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Sample records for atomic spectrometry techniques

  1. Determination of various extracted Al species and their fractions by atomic spectrometry techniques

    International Nuclear Information System (INIS)

    Complete text of publication follows. During the last few decades aluminium and its distribution in the environment has attracted much attention because of Al toxic effects to the plants, animals and humans. Its concentration in different environmental samples varies widely. While determination of high Al concentrations can be realized with no serious problem, reliable determination of its trace and ultratrace concentrations requires the development of enrichment techniques capable of improving both, the selectivity and also sensitivity for this analyte. Two extraction methods were used for selective separation and preconcentration of aluminium trace concentrations from model solutions. Solid phase extraction (SPE) using nanometer-sized titanium dioxide as a solid sorbent and cloud point extraction (CPE) using nonionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) were utilized. Spectrometry techniques such as flame (F AAS) and electrothermal (ET AAS) atomic absorption spectrometry, inductively coupled plasma optical emission spectrometry (ICP OES) or inductively coupled plasma mass spectrometry (ICP MS) were applied for the determination of aluminium. Direct TiO2-slurry sampling was used for sample injection into the graphite furnace of ET AAS in SPE. Optimized procedures were used for the determination of trace and ultratrace amounts of total aluminium and various aluminium species and their fractions in speciation analysis and fractionation studies using environmental samples such as natural waters, soils and sediments. The work was supported by Slovak Research and Development Agency under the contracts No. APVT-20-010204, LPP-0038-06, LPP-0146-09 and SK-CZ-0044-07, by Scientific Grant Agency of Ministry of Education of Slovak Republic and the Slovak Academy of Sciences under the contracts No. VEGA 1/4464/07 and VEGA 1/0272/08 and by Ministry of Education, Youth and Sports of Czech Republic under the contract No. MEB 080813.

  2. 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...

  3. 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,…

  4. Atomic spectrometry update : environmental analysis

    OpenAIRE

    Butler, O.T.; Cook, Jennifer; Harrington, C.F.; Hill, S. J.; Rieuwerts, J.; Miles, Douglas

    2007-01-01

    This is the twenty-second annual review published in JAAS of the application of atomic spectrometry to the chemical analysis of environmental samples. In the analysis of air, there is ongoing use of XRF techniques for the measurement of particles collected on filters. There is continuing interest in the determination of trace levels of mercury species in the atmosphere. Isotope ratio measurement protocols are attracting wider interest as a potential tool for source apport...

  5. Atomic spectrometry update : environmental analysis

    OpenAIRE

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

    2010-01-01

    This is the twenty-fifth annual review published in JAAS on the application of atomic spectrometry to the chemical analysis of environmental samples. This Update refers to papers published approximately between September 2008 and August 2009. In the analysis of air, work has focused on: the need to collect and characterise ultrafines; determination of elements such as Be, Hg and PGEs in air samples; application of SRXRF techniques and advances in the development of field deployable aerosol ma...

  6. Graphite filter atomizer in atomic absorption spectrometry

    Science.gov (United States)

    Katskov, Dmitri A.

    2007-09-01

    Graphite filter atomizers (GFA) for electrothermal atomic absorption spectrometry (ETAAS) show substantial advantages over commonly employed electrothermal vaporizers and atomizers, tube and platform furnaces, for direct determination of high and medium volatility elements in matrices associated with strong spectral and chemical interferences. Two factors provide lower limits of detection and shorter determination cycles with the GFA: the vaporization area in the GFA is separated from the absorption volume by a porous graphite partition; the sample is distributed over a large surface of a collector in the vaporization area. These factors convert the GFA into an efficient chemical reactor. The research concerning the GFA concept, technique and analytical methodology, carried out mainly in the author's laboratory in Russia and South Africa, is reviewed. Examples of analytical applications of the GFA in AAS for analysis of organic liquids and slurries, bio-samples and food products are given. Future prospects for the GFA are discussed in connection with analyses by fast multi-element AAS.

  7. 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...

  8. Atomic spectrometry update : environmental analysis

    OpenAIRE

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

    2013-01-01

    This is the 28th annual review published in JAAS on the application of atomic spectrometry to the chemical analysis of environmental samples. This Update refers to papers published approximately between September 2011 and August 2012 and continues the series of Atomic Spectrometry Updates (ASUs) in Environmental Analysis1 that should be read in conjunction with other related ASUs in the series, namely: clinical and biological materials, foods and beverages2; advances in atomic spectrometry an...

  9. Zeeman atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The design and development of a Zeeman atomic absorption spectrometer for trace element analysis are described. An instruction manual is included which details the operation, adjustment, and maintenance. Specifications and circuit diagrams are given

  10. Atomic spectrometry update : environmental analysis

    OpenAIRE

    Butler, Owen T.; Cook, Jennifer; Davidson, Christine M.; Harrington, Chris F.; Miles, Douglas

    2009-01-01

    This is the twenty-forth annual review published in JAAS of the application of atomic spectrometry to the chemical analysis of environmental samples. This Update refers to papers published approximately between September 2007 and August 2008. In the analysis of air, work is focused on the need to collect and characterise ultrafines, i.e. particles below 100 nm in size, and such research is being facilitated through the development of air sampler technologies for subsequent off-line analysis o...

  11. Assessment of elemental pollution in soil of Islamabad city using instrumental neutron activation analysis and atomic absorption spectrometry techniques

    Energy Technology Data Exchange (ETDEWEB)

    Daud, M.; Wasim, M.; Khalid, N.; Zaidi, J.H. [Pakistan Institute of Nuclear Science and Technology, Islamabad (Pakistan). Chemistry Div.; Iqbal, J. [University of the Punjab, Lahore (Pakistan). Inst. of Chemistry

    2009-07-01

    The soil samples of nine different sites in Islamabad were studied for their elemental composition. Instrumental neutron activation analysis and atomic absorption spectrometry were employed and 33 elements were determined. The acquired data were analyzed using descriptive statistics, principal component analysis, cluster analysis, pollution level index and enrichment factor. A perusal of results shows a distribution of elemental concentration in two major groups, one along the highway and the other in industrial area of Islamabad. The soil along the highway sites was found to be relatively less polluted than at the sites in the industrial area. The enrichment factor indicates the presence of As, Pb, Sb, Se and Sn at higher levels. The method validation was done by analyzing IAEA reference materials SL-1 (lake sediment) and S7 (soil). (orig.)

  12. 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

  13. Spectrometry techniques for radioactivity measurements

    International Nuclear Information System (INIS)

    The energy of the radiation emission following the nuclear decay is unique and the characteristic of the radio nuclide which undergoes decay. Thus measurement of the energy of the radiation offers a method of identifying the radio nuclides. The prime requirement of the energy measurement is a suitable detector which shows response proportional to the energy of the radiation rather than the presence of the radiation. The response from such detectors are suitably processed and distributed with respect to the signal strength which is proportional to incident energy. This distribution is normally referred as energy spectrum and is recorded in the multichannel analyser. The measurement of energy and intensity of radiation from the spectrum is called radiation spectrometry. Thus the radiation spectrometry allows the identification and quantification of radioactive isotopes in variety of matrices. The radiation spectrometry has now become a popular radioanalytical technique in wide area of nuclear fuel cycle programs. The popular spectrometry techniques commonly used for the radioactivity measurement and analysis are Alpha spectrometry, Gamma ray spectrometry and Beta spectrometry

  14. 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

  15. Estimation of zirconium in Zr-C-Nb alloy by Inductively Coupled Plasma-Atomic Emission Spectrometry technique

    International Nuclear Information System (INIS)

    The present paper discusses a new method developed for estimation of Zirconium (Zr) in Niobium alloy by Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES). The present procedure involves dissolution of Niobium alloy in a mixture of Sulfuric acid, Nitric acid and Hydro Fluoric acid and subsequent analysis of Zr in Niobium alloy by sequential ICP-AES (Model: JY Ultima 2C HR). A Relative Standard Deviation of less than ± 5% has been achieved in this method. (author)

  16. 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

  17. Analysis of heavy metals and minerals elements in the turmeric using Total-Reflection X-ray Fluorescence analysis technique and Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Currently, many studies demonstrate anti-cancer and anti-inflammatory benefits of turmeric. The aims of this work is to perform analysis of metals such as calcium, chromium, manganese, iron, cobalt, nickel, copper, zinc, arsenic, bromine, rubidium, strontium, cadmium and lead in the turmeric collected from various places in Madagascar. The analysis by total reflection X-ray fluorescence technique is used to determine the concentrations of heavy metals, while the atomic absorption spectrometry is used for the determination of trace elements. Analysis results show that the concentration of calcium in the turmeric is very high, its average concentration is 1025.8 mg.kg-1. The average concentrations of manganese, of copper and of iron are respectively 44.7 mg.kg-1; 19.7 mg.kg-1 and 53.6 mg.kg-1. The average concentrations of zinc, of rubidium and of strontium are respectively 17.3 mg.kg-1; 35.2 mg.kg-1 and 21.7 mg.kg-1

  18. 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.

  19. Suspended nanoparticles in surfactant media as a microextraction technique for simultaneous separation and preconcentration of cobalt, nickel and copper ions for electrothermal atomic absorption spectrometry determination.

    Science.gov (United States)

    Dadfarnia, Shayessteh; Shakerian, Farid; Shabani, Ali Mohammad Haji

    2013-03-15

    The aim of this study was to describe a new method of microextraction based on the suspension of alumina nanoparticles in the surfactant media for simultaneous separation and preconcentration of the ultra-traces of cobalt, nickel and copper ions. In this technique, the alumina nanoparticles were suspended in the non-ionic surfactant solution of Triton X-114. The analytes in the sample solution were adsorbed onto the nanoparticles. After the phase separation based on the cloud point of the mixture at 40 °C, the nanoparticles settled down in the surfactant rich phase. Then 120 μL of nitric acid (3.0 mol L(-1)) was added to the surfactant rich phase which caused desorption of the analytes. Finally, the liquid phase was separated by centrifugation from the nanoparticles and was used for the quantification of the analytes by the electrothermal atomic absorption spectrometry (ETAAS). The parameters affecting the extraction and detection processes were optimized. Under the optimized experimental conditions (i.e. pH∼8, Triton X-114, 0.05% (v/v); temperature 40 °C), a sample volume of 25 mL resulted in the enhancement factors of 198, 205 and 206 and detection limits (defined as 3Sb/m) of 2.5, 2.8 and 2.6 ng L(-1) for Co(II), Ni(II) and Cu(II) respectively. The sorbent showed high capacity for these metal ions (30-40 mg g(-1) sorbent). The method was successfully applied to the determination of the analytes in natural water samples. PMID:23598108

  20. Determination of mercury species by the diffusive gradient in thin film technique and liquid chromatography – atomic fluorescence spectrometry after microwave extraction

    International Nuclear Information System (INIS)

    Highlights: • DGT–MAE–LC–CV-AFS method was developed for determination of four mercury species. • The microwave extraction was used for isolation of mercury species from resin gels. • Optimized DGT–MAE–LC–CV-AFS method provides low detection limits (13–38 ng L−1). • The diffusion coefficients of four mercury species were simultaneously determined. - Abstract: A diffusive gradient in thin films technique (DGT) was combined with liquid chromatography (LC) and cold vapor atomic fluorescence spectrometry (CV-AFS) for the simultaneous quantification of four mercury species (Hg2+, CH3Hg+, C2H5Hg+, and C6H5Hg+). After diffusion through an agarose diffusive layer, the mercury species were accumulated in resin gels containing thiol-functionalized ion-exchange resins (Duolite GT73, and Ambersep GT74). A microwave-assisted extraction (MAE) in the presence of 6 M HCl and 5 M HCl (55 °C, 15 min) was used for isolation of mercury species from Ambersep and Duolite resin gels, respectively. The extraction efficiency was higher than 95.0% (RSD 3.5%). The mercury species were separated with a mobile phase containing 6.2% methanol + 0.05% 2-mercaptoethanol + 0.02 M ammonium acetate with a stepwise increase of methanol content up to 80% in the 16th min on a Zorbax C18 reverse phase column. The LODs of DGT–MAE–LC–CV-AFS method were 38 ng L−1 for CH3Hg+, 13 ng L−1 for Hg2+, 34 ng L−1 for C2H5Hg+ and 30 ng L−1 for C6H5Hg+ for 24 h DGT accumulation at 25 °C

  1. 原子吸收光谱分析中的绿色萃取富集技术%Green extraction and preconcentration techniques in atomic absorption spectrometry.

    Institute of Scientific and Technical Information of China (English)

    邓勃

    2011-01-01

    Sample pretreatment is an essential condition to obtain exact results in the analysis of complicated samples and trace components. Extraction has been extensively applied to the separation and preconcentra-tion of trace inorganic metallic ions. In recent years, analysts have developed several enviroment-friendly green extraction techniques, including single-drop microextraction, cloud point extraction, dispersive liquid-liquid microextraction, room-temperature ionic liquid extraction, solid-liquid extraction, solid phase microextraction and molecularly imprinted polymer extraction. Their common advantages over conventional liquid-liquid extraction are: (1) using only small quantities of organic solvents; (2) high extraction efficiency and large enrichment factor; (3) less consumption of samples and reagents; (4) fast and simple-to-operate; (5) easy to combine with instrumental analysis methods; and (6) wide application fields. In this paper, the advances of applications of these green extraction techniques in atomic absorption spectrometry during last three years are reviewed with 85 references.%分析复杂样品和测定痕量组分时,样品预处理是获得准确结果的必要条件.萃取是广泛使用的分离富集方法,近年来,分析工作者陆续开发了多种新型绿色微萃取技术,包括单滴微萃取、浊点萃取、分散液-液微萃取、室温离子液体萃取、固-液萃取、固相微萃取、分子印迹聚合物萃取等.他们共同的优点是:有机萃取溶剂用量非常小;萃取效率高,富集倍数大;样品和试剂消耗少;操作简便、快速;便于与其他分析仪器联用;应用范围广等.本文介绍这些新型绿色萃取技术近3年来的进展,引用文献85篇.

  2. Determination of mercury species by the diffusive gradient in thin film technique and liquid chromatography – atomic fluorescence spectrometry after microwave extraction

    Energy Technology Data Exchange (ETDEWEB)

    Pelcová, Pavlína, E-mail: pavlina.pelcova@mendelu.cz; Dočekalová, Hana, E-mail: hana.docekalova@mendelu.cz; Kleckerová, Andrea, E-mail: andrea.kleckerova@mendelu.cz

    2015-03-25

    Highlights: • DGT–MAE–LC–CV-AFS method was developed for determination of four mercury species. • The microwave extraction was used for isolation of mercury species from resin gels. • Optimized DGT–MAE–LC–CV-AFS method provides low detection limits (13–38 ng L{sup −1}). • The diffusion coefficients of four mercury species were simultaneously determined. - Abstract: A diffusive gradient in thin films technique (DGT) was combined with liquid chromatography (LC) and cold vapor atomic fluorescence spectrometry (CV-AFS) for the simultaneous quantification of four mercury species (Hg{sup 2+}, CH{sub 3}Hg{sup +}, C{sub 2}H{sub 5}Hg{sup +}, and C{sub 6}H{sub 5}Hg{sup +}). After diffusion through an agarose diffusive layer, the mercury species were accumulated in resin gels containing thiol-functionalized ion-exchange resins (Duolite GT73, and Ambersep GT74). A microwave-assisted extraction (MAE) in the presence of 6 M HCl and 5 M HCl (55 °C, 15 min) was used for isolation of mercury species from Ambersep and Duolite resin gels, respectively. The extraction efficiency was higher than 95.0% (RSD 3.5%). The mercury species were separated with a mobile phase containing 6.2% methanol + 0.05% 2-mercaptoethanol + 0.02 M ammonium acetate with a stepwise increase of methanol content up to 80% in the 16th min on a Zorbax C18 reverse phase column. The LODs of DGT–MAE–LC–CV-AFS method were 38 ng L{sup −1} for CH{sub 3}Hg{sup +}, 13 ng L{sup −1} for Hg{sup 2+}, 34 ng L{sup −1} for C{sub 2}H{sub 5}Hg{sup +} and 30 ng L{sup −1} for C{sub 6}H{sub 5}Hg{sup +} for 24 h DGT accumulation at 25 °C.

  3. 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.

  4. 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

  5. Advanced atomic force microscopy techniques

    OpenAIRE

    Thilo Glatzel; Hendrik Hölscher; Thomas Schimmel; Baykara, Mehmet Z; Schwarz, Udo D.; Ricardo Garcia

    2012-01-01

    Although its conceptual approach is as simple as the technique used in record players already introduced in the 19th century, the invention of the atomic force microscope (AFM) in 1986 by Binnig, Quate, and Gerber was a milestone for nanotechnology. The scanning tunneling microscope (STM), introduced some years earlier, had already achieved atomic resolution, but is limited to conductive surfaces. Since its operational principle is based on the detection of the forces acting between tip and s...

  6. Flow Injection and Atomic Absorption Spectrometry (FI-AAS) -

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    1996-01-01

    absorption spectrometry (AAS). Initially with flame-AAS (fAAS) procedures, later for hydride generation (HG) techniques, and most recently in combination with electrothermal AAS (ETAAS). The common denominator for all these procedures is the inherently precise and strictly reproducible timing in FI from the......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...

  7. 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...

  8. 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.

  9. Uranium determination using atomic spectrometric techniques: An overview

    International Nuclear Information System (INIS)

    This review focuses on the determination of uranium using spectroanalytical techniques that are aimed at total determination such as flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS), inductively coupled plasma optical emission spectrometry (ICP-OES); and inductively coupled plasma mass spectrometry (ICP-MS) that also enables the determination of uranium isotopes. The advantages and shortcomings related to interferences, precision, accuracy, sample type and equipment employed in the analysis are taken into account, as well as the complexity and costs (i.e., acquisition, operation and maintenance) associated with each of the techniques. Strategies to improve their performance that employ separation and/or preconcentration steps are considered, with an emphasis given to solid-phase extraction because of its advantages compared to other preconcentration procedures.

  10. 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.

  11. 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.

  12. 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.

  13. 液相色谱-原子荧光联用法测定鱼油中的甲基汞%Determination of methylmercury in fish oil by interface technique coupled high performance liquid chromatography with atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    徐君辉; 周向阳; 沈飚; 秦德元

    2011-01-01

    先后采用10% KOH+ 1%硫脲和20% HCl提取鱼油样品,用液相色谱-原子荧光联用技术测定样品中的甲基汞含量.试验结果表明,线性范围在0~ 10 μg/L之间,相关系数为0.999 3,检出限为0.2 μg/L,加标回收率在96.0%~105.0%之间,相对标准偏差小于5%.该方法快速、简便、准确.%Methylmercury was extracted from fish oil sample with 10% potassium hydroxide and 1% thio-urea, then with 20% hydrochloric acid, and then was determined by interface technique coupled high performance liquid chromatography with atomic fluorescence spectrometry. The results showed that the linear range was between 0 and 10 μg/L,the linear coefficient was 0.999 3 ,the detection limit was 0.2 μg/ L,recovery was between 96.0% and 105. 0% ,the relative standard was less than 5%. The method was rapid, simple, and accurate.

  14. Quantification of steroid conjugates using fast atom bombardment mass spectrometry

    International Nuclear Information System (INIS)

    Fast atom bombardment/mass spectrometry or liquid secondary ion mass spectrometry provides the capability for direct analysis of steroid conjugates (sulfates, glucuronides) without prior hydrolysis or derivatization. During the analysis of biologic extracts, limitations on the sensitivity of detection arise from the presence of co-extracted material which may suppress or obscure the analyte signal. A procedure is described for the quantitative determination of dehydroepiandrosterone sulfate in serum which achieved selective isolation of the analyte using immunoadsorption extraction and highly specific detection using tandem mass spectrometry. A stable isotope-labeled analog [( 2H2]dehydroepiandrosterone sulfate) was used as internal standard. Fast atom bombardment of dehydroepiandrosterone sulfate yielded abundant [M-H]- ions that fragmented following collisional activation to give HSO4-; m/z 97. During fast atom bombardment/tandem mass spectrometry of serum extracts, a scan of precursor ions fragmenting to give m/z 97 detected dehydroepiandrosterone sulfate and the [2H2]-labeled analog with a selectivity markedly superior to that observed using conventional mass spectrometry detection. Satisfactory agreement was observed between quantitative data obtained in this way and data obtained by gas chromatography/mass spectrometry of the heptafluorobutyrates of dehydroepiandrosterone sulfate and [2H2]dehydroepiandrosterone sulfate obtained by direct derivatization. 21 refs

  15. 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)

  16. Vapor generation and atom traps: Atomic absorption spectrometry at the ng/L level

    International Nuclear Information System (INIS)

    Atom-trapping atomic absorption spectrometry is a technique that allows detection at the ng/L level for several analytes such as As, Se, Sb, Pb, Bi, Cd, In, Tl, Te, Sn and Hg. The principle involves generation of volatile species, usually hydrides, trapping these species on the surface of an atom trap held at an optimized temperature and, finally, revolatilizing the analyte species by rapid heating of the trap and transporting them in a carrier gas to a heated quartz tube, as commonly used with hydride generation AAS systems. A transient signal having, in most cases, a full width at half maximum of less than 1 s is obtained. The atom trap may be a quartz surface or a W-coil; the former is heated externally and the latter is heated resistively. Both collection and revolatilization temperatures are optimized. In some cases, the W-coil itself is used as an electrothermal atomizer and a heated quartz tube is then not needed. The evolution of these traps starts with the well-known Watling's slotted quartz tube (SQT), continues with atom trapping SQT and finally reaches the present traps mentioned above. The analytical figures of merit for these traps need to be standardized. Naturally, enhancement is on characteristic concentration, C0, where the change in characteristic mass, m0, can be related to trapping efficiency. Novel terms are suggested for E, enhancement factor; such as Emax, maximum enhancement factor; Et, enhancement for 1.0 minute sampling and Ev, enhancement for 1.0 mL of sample. These figures will allow easy comparison of results from different laboratories as well as different analytes and/or traps

  17. Vapor generation and atom traps: Atomic absorption spectrometry at the ng/L level

    Energy Technology Data Exchange (ETDEWEB)

    Ataman, O. Yavuz [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey)], E-mail: ataman@metu.edu.tr

    2008-08-15

    Atom-trapping atomic absorption spectrometry is a technique that allows detection at the ng/L level for several analytes such as As, Se, Sb, Pb, Bi, Cd, In, Tl, Te, Sn and Hg. The principle involves generation of volatile species, usually hydrides, trapping these species on the surface of an atom trap held at an optimized temperature and, finally, revolatilizing the analyte species by rapid heating of the trap and transporting them in a carrier gas to a heated quartz tube, as commonly used with hydride generation AAS systems. A transient signal having, in most cases, a full width at half maximum of less than 1 s is obtained. The atom trap may be a quartz surface or a W-coil; the former is heated externally and the latter is heated resistively. Both collection and revolatilization temperatures are optimized. In some cases, the W-coil itself is used as an electrothermal atomizer and a heated quartz tube is then not needed. The evolution of these traps starts with the well-known Watling's slotted quartz tube (SQT), continues with atom trapping SQT and finally reaches the present traps mentioned above. The analytical figures of merit for these traps need to be standardized. Naturally, enhancement is on characteristic concentration, C{sub 0}, where the change in characteristic mass, m{sub 0}, can be related to trapping efficiency. Novel terms are suggested for E, enhancement factor; such as E{sub max}, maximum enhancement factor; E{sub t}, enhancement for 1.0 minute sampling and E{sub v}, enhancement for 1.0 mL of sample. These figures will allow easy comparison of results from different laboratories as well as different analytes and/or traps.

  18. Vapor generation and atom traps: Atomic absorption spectrometry at the ng/L level

    Science.gov (United States)

    Ataman, O. Yavuz

    2008-08-01

    Atom-trapping atomic absorption spectrometry is a technique that allows detection at the ng/L level for several analytes such as As, Se, Sb, Pb, Bi, Cd, In, Tl, Te, Sn and Hg. The principle involves generation of volatile species, usually hydrides, trapping these species on the surface of an atom trap held at an optimized temperature and, finally, revolatilizing the analyte species by rapid heating of the trap and transporting them in a carrier gas to a heated quartz tube, as commonly used with hydride generation AAS systems. A transient signal having, in most cases, a full width at half maximum of less than 1 s is obtained. The atom trap may be a quartz surface or a W-coil; the former is heated externally and the latter is heated resistively. Both collection and revolatilization temperatures are optimized. In some cases, the W-coil itself is used as an electrothermal atomizer and a heated quartz tube is then not needed. The evolution of these traps starts with the well-known Watling's slotted quartz tube (SQT), continues with atom trapping SQT and finally reaches the present traps mentioned above. The analytical figures of merit for these traps need to be standardized. Naturally, enhancement is on characteristic concentration, C0, where the change in characteristic mass, m0, can be related to trapping efficiency. Novel terms are suggested for E, enhancement factor; such as Emax, maximum enhancement factor; Et, enhancement for 1.0 minute sampling and Ev, enhancement for 1.0 mL of sample. These figures will allow easy comparison of results from different laboratories as well as different analytes and/or traps.

  19. Recent developments in generation of volatile species and in their atomization for atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Dědina, Jiří; Arslan, Y.; Mester, Z.; Sturgeon, R. E.; Kratzer, Jan; Matoušek, Tomáš; Musil, Stanislav; Svoboda, Milan

    2014. s. 221-221. [Rio Symposium on Atomic Spectrometry /13./. 19.10.2014-24.10.2014, Merida, Yucatan] R&D Projects: GA AV ČR(CZ) M200311202; GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : Arsenic * speciation analysis * sapphire tube atomizer Subject RIV: CB - Analytical Chemistry, Separation

  20. A Thermo-Chemical Reactor for analytical atomic spectrometry

    International Nuclear Information System (INIS)

    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

  1. 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.

  2. 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

  3. 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.

  4. Excimer laser-ablated plasma atomic spectrometry

    International Nuclear Information System (INIS)

    The characterization and evaluation of a new kind of excimer laser-ablated plasma and applications for direct spectrochemical analysis were investigated through time- and space-resolved spectroscopy. The shape, size, emission spectra, and excitation temperatures of the plasma are largely department on the atmospheric surroundings, the ambient gas composition, the pressure, and laser energy. Spatial discrimination may be desirable to increase the line-to-background (L/B) ratio in atomic emission spectroscopy. A direct spectrochemical analytical method for solid samples with good linearity was developed using the excimer laser-AES. The sensitivity of the analytical signal varied depending on the chemical matrix of the solid samples. A typical detection limit for potassium in a glass matrix was 0.13 μg/g.

  5. 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

  6. Evaluation of electrochemical generation of volatile zinc hydride by heated quartz tube atomizer atomic absorption spectrometry.

    Science.gov (United States)

    Arbab-Zavar, Mohammad-Hossein; Chamsaz, Mahmoud; Youssefi, Abbas; Aliakbari, Mostafa

    2012-01-01

    Electrochemical hydride generation (EcHG) as a sample introduction system for determination of zinc was developed. It was directly coupled to an electrically heated quartz tube atomizer (QTA) atomic absorption spectrometry (AAS) system. The hydride generator is a laboratory-made semi-batch electrolytic cell that consists of a lead-tin alloy cathode and a platinum anode. The effects of typical parameters on the generation efficiency of the technique, such as types of cathode material and catholyte and anolyte solutions, were studied. The influences of numerical experimental operating parameters on the analytical signal were evaluated in detail and optimum conditions were obtained. The analytical figures of merit for the developed method were determined. The calibration curve was linear up to 300 ng mL(-1) of Zn. A concentration detection limit (3σ, n = 9) of 11 ng mL(-1) Zn and a relative standard deviation of 5.0% (RSD, n = 9) for 200 ng mL(-1) Zn were accessed. In addition, the susceptibility of interference from various ions was evaluated. The accuracy of the method was verified by determination of Zn in a certified reference material and in tap water. The achieved concentrations were found to be in good agreement with both the certified value and the data obtained using flame AAS. PMID:22790376

  7. 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.

  8. 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.

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

    Czech Academy of Sciences Publication Activity Database

    Arslan, Y.; Musil, Stanislav; Matoušek, Tomáš; Kratzer, Jan; Dědina, Jiří

    103-104, JAN-FEB (2015), s. 155-163. ISSN 0584-8547 R&D Projects: GA ČR GA14-23532S Grant ostatní: GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : gold * volatile species generation * quartz atomizers * atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.176, year: 2014

  10. Atomization of volatile compounds for atomic absorption and atomic fluorescence spectrometry: On the way towards the ideal atomizer

    International Nuclear Information System (INIS)

    This review summarizes and discusses the individual atomizers of volatile compounds. A set of criteria important for analytical praxis is used to rank all the currently existing approaches to the atomization based on on-line atomization for atomic absorption (AAS) and atomic fluorescence spectrometry (AFS) as well as on in-atomizer trapping for AAS. Regarding on-line atomization for AAS, conventional quartz tubes are currently the most commonly used devices. They provide high sensitivity and low baseline noise. Running and investment costs are low. The most serious disadvantage is the poor resistance against atomization interferences and often unsatisfactory linearity of calibration graphs. Miniature diffusion flame (MDF) is extremely resistant to interferences, simple, cheap and user-friendly. Its essential disadvantage is low sensitivity. A novel device, known as a multiatomizer, was designed to overcome disadvantages of previous atomizers. It matches performance of conventional quartz tubes in terms of sensitivity and baseline noise as well as in running and investment costs. The multiatomizer, however, provides much better (i) resistance against atomization interferences and (ii) linearity of calibration graphs. In-atomizer trapping enhances the sensitivity of the determination and eliminates the effect of the generation kinetics and of surges in gas flow on the signal shape. This is beneficial for the accuracy of the determination. It could also be an effective tool for reducing some interferences in the liquid phase. In-situ trapping in graphite furnaces (GF) is presently by far the most popular approach to the in-atomizer trapping. Its resistance against interferences is reasonably good and it can be easily automated. In-situ trapping in GF is a mature method well established in various application fields. These are the reasons to rank in-situ trapping in GF as currently the most convenient approach to hydride atomization for AAS. The recently suggested

  11. Analytical control of wollastonite for biomedical applications by use of atomic absorption spectrometry and inductively coupled plasma atomic emission spectrometry.

    Science.gov (United States)

    De Aza, P N; Guitián, F; De Aza, S; Valle, F J

    1998-04-01

    Preliminary in vitro experiments revealed that wollastonite (CaSiO3) is a potentially highly bioactive material that forms a hyroxyapatite (HA) surface layer on exposure to simulated body fluid with an ion concentration, pH and temperature virtually identical with those of human blood plasma. The formation of the HA layer is an essential requirement for an artificial material to be used as bioactive bone substitute. This finding opens up a wide field for biomedical applications of wollastonite. Biomaterials used as implants in the human body require strict control of trace elements and of the toxic species specified in American Society for Testing and Materials F-1185-88 (As, Cd, Hg and Pb) in ceramic hydroxyapatite for surgical implantation. In this work, two types of pseudowollastonite, the high temperature form of wollastonite, were analysed by using cold vapour atomic absorption spectrometry and hydride generation atomic absorption spectrometry, in order to determine the elements stated in the above-mentioned norm, and inductively coupled plasma atomic emission spectrometry to establish the SiO2/CaO ratio of the two materials and analyse for all other impurities introduced by the raw materials and by the processes of synthesis, sintering and grinding. Barium and Mg were especially prominent in raw materials, and Zr, Y, Mg, W, Co and Ni come mainly from the processing. PMID:9684401

  12. Microwave Digestion of Hair Samples in Closed Vessels for the Determinations of Copper and Iron by Derivative Flame Atomic Absorption Spectrometry using Flow-injection Technique%微波溶样-流动注射-导数火焰原子吸收光谱测定人发中的铜和铁

    Institute of Scientific and Technical Information of China (English)

    陈兰菊; 郑连义; 孙汉文

    2002-01-01

      本文以微波消解人发样,利用流动注射-导数火焰原子吸收法测定其中微量铜、铁的含量。微波溶样技术具有快捷、污染小、损失少、消化完全等优点;流动注射进样技术可以克服常规火焰原子吸收法耗样量大和基体干扰严重的缺点;导数技术应用于火焰原子吸收可提高方法的灵敏度和信号的选择性。微波溶样、流动注射与导数技术相结合应用于火焰原子吸收成功地测定了人发中的微量铜和铁。%  A new method was presented for the determinations of copper and iron in hair samples,which was based on the technique of microwave digestion in closed vessels,flow-injection and derivative flame atomic absorption spectrometry. The technique of microwave digestion is convenient, little of pollution, less in loss, and complete digestion. The flaws that sampling is large and matrix interference is serious in conventional flame atomic absorption spectrometry(FAAS) were overcome by flow-injection sampling technique. The sensitivity and signal selectivity were enhanced when derivative technique was used. This new method that derivative flame atomic absorption spectrometry combined with microwave digestion and flow-injection technique is simple and rapid with satisfactory results for determination of copper and iron in hair.

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

    Czech Academy of Sciences Publication Activity Database

    Duben, Ondřej; Boušek, J.; Dědina, Jiří; Kratzer, Jan

    2015-01-01

    Roč. 111, SEP (2015), s. 57-63. ISSN 0584-8547 Grant ostatní: GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * hydride generation-atomic absorption spectrometry * selenium Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.176, year: 2014

  14. Determination of cadmium in aluminium by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A direct method for the determination of cadmium in elemental aluminium is described. Metal samples are dissolved in diluted hydrochloric acid and cadmium is determined by atomic absorption spectrometry in an air-acetylene flame. Interference by non-specific absorption observed at the analytical wavelength incorrected for by means of a non-absorbing line emitted by the hollow-cathode lamp. Relatively large amounts of arsenic do not interfere. The minimun determinable concentration of cadmium for this procedure is 2-3 ppm, expressed on aluminium basis. (author)

  15. Determination of metals in atmospheric particulates using atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Nineteen trace metals in atmospheric samples have been determined by atomic absorption spectrometry, using a graphite furnace for most elements. Paper filters have been used to collect air samples. The sample preparation procedure involves the removal of organic matter and the conversion of the metals to soluble salts by ashing the filters in an oxygen plasma at 125 deg C for 6 h. and by subsequent dissolution in HN03HCl solution. The sensitivities achieved are in the range of 2,5.10-5 and 6,3.10-3 μg/m3, for an air volume of 2000 m3. (author)

  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. Identification of bacteria using mass spectrometry techniques

    Czech Academy of Sciences Publication Activity Database

    Krásný, Lukáš; Hynek, R.; Hochel, I.

    2013-01-01

    Roč. 353, NOV 2013 (2013), s. 67-79. ISSN 1387-3806 R&D Projects: GA ČR GAP503/10/0664 Institutional support: RVO:61388971 Keywords : Mass spectrometry * Bacteria * Identification Subject RIV: EE - Microbiology, Virology Impact factor: 2.227, year: 2013

  18. On the expression 'external calibration' in atomic spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kantor, Tibor [Geological Institute of Hungary, Stefania Ave 14, 1143 Budapest (Hungary)], E-mail: kantib@t-online.hu

    2008-04-15

    The expressions 'calibration' and 'external calibration' appear together in the present literature of atomic spectrometry resulting in a dilemma of understanding and correct use. It is examined how the IUPAC can provide a guidance to the solution of this problem by recalling the definitions of related terms of optical, mass and X-ray atomic spectrometry techniques. The introduction and definition of these expressions in widely used text books are investigated and statistically evaluated for the articles published during the last 30 years in the periodical Spectrochimica Acta Part B. For the elimination of the literary difficulties with the use of the term 'calibration', attributes are proposed to express the degree of matrix matching of standards and samples.

  19. 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

  20. Determination of lead traces in water and liqueurs by derivative atom trapping flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sun, H. [Department of Chemistry, Hebei University, Baoding, 071002 (China); Yang Lili [Department of Chemistry, Hebei University, Baoding, 071002 (China); Zhang Deqiang [Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing (China); Wang Weixiao [Department of Chemistry, Hebei University, Baoding, 071002 (China); Sun Jianmin [Department of Chemistry, Hebei University, Baoding, 071002 (China)

    1997-07-01

    A new method for the direct determination of lead traces using derivative atom trapping flame atomic absorption spectrometry (DAT-FAAS) with an improved water-cooled stainless steel trapping equipment in an air-acetylene flame was investigated. The optimum conditions concerning the sensitivity were studied. For a 1 min collection, the characteristic concentration (given as derivative absorbance of 0.0044) and the detection limit (3s) were 1.4 ng/mL and 0.27 ng/mL, respectively. This is 361 and 74-fold better than those of the conventional flame atomic absorption spectrometry (FAAS) and comparable to those of graphite furnace atomic absorption spectrometry (GFAAS). The detection limit and sensitivity of DAT-FAAS for a 3 min collection time were 2 and 3 orders of magnitude higher than those of conventional FAAS. The present method was applied to the determination of lead in water and liqueur samples with a recovery range of 94-108% and a relative standard deviation of 3.5-5.6%. (orig.). With 5 figs., 5 tabs.

  1. 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…

  2. 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.

  3. 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.

  4. Determination of tetraalkyllead compounds in gasoline by liquid chromatography-atomic absorption spectrometry

    Science.gov (United States)

    Messman, J.D.; Rains, T.C.

    1981-01-01

    A liquid chromatography-atomic absorption spectrometry (LC-AAS) hybrid analytical technique is presented for metal speciation measurements on complex liquid samples. The versatility and inherent metal selectivity of the technique are Illustrated by the rapid determination of five tetraalkyllead compounds in commercial gasoline. Separation of the individual tetraalkyllead species is achieved by reversed-phase liquid chromatography using an acetonitrile/water mobile phase. The effluent from the liquid Chromatograph Is introduced directly into the aspiration uptake capillary of the nebulizer of an air/acetylene flame atomic absorption spectrometer. Spectral interferences due to coeluting hydrocarbon matrix constituents were not observed at the 283.3-nm resonance line of lead used for analysis. Detection limits of this LC-AAS hydrid analytical technique, based on a 20-??L injection, are approximately 10 ng Pb for each tetraalkyllead compound.

