secondary ion mass spectrometry images and analyte measurements, respectively. Cryo-preparation of tissue sections for ion microscopy proved to be simple and efficient (in terms of structural and chemical integrity) for both brain and heart samples derived from fresh organs. This technique, however, turned out to be reliable only on the brain tissue when applied to the preparation of standards, which required chemical fixation of portions of organs. Brain and heart tissues showed a totally different response to chemical fixation, from both a structural and an analytical point of view. On the one hand, we were able to estimate a relative sensitivity factor for 10B in the cryo-sectioned brain matrix; on the other hand, even without the possibility of an absolute quantification of the 99Tc signal and notwithstanding the presence of an isobaric interference, secondary ion mass spectrometry mapping however proved to be capable to resolve the specific response of the cardiac tissue to the perfusion mechanism.

  17. Determination of trace mercury in environmental and foods samples by online coupling of flow injection displacement sorption preconcentration to electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Li, Yan; Jiang, Yan; Yan, Xiu-Ping; Ni, Zhe-Ming

    2002-11-15

    The toxic effects of mercury are well-known. To establish sources of mercury contamination and to evaluate levels of mercury pollution, sensitive, selective, and accurate analytical methods with excellent reproducibility are required. We have developed a novel methodology for the determination of trace mercury in environmental and foods samples by online coupling of flow injection (FI) displacement sorption preconcentration in a knotted reactor (KR) to electrothermal atomic absorption spectrometry (ETAAS). The developed methodology involved the online formation of copper pyrrolidine dithiocarbamate (Cu-PDC), presorption of the resulting Cu-PDC onto the inner walls of the KR, and selective retention of the analyte Hg(ll) onto the inner walls of the KR through online displacement reaction between Hg(ll) and the presorbed Cu-PDC. The retained analyte was subsequently eluted by 50 microL of ethanol and online detected by ETAAS. Interferences from coexisting heavy metal ions with lower stability of their APDC complexes relative to Cu- PDC were minimized without the need of any masking reagents. The tolerable concentrations of Cu(II), Cd(II), Fe(III), Ni(III), and Zn(II) were up to 12, 20, 16, 20, and 60 mg L(-1), respectively. No additional chemical modifiers for the stabilization of mercury were required in the present system owing to the stability of Hg-PDC at the drying stage, and no pyrolysis stage was necessary due to the effective removal of the matrices. With consumption of 2.5 mL of sample solution, an enhancement factor of 91 was obtained in comparison with direct injection of 50 microL of aqueous solution. The relative detection limit (3s) was 6.2 ng L(-1), corresponding to an absolute detection limit of 15.5 pg. The precision (RSD, n = 13) was 1.1% at the 2 microg L(-1) level. The method was successfully applied to the determination of mercury in several certified environmental and foods reference materials and locally collected water samples. PMID:12487313

  18. Determination of cadmium and lead in urine samples after dispersive solid–liquid extraction on multiwalled carbon nanotubes by slurry sampling electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A new method for the determination of Cd and Pb in urine samples has been developed. The method involves dispersive solid-phase extraction (DSPE), slurry sampling (SS), and subsequent electrothermal atomic absorption spectrometry (ETAAS). Oxidized multiwalled carbon nanotubes (MWCNTs) were used as the sorbent material. The isolated MWCNT/analyte aggregates were treated with nitric acid to form a slurry and both metals were determined directly by injecting the slurry into the ETAAS-atomizer. The parameters that influence the adsorption of the metals on MWCNTs in the DSPE process, the formation and extraction of the slurry, and the ETAAS conditions were studied by different factorial design strategies. The detection and quantification limits obtained for Cd under optimized conditions were 9.7 and 32.3 ng L−1, respectively, and for Pb these limits were 0.13 and 0.43 μg L−1. The preconcentration factors achieved were 3.9 and 5.4. The RSD values (n = 10) were less than 4.1% and 5.9% for Cd and Pb, respectively. The accuracy of the method was assessed in recovery studies, with values in the range 96–102% obtained for Cd and 97–101% for Pb. In addition, the analysis of certified reference materials gave consistent results. The DSPE–SS–ETAAS method is a novel and useful strategy for the determination of Pb and Cd at low levels in human urine samples. The method is sensitive, fast, and free of matrix interferences, and it avoids the tedious and time-consuming on-column adsorption and elution steps associated with commonly used SPE procedures. The proposed method was used to determine Cd and Pb in urine samples of unexposed healthy people and satisfactory results were obtained. - Highlights: • Cd and Pb determination based on the combination of DSP, SS and ETAAS • Urine matrix was eliminated using DSPE based on multiwalled carbon nanotubes. • Slurry sampling technique permitted the direct injection of sample into the ETAAS atomizer. • Appropriate

  19. Determination of cadmium and lead in urine samples after dispersive solid–liquid extraction on multiwalled carbon nanotubes by slurry sampling electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Álvarez Méndez, J.; Barciela García, J.; García Martín, S.; Peña Crecente, R.M.; Herrero Latorre, C., E-mail: carlos.herrero@usc.es

    2015-04-01

    A new method for the determination of Cd and Pb in urine samples has been developed. The method involves dispersive solid-phase extraction (DSPE), slurry sampling (SS), and subsequent electrothermal atomic absorption spectrometry (ETAAS). Oxidized multiwalled carbon nanotubes (MWCNTs) were used as the sorbent material. The isolated MWCNT/analyte aggregates were treated with nitric acid to form a slurry and both metals were determined directly by injecting the slurry into the ETAAS-atomizer. The parameters that influence the adsorption of the metals on MWCNTs in the DSPE process, the formation and extraction of the slurry, and the ETAAS conditions were studied by different factorial design strategies. The detection and quantification limits obtained for Cd under optimized conditions were 9.7 and 32.3 ng L{sup −1}, respectively, and for Pb these limits were 0.13 and 0.43 μg L{sup −1}. The preconcentration factors achieved were 3.9 and 5.4. The RSD values (n = 10) were less than 4.1% and 5.9% for Cd and Pb, respectively. The accuracy of the method was assessed in recovery studies, with values in the range 96–102% obtained for Cd and 97–101% for Pb. In addition, the analysis of certified reference materials gave consistent results. The DSPE–SS–ETAAS method is a novel and useful strategy for the determination of Pb and Cd at low levels in human urine samples. The method is sensitive, fast, and free of matrix interferences, and it avoids the tedious and time-consuming on-column adsorption and elution steps associated with commonly used SPE procedures. The proposed method was used to determine Cd and Pb in urine samples of unexposed healthy people and satisfactory results were obtained. - Highlights: • Cd and Pb determination based on the combination of DSP, SS and ETAAS • Urine matrix was eliminated using DSPE based on multiwalled carbon nanotubes. • Slurry sampling technique permitted the direct injection of sample into the ETAAS atomizer.

  20. X-Ray Microanalysis and Electron Energy Loss Spectrometry in the Analytical Electron Microscope: Review and Future Directions

    Science.gov (United States)

    Goldstein, J. I.; Williams, D. B.

    1992-01-01

    This paper reviews and discusses future directions in analytical electron microscopy for microchemical analysis using X-ray and Electron Energy Loss Spectroscopy (EELS). The technique of X-ray microanalysis, using the ratio method and k(sub AB) factors, is outlined. The X-ray absorption correction is the major barrier to the objective of obtaining I% accuracy and precision in analysis. Spatial resolution and Minimum Detectability Limits (MDL) are considered with present limitations of spatial resolution in the 2 to 3 microns range and of MDL in the 0.1 to 0.2 wt. % range when a Field Emission Gun (FEG) system is used. Future directions of X-ray analysis include improvement in X-ray spatial resolution to the I to 2 microns range and MDL as low as 0.01 wt. %. With these improvements the detection of single atoms in the analysis volume will be possible. Other future improvements include the use of clean room techniques for thin specimen preparation, quantification available at the I% accuracy and precision level with light element analysis quantification available at better than the 10% accuracy and precision level, the incorporation of a compact wavelength dispersive spectrometer to improve X-ray spectral resolution, light element analysis and MDL, and instrument improvements including source stability, on-line probe current measurements, stage stability, and computerized stage control. The paper reviews the EELS technique, recognizing that it has been slow to develop and still remains firmly in research laboratories rather than in applications laboratories. Consideration of microanalysis with core-loss edges is given along with a discussion of the limitations such as specimen thickness. Spatial resolution and MDL are considered, recognizing that single atom detection is already possible. Plasmon loss analysis is discussed as well as fine structure analysis. New techniques for energy-loss imaging are also summarized. Future directions in the EELS technique will be

  1. Matrix elimination method for the determination of precious metals in ores using electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Salih, Bekir; Celikbiçak, Omür; Döker, Serhat; Doğan, Mehmet

    2007-03-28

    Poly(N-(hydroxymethyl)methacrylamide)-1-allyl-2-thiourea) hydrogels, poly(NHMMA-ATU), were synthesized by gamma radiation using (60)Co gamma source in the ternary mixture of NHMMA-ATU-H(2)O. These hydrogels were used for the specific gold, silver, platinum and palladium recovery, pre-concentration and matrix elimination from the solutions containing trace amounts of precious metal ions. Elimination of inorganic matrices such as different transition and heavy metal ions, and anions was performed by adjusting the solution pH to 0.5 that was the selective adsorption pH of the precious metal ions. Desorption of the precious metal ions was performed by using 0.8 M thiourea in 3M HCl as the most efficient desorbing agent with recovery values more than 95%. In the desorption medium, thiourea effect on the atomic signal was eliminated by selecting proper pyrolysis and atomization temperatures for all precious metal ions. Precision and the accuracy of the results were improved in the graphite furnace-atomic absorption spectrometer (GFAAS) measurements by applying the developed matrix elimination method performing the adsorption at pH 0.5. Pre-concentration factors of the studied precious metal ions were found to be at least 1000-fold. Detection limits of the precious metal ions were found to be less than 10 ng L(-1) of the all studied precious metal ions by using the proposed pre-concentration method. Determination of trace levels of the precious metals in the sea-water, anode slime, geological samples and photographic fixer solutions were performed using GFAAS clearly after applying the adsorption-desorption cycle onto the poly(NHMMA-UTU) hydrogels. PMID:17386783

  2. Pre-analytical and analytical variation of drug determination in segmented hair using ultra-performance liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Marie Katrine Klose; Johansen, Sys Stybe; Linnet, Kristian

    2014-01-01

    Assessment of total uncertainty of analytical methods for the measurements of drugs in human hair has mainly been derived from the analytical variation. However, in hair analysis several other sources of uncertainty will contribute to the total uncertainty. Particularly, in segmental hair analysis...... pre-analytical variations associated with the sampling and segmentation may be significant factors in the assessment of the total uncertainty budget. The aim of this study was to develop and validate a method for the analysis of 31 common drugs in hair using ultra-performance liquid chromatography...... variation was estimated to be less than 15% for almost all compounds. The method was successfully applied to 25 segmented hair specimens from deceased drug addicts showing a broad pattern of poly-drug use. The pre-analytical sampling variation was estimated from the genuine duplicate measurements of two...

  3. Consistent Analytic Embedded Atom Potential for Face-Centered Cubic Metals and Alloys

    Institute of Scientific and Technical Information of China (English)

    Iyad A. Hijazi; Young Ho Park

    2009-01-01

    A consistent empirical embedded-atom potential that includes a long range force was developed for fcc (face-centered cubic) metals and alloys. The proposed potential for pure metals does not require modification of the initial function form when being applied to alloy systems. The potential parameters of this model were determined by fitting lattice constant, three elastic constants, cohesive energy, and vacancy formation energies of the pure metals and the heats of solution of the binary alloys via an optimization technique. Parameters for Ag, Al, Au, Cu, Ni, Pd and Pt were obtained. The obtained parameters were used to calculate the bulk modulus, divacancy formation energy, crystal stability, stacking fault energy, vacancy migration energy, and melting point for each pure metal and the heats of formation and lattice constants for binary alloys. The predicted values were in good agreement with experimental results.

  4. Speciation of mercury in fish samples by flow injection catalytic cold vapour atomic absorption spectrometry.

    Science.gov (United States)

    Zhang, Yanlin; Adeloju, Samuel B

    2012-04-01

    A rapid flow injection catalytic cold vapour atomic absorption spectrometric (FI-CCV-AAS) method is described for speciation and determination of mercury in biological samples. Varying concentrations of NaBH(4) were employed for mercury vapour generation from inorganic and mixture of inorganic and organic (total) Hg. The presence of Fe(3+), Cu(2+) and thiourea had catalytic effect on mercury vapour generation from methylmercury (MeHg) and, when together, Cu(2+) and thiourea had synergistic catalytic effect on the vapour generation. Of the two metal ions, Fe(3+) gave the best sensitivity enhancement, achieving the same sensitivity for MeHg and inorganic Hg(2+). Due to similarity of resulting sensitivity, Hg(2+) was used successfully as a primary standard for quantification of inorganic and total Hg. The catalysis was homogeneous in nature, and it was assumed that the breaking of the C-Hg bond was facilitated by the delocalization of the 5d electron pairs in Hg atom. The extraction of MeHg and inorganic mercury (In-Hg) in fish samples were achieved quantitatively with hydrochloric acid in the presence of thiourea and determined by FI-CCV-AAS. The application of the method to the quantification of mercury species in a fish liver reference material DOLT-4 gave 91.5% and 102.3% recoveries for total and methyl mercury, respectively. The use of flow injection enabled rapid analysis with a sample throughput of 180 h(-1).

  5. Arsenic Speciation of Waters from the Aegean Region, Turkey by Hydride Generation: Atomic Absorption Spectrometry.

    Science.gov (United States)

    Çiftçi, Tülin Deniz; Henden, Emur

    2016-08-01

    Arsenic in drinking water is a serious problem for human health. Since the toxicity of arsenic species As(III) and As(V) is different, it is important to determine the concentrations separately. Therefore, it is necessary to develop an accurate and sensitive method for the speciation of arsenic. It was intended with this work to determine the concentrations of arsenic species in water samples collected from Izmir, Manisa and nearby areas. A batch type hydride generation atomic absorption spectrometer was used. As(V) gave no signal under the optimal measurement conditions of As(III). A certified reference drinking water was analyzed by the method and the results showed excellent agreement with the reported values. The procedure was applied to 34 water samples. Eleven tap water, two spring water, 19 artesian well water and two thermal water samples were analyzed under the optimal conditions. PMID:27236436

  6. A mass spectrometry primer for mass spectrometry imaging.

    Science.gov (United States)

    Rubakhin, Stanislav S; Sweedler, Jonathan V

    2010-01-01

    Mass spectrometry imaging (MSI), a rapidly growing subfield of chemical imaging, employs mass spectrometry (MS) technologies to create single- and multi-dimensional localization maps for a variety of atoms and molecules. Complimentary to other imaging approaches, MSI provides high chemical specificity and broad analyte coverage. This powerful analytical toolset is capable of measuring the distribution of many classes of inorganics, metabolites, proteins, and pharmaceuticals in chemically and structurally complex biological specimens in vivo, in vitro, and in situ. The MSI approaches highlighted in this Methods in Molecular Biology volume provide flexibility of detection, characterization, and identification of multiple known and unknown analytes. The goal of this chapter is to introduce investigators who may be unfamiliar with MS to the basic principles of the mass spectrometric approaches as used in MSI. In addition to guidelines for choosing the most suitable MSI method for specific investigations, cross-references are provided to the chapters in this volume that describe the appropriate experimental protocols.

  7. [Analytical figures of merit of Hildebrand grid and ultrasonic nebulizations in inductively coupled plasma atomic emission].

