Multielemental determination of trace elements in radiopharmaceuticals produced at the radiopharmacy center using ICP-OES technique

International Nuclear Information System (INIS)

Tavares, Angelica T.; Martins, Patricia de A.; Fukumori, Neuza T.O.; Mengatti, Jair; Matsuda, Margareth M.N.

2013-01-01

The control of chemical impurities in radiopharmaceuticals is critical to their safety and efficacy. According to the U.S. Pharmacopeia (USP), the elemental impurities with potential toxicity must be quantified. A proposed revision of USP 35 introduces the technique of atomic emission spectrometry for the analysis of elements. The aim of this work was to study the concentration of chemicals elements in FDG-Fluor-18, IPEN-TEC Generator and MIBI-TEC using an ICP-OES technique. One analytical curve composed by 27 elements (Ag, A1, B, Ba, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ga, K, Li, Mg, Mn, Mo, Na, Ni, Pb, Pd, Se, Sr, Te, T1, Zn) was constructed in two analytical ranges. The analyses were carried out simultaneously in an ICP-OES Vista MPX (Agilent). Some parameters for analysis and method validation were evaluated. The cleaning and maintenance of equipment influenced the emission intensity of the elements. 1.2 power and 10s sample uptake resulted in a consumption of 1.6 mL of sample and Mg II/Mg I ratio relation equal to 9.40. Linearity, LOD and LOQ were determined. The analysis were performed using 1:40 dilution with purified water. The main elements studied in this work were A1, Cu and Zn. The % recovery was determined with final concentrations of 0.3, 0.5 and 0.8 μg mL -1 . The analyses were performed in triplicate with three different batches. The % recovery was between 96.65 and 117.61% and the values for precision (CV) were less than 5% indicating good accuracy of the method. (author)

Determination of Heavy Metals in Almonds and Mistletoe as a Parasite Growing on the Almond Tree Using ICP-OES or ICP-MS.

Science.gov (United States)

Kamar, Veysi; Dağalp, Rukiye; Taştekin, Mustafa

2017-12-28

In this study, the elements of Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Ni, Sr, Pb, Ti, and Zn were determined in the leaves, fruits, and branches of mistletoe, (Viscum albüm L.), used as a medicinal plant, and in the leaves, branches and barks of almond tree which mistletoe grows on. The aim of the study is to investigate whether the mistletoe are more absorbent than the almond tree in terms of the heavy metal contents and the determination of the amount of the elements penetrated into the mistletoe from the almond tree. ICP-MS (inductively coupled plasma-mass spectrometry) was used for the analysis of As, Cd, Mo, and Pb, whereas ICP-OES (inductively coupled plasma optical emission spectrometry) was used for the other elements. The results obtained were statistically evaluated at 95% confidence level. Within the results obtained in this study, it was determined whether there is a significant difference between metal elements in almond tree and mistletoe, or not. As a result, it was observed that there were higher contents of B, Ba, K, Mg, and Zn in the mistletoe than in the almond tree. K was found much higher than other elements in the mistletoe. On the other hand, Al, As, Ca, Cd, Cr, Cu, Fe, Mo, Ni, Sr, Pb, and Ti contents were determined to be more in almond tree than mistletoe.

Improved documentation of spectral lines for inductively coupled plasma emission spectrometry

Science.gov (United States)

Doidge, Peter S.

2018-05-01

An approach to improving the documentation of weak spectral lines falling near the prominent analytical lines used in inductively coupled plasma optical emission spectrometry (ICP-OES) is described. Measurements of ICP emission spectra in the regions around several hundred prominent lines, using concentrated solutions (up to 1% w/v) of some 70 elements, and comparison of the observed spectra with both recent published work and with the output of a computer program that allows calculation of transitions between the known energy levels, show that major improvements can be made in the coverage of spectral atlases for ICP-OES, with respect to "classical" line tables. It is argued that the atomic spectral data (wavelengths, energy levels) required for the reliable identification and documentation of a large majority of the weak interfering lines of the elements detectable by ICP-OES now exist, except for most of the observed lines of the lanthanide elements. In support of this argument, examples are provided from a detailed analysis of a spectral window centered on the prominent Pb II 220.353 nm line, and from a selected line-rich spectrum (W). Shortcomings in existing analyses are illustrated with reference to selected spectral interferences due to Zr. This approach has been used to expand the spectral-line library used in commercial ICP-ES instruments (Agilent 700-ES/5100-ES). The precision of wavelength measurements is evaluated in terms of the shot-noise limit, while the absolute accuracy of wavelength measurement is characterised through comparison with a small set of precise Ritz wavelengths for Sb I, and illustrated through the identification of Zr III lines; it is further shown that fractional-pixel absolute wavelength accuracies can be achieved. Finally, problems with the wavelengths and classifications of certain Au I lines are discussed.

Analysis of soil and sewage sludge by ICP-OES and the German standard DIN 38414 sample preparation technique (P3)

International Nuclear Information System (INIS)

Edlund, M.; Heitland, P.; Visser, H.

2002-01-01

Full text: The elemental analyses of soil and sewage sludge has developed to become one of the main applications for ICP optical emission spectrometry (ICP-OES) and is described in many official procedures. These methods include different acid mixtures and digestion techniques. Even though the German standard DIN 38414 part 7 and the Dutch NEN 6465 do not guarantee complete recoveries for all elements, they are widely accepted in Europe. This paper describes sample preparation, line selection and investigates precision, accuracy and Limits of detection. The SPECTRO CIROSCCD EOP with axial plasma observation and the SPECTRO CIROSCCD SOP with radial observation were compared and evaluated for the analyses of soil and sewage sludge. Accuracy was investigated using the certified reference materials CRM-141 R, CRM-143 R and GSD 11. Both instruments show excellent performance in terms of speed, precision, accuracy and detection limits for the determination of trace metals in soil and sewage sludge. (author)

Multi-element determinations of N,N-dimethylformamide (DMF) coal slurries using ICP-OES

Energy Technology Data Exchange (ETDEWEB)

M. Mujuru; R.I. McCrindle; B.M. Botha; P.P. Ndibewu [Tshwane University of Technology, Pretoria (South Africa). Department of Chemistry

2009-04-15

A slurry nebulisation technique was applied for elemental analysis of bituminous coals SARM 18, SARM 19 and four coals from three different seams in Witbank, South Africa, by inductively coupled plasma optical emission spectroscopy (ICP-OES). Major elements (Al, Ca, Fe, Mg, S, Si and Ti) and trace elements (Ba, Cr, Mn, Ni, Sr, V, Zn and Zr) in coal were determined. Various slurry preparations were evaluated using two dispersants (glycerol and Triton X-100) and by varying the concentration of dispersants, between 0.1% and 1.0% (v/v). The effect of initially solubilising the ground coal in N,N-dimethylformamide (DMF) was investigated by varying the volume of DMF added. The effect of wet grinding with DMF was investigated. Wet grinding with DMF was shown to drastically reduce particle sizes (50.0% < 0.28 m and 90.0% < 6.17 {mu}m) as compared to dry grinding (50.0% < 5.25 {mu}m and 90.0% < 11.1 {mu}m). The reduced particle sizes and increased transport efficiency of the coal slurries led to improved analytical recoveries of elements in the reference coal, SARM 18. The best analytical recoveries for all elements were achieved using 0.1% Triton X-100 with 10.0% DMF. Results obtained by ICP-OES after wet grinding of the coal with DMF, using 0.1% Triton X-100, also gave excellent recoveries (Al, 100%; Ca, 103%; Cr, 106%; Fe, 102%; Mg, 100%; Mn, 104%; Ni, 109%; Si, 102%; Ti, 95.0%; and V, 108%). The results obtained with 10.0% DMF and 0.1% Triton X-100 were in agreement with certified values for all selected elements according to paired t-test at the 95.0% confidence level. Selected elements (Al, Ca, Fe, Mg, Mn, Si, Ti and V) were also analysed with X-ray fluorescence for comparison with results obtained from ICP-OES. Analysis by ICP-OES of microwave digested coal was also carried out. It is suggested that the DMF slurry technique could be used for routine analysis of bituminous coals. 27 refs., 4 figs., 4 tabs.

Direct rare earth determination by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Marin, Sergio; Cornejo, Silvia; Rojas, Jacqueline

2003-01-01

In the present work, the use of the inductively coupled plasma optical emission spectrometry (ICP-OES), for the sequential determination of Rare Earth elements in the metallurgical process samples is described. In the first place, the optimum parameters for the determination of the elements in study are established, like instrumental calibration, wavelengths spectral selection and interference of matrix. Next, the methodology for the digestion of solid samples (system of digestion with pressure) and the recovery of the interest elements are presented. Two material rocks as of reference Syenite SY3 are used. In order to assure the validity of the obtained data, the reference materials SY2 and SY3 were analyzed by means of two different techniques, ICP-OES and ICP-Mass, this last one was made by an international laboratory and a fusion with lithium metaborate was used with digestion method. Finally, the obtained results demonstrate that the reproducibility in the recovery of rare earth analyzed by both techniques is comparable, and that the methodology of digestion used for these elements is statistically valid (author)

DETERMINAÇÃO SIMULTÂNEA DE METAIS E ENXOFRE POR ICP-OES EM RESÍDUOS DE DESTILAÇÃO DE PETRÓLEO

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Gabriel T. Druzian

Full Text Available A method for digestion of crude oil distillation residues (atmospheric residue, AR and vacuum residue, VR using microwave-induced combustion (MIC was developed for simultaneous determination of metals (Ba, Co, Fe, Mg, Mn, Ni and V and sulfur by inductively coupled plasma optical emission spectrometry (ICP-OES. Samples were wrapped in polyethylene films and combusted using 20 bar of oxygen. Nitric acid solutions were evaluated using 5 min of reflux after combustion. Accuracy was evaluated using certified reference material and comparison with the results obtained by microwave-assisted wet digestion (MAWD. No statistical difference was observed between the certified values and those obtained using MIC as well as between the values obtained using MAWD or MIC. In spite of both methods have been apparently suitable for crude oil digestion, MIC was preferable in view of the possibility of using 3 mol L-1 HNO3 as absorbing solution. Furthermore, it is important to notice that using MIC, C content in digests was lower than 10 mg L-1, preventing interferences in ICP-OES. In addition, the simultaneous digestion of eight samples was possible in less than 30 min and without using concentrated acids and/or longer heating times, making the proposed method well-suited for routine analysis.

An easy and fast procedure for the determination of Ca, Cu, Fe, Mn, Mg, Na, K and Si in biodiesel by ICP OES using emulsification as sample preparation strategy

OpenAIRE

Lisboa, Meibel T.; Clasen, Caroline D.; Vellar, Daiane C. de Sousa; Oreste, Eliézer Q.; Saint'Pierre, Tatiana D.; Ribeiro, Anderson S.; Vieira, Mariana A.

2014-01-01

It is presented an alternative procedure for preparation of biodiesel samples for elemental determination by inductively coupled plasma optical emission spectrometry (ICP OES), based on the sample (10% m/v) emulsion formation with formic acid (15% v/v) and Triton X-100 (0.1% m/v). These concentrations were optimized and the stability of emulsified aqueous standards and samples was found to be of at least 3 h. Experimental conditions (1500 W of RF power and 0.5 L min-1 of Ar nebulizer flow rat...

Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: a tutorial review. Part II. Practical considerations.

Science.gov (United States)

Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

2015-07-23

Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review, Electrothermal Vaporization and Laser Ablation will also be shortly described. The second issue is devoted to the analytical strategies for elemental quantification in such matrices, with particular insight into the isotope dilution technique, particularly used in speciation analysis by ICP-coupled separation techniques. Copyright © 2015 Elsevier B.V. All rights reserved.

Utilization of ICP/OES for the determination of trace metal binding to different humic fractions.

Science.gov (United States)

de la Rosa, G; Peralta-Videa, J R; Gardea-Torresdey, J L

2003-02-28

In this study, the use of inductively coupled plasma/optical emission spectrometry (ICP/OES) to determine multi-metal binding to three biomasses, Sphagnum peat moss, humin and humic acids is reported. All the investigations were performed under part per billion (ppb) concentrations. Batch pH profile experiments were performed using multi-metal solutions of Cd(II), Cu(II), Pb(II), Ni(II), Cr(III) and Cr(VI). The results showed that at pH 2 and 3, the metal affinity of the three biomasses exposed to the multi-metal solution that included Cr(III) presented the following order: Cu(II), Pb(II)>Ni(II)>Cr(III)>Cd(II). On the other hand, when Cr(VI) was in the heavy metal mixture, Sphagnum peat moss and humin showed the following affinity: Cu(II), Pb(II)>Ni(II)>Cr(VI)>Cd(II); however, the affinity of the humic acids was: Cu(II)>Pb(II), Cr(VI)>Ni(II)>Cd(II). The results demonstrated that pH values of 4 and 5 were the most favorable for the heavy metal binding process. At pH 5, all the metals, except for Cr(VI), were bound between 90 and 100% to the three biomasses. However, the binding capacity of humic acids decreased at pH 6 in the presence of Cr(VI). The results showed that the ICP/OES permits the determination of heavy metal binding to organic matter at ppb concentration. These results will be very useful in understanding the role of humic substances in the fate and transport of heavy metals, and thus could provide information to develop new methodologies for the removal of low concentrations of toxic heavy metals from contaminated waters.

Determinação seletiva de tributilestanho na presença de Sn(IV em amostras ambientais usando HG-ICP OES e Saccharomyces cerevisiae como material sorvente Selective determination of tributyltin in the presence of Sn(IV in environmental samples using HG-ICP OES and Saccharomyces cerevisiae as sorbing material

Directory of Open Access Journals (Sweden)

Monizze Vannuci e Silva

2010-01-01

Full Text Available A method for selective determination of tributyltin in the presence of Sn(IV by combining hydride generation inductively coupled plasma optical emission spectrometry (HG-ICP OES and solid phase extraction (SPE using baker's yeast is proposed. The procedure is based on selective retention of TBT by the yeast at pH = 6. Detection limit of 1.9 µg L-1 and quantification limit of 6.3 µg L-1 were obtained. TBT and San(IV were determined in the range of 0-25 µg L-1 and the proposed approach was applied to analyze river water, sea water and biological extracts, with recoveries of 114, 101 and 86%, respectively.

Online Determination of Sm, Eu and Yb in Environmental Samples by Inductively Coupled Plasma – Optical Emission Spectrometry

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J. Dilip Kumar

2007-01-01

Full Text Available A procedure was developed for the determination of Sm, Eu and Yb in water samples by inductively coupled plasma-optical emission spectrometry (ICP-OES after preconcentration on synthesized 5-(4-pyridyl azo-8-quinolinol supported by Borassus flabellifer inflorescence (BFI. The sorbed element was subsequently eluted with 0.4 M HNO3 and the acid eluates were analyzed by ICP-OES. Under the optimal conditions, Sm, Eu and Yb in aqueous samples were concentrated 100-fold. Recoveries were obtained by the proposed method in the range of 98.6 -99.8%. This method was also applied for the analysis of spiked and natural water samples. The results provide strong evidence to support the hypothesis of an adsorption mechanism.

Characterization of bottom sediment of Adam bridge for its mineral content by spectrochemical and ICP-OES techniques

International Nuclear Information System (INIS)

Sharma, P.K.; Bassan, M.K.T.; Avhad, D.K.; Singhal, R.K.; UrsaI, G.R.

2012-01-01

Adam's Bridge also known as Rama's Bridge or Rama Setu is a chain of limestone shoals, between Rameswaram Island, off the southeastern coast of Tamil Nadu, India, and Mannar Island, off the northwestern coast of Sri Lanka. Geological evidence suggests that this bridge is a former land connection between India and Sri Lanka. During this work mineral content in the sand sample collected from four different locations were evaluated by using spectrochemical techniques such as FAAS (Flame atomic absorption spectroscopy), FES(Florescence Emission Spectroscopy), ICP-OES (Inductive coupled plasma optical emission spectroscopy) and UV - Visible Spectrophotometry. Various major elements like SiO 2 , Al 2 O 3 , Fe 2 O 3 , MgO, CaO , Na 2 O , K 2 O, minor elements like MnO, TiO 2 , P 2 O 5 and trace elements like Zr O2 ; V 2 O 5 , PbO and U etc. Validation of analytical methodology and reliability of analytical results were carried out by the analysis of the standard reference material. Trace elements were estimated after the selective removal of silica using AAS and ICP-OES technique. (author)

Online elemental analysis of process gases with ICP-OES: A case study on waste wood combustion

International Nuclear Information System (INIS)

Wellinger, Marco; Wochele, Joerg; Biollaz, Serge M.A.; Ludwig, Christian

2012-01-01

Highlights: ► Simultaneous measurements of 23 elements in process gases of a waste wood combustor. ► Mobile ICP spectrometer allows measurements of high quality at industrial plants. ► Continuous online measurements with high temporal resolution. ► Linear correlations among element concentrations in the raw flue gas were detected. ► Novel sampling and calibration methods for ICP-OES analysis of process gases. - Abstract: A mobile sampling and measurement system for the analysis of gaseous and liquid samples in the field was developed. An inductively coupled plasma optical emission spectrometer (ICP-OES), which is built into a van, was used as detector. The analytical system was calibrated with liquid and/or gaseous standards. It was shown that identical mass flows of either gaseous or liquid standards resulted in identical ICP-OES signal intensities. In a field measurement campaign trace and minor elements in the raw flue gas of a waste wood combustor were monitored. Sampling was performed with a highly transport efficient liquid quench system, which allowed to observe temporal variations in the elemental process gas composition. After a change in feedstock an immediate change of the element concentrations in the flue gas was detected. A comparison of the average element concentrations during the combustion of the two feedstocks showed a high reproducibility for matrix elements that are expected to be present in similar concentrations. On the other hand elements that showed strong differences in their concentration in the feedstock were also represented by a higher concentration in the flue gas. Following the temporal variations of different elements revealed strong correlations between a number of elements, such as chlorine with sodium, potassium and zinc, as well as arsenic with lead, and calcium with strontium.

Comparision of ICP-OES and MP-AES in determing soil nutrients by Mechlich3 method

Science.gov (United States)

Tonutare, Tonu; Penu, Priit; Krebstein, Kadri; Rodima, Ako; Kolli, Raimo; Shanskiy, Merrit

2014-05-01

Accurate, routine testing of nutrients in soil samples is critical to understanding soil potential fertility. There are different factors which must be taken into account selecting the best analytical technique for soil laboratory analysis. Several techniques can provide adequate detection range for same analytical subject. In similar cases the choise of technique will depend on factors such as sample throughput, required infrastructure, ease of use, used chemicals and need for gas supply and operating costs. Mehlich 3 extraction method is widely used for the determination of the plant available nutrient elements contents in agricultural soils. For determination of Ca, K, and Mg from soil extract depending of laboratory ICP and AAS techniques are used, also flame photometry for K in some laboratories. For the determination of extracted P is used ICP or Vis spectrometry. The excellent sensitivity and wide working range for all extracted elements make ICP a nearly ideal method, so long as the sample throughput is big enough to justify the initial capital outlay. Other advantage of ICP techniques is the multiplex character (simultaneous acquisition of all wavelengths). Depending on element the detection limits are in range 0.1 - 1000 μg/L. For smaller laboratories with low sample throughput requirements the use of AAS is more common. Flame AAS is a fast, relatively cheap and easy technique for analysis of elements. The disadvantages of the method is single element analysis and use of flammable gas, like C2H2 and oxidation gas N2O for some elements. Detection limits of elements for AAS lays from 1 to 1000 μg/L. MP-AES offers a unique alternative to both, AAS and ICP-OES techniques with its detection power, speed of analysis. MP-AES is quite new, simple and relatively inexpensive multielemental technique, which is use self-sustained atmospheric pressure microwave plasma (MP) using nitrogen gas generated by nitrogen generator. Therefore not needs for argon and

A simple, rapid and eco friendly method for determination of uranium in geological samples of low silicate matrix by ICP-OES

International Nuclear Information System (INIS)

Hanuman, V.V.; Chakrapani, G.; Singh, A.K.

2013-01-01

A simple, rapid, cost effective and eco friendly decomposition and dissolution method is developed for the determination of uranium (U 3 O 8 ) by Inductively Coupled Plasma - Optical Emission Spectrometer (ICP-OES) in low silicate geological samples. The salts of Sodium di-hydrogen phosphate monohydrate and Sodium pyrophosphate deca hydrate are used in the ratio of 1:1 (phosphate flux) for the decomposition of low silicate matrix geological samples. Samples are decomposed by fusion with the phosphate flux after ignition and the dissolution is carried out using distilled water. If the samples contain >10% silica, they have been treated with little amount of (HF+HNO 3 ) prior to fusion with phosphate flux. These samples, are analysed by ICP-OES directly without any separation from the matrix. The spectral interferences of major matrix elements (Al, Ti, Fe, Mn, etc present in the sample) on uranium are studied and it is observed that their interferences are negligible, as dilution is required to bring uranium concentration into calibration range of instrument. This is the first time, the phosphate flux is used for decomposition of low silicate geological samples for uranium determination by ICP-OES

Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: a tutorial review. Part I. Theoretical considerations.

Science.gov (United States)

Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

2015-07-23

Due to their outstanding analytical performances, inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are widely used for multi-elemental measurements and also for isotopic characterization in the case of ICP-MS. While most studies are carried out in aqueous matrices, applications involving organic/hydro-organic matrices become increasingly widespread. This kind of matrices is introduced in ICP based instruments when classical "matrix removal" approaches such as acid digestion or extraction procedures cannot be implemented. Due to the physico-chemical properties of organic/hydro-organic matrices and their associated effects on instrumentation and analytical performances, their introduction into ICP sources is particularly challenging and has become a full topic. In this framework, numerous theoretical and phenomenological studies of these effects have been performed in the past, mainly by ICP-OES, while recent literature is more focused on applications and associated instrumental developments. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP-OES and ICP-MS. The present Part I, provides theoretical considerations in connection with the physico-chemical properties of organic/hydro-organic matrices, in order to better understand the induced phenomena. This focal point is divided in four chapters highlighting: (i) the impact of organic/hydro-organic matrices from aerosol generation to atomization/excitation/ionization processes; (ii) the production of carbon molecular constituents and their spatial distribution in the plasma with respect to analytes repartition; (iii) the subsequent modifications of plasma fundamental properties; and (iv) the resulting spectroscopic and non spectroscopic interferences. This first part of this tutorial review is addressed either to beginners or to more experienced scientists who are interested in the

Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part I. Theoretical considerations

Energy Technology Data Exchange (ETDEWEB)

Leclercq, Amélie, E-mail: amelie.leclercq@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Nonell, Anthony, E-mail: anthony.nonell@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Todolí Torró, José Luis, E-mail: jose.todoli@ua.es [Universidad de Alicante, Departamento de Quimica Analitica, Nutricion y Bromatología, Ap. de Correos, 99, 03080 Alicante (Spain); Bresson, Carole, E-mail: carole.bresson@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vio, Laurent, E-mail: laurent.vio@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vercouter, Thomas, E-mail: thomas.vercouter@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Chartier, Frédéric, E-mail: frederic.chartier@cea.fr [CEA Saclay, DEN, DANS, DPC, 91191 Gif-sur-Yvette (France)

2015-07-23

Highlights: • Tutorial review addressed to beginners or more experienced analysts. • Theoretical background of effects caused by organic matrices on ICP techniques. • Spatial distribution of carbon species and analytes in plasma. • Carbon spectroscopic and non-spectroscopic interferences in ICP. - Abstract: Due to their outstanding analytical performances, inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are widely used for multi-elemental measurements and also for isotopic characterization in the case of ICP-MS. While most studies are carried out in aqueous matrices, applications involving organic/hydro-organic matrices become increasingly widespread. This kind of matrices is introduced in ICP based instruments when classical “matrix removal” approaches such as acid digestion or extraction procedures cannot be implemented. Due to the physico-chemical properties of organic/hydro-organic matrices and their associated effects on instrumentation and analytical performances, their introduction into ICP sources is particularly challenging and has become a full topic. In this framework, numerous theoretical and phenomenological studies of these effects have been performed in the past, mainly by ICP-OES, while recent literature is more focused on applications and associated instrumental developments. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP-OES and ICP-MS. The present Part I, provides theoretical considerations in connection with the physico-chemical properties of organic/hydro-organic matrices, in order to better understand the induced phenomena. This focal point is divided in four chapters highlighting: (i) the impact of organic/hydro-organic matrices from aerosol generation to atomization/excitation/ionization processes; (ii) the production of carbon molecular constituents and their spatial distribution in the

Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part I. Theoretical considerations

International Nuclear Information System (INIS)

Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

2015-01-01

Highlights: • Tutorial review addressed to beginners or more experienced analysts. • Theoretical background of effects caused by organic matrices on ICP techniques. • Spatial distribution of carbon species and analytes in plasma. • Carbon spectroscopic and non-spectroscopic interferences in ICP. - Abstract: Due to their outstanding analytical performances, inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are widely used for multi-elemental measurements and also for isotopic characterization in the case of ICP-MS. While most studies are carried out in aqueous matrices, applications involving organic/hydro-organic matrices become increasingly widespread. This kind of matrices is introduced in ICP based instruments when classical “matrix removal” approaches such as acid digestion or extraction procedures cannot be implemented. Due to the physico-chemical properties of organic/hydro-organic matrices and their associated effects on instrumentation and analytical performances, their introduction into ICP sources is particularly challenging and has become a full topic. In this framework, numerous theoretical and phenomenological studies of these effects have been performed in the past, mainly by ICP-OES, while recent literature is more focused on applications and associated instrumental developments. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP-OES and ICP-MS. The present Part I, provides theoretical considerations in connection with the physico-chemical properties of organic/hydro-organic matrices, in order to better understand the induced phenomena. This focal point is divided in four chapters highlighting: (i) the impact of organic/hydro-organic matrices from aerosol generation to atomization/excitation/ionization processes; (ii) the production of carbon molecular constituents and their spatial distribution in the

New developments in glow discharge optical emission and mass spectrometry

International Nuclear Information System (INIS)

Hoffmann, Volker; Dorka, Roland; Wilken, Ludger; Wetzig, Klaus

2000-01-01

This paper describes new developments in flow discharge optical emission (GD-OES) and mass spectrometry (GD-MS) at IFW and presents corresponding new applications (analysis of microelectronic multi-layer system by radio frequency glow discharge optical emission spectrometry (RF-GD-OES) and analysis of pure iron by a new Grimm-type GD-MS source)

Determination of total strontium in uruguayan rice by inductively coupled plasma optical emission spectrometry (ICP-OES

Directory of Open Access Journals (Sweden)

Mario E. Rivero Huguet

2011-04-01

Full Text Available Strontium (Sr is found naturally as a non-radioactive element and has 16 known isotopes. Naturally occurring Sr is found as four stable isotopes: Sr-84, -86, -87, and -88. Twelve other isotopes are radioactive. Sr-90 is the most important radioactive isotope in the environment, discovered mostly after the nuclear experiments conducted in the 1950s and 1960s. In the present work, 86 rice samples (Oryza saliva L. and 7 rice husk samples were digested by dry ashing for the purpose of determining the total Sr levels by ICP-OES. The mean concentrations found were: 0.281 µg g-1 for milled, 0.287 µg g-1 for parboiled milled, 0.564 µg g-1 for brown, 0.73 µg g-1 for parboiled brown, and 1.16 µg g-1 for paddy rice, and 3.44 µg g-1 for the rice husks. Validation of the method was conducted with a certified reference material, NIST CAM 8418 Wheat Gluten, and the recovery obtained ranged from 89-98%. As the outer layers (aleurone, pericarp of the grain are removed, the Sr concentration decreases. It can then be assumed that most of the Sr is stored in these layers. Although no extensive data exist for Sr levels in rice, the values obtained are in good agreement with the results reported for Sr in brown rice from Japan (0.25-0.72 µg g-1 and with non-contaminated foodstuffs from other parts of the world. Thus, the Uruguayan rice has Sr levels that match non-contaminated samples and its consumption presents no health threat.Publicado en: Atomic Spectroscopy.-- 2006, 27(3:80-85

LIBS coupled with ICP/OES for the spectral analysis of betel leaves

Science.gov (United States)

Rehan, I.; Rehan, K.; Sultana, S.; Khan, M. Z.; Muhammad, R.

2018-05-01

Laser-induced breakdown spectroscopy (LIBS) system was optimized and was applied for the elemental analysis and exposure of the heavy metals in betel leaves in air. Pulsed Nd:YAG (1064 nm) in conjunction with a suitable detector (LIBS 2000+, Ocean Optics, Inc) having the optical resolution of 0.06 nm was used to record the emission spectra from 200 to 720 nm. Elements like Al, Ba, Ca, Cr, Cu, P, Fe, K, Mg, Mn, Na, P, S, Sr, and Zn were found to be present in the samples. The abundances of observed elements were calculated through normalized calibration curve method, integrated intensity ratio method, and calibration free-LIBS approach. Quantitative analyses were accomplished under the assumption of local thermodynamic equilibrium (LTE) and optically thin plasma. LIBS findings were validated by comparing its results with the results obtained using a typical analytical technique of inductively coupled plasma-optical emission spectroscopy (ICP/OES). Limit of detection (LOD) of the LIBS system was also estimated for heavy metals.

Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part II. Practical considerations

Energy Technology Data Exchange (ETDEWEB)

Leclercq, Amélie, E-mail: amelie.leclercq@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Nonell, Anthony, E-mail: anthony.nonell@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Todolí Torró, José Luis, E-mail: jose.todoli@ua.es [Universidad de Alicante, Departamento de Quimica Analitica, Nutricion y Bromatología, Ap. de Correos, 99, 03080 Alicante (Spain); Bresson, Carole, E-mail: carole.bresson@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vio, Laurent, E-mail: laurent.vio@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vercouter, Thomas, E-mail: thomas.vercouter@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Chartier, Frédéric, E-mail: frederic.chartier@cea.fr [CEA Saclay, DEN, DANS, DPC, 91191 Gif-sur-Yvette (France)

2015-07-23

Graphical abstract: This tutorial review is dedicated to the analysis of organic/hydro-organic matrices by ICP techniques. A state-of-the-art focusing on sample introduction, relevant operating parameters optimization and analytical strategies for elemental quantification is provided. - Highlights: • Practical considerations to perform analyses in organic/hydro-organic matrices. • Description, benefits and drawbacks of recent introduction devices. • Optimization to improve plasma tolerance towards organic/hydro-organic matrices. • Analytical strategies for elemental quantification in organic/hydro-organic matrices. - Abstract: Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review

Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part II. Practical considerations

International Nuclear Information System (INIS)

Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

2015-01-01

Graphical abstract: This tutorial review is dedicated to the analysis of organic/hydro-organic matrices by ICP techniques. A state-of-the-art focusing on sample introduction, relevant operating parameters optimization and analytical strategies for elemental quantification is provided. - Highlights: • Practical considerations to perform analyses in organic/hydro-organic matrices. • Description, benefits and drawbacks of recent introduction devices. • Optimization to improve plasma tolerance towards organic/hydro-organic matrices. • Analytical strategies for elemental quantification in organic/hydro-organic matrices. - Abstract: Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review

DETERMINATION OF REFRACTORY ELEMENTS IN USED LUBRICATING OIL AND IN FUEL OIL BY ICP OES WITH EMULSIFIED SAMPLES

OpenAIRE

ROSELI MARTINS DE SOUZA

2003-01-01

O conhecimento da concentração dos elementos traço em óleo lubrificante usado é útil para a avaliação de desgastes de componentes específicos de motores.Em óleo combustível, este monitoramento permite avaliar a qualidade do combustível e prever o potencial das emissões de metais no meio ambiente. Neste trabalho, utilizou-se a espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES) para a determinação de elementos refratários em amostras de ól...

Evaluation of analytical procedures for the determination of cadmium, boron and lithium in UALx samples by inductively coupled plasma optical emission spectrometry (ICP OES)

International Nuclear Information System (INIS)

Guilhen, Sabine Neusatz; Kakazu, Mauricio H.; Cotrim, Marycel Elena Barboza; Pires, Maria Aparecida Faustino; Souza, Alexandre Luiz de

2013-01-01

Used in over 80% of the worldwide diagnostic procedures, Technetium-99m ( 99m Tc), which is obtained from the decay of molybdenum-99 ( 99 Mo), is the most important radioisotope in nuclear medicine. IPEN/CNEN-SP has been developing technologies in order to produce Mo-99 by the irradiation of low-enriched uranium (LEU < 20% of 235U) targets in its research reactor IEA-R1 (IPEN, Sao Paulo/Brazil). These targets consist of low enriched uranium dispersed in a matrix of aluminum (UAlx-Al). Several impurities may be incorporated during the target's production process, such as boron, cadmium and lithium, which have a high capture cross section that may reduce the irradiation's efficiency. This study describes a simple and rapid inductively coupled plasma optical emission spectrometric method for the determination of cadmium, boron and lithium in uranium aluminum (UAlx) dispersion targets. The method involves a previous separation step, in which uranium gets removed from the matrix by chromatographic extraction with the use of a divinylbenzene resin Amberlite XAD - 4 doped with tri-n-butyl phosphate (TBP). TBP selectively separates the uranium, leaving behind the impurities in an aqueous medium for a further quantification by ICP OES. Possible spectroscopic interferences are also discussed in this article, because of the high amount of aluminum in the remaining solution. Experimental and instrumental conditions, such as initial mass, acid solution ratio and amount, resin mass, emission lines and interfering concentrations are carefully established. This method is to be applied for the determination of several others impurities in UAlx in the future, providing means to verify the UAlx targets' compliance to the current established specifications through routine laboratory analysis. (author)

Quantification of Selected Trace and Mineral Elements in Royal Jelly from Bulgaria by Icp-Oes and Etaas

Directory of Open Access Journals (Sweden)

Balkanska Ralitsa

2017-12-01

Full Text Available The objective of the present study was to investigate selected trace and mineral elements in Royal Jelly (RJ from Bulgaria. A total of 30 RJ samples were included in the study. The analytical procedure consisted of the microwave digestion of the RJ samples with nitric acid followed by instrumental measurement. Concentrations of Al, Ba, Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P, Sr and Zn were determined using inductively coupled plasma optical emission spectroscopy (ICP-OES, while As, Cd, Co, Ni and Pb were determined by electrothermal atomic absorption spectrometry (ETAAS. Our results showed that elements K, Mg, Ca represented 96% from the total mineral content of the RJ samples from Bulgaria, while the most abundant trace element was Na, followed by Zn. The elements Ba, Cr, Cu, Fe, Mn and Sr were found in trace concentration levels and elements As, Pb, Cd, Co and Ni in microconcentration levels. Selected mineral and trace elements were found in relatively constant concentration levels in all of the analyzed RJ samples. It was concluded that chemical element content did not depend on geographical origin and was under homeostatic adjustment in RJs.

Electrolytic dissolution of aluminium alloys (chip form) and mullet-element determination by inductively coupled plasma optical emission spectrometry (ICP-OES)

International Nuclear Information System (INIS)

Grigoletto, Tania

2001-01-01

Several aluminum alloys with different chip's size were dissolved using aqua regia (HCl:HN0 3 ,3:1). The residues of the dissolution procedure were either rejected or used in silicon volatilization with hydrofluoric acid before determination of Fe, Cu, Mn, Mg, Cr, Ni, Zn, Pb, Sn, Ti and Zr by ICP-OES. The influence caused by crescent amounts of aluminum in the determination of other elements and the probable spectral interference by Cu in determination of Zn (with or without electrolytic separation of Cu) was evaluated. The electrolytic dissolution of aluminum alloys was performed by pressing chips against a platinum electrode for the electrolysis to occur, so that way the chips behaved as the anode. A tube (body of syringe of 2.5 mL) with perforations around the open base was used to contain the sample and Pt electrode. The alloy was placed on synthetic wool (perlon) in this tube. An acrylic dowel with a platinum wire across its interior was fixed in the superior part a tube with Teflon film, with an orifice through which the electrolytic solution flowed (HNO 3 1 mol L -1 ; 4.5 mL min -1 ). A platinum dish was fixed at the inferior extremity of the platinum wire to press the sample. The solution came out through the inferior orifices of the tube to a flask, from where it was again captured (with a peristaltic pump) to go into the superior part of the tube. In this flask, a Pt wire cathode was also placed. A current of 0.6 A and ten minutes of electrolysis provided good results. Due to the partial dissolution, the knowledge of percentages of previous elements analyzed after total dissolution, or using certified reference material are necessary. The results were normalized by knowledge percentages. The calculations were made by the ratio between the concentration of the element determined, with the determined concentration of aluminum; the ratio between concentration of the element and the sum of the concentrations of the elements determined, including Al; the ratio

Characterization of arsenic-contaminated aquifer sediments from eastern Croatia by ion microbeam, PIXE and ICP-OES techniques

Energy Technology Data Exchange (ETDEWEB)

Ujević Bošnjak, M., E-mail: magdalena.ujevic@hzjz.hr [Croatian National Institute of Public Health, Rockefelerova 7, 10000 Zagreb (Croatia); Fazinić, S. [Institute Ruđer Bošković, Bijenička cesta, 10000 Zagreb (Croatia); Duić, Ž. [University of Zagreb, Faculty of Mining, Geology and Petroleum Engineering, Pierottijeva 6, Zagreb (Croatia)

2013-10-01

Highlights: •ICP-OES and PIXE used in the characterization of As-contaminated sediments. •Observed high correlations between the results obtained by those techniques. •Discrepancies observed for Mn, and for the highest As concentrations. •Microbeam analyses showed As association with sulphides and iron. -- Abstract: Groundwater arsenic contamination has been evidenced in eastern Croatia and hydrochemical results suggest that the occurrence of arsenic in the groundwater depends on the local geology, hydrogeology, and geochemical characteristics of the aquifer. In order to perform the sediment characterization and to investigate arsenic association with the other elements in the sediments, 10 samples from two boreholes (PVc-3 and Gundinci 1) in eastern Croatia were analyzed using two techniques: PIXE (without sample pre-treatment) and ICP-OES (after digestion), as well by ion microbeam analyses. The results of the PIXE and ICP-OES techniques showed quite good agreement; however, greater discrepancies were observed at the higher arsenic and manganese mass ratios. According to both techniques, higher As mass ratios were observed in the sediments from the PVc-3 core (up to 651 mg/kg and 491 mg/kg using PIXE and ICP-OES analyses respectively) than from the Gundinci 1 core (up to 60 mg/kg using both techniques). Although arsenic association with Fe is expected, no correlation was observed. The microbeam analyses demonstrated that arsenic is associated with sulphides and iron in the most As-contaminated sample from the PVc-3 core, while this relationship was not evident in the most As-contaminated sample from the Gundinci 1 borehole.

Characterization of arsenic-contaminated aquifer sediments from eastern Croatia by ion microbeam, PIXE and ICP-OES techniques

International Nuclear Information System (INIS)

Ujević Bošnjak, M.; Fazinić, S.; Duić, Ž.

2013-01-01

Highlights: •ICP-OES and PIXE used in the characterization of As-contaminated sediments. •Observed high correlations between the results obtained by those techniques. •Discrepancies observed for Mn, and for the highest As concentrations. •Microbeam analyses showed As association with sulphides and iron. -- Abstract: Groundwater arsenic contamination has been evidenced in eastern Croatia and hydrochemical results suggest that the occurrence of arsenic in the groundwater depends on the local geology, hydrogeology, and geochemical characteristics of the aquifer. In order to perform the sediment characterization and to investigate arsenic association with the other elements in the sediments, 10 samples from two boreholes (PVc-3 and Gundinci 1) in eastern Croatia were analyzed using two techniques: PIXE (without sample pre-treatment) and ICP-OES (after digestion), as well by ion microbeam analyses. The results of the PIXE and ICP-OES techniques showed quite good agreement; however, greater discrepancies were observed at the higher arsenic and manganese mass ratios. According to both techniques, higher As mass ratios were observed in the sediments from the PVc-3 core (up to 651 mg/kg and 491 mg/kg using PIXE and ICP-OES analyses respectively) than from the Gundinci 1 core (up to 60 mg/kg using both techniques). Although arsenic association with Fe is expected, no correlation was observed. The microbeam analyses demonstrated that arsenic is associated with sulphides and iron in the most As-contaminated sample from the PVc-3 core, while this relationship was not evident in the most As-contaminated sample from the Gundinci 1 borehole

Trends in preconcentration procedures for metal determination using atomic spectrometry techniques

International Nuclear Information System (INIS)

Godoi Pereira, M. de; Arruda, M.A.Z.

2003-01-01

Methods for metal preconcentration are often described in the literature. However, purposes are often different, depending on whether the methods are applied in environmental, clinical or technological fields. The respective method needs to be efficient, give high sensitivity, and ideally also is selective which is useful when used in combination with atomic spectroscopy. This review presents the actual tendencies in metal preconcentration using techniques such as flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS), hydride generation atomic absorption spectrometry (HGAAS), inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS). Procedures based on related to electrochemical, coprecipitation/precipitation, liquid-liquid and solid-liquid extraction and atom trapping mechanisms are presented. (author)

Gas chromatography/plasma spectrometry - an important analytical tool for elemental speciation studies

International Nuclear Information System (INIS)

Wuilloud, Jorgelina C.A.; Wuilloud, Rodolfo G.; Vonderheide, Anne P.; Caruso, Joseph A.

2004-01-01

In this review, a full discussion and update of the state-of-the-art of gas chromatography (GC) coupled to all known plasma spectrometers is presented. A brief introductive discussion of the advantages and disadvantages of GC-plasma interfaces, as well as types of plasmas and mass spectrometers, is given. The plasma-based techniques covered include inductively coupled plasma mass spectrometry (ICP-MS) microwave-induced plasma optical emission spectrometry (MIP-OES), and inductively coupled plasma optical emission spectrometry (ICP-OES). Also, different variants of plasma sources, such as low power plasmas and glow discharge (GD) sources, are described and compared with respect to their capabilities in elemental speciation. Recent advances and alternative mass analyzers (collision/reaction cell; time-of-flight; double-focusing sector field) are also mentioned. Different aspects of the GC-plasma coupling are discussed with particular attention to the applications of these hyphenated techniques to the analysis of elemental species. Additionally, classical and modern sample preparation methods, including extraction and/or preconcentration and derivatization reactions, are presented and evaluated

Analytical chemistry of actinides

International Nuclear Information System (INIS)

Chollet, H.; Marty, P.

2001-01-01

Different characterization methods specifically applied to the actinides are presented in this review such as ICP/OES (inductively coupled plasma-optical emission spectrometry), ICP/MS (inductively coupled plasma spectroscopy-mass spectrometry), TIMS (thermal ionization-mass spectrometry) and GD/OES (flow discharge optical emission). Molecular absorption spectrometry and capillary electrophoresis are also available to complete the excellent range of analytical tools at our disposal. (authors)

Surfactant assisted chemical vapour generation of silver for AAS and ICP-OES: a mechanistic study

Czech Academy of Sciences Publication Activity Database

Matoušek, Tomáš; Sturgeon, R. E.

2003-01-01

Roč. 18, č. 5 (2003), s. 487-494 ISSN 0267-9477 Institutional research plan: CEZ:AV0Z4031919 Keywords : vapour generation * ICP-OES * silver Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.200, year: 2003

A rapid and practical strategy for the determination of platinum, palladium, ruthenium, rhodium, iridium and gold in large amounts of ultrabasic rock by inductively coupled plasma optical emission spectrometry combined with ultrasound extraction

Science.gov (United States)

Zhang, Gai; Tian, Min

2015-04-01

This proposed method regulated the determination of platinum, palladium, ruthenium, rhodium, iridium and gold in platinum-group ores by nickel sulfide fire assay—inductively coupled plasma optical emission spectrometry (ICP-OES) combined with ultrasound extraction for the first time. The quantitative limits were 0.013-0.023μg/g. The samples were fused to separate the platinum-group elements from matrix. The nickel sulfide button was then dissolved with hydrochloric acid and the insoluble platinum-group sulfide residue was dissolved with aqua regia by ultrasound bath and finally determined by ICP-OES. The proposed method has been applied into the determination of platinum-group element and gold in large amounts of ultrabasic rocks from the Great Dyke of Zimbabwe.

Uranium and thorium determination in Santa Quiteria liquor by ICP-OES analysis

International Nuclear Information System (INIS)

Pedro Junior, A.; Rezende, Paulo R.; Carvalho, Leonel M.; Ferreira, Elizabeth de Massena

2009-01-01

The mineral source of Itataia located in Santa Quiteria (Ceara/Brazil) is a phosphorus uraniferous one, where uranium occurs in collophanite (fluoroapatite) form. Phosphate minerals of the apatite family make possible the uses of uranium as a byproduct. The sulfuric leaching of the phosphate rock in order to obtain phosphoric acid also permits uranium recovery. Thus, the liquor coming from the leaching contains high levels of phosphoric acid as well as elements like Mg, Fe, U, Zr, Th and some rare earths in significant concentrations. The direct determination of U and Th content of this liquor is essential to a rapid response in the uranium separation and purification together process by solvent extraction, aiming its use for commercial purposes, as nuclear industry fuel. In this study U and Th were determined by Inductively Coupled Plasma Spectrometry (ICP-OES) in several samples of liquor, in high concentrations of H 3 PO 4 in environment. Several ratios of U/Th and H 3 PO 4 concentrations were studied, in order to find the optimal conditions for the direct determination of U and Th, without need to prior separation. (author)

Possibilities of High Resolution Inductively Coupled Plasma Optical Emission Spectrometry in the Determination of Trace Elements in Environmental Materials

Directory of Open Access Journals (Sweden)

Nikolaya Velitchkova

2013-01-01

Full Text Available This paper presents new quantitative data for the spectral interferences obtained by high resolution 40.68 MHz radial viewing inductively coupled plasma optical emission spectrometry (HR-ICP-OES in the determination of Zn, Cd, Sb, Cu, Mn, Pb, Sn, Cr, U, and Ba in environmental materials in the presence of a complex matrix, containing Al, Ca, Fe, Mg, and Ti. The -concept for quantification of spectral interferences was used. The optimum line selection for trace analysis of a variety of multicomponent matrices requires the choice of prominent lines, which are free or negligibly influenced by line interference problems. The versatility of -concept as basic methodology was experimentally demonstrated in the determination of trace of elements in soil and drinking water. The detection limits are lower in comparison with corresponding threshold concentration levels for soil and drinking water in accordance with environmental regulations. This paper shows the possibilities of present day ICP-OES equipment in the direct determination of trace elements (without preconcentration of impurities in environmental samples.

Application of femtosecond laser ablation inductively coupled plasma mass spectrometry for quantitative analysis of thin Cu(In,Ga)Se{sub 2} solar cell films

Energy Technology Data Exchange (ETDEWEB)

Lee, Seokhee [School of Mechatronics, Gwangju Institute of Science and Technology, 1 Oryong-dong, Buk-gu, Gwangju 500-712 (Korea, Republic of); Gonzalez, Jhanis J. [Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA 94720 (United States); Applied Spectra Inc., 46665 Fremont Boulevard, Fremont, CA 94538 (United States); Yoo, Jong H. [Applied Spectra Inc., 46665 Fremont Boulevard, Fremont, CA 94538 (United States); Chirinos, Jose R. [Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA 94720 (United States); Facultad de Ciencias, Universidad Central de Venezuela, Caracas 1041A (Venezuela, Bolivarian Republic of); Russo, Richard E. [Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA 94720 (United States); Applied Spectra Inc., 46665 Fremont Boulevard, Fremont, CA 94538 (United States); Jeong, Sungho, E-mail: shjeong@gist.ac.kr [School of Mechatronics, Gwangju Institute of Science and Technology, 1 Oryong-dong, Buk-gu, Gwangju 500-712 (Korea, Republic of)

2015-02-27

This work reports that the composition of Cu(In,Ga)Se{sub 2} (CIGS) thin solar cell films can be quantitatively predicted with high accuracy and precision by femtosecond laser ablation-inductively coupled plasma-mass spectrometry (fs-LA-ICP-MS). It is demonstrated that the results are strongly influenced by sampling conditions during fs-laser beam (λ = 1030 nm, τ = 450 fs) scanning on the CIGS surface. The fs-LA-ICP-MS signals measured at optimal sampling conditions generally provide a straight line calibration with respect to the reference concentrations measured by inductively coupled plasma optical emission spectroscopy (ICP-OES). The concentration ratios predicted by fs-LA-ICP-MS showed high accuracy, to 95–97% of the values measured with ICP-OES, for Cu, In, Ga, and Se elements. - Highlights: • Laser ablation inductively coupled plasma mass spectrometry of thin film is reported. • Concentration ratio prediction with a confidence level of 95–97% is achieved. • Quantitative determination of composition is demonstrated.

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)

Oliveira, Luis Claudio de; Silva, Adriana Mascarenhas Martins da; Gomide, Ricardo Goncalves; Silva, Ieda de Souza

2013-01-01

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)

On-line preconcentration and determination of chromium in parenteral solutions by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Gil, R.A.; Cerutti, S.; Gasquez, J.A.; Olsina, R.A.; Martinez, L.D.

2005-01-01

A method for the preconcentration and speciation of chromium was developed. On-line preconcentration and determination were obtained using inductively coupled plasma optical emission spectrometry (ICP-OES) coupled with flow injection. To determinate the chromium (III) present in parenteral solutions, chromium was retained on activated carbon at pH 5.0. On the other hand, a step of reduction was necessary in order to determine total chromium content. The Cr(VI) concentration was then determined by difference between the total chromium concentration and that of Cr(III). A sensitivity enrichment factor of 70-fold was obtained with respect to the chromium determination by ICP-OES without preconcentration. The detection limit for the preconcentration of 25 ml of sample was 29 ng l -1 . The precision for the 10 replicate determinations at the 5 μg l -1 Cr level was 2.3% relative standard deviation, calculated with the peak heights. The calibration graph using the preconcentration method for chromium species was linear with a correlation coefficient of 0.9995 at levels near the detection limits up to at least 60 μg l -1 . The method can be applied to the determination and speciation of chromium in parenteral solutions

In-situ optical emission spectrometry during galvanostatic aluminum anodising

International Nuclear Information System (INIS)

Mercier, D.; Van Overmeere, Q.; Santoro, R.; Proost, J.