  5. Precise atomic mass measurements by deflection mass spectrometry

    CERN Document Server

    Barber, R C

    2003-01-01

    Since its inception nearly 90 years ago by J.J. Thomson, the precise determination of atomic masses by the classical technique of deflecting charged particles in electric and magnetic fields has provided a large body of data on naturally occurring nuclides. Currently, such measurements on stable nuclides have frequently achieved a precision of better than two parts in 10 sup 9 of the mass. A review of the technique, together with a brief summary of the important historical developments in the field of precise atomic mass measurements, will be given. The more recent contributions to this field by the deflection mass spectrometer at the University of Manitoba will be provided as illustrations of the culmination of the techniques used and the applications that have been studied. A brief comparison between this and newer techniques using Penning traps will be presented.

  6. Precise atomic mass measurements by deflection mass spectrometry

    Science.gov (United States)

    Barber, R. C.; Sharma, K. S.

    2003-05-01

    Since its inception nearly 90 years ago by J.J. Thomson, the precise determination of atomic masses by the classical technique of deflecting charged particles in electric and magnetic fields has provided a large body of data on naturally occurring nuclides. Currently, such measurements on stable nuclides have frequently achieved a precision of better than two parts in 10 9 of the mass. A review of the technique, together with a brief summary of the important historical developments in the field of precise atomic mass measurements, will be given. The more recent contributions to this field by the deflection mass spectrometer at the University of Manitoba will be provided as illustrations of the culmination of the techniques used and the applications that have been studied. A brief comparison between this and newer techniques using Penning traps will be presented.

  7. Atmospheric deposition of heavy metals around the lead and copper-zinc smelters in Baia Mare, Romania, studied by the moss biomonitoring technique, neutron activation analysis and flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The mosses Pleurozium schreberi, Pseudoscleropodium purum and Rhytidiadelphus squarrosus were used as biomonitors to study the atmospheric deposition of metals around the lead and copper-zinc smelters in Baia Mare. Samples representing the last three years' growth of moss or its green part, collected on the ground at 28 sites located 2-17 km from the source area, were analyzed by instrumental neutron activation analysis using epithermal neutrons (ENAA) and by flame atomic absorption spectrometry (FAAS). A total of 31 elements were determined, including most of the heavy metals characteristic of emissions from this kind of industry. The observed data for Pb, As, Cu, and Cd are all high compared with those observed in other regions of Europe with similar industries, but the concentrations in moss approach regional background levels at a distance of about 8 km from the main source area. Factor analysis of the data distinguishes two industrial components, one characterized by Pb, Cu, As, and Sb, and another one by Zn and Cd. A strong crustal component including five major elements (Na, Mg, Al, Ti, Fe) and an additional number of trace elements (Sc, V, Cr, Cs, Ba, REE, Th) also appears to be derived mainly from industrial sources. The mean I value in the present material is 5 times lower than the corresponding level in moss in Norway, and also consistently lower than elsewhere in Europe, a fact which evidences the endemic character of the examined area due to iodine depletion. (author)

  8. Atmospheric deposition of heavy metals around the lead and copper-zinc smelters in Baia Mare, Romania, studied by the moss biomonitoring technique, neutron activation analysis and flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The mosses Pleurozium schreberi, Pseudoscleropodium purum and Rhytidiadelphus squarrosus were used as biomonitors to study the atmospheric deposition of heavy metals around the lead and copper-zinc smelters in Baia Mare. Samples representing the last three year's growth of moss or its green part, collected on the ground at 28 sites located 2-17 km from the source area, were analyzed by instrumental neutron activation analysis using epithermal neutrons and by flame atomic absorption spectrometry. A total of 31 elements were determined, including most of the heavy metals characteristic of emissions from this kind industry. The observed data for Pb, As, Cu, and Cd are all high compared with those observed in other regions of Europe with similar industries, but the concentrations in moss approach regional background levels at a distance of about 8 km from the main source area. Factor analysis of the data distinguishes two industrial components, one characterized by Pb, Cu, As, and Sb, and another one by Zn and Cd. A strong crustal component including five major elements (Na, Mg, Al, Ti, Fe) and an additional number of trace elements (Sc, V, Cr, Cs, Ba, REE, Th) also appears to be derived mainly from industrial sources. The mean I value in the present material is 5 times lower than the corresponding level in moss in Norway, and also consistently lower than elsewhere in Europe, a fact which evidence the endemic character of the examined area due to iodine depletion

  9. Atmospheric Deposition of Heavy Metals around the Lead and Copper-Zinc Smelters in Baia Mare, Romania, Studied by the Moss Biomonitoring Technique, Neutron Activation Analysis and Flame Atomic Absorption Spectrometry

    CERN Document Server

    Culicov, O A; Steinnes, E; Okina, O S; Santa, Z; Todoran, R

    2002-01-01

    The mosses Pleurozium schreberi, Pseudoscleropodium purum and Rhytidiadelphus squarrosus were used as biomonitors to study the atmospheric deposition of heavy metals around the lead and copper-zinc smelters in Baia Mare. Samples representing the last three years' growth of moss or its green part, collected on the ground at 28 sites located 2-17 km from the source area, were analyzed by instrumental neutron activation analysis using epithermal neutrons and by flame atomic absorption spectrometry. A total of 31 elements were determined, including most of the heavy metals characteristic of emissions from this kind industry. The observed data for Pb, As, Cu, and Cd are all high compared with those observed in other regions of Europe with similar industries, but the concentrations in moss approach regional background levels at a distance of about 8 km from the main source area. Factor analysis of the data distinguishes two industrial components, one characterized by Pb, Cu, As, and Sb, and another one by Zn and Cd...

  10. A Review on Mass Spectrometry: Technique and Tools

    Directory of Open Access Journals (Sweden)

    Ms. Ashwini Yerlekar

    2014-04-01

    Full Text Available Protein structure prediction has gain important in area of life sciences, because of its complex structure. The protein-protein interaction is necessary to study the behavior of protein in a specific environment, and study molecular relationship in living systems. Therefore, large scale proteomics technologies are required to measure physical connection of proteins in living organisms. Mass Spectrometry uses the technique to measure mass-to-charge ratio of ion. It's an evolving technique for characterization of proteins. A Mass Spectrometer can be more sensitive and specific, also complement with other LC detectors. Liquid Chromatography, unlike gas chromatography is a separation technique which helps to separate wide range of organic compounds from small molecular metabolites to peptides and proteins. This paper addresses the study of data analysis using mass Spectrometry. It also includes the study of various methods of Mass Spectrometry data analysis, the tools and various applications of Mass Spectrometry.This review briefs on Mass Spectrometry technique, its application, usage, and tools used by Mass Spectrometry

  11. 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

  12. Plutonium determination in urine by techniques of mass spectrometry

    International Nuclear Information System (INIS)

    The objective of this study was to develop an analytic method for quantification and plutonium reappraisal in plane tables of alpha spectrometry be means of the mass spectrometry technique of high resolution with plasma source inductively coupled and desolvator Aridus (Aridus-Hr-Icp-Ms) and mass spectrometry with accelerator (AMS). The obtained results were, the recovery percentage of Pu in the plane table was of ∼ 90% and activity minimum detectable obtained with Aridus-Hr-Icp-Ms and AMS was of ∼ 3 and ∼ 0.4 f g of 239Pu, respectively. Conclusion, the results demonstrate the aptitude of the Aridus-Hr-Icp-Ms and AMS techniques in the Pu reappraisal in plane tables with bigger speed and precision, improving the values notably of the activity minimum detectable that can be obtained with the alpha spectrometry (∼ 50 f g of 239Pu). (author)

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

    International Nuclear Information System (INIS)

    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−1 and 0.51 ng mL−1, respectively. Linear calibration plot was obtained in the range of 2.5–25.0 ng mL−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−1. • The technique is suggested for laboratories equipped with only a flame AA spectrometer

  14. 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

  15. Determination of gold by chemical hydride generation atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. The chemical vapour generation (CVG) of transition and noble metals opens a novel route for introduction of these elements into atomic spectrometric sources. It can be accomplished by merging an acidic sample with tetrahydroborate reductant solution (Y. L. Feng et al., J. of Anal. At. Spectrom., 20 (2005) 255-265). There have been some studies for determination of Au; however, only mg L-1 levels of gold have been determined by CVG - Atomic Absorption Spectrometry (AAS) (G. Ertas et al., Applied Spectroscopy, 60 (2006) 423-429). Volatile Au species were generated in flow injection arrangement from acid environment in presence of surfactants. The core of the system is a mixing manifold based on 3 concentric capillaries (T. Matousek et al., J. of Anal. At. Spectrom., 18 (2003) 487-494) protruding into the glass gas-liquid separator (glass, volume 3 ml). Optimum flow rate of Ar as a carrier gas was found at 240 mL/min. The study of generation parameters as well as the use of reaction modifiers-surfactants and dithiocarbamate- will be presented. Quartz tube multiatomizer for AAS was employed for atomization. Atomization conditions including composition of carrier gases and their flow rates and atomization temperature were optimized. 900 deg C was found as the optimum atomization temperature; over 900 deg C, peak area of Au signal decreased; in addition, peak shape was altered. A sharp maximum of 6 mL/min oxygen as the outer gas was observed. Another important point was that hydrogen-rich atmosphere caused signal depression. Analytical performance of this approach to generation and atomization will be discussed and perspectives of its future will be outlined. This work was supported by the GA ASCR (grant No. A400310507 and IAA400310704) and Institute of Analytical Chemistry of the ASCR, v.v.i. (project no. AV0Z40310501). This work also was supported from OYP (Faculty Development Program) from the Middle East Technical University

  16. New cryogenic trap design for speciation analysis of arsenic by hydride generation-atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Svoboda, Milan; Kratzer, Jan; Dědina, Jiří

    Praha, 2014. s. 240-240. ISBN 978-80-905704-1-2. [European Symposium on Atomic Spectrometry ESAS 2014 & Czech-Slovak Spectroscopic Conference /15./. 16.03.2014-21.03.2014, Praha] R&D Projects: GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : atomic absorption spectrometry * hydride generation * cryogenic trapping Subject RIV: CB - Analytical Chemistry, Separation

  17. 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)

  18. Slurry sampling hydride generation-cryotrapping-atomic absorption spectrometry for arsenic speciation analysis in baby food

    Czech Academy of Sciences Publication Activity Database

    Huber, C. S.; Vale, M. G. R.; Dessuy, M. B.; Svoboda, Milan; Dědina, Jiří

    Hungarian Chemical Society, 2016 - (Mihucz, V.). s. 165 ISBN 978-963-9970-65-6. [European Symposium on Atomic Spectrometry /ESAS 2016/ & Hungarian Spectrochemical Conference /59./. 31.03.2016-02.04.2016, Eger] Institutional support: RVO:68081715 Keywords : arsenic speciation * atomic spectrometry * hydride generation Subject RIV: CB - Analytical Chemistry, Separation

  19. Use of Atomic Absorption Technique in Environmental Studies

    International Nuclear Information System (INIS)

    This chapter consists of some points including the process of atomic absorption, historical hint, key basics, the atom ionization and formation of plasma, applications in the device of atomic absorption, quantum analysis with atomic absorption, components of the device of atomic absorption, standardization of this device, atomic absorption in the the graphite furnace, supervising the analytical interventions, spectral interventions, non-spectral interventions, the utmost electric energy for atomization, preparation of standards and samples, the system of acidic digestion, similar analytical techniques.

  20. 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...

  1. 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

  2. Determination of lithium in coloured alcoholic beverages by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. Lithium was first found in ashes from wine in 1878, and its presence was later confirmed by spectroscopy, but its determination in wine and beverages is not well documented, unlike the extensive research reported on other metals. Several methods can be implemented for determination of lithium, involving the use of atomic spectroscopy techniques. This paper reports on an analytical optimization to determine lithium by atomic absorption spectrometry (AAS). Good results in reproducibility, accuracy and precision were obtained. No significant interference was found. The method was applied for determination of lithium in six rum samples, eight brandy samples, four vermouth samples, eight whisky samples and two bourbon samples. The value of lithium content in samples ranges from 0,33 to 1,48 μg/ml. Recovery experiments were carried out in order to evaluate the accuracy of the method in samples determination. The values obtained ranges from 95,71% to 98%. The precision of the method in that samples determination was evaluated through variation coefficients. The values obtained ranges from 7,2% to 2,5%. The results have been statistically compared with those obtained using the Inductively Coupled Plasma Atomic Emission Spectrometry (ICP/AES) and reaches a 95% level of significance.

  3. Multielement analysis of Pakistan coal by X-ray fluorescence spectrometry and inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Major, minor and trace element concentration levels are determined for 21 tertiary lignites and sub-bituminous coal samples collected from seven major coal field in Pakistan. Samples are collected as channel samples and/or run of mine samples. All samples are analysed by the x-ray fluorescence spectrometry (XRFS) technique whereas samples from Cherat coal field and the Katha-Pale coal field are analysed by the inductively coupled plasma atomic emission spectrometry (ICP-AES). Significant concentrations of toxic elements such as S, Ce, Cd, Cr, Cu, Mn, Ni, P, Pb, U and V are found in these coal samples. Thus, continuous exposure to dust of these coals (by the mine workers and inhabitants of the nearby settlements) and their extensive use of domestic purpose (cooking/heating), or in brick kilns and in combustion chambers of thermal power plants may cause significant environmental pollution problems as well as health problems. Their use in the industrial and energy sectors will further pose engineering/operational problems in items of requirements of preventive measures against corrosion of the combustion units. (author) 8 tabs

  4. 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)

  5. Time amplifying techniques towards atomic time resolution

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    High speed imaging technology has opened applications in many fields,such as collision,detonating, high voltage discharge,disintegration and transfer of phonon and exciton in solid,photosynthesis primitive reaction,and electron dynamics inside atom shell.In principle,all of the transient processes need to be explained theoretically and,at the same time,the time amplifying technique is required for observations of these processes.The present review concerns the atomic time amplifying mechanism of optical information and the extremely-high speed imaging methods,which are expressed in terms of the short time amplifying techniques.It is well-known that for extremely-high speed imaging with the converter tube,the temporal resolution is in the order of sub-picosecond of the streak imaging,and the imaging frequency is 6×10 8 ―5×10 9 fps(frame per second)of the frame imaging.On the other hand,for the tubeless extremely-high speed imaging,the imaging frequency is 10 7 ―10 14 fps,and its mechanism of forming high speed and framing could involve a lot of factors of the light under investigation,for instance,light speed,light parallelism,the parameters of light wave such as amplitude,phase,polari- zation and wavelength,and even quantum properties of photon.In the cascaded system of electro- magnetic wave and particle wave,it is possible to simultaneously realize extremely-high resolution in time and space,which is higher than a kite resolution.Then it would be possible to break the limit of the Heisenberg uncertainty relation of the optical frequency band.

  6. Time amplifying techniques towards atomic time resolution

    Institute of Scientific and Technical Information of China (English)

    LI JingZhen

    2009-01-01

    High speed imaging technology has opened applications in many fields,such as collision,detonating,high voltage discharge,disintegration and transfer of phonon and exciton in solid,photosynthesis primitive reaction,and electron dynamics inside atom shell.In principle,all of the transient processes need to be explained theoretically and,st the same time,the time amplifying technique is required for observations of these processes.The present review concerns the atomic time amplifying mechanism of optical information and the extremely-high speed imaging methods,which are expressed in terms of the short time amplifying techniques.It is well-known that for extremely-high speed imaging with the converter tube,the temporal resolution is in the order of sub-picosecond of the streak imaging,and the imaging frequency is 6×10~8-5×10~9 fps(frame per second)of the frame imaging.On the other hand,for the tubeless extremely-high speed imaging,the imaging frequency is 10~7-10~(14) fps,and its mechanism of forming high speed and framing could involve a lot of factors of the light under investigation,for instance,light speed,light parallelism,the parameters of light wave such as amplitude,phase,polarization and wavelength,and even quantum properties of photon.In the cascaded system of electromagnetic wave and particle wave,it is possible to simultaneously realize extremely-high resolution in time and space,which is higher than a kite resolution.Then it would be possible to break the limit of the Heisenberg uncertainty relation of the optical frequency band.

  7. Optimization of trace molybdenum content determination in human nails by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The accurate determination of molybdenum (Mo) in biological materials is of considerable importance in medical science because of the essential role played by this element in human metabolism. Molybdenum is a component of enzymes responsible for the initial stages of nitrogen, carbon and sulfur metabolism of plants, animals and humans. This element is usually determined by neutron activation analysis (NAA) in variety of samples, but direct measurement of low levels of molybdenum in biological samples by NAA is difficult. Recently instrumental analysis procedures such as atomic absorption spectrometry (AAS) have been used in clinical measurements for determination of many trace elements in the biological samples. These techniques are much simpler and cheaper than NAA. In this paper we are reporting a method of sample preparation for determining molybdenum by using graphite furnace atomic absorption spectrometry (GF-AAS). This method is the most readily available technique for determination of molybdenum at the ng/g level in biological samples. It can be used for the routine hospital laboratory determination of molybdenum and has appropriate sensitivity and simplicity. The best and reliable results for molybdenum analysis was achieved by digestion of nails in HNO3 2 N and was determined in the range from 0.11 to 5.10 μg/g

  8. Fast atom bombardment tandem mass spectrometry of carotenoids

    Energy Technology Data Exchange (ETDEWEB)

    van Breeman, R.B. [Univ. of Illinois, Chicago, IL (United States); Schmitz, H.H.; Schwartz, S.J. [North Carolina State Univ., Raleigh, NC (United States)

    1995-02-01

    Positive ion fast atom bombardment (FAB) tandem mass spectrometry (MS-MS) using a double-focusing mass spectrometer with linked scanning at constant B/E and high-energy collisionally activated dissociation (CAD) was used to differentiate 17 different cartenoids, including {beta}-apo-8{prime}- carotenal, astaxanthin, {alpha}-carotene, {beta}-carotene, {gamma}-carotene, {zeta}-carotene, canthaxanthin, {beta}-cryptoxanthin, isozeaxanthin bis (pelargonate), neoxanthin, neurosporene, nonaprene, lutein, lycopene, phytoene, phytofluene, and zeaxanthin. The carotenoids were either synthetic or isolated from plant tissues. The use of FAB ionization minimized degradation or rearrangement of the carotenoid structures due to the inherent thermal instability generally ascribed to these compounds. Instead of protonated molecules, both polar xanthophylls and nonpolar carotenes formed molecular ions, M{sup {center_dot}+}, during FAB ionization. Following collisionally activated dissociation, fragment ions of selected molecular ion precursors showed structural features indicative of the presence of hydroxyl groups, ring systems, ester groups, and aldehyde groups and the extent of aliphatic polyene conjugation. The fragmentation patterns observed in the mass spectra herein may be used as a reference for the structural determination of carotenoids isolated from plant and animal tissues. 18 refs., 4 figs.

  9. 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

  10. Exploiting flow injection and sequential injection for trace metal determinations in conjunction with detection by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    Despite their excellent analytical chemical capacities, Electrothermal Atomic Absorption Spectrometry (ETAAS) and Inductively Coupled Plasma Mass Spectrometry (ICPMS), nevertheless, often require suitable pretreatment of the sample material in order to obtain the necessary sensitivity and...

  11. High sensitivity detection of selenium by laser excited atomic fluorescence spectrometry using electrothermal atomization

    International Nuclear Information System (INIS)

    The high sensitivity detection of the trace element selenium is reported. The analytical method applied is Laser Excited Atomic Fluorescence Spectrometry using Electrothermal Atomization within a graphite furnace atomizer. For the production of tunable laser radiation in the VUV spectral region a laser system was developed which consists of two dye lasers pumped by a Nd:YAG laser. The laser radiations are subsequently frequency doubled and sum frequency mixed by nonlinear optical KDP or BBO crystals, respectively. The system works with a repetition rate of 20 Hz and provides output energies of up to 100 μJ in the VUV at a pulse duration of 5 ns. The analytical investigations were focused on the detection of selenium in aqueous solutions and samples of human whole blood. From measurements on aqueous standards detection limits of 1.5 ng/l for selenium were obtained, with corresponding absolute detected masses of only 15 fg. The linear dynamic range spanned six orders of magnitude and good precision was achieved. In case of human whole blood samples the recovery was found to be within the range of 96% to 104%. The determination of the selenium content yielded medians of [119.5 ± 17.3] μg/l for 200 frozen blood samples taken in 1988 and [109.1 ± 15.6] μg/l for 103 fresh blood samples. (author)

  12. 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.

  13. 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

  14. Determination of antimony by using tungsten trap atomic absorption spectrometry

    International Nuclear Information System (INIS)

    An electrically heated tungsten coil was used as a trap in the determination of antimony. The technique consists of three steps. Initially, SbH3 is formed by hydride generation procedure; then the analyte species in vapor form are transported to W-coil trap heated at 370 deg. C. Following the preconcentration step, the trap is heated to 895 deg. C; analyte species are revolatilized and transported to the flame-heated quartz atom cell where atomization and the formation of signal take place. The experimental parameters were optimized both for trap and no-trap studies. The most important experimental parameters are concentrations of HCl and NaBH4 solutions, H2 and Ar gas flow rates, and collection and revolatilization temperatures of W-coil. Accuracy was tested using a certified reference material, waste water EU-L-1. Limit of detection for the system is 16 ng l-1 using a sample of 36 ml collected in 4.0 min. Enhancement factor in sensitivity was 17

  15. Speciation of mercury by chromatography coupled with atomic spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Armstrong, H.E.L

    2000-03-01

    A commercial GC-AFS instrument has been developed and optimised for the speciation of organomercury. This instrument couples a GC oven to a modified atomic fluorescence detector via a ceramic pyrolyser. Organomercury compounds in dichloromethane solvent were directly injected through a Programmable Temperature Vaporiser Injector onto a DB1 Megabore column. Once separated, the compounds eluted from the column and were atomised in the pyrolyser then detected by AFS. The direct injection technique, ceramic pyrolysis design and argon purged detector have improved previous instrument designs by enhancing and maintaining sensitivity. The instrumental limit of detection was determined to be 0.25 pg Hg absolute. Methods were developed for the extraction of methylmercury from a variety of marine samples. The techniques were validated using mussel homogenate and dogfish liver (IAEA 142, SRM 8044 and DOLT-2) certified reference materials. An interlaboratory comparison exercise was participated in and a method was developed for the determination of methylmercury in Fucus sea plant (IAEA 140). A concentration of 0.63 {+-} 0.006 ng g{sup -1} was reported. The material is now certified at 0.626 {+-} 0.139 ng g{sup -1}. Of all the participating laboratories, this was the closest result to the certified value. The instrument and methods were also applied to soil and sediment samples. Once again validation was performed with a CRM sediment, IAEA 356. Although this material has been reported to give positive artifact formation when using a steam distillation sample preparation procedure, good agreement and no artifacts were observed upon analysis. A further contaminated land, an uncontaminated soil and sediment sample were also studied. For all the samples studied by GC-AFS total mercury measurements were also made following an appropriate digestion procedure and CV-AFS. A gas chromatograph was also coupled with ICP-MS and HPLC was coupled to CV-AFS as comparative techniques. Both

  16. Speciation of mercury by chromatography coupled with atomic spectrometry

    International Nuclear Information System (INIS)

    A commercial GC-AFS instrument has been developed and optimised for the speciation of organomercury. This instrument couples a GC oven to a modified atomic fluorescence detector via a ceramic pyrolyser. Organomercury compounds in dichloromethane solvent were directly injected through a Programmable Temperature Vaporiser Injector onto a DB1 Megabore column. Once separated, the compounds eluted from the column and were atomised in the pyrolyser then detected by AFS. The direct injection technique, ceramic pyrolysis design and argon purged detector have improved previous instrument designs by enhancing and maintaining sensitivity. The instrumental limit of detection was determined to be 0.25 pg Hg absolute. Methods were developed for the extraction of methylmercury from a variety of marine samples. The techniques were validated using mussel homogenate and dogfish liver (IAEA 142, SRM 8044 and DOLT-2) certified reference materials. An interlaboratory comparison exercise was participated in and a method was developed for the determination of methylmercury in Fucus sea plant (IAEA 140). A concentration of 0.63 ± 0.006 ng g-1 was reported. The material is now certified at 0.626 ± 0.139 ng g-1. Of all the participating laboratories, this was the closest result to the certified value. The instrument and methods were also applied to soil and sediment samples. Once again validation was performed with a CRM sediment, IAEA 356. Although this material has been reported to give positive artifact formation when using a steam distillation sample preparation procedure, good agreement and no artifacts were observed upon analysis. A further contaminated land, an uncontaminated soil and sediment sample were also studied. For all the samples studied by GC-AFS total mercury measurements were also made following an appropriate digestion procedure and CV-AFS. A gas chromatograph was also coupled with ICP-MS and HPLC was coupled to CV-AFS as comparative techniques. Both approaches were

  17. 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)

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

    Czech Academy of Sciences Publication Activity Database

    Marschner, Karel; Musil, Stanislav; Dědina, Jiří

    2015-01-01

    Roč. 109, JUL (2015), s. 16-23. ISSN 0584-8547 R&D Projects: GA ČR GA14-23532S Grant ostatní: GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : hydride generation * arsenic * atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.176, year: 2014

  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. 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

  1. 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

  2. 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

  3. Ambient Mass Spectrometry Imaging Using Direct Liquid Extraction Techniques

    Energy Technology Data Exchange (ETDEWEB)

    Laskin, Julia; Lanekoff, Ingela

    2015-11-13

    Mass spectrometry imaging (MSI) is a powerful analytical technique that enables label-free spatial localization and identification of molecules in complex samples.1-4 MSI applications range from forensics5 to clinical research6 and from understanding microbial communication7-8 to imaging biomolecules in tissues.1, 9-10 Recently, MSI protocols have been reviewed.11 Ambient ionization techniques enable direct analysis of complex samples under atmospheric pressure without special sample pretreatment.3, 12-16 In fact, in ambient ionization mass spectrometry, sample processing (e.g., extraction, dilution, preconcentration, or desorption) occurs during the analysis.17 This substantially speeds up analysis and eliminates any possible effects of sample preparation on the localization of molecules in the sample.3, 8, 12-14, 18-20 Venter and co-workers have classified ambient ionization techniques into three major categories based on the sample processing steps involved: 1) liquid extraction techniques, in which analyte molecules are removed from the sample and extracted into a solvent prior to ionization; 2) desorption techniques capable of generating free ions directly from substrates; and 3) desorption techniques that produce larger particles subsequently captured by an electrospray plume and ionized.17 This review focuses on localized analysis and ambient imaging of complex samples using a subset of ambient ionization methods broadly defined as “liquid extraction techniques” based on the classification introduced by Venter and co-workers.17 Specifically, we include techniques where analyte molecules are desorbed from solid or liquid samples using charged droplet bombardment, liquid extraction, physisorption, chemisorption, mechanical force, laser ablation, or laser capture microdissection. Analyte extraction is followed by soft ionization that generates ions corresponding to intact species. Some of the key advantages of liquid extraction techniques include the ease

  4. Thermal Lens Spectrometry: Still a Technique on the Horizon?

    Science.gov (United States)

    Liu, Mingqiang; Franko, Mladen

    2016-07-01

    In this article, the historical development of thermal lens spectrometry (TLS) is briefly reviewed as an introduction. In continuation, the emphasis is on the recent progresses of TLS for measurements in ensembled sample cells and in microfluidic flow injection systems. Novel theories, instrumentation and their applications for high sample throughput for environmental, chemical and biomedical analysis, as well as thermal characterization and imaging, particularly in microspace, are presented. Discussion is given on the limitations of present TLS systems that open new horizons for future progress of this technique, which has already found place among routine techniques for chemical analysis. In the final section, proposals for the future development of TLS towards advanced applications in new research fields are presented.

  5. 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).

  6. Shape, size, and atomic composition analysis of nanostructures in 3D by Rutherford backscattering spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zolnai, Zsolt, E-mail: zolnai.zsolt@ttk.mta.hu

    2013-09-15

    The emergence of novel micro- and nanofabrication tools lead to the targeted research of highly ordered three-dimensional nanosystems, constructed from regular building blocks like spheres, cylinders, bricks, pyramids, which can be used in a wide range of applications. As a consequence, the exploration of the potential and limits of efficient analytical techniques to characterize structured nanosystems became a significant task. In this work the scope of conventional Rutherford backscattering spectrometry (RBS) analysis is extended to investigate highly ordered periodic nanostructures in three dimensions. Hexagonally arranged spherical and ellipsoidal silica particles, rectangular gold nano-arrays, and embedded structures in Si substrates and silica particles are analyzed. It is shown that the shape of the measured spectra can be correlated with the shape of individual nano-objects through geometrical considerations. The evaluation of the recorded data for different sample tilt angles can be carried out with the Monte-Carlo type 3D simulation model cell concept considering the details of the applied measurement geometry. It is demonstrated that macrobeam 3D-RBS can provide valuable information on the shape, size, spacing, and atomic composition of nanostructured samples as well as on nanoscale atomic transport processes and consequently, it can be utilized as a highly precise, non-destructive characterization tool for nanotechnology.

  7. 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)

  8. Using simple instrumentation to solve complex analytical problems: advanced AAS atomizers for volatile compounds and analyte trapping techniques

    Czech Academy of Sciences Publication Activity Database

    Dědina, Jiří; de Moraes, D. P.; Dessuy, M. B.; Kratzer, Jan; Řezáčová, Olga; Svoboda, Milan; Matoušek, Tomáš; de Moraes Flores, E. M.; Vale, M. G. R.

    2010. s. 59. [Rio Symposium on Atomic Spectrometry /11./. 24.10.2010-29.10.2010, Mar del Plata] R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : AAS * volatile compounds * analyte trapping techniques Subject RIV: CB - Analytical Chemistry, Separation http://www.11thriosymposium.com.ar/index.htm

  9. 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

  10. Evaluation of a method for the determination of chromium in urine by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A method for the determination of chromium in urine by atomic absorption spectrometry, using electrothermic atomization with pyrolytic graphite tubes, is proposed. The determinations are performed by standard addition. The method is applicable to biologic monitoring of populations with different degrees of exposition. It is also used in the analysis of chromium in sediments. Results of chromium in urine of a population group non-exposed to the metal are presented. 11 refs

  11. Arsenic speciation analysis by hydride generation – cryotrapping – atomic fluorescence spectrometry with flame-in-gas-shield atomizer

    Czech Academy of Sciences Publication Activity Database

    Svoboda, Milan; Musil, Stanislav; Matoušek, Tomáš; Rychlovský, P.; Dědina, Jiří

    Prague: Charles University in Prague, Faculty of Science, 2010 - (Nesměrák, K.), s. 19-22. (1). ISBN 978-80-7444-005-2. [International Students Conference "Modern Analytical Chemistry" /6./. Praha (CZ), 23.09.2010-24.09.2010] R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : arsenic speciation * cryogenic trapping * atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation

  12. 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

  13. An analysis of nuclear fuel burnup in the AGR-1 TRISO fuel experiment using gamma spectrometry, mass spectrometry, and computational simulation techniques

    International Nuclear Information System (INIS)

    Highlights: • The burnup of irradiated AGR-1 TRISO fuel was analyzed using gamma spectrometry. • The burnup of irradiated AGR-1 TRISO fuel was also analyzed using mass spectrometry. • Agreement between experimental results and neutron physics simulations was excellent. - Abstract: AGR-1 was the first in a series of experiments designed to test US TRISO fuel under high temperature gas-cooled reactor irradiation conditions. This experiment was irradiated in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL) and is currently undergoing post-irradiation examination (PIE) at INL and Oak Ridge National Laboratory. One component of the AGR-1 PIE is the experimental evaluation of the burnup of the fuel by two separate techniques. Gamma spectrometry was used to non-destructively evaluate the burnup of all 72 of the TRISO fuel compacts that comprised the AGR-1 experiment. Two methods for evaluating burnup by gamma spectrometry were developed, one based on the Cs-137 activity and the other based on the ratio of Cs-134 and Cs-137 activities. Burnup values determined from both methods compared well with the values predicted from simulations. The highest measured burnup was 20.1% FIMA (fissions per initial heavy metal atom) for the direct method and 20.0% FIMA for the ratio method (compared to 19.56% FIMA from simulations). An advantage of the ratio method is that the burnup of the cylindrical fuel compacts can be determined in small (2.5 mm) axial increments and an axial burnup profile can be produced. Destructive chemical analysis by inductively coupled mass spectrometry (ICP-MS) was then performed on selected compacts that were representative of the expected range of fuel burnups in the experiment to compare with the burnup values determined by gamma spectrometry. The compacts analyzed by mass spectrometry had a burnup range of 19.3% FIMA to 10.7% FIMA. The mass spectrometry evaluation of burnup for the four compacts agreed well with the gamma

  14. 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

  15. Determination of trace impurities in titanium dioxide by direct solid sampling electrothermal atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Vojtková, Blanka; Dočekal, Bohumil

    2005-01-01

    Roč. 99, S (2005), s489-s491. ISSN 0009-2770. [Meeting on Chemistry and Life /3./. Brno, 20.09.2005-22.09.2005] Institutional research plan: CEZ:AV0Z40310501 Keywords : solid sampling * electrothermal atomic absorption spectrometry * trace analysis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.445, year: 2005

  16. 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...

  17. 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.

  18. Air quality status in Kinshasa as determined by instrumental neutron activation analysis, atomic absorption spectrometry and ion-exchange chromatography

    International Nuclear Information System (INIS)

    Three independent analytical techniques - instrumental neutron activation analysis. Atomic absorption spectrometry and ion-exchange chromatography - were applied to airborne particulate collected on filters and to atmospheric acid gases collected in carbonate buffer solutions. 20 trace elements and 7 acid gases and acid aerosols were determined. Results were compared with those observed elsewhere and showed that air pollution is low in Kinshasa and does not give rise to anxieties. The main known sources of pollutants are: vehicle exhaust and aeolian process on stripped soils. (author). 13 refs, 2 figs, 6 tabs

  19. Ion beam analysis and spectrometry techniques for Cultural Heritage studies

    International Nuclear Information System (INIS)

    The implementation of experimental techniques for the characterisation of Cultural heritage materials has to take into account some requirements. The complexity of these past materials requires the development of new techniques of examination and analysis, or the transfer of technologies developed for the study of advanced materials. In addition, due to precious aspect of artwork it is also necessary to use the non-destructive methods, respecting the integrity of objects. It is for this reason that the methods using radiations and/or particles play a important role in the scientific study of art history and archaeology since their discovery. X-ray and γ-ray spectrometry as well as ion beam analysis (IBA) are analytical tools at the service of Cultural heritage. This report mainly presents experimental developments for IBA: PIXE, RBS/EBS and NRA. These developments were applied to the study of archaeological composite materials: layered materials or mixtures composed of organic and non-organic phases. Three examples are shown: evolution of silvering techniques for the production of counterfeit coinage during the Roman Empire and in the 16. century, the characterization of composites or mixed mineral/organic compounds such as bone and paint. In these last two cases, the combination of techniques gave original results on the proportion of both phases: apatite/collagen in bone, pigment/binder in paintings. Another part of this report is then dedicated to the non-invasive/non-destructive characterization of prehistoric pigments, in situ, for rock art studies in caves and in the laboratory. Finally, the perspectives of this work are presented. (author)

  20. Polymer architectures via mass spectrometry and hyphenated techniques: A review.

    Science.gov (United States)

    Crotty, Sarah; Gerişlioğlu, Selim; Endres, Kevin J; Wesdemiotis, Chrys; Schubert, Ulrich S

    2016-08-17

    This review covers the application of mass spectrometry (MS) and its hyphenated techniques to synthetic polymers of varying architectural complexities. The synthetic polymers are discussed as according to their architectural complexity from linear homopolymers and copolymers to stars, dendrimers, cyclic copolymers and other polymers. MS and tandem MS (MS/MS) has been extensively used for the analysis of synthetic polymers. However, the increase in structural or architectural complexity can result in analytical challenges that MS or MS/MS cannot overcome alone. Hyphenation to MS with different chromatographic techniques (2D × LC, SEC, HPLC etc.), utilization of other ionization methods (APCI, DESI etc.) and various mass analyzers (FT-ICR, quadrupole, time-of-flight, ion trap etc.) are applied to overcome these challenges and achieve more detailed structural characterizations of complex polymeric systems. In addition, computational methods (software: MassChrom2D, COCONUT, 2D maps etc.) have also reached polymer science to facilitate and accelerate data interpretation. Developments in technology and the comprehension of different polymer classes with diverse architectures have significantly improved, which allow for smart polymer designs to be examined and advanced. We present specific examples covering diverse analytical aspects as well as forthcoming prospects in polymer science. PMID:27286765

  1. Pulse nebulization atomic absorption spectrometry after preconcentration from acidic media

    International Nuclear Information System (INIS)

    The possible advantages of the combination: chlorinated solvent extraction - pulse nebulization, abomic absorption spectrometry (AAS), as well as application of this method to multi-element determination of several important trace elements in biological samples is investigated. Hexamethyleneammonium hexamethylenedithiocarbamate (HMA-HMDTC) and ammonium pyrrolidinedithiocarbamate (APDC) as regents and CCl4, CHCl3, butylacetate (BuOAc) and methylisobutyl ketone (MIBK) as organic solvents are utilized. There is a tendency that CCl4 is the best solvent and MIBK - the worst. The study of extraction efficiency versus the ratio of aqueous-to-organic phase also shows the advantages of chlorinated solvents for extraction from acidic media. Better results are obtained with HMA-HMDTC as a reagent for Cu and Pb, whereas, for Cd extraction APDC gave a more efficient extraction. Chloroform shows a higher sensitivity enhancement factor, especially for volatile and/or chloride-forming elements. The extraction is successfully applied to determination of Cd, Cu and Pb in tissues of alfalfa, cabbage, carrots, onions, potatoes and wheat, as well as two standard reference materials. The results are in good agreement with the certified values

  2. 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

  3. 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

  4. Vapor generation – atomic spectrometric techniques. Expanding frontiers through specific-species preconcentration. A review

    Energy Technology Data Exchange (ETDEWEB)

    Gil, Raúl A.; Pacheco, Pablo H.; Cerutti, Soledad [Área de Química Analítica, Facultad de Química Bioquímica y Farmacia, Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Instituto de Química de San Luis, INQUISAL, Centro Científico-Tecnológico de San Luis (CCT-San Luis), Consejo Nacional de Investigaciones Científicas y Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Martinez, Luis D., E-mail: ldm@unsl.edu.ar [Área de Química Analítica, Facultad de Química Bioquímica y Farmacia, Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Instituto de Química de San Luis, INQUISAL, Centro Científico-Tecnológico de San Luis (CCT-San Luis), Consejo Nacional de Investigaciones Científicas y Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina)

    2015-05-22

    This article reviews 120 articles found in SCOPUS and specific Journal cites corresponding to the terms ‘preconcentration’; ‘speciation’; ‘vapor generation techniques’ and ‘atomic spectrometry techniques’ in the last 5 years. - Highlights: • Recent advances in vapor generation and atomic spectrometry were reviewed. • Species-specific preconcentration strategies after and before VG were discussed. • New preconcentration and speciation analysis were evaluated within this framework. - Abstract: We review recent progress in preconcentration strategies associated to vapor generation techniques coupled to atomic spectrometric (VGT-AS) for specific chemical species detection. This discussion focuses on the central role of different preconcentration approaches, both before and after VG process. The former was based on the classical solid phase and liquid–liquid extraction procedures which, aided by automation and miniaturization strategies, have strengthened the role of VGT-AS in several research fields including environmental, clinical, and others. We then examine some of the new vapor trapping strategies (atom-trapping, hydride trapping, cryotrapping) that entail improvements in selectivity through interference elimination, but also they allow reaching ultra-low detection limits for a large number of chemical species generated in conventional VG systems, including complete separation of several species of the same element. This review covers more than 100 bibliographic references from 2009 up to date, found in SCOPUS database and in individual searches in specific journals. We finally conclude by giving some outlook on future directions of this field.