    Science.gov (United States)

    Tian, Mei; Han, Xiao-yuan; Zhuo, Shang-jun; Zhang, Rui-rong

    2012-05-01

    Hildebrand grid nebulizer is a kind of improved Babington nebulizer, which can nebulize solutions with high total dissolved solids. And the ultrasonic nebulizer (USN) possesses advantage of high nebulization efficiency and fine droplets. In the present paper, the detection limits, matrix effects, ICP robustness and memory effects of Hildebrand grid and ultrasonic nebulizers for ICP-AES were studied. The results show that the detection limits using USN are improved by a factor of 6-23 in comparison to Hildebrand grid nebulizer for Cu, Pb, Zn, Cr, Cd and Ni. With the USN the matrix effects were heavier, and the degree of intensity enhancement and lowering depends on the element line, the composition and concentrations of matrices. Moreover, matrix effects induced by Ca and Mg are more significant than those caused by Na and Mg, and intensities of ionic lines are affected more easily than those of atomic lines. At the same time, with the USN ICP has less robustness. In addition, memory effect of the USN is also heavier than that of Hildebrand grid nebulizer.

  8. Fast determination of trace elements in organic fertilizers using a cup-horn reactor for ultrasound-assisted extraction and fast sequential flame atomic absorption spectrometry.

    Science.gov (United States)

    Teixeira, Leonel Silva; Vieira, Heulla Pereira; Windmöller, Cláudia Carvalhinho; Nascentes, Clésia Cristina

    2014-02-01

    A fast and accurate method based on ultrasound-assisted extraction in a cup-horn sonoreactor was developed to determine the total content of Cd, Co, Cr, Cu, Mn, Ni, Pb and Zn in organic fertilizers by fast sequential flame atomic absorption spectrometry (FS FAAS). Multivariate optimization was used to establish the optimal conditions for the extraction procedure. An aliquot containing approximately 120 mg of the sample was added to a 500 µL volume of an acid mixture (HNO3/HCl/HF, 5:3:3, v/v/v). After a few minutes, 500 µL of deionized water was added and eight samples were simultaneously sonicated for 10 min at 50% amplitude, allowing a sample throughput of 32 extractions per hour. The performance of the method was evaluated with a certified reference material of sewage sludge (CRM 029). The precision, expressed as the relative standard deviation, ranged from 0.58% to 5.6%. The recoveries of analytes were found to 100%, 109%, 96%, 92%, 101%, 104% and 102% for Cd, Cr, Cu, Mn, Ni, Pb and Zn, respectively. The linearity, limit of detection and limit of quantification were calculated and the values obtained were adequate for the quality control of organic fertilizers. The method was applied to the analysis of several commercial organic fertilizers and organic wastes used as fertilizers, and the results were compared with those obtained using the microwave digestion procedure. A good agreement was found between the results obtained by microwave and ultrasound procedures with recoveries ranging from 80.4% to 117%. Two organic waste samples were not in accordance with the Brazilian legislation regarding the acceptable levels of contaminants.

  9. Graphene-based solid-phase extraction combined with flame atomic absorption spectrometry for a sensitive determination of trace amounts of lead in environmental water and vegetable samples

    Energy Technology Data Exchange (ETDEWEB)

    Wang Yukun; Gao Shutao; Zang Xiaohuan [Hebei Key Laboratory of Bioinorganic Chemistry, College of Sciences, Agricultural University of Hebei, Baoding 071001 (China); Li Jingci, E-mail: jingcili63@yahoo.com.cn [Hebei Key Laboratory of Bioinorganic Chemistry, College of Sciences, Agricultural University of Hebei, Baoding 071001 (China); Ma Jingjun, E-mail: majingjun@hebau.edu.cn [Hebei Key Laboratory of Bioinorganic Chemistry, College of Sciences, Agricultural University of Hebei, Baoding 071001 (China)

    2012-02-24

    Highlights: Black-Right-Pointing-Pointer Graphene as a novel sorbent material in a column for solid-phase extraction (SPE). Black-Right-Pointing-Pointer SPE for the determination of lead (Pb) in environment water samples and vegetable samples. Black-Right-Pointing-Pointer The system can be reused for many times. Black-Right-Pointing-Pointer The adsorption capacity of graphene over many other adsorbents. Black-Right-Pointing-Pointer Graphene has great potentials as an excellent sorbent material. - Abstract: Graphene, a novel class of carbon nanostructures, has great promise for use as sorbent materials because of its ultrahigh specific surface area. A new method using a column packed with graphene as sorbent was developed for the preconcentration of trace amounts of lead (Pb) using dithizone as chelating reagent prior to its determination by flame atomic absorption spectrometry. Some effective parameters on the extraction and complex formation were selected and optimized. Under optimum conditions, the calibration graph was linear in the concentration range of 10.0-600.0 {mu}g L{sup -1} with a detection limit of 0.61 {mu}g L{sup -1}. The relative standard deviation for ten replicate measurements of 20.0 and 400.0 {mu}g L{sup -1} of Pb were 3.56 and 3.25%, respectively. Comparative studies showed that graphene is superior to other adsorbents including C18 silica, graphitic carbon, and single- and multi-walled carbon nanotubes for the extraction of Pb. The proposed method was successfully applied in the analysis of environmental water and vegetable samples. Good spiked recoveries over the range of 95.3-100.4% were obtained. This work not only proposes a useful method for sample preconcentration, but also reveals the great potential of graphene as an excellent sorbent material in analytical processes.

  10. Development of new portable miniaturize solid phase microextraction of silver-APDC complex using micropipette tip in-syringe system couple with electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem Gul; Afridi, Hassan Imran; Shah, Faheem; Arain, Sadaf Sadia; Arain, Salma Aslam; Panhwar, Abdul Haleem; Arain, Mariam Shahzadi; Samoon, Muhammad Kashif

    2016-02-01

    An innovative and simple miniaturized solid phase microextraction (M-SPME) method, was developed for preconcentration and determination of silver(I) in the fresh and waste water samples. For M-SPME, a micropipette tip packed with activated carbon cloth (ACC) as sorbent, in a syringe system. The size, morphology and elemental composition of ACC before and after adsorption of analyte have been characterized by scanning electron microscopy and energy dispersive spectroscopy. The sample solution treated with a complexing reagent, ammonium pyrrolidine dithiocarbamate (APDC), was drawn into the syringe filled with ACC and dispensed manually for 2 to 10 aspirating/dispensing cycle. Then the Ag- complex sorbed on the ACC in micropipette was quantitatively eluted by drawing and dispensing of different concentrations of acids for 2 to 5 aspirating/dispensing cycles. The extracted Ag ions with modifier were injected directly into the electrothermal atomic absorption spectrometry for analysis. The influence of different variables on the extraction efficiency, including the concentration of ligand, pH, sample volume, eluent type, concentration and volume was investigated. Validity and accuracy of the developed method was checked by the standard addition method. Reliability of the proposed methodology was checked by the relative standard deviation (%RSD), which was found to be < 5%. Under the optimized experimental variables, the limits of detection (LOD) and enhancement factors (EF), were obtained to be 0.86 ng L- 1 and 120, respectively. The proposed method was successfully applied for the determination of trace levels of silver ions in fresh and waste water samples.

  11. Preconcentration and determination of vanadium and molybdenum in milk, vegetables and foodstuffs by ultrasonic-thermostatic-assisted cloud point extraction coupled to flame atomic absorption spectrometry.

    Science.gov (United States)

    Gürkan, Ramazan; Korkmaz, Sema; Altunay, Nail

    2016-08-01

    A new ultrasonic-thermostatic-assisted cloud point extraction procedure (UTA-CPE) was developed for preconcentration at the trace levels of vanadium (V) and molybdenum (Mo) in milk, vegetables and foodstuffs prior to determination via flame atomic absorption spectrometry (FAAS). The method is based on the ion-association of stable anionic oxalate complexes of V(V) and Mo(VI) with [9-(diethylamino)benzo[a]phenoxazin-5-ylidene]azanium; sulfate (Nile blue A) at pH 4.5, and then extraction of the formed ion-association complexes into micellar phase of polyoxyethylene(7.5)nonylphenyl ether (PONPE 7.5). The UTA-CPE is greatly simplified and accelerated compared to traditional cloud point extraction (CPE). The analytical parameters optimized are solution pH, the concentrations of complexing reagents (oxalate and Nile blue A), the PONPE 7.5 concentration, electrolyte concentration, sample volume, temperature and ultrasonic power. Under the optimum conditions, the calibration curves for Mo(VI) and V(V) are obtained in the concentration range of 3-340µgL(-1) and 5-250µgL(-1) with high sensitivity enhancement factors (EFs) of 145 and 115, respectively. The limits of detection (LODs) for Mo(VI) and V(V) are 0.86 and 1.55µgL(-1), respectively. The proposed method demonstrated good performances such as relative standard deviations (as RSD %) (≤3.5%) and spiked recoveries (95.7-102.3%). The accuracy of the method was assessed by analysis of two standard reference materials (SRMs) and recoveries of spiked solutions. The method was successfully applied into the determination of trace amounts of Mo(VI) and V(V) in milk, vegetables and foodstuffs with satisfactory results. PMID:27216654

  12. Determination of lead, cadmium, copper, and nickel in the tonghui river of beijing, china, by cloud point extraction-high resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Ren, Ting; Zhao, Li-Jiao; Sun, Bo-Si; Zhong, Ru-Gang

    2013-11-01

    Heavy metal contamination of water has become an important problem in recent years. Most hazardous heavy metals exist in environmental water in trace or ultra-trace amounts, which requires establishing highly sensitive analytical methods. In this research, quantitative analyses were performed using high-resolution continuum source graphite furnace atomic absorption spectrometry combined with cloud point extraction (CPE) to determine Pb, Cd, Cu, and Ni levels in environmental surface water. By optimizing the CPE conditions, the enrichment factors were 29 for Pb, Cd, and Cu and 25 for Ni. The limits of detection (LOD) were 0.080, 0.010, 0.035, and 0.014 μg L for Pb, Cd, Cu, and Ni, respectively. The sensitivity of the method is comparable with those reported in previous investigations using various methods and improves outcome by 2 to 3 orders of magnitude compared with the LODs of the current national standard methods of China. Our method was used to determine Pb, Cd, Cu, and Ni in 55 water samples collected from the Tonghui River, which is the principal river in the urban area of Beijing, China. The results indicated that the distributions of the four heavy metals in the Tonghui River were related with the environments. The levels of Pb and Ni exhibit increasing trends along the river from upstream to downstream possibly due to the existence of some chemical factories in the downstream area. Lead, Cd, Cu, and Ni averaged 13.9, 0.8, 46.8, and 38.5%, respectively, of the total amount of the determined heavy metals. The levels of the four heavy metals conformed to the Environmental Quality Standards for Surface Water (Grade I) of China. This work provides a reliable quantitative method to determine trace-amount heavy metals in water, which lays a foundation for establishing standards and regulations for environmental water protection.

  13. Preconcentration and determination of vanadium and molybdenum in milk, vegetables and foodstuffs by ultrasonic-thermostatic-assisted cloud point extraction coupled to flame atomic absorption spectrometry.

    Science.gov (United States)

    Gürkan, Ramazan; Korkmaz, Sema; Altunay, Nail

    2016-08-01

    A new ultrasonic-thermostatic-assisted cloud point extraction procedure (UTA-CPE) was developed for preconcentration at the trace levels of vanadium (V) and molybdenum (Mo) in milk, vegetables and foodstuffs prior to determination via flame atomic absorption spectrometry (FAAS). The method is based on the ion-association of stable anionic oxalate complexes of V(V) and Mo(VI) with [9-(diethylamino)benzo[a]phenoxazin-5-ylidene]azanium; sulfate (Nile blue A) at pH 4.5, and then extraction of the formed ion-association complexes into micellar phase of polyoxyethylene(7.5)nonylphenyl ether (PONPE 7.5). The UTA-CPE is greatly simplified and accelerated compared to traditional cloud point extraction (CPE). The analytical parameters optimized are solution pH, the concentrations of complexing reagents (oxalate and Nile blue A), the PONPE 7.5 concentration, electrolyte concentration, sample volume, temperature and ultrasonic power. Under the optimum conditions, the calibration curves for Mo(VI) and V(V) are obtained in the concentration range of 3-340µgL(-1) and 5-250µgL(-1) with high sensitivity enhancement factors (EFs) of 145 and 115, respectively. The limits of detection (LODs) for Mo(VI) and V(V) are 0.86 and 1.55µgL(-1), respectively. The proposed method demonstrated good performances such as relative standard deviations (as RSD %) (≤3.5%) and spiked recoveries (95.7-102.3%). The accuracy of the method was assessed by analysis of two standard reference materials (SRMs) and recoveries of spiked solutions. The method was successfully applied into the determination of trace amounts of Mo(VI) and V(V) in milk, vegetables and foodstuffs with satisfactory results.

  14. Determination of arsenic(III) and arsenic(V) by electrothermal atomic absorption spectrometry after complexation and sorption on a C-18 bonded silica column.

    Science.gov (United States)

    Pozebon, D; Dressler, V L; Gomes Neto, J A; Curtius, A J

    1998-04-01

    A flow injection procedure for the separation and pre-concentration of inorganic arsenic based on the complexation with ammonium diethyl dithiophosphate (DDTP) and sorption on a C-18 bonded silica gel minicolumn is proposed. During the sample injection by a time-based fashion, the As(3+)-DDTP complex is stripped from the solution and retained in the column. Arsenic(V) and other ions that do not form complexes are discarded. After reduction to the trivalent state by using potassium iodide plus ascorbic acid, total arsenic is determined by electrothermal atomic absorption spectrometry (ETAAS). Arsenic(V) concentration can be calculated by difference. After processing 6 ml sample volume, the As(3+)-DDTP complexes were eluted directly into the autosampler cup (120 mul). Ethanol was used for column rinsing. Influence of pH, reagent concentration, pre-concentration and elution time and column size were investigated. When 30 mul of eluate plus 10 mul of 0.1% (w/v) Pd(NO(3))(2) were dispensed into the graphite tube, analytical curve in the 0.3-3 mug As l(-1) range was obtained (r=0.9991). The accuracy was checked for arsenic determination in a certified water, spiked tap water and synthetic mixtures of arsenite and arsenate. Good recoveries (97-108%) of spiked samples were found. Results are precise (RSD 7.5 and 6% for 0.5 and 2.5 mug l(-1), n=10) and in agreement with the certified value of reference material at 95% confidence level. PMID:18967109

  15. Determination of nickel in blood and serum samples of oropharyngeal cancer patients consumed smokeless tobacco products by cloud point extraction coupled with flame atomic absorption spectrometry.

    Science.gov (United States)

    Arain, Sadaf Sadia; Kazi, Tasneem Gul; Arain, Jamshed Bashir; Afridi, Hassan Imran; Kazi, Atif Gul; Nasreen, Syeda; Brahman, Kapil Dev

    2014-10-01

    Oropharyngeal cancer is a significant public health issue in the world. The incidence of oropharyngeal cancer has been increased among people who have habit of chewing smokeless tobacco (SLT) in Pakistan. The aim of present study was to evaluate the concentration of nickel (Ni) in biological samples (whole blood, serum) of oral (n = 95) and pharyngeal (n = 84) male cancer patients. For comparison purposes, the biological samples of healthy age-matched referents (n = 150), who consumed and did not consumed SLT products, were also analyzed for Ni levels. As the Ni level is very low in biological samples, a preconcentration procedure has been developed, prior to analysis of analyte by flame atomic absorption spectrometry (FAAS). The Ni in acid-digested biological samples was complexed with ammonium pyrrolidinedithio carbamate (APDC), and a resulted complex was extracted in a surfactant Triton X-114. Acidic ethanol was added to the surfactant-rich phase prior to its analysis by FAAS. The chemical variables, such as pH, amounts of reagents (APDC, Triton X-114), temperature, incubation time, and sample volume were optimized. The resulted data indicated that concentration of Ni was higher in blood and serum samples of cancer patients as compared to that of referents who have or have not consumed different SLT products (p = 0.012-0.001). It was also observed that healthy referents who consumed SLT products have two to threefold higher levels of Ni in both biological samples as compared to those who were not chewing SLT products (p < 0.01).