2011-01-01

In this study, we report on the use of optical emission spectrometry (OES) for the online detection of changes in the Al concentration ejected in a 1.0 mol dm -3 sulphuric acid electrolyte during galvanostatic anodising of Al thin film substrates. The technique relies on the coupling of an Inductively Coupled Plasma (ICP) spectrometer to a specially designed electrochemical flow cell. This has allowed to correlate, for the first time, the kinetics of Al dissolution to well-established morphological changes related to porous anodic oxide formation and growth. A deconvolution algorithm was first developed in order to decompose the experimental ICP/OES signal into elementary distributions, each one characteristic for a specific kinetic regime. The highest dissolution rate systematically occurred during the first step, associated with barrier oxide formation. This is followed by a systematic decrease in the rate of Al dissolution during pore formation. During steady-state porous oxide growth, the Al dissolution rate increases again, but still remains below the level established during barrier oxide growth. In each of these three kinetic regimes, a linear variation of the Al dissolution rate with current density was observed in the range 0.5-5.0 mA cm -2 , with slope values of, respectively, 35 ± 2, 24 ± 2 and 28 ± 1 μg C -1 . Regarding the temporal transitions between the different regimes, a desynchronisation was observed between the kinetic (dissolution) and morphological transitions, the time offset going in opposite directions for barrier and steady-state porous oxide growth. Finally, using the measured Al dissolution rates, the current density dependence of the film formation efficiency for both porous and barrier oxide growth has been established.

Development of Exact Matrix-Matching Inductively Coupled Plasma-Optical Emission Spectroscopy for the Analysis of Cu and K in Infant Formula

Energy Technology Data Exchange (ETDEWEB)

Lee, Ye-Ji; Yim, Yong-Hyeon [University of Science and Technology, Daejeon (Korea, Republic of); Heo, Sung Woo; Han, Myung-Sub; Lim, Youngran [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

2016-08-15

In the present study, we have developed an exact matrix-matching inductively coupled plasma-optical emission spectroscopy (ICP-OES) as a low-cost alternative to the isotope dilution inductively coupled plasma mass spectrometry (ICP-MS) method for accurate and precise measurements of nutrient elements K and Cu in infant formula. In spite of its high precision and accuracy, ICP-OES analysis of complex samples was not reliable due to biases originating from various matrix effects. The elaborated exact matrix-matching approach tested here demonstrated its potential to minimize biases due to matrix mismatch. The exact matrix-matching ICP-OES method was successfully validated by comparing the results with those from an isotope dilution ICP-M S method. Because the model provides reliable results without significant loss of precision, it will be an excellent choice for major element analysis in a complex sample, especially when isotope dilution is not applicable due to the l ck of alternative isotopes or the high cost of enriched isotopes.

Experimental and theoretical investigations about the vaporization of laser-produced aerosols and individual particles inside inductively-coupled plasmas — Implications for the extraction efficiency of ions prior to mass spectrometry

International Nuclear Information System (INIS)

Flamigni, Luca; Koch, Joachim; Günther, Detlef

2012-01-01

Current quantification capabilities of laser ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS) are known to be restricted by elemental fractionation as a result of LA-, transport-, and ICP-induced effects which, particularly, may provoke inaccuracies whenever calibration strategies on the basis of non-matrix matched standard materials are applied. The present study is dealing with the role of ICP in this complex scenario. Therefore, the vaporization process of laser-produced aerosols and subsequent diffusion losses occurring inside ICP sources were investigated using 2-D optical emission spectrometry (OES) and ICP-quadrupole (Q)MS of individual particles. For instance, Na- and Ca-specific OES of aerosols produced by LA of silicate glasses or metals revealed axial shifts in the onset and maximum position of atomic emission which were in the range of a few millimeters. The occurrence of these shifts was found to arise from composition-dependent particle/aerosol penetration depths, i.e. the displacement of axial vaporization starting points controlling the ion extraction efficiency through the ICP-MS vacuum interface due to a delayed, diffusion-driven expansion of oxidic vs. metallic aerosols. Furthermore, ICP-QMS of individual particles resulted in 1/e half-value signal durations of approximately 100 μs, which complies with modeled values if OES maxima are assumed to coincide with positions of instantaneous vaporization and starting points for atomic diffusion. To prove phenomena observed for their consistency, in addition, “ab initio” as well as semi-empirical simulations of particle/aerosol penetration depths followed by diffusion-driven expansion was accomplished indicating differences of up to 15% in the relative ion extraction efficiency depending on whether analytes are supplied as metals or oxides. Implications of these findings on the accuracy achievable by state-of-the-art LA-ICP-MS systems are outlined. - Highlights: ► Specification

Comparative study of injection into a pneumatic nebuliser and tungsten coil electrothermal vaporisation for the determination of rare earth elements by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Dittrich, K.

1988-01-01

Injection into a pneumatic nebuliser and vaporisation using a tungsten coil electrothermal vaporisation system, with a 3-kW argon-nitrogen inductively coupled plasma (ICP), are compared for the determination of the rare earth elements. The sampling efficiency and thus also the absolute power of detection of the tungsten coil ICP optical emission spectrometric (ICP-OES) technique are better by two orders of magnitude, than the injection technique. The absolute detection limits for the rare earth elements are at the pg level; for the refractory rare earth elements (Er, La, Lu and Y), they are lower than those obtained by graphite furnace atomic absorption spectrometry, whereas for the other rare earth elements (Eu, Sc, Tm and Yb), the detection limits are comparable. With injection of samples into a pneumatic nebuliser and ICP-OES, matrix effects are low and absolute amounts of the order of mg of the rare earth matrix can be tolerated, giving relative detection limits down to 1 μg g -1 . The amount of rare earth matrix that can be tolerated with the tungsten-coil atomiser is two orders of magnitude lower. Thus the relatively detection limits of the two methods are of the same order, although the matrix effects are considerably higher with the tungsten coil. (author)

Passive neutralization of acid mine drainage using basic oxygen furnace slag as neutralization material: experimental and modelling

CSIR Research Space (South Africa)

Zvimba, JN

2015-12-01

Full Text Available emission 147 spectrometry (ICP-OES) (Varian: Vista Pro CCD Simultaneous ICP-OES). The pH, acidity, 148 alkalinity of the AMD were determined using a Mettler Toledo Auto-titrator following 149 filtration. Fe(II) was determined using standard permanganate...

Tin Content Determination in Canned Fruits and Vegetables by Hydride Generation Inductively Coupled Plasma Optical Emission Spectrometry

Directory of Open Access Journals (Sweden)

Sanda Rončević

2012-01-01

Full Text Available Tin content in samples of canned fruits and vegetables was determined by hydride generation inductively coupled plasma atomic emission spectrometry (HG-ICP-OES, and it was compared with results obtained by standard method of flame atomic absorption spectrometry (AAS. Selected tin emission lines intensity was measured in prepared samples after addition of tartaric acid and followed by hydride generation with sodium borohydride solution. The most favorable line at 189.991 nm showed the best detection limit (1.9 μg L−1 and limit of quantification (6.4 μg kg−1. Good linearity and sensitivity were established from time resolved analysis and calibration tests. Analytical accuracy of 98–102% was obtained by recovery study of spiked samples. Method of standard addition was applied for tin determination in samples from fully protected tinplate. Tin presence at low-concentration range was successfully determined. It was shown that tenth times less concentrations of Sn were present in protected cans than in nonprotected or partially protected tinplate.

Determination of various elements in the Malva Sylvestris L. from Manisa region in Turkey by using ICP-OES

International Nuclear Information System (INIS)

Hicsoenmez, Ue.; Erees, F. S.; Cam, S.; Ozdemir, C.; Oezdemir, A.

2006-01-01

Various elements are transmitted into living metabolism through food intake. Although some of these elements are beneficial for living body, some of them may be toxic or radioactive. 4 0K, 2 38U, 2 35U or the radioactive daughters in the U and Th natural decay chains may be taken via consumption of these elements. In particular, since these radioactive elements have very long half-life and emit alpha particles, they may cause internal radiation risk. Manisa region located in the Western part of the Turkey has very productive agricultural soil. The Malva sylvestris L. is a herbaceous being consumed by human and animals in the region. In this work, Malva sylvestris samples were collected from different points in Muradiye areas of Manisa. Then, they were classified according to leaf size. These leaves were dissolved by wet digestion method using a mixture of mineral acid. Concentrations of Co, Na, Ca, Mg, Al, B, Ba, Cu, Mn, Ni, Zn, Cr, Cd, Ag, Sn, K, Ti, Fe, Sr, Sb, Si, Pb, Bi, U, La and Zr in prepared solutions and region soil were determined by using Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), which is very sensitive and accurate detecting low level elements in sample, eg. in rocks, plants, animal tissue etc. Obtained values were compared with the internationally allowed values. The results of element were analyzed statistically. For different leaf sizes, concentration factors were calculated

Application of ICP-OES to the determination of barium in blood and urine in clinical and forensic analysis.

Science.gov (United States)

Lech, Teresa

2013-05-01

Exposure to barium (Ba) mostly occurs in the workplace or from drinking water, but it may sometimes be due to accidental or intentional intoxication. This paper presents a reliable, sensitive method for the determination of Ba in blood and urine: inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave digestion of samples. The overall procedure was checked using Seronorm Whole Blood L-2, Trace Elements Urine and spiked blood and urine samples (0.5-10 µg/mL of Ba). The accuracy of the whole procedure (relative error) was 4% (blood) and 7% (urine); the recovery was 76-104% (blood) and 85-101% (urine). The limits of detection and quantification (Ba λ = 455.403 nm) were 0.11 and 0.4 µg/L of Ba, respectively; precision (relative standard deviation) was below 6% at the level of 15 µg/L of Ba for blood. This method was applied to a case of the poisoning of a man who had been exposed at the workplace for over two years to powdered BaCO3, and who suffered from paralysis and heart disorders. The concentrations of Ba, in μg/L, were 160 (blood), 460 (serum) and 1,458 (urine) upon his admission to the hospital, and 6.1 (blood) and 4.9 (urine) after 11 months (reference values: 3.34 ± 2.20 µg/L of Ba for blood and 4.43 ± 4.60 µg/L of Ba for urine).

Leaching of heavy metals from contaminated soils using inductively coupled plasma optical emission spectrometer (ICP-OES) and atomic absorption spectrometer (AAS)

International Nuclear Information System (INIS)

Hussain, Z.; Islam, M.

2010-01-01

The clean-up of soils contaminated with heavy metals is one of the most difficult tasks for environmental engineering. Heavy metals are highly persistent in soil and a number of techniques have been developed that aim to remove heavy metals from contaminated soil. A method has been adopted to evaluate dynamic leaching of metal contaminants from industrial soil samples obtained from textile industrial sites in Lahore, Pakistan. In the extraction procedures employed five different leaching liquors were used: 0.01 M CaCl/sub 2/, 1 M HNO/sub 3/, a 1:1 mixture of 0.1M HCl and 0.1M NaCl, 0.01 M EDTA and pH controlled 0.5 M acetic acid. The qualitative and quantitative analyses were carried out by Atomic Absorption Spectroscopy (AAS) and Inductively Coupled Plasma-Optical Emission Spectrometer (ICP-OES). The results indicate that Cu, Zn, Cd, Ni, Pb, Fe and As were extracted in the soil samples in varying concentration when using the different leach liquors. The predominant metals which were leached were As 78.7 ng/ml in 0.01 M EDTA; Zn 1.81 mu g/ml and Fe 898.96 macro g/ml in HNO/sub 3/. (author)

Comparison of 15N analysis by optical emission spectrometry and mass spectrometry for clinical studies during total parenteral nutrition

International Nuclear Information System (INIS)

Ragon, A.; Reynier, J.P.; Guiraud, G.

1985-01-01

During total and stable parenteral nutrition, a branched chain amino acid enriched solution containing [ 15 N]leucine was infused into a patient to determine the fate of the nitrogen administered through this formulation. Measurements of 15 N isotopic enrichments were performed on the same biological samples (urinary urea, total plasma proteins and albumin) by optical emission spectrometry (OES) and mass spectrometry (MS) to determine if OES with its specific advantages (cost, handling maintenance) constituted even with low enrichments a useful alternative technique to MS considered as the reference method. The results show that OES constituted a very useful analytical technique to obtain reliable information in clinical metabolic studies when low 15 N enrichments must be determined. (Auth.)

Dispersive liquid-liquid microextraction for simultaneous determination of cadmium, cobalt, lead and nickel in water samples by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Dos Santos Silva, E.; Correia, L.O.; Dos Santos, L.O.; Dos Santos Vieira, E.V.; Lemos, V.A.

2012-01-01

We report on a new method for the dispersive liquid-liquid microextraction of Cd(II), Co(II), Pb(II) and Ni (II) from water samples prior to their simultaneous determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on the injection of a ternary solvent system composed of appropriate quantities of extraction solvent (trichloroethylene), dispersive solvent (ethanol), and the chelating reagent 2-(2'-benzothiazolylazo)-p-cresol into the sample solution. The solution turns turbid immediately after injection, and the analytes are extracted into the droplets of the organic phase which was dried and dissolved in a mixture of Triton X-114, nitric acid, and ethanol. The metal ions in this mixture were quantified by ICP-OES. The detection limits under optimized conditions are 0.2, 0.3, 0.2 and 0.7 μg L -1 for Cd(II), Co(II), Pb(II) and Ni(II), respectively. The enrichment factors were also calculated for Cd (13), Co (11), Pb (11) and Ni (8). The procedure was applied to the determination of cadmium, cobalt, lead and nickel in certified reference material (waterway sediment) and water samples. (author)

Qualitative and quantitative chemical investigation of orthopedic alloys by combining wet digestion, spectro analytical methods and direct solid analysis

Energy Technology Data Exchange (ETDEWEB)

Figueiredo, Caio M.; Castro, Jeyne P.; Sperança, Marco A.; Fialho, Lucimar L.; Nóbrega, Joaquim A.; Pereira-Filho, Edenir R., E-mail: erpf@ufscar.br [Universidade Federal de São Carlos (GAIA/UFSCar), SP (Brazil). Grupo de Análise Instrumental Aplicada

2018-05-01

In this study, two laser-based techniques, laser-induced breakdown spectroscopy (LIBS) and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) were used for analytical signal evaluation of Ti, Al, and V and investigation of possible harmful elements eventually present as minor elements in Ti alloys. Due to the lack of certified reference materials, samples were also analyzed by wavelength dispersive X-ray fluorescence (WDXRF) and inductively coupled plasma optical emission spectrometry (ICP OES) after microwave-assisted digestion. To maximize the efficiency of LIBS and LA-ICP-MS, operational conditions were adjusted aiming to find optimal analytical performance. LIBS showed several Ti emission lines and few signals for Al and V. LA-ICP-MS was able to detect all three major constituents. For quantitative analysis, the correlation of intensity signals from LIBS analysis with reference values obtained by ICP OES was not successful, showing that there are still difficulties for quantification using solid samples. Measurements using ICP OES showed that additionally to major constituents, only Fe was present in concentrations around 0.2%. Analysis by WDXRF confirmed the presence of Fe. Results using both methods, i.e., ICP OES and WDXRF, were in good agreement. (author)

Analysis of cobalt, tantalum, titanium, vanadium and chromium in tungsten carbide by inductively coupled plasma-optical emission spectrometry

CSIR Research Space (South Africa)

Archer, M

2003-12-01

Full Text Available Inductively coupled plasma optical emission spectroscopy (ICP-OES) was used to measure the concentrations of cobalt, tantalum, titanium, vanadium and chromium in solutions of tungsten carbide. The main advantage of the method described here lies...

Influence of binders on infrared laser ablation of powdered tungsten carbide pressed pellets in comparison with sintered tungsten carbide hardmetals studied by inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Hola, Marketa; Otruba, Vitezslav; Kanicky, Viktor

2006-01-01

Laser ablation (LA) was studied as a sample introduction technique for the analysis of powdered and sintered tungsten carbides (WC/Co) by inductively coupled plasma optical emission spectrometry (ICP-OES). The possibility to work with powdered and compact materials with close chemical composition provided the opportunity to compare LA sampling of similar substances in different forms that require different preparation procedures. Powdered WC/Co precursors of sintered hardmetals were prepared for the ablation as pressed pellets with and without powdered silver as a binder, while sintered hardmetal blocks were embedded into a resin to obtain discs, which were then smoothed and polished. A Q-switched Nd:YAG laser operated at its fundamental wavelength of 1064 nm with a pulse frequency of 10 Hz and maximum pulse energy of 220 mJ was used. A single lens was used for the laser beam focusing. An ablation cell (14 cm 3 ) mounted on a PC-controlled XY-translator was connected to an ICP spectrometer Jobin Yvon 170 Ultrace (laterally viewed ICP, mono- and polychromator) using a 1.5-m tubing (4 mm i.d.). Ablation was performed in a circular motion (2 mm diameter). Close attention was paid to the study of the crater parametres depending on hardness, cohesion and Ag binder presence in WC/Co samples. The influence of the Co content on the depth and structure of the ablation craters of the binderless pellets was also studied. Linear calibration plots of Nb, Ta and Ti were obtained for cemented WC/Co samples, binderless and binder-containing pellets. Relative widths of uncertainty intervals about the centroids vary between ± 3% and ± 7%, and exceptionally reach a value above 10%. The lowest determinable quantities (LDQ) of Nb, Ta and Ti calculated from the calibration lines were less than 0.5% (m/m). To evaluate the possibility of quantitative elemental analysis by LA-ICP-OES, two real sintered WC/Co samples and two real samples of powdered WC/Co materials were analysed. The

Influence of binders on infrared laser ablation of powdered tungsten carbide pressed pellets in comparison with sintered tungsten carbide hardmetals studied by inductively coupled plasma atomic emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Hola, Marketa [Research Centre for Environmental Chemistry and Ecotoxicology and Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University in Brno, Kotlarska 2, CZ 611 37 Brno (Czech Republic); Otruba, Vitezslav [Research Centre for Environmental Chemistry and Ecotoxicology and Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University in Brno, Kotlarska 2, CZ 611 37 Brno (Czech Republic); Kanicky, Viktor [Research Centre for Environmental Chemistry and Ecotoxicology and Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University in Brno, Kotlarska 2, CZ 611 37 Brno (Czech Republic)]. E-mail: viktork@chemi.muni.cz

2006-05-15

Laser ablation (LA) was studied as a sample introduction technique for the analysis of powdered and sintered tungsten carbides (WC/Co) by inductively coupled plasma optical emission spectrometry (ICP-OES). The possibility to work with powdered and compact materials with close chemical composition provided the opportunity to compare LA sampling of similar substances in different forms that require different preparation procedures. Powdered WC/Co precursors of sintered hardmetals were prepared for the ablation as pressed pellets with and without powdered silver as a binder, while sintered hardmetal blocks were embedded into a resin to obtain discs, which were then smoothed and polished. A Q-switched Nd:YAG laser operated at its fundamental wavelength of 1064 nm with a pulse frequency of 10 Hz and maximum pulse energy of 220 mJ was used. A single lens was used for the laser beam focusing. An ablation cell (14 cm{sup 3}) mounted on a PC-controlled XY-translator was connected to an ICP spectrometer Jobin Yvon 170 Ultrace (laterally viewed ICP, mono- and polychromator) using a 1.5-m tubing (4 mm i.d.). Ablation was performed in a circular motion (2 mm diameter). Close attention was paid to the study of the crater parametres depending on hardness, cohesion and Ag binder presence in WC/Co samples. The influence of the Co content on the depth and structure of the ablation craters of the binderless pellets was also studied. Linear calibration plots of Nb, Ta and Ti were obtained for cemented WC/Co samples, binderless and binder-containing pellets. Relative widths of uncertainty intervals about the centroids vary between {+-} 3% and {+-} 7%, and exceptionally reach a value above 10%. The lowest determinable quantities (LDQ) of Nb, Ta and Ti calculated from the calibration lines were less than 0.5% (m/m). To evaluate the possibility of quantitative elemental analysis by LA-ICP-OES, two real sintered WC/Co samples and two real samples of powdered WC/Co materials were analysed

Quantitative determination of total cesium in highly active liquid waste by using liquid electrode plasma optical emission spectrometry.

Science.gov (United States)

Do, Van-Khoai; Yamamoto, Masahiko; Taguchi, Shigeo; Takamura, Yuzuru; Surugaya, Naoki; Kuno, Takehiko

2018-06-01

A sensitive analytical method for determination of total cesium (Cs) in highly active liquid waste (HALW) by using modified liquid electrode plasma optical emission spectrometry (LEP-OES) is developed in this study. The instrument is modified to measure radioactive samples in a glove box. The effects of important factors, including pulsed voltage sequence and nitric acid concentration, on the emission of Cs are investigated. The limit of detection (LOD) and limit of quantification (LOQ) are 0.005 mg/L and 0.02 mg/L, respectively. The achieved LOD is one order lower than that of recently developed spectroscopic methods using liquid discharge plasma. The developed method is validated by subjecting a simulated HALW sample to inductively coupled plasma mass spectrometry (ICP-MS). The recoveries obtained from a spike-and-recovery test are 96-102%, implying good accuracy. The method is successfully applied to the quantification of Cs in a real HALW sample at the Tokai reprocessing plant in Japan. Apart from dilution and filtration of the HALW sample, no other pre-treatment process is required. The results agree well with the values obtained using gamma spectrometry. The developed method offers a reliable technique for rapid analysis of total Cs in HALW samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Metal and trace element concentration evaluation in sediment profiles of the TietÊ River, State Of SÃO Paulo, by INAA and ICP OES techniques

Energy Technology Data Exchange (ETDEWEB)

Soares, Josiane S., E-mail: josi.s@usp.br [Instituto de Pesquisas Tecnológicas do Estado de São Paulo (LAQ- CQuiM/IPT), São Paulo, SP (Brazil). Lab. de Análises Químicas; Rocha, Flavio R.; Fávaro, Déborah I. T., E-mail: defavaro@ipen.br [Instituto de Pesquisas Energéticas e Nucleares (LAN/IPEN/CNEN-SP), São Paulo, SP (Brazil). Lab. de Análise por Ativação Neutrônica

2017-07-01

The present study presents concentration results for heavy metals, major and trace elements, in two sediment cores collected along the Tietê River: Salto de Itu to Porto Feliz ( Core 4 at point T-5) and Laras to Anhembi (Core 6 at point T18). As, Ba, Br, Co, Cr, Cs, Hf, Rb, Sb, Sc, Ta, Th, U and Zn concentrations by Instrumental Neutron Activation Analysis (INAA) and Al, Ba, Cd, Co, Cr, Cu, Mn, Ni, Pb, Ti, V and Zn concentrations by Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES) were determined. The enrichment factor (EF), to assess the presence of anthropogenic pollution sources, was calculated and showed FE > 1.5 values for As, Br, Cs, Hf, Rb, Ta, Th, U and Zn, confirming the anthropogenic contribution for these elements, in all fractions from both cores. As, Cd, Cr, Cu, Ni, Pb and Zn concentrations were compared to guideline values (TEL and PEL) from the Canadian Council of Ministers of the Environment (CCME) and adopted by the São Paulo State Environmental Company (CETESB) and concentration values between TEL and PEL were found, for all fractions from both cores, presenting good and or regular sediment quality classification, the worst being Core 6. (author)

Metal and trace element concentration evaluation in sediment profiles of the TietÊ River, State Of SÃO Paulo, by INAA and ICP OES techniques

International Nuclear Information System (INIS)

Soares, Josiane S.; Rocha, Flavio R.; Fávaro, Déborah I. T.

2017-01-01

The present study presents concentration results for heavy metals, major and trace elements, in two sediment cores collected along the Tietê River: Salto de Itu to Porto Feliz ( Core 4 at point T-5) and Laras to Anhembi (Core 6 at point T18). As, Ba, Br, Co, Cr, Cs, Hf, Rb, Sb, Sc, Ta, Th, U and Zn concentrations by Instrumental Neutron Activation Analysis (INAA) and Al, Ba, Cd, Co, Cr, Cu, Mn, Ni, Pb, Ti, V and Zn concentrations by Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES) were determined. The enrichment factor (EF), to assess the presence of anthropogenic pollution sources, was calculated and showed FE > 1.5 values for As, Br, Cs, Hf, Rb, Ta, Th, U and Zn, confirming the anthropogenic contribution for these elements, in all fractions from both cores. As, Cd, Cr, Cu, Ni, Pb and Zn concentrations were compared to guideline values (TEL and PEL) from the Canadian Council of Ministers of the Environment (CCME) and adopted by the São Paulo State Environmental Company (CETESB) and concentration values between TEL and PEL were found, for all fractions from both cores, presenting good and or regular sediment quality classification, the worst being Core 6. (author)

Partial microwave-assisted wet digestion of animal tissue using a baby-bottle sterilizer for analyte determination by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Matos, Wladiana O.; Menezes, Eveline A.; Gonzalez, Mario H.; Costa, Leticia M.; Trevizan, Lilian C.; Nogueira, Ana Rita A.

2009-01-01

A procedure for partial digestion of bovine tissue is proposed using polytetrafluoroethylene (PTFE) micro-vessels inside a baby-bottle sterilizer under microwave radiation for multi-element determination by inductively coupled plasma optical emission spectrometry (ICP OES). Samples were directly weighed in laboratory-made polytetrafluoroethylene vessels. Nitric acid and hydrogen peroxide were added to the uncovered vessels, which were positioned inside the baby-bottle sterilizer, containing 500 mL of water. The hydrogen peroxide volume was fixed at 100 μL. The system was placed in a domestic microwave oven and partial digestion was carried out for the determination of Ca, Cu, Fe, Mg, Mn and Zn by inductively coupled plasma optical emission spectrometry. The single-vessel approach was used in the entire procedure, to minimize contamination in trace analysis. Better recoveries and lower residual carbon content (RCC) levels were obtained under the conditions established through a 2 4-1 fractional factorial design: 650 W microwave power, 7 min digestion time, 50 μL nitric acid and 50 mg sample mass. The digestion efficiency was ascertained according to the residual carbon content determined by inductively coupled plasma optical emission spectrometry. The accuracy of the proposed procedure was checked against two certified reference materials.

Effect of organic matrices on the determination of the trace element chemistry (Mg, Sr, Mg/Ca, Sr/Ca) of aragonitic bivalve shells (Arctica islandica). Comparison of ICP-OES and LA-ICP-MS data

International Nuclear Information System (INIS)

Schoene, Bernd R.; Zhang, Zengjie; Jacob, Dorrit; Soldate, Analia; Gillikin, David P.; Tuetken, Thomas; Garbe-Shoenberg, Dieter; McConnaughey, Ted

2010-01-01

The element chemistry of biogenic carbonates can provide important data on past environments. However, the Sr/Ca and Mg/Ca ratios as well as the Mg and Sr concentrations of biological carbonates, especially aragonitic bivalves often depart from apparent thermodynamic equilibrium. When measured in situ by means of LA-ICP-MS, the Mg concentration is often substantially enriched (two- to threefold) near the organic-rich, annual growth lines. To test the hypothesis that some organic components exert a major influence on the skeletal metal content, the element chemistry of different shell components (insoluble organic matrix, IOM; dissolved CaCO 3 and soluble organics, SOM) of Arctica islandica was measured by means of ICP-OES and LA-ICP-MS. The ICP-OES data indicate that the IOM is strongly enriched in Mg (130 ppm) and depleted in Sr and Ca (10 ppm and 0.22 wt%, respectively) when compared to the whole biomineral (Mg: 68 to 99 ppm, Sr: 860 to 1,060 ppm, Ca: ∼35.72 wt%). Although the average relative abundance of the IOM barely exceeds 0.46 wt%, its chemical composition in combination with its heterogeneous distribution across the shell can significantly increase estimates of the Mg concentration if measured in situ by LA-ICP-MS. Depending on the distribution of the IOM, the Ca concentration may be significantly lower locally than the average Ca concentration of the whole shell (35.72 wt%). If this remains undetected, the Mg concentration of shell portions with higher than average IOM content is overestimated by LA-ICP-MS and, conversely, the Mg concentration is underestimated in shell portions with lower than average IOM content. Removal of the IOM prior to the chemical analysis by LA-ICP-MS or mathematical correction for the IOM-derived magnesium concentrations is therefore strongly advised. The different chemistry of the IOM may also exert a major control on the trace element to calcium ratios. Shell portions enriched in IOM will show up to 200 times higher Mg

Matrix digestion of soil and sediment samples for extraction of lead, cadmium and antimony and their direct determination by inductively coupled plasma-mass spectrometry and atomic emission spectrometry

International Nuclear Information System (INIS)

Chattopadhyay, P.; Fisher, A.S.; Henon, D.N.; Hill, S.J.

2004-01-01

An environmentally friendly and simple method has been developed for complete digestion of lead, cadmium and antimony from soil samples using a magnesium nitrate assisted dry ashing procedure. Statistical data for a series of experiments with standard reference materials are presented, and precision values are found to be comparable for inductively coupled plasma-mass spectrometry and for inductively coupled plasma-atomic emission spectrometry. From a single digest solution all analytes are quantified without involving any preconcentration routes. Inter-method comparison of inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) shows that the probability of the results being different is less than 99 %. (author)

Determination of 18 kinds of trace impurities in the vanadium battery grade vanadyl sulfate by ICP-OES

Science.gov (United States)

Yong, Cheng

2018-03-01

The method that direct determination of 18 kinds of trace impurities in the vanadium battery grade vanadyl sulfate by inductively coupled plasma atomic emission spectrometry (ICP-OES) was established, and the detection range includes 0.001% ∼ 0.100% of Fe, Cr, Ni, Cu, Mn, Mo, Pb, As, Co, P, Ti, Zn and 0.005% ∼ 0.100% of K, Na, Ca, Mg, Si, Al. That the influence of the matrix effects, spectral interferences and background continuum superposition in the high concentrations of vanadium ions and sulfate coexistence system had been studied, and then the following conclusions were obtained: the sulfate at this concentration had no effect on the determination, but the matrix effects or continuous background superposition which were generated by high concentration of vanadium ions had negative interference on the determination of potassium and sodium, and it produced a positive interference on the determination of the iron and other impurity elements, so that the impacts of high vanadium matrix were eliminated by the matrix matching and combining synchronous background correction measures. Through the spectral interference test, the paper classification summarized the spectral interferences of vanadium matrix and between the impurity elements, and the analytical lines, the background correction regions and working parameters of the spectrometer were all optimized. The technical performance index of the analysis method is that the background equivalent concentration -0.0003%(Na)~0.0004%(Cu), the detection limit of the element is 0.0001%∼ 0.0003%, RSD<10% when the element content is in the range from 0.001% to 0.007%, RSD< 20% even if the element content is in the range from 0.0001% to 0.001% that is beyond the scope of the method of detection, recoveries is 91.0% ∼ 110.0%.

Avaliação de ICP OES com configuração axial ou radial para determinação de iodo em sal de cozinha

Directory of Open Access Journals (Sweden)

Adriana A. Oliveira

2012-01-01

Full Text Available The performance of inductively-coupled plasma optical emission spectrometers with axial and radial views for determination of iodine in table salt was evaluated. Interference and memory effects in nitric acid and water-soluble tertiary amines (CFA-C media were studied. Based on a factorial experiment, one optimum instrument operational condition for axial configuration, and two optima conditions for radial configuration was established. The ICP OES with axial view was 5-fold more sensitive than the radial view. Both matrix matching and standard addition methods were used for iodine quantification and for most samples, both strategies of calibration led to similar results. Recoveries ranged from 104 to 114%.

Inductively coupled plasma mass spectrometry (ICP-MS)

International Nuclear Information System (INIS)

Shimamura, Tadashi

1997-01-01

The period of investigation for the previous general remarks on the progress of ICP-MS was from January, 1991 to September, 1993. In the investigation of this time, for the object of the Chemical Abstracts from January, 1994 to September, 1996, retrieval was carried out by using the STN International. As the key words, ICP-MS, Inductively Coupled Plasma Mass Spectrometry or Inductively Coupled Plasma Mass Spectrometer was used. The number of hit was 373 in 1994, 462 in 1995, and 356 as of September, 1996, 1191 in total. The cumulative number of the papers from 1980 to 1996 is shown. It is known how rapidly the ICP-MS has pervaded as the means of analysis. In order to cope with the enormous number of papers, this time, it was decided to do the review by limiting to the papers which were published in the main journals deeply related to analytical chemistry. As to the tendency in the last three years, it is summarized as how to overcome the spectrum interference and matrix effect in the ICP-MS and the trend of using the ICP-MS as the high sensitivity detector for separation techniques. The technical basic research of the ICP-MS on spectrum interference, sample introduction method and others and the analysis of living body samples are reported. (K.I.)

Determination of ultratrace elements in natural waters by solid-phase extraction and atomic spectrometry methods.

Science.gov (United States)

Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Frache, Roberto

2003-01-01

A study was carried out on the preconcentration of ultratrace amounts of cadmium, lead, manganese, copper and iron from high-salinity aqueous samples and determination by atomic spectrometry methods. Sample volume, amount of resin, loading flow rate, and elution volume were optimized in order to obtain the simultaneous preconcentration of all the analytes. Quantitative recoveries were obtained by using 200 mg of iminodiacetic resin with a loading flow rate of 2 mL min(-1), elution volume of 3 mL and sample volume of 50-450 mL. Only copper in seawater samples was not completely retained by the resin (60-70% recovery), due to unfavorable competition of iminodiacetic-active groups with organically bound metal.To quantify the metals in the eluates, two atomic spectrometry techniques were compared: electrothermal atomization atomic absorption spectrometry (ETAAS) and inductively coupled plasma-optical emission spectrometry (ICP-OES) with simultaneous CCD detection system. Both techniques are suitable for sample analysis with detection limits of 1.0, 4.7, 3.3, 6.8, and 53 ng L(-1) using ETAAS and 12, 122, 3.4, 17, and 21 ng L(-1) using ICP-OES for Cd, Pb, Mn, Cu, and Fe, respectively. Relative standard deviations of the procedures ranged from 1.7 to 14% at the sub-microg L(-1) concentration level. The accuracy of both methods was verified by analyzing various certified reference materials (river water, estuarine water, coastal and off-shore seawater).

Determination of ultratrace elements in natural waters by solid-phase extraction and atomic spectrometry methods

Energy Technology Data Exchange (ETDEWEB)

Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Frache, Roberto [Department of Chemistry and Industrial Chemistry, University of Genoa, Via Dodecaneso, 31-16146, Genoa (Italy)

2003-01-01

A study was carried out on the preconcentration of ultratrace amounts of cadmium, lead, manganese, copper and iron from high-salinity aqueous samples and determination by atomic spectrometry methods. Sample volume, amount of resin, loading flow rate, and elution volume were optimized in order to obtain the simultaneous preconcentration of all the analytes. Quantitative recoveries were obtained by using 200 mg of iminodiacetic resin with a loading flow rate of 2 mL min{sup -1}, elution volume of 3 mL and sample volume of 50-450 mL. Only copper in seawater samples was not completely retained by the resin (60-70% recovery), due to unfavorable competition of iminodiacetic-active groups with organically bound metal.To quantify the metals in the eluates, two atomic spectrometry techniques were compared: electrothermal atomization atomic absorption spectrometry (ETAAS) and inductively coupled plasma-optical emission spectrometry (ICP-OES) with simultaneous CCD detection system. Both techniques are suitable for sample analysis with detection limits of 1.0, 4.7, 3.3, 6.8, and 53 ng L{sup -1} using ETAAS and 12, 122, 3.4, 17, and 21 ng L{sup -1} using ICP-OES for Cd, Pb, Mn, Cu, and Fe, respectively. Relative standard deviations of the procedures ranged from 1.7 to 14% at the sub-{mu}g L{sup -1} concentration level. The accuracy of both methods was verified by analyzing various certified reference materials (river water, estuarine water, coastal and off-shore seawater). (orig.)

Radionuclide content of simulated and fully radioactive SRLLL waste glasses: comparison of results from ICP-MS, gamma spectrometry and alpha spectrometry

International Nuclear Information System (INIS)

Wolf, S.F.; Bates, J.K.

1995-01-01

We have measured the transuranic content of two transuranic=doped, simulated waste glasses, using inductively coupled plasma-mass spectrometry (ICP-MS), γ-spectrometry, and α-spectrometry. Average concentrations measured by each technique were within ± 10% of the as-doped concentrations. We also report the transuranic content of three fully radioactive SRL waste glasses that were determined using γ- and α-spectrometry measurements to deconvolute isobaric interferences present in the ICP-MS analyses

Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

International Nuclear Information System (INIS)

Yim, Yong Hyeon; Park, Ji Youn; Han, Myung Sub; Park, Mi Kyung; Kim, Byung Joo; Lim, Young Ran; Hwang, Eui Jin; So, Hun Young

2005-01-01

A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties

Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Yim, Yong Hyeon; Park, Ji Youn; Han, Myung Sub; Park, Mi Kyung; Kim, Byung Joo; Lim, Young Ran; Hwang, Eui Jin; So, Hun Young [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

2005-03-15

A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.

Comparison of elemental quantity by PIXE and ICP-MS and/or ICP-AES for NIST standards

International Nuclear Information System (INIS)

Saitoh, K.; Sera, K.; Gotoh, T.; Nakamura, M.

2002-01-01

Urban particulate matter (SRM 1648), Buffalo River sediment (SRM 2704) and pine needle (SRM 1575) standard reference materials prepared by the National Institute of Standards and Technology (NIST, USA) were analyzed by three multi-element analysis methods, i.e., particle induced X-ray emission (PIXE), inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES); values determined by those analysis methods were compared with certified and/or non-certified values of NIST samples. Values determined by PIXE were 70-120% relative to certified and/or non-certified values of NIST samples except for Co in the urban particulate matter, for V and Co in Buffalo River sediment and for Ni and Br in the pine needles samples. In particular, Al, K, Ca, Cr, Mn, Fe, Cu, Zn and Pb were 85-110% in all samples. On the other hand, Na and Fe values determined by ICP-MS were very much different from the certified values in all samples, but the other elements were 70-120%. As for ICP-AES, all elements except for Na were 80-100% in all samples. Comparing the values determined by PIXE and those determined by ICP-MS and/or ICP-AES, there was a slight difference between the samples, but the range was 75-120% except for Na, V, Fe and Co determined by ICP-MS and Na determined by ICP-AES, which was generally consistent with PIXE

Multielement trace analyses of SINQ materials by ICP-OES

Energy Technology Data Exchange (ETDEWEB)

Keil, R.; Schwikowski, M. [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

1997-09-01

Inductively Coupled Plasma Optical Emission Spectrometry was used to analyse 70 elements in various materials used for construction of the SINQ. Detection limits for individual elements depend strongly on the matrix and had to be determined separately. (author) 1 tab.

Determination of cadmium(II), cobalt(II), nickel(II), lead(II), zinc(II), and copper(II) in water samples using dual-cloud point extraction and inductively coupled plasma emission spectrometry

International Nuclear Information System (INIS)

Zhao, Lingling; Zhong, Shuxian; Fang, Keming; Qian, Zhaosheng; Chen, Jianrong

2012-01-01

Highlights: ► A dual-cloud point extraction (d-CPE) procedure was firstly developed for simultaneous pre-concentration and separation of trace metal ions combining with ICP-OES. ► The developed d-CPE can significantly eliminate the surfactant of Triton X-114 and successfully extend to the determination of water samples with good performance. ► The designed method is simple, high efficient, low cost, and in accordance with the green chemistry concept. - Abstract: A dual-cloud point extraction (d-CPE) procedure has been developed for simultaneous pre-concentration and separation of heavy metal ions (Cd 2+ , Co 2+ , Ni 2+ , Pb 2+ , Zn 2+ , and Cu 2+ ion) in water samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on forming complexes of metal ion with 8-hydroxyquinoline (8-HQ) into the as-formed Triton X-114 surfactant rich phase. Instead of direct injection or analysis, the surfactant rich phase containing the complexes was treated by nitric acid, and the detected ions were back extracted again into aqueous phase at the second cloud point extraction stage, and finally determined by ICP-OES. Under the optimum conditions (pH = 7.0, Triton X-114 = 0.05% (w/v), 8-HQ = 2.0 × 10 −4 mol L −1 , HNO 3 = 0.8 mol L −1 ), the detection limits for Cd 2+ , Co 2+ , Ni 2+ , Pb 2+ , Zn 2+ , and Cu 2+ ions were 0.01, 0.04, 0.01, 0.34, 0.05, and 0.04 μg L −1 , respectively. Relative standard deviation (RSD) values for 10 replicates at 100 μg L −1 were lower than 6.0%. The proposed method could be successfully applied to the determination of Cd 2+ , Co 2+ , Ni 2+ , Pb 2+ , Zn 2+ , and Cu 2+ ion in water samples.

Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Oliveira Souza, Sidnei de; Silvério Lopes da Costa, Silvânio; Santos, Dayane Melo; Santos Pinto, Jéssica dos; Garcia, Carlos Alexandre Borges

2014-01-01

An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg −1 for Mn to 77.3 mg kg −1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento — MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO 3 and H 2 O 2 ) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The ICP OES technique can be

Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Oliveira Souza, Sidnei de [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); Silvério Lopes da Costa, Silvânio [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); Coordenação de Química, Universidade Federal de Alagoas (UFAL), Campus Arapiraca, 57309-005, Arapiraca, AL (Brazil); Santos, Dayane Melo; Santos Pinto, Jéssica dos; Garcia, Carlos Alexandre Borges [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); and others

2014-06-01

An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg{sup −1} for Mn to 77.3 mg kg{sup −1} for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento — MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO{sub 3} and H{sub 2}O{sub 2}) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The

speciation of heavy metals in street dust samples from sakarya

African Journals Online (AJOL)

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techniques [26], such as flame atomic absorption spectroscopy (FAAS) [27, 28], inductively coupled plasma-optical emission (ICP-OES) [29] and mass spectrometry ... Analytical validation was conducted through the analysis of certified ...

Current role of ICP-MS in clinical toxicology and forensic toxicology: a metallic profile.

Science.gov (United States)

Goullé, Jean-Pierre; Saussereau, Elodie; Mahieu, Loïc; Guerbet, Michel

2014-08-01

As metal/metalloid exposure is inevitable owing to its omnipresence, it may exert toxicity in humans. Recent advances in metal/metalloid analysis have been made moving from flame atomic absorption spectrometry and electrothermal atomic absorption spectrometry to the multi-elemental inductively coupled plasma (ICP) techniques as ICP atomic emission spectrometry and ICP-MS. ICP-MS has now emerged as a major technique in inorganic analytical chemistry owing to its flexibility, high sensitivity and good reproducibility. This in depth review explores the ICP-MS metallic profile in human toxicology. It is now routinely used and of great importance, in clinical toxicology and forensic toxicology to explore biological matrices, specifically whole blood, plasma, urine, hair, nail, biopsy samples and tissues.

Comparison of 4 analytical techniques based on atomic spectrometry for the determination of total tin in canned foodstuffs

OpenAIRE

2011-01-01

Abstract Different techniques for the determination of total tin in beverage and canned food by atomic spectrometry were compared. The performance characteristics of Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Hydride Generation Inductively Coupled Plasma Atomic Emission Spectrometry (HG-ICP-AES), Electrothermal Atomization Atomic Absorption Spectrometry (ETA-AAS) and Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) were determined in term of linearity, ...

The synergistic effect in coal/biomass blend briquettes combustion on elements behavior in bottom ash using ICP-OES

Energy Technology Data Exchange (ETDEWEB)

Lazaroiu, G.; Frentiu, T.; Maescu, L.; Mihaltan, A.; Ponta, M.; Frentiu, M.; Cordos, E. [Universitatea Politehnica din Bucuresti, Bucharest (Romania)

2009-05-15

This paper focuses on the study of the synergistic effect in coal/biomass blend briquettes combustion on behavior of Al, As, Ba, Cd, Co. Cr, Cu, Fe, Ga, K, Mn, Mo, Ni, P, Pb, Si, V, W, Zn, Zr and characterization of raw materials and bottom ashes. The manufacturing of coal/biomass briquettes although not commonly used is an attractive approach, as briquettes combustion is more technologically advantageous than the fluidized bed combustion. In the same time this technology is a way to render valuable materials of low calorific power and results in diminishing polluting emission. Raw materials and briquettes from different blends of pitcoal/sawdust were subjected to combustion in a 55 kW-boiler. The total content of elements after digestion in the HNO{sub 3} - HF mixture and the content in water leachate at a solid/liquid ratio of 1:2 were determined both in raw materials and bottom ash by ICP-OES. The total content of elements was higher in pitcoal than in sawdust. The synergistic effect depends both on coal/biomass ratio in blend and element nature. The water leachable fraction of elements from ash decreased along with the increase of sawdust weight excepting macronutrients (K, P) and Si.

Determination of cadmium(II), cobalt(II), nickel(II), lead(II), zinc(II), and copper(II) in water samples using dual-cloud point extraction and inductively coupled plasma emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Zhao, Lingling; Zhong, Shuxian; Fang, Keming; Qian, Zhaosheng [College of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua 321004 (China); Chen, Jianrong, E-mail: cjr@zjnu.cn [College of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua 321004 (China); College of Geography and Environmental Sciences, Zhejiang Normal University, Jinhua 321004 (China)

2012-11-15

Highlights: Black-Right-Pointing-Pointer A dual-cloud point extraction (d-CPE) procedure was firstly developed for simultaneous pre-concentration and separation of trace metal ions combining with ICP-OES. Black-Right-Pointing-Pointer The developed d-CPE can significantly eliminate the surfactant of Triton X-114 and successfully extend to the determination of water samples with good performance. Black-Right-Pointing-Pointer The designed method is simple, high efficient, low cost, and in accordance with the green chemistry concept. - Abstract: A dual-cloud point extraction (d-CPE) procedure has been developed for simultaneous pre-concentration and separation of heavy metal ions (Cd{sup 2+}, Co{sup 2+}, Ni{sup 2+}, Pb{sup 2+}, Zn{sup 2+}, and Cu{sup 2+} ion) in water samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on forming complexes of metal ion with 8-hydroxyquinoline (8-HQ) into the as-formed Triton X-114 surfactant rich phase. Instead of direct injection or analysis, the surfactant rich phase containing the complexes was treated by nitric acid, and the detected ions were back extracted again into aqueous phase at the second cloud point extraction stage, and finally determined by ICP-OES. Under the optimum conditions (pH = 7.0, Triton X-114 = 0.05% (w/v), 8-HQ = 2.0 Multiplication-Sign 10{sup -4} mol L{sup -1}, HNO{sub 3} = 0.8 mol L{sup -1}), the detection limits for Cd{sup 2+}, Co{sup 2+}, Ni{sup 2+}, Pb{sup 2+}, Zn{sup 2+}, and Cu{sup 2+} ions were 0.01, 0.04, 0.01, 0.34, 0.05, and 0.04 {mu}g L{sup -1}, respectively. Relative standard deviation (RSD) values for 10 replicates at 100 {mu}g L{sup -1} were lower than 6.0%. The proposed method could be successfully applied to the determination of Cd{sup 2+}, Co{sup 2+}, Ni{sup 2+}, Pb{sup 2+}, Zn{sup 2+}, and Cu{sup 2+} ion in water samples.

Multi-proxy Reconstructions of the Eastern Equatorial Pacific: Measuring Sr/Ca, Ba/Ca, and Li/Mg in Modern Corals Using ICP-OES

Science.gov (United States)

Cheung, A. H.; Cole, J. E.; Vetter, L.; Jimenez, G.; Thompson, D. M.; Tudhope, A. W.

2017-12-01

Sea surface temperature (SST) in the Eastern Equatorial Pacific (EEP) exhibits large variability on multiple timescales. These variations are often related to modes of climate variability that exert significant influence on global climate, such as the El Niño Southern Oscillation. However, the short length and sparsity of instrumental data in the EEP limits our ability to discern changes in this region. Geochemical signals in corals can help extend instrumental data further back in time. While δ18O and Sr/Ca are the most commonly analyzed geochemical tracers of SST in corals, they often have site-specific complications. Several alternatives (e.g., Li/Mg) have been proposed to overcome these challenges, but have yet to be applied to long climate records, in part due to the cost and time required to measure these elements. Here, we develop a new method that uses Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) to analyze Li/Mg, Sr/Ca, and Ba/Ca ratios in coral aragonite. We apply this method to two Porites spp. corals collected from the northern Galapagos archipelago (Wolf and Darwin Islands). We specifically assess the fidelity of Li/Mg and Sr/Ca to reconstruct SST, and Ba/Ca to reconstruct upwelling conditions. Our results confirm that both Li/Mg and Sr/Ca track SST. We show that despite analytical noise, downcore reconstructions of Li/Mg have the potential to provide additional information about SST that is not present in reconstructions generated from Sr/Ca alone. Skeletal Ba/Ca shows little relationship with upwelling, perhaps because of the distance of our sites from the center of upwelling in the southern Galapagos. These results demonstrate the potential for analyzing Sr, Li, Ba, Mg simultaneously in corals with a cost- and time- efficient method, which may be applied to coral paleoclimate sites worldwide.

On-line system for preconcentration and determination of metals in vegetables by Inductively Coupled Plasma Optical Emission Spectrometry

International Nuclear Information System (INIS)

Bezerra, Marcos A.; Santos, Walter N.L. dos; Lemos, Valfredo A.; Korn, Maria das Gracas A.; Ferreira, Sergio L.C.

2007-01-01

A procedure has been developed for the simultaneous determination of trace amounts of cadmium, copper, chromium, nickel and lead in digested vegetable samples. The method involves solid-phase extraction of the metals using a minicolumn of Amberlite XAD-4 modified with dihydroxybenzoic acid (DHB) and detection by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The elution of the metals from minicolumn was performed with 1.0 mol L -1 hydrochloric acid. Variables associated with flow preconcentration system performance, such as pH, buffer concentration, eluent concentration and sampling flow rate, were optimized. The developed procedure provides enrichment factors of 100, 72, 16, 91 and 53, for cadmium, copper, chromium, nickel and lead, respectively. Detection limits (3σ B ) were 0.02 (Cd), 0.23 (Cu), 0.58 (Cr), 0.060 (Ni) and 0.54 (Pb) μg L -1 . The procedure was applied for determination of metals in samples of guarana and cabbage. The accuracy of the method was checked by the analysis of a certified reference material (NIST 1571, Orchard leaves). Results found were in agreement with certified values

Construcción y caracterización de un nuevo nebulizador múltiple para técnicas analíticas basadas en plasma (ICP-OES, ICP-MS y MP-AES).

OpenAIRE

Lúñez Fernández, Claudia

2016-01-01

En la siguiente memoria, se presenta la metodología para la construcción de un nuevo nebulizador múltiple, resultado de una serie de nebulizadores anteriores, los cuales se han ido mejorando para optimizar las características del aerosol generado y con ello los parámetros analíticos de calidad en la espectrometría de emisión atómica con plasma de microondas (MP-AES) y espectrometría de emisión óptica con plasma de acoplamiento inductivo (ICP-OES). Este nuevo nebulizador multiconducto presenta...