  5. Structural analyses of sucrose laurate regioisomers by mass spectrometry techniques

    DEFF Research Database (Denmark)

    Lie, Aleksander; Stensballe, Allan; Pedersen, Lars Haastrup

    2015-01-01

    6- And 6′-O-lauroyl sucrose were isolated and analyzed by matrix-assisted laser desorption/ionisation (MALDI) time-of-flight (TOF) mass spectrometry (MS), Orbitrap high-resolution (HR) MS, and electrospray-ionization (ESI) tandem mass spectrometry (MS/MS). The analyses aimed to explore the physic......6- And 6′-O-lauroyl sucrose were isolated and analyzed by matrix-assisted laser desorption/ionisation (MALDI) time-of-flight (TOF) mass spectrometry (MS), Orbitrap high-resolution (HR) MS, and electrospray-ionization (ESI) tandem mass spectrometry (MS/MS). The analyses aimed to explore...

  6. Determination of mercury by multisyringe flow injection system with cold-vapor atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A new software-controlled time-based multisyringe flow injection system for mercury determination by cold-vapor atomic absorption spectrometry is proposed. Precise known volumes of sample, reducing agent (1.1% SnCl2 in 3% HCl) and carrier (3% HCl) are dispensed into a gas-liquid separation cell with a multisyringe burette coupled with one three-way solenoid valve. An argon flow delivers the reduced mercury to the spectrometer. The optimization of the system was carried out testing reaction coils and gas-liquid separators of different design as well as changing parameters, such as sample and reagents volumes, reagent concentrations and carrier gas flow rate, among others. The analytical curves were obtained within the range 50-5000 ng L-1. The detection limit (3σ b/S) achieved is 5 ng L-1. The relative standard deviation (R.S.D.) was 1.4%, evaluated from 16 successive injections of 250 ng L-1 Hg standard solution. The injection and sample throughput per hour were 44 and 11, respectively. This technique was validated by means of solid and water reference materials with good agreement with the certified values and was successfully applied to fish samples

  7. 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.

  8. Optimization of conditions for the determination of Eu, Gd and Sm by atomic absorption spectrometry (AAS) and atomic emission spectrometry (AES)

    International Nuclear Information System (INIS)

    The possibilities of the determination of Sm, Eu and Gd by atomic absorption and emission spectrometry were investigated. Measurement parameters on a Varian atomic absorption spectrometer were optimized (the height of the measurement above the nozzle of the burner, stoichiometry of the dinitrogen oxide-acetylene flame by statistical evaluation of the signals). The following optimal conditions were found for the Sm, Eu and Gd determinations: Samarium - measurement under the emission arrangement at 476.1 nm wavelength, slit width 0.05 nm, in reduction flame close to the outlet slit of the flame (at the lowest part of the flame). Europium - measurement under the absorption arrangement at 459.4 nm wavelength, slit width 1 nm, in reduction flame at the lowest part of the flame. Gadolinium - measurement under the emission arrangement at 461.7 nm wavelength, slit width 0.05 nm, at the lowest part of the flame. (author). 2 figs., 3 tabs., 2 refs

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

    International Nuclear Information System (INIS)

    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 μg 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)

  10. 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.

  11. 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

  12. Determination of Cu, Cr, and As in preserved wood (Eucalyptus sp.) using x-ray fluorescent spectrometry techniques

    International Nuclear Information System (INIS)

    Energy dispersive (EDXRF) and Portable (PXRF) X-ray fluorescence techniques are proposed for wood treatment control process and wood waste assortment. In this study, different retentions of chromated copper arsenate preservative were applied to Eucalyptus sp. sapwood samples. Cu, Cr and As were determined by XRF techniques in treated sapwood massive blocks and treated sapwood sawdust samples were analyzed by FAAS spectrometry (Flame Atomic Absorption) and INAA (Instrumental Neutron Activation Analysis). Cu, Cr and As mean values, obtained by FAASS and INAA, showed to be statically equal; however, XRF analysis showed considerable deviations, presenting the absorption and the enhancement effects in analytical lines. (author)

  13. Fast atom bombardment and field desorption mass spectrometry

    International Nuclear Information System (INIS)

    Both FD and FAB have been developed to methods of high sensitivity to bioanalytical applications, which so far has been comparable in most cases, if estimated by the amount of material required in sample preparations for measurement. Unequivocal molecular weight determinations as the primary goal for an unknown compound from biological material are greatly facilitated by comparison of FD and FAB spectra, thus minimizing the risk of mis-information e.g. by molecular-cluster or other artifact ions which have been shown to occur by both techniques, and may be especially a problem in FAB spectra. The differences in the fragmentation behaviour as evident from some studies also suggest that the FAB method may be particularly suited for the analysis of compounds of extreme thermal lability, while FD may be the preferential method in cases where chemical lability and solubility present problems in the matrix preparation for FAB analysis. (orig./EF)

  14. Exploiting flow Injection and sequential injection schemes for trace metal determinations by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    Determination of low or trace-level amounts of metals by electrothermal atomic absorption spectrometry (ETAAS) often requires the use of suitable preconcentration and/or separation procedures in order to attain the necessary sensitivity and selectivity. Such schemes are advantageously executed in...... compensated by superior performance and versatility. In fact, two approaches are conceivable: The analyte-loaded ion-exchange beads might either be transported directly into the graphite tube where they are pyrolized and the measurand is atomized and quantified; or the loaded beads can be eluted and the...

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

    DEFF Research Database (Denmark)

    Sidenius, U; Gammelgaard, Bente

    2000-01-01

    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...... 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 as...

  16. 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.

  17. Arsenic speciation analysis by HPLC postcolumn hydride generation and detection by atomic fluorescence spectrometry

    Czech Academy of Sciences Publication Activity Database

    Marschner, Karel; Musil, Stanislav; Rychlovský, P.; Dědina, Jiří

    Prague: Charles University in Prague, Faculty of Science, 2014 - (Nesměrák, K.), s. 74-77 ISBN 978-80-7444-030-4. [International Students Conference "Modern Analytical Chemistry" /10./. Prague (CZ), 22.09.2014-23.09.2014] R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : arsenic speciation analysis * hydride generation * atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation http://www.natur.cuni.cz/isc-mac/

  18. 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...

  19. 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.

  20. New diagnostic technique for Zeeman-compensated atomic beam slowing: technique and results

    OpenAIRE

    Molenaar, P.A.; Van Der Straten, P.; Heideman, H.G.M.; Metcalf, H.

    2001-01-01

    We have developed a new diagnostic tool for the study of Zeeman-compensated slowing of an alkali atomic beam. Our time-of-flight technique measures the longitudinal veloc- ity distribution of the slowed atoms with a resolution below the Doppler limit of 30 cm/s. Furthermore, it can map the position and velocity distribution of atoms in either ground hyperfine level inside the solenoid without any devices inside the solenoid. The technique reveals the optical pumping ef- fects, and shows in de...

  1. Three axis vector atomic magnetometer utilizing polarimetric technique

    CERN Document Server

    Pradhan, Swarupananda

    2016-01-01

    The three axis magnetic field measurement based on the interaction of a single elliptically polarized light beam with an atomic system is described. The magnetic field direction dependent atomic responses are extracted by the polarimetric detection in combination with laser frequency modulation and magnetic field modulation techniques. The magnetometer offers additional critical requirements like compact size and large dynamic range for space application. Further, the three axis magnetic field is measured using only reflected signal from the polarimeter, thus can be easily expanded to make spatial array of detectors or / and high sensitivity field gradient measurement as required for biomedical application.

  2. 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.

  3. 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

  4. Development and applications of ionization techniques in ambient mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Rejšek, Jan; Vrkoslav, Vladimír; Cvačka, Josef

    Prague : Charles University in Prague, Faculty of Science, 2014 - (Nesměrák, K.), s. 37-38 ISBN 978-80-7444-030-4. [International Students Conference "Modern Analytical Chemistry" /10./. Praha (CZ), 22.09.2014-23.09.2014] R&D Projects: GA ČR GAP206/12/0750 Grant ostatní: GA AV ČR(CZ) M200551204 Institutional support: RVO:61388963 Keywords : ambient mass spectrometry * desorption electrospray ionization * desorption atmospheric pressure photoionization * thin-layer chromatography * insect defense compounds * mass spectrometry imaging Subject RIV: CB - Analytical Chemistry, Separation

  5. Ultratrace determination of mercury in water following EN and EPA standards using atomic fluorescence spectrometry.

    Science.gov (United States)

    Labatzke, Thomas; Schlemmer, Gerhard

    2004-02-01

    Chemical vapour generation has been used in combination with atomic fluorescence spectrometry to determine mercury at ultratrace concentrations down to 0.1 ng L(-1). A time-based injection of 1 mL of solution for measurement was sufficient to generate a steady-state detector response in the direct mode of measurement. The detection limit calculated from a ten-point calibration curve according to DIN 32645 was 0.26 ng L(-1). Instrument noise is limited by reflected radiation from the light source rather than by the dark current of the photomultiplier. The detection limit is directly influenced by the reagent blank which was 2 ng L(-1) in the experiments described. Focusing by amalgamation and subsequent thermal desorption generates a detector response which is about eight times higher in peak intensity and about twice as large in integrated intensity. The detection limit under these conditions is 0.09 ng L(-1) which can be further improved by preconcentration of larger volumes of solution for measurement. The cycle time for one individual reading is about 40 s without amalgamation and 125 s with amalgamation. The linear dynamic range of the system is five orders of magnitude with a single photomultiplier gain setting. The carry-over is less than 0.3% in direct measurement mode. Reference water samples and a surface water containing approximately 5 ng L(-1) were used to prove the validity of the method for real samples. Good accuracy and recoveries of 103% were calculated using the fast direct determination technique. PMID:14673566

  6. Nitride semiconductors studied by atom probe tomography and correlative techniques

    OpenAIRE

    Bennett, Samantha

    2011-01-01

    Optoelectronic devices fabricated from nitride semiconductors include blue and green light emitting diodes (LEDs) and laser diodes (LDs). To design efficient devices, the structure and composition of the constituent materials must be well-characterised. Traditional microscopy techniques used to examine nitride semiconductors include transmission electron microscopy (TEM), and atomic force microscopy (AFM). This thesis describes the study of nitride semiconductor materials using these tradi...

  7. Precision atomic physics techniques for nuclear physics with radioactive beams

    OpenAIRE

    Blaum, Klaus; Dilling, Jens; Nörtershäuser, Wilfried

    2013-01-01

    Atomic physics techniques for the determination of ground-state properties of radioactive isotopes are very sensitive and provide accurate masses, binding energies, Q-values, charge radii, spins, and electromagnetic moments. Many fields in nuclear physics benefit from these highly accurate numbers. They give insight into details of the nuclear structure for a better understanding of the underlying effective interactions, provide important input for studies of fundamental symmetries in physics...

  8. Slurry sampling procedure for the determination of lead in human hair by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. Human hair is a stable matrix that presents numerous advantages for human biomonitoring, such as easy collection, low cost, easy transport and storage, information about short- and long-term exposure (Angerer J et al., Int. J. Hyg. Environ. Health, 2007, 201-228). The use of the slurry sampling procedure was applied for the determination of lead in human hair by electrothermal atomic absorption spectrometry (ETAAS). This technique presents high sensitivity, low cost and the possibility of direct determination. Hair samples were pulverized using a cryogenic mill. Ten milligrams of the hair powder were transferred into a polyethylene vial and 2 ml of 2.5% HNO3 and 1.5% H2O2 were added. The slurries were maintained homogeneous with air bubbling with an aquarium pump. Niobium and Rhodium were chosen from several potential permanent modifiers by evaluating the background and absorbance signals obtained under the conditions recommended by the manufacturer. A 23 factorial design and a central composite design (CCD) were realized to optimize permanent modifier and pyrolysis and atomization temperatures. The parameters of merit were obtained in the optimized conditions (Tp = 660 deg C, Ta = 1780 deg C and Rh), and they were as follows: linear working range up to 50 μg L-1; limit of detection (0.032 0.002) μg g-1; limit of quantification (0.106 0.005) μg g-1; matrix-matched calibration, with r2 > 0.99 and reproducibility ranged from 2.3 to 4.2 relative standard deviation (RSD). The accuracy was evaluated by recovery tests and comparing slurry sampling and microwave decomposition. The recovery values for different concentrations were in the range between 89 and 101% and non-significant differences were observed (t-test; p = 0.05) when comparing the average of lead values obtained from microwave decomposition method and proposed method. Lead concentrations in different samples ranged between 0.13 and 1.11 μg g-1. The authors kindly

  9. Fourier transform infrared spectrometry: a versatile technique for real world samples.

    Science.gov (United States)

    Rintoul, L; Panayiotou, H; Kokot, S; George, G; Cash, G; Frost, R; Bui, T; Fredericks, P

    1998-04-01

    The versatility of FTIR spectrometry was explored by considering a variety of samples drawn from industrial applications, materials science and biomedical research. These samples included polymeric insulators, bauxite ore, clay, human hair and human skin. A range of sampling techniques suitable for these samples is discussed, in particular FTIR microscopy, FTIR emission spectroscopy, attenuated total reflectance and photoacoustic FTIR spectrometry. The power of modern data processing techniques, particularly multivariate analysis, to extract useful information from spectral data is also illustrated. PMID:9684399

  10. 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

  11. Implementation of suitable flow injection/sequential-sample separation/preconcentration schemes for determination of trace metal concentrations using detection by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Wang, Jianhua

    Various preconditioning procedures encomprising appropriate separation/preconcentration schemes in order to obtain optimal sensitivity and selectivity characteristics when using electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICPMS) are...

  12. Implementation of suitable flow injection/sequential-sample separation/preconcentration schemes for determination of trace metal concentrations using detection by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Wang, Jianhua

    2002-01-01

    Various preconditioning procedures encomprising appropriate separation/preconcentration schemes in order to obtain optimal sensitivity and selectivity characteristics when using electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICPMS) are...

  13. On-Line Preconcentration and Speciation of Chromium by an 8-Hydroxyquinoline Microcolumn Immobilized on Surfactant-Coated Alumina and Flow Injection Atomic Absorption Spectrometry

    OpenAIRE

    AHMADI, Seyyed Hamid; SHABANI, Ali Mohammad HAJI

    2007-01-01

    An on-line technique for the determination of chromium species with atomic absorption spectrometry is described. The method is based on separation and preconcentration of Cr(III) on a microcolumn of immobilized 8-hydroxyquinoline on surfactant-coated alumina. The adsorbed analyte is then eluted with 400 m L of 20% ethanolic solution of 1.5 mol L-1 hydrochloric acid and is transported to a flame atomic absorption spectrometer for quantification. The effects of pH, sample and eluent f...

  14. Method development for the determination of manganese, cobalt and copper in green coffee comparing direct solid sampling electrothermal atomic absorption spectrometry and inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Oleszczuk, Nédio; Castro, Jacira T; da Silva, Márcia M; Korn, Maria das Graças A; Welz, Bernhard; Vale, Maria Goreti R

    2007-10-31

    A method has been developed for the determination of cobalt, copper and manganese in green coffee using direct solid sampling electrothermal atomic absorption spectrometry (SS-ET AAS). The motivation for the study was that only a few elements might be suitable to determine the origin of green coffee so that the multi-element techniques usually applied for this purpose might not be necessary. The three elements have been chosen as test elements as they were found to be significant in previous investigations. A number of botanical certified reference materials (CRM) and pre-analyzed samples of green coffee have been used for method validation, and inductively coupled plasma optical emission spectrometry (ICP OES) after microwave-assisted acid digestion of the samples as reference method. Calibration against aqueous standards could be used for the determination of Mn and Co by SS-ET AAS, but calibration against solid CRM was necessary for the determination of Cu. No significant difference was found between the results obtained with the proposed method and certified or independently determined values. The limits of detection for Mn, Cu and Co were 0.012, 0.006 and 0.004mugg(-1) using SS-ET AAS and 0.015, 0.13 and 0.10mugg(-1) using ICP OES. Seven samples of Brazilian green coffee have been analyzed, and there was no significant difference between the values obtained with SS-ET AAS and ICP OES for Mn and Cu. ICP OES could not be used as a reference method for Co, as essentially all values were below the limit of quantification of this technique. PMID:19073113

  15. Development and applications of ionization techniques in ambient mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Rejšek, Jan; Vrkoslav, Vladimír; Cvačka, Josef

    Brno : Institute of Analytical Chemistry AS CR, 2014 - (Foret, F.; Křenková, J.; Drobníková, I.; Guttman, A.; Klepárník, K.), s. 97-98 ISBN 978-80-904959-2-0. [CECE 2014. International Interdisciplinary Meeting on Bioanalysis /11./. Brno (CZ), 20.10.2014-22.10.2014] R&D Projects: GA ČR GP13-25137P; GA ČR GAP206/12/0750 Grant ostatní: GA AV ČR(CZ) M200551204 Institutional support: RVO:61388963 Keywords : ambient mass spectrometry * desorption electrospray ionization * desorption atmospheric pressure photoionization * thin-layer chromatography * insect defense compounds * mass spectrometry imaging Subject RIV: CB - Analytical Chemistry, Separation

  16. 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

  17. Inductively coupled plasma-atomic emission spectrometry (ICP-AES) in support of nuclear waste management

    International Nuclear Information System (INIS)

    Simulated complex nuclear waste solutions are characterized by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AEC). The system uses and ICP source focused on both a polychromator and a computer-controlled scanning monochromator for intensity measurements. This instrumentation allows for simultaneous and sequential measurements of liquid extraction distribution coefficients needed in the development of process flow sheets for component separations. A large number of elements are determined rapidly with adequate sensitivity and accuracy. The focus of this investigation centers on the analysis of nuclear fission products. 13 references, 13 tables

  18. 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

  19. Chloride isolation for accelerator mass spectrometry of 36Cl produced by atomic bomb neutrons

    International Nuclear Information System (INIS)

    Accelerator mass spectrometry was performed at the Munich tandem laboratory to determine the ratio of 36Cl/Cl in silicate rock samples exposed to neutrons of the Hiroshima atomic bomb. Chloride was chemically separated from silicate rock for this purpose. Five grams of silicate rock was fused with 30 g of sodium hydroxide and dissolved in 900 ml of water. The chloride in the resulting solution was spectrophotometrically determined. Chloride was precipitated as silver chloride by addition of appropriate amounts of silver nitrate, and silver chloride was then collected on a membrane filter. The chloride in the rock samples was thus isolated quantitatively. (author)

  20. 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.

  1. Speciation of organometallic compounds by Zeeman atomic absorption spectrometry with liquid chromatography

    International Nuclear Information System (INIS)

    A method for the determination of organometallic compounds in the ppB range includes separation of the desired species with a high pressure liquid chromatograph and determination of the trace element by Zeeman atomic absorption spectrometry. The analysis of a mixture of vitamin B12 and Co(NO3)2 is described as a demonstration of the method. Determination of many enzymes and coenzymes having a metal ion in their functional center and of many toxic metals in environmental samples are other fields for application of this method

  2. Atomization in graphite-furnace atomic absorption spectrometry. Peak-height method vs. integration method of measuring absorbance: heated graphite atomizer 2100

    International Nuclear Information System (INIS)

    The signal integration technique developed and reported earlier has been used for measuring atomic absorption signals generated by the Heated Graphite Atomizer 2100. Cd, Zn, Al, Sn, Cu, Mo, and V have been selected for this study. In theory, the integration method of measuring absorbance is superior to the conventional peak-height as the measure of absorbance. In practice, integration does offer some advantages over the peak-height method of measurement; absolute sensitivity is increased by a factor of 2- to 8-fold and the linear range of the working curves is increased by a factor of up to 2. This study shows the effect of the better cell geometry of the HGA 2100 (as opposed to the Carbon Rod Atomizer 63) on the integrated absorbance signals. Modifications to the Heated Graphite Atomizer 2100 which would improve the atomization conditions beneficial to the integration method of measuring are suggested. (U.S.)

  3. 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)

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

    International Nuclear Information System (INIS)

    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)

  5. ALCHEMI: a new technique for locating atoms in small crystals

    International Nuclear Information System (INIS)

    Atom Location by Channelling Enhanced Microanalysis (ALCHEMI) is a quantitative technique for identifying the crystallographic sites, distribution and types of substitutional impurities in many crystals. The method involves no adjustable parameters, can be applied to areas as small as a few hundred Angstroms and to impurity concentrations down to about 0.1 atomic per cent. It is capable of distinguishing neighbours in the periodic table. The method uses the incident electron beam orientation dependence of characteristic X-ray emission and uses an energy dispersive X-ray microanalyser fitted to a transmission electron microscope. The method does not require the specimen thickness or precise orientation to be known, and makes few assumptions about the form of the dynamical electron wavefunction, which need not be calculated or predicted. The classical problems of cation ordering in spinels, feldspars and olivine have now been studied by this method. (author)

  6. Improvements in cobalt determination by thermospray flame furnace atomic absorption spectrometry using an on-line derivatization strategy.

    Science.gov (United States)

    Matos, Geraldo Domingues; Arruda, Marco Aurélio Zezzi

    2008-07-15

    An on-line derivatization strategy was developed for improving cobalt sensitivity using thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) as the analytical technique. This strategy involves the generation of a volatile cobalt compound, providing better sample vaporization efficiency. The effect of sodium diethyldithiocarbamate (DDTC) as complexing agent on the integrated absorbance signal was evaluated. Parameters including the pH of complex formation, complex concentration and volume, sample volume, flame gas composition and tube atomization configuration were optimized. A wide linear range (from 23 microg L(-1) to 3 mg L(-1); r(2)=0.9786) was obtained, with the best one (r(2)=0.9992) attained from 23 to 400 microg L(-1) with a sample throughput of 30 h(-1). The improvement in the detection power was 17-fold when compared to FAAS, which provides 7 microg L(-1) as the limit of detection when considered TS-FF-AAS technique. A relative standard deviation (n=10) of 4% for a cobalt solution containing 50 microg L(-1) was attained, and the accuracy of the procedure was evaluated through certified reference materials (IAEA-SL-1, lake sediment; and ISS-MURST-A1, Antarctic marine sediment). Good agreement between the results at the 95% confidence level was observed. PMID:18585309

  7. 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.)

  8. 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:

  9. 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

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

    International Nuclear Information System (INIS)

    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 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

  11. Nonlinear control techniques for an atomic force microscope system

    Institute of Scientific and Technical Information of China (English)

    Yongchun FANG; Matthew FEEMSTER; Darren DAWSON; Nader M.JALILI

    2005-01-01

    Two nonlinear control techniques are proposed for an atomic force microscope system.Initially,a learning-based control algorithm is developed for the microcantilever-sample system that achieves asymptotic cantilever tip tracking for periodic trajectories.Specifically,the control approach utilizes a learning-based feedforward term to compensate for periodic dynamics and high-gain terms to account for non-periodic dynamics.An adaptive control algorithm is then developed to achieve asymptotic cantilever tip tracking for bounded tip trajectories despite uncertainty throughout the system parameters.Simulation results are provided to illustrate the efficacy and performance of the control strategies.

  12. 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

  13. Assessment of cadmium and iron adsorption in sediment, employing a flow injection analysis system with on line filtration and detection by flame atomic absorption spectrometry and thermospray flame furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Graphical abstract: -- Highlights: •A FIA system with on-line filtration for isotherms adsorption studies was proposed. •Isotherms for iron and cadmium elements in bottom lake sediment were done. •Inferences about adsorption/desorption mechanisms were feasible. •The proposed method turns the isotherm studies fast and reliable. -- Abstract: This work presents an evaluation of iron and cadmium adsorption in sediment of the Furnas Hydroelectric Plant Reservatory located in Alfenas, Minas Gerais (Brazil). The metal determination was done employing a flow injection analysis (FIA) with an on-line filtering system. As detection techniques, flame atomic absorption spectrometry (FAAS) for iron and thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) for cadmium determinations were used. The developed methodology presented good limits of detection, being 190 μg L−1 for iron and 1.36 μg L−1 for cadmium, and high sampling frequency for both metals 144 and 60 readings h−1 for iron and cadmium, respectively. Both metals obey the Langmuir model, with maximum adsorptive capacity of 0⋅169 mg g−1 for iron and 7⋅991 mg g−1 for cadmium. For iron, a pseudo-first-order kinetic model was obtained with a theoretical Qe = 9⋅8355 mg g−1 (experimental Qe = 9⋅5432 mg g−1), while for cadmium, a pseudo-second-order kinetic model was obtained, with a theoretical Qe = 0.3123 mg g−1 (experimental Qe = 0⋅3052 mg g−1)

  14. 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

  15. Cooperative analysis of alloying elements in zirconium alloys using inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    The Second Sub-Committee on Zircaloy Analysis, under Committee on Analytical Chemistry of Nuclear Fuels and Reactor Materials, JAERI, carried out a cooperative analysis with the nine laboratories on the determination of tin, iron, nickel and chromium in zirconium alloys to evaluate the practical applicability of inductively coupled plasma (ICP) atomic emission spectrometry. This report describes the sample decomposition procedures, determination conditions and procedures, and analytical results. The results obtained for alloying elements in samples for cooperative analysis (JAERI CRMs Z11 to Z14 and others) were compared with certified values or those obtained by X-ray fluorescence method, and were in good agreement with those values. ICP atomic emission spectrometry were shown to be an effective field method for determining alloying elements (C.V. % 2 to 7 for 0.5 to 1.90 % Sn, C.V. % 2 to 3 for 0.093 to 0.130 % Fe, C.V. % 3 to 6 for 0.095 to 0.110 % Ni and C.V. % 2 to 7 for 0.01 to 0.150 % Cr) in zirconium alloys. (author)

  16. 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)

  17. 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 .

  18. Electron--photon coincidence technique for electron impact on atoms

    International Nuclear Information System (INIS)

    A brief introduction is given to the general theory of the electron photon coincidence technique, and the specific application to 1P and 3P excitations in helium is described. The relation between the complex excitation amplitudes which characterize the collision process and the alignment and orientation of the excited atoms is emphasized. The data from the first electron photon angular correlation measurements are presented. These data yield values for the ratio of differential cross sections for exciting the degenerate sublevels and the relative phase of the corresponding amplitudes, or, equivalently, the alignment and orientation parameters. The results are obtained in dimensionless form and are free from absolute calibration or normalization difficulties. They are compared with various theoretical approximations. The application of the coincidence technique to a measurement of threshold polarization is described and results for 31P excitations are discussed

  19. Multivariate techniques of analysis for ToF-E recoil spectrometry data

    Energy Technology Data Exchange (ETDEWEB)

    Whitlow, H.J.; Bouanani, M.E.; Persson, L.; Hult, M.; Jonsson, P.; Johnston, P.N. [Lund Institute of Technology, Solvegatan, (Sweden), Department of Nuclear Physics; Andersson, M. [Uppsala Univ. (Sweden). Dept. of Organic Chemistry; Ostling, M.; Zaring, C. [Royal institute of Technology, Electrum, Kista, (Sweden), Department of Electronics; Johnston, P.N.; Bubb, I.F.; Walker, B.R.; Stannard, W.B. [Royal Melbourne Inst. of Tech., VIC (Australia); Cohen, D.D.; Dytlewski, N. [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1996-12-31

    Multivariate statistical methods are being developed by the Australian -Swedish Recoil Spectrometry Collaboration for quantitative analysis of the wealth of information in Time of Flight (ToF) and energy dispersive Recoil Spectrometry. An overview is presented of progress made in the use of multivariate techniques for energy calibration, separation of mass-overlapped signals and simulation of ToF-E data. 6 refs., 5 figs.

  20. Multivariate techniques of analysis for ToF-E recoil spectrometry data

    International Nuclear Information System (INIS)

    Multivariate statistical methods are being developed by the Australian -Swedish Recoil Spectrometry Collaboration for quantitative analysis of the wealth of information in Time of Flight (ToF) and energy dispersive Recoil Spectrometry. An overview is presented of progress made in the use of multivariate techniques for energy calibration, separation of mass-overlapped signals and simulation of ToF-E data. 6 refs., 5 figs

  1. Simultaneous multielement analysis of rock samples by inductively coupled plasma mass spectrometry using discrete microsampling technique

    International Nuclear Information System (INIS)

    Simultaneous multielement analysis of geological standard rock samples (JG-1 and JB-2) has been successfully performed by inductively coupled plasma mass spectrometry using a discrete microsampling technique. In this technique only 100 μl sample solution was used for simultaneous determination of 5-10 elements in solution. (author)

  2. Neutral atom beam technique enhances bioactivity of PEEK

    Energy Technology Data Exchange (ETDEWEB)

    Khoury, Joseph, E-mail: jkhoury@exogenesis.us [Exogenesis Corporation, Billerica, MA 01821 (United States); Kirkpatrick, Sean R.; Maxwell, Melissa; Cherian, Raymond E.; Kirkpatrick, Allen; Svrluga, Richard C. [Exogenesis Corporation, Billerica, MA 01821 (United States)

    2013-07-15

    Polyetheretherketone (PEEK) is currently gaining popularity in orthopedic and spinal applications but has potential drawbacks in use. PEEK is biocompatible, similar in elasticity to bone, and radiolucent; however, it has been shown to be inert and does not integrate well with bone. Recent efforts have focused on increasing the bioactivity of PEEK by modifying the surface to improve the bone-implant interface. We have employed a novel Accelerated Neutral Atom Beam technique (ANAB) to enhance the bioactivity of PEEK. ANAB employs an intense beam of cluster-like packets of accelerated unbonded neutral argon (Ar) gas atoms. These beams are created by first producing a highly energetic Gas Cluster Ion Beam (GCIB) comprised of van der Waals bonded Ar atoms, then transferring energy to the clusters so as to cause release of most of the interatomic bonds, and finally deflecting away the remaining electrically charged cluster cores of still bonded atoms. We identified that ANAB treatment of PEEK results in nanometer scale surface modifications as well as increased surface hydrophilicity. Human osteoblasts seeded onto the surface of ANAB-treated PEEK exhibited enhanced growth as compared to control PEEK as evidenced by cell proliferation assays and microscopy. This increase in bioactivity resulted in cell proliferation levels comparable to native titanium. An in vivo study using a rat calvarial critical size defect model revealed enhanced osseointegration where bone tissue formation was evident only on the ANAB treated PEEK. Taken together, these data suggest that ANAB treatment of PEEK has the potential to enhance its bioactivity, resulting in bone formation and significantly decreasing osseointegration time of orthopedic and spinal implants.

  3. Neutral atom beam technique enhances bioactivity of PEEK

    International Nuclear Information System (INIS)

    Polyetheretherketone (PEEK) is currently gaining popularity in orthopedic and spinal applications but has potential drawbacks in use. PEEK is biocompatible, similar in elasticity to bone, and radiolucent; however, it has been shown to be inert and does not integrate well with bone. Recent efforts have focused on increasing the bioactivity of PEEK by modifying the surface to improve the bone-implant interface. We have employed a novel Accelerated Neutral Atom Beam technique (ANAB) to enhance the bioactivity of PEEK. ANAB employs an intense beam of cluster-like packets of accelerated unbonded neutral argon (Ar) gas atoms. These beams are created by first producing a highly energetic Gas Cluster Ion Beam (GCIB) comprised of van der Waals bonded Ar atoms, then transferring energy to the clusters so as to cause release of most of the interatomic bonds, and finally deflecting away the remaining electrically charged cluster cores of still bonded atoms. We identified that ANAB treatment of PEEK results in nanometer scale surface modifications as well as increased surface hydrophilicity. Human osteoblasts seeded onto the surface of ANAB-treated PEEK exhibited enhanced growth as compared to control PEEK as evidenced by cell proliferation assays and microscopy. This increase in bioactivity resulted in cell proliferation levels comparable to native titanium. An in vivo study using a rat calvarial critical size defect model revealed enhanced osseointegration where bone tissue formation was evident only on the ANAB treated PEEK. Taken together, these data suggest that ANAB treatment of PEEK has the potential to enhance its bioactivity, resulting in bone formation and significantly decreasing osseointegration time of orthopedic and spinal implants

  4. Neutral atom beam technique enhances bioactivity of PEEK

    Science.gov (United States)

    Khoury, Joseph; Kirkpatrick, Sean R.; Maxwell, Melissa; Cherian, Raymond E.; Kirkpatrick, Allen; Svrluga, Richard C.

    2013-07-01

    Polyetheretherketone (PEEK) is currently gaining popularity in orthopedic and spinal applications but has potential drawbacks in use. PEEK is biocompatible, similar in elasticity to bone, and radiolucent; however, it has been shown to be inert and does not integrate well with bone. Recent efforts have focused on increasing the bioactivity of PEEK by modifying the surface to improve the bone-implant interface. We have employed a novel Accelerated Neutral Atom Beam technique (ANAB) to enhance the bioactivity of PEEK. ANAB employs an intense beam of cluster-like packets of accelerated unbonded neutral argon (Ar) gas atoms. These beams are created by first producing a highly energetic Gas Cluster Ion Beam (GCIB) comprised of van der Waals bonded Ar atoms, then transferring energy to the clusters so as to cause release of most of the interatomic bonds, and finally deflecting away the remaining electrically charged cluster cores of still bonded atoms. We identified that ANAB treatment of PEEK results in nanometer scale surface modifications as well as increased surface hydrophilicity. Human osteoblasts seeded onto the surface of ANAB-treated PEEK exhibited enhanced growth as compared to control PEEK as evidenced by cell proliferation assays and microscopy. This increase in bioactivity resulted in cell proliferation levels comparable to native titanium. An in vivo study using a rat calvarial critical size defect model revealed enhanced osseointegration where bone tissue formation was evident only on the ANAB treated PEEK. Taken together, these data suggest that ANAB treatment of PEEK has the potential to enhance its bioactivity, resulting in bone formation and significantly decreasing osseointegration time of orthopedic and spinal implants.

  5. 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

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Matoušek, Tomáš; Currier, J. M.; Stýblo, M.; Dědina, Jiří

    2014-01-01

    Roč. 86, č. 20 (2014), s. 10422-10428. ISSN 0003-2700 R&D Projects: GA ČR GA14-23532S; GA MŠk LH12040 Institutional support: RVO:68081715 Keywords : speciation analysis of arsenic * selective hydride generation * flame-in-gas-shield atomizer * cryotrapping-atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 5.636, year: 2014

  6. 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...

  7. Direct determination of lead in sweet fruit-flavored powder drinks by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Lima, Éder C.; Krug, Francisco José; Arruda, Marco A. Z.

    1998-04-01

    A simplified method for direct determination of lead in sweet fruit-flavored powder drinks, syrups and honeys by electrothermal atomic absorption spectrometry without sample digestion is proposed. Samples were dissolved in water, acidified to 0.2% (v/v) HNO 3, and directly injected into an end-capped transversely heated graphite atomizer (THGA). Building up of carbonaceous residue inside the atomizer was effectively precluded for sugar solutions not exceeding 8.0% (m/v) when a heating program with two pyrolysis steps (600 and 1000°C) was carried out without air-ashing. Under these conditions one atomizer supported about 250 firings. Among various chemical modifiers tested, better recovery and repeatability results were obtained with a 5 μg Pd + 3 μg Mg(NO 3) 2 mixture. Tests carried out with individual concomitants containing up to 1.0 μg Na, K, Ca or Cl, and up to 10.0 μg phosphate or sulphate, and several mixtures of these six concomitants, did not reveal significant interferences on lead atomization. Characteristic mass and detection limit based on integrated absorbance were 15 and 11 pg Pb, respectively. The relative standard deviation based on 10 measurements for typical samples (20-60 ng g -1 Pb) was always lower than 5.5%. The detection limit of 7.0 ng g -1 Pb attained the Codex recommendation for the maximum allowed lead contents in the sugar samples. Application of t-test to the results obtained by the proposed direct analysis, and the official method adopted by Food Chemical Codex, demonstrated that there were no significant differences at the 5% probability level.

  8. 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...

  9. 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.