  16. Determination of Pb (Lead, Cd (Cadmium, Cr (Chromium, Cu (Copper, and Ni (Nickel in Chinese tea with high-resolution continuum source graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Wen-Si Zhong

    2016-01-01

    Full Text Available The contents of lead, cadmium, chromium, copper, and nickel were determined in 25 tea samples from China, including green, yellow, white, oolong, black, Pu'er, and jasmine tea products, using high-resolution continuum source graphite furnace atomic absorption spectrometry. The methods used for sample preparation, digestion, and quantificational analysis were established, generating satisfactory analytical precisions (represented by relative standard deviations ranging from 0.6% to 2.5% and recoveries (98.91–101.32%. The lead contents in tea leaves were 0.48–10.57 mg/kg, and 80% of these values were below the maximum values stated by the guidelines in China. The contents of cadmium and chromium ranged from 0.01 mg/kg to 0.39 mg/kg and from 0.27 mg/kg to 2.45 mg/kg, respectively, remaining in compliance with the limits stipulated by China's Ministry of Agriculture. The copper contents were 7.73–63.71 mg/kg; only 64% of these values complied with the standards stipulated by the Ministry of Agriculture. The nickel contents ranged from 2.70 mg/kg to 13.41 mg/kg. Consequently, more attention must be paid to the risks of heavy metal contamination in tea. The quantitative method established in this work lays a foundation for preventing heavy metal toxicity in human from drinking tea and will help establish regulations to control the contents of heavy metals in tea.

  17. Determination of nickel in blood and serum samples of oropharyngeal cancer patients consumed smokeless tobacco products by cloud point extraction coupled with flame atomic absorption spectrometry.

    Science.gov (United States)

    Arain, Sadaf Sadia; Kazi, Tasneem Gul; Arain, Jamshed Bashir; Afridi, Hassan Imran; Kazi, Atif Gul; Nasreen, Syeda; Brahman, Kapil Dev

    2014-10-01

    Oropharyngeal cancer is a significant public health issue in the world. The incidence of oropharyngeal cancer has been increased among people who have habit of chewing smokeless tobacco (SLT) in Pakistan. The aim of present study was to evaluate the concentration of nickel (Ni) in biological samples (whole blood, serum) of oral (n = 95) and pharyngeal (n = 84) male cancer patients. For comparison purposes, the biological samples of healthy age-matched referents (n = 150), who consumed and did not consumed SLT products, were also analyzed for Ni levels. As the Ni level is very low in biological samples, a preconcentration procedure has been developed, prior to analysis of analyte by flame atomic absorption spectrometry (FAAS). The Ni in acid-digested biological samples was complexed with ammonium pyrrolidinedithio carbamate (APDC), and a resulted complex was extracted in a surfactant Triton X-114. Acidic ethanol was added to the surfactant-rich phase prior to its analysis by FAAS. The chemical variables, such as pH, amounts of reagents (APDC, Triton X-114), temperature, incubation time, and sample volume were optimized. The resulted data indicated that concentration of Ni was higher in blood and serum samples of cancer patients as compared to that of referents who have or have not consumed different SLT products (p = 0.012-0.001). It was also observed that healthy referents who consumed SLT products have two to threefold higher levels of Ni in both biological samples as compared to those who were not chewing SLT products (p < 0.01). PMID:24920259

  18. Determination of trace amounts of molybdenum in plant tissue by solvent extraction-atomic-absorption and direct-current plasma emission spectrometry.

    Science.gov (United States)

    Lajunen, L H; Kubin, A

    1986-03-01

    Methods are presented for determination of molybdenum in plant tissue by flame and graphite-furnace atomic-absorption spectrometry and direct-current argon-plasma emission spectrometry. The samples are digested in HNO(3)-H(2)SO(4)-HC1O(4) mixture, and Mo is separated and concentrated by chelation and extraction. Three organic solvents (methyl isobutyl ketone, di-isobutyl ketone and isoamyl alcohol) and two ligands (8-hydroxyquinoline and toluene-3,4-dithiol) were studied. The procedure were tested on pine needle and birch leaf samples. PMID:18964076

  19. Investigation of colloidal graphite as a matrix for matrix-assisted laser desorption/ionisation mass spectrometry of low molecular weight analytes.

    Science.gov (United States)

    Warren, Alexander D; Conway, Ulric; Arthur, Christopher J; Gates, Paul J

    2016-07-01

    The analysis of low molecular weight compounds by matrix-assisted laser desorption/ionisation mass spectrometry is problematic due to the interference and suppression of analyte ionisation by the matrices typically employed - which are themselves low molecular weight compounds. The application of colloidal graphite is demonstrated here as an easy to use matrix that can promote the ionisation of a wide range of analytes including low molecular weight organic compounds, complex natural products and inorganic complexes. Analyte ionisation with colloidal graphite is compared with traditional organic matrices along with various other sources of graphite (e.g. graphite rods and charcoal pencils). Factors such as ease of application, spectra reproducibility, spot longevity, spot-to-spot reproducibility and spot homogeneity (through single spot imaging) are explored. For some analytes, considerable matrix suppression effects are observed resulting in spectra completely devoid of matrix ions. We also report the observation of radical molecular ions [M(-●) ] in the negative ion mode, particularly with some aromatic analytes. Copyright © 2016 John Wiley & Sons, Ltd.

  20. Investigation of colloidal graphite as a matrix for matrix-assisted laser desorption/ionisation mass spectrometry of low molecular weight analytes.

    Science.gov (United States)

    Warren, Alexander D; Conway, Ulric; Arthur, Christopher J; Gates, Paul J

    2016-07-01

    The analysis of low molecular weight compounds by matrix-assisted laser desorption/ionisation mass spectrometry is problematic due to the interference and suppression of analyte ionisation by the matrices typically employed - which are themselves low molecular weight compounds. The application of colloidal graphite is demonstrated here as an easy to use matrix that can promote the ionisation of a wide range of analytes including low molecular weight organic compounds, complex natural products and inorganic complexes. Analyte ionisation with colloidal graphite is compared with traditional organic matrices along with various other sources of graphite (e.g. graphite rods and charcoal pencils). Factors such as ease of application, spectra reproducibility, spot longevity, spot-to-spot reproducibility and spot homogeneity (through single spot imaging) are explored. For some analytes, considerable matrix suppression effects are observed resulting in spectra completely devoid of matrix ions. We also report the observation of radical molecular ions [M(-●) ] in the negative ion mode, particularly with some aromatic analytes. Copyright © 2016 John Wiley & Sons, Ltd. PMID:27434807

  1. Atomic force microscopy as analytical tool to study physico-mechanical properties of intestinal cells

    Directory of Open Access Journals (Sweden)

    Christa Schimpel

    2015-07-01

    Full Text Available The small intestine is a complex system that carries out various functions. The main function of enterocytes is absorption of nutrients, whereas membranous cells (M cells are responsible for delivering antigens/foreign substances to the mucosal lymphoid tissues. However, to get a fundamental understanding of how cellular structures contribute to physiological processes, precise knowledge about surface morphologies, cytoskeleton organizations and biomechanical properties is necessary. Atomic force microscopy (AFM was used here as a powerful tool to study surface topographies of Caco-2 cells and M cells. Furthermore, cell elasticity (i.e., the mechanical response of a cell on a tip indentation, was elucidated by force curve measurements. Besides elasticity, adhesion was evaluated by recording the attraction and repulsion forces between the tip and the cell surface. Organization of F-actin networks were investigated via phalloidin labeling and visualization was performed with confocal laser scanning fluorescence microscopy (CLSM and scanning electron microscopy (SEM. The results of these various experimental techniques revealed significant differences in the cytoskeleton/microvilli arrangements and F-actin organization. Caco-2 cells displayed densely packed F-actin bundles covering the entire cell surface, indicating the formation of a well-differentiated brush border. In contrast, in M cells actins were arranged as short and/or truncated thin villi, only available at the cell edge. The elasticity of M cells was 1.7-fold higher compared to Caco-2 cells and increased significantly from the cell periphery to the nuclear region. Since elasticity can be directly linked to cell adhesion, M cells showed higher adhesion forces than Caco-2 cells. The combination of distinct experimental techniques shows that morphological differences between Caco-2 cells and M cells correlate with mechanical cell properties and provide useful information to understand

  2. Determination of platinum traces contamination by graphite furnace atomic absorption spectrometry after preconcentration by cloud point extraction

    International Nuclear Information System (INIS)

    A simple and sensitive method is described for the determination of platinum surface contamination originating from cisplatin, carboplatin and oxaliplatin. Following extraction from swabs and preconcentration with the cloud point extraction (CPE) method, detection was by graphite furnace atomic absorption spectrometry (GFAAS). After desorption of platinum compounds from the swab, CPE involved on preconcentration of platinum in aqueous solution with diethyldithiocarbamate (DDTC) as chelating agent and Triton X-114 as extraction medium. DDTC is not only a chelating agent, but may also be a good candidate for the inactivation of platinum compounds. DDTC is recommended by the Word Health Organization (WHO) for the destruction of platinum-based anticancer drugs. The main factors affecting CPE efficiency, pH of the sample solution, concentrations of DDTC and Triton X-114, equilibration temperature and incubation time, were evaluated in order to enhance sensitivity of the method. The desorption of platinum compounds from the swab was investigated in parallel. Since platinum is bound to DDTC, it must exchange with copper in order to enhance platinum atomizing by GFAAS. A preconcentration factor of 29 was obtained for 10 mL of a platinum solution at 10 μg mL-1. In optimal conditions, the limit of detection was 0.2 ng mL-1, corresponding to 2.0 ng of platinum metal on the swab. Absorbance was linear between 0.7 and 15 ng mL-1. The proposed method was applied for the determination of surface contamination by platinum compounds with correct results.

  3. Determination of mercury in gasoline by cold vapor atomic absorption spectrometry with direct reduction in microemulsion media

    International Nuclear Information System (INIS)

    The determination of Hg in gasoline by cold vapor atomic absorption spectrometry, after direct aqueous NaBH4 reduction in a three-component (microemulsion) medium, was investigated. Microemulsions were prepared by mixing gasoline with propan-1-ol and 50% v / v HNO3 at a 20 : 15 : 1 volume ratio. A long-term homogeneous system was immediately formed this way. After reduction, the Hg vapor generated in a reaction flask was transported to an intermediate K2Cr2O7/H2SO4 trap solution in order to avoid poisoning of the Au-Pt trap by the gasoline vapors. A second reduction step was then conducted and the generated Hg vapor transported to the Au-Pt trap, followed by thermal release of Hg0 and atomic absorption measurement. Purified N2 was used as purge and transport gas. After multivariate optimization by central composite design calibration graphs showed coefficients of correlation of 0.9999 and a characteristic mass of 2 ng was obtained. Typical coefficients of variation of 5% and 6% were found for ten consecutive measurements at concentration levels of 1 and 8 μg L-1 of Hg2+, respectively. The limit of detection was 0.10 μg L-1 (0.14 μg kg-1) in the original sample. A total measurement cycle took 11 min, permitting duplicate analysis of 3 samples per hour. The results obtained with the proposed procedure in the analysis of commercial gasoline samples were in agreement with those obtained by a comparative procedure. Gasoline samples of the Rio de Janeiro city have shown Hg concentrations below 0.27 μg L-1

  4. Study of matrix effects produced by inorganic species in inductively coupled plasma atomic emission spectrometry with several spray chambers

    International Nuclear Information System (INIS)

    In the present work, the influence of the spray chamber design on the matrix effects was investigated in Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). The study was carried out in terms of aerosol drop size distribution and emission signal. Solutions of two inorganic acids and salts were employed to characterize the extent of the matrix effects throughout this work. Several spray chambers. a double-pass (Scott - type), a conventional cyclonic, and two low-volume cyclonic - type spray chambers (i.e., Cinnabar, and Genie) were used in order to evaluate the matrix effects produced by nitric and sulphuric acid solutions. A glass concentric pneumatic micro nebulizer (Atom Mist) was used in conjunction with all four chambers. When nitric or sulphuric acid solutions were nebulized, the double pass spray chamber registered noticeable changes in the drop size distribution. The low-volume spray chambers, in turn, afforded changes in the aerosol drop size distributions similar to the conventional cyclonic one. The matrix effects on the signal were reduced with all three cyclonic spray chambers with respect to the double pass one. Concerning the effect of inorganic salts, the results obtained with a High Efficiency Nebulizer (HEN) coupled to a double pass spray chamber and to a cyclonic type one revealed several issues: (i) the matrix effects were more severe at low liquid and gas flow rates; (ii) as for inorganic acids, the use of a cyclonic spray chamber led to a mitigation of the matrix effects with respect to a double pass spray chamber. (author)

  5. Determination of platinum traces contamination by graphite furnace atomic absorption spectrometry after preconcentration by cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Chappuy, M. [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France); Caudron, E., E-mail: eric.caudron@eps.aphp.fr [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France); Groupe de Chimie Analytique de Paris-Sud, EA 4041, IFR 141, School of Pharmacy, Univ Paris-Sud, 92296 Chatenay-Malabry (France); Bellanger, A. [Department of Pharmacy, Pitie-Salpetriere Hospital (Paris Public Hospital Authority), 47 boulevard de l' hopital, 75013 Paris (France); Pradeau, D. [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France)

    2010-04-15

    A simple and sensitive method is described for the determination of platinum surface contamination originating from cisplatin, carboplatin and oxaliplatin. Following extraction from swabs and preconcentration with the cloud point extraction (CPE) method, detection was by graphite furnace atomic absorption spectrometry (GFAAS). After desorption of platinum compounds from the swab, CPE involved on preconcentration of platinum in aqueous solution with diethyldithiocarbamate (DDTC) as chelating agent and Triton X-114 as extraction medium. DDTC is not only a chelating agent, but may also be a good candidate for the inactivation of platinum compounds. DDTC is recommended by the Word Health Organization (WHO) for the destruction of platinum-based anticancer drugs. The main factors affecting CPE efficiency, pH of the sample solution, concentrations of DDTC and Triton X-114, equilibration temperature and incubation time, were evaluated in order to enhance sensitivity of the method. The desorption of platinum compounds from the swab was investigated in parallel. Since platinum is bound to DDTC, it must exchange with copper in order to enhance platinum atomizing by GFAAS. A preconcentration factor of 29 was obtained for 10 mL of a platinum solution at 10 {mu}g mL{sup -1}. In optimal conditions, the limit of detection was 0.2 ng mL{sup -1}, corresponding to 2.0 ng of platinum metal on the swab. Absorbance was linear between 0.7 and 15 ng mL{sup -1}. The proposed method was applied for the determination of surface contamination by platinum compounds with correct results.