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.

Determination of cadmium(II), cobalt(II), nickel(II), lead(II), zinc(II), and copper(II) in water samples using dual-cloud point extraction and inductively coupled plasma emission spectrometry.

Science.gov (United States)

Zhao, Lingling; Zhong, Shuxian; Fang, Keming; Qian, Zhaosheng; Chen, Jianrong

2012-11-15

A dual-cloud point extraction (d-CPE) procedure has been developed for simultaneous pre-concentration and separation of heavy metal ions (Cd2+, Co2+, Ni2+, Pb2+, Zn2+, and Cu2+ ion) in water samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on forming complexes of metal ion with 8-hydroxyquinoline (8-HQ) into the as-formed Triton X-114 surfactant rich phase. Instead of direct injection or analysis, the surfactant rich phase containing the complexes was treated by nitric acid, and the detected ions were back extracted again into aqueous phase at the second cloud point extraction stage, and finally determined by ICP-OES. Under the optimum conditions (pH=7.0, Triton X-114=0.05% (w/v), 8-HQ=2.0×10(-4) mol L(-1), HNO3=0.8 mol L(-1)), the detection limits for Cd2+, Co2+, Ni2+, Pb2+, Zn2+, and Cu2+ ions were 0.01, 0.04, 0.01, 0.34, 0.05, and 0.04 μg L(-1), respectively. Relative standard deviation (RSD) values for 10 replicates at 100 μg L(-1) were lower than 6.0%. The proposed method could be successfully applied to the determination of Cd2+, Co2+, Ni2+, Pb2+, Zn2+, and Cu2+ ion in water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Determination of Pb in river water samples by inductively coupled plasma optical emission spectrometry after ultrasound-assisted co-precipitation with manganese dioxide

International Nuclear Information System (INIS)

Sousa Bispo, Marcia; Santos da Boa Morte, Elane; Korn das Gracas Andrade, Maria; Sena Gomes Teixeira, Leonardo; Korn, Mauro; Costa, Antonio Celso Spinola

2005-01-01

A simple and efficient procedure for separation and pre-concentration using ultrasound-assisted co-precipitation with manganese dioxide was developed for Pb determination by inductively coupled plasma optical emission spectrometry (ICP OES). The optimization process was carried out using a two-level factorial design and a Doehlert matrix. Three variables (i.e. concentration of oxidizing solution-KMnO 4 , concentration of MnSO 4 solution and time of ultrasonic irradiation) were used as factors in the optimization. The recoveries, based on the analysis of spiked samples, were between 90% and 105%, and the precision was ≤ 5%. The detection limit and quantification limit for Pb determination were 3.2 and 10.7 μg L -1 , respectively. The proposed method was applied for the determination of Pb in water samples from a river heavily polluted by industrial effluents. The recovery measured by analyte addition technique showed that the proposed pre-concentration method had good accuracy

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

International Nuclear Information System (INIS)

Bings, N.H.; Orlandini von Niessen, J.O.; Schaper, J.N.

2014-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Bings, N.H., E-mail: bings@uni-mainz.de; Orlandini von Niessen, J.O.; Schaper, J.N.

2014-10-01

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

Laser ablation inductively coupled plasma optical emission spectrometry for analysis of pellets of plant materials

Energy Technology Data Exchange (ETDEWEB)

Gomes, Marcos S. [Departamento de Química, Universidade Federal de São Carlos, Rod. Washington Luís, km 235, 13565-905 São Carlos, SP (Brazil); Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, Av. Centenário 303, 13416-000 Piracicaba, SP (Brazil); Schenk, Emily R. [Department of Chemistry and Biochemistry, Florida International University, Miami, FL (United States); International Forensic Research Institute, Florida International University, Miami, FL (United States); Santos, Dário [Departamento de Ciências Exatas e da Terra, Universidade Federal de São Paulo, Rua Professor Arthur Riedel 275, Diadema, SP (Brazil); Krug, Francisco José [Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, Av. Centenário 303, 13416-000 Piracicaba, SP (Brazil); Almirall, José R., E-mail: almirall@fiu.edu [Department of Chemistry and Biochemistry, Florida International University, Miami, FL (United States); International Forensic Research Institute, Florida International University, Miami, FL (United States)

2014-04-01

An evaluation of laser ablation inductively coupled plasma optical emission spectroscopy (LAICP OES) for the direct analysis of pelleted plant material is reported. Ground leaves of orange citrus, soy and sugarcane were comminuted using a high-speed ball mill, pressed into pellets and sampled directly with laser ablation and analyzed by ICP OES. The limits of detection (LODs) for the method ranged from as low as 0.1 mg kg{sup −1} for Zn to as high as 94 mg kg{sup −1} for K but were generally below 6 mg kg{sup −1} for most of the elements of interest. A certified reference material consisting of a similar matrix (NIST SRM 1547 peach leaves) was used to check the accuracy of the calibration and the reported method resulted in an average bias of ∼ 5% for all the elements of interest. The precision for the reported method ranged from as low as 4% relative standard deviation (RSD) for Mn to as high as 17% RSD for Zn but averaged ∼ 6.5% RSD for all the elements (n = 10). The proposed method was tested for the determination of Ca, Mg, P, K, Fe, Mn, Zn and B, and the results were in good agreement with those obtained for the corresponding acid digests by ICP-OES, no differences being observed by applying a paired t-test at the 95% confidence level. The reported direct solid sampling method provides a fast alternative to acid digestion that results in similar and appropriate analytical figures of merit with regard to sensitivity, accuracy and precision for plant material analysis. - Highlights: • An evaluation of LA-ICP-OES for the direct analysis of pelleted plant material is reported. • Orange citrus, soy and sugarcane plants were pressed into pellets and sampled directly. • The element menu consisted of Ca, Mg, P, K, Fe, Mn, Zn and B. • LODs for the method ranged from 0.1 mg kg{sup −1} for Zn to 94 mg kg{sup −1} for K. • The precision ranged from 4% RSD for Mn to 17% RSD for Zn (∼ 6.5% RSD average)

Determination of lead content in drilling fueled soil using laser induced spectral analysis and its cross validation using ICP/OES method.

Science.gov (United States)

Rehan, I; Gondal, M A; Rehan, K

2018-05-15

A detection system based on Laser Induced Breakdown Spectroscopy (LIBS) was designed, optimized, and successfully employed for the estimation of lead (Pb) content in drilling fueled soil (DFS) collected from oil field drilling areas in Pakistan. The concentration of Pb was evaluated by the standard calibration curve method as well as by using an approach based on the integrated intensity of strongest emission of an element of interest. Remarkably, our investigation clearly demonstrated that the concentration of Pb in drilling fueled soil collected at the exact drilling site was greater than the safe permissible limits. Furthermore, the Pb concentration was observed to decline with increasing distance away from the specific drilling point. Analytical determinations were carried out under the assumptions that laser generated plasma was optically thin and in local thermodynamic equilibrium (LTE). In order to improve the sensitivity of our LIBS detection system, various parametric dependence studies were performed. To further validate the precision of our LIBS results, the concentration of Pb present in the acquired samples were also quantified via a standard analytical tool like inductively coupled plasma/optical emission spectroscopy (ICP/OES). Both results were in excellent agreement, implying remarkable reliability for the LIBS data. Furthermore, the Limit of detection (LOD) of our LIBS system for Pb was estimated to be 125.14 mg L -1 . Copyright © 2018 Elsevier B.V. All rights reserved.

Multielement determination and speciation of major-to-ultratrace elements in green tea leaves by ICP-AES and ICP-MS

International Nuclear Information System (INIS)

Matsuura, Hirotaka; Hokura, Akiko; Haraguchi, Hiroki

2000-01-01

In order to investigate the multi-elemental composition of green tea leaves as well as chemical species in tea infusions, inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS) were used for elemental analysis and elemental speciation with the aid of size exclusion chromatography (SEC). As a result, the multielement determination of major-to-ultratrace elements in green tea leaves and green tea infusions was carried out by ICP-AES and ICP-MS. About 40 elements in these tea samples could be determined in a wide concentration range of over 8 orders of magnitude. The extraction efficiency of each element was estimated as the ratio of its concentration in tea infusion to that in tea leaves. It was found from the experimental results that the elements in tea leaves could be classified into three characteristic groups, depending on their extraction efficiencies. Furthermore, tea infusions were analyzed by a combined system of SEC, UV absorption detector, and ICP-AES (or ICP-MS) for the speciation of major-to-ultratrace elements. Most of the elements in tea infusions were found to be present as associated complexes with large organic molecules. (author)

Determination of aluminium, scandium and rare earth elements by emission flame spectrometry

International Nuclear Information System (INIS)

Otruba, V.; Sommer, L.

1989-01-01

Emission spectrometry in nitrous oxide-acetylene flames in combination with a highly resolving double monochromator and sensitive detecting system enables simple, sensitive and selective determinations of aluminium, scandium and all rare earth elements with exception of cerium in complicated matrices. Calibration plots are linear for a large concentration interval (≤ 100 μgxml -1 ), detection limits are in ngxml -1 level and RSD does not exceed 3% on the optimal concentration level of the particular element. The determination of Al, Sc, Eu and Yb showed particular advantages as to methods using ICP-spectrometry. (orig.)

Plutonium bioassay by inductively coupled plasma mass spectrometry ICP/MS

International Nuclear Information System (INIS)

Wyse, E.J.; Fisher, D.R.

1993-04-01

The determination of plutonium in urine poses several analytical challenges, e.g., detectability, matrix, etc. We have investigated the feasibility of analyzing plutonium in processed urine by inductively coupled plasma mass spectrometry (ICP/MS). The urine samples are first spiked with 244 Pu as a tracer and internal standard, then processed by co-precipitation and column chromatography using TRU-Spec trademark, an extraction resin. By enhancing ICP/MS detection capabilities via improved sample introduction and data acquisition efficiencies, an instrumental detection limit of 5 to 50 fg (0.3 to 3 fCi for 239 pu) is typically obtained, depending on the desired degree of quantitation. A brief summary of the analytical method as well as the basis for measuring radionuclides by ICP/MS are submitted; the separation procedure, methods of sample introduction, and data acquisition techniques are then highlighted

Application of cotton as a solid phase extraction sorbent for on-line preconcentration of copper in water samples prior to inductively coupled plasma optical emission spectrometry determination.

Science.gov (United States)

Faraji, Mohammad; Yamini, Yadollah; Shariati, Shahab

2009-07-30

Copper, as a heavy metal, is toxic for many biological systems. Thus, the determination of trace amounts of copper in environmental samples is of great importance. In the present work, a new method was developed for the determination of trace amounts of copper in water samples. The method is based on the formation of ternary Cu(II)-CAS-CTAB ion-pair and adsorption of it into a mini-column packed with cotton prior applying inductively coupled plasma optical emission spectrometry (ICP-OES). The experimental parameters that affected the extraction efficiency of the method such as pH, flow rate and volume of the sample solution, concentration of chromazurol S (CAS) and cethyltrimethylammonium bromide (CTAB) as well as type and concentration of eluent were investigated and optimized. The ion-pair (Cu(II)-CAS-CTAB) was quantitatively retained on the cotton under the optimum conditions, then eluted completely using a solution of 25% (v/v) 1-propanol in 0.5 mol L(-1) HNO(3) and directly introduced into the nebulizer of the ICP-OES. The detection limit (DL) of the method for copper was 40 ng L(-1) (V(sample)=100mL) and the relative standard deviation (R.S.D.) for the determination of copper at 10 microg L(-1) level was found to be 1.3%. The method was successfully applied to determine the trace amounts of copper in tap water, deep well water, seawater and two different mineral waters, and suitable recoveries were obtained (92-106%).

Use of fractional factorial design for optimization of digestion procedures followed by multi-element determination of essential and non-essential elements in nuts using ICP-OES technique.

Science.gov (United States)

Momen, Awad A; Zachariadis, George A; Anthemidis, Aristidis N; Stratis, John A

2007-01-15

Two digestion procedures have been tested on nut samples for application in the determination of essential (Cr, Cu, Fe, Mg, Mn, Zn) and non-essential (Al, Ba, Cd, Pb) elements by inductively coupled plasma-optical emission spectrometry (ICP-OES). These included wet digestions with HNO(3)/H(2)SO(4) and HNO(3)/H(2)SO(4)/H(2)O(2). The later one is recommended for better analytes recoveries (relative errortime, pre-digestion time, temperature of the hot plate and sample weight) were used for optimization of sample digestion procedures. For this purpose Plackett-Burman fractional factorial design, which involve eight experiments was adopted. The factors HNO(3) and H(2)O(2) volume, and the digestion time were found to be the most important parameters. The instrumental conditions were also optimized (using peanut matrix rather than aqueous standard solutions) considering radio-frequency (rf) incident power, nebulizer argon gas flow rate and sample uptake flow rate. The analytical performance, such as limits of detection (LOD<0.74mugg(-1)), precision of the overall procedures (relative standard deviation between 2.0 and 8.2%) and accuracy (relative errors between 0.4 and 11%) were assessed statistically to evaluate the developed analytical procedures. The good agreement between measured and certified values for all analytes (relative error <11%) with respect to IAEA-331 (spinach leaves) and IAEA-359 (cabbage) indicates that the developed analytical method is well suited for further studies on the fate of major elements in nuts and possibly similar matrices.

Determination of five kinds of impurity elements such as titanium in uranium titanium alloy by ICP-OES

International Nuclear Information System (INIS)

Jiao Yan; Hu Haihong

2010-01-01

New description is given of an ICP-OES method in which 5 impurities, Ti, Fe, Ni, Cu, and Al in U-Ti alloy can be determined simultaneously. Studying the dissolution of the sample preparation, separation condition of impurity elements; determining analysis of instrument line, detection limit and detection lower limit; eliminating the matrix effect of Ti and TiO 2 on the measurement of precipitation; standard addition method verify the method accuracy and precision. The results show: taking Uranium titanium alloys containing 0.1000 g sample, 5 kinds of elements Ti detection lower limits is 0.2-0.7 μg·g -1 , recovery were in the range of 98.8%-102.1%, and RSD'S found were less than 8%. The method of measurement proved is accurate and reliable. (authors)

Investigation of a measure of robustness in inductively coupled plasma mass spectrometry

Science.gov (United States)

Makonnen, Yoseif; Beauchemin, Diane

2015-01-01

In industrial/commercial settings where operators often have minimal expertise in inductively coupled plasma (ICP) mass spectrometry (MS), there is a prevalent need for a response factor indicating robust plasma conditions, which is analogous to the Mg II/Mg I ratio in ICP optical emission spectrometry (OES), whereby a Mg II/Mg I ratio of 10 constitutes robust conditions. While minimizing the oxide ratio usually corresponds to robust conditions, there is no specific target value that is widely accepted as indicating robust conditions. Furthermore, tuning for low oxide ratios does not necessarily guarantee minimal matrix effects, as they really address polyatomic interferences. From experiments, conducted in parallel for both MS and OES, there were some element pairs of similar mass and very different ionization potential that were exploited for such a purpose, the rationale being that, if these elements were ionized to the same extent, then that could be indicative of a robust plasma. The Be II/Li I intensity ratio was directly related to the Mg II/Mg I ratio in OES. Moreover, the 9Be+/7Li+ ratio was inversely related to the CeO+/Ce+ and LaO+/La+ oxide ratios in MS. The effects of different matrices (i.e. 0.01-0.1 M Na) were also investigated and compared to a conventional argon plasma optimized for maximum sensitivity. The suppression effect of these matrices was significantly reduced, if not eliminated in the case of 0.01 M Na, when the 9Be+/7Li+ ratio was around 0.30 on the Varian 820 MS instrument. Moreover, a very similar ratio (0.28) increased robustness to the same extent on a completely different ICP-MS instrument (PerkinElmer NEXION). Much greater robustness was achieved using a mixed-gas plasma with nitrogen in the outer gas and either nitrogen or hydrogen as a sheathing gas, as the 9Be+/7Li+ ratio was then around 1.70. To the best of our knowledge, this is the first report on using a simple analyte intensity ratio, 9Be+/7Li+, to gauge plasma robustness.

The Diagnosis of Plasma Parameters in Surface Alloying Technique by Optical Emission Spectrometry

International Nuclear Information System (INIS)

Fu Yabo; Zhang Yuefei; Chen Qiang; Zhang Guangqiu; Gao Yuan; Wang Jianzhong; Kui Xiaoyun

2006-01-01

Electron density (Ne) in a glow discharge plasma for the surface alloying technique is diagnosed by optical emission spectrometry (OES). With CH 4 as the feeding gas, Ne is obtained by comparing the Hβ spectrum according to the Stark broadening effect. It is noticed that Ne varies with the working pressures (30 Pa to 70 Pa) and cathode voltages (500 V to 1000 V), respectively. Due to an abnormal glow discharge, Ne is between 1.71x10 15 /cm 3 to 6.64x10 15 /cm 3 and increases rapidly with working gas pressures and cathode voltages. The results show that OES is a useful method to measure the plasma parameters in a surface alloying glow discharge plasma

Measurement of inclusion size by laser ablation ICP mass spectrometry

International Nuclear Information System (INIS)

Karasev, Andrey V.; Suito, Hideaki

2004-01-01

By using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), the measurement of particle size has been made for one component oxide (Al 2 O 3 and MgO) and multicomponent oxide (12CaO·7Al 2 O 3 and CaO-Al 2 O 3 -MgO) located on surface of iron or glass sample. The method of particle size estimation by LA-ICP-MS has been developed coupled with a new method of making samples with particles. The size calibration lines for Al 2 O 3 , MgO and CaO particles have been obtained. The results of particle size measurement by LA-ICP-MS are compared with those by SEM and single-particle optical sensing (SPOS) methods. It was confirmed that LA-ICP-MS has the perspective to be used for the quick measurement of inclusion composition and size in metal and other materials. The size frequency distributions of Al 2 O 3 particles measured by LA-ICP-MS in iron samples with particles agree reasonably well with those by SEM and SPOS in the range of particle diameter from 2 to 20 μm. The size of Al 2 O 3 , MgO and complex oxide (12CaO·7Al 2 O 3 and CaO-Al 2 O 3 -MgO) particles measured by LA-ICP-MS is in good agreement with that by SEM in the range of particle diameter from 10 to 40 μm. (author)

Depth-profile analysis of thermoelectric layers on Si wafers by pulsed r.f. glow discharge time-of-flight mass spectrometry

International Nuclear Information System (INIS)

Reinsberg, K.-G.; Schumacher, C.; Tempez, A.; Nielsch, K.; Broekaert, J.A.C.

2012-01-01

In this work the depth-profile analysis of thermoelectric layers deposited on Au and Cr covered Si wafers with the aid of pulsed radiofrequency glow discharge time-of-flight mass spectrometry (pulsed RF-GD-TOFMS also called plasma profiling TOFMS (PP-TOFMS™)) is described. For thermoelectric materials the depth resolutions obtained with both PP-TOFMS and secondary ion mass spectrometry (SIMS) are shown to be well comparable and in the order of the roughness of the corresponding layers (between 20 and 3700 nm). With both methods a direct solid analysis without any preparation steps is possible. In addition, the analysis of the samples with PP-TOFMS proved to be faster by a factor of 26 compared to SIMS, as sputtering rates were found to be 80 nm s −1 and 3 nm s −1 , respectively. For the analyzed samples the results of PP-TOFMS and SIMS show that a homogeneous deposition was obtained. Quantitative results for all samples could also be obtained directly by PP-TOFMS when the stoichiometry of one sample was determined beforehand for instance by inductively coupled plasma optical emission spectrometry (ICP-OES) and scanning electron microscopy energy dispersive X-ray fluorescence spectrometry (SEM-EDX). For Bi 2 Te 3 the standard deviation for the main component concentrations within one sample then is found to be between 1.1% and 1.9% and it is 3.6% from sample to sample. For Sb 2 Te 3 the values within one sample are from 1.7% to 4.2% and from sample to sample 5.3%, respectively. - Highlights: ► Depth resolution in sub micrometer size by glow discharge mass spectrometry. ► Bi and Sb telluride layers composition with GD-TOF-MS, ICP-OES and SEM-EDX agree. ► Homogeneities of layers measured with GD-TOF-MS and SIMS agree.

ICP-MS determination of boron: method optimization during preparation of graphite reference material for boron

International Nuclear Information System (INIS)

Granthali, S.K.; Shailaja, P.P.; Mainsha, V.; Venkatesh, K.; Kallola, K.S.; Sanjukta, A.K.

2017-01-01

Graphite finds widespread use in nuclear reactors as moderator, reflector, and fuel fabricating components because of its thermal stability and integrity. The manufacturing process consists of various mixing, moulding and baking operations followed by heat-treatment between 2500 °C and 3000 °C. The high temperature treatment is required to drive the amorphous carbon-to-graphite phase transformation. Since synthetic graphite is processed at high temperature, impurity concentrations in the precursor carbon get significantly reduced due to volatilization. However boron may might partly gets converted into boron carbide at high temperatures in the carbon environment of graphite and remains stable (B_4C: boiling point 3500 °C) in the matrix. Literature survey reveals the use of various methods for determination of boron. Previously we have developed a method for determination of boron in graphite electrodes using inductively coupled plasma mass spectrometry (ICP-MS). The method involves removal of graphite matrix by ignition of the sample at 800°C in presence of saturated barium hydroxide solution to prevent the loss of boron. Here we are reporting a modification in the method by using calcium carbonate in place of barium hydroxide and using beryllium (Be) as an internal standard, which resulted in a better precession. The method was validated by spike recovery experiments as well as using another technique viz. Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The modified method was applied in evaluation of boron concentration in the graphite reference material prepared

Sequential cloud point extraction for the speciation of mercury in seafood by inductively coupled plasma optical emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Li Yingjie [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)], E-mail: binhu@whu.edu.cn

2007-10-15

A novel nonchromatographic speciation technique for the speciation of mercury by sequential cloud point extraction (CPE) combined with inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. The method based on Hg{sup 2+} was complexed with I{sup -} to form HgI{sub 4}{sup 2-}, and the HgI{sub 4}{sup 2-} reacted with the methyl green (MG) cation to form hydrophobic ion-associated complex, and the ion-associated complex was then extracted into the surfactant-rich phase of the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114), which are subsequently separated from methylmercury (MeHg{sup +}) in the initial solution by centrifugation. The surfactant-rich phase containing Hg(II) was diluted with 0.5 mol L{sup -1} HNO{sub 3} for ICP-OES determination. The supernatant is also subjected to the similar CPE procedure for the preconcentration of MeHg{sup +} by the addition of a chelating agent, ammonium pyrrolidine dithiocarbamate (APDC), in order to form water-insolvable complex with MeHg{sup +}. The MeHg{sup +} in the micelles was directly analyzed after disposal as describe above. Under the optimized conditions, the extraction efficiency was 93.5% for Hg(II) and 51.5% for MeHg{sup +} with the enrichment factor of 18.7 for Hg(II) and 10.3 for MeHg{sup +}, respectively. The limits of detection (LODs) were 56.3 ng L{sup -1} for Hg(II) and 94.6 ng L{sup -1} for MeHg{sup +} (as Hg) with the relative standard deviations (RSDs) of 3.6% for Hg(II) and 4.5% for MeHg{sup +} (C = 10 {mu}g L{sup -1}, n = 7), respectively. The developed technique was applied to the speciation of mercury in real seafood samples and the recoveries for spiked samples were found to be in the range of 93.2-108.7%. For validation, a certified reference material of DORM-2 (dogfish muscle) was analyzed and the determined values are in good agreement with the certified values.

Sequential cloud point extraction for the speciation of mercury in seafood by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Li Yingjie; Hu Bin

2007-01-01

A novel nonchromatographic speciation technique for the speciation of mercury by sequential cloud point extraction (CPE) combined with inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. The method based on Hg 2+ was complexed with I - to form HgI 4 2- , and the HgI 4 2- reacted with the methyl green (MG) cation to form hydrophobic ion-associated complex, and the ion-associated complex was then extracted into the surfactant-rich phase of the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114), which are subsequently separated from methylmercury (MeHg + ) in the initial solution by centrifugation. The surfactant-rich phase containing Hg(II) was diluted with 0.5 mol L -1 HNO 3 for ICP-OES determination. The supernatant is also subjected to the similar CPE procedure for the preconcentration of MeHg + by the addition of a chelating agent, ammonium pyrrolidine dithiocarbamate (APDC), in order to form water-insolvable complex with MeHg + . The MeHg + in the micelles was directly analyzed after disposal as describe above. Under the optimized conditions, the extraction efficiency was 93.5% for Hg(II) and 51.5% for MeHg + with the enrichment factor of 18.7 for Hg(II) and 10.3 for MeHg + , respectively. The limits of detection (LODs) were 56.3 ng L -1 for Hg(II) and 94.6 ng L -1 for MeHg + (as Hg) with the relative standard deviations (RSDs) of 3.6% for Hg(II) and 4.5% for MeHg + (C = 10 μg L -1 , n = 7), respectively. The developed technique was applied to the speciation of mercury in real seafood samples and the recoveries for spiked samples were found to be in the range of 93.2-108.7%. For validation, a certified reference material of DORM-2 (dogfish muscle) was analyzed and the determined values are in good agreement with the certified values

Preliminary studies of laser-induced breakdown spectrometry for the determination of Ba, Cd, Cr and Pb in toys

International Nuclear Information System (INIS)

Godoi, Quienly; Santos, Dario; Nunes, Lidiane C.; Leme, Flavio O.; Rufini, Iolanda A.; Agnelli, Jose A.M.; Trevizan, Lilian C.; Krug, Francisco J.

2009-01-01

The performance of laser-induced breakdown spectrometry (LIBS) for the determination of Ba, Cd, Cr and Pb in toys has been evaluated by using a Nd:YAG laser operating at 1064 nm and an Echelle spectrometer with intensified charge-coupled device detector. Samples were purchased in different cities of Sao Paulo State market and analyzed directly without sample preparation. Laser-induced breakdown spectrometry experimental conditions (number of pulses, delay time, integration time gate and pulse energy) were optimized by using a Doehlert design. Laser-induced breakdown spectrometry signals correlated reasonably well with inductively coupled plasma optical emission spectrometry (ICP OES) concentrations after microwave-assisted acid digestion of selected samples. Thermal analysis was used for polymer identification and scanning electron microscopy to visualize differences in crater geometry of different polymers employed for toy fabrication. Results indicate that laser-induced breakdown spectrometry can be proposed as a rapid screening method for investigation of potentially toxic elements in toys. The unique application of laser-induced breakdown spectrometry for identification of contaminants in successive layers of ink and polymer is also demonstrated.

Improved sample preparation method for environmental plutonium analysis by ICP-SFMS and alpha-spectrometry

International Nuclear Information System (INIS)

Varga, Z.; Stefanka, Z.; Suranyi, G.; Vajda, N.

2007-01-01

A rapid and simple sample preparation method for plutonium determination in environmental samples by inductively coupled plasma sector field mass spectrometry (ICP-SFMS) and alpha-spectrometry is described. The developed procedure involves a selective CaF 2 co-precipitation for preconcentration followed by extraction chromatographic separation. The proposed method effectively eliminates the possible interferences in mass spectrometric analysis and also removes interfering radionuclides that may disturb alpha-spectrometric measurement. For 239 Pu, 240 Pu and 241 Pu limits of detection of 9.0 fg x g -1 (0.021 mBq), 1.7 fg x g -1 (0.014 mBq) and 3.1 fg x g -1 (11.9 mBq) were achieved by ICP-SFMS, respectively, and 0.02 mBq by alpha-spectrometry. Results of certified reference materials agreed well with the recommended values. (author)

Multielemental fingerprinting as a tool for authentication of organic wheat, barley, faba bean, and potato

DEFF Research Database (Denmark)

Laursen, Kristian Holst; Schjørring, Jan Kofod; Olesen, Jørgen Eivind

2011-01-01

The multielemental composition of organic and conventional winter wheat, spring barley, faba bean, and potato was analyzed with inductively coupled plasma−optical emission spectrometry (ICP-OES) and −mass spectrometry (ICP-MS). The crops were cultivated in two years at three geographically...... different field locations, each accommodating one conventional and two organic cropping systems. The conventional system produced the highest harvest yields for all crops except the nitrogen-fixing faba bean, whereas the dry matter content of each crop was similar across systems. No systematic differences...

Determination of Th and REE in columbite - tantalite samples by ICP-OES

International Nuclear Information System (INIS)

Hanuman, V.V.; Khorge, C.R.; Radhamai, R.; Nair, Sajitha; Srivastava, P.K.

2007-01-01

A simple method of decomposition and separation of Th and REE in columbite- tantalite is developed for determination by ICP- OES. The sample is decomposed with hydrofluoric and hydrochloric acid in presence of little sulphuric acid to avoid drying on water bath. Th and rare earths are separated as fluoride together with undecomposed sample. The residue is fused with a 1: 1 mixture of sodium di hydrogen orthophosphate and sodium pyrophosphate. The melt is dissolved in water for measurement. Nitric acid is found unsuitable due to loss in Ce in some of the samples. Matrix elements (more than 97.5) are removed in single step by both the treatments. The free cassiterite present in samples is not attacked during acid digestion. However, the same is easily decomposed in fusion. U (IV) is also precipitated along with Th and REE when hydrochloric acid is used. As expected uranium is lost when nitric acid is used. The results are compared with existing well-established procedure involving peroxide fusion for decomposition; hydroxide and fluoride precipitation separation. Both the methods yielded comparable result. The method is simple, comparatively rapid and suitable for routine application for determination of REE , Th and U(IV) content. The RSD of the method was found to be in the range of 1- 1.5% for various elements. (author)

Flow injection analysis in inductively coupled plasma spectrometry

International Nuclear Information System (INIS)

Rosias, Maria F.G.G.

1995-10-01

The main features of flow injection analysis (FIA) as contribution to the inductively coupled plasma (Icp) spectrometry are described. A systematic review of researches using the combined FIA-Icp and the benefits of this association are presented. Flow systems were proposed to perform on-line Icp solution management for multielemental determination by atomic emission spectrometry (Icp-AES) or mass spectrometry. The inclusion of on-line ion exchangers in flow systems for matrix separation and/or analyte preconcentration are presented. Together with those applications the new advent of instruments with facilities for multielement detection on flow injection signals are described. (author). 75 refs., 19 figs

IBA and ICP-OES determination of trace elements in indigenous medicinal herbs and their extracts on the infertility in the human male reproductive system

Energy Technology Data Exchange (ETDEWEB)

Mars, J.A.; Fisher, D.; Henkel, R. [Department of Medical Bioscience, Universily of the Weslern Cape, Bellville (South Africa); Weilz, F. [Department of Biodiversily and Conservation Biology, University of the Weslern Cape, Bellville (South Africa)

2013-07-01

Full text: The abnormality of infertility in humans is biologically defined (Mader, 2004; Wood, 1994; Ellison, 2001) as the inability of a species to reproduce its own kind after period of 12 month of unprotected sexual intercourse/copulation. It is however difficult when one wishes to quantify the occurrence of infertility, since it is seldom expressed explicitly, but mostly in conjunction with population growth dynamics which include socio-economic factors. Various plants (herbs) have been used as treatment for infertility. These plants however have not yet been scientifically analysed. In this paper we determined the major and trace element composition of Typha capensis (rhizome and leaves) Cissampe/os capensis (Ieaves) and Hermannia cilliata, which were sourced from the Cape Flats Nature Reserve, Bellville, Western Cape Province, South Africa. The trace element concentration determination are at time cumbersome, especially when destructive analytical methods such as ICP-OES are used. For our determination, the various samples were freeze-dried. Part of the freeze-dried sample was used for ICP-OES and the other for PIXE analysis. For PIXE the dried sample was pressed into a pellet, then coated with a layer of carbon and irradiated with a 3 MeV proton beam. We report on the trace element content of the various parts of the plant and comment on the applicability of the part in male infertility. (author)

IBA and ICP-OES determination of trace elements in indigenous medicinal herbs and their extracts on the infertility in the human male reproductive system

International Nuclear Information System (INIS)

Mars, J.A.; Fisher, D.; Henkel, R.; Weilz, F.

2013-01-01

Full text: The abnormality of infertility in humans is biologically defined (Mader, 2004; Wood, 1994; Ellison, 2001) as the inability of a species to reproduce its own kind after period of 12 month of unprotected sexual intercourse/copulation. It is however difficult when one wishes to quantify the occurrence of infertility, since it is seldom expressed explicitly, but mostly in conjunction with population growth dynamics which include socio-economic factors. Various plants (herbs) have been used as treatment for infertility. These plants however have not yet been scientifically analysed. In this paper we determined the major and trace element composition of Typha capensis (rhizome and leaves) Cissampe/os capensis (Ieaves) and Hermannia cilliata, which were sourced from the Cape Flats Nature Reserve, Bellville, Western Cape Province, South Africa. The trace element concentration determination are at time cumbersome, especially when destructive analytical methods such as ICP-OES are used. For our determination, the various samples were freeze-dried. Part of the freeze-dried sample was used for ICP-OES and the other for PIXE analysis. For PIXE the dried sample was pressed into a pellet, then coated with a layer of carbon and irradiated with a 3 MeV proton beam. We report on the trace element content of the various parts of the plant and comment on the applicability of the part in male infertility. (author)

Determination of rare earth elements by liquid chromatography/inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Yoshida, K.; Haraguchi, H.

1984-01-01

Inductively coupled plasma atomic emission spectrometry (ICP-AES) interfaced with high-performance liquid chromatography (HPLC) has been applied to the determination of rare earth elements. ICP-AES was used as an element-selective detector for HPLC. The separation of rare earth elements with HPLC helped to avoid erroneous analytical results due to spectral interferences. Fifteen rare earth elements (Y and 14 lanthanides) were determined selectively with the HPLC/ICP-AES system using a concentration gradient method. The detection limits with the present HPLC/ICP-AES system were about 0.001-0.3 μg/mL with a 100-μL sample injection. The calibration curves obtained by the peak height measurements showed linear relationships in the concentration range below 500 μg/mL for all rare earth elements. A USGS rock standard sample, rare earth ores, and high-purity lanthanide reagents (>99.9%) were successfully analyzed without spectral interferences

Direct isotope ratio measurement of uranium metal by emission spectrometry on a laser-produced plasma

International Nuclear Information System (INIS)

Pietsch, W.; Petit, A.; Briand, A.

1995-01-01

The method of Optical Emission Spectrometry on a Laser-Produced Plasma (OES/LPP) at reduced pressure has been studied for the determination of the uranium isotope ratio ( 235 U/ 238 U). Spectral profiles of the investigated transition U-II 424.437 nm show the possibility to obtain an isotopic spectral resolution in a laser-produced plasma under exactly defined experimental conditions. Spectroscopic data and results are presented. (author)

Determination of trace elements in seawater by air-flow injection/ICP-MS with chelating resin preconcentration

International Nuclear Information System (INIS)

Lee, Kyue-Hyung; Ohshima, Mitsuko; Motomizu, Shoji

2002-01-01

Multielement determination of major to trace metals in a deep seawater malt was accomplished by inductively coupled plasma-mass spectrometry (ICP-MS) together with inductively coupled plasma-atomic emission spectrometry (ICP-AES). Major elements, such as Na, K, Mg, and Ca, were measured by ICP-AES and normal continuos nebulization ICP-MS after sample dilution by 10 3 -10 6 fold. Fifteen trace elements in the concentrated metal solutions pretreated with cation-exchange resin or chelating resin could be simultaneously determined by air-flow injection/ICP-mass spectrometry (AFI/ICP-MS). Since the injection volume for AFI/ICP-MS was 25 μl, final samples volumes less than 500 μl were enough for several replicate measurements. Three different preconcentration methods assisted with AFI/ICP-MS were examined and could be successfully applied to a deep seawater malt. The analytical results of rate earth elements (REEs) and Co, Ni, Cu, Zn, Cd, and Pb obtained by AFI/ICP-MS coupled with disk filtration method using iminodiacetate (IDA)-type chelating resin were favorably agreed with the data obtained by AFI/ICP-MS coupled with column preconcentration method using chitosan-based chelating resin. (author)

Multielement analytical procedure coupling INAA, ICP-MS and ICP-AES: Application to the determination of major and trace elements in sediment samples of the Bouregreg river (Morocco)

International Nuclear Information System (INIS)

Bounouira, H.; CEA - CNRS/UMR, Centre de Saclay, 91 - Gif sur Yvette; Choukri, A.; Hakam, O.K.; Cherkaoui, R.; Gaudry, A.; Delmas, R.; Mariet, C.; Chakiri, S.

2008-01-01

Instrumental neutron activation analysis (INAA), inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) were used for the determination of major and trace elements in sediment samples of the Bouregreg river (Morocco). The reliability of the results was checked, by using IAEA Soil-7 certified reference material. Results obtained by the three techniques were compared to control digestions efficiencies. A general good agreement was found between INAA and both ICP-MS and ICP-AES after alkaline fusion (ICPf). The ICP-MS technique used after acid attack (ICPa) was satisfactory for a few elements. A principal component analysis (PCA) has been used for analyzing the variability of concentrations, and defining the most influential sites with respect to the general variation trends. Three groups of elements could be distinguished. For these groups a normalization of concentrations to the central element concentration (that means Mn, Si or Al) is proposed. (author)

Evaluation of a new optic-enabled portable X-ray fluorescence spectrometry instrument for measuring toxic metals/metalloids in consumer goods and cultural products

Science.gov (United States)

Guimarães, Diana; Praamsma, Meredith L.; Parsons, Patrick J.

2016-08-01

X-ray fluorescence spectrometry (XRF) is a rapid, non-destructive multi-elemental analytical technique used for determining elemental contents ranging from percent down to the μg/g level. Although detection limits are much higher for XRF compared to other laboratory-based methods, such as inductively coupled plasma mass spectrometry (ICP-MS), ICP-optical emission spectrometry (OES) and atomic absorption spectrometry (AAS), its portability and ease of use make it a valuable tool, especially for field-based studies. A growing necessity to monitor human exposure to toxic metals and metalloids in consumer goods, cultural products, foods and other sample types while performing the analysis in situ has led to several important developments in portable XRF technology. In this study, a new portable XRF analyzer based on the use of doubly curved crystal optics (HD Mobile®) was evaluated for detecting toxic elements in foods, medicines, cosmetics and spices used in many Asian communities. Two models of the HD Mobile® (a pre-production and a final production unit) were investigated. Performance parameters including accuracy, precision and detection limits were characterized in a laboratory setting using certified reference materials (CRMs) and standard solutions. Bias estimates for key elements of public health significance such as As, Cd, Hg and Pb ranged from - 10% to 11% for the pre-production, and - 14% to 16% for the final production model. Five archived public health samples including herbal medicine products, ethnic spices and cosmetic products were analyzed using both XRF instruments. There was good agreement between the pre-production and final production models for the four key elements, such that the data were judged to be fit-for-purpose for the majority of samples analyzed. Detection of the four key elements of interest using the HD Mobile® was confirmed using archived samples for which ICP-OES data were available based on digested sample materials. The HD

Determination of hafnium at the 10−4% level (relative to zirconium content) using neutron activation analysis, inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Smolik, Marek; Polkowska-Motrenko, Halina; Hubicki, Zbigniew; Jakóbik-Kolon, Agata; Danko, Bożena

2014-01-01

Graphical abstract: -- Highlights: •We worked out ICP-MS method of Hf determination in Zr and Zr compounds. •We used NAA method as reference one. •We obtained pure zirconium matrix by ion exchange (Diphonix ® resin). •These permit to determine ≥1 × 10 −4 % Hf in Zr sample by ICP MS with good precision and accuracy. -- Abstract: Hafnium at the very low level of 1–8 ppm (in relation to zirconium) was determined in zirconium sulfate solutions (originating from investigations of the separation of ca. 44 ppm Hf from zirconium by means of the ion exchange method) by using three independent methods: inductively coupled plasma mass spectrometry (ICP MS), neutron activation analysis (NAA) and inductively coupled plasma atomic emission spectrometry (ICP-AES). The results of NAA and ICP MS determinations were consistent with each other across the entire investigated range (the RSD of both methods did not exceed 38%). The results of ICP-AES determination were more diverse, particularly at less than 5 ppm Hf (RSD was significantly higher: 29–253%). The ion exchange method exploiting Diphonix ® resin proved sufficient efficiency in Zr–Hf separation when the initial concentration ratio of the elements ([Zr] 0 /[Hf] 0 ) ranged from 1200 to ca. 143,000

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

International Nuclear Information System (INIS)

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

2007-01-01

A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO 3 ) 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)

Preconcentration of heavy metals on activated carbon and their determination in fruits by inductively coupled plasma optical emission spectrometry.

Science.gov (United States)

Feist, Barbara; Mikula, Barbara

2014-03-15

A method of separation and preconcentration of cadmium, cobalt, copper, nickel, lead, and zinc at trace level using activated carbon is proposed. Activated carbon with the adsorbed trace metals was mineralised using a high-pressure microwave mineraliser. The heavy metals were determined after preconcentration by inductively coupled plasma optical emission spectrometry (ICP-OES). The influence of several parameters, such as pH, sorbent mass, shaking time was examined. Moreover, effects of inorganic matrix on recovery of the determined elements were studied. The experiment shows that foreign ions did not influence recovery of the determined elements. The detection limits (DL) of Cd, Co, Cu, Ni, Pb, and Zn were 0.17, 0.19, 1.60, 2.60, 0.92 and 1.50 μg L(-)(1), respectively. The recovery of the method for the determined elements was better than 95% with relative standard deviation from 1.3% to 3.7%. The preconcentration factor was 80. The proposed method was applied for determination of Cd, Co, Cu, Ni, Pb, and Zn in fruits materials. Accuracy of the proposed method was verified using certified reference material (NCS ZC85006 Tomato). Copyright © 2013 Elsevier Ltd. All rights reserved.

Recent advances in nuclear techniques for environmental radioactivity monitoring

International Nuclear Information System (INIS)

Kumar, Ajay; Tripathi, R.M.

2016-01-01

The environmental radioactivity monitoring was first started in the late 1950s following the global fallout from testing of nuclear weapons in the atmosphere. Nuclear analytical techniques are generally classified into two categories: destructive and non-destructive. Destructive techniques are carried out through several analytical methods such as α-spectrometry, liquid Scintillation counting system, solid state nuclear track detector, spectrophotometry, fluorimetry, atomic absorption spectrometry (AAS), inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma optical emission spectrometry (ICP-OES), chromatography techniques, electro-analytical techniques etc. However, nondestructive methods include gamma spectrometry, X-Ray fluorescence (XRF) spectrometry, neutron activation analysis (NAA) etc. The development of radiochemical methods and measurement techniques using alpha and gamma spectrometry have been described in brief

Development of routines for simultaneous in situ chemical composition and stable Si isotope ratio analysis by femtosecond laser ablation inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Frick, Daniel A., E-mail: dfrick@gfz-potsdam.de [GFZ German Research Centre for Geosciences, 14473 Potsdam (Germany); Schuessler, Jan A. [GFZ German Research Centre for Geosciences, 14473 Potsdam (Germany); Blanckenburg, Friedhelm von [GFZ German Research Centre for Geosciences, 14473 Potsdam (Germany); Institute of Geological Science, Freie Universität Berlin, 12249 Berlin (Germany)

2016-09-28

Stable metal (e.g. Li, Mg, Ca, Fe, Cu, Zn, and Mo) and metalloid (B, Si, Ge) isotope ratio systems have emerged as geochemical tracers to fingerprint distinct physicochemical reactions. These systems are relevant to many Earth Science questions. The benefit of in situ microscale analysis using laser ablation (LA) over bulk sample analysis is to use the spatial context of different phases in the solid sample to disclose the processes that govern their chemical and isotopic compositions. However, there is a lack of in situ analytical routines to obtain a samples' stable isotope ratio together with its chemical composition. Here, we evaluate two novel analytical routines for the simultaneous determination of the chemical and Si stable isotope composition (δ{sup 30}Si) on the micrometre scale in geological samples. In both routines, multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) is combined with femtosecond-LA, where stable isotope ratios are corrected for mass bias using standard-sample-bracketing with matrix-independent calibration. The first method is based on laser ablation split stream (LASS), where the laser aerosol is split and introduced simultaneously into both the MC-ICP-MS and a quadrupole ICP-MS. The second method is based on optical emission spectroscopy using direct observation of the MC-ICP-MS plasma (LA-MC-ICP-MS|OES). Both methods are evaluated using international geological reference materials. Accurate and precise Si isotope ratios were obtained with an uncertainty typically better than 0.23‰, 2SD, δ{sup 30}Si. With both methods major element concentrations (e.g., Na, Al, Si, Mg, Ca) can be simultaneously determined. However, LASS-ICP-MS is superior over LA-MC-ICP-MS|OES, which is limited by its lower sensitivity. Moreover, LASS-ICP-MS offers trace element analysis down to the μg g{sup −1}-range for more than 28 elements due to lower limits of detection, and with typical uncertainties better than 15%. For in situ

Development of routines for simultaneous in situ chemical composition and stable Si isotope ratio analysis by femtosecond laser ablation inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Frick, Daniel A.; Schuessler, Jan A.; Blanckenburg, Friedhelm von

2016-01-01

Stable metal (e.g. Li, Mg, Ca, Fe, Cu, Zn, and Mo) and metalloid (B, Si, Ge) isotope ratio systems have emerged as geochemical tracers to fingerprint distinct physicochemical reactions. These systems are relevant to many Earth Science questions. The benefit of in situ microscale analysis using laser ablation (LA) over bulk sample analysis is to use the spatial context of different phases in the solid sample to disclose the processes that govern their chemical and isotopic compositions. However, there is a lack of in situ analytical routines to obtain a samples' stable isotope ratio together with its chemical composition. Here, we evaluate two novel analytical routines for the simultaneous determination of the chemical and Si stable isotope composition (δ 30 Si) on the micrometre scale in geological samples. In both routines, multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) is combined with femtosecond-LA, where stable isotope ratios are corrected for mass bias using standard-sample-bracketing with matrix-independent calibration. The first method is based on laser ablation split stream (LASS), where the laser aerosol is split and introduced simultaneously into both the MC-ICP-MS and a quadrupole ICP-MS. The second method is based on optical emission spectroscopy using direct observation of the MC-ICP-MS plasma (LA-MC-ICP-MS|OES). Both methods are evaluated using international geological reference materials. Accurate and precise Si isotope ratios were obtained with an uncertainty typically better than 0.23‰, 2SD, δ 30 Si. With both methods major element concentrations (e.g., Na, Al, Si, Mg, Ca) can be simultaneously determined. However, LASS-ICP-MS is superior over LA-MC-ICP-MS|OES, which is limited by its lower sensitivity. Moreover, LASS-ICP-MS offers trace element analysis down to the μg g −1 -range for more than 28 elements due to lower limits of detection, and with typical uncertainties better than 15%. For in situ

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

International Nuclear Information System (INIS)

Montaser, A.

1993-01-01

In this research, 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. During the period January 1993--December 1993, emphasis was placed on (a) analytical investigations of atmospheric-pressure helium inductively coupled plasma (He ICP) that are suitable for atomization, excitation, and ionization of elements possessing high excitation and ionization energies; (b) simulation and computer modeling of plasma sources to predict their structure and fundamental and analytical properties without incurring the enormous cost of experimental studies; (c) spectrosopic imaging and diagnostic studies of high-temperature plasmas; (d) fundamental studies of He ICP discharges and argon-nitrogen plasma by high-resolution Fourier transform spectrometry; and (e) fundamental and analytical investigation of new, low-cost devices as sample introduction systems for atomic spectrometry and examination of new diagnostic techniques for probing aerosols. Only the most important achievements are included in this report to illustrate progress and obstacles. Detailed descriptions of the authors' investigations are outlined in the reprints and preprints that accompany this report. The technical progress expected next year is briefly described at the end of this report

Levels of Major and Minor Elements in Some Commercial Fruit ...

African Journals Online (AJOL)

Purpose: To evaluate the macro- and micro-nutrient elements of some commercially available fruit juices in Serbia. Methods: Inductively coupled plasma optical emission spectrometry (ICP-OES) technique was employed for determination of the major and minor elements in samples of two different types of fruit juices - clear ...

Liquid electrode plasma-optical emission spectrometry combined with solid-phase preconcentration for on-site analysis of lead.

Science.gov (United States)

Barua, Suman; Rahman, Ismail M M; Alam, Iftakharul; Miyaguchi, Maho; Sawai, Hikaru; Maki, Teruya; Hasegawa, Hiroshi

2017-08-15

A relatively rapid and precise method is presented for the determination of lead in aqueous matrix. The method consists of analyte quantitation using the liquid electrode plasma-optical emission spectrometry (LEP-OES) coupled with selective separation/preconcentration by solid-phase extraction (SPE). The impact of operating variables on the retention of lead in SPEs such as pH, flow rate of the sample solution; type, volume, flow rate of the eluent; and matrix effects were investigated. Selective SPE-separation/preconcentration minimized the interfering effect due to manganese in solution and limitations in lead-detection in low-concentration samples by LEP-OES. The LEP-OES operating parameters such as the electrical conductivity of sample solution; applied voltage; on-time, off-time, pulse count for applied voltage; number of measurements; and matrix effects have also been optimized to obtain a distinct peak for the lead at λ max =405.8nm. The limit of detection (3σ) and the limit of quantification (10σ) for lead determination using the technique were found as 1.9 and 6.5ng mL -1 , respectively. The precision, as relative standard deviation, was lower than 5% at 0.1μg mL -1 Pb, and the preconcentration factor was found to be 187. The proposed method was applied to the analysis of lead contents in the natural aqueous matrix (recovery rate:>95%). The method accuracy was verified using certified reference material of wastewaters: SPS-WW1 and ERM-CA713. The results from LEP-OES were in good agreement with inductively coupled plasma optical emission spectrometry measurements of the same samples. The application of the method is rapid (≤5min, without preconcentration) with a reliable detection limit at trace levels. Copyright © 2017 Elsevier B.V. All rights reserved.