  10. Determination of bismuth in environmental samples by slurry sampling graphite furnace atomic absorption spectrometry using combined chemical modifiers.

    Science.gov (United States)

    Dobrowolski, Ryszard; Dobrzyńska, Joanna; Gawrońska, Barbara

    2015-01-01

    Slurry sampling graphite furnace atomic absorption spectrometry technique was applied for the determination of Bi in environmental samples. The study focused on the effect of Zr, Ti, Nb and W carbides, as permanent modifiers, on the Bi signal. Because of its highest thermal and chemical stability and ability to substantially increase Bi signal, NbC was chosen as the most effective modifier. The temperature programme applied for Bi determination was optimized based on the pyrolysis and atomization curves obtained for slurries prepared from certified reference materials (CRMs) of the soil and sediments. To overcome interferences caused by sulfur compounds, Ba(NO₃)₂ was used as a chemical modifier. Calibration was performed using the aqueous standard solutions. The analysis of the CRMs confirmed the reliability of the proposed analytical method. The characteristic mass for Bi was determined to be 16 pg with the detection limit of 50 ng/g for the optimized procedure at the 5% (w/v) slurry concentration. PMID:25384374

  11. Determination of vanadium in soils and sediments by the slurry sampling graphite furnace atomic absorption spectrometry using permanent modifiers.

    Science.gov (United States)

    Dobrowolski, Ryszard; Adamczyk, Agnieszka; Otto, Magdalena

    2013-09-15

    A new analytical procedure for vanadium (V) determination in soils and sediments by the slurry sampling graphite furnace atomic absorption spectrometry (slurry sampling GFAAS) using the mixed permanent modifiers is described. Moreover, the comparison of action of the modifiers based on the iridium (Ir) and carbide-forming elements: tungsten (W) and niobium (Nb) deposited on the graphite tubes is studied, especially in terms of their analytical utility and determination sensitivity. The mechanism of their action was investigated using an X-ray diffraction technique (XRD) and scanning electron microscopy (SEM) equipped with an energy dispersive X-ray detector (EDX). Finally, the mixture of 0.3 μg of Ir and 0.04 μg of Nb was used for the graphite tube permanent modification. The analytical procedure was optimized on the basis of the data from pyrolysis and atomization temperature curves studies. The results obtained for the four certified reference materials (marine sediments: PACS-1 and MESS-1, lake sediment: SL-1, soil: San Joaquin Soil SRM 2709), using the slurry sampling GFAAS and the standard calibration method, were in good agreement with the certified values. The detection and quantification limits and characteristic mass calculated for the proposed procedure were 0.04 µg/g, 0.16 µg/g and 11.9 pg, respectively. The precision (RSD% less than 8%) and the accuracy of vanadium determination in the soil and sediment samples were acceptable. PMID:23708618

  12. 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

  13. Synchrotron radiation, neutron, and mass spectrometry techniques at user facilities

    OpenAIRE

    Sutton, S. R.; Caffee, M. W.; Dove, M. T.

    2006-01-01

    User research facilities around the world offer tremendous opportunities for scientific experimentation by members of the Earth science community. Synchrotron radiation sources, neutron sources, mass spectrometers, and others represent a powerful force in tackling complex scientific problems. In these techniques, Earth materials are bombarded with beams of ions, subatomic particles and/or photons to learn the secr...

  14. 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

  15. Different platform and tube geometries and atomization temperatures in graphite furnace atomic absorption spectrometry: Cadmium determination in whole blood as a case study

    International Nuclear Information System (INIS)

    In the present work the performance of different platform and tube geometries and atomization temperatures in graphite furnace atomic absorption spectrometry was investigated, using the determination of Cd in whole blood as an example. Grooved, integrated and fork platforms as well as atomization temperatures between 1200 deg. C and 2200 deg. C were investigated in a longitudinally heated graphite atomizer and compared with the performance of a transversely heated furnace. In the longitudinally heated furnace the increase of the atomization temperature in the studied range resulted in an increase of matrix effects for all platform geometries. The integrated platform exhibited slightly lower sensitivity and increased multiplicative interferences in comparison to the other two platform designs. Interference-free Cd determination was possible with all types of platforms and 1200 deg. C as the atomization temperature as well as with grooved and fork platforms at 1700 deg. C. On the other hand, lower atomization temperatures resulted in poorer limits of detection, due to the longer integration time needed. No matrix effect was observed at any atomization temperature using the transversely heated atomizer; in addition, limits of detection were better than those observed with the longitudinally heated atomizer. Best values were around 0.02 μg L-1 with the latter atomizer compared to values around 0.02 μg L-1 with the former one

  16. 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.

  17. 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.

  18. 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)

  19. 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.

  20. 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)

  1. 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.

  2. 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)%.

  3. Determination of mineral elements in fresh olive fruits by flame atomic spectrometry

    International Nuclear Information System (INIS)

    The mineral element characterisation of olive fruits is acquiring interest to evaluate the link between their nutritional status and the olive oil quality. A method for the analysis of mineral elements in fresh olive fruits is proposed. The presence of mineral elements such as potassium, sodium, calcium, magnesium, zinc, copper, iron, and manganese in olive fruits was quantified by flame atomic absorption spectrometry. The limits of quantification were (expressed in mg kg.1 of dry weight) 1.266, 1.569, 0.272, 0.172, 0.268, 0.316, 1.017 and 0.513 for K, Na, Ca, Mg, Zn, Cu, Fe and Mn, respectively. The results showed the method is a robust, reliable, and simple analytical procedure for the mineral element characterisation of olive fruit. (Author).

  4. 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

    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...... spectrometry (ICP-MS). The signal-to-noise ratio of the FAAS detector was optimized using a hydrogen-argon entrained-air flame and a slotted-tube atom trap (STAT) in the flame. The limit of detection (3 sigma) achieved by the HPLC-FAAS system was 1 mg L-1 of selenium (100 mu L injections) for each of the four...

  5. On-line sample processing involving microextraction techniques as a front-end to atomic spectrometric detection for trace metal assays: A review

    Energy Technology Data Exchange (ETDEWEB)

    Miró, Manuel, E-mail: manuel.miro@uib.es [FI-TRACE Group, Department of Chemistry, Faculty of Sciences, University of the Balearic Islands, E-07122 Palma de Mallorca, Illes Balears (Spain); Hansen, Elo Harald [Granåsen 93, DK-2800 Kgs. Lyngby (Denmark)

    2013-06-11

    Graphical abstract: -- Highlights: •Role of flow injection in automation of microextraction techniques for metal assays. •On-line coupling of liquid phase microextraction (LPME) to atomic spectrometry. •Critical evaluation of on-line single drop and dispersive LPME. •On-line coupling of micro-solid phase extraction (μSPE) to atomic spectrometry. •Critical appraisal of magnetic/carbon nanoparticles and biomass for on-line μSPE. -- Abstract: Within the last decade, liquid-phase microextraction (LPME) and micro-solid phase extraction (μSPE) approaches have emerged as substitutes for conventional sample processing procedures for trace metal assays within the framework of green chemistry. This review surveys the progress of the state of the art in simplification and automation of microextraction approaches by harnessing to the various generations of flow injection (FI) as a front end to atomic absorption spectrometry (AAS), atomic fluorescence spectrometry (AFS) or inductively coupled plasma atomic emission spectrometry or mass spectrometry (ICP-AES/MS). It highlights the evolution of flow injection analysis and related techniques as vehicles for appropriate sample presentation to the detector and expedient on-line matrix separation and pre-concentration of trace levels of metals in troublesome matrices. Rather than being comprehensive this review is aimed at outlining the pros and cons via representative examples of recent attempts in automating green sample preparation procedures in an FI or sequential injection (SI) mode capitalizing on single-drop microextraction, dispersive liquid-phase microextraction and advanced sorptive materials including carbon and metal oxide nanoparticles, ion imprinted polymers, superparamagnetic nanomaterials and biological/biomass sorbents. Current challenges in the field are identified and the synergetic combination of flow analysis, nanotechnology and metal-tagged biomolecule detection is envisaged.

  6. Analytical performance of a low-gas-flow torch optimized for inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Montaser, A.; Huse, G.R.; Wax, R.A.; Chan, S.-K.; Golightly, D.W.; Kane, J.S.; Dorrzapf, A.F., Jr.

    1984-01-01

    An inductively coupled Ar plasma (ICP), generated in a lowflow torch, was investigated by the simplex optimization technique for simultaneous, multielement, atomic emission spectrometry (AES). The variables studied included forward power, observation height, gas flow (outer, intermediate, and nebulizer carrier) and sample uptake rate. When the ICP was operated at 720-W forward power with a total gas flow of 5 L/min, the signal-to-background ratios (S/B) of spectral lines from 20 elements were either comparable or inferior, by a factor ranging from 1.5 to 2, to the results obtained from a conventional Ar ICP. Matrix effect studies on the Ca-PO4 system revealed that the plasma generated in the low-flow torch was as free of vaporizatton-atomizatton interferences as the conventional ICP, but easily ionizable elements produced a greater level of suppression or enhancement effects which could be reduced at higher forward powers. Electron number densities, as determined via the series until line merging technique, were tower ht the plasma sustained in the low-flow torch as compared with the conventional ICP. ?? 1984 American Chemical Society.

  7. 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

  8. Ultrasound-assisted emulsification of cosmetic samples prior to elemental analysis by different atomic spectrometric techniques.

    Science.gov (United States)

    Lavilla, I; Cabaleiro, N; Costas, M; de la Calle, I; Bendicho, C

    2009-11-15

    In this work, ultrasound-assisted emulsification with a probe system is proposed as a rapid and simple sample treatment for atomic spectrometric determinations (Electrothermal Atomic Absorption Spectrometry, Inductively Coupled Plasma Optical Emission Spectrometry, Flame Atomic Absorption Spectrometry and Cold Vapour Atomic Absorption Spectrometry) of trace elements (As, Cd, Cr, Cu, Hg, Mg, Mn, Ni, Sr and Zn) in cosmetic samples such as shampoos, gel (hair gel), crèmes (body milk, hair conditioner) and oil (body oil). The type of dispersion medium, the sample mass-to-dispersion medium volume ratio, as well as the parameters related to the ultrasound-assisted emulsification (sonication amplitude and treatment time) were exhaustively studied. Only 1 min of ultrasonic shaking and a dispersion medium containing 0.5% (w/v) of SDS+3% (v/v) of HNO(3) or HCl allows obtaining a stable emulsion at least for 3 months. Thermal programs, nebulization of emulsions, speed of pumps and concentration of reagents used in cold vapour generation were optimized. Calibration using aqueous standards was feasible in all cases. Calibration by the standard addition method and recovery studies was also applied for validation. Microwave-assisted digestion and Inductively Coupled Plasma Mass Spectrometry were used for comparison purposes. Relative standard deviations from analysis of five independent emulsions were less than 9% in all cases. PMID:19782199

  9. Arsenic speciation in drugs by selective hydride generation-cryotrapping-gas chromatography-atomic absorption spectrometry with the multiatomizer

    Czech Academy of Sciences Publication Activity Database

    de Moraes, D. P.; Dědina, Jiří; Matoušek, Tomáš; de Moraes Flores, E. M.

    2010. s. 183. [Rio Symposium on Atomic Spectrometry /11./. 24.10.2010-29.10.2010, Mar del Plata] R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : arsenic * HG-CT-AAS * multiatomizer Subject RIV: CB - Analytical Chemistry, Separation http://www.11thriosymposium.com.ar/index.htm

  10. New cryogenic trap design for speciation analysis of Arsenic by generation of substituted hydrides-atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Svoboda, Milan; Kratzer, Jan; Dědina, Jiří

    2014. s. 196-196. [Rio Symposium on Atomic Spectrometry /13./. 19.10.2014-24.10.2014, Merida, Yucatan] R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : cryotrapping * hydride generation * arsenic speciation analysis Subject RIV: CB - Analytical Chemistry, Separation

  11. 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

  12. 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...

  13. 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…

  14. Determination of total selenium in nutritional supplements and selenised yeast by Zeeman-effect graphite furnace atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Ekelund, J.

    1989-01-01

    -effect background corrected graphite furnace atomic absorption spectrometry. A furnace ashing step at 1100 °C was necessary in order to obtain a total recovery of selenium when present in the organic form. Palladium nitrate-magnesium nitrate was used as a matrix modifier. Independent methods were used to determine...

  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 tellurium in indium antimonide semiconductor material by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Shiue, M Y; Sun, Y C; Yang, M H

    2001-08-01

    A method for the determination of the dopant concentration of tellurium in dissolved indium antimonide semiconductor material by electrothermal atomic absorption spectrometry (ETAAS) was developed. Efforts were made to investigate the optimal conditions of the furnace heating program and the effect of palladium modifier on the variation of tellurium and the background absorbance. According to the results obtained, the presence of palladium chemical modifier in the analysis of indium antimonide allowed the successful retention of tellurium in the graphite tube, and the optimum mass of palladium modifier was found to be dependent on the sample matrix concentration. The absorbance profile of tellurium and the background level were significantly improved when a pyrolysis temperature of 1100 degrees C and an atomization temperature of 2200 degrees C were employed in the optimized heating program. With the use of this method, a detection limit of 0.8 microg g(-1) tellurium in indium antimonide could be achieved. The applicability of the proposed method was evaluated by comparison with two independent methods, i.e. slurry sampling-ETAAS and ICP-MS. From the good agreement between the results, it was demonstrated that the proposed method is suitable for the determination of typical dopant concentrations of tellurium in indium antimonide. PMID:11534624

  17. Test of the Pauli exclusion principle for nucleons and atomic electrons by accelerator mass spectrometry

    International Nuclear Information System (INIS)

    The Pauli exclusion principle was tested by searching with accelerator mass spectrometry for non-Paulian atoms with three electrons in the K-shell and for non-Paulian nuclei with three protons or three neutrons in the nuclear 1 s1/2 shell. For non-Paulian atoms of 20Ne and 36Ar the following limits have been obtained: N(20Ne)/N(20Ne)-21 and N(36Ar)/N(36Ar)-17. For non-Paulian nuclei of 5Li and 5He with three protons or three neutrons, respectively, in the nuclear 1 s1/2 shell the following limits have been measured: N(5Li)/N(6Li)-17 for a range of proton separation energies of 5Li between 0 and 50 MeV and N(5He)/N(4He)-15 for neutron separation energies between 0 and 32 MeV. The result for 5Li is used to deduce a limit for the probability β2/2 of finding two colliding protons in the symmetric state with respect to exchange to be β2/2-32. (orig.)

  18. 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.

  19. Determination of lead in dolomite by Zeeman electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The mineral lorandite (TlAsS2), present in the Alshar deposit (Republic of Macedonia), is a possible solar neutrino detector (Freedman et al., 1976). As a result of nuclear reaction between the isotopes of thallium 205Tl and the solar neutrino, 205 Pb is produced. The aim of the idea is to determine the content of Pb in the lorandite, that could give information for the value of solar neutrino flux over extended time (Pavicevic, 1994). A method for the lead determination in dolomite by Zeeman electrothermal atomic absorption spectrometry, is presented. After the dissolution of samples, lead was extracted with sodium diethyldithio-carbamate. The lead-diethyldithiocarbamate complex was extracted into methylisobutyl ketone from a medium of pH 6.0-10.0. The procedure was verified by method of standard additions and by analyzing referent standard samples. A calibration curve (for organic solutions containing up to 1 ng Pb) was made using the proposed extraction procedure for standard solutions of lead. The standard deviation (SD) for 0.5 ng Pb is 0.01 ng and the relative standard deviation ranges from 2.5 to 3.5%. The detection limit of the method, calculated as 3 SD of the blank, was found to be 1.5 ng.g-1. The operation conditions in electrothermal atomic absorption measurements (temperature and time) were: drying - 90oC, 20 s; charring - 400oC, 20 s; atomizing - 1900oC, 3 s; cleaning - 2650oC, 3 s (Author)

  20. 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.

  1. Emerging Techniques in Vegetable Oil Analysis Using Stable Isotope Ratio Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kelly, S. D.; Rhodes, C.

    2002-07-01

    As the practice of vegetable oil adulteration becomes more sophisticated, the possibility to subvert detection using established techniques such as capillary gas chromatography is increasing. One of the most powerful techniques to be used in food authenticity studies is stable isotope ratio mass spectrometry (SIRMS) which utilises differences in the natural abundance of the stable isotopes of the light bio elements hydrogen, nitrogen, carbon, oxygen and sulfur to detect food fraud. SIRMS has found application in the authentication of a wide range of foodstuffs, including fruit juices, wines, spirits, honey and to detect the adulteration of flavour compounds with synthetic analogues. This papers reviews the current state-of-the-art for the authentication of vegetable oils using SIRMS and highlights emergent techniques such as compound-an position specific-isotope mass spectrometry. These latter developments offer the potential to provide more rapid and improved detection of the economic adulteration of vegetable oils. (Author) 38 refs.

  2. 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.

  3. 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.

  4. Scattering of low-energy electrons by excited sodium atoms using a photon and electron atomic beam recoil technique

    International Nuclear Information System (INIS)

    A new method for measuring cross sections for the scattering of electrons by laser-excited atoms is described. It is a generalization of the atomic-beam recoil technique, taking advantage of the recoil of atoms during resonant photon interactions to spatially separate excited from nonexcited atoms. A preliminary value for the total cross section for the scattering of electrons by the 32P3/2(m/sub F/=3) state of sodium at 4.4 eV is presented

  5. Wall loss of atomic nitrogen determined by ionization threshold mass spectrometry

    International Nuclear Information System (INIS)

    In the afterglow of an inductively coupled N2 plasma, relative N atom densities are measured by ionization threshold mass spectrometry as a function of time in order to determine the wall loss time twN from the exponential decay curves. The procedure is performed with two mass spectrometers on different positions in the plasma chamber. twN is determined for various pressures, i.e., for 3.0, 5.0, 7.5, and 10 Pa. For this conditions also the internal plasma parameters electron density ne and electron temperature Te are determined with the Langmuir probe and the rotational temperature TrotN2 of N2 is determined with the optical emission spectroscopy. For TrotN2, a procedure is presented to evaluate the spectrum of the transition υ′=0→υ″=2 of the second positive system (C3Πu→B3Πg) of N2. With this method, a gas temperature of 610 K is determined. For both mass spectrometers, an increase of the wall loss times of atomic nitrogen with increasing pressure is observed. The wall loss time measured with the first mass spectrometer in the radial center of the cylindrical plasma vessel increases linearly from 0.31 ms for 3 Pa to 0.82 ms for 10 Pa. The wall loss time measured with the second mass spectrometer (further away from the discharge) is about 4 times higher. A model is applied to describe the measured twN. The main loss mechanism of atomic nitrogen for the considered pressure is diffusion to the wall. The surface loss probability βN of atomic nitrogen on stainless steel was derived from twN and is found to be 1 for the present conditions. The difference in wall loss times measured with the mass spectrometers on different positions in the plasma chamber is attributed to the different diffusion lengths

  6. 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.

  7. 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.

  8. 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

  9. 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

  10. Direct analysis of silica by means of solid sampling graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    This paper reports on the use of solid sampling-graphite furnace atomic absorption spectrometry for the direct analysis of synthetic amorphous silica. In particular, determination of hazardous elements such As, Cd, Cr, Cu, Pb and Sb is investigated, as required by regulations of the food industry. The conclusion of the work is that, after proper optimization of the working conditions, paying particular attention to the atomization temperature and the use of proper modifiers (graphite powder, HNO3 or Pd), it is possible to develop suitable procedures that rely on the use of aqueous standard solutions to construct the calibration curves for all the elements investigated. The proposed method shows important benefits for the cost-effective analysis of such difficult samples in routine labs, permitting fast screening of those elements that are very rarely present in this type of sample, but also accurate quantification of those often found, while offering low limits of detection (always below 0.1 mg g−1) that comply well with legal requirements, and precision levels that are fit for the purpose (approx. 6–9% R.S.D.). - Highlights: ► Solid sampling GFAAS is investigated for the direct analysis of silica samples; ► a fast and simple methodology with aqueous standards for calibration is proposed; ► this method permits accurate determination of As, Cd, Cr, Cu, Pb and Sb in the samples of interest; ► LODs below 100 ng g−1 and precision values in the 6–10% RSD range are achieved.

  11. Inductively coupled plasma atomic spectrometry (ICP-AES) and associated tecgniques

    International Nuclear Information System (INIS)

    Plasma emission spectroscopy is now an established technique for the analysis and quality control of modern inorganic and polymeric materials. The detection limit of < mu g iota /sup -1/ achieved by ICP-MS and atomic fluorescence methods with multielement capability has led to the explosive growth of trends and methodologies in thousands of published articles. The major development has been in the evolution of powerful computer controlled instruments with advanced optics and highly sophisticated detection and data processing systems. The high resolution spectrometers developed by several companies have reduced the inter element and molecular interference relieving the analyst of tedious and time-consuming routines of matrix matching and spectral corrections. The cost of analysis per sample has been drastically reduced due to rapid and reliable results in a short time. However the costs of such systems remains high and require very clean environment for the installation and operation of modern high resolution instruments. Major applications of atomic spectrometric methods are in semiconductor and high purity industrial materials where the purchase of such expensive units can be justified. Applications in pharmaceutical, chemical and material sciences are also on the increase. Assessment of natural resources and environmental and toxic element studies are also justifying the social services provided by modern instrumental techniques. The trend of inter comparison is also growing due to the availability of large number of instruments / techniques. (author)

  12. 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)

  13. 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)

  14. 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.

  15. Determination of nickel in active pharmaceutical ingredients by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Bubnič, Zoran; Urleb, Uroš; Kreft, Katjuša; Veber, Marjan

    2010-03-01

    An electrothermal atomic absorption spectrometric procedure for the determination of nickel in active pharmaceutical ingredients was developed. Since the recoveries of nickel by the direct dissolution of samples in diluted nitric acid were low and caused errors in the determination of Ni in pharmaceutical samples, different approaches for sample pre-treatment were examined. It was found that the microwave digestion was the most suitable way for sample preparation. Various combinations of digestion agents and different microwave conditions were tested. The combination of nitric acid and hydrogen peroxide was found to be the most appropriate. The validity of the method was evaluated by recovery studies of spiked samples and by the comparison of the results obtained by inductively coupled plasma mass spectrometry (ICP-MS). The recovery ranged from 87.5 to 104.0% and a good agreement was achieved between both methods. The detection limit and the limit of quantification were 0.6 and 2.1 µg g-1 respectively. The precision of the method was confirmed by the determination of Ni in the spiked samples and was below 4%, expressed in terms of a relative standard deviation. The method was applied to the determination of nickel in production samples of active pharmaceutical ingredients and intermediates. PMID:24061653

  16. 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.)

  17. Determination of cadmium in real water samples by flame atomic absorption spectrometry after cloud point extraction

    International Nuclear Information System (INIS)

    Water pollution is a global threat and it is the leading world wide cause of death and diseases. The awareness of the potential danger posed by heavy metals to the ecosystems and in particular to human health has grown tremendously in the past decades. Separation and preconcentration procedures are considered of great importance in analytical and environmental chemistry. Cloud point is one of the most reliable and sophisticated separation methods for determination of traces quantities of heavy metals. Cloud point methodology was successfully employed for preconcentration of trace quantities of cadmium prior to their determination by flame atomic absorption spectrometry (FAAS). The metals react with 8-hydroxquinoline in a surfactant Triton X-114 medium. The following parameters such as pH, concentration of the reagent and Triton X-114, equilibrating temperature and centrifuging time were evaluated and optimized to enhance the sensitivity and extraction efficiency of the proposed method. Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation and the cadmium content was measured by FAAS. The validation of the procedure was carried out by spiking addition methods. The method was applied for determination of Cd in water samples of different ecosystems (lake and river). (author)

  18. 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.

  19. 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. PMID:22497165

  20. 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.

  1. 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.

  2. 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%.

  3. 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.

  4. 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)

  5. 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.

  6. Determination of mercury by intermittent flow electrochemical cold vapor generation coupled to atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    A novel method for determination of mercury was developed using an intermittent flow electrochemical cold vapor generation coupled to atomic fluorescence spectrometry (IF-ECVG-AFS). The mercury vapor was generated on the surface of glassy carbon cathode in the flow cell. The operating conditions for the electrochemical generation of mercury vapor were investigated in detail, and the interferences from various ions were evaluated. Under the optimized conditions, no evident memory effects of mercury were observed. The calibration curve was linear up to 5 μg L-1 Hg at 0.54 A cm-2. A detection limit of 1.2 ng L-1 Hg and a relative standard deviation of 1.8% for 1 μg L-1 Hg were obtained. The accuracy of method was verified by the determination of mercury in the certified reference human hair. The ECVG avoided the use of reductants, thereby greatly reducing the contamination sources. In addition, the manifold of IF-ECVG-AFS was simple and amenable to automation

  7. 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.

  8. Analysis of the release characteristics of cu-treated antimicrobial implant surfaces using atomic absorption spectrometry.

    Science.gov (United States)

    Zietz, Carmen; Fritsche, Andreas; Finke, Birgit; Stranak, Vitezslav; Haenle, Maximilian; Hippler, Rainer; Mittelmeier, Wolfram; Bader, Rainer

    2012-01-01

    New developments of antimicrobial implant surfaces doped with copper (Cu) ions may minimize the risk of implant-associated infections. However, experimental evaluation of the Cu release is influenced by various test parameters. The aim of our study was to evaluate the Cu release characteristics in vitro according to the storage fluid and surface roughness. Plasma immersion ion implantation of Cu (Cu-PIII) and pulsed magnetron sputtering process of a titanium copper film (Ti-Cu) were applied to titanium alloy (Ti6Al4V) samples with different surface finishing of the implant material (polished, hydroxyapatite and corundum blasted). The samples were submersed into either double-distilled water, human serum, or cell culture medium. Subsequently, the Cu concentration in the supernatant was measured using atomic absorption spectrometry. The test fluid as well as the surface roughness can alter the Cu release significantly, whereby the highest Cu release was determined for samples with corundum-blasted surfaces stored in cell medium. PMID:22162672

  9. 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)

  10. Unravelling associations between unassigned mass spectrometry peaks with frequent itemset mining techniques

    OpenAIRE

    Trung Nghia, Vu; Mrzic, Aida; Valkenborg, Dirk; Maes, Evelyne; Lemiere, Filip; Goethals, Bart; Laukens, Kris

    2014-01-01

    Background Mass spectrometry-based proteomics experiments generate spectra that are rich in information. Often only a fraction of this information is used for peptide/protein identification, whereas a significant proportion of the peaks in a spectrum remain unexplained. In this paper we explore how a specific class of data mining techniques termed “frequent itemset mining” can be employed to discover patterns in the unassigned data, and how such patterns can help us interpret the origin of th...

  11. Collisions of metastable Ne*, He* atoms with ground-state He, Ne atoms studied by atomic beam and laser techniques

    International Nuclear Information System (INIS)

    A crossed nozzle-beam experiment is used to investigate thermal energy collisions: Ne* (2p53s, 3P0,2) + He(1s2, 1S0), almost purely elastic, and He*(1s2s, 1,3S + Ne(2p6, 1S0), in which inelastic excitation transfers occur. State and velocity selection of the scattered Ne* atoms is performed using a tunable cw dye laser frequency locked on a definite Zeeman component of the transition 1s5 → 2p6 (λ = 614.3 nm) of 20Ne or 22Ne. In the purely elastic case, this technique allows the selection of one of the two final velocities, and then an unambiguous transformation of the differential cross section at 62 meV tallies on accords with a calculation using a single effective potential. In He* on Ne collisions, the main inelastic processes are endothermic excitation transfers from He*(21S). Experimental results obtained at different energies (62, 95, 109, 124 meV) show that the transfers essentially result in levels 3s and 4d of Ne. (orig.)

  12. Determination of cadmium, cobalt, manganese, copper, nickel, and chromium in concentrated solutions of calcium chloride by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A procedure is developed for the direct determination of Cd, Co, Cr, Cu, Mn, and Ni in concentrated solutions of calcium chloride by electrothermal atomic absorption spectrometry. Ascorbic and oxalic acids and magnesium nitrate were examined as chemical modifiers. Oxalic acid was found to be the best modifier. Although an atomic absorption spectrometer with a background correction system of relatively low efficiency (deuterium lamp) was used, elements under study can be reliably determined in the presence of oxalic acid at concentrations of calcium chloride in the solution up to 6%. Because cadmium is evaporated before the major part of the given matrix, it can be determined without modifier

  13. 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.

  14. 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.

  15. Gas phase studies on terpenes by ion mobility spectrometry using different atmospheric pressure chemical ionization techniques

    Science.gov (United States)

    Borsdorf, H.; Stone, J. A.; Eiceman, G. A.

    2005-11-01

    The ionization pathways and drift behavior were determined for sets of constitutional isomeric and stereoisomeric non-polar hydrocarbons (unsaturated monocyclic terpenes, unsaturated and saturated bicyclic terpenes) using ion mobility spectrometry (IMS) with different techniques of atmospheric pressure chemical ionization (APCI) to assess how structural and stereochemical differences influence ion formation. Depending on the structural features, different ions were observed for constitutional isomers using ion mobility spectrometry with photoionization (PI) and corona discharge (CD) ionization. Photoionization provides ion mobility spectra containing one major peak for saturated compounds while at two peaks were observed for unsaturated compounds, which can be assigned to product ions related to monomer and dimer ions. However, differences in relative abundance of product ions were found depending on the position of the double bond. Although IMS using corona discharge ionization permits the most sensitive detection of non-polar hydrocarbons, the spectra are complex and differ from those obtained using photoionization. Additional cluster ions and fragment ions were detected. Only small differences in ion mobility spectra were observed for the diastereomers while the enantiomers provide identical spectra. The structure of the product ions formed was checked by investigations using the coupling of ion mobility spectrometry with mass spectrometry (IMS-MS).

  16. Speciation analysis of arsenic by hydride generation-cryotrapping-atomic fluorescence spectrometry: achieving extremely low detection limits with inexpensive instrumentation

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Matoušek, Tomáš; Svoboda, Milan; Selecká, Anna; Rychlovský, P.; Dědina, Jiří

    Buzios, Rio de Janeiro, 2011. TH43. ISBN 978-85-8006-046-1. [Colloquium Spectroscopicum Internationale /37./. 28.08.2011-02.09.2011, Buzios, Rio de Janeiro] R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : arsenic speciation analysis * hydride generation * atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation

  17. Speciation analysis of arsenic by hydride generation-cryotrapping-atomic fluorescence spectrometry: achieving extremely low detection limits with inexpensive instrumentation

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Matoušek, Tomáš; Svoboda, Milan; Selecká, Anna; Rychlovský, P.; Dědina, Jiří

    Münster, 2011. FTM 17. [International Symposium on Metallomics /3./. 15.06.2011-18.06.2011, Münster] R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : arsenic speciation analysis * hydride generation * atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation http://www.metallomics2011.org/event/Metallomics2011/Scientific_program.html

  18. Arsenic speciation analysis by cryogenic trapping – hydride generation – atomic absorption spectrometry; Investigation of water vapour dryers

    Czech Academy of Sciences Publication Activity Database

    Svoboda, Milan; Taurková, Petra; Matoušek, Tomáš; Rychlovský, P.; Dědina, Jiří

    Prague: Charles University in Prague, Faculty of Science, 2010 - (Nesměrák, K.), s. 15-18. (1). ISBN 978-80-7444-005-2. [International Students Conference "Modern Analytical Chemistry" /6./. Praha (CZ), 23.09.2010-24.09.2010] R&D Projects: GA ČR GA203/09/1783 Institutional research plan: CEZ:AV0Z40310501 Keywords : arsenic speciation * cryogenic trapping * atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation

  19. Determination of trace amounts of selenium in minerals and rocks by flame less atomic-absorption spectrometry

    International Nuclear Information System (INIS)

    The determination of trace amounts of selenium In silicate rocks and feldspar by solvent extraction and graphite furnace atomic-absorption spectrometry has been stu- died. Sodium diethyl-ditio carbamate and ammonium pyrrolidine dithiocarbamate have been tried as chelating agents. The best results are achieved when selenium is extracted Into carbon tetrachloride as the sodium diethyldithiocarbamate complex. The method allows to detect 0,75 ppm of selenium in the sample. Recoveries are about 100%. (Author) 7 refs

  20. Determination of calcium, copper, chromium, iron, magnesium, manganese, potassium, sodium and zinc in ethanol by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The direct determinacao of calcium, copper, chomium, iron, magnesium, manganese, potassium, sodium and zinc in ethanol by atomic absorption spectrometry with, air-acetylene flame is proposed. Effects of fuel/oxidant ratio, burner height and water content in the samples were investigated in detail. The method allows the determition of the elements with good precision (r.s.d. -1 for the elements tested. (author)

  1. 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)

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

    OpenAIRE

    Teslima Daşbaşı; Şenol Kartal; Şerife Saçmacı; Ahmet Ülgen

    2016-01-01

    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 ...

  3. Trace elements analysis by PIXE (particle induced x-ray excitation) and AAS (atomic absorption spectrometry) from environmental samples

    International Nuclear Information System (INIS)

    The aim of this work is the micro elemental analysis of environmental samples by PIXE (Particle Induced X-ray Excitation) method and AAS (Atomic Absrobtion Spectrometry). The samples were collected from neighborhood of Targoviste city (mulberry, apple, poplar, walnut, prune, maple). The concentration data have been obtain for the elements: S, Cl, K, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Br, Sr by PIXE method and Mn, Fe, Cu, Cr, Se, Zn by AAS method. A good correlation b

  4. 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...

  5. 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...

  6. 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)

  7. 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...

  8. Survey on result promotion of the atomic force technique

    International Nuclear Information System (INIS)

    By change of environment around research and development of atomic force, investigation has been recently executed not only on a theme directing a specific aim, but also on technical development considering some applications to the other field reflected by social needs. Therefore, an effective procedure and program capable of reflecting and promoting results of the atomic fore development to other industrial field were necessary. In this study, methods of evaluation and industrialization on study results of the atomic force were investigated. As a result, in order to promote the study results to other field, it was found to be important that some free reasons and concept engineering to mediate between developing and applying sides were to be present. In addition, it was suggested by some searches that a new atomic industry has a probability to be created by using potential energies such as heat, radiation, pulse, and so on. In this paper, evaluation on industrialization of the atomic force technical resources, and establishment of the industrialization program were described. (G.K.)

  9. Gamma-ray Spectrometry in Geothermal Exploration: State of the Art Techniques

    Directory of Open Access Journals (Sweden)

    Alistair T. McCay

    2014-07-01

    Full Text Available Gamma-ray spectrometry is a surveying technique that allows the calculation of the heat produced during radioactive decay of potassium, uranium, and thorium within rock. Radiogenic heat producing rocks are often targets for geothermal exploration and production. Hence, refinements in gamma-ray spectrometry surveying will allow better constraint of resources estimation and help to target drilling. Gamma-rays have long half-lengths compared to other radiation produced during radiogenic decay. This property allows the gamma-rays to penetrate far enough through media to be detected by airborne or ground based surveying. A recent example of ground-based surveying in Scotland shows the ability of gamma-ray spectrometry to quickly and efficiently categorize granite plutons as low or high heat producing. Some sedimentary rocks (e.g., black shales also have high radiogenic heat production properties and could be future geothermal targets. Topographical, atmospheric and spatial distribution factors (among others can complicate the collection of accurate gamma-ray data in the field. Quantifying and dealing with such inaccuracies represents an area for further improvement of these techniques for geothermal applications.

  10. Review of in situ derivatization techniques for enhanced bioanalysis using liquid chromatography with mass spectrometry.

    Science.gov (United States)

    Baghdady, Yehia Z; Schug, Kevin A

    2016-01-01

    Accurate and specific analysis of target molecules in complex biological matrices remains a significant challenge, especially when ultra-trace detection limits are required. Liquid chromatography with mass spectrometry is often the method of choice for bioanalysis. Conventional sample preparation and clean-up methods prior to the analysis of biological fluids such as liquid-liquid extraction, solid-phase extraction, or protein precipitation are time-consuming, tedious, and can negatively affect target recovery and detection sensitivity. An alternative or complementary strategy is the use of an off-line or on-line in situ derivatization technique. In situ derivatization can be incorporated to directly derivatize target analytes in their native biological matrices, without any prior sample clean-up methods, to substitute or even enhance the extraction and preconcentration efficiency of these traditional sample preparation methods. Designed appropriately, it can reduce the number of sample preparation steps necessary prior to analysis. Moreover, in situ derivatization can be used to enhance the performance of the developed liquid chromatography with mass spectrometry-based bioanalysis methods regarding stability, chromatographic separation, selectivity, and ionization efficiency. This review presents an overview of the commonly used in situ derivatization techniques coupled to liquid chromatography with mass spectrometry-based bioanalysis to guide and to stimulate future research. PMID:26496130

  11. 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

  12. 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

  13. 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.

  14. 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

  15. Techniques to measure quantum criticality in cold atoms

    International Nuclear Information System (INIS)

    We describe how rescaling experimental data obtained from cold atom density profiles can reveal signatures of quantum criticality. We identify a number of important questions which can be answered by analyzing experimental data in this manner. We show that such experiments can distinguish different universality classes and that the signatures are robust against temperature, noise, and finite system size.

  16. Graphene for Preconcentration of Trace Amounts of Ni in Water and Paraffin-Embedded Tissues from Liver Loggerhead Turtles Specimens Prior to flame Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    Hanie Arbabi Rashid

    2014-03-01

    Full Text Available A new sensitive and simple method was developed for the preconcentration of trace amounts of Ni using 1-(2-pyridylazo-2-naphthol (PAN as chelating reagent prior to its determination by flame atomic absorption spectrometry. The proposed method is based on the uti- lization of a column packed with graphene as sorbent. Several 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 5.0–240.0 µg L-1 with a detection limit of 0.36 µg L-1. The relative standard deviation for ten replicate measurements of 20.0 and 100.0 µg L-1 of Ni were 3.45 and 3.18%, 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 Ni. In the present study, we report the application of preconcentration techniques still continues increasingly for trace metal determinations by flame atomic absorption spectrometry (FAAS for quantification of Ni in Formalin-fixed paraffin-embedded (FFPE tissues from Liver loggerhead turtles. The proposed method was successfully applied in the analysis of four real environmental water samples. Good spiked recoveries over the range of 95.8–102.6% were obtained.