  6. Determination of mercury in gasoline by cold vapor atomic absorption spectrometry with direct reduction in microemulsion media

    Science.gov (United States)

    Brandão, Geisamanda Pedrini; de Campos, Reinaldo Calixto; Luna, Aderval Severino

    2005-06-01

    The determination of Hg in gasoline by cold vapor atomic absorption spectrometry, after direct aqueous NaBH 4 reduction in a three-component (microemulsion) medium, was investigated. Microemulsions were prepared by mixing gasoline with propan-1-ol and 50% v / v HNO 3 at a 20 : 15 : 1 volume ratio. A long-term homogeneous system was immediately formed this way. After reduction, the Hg vapor generated in a reaction flask was transported to an intermediate K 2Cr 2O 7/H 2SO 4 trap solution in order to avoid poisoning of the Au-Pt trap by the gasoline vapors. A second reduction step was then conducted and the generated Hg vapor transported to the Au-Pt trap, followed by thermal release of Hg 0 and atomic absorption measurement. Purified N 2 was used as purge and transport gas. After multivariate optimization by central composite design calibration graphs showed coefficients of correlation of 0.9999 and a characteristic mass of 2 ng was obtained. Typical coefficients of variation of 5% and 6% were found for ten consecutive measurements at concentration levels of 1 and 8 μg L -1 of Hg 2+, respectively. The limit of detection was 0.10 μg L -1 (0.14 μg kg -1) in the original sample. A total measurement cycle took 11 min, permitting duplicate analysis of 3 samples per hour. The results obtained with the proposed procedure in the analysis of commercial gasoline samples were in agreement with those obtained by a comparative procedure. Gasoline samples of the Rio de Janeiro city have shown Hg concentrations below 0.27 μg L -1.

  7. Ultra-trace determination of methylmercuy in seafood by atomic fluorescence spectrometry coupled with electrochemical cold vapor generation.

    Science.gov (United States)

    Zu, Wenchuan; Wang, Zhenghao

    2016-03-01

    A homemade electrochemical flow cell was adopted for the determination of methylmercury. The cold vapor of mercury atoms was generated from the surface of glassycarbon cathode through the method of electrolytic reduction and detected by atomic fluorescence spectroscopy subsequently. The operating conditions were optimized with 2 ng mL(-1) methylmercury standard solution. The caliberation curve was favorably linear when the concentrations of standard HgCH3(+) solutions were in the range of 0.2-5 ng mL(-1)(as Hg). Under the optimized conditions, the limit of detection (LOD) for methylmercury was 1.88×10(-3)ng mL(-1) and the precision evaluated by relative standard deviation was 2.0% for six times 2 ng mL(-1) standard solution replicates. The terminal analytical results of seafood samples, available from local market, showed that the methylmercury content ranged within 3.7-45.8 ng g(-1). The recoveries for methylmercury spiked samples were found to be in the range of 87.6-103.6% and the relative standard deviations below 5% (n=6) were acquired, which showed this method was feasible for real sample analysis. PMID:26615576

  8. The determination of trace elements in crude oil and its heavy fractions by atomic spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Duyck, Christiane; Miekeley, Norbert; Porto da Silveira, Carmem L.; Aucelio, Ricardo Q. [Departamento de Quimica da Pontificia Universidade Catolica do Rio de Janeiro, Rua Marques de Sao Vicente 225, 22451-900 Rio de Janeiro (Brazil); Campos, Reinaldo C. [Departamento de Quimica da Pontificia Universidade Catolica do Rio de Janeiro, Rua Marques de Sao Vicente 225, 22451-900 Rio de Janeiro (Brazil)], E-mail: rccampos@rdc.puc-rio.br; Grinberg, Patricia; Brandao, Geisamanda P. [Departamento de Quimica da Pontificia Universidade Catolica do Rio de Janeiro, Rua Marques de Sao Vicente 225, 22451-900 Rio de Janeiro (Brazil)

    2007-09-15

    A literature review on the determination of trace elements in crude oil and heavy molecular mass fractions (saturates, aromatics, resins and asphaltenes) by ICP-MS, ICP OES and AAS is presented. Metal occurrences, forms and distributions are examined as well as their implications in terms of reservoir geochemistry, oil refining and environment. The particular analytical challenges for the determination of metals in these complex matrices by spectrochemical techniques are discussed. Sample preparation based on ashing, microwave-assisted digestion and combustion decomposition procedures is noted as robust and long used. However, the introduction of non-aqueous solvents and micro-emulsions into inductively coupled plasmas is cited as a new trend for achieving rapid and accurate analysis. Separation procedures for operationally defined fractions in crude oil are more systematically applied for the observation of metal distributions and their implications. Chemical speciation is of growing interest, achieved by the coupling of high efficiency separation techniques (e.g., HPLC and GC) to ICP-MS instrumentation, which allows the simultaneous determination of multiple organometallic species of geochemical and environmental importance.

  9. The determination of trace elements in crude oil and its heavy fractions by atomic spectrometry

    Science.gov (United States)

    Duyck, Christiane; Miekeley, Norbert; Porto da Silveira, Carmem L.; Aucélio, Ricardo Q.; Campos, Reinaldo C.; Grinberg, Patrícia; Brandão, Geisamanda P.

    2007-09-01

    A literature review on the determination of trace elements in crude oil and heavy molecular mass fractions (saturates, aromatics, resins and asphaltenes) by ICP-MS, ICP OES and AAS is presented. Metal occurrences, forms and distributions are examined as well as their implications in terms of reservoir geochemistry, oil refining and environment. The particular analytical challenges for the determination of metals in these complex matrices by spectrochemical techniques are discussed. Sample preparation based on ashing, microwave-assisted digestion and combustion decomposition procedures is noted as robust and long used. However, the introduction of non-aqueous solvents and micro-emulsions into inductively coupled plasmas is cited as a new trend for achieving rapid and accurate analysis. Separation procedures for operationally defined fractions in crude oil are more systematically applied for the observation of metal distributions and their implications. Chemical speciation is of growing interest, achieved by the coupling of high efficiency separation techniques (e.g., HPLC and GC) to ICP-MS instrumentation, which allows the simultaneous determination of multiple organometallic species of geochemical and environmental importance.

  10. Separation of seven arsenic compounds by high performance liquid chromatography with on-line detection by hydrogen-argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, Erik Huusfeldt; Pritzl, G.;

    1992-01-01

    Seven molecular forms of arsenic were separated by anion- and cation-exchange high-performance liquid chromatography (HPLC) with on-line detection by flame atomic absorption spectrometry (FAAS). The interfacing was established by a vented poly(tetrafluoroethylene) capillary tubing connecting......-to-noise ratio of the on-line AAS detector was optimized. This involved the use of the hydrogen-argon-entrained air flame, a slotted tube atom trap in the flame for signal enhancement, electronic noise damping and a high-intensity light source. The detection limits in mu-g cm-3, using 100 mm3 injections...

  11. Separation of seven arsenic compounds by high-performance liquid chromatography with on-line detection by hydrogen–argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, E. H.; Pritzl, G.;

    1992-01-01

    Seven molecular forms of arsenic were separated by anion- and cation-exchange high-performance liquid chromatography (HPLC) with on-line detection by flame atomic absorption spectrometry (FAAS). The interfacing was established by a vented poly(tetrafluoroethylene) capillary tubing connecting......-to-noise ratio of the on-line AAS detector was optimized. This involved the use of the hydrogen-argon-entrained air flame, a slotted tube atom trap in the flame for signal enhancement, electronic noise damping and a high-intensity light source. The detection limits in mu-g cm-3, using 100 mm3 injections...

  12. Determination of trace elements in refined gold samples by inductively coupled plasma atomic emission spectrometry

    Directory of Open Access Journals (Sweden)

    Steharnik Mirjana

    2013-01-01

    Full Text Available This paper presents a method for determination the trace contents of silver, copper, iron, palladium, zinc and platinum in refined gold samples. Simultaneous inductively coupled plasma atomic emission spectrometer with radial torch position and cross flow nebulizer was used for determination. In order to compare the different calibration strategies, two sets of calibration standards were prepared. The first set was based on matrix matched calibration standards and the second was prepared without the addition of matrix material. Detection limits for matrix matching calibrations were higher for some elements than those without matrix matching. In addition, the internal standardization method was applied and experiments indicated that indium was the best option as internal standard. The obtained results for gold sample by matrix matching and matrix free calibrations were compared with the obtained results by standard addition method. The accuracy of the methods was tested performing recovery test. Recoveries for spiked sample were in the range of 90-115 %. The accuracy of the methods was also tested by analysis of certified reference material of high pure goldAuGHP1. The best results were achieved by matrix free calibration and standard addition method using indium as internal standard at wavelength of 230 nm. [Projekat Ministarstva nauke Republike Srbije, br. 34024: Development of Technologies for Recycling of Precious, Rare and Associated Metals from Solid Waste in Serbia to High Purity Products

  13. Different Analytical Procedures for the Study of Organic Residues in Archeological Ceramic Samples with the Use of Gas Chromatography-mass Spectrometry.

    Science.gov (United States)

    Kałużna-Czaplińska, Joanna; Rosiak, Angelina; Kwapińska, Marzena; Kwapiński, Witold

    2016-01-01

    The analysis of the composition of organic residues present in pottery is an important source of information for historians and archeologists. Chemical characterization of the materials provides information on diets, habits, technologies, and original use of the vessels. This review presents the problem of analytical studies of archeological materials with a special emphasis on organic residues. Current methods used in the determination of different organic compounds in archeological ceramics are presented. Particular attention is paid to the procedures of analysis of archeological ceramic samples used before gas chromatography-mass spectrometry. Advantages and disadvantages of different extraction methods and application of proper quality assurance/quality control procedures are discussed. PMID:25830900

  14. Determination of methylmercury by electrothermal atomic absorption spectrometry using headspace single-drop microextraction with in situ hydride generation

    International Nuclear Information System (INIS)

    A new method is proposed for preconcentration and matrix separation of methylmercury prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Generation of methylmercury hydride (MeHgH) from a 5-ml solution is carried out in a closed vial and trapped onto an aqueous single drop (3-μl volume) containing Pd(II) or Pt(IV) (50 and 10 mg/l, respectively). The hydrogen evolved in the headspace (HS) after decomposition of sodium tetrahydroborate (III) injected for hydride generation caused the formation of finely dispersed Pd(0) or Pt(0) in the drop, which in turn, were responsible for the sequestration of MeHgH. A preconcentration factor of ca. 40 is achieved with both noble metals used as trapping agents. The limit of detection of methylmercury was 5 and 4 ng/ml (as Hg) with Pd(II) or Pt(IV) as trapping agents, and the precision expressed as relative standard deviation was about 7%. The preconcentration system was fully characterised through optimisation of the following variables: Pd(II) or Pt(IV) concentration in the drop, extraction time, pH of the medium, temperatures of both sample solution and drop, concentration of salt in the sample solution, sodium tetrahydroborate (III) concentration in the drop and stirring rate. The method has been successfully validated against two fish certified reference materials (CRM 464 tuna fish and CRM DORM-2 dogfish muscle) following selective extraction of methylmercury in 2 mol/l HCl medium

  15. Evaluation of four sample treatments for determination of platinum in automotive catalytic converters by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Conventional and microwave assisted digestion, both using aqua regia, alkaline fusion with lithium metaborate and aqueous slurries were evaluated as sample treatments for determination of Pt in automotive catalytic converters by Graphite Furnace Atomic Absorption Spectrometry (GF-AAS). Determination of platinum by GF-AAS in samples of the catalytic converter's substrates, prepared by the four methods described, indicates that the highest platinum concentration i.e. maximum Pt extraction in the range of 748 ± 15-998 ± 10 μg mL-1, is obtained for samples dissolved by alkaline fusion, closely followed by analysis of aqueous plus Triton X-100 slurries 708 ± 14-958 ± 10 μg mL-1, while neither one of the acid digestion procedures achieved total dissolution of the samples. Slurry analysis is thus shown to be a viable alternative and is recommended, based on its speed and ease of implementation. Aqueous standards calibration curves and the standard addition methods were also compared. The results showed that no appreciable matrix effects are present, regardless of the sample preparation procedure used. Precision of the measurements, expressed as percentage relative standard deviation, ranged between 2.5 to 4.9%. Accuracy of the results was assessed by recovery tests which rendered values between 98.9 and 100.9%

  16. Determination of micro yttrium in an ytterbium matrix by inductively coupled plasma atomic emission spectrometry and wavelet transform

    Institute of Scientific and Technical Information of China (English)

    MA Xiaoguo

    2005-01-01

    In the determination of trace yttrium (Y) in an ytterbium (Yb) matrix by inductively coupled plasma atomic emission spectrometry (ICP-AES), the most prominent line of yttrium, Y 371.030 nm line, suffers from strong interference due to an emission line of ytterbium. In this work, a method based on wavelet transform was proposed for the spectral interference correction. Haar wavelet was selected as the mother wavelet. The discrete detail after the third decomposition, D3,was chosen for quantitative analysis based on the consideration of both separation degree and peak height. The linear correlation coefficient between the height of the left positive peak in D3 and the concentration of Y was calculated to be 0.9926.Six synthetic samples were analyzed, and the recovery for yttrium varied from 96.3% to 110.0%. The amounts of yttrium in three ytterbium metal samples were determined by the proposed approach with an average relative standard deviation (RSD)of 2.5%, and the detection limit for yttrium was 0.016%. This novel correction technique is fast and convenient, since neither complicated model assumption nor time-consuming iteration is required. Furthermore, it is not affected by the wavelength drift inherent in monochromators that will severely reduce the accuracy of results obtained by some chemometric methods.

  17. Determination of ultra-trace aluminum in human albumin by cloud point extraction and graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A cloud point extraction (CPE) method for the preconcentration of ultra-trace aluminum in human albumin prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) had been developed in this paper. The CPE method was based on the complex of Al(III) with 1-(2-pyridylazo)-2-naphthol (PAN) and Triton X-114 was used as non-ionic surfactant. The main factors affecting cloud point extraction efficiency, such as pH of solution, concentration and kind of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time, were investigated in detail. An enrichment factor of 34.8 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of Al(III) was 0.06 ng mL-1. The relative standard deviation (n = 7) of sample was 3.6%, values of recovery of aluminum were changed from 92.3% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to the determination of ultra-trace aluminum in human albumin.

  18. Determination of total arsenic in coal and wood using oxygen flask combustion method followed by hydride generation atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A simple and sensitive procedure for the determination of total arsenic in coal and wood was conducted by use of oxygen flask combustion (OFC) followed by hydride generation atomic absorption spectrometry (HGAAS). The effect of various items (composition of absorbent, standing time between the combustion and filtration, particle size and mass of sample) was investigated. Under the optimized conditions of the OFC method, nine certified reference materials were analyzed, and the values of arsenic concentration obtained by this method were in good accordance with the certified values. The limit of detection (LOD) and relative standard deviation (RSD) of the method were 0.29 μg g-1 and less than 8%, respectively. In addition, eight kinds of coals and four chromated copper arsenate (CCA)-treated wood wastes were analyzed by the present method, and the data were compared to those from the microwave-acid digestion (MW-AD) method. The determination of arsenic in solid samples was discussed in terms of applicable scope and concentration range of arsenic.

  19. Determination of lead in environmental waters with dispersive liquid-liquid microextraction prior to atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Qingxiang, E-mail: zhouqx@cup.edu.cn [School of Chemistry and Environmental Sciences, Henan Normal University, Henan Key Laboratory for Environmental Pollution Control, Key Laboratory for Yellow River and Huaihe River Water Environment and Pollution Control, Ministry of Education, Xinxiang 453007 (China); State Laboratory of Petroleum Resource and Prospecting, College of Geosciences, China University of Petroleum Beijing, Beijing 102249 (China); Zhao, Na [State Laboratory of Petroleum Resource and Prospecting, College of Geosciences, China University of Petroleum Beijing, Beijing 102249 (China); Xie, Guohong [College of Resources and Environment, Henan Institute of Science and Technology, Xinxiang 453003 (China)

    2011-05-15

    This paper established a new, rapid and sensitive method for the determination of lead in water samples preconcentrated by dispersive liquid-liquid microextraction (DLLME) prior to atomic fluorescence spectrometry. Dithizone was used as the chelating agent. In the DLLME procedure, lead formed lead-dithizone complex and migrated into the carbon tetrachloride micro-droplets. Important factors that would affect the extraction efficiency had been investigated including the kind and volume of extraction solvent and dispersive solvent, sample pH, the amount of chelating agent, extraction time and centrifugation time. The results showed that the coexisting ions containing in water samples had no obvious negative effect on the determination of lead. The experimental results indicated that the proposed method had a good linear range of 0.01-100 ng mL{sup -1} (r{sup 2} = 0.9990). The precision was 2.12% (RSD, n = 7) and the detection limit was 0.95 ng L{sup -1}. Proposed method was validated with four real environmental samples and the results indicated that the proposed method was excellent for the future use and satisfied spiked recoveries were in the range of 92.9-97.4%.