Sample introduction systems for the analysis of liquid microsamples by ICP-AES and ICP-MS

Energy Technology Data Exchange (ETDEWEB)

Todoli, Jose L. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, 03080 Alicante (Spain)]. E-mail: jose.todoli@ua.es; Mermet, Jean M. [Spectroscopy Forever, 01390 Tramoyes (France)

2006-03-15

There are many fields in which the available sample volume is the limiting factor for an elemental analysis. Over the last ten years, sample introduction systems used in plasma spectrometry (i.e., Inductively Coupled Plasma Atomic Emission Spectrometry, ICP-AES, and Mass Spectrometry, ICP-MS) have evolved in order to expand the field of applicability of these techniques to the analysis of micro- and nanosamples. A full understanding of the basic processes occurring throughout the sample introduction system is absolutely necessary to improve analytical performance. The first part of the present review deals with fundamental studies concerning the different phenomena taking place from aerosol production to analyte excitation/ionization when the liquid consumption rate does not exceed 100 {mu}l/min. Existing sample introduction systems are currently far from the ideal and a significant effort has been made to develop new and efficient devices. Different approaches for continuously introducing small sample volumes (i.e., microsamples) have been reviewed and compared in the present work. Finally, applications as well as basic guidelines to select the best sample introduction system according to the sample particularities are given at the end of this review.

Sample introduction systems for the analysis of liquid microsamples by ICP-AES and ICP-MS

International Nuclear Information System (INIS)

Todoli, Jose L.; Mermet, Jean M.

2006-01-01

There are many fields in which the available sample volume is the limiting factor for an elemental analysis. Over the last ten years, sample introduction systems used in plasma spectrometry (i.e., Inductively Coupled Plasma Atomic Emission Spectrometry, ICP-AES, and Mass Spectrometry, ICP-MS) have evolved in order to expand the field of applicability of these techniques to the analysis of micro- and nanosamples. A full understanding of the basic processes occurring throughout the sample introduction system is absolutely necessary to improve analytical performance. The first part of the present review deals with fundamental studies concerning the different phenomena taking place from aerosol production to analyte excitation/ionization when the liquid consumption rate does not exceed 100 μl/min. Existing sample introduction systems are currently far from the ideal and a significant effort has been made to develop new and efficient devices. Different approaches for continuously introducing small sample volumes (i.e., microsamples) have been reviewed and compared in the present work. Finally, applications as well as basic guidelines to select the best sample introduction system according to the sample particularities are given at the end of this review

Determination of Trace Iron in Red Wine by Isotope Dilution Mass Spectrometry Using Multiple-Collector Inductively Coupled Plasma Mass Spectrometry

International Nuclear Information System (INIS)

Zhou Tao; Wang Jun; Lu Hai; Zhou Yuanjing; Li Haifeng

2009-01-01

This paper introduces determination of trace iron in red wine certified reference material by isotope dilution mass spectrometry (IDMS) method using a multiplecollector inductively coupled plasma mass spectrometry, equipped with a hexapole collision cell. The measurement procedure of iron isotopic abundance ratios was deeply researched. Reduced polyatomic ion interferences to iron isotopes ion by collision reaction using Ar and H 2 gas, high precise isotopic abundance ratios were achieved. Two relative measurement methods (ICP-MS and ICP-OES) were used to analyze trace iron in red wine. The results are compared with IDMS results, which indicate that they are accordant. The uncertainty analyses include each uncertainty factor in whole experiment and the uncertainty of used certified reference material and it shows that the procedure blank is not neglectable to detect limit and precision of the method. The establishment of IDMS method for analysis of trace iron in red wine supports the certification of certified reference materials. (authors)

Metal carbonyl vapor generation coupled with dielectric barrier discharge to avoid plasma quench for optical emission spectrometry.

Science.gov (United States)

Cai, Yi; Li, Shao-Hua; Dou, Shuai; Yu, Yong-Liang; Wang, Jian-Hua

2015-01-20

The scope of dielectric barrier discharge (DBD) microplasma as a radiation source for optical emission spectrometry (OES) is extended by nickel carbonyl vapor generation. We proved that metal carbonyl completely avoids the extinguishing of plasma, and it is much more suitable for matching the DBD excitation and OES detection with respect to significant DBD quenching by concomitant hydrogen when hydride generation is used. A concentric quartz UV reactor allows sample solution to flow through the central channel wherein to efficiently receive the uniformly distributed UV irradiation in the confined cylindrical space between the concentric tubes, which facilitates effective carbonyl generation in a nickel solution. The carbonyl is transferred into the DBD excitation chamber by an argon stream for nickel excitation, and the characteristic emission of nickel at 232.0 nm is detected by a charge-coupled device (CCD) spectrometer. A 1.0 mL sample solution results in a linear range of 5-100 μg L(-1) along with a detection limit of 1.3 μg L(-1) and a precision of 2.4% RSD at 50 μg L(-1). The present DBD-OES system is validated by nickel in certified reference materials.

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)

Papadopoulou, D.N.; Zachariadis, G.A.; Anthemidis, A.N.; Tsirliganis, N.C.; Stratis, J.A.

2004-01-01

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)

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

Energy Technology Data Exchange (ETDEWEB)

Papadopoulou, D.N. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Zachariadis, G.A. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Anthemidis, A.N. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Tsirliganis, N.C. [Archaeometry Laboratory, Cultural and Educational Technology Institute, Tsimiski 58, GR-67100, Xanthi (Greece); Stratis, J.A. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece)]. E-mail: jstratis@chem.auth.gr

2004-12-01

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)

Studies the alterations of biochemical and mineral contents in bone tissue of mus musculus due to aluminum toxicity and the protective action of desferrioxamine and deferiprone by FTIR, ICP-OES, SEM and XRD techniques.

Science.gov (United States)

Sivakumar, S; Khatiwada, Chandra Prasad; Sivasubramanian, J

2014-05-21

The present study has attempt to analyze the changes in the biochemical and mineral contents of aluminum intoxicated bone and determine the protective action of desferrioxamine (DFO) and deferiprone (DFP) by using Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), inductively coupled plasma optical emission spectroscopy (ICP-OES), and scanning electron microscopy (SEM) techniques for four groups of animals such as control (Group I), aluminum intoxicated (Group II), Al+DFP (Group III) and Al+DFO+DFP (Group IV) treated groups respectively. The FTIR spectra of the aluminum intoxicated bone showed significant alteration in the biochemical constituents. The bands ratio at I1400/I877 significantly decreased from control to aluminum, but enhanced it by Al+DFP to Al+DFO+DFP treated bone tissue for treatments of 16 weeks. This result suggests that DFO and DFP are the carbonate inhibitor, recovered from chronic growth of bone diseases and pathologies. The alteration of proteins profile indicated by Amide I and Amide II, where peak area values decreased from control to aluminum respectively, but enhanced by treated with DFP (p.o.) and DFO+DFP (i.p.) respectively. The XRD analysis showed a decrease in crystallinity due to aluminum toxicity. Further, the Ca, Mg, and P contents of the aluminum exposed bone were less than those of the control group, and enhanced by treatments with DFO and DFP. The concentrations of trace elements were found by ICP-OES. Therefore, present study suggests that due to aluminum toxicity severe loss of bone minerals, decrease in the biochemical constituents and changes in the surface morphology. Copyright © 2014 Elsevier B.V. All rights reserved.

Depth-profile analysis of thermoelectric layers on Si wafers by pulsed r.f. glow discharge time-of-flight mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Reinsberg, K.-G. [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany); Schumacher, C. [Institute for Applied Physics, University of Hamburg, Jungiusstrasse 11, D-20355 Hamburg (Germany); Tempez, A. [HORIBA Jobin Yvon, 16-18 rue du Canal, F-91160 Longjumeau (France); Nielsch, K. [Institute for Applied Physics, University of Hamburg, Jungiusstrasse 11, D-20355 Hamburg (Germany); Broekaert, J.A.C., E-mail: jose.broekaert@chemie.uni-hamburg.de [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)

2012-10-15

In this work the depth-profile analysis of thermoelectric layers deposited on Au and Cr covered Si wafers with the aid of pulsed radiofrequency glow discharge time-of-flight mass spectrometry (pulsed RF-GD-TOFMS also called plasma profiling TOFMS (PP-TOFMS Trade-Mark-Sign )) is described. For thermoelectric materials the depth resolutions obtained with both PP-TOFMS and secondary ion mass spectrometry (SIMS) are shown to be well comparable and in the order of the roughness of the corresponding layers (between 20 and 3700 nm). With both methods a direct solid analysis without any preparation steps is possible. In addition, the analysis of the samples with PP-TOFMS proved to be faster by a factor of 26 compared to SIMS, as sputtering rates were found to be 80 nm s{sup -1} and 3 nm s{sup -1}, respectively. For the analyzed samples the results of PP-TOFMS and SIMS show that a homogeneous deposition was obtained. Quantitative results for all samples could also be obtained directly by PP-TOFMS when the stoichiometry of one sample was determined beforehand for instance by inductively coupled plasma optical emission spectrometry (ICP-OES) and scanning electron microscopy energy dispersive X-ray fluorescence spectrometry (SEM-EDX). For Bi{sub 2}Te{sub 3} the standard deviation for the main component concentrations within one sample then is found to be between 1.1% and 1.9% and it is 3.6% from sample to sample. For Sb{sub 2}Te{sub 3} the values within one sample are from 1.7% to 4.2% and from sample to sample 5.3%, respectively. - Highlights: Black-Right-Pointing-Pointer Depth resolution in sub micrometer size by glow discharge mass spectrometry. Black-Right-Pointing-Pointer Bi and Sb telluride layers composition with GD-TOF-MS, ICP-OES and SEM-EDX agree. Black-Right-Pointing-Pointer Homogeneities of layers measured with GD-TOF-MS and SIMS agree.

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

International Nuclear Information System (INIS)

Cheung, Yan; Schwartz, Andrew J.; Chan, George C.-Y.; Hieftje, Gary M.

2015-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Cheung, Yan; Schwartz, Andrew J.; Chan, George C.-Y.; Hieftje, Gary M., E-mail: hieftje@indiana.edu

2015-08-01

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

The determination of precious metals in geological samples by ICP - Mass Spectrometry

International Nuclear Information System (INIS)

Denoyer, E.; Ediger, R.; Hager, J.

1989-01-01

ICP - mass spectrometry with laser sampling has been used to determine gold directly in solid fire assay beads. A small portion of the lead bead is vaporized by Nd: YAG laser, and the resulting particulate material is passed by a flow of argon an ICP-mass spectrometer for quantitation of the gold content. Calibration with known geological materials gives linear calibration curves, and detection limits for gols are estimated to be 0.07 micrograms/gram in the original ore sample. The repeatability of the method is similar to that expected for traditional fire assay methods, and the analysis time for the solid lead bead is less than five minutes per sample. (author) [pt

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

Energy Technology Data Exchange (ETDEWEB)

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

2007-10-17

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

A single stage simultaneous separation and pre concentration of rare earth elements on activated carbon for its determination by ICP-OES after wet ashing - application to soil samples

International Nuclear Information System (INIS)

Chakrapani, G.; Mahanta, P.L.; Hanuman, V.V.; Srivastava, P.K.

2007-01-01

A simple, rapid, cost effective simultaneous separation and pre concentration method is developed for determination of Rare earth elements in soil samples at sub ppm levels by inductively coupled plasma-optical emission spectrometry (ICP-OES). The method is based on sorption of REEs on powered activated carbon (AC) in 2 - 3 M HF medium. The soil samples are decomposed by HF-HCl treatment followed by fusion of residue with Na 2 CO 3 . Keeping in view its application to soil samples, experimental parameters such as effect of HF, amount of AC, contact time, sample weight were optimized for quantitative sorption. The unique feature of the method is, REEs are desorbed quantitatively from activated carbon, by completely oxidizing and solubilizing AC by wet digestion (HNO 3 - HClO 4 treatment). Thus the time consuming and tedious method of ignition of charcoal to ashes is avoided, to increase the sample throughput in geochemical exploration studies. The precision of the method is ± 7 % at 1 ppm level. The accuracy of the method is evaluated by analyzing soil standard reference materials i.e. by using CANMET (Canada Center for Mineral and Energy Technology) standards, such as SO-2, SO-3 and SO-4. The composition of these soil standards closely match with the composition of soil samples under investigation. The method is being applied on numerous soil samples collected during geochemical exploration of uranium. The REEs in soil samples are determined down to ppm and sub ppm levels, based on separation of REEs from two gram soil sample, making up to final volume of 25 ml . The method could be adopted by any laboratory as the input involved is inexpensive activated carbon associated with minimal skill unlike the reported methods of ion exchange and solvent extraction. (author)

The determination of long life radionuclides by means of sector field ICP mass spectrometry

International Nuclear Information System (INIS)

Kerl, W.; Becker, J.S.; Dietze, H.J.; Dannecker, W.

1996-01-01

Different analytical processes for determining long life radionuclides by means of double-focussing sector field ICP mass spectrometry are described. In determining long life radionuclides by means of ICP-MS, on the one hand the analytical problem areas are in the interference of isobaric atom or molecule ions (eg: 151 Eu + - 151 Sm + , 79 Se + - 39 Ar 40 ArH + ) and on the other hand in the high detection limits when using commercial sample introduction systems (eg: For 129 I). An online coupling of HPLC and ICP-MS was built up for the separation of isobaric atom ions and was tested for the separation of isobaric atom ions and was tested for its efficiency in the separation of lanthanides. Special sample introduction systems for ICP-MS were developed for the analysis of 129 I, by which the sensitivity of detection can be appreciably improved compared to commercial sample introduction systems. (orig.) [de

Total sulfur determination in gasoline, kerosene and diesel fuel using inductively coupled plasma optical emission spectrometry after direct sample introduction as detergent emulsions

International Nuclear Information System (INIS)

Santelli, Ricardo Erthal; Padua Oliveira, Eliane; Batista de Carvalho, Maria de Fatima; Almeida Bezerra, Marcos; Soares Freire, Aline

2008-01-01

Herein, we present the development of a procedure for the determination of total sulfur in petroleum-derived products (gasoline, kerosene and diesel fuel) employing inductively coupled plasma optical emission spectrometry (ICP OES). For this procedure, samples were prepared as emulsions that were made using concentrated nitric acid, Triton X-100, sample, and ultra pure water in proportions of 5/10/7/78% (v/v), respectively. Sample volumes were weighed because of the density differences, and oxygen was added to the sheat gas entrance of the ICP OES in order to decrease carbon deposition in the torch and to minimize background effects. A Doehlert design was applied as an experimental matrix to investigate the flow ratios of argon (sheat and plasma gas) and oxygen in relation to the signal-to-background ratio. A comparative study among the slopes of the analytical curves built in aqueous media, surfactant/HNO 3 , and by spike addition for several sample emulsions indicates that a unique solution of surfactant in acidic media can be employed to perform the external calibration for analysis of the emulsions. The developed procedure allows for the determination of the total sulfur content in petroleum derivatives with a limit of detection (LOD) and limit of quantification (LOQ) of 0.72 and 2.4 μg g -1 , respectively. Precision values, expressed as the relative standard deviations (% RSD, n = 10) for 12 and 400 μg g -1 , were 2.2% and 1.3%, respectively. The proposed procedure was applied toward the determination of total sulfur in samples of gasoline, kerosene, and diesel fuel commercialized in the city of Niteroi/RJ, Brazil. The accuracy of the proposed method was evaluated by the determination of the total sulfur in three different standard reference materials (SRM): NIST 2723a (sulfur in diesel fuel oil), NIST 1616b (sulfur in kerosene), and NIST 2298 (sulfur in gasoline). The data indicate that the methodology can be successfully applied to these types of samples

Uranium determination using atomic spectrometric techniques: An overview

International Nuclear Information System (INIS)

Santos, Juracir S.; Teixeira, Leonardo S.G.; Santos, Walter N.L. dos; Lemos, Valfredo A.; Godoy, Jose M.; Ferreira, Sergio L.C.

2010-01-01

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.

Optimisation and application of ICP-MS and alpha-spectrometry for determination of isotopic ratios of depleted uranium and plutonium in samples collected in Kosovo

OpenAIRE

Boulyga, S. F.; Testa, C.; Desideri, D.; Becker, J. S.

2001-01-01

The determination of environmental contamination with natural and artificial actinide isotopes and evaluation of their source requires precise isotopic determination of actinides, above all uranium and plutonium. This can be achieved by alpha spectrometry or by inductively coupled plasma mass spectrometry (ICP-MS) after chemical separation of actinides. The performance of a sector-field ICP-MS (ICP-SFMS) coupled to a low-flow micronebulizer with a membrane desolvation unit, "Aridus'', was stu...

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)

Ochsenkuehn-Petropoulou, Maria; Luck, Joachim

1991-01-01

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)

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

Science.gov (United States)

Chan, George C. Y. [Bloomington, IN; Hieftje, Gary M [Bloomington, IN

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.

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-05-30

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

Determination of As, Cd, Hg and Pb in continuous use drugs and excipients by plasma-based techniques in compliance with the United States Pharmacopeia requirements

Science.gov (United States)

da Silva, Caroline Santos; Pinheiro, Fernanda Costa; do Amaral, Clarice Dias Britto; Nóbrega, Joaquim Araújo

2017-12-01

Some inorganic impurities are toxic to human health even when present at low concentrations and therefore must be carefully monitored in products as continuous use drugs. This work aimed the development of a simple microwave-assisted digestion procedure for different types of drugs and excipients and the analytical determination of elemental impurities according to the new regulations of the United States Pharmacopeia (USP) 232 and 233 using inductively coupled plasma optical emission spectrometry (ICP-OES) or inductively coupled plasma mass spectrometry (ICP-MS). Eight drugs samples and two excipients of different brands were microwave-assisted digested with inverse aqua regia. Addition and recovery experiments were performed according to J values, once permissible daily exposure value is specific for each element and estimated according to the maximum daily dose of drug indicated by the label. Samples were spiked with values of 1.5J in order to check accuracies for As, Cd, Hg, and Pb. Recoveries obtained by ICP-OES ranged from 75 to 148% and for ICP-MS ranged from 74 to 120%. The limits of detection for ICP-OES ranged from 0.4 to 17 mg kg- 1 and for ICP-MS from 7.4 to 41.6 μg kg- 1. Both analytical methods were adequate in terms of accuracies and sensitivities. Considering the maximum daily dose, all drugs samples and excipients contained As, Cd, Hg and Pb below the maximum limits stipulated by USP since all of them presented contents below respective limits of detection.

Determination of 241Am in sediments by isotope dilution high resolution inductively coupled plasma mass spectrometry (ID HR ICP-MS).

Science.gov (United States)

Agarande, M; Benzoubir, S; Bouisset, P; Calmet, D

2001-08-01

Trace levels (pg kg(-1)) of 241Am in sediments were determined by isotope dilution high resolution inductively coupled plasma mass spectrometry (ID HR ICP-MS) using a microconcentric nebulizer. 241Am was isolated from major elements like Ca and Fe by different selective precipitations. In further steps. Am was first separated from other transuranic elements and purified by anion exchange and extraction chromatography prior to the mass spectrometric measurements. The ID HR ICP-MS results are compared with isotope dilution alpha spectrometry.

Multielement determination of major-to-ultratrace elements in vegetable samples by ICP-MS and ICP-AES after acid digestion

Energy Technology Data Exchange (ETDEWEB)

Hokura, Akiko; Oguri, Sachiko; Matsuura, Hirotaka; Haraguchi, Hiroki [Dept. of Applied Chemistry, Graduate School of Engineering, Nagoya Univ. (Japan)

2000-06-01

A multielement determination of major-to-ultratrace elements in vegetable samples was carried out by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES). Spinach samples (0.5 g) were digested with nitric acid and hydrofluoric acid in a Teflon beaker on a hot plate. The decomposed samples were dissolved in a 1 M ( = mol dm{sup -3}) HNO{sub 3} solution containing internal standard elements (Ge, In, and Re, 10 ppb each), and were subjected to multielement analyses by ICP-AES and ICP-MS. As a result, about 40 elements were successfully determined over a wide concentration range from % to ppb level. Spinach samples grown in different production areas were also analyzed in order to understand the influences of the environmental conditions on growth. Among the major and minor elements, the values of the coefficient of variance (CV) for B, Mg, P, and K were < 20%, and those for Ca, Na, Al, and Mn were higher than 50%. On the other hand, the values of CV for trace and ultratrace elements were significantly high. Furthermore, the present analytical method was also applied to the determination of major-to-ultratrace elements in various vegetable samples (23 species in 11 families); the similarities and differences of the elemental distributions in vegetables were found in the experimental results. (author)

Multielement determination of major-to-ultratrace elements in vegetable samples by ICP-MS and ICP-AES after acid digestion

International Nuclear Information System (INIS)

Hokura, Akiko; Oguri, Sachiko; Matsuura, Hirotaka; Haraguchi, Hiroki

2000-01-01

A multielement determination of major-to-ultratrace elements in vegetable samples was carried out by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES). Spinach samples (0.5 g) were digested with nitric acid and hydrofluoric acid in a Teflon beaker on a hot plate. The decomposed samples were dissolved in a 1 M ( = mol dm -3 ) HNO 3 solution containing internal standard elements (Ge, In, and Re, 10 ppb each), and were subjected to multielement analyses by ICP-AES and ICP-MS. As a result, about 40 elements were successfully determined over a wide concentration range from % to ppb level. Spinach samples grown in different production areas were also analyzed in order to understand the influences of the environmental conditions on growth. Among the major and minor elements, the values of the coefficient of variance (CV) for B, Mg, P, and K were < 20%, and those for Ca, Na, Al, and Mn were higher than 50%. On the other hand, the values of CV for trace and ultratrace elements were significantly high. Furthermore, the present analytical method was also applied to the determination of major-to-ultratrace elements in various vegetable samples (23 species in 11 families); the similarities and differences of the elemental distributions in vegetables were found in the experimental results. (author)

Determination of low cadmium concentrations in wine by on-line preconcentration in a knotted reactor coupled to an inductively coupled plasma optical emission spectrometer with ultrasonic nebulization

Energy Technology Data Exchange (ETDEWEB)

Lara, R.F. [Inst. de Investigaciones Mineras, Universidad Nacional de San Juan (Argentina); Wuilloud, R.G.; Salonia, J.A. [Dept. of Analytical Chemistry, National University of San Luis (Argentina); Olsina, R.A.; Martinez, L.D. [Dept. of Analytical Chemistry, National University of San Luis (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina)

2001-12-01

An on-line cadmium preconcentration and determination system implemented with inductively coupled plasma optical emission spectrometry (ICP-OES) associated to flow injection (FI) with ultrasonic nebulization system (USN) was studied. The cadmium was retained as the cadmium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol, Cd-(5-Br-PADAP), complex, at pH 9.5. The cadmium complex was removed from the knotted reactor (KR) with 3.0 mol/L nitric acid. A total enhancement factor of 216 was obtained with respect to ICP-OES using pneumatic nebulization (12 for USN and 18 for KR) with a preconcentration time of 60 s. The value of the detection limit for the preconcentration of 5 mL of sample solution was 5 ng/L. The precision for 10 replicate determinations at the 5 {mu}g/L Cd level was 2.9% relative standard deviation (RSD), calculated from the peak heights obtained. The calibration graph using the preconcentration system for cadmium was linear with a correlation coefficient of 0.9998 at levels near the detection limits up to at least 1000 {mu}g/L. The method was successfully applied to the determination of cadmium in wine samples. (orig.)

{sup 99}Tc bioassay by inductively coupled plasma mass spectrometry (ICP-MS)

Energy Technology Data Exchange (ETDEWEB)

Lewis, L.A.

1998-05-01

A means of analyzing {sup 99}Tc in urine by inductively coupled plasma mass spectrometry (ICP-MS) has been developed. Historically, {sup 99}Tc analysis was based on the radiometric detection of the 293 keV E{sub Max} beta decay product by liquid scintillation or gas flow proportional counting. In a urine matrix, the analysis of{sup 99}Tc is plagued with many difficulties using conventional radiometric methods. Difficulties originate during chemical separation due to the volatile nature of Tc{sub 2}O{sub 7} or during radiation detection due to color or chemical quenching. A separation scheme for {sup 99}Tc detection by ICP-MS is given and is proven to be a sensitive and robust analytical alternative. A comparison of methods using radiometric and mass quantitation of {sup 99}Tc has been conducted in water, artificial urine, and real urine matrices at activity levels between 700 and 2,200 dpm/L. Liquid scintillation results based on an external standard quench correction and a quench curve correction method are compared to results obtained by ICP-MS. Each method produced accurate results, however the precision of the ICP-MS results is superior to that of liquid scintillation results. Limits of detection (LOD) for ICP-MS and liquid scintillation detection are 14.67 and 203.4 dpm/L, respectively, in a real urine matrix. In order to determine the basis for the increased precision of the ICP-MS results, the detection sensitivity for each method is derived and measured. The detection sensitivity for the {sup 99}Tc isotope by ICP-MS is 2.175 x 10{sup {minus}7} {+-} 8.990 x 10{sup {minus}9} and by liquid scintillation is 7.434 x 10{sup {minus}14} {+-} 7.461 x 10{sup {minus}15}. A difference by seven orders of magnitude between the two detection systems allows ICP-MS samples to be analyzed for a period of 15 s compared to 3,600 s by liquid scintillation counting with a lower LOD.

Carbon-based magnetic nanocomposites in solid phase dispersion for the preconcentration some of lanthanides, followed by their quantitation via ICP-OES

International Nuclear Information System (INIS)

Tajabadi, F.; Sovizi, M.R.; Yamini, Y.

2013-01-01

We report on a method for the extraction of the lanthanide ions La(III), Sm(III), Nd(III) and Pr(III) using a carbon-ferrite magnetic nanocomposite as a new adsorbent, and their determination via flow injection ICP-OES. The lanthanide ions were converted into their complexes with 4-(2-pyridylazo)resorcinol, and these were adsorbed onto the nanocomposite. Fractional factorial design and central composite design were applied to optimize the extraction efficiencies to result in preconcentration factors in the range of 141-246. Linear calibration plots were obtained, the limits of detection (at S/N = 3) are between 0. 5 and 10 μg L -1 , and the intra-day precisions (n = 3) range from 3.1 to 12.8 %. The method was successfully applied to a certified reference material. (author)

Determination of Pt, Pd and Rh in Brassica Napus using solid sampling electrothermal vaporization inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Nischkauer, Winfried; Herincs, Esther; Puschenreiter, Markus; Wenzel, Walter; Limbeck, Andreas

2013-01-01

Conventional approaches for the analysis of platinum group elements (PGEs) in plant material suffer from sample digestion which results in sample dilution and therefore requires high sample intakes to maintain the sensitivity. The presented solid-sampling method avoids sample digestion while improving sensitivity when compared to digestion-based inductively coupled plasma optical emission spectrometry (ICP-OES) methods and allows the analysis of sample masses of 5 mg or less. Detection limits of 0.38 μg g −1 , 0.14 μg g −1 and 0.13 μg g −1 were obtained for Pt, Pd and Rh, respectively using a sample intake of 5 mg. The reproducibility of the procedure ranged between 4.7% (Pd) relative standard deviation (RSD, n = 7) and 7.1% (Rh) RSD for 25 ng analytes. For quantification, aqueous standards were applied on paper filter strips and dried. Only the dried filters were introduced into the electrothermal vaporization unit. This approach successfully removed memory-effects observed during analysis of platinum which occurred only if liquid standards came into contact with the graphite material of the furnace. The presented method for overcoming the Pt-memory-effects may be of further interest for the analysis of other carbide-forming analytes as it does not require any technical modification of the graphite furnace (e.g., metal inlays, pyrolytic coating). Owing to lack of suitable certified reference materials, the proposed method was compared with conventional ICP-OES analysis of digested samples and a good agreement was obtained. As a result of the low sample consumption, it was possible to determine the spatial distribution of PGEs within a single plant. Significant differences in PGE concentrations were observed between the shoots (stem, leaves) and the roots. Pd was mainly found in the roots, whereas Pt and Rh were also found in higher concentrations in the shoots. - Highlights: • The uptake of Pt, Pd and Rh by hydroponically grown plants was investigated

Determination of Pt, Pd and Rh in Brassica Napus using solid sampling electrothermal vaporization inductively coupled plasma optical emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Nischkauer, Winfried [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria); Herincs, Esther [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria); University of Natural Resources and Life Sciences, Department of Forest and Soil Sciences, Institute of Soil Research, Konrad Lorenz Straße 24, A-3430 Tulln (Austria); Puschenreiter, Markus; Wenzel, Walter [University of Natural Resources and Life Sciences, Department of Forest and Soil Sciences, Institute of Soil Research, Konrad Lorenz Straße 24, A-3430 Tulln (Austria); Limbeck, Andreas, E-mail: A.Limbeck@tuwien.ac.at [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria)

2013-11-01

Conventional approaches for the analysis of platinum group elements (PGEs) in plant material suffer from sample digestion which results in sample dilution and therefore requires high sample intakes to maintain the sensitivity. The presented solid-sampling method avoids sample digestion while improving sensitivity when compared to digestion-based inductively coupled plasma optical emission spectrometry (ICP-OES) methods and allows the analysis of sample masses of 5 mg or less. Detection limits of 0.38 μg g{sup −1}, 0.14 μg g{sup −1} and 0.13 μg g{sup −1} were obtained for Pt, Pd and Rh, respectively using a sample intake of 5 mg. The reproducibility of the procedure ranged between 4.7% (Pd) relative standard deviation (RSD, n = 7) and 7.1% (Rh) RSD for 25 ng analytes. For quantification, aqueous standards were applied on paper filter strips and dried. Only the dried filters were introduced into the electrothermal vaporization unit. This approach successfully removed memory-effects observed during analysis of platinum which occurred only if liquid standards came into contact with the graphite material of the furnace. The presented method for overcoming the Pt-memory-effects may be of further interest for the analysis of other carbide-forming analytes as it does not require any technical modification of the graphite furnace (e.g., metal inlays, pyrolytic coating). Owing to lack of suitable certified reference materials, the proposed method was compared with conventional ICP-OES analysis of digested samples and a good agreement was obtained. As a result of the low sample consumption, it was possible to determine the spatial distribution of PGEs within a single plant. Significant differences in PGE concentrations were observed between the shoots (stem, leaves) and the roots. Pd was mainly found in the roots, whereas Pt and Rh were also found in higher concentrations in the shoots. - Highlights: • The uptake of Pt, Pd and Rh by hydroponically grown plants was

Inductively coupled plasma as atomization, excitation and ionization sources in analytical atomic spectrometry

International Nuclear Information System (INIS)

Kawaguchi, Hiroshi

1996-01-01

Studies on inductively coupled plasma (ICP) for atomic emission and mass spectrometry accomplished in our laboratory since 1978 are reviewed. In emission spectrometry, the characteristics of the plasma are studied concerning the spatial profiles of spectral line intensity, axial profiles of gas and excitation temperatures, spectral line widths and matrix effect. The studies are particularly emphasized on the instrumentation such as developments of plasma generator, emission spectrometers, water-cooled torches and sample introduction methods. A slew-scan type spectrometer developed in these works represents a predecessor of the current commercial spectrometers. An ICP mass spectrometer was first developed in Japan in this laboratory in 1984. Non-spectroscopic interference of this method was found to have the correlation with the atomic weight of the matrix element. Plasma gases other than argon such as nitrogen and oxygen were used for the ICP to evaluate their performance in mass spectrometry as for the sensitivity and interferences. (author). 63 refs

Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

Science.gov (United States)

de Oliveira Souza, Sidnei; da Costa, Silvânio Silvério Lopes; Santos, Dayane Melo; dos Santos Pinto, Jéssica; Garcia, Carlos Alexandre Borges; Alves, José do Patrocínio Hora; Araujo, Rennan Geovanny Oliveira

2014-06-01

An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg- 1 for Mn to 77.3 mg kg- 1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento - MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES).

Identification and characterization of gadolinium(III) complexes in biological tissue extracts.

Science.gov (United States)

Kahakachchi, Chethaka L; Moore, Dennis A

2010-07-01

The gadolinium species present in a rat kidney following intravenous administration of a gadolinium-based magnetic resonance contrast agent (Optimark™, Gadoversetamide injection) to a rat was examined in the present study. The major gadolinium species in the supernatant of the rat kidney tissue extracts was determined by reversed-phase liquid chromatography with online inductively coupled plasma optical emission spectrometry (HPLC-ICP-OES). The identity of the compound was established by liquid chromatography electrospray ionization mass spectrometry (LC-ESI-MS) detection. The principal gadolinium(III) complex in a rat kidney tissue extract was identified as Gd-DTPA-BMEA 24 Hrs and 7 days after a single intravenous injection of Optimark™ (gadoversetamide; Gd-DTPA-BMEA) at a dose of 5 mmol Gd/kg body weight. The study demonstrated for the first time the feasibility of the use of two complementary techniques, HPLC-ICP-OES and HPLC-ESI-MS to study the in vivo behavior of gadolinium-based magnetic resonance contrast media.

Understanding the effects of potassium ferricyanide on lead hydride formation in tetrahydroborate system and its application for determination of lead in milk using hydride generation inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Deng, Biyang; Xu, Xiangshu; Xiao, Yan; Zhu, Pingchuan; Wang, Yingzi

2015-01-01

Highlights: • Proposed a novel explanation for plumbane generation. • Expounded the role of K 3 Fe(CN) 6 in plumbane generation. • Clarified the controversial aspects in the mechanism of K 3 Fe(CN) 6 enhancement. • Used X-ray diffractometry to analyze the intermediates. • Developed a method to analyze lead in milk using K 3 Fe(CN) 6 and K 4 Fe(CN) 6 as new additives. - Absract: To understand the formation of plumbane in the Pb II -NaBH 4 -K 3 Fe(CN) 6 system, the intermediate products produced in the reaction of lead(II) and NaBH 4 in the presence of K 3 Fe(CN) 6 were studied. The produced plumbane and elemental lead were measured through continuous flow hydride generation (HG)-inductively coupled plasma optical emission spectrometry (ICP OES) and X-ray diffraction spectrometry techniques, respectively. Based on the experimental results, the explanations can be depicted in the following steps: (1) plumbane and black lead sediment (black Pb) are formed in the reaction of lead(II) and NaBH 4 ; (2) the black Pb is oxidized by K 3 Fe(CN) 6 to form Pb 2 [Fe(CN) 6 ], which further reacts with NaBH 4 to form more plumbane and black Pb; and (3) another round starts in which the produced black Pb from the step 2 is then oxidized continuously by K 3 Fe(CN) 6 to form more Pb 2 [Fe(CN) 6 ] complex, which would produce more plumbane. In short, the black Pb and Pb 2 [Fe(CN) 6 ] complex are the key intermediate products for the formation of plumbane in the Pb II -NaBH 4 -K 3 Fe(CN) 6 system. Based on the enhancement effect of potassium ferricyanide and potassium ferrocyanide, a method was developed to analyze lead in milk with HG-ICP OES technique. The detection limit of the method was observed as 0.081 μg L −1 . The linearity range of lead was found between 0.3 and 50,000 μg L −1 with correlation coefficient of 0.9993. The recovery of lead was determined as 97.6% (n = 5) for adding 10 μg L −1 lead into the milk sample

Laser ablation ICP-mass spectrometry determination of Th230 in soils at the Gunnison, Colorado UMTRA site

International Nuclear Information System (INIS)

Anderson, M.S.; Braymen, S.; McIntosh, R.

1994-01-01

This report describes an innovative technology, laser ablation-inductively couple plasma-mass spectrometry (LA-ICP-MS), operated in a mobile laboratory, to rapidly detect thorium 230 activity levels in soil samples. This technology was demonstrated on-site during November 1993 at the Gunnison, Colorado, UMTRA project site in support of their remediation effort. The LA-ICP-MS sampling and analysis technique was chosen because of the capability for rapid analysis, approximately three samples per hour, with minimal sample preparation

Study of uranium in soil employing Inductively Coupled Plasma Optical Emission Spectrometry

International Nuclear Information System (INIS)

Srivastava, A.; Sharma, P.K.; Bassan, M.K.T.; Avhad, D.K.; Singhal, R.K.; Reddy, A.V.R.

2015-01-01

Soil samples were collected from different locations in Punjab and Jharkhand States of India. Their Uranium content was measured using ICP-OES with and without chemical separation. It was observed that 98 percent of the uranium could be adsorbed using chitosan based micro-extractant at pH 5. The concentration of uranium in the studied soil samples was found to be higher than its normal natural abundance. (author)

[Pretreatment of Aluminum-Lithium Alloy Sample and Determination of Argentum and Lithium by Spectral Analysis].

Science.gov (United States)

Zhou, Hui; Tan, Qian; Gao, Ya-ling; Sang, Shi-hua; Chen, Wen

2015-10-01

Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), Flame Atomic Absorption Spectrometry (FAAS) and Visible Spectrometry (VS) was applied for determination of Ag and Li in lithium-aluminium alloy standard sample and test sample, their respective advantages and disadvantages were compared, the excellent selectivity of ICP-OES was confirmed by analyses of certified standard sample. Three different sample digestion methods were compared and discussed in this study. It was found that the better accuracy would be obtained by digesting sample with chloroazotic acid while the content of Li was measured by FAAS, and it was better to digest sample with hydrochloric acid and hydrogen peroxide while determining Ag and Li by ICP-OES simultaneously and determining Ag by FAAS and VS. The interference of co-existing elements and elimination methods was detailedly discussed. Ammonium hydroxide was added to adjust the sample solution into alkalescent and Al, Ti, Zr was precipitated by forming hydroxide precipitation, Mg and Cu was formed complex precipitation with 8-hydroxyquinoline in this condition, then the interference from matrix element to determinate Ag by FAAS was eliminated. In addition, phosphate was used to precipitate Ti to eliminate its interference for determination of Li by FAAS. The same treatment of determination for Ag by FAAS was used to eliminate the interference of matrix element for determination of Ag by VS, the excess of nitrate was added into sample and heated to release Ag+ from silver chloride complex, and the color of 8-hydroxyquinoline was eliminated because of decomposed by heating. The accuracy of analysis result for standard sample was conspicuously improved which confirms the efficient of the method to eliminate interference in this study. The optimal digestion method and eliminate interference method was applied to lithium-aluminium alloy samples. The recovery of samples was from 100.39% to 103.01% by ICP-OES determination for Ag

Experimental evidence of state-selective charge transfer in inductively coupled plasma-atomic emission spectrometry

International Nuclear Information System (INIS)

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

2004-01-01

State-selective charge-transfer behavior was observed for Fe, Cr, Mn and Cu in inductively coupled plasma (ICP)-atomic emission spectrometry. Charge transfer from Ar + to Fe, Cr and Mn is state-selective because of inefficient collisional mixing of the quasiresonant charge-transfer energy levels with nearby levels. This low efficiency is the consequence of differences in electronic configuration of the core electrons. The reason for state-selective charge-transfer behavior to Cu is not clear, although a tentative explanation based on efficiency of intramultiplet and intermultiplet mixing for this special case is offered

Determination of inorganic beryllium species in the particulate matter of emissions and working areas

Energy Technology Data Exchange (ETDEWEB)

Profumo, A.; Spini, G.; Cucca, L.; Pesavento, M. [Dipartimento di Chimica Gen., Pavia (Italy)

2002-07-01

A sequential extraction procedure for separating and determining Be(0), soluble Be(II) inorganic compounds, BeO and beryllium silicates in samples, such as particulate matter of emissions and working areas, has been developed. The proposed procedure has been tested on synthetic samples prepared with the inorganic beryllium compounds, in the presence of atmospherical particulate matter sampled in a laboratory, previously checked for the absence of beryllium. The speciation was then repeated on a sample of fly ash deriving from a solid waste incinerator and on a reference material (Coal Fly ash SRM 1633a, by NIST), followed by an evaluation of matrix spiking and recovery analyses. Performing multiple analyses of the spiked samples assessed the repeatability of the procedure. Quantitative determinations have been made by inductively coupled plasma optical emission spectrometry (ICP-OES) and electrothermal atomic absorption spectrometry (ETAAS). The possible interferences of the most common ions have been investigated. The selective sequential extractions allow one to separate and to determine different inorganic beryllium species, to which a different toxicity and therefore, a different risk are related: it is the case for example of metallic beryllium and beryllium oxide.

230Th, 232Th and 238U determinations in phosphoric acid fertilizer and process products by ICP-MS

International Nuclear Information System (INIS)

Nascimento, Marcos R.L. do; Guerreiro, Luisa M.R.; Bonifacio, Rodrigo L.; Taddei, Maria H.T.

2015-01-01

Through processing of Santa Quiteria-CE mine phosphate rock, Brazil has established a project for production of phosphoric acid fertilizer and uranium as a by-product. Under leaching conditions of phosphate rock with sulfuric acid, which is the common route for preparing phosphoric acid fertilizer, a large part of uranium, thorium and their decay products naturally present in the rock are solubilized. In order to assess the contamination potential in phosphoric acid and others process products, this paper describes a previous precipitation and direct methods for routine analysis of thorium and uranium isotopes by ICP-MS. In all samples, 230 Th, 232 Th and 238 U were directly determined after dilution, except 230 Th in phosphoric acid loaded with uranium sample, which to overcome equipment contamination effect, was determined after its separation by oxalate precipitation using lanthanum as a carrier. The results obtained by the proposed method by ICP-MS, were in good agreement when compared to alpha spectrometry for 230 Th, and ICP-OES and spectrophotometry with arsenazo III for elementary uranium and thorium determinations. (author)

Macro- and micro-element analysis in milk samples by inductively coupled plasma-optical emission spectrometry

Directory of Open Access Journals (Sweden)

Petrović Sanja M.

2016-01-01

Full Text Available The paper describes the determination of Ag, Al, B, Ba, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Na, Ni, Pb, Sr, Tl and Zn, as well as total fat content of milk samples, originated from different sources. The analyzed milk samples were: human milk, fresh cow milk, pasteurized cow milk from a local market, and reconstituted powder milk. The milk samples were obtained from Jablanica District (Serbia territory. Preparation of samples for macro- and micro-analyses was done by wet digestion. Concentrations of the elements after digestion were determined by inductively coupled plasma optical emission spectrometry (ICP-OES. Total fat content of milk samples was determinate by the Weibull and Stoldt method. The results showed that potassium and calcium concentrations were the highest in all samples: 1840.64 - 2993.26 mg/L and 456.05 - 1318.08 mg/L, respectively. Of all heavy metals from the examined milk samples (copper, zinc, manganese, nickel, cadmium, and lead, the most common were zinc and copper, with approximately similar content in the range of 5 - 12 mg/l, while cadmium nickel and manganese were not detected at all. Samples of fresh cow milk and human milk showed the highest fat content of 3.6 and 4.2 %, respectively. Results for total fat and macro- and micro-analyses showed that fresh cow milk has the highest contents of fat and calcium, making it the most nutritious. [Projekat Ministarstva nauke Republike Srbije, br. TR 34012

Sample Preprocessing For Atomic Spectrometry

International Nuclear Information System (INIS)

Kim, Sun Tae

2004-08-01

This book gives descriptions of atomic spectrometry, which deals with atomic absorption spectrometry such as Maxwell-Boltzmann equation and Beer-Lambert law, atomic absorption spectrometry for solvent extraction, HGAAS, ETASS, and CVAAS and inductively coupled plasma emission spectrometer, such as basic principle, generative principle of plasma and device and equipment, and interferences, and inductively coupled plasma mass spectrometry like device, pros and cons of ICP/MS, sample analysis, reagent, water, acid, flux, materials of experiments, sample and sampling and disassembling of sample and pollution and loss in open system and closed system.

Method development and validation for simultaneous determination of IEA-R1 reactor’s pool water uranium and silicon content by ICP OES

Science.gov (United States)

Ulrich, J. C.; Guilhen, S. N.; Cotrim, M. E. B.; Pires, M. A. F.

2018-03-01

IPEN’s research reactor, IEA-R1, an open pool type research reactor moderated and cooled by light water. High quality water is a key factor in preventing the corrosion of the spent fuel stored in the pool. Leaching of radionuclides from the corroded fuel cladding may be prevented by an efficient water treatment and purification system. However, as a safety management policy, IPEN has adopted a water chemistry control which periodically monitors the levels of uranium (U) and silicon (Si) in the pool’s reactor, since IEA-R1 employs U3Si2-Al dispersion fuel. An analytical method was developed and validated for the determination of uranium and silicon by ICP OES. This work describes the validation process, in a context of quality assurance, including the parameters selectivity, linearity, quantification limit, precision and recovery.

Recent Studies on the Speciation and Determination of Mercury in Different Environmental Matrices Using Various Analytical Techniques

Directory of Open Access Journals (Sweden)

Lakshmi Narayana Suvarapu

2017-01-01

Full Text Available This paper reviews the current research on the speciation and determination of mercury by various analytical techniques, including the atomic absorption spectrometry (AAS, voltammetry, inductively coupled plasma optical emission spectrometry (ICP-OES, ICP-mass spectrometry (MS, atomic fluorescence spectrometry (AFS, spectrophotometry, spectrofluorometry, and high performance liquid chromatography (HPLC. Approximately 96 research papers on the speciation and determination of mercury by various analytical instruments published in international journals since 2015 were reviewed. All analytical parameters, including the limits of detection, linearity range, quality assurance and control, applicability, and interfering ions, evaluated in the reviewed articles were tabulated. In this review, we found a lack of information in speciation studies of mercury in recent years. Another important conclusion from this review was that there were few studies regarding the concentration of mercury in the atmosphere.

ICP-AES determination of trace elements in carbon steel

International Nuclear Information System (INIS)

Sengupta, Arijit; Rajeswari, B.; Kadam, R.M.; Babu, Y.; Godbole, S.V.

2010-01-01

Full text: Carbon steel, a combination of the elements iron and carbon, can be classified into four types as mild, medium, high and very high depending on the carbon content which varies from 0.05% to 2.1%. Carbon steel of different types finds application in medical devices, razor blades, cutlery and spring. In the nuclear industry, it is used in feeder pipes in the reactor. A strict quality control measure is required to monitor the trace elements, which have deleterious effects on the mechanical properties of the carbon steel. Thus, it becomes imperative to check the purity of carbon steel as a quality control measure before it is used in feeder pipes in the reactor. Several methods have been reported in literature for trace elemental determination in high purity iron. Some of these include neutron activation analysis, atomic absorption spectrometry and atomic emission spectrometry. Inductively coupled plasma atomic emission spectrometry (ICP-AES) is widely recognized as a sensitive technique for the determination of trace elements in various matrices, its major advantages being good accuracy and precision, high sensitivity, multi-element capability, large linear dynamic range and relative freedom from matrix effects. The present study mainly deals with the direct determination of trace elements in carbon steel using ICP-AES. An axially viewing ICP spectrometer having a polychromator with 35 fixed analytical channels and limited sequential facility to select any analytical line within 2.2 nm of a polychromator line was used in these studies. Iron, which forms one of the main constituents of carbon steel, has a multi electronic configuration with line rich emission spectrum and, therefore, tends to interfere in the determination of trace impurities in carbon steel matrix. Spectral interference in ICP-AES can be seriously detrimental to the accuracy and reliability of trace element determinations, particularly when they are performed in the presence of high

Determination of aluminium in groundwater samples by GF-AAS, ICP-AES, ICP-MS and modelling of inorganic aluminium complexes.

Science.gov (United States)

Frankowski, Marcin; Zioła-Frankowska, Anetta; Kurzyca, Iwona; Novotný, Karel; Vaculovič, Tomas; Kanický, Viktor; Siepak, Marcin; Siepak, Jerzy

2011-11-01

The paper presents the results of aluminium determinations in ground water samples of the Miocene aquifer from the area of the city of Poznań (Poland). The determined aluminium content amounted from aluminium determinations were performed using three analytical techniques: graphite furnace atomic absorption spectrometry (GF-AAS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). The results of aluminium determinations in groundwater samples for particular analytical techniques were compared. The results were used to identify the ascent of ground water from the Mesozoic aquifer to the Miocene aquifer in the area of the fault graben. Using the Mineql+ program, the modelling of the occurrence of aluminium and the following aluminium complexes: hydroxy, with fluorides and sulphates was performed. The paper presents the results of aluminium determinations in ground water using different analytical techniques as well as the chemical modelling in the Mineql+ program, which was performed for the first time and which enabled the identification of aluminium complexes in the investigated samples. The study confirms the occurrence of aluminium hydroxy complexes and aluminium fluoride complexes in the analysed groundwater samples. Despite the dominance of sulphates and organic matter in the sample, major participation of the complexes with these ligands was not stated based on the modelling.

Accuracy and Precision in Elemental Analysis of Environmental Samples using Inductively Coupled Plasma-Atomic Emission Spectrometry

International Nuclear Information System (INIS)

Quraishi, Shamsad Begum; Chung, Yong-Sam; Choi, Kwang Soon

2005-01-01

Inductively Coupled Plasma-Atomic Emission Spectrometry followed by micro-wave digestion have been performed on different environmental Certified Reference Materials (CRMs). Analytical results show that accuracy and precision in ICP-AES analysis were acceptable and satisfactory in case of soil and hair CRM samples. The relative error of most of the elements in these two CRMs is within 10% with few exceptions and coefficient of variation is also less than 10%. Z-score as an analytical performance was also within the acceptable range (±2). ICP-AES was found as an inadequate method for Air Filter CRM due to incomplete dissolution, low concentration of elements and very low mass of the sample. However, real air filter sample could have been analyzed with high accuracy and precision by increasing sample mass during collection. (author)

Multielement determination and speciation of major-to-trace elements in black tea leaves by ICP-AES and ICP-MS with the aid of size exclusion chromatography

International Nuclear Information System (INIS)

Matsuura, Hirotaka; Hokura, Akiko; Katsuki, Fumie; Itoh, Akihide; Haraguchi, Hiroki

2001-01-01

A multielement determination of major-to-trace elements in black tea leaves and their tea infusions was carried out by ICP-AES (inductively coupled plasma atomic emission spectrometry) and ICP-MS (inductively coupled plasma mass spectrometry). Tea infusions were prepared as usual tea beverage by brewing black tea leaves in boiling water for 5 min. About 40 elements in tea leaves and tea infusions could be determined over the wide concentration range in 8 orders of magnitude. The extraction efficiency of each element was estimated as the ratio of its concentration in tea infusions to that in tea leaves. From the experimental results for the extraction efficiencies, the elements in black tea leaves were classified into three characteristic groups: (i) highly-extractable elements (>55%): Na, K, Co, Ni, Rb, Cs and Tl, (ii) moderately-extractable elements (20-55%): Mg, Al, P, Mn and Zn, and (iii) poorly-extractable elements (<20%): Ca, Fe, Cu, Sr, Y, Zr, Mo, Sn, Ba and lanthanoid elements. Furthermore, speciation of major-to-trace elements in tea infusions was performed by using a combined system of size exclusion chromatography (SEC) and ICP-MS (or ICP-AES). As a result, many diverse elements were found to be present as complexes associated with large organic molecules in tea infusions. (author)

Elemental mapping of structural materials for a nuclear reactor by means of LA-ICP-MS

Czech Academy of Sciences Publication Activity Database

Vaculovič, T.; Warchilová, T.; Šimo, T.; Matal, O.; Otruba, V.; Mikuška, Pavel; Kanický, V.