  17. Flow injection-chemical vapor generation atomic fluorescence spectrometry hyphenated system for organic mercury determination: A step forward

    Energy Technology Data Exchange (ETDEWEB)

    Angeli, Valeria [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Biagi, Simona [National Research Council of Italy, C.N.R., Istituto per i Processi Chimico-Fisici - IPCF-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Ghimenti, Silvia [University of Pisa, Department of Chemistry and Industrial Chemistry, Via Risorgimento 35, 56126 Pisa (Italy); Onor, Massimo; D' Ulivo, Alessandro [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Bramanti, Emilia, E-mail: bramanti@pi.iccom.cnr.it [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy)

    2011-11-15

    Monomethylmercury and ethylmercury were determined on line using flow injection-chemical vapor generation atomic fluorescence spectrometry without neither requiring a pre-treatment with chemical oxidants, nor UV/MW additional post column interface, nor organic solvents, nor complexing agents, such as cysteine. Inorganic mercury, monomethylmercury and ethylmercury were detected by atomic fluorescence spectrometry in an Ar/H{sub 2} miniaturized flame after sodium borohydride reduction to Hg{sup 0}, monomethylmercury hydride and ethylmercury hydride, respectively. The effect of mercury complexing agent such as cysteine, ethylendiaminotetracetic acid and HCl with respect to water and Ar/H{sub 2} microflame was investigated. The behavior of inorganic mercury, monomethylmercury and ethylmercury and their cysteine-complexes was also studied by continuous flow-chemical vapor generation atomic fluorescence spectrometry in order to characterize the reduction reaction with tetrahydroborate. When complexed with cysteine, inorganic mercury, monomethylmercury and ethylmercury cannot be separately quantified varying tetrahydroborate concentration due to a lack of selectivity, and their speciation requires a pre-separation stage (e.g. a chromatographic separation). If not complexed with cysteine, monomethylmercury and ethylmercury cannot be separated, as well, but their sum can be quantified separately with respect to inorganic mercury choosing a suitable concentration of tetrahydroborate (e.g. 10{sup -5} mol L{sup -1}), thus allowing the organic/inorganic mercury speciation. The detection limits of the flow injection-chemical vapor generation atomic fluorescence spectrometry method were about 45 nmol L{sup -1} (as mercury) for all the species considered, a relative standard deviation ranging between 1.8 and 2.9% and a linear dynamic range between 0.1 and 5 {mu}mol L{sup -1} were obtained. Recoveries of monomethylmercury and ethylmercury with respect to inorganic mercury were

  18. Comparison of inductively coupled plasma mass spectrometry with inductively coupled plasma atomic emission spectrometry and instrumental neutron activation analysis for the determination of rare earth elements in Greek bauxites

    International Nuclear Information System (INIS)

    Fore the determination of rare earth elements (REE) in bauxitic materials the techniques of inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and instrumental neutron activation analysis (INAA) were compared. In the NIST (National Institute of Standards and Technology) bauxites SRM 697 Dominican, and SRM 69 b Arkansas, the concentration of some REEs were determined. With the reference bauxite BX-N of the ARNT (Association Nationale de la Recherche Technique) the precision and accuracy of ICP-AES for the determination of REEs in bauxites was tested. Furthermore, Greek bauxites of the Parnassos-Giona area were investigated. In a comparison of the three methods it was possible to calculate from the data series the precision of each method, which showed that the tendency found in the deviations for the different REEs is in accordance with published values. Also the limits of detection for REEs in bauxites were calculated and found to be in the same range as those in the literature. (author)

  19. 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.

  20. 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

  1. Species selective preconcentration and quantification of gold nanoparticles using cloud point extraction and electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Highlights: ► We optimized cloud point extraction and ET-AAS parameters for Au-NPs measurement. ► A selective ligand (sodium thiosulphate) is introduced for species separation. ► A limit of detection of 5 ng Au-NP per L is achieved for aqueous samples. ► Measurement of samples with high natural organic mater content is possible. ► 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−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−1. The precision of the method expressed as the standard deviation of 12 replicates at an Au-NP concentration of 100 ng L−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.

  2. Sensitivity enhancement of beryllium determination in graphite furnace-atomic absorption spectrometry by use of atomization under pressure

    International Nuclear Information System (INIS)

    Using pressurized atomization both peak height and area sensitivity of beryllium is considerably improved. The enhancement may probably be explained by the fact that the Lorentz broadening and shift is more than compensated for by the lower diffusion rate of atoms with increasing pressures. The alteration of peak shapes and parameters should result in a diminishment of vapor phase interferences with increasing pressure. The relative time resolution of the detection system also improves with increasing pressures, with a consequent improvement of precision and accuracy. In the absorbance domain calibration curves are more linear with pressurized atomization than at atmospheric pressure. (Author)

  3. A technique of enhanced sensitivity and overcome radioactive contamination in thermal ionization mass spectrometry

    International Nuclear Information System (INIS)

    In order to overcome the radioactive contamination and enhance the sensitivity of thermal ionization mass spectrometry, some quantities of uranium of plutonium are electroplated on the single rhenium filament, then a thin layer of platinum is overlaid on the filament. The sample atoms thermally diffuse through a platinum layer before they can evaporate as neutral atoms or as ions. Since thermal diffusion is generally a much slower process than direct evaporation and a platinum layer limits the prompt escape of neutral atoms, the filament can be operated at higher temperature, yielding higher ionization efficiency without rapid loss of the sample. The samples of uranium and plutonium are prepared for electrode position by adding 1.0 mol·L-1 HCl to dilute the uranium and plutonium concentrations to 0.1 g/L and 0.01 g/L, respectively. Three kinds of sample plating solutions are the mixtures of the ammonium chloride and chlorhydric acid; the ammonium chloride, chlorhydric acid and oxalic acid; the nitric acid, ammonia and oxalic acid, respectively. Two kinds of platinum solutions in the electrolyte are the chloroplatinic acid, chlorhydric acid and oxalic acid; the platinic sodium hydroxide, sodium hydroxide and oxalic acid, respectively. The ion currents observed for the 100 ng uranium or 50 ng plutonium are 2 x 10-14 A during 40∼60 min

  4. Development of High Resolution Resonance Ionization Mass Spectrometry for Neutron Dosimetry Technique with93Nb(n,n')93mNb Reaction

    Science.gov (United States)

    Tomita, Hideki; Takatsuka, Takaaki; Takamatsu, Takahide; Adachi, Yoshitaka; Furuta, Yujin; Noto, Takuma; Iguchi, Tetsuo; Sonnenschein, Volker; Wendt, Klaus; Ito, Chikara; Maeda, Shigetaka

    2016-02-01

    We have proposed an advanced technique to measure the 93mNb yield precisely by Resonance Ionization Mass Spectrometry, instead of conventional characteristic X-ray spectroscopy. 93mNb-selective resonance ionization is achievable by distinguishing the hyperfine splitting of the atomic energy levels between 93Nb and 93mNb at high resolution. In advance of 93mNb detection, we could successfully demonstrate high resolution resonant ionization spectroscopy of stable 93Nb using an all solid-state, narrow-band and tunable Ti:Sapphire laser system operated at 1 kHz repetition rate.

  5. 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

    Energy Technology Data Exchange (ETDEWEB)

    Pedersen, G.A. [National Food Agency of Denmark, Institute of Food Chemistry and Nutrition, Moerkhoej Bygade 19, DK-2860 Soeborg (Denmark); Larsen, E.H. [National Food Agency of Denmark, Institute of Food Chemistry and Nutrition, Moerkhoej Bygade 19, DK-2860 Soeborg (Denmark)

    1997-07-01

    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{sup -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 spectrometry (ICP-MS). The signal-to-noise ratio of the FAAS detector was optimized using a hydrogen-argon entrained-air flame and a slotted-tube atom trap (STAT) in the flame. The limit of detection (3 {sigma}) achieved by the HPLC-FAAS system was 1 mg L{sup -1} of selenium (100 {mu}L injections) for each of the four selenium species. More powerful selenium detection was achieved using an ELAN 5000 ICP-MS instrument. Selenium was measured at m/z = 82. The ICP-MS signal intensity was enhanced by a factor of 3-4 after addition of 3% methanol to the chromatographic mobile phase and by using an increased plasma power input of 1300 W. The limit of detection achieved under these conditions was 1 {mu}g L{sup -1} (100 {mu}L injections). The HPLC-ICP-MS system was used for selenium speciation of selenite and selenate in aqueous solutions during a BCR certification exercise and for selenium speciation in the certified reference material, BCR No. 402 White Clover. Extraction experiments revealed that the selenium species in the biological material were extractable only in the presence of water in the extraction medium. The results indicated that selenate and a compound of unknown identity U were present in the plant sample. (orig.). With 5 figs., 5 tabs.

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

    International Nuclear Information System (INIS)

    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

  7. ULSI technology and materials: Quantitative answers by combined mass spectrometry surface techniques

    International Nuclear Information System (INIS)

    The progressive microelectronics ULSI device shrinking towards improving the performances has driven the development of new materials and process technologies. A good example is given by oxynitride, an innovative material which is thought for the next generation of 0.25 μm MOS circuits. Oxynitrides have replaced thermal silicon oxides as gate insulator due to the properties of good masking against impurity diffusion, together with the excellent dielectric strength and the better resistance to dielectric breakdown. The strong request from microelectronics industries for a complete and accurate characterization of this new material and the technological processes concerned, has considerably stimulated the research, particularly in the field of analytical methodology. Secondary Ion Mass Spectrometry, linked since the beginning with microelectronics development, shows again to be the most reliable and suitable microanalytical technique to give answers to this topics. In this work we present some examples of methodologies applied to an accurate quantitative characterization of this new material, together with its impact on the production processes. We show how the complementary employing of several mass spectrometry techniques, such as magnetic sector SIMS, SNMS and ToF-SIMS, can give a more complete overview both to process issues and to methodological developements of the techniques themselves

  8. ULSI technology and materials: Quantitative answers by combined mass spectrometry surface techniques

    Science.gov (United States)

    Bersani, M.; Fedrizzi, M.; Sbetti, M.; Anderle, M.

    1998-11-01

    The progressive microelectronics ULSI device shrinking towards improving the performances has driven the development of new materials and process technologies. A good example is given by oxynitride, an innovative material which is thought for the next generation of 0.25 μm MOS circuits. Oxynitrides have replaced thermal silicon oxides as gate insulator due to the properties of good masking against impurity diffusion, together with the excellent dielectric strength and the better resistance to dielectric breakdown. The strong request from microelectronics industries for a complete and accurate characterization of this new material and the technological processes concerned, has considerably stimulated the research, particularly in the field of analytical methodology. Secondary Ion Mass Spectrometry, linked since the beginning with microelectronics development, shows again to be the most reliable and suitable microanalytical technique to give answers to this topics. In this work we present some examples of methodologies applied to an accurate quantitative characterization of this new material, together with its impact on the production processes. We show how the complementary employing of several mass spectrometry techniques, such as magnetic sector SIMS, SNMS and ToF-SIMS, can give a more complete overview both to process issues and to methodological developements of the techniques themselves.

  9. EVALUATION OF CORROSION OF ENGINEERING CERAMICS BY ATOMIC EMISSION SPECTROMETRY IN INDUCTIVELY COUPLED PLASMA

    Directory of Open Access Journals (Sweden)

    DAGMAR GALUSKOVÁ

    2014-03-01

    Full Text Available An analytical method has been developed and verified, facilitating chemical analysis of saline aqueous solutions from corrosion tests of two types of engineering ceramics, i.e. polycrystalline alumina, and silicon nitride. The method is capable of providing complementary information related to mechanisms of corrosion and kinetics of dissolution of the two main components of the ceramics, i.e. Al in α-Al2O3, and Si in Si3N4. A radially viewed inductively coupled plasma atomic emission spectroscopy was used, and the operating conditions for the analysis were optimised. The method was validated. Internal standardisation, matrix matching, standard addition technique and direct measurement without matrix correction were applied, and the results were critically discussed. The technique of internal standard was shown to be the most sensitive. The method exhibited satisfactory precision (relative standard deviation up to 5 %, analytical recoveries from 95 to 100 %, and acceptable limits of detection based on 3σ criterion of 0.095 mg∙l-1 for Al (measured at 308.215 nm and 0.099 mg∙l-1 for Si (at 251.611 nm.

  10. Complementarity of nuclear spectrometry and multi-elements techniques for radio-toxicological analysis. Application to urine and faeces

    International Nuclear Information System (INIS)

    Complementarity of nuclear spectrometry and multi-element techniques for radio-toxicological analysis. Application to urine and faeces. The method routinely used to determine a possible contamination by actinides, alpha emitters, is the measurement of the fraction transferred to the excreta (urine and/or faeces). The first step of the procedure commonly used consists in a radiochemical specific separation of each element. In the second step an electroplated source is prepared to allow the measurement of its activity by alpha spectrometry. In order to simplify this procedure, the performance of the analysis of actinides by mass spectrometry is estimated based o two analytical tools, the ICP-MS and the SIMS. The use of the three techniquesspectrometry, ICP-MS, SIMS) is investigated based on recent results published in the literature or research work carried out in the laboratory. The results reported in this study allow to compare assess the advantages of each technique. (authors)

  11. Improved detection limit for 59Ni using the technique of accelerator mass spectrometry

    International Nuclear Information System (INIS)

    59 Ni is produced by neutron activation in the stainless steel close to the core of a nuclear reactor. To be able to classify the different parts of the reactor with respect to their content of long-lived radionuclides before final storage it is important to measure the 59 Ni level. Accelerator mass spectrometry is an ultra-sensitive method for counting atoms, suitable for 59 Ni measurements. Improvements in the reduction of the background and in the chemical reduction of cobalt, the interfering isobar, have been made. This chemical purification is essential when using small tandem accelerators, <3 MV, combined with the detection of characteristic projectile X-rays. These improvements have lowered the detection limit for 59 Ni by a factor of twenty compared with the first value reported for the Lund AMS facility. Material from the Swedish nuclear industry has been analysed and examples of the results are presented

  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. Rapid diagnosis of Zellweger syndrome and infantile Refsum's disease by fast atom bombardment-mass spectrometry of urine bile salts

    International Nuclear Information System (INIS)

    A method is described for the rapid determination of urinary bile salt profiles by fast atom bombardment-mass spectrometry (FAB-MS). Negative ion FAB spectra could be obtained from the equivalent of 10 μl of urine loaded onto the target probe with glycerol as matrix. In samples from infants and children with cholestasis the major peaks were produced by the taurine and glycine conjugates of di-, tri- and tetrahydroxycholanoic acids. In samples from patients with Zellweger syndrome and infantile Refsum's disease, a unique ion at m/z 572 indicated the presence of taurine-conjugated tetrahydroxycholestanoic acid(s). Capillary gas chromatography-mass spectrometry (GC-MS) of the bile acids liberated by alkaline hydrolysis indicated the presence of at least two nuclear-tetrahydroxylated cholestanoic acids, probably the 6α- and 1β-hydroxylated derivatives of 3α, 7α, 12α-trihydroxy-5β-cholestan-26-oic acid. (Auth.)

  14. Direct determination of selenium in rat blood plasma by Zeeman atomic absorption spectrometry.

    Science.gov (United States)

    Kabirov, K K; Kapetanovic, I M; Lyubimov, A V

    2008-01-30

    The method was developed to be applied for direct determination of selenium in rat plasma by graphite-furnace atomic absorption spectrometry with Zeeman background correction. Blood was obtained from CD rats of both sexes 2h after dosing in weeks 7 and 13 in order to acquire data on the levels of selenium in these animals during 13-week gavage administration of l-seleno-methylselenocysteine (SeMC), a new candidate chemopreventive agent under development. Application of the commonly used method of standard addition was found to be unsuitable to calculate the selenium content in rat plasma (within-run and between-run accuracy and precision parameters were less than 85%). Therefore, a new analytical method was developed. In this method, samples of rat plasma (50 microL) were diluted 10-fold with a reducing agent containing l-ascorbic acid, a modifier solution containing palladium chloride and Triton X-100. Samples were atomized in pyrolytically coated graphite tubes and peak height signals were measured. Selenium concentrations were determined by linear least squares regression analysis based on the standard curve generated in pooled rat blank plasma. Since selenium is normally present in plasma, a three-step approach was used to calculate selenium plasma levels. Initially selenium levels were determined based on the standard curve with selenium-spiked pool plasma. In the second step, background selenium levels in the pooled plasma were determined based on the same standard curve. In the third step, background level was added to the previously derived number. The relative errors were in the range from -4.6 to 11.4% (intra-day assay) and from -0.4 to 8.8% (inter-day assay) which proved good accuracy. The relative standard deviations were in the range from 1.88 to 4.70% (intra-day precision) and from 3.28 to 5.38% (inter-day precision). In rat plasma, the following dose-dependent selenium levels (mean+/-S.D.) in males and females, respectively, were observed at 13 weeks

  15. 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)

  16. Accelerating all-atom MD simulations of lipids using a modified virtual-sites technique

    DEFF Research Database (Denmark)

    Loubet, Bastien; Kopec, Wojciech; Khandelia, Himanshu

    2014-01-01

    We present two new implementations of the virtual sites technique which completely suppresses the degrees of freedom of the hydrogen atoms in a lipid bilayer allowing for an increased time step of 5 fs in all-atom simulations of the CHARMM36 force field. One of our approaches uses the derivation of...

  17. 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.

  18. Application of High Resolution-Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS): determination of trace elements in tea and tisanes.

    Science.gov (United States)

    Paz-Rodríguez, Beatriz; Domínguez-González, María Raquel; Aboal-Somoza, Manuel; Bermejo-Barrera, Pilar

    2015-03-01

    A new application of HR-CS FAAS (High Resolution-Continuum Source Flame Atomic Absorption Spectrometry) has been developed for the determination of several trace elements (Ca, Co, Cu, Fe, Mn, Ni, Na and Zn) in infusions made from tea, rooibos and tea with seaweed samples. The proposed methods are fast, inexpensive and show good performances: the mean analytical recovery was approximately 100%. The mean limit of detection was 29.4 μg/l, and the mean limit of quantification was 98.0 μg/l (both limits refer to the brewed samples). Due to the matrix effect observed, the standard addition method had to be applied. Preliminary classification (based on metal contents) using chemometric techniques such as PCA (Principal Component Analysis) and CA (Cluster Analysis), was successful for infusions made from rooibos and tea with seaweed, but inconclusive for black and green teas. PMID:25306375

  19. Comparison of a portable micro-X-ray fluorescence spectrometry with inductively coupled plasma atomic emission spectrometry for the ancient ceramics analysis

    International Nuclear Information System (INIS)

    Two multielement instrumental methods of analysis, micro X-ray fluorescence spectrometry (micro-XRF) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were applied for the analysis of 7th and 5th century B.C. ancient ceramic sherds in order to evaluate the above two methods and to assess the potential to use the current compact and portable micro-XRF instrument for the in situ analysis of ancient ceramics. The distinguishing factor of interest is that micro-XRF spectrometry offers the possibility of a nondestructive analysis, an aspect of primary importance in the compositional analysis of cultural objects. Micro-XRF measurements were performed firstly directly on the ceramic sherds with no special pretreatment apart from surface cleaning (micro-XRF on sherds) and secondly on pressed pellet disks which were prepared for each ceramic sherd (micro-XRF on pellet). For the ICP-AES determination of elements, test solutions were prepared by the application of a microwave-assisted decomposition procedure in closed high-pressure PFA vessels. Also, the standard reference material SARM 69 was used for the efficiency calibration of the micro-XRF instrument and was analysed by both methods. In order to verify the calibration, the standard reference materials NCS DC 73332 and SRM620 as well as the reference materials AWI-1 and PRI-1 were analysed by micro-XRF. Elemental concentrations determined by the three analytical procedures (ICP-AES, micro-XRF on sherds and micro-XRF on pellets) were statistically treated by correlation analysis and Student's t-test (at the 95% confidence level)

  20. In situ collection of volatile silver species in a new modular quartz tube atomizer for atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Kratzer, Jan; Vobecký, Miloslav; Matoušek, Tomáš

    2012-01-01

    Roč. 27, č. 9 (2012), s. 1382-1390. ISSN 0267-9477 R&D Projects: GA ČR GA203/09/1783 Institutional support: RVO:68081715 Keywords : volatile species generation * in-situ collection * quartz tube atomizer Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.155, year: 2012

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

    Czech Academy of Sciences Publication Activity Database

    Musil, Stanislav; Matoušek, Tomáš; Dědina, Jiří

    2015-01-01

    Roč. 108, JUN (2015), s. 61-67. ISSN 0584-8547 R&D Projects: GA ČR GA14-23532S Grant ostatní: GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : silver * volatile species generation * sapphire tube atomizer Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.176, year: 2014

  2. Element analysis and characteristic identification of non-fumigated and sulfur-fumigated Fritillaria thunbergii Miq. using microwave digestion-inductively coupled plasma atomic emission spectrometry combined with Fourier transform infrared spectrometry

    Directory of Open Access Journals (Sweden)

    Yajing Lou

    2014-01-01

    Full Text Available Background: Sulfur-fumigation may induce chemical transformation of traditional Chinese medicines leading to harmful effects following patient ingestion. For quality control, it is urgently needed to develop a reliable and efficient method for sulfur-fumigation identification. Materials and Methods: The spectrochemical identification of non-fumigated and sulfur-fumigated Fritillaria thunbergii Miq. was carried out to evaluate inorganic elements and organic components. The concentrations of 12 elements, including Zn, Mn, Cu, Fe, Li, Mg, Sr, Pb, As, Cd, Hg, and S of samples were determined by microwave digestion - inductively coupled plasma atomic emission spectrometry (ICP-AES. Meanwhile, Fourier transform infrared spectrometry (FTIR was used for the study of chemical group characteristic reactions after sulfur-fumigation. Results: The concentrations of Fe, Mg, Hg, and S elements showed significant differences between non-fumigated and sulfur-fumigated Fritillaria thunbergii Miq. The characteristic stretching vibrations of some groups in FTIR spectra, such as -OH, -S = O and -S-O, provided the identification basis for the discrimination of non-fumigated and sulfur-fumigated Fritillaria thunbergii Miq. Conclusion: The application of microwave digestion - ICP-AES was successfully used in combination with FTIR to authenticate and evaluate the quality of medicinal Fritillaria thunbergii Miq. Further applications of this technique should be explored.

  3. 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

  4. 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...

  5. Flow injection sorbent extraction of metals with activated carbon and its application to flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    In the present study activated carbon was used as a sorbent material for the flow injection on-line sorbent extraction of metal ions combined with atomic absorption spectrometry. On-line chelation of zinc was performed with 8-Hydroxyquinoline and the resultant metal chelate was adsorbed on the activated carbon, then adsorbed with zinc acid and on-line detected with flame AAS. Various parameters affecting the zinc enrichment were optimized and the method was applied for the determination of zinc in tap water, natural water, boiled and tea samples. The results obtained with the present method were compared with those obtained by the ICP-AES. (author)

  6. On atomization of europium and dysprosium in U-Pu matrix after chemical separation using GF-AAS technique

    International Nuclear Information System (INIS)

    Direct analysis of U-Pu bearing material by atomic emission spectrometry (AES) is not possible for determination of Eu and Dy at trace level, because of their rich emission line spectra, which can cause severe spectral interference. Atomic absorption spectrometry (AAS) is the alternate method for determination of these elements. Though the direct determination of Dy and Eu is possible by AAS, the atomization of these elements in U-Pu matrix is the result of analyte-matrix-carbon type of interactions. During the method development for Dy and Eu by AAS, absorbance signal was significantly suppressed in presence of U-Pu as compared to matrix free solution

  7. Investigation of ion-atom collision dynamics through imaging techniques

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    The principle and technique details of recoil ion momentum imaging are discussed and summarized. The recoil ion momentum spectroscopy built at the Institute of Modern Physics (Lanzhou) is presented. The first results obtained at the setup are analyzed. For 30 keV He2+ on He collision, it is found that the capture of single electron occurs dominantly into the first excited states, and the related scattering angle results show that the ground state capture occurs at large impact parameters, while the capture into excited states occurs at small impact parameters. The results manifest the collision dynamics for the sub-femto-second process can be studied through the techniques uniquely. Finally, the future possibilities of applications of the recoil ion momentum spectroscopy in other fields are outlined.

  8. Plutonium determination in urine by techniques of mass spectrometry; Determinacion de plutonio en orina por tecnicas de espectrometria de masas

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez M, H. [ININ, Departamento de Quimica, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico); Yllera de Ll, A., E-mail: hector.hernandez520@gmail.com [Centro de Investigaciones Energeticas, Medioambientales y Tecnologicas, Departamento de Medio Ambiente, Av. Complutense 22, 28040 Madrid (Spain)

    2013-10-15

    The objective of this study was to develop an analytic method for quantification and plutonium reappraisal in plane tables of alpha spectrometry be means of the mass spectrometry technique of high resolution with plasma source inductively coupled and desolvator Aridus (Aridus-Hr-Icp-Ms) and mass spectrometry with accelerator (AMS). The obtained results were, the recovery percentage of Pu in the plane table was of ∼ 90% and activity minimum detectable obtained with Aridus-Hr-Icp-Ms and AMS was of ∼ 3 and ∼ 0.4 f g of {sup 239}Pu, respectively. Conclusion, the results demonstrate the aptitude of the Aridus-Hr-Icp-Ms and AMS techniques in the Pu reappraisal in plane tables with bigger speed and precision, improving the values notably of the activity minimum detectable that can be obtained with the alpha spectrometry (∼ 50 f g of {sup 239}Pu). (author)

  9. Studies on atom deceleration process by using the Zeeman-tuned technique

    International Nuclear Information System (INIS)

    The Zeeman-tuned technique to slow an atomic beam of sodium atoms was detailed studied. A new technique to study the deceleration which consists in monitoring the fluorescence along the deceleration path is used. This allows a direct observation of the process and open possibilities to investigate the adiabatic following of atoms in the magnetic field, and others very important aspects of the process. With a single laser and some modification of the magnetic field profile it is possible stop atoms outside the slower solenoid, which make a lot of experiments much simpler. A systematic study of the optical pumping effects and adiabatic following conditions allow to produce a very strong slow motion atomic beam. (author)

  10. 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...

  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. Enhancement reagents for simultaneous vapor generation of zinc and cadmium with intermittent flow system coupled to atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    Simultaneous vapor generation of zinc (Zn) and cadmium (Cd) was evaluated by atomic fluorescence spectrometry coupled with an intermittent flow vapor generation system. Some complexing reagents, surfactant and transition metal ions were respectively tested as enhancement reagents. Experiments showed that an appropriate amount of 8-hydroxyquinoline or phenanthroline and nickel ion simultaneously, effectively improved the vapor generation efficiency of Zn and Cd. The volatile species generation was presumed to be a hydrogenation process interpreting how the enhancement reagents played an important role in vapor generation. Additionally, due to the instability of volatile species, reaction temperature, rapid and sufficient mixing of reagents and rapid separation of the volatile species from liquid phase were also crucial. The method of simultaneous determination of Zn and Cd by intermittent flow vapor generation led to the development of atomic fluorescence spectrometry. The detection limits (3σb) were 1.6 μg l-1 for Zn and 0.01 μg l-1 for Cd and the relative standard deviations were 3.6% for Zn (50 μg l-1, n=11) and 1.7% for Cd (2 μg l-1, n=11) respectively. Results for the determination of Zn and Cd have been confirmed by the analysis of CRMs with good agreement between the certified and found values

  13. 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

  14. 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.

  15. Development of a MSFIA system for sequential determination of antimony, arsenic and selenium using hydride generation atomic fluorescence spectrometry.

    Science.gov (United States)

    de Santana, Fernanda A; Portugal, Lindomar A; Serra, Antonio M; Ferrer, Laura; Cerdà, Víctor; Ferreira, Sergio L C

    2016-08-15

    This paper proposed a multisyringe flow injection analysis (MSFIA) system for antimony, arsenic and selenium determination in peanut samples by hydride generation atomic fluorescence spectrometry (HG-AFS). The optimization step of the hydride generation was performed using a two-level full factorial design involving the parameters: hydrochloric acid, sodium tetrahydroborate and potassium iodide concentrations. So, using the chemical conditions optimized, this method allows the determination of these elements employing the external calibration technique using aqueous standards with limits of detection and quantification of 0.04 and 0.14µgL(-1) for antimony, 0.04 and 0.14µgL(-1) for arsenic and 0.14 and 0.37µgL(-1) for selenium, respectively. Additionally, the effect of vanadium, chromium, cobalt, nickel, zinc, copper, iron and molybdenum on the generation of chemical vapour was also studied. The precision expressed as relative standard deviation varied from 1.2 to 3.6% for antimony, 1.8-3.9% for arsenic and 1.8-2% for selenium. The accuracy for arsenic and selenium was confirmed using the certified peach leaves reference material SRM 1547 produced by National Institute of Standard and Technology. The proposed method showed 45 injection throughput (h(-1)) using 1.6mL sample volume for each element, 0.8mL NaBH4 0.5% (w/v) containing NaOH 0.05% (w/v), 0.8mL HCl 5M and 0.4mL KI 14% (w/v) containing L-ascorbic acid 2.5% (w/v). The method was applied to the determination of antimony, arsenic and selenium in peanut samples, which were firstly lyophilized and afterward digested using microwave assisted radiation. Six samples were analyzed and the contents of the elements found were: 28.7-41.3µgkg(-1) for arsenic, 86.4-480.1µgkg(-1) for selenium and 32.6-52.4µgkg(-1) for antimony. Addition/recovery tests were also performed to confirm the method accuracy for the three elements. PMID:27260431

  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. Ultrasensitive determination of cadmium in seawater by hollow fiber supported liquid membrane extraction coupled with graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    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 HNO3 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

  19. 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.

  20. Cosmology with intensity mapping techniques using atomic and molecular lines

    CERN Document Server

    Fonseca, José; Santos, Mário G; Cooray, Asantha

    2016-01-01

    We present a systematic study of the intensity mapping technique using updated models for the different emission lines from galaxies and identify which ones are more promising for cosmological studies of the post reionization epoch. We consider the emission of ${\\rm Ly\\alpha}$, ${\\rm H\\alpha}$, H$\\beta$, optical and infrared oxygen lines, nitrogen lines, CII and the CO rotational lines. We then identify that ${\\rm Ly\\alpha}$, ${\\rm H\\alpha}$, OII, CII and the lowest rotational CO lines are the best candidates to be used as IM probes. These lines form a complementary set of probes of the galaxies emission spectra. We then use reasonable experimental setups from current, planned or proposed experiments to access the detectability of the power spectrum of each emission line. Intensity mapping of ${\\rm Ly\\alpha}$ emission from $z=2$ to 3 will be possible in the near future with HETDEX, while far-infrared lines require new dedicated experiments. We also show that the proposed SPHEREx satellite can use OII and ${\\r...

  1. 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

  2. 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.

  3. 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

    International Nuclear Information System (INIS)

    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−1 N (r = 0.9994), 100–2000 mg L−1 P (r = 0.9946), and 100–2500 mg L−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% (NO3−-N), 95–103% (NH4+-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 H2O2 allows analysis of fertilizers with different nitrogen species. • Proposal provides advantages over traditional methods in terms of cost and time

  4. 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.

  5. A novel analytical system involving hydride generation and gold-coated W-coil trapping atomic absorption spectrometry for selenium determination at ng l-1 level

    International Nuclear Information System (INIS)

    A novel analytical technique was developed where gaseous hydrogen selenide formed by sodium tetrahydroborate reduction is transported to and trapped on a resistively heated gold-coated W-coil atom trap for in situ preconcentration. Gold coating on W-coil was prepared by using an organic solution of Au. The atom trap is held at 165 oC during the collection stage and is heated up to 675 deg. C for revolatilization; analyte species formed are transported to an externally heated quartz T-tube where the atomization takes place and the transient signal is obtained. The carrier gas consisted of 112.5 ml min-1 Ar with 75 ml min-1 H2 during the collection step and 112.5 ml min-1 Ar with 450 ml min-1 H2 in the revolatilization step. The half width of the transient signal obtained is less than 0.5 s. The RSD for the measurements was found to be 3.9% (n = 11) for 0.10 μg l-1 Se using peak height measurements. The calibration plot for 27.0 ml of sample collected in 4.0 min using a flow rate of 6.75 ml min-1 was linear between 0.13 and 2.0 μg l-1 of Se. The limit of detection (3 s) is 39 ng l-1. The enhancement factor for the characteristic concentration (Co) was found to be 20.1 when compared to conventional hydride generation atomic absorption spectrometry system without trap. In order to check the accuracy of the method, standard reference material, natural water NIST 1640 was employed; the result was found to be in good agreement with the certified value at the 95% confidence level

  6. 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.

  7. 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

  8. 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...

  9. Mass spectrometry in oceanography

    International Nuclear Information System (INIS)

    Mass spectrometry plays an important role in oceanography for various applications. Different types of inorganic as well as organic mass spectrometric techniques are being exploited world-wide to understand the different aspects of marine science, for palaeogeography, palaeoclimatology and palaeoecology, for isotopic composition and concentrations of different elements as well as for speciation studies. The present paper reviews some of the applications of atomic mass spectrometric techniques in the area of oceanography

  10. Ultratrace determination of tin by hydride generation in-atomizertrapping atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Průša, Libor; Dědina, Jiří; Kratzer, Jan

    2013-01-01

    Roč. 804, DEC (2013), s. 50-58. ISSN 0003-2670 R&D Projects: GA ČR(CZ) GPP206/11/P002 Grant ostatní: GA MŠk(CZ) MSM0021620857 Institutional support: RVO:68081715 Keywords : hydride generation * tin preconcentration * in-atomizer trapping * trap-and-atomizer device * stannane Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.517, year: 2013

  11. 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.

  12. Analysis of aluminium by atomic absorption spectrometry and analysis of thorium and uranium by alpha spectrometry in the black sand of Egypt

    International Nuclear Information System (INIS)

    Throughout the period of our project of end of study carried out in the Center ; main road Sciences and Nuclear Engineering's CNSTN in one is tallied took one Egypt black sand simple with an aim has of knowing the activities of the existing radio elements and especially Uranium and Thorium. In the same mining, we try to take another Egypt black sand simple an aim has knowing the mass of aluminum by using a techniques in Atomique Absorption Spectrophotometer. After the radio chemical and Spectrometry analysis of the black sand sample we found the results following: - Egypt black sand is contains isotopes of Uranium such as 234U and 238U; - The Egypt black sand is contains isotopes of Thorium such as 230Th and 232Th. - L' Aluminum is a major. (Author)

  13. High sensitivity probe absorption technique for time-of-flight measurements on cold atoms

    Indian Academy of Sciences (India)

    A K Mohapatra; C S Unnikrishnan

    2006-06-01

    We report on a phase-sensitive probe absorption technique with high sensitivity, capable of detecting a few hundred ultra-cold atoms in flight in an observation time of a few milliseconds. The large signal-to-noise ratio achieved is sufficient for reliable measurements on low intensity beams of cold atoms. We demonstrate the high sensitivity and figure of merit of the simple method by measuring the time-of-flight of atoms moving upwards from a magneto-optical trap released in the gravitational field.

  14. 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.

  15. 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

  16. Graphite furnace atomic absorption spectrometry as a routine method for the quantification of beryllium in blood and serum

    Directory of Open Access Journals (Sweden)

    Brousseau Pauline

    2008-07-01

    Full Text Available Abstract Background A routine method for the quantification of beryllium in biological fluids is essential for the development of a chelation therapy for Chronic Beryllium Disease (CBD. We describe a procedure for the direct determination of beryllium in undigested micro quantities of human blood and serum using graphite furnace atomic absorption spectrometry. Blood and serum samples are prepared respectively by a simple 8-fold and 5-fold dilution with a Nash Reagent. Three experimental setups are compared: using no modifier, using magnesium nitrate and using palladium/citric acid as chemical modifiers. Results In serum, both modifiers did not improve the method sensitivity, the optimal pyrolysis and atomization temperatures are 1000°C and 2900°C, respectively. In blood, 6 μg of magnesium nitrate was found to improve the method sensitivity. The optimal pyrolysis and atomization temperatures were 800°C and 2800°C respectively. Conclusion In serum, the method detection limit was 2 ng l-1, the characteristic mass was 0.22 (± 0.07 pg and the accuracy ranged from 95 to 100%. In blood, the detection limit was 7 ng l-1, the characteristic mass was 0.20 (± 0.02 pg and the accuracy ranged from 99 to 101%.