  20. Determination of lead in environmental waters with dispersive liquid-liquid microextraction prior to atomic fluorescence spectrometry.

    Science.gov (United States)

    Zhou, Qingxiang; Zhao, Na; Xie, Guohong

    2011-05-15

    This paper established a new, rapid and sensitive method for the determination of lead in water samples preconcentrated by dispersive liquid-liquid microextraction (DLLME) prior to atomic fluorescence spectrometry. Dithizone was used as the chelating agent. In the DLLME procedure, lead formed lead-dithizone complex and migrated into the carbon tetrachloride micro-droplets. Important factors that would affect the extraction efficiency had been investigated including the kind and volume of extraction solvent and dispersive solvent, sample pH, the amount of chelating agent, extraction time and centrifugation time. The results showed that the coexisting ions containing in water samples had no obvious negative effect on the determination of lead. The experimental results indicated that the proposed method had a good linear range of 0.01-100 ng mL(-1) (r(2) = 0.9990). The precision was 2.12% (RSD, n = 7) and the detection limit was 0.95 ng L(-1). Proposed method was validated with four real environmental samples and the results indicated that the proposed method was excellent for the future use and satisfied spiked recoveries were in the range of 92.9-97.4%. PMID:21398026

  1. Ultrasensitive determination of mercury in human saliva by atomic fluorescence spectrometry based on solidified floating organic drop microextraction

    International Nuclear Information System (INIS)

    We report on a new, rapid and simple method for the determination of ultra-trace quantities of mercury ion in human saliva. It is based on solidified floating organic drop microextraction and detection by cold vapor atomic fluorescence spectrometry (CV-AFS). Mercury ion was complexed with diethyldithiocarbamate, and the hydrophobic complex was then extracted into fine droplets of 1-undecanol. By cooling in an ice bath after extraction, the droplets in solution solidify to form a single ball floating on the surface of solution. The solidified micro drop containing the mercury complex was then transferred for determination by CV-AFS. The effects of pH value, concentration of chelating reagent, quantity of 1-undecanol, sample volume, equilibration temperature and time were investigated. Under the optimum conditions, the preconcentration of a 25-mL sample is accomplished with an enrichment factor of 182. The limit of detection is 2.5 ng L-1. The relative standard deviation for seven replicate determinations at 0.1 ng mL-1 level is 4.1%. The method was applied to the determination of mercury in saliva samples collected from four volunteers. Two volunteers having dental amalgam fillings had 0.4 ng mL-1 mercury in their saliva, whereas mercury was not detectable in the saliva of two volunteers who had no dental fillings. (author)

  2. An automatic countercurrent liquid-liquid micro-extraction system coupled with atomic absorption spectrometry for metal determination.

    Science.gov (United States)

    Mitani, Constantina; Anthemidis, Aristidis N

    2015-02-01

    A novel and versatile automatic sequential injection countercurrent liquid-liquid microextraction (SI-CC-LLME) system coupled with atomic absorption spectrometry (FAAS) is presented for metal determination. The extraction procedure was based on the countercurrent flow of aqueous and organic phases which takes place into a newly designed lab made microextraction chamber. A noteworthy feature of the extraction chamber is that it can be utilized for organic solvents heavier or lighter than water. The proposed method was successfully demonstrated for on-line lead determination and applied in environmental water samples using an amount of 120 μL of chloroform as extractant and ammonium diethyldithiophosphate as chelating reagent. The effect of the major experimental parameters including the volume of extractant, as well as the flow rate of aqueous and organic phases were studied and optimized. Under the optimum conditions for 6 mL sample consumption an enhancement factor of 130 was obtained. The detection limit was 1.5 μg L(-1) and the precision of the method, expressed as relative standard deviation (RSD) was 2.7% at 40.0 μg L(-1) Pb(II) concentration level. The proposed method was evaluated by analyzing certified reference materials and spiked environmental water samples. PMID:25435230

  3. Preconcentration procedure using cloud point extraction in the presence of electrolyte for cadmium determination by flame atomic absorption spectrometry

    Science.gov (United States)

    Coelho, Luciana Melo; Arruda, Marco Aurélio Zezzi

    2005-06-01

    This paper describes a micelle-mediated phase separation in the presence of electrolyte as a preconcentration method for cadmium determination by flame atomic absorption spectrometry (FAAS). Cadmium was complexed with ammonium O,O-diethyldithiophosphate (DDTP) in an acidic medium (0.32 mol l- 1 HCl) using Triton X-114 as surfactant and quantitatively extracted into a small volume (about 20 μl) of the surfactant-rich phase after centrifugation. The chemical variables that affect the cloud point extraction, such as complexing time (0 20 min), Triton X114 concentration (0.043 0.87% w/v) and complexing agent concentration (0.01 0.1 mol l- 1), were investigated. The cloud point is formed in the presence of NaCl at room temperature (25 °C), and the electrolyte concentration (0.5 5% w/v) was also investigated. Under optimized conditions, only 8 ml of sample was used in the presence of 0.043% w/v Triton X-114 and 1% (w/v) NaCl. This method permitted limits of detection and quantification of 0.9 μg l- 1 and 2.9 μg l- 1 Cd, respectively, and a linear calibration range from 3 to 400 μg l- 1 Cd. The proposed method was applied to Cd determination in physiological solutions (containing 0.9% (w/v) of NaCl), mineral water, lake water and cigarette samples (tobacco).

  4. Determination of ultra-trace aluminum in human albumin by cloud point extraction and graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sun Mei, E-mail: sunmei@ustc.edu.cn [Hefei National Laboratory for Physical Sciences on Microscale, University of Science and Technology of China, No. 96, Jinzhai Road, Hefei 230026 (China); Wu Qianghua [Department of Polymer Science and Engineering, University of Science and Technology of China, Hefei 230026 (China)

    2010-04-15

    A cloud point extraction (CPE) method for the preconcentration of ultra-trace aluminum in human albumin prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) had been developed in this paper. The CPE method was based on the complex of Al(III) with 1-(2-pyridylazo)-2-naphthol (PAN) and Triton X-114 was used as non-ionic surfactant. The main factors affecting cloud point extraction efficiency, such as pH of solution, concentration and kind of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time, were investigated in detail. An enrichment factor of 34.8 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of Al(III) was 0.06 ng mL{sup -1}. The relative standard deviation (n = 7) of sample was 3.6%, values of recovery of aluminum were changed from 92.3% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to the determination of ultra-trace aluminum in human albumin.

  5. Cloud point extraction-flame atomic absorption spectrometry method for preconcentration and determination of trace cadmium in water samples.

    Science.gov (United States)

    Ning, Jinyan; Jiao, Yang; Zhao, Jiao; Meng, Lifen; Yang, Yaling

    2014-01-01

    A method based on cloud point extraction (CPE) separation/preconcentration of trace cadmium (Cd) as a prior step to its determination by flame atomic absorption spectrometry has been developed. Cadmium reacted with 8-hydroxyquinoline to form hydrophobic chelates, which were extracted into the micelles of nonionic surfactant oligoethylene glycol monoalkyl ether (Genapol X-080) in an alkaline medium. Octanol was used to depress the cloud point of Genapol X-080 in the extraction process. The chemical variables that affect the CPE, such as pH of complexation reaction, amount of chelating agent, Genapol X-080 and octanol were evaluated and optimized. Under optimized conditions, linearity was obeyed in the range of 10-500 μg/L, with the correlation coefficient of 0.9993. For 5 mL of sample solution, the enhancement factor was about 20. The limit of detection and limit of quantification of the method were 0.21 and 0.63 μg/L, respectively. The relative standard deviations (n = 6) was 3.2% for a solution containing 100 μg/L of Cd. The accuracy of the preconcentration system was evaluated by recovery measurements on spiked water samples. Recoveries of spiked samples varied in the range of 94.1-103.8%.

  6. Cloud point extraction for trace inorganic arsenic speciation analysis in water samples by hydride generation atomic fluorescence spectrometry

    Science.gov (United States)

    Li, Shan; Wang, Mei; Zhong, Yizhou; Zhang, Zehua; Yang, Bingyi

    2015-09-01

    A new cloud point extraction technique was established and used for the determination of trace inorganic arsenic species in water samples combined with hydride generation atomic fluorescence spectrometry (HGAFS). As(III) and As(V) were complexed with ammonium pyrrolidinedithiocarbamate and molybdate, respectively. The complexes were quantitatively extracted with the non-ionic surfactant (Triton X-114) by centrifugation. After addition of antifoam, the surfactant-rich phase containing As(III) was diluted with 5% HCl for HGAFS determination. For As(V) determination, 50% HCl was added to the surfactant-rich phase, and the mixture was placed in an ultrasonic bath at 70 °C for 30 min. As(V) was reduced to As(III) with thiourea-ascorbic acid solution, followed by HGAFS. Under the optimum conditions, limits of detection of 0.009 and 0.012 μg/L were obtained for As(III) and As(V), respectively. Concentration factors of 9.3 and 7.9, respectively, were obtained for a 50 mL sample. The precisions were 2.1% for As(III) and 2.3% for As(V). The proposed method was successfully used for the determination of trace As(III) and As(V) in water samples, with satisfactory recoveries.

  7. Determination of Trace Amounts of Nickel (Ⅱ) by Graphite Furnace Atomic Absorption Spectrometry Coupled with Cloud Point Extraction

    Institute of Scientific and Technical Information of China (English)

    SHAH Syed Mazhar; WANG Hao-nan; SU Xing-guang

    2011-01-01

    A new method based on the cloud point extraction(CPE) for separation and preconcentration of nickel(Ⅱ)and its subsequent determination by graphite furnace atomic absorption spectrometry(GFAAS) was proposed,8-hydroxyquinoline and Triton X-100 were usedl as the ligand and surfactant respectively. Nickel(Ⅱ) can form a hydrophobic complex with 8-hydroxyquinoline, the complex can be extracted into the small volume surfactant rich phase at the cloud point temperature(CPT) for GFAAS determination. The factors affecting the cloud point extraction,such as pH, ligand concentration, surfactant concentration, and the incubation time were optimized. Under the optimal conditions, a detection limit of 12 ng/L and a relative standard deviation(RSD) of 2.9% were obtained for Ni(Ⅱ) determination. The enrichment factor was found to be 25. The proposed method was successfully applied to the determination of nickel(Ⅱ) in certified reference material and different types of water samples and the recovery was in a range of 95% 103%.

  8. Determination of trace nickel in water samples by cloud point extraction preconcentration coupled with graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sun Zhimei [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China); Department of Chemistry and Biology, Huainan Normal University, Huainan 232001 (China); Liang Pei [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China)]. E-mail: liangpei@mail.ccnu.edu.cn; Ding Qiong [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China); Cao Jing [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China)

    2006-09-21

    A new method based on the cloud point extraction (CPE) preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the determination of trace nickel in water samples. When the micelle solution temperature is higher than the cloud point of surfactant p-octylpolyethyleneglycolphenyether (Triton X-100), the complex of Ni{sup 2+} with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) could enter surfactant-rich phase and be concentrated, then determined by GFAAS. The main factors affecting the cloud point extraction were investigated in detail. An enrichment factor of 27 was obtained for the preconcentration of Ni{sup 2+} with 10 mL solution. Under the optimal conditions, the detection limit of Ni{sup 2+} is 0.12 ng mL{sup -1} with R.S.D. of 4.3% (n = 10, c = 100 ng mL{sup -1}). The proposed method was applied to determination of trace nickel in water samples with satisfactory results.

  9. Evaluation of four sample treatments for determination of platinum in automotive catalytic converters by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Puig, Ana I.; Alvarado, José I.

    2006-09-01

    Conventional and microwave assisted digestion, both using aqua regia, alkaline fusion with lithium metaborate and aqueous slurries were evaluated as sample treatments for determination of Pt in automotive catalytic converters by Graphite Furnace Atomic Absorption Spectrometry (GF-AAS). Determination of platinum by GF-AAS in samples of the catalytic converter's substrates, prepared by the four methods described, indicates that the highest platinum concentration i.e. maximum Pt extraction in the range of 748 ± 15-998 ± 10 μg mL - 1 , is obtained for samples dissolved by alkaline fusion, closely followed by analysis of aqueous plus Triton X-100 slurries 708 ± 14-958 ± 10 μg mL - 1 , while neither one of the acid digestion procedures achieved total dissolution of the samples. Slurry analysis is thus shown to be a viable alternative and is recommended, based on its speed and ease of implementation. Aqueous standards calibration curves and the standard addition methods were also compared. The results showed that no appreciable matrix effects are present, regardless of the sample preparation procedure used. Precision of the measurements, expressed as percentage relative standard deviation, ranged between 2.5 to 4.9%. Accuracy of the results was assessed by recovery tests which rendered values between 98.9 and 100.9%.

  10. Cadmium and lead determination in foods by beam injection flame furnace atomic absorption spectrometry after ultrasound-assisted sample preparation

    International Nuclear Information System (INIS)

    A simple method for cadmium and lead determination in foods by beam injection flame furnace atomic absorption spectrometry (BIFF-AAS) was proposed. Food slurries were prepared by transferring an exact amount of cryogenic-ground homogenized material (50-100 mg) to centrifuge tubes, followed by addition of 5 ml (up to 2.8 mol l-1) nitric acid solution and sonication in an ultrasonic bath during 5-10 min. Thereafter, slurries were diluted with water to 10 ml, centrifuged during 5 min at 5400 rpm and 400 μl aliquot of the supernatant was analyzed by BIFF-AAS. The detection limits based on peak height measurements were 0.03 μg g-1 Cd and 1.6 μg g-1 Pb for 2% (m/v) slurry (200 mg/10 ml). For method validation, the certified reference materials Pig Kidney (BCR 186) and Rice Flour (NIES 10) were used. Quantitative cadmium and lead recoveries were obtained and no statistical differences were found at 95% level by applying the t-test

  11. Cloud Point Extraction Using Tergitol TMN-6 of Gold(III)in Real Samples by Flame Atomic Absorption Spectrometry Determination

    International Nuclear Information System (INIS)

    A simple, safe and rapid method on the basis of cloud point extraction (CPE) with tergitol TMN-6 had been used for the preconcentration and extraction of gold(Au) ion in selenium reduction solution sample prior to flame atomic absorption spectrometry (FAAS).Pyrrolidine dithio formic acid salt (PDFAS) which was regarded as a selective complexing agent could formed stable Au-complex with Au ion, and Au-complex could be extracted by TMN-6 at a short time. Some influencing factors such as sample pH, concentration of TMN-6, concentration of PDFAS and the effect of foreign ions were further researched .Under the optimum conditions, the limit of detection (LOD) was 1.3 meu g L/sup -1/, the calibration graph was linear in the range of 0-500 meu g/L and the relative standard deviation (RSD%) was 2.0%(n=8). The CPE method had been shown to be a useful and effective methodology for the separation of Au, with a preconcentration factor of 30. The recoveries of the spiked Au(?) ions were got in the range 95-103%. (author)

  12. Investigation of the levels of some element in edible oil samples produced in Turkey by atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mendil, Durali, E-mail: dmendil@gop.edu.tr [Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Uluoezlue, Ozguer Dogan; Tuezen, Mustafa [Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Soylak, Mustafa [Erciyes University, Faculty of Science and Arts, Department of Chemistry, 38039 Kayseri (Turkey)

    2009-06-15

    The element contents (Fe, Mn, Zn, Cu, Pb, Co, Cd, Na, K, Ca and Mg) in edible oils (olive oil, hazelnut oil, sunflower oil, margarine, butter and corn oil) from Turkey were determined using atomic absorption spectrometry after microwave digestion. The concentrations of trace element in the samples were found to be 291.0-52.0, 1.64-0.04, 3.08-1.03, 0.71-0.05, 0.03-0.01, 1.30-0.50, 84.0-0.90, 50.1-1.30, 174.2-20.8 and 20.8-0.60 {mu}g/g for iron, manganese, zinc, copper, lead, cobalt, sodium, potassium, calcium, and magnesium, respectively. Cadmium was found to be 4.57-0.09 {mu}g/kg. The high heavy metal and minerals accumulation levels in the samples were found in olive oil for Cu, Pb, Co, margarine for Fe, K, corn oil for Zn, Mn, butter for Na, Mg, sunflower oil for Ca and hazelnut oil for Cd, respectively.