2012-01-01

Roč. 27, č. 8 (2012), s. 1321-1326 ISSN 0267-9477 Institutional research plan: CEZ:AV0Z40310501 Keywords : LA- ICP -MS * ICP -OES * LiF–NaF salts Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.155, year: 2012

Major and trace elements assessment in sediment from Ituparanga reservoir, by activation analysis and ICP OES

Energy Technology Data Exchange (ETDEWEB)

Silva, Sharlleny A., E-mail: sharllenya@cetesbnet.sp.gov.br [Companhia de Tecnologia de Saneamento Ambiental (CETESB), Sao Paulo, SP (Brazil). Lab. de Quimica Inorganica; Bevilacqua, Jose Eduardo [Companhia de Tecnologia de Saneamento Ambiental (CETESB), Sao Paulo, SP (Brazil). Diretoria de Tecnologia, Qualidade e Avaliacao Ambiental; Favaro, Deborah I.T., E-mail: defavaro@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Lab. de Analise por Ativacao Neutronica

2011-07-01

The Ituparanga reservoir was built to generate electric power by the LIGHT Company and started its operation in 1912. It is fed by the Una, Sorocamirim and Sorocabucu rivers. This reservoir supplies water to a population of 600.000. This water system is affected by irregular soil occupation and urban development which has caught CETESB's (Environmental Company of Sao Paulo State) attention. In this study four geo-referenced sampling points were used and bottom sediment samples were collected. The sediment samples were dried at 400 deg C, ground in an agate mortar, sieved (200 mesh) and again homogenized. The instrumental neutron activation analysis was applied to the sediment samples in order to determine some major elements (Fe, K and Na), trace (As, Ba, Br, Co, Cr, Cs, Hf, Rb, Sb, Sc, Ta, Tb, Th, U and Zn) and rare earth (Ce, Eu, La, Lu, Nd, Sm, Tb and Yb) elements. By using ICP OES metals determination for Cd, Cr, Cu, Pb and Ni was undertaken after digestion procedure according to the 3051 method from US EPA. The methodology validation for precision and accuracy was carried out by reference material analyses. For metals Cd, Cr, Cu, Pb and Ni the concentration values were compared to the oriented values from Environmental Canada (TEL and PEL). The Enrichment Factor (EF) was calculated for sediment contamination assessment. (author)

Major and trace elements assessment in sediment from Ituparanga reservoir, by activation analysis and ICP OES

International Nuclear Information System (INIS)

Silva, Sharlleny A.; Bevilacqua, Jose Eduardo; Favaro, Deborah I.T.

2011-01-01

The Ituparanga reservoir was built to generate electric power by the LIGHT Company and started its operation in 1912. It is fed by the Una, Sorocamirim and Sorocabucu rivers. This reservoir supplies water to a population of 600.000. This water system is affected by irregular soil occupation and urban development which has caught CETESB's (Environmental Company of Sao Paulo State) attention. In this study four geo-referenced sampling points were used and bottom sediment samples were collected. The sediment samples were dried at 400 deg C, ground in an agate mortar, sieved (200 mesh) and again homogenized. The instrumental neutron activation analysis was applied to the sediment samples in order to determine some major elements (Fe, K and Na), trace (As, Ba, Br, Co, Cr, Cs, Hf, Rb, Sb, Sc, Ta, Tb, Th, U and Zn) and rare earth (Ce, Eu, La, Lu, Nd, Sm, Tb and Yb) elements. By using ICP OES metals determination for Cd, Cr, Cu, Pb and Ni was undertaken after digestion procedure according to the 3051 method from US EPA. The methodology validation for precision and accuracy was carried out by reference material analyses. For metals Cd, Cr, Cu, Pb and Ni the concentration values were compared to the oriented values from Environmental Canada (TEL and PEL). The Enrichment Factor (EF) was calculated for sediment contamination assessment. (author)

Determination of {sup 126}Sn half-life from ICP-MS and gamma spectrometry measurements

Energy Technology Data Exchange (ETDEWEB)

Bienvenu, P.; Arnal, N.; Comte, J. [CEA Cadarache DEN/DEC/SA3C/LARC, Paul Lez Durance (France); Ferreux, L.; Lepy, M.C.; Be, M.M. [CEA Saclay LIST LNE/LNHB, Gif sur Yvette (France); Andreoletti, G. [AREVA Cogema SL/UP2-800, Beaumont Hague (France)

2009-07-01

A new value of {sup 126}Sn half-life was determined by combination of inductively coupled plasma-mass spectrometry (ICP-MS) and gamma spectrometry measurements on purified sample solutions collected from nuclear fuel reprocessing. {sup 126}Sn was isolated through dissolution of fission product precipitates and liquid-liquid extraction with N-benzoyl-N-phenyl-hydroxylamine (BPHA). The abundance of {sup 126}Sn atoms together with the absence of interfering species in the analysed solutions made it possible to measure both mass concentration and nuclide activity with high precision and accuracy. This led to a {sup 126}Sn half-life value of 1.980 (57) x 10{sup 5} a. (orig.)

Determination of heavy metal content of processed fruit products from Tehran's market using ICP- OES: A risk assessment study.

Science.gov (United States)

Fathabad, Ayub Ebadi; Shariatifar, Nabi; Moazzen, Mojtaba; Nazmara, Shahrokh; Fakhri, Yadolah; Alimohammadi, Mahmood; Azari, Ali; Mousavi Khaneghah, Amin

2018-05-01

In this study, the levels of Cd, Hg, Sn, Al, Pb and As of 72 samples (36 samples for fruits juices and 36 samples for fruits canned) of three different brands including of Peach, Orange, Cherry, and Pineapple (18 samples of each fruits) marketed in Tehran, Iran (2015) were evaluated using Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) technique. Also, Probabilistic risk assessment (non-carcinogenic and carcinogenic risks) was estimated by models include target hazard quotient (THQ) and cancer risk (CR) in the Monte Carlo Simulation (MCS) model. However, all samples were contaminated with the heavy metals investigated, most of them not surpassed established standards. The range of concentration for Al, Sn, As, Cd, Hg, and Pb as average in fruit juices were reported as 340.62 (65.17-1039.2), 72.33 (49.76-119.4), 3.76 (1.137-18.36), 2.12 (0.89-3.44), 0.351 and 40.86 (27.87-66.1) μg/kg, respectively. The level of heavy metals measured in different kinds of fruit juices was ranked as Al > Sn > Pb > As > Cd > Hg, and for fruits canned this rank was Pb > Al > Sn > As > Cd > Hg. The range of concentration for Al, Sn, As, Cd, Hg, and Pb in fruits canned were reported as 361.23 (43.15-1121.2), 101.42 (71.45-141.61), 3.92 (1.279-19.50), 2.78 (1.09-5.56), 0.35 and 690.54 (470.56-910.14) μg/kg, respectively. The lead (Pb) concentration in 97.22% (35 out of 36 samples) of fruit juices samples surpassed Codex limit (0.05 mg/kg) and in all samples of FC was lower than the legal limit of Codex limit (1 mg/kg). All of the samples had Tin (Sn) lower than the legal limit of Codex (fruit juices 100 mg/kg and FC 250 mg/kg). The MCS indicated that the rank order of heavy metals in both adults and children based on THQ was Al > Sn > As > Pb > Cd > Hg. The THQ of Al and Sn in the FJ and FC, for both adults, and children, was considerably higher than 1 value. Also, CR of As in both adults and children

Multi-elemental analysis of aqueous geochemical samples by quadrupole inductively coupled plasma-mass spectrometry (ICP-MS)

Science.gov (United States)

Wolf, Ruth E.; Adams, Monique

2015-01-01

Typically, quadrupole inductively coupled plasma-mass spectrometry (ICP-MS) is used to determine as many as 57 major, minor, and trace elements in aqueous geochemical samples, including natural surface water and groundwater, acid mine drainage water, and extracts or leachates from geological samples. The sample solution is aspirated into the inductively coupled plasma (ICP) which is an electrodeless discharge of ionized argon gas at a temperature of approximately 6,000 degrees Celsius. The elements in the sample solution are subsequently volatilized, atomized, and ionized by the ICP. The ions generated are then focused and introduced into a quadrupole mass filter which only allows one mass to reach the detector at a given moment in time. As the settings of the mass analyzer change, subsequent masses are allowed to impact the detector. Although the typical quadrupole ICP-MS system is a sequential scanning instrument (determining each mass separately), the scan speed of modern instruments is on the order of several thousand masses per second. Consequently, typical total sample analysis times of 2–3 minutes are readily achievable for up to 57 elements.

934 -IJBCS-Article-Dr Emmanuel A Oluyemi

African Journals Online (AJOL)

DR GATSING

coupled plasma-optical emission spectrometer. (ICP-OES) was ... Table 2: Hair standard (NCS DC 73347) analysis with ICP-OES. Elements ..... electrons from the lipids in cell membranes. The HO. ... cereals, vegetable and milk (Goyer and.

Flame emission, atomic absorption and fluorescence spectrometry

International Nuclear Information System (INIS)

Horlick, G.

1980-01-01

Six hundred and thirty references are cited in this review. The information in the review is divided into 12 major areas: books, reviews, and bibliographies; fundamental studies in flames; developments in instrumentation; measurement techniques and procedure; flame emission spectrometry; flame atomic absorption spectrometry; flame molecular absorption spectrometry; electrothermal atomization atomic absorption spectroscopy; hydride generation techniques; graphite furnace atomic emission spectrometry; atomic fluorescence spectrometry; and analytical comparisons

Determination of boron content and isotopic composition in gypsum by inductively coupled plasma optical emission spectroscopy and positive thermal ionization mass spectrometry using phase transformation.

Science.gov (United States)

Ma, Yun-Qi; Peng, Zhang-Kuang; Yang, Jian; Xiao, Ying-Kai; Zhang, Yan-Ling

2017-12-01

As a stable isotope, boron plays an important role in hydrogeology, environmental geochemistry, ore deposit geochemistry and marine paleoclimatology. However, there is no report of boron isotopic composition in gypsum. This is mainly confined to complete dissolution of Gypsum by water or acid. In this study, gypsum was converted to calcium carbonate (CaCO 3 ) with ammonium bicarbonate(NH 4 HCO 3 ) by two steps at 50°C. In every step, the mass ratio of NH 4 HCO 3 /CaSO 4 ·2H 2 O was twice, and conversion rate reached more than 98%. Converted CaCO 3 was totally dissolved with hydrochloric acid (the dissolution rate was over 99%). In order to overcome the difficulties of the matrix interference and the detection limit of Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES), we use Amberlite IRA 743 resin to purify and enrichment the boron at first, then eluting boron from the resin with 10mL 0.1mol/L hydrochloric acid at 75°C. The boron isotopic composition of natural gypsum samples was determined using positive thermal ionization mass spectrometry (P-TIMS). The boron isotopic composition of gypsum may be an excellent indicator for the formation environment. Copyright © 2017 Elsevier B.V. All rights reserved.

Mineral distribution in rice: Measurement by Microwave Plasma Atomic Emission Spectroscopy (MP-AES)

International Nuclear Information System (INIS)

Ramos, Nerissa C.; Ramos, R.G.A.; Quirit, L.L.; Arcilla, C.A.

2015-01-01

Microwave Plasma Atomic Emission Spectroscopy (MP-AES) is a new technology with comparable performance and sensitivity to Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). Both instrument use plasma as the energy source that produces atomic and ionic emission lines. However, MP-AES uses nitrogen as the plasma gas instead of argon which is an additional expense for ICP-OES. Thus, MP-AES is more economical. This study quantified six essential minerals (Se, Zn, Fe, Cu, Mn and K) in rice using MP-AES. Hot plate digestion was used for sample extraction and the detection limit for each instrument was compared with respect to the requirement for routine analysis in rice. Black, red and non-pigmented rice samples were polished in various intervals to determine the concentration loss of minerals. The polishing time corresponds to the structure of the rice grains such as outer bran layer (0 to 15), inner bran layer (15 to 30), outer endosperm layer (30 to 45), and middle endosperm layer (45 to 60). Results of MP-AES analysis showed that black rice had all essential materials (except K) in high concentration at the outer bran layer. The red and non-pigmented rice samples on the other hand, contained high levels of Se, Zn, Fe, and Mn in the whole bran portion. After 25 seconds, the mineral concentrations remained constant. The concentration of Cu however, gave consistent value in all polishing intervals, hence Cu might be located in the inner endosperm layer. Results also showed that K was uniformly distributed in all samples where 5% loss was consistently observed for every polishing interval. Therefore, the concentration of K was also affected by polishing time. Thus, the new MP-AES technology with comparable performance to ICP-OES is a promising tool for routine analysis in rice. (author)

Inductively coupled plasma – Tandem mass spectrometry (ICP-MS/MS): A powerful and universal tool for the interference-free determination of (ultra)trace elements – A tutorial review

Energy Technology Data Exchange (ETDEWEB)

Balcaen, Lieve; Bolea-Fernandez, Eduardo [Ghent University, Department of Analytical Chemistry, Krijgslaan 281-S12, B-9000 Ghent (Belgium); Resano, Martín [University of Zaragoza, Department of Analytical Chemistry, Pedro Cerbuna 12, E-50009 Zaragoza (Spain); Vanhaecke, Frank, E-mail: Frank.Vanhaecke@UGent.be [Ghent University, Department of Analytical Chemistry, Krijgslaan 281-S12, B-9000 Ghent (Belgium)

2015-09-24

This paper is intended as a tutorial review on the use of inductively coupled plasma – tandem mass spectrometry (ICP-MS/MS) for the interference-free quantitative determination and isotope ratio analysis of metals and metalloids in different sample types. Attention is devoted both to the instrumentation and to some specific tools and procedures available for advanced method development. Next to the more typical reaction gases, e.g., H{sub 2}, O{sub 2} and NH{sub 3}, also the use of promising alternative gases, such as CH{sub 3}F, is covered, and the possible reaction pathways with those reactive gases are discussed. A variety of published applications relying on the use of ICP-MS/MS are described, to illustrate the added value of tandem mass spectrometry in (ultra)trace analysis. - Highlights: • First review on tandem ICP-mass spectrometry (ICP-MS/MS). • Clear description of operating principles of ICP-MS/MS. • Description on how to make use of product ion scans, precursor ion scans and neutral gain scans in method development. • Overview of applications published so far.

Inductively coupled plasma – Tandem mass spectrometry (ICP-MS/MS): A powerful and universal tool for the interference-free determination of (ultra)trace elements – A tutorial review

International Nuclear Information System (INIS)

Balcaen, Lieve; Bolea-Fernandez, Eduardo; Resano, Martín; Vanhaecke, Frank

2015-01-01

This paper is intended as a tutorial review on the use of inductively coupled plasma – tandem mass spectrometry (ICP-MS/MS) for the interference-free quantitative determination and isotope ratio analysis of metals and metalloids in different sample types. Attention is devoted both to the instrumentation and to some specific tools and procedures available for advanced method development. Next to the more typical reaction gases, e.g., H_2, O_2 and NH_3, also the use of promising alternative gases, such as CH_3F, is covered, and the possible reaction pathways with those reactive gases are discussed. A variety of published applications relying on the use of ICP-MS/MS are described, to illustrate the added value of tandem mass spectrometry in (ultra)trace analysis. - Highlights: • First review on tandem ICP-mass spectrometry (ICP-MS/MS). • Clear description of operating principles of ICP-MS/MS. • Description on how to make use of product ion scans, precursor ion scans and neutral gain scans in method development. • Overview of applications published so far.

An ultrasound-assisted digestion method for the determination of toxic element concentrations in ash samples by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Ilander, Aki; Vaeisaenen, Ari

2007-01-01

A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of toxic element concentrations (arsenic, barium, cobalt, copper, lead, nickel, strontium, vanadium and zinc) in ash samples was developed. All the measurements were performed in robust plasma conditions which were tested by measuring the Mg(II) 280.270 nm/Mg(I) 285.213 nm line intensity ratios. The highest line intensity ratios were observed when a nebulizer gas flow of 0.6 L min -1 , auxiliary gas flow of 0.2 L min -1 and plasma power of 1400 W were used for radially viewed plasma. The analysis of SRM 1633b showed that the ultrasound-assisted method developed is highly comparable with the microwave digestion method standardized by the United States Environmental Protection Agency (EPA-3052). The ultrasound-assisted digestion with a digestion solution of aqua regia and hydrofluoric acid (HF) resulted in recovery rates of over 81%. One exception is arsenic which resulted in recoveries of about 60% only; however, it could be digested with good recovery (>90%) using a digestion solution of 5 mL of water and 5 mL of aqua regia. The major advantage of the ultrasound-assisted digestion over microwave digestion is the high treatment rate (30 samples simultaneously with a sonication time of 18 min)

Inductively coupled plasma-atomic emission spectrometry: analytical assessment of the technique at the beginning of the 90's

International Nuclear Information System (INIS)

Sanz-Medel, A.

1991-01-01

The main application of the inductively coupled plasma (ICP) today is in atomic emission spectroscopy (AES), as an excitation spectrochemical source, although uses of an ICP for fluorescence as just an atomizer, and specially for mass spectrometry, as an ionization source, are rocketing in the last few years. Since its inception, only a quarter of a century ago, ICP-AES has rapidly evolved to one of the preferred routine analytical techniques for convenient determination of many elements with high speed, at low levels and in the most varied samples. Perhaps its comparatively high kinetic temperature (capable of atomizing virtually every compound of any sample), its high excitation and ionization temperatures, and its favourable spatial structure at the core of the ICP success. By now, the ICP-AES can be considered as having achieved maturity in that a huge amount of analytical problems can be tackled with this technique, while no major or fundamental changes have been adopted for several years. Despite this fact, important driving forces are still in operation to further improve the ICP-AES sensitivity, selectivity, precision, sample throughput, etc. Moreover, proposals to extend the scope of the technique to traditionally elusive fields (e.g. non-metals and organic compound analysis) are also appearing in the recent literature. In this paper the 'state of the art', the last developments and the expectations in trying to circumvent the limitations of the ICP-AES (on the light of literature data and personal experience) are reviewed. (author)

A rapid sample decomposition procedure for bromo-heavies containing ferruginous material: determination of REEs and thorium by ICP-AES

International Nuclear Information System (INIS)

Khorge, C.R.; Murugesan, P.; Chakrapani, G.

2013-01-01

A rapid method of sample decomposition and dissolution for bromoform heavies is described for the determination of REEs and thorium by inductively coupled plasma- optical emission spectrometry. For application to geochemical exploration to achieve the high sample throughput; a simple and rapid analytical procedure is a prerequisite. In order to speed-up the existing methodology, phosphate fusion was introduced for decomposition of samples. In the proposed method, bromoform-heavies material are fused with 1:1 mixture of sodium dihydrogen orthophosphate and tetra-sodium pyrophosphate and dissolved in distilled water. After disintegration of melt, the solution was subjected to oxalate precipitation followed by R 2 O 3 separation for separating the REEs from major matrix interfering elements. The rare earth elements and thorium in the resultant solution were determined by ICP-OES. The results are compared with the results obtained by well-established existing dissolution procedures involving HF-HCl-HClO 4 acid treatment and NaF/KHF 2 fusion followed by H 2 SO 4 acid fuming. The accuracy of the method was evaluated by doping the phosphate blank with known amount of REEs and comparing the recoveries obtained using the present method. The method is simple, rapid and is suitable for the routine determination of REEs and Th in bromoform-heavies. The RSD of the method was found to be within 1-3% for Th and REEs by ICP-AES. (author)

Experimental half-life determination of 176Lu

International Nuclear Information System (INIS)

Kossert, Karsten; Jörg, Gerhard; Gostomski, Christoph Lierse v.

2013-01-01

The half-life of the naturally occurring long-lived rare earth isotope 176 Lu was determined by a combination of highly sophisticated experimental procedures in order to further improve the reliability and the precision of literature data. The amount of lutetium in the samples was determined by inductively coupled plasma optical emission spectrometry (ICP-OES) using a NIST reference standard. The isotopic ratio N( 176 Lu)/N(Lu) in the samples was measured by means of inductively coupled plasma high resolution mass spectrometry (ICP-HRMS). The activity divided by the mass of Lu was determined by applying liquid scintillation (LS) counting. The LS counting efficiency of the beta/gamma emitter 176 Lu was determined with the CIEMAT/NIST efficiency tracing technique with low uncertainty. The influences of colour quenching and background effects are discussed in this paper. The half-life was found to be 3.640(35)×10 10 y. The result is in good agreement with other evaluations and the relative standard uncertainty of 0.95% is among the lowest of previously published data. - Highlights: • The half-life of 176 Lu was determined by ICP-OES, ICP-HRMS and LSC. • The LSC efficiency was determined with the CIEMAT/NIST method. • The half-life was found to be 3.640(35)×10 10 y

ICP analysis of zinc and zamak alloys

International Nuclear Information System (INIS)

Gomez Coedo, A.; Dorado Lopez, M.T.

1987-01-01

A study was carried out on the possibilities of inductively coupled plasma emission spectrometry (ICP) in the determination of Cu, Cd, Fe, Pb, Sn, Al and Mg in zinc-base materials using direct sample solutions. A selection of analytical lines is made, on account of both their sensitivity and the corresponding study of spectral interferences; measurable minimum contents and calibrated terms are also established, to conduce therefore to a complete methodology which allows determination of the mentioned elements within the contents established on the specifications of these materials. (author)

Characterization of used lubricating oil by spectrometric techniques

Energy Technology Data Exchange (ETDEWEB)

Souza, Andressa Moreira de, E-mail: andressa@ctaa.embrapa.br [Embrapa Agroindustria de Alimentos, Guaratiba, Rio de Janeiro, RJ (Brazil); Correa, Sergio Machado [Faculdade de Engenharia. Universidade do Estado do Rio de Janeiro (UERJ), Resende, RJ (Brazil); Silva, Glauco Correa da [Instituto de Engenharia Nuclear (IEN/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

2011-07-01

Full text: The engine lubricating oil drags all kinds of impurities generated by wear of internal components. Thus, it is necessary to monitor the physical and chemical properties and concentration of metals in lubricants used to determine the appropriate time to replace them. Moreover, one can monitor the wear of the engines through the levels of metals in oils. To achieve these goals, some detection techniques such as Flame atomic absorption spectrometry (FAAS), Inductively coupled plasma optical emission spectrometry (ICP-OES) and X-ray fluorescence (XRF), have been widely used to determine metals in lubricating oils and also in other oil derivatives. Thus, some of these techniques were used in this study. Also the technique used was Gas chromatography mass spectrometry (GC / MS) for characterization of chromatographic profile of the engine lubricating oil after use. Through the technique of ICP-OES for method of United States Environmental Protection Agency (USEPA) METHOD 6010B - Inductively coupled plasma optical emission spectrometry was performed to characterize metals in lubricating oil motor, using equipment from ICP-OES Perkin-Elmer{sup R} OPTIMA 3000 ICP-Winlab and software, obtaining the following identification of metals: barium (Ba), calcium (Ca), lead (Pb), copper (Cu), Chromium (Cr), iron (Fe), magnesium (Mg), molybdenum (Mo) and zinc (Zn). Using the XRF technique, through the equipment EDFRX Shimadzu{sup R} model 800HS EDX, Rh tube, applied voltage of 50kV, amperage 100{mu}A, detector Si (Li) cooled with liquid nitrogen and collimator 10mm, we analyzed all the components comprised in the range of Ti to U and Na to SC, identified the following metals: calcium (Ca), zinc (Zn), iron (Fe), copper (Cu), molybdenum (Mo) and nickel (Ni). The characterization was performed by chromatographic methods: USEPA METHOD 5021A - Volatile organic compounds in various sample matrices using equilibrium headspace analysis, USEPA METHOD 8015B - Nonhalogenated Organics

Characterization of used lubricating oil by spectrometric techniques

International Nuclear Information System (INIS)

Souza, Andressa Moreira de; Correa, Sergio Machado; Silva, Glauco Correa da

2011-01-01

Full text: The engine lubricating oil drags all kinds of impurities generated by wear of internal components. Thus, it is necessary to monitor the physical and chemical properties and concentration of metals in lubricants used to determine the appropriate time to replace them. Moreover, one can monitor the wear of the engines through the levels of metals in oils. To achieve these goals, some detection techniques such as Flame atomic absorption spectrometry (FAAS), Inductively coupled plasma optical emission spectrometry (ICP-OES) and X-ray fluorescence (XRF), have been widely used to determine metals in lubricating oils and also in other oil derivatives. Thus, some of these techniques were used in this study. Also the technique used was Gas chromatography mass spectrometry (GC / MS) for characterization of chromatographic profile of the engine lubricating oil after use. Through the technique of ICP-OES for method of United States Environmental Protection Agency (USEPA) METHOD 6010B - Inductively coupled plasma optical emission spectrometry was performed to characterize metals in lubricating oil motor, using equipment from ICP-OES Perkin-Elmer R OPTIMA 3000 ICP-Winlab and software, obtaining the following identification of metals: barium (Ba), calcium (Ca), lead (Pb), copper (Cu), Chromium (Cr), iron (Fe), magnesium (Mg), molybdenum (Mo) and zinc (Zn). Using the XRF technique, through the equipment EDFRX Shimadzu R model 800HS EDX, Rh tube, applied voltage of 50kV, amperage 100μA, detector Si (Li) cooled with liquid nitrogen and collimator 10mm, we analyzed all the components comprised in the range of Ti to U and Na to SC, identified the following metals: calcium (Ca), zinc (Zn), iron (Fe), copper (Cu), molybdenum (Mo) and nickel (Ni). The characterization was performed by chromatographic methods: USEPA METHOD 5021A - Volatile organic compounds in various sample matrices using equilibrium headspace analysis, USEPA METHOD 8015B - Nonhalogenated Organics Using GC

Determination of 236U and transuranium elements in depleted uranium ammunition by α-spectrometry and ICP-MS

International Nuclear Information System (INIS)

Desideri, D.; Meli, M.A.; Roselli, C.; Testa, C.; Boulyga, S.F.; Becker, J.S.

2002-01-01

It is well known that ammunition containing depleted uranium (DU) was used by NATO during the Balkan conflict. To evaluate the origin of DU (the enrichment of natural uranium or the reprocessing of spent nuclear fuel) it is necessary to directly detect the presence of activation products ( 236 U, 239 Pu, 240 Pu, 241 Am, and 237 Np) in the ammunition. In this work the analysis of actinides by α-spectrometry was compared with that by inductively coupled plasma mass spectrometry (ICP-MS) after selective separation of ultratraces of transuranium elements from the uranium matrix. 242 Pu and 243 Am were added to calculate the chemical yield. Plutonium was separated from uranium by extraction chromatography, using tri-n-octylamine (TNOA), with a decontamination factor higher than 10 6 ; after elution plutonium was determined by ICP-MS ( 239 Pu and 240 Pu) and α-spectrometry ( 239+240 Pu) after electroplating. The concentration of Pu in two DU penetrator samples was 7 x 10 -12 g g -1 and 2 x 10 -11 g g -1 . The 240 Pu/ 239 Pu isotope ratio in one penetrator sample (0.12±0.04) was significantly lower than the 240 Pu/ 239 Pu ratios found in two soil samples from Kosovo (0.35±0.10 and 0.27±0.07). 241 Am was separated by extraction chromatography, using di(2-ethylhexyl)phosphoric acid (HDEHP), with a decontamination factor as high as 10 7 . The concentration of 241 Am in the penetrator samples was 2.7 x 10 -14 g g -1 and -15 g g -1 . In addition 237 Np was detected at ultratrace levels. In general, ICP-MS and α-spectrometry results were in good agreement.The presence of anthropogenic radionuclides ( 236 U, 239 Pu, 240 Pu, 241 Am, and 237 Np) in the penetrators indicates that at least part of the uranium originated from the reprocessing of nuclear fuel. Because the concentrations of radionuclides are very low, their radiotoxicological effect is negligible. (orig.)

Determination of (236)U and transuranium elements in depleted uranium ammunition by alpha-spectrometry and ICP-MS.

Science.gov (United States)

Desideri, D; Meli, M A; Roselli, C; Testa, C; Boulyga, S F; Becker, J S

2002-11-01

It is well known that ammunition containing depleted uranium (DU) was used by NATO during the Balkan conflict. To evaluate the origin of DU (the enrichment of natural uranium or the reprocessing of spent nuclear fuel) it is necessary to directly detect the presence of activation products ((236)U, (239)Pu, (240)Pu, (241)Am, and (237)Np) in the ammunition. In this work the analysis of actinides by alpha-spectrometry was compared with that by inductively coupled plasma mass spectrometry (ICP-MS) after selective separation of ultratraces of transuranium elements from the uranium matrix. (242)Pu and (243)Am were added to calculate the chemical yield. Plutonium was separated from uranium by extraction chromatography, using tri- n-octylamine (TNOA), with a decontamination factor higher than 10(6); after elution plutonium was determined by ICP-MS ((239)Pu and (240)Pu) and alpha-spectrometry ((239+240)Pu) after electroplating. The concentration of Pu in two DU penetrator samples was 7 x 10(-12) g g(-1) and 2 x 10(-11) g g(-1). The (240)Pu/(239)Pu isotope ratio in one penetrator sample (0.12+/-0.04) was significantly lower than the (240)Pu/(239)Pu ratios found in two soil samples from Kosovo (0.35+/-0.10 and 0.27+/-0.07). (241)Am was separated by extraction chromatography, using di(2-ethylhexyl)phosphoric acid (HDEHP), with a decontamination factor as high as 10(7). The concentration of (241)Am in the penetrator samples was 2.7 x 10(-14) g g(-1) and <9.4 x 10(-15) g g(-1). In addition (237)Np was detected at ultratrace levels. In general, ICP-MS and alpha-spectrometry results were in good agreement. The presence of anthropogenic radionuclides ((236)U, (239)Pu,(240)Pu, (241)Am, and (237)Np) in the penetrators indicates that at least part of the uranium originated from the reprocessing of nuclear fuel. Because the concentrations of radionuclides are very low, their radiotoxicological effect is negligible.

Application of multivariate techniques in the optimization of a procedure for the determination of bioavailable concentrations of Se and As in estuarine sediments by ICP OES using a concomitant metals analyzer as a hydride generator.

Science.gov (United States)

Lopes, Watson da Luz; Santelli, Ricardo Erthal; Oliveira, Eliane Padua; de Carvalho, Maria de Fátima Batista; Bezerra, Marcos Almeida

2009-10-15

A procedure has been developed for the determination of bioavailable concentrations of selenium and arsenic in estuarine sediments employing inductively coupled plasma optical emission spectrometry (ICP OES) using a concomitant metals analyzer device to perform hydride generation. The optimization of hydride generation was done in two steps: using a two-level factorial design for preliminary evaluation of studied factors and a Doehlert design to assess the optimal experimental conditions for analysis. Interferences of transition metallic ions (Cd(2+), Co(2+), Cu(2+), Fe(3+) and Ni(2+)) to selenium and arsenic signals were minimized by using higher hydrochloric acid concentrations. In this way, the procedure allowed the determination of selenium and arsenic in sediments with a detection limit of 25 and 30 microg kg(-1), respectively, assuming a 50-fold sample dilution (0.5 g sample extraction to 25 mL sample final volume). The precision, expressed as a relative standard deviation (% RSD, n=10), was 0.2% for both selenium and arsenic in 200 microg L(-1) solutions, which corresponds to 10 microg g(-1) in sediment samples after acid extraction. Applying the proposed procedure, a linear range of 0.08-10 and 0.10-10 microg g(-1) was obtained for selenium and arsenic, respectively. The developed procedure was validated by the analysis of two certified reference materials: industrial sludge (NIST 2782) and river sediment (NIST 8704). The results were in agreement with the certified values. The developed procedure was applied to evaluate the bioavailability of both elements in four sediment certified reference materials, in which there are not certified values for bioavailable fractions, and also in estuarine sediment samples collected in several sites of Guanabara Bay, an impacted environment in Rio de Janeiro, Brazil.

Environmental samples analysis by Atomic Absorption Spectrophotometry and Inductively Coupled Plasma-Optical Emission Spectroscopy

International Nuclear Information System (INIS)

Popescu, I.V.; Iordan, M.; Stihi, C.; Bancuta, A.; Busuioc, G.; Dima, G.; Ciupina, V.; Belc, M.; Vlaicu, Gh.; Marian, R.

2002-01-01

Biological samples are interesting from many aspects of environmental monitoring. By analyzing tree leaves conclusions can be drown regarding the metal loading in the growth medium. So that, starting from assumption that the pollution factors from environmental medium can modify the normal concentration of elements, we decided to control the presence of toxic elements and the deviation from normal state of elements in leaves of different trees from areas situated at different distances of pollution source. The aim of this work is to determine the elemental composition of tree leaves using Atomic Absorption Spectrophotometry (AAS) method and Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) method. Using AAS spectrophotometer SHIMADZU we identified and determined the concentration of: Cd, Co, Cu, Zn, Mn, Cr, Fe, Se, Pb with an instrumental error less than 1% for most of the elements analyzed. The same samples were analyzed by ICP-OES spectrometer, BAIRD ICP2070-Sequential Plasma spectrometer. We identified and determined in leaves of different trees the concentration of Mg, Ca, and Sr with a precision less than 6%. (authors)

Laser solid sampling for a solid-state-detector ICP emission spectrometer

International Nuclear Information System (INIS)

Noelte, J.; Moenke-Blankenburg, L.; Schumann, T.

1994-01-01

Solid sampling with laser vaporization has been coupled to an ICP emission spectrometer with an Echelle optical system and a solid-state-detector for the analysis of steel and soil samples. Pulsation of the vaporized material flow was compensated by real-time background correction and internal standardization, resulting in good accuracy and precision. (orig.)

Direct multielement trace analyses of silicon carbide powders by spark ablation simultaneous inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Kiera, Arne F.; Schmidt-Lehr, Sebastian; Song, Ming; Bings, Nicolas H.; Broekaert, Jose A.C.

2008-01-01

A procedure for the direct analysis of silicon carbide powders (SiC) by simultaneous detection inductively coupled plasma optical emission spectrometry using a Spectro-CIROS TM spectrometer (CCD-ICP-OES) and a novel spark ablation system Spectro-SASSy (SA) as sample introduction technique is described. The sample preparation procedure for SA of non-conducting material is based on mixing the sample powders with a conducting matrix, in this case copper and briquetting pellets. Pressing time, pressure and mixing ratio are shown to be important parameters of the pelleting technique with respect to their mechanical stability for the reliability of the analysis results. A mixing ratio of 0.2 g +0.6 g for SiC and Cu, a pressure of 10 t cm -2 and a pressing time of 8 min have been found optimum. It has also been shown that the spark parameters selected are crucial for uniform volatilization. Electron probe micrographs of the burning spots and the analytical signal magnitude showed that a rather hard spark at 100 Hz was optimum. The determination of trace elements in silicon carbide powders is demonstrated using a calibration based on the addition of standard solutions. For Al, Ti, V, Mn and Fe detection limits in the lower μg g -1 range can be achieved. Internal standardization with Y in combination with the addition of standard solutions allows relative standard deviations in the range of 4 to 24% for concentration levels of the order of 3 to 350 μg g -1

Direct multielement trace analyses of silicon carbide powders by spark ablation simultaneous inductively coupled plasma optical emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Kiera, Arne F.; Schmidt-Lehr, Sebastian; Song, Ming [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany); Bings, Nicolas H. [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)], E-mail: bings@chemie.uni-hamburg.de; Broekaert, Jose A.C. [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)

2008-02-15

A procedure for the direct analysis of silicon carbide powders (SiC) by simultaneous detection inductively coupled plasma optical emission spectrometry using a Spectro-CIROS{sup TM} spectrometer (CCD-ICP-OES) and a novel spark ablation system Spectro-SASSy (SA) as sample introduction technique is described. The sample preparation procedure for SA of non-conducting material is based on mixing the sample powders with a conducting matrix, in this case copper and briquetting pellets. Pressing time, pressure and mixing ratio are shown to be important parameters of the pelleting technique with respect to their mechanical stability for the reliability of the analysis results. A mixing ratio of 0.2 g +0.6 g for SiC and Cu, a pressure of 10 t cm{sup -2} and a pressing time of 8 min have been found optimum. It has also been shown that the spark parameters selected are crucial for uniform volatilization. Electron probe micrographs of the burning spots and the analytical signal magnitude showed that a rather hard spark at 100 Hz was optimum. The determination of trace elements in silicon carbide powders is demonstrated using a calibration based on the addition of standard solutions. For Al, Ti, V, Mn and Fe detection limits in the lower {mu}g g{sup -1} range can be achieved. Internal standardization with Y in combination with the addition of standard solutions allows relative standard deviations in the range of 4 to 24% for concentration levels of the order of 3 to 350 {mu}g g{sup -1}.

Lead isotope ratios in lichen samples evaluated by ICP-ToF-MS to assess possible atmospheric pollution sources in Havana, Cuba.

Science.gov (United States)

Alvarez, Alfredo Montero; Estévez Alvarez, Juan R; do Nascimento, Clístenes Williams Araújo; González, Iván Pupo; Rizo, Oscar Díaz; Carzola, Lázaro Lima; Torres, Roberto Ayllón; Pascual, Jorge Gómez

2017-01-01

Epiphytic lichens, collected from 119 sampling sites grown over "Roistonea Royal Palm" trees, were used to assess the spatial distribution pattern of lead (Pb) and identify possible pollution sources in Havana (Cuba). Lead concentrations in lichens and topsoils were determined by flame atomic absorption spectrophotometry and inductively coupled plasma (ICP) atomic emission spectrometry, respectively, while Pb in crude oils and gasoline samples were measured by ICP-time of flight mass spectrometry (ICP-ToF-MS). Lead isotopic ratios measurements for lichens, soils, and crude oils were obtained by ICP-ToF-MS. We found that enrichment factors (EF) reflected a moderate contamination for 71% of the samples (EF > 10). The 206 Pb/ 207 Pb ratio values for lichens ranged from 1.17 to 1.20 and were a mixture of natural radiogenic and industrial activities (e.g., crude oils and fire plants). The low concentration of Pb found in gasoline (leaded gasoline is no longer used in Cuba.

Some aspects of ICP-AES analysis of high purity rare earths

International Nuclear Information System (INIS)

Murty, P.S.; Biswas, S.S.

1991-01-01

Inductively coupled plasma atomic emission spectrometry (ICP-AES) is a technique capable of giving high sensitivity in trace elemental analysis. While the technique possesses high sensitivity, it lacks high selectivity. Selectivity is important where substances emitting complex spectra are to be analysed for trace elements. Rare earths emit highly complex spectra in a plasma source and the determination of adjacent rare earths in a high purity rare earth matrix, with high sensitivity, is not possible due to the inadequate selectivity of ICP-AES. One approach that has yielded reasonably good spectral selectivity in the high purity rare earth analysis by ICP-AES is by employing a combination of wavelength modulation techniques and high resolution echelle grating. However, it was found that by using a high resolution monochromator senstitivities either comparable to or better than those reported by the wavelength modulation technique could be obtained. (author). 2 refs., 2 figs., 2 tabs

Dielectric barrier discharge micro-plasma emission spectrometry for the detection of acetone in exhaled breath.

Science.gov (United States)

Yang, Ting; Gao, Dong-Xue; Yu, Yong-Liang; Chen, Ming-Li; Wang, Jian-Hua

2016-01-01

Acetone is a predominant volatile organic compound (VOC) in the exhaled breath and a promising biomarker for diabetes and ketoacidosis. A non-thermal micro-plasma generated in a planar dielectric barrier discharge (DBD) is used as a radiation source for the excitation of gaseous acetone followed by its quantification with optical emission spectrometry (OES). Gaseous acetone can be directly sampled, while liquid acetone is evaporated by heated tungsten coil and then introduced into the DBD micro-plasma by a helium carrier flow for performing optical emission and detection at a 519 nm emission line. In the present study, the exhaled breath is collected and transferred into aqueous medium for sampling. With a sampling volume of 7 μL in a micro-drop, a linear range of 40-1600 mg L(-1) is obtained along with a detection limit of 44 ng and a precision of 5.7% RSD. The present system is successfully applied to the determination of breath acetone for both diabetic patients and healthy volunteers. Copyright © 2015 Elsevier B.V. All rights reserved.

ICP-MS analysis for long-lived radionuclides

International Nuclear Information System (INIS)

Roos, P.

2010-01-01

Full text: Inductively coupled plasma mass spectrometry (ICP-MS) is an attractive alternative for the analysis of radioisotopes having a half-life in the order of several hundred years and above. The technique should not be considered a replacement for radiometric measurements of these isotopes but merely an alternative. Similarly to radiometric techniques like alpha and beta spectrometry most analysis of 'low-level' concentrations by ICP-MS requires chemical isolation of the element in question. For 'ultra-low-level' concentrations this clean-up of the sample is usually even more necessary than for the alternative radiometric techniques. The presentation gives an overview of advantages and disadvantages in using ICP-MS and compares it to relevant radiometric alternatives. (author)

Antimony removal from aqueous solutions using Zirconium hydroxide

International Nuclear Information System (INIS)

Petrescu, D.; Velciu, L.; Bucur, C.

2016-01-01

In this paper it is presented an experimental test for non-radioactive antimony removal from aqueous solutions using zirconium hydroxide powder. Also, it was studied how the temperature and pH influences antimony adsorption onto zirconium hydroxide surface. After the adsorption, solutions were filtered on Cellulose Mixed Ester Membrane with 0.2 μm pore size to remove the zirconium powder and then the aqueous solutions were sent to Inductively Coupled Plasma Optic Emission Spectrometry (ICP-OES) for quantitative analysis of Sb. Zirconium hydroxide powders were examined by optical microscopy. For the solutions that were tested at pH 4.5 and 10.2 the antimony concentration dropped below the detection limit of ICP-OES device, proof of antimony adsorption on zirconium hydroxide. Also, for the other tested solutions which had pH=12 the antimony concentration reduced with 77% and 80%. The temperature had no influence upon adsorption mechanism. (authors)

Forensic discrimination of aluminum foil by SR-XRF and ICP-AES

International Nuclear Information System (INIS)

Kasamatsu, Masaaki; Suzuki, Yasuhiro; Suzuki, Shinichi; Miyamoto, Naoki; Watanabe, Seiya; Shimoda, Osamu; Takatsu, Masahisa; Nakanishi, Toshio

2010-01-01

The application of synchrotron radiation X-ray fluorescence spectrometry (SR-XRF) was investigated for the forensic discrimination of aluminum foil by comparisons of the elemental components. Small fragments (1 x 1 mm) were taken from 4 kinds of aluminum foils produced by different manufactures and used for measurements of the XRF spectrum at BL37XU of SPring-8. A comparison of the XRF spectra was effective for the discrimination of aluminum foils from different sources, because significant differences were observed in the X-ray peak intensities of Fe, Cu, Zn, Ga, Zr and Sn. These elements, except for Zr and Sn in the aluminum foils and NIST SRM1258 (Aluminium Alloy 6011), were also determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The observed values of Fe, Cu, Zn and Ga in NIST standard samples by ICP-AES showed satisfactorily good agreements with the certified or information values with relative standard deviations from 1.1% for Zn to 6.7% for Ga. The observed values for the aluminum foils by ICP-AES were compared with those by SR-XRF. Correlation coefficients from 0.997 for Cu/Fe to 0.999 for Zn/Fe and Ga/Fe were obtained between the ratio of the elemental concentration by ICP-AES and normalized the X-ray intensity by SR-XRF. This result demonstrates that a comparison of the normalized X-ray intensity is nearly as effective for the discrimination of aluminum foils as quantitative analysis by ICP-AES. Comparisons of the analytical results by SR-XRF allow the discrimination of all aluminum foils using only a 1 mm 2 fragment with no destruction of the samples. (author)

High-resolution line-scan analysis of resin-embedded sediments using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS)

NARCIS (Netherlands)

Hennekam, R.; Jilbert, T.; de Lange, G.J.; Reichart, G.J.

2015-01-01

Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) line-scanning is a promising technique for producing high-resolution (µm-scale) geochemical records on resin-embedded sediments. However, this approach has not yet been thoroughly tested on sediment samples of known elemental

Analysis of plutonium isotope ratios including 238Pu/239Pu in individual U-Pu mixed oxide particles by means of a combination of alpha spectrometry and ICP-MS.

Science.gov (United States)

Esaka, Fumitaka; Yasuda, Kenichiro; Suzuki, Daisuke; Miyamoto, Yutaka; Magara, Masaaki

2017-04-01

Isotope ratio analysis of individual uranium-plutonium (U-Pu) mixed oxide particles contained within environmental samples taken from nuclear facilities is proving to be increasingly important in the field of nuclear safeguards. However, isobaric interferences, such as 238 U with 238 Pu and 241 Am with 241 Pu, make it difficult to determine plutonium isotope ratios in mass spectrometric measurements. In the present study, the isotope ratios of 238 Pu/ 239 Pu, 240 Pu/ 239 Pu, 241 Pu/ 239 Pu, and 242 Pu/ 239 Pu were measured for individual Pu and U-Pu mixed oxide particles by a combination of alpha spectrometry and inductively coupled plasma mass spectrometry (ICP-MS). As a consequence, we were able to determine the 240 Pu/ 239 Pu, 241 Pu/ 239 Pu, and 242 Pu/ 239 Pu isotope ratios with ICP-MS after particle dissolution and chemical separation of plutonium with UTEVA resins. Furthermore, 238 Pu/ 239 Pu isotope ratios were able to be calculated by using both the 238 Pu/( 239 Pu+ 240 Pu) activity ratios that had been measured through alpha spectrometry and the 240 Pu/ 239 Pu isotope ratios determined through ICP-MS. Therefore, the combined use of alpha spectrometry and ICP-MS is useful in determining plutonium isotope ratios, including 238 Pu/ 239 Pu, in individual U-Pu mixed oxide particles. Copyright © 2016 Elsevier B.V. All rights reserved.

Bioimaging mass spectrometry of trace elements – recent advance and applications of LA-ICP-MS: A review

Energy Technology Data Exchange (ETDEWEB)

Becker, J.Sabine, E-mail: s.becker@fz-juelich.de [Central Institute for Engineering, Electronics and Analytics (ZEA-3), Forschungszentrum Jülich, Jülich D-52425 (Germany); Matusch, Andreas, E-mail: a.matusch@fz-juelich.de [Institute for Neuroscience and Medicine (INM-2), Forschungszentrum Jülich, Jülich D-52425 (Germany); Wu, Bei, E-mail: b.wu@fz-juelich.de [Central Institute for Engineering, Electronics and Analytics (ZEA-3), Forschungszentrum Jülich, Jülich D-52425 (Germany)

2014-07-04

Highlights: • Bioimaging LA-ICP-MS is established for trace metals within biomedical specimens. • Trace metal imaging allows to study brain function and neurodegenerative diseases. • Laser microdissection ICP-MS was applied to mouse brain hippocampus and wheat root. - Abstract: Bioimaging using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) offers the capability to quantify trace elements and isotopes within tissue sections with a spatial resolution ranging about 10–100 μm. Distribution analysis adds to clarifying basic questions of biomedical research and enables bioaccumulation and bioavailability studies for ecological and toxicological risk assessment in humans, animals and plants. Major application fields of mass spectrometry imaging (MSI) and metallomics have been in brain and cancer research, animal model validation, drug development and plant science. Here we give an overview of latest achievements in methods and applications. Recent improvements in ablation systems, operation and cell design enabled progressively better spatial resolutions down to 1 μm. Meanwhile, a body of research has accumulated covering basic principles of the element architecture in animals and plants that could consistently be reproduced by several laboratories such as the distribution of Fe, Cu, Zn in rodent brain. Several studies investigated the distribution and delivery of metallo-drugs in animals. Hyper-accumulating plants and pollution indicator organisms have been the key topics in environmental science. Increasingly, larger series of samples are analyzed, may it be in the frame of comparisons between intervention and control groups, of time kinetics or of three-dimensional atlas approaches.

[A comparative study of cadmium, lead, mercury, arsenic, selenium, manganese, copper and zinc in brown rice and fish by inductively coupled plasma-mass spectrometry (ICP-MS) and atomic absorption spectrometry].

Science.gov (United States)

Oshima, Harumi; Ueno, Eiji; Saito, Isao; Matsumoto, Hiroshi

2004-10-01

A study was conducted to evaluate the applicability of ICP-MS techniques for determination of metals in brown rice and fish. Cadmium, lead, mercury, arsenic, selenium, manganese, copper and zinc were determined by this method. An open digestion with nitric acid (Method A) and a rapid open digestion with nitric acid and hydrochloric acid (Method B) were used to solubilize analytes in samples, and these procedures were followed by ICP-MS analysis. Recovery of certified elements from standard reference materials by Method A and Method B ranged from 92 to 110% except for mercury (70 to 100%). Analytical results of brown rice and fish samples obtained by this ICP-MS agreed with those obtained by atomic absorption spectrometry (AAS). The results of this study demonstrate that quadrupole ICP-MS provides precise and accurate measurements of the elements tested in brown rice and fish samples.