  17. A highly sensitive method for the determination of mercury using vapor generation gold wire microextraction and electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The study introduces a new simple and highly sensitive method for headspace solid phase microextraction (HS-SPME) coupled with electrothermal atomic absorption spectrometric determination of mercury. In the proposed method, a gold wire, mounted in the headspace of a sample solution in a sealed bottle, is used for collection of mercury vapor generated by addition of sodium tetrahydroborate. The gold wire is then simply inserted in the sample introduction hole of a graphite furnace of an electrothermal atomic absorption spectrometry instrument. By applying an atomization temperature of 600 deg. C, mercury is rapidly desorbed from the wire and determined with high sensitivity. Factorial design and response surface analysis methods were used for optimization of the effect of five different variables in order to maximize the mercury signal. By using a 0.75 mm diameter gold wire, a sample volume of about 8 ml and an extraction time of 11 min, the sensitivity of mercury determination was enhanced up to 104 times in comparison to its ordinary ETAAS determination with direct injection of 10 μl sample solutions. A detection limit of 0.006 ng ml-1 and a precision better than 4.6% (relative standard deviation) were obtained. The method was successfully applied to the determination of mercury in industrial wastewaters and tuna fish samples

  18. A highly sensitive method for the determination of mercury using vapor generation gold wire microextraction and electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hashemi, Payman [Department of Chemistry, Lorestan University, Khorram Abad (Iran, Islamic Republic of)], E-mail: payman_hashemi@yahoo.com; Rahimi, Akram [Department of Chemistry, Lorestan University, Khorram Abad (Iran, Islamic Republic of)

    2007-04-15

    The study introduces a new simple and highly sensitive method for headspace solid phase microextraction (HS-SPME) coupled with electrothermal atomic absorption spectrometric determination of mercury. In the proposed method, a gold wire, mounted in the headspace of a sample solution in a sealed bottle, is used for collection of mercury vapor generated by addition of sodium tetrahydroborate. The gold wire is then simply inserted in the sample introduction hole of a graphite furnace of an electrothermal atomic absorption spectrometry instrument. By applying an atomization temperature of 600 deg. C, mercury is rapidly desorbed from the wire and determined with high sensitivity. Factorial design and response surface analysis methods were used for optimization of the effect of five different variables in order to maximize the mercury signal. By using a 0.75 mm diameter gold wire, a sample volume of about 8 ml and an extraction time of 11 min, the sensitivity of mercury determination was enhanced up to 10{sup 4} times in comparison to its ordinary ETAAS determination with direct injection of 10 {mu}l sample solutions. A detection limit of 0.006 ng ml{sup -1} and a precision better than 4.6% (relative standard deviation) were obtained. The method was successfully applied to the determination of mercury in industrial wastewaters and tuna fish samples.

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

    International Nuclear Information System (INIS)

    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(NO3)2 and (NH4)H2PO4-Mg(NO3)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 μg L-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 -1

  20. [Determination of aluminum in wheat flour food by microwave digestion-high resolution continuum source graphite furnace atomic absorption spectrometry].

    Science.gov (United States)

    Ren, Ting; Zhao, Li-jiao; Zhong, Ru-gang

    2011-12-01

    The contents of aluminum (Al) in four kinds of wheat flour food (noodle, dumpling wrapper, twisted cruller and soda biscuit) were determined by high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) combined with microwave digestion. The samples were completely digested by the mixture of HNO3 and H2O2 in closed polytetrafluoroethylene (PTFE) vessels. The conditions for microwave digestion, pyrolysis temperature and atomization temperature were optimized. The optimum experimental conditions were determined as follows. The microwave digestion was performed with HNO3/H2O2 7:1 (volume ratio), microwave power 1000 W and 190 degrees C for 40 minutes. The optimum pyrolysis temperature was 1350 degrees C and the optimum atomization temperature was 2400 degrees C. Magnesium nitrate solution with the concentration of 1 g x L(-1) was used as the matrix modifier. The correlation coefficient for the standard curve was 0.9999, the relative standard deviation (RSD) was from 1.7% to 2.4%, and the recovery for the samples was from 98.16% to 102.67%. The assay method for the determination of Al in wheat flour food established in this study has referential importance for the constituent of the correlated food standards. PMID:22295801

  1. 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).

  2. Direct determination of P in biodiesel by high-resolution continuum source graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The direct determination of P in biodiesel by high-resolution continuum source graphite furnace atomic absorption spectrometry has been investigated. A slow drying stage proved to be essential for good repeatability. Optimization was performed by a D optimal planning. The atomization temperature and modifier composition were the most relevant parameters. Thus, using a mixture of Pd (30 μg) and Mg(NO3)2 (20 μg) as the modifier, previously deposited onto the platform of the graphite tube and dried, a five step drying stage, and pyrolysis and atomization temperatures of 1000 and 2700 deg. C, respectively, a limit of detection of 0.5 μg g-1 was obtained. The analysis of biodiesel of different origins confirmed that external calibration with organic P standard solutions, diluted in P-free biodiesel, could be used. In this way, excellent agreement between the found and expected results was observed in the analysis of an ANP interlaboratorial exercise sample.

  3. Sensitive determination of bismuth by flame atomic absorption spectrometry using atom trapping in a slotted quartz tube and revolatilization with organic solvent pulse

    International Nuclear Information System (INIS)

    Sensitivity of flame atomic absorption spectrometry (FAAS) for Bi determination was improved by slotted quartz tube (SQT) that was used also for atom trapping (AT). The trapped analyte was released by aspirating a small volume of organic solvent after a reasonable analyte collection time. Sensitivity was improved by 2.9 times by SQT-FAAS and 256 times by SQT-AT-FAAS with respect to FAAS. Optimum trapping period was found to be 6.0 min (36.0 mL of solution). Limit of detection (LOD) for SQT-AT-FAAS was found to be 1.6 ng mL−1. %RSD was calculated as 4.0% for five replicate measurements of 7.5 ng mL−1 Bi by SQT-AT-FAAS. Accuracy of the method developed was checked by analyzing a standard reference material of simulated fresh water (NIST 1643e) and result found was in good agreement with the certified one. The method can be applied in any laboratory equipped with a flame AA spectrometer. The consumption of time and sample volume is fairly low and application is simple and easy.

  4. Mass spectrometry based imaging techniques for spatially resolved analysis of molecules

    Directory of Open Access Journals (Sweden)

    Andrea eMatros

    2013-04-01

    Full Text Available Higher plants are composed of a multitude of tissues with specific functions, reflected by distinct profiles for transcripts, proteins and metabolites. Comprehensive analysis of metabolites and proteins has advanced tremendously within recent years, and this progress has been driven by the rapid development of sophisticated mass spectrometrical techniques. In most of the current omics-studies, analysis is performed on whole organ or whole plant extracts, rendering to the loss of spatial information. Mass spectrometry based imaging (MSI techniques have opened a new avenue to obtain information on the spatial distribution of metabolites and of proteins. Pioneered in the field of medicine, the approaches are now applied to study the spatial profiles of molecules in plant systems. A range of different plant organs and tissues have been successfully analyzed by MSI, and patterns of various classes of metabolites from primary and secondary metabolism could be obtained. It can be envisaged that MSI approaches will substantially contribute to build spatially resolved biochemical networks.

  5. Study of bioaccumulation, biovolatilization and biosorption of aluminium and thallous species by microscopic fungi using atomic spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. The metal bioaccumulation, biovolatilization and biosorption processes can be defined as a physico-chemical interaction which may occur between metal species and cellular compounds including chitin, chitosan, carboxyls, amines, hydroxyls, phosphates, sulfhydryls and other functional groups present in e.g. fungal biomass. The bioaccumulation, biovolatilization and biosorption of Al(III) and Tl(I) species from synthetic solutions by compact and pelletized biomass of three strains of microscopic filamentous fungi (Neosartorya fischeri, Aspergillus niger, Aspergillus clavatus) were studied under laboratory conditions. The recoveries of studied processes were quantified by atomic spectrometry techniques (F AAS, ET AAS, ICP OES). The speciation of Al(III) and Tl(I) in synthetic solutions was obtained by computer modelling. Further the changes of pH values, the fungi resistance to Al and Tl and the influence of fungi metabolism on the studied processes were observed and investigated. Results showed that the highest amounts of Al were bioaccumulated and biosorbed by Aspergillus clavatus. The bioavailable aqua cations Al3+, Al(OH)2+ and Al(OH)2+ are the prevailing species below pH 5.0. In the pH range between 5.0 and 6.2, there is a mixture of these cations and colloidal Al(OH)3 species. At pH higher than 6.2, the dominant species is Al(OH)4-1. The amounts of bioaccumulated, biovolatilized and biosorbed of labile Tl by Neosartorya fischeri were described also. The bioavailable cations Tl+ and relatively weak neutral complexes (TlNO3, TlOH) are the prevailing species at given conditions. It is assumed that dimethylthallium (Me2Tl+) is the main biovolatilized Tl chemical form. In certain conditions the studied fungi can be used as the bioanalytical tools for in-situ separation and preconcentration of bioavailable species of Al and Tl or their fractions directly in the ecosystem, e.g. in the analysis of polluted waters. The

  6. 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

  7. Analysis of neodymium oxide for rare earth impurities by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    A procedure for the determination of the rare earths elements in neodymium oxide with purity grade above 99% by inductively coupled plasma optical emission spectrometry is described. Determination limits were 0,005% for the elements Eu, Dy, Gd, Tb, Ho and Y and 0,01% for Sm and La. The precision of the method was evaluated through the relative standard deviation (RSD) for individual rare earth elements. The values lies in the range of 3 -7% for most of them but lanthanum, has shown 13% RSD. (author)

  8. 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.

  9. Atomic and molecular physics using positron accumulation techniques - Summary and a look to the future

    International Nuclear Information System (INIS)

    An overview is presented of current techniques to accumulate and cool large numbers of positrons from a radioactive 22Na source and neon moderator, and the first operation of a new generation of positron accumulator is described. Experiments are discussed that use these techniques to study the interaction of positrons with atoms and molecules at low energies (i.e., below the threshold for positronium formation), including systematic studies of the dependence of positron annihilation on chemical composition. By measuring the Doppler-broadening of gamma-ray annihilation radiation, the quantum state of the annihilating electrons in atoms and molecules was identified. These experiments indicate that positrons annihilate with approximately equal probability on any valence electron. Annihilation with inner shell electrons is infrequent, but is measurable at the level of a few percent in heavier atoms. Measurements of annihilation rates in molecules as a function of positron temperature revealed a number of interesting trends that are briefly discussed. We have developed a new technique to make a cold, bright positron beam. This technique is now being used for a new generation of scattering experiments in the range of energies ≤1 eV. Other possible experiments to study aspects of atomic and molecular physics using positron accumulation techniques and this cold positron beam are briefly discussed

  10. Determination of boron in the waters of Troia by inductively coupled plasma-atomic emission spectrometry (ICP-AES

    Directory of Open Access Journals (Sweden)

    HASAN OZCAN

    2005-10-01

    Full Text Available The inductively coupled plasma-atomic emission spectrometry method (ICP-EAS is proposed for the determination of boron in Troia water sources. In this study, boron samples were taken from 25 different locations during November 2002 and May 2003. The 249.773 nm boron emmision line was not affected by the samplematrix. The boron content was determined without further pretreatment of samples proposed ICP-AES method. An analysis of a given sample was completed in about 15 min. The determined boron concentrations in surface and ground water sources were between 0.00444–1.11200mgl-1. Inorder to compare the results obtained by the proposed method, selected water samples were also analysed titrimetically. Pearson correlation coefficient analysis showed that there is a close relationship between the ICP-AES and the titrimetric method and the determination coefficient (R2 was calculated to be 91.34 %.

  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. 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

  13. Development of an axially viewed inductively coupled plasma for atomic emission spectrometry and comparison between the detection limits of lead

    International Nuclear Information System (INIS)

    An ICP(Inductively Coupled plasma) emission spectrometer was developed with an axially viewed ICP source incorporated by a 5-turned induction coil and a torch, outer quartz tube of which was 50 mm longer than that used in conventional ICP/AES(Inductively Coupled Plasma Atomic Emission Spectrometry). The optimization of the system has been performed in terms of the determination of signal-to-noise ratio and background intensity at various rf powers, sample flow rates, argon gas flow rates and cut-off gas flow rates. The spectro-analytical characteristics of the spectrum obtained between 200 and 500 nm was revealed to be similar compared with a vertically viewed ICP source. The detection limit of Pb(II) at 220.35 nm was 11 ppb which was 5 times lower than that obtained with a vertically viewed ICP source. (author)

  14. 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)

  15. 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)

  16. Determination of mercury by electrochemical cold vapor generation atomic fluorescence spectrometry using polyaniline modified graphite electrode as cathode

    Energy Technology Data Exchange (ETDEWEB)

    Jiang Xianjuan [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China); Gan Wuer, E-mail: wgan@ustc.edu.c [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China); Wan Lingzhong; Zhang Hanchang; He Youzhao [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China)

    2010-02-15

    An electrochemical cold vapor generation system with polyaniline modified graphite electrode as cathode material was developed for Hg (II) determination by coupling with atomic fluorescence spectrometry. This electrochemical cold vapor generation system with polyaniline/graphite electrode exhibited higher sensitivity; excellent stability and lower memory effect compared with graphite electrode electrochemical cold vapor generation system. The relative standard deviation was 2.7% for eleven consecutive measurements of 2 ng mL{sup -1} Hg (II) standard solution and the mercury limit of detection for the sample blank solution was 1.3 rg mL{sup -1} (3sigma). The accuracy of the method was evaluated through analysis of the reference materials (GBW09101) (Human hair) and GBW (08517) (Laminaria Japonica Aresch) and the proposed method was successfully applied to the analysis of human hairs.

  17. Application of radiochemical neutron activation and atomic absorption spectrometry methods for the study of nutrition-pollution interactions in children

    International Nuclear Information System (INIS)

    The application of radiochemical neutron activation analysis (RNAA) and atomic absorption spectrometry (AAS) is expected to aid in understanding and evaluating the effects of environmental pollution on the nutritional status of children already exposed to marginal malnutrition. Samples of placenta, of low-weight and control newborns groups, were collected for determination of nutritional elements and pollutants. The mean ratios of pollutants and nutrients such as Cd/Zn, Hg/Se and Pb/Ca were evaluated for both groups. All these ratios in the placenta of the low-weight newborns are higher than that of the healthy group. The degree of the nutrient-pollutant interaction is evaluated by quantity R, with mercury considered as the most active pollutant while calcium the most active nutrient among the involved elements in process of the interaction. (author)

  18. 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.

  19. UV-assisted Fenton digestion of rice for the determination of trace cadmium by hydride generation atomic fluorescence spectrometry.

    Science.gov (United States)

    Yu, Huimin; Ai, Xi; Xu, Kailai; Zheng, Chengbin; Hou, Xiandeng

    2016-02-21

    A new digestion method using UV-assisted Fe(0) Fenton reaction was developed for the determination of trace Cd in rice by hydride generation atomic fluorescence spectrometry. The proposed method integrated the advantages of simplicity, small dose of reagents, low cost and moderate reaction conditions, and was successfully utilized to analyze a Certified Reference Material (CRM) and real rice samples. A 1 mL mixture of the sample and reagents (0.0500 g rice powder, 0.2% (m/v) Fe(0), 0.75% (v/v) HNO3 and 18% (v/v) H2O2) was irradiated by UV-light for 50 min and then a clear solution was obtained by separating excess Fe(0) with a magnet prior to spectral analysis. The limit of detection (LOD) for Cd was found to be 0.02 mg kg(-1) and the relative standard deviation was better than 5.0% at a concentration level of 0.40 mg kg(-1). The recovery obtained by analyzing the CRM was 103% and spiked recoveries with 0.40 mg kg(-1) Cd in rice samples were 93% and 101%. The t-test proved that there is no significant difference between the certified value and the determined value of the CRM, and between the proposed method and microwave-assisted digestion coupled with inductively coupled plasma mass spectrometry (MWD-ICP-MS) at 95% confidence level. PMID:26759832

  20. 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

  1. Flotation separation of iron, copper and lead in environmental samples and their determination by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Complete text of publication follows. Some of the heavy metals are among the most harmful of the elemental pollutants and are of particular concern because of their toxicities to humans. Heavy metals include essential elements like iron as well as toxic metals like cadmium and mercury. Direct determination of trace heavy metals, by flame atomic absorption spectrometry (FAAS) or electrothermal atomic spectrometry (ETAAS) is not possible, because of their low concentrations and matrix effects. In order to know the accurate concentrations of trace heavy metals, enrichment processes are necessary. The most common, simple, rapid, low cost and effective method used for preconcentration is flotation. Only a small amount of surfactant, collector agent and tiny air bubbles is required to perform the proper flotation. Most of them have a tremendous affinity for sulfur and disrupt enzyme function by forming bonds with sulfur groups in enzymes. In this work a simple, sensitive and accurate procedure for flotation separation followed by ETAAS determination of Fe, Cu and Pb is proposed. 2-(2-methoxy phenyl) benzimidazole was used as the new collector agent. The optimum conditions of flotation were studied and important parameters were optimized. The experiment was done at pH =5. The linear ranges are 0-58, 0.350, 0-28 μg L-1 for Fe, Cu, and Pb respectively. The detection limits of the method for Fe, Cu and Pb are 0.08, 0.001, 0.08 μg L-1 respectively. This method was successfully applied for separation and determination of Cu, Pb and Fe in some environmental samples.

  2. 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.

  3. Determination of cobalt in biological samples by line-source and high-resolution continuum source graphite furnace atomic absorption spectrometry using solid sampling or alkaline treatment

    International Nuclear Information System (INIS)

    Two procedures for the determination of Co in biological samples by graphite furnace atomic absorption spectrometry (GF AAS) were compared: solid sampling (SS) and alkaline treatment with tetramethylammonium hydroxide (TMAH) using two different instruments for the investigation: a conventional line-source (LS) atomic absorption spectrometer and a prototype high-resolution continuum source atomic absorption spectrometer. For the direct introduction of the solid samples, certified reference materials (CRM) were ground to a particle size ≤50 μm. Alkaline treatment was carried out by placing about 250 mg of the sample in polypropylene flasks, adding 2 mL of 25% m/v tetramethylammonium hydroxide and de-ionized water. Due to its unique capacity of providing a 3-D spectral plot, a high-resolution continuum source (HR-CS) graphite furnace atomic absorption spectrometry was used as a tool to evaluate potential spectral interferences, including background absorption for both sample introduction procedures, revealing that a continuous background preceded the atomic signal for pyrolysis temperatures lower than 700 deg. C. Molecular absorption bands with pronounced rotational fine structure appeared for atomization temperatures >1800 deg. C probably as a consequence of the formation of PO. After optimization had been carried out using high resolution continuum source atomic absorption spectrometry, the optimized conditions were adopted also for line-source atomic absorption spectrometry. Six biological certified reference materials were analyzed, with calibration against aqueous standards, resulting in agreement with the certified values (according to the t-test for a 95% confidence level) and in detection limits as low as 5 ng g-1

  4. 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

  5. Gamma-ray spectrometry combined with acceptable knowledge (GSAK). A technique for characterization of certain remote-handled transuranic (RH-TRU) wastes. Part 1. Methodology and techniques

    International Nuclear Information System (INIS)

    Gamma-ray spectrometry combined with acceptable knowledge (GSAK) is a technique for the characterization of certain remote-handled transuranic (RH-TRU) wastes. GSAK uses gamma-ray spectrometry to quantify a portion of the fission product inventory of RH-TRU wastes. These fission product results are then coupled with calculated inventories derived from acceptable process knowledge to characterize the radionuclide content of the assayed wastes. GSAK has been evaluated and tested through several test exercises. GSAK approach is described, while test results are presented in Part II. (author)

  6. Salt-assisted liquid-liquid microextraction of Cr(VI) ion using an ionic liquid for preconcentration prior to its determination by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    We report on the salt-assisted liquid-liquid microextraction of cationic complexes of Cr(VI) ion using the hydrophilic ionic liquid (IL) 1-butyl-3-methylimidazolium tetrafluoraborate and potassium hydrogen phosphate. This is a novel, simple, non-toxic and effective technique for sample pretreatment technique that displays large extraction efficiency and represents a new platform where Cr(VI) is complexed with 1,5-diphenylcarbazide (DPC) in sulfuric acid medium. It was applied to the extraction of Cr(VI) in the form of the Cr(VI)-DPC complex prior to its determination by flame atomic absorption spectrometry. Cr(III) ion also can be determined by this procedure after oxidation to Cr(VI). Extraction is mainly affected by the amount of water-soluble IL, the kind and quantity of inorganic salts, by pH and the concentration of DPC. Calibration plots are linear in the range from 3 to 150 μg L-1 of Cr(VI), and the limit of detection is 1. 25 μg L-1. The method was successfully applied to the speciation and determination of trace levels of Cr(III) and Cr(VI) in environmental water samples containing high levels of dissolved salts or food grade salts. (author)

  7. Immersed single-drop microextraction interfaced with sequential injection analysis for determination of Cr(VI) in natural waters by electrothermal-atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Single-drop microextraction (SDME) and sequential injection analysis have been hyphenated for ultratrace metal determination by Electrothermal-Atomic Absorption Spectrometry (ETAAS). The novel method was targeted on extraction of the Cr(VI)-APDC chelate and encompasses the potential of SDME as a miniaturized and virtually solvent-free preconcentration technique, the ability of sequential injection analysis to handle samples and the versatility of furnace autosamplers for introducing microliter samples in ETAAS. The variables influencing the microextraction of Cr(VI) onto an organic solvent drop, i.e., type of organic solvent, microextraction time, stirring rate of the sample solution, drop volume, immersion depth of the drop, salting-out effect, temperature of the sample, concentration of the complexing agent and pH of the sample solution were fully investigated. For a 5 and 20 min microextraction time, the preconcentration factors were 20 and 70, respectively. The detection limit was 0.02 μg/L of Cr(VI) and the repeatability expressed as relative standard deviation was 7%. The SDME-SIA-ETAAS technique was validated against BCR CRM 544 (lyophilized solution) and applied to ultrasensitive determination of Cr(VI) in natural waters

  8. Characterization of the Plasma Edge for Technique of Atomic Helium Beam in the CIEMAT Fusion Device

    International Nuclear Information System (INIS)

    In this report, the measurement of Electron Temperature and Density in the Boundary Plasma of TJ-II with a Supersonic Helium Beam Diagnostic and work devoted to the upgrading of this technique are described. Also, simulations of Laser Induced Fluorescence (LIF) studies of level populations of electronically excited He atoms are shown. This last technique is now being installed in the CIEMAT fusion device. (Author )

  9. 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…

  10. Determination of bismuth by dielectric barrier discharge atomic absorption spectrometry coupled with hydride generation: Method optimization and evaluation of analytical performance

    Czech Academy of Sciences Publication Activity Database

    Kratzer, Jan; Boušek, J.; Sturgeon, R. E.; Mester, Z.; Dědina, Jiří

    2014-01-01

    Roč. 86, č. 19 (2014), s. 9620-9625. ISSN 0003-2700 Grant ostatní: GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * hydride generation * atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 5.636, year: 2014

  11. 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...

  12. 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).

  13. 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...

  14. 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 ketone...

  15. Feasibility guidelines for kaonic atom experiments with ultra-high-resolution X-ray spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Friedman, E., E-mail: elifried@cc.huji.ac.il [Racah Institute of Physics, The Hebrew University, 91904 Jerusalem (Israel); Okada, S. [RIKEN Nishina Center, RIKEN, Wako 351-0198 (Japan)

    2013-10-03

    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{sup −}–nucleon interaction in the nuclear medium.

  16. 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

  17. 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)

  18. The determination of caesium and silver in soil and fungal fruiting bodies by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Methods have been developed for the determination of caesium and silver in soil and fungal samples by microwave-assisted aqua regia digestion, followed by electrothermal atomic absorption spectrometry. The procedure was found to be repeatable (for soil, RSD -1, respectively, and for fungi, RSD -1, respectively) and reasonably efficient. Silver was recovered quantitatively from reference soils, but only about 80-85% of the caesium present could be extracted. Poorer caesium recoveries (< 70%) were obtained if, as part of the sample preparation procedure, solutions were taken to dryness in glass beakers prior to analysis. The detection limits were 0.02 mg Ag and 0.09 mg Cs per gram of dry soil, which are adequate for the determination of the analytes at typical environmental levels. The methods were applied in the analysis of three types of soil, a peaty podzol, a clay loam and a sandy loam and no significant matrix interferences were observed except in the determination of caesium in the sandy loam. For caesium, non-linear response curves, thought to be due to ionisation interference, were encountered using one atomic absorption spectrometer, but were not observed with the other instrument

  19. 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

  20. On-line preconcentration and determination of mercury in biological and environmental samples by cold vapor-atomic absorption spectrometry

    International Nuclear Information System (INIS)

    An on-line procedure for the determination of traces of total mercury in environmental and biological samples is described. The present methodology combines cold vapor generation associated to atomic absorption spectrometry (CV-AAS) with preconcentration of the analyte on a minicolumn packed with activated carbon. The retained analyte was quantitatively eluted from the minicolumn with nitric acid. After that, volatile specie of mercury was generated by merging the acidified sample and sodium tetrahydroborate(III) in a continuous flow system. The gaseous analyte was subsequently introduced via a stream of Ar carrier into the atomizer device. Optimizations of both, preconcentration and mercury volatile specie generation variables were carried out using two level full factorial design (23) with 3 replicates of the central point. Considering a sample consumption of 25 mL, an enrichment factor of 13-fold was obtained. The detection limit (3σ) was 10 ng L-1 and the precision (relative standard deviation) was 3.1% (n = 10) at the 5 μg L-1 level. The calibration curve using the preconcentration system for mercury was linear with a correlation coefficient of 0.9995 at levels near the detection limit up to at least 1000 μg L-1. Satisfactory results were obtained for the analysis of mercury in tap water and hair samples

  1. Determination of antimony in sediments and soils by slurry sampling graphite furnace atomic absorption spectrometry using a permanent chemical modifier

    Energy Technology Data Exchange (ETDEWEB)

    Dobrowolski, Ryszard, E-mail: rdobrow@poczta.umcs.lublin.pl; Adamczyk, Agnieszka; Otto, Magdalena; Dobrzynska, Joanna

    2011-07-15

    For comparison of action of mixed permanent modifiers Ir/Nb and Ir/W, the influence of the amounts of modifier components was studied and the atomic absorption pyrolysis and atomization curves were determined with different modifiers. The optimum amounts of modifier components were 30 {mu}g Ir and 40 {mu}g of Nb that were deposited onto the L'vov platform in advance to analytical measurements. The long-term performance of the Ir and Nb permanent modifiers was derived from the investigations by scanning electron microscopy and energy dispersive X-ray spectrometry. The soil and sediment slurries were prepared in 4% hydrofluoric acid and 6% suspension of polytetrafluoroethylene in order to remove the high concentration of silica during the pyrolysis step of 900 deg. C. The calibration was made by using aqueous standards. The analysis of certified reference materials confirmed the accuracy and reliability of the proposed analytical approach. The precision of Sb determination was characterized with less than 6% RSD.

  2. 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

  3. 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

  4. Mapping of explosive contamination using GC/chemiluminescence and ion mobility spectrometry techniques

    Science.gov (United States)

    Miller, Carla J.; Glenn, D. F.; Hartenstein, Steven D.; Hallowell, Susan F.

    1998-12-01

    Recent efforts at the Idaho National Engineering and Environmental Laboratory (INEEL) have included mapping explosive contamination resulting from manufacturing and carrying improvised explosive devices (IEDs). Two types of trace detection equipment were used to determine levels of contamination from designated sampling areas. A total of twenty IEDs were constructed: ten using TNT and ten using C-4. Two test scenarios were used. The first scenario tracked the activities of a manufacturer who straps the device onto an independent courier. The courier then performed a series of activities to simulate waiting in an airport. The second scenario tracked the activities of a manufacturer who also served as the courier. A sample set for each test consisted of thirty samples from various locations on each IED manufacturer, thirty from each IED courier, twenty-five from the manufacturing area, and twenty-five from the courier area. Pre-samples and post-samples were collected for analysis with each detection technique. Samples analyzed by gc/chemiluminescence were taken by swiping a teflon- coated sampling swipe across the surface of the sampling area to pick up any explosive particles. Samples analyzed by ion mobility spectrometry (IMS) were taken from the clothing of the manufacturer and courier by vacuuming the surface and collecting particulates on a fiberglass filter. Samples for IMS analysis from the manufacturing and courier rooms were taken by wiping a cotton sampling swipe across the surface area. Currently, building IEDs and monitoring the explosive contamination is being directed toward detection with portal monitors.

  5. Imaging spectrometry and GIS techniques application for the study of seawater quality and pollution hazard

    Science.gov (United States)

    Marino, Alessandra; Ludovisi, Giancarlo; Moccaldi, Antonio; Bellagamba, Sergio

    2002-01-01

    The aim of this paper is to outline the potential of imaging spectrometry and GIS techniques as tools for the monitoring of coastal sea waters and for the management of industrial/agricultural pollution phenomena. A specific flight was realized on September 30, 1999 using a hyperspectral MIVIS sensor that collected data in 102 spectral channels between 0.43 and 12.7 micrometers . Hyperspectral aerial images have been processed in order to obtain updated and accurate water quality maps. Furthermore important information on bathymetry, sea bottom features and hydrodynamic circulation have been derived from image processing and on-site surveys. The obtained information layers have been inserted in a specific GIS database and integrated with further information. The processing of data layers was performed, using a dedicated software, through typical GIS operators like indexing, recording, matrix analysis, proximity analysis. The interactions between sea water, industrial installations, agricultural areas, water resources, urban settlements and natural risks have been analyzed. This allowed the creation and processing of different thematic layers like quality, vulnerability, risk and impact maps.

  6. High-resolution accurate mass spectrometry as a technique for characterization of complex lysimeter leachate samples.

    Science.gov (United States)

    Hand, Laurence H; Marshall, Samantha J; Saeed, Mansoor; Earll, Mark; Hadfield, Stephen T; Richardson, Kevan; Rawlinson, Paul

    2016-06-01

    Lysimeter studies can be used to identify and quantify soil degradates of agrochemicals (metabolites) that have the potential to leach to groundwater. However, the apparent metabolic profile of such lysimeter leachate samples will often be significantly more complex than would be expected in true groundwater samples. This is particularly true for S-metolachlor, which has an extremely complex metabolic pathway. Consequently, it was not practically possible to apply a conventional analytical approach to identify all metabolites in an S-metolachlor lysimeter study, because there was insufficient mass to enable the use of techniques such as nuclear magnetic resonance. Recent advances in high-resolution accurate mass spectrometry, however, allow innovative screening approaches to characterize leachate samples to a greater extent than previously possible. Leachate from the S-metolachlor study was screened for accurate masses (±5 ppm of the nominal mass) corresponding to more than 400 hypothetical metabolite structures. A refined list of plausible metabolites was constructed from these data to provide a comprehensive description of the most likely metabolites present. The properties of these metabolites were then evaluated using a principal component analysis model, based on molecular descriptors, to visualize the entire chemical space and to cluster the metabolites into a number of subclasses. This characterization and principal component analysis evaluation enabled the selection of suitable representative metabolites that were subsequently used as exemplars to assess the toxicological relevance of the leachate as a whole. Environ Toxicol Chem 2016;35:1401-1412. © 2015 SETAC. PMID:26627902

  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. Determination of 36Cl/Cl ratio in ground water using the accelerator mass spectrometry technique

    International Nuclear Information System (INIS)

    The Accelerator Mass Spectrometry (AMS) programme using the 14 MV Pelletron Accelerator at Mumbai has been initiated with major emphasis on the determination of 36Cl in water samples, of interest to hydrology and environment. In order to carry out the AMS measurement, a beam chopper to cut down beam intensity by a factor of 20 has been developed and commissioned. A multi-anode gas -si detector has been built to separate 36Cl from the interfering 36S. A new TPS system has been procured to operate the machine in the GVM mode. Standard and blank samples from Prime lab, Purdue have been employed in these measurements to standardise the technique for 36Cl/Cl ratio determination. The detector was calibrated using the stable 35,37Cl ions. The background 36Cl in the system has been measured using the blank sample from Purdue and it was estimated that the ratio of 36Cl/Cl was of the order of 10-13 in the present setup. Ground water samples collected from South India were converted to AgCl and put in the SNICS ion source for the AMS measurements. These ground water samples, with 14C content estimated to be in the range of 1 to 4 pMC indicate that the samples may be more than 35,000 years old. Using the AMS technique we have determined the 36Cl/Cl ratio values for these ground water samples. They are found to range between 2 to 5 x 10-12. Additional measurements are planned to determine the age of the water samples and to understand the reasons for the observed high values of 36Cl in these samples. (author)

  9. The radioactivity measurements in soils and fertilizers using gamma spectrometry technique

    International Nuclear Information System (INIS)

    Because of their mineral content, soils are naturally radioactive and one of the sources of radioactivity other than those of natural origin is mainly due to the extensive use of fertilizers. The main aim of this paper is to evaluate the fluxes of natural radionuclides in local production of phosphate fertilizers to determine the content of radioactivity in several commercial fertilizers produced in Algeria and to estimate their radiological impact in a cultivated soil even for the long-term exposure due to their application. For these purposes, virgin and fertilized soils were collected from outlying Setif region in Algeria and from phosphate fertilizers used in this area. Gamma spectrometry was exploited to determine activity concentration due to naturally occurring 226Ra, 232Th and 40K in five types of samples (two different sorts of fertilizers, virgin and fertilized soils and well water used for irrigation) taken from Setif's areas. The results show that these radionuclides were present in an average concentration of 134.7 ± 24.1, 131.8 ± 16.7, 11644 ± 550 Bq/kg for the first fertilizer NPK and 190.3 ± 30, 117.2 ± 10.3, 5312 ± 249 Bq/kg for the second fertilizer (NPKs). For the virgin and the fertilized soils, the corresponding values were respectively 47.01 ± 7.3, 33 ± 7, 329.4 ± 19.7 Bq/kg and 53.2 ± 10.6, 50.0 ± 7, 311.4 ± 18.7 Bq/kg. For well water, the values were 1.93 and 0.12 Bq/kg; however the third value was below the Minimum Detectable Activity (MDA). The radium equivalent activity (Raeq) and the representative level index Iγr for all samples were also calculated. The data were discussed and compared with those given in the literature. - Highlights: → We analyze radioactivity in Fertilizers and agricultural soils using Gamma spectrometry technique. → The activity concentration of naturally occurring radionuclides in soil samples were within the world average. → The fertilizer samples show much higher concentrations.

  10. Use of Atomic and Nuclear Techniques in Elemental and Isotopic Analysis

    International Nuclear Information System (INIS)

    This book is divided into four chapters which were presented by six authors of the best Arab specialists who have used the atomic and nuclear techniques for a long time and recognized their importance and capabilities in scientific researches. Atomic and Nuclear techniques are very successful in the field of analysis because they are the only way to proceed the analysis process with the requested accuracy and they are the cheapest at the same time. A number of these techniques were collected in this book on the basis of their accuracy and the abundance of using them in the analysis of material components, specially when these elements exist with insignificant percentage as in the case of poisons science, archaeology, nutrition, medicine and other applications.

  11. Development of a 2D temperature measurement technique for combustion diagnostics using 2-line atomic fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Engstroem, Johan

    2001-01-01

    The present thesis is concerned with the development and application of a novel planar laser-induced fluorescence (PLIF) technique for temperature measurements in a variety of combusting flows. Accurate measurement of temperature is an essential task in combustion diagnostics, since temperature is one of the most fundamental quantities for the characterization of combustion processes. The technique is based on two-line atomic fluorescence (TLAF) from small quantities of atomic indium (In) seeded into the fuel. It has been developed from small-scale experiments in laboratory flames to the point where practical combustion systems can be studied. The technique is conceptually simple and reveals temperature information in the post-flame regions. The viability of the technique has been tested in three extreme measurement situations: in spark ignition engine combustion, in ultra-lean combustion situations such as lean burning aero-engine concepts and, finally, in fuel-rich combustion. TLAF was successfully applied in an optical Sl engine using isooctane as fuel. The wide temperature sensitivity, 700 - 3000 K, of the technique using indium atoms allowed measurements over the entire combustion cycle in the engine to be performed. In applications in lean combustion a potential problem caused by the strong oxidation processes of indium atoms was encountered. This limits measurement times due to deposits of absorbing indium oxide on measurement windows. The seeding requirement is a disadvantage of the technique and can be a limitation in some applications. The results from experiments performed in sooting flames are very promising for thermometry measurements in such environments. Absorption by hydrocarbons and other native species was found to be negligible. Since low laser energies and low seeding concentrations could be used, the technique did not, unlike most other incoherent optical thermometry techniques, suffer interferences from LII of soot particles or LIF from PAH

  12. Atoms

    International Nuclear Information System (INIS)

    Completed by recent contributions on various topics (atoms and the Brownian motion, the career of Jean Perrin, the evolution of atomic physics since Jean Perrin, relationship between scientific atomism and philosophical atomism), this book is a reprint of a book published at the beginning of the twentieth century in which the author addressed the relationship between atomic theory and chemistry (molecules, atoms, the Avogadro hypothesis, molecule structures, solutes, upper limits of molecular quantities), molecular agitation (molecule velocity, molecule rotation or vibration, molecular free range), the Brownian motion and emulsions (history and general features, statistical equilibrium of emulsions), the laws of the Brownian motion (Einstein's theory, experimental control), fluctuations (the theory of Smoluchowski), light and quanta (black body, extension of quantum theory), the electricity atom, the atom genesis and destruction (transmutations, atom counting)

  13. 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

  14. Matrix elimination method for the determination of precious metals in ores using electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Poly(N-(hydroxymethyl)methacrylamide)-1-allyl-2-thiourea) hydrogels, poly(NHMMA-ATU), were synthesized by gamma radiation using 60Co γ source in the ternary mixture of NHMMA-ATU-H2O. 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 3 M 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

  15. EVALUATION OF CORROSION OF ENGINEERING CERAMICS BY ATOMIC EMISSION SPECTROMETRY IN INDUCTIVELY COUPLED PLASMA

    OpenAIRE

    DAGMAR GALUSKOVÁ; DUŠAN GALUSEK; PAVOL ŠAJGALÍK

    2014-01-01

    An analytical method has been developed and verified, facilitating chemical analysis of saline aqueous solutions from corrosion tests of two types of engineering ceramics, i.e. polycrystalline alumina, and silicon nitride. The method is capable of providing complementary information related to mechanisms of corrosion and kinetics of dissolution of the two main components of the ceramics, i.e. Al in α-Al2O3, and Si in Si3N4. A radially viewed inductively coupled plasma atomic emission spectros...