  13. Determination of essential and toxic elements in commercial baby foods by instrumental neutron activation analysis and atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The World Health Organization recommends that infants should be breast fed exclusively for at least six months after birth. After this period, it is recommended to start introducing complementary foods, in order to meet the child's nutritional, mineral and energy needs. Commercial food products for infants form an important part of the diet for many babies. Thus, it is very important that such food contains sufficient amounts of minerals. Inadequate complementary feeding is a major cause of high rates of infant malnutrition in developing countries. In this study, essential elements: Ca, Cl, Co, Cr, Fe, K, Mg, Mn, Na, Se and Zn and toxic elements: As, Cd, Hg levels were determined in twenty seven different commercial infant food product samples by Instrumental Neutron Activation Analysis (INAA) and Atomic Absorption Spectrometry (AAS). In order to validate both methodologies the reference material: INCT MPH-2 Mixed Polish Herbs and NIST - SRM 1577b Bovine Liver by INAA and NIST - SRM 1548th Typical Diet and NIST - SRM 1547 Peach Leaves by AAS were analyzed. The twenty seven baby food samples were acquired from Sao Paulo city supermarkets and stores. Essential and toxic elements were determined. Most of the essential element concentrations obtained were lower than the World Health Organization requirements, while concentrations of toxic elements were below the tolerable upper limit. These low essential element concentrations in these samples indicate that infants should not be fed only with commercial complementary foods. (author)

  14. [Study on adsorption behavior of crosslinked polyarylonitrile for copper, lead, cadmium and zinc ions by atomic absorption spectrometry].

    Science.gov (United States)

    Shawket, Abliz; Peng, Yang; Wang, Ji-De; Ismayil, Nurulla

    2010-04-01

    The crosslinked polymer polyacrylonitrile was synthesized by suspension polymerization using acrylonitrile and divinylbenzene. It has been used as adsorbent of some toxic heavy metals in environmental waters. Its adsorption for metals and the factors which affect the adsorption capacity were studied by atomic absorption spectrometry (AAS). The experimental results showed that under the optimal adsorption conditions, the pH of adsorbate solution was 5-6, static adsorption time was 1.5-2 h, and adsorption procedure was carried out at room temperature, polyacrylonitrile as adsorbent has high adsorption capacity (mg x g(-1)) for Cu2+, Pb2+, Cd2+ and Zn2+, which can reach 26.6, 45.2, 39.7 and 32.5 separately. Adsorption rate (%) was 83.6, 87.1, 85.3 and 86.7 respectively during the 1.5-2 h static adsorption time. It will be more than five-hour static adsorption time before adsorption rate reaches more than 96%. Using 0.10 mol x L(-1) chloride acid as the best desorption solvent to desorb the adsorbates, the recovery of them reached 95%. At the same time the adsorption mechanism of polymer was studied. PMID:20545173

  15. The use of a sequential extraction procedure for heavy metal analysis of house dusts by atomic absorption spectrometry.

    Science.gov (United States)

    Altundag, Huseyin; Dundar, Mustafa Sahin; Doganci, Secil; Celik, Muhammed; Tuzen, Mustafa

    2013-01-01

    In general, dust is considered as house or street dust. Indoor dust, as a contamination source, has been studied for many years. In this work, the original Community Bureau of Reference of the European Commission (BCR) three-stage sequential extraction procedure was applied to the fractionation of Cr, Cu, Fe, Mn, Pb, and Zn in 20 house dust samples from five different areas of Sakarya, Turkey. Acetic acid, hydroxylammonium chloride, and hydrogen peroxide plus ammonium acetate were used for the first, second, and third steps of the BCR method, respectively. The extracts were analyzed for the studied heavy metals using flame atomic absorption spectrometry. Validation of the results was performed by using a standard reference material (BCR 701 Sediment) to certify the experimental results obtained and to evaluate the reliability of the method used. The elemental loadings typically increased in magnitude according to the area order: Izmit Caddesi>Ankara Caddesi >Erenler>Karaman>Korucuk. The results were in agreement with values reported in the literature.

  16. Analysis of trace element in intervertebral disc by Atomic Absorption Spectrometry techniques in degenerative disc disease in the Polish population

    Directory of Open Access Journals (Sweden)

    Andrzej Nowakowski

    2015-05-01

    Full Text Available Objective. Although trace elements are regarded crucial and their content has been determined in number of tissue there are only few papers addressing this problem in intervertebral disc in humans. Most of the trace elements are important substrates of enzymes influencing metabolism and senescence process. Others are markers of environmental pollution. Therefore the aim of the research was to analyzed of the trace element content in the intervertebral disc, which may be a vital argument recognizing the background of degenerative changes to be the effect of the environment or metabolic factors. Materials and methods. Material consist of 18 intervertebral disc from 15 patients, acquired in surgical procedure of due to the degenerative disease with Atomic Absorption Spectrometry content of Al, Cd, Co, Pb, Cu, Ni, Mo, Mg, Zn was evaluated. Results. Only 4 of the trace elements were detected in all samples. The correlation analysis showed significant positive age correlation with Al and negative in case of Co. Among elements significant positive correlation was observed between Al/Pb, Co/Mo, Al/Mg, Al/Zn Pb/Zn and Mg/Zn. Negative correlation was observed in Al/Co, Cd/Mg, Co/Mg, Mo/Mg, Co/Zn and Mo/Zn. Conclusions. This study is the first to our knowledge that profiles the elements in intervertebral disc in patients with degenerative changes. We have confirmed significant differences between the trace element contents in intervertebral disc and other tissue. It can be ground for further investigation.

  17. Selective quantification of trace palladium in road dusts and roadside soils by displacement solid-phase extraction online coupled with electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Fang, Jing; Jiang, Yan; Yan, Xiu-Ping; Ni, Zhe-Ming

    2005-01-01

    There is a growing concern about the effect of palladium on human health because of the toxicity and increasing occurrence of palladium as a result of its extensive use in automotive catalytic converters. Development of reliable analytical methodologies for the determination of palladium in environmental materials is of great importance for critical evaluation of the possible risks for human health. In this work, a displacement solid-phase extraction technique was developed and online coupled to electrothermal atomic absorption spectrometry (ETAAS) for selective and sensitive determination of trace palladium in environmental samples without need of any special selective complexing agents, selective sorbents, and masking agents. The developed methodology involved the online formation of copper pyrrolidine dithiocarbamate (Cu-PDC), and the resultant Cu-PDC was extracted onto a microcolumn packed with the sorbent from a cigarette filter. Trace Pd(II) was selectively preconcentrated through loading the sample solution onto the microcolumn by online displacement reaction between Pd(II) and the extracted Cu-PDC on the microcolumn. The retained analyte was subsequently eluted with 40 microL of ethanol for online ETAAS determination. Interferences from coexisting heavy metal ions with lower stability of their PDC complexes relative to Cu-PDC were minimized. The tolerable concentrations of Cd-(II), Fe(III), Co(II), Mn(II), Cr(III), and Zn(II) were up to 2, 6, 40, 2, 1.5, and at least 100 mg L(-1), respectively. Compared with conventional solid-phase extraction methodology, the developed displacement solid-phase extraction protocol gave 2-4 orders of magnitude improvement in the maximum tolerable concentrations of coexisting heavy metal ions. With the consumption of only 2.8 mL of sample solution, an enhancement factor of 52 and a detection limit (3sigma) of 18 ng L(-1) were achieved at a sample throughput of 30 samples h(-1). The precision (RSD, n = 13) was 2.5% at the 1

  18. On-line cloud point extraction combined with electrothermal vaporization inductively coupled plasma atomic emission spectrometry for the speciation of inorganic antimony in environmental and biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Li Yingjie [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)]. E-mail: binhu@whu.edu.cn; Jiang Zucheng [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2006-08-25

    A new method for the determination of inorganic Sb species by on-line cloud point extraction combined with electrothermal vaporization inductively coupled plasma atomic emission spectrometry (ETV-ICP-AES) is presented and evaluated. The method is based on the complexation of Sb(III) with pyrrolidine dithiocarbamate (PDC) which form an hydrophobic complex at pH 5.5 and subsequently enter surfactant-rich phase at pH 5.5, whereas Sb(V) remained in aqueous solutions. The preconcentration step is mediated by micelles of the non-ionic surfactant Triton X-114 with ammonium pyrrolidine dithiocarbamate (APDC). The micellar system containing the complex was loaded into the FIA manifold at a flow rate of 2.5 mL min{sup -1}, and the surfactant-rich phase was retained in a microcolumn packed with absorbent cotton, at pH 5.5. After the surfactant-rich phase was eluted with 100 {mu}L acetonitrile, it was determined by ETV-ICP-AES. Sb(V) is reduced to Sb(III) by L-cysteine prior to determined total Sb, and its assay is based on subtracting Sb(III) from total antimony. The main factors affecting separation/preconcentration and the vaporization behavior of analyte in graphite tube were investigated in detail. Under the optimized conditions, the precision relative standard deviation (R.S.D.) for eight replicate measurements of 0.2 {mu}g mL{sup -1} Sb(III) was 4.3%. The apparent concentration factor, which is defined as the concentration ratio of the analyte in the final diluted surfactant-rich extract ready for ETV-ICP-AES detection and in the initial solution, was 872 for Sb(III). The limit of detection (LOD) for Sb(III) was 0.09 {mu}g L{sup -1}. The proposed method was successfully applied for the speciation of inorganic antimony in different water samples and urine sample with satisfactory results.

  19. Method development for the determination of cadmium in fertilizer samples using high-resolution continuum source graphite furnace atomic absorption spectrometry and slurry sampling

    Energy Technology Data Exchange (ETDEWEB)

    Borges, Aline R. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq-INCT de Energia e Ambiente, Universidade Federal de Bahia, Salvador, BA (Brazil); Becker, Emilene M. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Lequeux, Celine [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Universite de Rennes 1, Rennes (France); Vale, Maria Goreti R., E-mail: mgrvale@ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq-INCT de Energia e Ambiente, Universidade Federal de Bahia, Salvador, BA (Brazil); Ferreira, Sergio L.C. [Instituto Nacional de Ciencia e Tecnologia do CNPq-INCT de Energia e Ambiente, Universidade Federal de Bahia, Salvador, BA (Brazil); Instituto de Quimica, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil); Welz, Bernhard [Instituto Nacional de Ciencia e Tecnologia do CNPq-INCT de Energia e Ambiente, Universidade Federal de Bahia, Salvador, BA (Brazil); Departamento de Quimica, Universidade Federal de Santa Catarina, Florianopolis, SC (Brazil)

    2011-07-15

    The determination of cadmium (Cd) in fertilizers is of major interest, as this element can cause growth problems in plants, and also affect animals and humans. High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) with charge-coupled device (CCD) array detection overcomes several of the limitations encountered with conventional line source AAS, especially the problem of accurate background measurement and correction. In this work an analytical method has been developed to determine Cd in fertilizer samples by HR-CS GF AAS using slurry sampling. Both a mixture of 10 {mu}g Pd + 6 {mu}g Mg in solution and 400 {mu}g of iridium as permanent modifier have been investigated and aqueous standards were used for calibration. Pyrolysis and atomization temperatures were 600 {sup o}C and 1600 {sup o}C for the Pd-Mg modifier, and 500 deg. C and 1600 deg. C for Ir, respectively. The results obtained for Cd in the certified reference material NIST SRM 695 (Trace Elements in Multi-Nutrient Fertilizer) of 16.7 {+-} 1.3 {mu}g g{sup -1} and 16.4 {+-} 0.75 {mu}g g{sup -1} for the Pd-Mg and Ir modifier, respectively, were statistically not different from the certified value of 16.9 {+-} 0.2 {mu}g g{sup -1} on a 95% confidence level; however, the results obtained with the Ir modifier were significantly lower than those for the Pd-Mg modifier for most of the samples. The characteristic mass was 1.0 pg for the Pd-Mg modifier and 1.1 pg Cd for the Ir modifier, and the correlation coefficients (R{sup 2}) of the calibration were > 0.99. The instrumental limits of detection were 7.5 and 7.9 ng g{sup -1}, and the limits of quantification were 25 and 27 ng g{sup -1} for Pd-Mg and Ir, respectively, based on a sample mass of 5 mg. The cadmium concentration in the investigated samples was between 0.07 and 5.5 {mu}g g{sup -1} Cd, and hence below the maximum value of 20 {mu}g g{sup -1} Cd permitted by Brazilian legislation.

  20. Continuous Determination of 12 Elements in Geochemical Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry and Flame Atomic Absorption Spectrometry%电感耦合等离子体发射光谱法和火焰原子吸收光谱法连续测定化探样品中12个元素

    Institute of Scientific and Technical Information of China (English)

    于阗; 张连起; 陈小迪

    2011-01-01

    The continuous determination of 12 elements in geochemical samples by inductive coupled plasma-atomic emission spectrometry (ICP-AES) and flame atomic absorption spectrometry ( FAAS) was reported in this paper. Samples were digested with mixed acid of HCI-HF-HNO3-HC1O4 and Cu, Pb, Zn, Co, Ni, Cr, Sr, Ba, V, Mn in the sample solution were determined directly by ICP-AES. Then, Ag and Cd in the same sample solution were enriched by extraction with potassium iodide-methyl isobutyl ketone ( KI-MIBK) and determined by FAAS. The precision of FAAS method for Ag and Cd was 6. 5% and 4. 7% RSD ( n = 12) , respectively. In comparison with the common analytical method, the proposed method provides the higher sensitivity, good accuracy and precision, high economy, high efficiency and is suitable for routine analysis of these elements in geochemical samples.%建立了地质化探样品中不同含量和检出限要求的12个元素的连续测定方法.样品经一次取样,用盐酸-氢氟酸-硝酸-高氯酸溶样,电感耦合等离子体发射光谱法测定铜、铅、锌、钴、镍、镉、锶、钡、钒、锰后,加碘化钾-甲基异丁基甲酮萃取分离,火焰原子吸收光谱法测定银、镉.银、镉的相对标准偏差(RSD,n=12)分别为6.5%、4.7%.与现行分析方法相比,建立的方法灵敏度和精密度高、准确度好,降低了生产成本,缩短了检测时间,尤其适合大量化探样品的测定.

  1. Method development for the redox speciation analysis of iron by ion chromatography-inductively coupled plasma mass spectrometry and carryover assessment using isotopically labeled analyte analogues.