High-resolution line-scan analysis of resin-embedded sediments using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS)

NARCIS (Netherlands)

Hennekam, Rick; Jilbert, Tom; Mason, Paul R D; de Lange, Gert J.; Reichart, Gert Jan

2015-01-01

Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) line-scanning is a promising technique for producing high-resolution (μm-scale) geochemical records on resin-embedded sediments. However, this approach has not yet been thoroughly tested on sediment samples of known elemental

Simultaneous determination of bromine and iodine in milk powder for adult and infant nutrition by plasma based techniques after digestion using microwave-induced combustion

Energy Technology Data Exchange (ETDEWEB)

Picoloto, Rochele S. [Núcleo de Química, Universidade Tecnológica Federal do Paraná, 85884-000 Medianeira, PR (Brazil); Doneda, Morgana [Departamento de Química, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil); Flores, Eder L.M. [Núcleo de Química, Universidade Tecnológica Federal do Paraná, 85884-000 Medianeira, PR (Brazil); Mesko, Marcia F. [Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, 96010-610 Pelotas, RS (Brazil); Flores, Erico M.M. [Departamento de Química, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil); Mello, Paola A., E-mail: paola.mello@ufsm.br [Departamento de Química, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil)

2015-05-01

In this work, bromine and iodine determination in milk powder for adult and infant nutrition was performed by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES) after digestion by microwave-induced combustion (MIC). Contrarily to previous works using MIC, a higher sample mass was digested (700 mg). Water and ammonium hydroxide (10 to 100 mmol L{sup −1}) were investigated as absorbing solutions and accurate results were achieved using a 25 mmol L{sup −1} NH{sub 4}OH solution. Moreover, the high stability of analytes after digestion (up to 30 days) using this solution was observed. The accuracy of the proposed MIC method was evaluated using certified and reference materials of milk powder (NIST 1549 and NIST 8435). No statistical difference was observed between results obtained by MIC-ICP-MS and reference values. Results for samples were also compared with those obtained by ICP-OES and no statistical difference was observed. Microwave-assisted alkaline extraction (MW-AE) was also evaluated for milk powder using NH{sub 4}OH and tetramethylammonium hydroxide solutions. Solutions obtained after digestion by MIC (whole milk powder) presented low carbon content in digests (< 25 mg L{sup −1}) while solutions obtained after alkaline extraction presented up to 10,000 mg L{sup −1} of C. MIC method was preferable in view of the possibility of obtaining solutions with low carbon content even using a relatively high sample mass (up to 700 mg) avoiding additional dilution prior to ICP-MS analysis, thus allowing better detection limits. Limits of detection obtained by MIC-ICP-MS were 0.007 and 0.003 μg g{sup −1} for Br and I, respectively, while for MW-AE were 0.1 and 0.05 μg g{sup −1} respectively for Br and I. Among the main advantages of the proposed method are the use of diluted alkaline solutions that is in agreement with green analytical chemistry recommendations, the high stability of

Simultaneous determination of bromine and iodine in milk powder for adult and infant nutrition by plasma based techniques after digestion using microwave-induced combustion

International Nuclear Information System (INIS)

Picoloto, Rochele S.; Doneda, Morgana; Flores, Eder L.M.; Mesko, Marcia F.; Flores, Erico M.M.; Mello, Paola A.

2015-01-01

In this work, bromine and iodine determination in milk powder for adult and infant nutrition was performed by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES) after digestion by microwave-induced combustion (MIC). Contrarily to previous works using MIC, a higher sample mass was digested (700 mg). Water and ammonium hydroxide (10 to 100 mmol L −1 ) were investigated as absorbing solutions and accurate results were achieved using a 25 mmol L −1 NH 4 OH solution. Moreover, the high stability of analytes after digestion (up to 30 days) using this solution was observed. The accuracy of the proposed MIC method was evaluated using certified and reference materials of milk powder (NIST 1549 and NIST 8435). No statistical difference was observed between results obtained by MIC-ICP-MS and reference values. Results for samples were also compared with those obtained by ICP-OES and no statistical difference was observed. Microwave-assisted alkaline extraction (MW-AE) was also evaluated for milk powder using NH 4 OH and tetramethylammonium hydroxide solutions. Solutions obtained after digestion by MIC (whole milk powder) presented low carbon content in digests (< 25 mg L −1 ) while solutions obtained after alkaline extraction presented up to 10,000 mg L −1 of C. MIC method was preferable in view of the possibility of obtaining solutions with low carbon content even using a relatively high sample mass (up to 700 mg) avoiding additional dilution prior to ICP-MS analysis, thus allowing better detection limits. Limits of detection obtained by MIC-ICP-MS were 0.007 and 0.003 μg g −1 for Br and I, respectively, while for MW-AE were 0.1 and 0.05 μg g −1 respectively for Br and I. Among the main advantages of the proposed method are the use of diluted alkaline solutions that is in agreement with green analytical chemistry recommendations, the high stability of analytes in solution and the

Molecules and elements for quantitative bioanalysis: The allure of using electrospray, MALDI, and ICP mass spectrometry side-by-side.

Science.gov (United States)

Linscheid, Michael W

2018-03-30

To understand biological processes, not only reliable identification, but quantification of constituents in biological processes play a pivotal role. This is especially true for the proteome: protein quantification must follow protein identification, since sometimes minute changes in abundance tell the real tale. To obtain quantitative data, many sophisticated strategies using electrospray and MALDI mass spectrometry (MS) have been developed in recent years. All of them have advantages and limitations. Several years ago, we started to work on strategies, which are principally capable to overcome some of these limits. The fundamental idea is to use elemental signals as a measure for quantities. We began by replacing the radioactive 32 P with the "cold" natural 31 P to quantify modified nucleotides and phosphorylated peptides and proteins and later used tagging strategies for quantification of proteins more generally. To do this, we introduced Inductively Coupled Plasma Mass Spectrometry (ICP-MS) into the bioanalytical workflows, allowing not only reliable and sensitive detection but also quantification based on isotope dilution absolute measurements using poly-isotopic elements. The detection capability of ICP-MS becomes particularly attractive with heavy metals. The covalently bound proteins tags developed in our group are based on the well-known DOTA chelate complex (1,4,7,10-tetraazacyclododecane-N,N',N″,N‴-tetraacetic acid) carrying ions of lanthanoides as metal core. In this review, I will outline the development of this mutual assistance between molecular and elemental mass spectrometry and discuss the scope and limitations particularly of peptide and protein quantification. The lanthanoide tags provide low detection limits, but offer multiplexing capabilities due to the number of very similar lanthanoides and their isotopes. With isotope dilution comes previously unknown accuracy. Separation techniques such as electrophoresis and HPLC were used and just

Nutritional and environmental properties of algal products used in healthy diet by INAA and ICP-AES

International Nuclear Information System (INIS)

Avino, P.; Lepore, L.; Carconi, P.L.; Moauro, A.

2000-01-01

Spirulina platensis alga sampled in the Caribbean Sea and seven other commercial algal products available on the Italian market of different origin and aspect, have been analyzed by instrumental neutron activation analysis (INAA) and inductively coupled plasma-atomic emission spectrometry (ICP-AES). By neutron irradiation and γ-ray spectrometry (INAA), as many as 20 elements could be measured instrumentally without any chemical treatment. Cu, Mg, Mn and Pb were determined after dissolution of the sample by ICP-AES. The cross-checking of the data, specifically by comparing those of Ca, Cr, Fe and Zn, obtained by the two techniques was found to be in good agreement. Special attention from analytical and nutritional point of view has been devoted to the toxic metals. The measurements have been carried out employing the reference algal material prepared by International Atomic Energy Agency (IAEA). (author)

Development of ICP-AES based method for the characterization of high level waste

International Nuclear Information System (INIS)

Seshagiri, T.K.; Thulsidas, S.K.; Adya, V.C.; Kumar, Mithlesh; Radhakrishnan, K.; Mary, G.; Kulkarni, P.G.; Bhalerao, Bharti; Pant, D.K.

2011-01-01

An Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) method was developed for the trace metal characterization of high level waste solutions (HLW) of different origin and the method was validated by analysis of synthetic samples of simulated high level waste solutions (SHLW) from spent fuels of varying composition. In this context, an inter-laboratory comparison exercise (ILCE) was carried out with the simulated HLW of different spent fuel types, viz., research reactor (RR), pressurized heavy water reactor (PHWR) and fast breeder reactor (FBR). An over view of the ICP-AES determination of trace metallic constituents in such SHLW solutions is presented. The overall agreement between the various laboratories was good. (author)

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

International Nuclear Information System (INIS)

Jat, J.R.; Nayak, A.K.; Balaji Rao, Y.; Ravindra, H.R.

2013-01-01

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)

Arsenic speciation in marine organisms: from the analytical methodology to the constitution of reference materials

Energy Technology Data Exchange (ETDEWEB)

El Moll, A. [Laboratoire de Chimie Minerale et Analytique, URA 405 du CNRS, E. H. I. C. S., 1 rue Blaise Pascal, F-67008 Strasbourg Cedex (France); Heimburger, R. [Laboratoire de Chimie Minerale et Analytique, URA 405 du CNRS, E. H. I. C. S., 1 rue Blaise Pascal, F-67008 Strasbourg Cedex (France); Lagarde, F. [Laboratoire de Chimie Minerale et Analytique, URA 405 du CNRS, E. H. I. C. S., 1 rue Blaise Pascal, F-67008 Strasbourg Cedex (France); Leroy, M.J.F. [Laboratoire de Chimie Minerale et Analytique, URA 405 du CNRS, E. H. I. C. S., 1 rue Blaise Pascal, F-67008 Strasbourg Cedex (France); Maier, E. [Commission of the European Communities, Measurements and Testing Programme (BCR), 75 rue Montoyer, B-1049 Brussels (Belgium)

1996-03-01

An analytical procedure for total arsenic and arsenic species quantification in marine organisms has been developed. Fresh materials are freeze-dried and reduced to powders before analysis. Arsenic is determined either by energy dispersive X-ray fluorescence (EDXRF) directly or by inductively coupled plasma optical emission spectrometry (ICP/OES) after microwave digestion. Arsenic speciation is performed on the extracted sample using liquid chromatography coupled to ICP/OES for arsenobetaine and arsenocholine determination and to the hydride generation-quartz furnace atomic absorption spectrometric technique for arsenite, arsenate, monomethylarsonic and dimethylarsinic acids quantification. Special precautions are taken to avoid losses or contaminations as well as to prevent analytical errors during the quantification stage. Other methods are applied and the corresponding results compared for each step of the procedure. The method is finally validated by means of intercomparison studies within the Measurements and Testing Programme of the European Community (formely BCR). (orig.). With 9 figs., 5 tabs.

Understanding the effects of potassium ferricyanide on lead hydride formation in tetrahydroborate system and its application for determination of lead in milk using hydride generation inductively coupled plasma optical emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Deng, Biyang, E-mail: dengby16@163.com; Xu, Xiangshu; Xiao, Yan; Zhu, Pingchuan; Wang, Yingzi

2015-01-01

Highlights: • Proposed a novel explanation for plumbane generation. • Expounded the role of K{sub 3}Fe(CN){sub 6} in plumbane generation. • Clarified the controversial aspects in the mechanism of K{sub 3}Fe(CN){sub 6} enhancement. • Used X-ray diffractometry to analyze the intermediates. • Developed a method to analyze lead in milk using K{sub 3}Fe(CN){sub 6} and K{sub 4}Fe(CN){sub 6} as new additives. - Absract: To understand the formation of plumbane in the Pb{sup II}-NaBH{sub 4}-K{sub 3}Fe(CN){sub 6} system, the intermediate products produced in the reaction of lead(II) and NaBH{sub 4} in the presence of K{sub 3}Fe(CN){sub 6} were studied. The produced plumbane and elemental lead were measured through continuous flow hydride generation (HG)-inductively coupled plasma optical emission spectrometry (ICP OES) and X-ray diffraction spectrometry techniques, respectively. Based on the experimental results, the explanations can be depicted in the following steps: (1) plumbane and black lead sediment (black Pb) are formed in the reaction of lead(II) and NaBH{sub 4}; (2) the black Pb is oxidized by K{sub 3}Fe(CN){sub 6} to form Pb{sub 2}[Fe(CN){sub 6}], which further reacts with NaBH{sub 4} to form more plumbane and black Pb; and (3) another round starts in which the produced black Pb from the step 2 is then oxidized continuously by K{sub 3}Fe(CN){sub 6} to form more Pb{sub 2}[Fe(CN){sub 6}] complex, which would produce more plumbane. In short, the black Pb and Pb{sub 2}[Fe(CN){sub 6}] complex are the key intermediate products for the formation of plumbane in the Pb{sup II}-NaBH{sub 4}-K{sub 3}Fe(CN){sub 6} system. Based on the enhancement effect of potassium ferricyanide and potassium ferrocyanide, a method was developed to analyze lead in milk with HG-ICP OES technique. The detection limit of the method was observed as 0.081 μg L{sup −1}. The linearity range of lead was found between 0.3 and 50,000 μg L{sup −1} with correlation coefficient of 0

Analysis of metals and phosphorus in biodiesel B100 from different feedstock using a Flow Blurring^® multinebulizer in inductively coupled plasma-optical emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Avila Orozco, Francisco D. [Lab. FIA, Sección Química Analítica, INQUISUR (UNS-CONICET), Universidad Nacional del Sur, Avenida Alem 1253, B8000CPB, Bahía Blanca (Argentina); Kovachev, Nikolay; Aguirre Pastor, Miguel Ángel [Dpto. Química Analítica, Nutrición y Bromatología e Instituto Universitario de Materiales, Facultad de Ciencias, Universidad de Alicante, Apdo. 99, Alicante (Spain); Domini, Claudia E.; Fernández Band, Beatriz S. [Lab. FIA, Sección Química Analítica, INQUISUR (UNS-CONICET), Universidad Nacional del Sur, Avenida Alem 1253, B8000CPB, Bahía Blanca (Argentina); Canals Hernández, Antonio, E-mail: a.canals@ua.es [Dpto. Química Analítica, Nutrición y Bromatología e Instituto Universitario de Materiales, Facultad de Ciencias, Universidad de Alicante, Apdo. 99, Alicante (Spain)

2014-05-01

Highlights: • The elemental analysis of biodiesel by the proposed method is simple and fast. • Two-nozzles Flow Blurring^® nebulizer allow to reduce the spectral interferences. • Two-nozzles Flow Blurring^® nebulizer avoid the formation of carbon deposits. • The analysis may be carried out without any sample pretreatment. Abstract: A simple and fast method for determining the content of Na, K, Ca, Mg, P, and 20 heavy metals in biodiesel samples with inductively coupled plasma optical emission spectrometry (ICP OES) using a two-nozzle Flow Blurring^® multinebulizer prototype and on-line internal standard calibration, are proposed. The biodiesel samples were produced from different feedstock such as sunflower, corn, soybean and grape seed oils, via a base catalyst transesterification. The analysis was carried out without any sample pretreatment. The standards and samples were introduced through one of the multinebulizer nozzles, while the aqueous solution containing yttrium as an internal standard was introduced through the second nozzle. Thus, the spectral interferences were compensated and the formation of carbon deposits on the ICP torch was prevented. The determination coefficients (R²) were greater than 0.99 for the studied analytes, in the range 0.21–14.75 mg kg⁻¹. Short-term and long-term precisions were estimated as relative standard deviation. These were acceptable, their values being lower than 10%. The LOQ for major components such as Ca, K, Mg, Na, and P, were within a range between 4.9 ng g⁻¹ for Mg (279.553 nm) and 531.1 ng g⁻¹ for Na (588.995 nm), and for the other 20 minor components they were within a range between 1.1 ng g⁻¹ for Ba (455.403 nm) and 2913.9 ng g⁻¹ for Pb (220.353 nm). Recovery values ranged between 95% and 106%.

Determination of {sup 236}U and transuranium elements in depleted uranium ammunition by {alpha}-spectrometry and ICP-MS

Energy Technology Data Exchange (ETDEWEB)

Desideri, D.; Meli, M.A.; Roselli, C.; Testa, C. [General Chemistry Institute, Urbino University, Urbino (Italy); Boulyga, S.F.; Becker, J.S. [Central Department of Analytical Chemistry, Research Centre Juelich, Juelich (Germany)

2002-11-01

It is well known that ammunition containing depleted uranium (DU) was used by NATO during the Balkan conflict. To evaluate the origin of DU (the enrichment of natural uranium or the reprocessing of spent nuclear fuel) it is necessary to directly detect the presence of activation products ({sup 236}U, {sup 239}Pu, {sup 240}Pu, {sup 241}Am, and {sup 237}Np) in the ammunition. In this work the analysis of actinides by {alpha}-spectrometry was compared with that by inductively coupled plasma mass spectrometry (ICP-MS) after selective separation of ultratraces of transuranium elements from the uranium matrix. {sup 242}Pu and {sup 243}Am were added to calculate the chemical yield. Plutonium was separated from uranium by extraction chromatography, using tri-n-octylamine (TNOA), with a decontamination factor higher than 10{sup 6}; after elution plutonium was determined by ICP-MS ({sup 239}Pu and {sup 240}Pu) and {alpha}-spectrometry ({sup 239+240}Pu) after electroplating. The concentration of Pu in two DU penetrator samples was 7 x 10{sup -12} g g{sup -1} and 2 x 10{sup -11} g g{sup -1}. The {sup 240}Pu/{sup 239}Pu isotope ratio in one penetrator sample (0.12{+-}0.04) was significantly lower than the {sup 240}Pu/{sup 239}Pu ratios found in two soil samples from Kosovo (0.35{+-}0.10 and 0.27{+-}0.07). {sup 241}Am was separated by extraction chromatography, using di(2-ethylhexyl)phosphoric acid (HDEHP), with a decontamination factor as high as 10{sup 7}. The concentration of {sup 241}Am in the penetrator samples was 2.7 x 10{sup -14} g g{sup -1} and <9.4 x 10{sup -15} g g{sup -1}. In addition {sup 237}Np was detected at ultratrace levels. In general, ICP-MS and {alpha}-spectrometry results were in good agreement.The presence of anthropogenic radionuclides ({sup 236}U, {sup 239}Pu,{sup 240}Pu, {sup 241}Am, and {sup 237}Np) in the penetrators indicates that at least part of the uranium originated from the reprocessing of nuclear fuel. Because the concentrations of

Analytical data and sample locality map for aqua-regia leachates of stream sediments analyzed by ICP, and emission spectrographic and ICP results for many NURE stream sediments from the Killik River Quadrangle, Alaska

International Nuclear Information System (INIS)

Motooka, J.M.; Adrian, B.M.; Church, S.E.; McDougal, C.M.; Fife, J.B.

1989-01-01

A U.S. Geological Survey report is presented giving analytical data and sample locality map for aqua-regia leachates of stream sediments analyzed by ICP, and emission spectrographic and ICP results for many NURE stream sediments from the Killik River Quadrangle, Alaska

Multielement determination of major-to-ultratrace elements in plant reference materials by ICP-AES/ICP-MS and evaluation of their enrichment factors

International Nuclear Information System (INIS)

Hokura, Akiko; Matsuura, Hirotaka; Katsuki, Fumie; Haraguchi, Hiroki

2000-01-01

The multielement determination of major-to-ultratrace elements in plant reference materials (SRM Pine Needles, SRM Tomato Leaves, and NIES Tea Leaves) was carried out by ICP-AES (inductively coupled plasma atomic emission spectrometry) and ICP-MS (inductively coupled plasma mass spectrometry). The plant sample was decomposed with nitric acid and hydrofluoric acid in a Teflon beaker on a hot plate. The digest was dissolved in 1 M HNO 3 solution, and then subjected to elemental analyses. As a consequence, the analytical data for about 40 elements including rare earth elements (REEs) were obtained over a wide concentration range, for example, from 49600 μg g -1 of Ca to 6.2 ng g -1 of Lu in Tomato Leaves. The enrichment factors, which were estimated by normalizing the observed concentrations of analyte elements in plant reference materials to their soil abundances, were evaluated in order to discuss the relative abundances of various elements between plants and soil. It was found that most of the elements, except for REEs in Pine Needles and Tea Leaves, were significantly accumulated in the plant reference materials. In particular, the essential elements (K, Mg, Ca, Mn, Cu, Zn, B and P) for plant growth provided large enrichment factors. (author)

Microwave-assisted Extraction of Rare Earth Elements from Petroleum Refining Catalysts and Ambient Fine Aerosols Prior to Inductively Coupled Plasma - Mass Spectrometry

Science.gov (United States)

Mittlefehldt, David W.; Kulkarni, Pranav; Chellam, Shankar

2006-01-01

In the absence of a certified reference material, a robust microwave-assisted acid digestion procedure followed by inductively coupled plasma - mass spectrometry (ICP-MS) was developed to quantify rare earth elements (REEs) in fluidized-bed catalytic cracking (FCC) catalysts and atmospheric fine particulate matter (PM2.5). High temperature (200 C), high pressure (200 psig), acid digestion (HNO3, HF, and H3BO3) with 20 minute dwell time effectively solubilized REEs from six fresh catalysts, a spent catalyst, and PM2.5. This method was also employed to measure 27 non-REEs including Na, Mg, Al, Si, K, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Zr, Mo, Cd, Cs, Ba, Pb, and U. Complete extraction of several REEs (Y, La, Ce, Pr, Nd, Tb, Dy, and Er) required HF indicating that they were closely associated with the aluminosilicate structure of the zeolite FCC catalysts. Internal standardization using 115In quantitatively corrected non-spectral interferences in the catalyst digestate matrix. Inter-laboratory comparison using ICP-optical emission spectroscopy (ICP-OES) and instrumental neutron activation analysis (INAA) demonstrated the applicability of the newly developed analytical method for accurate analysis of REEs in FCC catalysts. The method developed for FCC catalysts was also successfully implemented to measure trace to ultra-trace concentrations of La, Ce, Pr, Nd, Sm, Gd, Eu, and Dy in ambient PM2.5 in an industrial area of Houston, TX.

Microwave-assisted extraction of rare earth elements from petroleum refining catalysts and ambient fine aerosols prior to inductively coupled plasma-mass spectrometry

International Nuclear Information System (INIS)

Kulkarni, Pranav; Chellam, Shankararaman; Mittlefehldt, David W.

2007-01-01

A robust microwave-assisted acid digestion procedure followed by inductively coupled plasma-mass spectrometry (ICP-MS) was developed to quantify rare earth elements (REEs) in fluidized-bed catalytic cracking (FCC) catalysts and atmospheric fine particulate matter (PM 2.5 ). High temperature (200 deg. C), high pressure (200 psig), acid digestion (HNO 3 , HF and H 3 BO 3 ) with 20 min dwell time effectively solubilized REEs from six fresh catalysts, a spent catalyst and PM 2.5 . This method was also employed to measure 27 non-REEs including Na, Mg, Al, Si, K, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Zr, Mo, Cd, Cs, Ba, Pb and U. Complete extraction of several REEs (Y, La, Ce, Pr, Nd, Tb, Dy and Er) required HF indicating that they were closely associated with the aluminosilicate structure of the zeolite FCC catalysts. Internal standardization using 115 In quantitatively corrected non-spectral interferences in the catalyst digestate matrix. Inter-laboratory comparison using ICP-optical emission spectroscopy (ICP-OES) and instrumental neutron activation analysis (INAA) demonstrated the applicability of the newly developed analytical method for accurate analysis of REEs in FCC catalysts. The method developed for FCC catalysts was also successfully implemented to measure trace to ultra-trace concentrations of La, Ce, Pr, Nd, Sm, Gd, Eu and Dy in ambient PM 2.5 in an industrial area of Houston, TX

Comparison of ultra-violet and inductively coupled plasma-atomic emission spectrometry for the on-line quantification of selenium species after their separation by reversed-phase liquid chromatography

International Nuclear Information System (INIS)

Tsopelas, Fotios N.; Ochsenkuehn-Petropoulou, Maria Th.; Mergias, Ioannis G.; Tsakanika, Lambrini V.

2005-01-01

An analytical approach for selenium speciation using liquid chromatography (LC) coupled with ultra-violet (UV) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) was developed. The separation of the investigated selenium species, selenites, selenates, selenomethionine, selenocystine, selenocystamine and dimethyldiselenide was accomplished in less than 6 min on a BIO Wide Pore RP-18 column using sodium salt of n-octanesulfonic acid as ion-pairing modifier. The on-line detection of the separated selenium species was performed using UV spectrometry at the optimum wavelength of 192 nm, obtained by the UV spectra of the investigated individual selenium species. ICP-AES was also used as element specific on-line detector, after its coupling with the chromatographic system. The UV and ICP-AES detectors were compared for their suitability, including sensitivity and detection limits, for the on-line quantification of the six selenium species. The developed LC-UV as well as LC-ICP-AES techniques were successfully applied to a selenized yeast candidate reference material, after its enzymatic extraction with protease XIV. It was found that the described LC-UV technique is suitable for the determination of selenomethionine, the main selenium compound in the yeast, with an accuracy of 5%, although the UV detector is not element specific and it is rarely used for selenium speciation. This finding can prove valuable for routine laboratories to perform selenium speciation in such materials

Rapid method of element determination in rye crispbread by ICP OES

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Anna Szymczycha-Madeja

2017-05-01

Full Text Available In this work, various sample preparation procedures, i.e., microwave-assisted acid digestion in a mixture of HNO3 and H2O2 solutions, solubilisation in aqua regia or tetramethyl ammonium hydroxide and extraction in diluted HNO3 or in HCl, for the determination of the total content of Ba, Ca, Cd, Cr, Cu, Fe, Mg, Mn, Ni, P, Pb, Sr and Zn in rye crispbread using inductively coupled plasma optical emission spectrometry were compared. Analytical characteristic was evaluated by comparing the accuracy and precision of the results and limits of detection of elements. Among these five procedures solubilisation in aqua regia provides the best results, i.e., limits of detection of elements within 0.12–31.4 ng mL−1, precision of 0.4–5% and accuracy better than 5%. Additionally, a good agreement between the measured and certified values of the NIST 1567a was found for all elements. The proposed procedure is simple, reduces sample handling and minimises time and reagent consumption. Thus, it can be alternatively used instead of microwave-assisted acid digestion for routine analysis. Six different rye crispbreads were analysed with this procedure.

Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Amberger, Martin A.; Hoeltig, Michael; Broekaert, Jose A.C.

2010-01-01

The use of slurry sampling total reflection X-ray fluorescence spectrometry (SlS-TXRF) for the direct determination of Ca, Cr, Cu, Fe, Mn and Ti in four boron nitride powders has been described. Measurements of the zeta potential showed that slurries with good stabilities can be obtained by the addition of polyethylenimine (PEI) at a concentration of 0.1 wt.% and by adjusting the pH at 4. For the optimization of the concentration of boron nitride in the slurries the net line intensities and the signal to background ratios were determined for the trace elements Ca and Ti as well as for the internal standard element Ga in the case of concentrations of boron nitride ranging from 1 to 30 mg mL -1 . As a compromise with respect to high net line intensities and high signal to background ratios, concentrations of 5 mg mL -1 of boron nitride were found suitable and were used for all further measurements. The limits of detection of SlS-TXRF for the boron nitride powders were found to range from 0.062 to 1.6 μg g -1 for Cu and Ca, respectively. Herewith, they are higher than those obtained in solid sampling and slurry sampling graphite furnace atomic absorption spectrometry (SoS-GFAAS, SlS-GFAAS) as well as those of solid sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SoS-ETV-ICP-OES). For Ca and Fe as well as for Cu and Fe, however, they were found to be lower than for GFAAS and for ICP-OES subsequent to wet chemical digestion, respectively. The universal applicability of SlS-TXRF to the analysis of samples with a wide variety of matrices could be demonstrated by the analysis of certified reference materials such as SiC, Al 2 O 3 , powdered bovine liver and borate ore with a single calibration. The correlation coefficients of the plots for the values found for Ca, Fe and Ti by SlS-TXRF in the boron nitride powders as well as in the before mentioned samples versus the reference values for the respective samples over a

Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Amberger, Martin A.; Hoeltig, Michael [University of Hamburg, Institute for Inorganic and Applied Chemistry, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany); Broekaert, Jose A.C., E-mail: jose.broekaert@chemie.uni-hamburg.d [University of Hamburg, Institute for Inorganic and Applied Chemistry, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)

2010-02-15

The use of slurry sampling total reflection X-ray fluorescence spectrometry (SlS-TXRF) for the direct determination of Ca, Cr, Cu, Fe, Mn and Ti in four boron nitride powders has been described. Measurements of the zeta potential showed that slurries with good stabilities can be obtained by the addition of polyethylenimine (PEI) at a concentration of 0.1 wt.% and by adjusting the pH at 4. For the optimization of the concentration of boron nitride in the slurries the net line intensities and the signal to background ratios were determined for the trace elements Ca and Ti as well as for the internal standard element Ga in the case of concentrations of boron nitride ranging from 1 to 30 mg mL{sup -1}. As a compromise with respect to high net line intensities and high signal to background ratios, concentrations of 5 mg mL{sup -1} of boron nitride were found suitable and were used for all further measurements. The limits of detection of SlS-TXRF for the boron nitride powders were found to range from 0.062 to 1.6 mug g{sup -1} for Cu and Ca, respectively. Herewith, they are higher than those obtained in solid sampling and slurry sampling graphite furnace atomic absorption spectrometry (SoS-GFAAS, SlS-GFAAS) as well as those of solid sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SoS-ETV-ICP-OES). For Ca and Fe as well as for Cu and Fe, however, they were found to be lower than for GFAAS and for ICP-OES subsequent to wet chemical digestion, respectively. The universal applicability of SlS-TXRF to the analysis of samples with a wide variety of matrices could be demonstrated by the analysis of certified reference materials such as SiC, Al{sub 2}O{sub 3}, powdered bovine liver and borate ore with a single calibration. The correlation coefficients of the plots for the values found for Ca, Fe and Ti by SlS-TXRF in the boron nitride powders as well as in the before mentioned samples versus the reference values for the respective

The use of ICP-MS and LA-ICP-MS techniques for uranium analysis in real-life swipe samples for safeguards purposes

Energy Technology Data Exchange (ETDEWEB)

Pestana, Rafael C.B.; Sarkis, Jorge E.S.; Carvalho, Elita F.U., E-mail: rcbpestana@gmail.com, E-mail: jesarkis@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Abreu Junior, Cassio H. [Centro de Energia Nuclear na Agricultura (CENA/USP), Piracicaba, SP (Brazil)

2013-07-01

Environmental swipe sampling for safeguards purposes is a powerful tool to detect undeclared materials and activities, and has been used by the International Atomic Energy Agency since 1997. This work describes the utilization of the inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for determining uranium isotopic ratios in a real-life swipe samples collected in a conversion plant at IPEN/CNEN, Brazil. Uncertainties were estimated by following the International Organization for Standardization - Guide to the Expression of Uncertainties in Measurement (ISO GUM), with a confidence level of 95%. The major uncertainties percentage for n({sup 235}U)/n({sup 238}U) ratio for ICP-MS was 3% and for LA-ICP-MS was 30% The values of uranium isotopic ratios obtained for each technique demonstrate the viability of these analytical techniques as an alternative tool for uranium analysis in swipe samples for safeguards purposes. (author)

The use of ICP-MS and LA-ICP-MS techniques for uranium analysis in real-life swipe samples for safeguards purposes

International Nuclear Information System (INIS)

Pestana, Rafael C.B.; Sarkis, Jorge E.S.; Carvalho, Elita F.U.; Abreu Junior, Cassio H.

2013-01-01

Environmental swipe sampling for safeguards purposes is a powerful tool to detect undeclared materials and activities, and has been used by the International Atomic Energy Agency since 1997. This work describes the utilization of the inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for determining uranium isotopic ratios in a real-life swipe samples collected in a conversion plant at IPEN/CNEN, Brazil. Uncertainties were estimated by following the International Organization for Standardization - Guide to the Expression of Uncertainties in Measurement (ISO GUM), with a confidence level of 95%. The major uncertainties percentage for n( 235 U)/n( 238 U) ratio for ICP-MS was 3% and for LA-ICP-MS was 30% The values of uranium isotopic ratios obtained for each technique demonstrate the viability of these analytical techniques as an alternative tool for uranium analysis in swipe samples for safeguards purposes. (author)

Determination of lithium and potassium in uranium oxide powders and pellets by Flame Atomic Emission Spectrometric method

International Nuclear Information System (INIS)

Jat, J.R.; Balaji Rao, Y.; Prasada Rao, G.; Prahlad, B.

2012-01-01

The present paper describes a method developed at Control Laboratory, NFC which includes prior separation of lithium and potassium from uranium matrix before their measurements. Solvent extraction, using Tri-n-Butyl Phosphate (TBP) in CCI 4 followed by Tri-n-Octyl Phosphine Oxide (TOPO) in CCI 4 , is employed for prior separation of Li and K. The resultant aqueous solution was analyzed by Flame-Atomic Emission Spectrometric (AES) method. Solvent extraction conditions are optimized for measurement of Li and K in the same aliquot. Experimental conditions such as instrument calibration, flame condition, fuel flow, sample flow rate through nebulizer, burner height etc. are also optimized. Under the optimal condition the detection limits achieved for lithium is 0.02 ppm and 0.2 ppm for potassium. A RSD of ± 3 % for Li at 0.05 ppm and ± 4% for K at 1 ppm level has been achieved in this method. The results of lithium in the sample are compared with the values obtained by Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). Similarly, values of potassium are compared with Flame-Atomic Absorption Spectrometry (Flame-AAS) technique. The comparisons are in good agreement. The above method is simple, sensitive, reproducible and can be used for measurement of lithium and potassium in UO 2 powder and pellets on regular basis

Speciation analysis of organomercurial compounds in Fish Tissue by capillary gas chromatography coupled to microwave-induced plasma atomic emission detection

Directory of Open Access Journals (Sweden)

Dorfe Díaz

Full Text Available This paper describes a novel approach for analysis of mercury speciation in fish using gas chromatography coupled with microwave-induced plasma optical emission spectrometry (GC-MIP-OES in surfatron resonant cavity. Sample treatment was based on quantitative leaching of mercury species from fish tissue with ultrasound-assisted acid-toluene extraction. The extracted mercury species analyzed with GC-MIP-OES attained detection limits of 5 and 9 pg for methylmercury (MeHg and ethylmercury (EtHg, respectively. A complete chromatogram could be completed in 1.5 min. MeHg values obtained with GC-MIP-OES were matched with organic mercury values obtained with selective reduction cold vapour- atomic absorption spectrometry (CV-AAS.

Use of gradient dilution to flag and overcome matrix interferences in axial-viewing inductively coupled plasma-atomic emission spectrometry

International Nuclear Information System (INIS)

Cheung, Yan; Schwartz, Andrew J.; Hieftje, Gary M.

2014-01-01

Despite the undisputed power of inductively coupled plasma-atomic emission spectrometry (ICP-AES), its users still face serious challenges in obtaining accurate analytical results. Matrix interference is perhaps the most important challenge. Dilution of a matrix-containing sample is a common practice to reduce matrix interference. However, determining the optimal dilution factor requires tedious and time-consuming offline sample preparation, since emission lines and the effect of matrix interferences are affected differently by the dilution. The current study exploits this difference by employing a high-performance liquid chromatography gradient pump prior to the nebulizer to perform on-line mixing of a sample solution and diluent. Linear gradient dilution is performed on both the calibration standard and the matrix-containing sample. By ratioing the signals from two emission lines (from the same or different elements) as a function of dilution factor, the analyst can not only identify the presence of a matrix interference, but also determine the optimal dilution factor needed to overcome the interference. A ratio that does not change with dilution signals the absence of a matrix interference, whereas a changing ratio indicates the presence of an interference. The point on the dilution profile where the ratio stabilizes indicates the optimal dilution factor to correct the interference. The current study was performed on axial-viewing ICP-AES with o-xylene as the solvent

Chemical quality of bottled mineral waters from markets of Curitiba-PR-Brazil

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Éder José dos Santos

Full Text Available ABSTRACT Twenty-seven bottled mineral waters from local markets in Curitiba, State of Paraná, Brazil were analyzed for a number of constituents, including: pH, conductivity, total dissolved solids, hardness, HCO3 - and CO 3 2-, as well as Ca2+, Mg2+, Na+, K+, NH4 + , F-, Cl-, NO3 -, NO2 - and SO4 2- by ion chromatography (IC; Al, Ba, Cd, Cr, Cu, Fe, Li, Mn, Ni, Sr, V and Zn by inductively coupled plasma optical emission spectrometry (ICP OES; Hg by cold vapor generation-ICP OES and As, Pb, Sb and Se by ICP-mass spectrometry (ICP-MS. The obtained limits of quantitation (LOQ were adequate for the determination of all analytes using the various analytical techniques. Results for the analysis of AccuStandard certified reference materials QCS-01-5, QCS-02-R1-5 and TCLP-02-1 as well as spike recoveries to samples show acceptable values, within 90-111 % of expected concentrations with relative standard deviations below 10 %, demonstrating the accuracy of the determinations. Both NO2 - and NO 3 - were above the maximum limits set by Brazilian legislation in two samples, indicating a microbiological contamination. One imported sample presented As (6.1 ± 0.2 µg L-1 near the maximum limit (10 µg L-1 while all other elements of interest were below the values specified by Brazilian legislation. Principal component analysis revealed that four imported samples and one from the Minas Gerais State have the highest mineral concentrations.

Trace metal analysis of road dust by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Powell, M.J.; Liu, L.; Gnanalingham, N.; Peters, L.

2000-01-01

Dust from roads in an air impingement zone close to anthropogenic sources of air pollutants can be a concern for people living in the immediate vicinity. The Ministry of the Environment (MOE) has conducted a case study to monitor the concentration of uranium, strontium, thorium and arsenic in road dust from one such area. A method for the analysis of road dust by inductively coupled plasma mass spectrometry (ICP-MS) has been developed with detection limits in the ng/1 range. A digestion technique has been developed by conducting experiments using single and combinations of acids in open-vessel wet digestions. Accuracy has been determined by the use of matrix representative certified reference materials (CRMs). Digestion precision was determined by elemental concentration measurements of the most representative CRM through replicates. Spike recovery data were from 95% to 110% for all elements, and inter-method comparison studies between hydride generation atomic absorption spectrometry (AAS) inductively coupled plasma atomic emission spectrometry (ICP-AES) and ICP-MS for arsenic and strontium show good agreement. (author)

Determination of the mineral compositions of in six beans by microwave digestion with inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Yan, Q.; Yang, L.; Chen, S.; Liu, X.; Ma, X.

2012-01-01

In the study, microwave digestion procedure optimized was applied for digesting beans. Nineteen mineral element concentrations were determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). The result indicated detection limits for the 19 elements were less than 0.0998, and relative standard deviations were 1.01% - 5.02% for all the elements, and recoveries were 90.89% - 104.55% by adding standard recovery experiment. The study showed the beans selected were abundant in mineral element contents in human nutrition, determination mineral element contents by ICP-AES with microwave digestion technology were a lot of merits of small environmental pollution, fast and accurate determination result, which could satisfy the examination request of bean samples. The results provided evidence that the six beans were a good source of K, P, Mg and Ca. This study is to give important reference value to people due to individual differences by adjusting the dietary to complement the different mineral elements. (author)

Metabolite profiling with HPLC-ICP-MS as a tool for in vivo characterization of imaging probes.

Science.gov (United States)

Boros, Eszter; Pinkhasov, Omar R; Caravan, Peter

2018-01-01

Current analytical methods for characterizing pharmacokinetic and metabolic properties of positron emission tomography (PET) and single photon emission computed tomography (SPECT) probes are limited. Alternative methods to study tracer metabolism are needed. The study objective was to assess the potential of high performance liquid chromatography - inductively coupled plasma - mass spectrometry (HPLC-ICP-MS) for quantification of molecular probe metabolism and pharmacokinetics using stable isotopes. Two known peptide-DOTA conjugates were chelated with nat Ga and nat In. Limit of detection of HPLC-ICP-MS for 69 Ga and 115 In was determined. Rats were administered 50-150 nmol of Ga- and/or In-labeled probes, blood was serially sampled, and plasma analyzed by HPLC-ICP-MS using both reverse phase and size exclusion chromatography. The limits of detection were 0.16 pmol for 115 In and 0.53 pmol for 69 Ga. Metabolites as low as 0.001 %ID/g could be detected and transchelation products identified. Simultaneous administration of Ga- and In-labeled probes allowed the determination of pharmacokinetics and metabolism of both probes in a single animal. HPLC-ICP-MS is a robust, sensitive and radiation-free technique to characterize the pharmacokinetics and metabolism of imaging probes.

Comparison of standard and reaction cell inductively coupled plasma mass spectrometry in the determination of chromium and selenium species by HPLC-ICP-MS

International Nuclear Information System (INIS)

Bednar, A.J.; Kirgan, R.A.; Jones, W.T.

2009-01-01

Elemental speciation is becoming a common analytical procedure for geochemical investigations. The various redox species of environmentally relevant metals can have vastly different biogeochemical properties, including sorption, solubility, bioavailability, and toxicity. The use of high performance liquid chromatography (HPLC) coupled to elemental specific detectors, such as inductively coupled plasma mass spectrometry (ICP-MS), has become one of the most important speciation methods employed. This is due to the separation versatility of HPLC and the sensitive and selective detection capabilities of ICP-MS. The current study compares standard mode ICP-MS to recently developed reaction cell (RC) ICP-MS, which has the ability to remove or reduce many common polyatomic interferences that can limit the ability of ICP-MS to quantitate certain analytes in complex matrices. Determination of chromium and selenium redox species is achieved using ion-exchange chromatography with elemental detection by standard and RC-ICP-MS, using various chromium and selenium isotopes. In this study, method performance and detection limits for the various permutations of the method (isotope monitored or ICP-MS detection mode) were found to be comparable and generally less than 1 μg L -1 . The method was tested on synthetic laboratory samples, surface water, groundwater, and municipal tap water matrices

Sensitivity of DF-ICP-MS, PERALS and alpha-spectrometry for the determination of actinides. A comparison

International Nuclear Information System (INIS)

Ayranov, M.; Kraehenbuehl, U.

2009-01-01

We applied three techniques (DF-ICP-MS, PERALS and alpha-spectrometry) for the determination of minor actinides at environmental levels. For each method the limit of detection and the resolution were estimated in order to study the content and isotopic composition of the actinides. Two international reference materials, IAEA-135 (Irish Sea Sediment) and IAEA-300 (Baltic Sea sediment) were analyzed for activity concentrations of 238 Pu, 239 Pu, 240 Pu, 241 Pu and 241 Am. The sensitivities of the three determination techniques were compared. (author)

Selective Iron(III ion uptake using CuO-TiO2 nanostructure by inductively coupled plasma-optical emission spectrometry

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Rahman Mohammed M

2012-12-01

Full Text Available Abstract Background CuO-TiO2 nanosheets (NSs, a kind of nanomaterials is one of the most attracting class of transition doped semiconductor materials due to its interesting and important optical, electrical, and structural properties and has many technical applications, such as in metal ions detection, photocatalysis, Chemi-sensors, bio-sensors, solar cells and so on. In this paper the synthesis of CuO-TiO2 nanosheets by the wet-chemically technique is reported. Methods CuO-TiO2 NSs were prepared by a wet-chemical process using reducing agents in alkaline medium and characterized by UV/vis., FT-IR spectroscopy, X-ray photoelectron spectroscopy (XPS, powder X-ray diffraction (XRD, and field-emission scanning electron microscopy (FE-SEM etc. Results The structural and optical evaluation of synthesized NSs were measured by XRD pattern, Fourier transform infrared (FT-IR and UV–vis spectroscopy, respectively which confirmed that the obtained NSs are well-crystalline CuO-TiO2 and possessing good optical properties. The morphological analysis of CuO-TiO2 NSs was executed by FE-SEM, which confirmed that the doped products were sheet-shaped and growth in large quantity. Here, the analytical efficiency of the NSs was applied for a selective adsorption of iron(III ion prior to detection by inductively coupled plasma-optical emission spectrometry (ICP-OES. The selectivity of NSs towards various metal ions, including Au(III, Cd(II, Co(II, Cr(III, Fe(III, Pd(II, and Zn(II was analyzed. Conclusions Based on the selectivity study, it was confirmed that the selectivity of doped NSs phase was the most towards Fe(III ion. The static adsorption capacity for Fe(III was calculated to be 110.06 mgg−1. Results from adsorption isotherm also verified that the adsorption process was mainly monolayer-adsorption onto a surface containing a finite number of CuO-TiO2 NSs adsorption sites.

Determination of the mineral compositions of some selected oil-bearing seeds and kernels using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES

Directory of Open Access Journals (Sweden)

Musa Özcan, M.

2006-06-01

Full Text Available The aim of this paper was to establish the mineral contents of oil-bearing seeds and kernels such as peanut, turpentine, walnut, hazelnut, sesame, corn, poppy, almond, sunflower etc., using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES. Significant differences in mineral composition were observed among crops. All seeds and kernels contained high amounts of Al, Ca, Fe, K, Mg, Na, P and Zn. B, Cr, Cu, Li, Ni, Sr, Ti while V contents of the crops were found to be very low. The levels of K and P of all crops in this study were found to be higher than those of other seeds and kernels. The results obtained from analyses of the crops showed that the mean levels of potassiumcontent ranged from 1701.08 mg/kg (corn to 20895.8 mg/kg (soybean, the average content of phosphorus ranged from 3076.9 mg/kg (turpentine to 12006,5 mg/kg to 2617.4 mg/kg (cotton seed, and Ca from 68.4 mg/kg (corn to 13195.7 mg/kg (poppy seed. The results show that these values may  be useful for the evaluation of dietary information. Particularly the obtained results provide evidence that soybean, pinestone and poppy seed are a good source of K, P and Ca, respectively. Whereas pinestone is a good source of zinc.La finalidad del trabajo es establecer el contenido en elementos minerales de semillas oleaginosas tales como cacahuetes, trementina, avellana, sesamo, maiz, almendras, girasol, utilizando ICP-AES. Se han observado diferencias significativas en la composición de minerales entre cosechas. Todas las semillas contienen cantidades elevadas de Al, Ca, Fe, K, Mg, Na, P y Zn. Los contenidos de B, Cr, Cu, Li, Ni, Sr, Ti y V, sin embargo, fueron bajos. Los contenidos de K y P en todas las semillas estudiadas fueron superiores a las de otras semillas. El contenido medio de K osciló entre 1.701,1 mg/kg (maiz a 20.895,8 mg/kg (soja, el P entre 3.076.9 mg/kg (trementina a 12.006.5 mg/kg o 2.617,4 mg/kg (semilla de algodón, y Ca de 68,4 mg/kg (maiz a 13.195,7 mg

Simultaneous preconcentration of copper, zinc, cadmium, and nickel in water samples by cloud point extraction using 4-(2-pyridylazo)-resorcinol and their determination by inductively coupled plasma optic emission spectrometry

International Nuclear Information System (INIS)

Silva, Edson Luiz; Santos Roldan, Paulo dos; Gine, Maria Fernanda

2009-01-01

A procedure for simultaneous separation/preconcentration of copper, zinc, cadmium, and nickel in water samples, based on cloud point extraction (CPE) as a prior step to their determination by inductively coupled plasma optic emission spectrometry (ICP-OES), has been developed. The analytes reacted with 4-(2-pyridylazo)-resorcinol (PAR) at pH 5 to form hydrophobic chelates, which were separated and preconcentrated in a surfactant-rich phase of octylphenoxypolyethoxyethanol (Triton X-114). The parameters affecting the extraction efficiency of the proposed method, such as sample pH, complexing agent concentration, buffer amount, surfactant concentration, temperature, kinetics of complexation reaction, and incubation time were optimized and their respective values were 5, 0.6 mmol L -1 , 0.3 mL, 0.15% (w/v), 50 deg. C, 40 min, and 10 min for 15 mL of preconcentrated solution. The method presented precision (R.S.D.) between 1.3% and 2.6% (n = 9). The concentration factors with and without dilution of the surfactant-rich phase for the analytes ranged from 9.4 to 10.1 and from 94.0 to 100.1, respectively. The limits of detection (L.O.D.) obtained for copper, zinc, cadmium, and nickel were 1.2, 1.1, 1.0, and 6.3 μg L -1 , respectively. The accuracy of the procedure was evaluated through recovery experiments on aqueous samples.

Copper Determination in Gunshot Residue by Cyclic Voltammetric and Inductive Coupled Plasma-Optical Emission Spectroscopy

Directory of Open Access Journals (Sweden)

Mohd Hashim Nurul’Afiqah Hashimah

2016-01-01

Full Text Available Analysis of gunshot residue (GSR is a crucial evidences for a forensic analyst in the fastest way. GSR analysis insists a suitable method provides a relatively simple, rapid and precise information on the spot at the crime scene. Therefore, the analysis of Cu(II in GSR using cyclic voltammetry (CV on screen printed carbon electrode (SPCE is a better choice compared to previous alternative methods such as Inductive Coupled Plasma-Optical Emission Spectroscopy (ICP-OES those required a long time for analysis. SPCE is specially designed to handle with microvolumes of sample such as GSR sample. It gives advantages for identification of copper in GSR on-site preliminary test to prevent the sample loss on the process to be analyzed in the laboratory. SPCE was swabbed directly on the shooter’s arm immediately after firing and acetate buffer was dropped on SPCE before CV analysis. For ICP-OES analysis, cotton that had been soaked in 0.5 M nitric acid was swabbed on the shooter’s arm immediately after firing and kept in a tightly closed sampling tube. Gold coated SPCE that had been through nanoparticles modification exhibits excellent performance on voltammograms. The calibration was linear from 1 to 50 ppm of copper, the limit of detection for copper was 0.3 ppm and a relative standard deviation was 6.1 %. The method was successfully applied to the determination of copper in GSR. The Cu determination on SPCE was compared and validated by ICP-OES method with 94 % accuracy.

Hyphenation of ultra performance liquid chromatography (UPLC) with inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of bromine containing preservatives

DEFF Research Database (Denmark)

Bendahl, Lars; Hansen, Steen Honoré; Gammelgaard, Bente

2006-01-01

Ultra performance liquid chromatography (UPLC) was coupled to inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of three bromine-containing preservatives, monitoring the 79Br and 81Br isotopes simultaneously. Due to the efficiency of the 1.7 microm column packing material, t...... analysis of bromine-containing preservatives in commercially available cosmetic products.......Ultra performance liquid chromatography (UPLC) was coupled to inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of three bromine-containing preservatives, monitoring the 79Br and 81Br isotopes simultaneously. Due to the efficiency of the 1.7 microm column packing material...... at an intermediate and at a high linear velocity. The precision was better than 2.2% R.S.D. and regression analysis showed that a linear response was achieved at both flow rates (R2 > 0.9993, n = 36). The analysis time was less than 4.5 min at a flow rate of 50 microL min(-1) and limits of detection...

Isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS) for the certification of lead and cadmium in environmental standard reference materials.

Science.gov (United States)

Murphy, K E; Beary, E S; Rearick, M S; Vocke, R D

2000-10-01

Lead (Pb) and cadmium (Cd) have been determined in six new environmental standard reference materials (SRMs) using isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS). The SRMs are the following: SRM 1944, New York-New Jersey Waterway Sediment, SRMs 2583 and 2584, Trace Elements in Indoor Dust, Nominal 90 mg/kg and 10,000 mg/kg Lead, respectively, SRMs 2586 and 2587, Trace Elements in Soil Containing Lead from Paint, Nominal 500 mg/kg and 3,000 mg/kg Lead, respectively, and SRM 2782, Industrial Sludge. The capabilities of ID ICP-MS for the certification of Pb and Cd in these materials are assessed. Sample preparation and ratio measurement uncertainties have been evaluated. Reproducibility and accuracy of the established procedures are demonstrated by determination of gravimetrically prepared primary standard solutions and by comparison with isotope dilution thermal ionization mass spectrometry (ID TIMS). Material heterogeneity was readily demonstrated to be the dominant source of uncertainty in the certified values.