  16. Emerging techniques in vegetable oil analysis using stable isotope ratio mass spectrometry

    Directory of Open Access Journals (Sweden)

    Rhodes, Christopher

    2002-03-01

    Full Text Available As the practice of vegetable oil adulteration becomes more sophisticated, the possibility to subvert detection using established techniques such as capillary gas chromatography is increasing. One of the most powerful techniques to be used in food authenticity studies is stable isotope ratio mass spectrometry (SIRMS which utilises differences in the natural abundance of the stable isotopes of the ‘light’ bio-elements hydrogen, nitrogen, carbon, oxygen and sulfur to detect food fraud. SIRMS has found application in the authentication of a wide range of foodstuffs, including fruit juices, wines, spirits, honey and to detect the adulteration of flavour compounds with synthetic analogues. This papers reviews the current state-of-the-art for the authentication of vegetable oils using SIRMS and highlights emergent techniques such as compound- and position specific-isotope mass spectrometry. These latter developments offer the potential to provide more rapid and improved detection of the economic adulteration of vegetable oils.A medida que la práctica de la adulteración de aceites vegetales se hace más sofisticada, las posibilidades de evitar la detección utilizando técnicas tradicionales como la cromatografía de gases en columna capilar aumentan. Una de las técnicas más poderosas que más se utilizan en los estudios de autentificación de alimentos es la espectrometría de masas de relaciones isotópicas, que utiliza diferencias en la abundancia natural de isótopos estables de elementos ligeros biológicos hidrógeno, nitrógeno, carbón, oxigeno y azufre para detectar fraude en los alimentos. La espectrometría de masas de relaciones isotópicas ha encontrado aplicación en la autentificación de una amplia gama de alimentos, incluyendo zumos de frutas, vinos, bebidas alcohólicas de alta graduación, miel, y en la detección de la adulteración de los compuestos aromáticos con sus análogos de origen sintético. Este trabajo

  17. Determination of selenium in blood serum by inductively coupled plasma atomic emission spectrometry with pneumatic nebulization

    Energy Technology Data Exchange (ETDEWEB)

    Machat, Jiri; Kanicky, Viktor; Otruba, Vitezslav [Laboratory of Plasma Sources for Chemical Analysis-Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University Brno (Czech Republic)

    2002-02-01

    The possibility of determining selenium in blood serum using inductively coupled plasma emission spectrometry with conventional pneumatic nebulization was studied. A high-resolution spectrometer (SBW=6 pm) with laterally viewed ICP was employed. Analysis with conventional pneumatic nebulization could overcome laborious and demanding digestion, which is necessary for hydride generation. A pressure digestion with nitric acid at 160 C was sufficient to decrease the carbon content in the serum sample to 5%-10% of its original value. Spectral interference of the CN band was observed and mathematically corrected. It was found that the carbon-induced selenium line emission enhancement occurred even under ICP optimized conditions. A method of determination was developed and applied to the analysis of blood serum. True limit of detection in real samples is 0.01-0.02 mg/L and the limit of quantification (RSD 10%) is 0.03-0.07 mg/L using Se I 196.090 nm line at an integration time of 10-2 s. The method was tested by analysis of porcine blood serum and the serum reference material Seronorm MI 0181. (orig.)

  18. 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

  19. An investigation of polarized atomic photofragments using the ion imaging technique

    Energy Technology Data Exchange (ETDEWEB)

    Bracker, A.S.

    1997-12-01

    This thesis describes measurement and analysis of the recoil angle dependence of atomic photofragment polarization (atomic v-J correlation). This property provides information on the electronic rearrangement which occurs during molecular photodissociation. Chapter 1 introduces concepts of photofragment vector correlations and reviews experimental and theoretical progress in this area. Chapter 2 described the photofragment ion imaging technique, which the author has used to study the atomic v-J correlation in chlorine and ozone dissociation. Chapter 3 outlines a method for isolating and describing the contribution to the image signal which is due exclusively to angular momentum alignment. Ion imaging results are presented and discussed in Chapter 4. Chapter 5 discusses a different set of experiments on the three-fragment dissociation of azomethane. 122 refs.

  20. 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

    vehicle for reproducible sample presentation to the AAS instrument, as a means for facilitating conversion techniques for determination of anions, for allowing on-line preconcentration procedures via incorporated column reactors or via (co)precipitation, for exploiting kinetic discrimination schemes in...

  1. Method development for the determination of iron in milligram amounts of rice plants (Oryza sativa L.) from cultivation experiments using graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Marcia M.; Vale, Maria Goreti R.; Damin, Isabel C. Ferreira [Instituto de Quimica, Universidade Federal do Rio Grande do Sul (UFRGS), Av. Bento Goncalves 9500, 91501-970, Porto Alegre RS (Brazil); Welz, Bernhard [Departamento de Quimica, Universidade Federal de Santa Catarina (UFSC), 88040-900, Florianopolis SC (Brazil); Mandaji, Marcos; Fett, Janette P. [Departamento de Botanica e Centro de Biotecnologia, Instituto de Biociencias, Universidade Federal do Rio Grande do Sul (UFRGS), Av. Bento Goncalves 9500, 91501-970, Porto Alegre RS (Brazil)

    2003-09-01

    The amount of sample that is available for analysis in laboratory plant cultivation experiments is usually very limited. Highly sensitive analytical techniques are therefore required, even for elements that are present in the plants at mg g{sup -1} concentrations, and graphite furnace atomic absorption spectrometry (GFAAS) was chosen in this work because of its micro-sampling capability, and its relatively simple operation. Four micro-methods were investigated for the determination of iron in roots and leaves of rice plants: (i) a micro-digestion with nitric and hydrochloric acids, (ii) a slurry procedure using tetramethylammonium hydroxide (TMAH) tissue solubilizer, (iii) a slurry prepared in 1.4 mol L{sup -1} nitric acid, and treated in an ultrasonic bath, and (iv) the direct analysis of solid samples. The micro-digestion was suffering from high blank values and contamination problems, so that it could not be recommended for routine purposes. The TMAH method exhibited poor precision and occasional low recoveries, particularly for real samples. Direct solid sampling analysis gave results similar to those obtained with the slurry technique with ultrasonic agitation for the determination of iron in certified reference materials with iron content up to about 100 {mu}g g{sup -1}, but was too sensitive for the investigated rice plants, which had an iron content up to several mg g{sup -1}. The slurry technique with ultrasonic treatment of the samples, suspended in dilute nitric acid, was finally adopted as the method of choice. The method was then applied for the determination of iron in the leaves and in different compartments of the roots of two rice cultivars, one sensitive to iron toxicity, an important nutritional disorder, and the other one resistant to iron toxicity. The results suggest that the higher resistance to iron toxicity of the second cultivar is due to a smaller uptake of iron from the soil, resulting in lower iron levels in all compartments of the

  2. Ionizing radiation effects in Acai oil analysed by gas chromatography coupled to mass spectrometry technique

    International Nuclear Information System (INIS)

    The Acai fruit is a well know Brazilian seed plant used in large scale as a source of feed stock, specially in the Brazilian North-east region. The Acai oil is use in many purposes from fuel sources to medicine. The scope of this paper is to analyzed the chemical structures modification of the acai oil after the ionizing radiation. The radiation were set in the range of 10 to 25 kGy in the extracted Acai oil. The analyses were made by gas chromatography coupled to mass spectrometry techniques. A GC/MS Shimatzu QP-5000 equipped with 30 meters DB-5 capillary column with internal diameter of 0.25 mm and 0.25 μm film thickness was used. Helium was used as carried gas and gave a column head pressure of 12 p.s.i. (1 p.s.i. = 6894.76 Pa) and an average flux of 1 ml/min. The temperature program for the GC column consisted of a 4-minutes hold at 75 deg C, a 15 deg C /min ramp to 200 deg C, 8 minutes isothermal. 20 deg C/min ramp to 250 deg C, 2 minutes isothermal. The extraction of the fatty acids was based on liquid-liquid method using chloroform as solvent. The chromatograms resulted shows the presences of the oleic acid and others fatty acids identify by the mass spectra library (NIST-92). The ionization radiation deplete the fatty acids presents in the Acai oil. Details on the chemical qualitative analytical is present as well in this work. (author)

  3. Ionizing radiation effects in Acai oil analysed by gas chromatography coupled to mass spectrometry technique

    Energy Technology Data Exchange (ETDEWEB)

    Valli, Felipe; Fernandes, Carlos Eduardo; Moura, Sergio; Machado, Ana Carolina; Furasawa, Helio Akira; Pires, Maria Aparecida Faustino; Bustillos, Oscar Vega [Instituto de Pesquisas Energeticas e Nucleares (IPEN-CNEN/SP), Sao Paulo, SP (Brazil)], E-mail: ovega@ipen.br

    2007-07-01

    The Acai fruit is a well know Brazilian seed plant used in large scale as a source of feed stock, specially in the Brazilian North-east region. The Acai oil is use in many purposes from fuel sources to medicine. The scope of this paper is to analyzed the chemical structures modification of the acai oil after the ionizing radiation. The radiation were set in the range of 10 to 25 kGy in the extracted Acai oil. The analyses were made by gas chromatography coupled to mass spectrometry techniques. A GC/MS Shimatzu QP-5000 equipped with 30 meters DB-5 capillary column with internal diameter of 0.25 mm and 0.25 {mu}m film thickness was used. Helium was used as carried gas and gave a column head pressure of 12 p.s.i. (1 p.s.i. = 6894.76 Pa) and an average flux of 1 ml/min. The temperature program for the GC column consisted of a 4-minutes hold at 75 deg C, a 15 deg C /min ramp to 200 deg C, 8 minutes isothermal. 20 deg C/min ramp to 250 deg C, 2 minutes isothermal. The extraction of the fatty acids was based on liquid-liquid method using chloroform as solvent. The chromatograms resulted shows the presences of the oleic acid and others fatty acids identify by the mass spectra library (NIST-92). The ionization radiation deplete the fatty acids presents in the Acai oil. Details on the chemical qualitative analytical is present as well in this work. (author)

  4. 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

  5. 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

  6. 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

  7. Analysis of Si3N4 ultra fine powder using high-pressure acid digestion and slurry injection in inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Si3N4 powder has been analyzed by inductively coupled plasma atomic emission spectrometry (ICP-AES). The sample was dissolved by high-pressure acid digestion with HF, H2SO4 (1+1), and HNO3 mixture. This technique is well suited for the impurity analysis of Si3N4 because the matrix interference is eliminated. A round robin samples trace elements, such as Ca, W, Co, Al, Fe, Mg, and Na, were determined. For the direct analysis, slurry nebulization of 0.96 mm Si3N4 powder also has been studied by ICP-AES. Emission intensities of Fe were measure as ICP operational conditions were changed. Significant signal difference between slurry particles and aqueous solution was observed in the present experiment. Analytical results of slurry injection and high-pressure acid digestion were compared. For the use of aqueous standard solution for calibration, k-factor was determined to be 1.71 for further application

  8. Preconcentrative separation of chromium(III) species from chromium(VI) by cloud point extraction and determination by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    We describe a high-throughput technique for the determination of chromium species in water samples by flame atomic absorption spectrometry (FAAS) after preconcentrative separation of Cr(III) species from Cr(VI) by cloud point extraction (CPE) using diethyldithiocarbamate (DDTC) as the chelating agent and the nonionic surfactant Triton X-100 as the extractant. The Cr(III)-DDTC complex is extracted if the temperature is higher than the CPE temperature of Triton X-100, while Cr(VI) remains in the aqueous phase. The Cr(III) in the surfactant phase was analyzed by FAAS, and the concentration of Cr(VI) was calculated by subtraction of Cr(III) from total chromium which was directly determined by FAAS. The effect of pH, concentration of chelating agent, surfactant, and equilibration temperature were investigated. The detection limit for Cr(III) was 0. 08 μg L-1with an enrichment factor of 98, and the relative standard deviation was 1. 2% (n = 3, c = 100 μg L-1). A certified reference material and several water samples were analyzed with satisfactory results. (author)

  9. Application of l-cystine modified zeolite for preconcentration and determination of ultra-trace levels of cadmium by flame atomic absorption spectrometry.

    Science.gov (United States)

    Rezvani, Seyyed Ahmad; Soleymanpour, Ahmad

    2016-03-01

    A very convenient, sensitive and precise solid phase extraction (SPE) system was developed for enrichment and determination of ultra-trace of cadmium ion in water and plant samples. This method was based on the retention of cadmium(II) ions by l-cystine adsorbed in Y-zeolite and carry out in a packed mini-column. The retained cadmium ions then were eluted and determined by flame atomic absorption spectrometry. The scanning electron microscopy (SEM), powder X-ray diffraction (XRD) and Fourier Transform Infrared (FT-IR) spectroscopy techniques were applied for the characterization of cystine modified zeolite (CMZ). Some experimental conditions affecting the analytical performance such as pH, eluent type, concentration of sample, eluent flow rate and also the presence of interfering ions were investigated. The calibration graph was linear within the range of 0.1-7.5ngmL(-1) and limit of detection was obtained 0.04ngmL(-1) with the preconcentration factor of 400. The relative standard deviation (RSD) was obtained 1.4%, indicating the excellent reproducibility of this method. The proposed method was successfully applied for the extraction and determination of cadmium(II) ion in black tea, cigarette's tobacco and also various water samples. PMID:26852265

  10. Method development for the determination of calcium, copper, magnesium, manganese, iron, potassium, phosphorus and zinc in different types of breads by microwave induced plasma-atomic emission spectrometry.

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2016-06-01

    A novel method was developed for the determination of calcium, magnesium, potassium, iron, copper, zinc, and manganese and phosphorous in various kinds of breads samples sold in Turkey by microwave plasma-atomic emission spectrometry (MIP-AES). Breads were dried at 100 °C for one day, ground thoroughly and then digested using nitric acid/hydrogen per oxide (3:1). The analytes in certified reference wheat flour and maize flour samples were determined in the uncertainty limits of the certified values as well as the analytes added to the mixture of ground bread and acid mixture prior to digestion were recovered quantitatively (>90%). Therefore, all determinations were made by linear calibration technique using aqueous standards. The LOD values for Ca, Cu, Fe, K, Mg, Mn, P and Zn were 13.1, 0.28, 4.47, 118, 1.10, 0.41, 7550 and 3.00 ng mL(-1), respectively. No spectral interference was detected at the working wavelengths of the analytes. PMID:26830585

  11. Direct determination of arsenic and antimony in naphtha by electrothermal atomic absorption spectrometry with microemulsion sample introduction and iridium permanent modifier

    Energy Technology Data Exchange (ETDEWEB)

    Cassella, Ricardo J. [Departamento de Quimica Analitica, Universidade Federal Fluminense, Outeiro de Sao Joao Batista s/n, Centro, 24020-007, Niteroi/RJ (Brazil); Barbosa, Bruno Alberto R.S.; Santelli, Ricardo E. [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro de Sao Joao Batista s/n, Centro, 24020-007, Niteroi/RJ (Brazil); Rangel, Alessandra T. [PETROBRAS, CENPES, PDEDS/QM, Rio de Janeiro (Brazil)

    2004-05-01

    This paper reports the determination of arsenic and antimony in naphtha by employing electrothermal atomic absorption spectrometry (ETAAS) as the analytical technique. In order to promote the direct determination of the analytes in the very volatile naphtha, the formation of a microemulsion with different surfactants (Triton X-100 and Brij-35) and different chemical modification strategies were tested. The results indicated that Triton X-100 is the best emulsification agent for naphtha in both As and Sb determination when it is employed at a concentration of 1% w/v in the microemulsion. Under these conditions, the microemulsion was stabile for at least 2 h. By using Brij-35 it was possible to achieve good stability only in the first 15 min. Among all chemical modification approaches investigated (Ir permanent modifier, W-Ir permanent modifier, and Pd modifier), the Ir permanent modifier provided better sensitivity for both analytes and allowed a higher pyrolysis temperature, which decreased the background signals at lower levels. Under the best conditions established in this work, an RSD of 4.6% (20 {mu}g L{sup -1}) and a detection limit of 2.7 {mu}g L{sup -1} were observed for arsenic. For antimony, an RSD of 4.0% (20 {mu}g L{sup -1}) and a detection limit of 2.5 {mu}g L{sup -1} were obtained. The accuracy of the procedure was assessed by analyzing spiked samples of naphtha from different origins. (orig.)

  12. 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

  13. Determination of the species generated in atmospheric-pressure laser-induced plasmas by mass spectrometry techniques

    CERN Document Server

    Valle, F; Apiñaniz, J I; Carpentier, A V; Albaneda, M Sánchez; Roso, L; Raposo, C; Padilla, C; Conde, A Peralta

    2015-01-01

    We present temporal information obtained by mass spectrometry techniques about the evolution of plasmas generated by laser filamentation in air. The experimental setup used in this work allowed us to study not only the dynamics of the filament core but also of the energy reservoir that surrounds it. Furthermore, valuable insights about the chemistry of such systems like the photofragmentation and/or formation of molecules were obtained. The interpretation of the experimental results are supported by PIC (particle in cell) simulations.

  14. Characterization of phenolic compounds using separation techniques coupled to mass spectrometry of plant extracts with demonstrated bioactivity

    OpenAIRE

    Iswaldi, Ihsan

    2012-01-01

    This doctoral thesis, entitled "Characterization of phenolic compounds using separation techniques coupled to mass spectrometry of plant extracts with demonstrated bioactivity", consists of two main sections: the Introduction and the Experimental Section. The first section describes an overview of traditional medicine and functional food, plant foods as natural source of bioactive compounds, polyphenols and bioactivity and the analytical tools used to identify polyphenols such as high-pe...

  15. Determination of the species generated in atmospheric-pressure laser-induced plasmas by mass spectrometry techniques

    Science.gov (United States)

    Valle Brozas, F.; Salgado, C.; Apiñaniz, J. I.; Carpentier, A. V.; Sánchez Albaneda, M.; Roso, L.; Raposo, C.; Padilla, C.; Peralta Conde, A.

    2016-05-01

    We present temporal information obtained by mass spectrometry techniques about the evolution of plasmas generated by laser filamentation in air. The experimental setup used in this work allowed us to study not only the dynamics of the filament core but also the energy reservoir that surrounds it. Furthermore, valuable insight into the chemistry of systems such as the photofragmentation and/or formation of molecules was obtained. The interpretation of the experimental results are supported by PIC (particle in cell) simulations.

  16. Speciation of mercury in fish samples by flow injection catalytic cold vapour atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Highlights: ► Successful speciation of inorganic and organic Hg with Fe3+, Cu2+ and thiourea as catalysts. ► Best sensitivity enhancement and similar sensitivity for MeHg and Hg2+ with Fe3+. ► Successful use of Hg2+ as the primary standard for quantification of inorganic and total-Hg. ► Quantitative extraction of Hg and MeHg with 2 M HCl which contained thiourea. ► Integration with FIA for rapid analysis with a sample throughput of 180 h−1. - Abstract: 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 NaBH4 were employed for mercury vapour generation from inorganic and mixture of inorganic and organic (total) Hg. The presence of Fe3+, Cu2+ and thiourea had catalytic effect on mercury vapour generation from methylmercury (MeHg) and, when together, Cu2+ and thiourea had synergistic catalytic effect on the vapour generation. Of the two metal ions, Fe3+ gave the best sensitivity enhancement, achieving the same sensitivity for MeHg and inorganic Hg2+. Due to similarity of resulting sensitivity, Hg2+ 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.

  17. Advancement and application of gas chromatography isotope ratio mass spectrometry techniques for atmospheric trace gas analysis

    Science.gov (United States)

    Giebel, Brian M.

    2011-12-01

    The use of gas chromatography isotope ratio mass spectrometry (GC-IRMS) for compound specific stable isotope analysis is an underutilized technique because of the complexity of the instrumentation and high analytical costs. However stable isotopic data, when coupled with concentration measurements, can provide additional information on a compounds production, transformation, loss, and cycling within the biosphere and atmosphere. A GC-IRMS system was developed to accurately and precisely measure delta13C values for numerous oxygenated volatile organic compounds having natural and anthropogenic sources. The OVOCs include methanol, ethanol, acetone, methyl ethyl ketone, 2-pentanone, and 3-pentanone. Guided by the requirements for analysis of trace components in air, the GC-IRMS system was developed with the goals of increasing sensitivity, reducing dead-volume and peak band broadening, optimizing combustion and water removal, and decreasing the split ratio to the IRMS. The technique relied on a two-stage preconcentration system, a low-volume capillary reactor and water trap, and a balanced reference gas delivery system. Measurements were performed on samples collected from two distinct sources (i.e. biogenic and vehicle emissions) and ambient air collected from downtown Miami and Everglades National Park. However, the instrumentation and the method have the capability to analyze a variety of source and ambient samples. The measured isotopic signatures that were obtained from source and ambient samples provide a new isotopic constraint for atmospheric chemists and can serve as a new way to evaluate their models and budgets for many OVOCs. In almost all cases, OVOCs emitted from fuel combustion were enriched in 13C when compared to the natural emissions of plants. This was particularly true for ethanol gas emitted in vehicle exhaust, which was observed to have a uniquely enriched isotopic signature that was attributed to ethanol's corn origin and use as an alternative

  18. Production of polymer particles in powder form using an atomization technique

    OpenAIRE

    Levendis, Yiannis A.; Panagiotou, Thomai; Flagan, Richard C.

    1993-01-01

    A process for producing spherical polymer particles which may be either monodisperse of a predetermined and controlled size, or polydisperse, using a liquid atomization technique. The process includes an aerosol generator to create a stream or multiple streams of liquid droplets sprayed into a thermal reactor. The aerosol generator sprays the feed solution which comprises liquid organic monomers or semi-polymerized monomers, a polymerization catalyst and optionally, a solvent, into the therma...

  19. 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.

  20. 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

  1. 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.

  2. 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)

  3. X-ray photoelectron spectroscopy study of pyrolytically coated graphite platforms submitted to simulated electrothermal atomic absorption spectrometry conditions

    Energy Technology Data Exchange (ETDEWEB)

    Ruiz, Frine [Laboratorio de Quimica Analitica, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Benzo, Zully [Laboratorio de Quimica Analitica, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Quintal, Manuelita [Laboratorio de Quimica Analitica, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Garaboto, Angel [Laboratorio de Quimica Analitica, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Albornoz, Alberto [Laboratorio de Fisicoquimica de Superficies, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela); Brito, Joaquin L. [Laboratorio de Fisicoquimica de Superficies, Centro de Quimica, Instituto Venezolano de Investigaciones Cientificas, IVIC, Apartado Postal 21827, Caracas 1020-A (Venezuela)]. E-mail: joabrito@ivic.ve

    2006-10-15

    The present work is part of an ongoing project aiming to a better understanding of the mechanisms of atomization on graphite furnace platforms used for electrothermal atomic absorption spectrometry (ETAAS). It reports the study of unused pyrolytic graphite coated platforms of commercial origin, as well as platforms thermally or thermo-chemically treated under simulated ETAAS analysis conditions. X-ray photoelectron spectroscopy (XPS) was employed to study the elements present at the surfaces of the platforms. New, unused platforms showed the presence of molybdenum, of unknown origin, in concentrations up to 1 at.%. Species in two different oxidations states (Mo{sup 6+} and Mo{sup 2+}) were detected by analyzing the Mo 3d spectral region with high resolution XPS. The analysis of the C 1s region demonstrated the presence of several signals, one of these at 283.3 eV related to the presence of Mo carbide. The O 1s region showed also various peaks, including a signal that can be attributed to the presence of MoO{sub 3}. Some carbon and oxygen signals were consistent with the presence of C=O and C-O- (probably C-OH) groups on the platforms surfaces. Upon thermal treatment up to 2900 deg. C, the intensity of the Mo signal decreased, but peaks due to Mo oxides (Mo{sup 6+} and Mo{sup 5+}) and carbide (Mo{sup 2+}) were still apparent. Thermo-chemical treatment with 3 vol.% HCl solutions and heating up to 2900 deg. C resulted in further diminution of the Mo signal, with complete disappearance of Mo carbide species. Depth profiling of unused platforms by Ar{sup +} ion etching at increasing time periods demonstrated that, upon removal of several layers of carbonaceous material, the Mo signal disappears suggesting that this contamination is present only at the surface of the pyrolytic graphite platform.

  4. Determination of total tin in silicate rocks by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Elsheimer, H.N.; Fries, T.L.

    1990-01-01

    A method is described for the determination of total tin in silicate rocks utilizing a graphite furnace atomic absorption spectrometer with a stabilized-temperature platform furnace and Zeeman-effect background correction. The sample is decomposed by lithium metaborate fusion (3 + 1) in graphite crucibles with the melt being dissolved in 7.5% hydrochloric acid. Tin extractions (4 + 1 or 8 + 1) are executed on portions of the acid solutions using a 4% solution of tricotylphosphine oxide in methyl isobutyl ketone (MIBK). Ascorbic acid is added as a reducing agent prior to extraction. A solution of diammonium hydrogenphosphate and magnesium nitrate is used as a matrix modifier in the graphite furnace determination. The limit of detection is > 10 pg, equivalent to > 1 ??g l-1 of tin in the MIBK solution or 0.2-0.3 ??g g-61 in the rock. The concentration range is linear between 2.5 and 500 ??g l-1 tin in solution. The precision, measured as relative standard deviation, is < 20% at the 2.5 ??g l-1 level and < 7% at the 10-30 ??g l-1 level of tin. Excellent agreement with recommended literature values was found when the method was applied to the international silicate rock standards BCR-1, PCC-1, GSP-1, AGV-1, STM-1, JGb-1 and Mica-Fe. Application was made to the determination of tin in geological core samples with total tin concentrations of the order of 1 ??g g-1 or less.

  5. Monte Carlo Technique Used to Model the Degradation of Internal Spacecraft Surfaces by Atomic Oxygen

    Science.gov (United States)

    Banks, Bruce A.; Miller, Sharon K.

    2004-01-01

    Atomic oxygen is one of the predominant constituents of Earth's upper atmosphere. It is created by the photodissociation of molecular oxygen (O2) into single O atoms by ultraviolet radiation. It is chemically very reactive because a single O atom readily combines with another O atom or with other atoms or molecules that can form a stable oxide. The effects of atomic oxygen on the external surfaces of spacecraft in low Earth orbit can have dire consequences for spacecraft life, and this is a well-known and much studied problem. Much less information is known about the effects of atomic oxygen on the internal surfaces of spacecraft. This degradation can occur when openings in components of the spacecraft exterior exist that allow the entry of atomic oxygen into regions that may not have direct atomic oxygen attack but rather scattered attack. Openings can exist because of spacecraft venting, microwave cavities, and apertures for Earth viewing, Sun sensors, or star trackers. The effects of atomic oxygen erosion of polymers interior to an aperture on a spacecraft were simulated at the NASA Glenn Research Center by using Monte Carlo computational techniques. A two-dimensional model was used to provide quantitative indications of the attenuation of atomic oxygen flux as a function of the distance into a parallel-walled cavity. The model allows the atomic oxygen arrival direction, the Maxwell Boltzman temperature, and the ram energy to be varied along with the interaction parameters of the degree of recombination upon impact with polymer or nonreactive surfaces, the initial reaction probability, the reaction probability dependence upon energy and angle of attack, degree of specularity of scattering of reactive and nonreactive surfaces, and the degree of thermal accommodation upon impact with reactive and non-reactive surfaces to be varied to allow the model to produce atomic oxygen erosion geometries that replicate actual experimental results from space. The degree of

  6. 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.

  7. 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.

  8. 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.

  9. 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%.

  10. 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

  11. Dithizone immobilized silica gel on-line preconcentration of trace copper with detection by flame atomic absorption spectrometry.

    Science.gov (United States)

    Yu, Hong-Mei; Song, Hua; Chen, Ming-Li

    2011-07-15

    A novel adsorbent-silica gel bound dithizone (H(2)Dz-SG) was prepared and used as solid-phase extraction of copper from complex matrix. The H(2)Dz-SG is investigated by means of FT-IR spectra and the SEM images, demonstrating the bonding of dithizone. The H(2)Dz-SG quantitatively adsorb copper ions, and the retained copper is afterwards collected by elution of 10% (v/v) nitric acid. An on-line flow injection solid-phase extraction procedure was developed for trace copper separation and preconcentration with detection by flame atomic spectrometry. By loading 5.4 mL of sample solution, a liner range of 0.5-120 μg L(-1), an enrichment factor of 42.6, a detection limit of 0.2 μg L(-1) and a precision of 1.7% RSD at the 40 μg L(-1) level (n=11) were obtained, along with a sampling frequency of 47 h(-1). The dynamic sorption capacity of H(2)Dz-SG to Cu(2+) was 0.76 mg g(-1). The accuracy of the proposed procedure was evaluated by determination of copper in reference water sample. The potential applications of the procedure for extraction of trace copper were successfully accomplished in water samples (tap, rain, snow, sea and river). The spiking recoveries within 91-107% are achieved. PMID:21645750

  12. 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)

  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. Determination of trace mercury in environmental samples by cold vapor atomic fluorescence spectrometry after cloud point extraction

    International Nuclear Information System (INIS)

    A sensitive method is presented for the determination of ultra-trace levels of mercury using cold vapor atomic fluorescence spectrometry along with cloud point extraction. Preconcentration is based on the complexation of Hg(II) by dithizone, followed by micelle-mediated extraction of the complex using the surfactant Triton X-114. Foaming, which is always observed when generating vapor mercury in the presence of surfactant, was strongly reduced by using SnCl2 as a reducing reagent, and a homemade gas-liquid separator. Variables that affect the assay were optimized. These included pH value, concentration of chelating reagent, concentration of Triton X-114, equilibration temperature and time. The preconcentration of a 45-mL sample gave an enhancement factor of 29. The calibration graph is linear in the range from 0. 05 to 5. 0 ng mL-1 with a correlation coefficient of 0. 9991. The limit of detection obtained under the optimal conditions is 5 pg mL-1. The relative standard deviation for seven replicate determinations at 0. 5 ng mL-1 level is 5. 2%. The method was successfully applied to the determination of Hg in real samples. (author)

  15. Determination of Nickel in Water and Wastewater at Ultratrace Level by Solid-Phase Extraction-Flame Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Solid-phase extraction using octadecyl silica membrane disk modified with 2[(2-mercaptophenylimino)methyl] phenol (MPMP) ligand was utilized in FAAS determination of ultratrace amount of nickel in water and wastewater samples. Ni2+ ions were adsorbed quantitatively during the passage of an aqueous sample through the modified octadecyl silica membrane disk. The retained Ni2+ ions were then eluted from the disk with 5 mL of 0.5 mol L-1 nitric acid as an eluent, and subsequently determined by FAAS. The break-through volume of the method was 2000 mL, which corresponded to the enrichment factor of 400. Maximum capacity of the membrane disk modified with 6 mg of the ligand was 210 μg of Ni2+, and the limit of determination was 0.17 μg L-1. The effect of various ionic interferences on preconcentration and determination of nickel in binary mixture was studied. The method was successfully applied to determination of nickel in water and wastewater samples; accuracy was examined in recovery experiment and by independent GFAAS analysis (graphite furnace atomic absorption spectrometry). The accuracy was further confirmed by applying the proposed method to the analysis of standard reference alloy (BCR No 112) and comparing the result with the declared value. (authors)

  16. 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.

  17. 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

  18. 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)

  19. Determination of molybdenum in plants by vortex-assisted emulsification solidified floating organic drop microextraction and flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A fast and sensitive procedure for extraction and preconcentration of molybdenum in plant samples based on solidified floating organic drop microextraction combined with flame atomic absorption spectrometry and discrete nebulization was developed. 8-Hydroxyquinoline (8-HQ) was used as complexing agent. The experimental conditions established were: 0.5% m v−1 of 8-HQ, 60 μL of 1-undecanol as the extractant phase, 2 min vortex extraction time, centrifugation for 2 min at 2000 rpm, 10 min into an ice bath and discrete nebulization by introducing 200 μL of solution. The calibration curve was linear from 0.02 to 4.0 mg L−1 with a limit of detection of 4.9 μg L−1 and an enhancement factor of 67. The relative standard deviations for ten replicate measurements of 0.05 and 1.0 mg L−1 Mo were 6.0 and 14.5%, respectively. The developed procedure was applied for determining molybdenum in corn samples and accuracy was proved using certified reference materials. - Highlights: ► Molybdenum was determined in plants by flame AAS. ► Flame AAS sensitivity was improved using microextraction and discrete nebulization. ► The developed procedure can be easily implemented in routine analysis. ► Green chemistry principles are followed

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

    Science.gov (United States)

    Daşbaşı, Teslima; Kartal, Şenol; Saçmacı, Şerife; Ülgen, Ahmet

    2016-01-01

    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). PMID:26881186

  1. 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%

  2. 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

  3. Determination of molybdenum in plants by vortex-assisted emulsification solidified floating organic drop microextraction and flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Oviedo, Jenny A.; Fialho, Lucimar L.; Nóbrega, Joaquim A., E-mail: djan@terra.com.br

    2013-08-01

    A fast and sensitive procedure for extraction and preconcentration of molybdenum in plant samples based on solidified floating organic drop microextraction combined with flame atomic absorption spectrometry and discrete nebulization was developed. 8-Hydroxyquinoline (8-HQ) was used as complexing agent. The experimental conditions established were: 0.5% m v{sup −1} of 8-HQ, 60 μL of 1-undecanol as the extractant phase, 2 min vortex extraction time, centrifugation for 2 min at 2000 rpm, 10 min into an ice bath and discrete nebulization by introducing 200 μL of solution. The calibration curve was linear from 0.02 to 4.0 mg L{sup −1} with a limit of detection of 4.9 μg L{sup −1} and an enhancement factor of 67. The relative standard deviations for ten replicate measurements of 0.05 and 1.0 mg L{sup −1} Mo were 6.0 and 14.5%, respectively. The developed procedure was applied for determining molybdenum in corn samples and accuracy was proved using certified reference materials. - Highlights: ► Molybdenum was determined in plants by flame AAS. ► Flame AAS sensitivity was improved using microextraction and discrete nebulization. ► The developed procedure can be easily implemented in routine analysis. ► Green chemistry principles are followed.

  4. Determination of molybdenum in plants by vortex-assisted emulsification solidified floating organic drop microextraction and flame atomic absorption spectrometry

    Science.gov (United States)

    Oviedo, Jenny A.; Fialho, Lucimar L.; Nóbrega, Joaquim A.

    2013-08-01

    A fast and sensitive procedure for extraction and preconcentration of molybdenum in plant samples based on solidified floating organic drop microextraction combined with flame atomic absorption spectrometry and discrete nebulization was developed. 8-Hydroxyquinoline (8-HQ) was used as complexing agent. The experimental conditions established were: 0.5% m v- 1 of 8-HQ, 60 μL of 1-undecanol as the extractant phase, 2 min vortex extraction time, centrifugation for 2 min at 2000 rpm, 10 min into an ice bath and discrete nebulization by introducing 200 μL of solution. The calibration curve was linear from 0.02 to 4.0 mg L- 1 with a limit of detection of 4.9 μg L- 1 and an enhancement factor of 67. The relative standard deviations for ten replicate measurements of 0.05 and 1.0 mg L- 1 Mo were 6.0 and 14.5%, respectively. The developed procedure was applied for determining molybdenum in corn samples and accuracy was proved using certified reference materials.

  5. 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

  6. In-situ suspended aggregate microextraction of gold nanoparticles from water samples and determination by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Choleva, Tatiana G; Kappi, Foteini A; Tsogas, George Z; Vlessidis, Athanasios G; Giokas, Dimosthenis L

    2016-05-01

    This work describes a new method for the extraction and determination of gold nanoparticles in environmental samples by means of in-situ suspended aggregate microextraction and electrothermal atomic absorption spectrometry. The method relies on the in-situ formation of a supramolecular aggregate phase through ion-association between a cationic surfactant and a benzene sulfonic acid derivative. Gold nanoparticles are physically entrapped into the aggregate phase which is separated from the bulk aqueous solution by vacuum filtration on the surface of a cellulose filter in the form of a thin film. The film is removed from the filter surface and is dissociated into an acidified methanolic solution which is used for analysis. Under the optimized experimental conditions, gold nanoparticles can be efficiently extracted from water samples with recovery rates between 81.0-93.3%, precision 5.4-12.0% and detection limits as low as 75femtomolL(-1) using only 20mL of sample volume. The satisfactory analytical features of the method along with the simplicity indicate the efficiency of this new approach to adequately collect and extract gold nanoparticle species from water samples. PMID:26946014

  7. 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%.

  8. 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.

  9. Determination of toxic elements in different brands of cigarette by atomic absorption spectrometry using ultrasonic assisted acid digestion.

    Science.gov (United States)

    Kazi, Tasneem Gul; Jalbani, Nusrat; Arain, Muhammad Balal; Jamali, Muhammad Khan; Afridi, Hassan Imran; Shah, Abdul Qadir

    2009-07-01

    In this paper, a sample preparation method based on ultrasonic assisted acid extraction (UAE) of Al, As, Cd, Ni and Pb from filler tobacco (FT) of different local branded (LBCs) and imported branded cigarettes (IBCs) consumed in Pakistan. Acid extracts obtained upon sonication were determined by atomic absorption spectrometry. Parameters influencing extraction such as pre-sonication time 10-15 min, sonication time 2-10 min, mass of sample 0.1-0.5 g, particle size VTL-2), and also applied a conventional acid digestion method (CDM) on same CRM, for comparative purpose. The average relative standard deviation of UAE method of CRM, ranged as 1.64-8.42% for N = 6, depending on the analytes. Extraction efficiencies for CRM were close to 97.1, 97.5, 98.5, 97.8 and 96.7 for Al, As, Cd, Ni and Pb, respectively. The concentrations of Al, As, Cd, Ni and Pb in cigarettes were present in all branded cigarettes, there is no any significance difference among LBCs and IBCs, except in few cases of LBCs, have high level of Cd and Al. Our results were compared with other worldwide studies. PMID:18600465

  10. Slurry sampling for the determination of thallium in soils and sediments by graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dobrowolski, R. [Analytical Laboratory, Faculty of Chemistry, Maria Curie-Sklodowska University, M.C. Sklodowska Sq.3, 20-031 Lublin (Poland)

    2002-12-01

    The analytical conditions for thallium determination in soils and sediments by slurry sampling graphite furnace atomic absorption spectrometry were studied and optimized. Elimination of a strong background for soils rich in organic materials by application of tungsten carbides coated graphite tubes/platforms was studied in detail. Tungsten carbides increased the maximum permissible pyrolysis temperature from 300 to 900 C. The mechanism of tungsten carbide formation on different graphite surfaces was proposed. Application of a strong basic anion-exchange resin for interference elimination in thallium determination in marine sediments was described. Calibration was performed directly using aqueous standards both for soil and sediment analysis. Analysis of CRM confirmed the reliability of the approach. The precision and accuracy of thallium determination by the described method for soils and sediments was acceptable. A characteristic mass of 13.8 pg was obtained and the limit of detection for the proposed method was around 0.06 {mu}g g{sup -1} Tl. (orig.)