    Science.gov (United States)

    Wolle, Mesay Mulugeta; Fahrenholz, Timothy; Rahman, G M Mizanur; Pamuku, Matt; Kingston, H M 'Skip'; Browne, Damien

    2014-06-20

    An ion chromatography-inductively coupled plasma mass spectrometry (IC-ICP-MS) method was developed for the redox speciation analysis of iron (Fe) based on in-column complexation of Fe(2+) and Fe(3+) by dipicolinic acid (DPA). The effects of column type, mobile phase composition and molecular ion interference were studied in the method optimization. The carryover of the target species in the IC-ICP-MS method was uniquely and effectively evaluated using isotopically enriched analogues of the analytes ((54)Fe(2+) and (57)Fe(3+)). Standard solutions of the enriched standards were injected into the system following analysis of a sample, and the ratios of the isotopes of iron in the enriched standards were calculated based on the chromatographic peak areas. The concentrations of the analytes carried over from the sample to the enriched standards were determined using the quantitative relationship in isotope dilution mass spectrometry (IDMS). In contrast to the routine way of evaluating carryover effect by injecting a blank solution after sample analysis, the use of isotopically enriched standards identified significant analyte carryover in the present method. Extensive experiments were carried out to systematically identify the source of the carryover and to eliminate the problem; the separation column was found to be the exclusive source. More than 95% of the analyte carryover was eliminated by reducing the length of the column. The detection limit of the IC-ICP-MS method (MDL) for the iron species was 2ngg(-1). The method was used to determine Fe(2+) and Fe(3+) in synthetic aqueous standard solutions and a beverage sample.

  2. Determination of trace selenium in high purity tellurium by hydride generation atomic fluorescence spectrometry after solid phase extraction of a diaminobenzidine-selenium chelate

    Science.gov (United States)

    Tong, Wang; Ying, Zeng; Jinyong, Xu

    2016-09-01

    Macroporous adsorption resin was used as the sorbent for solid phase extraction and determination of the trace Se content in high purity tellurium prior to hydride generation atomic fluorescence spectrometry analysis. Selenium was converted into an organic Se chelate using 3,3‧-diaminobenzidine and was separated from the tellurium matrix by solid phase extraction. The resin was packed as a column for solid phase extraction. Under optimum conditions, trace Se can be quantitatively extracted and the tellurium matrix can be removed. The Se in the eluate was determined by hydride generation atomic fluorescence spectrometry. The limit of detection (3σ) of this method was 0.22 ng g- 1 and the relative standard deviation (RSD, n = 5) ranged from 2.0 to 2.5% for the three investigated tellurium samples. The proposed method was successfully applied for the determination of the trace Se content in high purity tellurium samples.

  3. Determination of Pb(Ⅱ) and Cu(Ⅱ) by Electrothermal Atomic Absorption Spectrometry after Preconcentration by a Schiff Base Adsorbed on Surfactant Coated Alumina

    Institute of Scientific and Technical Information of China (English)

    SABER TEHRANI Mohammad; RASTEGAR Faramarz; PARCHEHBAF Ayob; KHATAMIAN Masoomeh

    2006-01-01

    1,2-Bis(salicylidenamino)ethane loaded onto sodium dodecyl sulfate-coated alumina was used as a new chelating sorbent for the preconcentration of traces of Pb(Ⅱ) and Cu(Ⅱ) prior to atomic absorption spectrometric determination. The influence of pH, flow rates of sample and eluent solutions, and foreign ions on the recovery of Pb(Ⅱ)by electrothermal atomic absorption spectrometry (ETAAS). The data of limit of detection (3σ) for Pb(Ⅱ) and Cu(Ⅱ)posed method was successfully applied to determination of lead and copper in different water samples.

  4. Quantitation of motexafin lutetium in human plasma by liquid chromatography-tandem mass spectrometry and inductively coupled plasma-atomic emission spectroscopy

    OpenAIRE

    Miles, Dale; Mody, Tarak D.; Hatcher, Lori I.; Fiene, John; Stiles, Mark; Patrick P. Lin; Lee, J.W.

    2003-01-01

    Liquid chromatography-tandem mass spectrometry (LC-MS/MS) and inductively coupled plasma-atomic emission spectroscopy (ICP-AES) methods were developed and validated for the evaluation of motexafin lutetium (MLu, lutetium texaphyrin, PCI-0123) pharmacokinetics in human plasma. The LC-MS/MS method was specific for MLu, whereas the ICP-AES method measured total elemental lutetium. Both methods were fast, simple, precise, and accurate. For the LC-MS/MS method, a closely related analogue (PCI-0353...

  5. Application of atomic absorption spectrometry with continuous light source to analyze selected metals important for human health in different parts of oranges

    OpenAIRE

    Szwerc Wojciech; Sowa Ireneusz

    2014-01-01

    The publication describes the application of high-resolution continuum source atomic absorption spectrometry (H-R CS AAS) to determine some physiologically essential and toxic elements occurring in citrus fruits of different origins. Before analysis, the samples were mineralized using a mixture of deionized water and 69% nitric acid 3:1 (v/v) in high pressure microwave digestion at 188°C during one hour.

  6. Selective Flow Injection Analysis of Ultra-trace Amounts of Cr(VI), Preconcentration of It by Solvent Extraction, and Determination by Electrothermal Atomic Absorption Spectrometry (ETAAS)

    DEFF Research Database (Denmark)

    Nielsen, Steffen; Sturup, Stefan; Spliid, Henrik;

    1999-01-01

    A rapid, robust, sensitive and selective time-based flow injection (FI) on-line solvent extraction system interfaced with electrothermal atomic absorption spectrometry (ETAAS) is described for analyzing ultra-trace amounts of Cr(VI). The sample is initially mixed on-line with isobutyl methyl keto......(VI)-reference material, synthetic seawater and waste waters, and waste water samples from an incineration plant and a desulphurization plant, respectively....

  7. RAPID AND SENSITIVE DETERMINATION OF PALLADIUM USING HOMOGENEOUS LIQUID-LIQUID MICROEXTRACTION VIA FLOTATION ASSISTANCE FOLLOWED BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROMETRY

    OpenAIRE

    Mohammad Rezaee; Reyhaneh Shadaniyan; Majid Haji Hosseini; Faezeh Khalilian

    2015-01-01

    A method for the determination of trace amounts of palladium was developed using homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA) followed by graphite furnace atomic absorption spectrometry (GFAAS). Ammonium pyrrolidine dithiocarbamate (APDC) was used as a complexing agent. This was applied to determine palladium in three types of water samples. In this study, a special extraction cell was designed to facilitate collection of the low-density solvent extraction. No...

  8. Trace mercury determination in drinking and natural water after preconcentration and separation by DLLME-SFO method coupled with cold vapor atomic absorption spectrometry

    OpenAIRE

    Abdollahi Atousa; Amirkavehei Mooud; Gheisari Mohammad Mehdi; Tadayon Fariba

    2014-01-01

    A novel dispersive liquid–liquid microextraction based on solidification of floating organic drop (DLLME-SFO) for simultaneous separation/preconcentration of ultra trace amounts of mercury was used. A method based on amalgamation was used for collection of gaseous mercury on gold coated sand (Gold trap). The concentration of mercury was determined by cold vapor atomic absorption spectrometry (CV-AAS). The DLLME-SFO behavior of mercury by using dithizone as complexing agent was systematically ...

  9. Application of atomic absorption spectrometry with continuous light source to analyze selected metals important for human health in different parts of oranges

    Directory of Open Access Journals (Sweden)

    Szwerc Wojciech

    2014-09-01

    Full Text Available The publication describes the application of high-resolution continuum source atomic absorption spectrometry (H-R CS AAS to determine some physiologically essential and toxic elements occurring in citrus fruits of different origins. Before analysis, the samples were mineralized using a mixture of deionized water and 69% nitric acid 3:1 (v/v in high pressure microwave digestion at 188°C during one hour.

  10. Automated continuous monitoring of inorganic and total mercury in wastewater and other waters by flow-injection analysis and cold-vapour atomic absorption spectrometry

    OpenAIRE

    Birnie, S. E.

    1988-01-01

    An automated continuous monitoring system for the determination of inorganic and total mercury by flow-injection analysis followed by cold-vapour atomic absorption spectrometry is described. The method uses a typical flow-injection manifold where digestion and reduction of the injected sample takes place. Mercury is removed by aeration from the flowing stream in a specially designed air-liquid separator and swept into a silica cell for absorption measurement at a wavelength of 253.7 nm. A cal...

  11. Improved limit of detection and quantitation development and validation procedure for quantification of zinc in Insulin by atomic absorption spectrometry.

    Science.gov (United States)

    Qadir, Muhammad Abdul; Ahmed, Mahmood; Haq, Iftikharul; Ahmed, Saghir

    2015-05-01

    A simple and expeditious analytical method for determination of zinc in human insulin isophane suspension by flame atomic absorption spectrophotometer (FAAS) was validated. The method was carried out on atomic absorption spectrometer with 0.4 nm bandwidth, 1.0 filter factor on deuterium (D2) background correction. The integration time was set at 3.0 second with 5.0 mA lamp current. The parameters of method validation showed adequate linearity, efficiency and relative standard deviation values were between 0.64%-1.69% (n=7), 1.31%-1.58% (n=10) for repeatability and intermediate precision respectively. The limit of detection 0.0032 μg/mL, 0.0173 μg/mL, 0.0231 μg/mL and limit of quantitation 0.0107μg/mL, 0.0578 μg/mL, 0.0694 μg/mL based on signal to noise (SN), calibration curve method (CCM) and fortification of blank (FB) were obtained respectively. The percentages of recovery for low, medium and high spiked concentration levels of zinc in human insulin were 99.38 ± 0.04 to 100.3 ± 0.03, 98.45 ± 0.38 to 100.3 ± 0.07 and 99.42 ± 0.03 to 99.42 ± 0.08 respectively. With the use of this method, five samples from each vial of human insulin isophane suspension were analyzed and the zinc content was determined. The zinc content were 22.1 ± 0.025 μg/mL and 24.3 ± 0.028 μg/mL which compliance the British Pharmacopoeia standard. PMID:26004720

  12. Coacervative extraction of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Hagarová, Ingrid; Bujdoš, Marek; Matúš, Peter; Kubová, Jana

    2013-10-01

    In this work, a relatively simple and sensitive method for separation/preconcentration of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry has been proposed. The method is based on the extraction of Pb-dithizone chelate with coacervates made up of lauric acid in the presence of potassium ions and methanol. Several important factors affecting extraction efficiency such as pH, concentration of lauric acid and dithizone, ionic strength, incubation and centrifugation time were investigated and optimized. After separation of aqueous bulk solution from surfactant-rich phase, the final extract was redissolved by using 500 μl of methanol acidified with 0.2 mol l- 1 HNO3. Under the optimized conditions (using initial sample volume of 10 ml), enrichment factor of 17.0, detection limit of 0.12 μg l- 1, quantification limit of 0.38 μg l- 1, relative standard deviation of 4.2% (for 2 μg l- 1 of Pb; n = 26), linearity of the calibration graph in the range of 0.5-4.0 μg l- 1 (with correlation coefficient better than 0.995) were achieved. The method was validated by the analysis of certified reference material (TMDA-61). Extraction recoveries for the CRM, spiked model solutions and spiked natural water samples were in the range of 91-96%. Finally, the method was applied to the separation/preconcentration and determination of trace lead in natural waters.

  13. Preconcentration of gold ions from water samples by modified organo-nanoclay sorbent prior to flame atomic absorption spectrometry determination

    Energy Technology Data Exchange (ETDEWEB)

    Afzali, Daryoush, E-mail: daryoush_afzali@yahoo.com [Nanochemistry Department, Research Institute of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Mostafavi, Ali [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Mirzaei, Mohammad [Nanochemistry Department, Research Institute of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

    2010-09-15

    In this work, the applicability of modified organo nanoclay as a new and easy prepared solid sorbent for the preconcentration of trace amounts of Au(III) ion from water samples is studied. The organo nanoclay was modified with 5-(4'-dimethylamino benzyliden)-rhodanine and used as a sorbent for separation of Au(III) ions. The sorption of gold ions was quantitative in the pH range of 2.0-6.0. Quantitative desorption occurred with 6.0 mL of 1.0 mol L{sup -1} Na{sub 2}S{sub 2}O{sub 3}. The amount of eluted Au(III) was measured using flame atomic absorption spectrometry. In the initial solution the linear dynamic range was in the range of 0.45 ng mL{sup -1} to 10.0 {mu}g mL{sup -1}, the detection limit was 0.1 ng mL{sup -1} and the preconcentration factor was 105. Also, the relative standard deviation was {+-}2.3% (n = 8 and C = 2.0 {mu}g mL{sup -1}) and the maximum capacity of the sorbent was 3.9 mg of Au(III) per gram of modified organo nanoclay. The influences of the experimental parameters including sample pH, eluent volume and eluent type, sample volume, and interference of some ions on the recoveries of the gold ion were investigated. The proposed method was applied for preconcentration and determination of gold in different samples.

  14. Species selective preconcentration and quantification of gold nanoparticles using cloud point extraction and electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hartmann, Georg, E-mail: georg.hartmann@tum.de [Department of Chemistry, Technische Universitaet Muenchen, 85748 Garching (Germany); Schuster, Michael, E-mail: michael.schuster@tum.de [Department of Chemistry, Technische Universitaet Muenchen, 85748 Garching (Germany)

    2013-01-25

    Highlights: Black-Right-Pointing-Pointer We optimized cloud point extraction and ET-AAS parameters for Au-NPs measurement. Black-Right-Pointing-Pointer A selective ligand (sodium thiosulphate) is introduced for species separation. Black-Right-Pointing-Pointer A limit of detection of 5 ng Au-NP per L is achieved for aqueous samples. Black-Right-Pointing-Pointer Measurement of samples with high natural organic mater content is possible. Black-Right-Pointing-Pointer Real water samples including wastewater treatment plant effluent were analyzed. - Abstract: The determination of metallic nanoparticles in environmental samples requires sample pretreatment that ideally combines pre-concentration and species selectivity. With cloud point extraction (CPE) using the surfactant Triton X-114 we present a simple and cost effective separation technique that meets both criteria. Effective separation of ionic gold species and Au nanoparticles (Au-NPs) is achieved by using sodium thiosulphate as a complexing agent. The extraction efficiency for Au-NP ranged from 1.01 {+-} 0.06 (particle size 2 nm) to 0.52 {+-} 0.16 (particle size 150 nm). An enrichment factor of 80 and a low limit of detection of 5 ng L{sup -1} is achieved using electrothermal atomic absorption spectrometry (ET-AAS) for quantification. TEM measurements showed that the particle size is not affected by the CPE process. Natural organic matter (NOM) is tolerated up to a concentration of 10 mg L{sup -1}. The precision of the method expressed as the standard deviation of 12 replicates at an Au-NP concentration of 100 ng L{sup -1} is 9.5%. A relation between particle concentration and the extraction efficiency was not observed. Spiking experiments showed a recovery higher than 91% for environmental water samples.