Separation techniques for the clean-up of radioactive mixed waste for ICP-AES/ICP-MS analysis

International Nuclear Information System (INIS)

Swafford, A.M.; Keller, J.M.

1993-01-01

Two separation techniques were investigated for the clean-up of typical radioactive mixed waste samples requiring elemental analysis by Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) or Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). These measurements frequently involve regulatory or compliance criteria which include the determination of elements on the EPA Target Analyte List (TAL). These samples usually consist of both an aqueous phase and a solid phase which is mostly an inorganic sludge. Frequently, samples taken from the waste tanks contain high levels of uranium and thorium which can cause spectral interferences in ICP-AES or ICP-MS analysis. The removal of these interferences is necessary to determine the presence of the EPA TAL elements in the sample. Two clean-up methods were studied on simulated aqueous waste samples containing the EPA TAL elements. The first method studied was a classical procedure based upon liquid-liquid extraction using tri-n- octylphosphine oxide (TOPO) dissolved in cyclohexane. The second method investigated was based on more recently developed techniques using extraction chromatography; specifically the use of a commercially available Eichrom TRU·Spec trademark column. Literature on these two methods indicates the efficient removal of uranium and thorium from properly prepared samples and provides considerable qualitative information on the extraction behavior of many other elements. However, there is a lack of quantitative data on the extraction behavior of elements on the EPA Target Analyte List. Experimental studies on these two methods consisted of determining whether any of the analytes were extracted by these methods and the recoveries obtained. Both methods produced similar results; the EPA target analytes were only slightly or not extracted. Advantages and disadvantages of each method were evaluated and found to be comparable

Imaging of Selenium by Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) in 2-D Electrophoresis Gels and Biological Tissues.

Science.gov (United States)

Cruz, Elisa Castañeda Santa; Susanne Becker, J; Sabine Becker, J; Sussulini, Alessandra

2018-01-01

Selenium and selenoproteins are important components of living organisms that play a role in different biological processes. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is a powerful analytical technique that has been employed to obtain distribution maps of selenium in biological tissues in a direct manner, as well as in selenoproteins, previously separated by their molecular masses and isoelectric points using two-dimensional polyacrylamide gel electrophoresis (2-D PAGE). In this chapter, we present the protocols to perform LA-ICP-MS imaging experiments, allowing the distribution visualization and determination of selenium and/or selenoproteins in biological systems.

Comparison of Titration ICP and XRF Spectrometry Methods in Determination of Cerium in Lens Polishing Powder

International Nuclear Information System (INIS)

Ninlaphruk, Sumalee; Pichestapong, Pipat; Mungpayabal, Harinate; Jiyavaranant, Thitima; Srisukho, Supapan; Chaisai, Prapassurn

2004-10-01

Three analytical methods in determination of cerium in cerium oxide separated from monazite ore for producing lens polishing powder were compared. These methods are titration ICP and XRF spectrometry techniques. The cerium oxide sample with estimated 45% cerium content needed to be digested and converted into solution before the analysis. The analytical results shown significantly no difference between each method. However, the titration method was found to be more convenient and suitable for quality control in the production of cerium oxide as it does not require standard cerium and the complicated analytical instruments

Semi-automatic determination of tin in marine materials by continuous flow hydride generation inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Feng Yonglai; Narasaki, Hisataki; Chen Hongyuan; Tian Liching

1997-01-01

A semi-automated continuous flow hydride generation system with inductively coupled plasma atomic emission spectrometry (ICP-AES) was used for the determination of tin in marine materials. The effects of acids (H 2 SO 4 and HCl) were studied. The analytical parameters were thoroughly investigated. Under optimized conditions, the detection limit is 0.4 ng/ml. Interferences from transition elements were investigated and seven masking reagents were tested. L-cysteine hydrochloride monohydrate (1%) was used to mask the interferences from foreign ions. Finally, the accuracy, checked with a marine standard reference material obtained from the National Research Council (NRC), was within the certified value. (orig.). With 6 figs., 4 tabs

A critical review of inductively coupled plasma-mass spectrometry for geoanalysis, geochemistry and hydrology, Part 1. Analytical performance

Science.gov (United States)

Brenner, I.B.; Taylor, Howard E.

1992-01-01

Present-day inductively coupled plasma-mass spectrometry (ICP-MS) instrumentation is described briefly. Emphasis is placed on performance characteristics for geoanalysis, geochemistry, and hydrology. Applications where ICP-MS would be indispensable are indicated. Determination of geochemically diagnostic trace elements (such as the rare earth elements [REE], U and Th), of isotope ratios for fingerprinting, tracer and other geo-isotope applications, and benchmark isotope dilution determinations are considered to be typical priority applications for ICP-MS. It is concluded that ICP-MS furnishes unique geoanalytical and environmental data that are not readily provided by conventional spectroscopic (emission and absorption) techniques.

Integrated Design for Marketing and Manufacturing team: An examination of LA-ICP-AES in a mobile configuration. Final report

International Nuclear Information System (INIS)

1994-05-01

The Department of Energy (DOE) has identified the need for field-deployable elemental analysis devices that are safer, faster, and less expensive than the fixed laboratory procedures now used to screen hazardous waste sites. As a response to this need, the Technology Integration Program (TIP) created a mobile, field-deployable laser ablation-inductively coupled plasma-atomic emission spectrometry (LA-ICP-AES) sampling and analysis prototype. Although the elemental. screening prototype has been successfully field-tested, continued marketing and technical development efforts are required to transfer LA-ICP-AES technology to the commercial sector. TIP established and supported a student research and design group called the Integrated Design for Marketing and Manufacturing (IDMM) team to advance the technology transfer of mobile, field-deployable LA-ICP-AES. The IDMM team developed a conceptual design (which is detailed in this report) for a mobile, field-deployable LA-ICP-AES sampling and analysis system, and reports the following findings: Mobile, field-deployable LA-ICP-AES is commercially viable. Eventual regulatory acceptance of field-deployable LA-ICP-AES, while not a simple process, is likely. Further refinement of certain processes and components of LA-ICP-AES will enhance the device's sensitivity and accuracy

Analysis of metal-laden water via portable X-ray fluorescence spectrometry

Science.gov (United States)

Pearson, Delaina; Weindorf, David C.; Chakraborty, Somsubhra; Li, Bin; Koch, Jaco; Van Deventer, Piet; de Wet, Jandre; Kusi, Nana Yaw

2018-06-01

A rapid method for in-situ elemental composition analysis of metal-laden water would be indispensable for studying polluted water. Current analytical lab methods to determine water quality include flame atomic absorption spectrometry (FAAS), atomic absorption spectrophotometry (AAS), electrothermal atomic absorption spectrometry (EAAS), and inductively coupled plasma (ICP) spectroscopy. However only two field methods, colorimetry and absorptiometry, exist for elemental analysis of water. Portable X-ray fluorescence (PXRF) spectrometry is an effective method for elemental analysis of soil, sediment, and other matrices. However, the accuracy of PXRF is known to be affected while scanning moisture-laden soil samples. This study sought to statistically establish PXRF's predictive ability for various elements in water at different concentrations relative to inductively coupled plasma atomic emission spectroscopy (ICP-AES). A total of 390 metal-laden water samples collected from leaching columns of mine tailings in South Africa were analyzed via PXRF and ICP-AES. The PXRF showed differential effectiveness in elemental quantification. For the collected water samples, the best relationships between ICP and PXRF elemental data were obtained for K and Cu (R2 = 0.92). However, when scanning ICP calibration solutions with elements in isolation, PXRF results indicated near perfect agreement; Ca, K, Fe, Cu and Pb produced an R2 of 0.99 while Zn and Mn produced an R2 of 1.00. The utilization of multiple PXRF (stacked) beams produced stronger correlation to ICP relative to the use of a single beam in isolation. The results of this study demonstrated the PXRF's ability to satisfactorily predict the composition of metal-laden water as reported by ICP for several elements. Additionally this study indicated the need for a "Water Mode" calibration for the PXRF and demonstrates the potential of PXRF for future study of polluted or contaminated waters.

Visualisation of axolotl blastema cells and pig endothelial progenitor cells using very small super paramagnetic iron oxide particles in MRI: A technique with applications for non invasive visualisation of regenerative processes

DEFF Research Database (Denmark)

Lauridsen, Henrik; Kjær, N.B.; Bek, Maria

oxide particles (VSOP) in animal cells enable non invasive cell tracking using magnetic resonance imaging (MRI) and can prove useful, when visualising regenerative processes. This study examines the possibility of labelling limited numbers of axolotl blastema cells (aBC) and pig endothelial progenitor...... implanted in live axolotl tail and dead porcine heart, respectively. Cellular iron uptake was determined using inductively coupled plasma optical emission spectrometry (ICP-OES). Results: T2*-weighted 2D gradient-echo sequences on samples of 10˄5 cells yielded at significant linear correlations between...

Study of the removal of cesium from aqueous solutions by graphene oxide; Estudo da remocao de cesio em solucoes aquosas por oxido de grafeno

Energy Technology Data Exchange (ETDEWEB)

Bueno, Vanessa N.; Rodrigues, Debora F. [University of Houston (UH), Houston, TX (United States); Vitta, Patricia B. Di [Universidade de Sao Paulo (STRES/USP), Sao Paulo, SP (Brazil). Inst. de Quimica. Setor Tecnico de Residuos Quimicos e Solventes; Oshiro, Mauricio T.; Vicente, Roberto; Hiromoto, Goro; Potiens Junior, Ademar; Sakata, Solange K., E-mail: sksakata@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

2013-07-01

Graphene oxide, used in this work, was synthesized from the oxidation of graphite by Hummer method. The experiments were performed in batch and analyzed for the following parameters: contact time, pH, cesium ion concentration in aqueous solution and removing capacity of the graphene oxide. After the experiments the samples were vacuum filtered and the remaining cesium in solution was quantified by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The equilibrium was reached after 60 minutes of contact in neutral solution. The percentage of removal was around 80%.

Study of the removal of cesium from aqueous solutions by graphene oxide

International Nuclear Information System (INIS)

Bueno, Vanessa N.; Rodrigues, Debora F.; Vitta, Patricia B. Di

2013-01-01

Graphene oxide, used in this work, was synthesized from the oxidation of graphite by Hummer method. The experiments were performed in batch and analyzed for the following parameters: contact time, pH, cesium ion concentration in aqueous solution and removing capacity of the graphene oxide. After the experiments the samples were vacuum filtered and the remaining cesium in solution was quantified by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The equilibrium was reached after 60 minutes of contact in neutral solution. The percentage of removal was around 80%

Forensic analysis of tempered sheet glass by particle induced X-ray emission (PIXE)

Energy Technology Data Exchange (ETDEWEB)

Jisonna, L.J. [Department of Chemistry and Department of Physics, Hope College, Holland, MI 49422-9000 (United States); DeYoung, P.A., E-mail: deyoung@hope.ed [Department of Chemistry and Department of Physics, Hope College, Holland, MI 49422-9000 (United States); Ferens, J.; Hall, C.; Lunderberg, J.M.; Mears, P. [Department of Chemistry and Department of Physics, Hope College, Holland, MI 49422-9000 (United States); Padilla, D. [Department of Physics, San Diego State University, San Diego, CA 92182-1233 (United States); Peaslee, G.F. [Department of Chemistry and Department of Physics, Hope College, Holland, MI 49422-9000 (United States); Sampson, R. [Department of Physics, Columbia University, New York, NY 10027 (United States)

2011-05-15

Highlights: {yields} PIXE was found to give the same results for trace elements in glass as ICP. {yields} PIXE can non-destructively determine trace element concentrations in auto glass. {yields} Measured Ca, Fe, Ti, Mn, and Sr in auto glass with PIXE. -- Abstract: The elemental concentrations of five trace elements in tempered sheet glass fragments were determined using particle-induced X-ray emission (PIXE) spectrometry. The trace element concentrations for calcium, iron, manganese, strontium, and titanium are compared to those obtained by inductively-coupled plasma-atomic emission spectrometry (ICP-AES) following complete digestion by hydrofluoric acid. For these five elements, the absolute concentrations obtained by both methods are shown to agree well over a wide range of concentrations. The limits of detection for trace elements are typically lower for the ICP-AES method. However, we show that the concentrations of these five elements can be accurately measured by the PIXE method. Since PIXE is an entirely non-destructive method, there exists a niche for this technique to be used as a complement to the more sensitive ICP-AES technique in the forensic analysis of sheet glass.

Determination of inorganic pollutants in soil after volatilization using microwave-induced combustion

Energy Technology Data Exchange (ETDEWEB)

Picoloto, Rochele S. [Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil and Instituto Nacional de Ciência e Tecnologia de Bioanalítica, Campinas, SP (Brazil); Wiltsche, Helmar; Knapp, Günter [Institute of Analytical Chemistry and Food Chemistry, Graz University of Technology, Graz (Austria); Mello, Paola A. [Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil and Instituto Nacional de Ciência e Tecnologia de Bioanalítica, Campinas, SP (Brazil); Barin, Juliano S. [Departamento de Tecnologia e Ciência dos Alimentos, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS (Brazil); Flores, Erico M.M., E-mail: ericommf@gmail.com [Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil and Instituto Nacional de Ciência e Tecnologia de Bioanalítica, Campinas, SP (Brazil)

2013-08-01

Microwave-induced combustion (MIC) was applied for analyte volatilization from soil and subsequent determination of As, Cd and Pb by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES), and Hg by cold vapor generation inductively coupled plasma mass spectrometry (CVG-ICP-MS). Soil samples (up to 300 mg) were mixed with microcrystalline cellulose, pressed as pellets and combusted in closed quartz vessels pressurized with 20 bar O{sub 2}. Analytes were volatilized from soil during combustion and quantitatively absorbed in a suitable solution: nitric acid (1, 2, 4 or 6 mol L{sup −1}) or a solution of nitric (2 mol L{sup −1}) and hydrochloric (1, 2 or 4 mol L{sup −1}) acids. Accuracy was evaluated using certified reference materials of soil (NIST 2709, San Joaquin Soil) and sediment (SUD-1, Sudbury sediment for trace elements). Agreement with certified values was better than 95% (t-test, 95% confidence level) for all analytes when 6 mL of a solution of 2 mol L{sup −1} HNO{sub 3} and 2 mol L{sup −1} HCl was used with a reflux step of 5 min. The limit of detection was 0.010, 0.002, 0.009 and 0.012 μg g{sup −1} for As, Cd, Hg and Pb, respectively using ICP-MS determination. A clear advantage of the proposed method over classical approaches is that only diluted solution is used. Moreover, a complete separation of the analytes from matrix is achieved minimizing potential interferences in ICP-MS or ICP-OES determination. Up to eight samples can be digested in a single run of only 25 min, resulting in a solution suitable for the determination of all analytes by both techniques. - Highlights: ► Microwave-induced combustion method was applied for soil samples. ► Analytes were volatilized during MIC allowing a suitable separation from matrix. ► Matrix interferences during the determination step are minimized. ► As, Cd, Hg and Pb were determined by ICP-MS. ► Diluted acid solutions were

Algal Biomass Analysis by Laser-Based Analytical Techniques—A Review

Czech Academy of Sciences Publication Activity Database

Pořízka, P.; Procházková, P.; Procházka, D.; Sládková, L.; Novotný, J.; Petrilak, M.; Brada, M.; Samek, Ota; Pilát, Zdeněk; Zemánek, Pavel; Adam, V.; Kizek, R.; Novotný, K.; Kaiser, J.

2014-01-01

Roč. 14, 23 SEP (2014), s. 17725-17752 ISSN 1424-8220 R&D Projects: GA MŠk(CZ) LO1212; GA MŠk ED0017/01/01; GA ČR GAP205/11/1687 Institutional support: RVO:68081731 Keywords : Laser-Induced Breakdown Spectroscopy * LIBS * Laser-Ablation Inductively Coupled Plasma coupled with Mass Spectroscopy and Optical Emission Spectroscopy * LA-ICP-MS * LA-ICP-OES * ICP-OES * Raman spectroscopy * algae * algal biomass * biofuel * bioremediation Subject RIV: BH - Optics, Masers, Lasers Impact factor: 2.245, year: 2014

Mass spectrometry of long-lived radionuclides

International Nuclear Information System (INIS)

Becker, Johanna Sabine.

2003-01-01

The capability of determining element concentrations at the trace and ultratrace level and isotope ratios is a main feature of inorganic mass spectrometry. The precise and accurate determination of isotope ratios of long-lived natural and artificial radionuclides is required, e.g. for their environmental monitoring and health control, for studying radionuclide migration, for age dating, for determining isotope ratios of radiogenic elements in the nuclear industry, for quality assurance and determination of the burn-up of fuel material in a nuclear power plant, for reprocessing plants, nuclear material accounting and radioactive waste control. Inorganic mass spectrometry, especially inductively coupled plasma mass spectrometry (ICP-MS) as the most important inorganic mass spectrometric technique today, possesses excellent sensitivity, precision and good accuracy for isotope ratio measurements and practically no restriction with respect to the ionization potential of the element investigated--therefore, thermal ionization mass spectrometry (TIMS), which has been used as the dominant analytical technique for precise isotope ratio measurements of long-lived radionuclides for many decades, is being replaced increasingly by ICP-MS. In the last few years instrumental progress in improving figures of merit for the determination of isotope ratio measurements of long-lived radionuclides in ICP-MS has been achieved by the application of a multiple ion collector device (MC-ICP-MS) and the introduction of the collision cell interface in order to dissociate disturbing argon-based molecular ions, to reduce the kinetic energy of ions and neutralize the disturbing noble gas ions (e.g. of 129 Xe + for the determination of 129 I). The review describes the state of the art and the progress of different inorganic mass spectrometric techniques such as ICP-MS, laser ablation ICP-MS vs. TIMS, glow discharge mass spectrometry, secondary ion mass spectrometry, resonance ionization mass

Precise and accurate isotope ratio measurements by ICP-MS.

Science.gov (United States)

Becker, J S; Dietze, H J

2000-09-01

The precise and accurate determination of isotope ratios by inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS (LA-ICP-MS) is important for quite different application fields (e.g. for isotope ratio measurements of stable isotopes in nature, especially for the investigation of isotope variation in nature or age dating, for determining isotope ratios of radiogenic elements in the nuclear industry, quality assurance of fuel material, for reprocessing plants, nuclear material accounting and radioactive waste control, for tracer experiments using stable isotopes or long-lived radionuclides in biological or medical studies). Thermal ionization mass spectrometry (TIMS), which used to be the dominant analytical technique for precise isotope ratio measurements, is being increasingly replaced for isotope ratio measurements by ICP-MS due to its excellent sensitivity, precision and good accuracy. Instrumental progress in ICP-MS was achieved by the introduction of the collision cell interface in order to dissociate many disturbing argon-based molecular ions, thermalize the ions and neutralize the disturbing argon ions of plasma gas (Ar+). The application of the collision cell in ICP-QMS results in a higher ion transmission, improved sensitivity and better precision of isotope ratio measurements compared to quadrupole ICP-MS without the collision cell [e.g., for 235U/238U approximately 1 (10 microg x L(-1) uranium) 0.07% relative standard deviation (RSD) vs. 0.2% RSD in short-term measurements (n = 5)]. A significant instrumental improvement for ICP-MS is the multicollector device (MC-ICP-MS) in order to obtain a better precision of isotope ratio measurements (with a precision of up to 0.002%, RSD). CE- and HPLC-ICP-MS are used for the separation of isobaric interferences of long-lived radionuclides and stable isotopes by determination of spallation nuclide abundances in an irradiated tantalum target.

Inductively coupled plasma emission spectrometric detection of simulated high performance liquid chromatographic peaks

International Nuclear Information System (INIS)

Fraley, D.M.; Yates, D.; Manahan, S.E.

1979-01-01

Because of its multielement capability, element-specificity, and low detection limits, inductively coupled plasma optical emission spectrometry (ICP) is a very promising technique for the detection of specific elemental species separated by high performance liquid chromatography (HPLC). This paper evaluated ICP as a detector for HPLC peaks containing specific elements. Detection limits for a number of elements have been evaluated in terms of the minimum detectable concentration of the element at the chromatographic peak maximum. The elements studies were Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, Sb, Se, Sr, Ti, V, and Zn. In addition, ICP was compared with atomic absorption spectrometry for the detection of HPLC peaks composed of EDTA and NTA chelates of copper. Furthermore, ICP was compared to uv solution absorption for the detection of copper chelates. 6 figures, 4 tables

Uranium isotopes determination in urine samples using alpha spectrometry and ICP-MS

International Nuclear Information System (INIS)

Rosa, Mychelle M.L.; Maihara, Vera A.; Tine, Fernanda D.; Santos, Sandra M.C.; Bonifacio, Rodrigo L.; Taddei, Maria HelenaT.

2015-01-01

The action of determining the concentration of uranium isotopes in biological samples, 'in vitro' bioassay, is an indirect method for evaluating the incorporation and quantification of these radionuclides internally deposited. When incorporated, these radionuclides tend to be disposed through excretion, with urine being the main source of data because it can be easily collected and analyzed. The most widely used methods for determination of uranium isotopes ( 234 U, 235 U and 238 U) are Alpha Spectrometry and ICP-MS. This work presents a comparative study for the determination of uranium isotopes using these two methodologies in real samples from occupationally exposed workers. In order to validate the methodology, a sample of the intercomparison exercise organized by PROCORAD (Association pour la Promotion du Controle de Qualite des Analyses de Biologie Medicale em Radiotoxicologie) was used, and the results were statistically compared applying the Student's t-test. (author)

Chemical characterization of airborne particulate matter in ambient air of Nagoya, Japan, as studied by the multielement determination with ICP-AES and ICP-MS

International Nuclear Information System (INIS)

Fukai, Taku; Kobayashi, Tatsuya; Sakaguchi, Masahiro; Aoki, Masanori; Saito, Tsuyoshi; Fujimori, Eiji; Haraguchi, Hiroki

2007-01-01

The multielement determination of PM 10 (airborne particulate matter smaller than 10 μm) samples, which was collected by a high volume air sampler at the urban site of Nagoya City, was carried out by inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). The present analytical method was validated by analyzing urban particulate matter standard reference material of NIST SRM 1648. The analytical data for ca. 30 elements in PM 10 samples collected during a period from 8 September to 9 October, 2003, were obtained in the concentration range from sub-μg g -1 to several-10 mg g -1 , but the data for 18 elements among ca. 30 elements were available for the characterization of PM 10 samples in ambient air, because of problems caused by the filter blanks. Then, the trends concerning the distributions of diverse elements in PM 10 samples were analyzed based on the enrichment factors and size distribution factors. The lithophile and siderophile elements were distributed more than 50% in coarse particle fraction (>2.1 μm), which was derived mainly from natural sources, such as soils and crustal minerals. On the other hand, chalcophile elements were distributed more than 50% in fine particle fraction ( 10 samples as well as their mining influence factors (MIFs) suggested their wide use in industrial productions. (author)

Evaluation of laser induced breakdown spectroscopy for cadmium determination in soils

International Nuclear Information System (INIS)

Santos, Dario; Nunes, Lidiane C.; Trevizan, Lilian C.; Godoi, Quienly; Leme, Flavio O.; Braga, Jez Willian B.; Krug, Francisco Jose

2009-01-01

Cadmium is known to be a toxic agent that accumulates in the living organisms and present high toxicity potential over lifetime. Efforts towards the development of methods for microanalysis of environmental samples, including the determination of this element by graphite furnace atomic absorption spectrometry (GFAAS), inductively coupled plasma optical emission spectrometry (ICP OES), and inductively coupled plasma-mass spectrometry (ICP-MS) techniques, have been increasing. Laser induced breakdown spectroscopy (LIBS) is an emerging technique dedicated to microanalysis and there is a lack of information dealing with the determination of cadmium. The aim of this work is to demonstrate the feasibility of LIBS for cadmium detection in soils. The experimental setup was designed using a laser Q-switched (Nd:YAG, 10 Hz, λ = 1064 nm) and the emission signals were collimated by lenses into an optical fiber coupled to a high-resolution intensified charge-coupled device (ICCD)-echelle spectrometer. Samples were cryogenically ground and thereafter pelletized before LIBS analysis. Best results were achieved by exploring a test portion (i.e. sampling spots) with larger surface area, which contributes to diminish the uncertainty due to element specific microheterogeneity. Calibration curves for cadmium determination were achieved using certified reference materials. The metrological figures of merit indicate that LIBS can be recommended for screening of cadmium contamination in soils.

Determination of trace elements and screening of metalloproteins in human blood and tissues

International Nuclear Information System (INIS)

Prohaska, K.

2003-02-01

Sequential and simultaneous atomic spectrometric detection was applied for the determination of metals in human whole blood, blood fractions and joint tissues. For this purpose ICP-OES (inductively coupled plasma - optical emission spectrometry) and GFAAS (graphite furnace - atomic absorption spectrometry) were optimized. The nebulizing technique of the ICP-OES causes a high consumption of the sample (2.4 mL /min uptake rate). Using the simultaneous modus of measurement it is possible to determine up to 20 elements in the samples of interest. Using GFAAS the elements can be detected sequentially only, the method is more time consuming in comparison. For the direct sample injection into the graphite tube only 20 aeL are needed. Since 1 mL sample has to be filled in the sample vessel of the autosampler, up to six elements can be determined in this volume. The most important advantage of the simultaneous multi-element detection is the low sample consumption, which is essential for analysis of biological samples. Normally only small amounts of human blood or tissues can be collected, and the concentrations of analytes are usually very low. Therefore in many cases a sample preparation is of advantage, which enables a pre-concentration of the analyte. The sample digestion was optimized with respect to the possible pre-concentration of the analytes. Ashing of the freeze-dried blood enabled a six fold higher concentration in the measuring solution compared with wet digestion of blood. For the ICP-OES sample introduction system two different nebulizers were tested in the complex matrix of the digested blood samples. A Meinhard and the microconcentric nebulizer were compared according to their analytical performance. The matrix of the samples caused LODs three to five times higher than in the aqueous standards. The application of the Meinhard nebulizer enabled sufficiently low LODs in the matrix for some elements of interest (Ca, Cu, Fe, Mg, P, S, Zn in freeze-dried blood

Programs in Fortran language for reporting the results of the analyses by ICP emission spectroscopy

International Nuclear Information System (INIS)

Roca, M.

1985-01-01

Three programs, written in FORTRAN IV language, for reporting the results of the analyses by ICP emission spectroscopy from data stored in files on floppy disks have been developed. They are intended, respectively, for the analyses of: 1) waters, 2) granites and slates, and 3) different kinds of geological materials. (Author) 8 refs

A Plasma Based OES-CRDS Dual-mode Portable Spectrometer for Trace Element Detection: Emission and Ringdown Measurements of Mercury

Science.gov (United States)

Sahay, Peeyush; Scherrer, Susan; Wang, Chuji

2012-10-01

Design and development of a plasma based optical emission spectroscopy-cavity ringdown spectroscopy (OES-CRDS) dual-mode portable spectrometer for in situ monitoring of trace elements is described. A microwave plasma torch (MPT) has been utilized, which serves both as an atomization and excitation source for the two modes, viz. OES and CRDS, of the spectrometer. Operation of both modes of the instrument is demonstrated with initial measurements of elemental mercury (Hg). A detection limit of 44 ng mL-1 for Hg at 253.65 nm was determined with the emission mode of the instrument. Severe radiation trapping of 253.65 nm line hampers the measurement of Hg in higher concentration region (> 50 μg ml-1). Therefore, a different wavelength, 365.01 nm, is suggested to measure Hg in that region. Ringdown measurements of the metastable 6s6p ^3P0 state of Hg in the plasma using a 404.65 nm palm size diode laser was conducted to demonstrate the CRDS mode of the instrument. Along with being portable, dual-mode, and self-calibrated, the instrument is capable of measuring a wide range of concentration ranging from sub ng mL-1 to several μg ml-1 for a number of elements.

Multielement determination of rare earth elements by liquid chromatography/inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Sawatari, Hideyuki; Asano, Takaaki; Hu, Xincheng; Saizuka, Tomoo; Itoh, Akihide; Hirose, Akio; Haraguchi, Hiroki

1995-01-01

The rapid determination of rare earth elements (REEs) has been investigated by an on-line system of high performance liquid chromatography/multichannel inductively coupled plasma atomic emission spectrometry. In the present system, all REEs could be detected simultaneously in a single chromatographic measurement without spectral interferences. Utilizing a cation exchange column and 2-hydroxy-2-methylpropanoic acid aqueous solution as the mobile phase, the detection limits of 0.4-30 ng ml -1 for all REEs were obtained. The system was applied to the determination of REEs in geological standard rock samples and rare earth impurities in high purity rare earth oxides. The REEs in standard rocks could be determined by the present HPLC/ICP-AES system without pretreatment after acid digestion, although the detection limits were not sufficient for the analysis of rare earth oxides. (author)

Radiochemical separation of actinides from environmental samples for determination with DF-ICP-MS and alpha spectrometry

International Nuclear Information System (INIS)

Ayranov, M.; Kraehenbuehl, U.; Sahli, H.; Roellin, S.; Burger, M.

2005-01-01

The purpose of this study was to develop an optimised sample preparation method for the determination of Pu, Am, and Cm in environmental samples, soils, and sediments, and to compare the sensitivities of DF-ICP-MS, alpha spectrometry, and liquid scintillation alpha spectrometry. Borate fusion was used for sample material digestion. Two methods based on TOPO liquid-liquid extraction and combination of TEVA and TRU extraction chromatography showed highest yields of 92.7% for Pu, 86.8% for Am, and 87.6% for Cm. The detection limits were between 0.014-0.034 Bq/kg for 239 Pu, 0.014-0.093 Bq/kg for 240 Pu, and 0.011-1.20 Bq/kg for 241 Am. Analytical results for 238 Pu, 239 Pu, 240 Pu, 241 Pu and 241 Am and their isotope ratios in certified reference materials (IAEA-135 and IAEA-300) indicated very good accuracy of the methods proposed. (orig.)

Quantification of trace amounts of rare earth elements in high purity gadolinium oxide by sector field inductively coupled plasma mass spectrometry (ICP-MS)

International Nuclear Information System (INIS)

Pedreira, W.R.; Silva Queiroz, C.A. da; Abrao, A.; Pimentel, M.M.

2004-01-01

In recent years, rare earth elements (REEs) have received much attention in the fields of geochemistry and industry. Gadolinium oxide is used for many different high technology applications such as infrared absorbing automotive glass, petroleum cracking catalyst, gadolinium-yttrium garnets, microwave applications, and color TV tube phosphors. It can also be used in optical glass manufacturing and in the electronic industry. Rapid and accurate determinations of the rare earth elements are increasingly required as industrial demands expand. In general, the inductively coupled plasma mass spectrometry (ICP-MS) presents some advantages for trace element analysis, due to high sensitivity and resolution, when compared with other analytical techniques. In this work, sector field inductively coupled plasma mass spectrometry was used. Sixteen elements (Sc, Y, and 14 lanthanides) were determined selectively with the ICP-MS system using a concentration gradient method. The detection limits with the ICP-MS system were about 0.2-8 pg ml -1 . The recovery percentage ranged from 95 to 100% for different rare earth elements. The %R.S.D. of the methods varying between 1.5 and 2.5% for a set of five (n=5) replicates was found for the IPEN's material and for the certificate reference sample. Determination of trace REEs in two high pure gadolinium oxides samples (IPEN and JMC) was performed. IPEN's material is highly pure (>99.99%) and was successfully analyzed without spectral interference

[Enhancement effect of double-beam laser processed aqueous solution on ICP emission spectrum].

Science.gov (United States)

Chen, Jin-zhong; Xu, Li-jing; Su, Hong-xin; Li, Xu; Wang, Shu-fang

2015-01-01

In order to change the physical properties of aqueous solution and improve the radiation intensity of the ICP emission spectrum, the effects of different laser power density and irradiation time on the surface tension and viscosity of aqueous solution were investigated by using near infrared laser at 976 nm and CO2 laser at 10. 6 µm to irradiate aqueous solution orthogonally, then the enhancement of ICP spectral intensity with processed solution was discussed. The results showed that the surface tension and viscosity of aqueous solution reduced by 42. 13% and 14. 03% compared with the untreated, and the atomization efficiency increased by 51.26% at the laser power density 0. 265 7 W . cm-2 of 976 nm and 0. 206 9 W . cm-2 of CO2 laser with 40 min irradiation time. With the optimized aqueous solution introduced into the ICP source, the spectral line intensity of sample elements As, Cd, Cr, Hg and Pb was enhanced by 46.29%, 94. 65%, 30. 76%, 33.07% and 94. 58% compared to the untreated aqueous solution, while the signal-to-background ratio increased by 43. 84%, 85. 35%, 28. 71%, 34. 37% and 90. 91%, respectively. Plasma temperature and electron density also increased by 5. 94% and 1. 18% respectively. It is obvious that the method of double-beam laser orthogonal irradiation on solution can reduce the surface tension and viscosity of aqueous solution significantly, and raise the radiationintensity of ICP source, and will provide a better condition for detecting the trace heavy metal elements in water samples.

Uranium isotopes determination in urine samples using alpha spectrometry and ICP-MS

Energy Technology Data Exchange (ETDEWEB)

Rosa, Mychelle M.L.; Maihara, Vera A. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Tine, Fernanda D.; Santos, Sandra M.C.; Bonifacio, Rodrigo L.; Taddei, Maria HelenaT. [Comissao Nacional de Energia Nuclear (LAPOC/CNEN-MG), Pocos de Caldas, MG (Brazil). Laboratorio de Pocos de Caldas

2015-07-01

The action of determining the concentration of uranium isotopes in biological samples, 'in vitro' bioassay, is an indirect method for evaluating the incorporation and quantification of these radionuclides internally deposited. When incorporated, these radionuclides tend to be disposed through excretion, with urine being the main source of data because it can be easily collected and analyzed. The most widely used methods for determination of uranium isotopes ({sup 234}U, {sup 235}U and {sup 238}U) are Alpha Spectrometry and ICP-MS. This work presents a comparative study for the determination of uranium isotopes using these two methodologies in real samples from occupationally exposed workers. In order to validate the methodology, a sample of the intercomparison exercise organized by PROCORAD (Association pour la Promotion du Controle de Qualite des Analyses de Biologie Medicale em Radiotoxicologie) was used, and the results were statistically compared applying the Student's t-test. (author)

Assessment of high precision, high accuracy Inductively Coupled Plasma-Optical Emission Spectroscopy to obtain concentration uncertainties less than 0.2% with variable matrix concentrations

International Nuclear Information System (INIS)

Rabb, Savelas A.; Olesik, John W.

2008-01-01

The ability to obtain high precision, high accuracy measurements in samples with complex matrices using High Performance Inductively Coupled Plasma-Optical Emission Spectroscopy (HP-ICP-OES) was investigated. The Common Analyte Internal Standard (CAIS) procedure was incorporated into the High Performance Inductively Coupled Plasma-Optical Emission Spectroscopy method to correct for matrix-induced changes in emission intensity ratios. Matrix matching and standard addition approaches to minimize matrix-induced errors when using High Performance Inductively Coupled Plasma-Optical Emission Spectroscopy were also assessed. The High Performance Inductively Coupled Plasma-Optical Emission Spectroscopy method was tested with synthetic solutions in a variety of matrices, alloy standard reference materials and geological reference materials

OeFAD8, OeLIP and OeOSM expression and activity in cold-acclimation of Olea europaea, a perennial dicot without winter-dormancy.

Science.gov (United States)

D'Angeli, Simone; Matteucci, Maya; Fattorini, Laura; Gismondi, Angelo; Ludovici, Matteo; Canini, Antonella; Altamura, Maria Maddalena

2016-05-01

Cold-acclimation genes in woody dicots without winter-dormancy, e.g., olive-tree, need investigation. Positive relationships between OeFAD8, OeOSM , and OeLIP19 and olive-tree cold-acclimation exist, and couple with increased lipid unsaturation and cutinisation. Olive-tree is a woody species with no winter-dormancy and low frost-tolerance. However, cold-tolerant genotypes were empirically selected, highlighting that cold-acclimation might be acquired. Proteins needed for olive-tree cold-acclimation are unknown, even if roles for osmotin (OeOSM) as leaf cryoprotectant, and seed lipid-transfer protein for endosperm cutinisation under cold, were demonstrated. In other species, FAD8, coding a desaturase producing α-linolenic acid, is activated by temperature-lowering, concomitantly with bZIP-LIP19 genes. The research was focussed on finding OeLIP19 gene(s) in olive-tree genome, and analyze it/their expression, and that of OeFAD8 and OeOSM, in drupes and leaves under different cold-conditions/developmental stages/genotypes, in comparison with changes in unsaturated lipids and cell wall cutinisation. Cold-induced cytosolic calcium transients always occurred in leaves/drupes of some genotypes, e.g., Moraiolo, but ceased in others, e.g., Canino, at specific drupe stages/cold-treatments, suggesting cold-acclimation acquisition only in the latter genotypes. Canino and Moraiolo were selected for further analyses. Cold-acclimation in Canino was confirmed by an electrolyte leakage from leaf/drupe membranes highly reduced in comparison with Moraiolo. Strong increases in fruit-epicarp/leaf-epidermis cutinisation characterized cold-acclimated Canino, and positively coupled with OeOSM expression, and immunolocalization of the coded protein. OeFAD8 expression increased with cold-acclimation, as the production of α-linolenic acid, and related compounds. An OeLIP19 gene was isolated. Its levels changed with a trend similar to OeFAD8. All together, results sustain a positive

Chemical analysis of zinc electroplating solutions by x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Jung, Sung-Mo; Cho, Young-Mo; Na, Han-Gil

2007-01-01

A quantitative analysis method used to analyze chlorine, iron and zinc in electroplating solutions, using X-ray spectrometry in atmospheric He mode, is proposed. The present research concerns the replacement of the conventional analyses of electroplating solutions with rapid and reproducible quantification using X-ray fluorescence spectrometer. An in-depth investigation conducted in the present study identifies the species present in the real electroplating solutions. XRD patterns and semi-quantitative results for the electroplating solutions show synthetic standards based on the compositional range of solutions by analyzing the electroplating solutions obtained in real processes. 28 calibration standard solutions are prepared by diluting liquid standard solutions certified by titration and ICP-OES analyses used to construct the XRF calibration curves for Cl, Fe and Zn. The suggested method showed satisfactory precision and accuracy in the analysis of electroplating solutions. The present study provides evidences that the proposed XRF spectrometry could be an alternative analytical method to replace the conventional techniques by comparing the uncertainties estimated for each method. (author)

Environmental atmospheric impact assessment by the emission of particles in an industrial area

International Nuclear Information System (INIS)

Gomez, Dario R.; Ledesma, Ariel G.; Vazquez, Cristina; Smichowski, Patricia N.; Romero, Carlos A.; Dawidowski, Laura E.; Ortiz, Maria; Marrero, Julieta G.

1999-01-01

The content of metals present in suspended particulate matter was evaluated using analytical related nuclear techniques, in order to discriminate the contribution of different emission sources to the atmospheric concentration in the area of Campana, located in the Province of Buenos Aires. The levels of Ti, V, Cr, Mn, Ni, Cu, Zn, Sr, Ag, Cd y Pb were quantified by Wave Dispersion X-Ray Florescence spectrometry (WDXRF), Total Reflection X-Ray Fluorescence spectrometry (TRXRF) and Inducted Coupled Plasma Absorption Emission spectroscopy (ICP-AES). (author)

ICP-AES method for metals in air. Pt 2 - analysis; final report on project R48113

International Nuclear Information System (INIS)

Taylor, C.; Howe, A.

2002-04-01

An ICP-AES instrument operating procedure has been drafted and incorporated in ISO 15202-3 Workplace air - Determination of metals and metalloids in airborne particulate matter by inductively coupled plasma atomic emission spectrometry: Part 3 - Analysis. It is expected that this International Standard will be published during 2003. The performance of the analytical method described ISO 15202-3 was evaluated by carrying out laboratory experiments to determine analytical precision. The uncertainty associated with analytical variability was then combined with other sources of uncertainty arising from the sampling method described in ISO 15202-1. A first draft of a proposed new MDHS on Metals and metalloids in workplace air by Inductively Coupled Plasma Atomic Emission Spectrometry has been prepared based on ISO 15202-1, ISO 15202-2 and ISO 15202-3. It is expected that this will be published in late 2002 or early 2003

Spectroscopic investigations of ceramic materials using ICP-OES with modern vaporisation systems

International Nuclear Information System (INIS)

Reisch, M.U.; Mazurkiewicz, M.; Nickel, H.

1990-10-01

The object of this work was to study the evaporation and excitation process in the analysis of ceramic powders by the direct insertion of the samples into an inductively coupled plasma (ICP) as well as by external electrothermal evaporation. The evaporation rates were monitored by using 59 Fe and 115 Cd radiaoactive isotopes. The influence of various parameters such as the geometrical conditions, the carrier gas injection and the flow characteristics have been investigated. These methods have the advantage of easy preparation, no dilution and short experiment durations. The influence of different thermochemical additives as well as third elements, matrix compositions and grain size of the powders was determined. (orig.) [de

Rapid Analysis of Ash Composition Using Laser-Induced Breakdown Spectroscopy (LIBS)

Energy Technology Data Exchange (ETDEWEB)

Tyler L. Westover

2013-01-01

Inorganic compounds are known to be problematic in the thermochemical conversion of biomass to syngas and ultimately hydrocarbon fuels. The elements Si, K, Ca, Na, S, P, Cl, Mg, Fe, and Al are particularly problematic and are known to influence reaction pathways, contribute to fouling and corrosion, poison catalysts, and impact waste streams. Substantial quantities of inorganic species can be entrained in the bark of trees during harvest operations. Herbaceous feedstocks often have even greater quantities of inorganic constituents, which can account for as much as one-fifth of the total dry matter. Current methodologies to measure the concentrations of these elements, such as inductively coupled plasma-optical emission spectrometry/mass spectrometry (ICP-OES/MS) are expensive in time and reagents. This study demonstrates that a new methodology employing laser-induced breakdown spectroscopy (LIBS) can rapidly and accurately analyze the inorganic constituents in a wide range of biomass materials, including both woody and herbaceous examples. This technique requires little or no sample preparation, does not consume any reagents, and the analytical data is available immediately. In addition to comparing LIBS data with the results from ICP-OES methods, this work also includes discussions of sample preparation techniques, calibration curves for interpreting LIBS spectra, minimum detection limits, and the use of internal standards and standard reference materials.

Simultaneous determination of macro and trace elements in biological reference materials by microwave induced plasma optical emission spectrometry with slurry sample introduction

International Nuclear Information System (INIS)

Matusiewicz, Henryk; Golik, Bartosz

2004-01-01

A slurry sampling technique (SST) has been utilized for simultaneous multi-element analysis by microwave-induced plasma optical emission spectrometry (MIP-OES). Slurry samples from a spray chamber are fed directly into the microwave cavity-torch assembly (power 300 W) with no desolvation apparatus. The performance of SST-MIP-OES was demonstrated by the determination of macro (Na, K, Ca, Mg, P) and trace (Cd, Cu, Mn, Sr, Zn) elements in three biological certified reference materials using a V-groove, clog-free Babington-type nebulizer. Slurry concentrations up to 1% m/v (particles 3 (pH 1.2) containing 0.01% of Triton X-100, were used with calibration by the standard additions method. The method offers relatively good precision (R.S.D. ranged from 7 to 11%) with measured concentrations being in satisfactory agreement with certified values for NRCC TORT-1 (Lobster hepatopancreas), NRCC LUTS-1 (Lobster hepatopancreas) and IAEA-153 (Milk powder). The concentrations of Na, K, Ca, Mg, P and Cd, Cu, Mn, Sr, Zn were determined in the range 90-22 000 μg/g and 1-420 μg/g, respectively. The method could be useful as a routine procedure

Neutron activation analysis and ICP-AES to determine metal traces in antarctic krill. CNEA laboratories participation in the certification of a reference material

International Nuclear Information System (INIS)

Smichowski, Patricia N.; Farias, Silvia S.; Resnizky, Sara M.; Marrero, Julieta G.

1999-01-01

For the international certification of a reference material based on krill, As and Hg were determined by instrumental neutron activation analysis and Br, Co and Se by radiochemical neutron activation analysis. Inductive coupling plasma atomic emission spectrometry (ICP-AES) was used to determine Cu, Fe, Mn, and Zn. The results, which are in good agreement with those obtained by other laboratories, are discussed

The influence of laser-particle interaction in laser induced breakdown spectroscopy and laser ablation inductively coupled plasma spectrometry

International Nuclear Information System (INIS)

Lindner, Helmut; Loper, Kristofer H.; Hahn, David W.; Niemax, Kay

2011-01-01

Particles produced by previous laser shots may have significant influence on the analytical signal in laser-induced breakdown spectroscopy (LIBS) and laser ablation inductively coupled plasma (LA-ICP) spectrometry if they remain close to the position of laser sampling. The effects of these particles on the laser-induced breakdown event are demonstrated in several ways. LIBS-experiments were conducted in an ablation cell at atmospheric conditions in argon or air applying a dual-pulse arrangement with orthogonal pre-pulse, i.e., plasma breakdown in a gas generated by a focussed laser beam parallel and close to the sample surface followed by a delayed crossing laser pulse in orthogonal direction which actually ablates material from the sample and produces the LIBS plasma. The optical emission of the LIBS plasma as well as the absorption of the pre-pulse laser was measured. In the presence of particles in the focus of the pre-pulse laser, the plasma breakdown is affected and more energy of the pre-pulse laser is absorbed than without particles. As a result, the analyte line emission from the LIBS plasma of the second laser is enhanced. It is assumed that the enhancement is not only due to an increase of mass ablated by the second laser but also to better atomization and excitation conditions favored by a reduced gas density in the pre-pulse plasma. Higher laser pulse frequencies increase the probability of particle-laser interaction and, therefore, reduce the shot-to-shot line intensity variation as compared to lower particle loadings in the cell. Additional experiments using an aerosol chamber were performed to further quantify the laser absorption by the plasma in dependence on time both with and without the presence of particles. The overall implication of laser-particle interactions for LIBS and LA-ICP-MS/OES are discussed.

The influence of laser-particle interaction in laser induced breakdown spectroscopy and laser ablation inductively coupled plasma spectrometry

Science.gov (United States)

Lindner, Helmut; Loper, Kristofer H.; Hahn, David W.; Niemax, Kay

2011-02-01

Particles produced by previous laser shots may have significant influence on the analytical signal in laser-induced breakdown spectroscopy (LIBS) and laser ablation inductively coupled plasma (LA-ICP) spectrometry if they remain close to the position of laser sampling. The effects of these particles on the laser-induced breakdown event are demonstrated in several ways. LIBS-experiments were conducted in an ablation cell at atmospheric conditions in argon or air applying a dual-pulse arrangement with orthogonal pre-pulse, i.e., plasma breakdown in a gas generated by a focussed laser beam parallel and close to the sample surface followed by a delayed crossing laser pulse in orthogonal direction which actually ablates material from the sample and produces the LIBS plasma. The optical emission of the LIBS plasma as well as the absorption of the pre-pulse laser was measured. In the presence of particles in the focus of the pre-pulse laser, the plasma breakdown is affected and more energy of the pre-pulse laser is absorbed than without particles. As a result, the analyte line emission from the LIBS plasma of the second laser is enhanced. It is assumed that the enhancement is not only due to an increase of mass ablated by the second laser but also to better atomization and excitation conditions favored by a reduced gas density in the pre-pulse plasma. Higher laser pulse frequencies increase the probability of particle-laser interaction and, therefore, reduce the shot-to-shot line intensity variation as compared to lower particle loadings in the cell. Additional experiments using an aerosol chamber were performed to further quantify the laser absorption by the plasma in dependence on time both with and without the presence of particles. The overall implication of laser-particle interactions for LIBS and LA-ICP-MS/OES are discussed.

Development of a certified reference material (NMIJ CRM 7505-a) for the determination of trace elements in tea leaves.

Science.gov (United States)

Zhu, Yanbei; Narukawa, Tomohiro; Inagaki, Kazumi; Kuroiwa, Takayoshi; Chiba, Koichi

2011-01-01

A certified reference material (CRM) for trace elements in tea leaves has been developed in National Metrology Institute of Japan (NMIJ). The CRM was provided as a dry powder (<90 µm) after frozen pulverization of washed and dried fresh tea leaves from a tea plant farm in Shizuoka Prefecture, Japan. Characterization of the property value for each element was carried out exclusively by NMIJ with at least two independent analytical methods, including inductively coupled plasma mass spectrometry (ICP-MS), high-resolution (HR-) ICP-MS, isotope-dilution (ID-) ICP-MS, inductively coupled plasma optical emission spectrometry (ICP-OES), graphite-furnace atomic-absorption spectrometry (GF-AAS) and flame atomic-absorption spectrometry (FAAS). Property values were provided for 19 elements (Ca, K, Mg, P, Al, B, Ba, Cd, Cu, Fe, Li, Mn, Na, Ni, Pb, Rb, Sr, Zn and Co) and informative values for 18 elements (Ti, V, Cr, Y, and all of the lanthanides, except for Pm whose isotopes are exclusively radioactive). The concentration ranges of property values and informative values were from 1.59% (mass) of K to 0.0139 mg kg(-1) of Cd and from 0.6 mg kg(-1) of Ti to 0.0014 mg kg(-1) of Lu, respectively. Combined relatively standard uncertainties of the property values were estimated by considering the uncertainties of the homogeneity, analytical methods, characterization, calibration standard, and dry-mass correction factor. The range of the relative combined standard uncertainties was from 1.5% of Mg and K to 4.1% of Cd.

Computer simulation of ICP spectra: A new tool for the study of excitation, emission, and line overlap

International Nuclear Information System (INIS)

Blades, M.W.; Burton, L.L.