  11. The determination of wear metals in used lubricating oils by flame atomic absorption spectrometry using sulphanilic acid as ashing agent.

    Science.gov (United States)

    Ekanem, E J; Lori, J A; Thomas, S A

    1997-11-01

    A simple and reliable ashing procedure is proposed for the preparation of used lubricating oil samples for the determination of calcium, magnesium, zinc, iron, chromium and nickel by flame atomic absorption spectrometry. Sulphanilic acid was added to oil samples and the mixture coked and the coke ashed at 550 degrees C. The solutions of the ash were analysed by flame AAS for the metals. The release of calcium, zinc, iron and chromium was improved by the addition of sulphanilic acid to samples. The relative standard deviations of metal concentration results in the initial oil samples were 1.5% for Ca (1500 mg l(-1) level), 0.3% for Mg (100 mg l(-1) level), 3.1% for Zn (1500 mg l(-1) level), 0.7% for Fe (500 mg l(-1) level), 0.02% for Cr (50 mg l(-1) level) and 0.002% for Ni (10 mg l(-1) level). The optimum sample size for efficient metal release was 20 g while the optimum sulphanilic acid to oil ratio was 0.05 g per gram of oil for Zn and Cr and 0.10 g for Ca and Fe. Results obtained by this procedure were highly reproducible and comparable with those obtained for the same samples using standard procedures. PMID:18966959

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

    International Nuclear Information System (INIS)

    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 ΔλInstr and the absorption line width ΔλAbs, 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. 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

  14. Microwave digestion of sludge, soil and sediment samples for metal analysis by inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Three digestion programs for the Anton Paar multiwave microwave were investigated to obtain a simple, rapid method for the determination of metals in sludge, soil and sediment samples. The digests were subsequently analysed for metal content by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The trace metals determined were Mn, Ni, Zn, Pb, Cr, Cd, Cu and V, and the major elements determined were Mg, Ca, Fe and Al. In addition to the heating programs used, different combinations and volumes of hydrofluoric, nitric and hydrochloric acids were evaluated for digestion efficiency. Three standard reference materials (SRMs) were used in the comparison. From the results obtained, the fastest microwave program (36 min) provided the most consistent recovery data for all three SRMs. Six millilitres of HNO3 was the optimum acid mixture for the digestion of LGC6136 sewage sludge (with the exception of Al) and for LGC6138 coal carbonisation site soil. For PACS-1 marine sediment (and for the determination of Al in LGC6136), a mixture of 3 ml of HNO3+2 ml of HF produced the best analytical results. The experimental results were in agreement with the certified values and demonstrated that the proposed method was precise and accurate

  15. Determination of arsenite, arsenate, monomethylarsonic acid and dimethylarsinic acid in cereals by hydride generation atomic fluorescence spectrometry

    Science.gov (United States)

    Matos Reyes, M. N.; Cervera, M. L.; Campos, R. C.; de la Guardia, M.

    2007-09-01

    A fast, sensitive and simple non-chromatographic analytical method was developed for the speciation analysis of toxic arsenic species in cereal samples, namely rice and wheat semolina. An ultrasound-assisted extraction of the toxic arsenic species was performed with 1 mol L - 1 H 3PO 4 and 0.1% (m/v) Triton XT-114. After extraction, As(III), As(V), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) concentrations were determined by hydride generation atomic fluorescence spectrometry using a series of proportional equations corresponding to four different experimental reduction conditions. The detection limits of the method were 1.3, 0.9, 1.5 and 0.6 ng g - 1 for As(III), As(V), DMA and MMA, respectively, expressed in terms of sample dry weight. Recoveries were always greater than 90%, and no species interconversion occurred. The speciation analysis of a rice flour reference material certified for total arsenic led to coherent results, which were also in agreement with other speciation studies made on the same certified reference material.

  16. Mercury determination in non- and biodegradable materials by cold vapor capacitively coupled plasma microtorch atomic emission spectrometry

    International Nuclear Information System (INIS)

    Highlights: → Use of a miniaturized analytical system with microtorch plasma for Hg determination. → Determination of Hg in non- and biodegradable materials using cold vapor generation. → Figures of merit and advantages of the miniaturized system for Hg determination. - Abstract: A new analytical system consisting of a low power capacitively coupled plasma microtorch (20 W, 13.56 MHz, 150 ml min-1 Ar) and a microspectrometer was investigated for the Hg determination in non- and biodegradable materials by cold-vapor generation, using SnCl2 reductant, and atomic emission spectrometry. The investigated miniaturized system was used for Hg determination in recyclable plastics from electronic equipments and biodegradable materials (shopping bags of 98% biodegradable polyethylene and corn starch) with the advantages of easy operation and low analysis costs. Samples were mineralized in HNO3-H2SO4 mixture in a high-pressure microwave system. The detection limits of 0.05 ng ml-1 or 0.08 μg g-1 in solid sample were compared with those reported for other analytical systems. The method precision was 1.5-9.4% for Hg levels of 1.37-13.9 mg kg-1, while recovery in two polyethylene certified reference materials in the range 98.7 ± 4.5% (95% confidence level).

  17. 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.

  18. The determination of trace elements in crude oil and its heavy fractions by atomic spectrometry

    International Nuclear Information System (INIS)

    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

  19. Simultaneous determination of cadmium, iron and tin in canned foods using high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Leao, Danilo J; Junior, Mario M S; Brandao, Geovani C; Ferreira, Sergio L C

    2016-06-01

    A method was established to simultaneously determine cadmium, iron and tin in canned-food samples using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). The quantification step has been performed using the primary line (228.802nm) for cadmium and the adjacent secondary lines (228.725nm and 228.668nm) for iron and tin, respectively. The selected chemical modifier was an acid solution that contained a mixture of 0.1% (w/v) Pd and 0.05% (w/v) Mg. The absorbance signals were measured based on the peak area using 3 pixels for cadmium and 5 pixels for iron and tin. Under these conditions, cadmium, iron and tin have been determined in canned-food samples using the external calibration technique based on aqueous standards, where the limits of quantification were 2.10ngg(-1) for cadmium, 1.95mgkg(-1) for iron and 3.00mgkg(-1) for tin, and the characteristic masses were 1.0pg for cadmium, 0.9ng for iron and 1.1ng for tin. The precision was evaluated using two solutions of each metal ion, and the results, which were expressed as the relative standard deviation (RSD%), were 3.4-6.8%. The method accuracy for cadmium and iron was confirmed by analyzing a certified reference material of apple leaves (NIST 1515), which was supplied by NIST. However, for tin, the accuracy was confirmed by comparing the results of the proposed method and another analytical technique (inductively coupled plasma optical emission spectrometry). The proposed procedure was applied to determine cadmium, iron and tin in canned samples of peeled tomato and sardine. Eleven samples were analyzed, and the analyte concentrations were 3.57-62.9ngg(-1), 2.68-31.48mgkg(-1) and 4.06-122.0mgkg(-1) for cadmium, iron and tin, respectively. In all analyzed samples, the cadmium and tin contents were lower than the permissible maximum levels for these metals in canned foods in the Brazilian legislation. PMID:27130088

  20. Flow injection on-line dilution for zinc determination in human saliva with electrothermal atomic absorption spectrometry detection

    International Nuclear Information System (INIS)

    An automated method is described for the determination of zinc in human saliva by electrothermal atomic absorption spectrometry (ET AAS) after on-line dilution of samples with a significant reduction of sample consumption per analysis (1) which allowed the introduction of 10 μL of either solution in the diluent stream. To avoid unnecessary waste of samples, the TBSI1 also permitted the recirculation of the solutions to their respective autosampler cups. The downstream diluted solution fills a home made sampling arm assembly. The sequential deposition of 20 μL aliquots of samples or standards on the graphite tube platform was carried out by air displacement with a similar time based solenoid injector (TBSI2). The dilution procedure and the injection of solutions into the atomizer are computer controlled and synchronized with the operation of the temperature program. Samples or standards solutions were submitted to two drying steps (at 90 and 130 deg. C), followed by pyrolysis and atomization at 700 and 1700 deg. C, respectively. The aqueous calibration was linear up to 120.0 μg L-1 for diluted standard solutions/samples and its slope was similar (p > 0.05) to the standard addition curve, indicating lack of matrix effect. The precision tested by repeated analysis of real saliva samples was less than 3% and the detection limit (3σ) was of 0.35 μg L-1. To test the accuracy of the proposed procedure, recovery tests were performed, obtaining mean recovery of added zinc of 97.8 ± 1.3%. Furthermore, Zn values estimated by the procedure developed in this work were compared with those obtained by a standard addition flame-AAS method applied to 20 randomly selected saliva samples. No significant differences (p > 0.05) were obtained between the two methods. Zinc levels in saliva samples from 44 healthy volunteers, 15 male and 29 female, with ages between 20 and 51 years (mean 30.50 ± 9.14 years) were in the range 22-98 μg L-1 (mean of 55 ± 17 μg L-1), similar to some

  1. 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)

  2. Atomic-absorption spectrometric, neutron-activation and radioanalytical techniques for the determination of trace metals in environmental, biochemical and toxicological research

    International Nuclear Information System (INIS)

    Radioanalytical techniques and atomic-absorption spectrometry have been used for the micro-determination of vanadium in biological specimens such as human tissues and body fluids in environmental, biochemical and toxicological research. The use of 48V as a radiotracer permitted investigations on the vaporisation and retention mechanisms of vanadium. Higher vanadium oxides are probably converted into lower oxides, decomposing to VO in gaseous form, followed by the dissociation to 'free vanadium' and oxygen. It was found that about 20% of the 48V radioactivity was consistently retained in the graphite tube after 10 repeated introductions and firings of 50 μl of 50 ng ml-148V-labelled vanadium solution. However, the amount retained, probably in the form of carbide, does not vaporise under the conditions used for the analysis. Determinations of vanadium at the parts per billion level in 10 urine samples by neutron-activation analysis and by graphite furnace atomic-absorption spectrometry showed agreement that can be considered satisfactory for practical purposes. (author)

  3. Characterization of the occupational exposure and air transported particles using the techniques of PIXE 252Cf PMDS and alpha spectrometry

    International Nuclear Information System (INIS)

    The risk for human health due to exposure to aerosols depends on the intake pattern, the mass concentration and the speciation of the elements present in airborne particles. In this work PDMS (Plasma Desorption Mass Spectrometry) was used as complementary technique to the PIXE (Particle Induced X ray Emission) technique to characterize aerosols samples collected in the environment. The PIXE technique allows the identification of the elements present in the sample and to determine their mass concentrations. The mass spectrometry (PDMS) was used to identify the speciation of these elements present in the samples. The aerosol samples were collected using a six stage cascade impactor in three sites. The Mass Median Aerodynamic Diameter (MMAD) measured indicated that the airborne particulate were in the fine fraction of the aerosols. The theoretical uranium concentration in urine samples using ICRP lung model parameters suggest that the elemental mass concentration in respirable fraction of aerosol and the chemical speciation are important factors to determine the uranium concentration in urine and that the determination of specific solubility parameters for each compound is the most important factor to calculate the uranium concentration in urine. PIXE allows to identify and quantify the elements heavier than Na (Z=11) while PDMS allows to identify the organic and inorganic compounds present in the samples. As these techniques are used as complementary techniques they provide important information about the aerosols characterization. (author)

  4. Comparison of direct sampling and emulsion analysis using a filter furnace for the determination of lead in crude oil by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    The determination of trace elements in crude oil is difficult due to the complex nature of the sample and the various different chemical forms in which the metals can occur. The advantage of graphite furnace atomic absorption spectrometry is that only a minimum of sample pretreatment is required. In this work two techniques have been compared to establish a fast and reliable method for lead determination in crude oil. In the first one the crude oil samples were weighed directly onto solid sampling (SS) platforms and introduced into the graphite tube for analysis. In the second one the samples were prepared as oil-in-water emulsions and analyzed in a filter furnace (FF). Twenty μL of a mixture of 0.5 mg L- 1 Pd + 0.3 mg L- 1 Mg + Triton X-100 has been used as the modifier, and calibration against aqueous solutions has been used for both methods. The sensitivity obtained with the FF was more than a factor of two better than that with SS; however, as a larger sample mass could be introduced in the latter case, so that the limits of detection for both techniques were 0.004 mg kg- 1. Seven crude oil samples were analyzed using the two procedures, and all results were in agreement at a 95% confidence level using a paired Student's t-test. For validation purposes, three crude oil samples have been mineralized using an open-vessel acid digestion, and the results were in agreement with those found with direct sampling and with emulsion sampling using FF according to ANOVA test. Both methods are simple, fast and reliable, being appropriated for routine analysis; however, the direct method using SS technology should be preferred because of its simplicity, speed and commercial availability.

  5. Comparison of direct sampling and emulsion analysis using a filter furnace for the determination of lead in crude oil by graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Damin, Isabel C.F.; Dessuy, Morgana B.; Castilhos, Tamara S. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre - RS (Brazil); Silva, Marcia M. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre - RS (Brazil)], E-mail: mmsilva@iq.ufrgs.br; Vale, Maria Goreti R. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre - RS (Brazil); Welz, Bernhard [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)

    2009-06-15

    The determination of trace elements in crude oil is difficult due to the complex nature of the sample and the various different chemical forms in which the metals can occur. The advantage of graphite furnace atomic absorption spectrometry is that only a minimum of sample pretreatment is required. In this work two techniques have been compared to establish a fast and reliable method for lead determination in crude oil. In the first one the crude oil samples were weighed directly onto solid sampling (SS) platforms and introduced into the graphite tube for analysis. In the second one the samples were prepared as oil-in-water emulsions and analyzed in a filter furnace (FF). Twenty {mu}L of a mixture of 0.5 mg L{sup - 1} Pd + 0.3 mg L{sup - 1} Mg + Triton X-100 has been used as the modifier, and calibration against aqueous solutions has been used for both methods. The sensitivity obtained with the FF was more than a factor of two better than that with SS; however, as a larger sample mass could be introduced in the latter case, so that the limits of detection for both techniques were 0.004 mg kg{sup - 1}. Seven crude oil samples were analyzed using the two procedures, and all results were in agreement at a 95% confidence level using a paired Student's t-test. For validation purposes, three crude oil samples have been mineralized using an open-vessel acid digestion, and the results were in agreement with those found with direct sampling and with emulsion sampling using FF according to ANOVA test. Both methods are simple, fast and reliable, being appropriated for routine analysis; however, the direct method using SS technology should be preferred because of its simplicity, speed and commercial availability.

  6. Reflection mass spectrometry technique for monitoring and controlling composition during molecular beam epitaxy

    Science.gov (United States)

    Brennan, Thomas M.; Hammons, B. Eugene; Tsao, Jeffrey Y.

    1992-01-01

    A method for on-line accurate monitoring and precise control of molecular beam epitaxial growth of Groups III-III-V or Groups III-V-V layers in an advanced semiconductor device incorporates reflection mass spectrometry. The reflection mass spectrometry is responsive to intentional perturbations in molecular fluxes incident on a substrate by accurately measuring the molecular fluxes reflected from the substrate. The reflected flux is extremely sensitive to the state of the growing surface and the measurements obtained enable control of newly forming surfaces that are dynamically changing as a result of growth.

  7. Measurement of copper in biological samples by flame or electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Evenson, M A

    1988-01-01

    Guidelines presented here allow for copper analysis of biological materials by methods that are very sensitive, that require little sample preparation, that have few chemical or spectral interferences, that are inexpensive, and that require only usual care in contamination control. The commercial instruments for FAAS and ETAAS from Perkin-Elmer, from Varian, and from Instrumentation Laboratories Inc. (Allied Analytical Systems) all work well in either the flame or the flameless mode. Background correction techniques are not essential for copper analysis if care is taken with the sample preparation to minimize the background signals. Different types of burners will work adequately if one makes certain that the viscosity of the sample and the control products are similar to the calibration standards. Further, dilution of samples is preferred over increasing the viscosity of the calibration standards by the addition of a protein containing solution or a substance such as glycerol. A 1:10 dilution of blood plasma or serum with dilute nitric acid or water is all that is necessary for copper analysis by the FFAS methods. Cation and anion effects should be tested by bracketing the concentrations of the ions found in the sample with known amounts of ions in the sample solutions. Increasing the concentrations of the ions thought to interfere while keeping the copper concentration constant is another way to test for ion interferences.(ABSTRACT TRUNCATED AT 250 WORDS) PMID:3374386

  8. Infrared laser ablation study of pressed soil pellets with inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mikolas, J.; Musil, P.; Stuchlikova, V.; Novotny, K.; Otruba, V.; Kanicky, V. [Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University Brno, Kotlarska 2, 61137 Brno (Czech Republic)

    2002-09-01

    Potential of infrared laser ablation (LA) coupled with ICP-AES as a technique suitable for the determination of trace elements (Zn, Cu, Ni, Cr, and V) in agricultural soils was studied. Operating parameters such as laser beam energy, laser beam focusing with respect to the sample surface, and velocity of the sample translation in the plane perpendicular to the laser beam were optimized. Soil samples were mixed with powdered Ag as a binder, and an internal standard (GeO{sub 2}), and pressed into pellets. Calibration samples were prepared by adding known amounts of oxides of elements of interest into soils of known elemental composition and then processed in the same way as the analyzed samples. Calibration curves were found to be linear at least up to several hundreds of mg kg{sup -1} for the elements of interest. The elemental contents obtained by using LA-ICP-AES were compared with those obtained by analysis using wet chemistry followed by ICP-AES with pneumatic nebulization (PN). The results were in good agreement. Accuracy was also tested using certified reference soils with a bias not exceeding 10% relative. (orig.)

  9. Solid sampling in analysis of animal organs by two-jet plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    A study of high-power two-jet plasma capabilities for the direct multi-elemental analysis of animal organs was undertaken. The experimental conditions chosen allow the direct analysis of different animal organs after drying and grinding to powder (particle size 20–200 μm). It was found that evaporation efficiency of the samples depends on the particle size and thermal stability of tissues and can be improved by reduction of a carrier gas flow. Calibration samples based on graphite powder and a tenfold dilution of powdered samples with buffer (graphite powder containing 15% NaCl) were used. 5–10 mg of the sample was quite enough to get the detection limits of elements at the level of 0.1–10 μg g−1. A prior carbonization procedure (not ashing) makes it possible to decrease the detection limits of elements by an order of magnitude. The validation of the techniques was confirmed by the analysis of certified reference materials NIST 8414, BCR 278R and NCS ZC 81001 as well as by using different sample preparation procedures. - Highlights: ► A two-jet plasma was used for direct analysis of powdered animal organs. ► The analysis of powders with particles 20–200 μm in size was possible. ► Calibration samples based on graphite powder were used. ► Carbonization of the sample allows decreasing detection limits of elements.

  10. 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.

  11. 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.

  12. Volatile organo-selenium speciation in biological matter by solid phase microextraction–moderate temperature multicapillary gas chromatography with microwave induced plasma atomic emission spectrometry detection

    OpenAIRE

    Dietz, Christian; Sanz Landaluze, Jon; Ximenez Embun, Pilar; Madrid Albarrán, Yolanda; Cámara, Carmen

    2004-01-01

    Microwave induced plasma atomic emission spectrometry (MIP-AES) in combination with multicapillary (MC) gas chromatography could be proven to be useful for element specific detection of volatile species. Solid phase microextraction (SPME) was used for preconcentration and sample-matrix separation. The fiber desorption unit as well as the heating control for the MCcolumn were in-house developed and multicapillary column was operated at moderate temperatures (30–100 ◦C). The method was...

  13. 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...

  14. 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...

  15. 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 ...

  16. 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...

  17. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Urine Samples by Isotope Ratio Mass Spectrometry

    International Nuclear Information System (INIS)

    The IAEA has fostered the more widespread use of a stable isotope technique to assess body composition in different population groups to address priority areas in public health nutrition in Member States. It has done this by supporting national and regional nutrition projects through its technical cooperation programme and coordinated research projects over many years. This publication was developed by an international group of experts to provide practical hands-on guidance in the use of this technique in settings where analysis of stable isotope ratios in biological samples is to be made by isotope ratio mass spectrometry. The publication is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical applications of state of the art methodologies to monitor changes in body composition can be found in IAEA Human Health Series No. 3, Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques

  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

    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.

  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

    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

  20. Identification of celiac-related proteins by combination of separation techniques and mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Šalplachta, Jiří; Chmelík, Josef

    Pardubice: Univerzita Pardubice, 2005 - (Jandera, P.). s. 232 ISBN 80-7194-771-7. [International Symposium on Separation Sciences (ISSS 2005) /11./. 12.09.2005-14.09.2005, Pardubice] R&D Projects: GA MŠk 1M0570 Keywords : mass spectrometry * celiac disease * gluten Subject RIV: CB - Analytical Chemistry, Separation

  1. Ion storage techniques and time-of-flight mass spectrometry in physical forensic science

    Energy Technology Data Exchange (ETDEWEB)

    Chambers, D M; Grace, L I

    2000-06-27

    Effective investigative analysis requires proper selection of sample-collection procedures, preservation, and analysis methods. To achieve these objectives it is essential to tailor the collection and analysis methods to the application requirements, which are constrained by different parameters such as analysis time, sample concentration, matrix interferences, and analyte stability (e.g., surface activity (''stickiness'') and chemical reactivity). In addition, method optimization must be accomplished without compromising sample integrity. Maintaining sample integrity requires minimizing and characterizing contamination as well as reducing sample degradation and loss to prevent both false positive and negative detection, respectively. When specific constraints are defined, depending on target chemical(s) and application scenarios, it is sometimes necessary to modify or develop new equipment and methods to best satisfy the application requirements. For this work, we are interested in real-time monitoring of airborne chemicals, which are commonly referred to as volatile organic compounds (VOC). Although there are a number of techniques for remote analysis of VOCs, many of these applications do not provide the specificity and sensitivity needed in real-time application scenarios. For example, spectroscopic techniques are capable of providing low part-per-billion volume/volume (ppb v/v) detection if a compound is distributed over a large area, however, they provide limited compound structural information. A different approach using air monitoring mass spectrometry can provide more specific chemical information in terms of compound molecular weight and structural information, however, preconcentration is required to achieve low ppb detection. Operation of the trap as a pulsed extraction eliminates many of the limitations that accompany operating the trap using mass selective axial ejection. As pulsed extraction source, the IS can be operated under

  2. 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.

  3. Comparative Studies of the Determination of Divalent Cadmium, Lead and Copper in the Boiling Medicinal Herbs by Stripping Voltammetry and by Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    Ahmed Hassan

    2009-01-01

    Full Text Available Cadmium, lead and copper were determined in ten Libyian boiling medicinal herbs samples by differential pulse anodic stripping voltammetry as well as by atomic absorption spectrometry. Voltammetric method was done at Hanging Mercury Dropping Electrode (HMDE in Briton-Robinson buffer solution of pH ~2.1 at 25± 0.1°C. The sample preparation was carried out by boiling 2.0g of a finely pulverized plant sample for 10 min, cooled, filtered and completed to 50 mL measuring flask by deionized water. The optimal preconcentration potentials and times for the detection of these metal ions in all sample solutions have been studied. The concentration of each metal ion was determined by the standard addition method. The statistical parameters i.e. slope, standard deviation, correlation coefficient and confidence have been calculated. The levels of Cd(II, Pb(II and Cu(II ranged from 0.006-0.103, 0.205-1.751 and 0.198-2.124 µg g-1 respectively. Copper was determined by Flame Atomic Absorption Spectrometry (FAAS and the mean level was ranged from 0.202-2.010 µg g-1 . On the other hand the mean levels obtained for determination of cadmium and lead by Graphite Furnace Atomic Absorption Spectrometry (GFAAS ranged from 0.006 to 0.085 and from 0.220-1.850 µg g-1 respectively.

  4. 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

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

    International Nuclear Information System (INIS)

    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+ 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 heterostructures

  6. L2 discretization of atomic and molecular electronic continua: moment, quadrature and J-matrix techniques

    International Nuclear Information System (INIS)

    A review of the process of extraction of continuum information from operators discretized in finite sets of square integrable (L2) basis functions is given, with emphasis on the close relationships between the Stieltjes method and Gaussian integration. Examples of recent applications are given in the areas of atomic and molecular photoabsorption (He, Ne*, H2, Ar2*), Stieltjes determination of e- -atom/molecule resonances (He, He-, Mg-, N2-) and e+ -H scattering at intermediate energies. Finally, photoabsorption of H- leading to H+ + 2e is discussed using the J-matrix technique, which involves an infinite L2 expansion, and combines advantages of the finite L2 methods with those of the traditional close coupling method. (Auth.)

  7. Determination of the 240Pu/239Pu atom ratio in low activity environmental samples by alpha spectrometry and spectral deconvolution

    International Nuclear Information System (INIS)

    In this paper, a simple technique, based on commercially-available software developed for gamma spectra analysis (MicroSAMPO trademark), is described by which this complex multiplet can be resolved at the much lower activities typical of many environmental samples. In our approach, it is not necessary to make any alterations to the normal alpha spectrometric set-up (including energy dispersion), other than to improve collimation. The instrumental function is defined for each spectrum by fitting a modified gaussian with exponential tails to the comparatively well-resolved 242Pu ''doublet'' (used as tracer) and, if present, the 238Pu ''doublet''. The fitted peaks are used to create an energy calibration file with which, using published energy data, the positions (in channels) of the component peaks of the multiplet are predicted. These positions are not altered subsequently when MicroSAMPO's interactive multiplet analysis facility is used to quantify the relative spectral intensities of the components. Before calculating the 240Pu/239Pu ratio, it is advisable to correct for coincidence summing of alpha particles and conversion electrons. The technique has been applied to the determination of the 240Pu/239Pu ratio in a set of environmental samples, most of which were supplied by IAEA-MEL under their laboratory intercomparison programme. Subsequently, replicate samples were analysed independently using thermal ionisation mass spectrometry. The agreement between the two sets of data was most satisfactory. Further validation of this deconvolution technique was provided by the good agreement between the measured alpha-emission probabilities for the component peaks in the 239,240Pu multiplet and published values. (orig.)

  8. Dynamic light scattering and atomic force microscopy techniques for size determination of polyurethane nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Giehl Zanetti-Ramos, Betina [Laboratorio de Bioenergetica e Bioquimica de Macromoleculas, Departamento de Ciencias Farmaceuticas (Brazil)], E-mail: betinagzramos@pq.cnpq.br; Beddin Fritzen-Garcia, Mauricia [Laboratorio de Bioenergetica e Bioquimica de Macromoleculas, Departamento de Ciencias Farmaceuticas (Brazil); Schweitzer de Oliveira, Cristian; Avelino Pasa, Andre [Laboratorio de Filmes Finos e Superficie, Departamento de Fisica (Brazil); Soldi, Valdir [Grupo de Estudos em Materiais Polimericos, Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Borsali, Redouane [Centre de Recherche sur les Macromolecules Vegetales CERMAV/CNRS, 38041 - Grenoble (France); Creczynski-Pasa, Tania Beatriz [Laboratorio de Bioenergetica e Bioquimica de Macromoleculas, Departamento de Ciencias Farmaceuticas (Brazil)

    2009-03-01

    Nanoparticles have applications in various industrial fields principally in drug delivery. Nowadays, there are several processes for manufacturing colloidal polymeric systems and methods of preparation as well as of characterization. In this work, Dynamic Light Scattering and Atomic Force Microscopy techniques were used to characterize polyurethane nanoparticles. The nanoparticles were prepared by miniemulsion technique. The lipophilic monomers, isophorone diisocyanate (IPDI) and natural triol, were emulsified in water containing surfactant. In some formulations the poly(ethylene glycol) was used as co-monomer to obtain the hydrophilic and pegylated nanoparticles. Polyurethane nanoparticles observed by atomic force microscopy (AFM) were spherical with diameter around 209 nm for nanoparticles prepared without PEG. From AFM imaging two populations of nanoparticles were observed in the formulation prepared with PEG (218 and 127 nm) while dynamic light scattering (DLS) measurements showed a monodisperse size distribution around 250 nm of diameters for both formulations. The polydispersity index of the formulations and the experimental procedures could influence the particle size determination with these techniques.

  9. 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.

  10. 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.

  11. 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.

  12. Speciation of Chromium in Water Samples with Homogeneous Liquid-Liquid Extraction and Determination by Flame Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    A novel method was developed for the speciation of chromium in natural water samples based on homogeneous liquid-liquid extraction and determination by flame atomic absorption spectrometry (FAAS). In this method, Cr(III) reacts with a new Schiff's base ligand to form the hydrophobic complex, which is subsequently entrapped in the sediment phase, whereas Cr(VI) remained in aqueous phase. The Cr(VI) assay is based on its reduction to Cr(III) by the addition of sodium sulfite to the sample solution. Thus, separation of Cr(III) and Cr(VI) could be realized. Homogeneous liquid-liquid extraction based on the pH-independent phase-separation process was investigated using a ternary solvent system (water-tetrabutylammonium ion (TBA+)-chloroform) for the preconcentration of chromium. The phase separation phenomenon occurred by an ion-pair formation of TBA and perchlorate ion. Then sedimented phase was separated using a 100 μL micro-syringe and diluted to 1.0 mL with ethanol. The sample was introduced into the flame by conventional aspiration. After the optimization of complexation and extraction conditions such as pH = 9.5, [ligand] = 1.0 x 10-4 M, [TBA+] = 2.0 x 10-2 M, [CHCl3] = 100.0 μL and [ClO4-] = 2.0 x 10-2 M, a preconcentration factor (Va/Vs) of 100 was obtained for only 10 mL of the sample. The relative standard deviation was 2.8% (n = 10). The limit of detection was sufficiently low and lie at ppb level. The proposed method was applied for the extraction and determination of chromium in natural water samples with satisfactory results

  13. Feasibility of using direct determination of cadmium and lead in fresh meat by electrothermal atomic absorption spectrometry for screening purposes

    International Nuclear Information System (INIS)

    A method for the direct determination of cadmium and lead in fresh meat for screening purposes is proposed using electrothermal atomic absorption spectrometry. The fresh meat samples were homogenized, weighed directly onto solid sampling platforms and introduced into a transversely heated solid sampling graphite tube. The main challenges associated with this procedure, such as weighing errors and optimization of the temperature program were investigated in detail. Calibration was performed against aqueous standards and two modifiers were investigated: 0.05% Pd + 0.03% Mg + 0.05% Triton X-100 and 0.01% Pd + 10% NH4NO3 + 0.05% Triton X-100. The former one is recommended due to the higher pyrolysis temperature obtained for cadmium and the better limits of detection of 1.9 μg kg-1 for lead and 0.13 μg kg-1 for cadmium, based on 10 mg of sample mass. The results obtained for cadmium and lead in two certified reference materials were statistically not different from the certified values on a 95% confidence level, indicating that calibration against aqueous standards is suitable for this application. In order to evaluate weighing errors the fresh samples were dried (at 60 deg. C) to constant weight; the results obtained with fresh and dried samples were in agreement, taking the loss of weight into consideration for the latter ones. The average relative standard deviation of 14% is in concordance with the results of others using fresh meat. Comparison with the digestion method adopted by the Brazilian Ministry of Agriculture shows no significant differences between the results at the 95% confidence level. This study shows that direct analysis of fresh meet can be applied as a rapid routine screening procedure for residue control in products of animal origin, helping the implementation and maintenance of sanitary control

  14. 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)

  15. 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

  16. Detection of hepatitis C virus core protein in serum by atomic force microscopy combined with mass spectrometry

    Directory of Open Access Journals (Sweden)

    Ivanov YD

    2015-02-01

    Full Text Available Yuri D Ivanov,1 Anna L Kaysheva,1,2 Pavel A Frantsuzov,1 Tatyana O Pleshakova,1 Nikolay V Krohin,1 Alexander A Izotov,1 Ivan D Shumov,1 Vasiliy F Uchaikin,1 Vladimir A Konev,1 Vadim S Ziborov,1 Alexander I Archakov11Institute of Biomedical Chemistry, 2PostgenTech Ltd, Moscow, RussiaAbstract: A method for detection and identification of core antigen of hepatitis C virus (HCVcoreAg-containing particles in the serum was proposed, with due account taken of the interactions of proteotypic peptides with Na+, K+, and Cl- ions. The method is based on a combination of reversible biospecific atomic force microscopy (AFM-fishing and mass spectrometry (MS. AFM-fishing enables concentration, detection, and counting of protein complexes captured on the AFM chip surface, with their subsequent MS identification. Biospecific AFM-fishing of HCVcoreAg-containing particles from serum samples was carried out using AFM chips with immobilized antibodies against HCVcoreAg (HCVcoreAgim. Formation of complexes between anti-HCVcoreAgim and HCVcoreAg-containing particles on the AFM chip surface during the fishing process was demonstrated. These complexes were registered and counted by AFM. Further MS analysis allowed reliable identification of HCVcoreAg within the complexes formed on the AFM chip surface. It was shown that MS data processing, with account taken of the interactions between HCVcoreAg peptides and Na+, K+ cations, and Cl- anions, allows an increase in the number of peptides identified.Keywords: hepatitis C virus, molecular detector, biospecific fishing

  17. 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.

  18. 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...

  19. Fast heating induced impulse halogenation of refractory sample components in electrothermal atomic absorption spectrometry by direct injection of a liquid halogenating agent.

    Science.gov (United States)

    György, Krisztina; Ajtony, Zsolt; Van Meel, Katleen; Van Grieken, René; Czitrovszky, Aladár; Bencs, László

    2011-09-15

    A novel electrothermal atomic absorption spectrometry (ETAAS) method was developed for the halogenation of refractory sample components (Er, Nd and Nb) of lithium niobate (LiNbO(3)) and bismuth tellurite (Bi(2)TeO(5)) optical single crystals to overcome memory effects and carry-over. For this purpose, the cleaning step of a regular graphite furnace heating program was replaced with a halogenation cycle. In this cycle, after the graphite tube cooled to room temperature, a 20 μL aliquot of liquid carbon tetrachloride (CCl(4)) was dispensed with a conventional autosampler into the graphite tube. The CCl(4) was partially dried at 80°C under the mini-flow (40 cm(3) min(-1)) condition of the Ar internal furnace gas (IFG), then the residue was decomposed (pyrolyzed) by fast furnace heating at 1900-2100°C under interrupted flow of the IFG. This step was followed by a clean-out stage at 2100°C under the maximum flow of the IFG. The advantage of the present method is that it does not require any alteration to the graphite furnace gas supply system in contrast to most of the formerly introduced halogenation techniques. The effectiveness of the halogenation method was verified with the determination of Er and Nd dopants in the optical crystals. In these analyses, a sensitivity decrease was observed, which was likely due to the enhanced deterioration of the graphite tube surface. Therefore, the application of mathematical correction (resloping) of the calibration was also required. The calibration curves were linear up to 1.5 and 10 μmol L(-1) for Er and Nd, respectively. Characteristic masses of 18 and 241 pg and the limit of detection (LOD) values of 0.017 and 0.27 μmol L(-1) were found for Er and Nd, respectively. These LOD data correspond to 0.68 μmol mol(-1) Er and 11 μmol mol(-1) Nd in solid bismuth tellurite samples. The analytical results were compared with those obtained by a conventional ETAAS method and validated with X-ray fluorescence spectrometry analysis

  20. Accelerator mass spectrometry of 63Ni at the Munich Tandem Laboratory for estimating fast neutron fluences from the Hiroshima atomic bomb.

    Science.gov (United States)

    Rühm, W; Knie, K; Rugel, G; Marchetti, A A; Faestermann, T; Wallner, C; McAninch, J E; Straume, T; Korschinek, G

    2000-10-01

    After the release of the present dosimetry system DS86 in 1987, measurements have shown that DS86 may substantially underestimate thermal neutron fluences at large distances (>1,000 m) from the hypocenter in Hiroshima. This discrepancy casts doubts on the DS86 neutron source term and, consequently, the survivors' estimated neutron doses. However, the doses were caused mainly by fast neutrons. To determine retrospectively fast neutron fluences in Hiroshima, the reaction 63Cu(n, p)63Ni can be used, if adequate copper samples can be found. Measuring 63Ni (half life 100 y) in Hiroshima samples requires a very sensitive technique, such as accelerator mass spectrometry (AMS), because of the relatively small amounts of 63Ni expected (approximately 10(5)-10(6) atoms per gram of copper). Experiments performed at Lawrence Livermore National Laboratory have demonstrated in 1996 that AMS can be used to measure 63Ni in Hiroshima copper samples. Subsequently, a collaboration was established with the Technical University of Munich in view of its potential to perform more sensitive measurements of 63Ni than the Livermore facility and in the interest of interlaboratory validation. This paper presents the progress made at the Munich facility in the measurement of 63Ni by AMS. The Munich accelerator mass spectrometry facility is a combination of a high energy tandem accelerator and a detection system featuring a gas-filled magnet. It is designed for high sensitivity measurements of long-lived radioisotopes. Optimization of the ion source setup has further improved the sensitivity for 63Ni by reducing the background level of the 63Cu isobar interference by about two orders of magnitude. Current background levels correspond to a ratio of 63Ni/Nineutron fluences in Hiroshima and Nagasaki is possible for ground distances of up to 1500 m, and--under favorable conditions--even beyond. To demonstrate this capability, we have measured successfully 6Ni/Ni ratios as low as (3.5 +/- 0.6) x 10