  15. Preconcentration procedure using cloud point extraction in the presence of electrolyte for cadmium determination by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Melo Coelho, Luciana [Departamento de Quimica Analitica, Universidade Estadual de Campinas (Unicamp), Cidade Universitaria ' Zeferino Vaz' , 13084-971, Campinas, Sao Paulo (Brazil); Arruda, Marco Aurelio Zezzi [Departamento de Quimica Analitica, Universidade Estadual de Campinas (Unicamp), Cidade Universitaria ' Zeferino Vaz' , 13084-971, Campinas, Sao Paulo (Brazil)]. E-mail: zezzi@iqm.unicamp.br

    2005-06-30

    This paper describes a micelle-mediated phase separation in the presence of electrolyte as a preconcentration method for cadmium determination by flame atomic absorption spectrometry (FAAS). Cadmium was complexed with ammonium O,O-diethyldithiophosphate (DDTP) in an acidic medium (0.32 mol l{sup -} {sup 1} HCl) using Triton X-114 as surfactant and quantitatively extracted into a small volume (about 20 {mu}l) of the surfactant-rich phase after centrifugation. The chemical variables that affect the cloud point extraction, such as complexing time (0-20 min), Triton X114 concentration (0.043-0.87% w/v) and complexing agent concentration (0.01-0.1 mol l{sup -} {sup 1}), were investigated. The cloud point is formed in the presence of NaCl at room temperature (25 deg. C), and the electrolyte concentration (0.5-5% w/v) was also investigated. Under optimized conditions, only 8 ml of sample was used in the presence of 0.043% w/v Triton X-114 and 1% (w/v) NaCl. This method permitted limits of detection and quantification of 0.9 {mu}g l{sup -} {sup 1} and 2.9 {mu}g l{sup -} {sup 1} Cd, respectively, and a linear calibration range from 3 to 400 {mu}g l{sup -} {sup 1} Cd. The proposed method was applied to Cd determination in physiological solutions (containing 0.9% (w/v) of NaCl), mineral water, lake water and cigarette samples (tobacco)

  16. Determination of ultra trace arsenic species in water samples by hydride generation atomic absorption spectrometry after cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Ulusoy, Halil Ibrahim, E-mail: hiulusoy@yahoo.com [University of Cumhuriyet, Faculty of Science, Department of Chemistry, TR-58140, Sivas (Turkey); Akcay, Mehmet; Ulusoy, Songuel; Guerkan, Ramazan [University of Cumhuriyet, Faculty of Science, Department of Chemistry, TR-58140, Sivas (Turkey)

    2011-10-10

    Graphical abstract: The possible complex formation mechanism for ultra-trace As determination. Highlights: {yields} CPE/HGAAS system for arsenic determination and speciation in real samples has been applied first time until now. {yields} The proposed method has the lowest detection limit when compared with those of similar CPE studies present in literature. {yields} The linear range of the method is highly wide and suitable for its application to real samples. - Abstract: Cloud point extraction (CPE) methodology has successfully been employed for the preconcentration of ultra-trace arsenic species in aqueous samples prior to hydride generation atomic absorption spectrometry (HGAAS). As(III) has formed an ion-pairing complex with Pyronine B in presence of sodium dodecyl sulfate (SDS) at pH 10.0 and extracted into the non-ionic surfactant, polyethylene glycol tert-octylphenyl ether (Triton X-114). After phase separation, the surfactant-rich phase was diluted with 2 mL of 1 M HCl and 0.5 mL of 3.0% (w/v) Antifoam A. Under the optimized conditions, a preconcentration factor of 60 and a detection limit of 0.008 {mu}g L{sup -1} with a correlation coefficient of 0.9918 was obtained with a calibration curve in the range of 0.03-4.00 {mu}g L{sup -1}. The proposed preconcentration procedure was successfully applied to the determination of As(III) ions in certified standard water samples (TMDA-53.3 and NIST 1643e, a low level fortified standard for trace elements) and some real samples including natural drinking water and tap water samples.

  17. Cloud point extraction for trace inorganic arsenic speciation analysis in water samples by hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li, Shan, E-mail: ls_tuzi@163.com; Wang, Mei, E-mail: wmei02@163.com; Zhong, Yizhou, E-mail: yizhz@21cn.com; Zhang, Zehua, E-mail: kazuki.0101@aliyun.com; Yang, Bingyi, E-mail: e_yby@163.com

    2015-09-01

    A new cloud point extraction technique was established and used for the determination of trace inorganic arsenic species in water samples combined with hydride generation atomic fluorescence spectrometry (HGAFS). As(III) and As(V) were complexed with ammonium pyrrolidinedithiocarbamate and molybdate, respectively. The complexes were quantitatively extracted with the non-ionic surfactant (Triton X-114) by centrifugation. After addition of antifoam, the surfactant-rich phase containing As(III) was diluted with 5% HCl for HGAFS determination. For As(V) determination, 50% HCl was added to the surfactant-rich phase, and the mixture was placed in an ultrasonic bath at 70 °C for 30 min. As(V) was reduced to As(III) with thiourea–ascorbic acid solution, followed by HGAFS. Under the optimum conditions, limits of detection of 0.009 and 0.012 μg/L were obtained for As(III) and As(V), respectively. Concentration factors of 9.3 and 7.9, respectively, were obtained for a 50 mL sample. The precisions were 2.1% for As(III) and 2.3% for As(V). The proposed method was successfully used for the determination of trace As(III) and As(V) in water samples, with satisfactory recoveries. - Highlights: • Cloud point extraction was firstly established to determine trace inorganic arsenic(As) species combining with HGAFS. • Separate As(III) and As(V) determinations improve the accuracy. • Ultrasonic release of complexed As(V) enables complete As(V) reduction to As(III). • Direct HGAFS analysis can be performed.

  18. Trace-element determination in lichens of Cordoba (Argentina) using neutron activation analysis and atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Ramalina ecklonii (Spreng.) Mey. and Flot. is a lichen widely distributed in Cordoba, a central province of Argentina. The ability of this lichen as an atmospheric pollution bioindicator has already been studied in relation to its physiological response to air pollutants. This work has to do with the study of R. ecklonii in terms of its capacity to accumulate heavy metals and other trace elements. The sampled area, located in the province of Cordoba, covered 50,000 km2 and was divided following a grid of 25 x 25 km. Lichens were collected at the intersecting points, no least than 500 m from main routes or highly populated centres and individuals were randomly gathered following the four cardinal directions and no more than 100 m from the geographically settled point. From each pool, three sub-samples were taken for independent analysis using atomic absorption spectrometry (AAS) and neutron activation analysis (NAA), for the determination of twenty nine elements (Cu, Ni, Mn, and Pb (AAS) and As, Ba, Br, Ca, Ce, Co, Cr, Cs, Eu, Fe, Hf, K, La, Lu, Na, Rb, Sb, Sc, Sm, Ta, Tb, Th, U, Yb, and Zn (NAA). The quality of the determinations was checked using standard reference material and data sets were evaluated using descriptive statistics, correlation analysis, and factor analysis. The highest variation coefficients correspond to Ca, Cr, and Zn. The studied elements were identified as of physiological importance and as emitted by natural (soil and rocks) and anthropogenic sources (non-ferrous metallurgy, coal combustion, oil-fired plants, fossil fuel combustion and, other industries). (author)

  19. Cloud point extraction for trace inorganic arsenic speciation analysis in water samples by hydride generation atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    A new cloud point extraction technique was established and used for the determination of trace inorganic arsenic species in water samples combined with hydride generation atomic fluorescence spectrometry (HGAFS). As(III) and As(V) were complexed with ammonium pyrrolidinedithiocarbamate and molybdate, respectively. The complexes were quantitatively extracted with the non-ionic surfactant (Triton X-114) by centrifugation. After addition of antifoam, the surfactant-rich phase containing As(III) was diluted with 5% HCl for HGAFS determination. For As(V) determination, 50% HCl was added to the surfactant-rich phase, and the mixture was placed in an ultrasonic bath at 70 °C for 30 min. As(V) was reduced to As(III) with thiourea–ascorbic acid solution, followed by HGAFS. Under the optimum conditions, limits of detection of 0.009 and 0.012 μg/L were obtained for As(III) and As(V), respectively. Concentration factors of 9.3 and 7.9, respectively, were obtained for a 50 mL sample. The precisions were 2.1% for As(III) and 2.3% for As(V). The proposed method was successfully used for the determination of trace As(III) and As(V) in water samples, with satisfactory recoveries. - Highlights: • Cloud point extraction was firstly established to determine trace inorganic arsenic(As) species combining with HGAFS. • Separate As(III) and As(V) determinations improve the accuracy. • Ultrasonic release of complexed As(V) enables complete As(V) reduction to As(III). • Direct HGAFS analysis can be performed

  20. Recent Developments in the Speciation and Determination of Mercury Using Various Analytical Techniques

    Directory of Open Access Journals (Sweden)

    Lakshmi Narayana Suvarapu

    2015-01-01

    Full Text Available This paper reviews the speciation and determination of mercury by various analytical techniques such as atomic absorption spectrometry, voltammetry, inductively coupled plasma techniques, spectrophotometry, spectrofluorometry, high performance liquid chromatography, and gas chromatography. Approximately 126 research papers on the speciation and determination of mercury by various analytical techniques published in international journals since 2013 are reviewed.

  1. Determination of arsenic speciation in sulfidic waters by Ion Chromatography Hydride-Generation Atomic Fluorescence Spectrometry (IC-HG-AFS).

    Science.gov (United States)

    Keller, Nicole S; Stefánsson, Andri; Sigfússon, Bergur

    2014-10-01

    A method for the analysis of arsenic species in aqueous sulfide samples is presented. The method uses an ion chromatography system connected with a Hydride-Generation Atomic Fluorescence Spectrometer (IC-HG-AFS). With this method inorganic As(III) and As(V) species in water samples can be analyzed, including arsenite (HnAs(III)O3(n-3)), thioarsenite (HnAs(III)S3(n-3)), arsenate (HnAs(V)O4(n-3)), monothioarsenate (HnAs(V)SO3(n-3)), dithioarsenate (HnAs(V)S2O2(n-3)), trithioarsenate (HnAs(V)S3O(n-3)) and tetrathioarsenate (HnAs(V)S4(n-3)). The peak identification and retention times were determined based on standard analysis of the various arsenic compounds. The analytical detection limit was ~1-3 µg L(-1) (LOD), depending on the quality of the baseline. This low detection limit makes this method also applicable to discriminate between waters meeting the drinking water standard of max. 10 µg L(-1) As, and waters that do not meet this standard. The new method was successfully applied for on-site determination of arsenic species in natural sulfidic waters, in which seven species were unambiguously identified.

  2. Comparative mass spectrometric analyses of Photofrin oligomers by fast atom bombardment mass spectrometry, UV and IR matrix-assisted laser desorption/ionization mass spectrometry, electrospray ionization mass spectrometry and laser desorption/jet-cooling photoionization mass spectrometry.

    Science.gov (United States)

    Siegel, M M; Tabei, K; Tsao, R; Pastel, M J; Pandey, R K; Berkenkamp, S; Hillenkamp, F; de Vries, M S

    1999-06-01

    Photofrin (porfimer sodium) is a porphyrin derivative used in the treatment of a variety of cancers by photodynamic therapy. This oligomer complex and a variety of porphyrin monomers, dimers and trimers were analyzed with five different mass spectral ionization techniques: fast atom bombardment, UV and IR matrix-assisted laser desorption/ionization, electrospray ionization, and laser desorption/jet-cooling photoionization. All five approaches resulted in very similar oligomer distributions with an average oligomer length of 2.7 +/- 0.1 porphyrin units. In addition to the Photofrin analysis, this study provides a side-by-side comparison of the spectra for the five different mass spectrometric techniques.

  3. A method for determining the analytical form of a radionuclide depth distribution using multiple gamma spectrometry measurements

    Energy Technology Data Exchange (ETDEWEB)

    Dewey, Steven Clifford, E-mail: sdewey001@gmail.com [United States Air Force School of Aerospace Medicine, Occupational Environmental Health Division, Health Physics Branch, Radiation Analysis Laboratories, 2350 Gillingham Drive, Brooks City-Base, TX 78235 (United States); Whetstone, Zachary David, E-mail: zacwhets@umich.edu [Radiological Health Engineering Laboratory, Department of Nuclear Engineering and Radiological Sciences, University of Michigan, 2355 Bonisteel Boulevard, 1906 Cooley Building, Ann Arbor, MI 48109-2104 (United States); Kearfott, Kimberlee Jane, E-mail: kearfott@umich.edu [Radiological Health Engineering Laboratory, Department of Nuclear Engineering and Radiological Sciences, University of Michigan, 2355 Bonisteel Boulevard, 1906 Cooley Building, Ann Arbor, MI 48109-2104 (United States)

    2011-06-15

    When characterizing environmental radioactivity, whether in the soil or within concrete building structures undergoing remediation or decommissioning, it is highly desirable to know the radionuclide depth distribution. This is typically modeled using continuous analytical expressions, whose forms are believed to best represent the true source distributions. In situ gamma ray spectroscopic measurements are combined with these models to fully describe the source. Currently, the choice of analytical expressions is based upon prior experimental core sampling results at similar locations, any known site history, or radionuclide transport models. This paper presents a method, employing multiple in situ measurements at a single site, for determining the analytical form that best represents the true depth distribution present. The measurements can be made using a variety of geometries, each of which has a different sensitivity variation with source spatial distribution. Using non-linear least squares numerical optimization methods, the results can be fit to a collection of analytical models and the parameters of each model determined. The analytical expression that results in the fit with the lowest residual is selected as the most accurate representation. A cursory examination is made of the effects of measurement errors on the method. - Highlights: > A new method for determining radionuclide distribution as a function of depth is presented. > Multiple measurements are used, with enough measurements to determine the unknowns in analytical functions that might describe the distribution. > The measurements must be as independent as possible, which is achieved through special collimation of the detector. > Although the effects of measurements errors may be significant on the results, an improvement over other methods is anticipated.

  4. Comparison of reactant and analyte ions for ⁶³Nickel, corona discharge, and secondary electrospray ionization sources with ion mobility-mass spectrometry.

    Science.gov (United States)

    Crawford, C L; Hill, H H

    2013-03-30

    (63)Nickel radioactive ionization ((63)Ni) is the most common and widely used ion source for ion mobility spectrometry (IMS). Regulatory, financial, and operational concerns with this source have promoted recent development of non-radioactive sources, such as corona discharge ionization (CD), for stand-alone IMS systems. However, there has been no comparison of the negative ion species produced by all three sources in the literature. This study compares the negative reactant and analyte ions produced by three sources on an ion mobility-mass spectrometer: conventional (63)Ni, CD, and secondary electrospray ionization (SESI). Results showed that (63)Ni and SESI produced the same reactant ion species while CD produced only the nitrate monomer and dimer ions. The analyte ions produced by each ion source were the same except for the CD source which produced a different ion species for the explosive RDX than either the (63)Ni or SESI source. Accurate and reproducible reduced mobility (K0) values, including several values reported here for the first time, were found for each explosive with each ion source. Overall, the SESI source most closely reproduced the reactant ion species and analyte ion species profiles for (63)Ni. This source may serve as a non-radioactive, robust, and flexible alternative for (63)Ni. PMID:23598216

  5. Direct sample introduction of wines in graphite furnace atomic absorption spectrometry for the simultaneous determination of arsenic, cadmium, copper and lead content.

    Science.gov (United States)

    Ajtony, Zsolt; Szoboszlai, Norbert; Suskó, Emoke Klaudia; Mezei, Pál; György, Krisztina; Bencs, László

    2008-07-30

    A multi-element graphite furnace atomic absorption spectrometry (GFAAS) method was elaborated for the simultaneous determination of As, Cd, Cu, and Pb in wine samples of various sugar contents using the transversally heated graphite atomizer (THGA) with end-capped tubes and integrated graphite platforms (IGPs). For comparative GFAAS analyses, direct injection (i.e., dispensing the sample onto the IGP) and digestion-based (i.e., adding oxidizing agents, such as HNO(3) and/or H(2)O(2) to the sample solutions) methods were optimized with the application of chemical modifiers. The mixture of 5 microg Pd (applied as nitrate) plus 3 microg Mg(NO(3))(2) chemical modifier was proven to be optimal for the present set of analytes and matrix, it allowing the optimal 600 degrees C pyrolysis and 2200 degrees C atomization temperatures, respectively. The IGP of the THGA was pre-heated at 70 degrees C