1986-01-01

It is well known that the relatively high temperature of ICP sources provides an excitation environment relatively free from dissociation and vaporization interferences and, in addition, produces intense analyte line spectra and hence high analytical sensitivity. However, this feature also introduces the potential for spectral overlaps from sample concomitants. The degree to which an analyte spectral line intensity can be corrected for interfering spectral overlaps depends on many factors including spectrometer resolution, sample composition and ICP operating conditions. The authors have been using a computer program to assist them in the study of ICP analyte emission spectra. This program is being used to study the spectral distribution of line intensity information and also to do detailed investigations on spectral overlaps in complex sample mixtures. As input data the program uses tabulated wavelengths, transition probabilities (gA values), partition functions, excitation energies of the transitions, ionization energy, temperature, and Doppler and Stark linewidths

Analysis of Uranium and Thorium in Waste Water from Rare Earth Research and Development by ICP Spectrometry

International Nuclear Information System (INIS)

Pichestapong, Pipat; Injareon, Uthaiwan

2007-08-01

Full text: Waste water from Rare Earth Research and Development Center (RRDC) was analyzed to determine uranium and thorium concentration using ICP spectrometry. RRDC processes monazite ore to separate uranium, thorium and rare earth elements from the ore. Water samples from the ditch surrounding the center and from the canal nearby were also analyzed. Matrix spike technique was applied in this analysis. It was found that the highest concentration of uranium and thorium in the waste water samples were 3028±11 and 439±7 ppb, respectively. The concentration of uranium and thorium in the waste water samples were higher than those in water samples from the ditch and canal

Investigating the Effect of Glass Ion Release on the Cytocompatibility, Antibacterial Eflcacy and Antioxidant Activity of Y2O3 / CeO2 doped SiO2-SrO-Na2O glasses

Directory of Open Access Journals (Sweden)

Placek L. M.

2018-02-01

Full Text Available The effect on ion release and cytocompatibility of Yttrium (Y and Cerium (Ce are investigated when substituted for Sodium (Na in a 0.52SiO2-0.24SrO-0.24-Na2OMOglass series (where MO= Y2O3 or CeO2. Glass leaching was evaluated through pH measurements and Inductive Coupled Plasma-Optical Emission Spectrometry (ICP-OES analysiswhere the extract pH increased during incubation (11.2 - 12.5. Ion release of Silicon (Si, Na and Strontium (Sr from the Con glass was at higher than that of glasses containing Y or Ce, and reached a limit after 1 day. Ion release from Y and Ce containing glasses reached a maximum of 1800 μg/mL, 1800 μg/mL, and 10 μg/mL for Si, Na, and Sr, respectively. Release of Y and Cewas below the ICP- OES detection limit 75% of bacteria at a 9% extract concentration. Antioxidant capacity (mechanism for neuroprotection was evaluated using the ABTS assay. All glasses had inherent radical oxygen species (ROS scavenging capability with Con reaching 9.5 mMTE.

Tissue gadolinium deposition in hepatorenally impaired rats exposed to Gd-EOB-DTPA: evaluation with inductively coupled plasma mass spectrometry (ICP-MS).

Science.gov (United States)

Sato, Tomohiro; Tamada, Tsutomu; Watanabe, Shigeru; Nishimura, Hirotake; Kanki, Akihiko; Noda, Yasufumi; Higaki, Atsushi; Yamamoto, Akira; Ito, Katsuyoshi

2015-06-01

This study was undertaken to quantify tissue gadolinium (Gd) deposition in hepatorenally impaired rats exposed to gadolinium ethoxybenzyl diethylenetriamine pentaacetic acid (Gd-EOB-DTPA) by means of inductively coupled plasma mass spectrometry (ICP-MS) and to compare differences in Gd distribution among major organs as possible triggers for nephrogenic systemic fibrosis. Five hepatorenally impaired rats (5/6-nephrectomized, with carbon-tetrachloride-induced liver fibrosis) were injected with Gd-EOB-DTPA. Histological assessment was conducted and Gd content of the skin, liver, kidneys, lungs, heart, spleen, diaphragm, and femoral muscle was measured by inductively coupled plasma mass spectrometry (ICP-MS) at 7 days after last injection. In addition, five renally impaired rats were injected with Gd-EOB-DTPA and the degree of tissue Gd deposition was compared with that in the hepatorenally impaired rats. ICP-MS analysis revealed significantly higher Gd deposition in the kidneys, spleen, and liver (p = 0.009-0.047) in the hepatorenally impaired group (42.6 ± 20.1, 17.2 ± 6.1, 8.4 ± 3.2 μg/g, respectively) than in the renally impaired group (17.2 ± 7.7, 5.4 ± 2.1, 2.8 ± 0.7 μg/g, respectively); no significant difference was found for other organs. In the hepatorenally impaired group, Gd was predominantly deposited in the kidneys, followed by the spleen, liver, lungs, skin, heart, diaphragm, and femoral muscle. Histopathological investigation revealed hepatic fibrosis in the hepatorenally impaired group. Compared with renally impaired rats, tissue Gd deposition in hepatorenally impaired rats exposed to Gd-EOB-DTPA was significantly increased in the kidneys, spleen, and liver, probably due to the impairment of the dual excretion pathways of the urinary and biliary systems.

Plasma-based determination of inorganic contaminants in waste of electric and electronic equipment after microwave-induced combustion

Energy Technology Data Exchange (ETDEWEB)

Mello, Paola A.; Diehl, Lisarb O.; Oliveira, Jussiane S.S.; Muller, Edson I. [Departamento de Química, Universidade Federal de Santa Maria, Av. Roraima, 1000, 97105-900, Santa Maria (Brazil); Mesko, Marcia F. [Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, Campus Capão do Leão, 96900-010 Pelotas, RS (Brazil); Flores, Erico M.M., E-mail: ericommf@gmail.com [Departamento de Química, Universidade Federal de Santa Maria, Av. Roraima, 1000, 97105-900, Santa Maria (Brazil)

2015-03-01

A systematic study was performed for the determination of inorganic contaminants in polymeric waste from electrical and electronic equipment (EEE) for achieving an efficient digestion to minimize interferences in determination using plasma-based techniques. The determination of As, Br, Cd, Co, Cr, Cu, Ni, Pb, Sb, and Zn by inductively coupled plasma mass spectrometry (ICP-MS) and also by inductively coupled plasma optical emission spectrometry (ICP OES) was carried out after digestion using microwave-induced combustion (MIC). Arsenic and Hg were determined by flow-injection chemical vapor generation inductively coupled plasma mass spectrometry (FI-CVG-ICP-MS). Dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS) with ammonia was also used for Cr determination. The suitability of MIC for digestion of sample masses up to 400 mg was demonstrated using microcrystalline cellulose as aid for combustion of polymers from waste of EEEs that usually contain flame retardants that impair the combustion. The composition and concentration of acid solutions (HNO{sub 3} or HNO{sub 3} plus HCl) were evaluated for metals and metalloids and NH{sub 4}OH solutions were investigated for Br absorption. Accuracy was evaluated by comparison of results with those obtained using high pressure microwave-assisted wet digestion (HP-MAWD) and also by the analysis of certified reference material (CRM) of polymer (EC680k—low-density polyethylene). Bromine determination was only feasible using digestion by MIC once losses were observed when HP-MAWD was used. Lower limits of detection were obtained for all analytes using MIC (from 0.005 μg g{sup −1} for Co by ICP-MS up to 3.120 μg g{sup −1} for Sb by ICP OES) in comparison to HP-MAWD due to the higher sample mass that can be digested (400 mg) and the use of diluted absorbing solutions. The combination of HNO{sub 3} and HCl for digestion showed to be crucial for quantitative recovery of some elements, as Cr and Sb

Matrix separation by chelation to prepare biological materials for isotopic zinc analysis by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Durrant, S.F.; Krushevska, A.; Amarasiriwardena, D.; Argentine, M.D.; Romon-Guesnier, S.; Barnes, R.M.

1994-01-01

Following an evaluation of three chelating resins [Chelex-100, poly(dithiocarbamate) (PDTC) and carboxymethylated poly(ethyleneimine)-poly(methylenepolyphenylene) isocyanate (CPPI)], a procedure was established with the last of these for the separation of Zn from biological matrix elements prior to 70 Zn: 68 Zn isotopic analysis by inductively coupled plasma mass spectrometry (ICP-MS). The method was verified by establishing Zn recoveries and by determining its effectiveness in removing Cl and Na from buffered test solutions. Calcium, Na, and Zn concentration data were determined by inductively coupled plasma atomic emission spectrometry. Chlorine was measured by electrothermal vaporization ICP-MS. The efficacy of the technique was demonstrated by the determination of zinc isotope ratios in bovine milk and human urine. (Author)

Use of oxidative and reducing vapor generation for reducing the detection limits of iodine in biological samples by inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Vtorushina, Eh.A.; Saprykin, A.I.; Knapp, G.

2009-01-01

Procedures of microwave combustion in an oxygen flow and microwave acid decomposition of biological samples were optimized for the subsequent determination of iodine. A new method was proposed for the generation of molecular iodine from periodate iona using hydrogen peroxide as a reductant. Procedures were developed for determining iodine in biological samples by inductively coupled plasma atomic emission spectrometry (ICP-AES) using oxidative and reducing vapor generation; these allowed the detection limit for iodine to be lowered by 3-4 orders of magnitude. The developed procedures were used to analyze certified reference materials of milk (Skim Milk Powder BCR 150) and seaweed (Sea Lettuce BCR 279) and a Supradyn vitamin complex

Can we trust mass spectrometry for determination of arsenic peptides in plants: comparison of LC-ICP-MS and LC-ES-MS/ICP-MS with XANES/EXAFS in analysis of Thunbergia alata.

Science.gov (United States)

Bluemlein, Katharina; Raab, Andrea; Meharg, Andrew A; Charnock, John M; Feldmann, Jörg

2008-04-01

The weakest step in the analytical procedure for speciation analysis is extraction from a biological material into an aqueous solution which undergoes HPLC separation and then simultaneous online detection by elemental and molecular mass spectrometry (ICP-MS/ES-MS). This paper describes a study to determine the speciation of arsenic and, in particular, the arsenite phytochelatin complexes in the root from an ornamental garden plant Thunbergia alata exposed to 1 mg As L(-1) as arsenate. The approach of formic acid extraction followed by HPLC-ES-MS/ICP-MS identified different As(III)-PC complexes in the extract of this plant and made their quantification via sulfur (m/z 32) and arsenic (m/z 75) possible. Although sulfur sensitivity could be significantly increased when xenon was used as collision gas in ICP-qMS, or when HR-ICP-MS was used in medium resolution, the As:S ratio gave misleading results in the identification of As(III)-PC complexes due to the relatively low resolution of the chromatography system in relation to the variety of As-peptides in plants. Hence only the parallel use of ES-MS/ICP-MS was able to prove the occurrence of such arsenite phytochelatin complexes. Between 55 and 64% of the arsenic was bound to the sulfur of peptides mainly as As(III)(PC(2))(2), As(III)(PC(3)) and As(III)(PC(4)). XANES (X-ray absorption near-edge spectroscopy) measurement, using the freshly exposed plant root directly, confirmed that most of the arsenic is trivalent and binds to S of peptides (53% As-S) while 38% occurred as arsenite and only 9% unchanged as arsenate. EXAFS data confirmed that As-S and As-O bonds occur in the plants. This study confirms, for the first time, that As-peptides can be extracted by formic acid and chromatographically separated on a reversed-phase column without significant decomposition or de-novo synthesis during the extraction step.

Determination of the impurities Al, Mn, Fe, Ni, Cu and Zn in nuclear grade uranium by ICP-OES

Energy Technology Data Exchange (ETDEWEB)

Kakazu, Mauricio H.; Cotrim, Marycel E.B.; Silva, Douglas B. da; Pires, Maria Aparecida F., E-mail: mhkakazu@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

2011-07-01

Uranium compounds are specially produced for use in nuclear reactors and must meet strict physical and chemicals specifications. The current study discusses the separation of Al, Mn, Fe, Ni, Cu and Zn from uranium compounds and their quantitative determination using inductively coupled plasma optical emission spectrometry. To avoid interference effect caused by uranium in the spectroscopic emission lines of elements of interest, the chromatographic behavior of TBP impregnated macroporous Amberlite XAD-4 column was investigated. The break through curves of uranium obtained showed maximum retention of up to 11 grams of uranium and the elution curves for the elements showed reproducible recovery rate of 90% on 50 mL elution. Synthetic samples of nuclear grade uranium prepared with the addition of 250 {mu}g/g of U of the above individual elements were used to verify the performance of the method. The method showed a recovery rate of 80 to 90% for the elements under study. (author)

Determination of the impurities Al, Mn, Fe, Ni, Cu and Zn in nuclear grade uranium by ICP-OES

International Nuclear Information System (INIS)

Kakazu, Mauricio H.; Cotrim, Marycel E.B.; Silva, Douglas B. da; Pires, Maria Aparecida F.

2011-01-01

Uranium compounds are specially produced for use in nuclear reactors and must meet strict physical and chemicals specifications. The current study discusses the separation of Al, Mn, Fe, Ni, Cu and Zn from uranium compounds and their quantitative determination using inductively coupled plasma optical emission spectrometry. To avoid interference effect caused by uranium in the spectroscopic emission lines of elements of interest, the chromatographic behavior of TBP impregnated macroporous Amberlite XAD-4 column was investigated. The break through curves of uranium obtained showed maximum retention of up to 11 grams of uranium and the elution curves for the elements showed reproducible recovery rate of 90% on 50 mL elution. Synthetic samples of nuclear grade uranium prepared with the addition of 250 μg/g of U of the above individual elements were used to verify the performance of the method. The method showed a recovery rate of 80 to 90% for the elements under study. (author)

Simultaneous determination of macro and trace elements in biological reference materials by microwave induced plasma optical emission spectrometry with slurry sample introduction

Energy Technology Data Exchange (ETDEWEB)

Matusiewicz, Henryk E-mail: Henryk.Matusiewicz@put.poznan.pl; Golik, Bartosz

2004-05-21

A slurry sampling technique (SST) has been utilized for simultaneous multi-element analysis by microwave-induced plasma optical emission spectrometry (MIP-OES). Slurry samples from a spray chamber are fed directly into the microwave cavity-torch assembly (power 300 W) with no desolvation apparatus. The performance of SST-MIP-OES was demonstrated by the determination of macro (Na, K, Ca, Mg, P) and trace (Cd, Cu, Mn, Sr, Zn) elements in three biological certified reference materials using a V-groove, clog-free Babington-type nebulizer. Slurry concentrations up to 1% m/v (particles <20 {mu}m), prepared in 10% HNO{sub 3} (pH 1.2) containing 0.01% of Triton X-100, were used with calibration by the standard additions method. The method offers relatively good precision (R.S.D. ranged from 7 to 11%) with measured concentrations being in satisfactory agreement with certified values for NRCC TORT-1 (Lobster hepatopancreas), NRCC LUTS-1 (Lobster hepatopancreas) and IAEA-153 (Milk powder). The concentrations of Na, K, Ca, Mg, P and Cd, Cu, Mn, Sr, Zn were determined in the range 90-22 000 {mu}g/g and 1-420 {mu}g/g, respectively. The method could be useful as a routine procedure.

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

International Nuclear Information System (INIS)

Leon, G.C. de; Shiraishi, K.; Kawamura, H.; Igaraishi, Y.; Palattao, M.V.; Azanon, E.M.

1990-10-01

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

A comparison of portable XRF and ICP-OES analysis for lead on air filter samples from a lead ore concentrator mill and a lead-acid battery recycler.

Science.gov (United States)

Harper, Martin; Pacolay, Bruce; Hintz, Patrick; Andrew, Michael E

2006-03-01

Personal and area samples for airborne lead were taken at a lead mine concentrator mill, and at a lead-acid battery recycler. Lead is mined as its sulfidic ore, galena, which is often associated with zinc and silver. The ore typically is concentrated, and partially separated, on site by crushing and differential froth flotation of the ore minerals before being sent to a primary smelter. Besides lead, zinc and iron are also present in the airborne dusts, together with insignificant levels of copper and silver, and, in one area, manganese. The disposal of used lead-acid batteries presents environmental issues, and is also a waste of recoverable materials. Recycling operations allow for the recovery of lead, which can then be sold back to battery manufacturers to form a closed loop. At the recycling facility lead is the chief airborne metal, together with minor antimony and tin, but several other metals are generally present in much smaller quantities, including copper, chromium, manganese and cadmium. Samplers used in these studies included the closed-face 37 mm filter cassette (the current US standard method for lead sampling), the 37 mm GSP or "cone" sampler, the 25 mm Institute of Occupational Medicine (IOM) inhalable sampler, the 25 mm Button sampler, and the open-face 25 mm cassette. Mixed cellulose-ester filters were used in all samplers. The filters were analyzed after sampling for their content of the various metals, particularly lead, that could be analyzed by the specific portable X-ray fluorescence (XRF) analyzer under study, and then were extracted with acid and analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES). The 25 mm filters were analyzed using a single XRF reading, while three readings on different parts of the filter were taken from the 37 mm filters. For lead at the mine concentrate mill, all five samplers gave good correlations (r2 > 0.96) between the two analytical methods over the entire range of found lead mass

Tandem on-line continuous separations for atomic spectroscopic indirect analysis: iodide determination by ICP-AES

International Nuclear Information System (INIS)

Garcia, A.M.; Sanchez Uria, J.E.; Sanz-Medel, A.; Quintero Ortega, M.C.; Bautista, J.C.

1992-01-01

A sensitive and selective indirect determination of iodide by inductively coupled plasma emission spectrometry (ICP-AES) based on the principle of tandem on-line continuous separations as an alternative means of introducing samples into plasmas is proposed. Iodide is continuously extracted as an ion-pair into xylene by mixing the sample with Hg(II) and dipyridil solutions. The organic phase (containing the analyte in [Hg(Dipy) 2 ]I 2 form) is on-line continuously mixed with NaBH 4 (in DMF) and acetic acid solutions. Mercury vapour continuously generated from this organic phase is separated in a classical U-type gas-liquid separation device. The system has been optimized for the continuous extraction of KI, for the direct generation of cold mercury vapour from xylene and for the final ICP-AES determination of mercury. The optimised method has been applied to the determination of iodide (detection limit 20 ng/ml of iodide) in table salt and in synthetic samples. Very good agreement between found and certified results was observed. The usefulness and convenience of such alternative sample chemical pretreatment/presentation to the ICP is thus demonstrated for indirect determinations to be carried out by atomic spectroscopy methods. (authors)

A long-term validation of the modernised DC-ARC-OES solid-sample method.

Science.gov (United States)

Flórián, K; Hassler, J; Förster, O

2001-12-01

The validation procedure based on ISO 17025 standard has been used to study and illustrate both the longterm stability of the calibration process of the DC-ARC solid sample spectrometric method and the main validation criteria of the method. In the calculation of the validation characteristics depending on the linearity(calibration), also the fulfilment of predetermining criteria such as normality and homoscedasticity was checked. In order to decide whether there are any trends in the time-variation of the analytical signal or not, also the Neumann test of trend was applied and evaluated. Finally, a comparison with similar validation data of the ETV-ICP-OES method was carried out.

Electrothermal vaporisation ICP-mass spectrometry (ETV-ICP-MS) for the determination and speciation of trace elements in solid samples - A review of real-life applications from the author's lab

Energy Technology Data Exchange (ETDEWEB)

Vanhaecke, Frank; Resano, Martin; Moens, Luc [Laboratory of Analytical Chemistry, Ghent University, Institute for Nuclear Sciences, Proeftuinstraat 86, 9000 Ghent (Belgium)

2002-09-01

The use of electrothermal vaporisation (ETV) from a graphite furnace as a means of sample introduction in inductively coupled plasma mass spectrometry (ICP-MS) permits the direct analysis of solid samples. A multi-step furnace temperature programme is used to separate the vaporisation of the target element(s) and of the matrix components from one another. Sometimes, a chemical modifier is used to enable a higher thermal pre-treatment temperature, by avoiding premature analyte losses (stabilisation) or promoting the selective volatilisation of matrix components. In almost all instances, accurate results can be obtained via external calibration or single standard addition using an aqueous standard solution. Absolute limits of detection are typically 1 pg, which corresponds to 1 ng/g for a typical sample mass of 1 mg. Real-life applications carried out in the author's lab are used to illustrate the utility of this approach. These applications aim at trace element determination in industrial and environmental materials. The industrial materials analysed include different types of plastics - Carilon, polyethylene, poly(ethyleneterephtalate) and polyamide - and photo- and thermographic materials. As samples from environmental origin, plant material, animal tissue and sediments were investigated. Some applications aimed at a multi-element determination, while in other, the content of a single, but often challenging, element (e.g., Si or S) had to be measured. ETV-ICP-MS was also used in elemental speciation studies. Separation of Se-containing proteins was accomplished using polyacrylamide gel electrophoresis (PAGE). Subsequent quantification of the Se content in the protein spots was carried out using ETV-ICP-MS. As the volatilisation of methylmercury and inorganic mercury could be separated from one another with respect to time, no chromatographic or electrophoretic separation procedure was required, but ETV-ICP-MS as such sufficed for Hg speciation in fish tissue

Utilization of bromeliad Tillandsia Usneoides L. in biomonitoring of air pollution in the metropolitan region of Sao Paulo - SP, Brazil

International Nuclear Information System (INIS)

Albuquerque, Caroline R.; Figueiredo, Ana M.G.; Silva, Barbara C. da; Ticianelli, Regina B.; Figueira, Rubens C.L.; Ribeiro, Andreza P.

2013-01-01

In this study, it was determined the metals Cd, Cu, Fe, Mo, Ni, Pb and Sb in plant Tillandsia Usneoides L., an epiphyte species popularly known as old beard and able to absorb water and nutrients directly from air, aiming to estimate the contribution of human activities in atmospheric metal pollution in the metropolitan region of Sao Paulo. The samples were collected at five different points, located near the South West and stretches of highway Mario Covas (SP-21). The Neutron Activation Analysis (NAA) and Optical Emission Spectrometry with Inductively Coupled Plasma (ICP-OES) were the analytical techniques used in the quantification of metals of interest

Digestão de óleo lubrificante encapsulado em forno de microondas com radiação focalizada por adição de amostra ao reagente pré-aquecido

Directory of Open Access Journals (Sweden)

Flavia A. Bressani

2006-12-01

Full Text Available The applicability of the recently proposed procedure based on gradual sample addition to microwave-assisted pre-heated concentrated acid is limited by the sample viscosity. In this work, lubricating oil samples with high viscosity were encapsulated and manually added to the microwave-assisted pre-heated concentrated digestion mixture. The procedure was applied for determination of Al, Ca, Cr, Cu, Fe, Mg, Ni, P, Pb, Si, Sn, Sr, V, W, and Zn in lubricating oil by inductively coupled plasma optical emission spectrometry (ICP OES. Determined and certified values for Ca, Mg, P, and Zn in lubricating oil were in agreement at a 95% confidence level.

Surface modification-a novel way of attaching cocatalysts on CdS semiconductors for photocatalytic hydrogen evolution

KAUST Repository

Yu, Weili

2014-08-22

Noble metals as cocatalysts for hydrogen evolution are widely investigated for semiconductor photocatalytic water splitting. In this paper, we present a novel way to attach not only noble metals, but also transitional metals onto CdS nanocrystals as cocatalysts for hydrogen evolution. The hydrogen evolution performances for each metal were compared and result shows that Pd attached CdS gives the highest hydrogen evolution rate of 250 μmol/h. The amounts of metal ions attached on the surface were measured by inductively coupled plasma optical emission spectrometry (ICP-OES). This work confirms that surface modification is a promising way of attaching cocatalysts onto semiconductor photocatalysts.

Utilization of bromeliad Tillandsia Usneoides L. in biomonitoring of air pollution in the metropolitan region of Sao Paulo - SP, Brazil; Utilizacao da bromelia Tillandsia Usneoides L. no biomonitoramento da poluicao atmosferica na Regiao metropolitana de Sao Paulo - SP, Brasil

Energy Technology Data Exchange (ETDEWEB)

Albuquerque, Caroline R.; Figueiredo, Ana M.G.; Silva, Barbara C. da; Ticianelli, Regina B., E-mail: calbuuquerque@gmail.com, E-mail: anamaria@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Figueira, Rubens C.L., E-mail: aportellar@yahoo.com.br [Universidade de Sao Paulo (USP), Sao Paulo, SP (Brazil). Instituto Oceanografico; Nievola, Catarina C.; Alves, Edenise S.; Domingos, Marisa, E-mail: ccnievola@uol.com.br, E-mail: ealves@ibot.sp.gov.br, E-mail: mmingos@superig.com.br [Instituto de Botanica (IBt-SMA/SP), Sao Paulo, SP (Brazil); Ribeiro, Andreza P., E-mail: andrezp@uninove.br [Universidade Nove de Julho (UNINOVE), Sao Paulo, SP (Brazil)

2013-07-01

In this study, it was determined the metals Cd, Cu, Fe, Mo, Ni, Pb and Sb in plant Tillandsia Usneoides L., an epiphyte species popularly known as old beard and able to absorb water and nutrients directly from air, aiming to estimate the contribution of human activities in atmospheric metal pollution in the metropolitan region of Sao Paulo. The samples were collected at five different points, located near the South West and stretches of highway Mario Covas (SP-21). The Neutron Activation Analysis (NAA) and Optical Emission Spectrometry with Inductively Coupled Plasma (ICP-OES) were the analytical techniques used in the quantification of metals of interest.

Surface modification-a novel way of attaching cocatalysts on CdS semiconductors for photocatalytic hydrogen evolution

KAUST Repository

Yu, Weili; Isimjan, Tayirjan; Lin, Bin; Takanabe, Kazuhiro

2014-01-01

Noble metals as cocatalysts for hydrogen evolution are widely investigated for semiconductor photocatalytic water splitting. In this paper, we present a novel way to attach not only noble metals, but also transitional metals onto CdS nanocrystals as cocatalysts for hydrogen evolution. The hydrogen evolution performances for each metal were compared and result shows that Pd attached CdS gives the highest hydrogen evolution rate of 250 μmol/h. The amounts of metal ions attached on the surface were measured by inductively coupled plasma optical emission spectrometry (ICP-OES). This work confirms that surface modification is a promising way of attaching cocatalysts onto semiconductor photocatalysts.

The effect of dielectric top lids on materials processing in a low frequency inductively coupled plasma (LF-ICP) reactor

International Nuclear Information System (INIS)

Lim, J.W.M.; Chan, C.S.; Xu, L.; Xu, S.

2014-01-01

The advent of the plasma revolution began in the 1970's with the exploitation of plasma sources for anisotropic etching and processing of materials. In recent years, plasma processing has gained popularity, with research institutions adopting projects in the field and industries implementing dry processing in their production lines. The advantages of utilizing plasma sources would be uniform processing over a large exposed surface area, and the reduction of toxic emissions. This leads to reduced costs borne by manufacturers which could be passed down as consumer savings, and a reduction in negative environmental impacts. Yet, one constraint that plagues the industry would be the control of contaminants in a plasma reactor which becomes evident when reactions are conducted in a clean vacuum environment. In this work, amorphous silicon (a-Si) thin films were grown on glass substrates in a low frequency inductively coupled plasma (LF-ICP) reactor with a top lid made of quartz. Even though the chamber was kept at high vacuum (~10 −4 Pa), it was evident through secondary ion mass spectroscopy (SIMS) and Fourier-transform infra-red spectroscopy (FTIR) that oxygen contaminants were present. With the aid of optical emission spectroscopy (OES) the contaminant species were identified. The design of the LF-ICP reactor was then modified to incorporate an Alumina (Al 2 O 3 ) lid. Results indicate that there were reduced amounts of contaminants present in the reactor, and that an added benefit of increased power transfer to the plasma, improving deposition rate of thin films was realized. The results of this study is conclusive in showing that Al 2 O 3 is a good alternative as a top-lid of an LF-ICP reactor, and offers industries a solution in improving quality and rate of growth of thin films. (author)

Assessment of metal concentrations in sediment samples from Billings Reservoir, Rio Grande tributary, Sao Paulo, Brazil

International Nuclear Information System (INIS)

Bostelmann, Eleine

2006-01-01

The present study chemically characterized sediment samples from the Billings reservoir, Rio Grande tributary, in the Metropolitan region of Sao Paulo, by determining metal concentration and other elements of interest. The chosen chemical parameters for this characterization were Aluminum, Arsenic, Barium, Cadmium, Copper, Chromium, Iron, Lead, Manganese, Mercury, Nickel, Selenium and Zinco. These parameters are also used in the water quality index, with the exception of Selenium. The concentrations were determined through different analytical techniques such as atomic absorption spectrometry (FAAS, GFAAS and CVAAS), optical emission spectrometry (ICP OES) and neutron activation analysis. These analytical methodologies were assessed for precision, accuracy and detection and/or quantification limits for the sediment elements in question. Advantages and disadvantages of each technique for each element and its concentration were also discussed. From these assessments the most adequate technique was selected for the routine analysis of sediment samples for each element concentration determination. This assessment verified also that digestion in a closed microwave system with nitric acid is efficient for the evaluation of extracted metals of environmental interest. The analytical techniques chosen were equally efficient for metals determination. In the case of Cd and Pb, the FAAS technique was selected due to better results than ICP OES, as it does not present matrix interference. The concentration values obtained for metals As, Cd, Cu, Cr, Hg, Ni, Pb and Zn in the sediment samples were compared to Canadian Council of Minister of the Environment (CCME) TEL and PEL values. (author)

Assessment of metal concentrations in sediment samples from Billings reservoir, Rio Grande tributary, Sao Paulo, Brazil

International Nuclear Information System (INIS)

Bostelmann, Eleine

2006-01-01

The present study chemically characterized sediment samples from the Billings reservoir, Rio Grande tributary, in the Metropolitan region of Sao Paulo, by determining metal concentration and other elements of interest. The chosen chemical parameters for this characterization were Aluminum, Arsenic, Barium, Cadmium, Copper, Chromium, Iron, Lead, Manganese, Mercury, Nickel, Selenium and Zinc. These parameters are also used in the water quality index, with the exception of Selenium. The concentrations were determined through different analytical techniques such as atomic absorption spectrometry (FAAS, GFAAS and CVAAS), optical emission spectrometry (ICP OES) and neutron activation analysis. These analytical methodologies were assessed for precision, accuracy and detection and/or quantification limits for the sediment elements in question. Advantages and disadvantages of each technique for each element and its concentration were also discussed. From these assessment the most adequate technique was selected for the routine analysis of sediment samples for each element concentration determination. This assessment verified also that digestion in a closed microwave system with nitric acid is efficient for the evaluation of extracted metals of environmental interest. The analytical techniques chosen were equally efficient for metals determination. In the case of Cd and Pb, the FAAS technique was selected due to better results than ICP OES, as it does not present matrix interference. The concentration values obtained for metals As, Cd, Cu, Cr, Hg, Ni, Pb and Zn in the sediment samples were compared to Canadian Council of Minister of the Environment (CCME) TEL and PEL values. (author)

Assessment of metal concentrations in sediment samples from Billings Reservoir, Rio Grande tributary, Sao Paulo, Brazil; Avaliacao da concentracao de metais em amostras de sedimento do Reservatorio Billings, Braco Rio Grande, Sao Paulo, Brasil

Energy Technology Data Exchange (ETDEWEB)

Bostelmann, Eleine

2006-07-01

The present study chemically characterized sediment samples from the Billings reservoir, Rio Grande tributary, in the Metropolitan region of Sao Paulo, by determining metal concentration and other elements of interest. The chosen chemical parameters for this characterization were Aluminum, Arsenic, Barium, Cadmium, Copper, Chromium, Iron, Lead, Manganese, Mercury, Nickel, Selenium and Zinco. These parameters are also used in the water quality index, with the exception of Selenium. The concentrations were determined through different analytical techniques such as atomic absorption spectrometry (FAAS, GFAAS and CVAAS), optical emission spectrometry (ICP OES) and neutron activation analysis. These analytical methodologies were assessed for precision, accuracy and detection and/or quantification limits for the sediment elements in question. Advantages and disadvantages of each technique for each element and its concentration were also discussed. From these assessments the most adequate technique was selected for the routine analysis of sediment samples for each element concentration determination. This assessment verified also that digestion in a closed microwave system with nitric acid is efficient for the evaluation of extracted metals of environmental interest. The analytical techniques chosen were equally efficient for metals determination. In the case of Cd and Pb, the FAAS technique was selected due to better results than ICP OES, as it does not present matrix interference. The concentration values obtained for metals As, Cd, Cu, Cr, Hg, Ni, Pb and Zn in the sediment samples were compared to Canadian Council of Minister of the Environment (CCME) TEL and PEL values. (author)

Internal standardization in atomic-emission spectrometry using inductively coupled plasma

International Nuclear Information System (INIS)

Moore, G.L.

1985-01-01

The principle of internal standardization has been used in quantitative analytical emission spectroscopy since 1925 to minimize the errors arising from fluctuations in sample preparation, excitation-source conditions, and detection parameters. Although modern spectroscopic excitation sources are far more stable and electronic detection methods are more precise than before, the system for the introduction of the sample in spectrometric analysis using inductively coupled plasma (ICP) introduces significant errors, and internal standardization can still play a useful role in improving the overall precision of the analytical results. The criteria for the selection of the elements to be used as internal standards in arc and spark spectrographic analysis apply to a much lesser extent in ICP-spectrometric analysis. Internal standardization is recommended for use in routine ICP-simultaneous spectrometric analysis to improve its accuracy and precision and to provide a monitor for the reassurance of the analyst. However, the selection of an unsuitable reference element can result in misuse of the principle of internal standardization and, although internal standardization can be applied when a sequential monochromator is used, the main sources of error will not be minimized

The Determination of Composite Elements in Zircaloy-2 by X-Ray Fluorescence and Emission Spectrometry Method

International Nuclear Information System (INIS)

Dian Anggraini; Rosika Kriswarini; Yusuf N

2007-01-01

Analysis of composing elements in zircaloy-2 has been done by Emission Spectrometry method and X-Ray Fluorescence (XRF). The aim of the analysis is to verify conformity between composing elements in zircaloy-2 and the material certificate. Spectrometry Emission method has higher sensitivity in element determination of a material than that of XRF method, so can be estimated that emission spectrometry method has higher accuracy than that of XRF method. The result of qualitative analysis by Emission Spectrometry indicate that the composing elements in zircaloy-2 were Sn, Cr and Ni. However, the qualitative analysis result by XRF method indicated that the composing elements in zircaloy 2 were Sn, Cr, Ni and Fe. Fe element can not be analysed by Emission Spectrometry method because Emission Spectrometer did not equipped with Fe detector. The quantitative analysis result of the composing elements in the material with both methods showed that Sn, Cr and Ni concentration of zircaloy 2 existed in concentration ranges of the material certificate. Result of statistical test (F and t-test) of analysis result of both methods can be used for analyzing composing elements in zircaloy 2. Emission Spectrometry method was more sensitive and accurate for determining Cr and Ni element in zircaloy 2 than that of emission Spectrometry method but both methods had same accuracy. The precision of measurement of Sn, Cr and Ni element using XRF method was better than that of Emission spectrometry method. (author)

Determination of essential trace elements in wine by neutron activation analysis; Determinacao de elementos essenciais em vinhos por analise por ativacao com neutrons

Energy Technology Data Exchange (ETDEWEB)

Daniele, Anna Paula

2016-07-01

Several studies have been carried out for determining essential elements in foodstuffs, including wine, due to its important nutritional role in human body functions. It was shown that daily consumption of wine in moderation contributes significantly to the needs of essential elements in human body such as Ca, Co, Cr, Fe, K, Mg, Mn, Zn, V, among others, and has health benefits in the prevention of numerous diseases and longer life expectancy, related in particular to the intake of antioxidants such as polyphenolic compounds. Trace elements are good indicators of origin of wines and their concentrations can be used as criteria to ensure authenticity, quality and show that the tolerance limits established by law were respected throughout the production process. However, although Brazilian wine industry is among the 15 largest in the world, analytical studies for organic and inorganic compounds of wine content are still small when compared to other major producers. In this sense, this study aimed to evaluate some procedures of wine sample preparation to determine essential elements by Instrumental Neutron Activation Analysis (INAA) and compare the results with those determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP OES). Three sample preparation procedures were studied: freeze-drying, evaporation and dry ashing. The parameters studied were precision, accuracy and detection limit. ANOVA and Tukey-Kramer tests were applied to verify the statistical differences between the mean values obtained by the three wine preparation procedures for INAA with those means obtained by ICP OES. It was noticed that about 60% of results obtained by freeze-drying agreed with those obtained by ICP OES. (author)

Determination of essential trace elements in wine by neutron activation analysis

International Nuclear Information System (INIS)

Daniele, Anna Paula

2016-01-01

Several studies have been carried out for determining essential elements in foodstuffs, including wine, due to its important nutritional role in human body functions. It was shown that daily consumption of wine in moderation contributes significantly to the needs of essential elements in human body such as Ca, Co, Cr, Fe, K, Mg, Mn, Zn, V, among others, and has health benefits in the prevention of numerous diseases and longer life expectancy, related in particular to the intake of antioxidants such as polyphenolic compounds. Trace elements are good indicators of origin of wines and their concentrations can be used as criteria to ensure authenticity, quality and show that the tolerance limits established by law were respected throughout the production process. However, although Brazilian wine industry is among the 15 largest in the world, analytical studies for organic and inorganic compounds of wine content are still small when compared to other major producers. In this sense, this study aimed to evaluate some procedures of wine sample preparation to determine essential elements by Instrumental Neutron Activation Analysis (INAA) and compare the results with those determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP OES). Three sample preparation procedures were studied: freeze-drying, evaporation and dry ashing. The parameters studied were precision, accuracy and detection limit. ANOVA and Tukey-Kramer tests were applied to verify the statistical differences between the mean values obtained by the three wine preparation procedures for INAA with those means obtained by ICP OES. It was noticed that about 60% of results obtained by freeze-drying agreed with those obtained by ICP OES. (author)

Performance of laser ablation. Quadrupole-based ICP-MS coupling for the analysis of single micrometric uranium particles

International Nuclear Information System (INIS)

Fabien Pointurier; Amelie Hubert; Anne-Claire Pottin

2013-01-01

In this paper we describe the application of laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) coupling to particle analysis, i.e., the determination of the isotopic composition of micrometric uranium particles. The performances of this analysis technique are compared with those of the two reference particle analysis techniques: secondary ion mass spectrometry (SIMS) and fission track-thermo-ionization mass spectrometry (FT-TIMS), based on the measurement of the isotopic ratios of 235 U/ 238 U in particles present in an inter-comparison particulate sample. The agreement of the results obtained using LA-ICP-MS with target values and with the results obtained using FT-TIMS and SIMS was good. Accuracy was equivalent to that of the other two techniques (±3 % deviation). However, relative experimental uncertainties present with LA-ICP-MS (7 %) were higher than those present with FT-TIMS (4.5 %) and SIMS (3 %). Furthermore, measurement yield of LA-ICP-MS coupling was close to that obtained with the same quadrupole ICP-MS for the measurement of a liquid sample (∼10 -4 ), but lower than that obtained with FT-TIMS and SIMS, respectively, by a factor of 10 and 20, although the particles analyzed using LA-ICP-MS were most likely smaller (diameter ∼0.6 μm, containing 4-7 fg of 235 U). Nevertheless, thanks to the brevity of the signals obtained, the detection capacity for low isotopic concentrations by LA-ICP-MS coupling is equivalent to that of FT-TIMS, although it remains well below that of SIMS (x 15). However, with more sensitive double focusing ICP-MS, performances equivalent to those achieved using SIMS could be obtained. (author)

Determination of rare-earth elements content in granitic rocks by argon plasma emission spectrometry

International Nuclear Information System (INIS)

Merodio, J.C.; Martinez, J.M.

1990-01-01

A method has been developed that enables the rare-earth elements in granitic rocks to be measured sequentially, using an inductively coupled plasma (ICP) source spectrometer with medium spectral resolution (0,02nm). The rocks were dissolved in an open system with a mixture of nitric-hydrofluoric-perchloric acids. Any residues remaining at this stage were removed by filtration and digested using a mini-fusion method with lithium tetraborate. Prior to the excitation in the spectrometer the rare-earth group was separated from other constituents using cation-exchange chromatography. A detailed study of spectral interferences and the evaluation of the detection limits have been performed. Five geochemical reference sample (granitic rocks) were analyzed and the obtained results agree favourably with recommended values and with reported determinations, using high spectral resolution ICP spectrometry. (Author) [es

ICP magnetic sector multiple collector mass spectrometry and the precise measurement of isotopic compositions using nebulization of solutions and laser ablation of solids

International Nuclear Information System (INIS)

Halliday, A.N.; Lee, D-C.; Christensen, J.N.; Yi, W.; Hall, C.M.; Jones, C.E.; Teagle, D.A.H.; Freedman, P.A.

1996-01-01

Inductively-coupled plasma (ICP) sources offer considerable advantages over thermal sources because the high ionization efficiency facilitates measurements of relatively high sensitivity for elements such as Hf or Sn, which can be difficult to measure precisely with thermal ionization mass spectrometry (TIMS). The mass discrimination (bias) is larger than for TIMS, favours the heavier ions, and decreases in magnitude with increasing mass. However, in contrast to TIMS, this discrimination is largely independent of the chemical or physical properties of the element or the duration of the analysis. This has been demonstrated to high precision with a double focussing multiple collector magnetic sector mass spectrometer with an ICP source. The principle of this instrument is briefly described. The potential of the instrument for high precision isotopic measurements of a very broad range of elements, using solution aspiration or laser ablation, is indicated. 15 refs

GD-OES and XPS coupling: A new way for the chemical profiling of photovoltaic absorbers

Energy Technology Data Exchange (ETDEWEB)

Mercier, Dimitri, E-mail: dimitri.mercier@uvsq.fr [Institut Lavoisier de Versailles, 45 av. des Etats-Unis, 78035 Versailles Cedex (France); Bouttemy, Muriel; Vigneron, Jackie [Institut Lavoisier de Versailles, 45 av. des Etats-Unis, 78035 Versailles Cedex (France); Chapon, Patrick [HORIBA Jobin Yvon SAS, F-91165 Longjumeau (France); Etcheberry, Arnaud [Institut Lavoisier de Versailles, 45 av. des Etats-Unis, 78035 Versailles Cedex (France)

2015-08-30

Highlights: • The coupling between GD-OES and XPS analysis is a promising way for fine characterization of thin layers. • Crater surface modifications obtained after GD-OES sputtering depend to the plasma gas. • Inversion of the gas flow improves the surface of the crater. • The modified layer is totally eliminated a few seconds after restarting GD-OES sputtering. - Abstract: In this paper, we examine the complementarity of Glow Discharge Optical Emission Spectroscopy (GD-OES) and X Ray Photoelectron Spectroscopy (XPS) for the realization of fine chemical depth profiling of photovoltaic absorbers using Cu(In,Ga)Se{sub 2} (CIGS) materials. The possibility to use sequentially these two techniques is discussed in this paper. We have evaluated the chemical modifications of the crater after GD-OES analyses which depend on the manner of finishing the plasma etching sequence; and we propose different ways to limit or eliminate this effect. For the moment, an intermediate step (wet chemical etching or weak sputtering) is required to obtain a CIGS phase in the crater. Finally, we have demonstrated the possibility to restart the GD-OES analyses of the materials after XPS quantification or GD-OES breaking without modifying the profile shape.

Inductively Coupled Plasma: Fundamental Particle Investigations with Laser Ablation and Applications in Magnetic Sector Mass Spectrometry

International Nuclear Information System (INIS)

Nathan Joe Saetveit

2008-01-01

Particle size effects and elemental fractionation in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) are investigated with nanosecond and femtosecond laser ablation, differential mobility analysis, and magnetic sector ICP-MS. Laser pulse width was found to have a significant influence on the LA particle size distribution and the elemental composition of the aerosol and thus fractionation. Emission from individual particles from solution nebulization, glass, and a pressed powder pellet are observed with high speed digital photography. The presence of intact particles in an ICP is shown to be a likely source of fractionation. A technique for the online detection of stimulated elemental release from neural tissue using magnetic sector ICP-MS is described. Detection limits of 1 (micro)g L -1 or better were found for P, Mn, Fe, Cu, and Zn in a 60 (micro)L injection in a physiological saline matrix

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

International Nuclear Information System (INIS)

Naveen Kumar, P.; Sanjay Kumar; Vijay Kumar; Nandakishore, S.S.; Bangroo, P.N.

2013-01-01

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

Multielement Determination of Major-to Ultratrace Elements in a Cabbage, Spinach, and the Japanese Radish by ICP-AES After Acid Digestion

OpenAIRE

畑山, 友紀; 奴田原, 杏奈; 藤井, 和美; 西島, 基弘; ハタヤマ, ユキ; ヌタハラ, アンナ; フジイ, カズミ; ニシジマ, モトヒロ; Yuki, Hatayama; anna, Nutahara; Kazumi, Fujii; Motohiro, Nishijima

2011-01-01

A multi-element determination in a cabbage, spinach, and the Japanese radish was carried out by inductively coupled plasma atomic emission spectrometry (ICP). We investigated whether there was a difference in content according to the part of the vegetables. The dried vegetables (0.5g) were digested with nitric acid and with hydrogen peroxide acid in a resolution device As a result, about 9 elements were successfully determined. The values of the coefficient of variance for part interval by ea...

A laser ablation ICP-MS based method for multiplexed immunoblot analysis

DEFF Research Database (Denmark)

de Bang, Thomas Christian; Petersen, Jørgen; Pedas, Pai Rosager

2015-01-01

developed a multiplexed antibody-based assay and analysed selected PSII subunits in barley (Hordeum vulgare L.). A selection of antibodies were labelled with specific lanthanides and immunoreacted with thylakoids exposed to Mn deficiency after western blotting. Subsequently, western blot membranes were...... analysed by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), which allowed selective and relative quantitative analysis via the different lanthanides. The method was evaluated against established liquid chromatography electrospray ionization tandem mass spectrometry (LC...... by more than one technique. The developed method enables a higher number of proteins to be multiplexed in comparison to existing immunoassays. Furthermore, multiplexed protein analysis by LA-ICP-MS provides an analytical platform with high throughput appropriate for screening large collections of plants....

Determination of copper in liquid and solid insulation for large electrical equipment by ICP-OES. Application to copper contamination assessment in power transformers.

Science.gov (United States)

Bruzzoniti, Maria Concetta; De Carlo, Rosa Maria; Sarzanini, Corrado; Maina, Riccardo; Tumiatti, Vander

2012-09-15

Copper is one of the main constituents of the components in power transformers and its presence both in liquid (mineral oil) and in solid (Kraft paper) insulators can lead to enhanced dielectric losses and to the subsequent deterioration of their insulating properties. Recently the latter have been correlated to plant failures which in turn may have severe impact on the environment. This paper describes the direct analysis of copper in insulating mineral oil by ICP-OES and how it was first optimized compared to the official American Society for Testing and Materials (ASTM) D7151 method. Detection and quantification limits of 8.8 μg kg(-1) and 29.3 μg kg(-1) were obtained. Secondly, copper determination was improved by coupling a microwave assisted dissolution procedure of the mineral oil which avoided the problems, in the real samples, due to the presence of solid species of copper which cannot be nebulized following traditional methods described in literature. Sixteen mineral insulating oils sampled from transformers in service were analyzed before and after dissolution. In order to evaluate copper speciation, size fractionation was performed by filtration on PTFE filters (0.45, 1 and 5 μm). This test was performed on all the oil samples. Finally, because of the key role of the solid insulator in failed transformers, the Authors applied the developed method to study the copper deposition tendency onto the insulating Kraft paper tapes exerted by two unused oils (a corrosive and a non-corrosive one) under defined ageing conditions. Copyright © 2012 Elsevier B.V. All rights reserved.

Electronic structure and photocatalytic activity of wurtzite Cu–Ga–S nanocrystals and their Zn substitution

KAUST Repository

Kandiel, Tarek; Anjum, Dalaver H.; Sautet, Philippe; Le Bahers, Tangui; Takanabe, Kazuhiro

2015-01-01

by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), diffuse reflectance spectroscopy (DRS), photoluminescence (PL), and inductively coupled plasma atomic emission spectroscopy (ICP-OES). Electronic

In-situ determination of cross-over point for overcoming plasma-related matrix effects in inductively coupled plasma-atomic emission spectrometry

International Nuclear Information System (INIS)

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

2008-01-01

A novel method is described for overcoming plasma-related matrix effects in inductively coupled plasma-atomic emission spectrometry (ICP-AES). The method is based on measurement of the vertically resolved atomic emission of analyte within the plasma and therefore requires the addition of no reagents to the sample solution or to the plasma. Plasma-related matrix effects enhance analyte emission intensity low in the plasma but depress the same emission signal at higher positions. Such bipolar behavior is true for all emission lines and matrices that induce plasma-related interferences. The transition where the enhancement is balanced by the depression (the so-called cross-over point) results in a spatial region with no apparent matrix effects. Although it would be desirable always to perform determinations at this cross-over point, its location varies between analytes and from matrix to matrix, so it would have to be found separately for every analyte and for every sample. Here, a novel approach is developed for the in-situ determination of the location of this cross-over point. It was found that the location of the cross-over point is practically invariant for a particular analyte emission line when the concentration of the matrix was varied. As a result, it is possible to determine in-situ the location of the cross-over point for all analyte emission lines in a sample by means of a simple one-step sample dilution. When the original sample is diluted by a factor of 2 and the diluted sample is analyzed again, the extent of the matrix effect is identical (zero) between the original sample and the diluted sample at one and only one location - the cross-over point. This novel method was verified with several single-element matrices (0.05 M Na, Ca, Ba and La) and some mixed-element matrices (mixtures of Na-Ca, Ca-Ba, and a plant-sample digest). The inaccuracy in emission intensity due to the matrix effect could be as large as - 30% for conventional measurements in the

Investigation of the remaining major and trace elements in clean coal generated by organic solvent extraction

Energy Technology Data Exchange (ETDEWEB)

Jie Wang; Chunqi Li; Kinya Sakanishi; Tetsuya Nakazato; Hiroaki Tao; Toshimasa Takanohashi; Takayuki Takarada; Ikuo Saito [National Institute Advanced Industrial Science and Technology (AIST), Ibaraki (Japan). Energy Technology Research Institute

2005-09-01

A sub-bituminous Wyodak coal (WD coal) and a bituminous Illinois No. 6 coal (IL coal) were thermally extracted with 1-methylnaphthalene (1-MN) and N-methyl-2-pyrrolidone (NMP) to produce clean extract. A mild pretreatment with acetic acid was also carried out. Major and trace inorganic elements in the raw coals and resultant extracts were determined by means of inductively coupled plasma optical emission spectrometry (ICP-OES), flow injection inductively coupled plasma mass spectrometry (FI-ICP-MS), and cold vapor atomic absorption spectrometry (CV-AAS). It was found that the extraction with 1-MN resulted in 73-100% reductions in the concentration of Li, Be, V, Ga, As, Se, Sr, Cd, Ba, Hg, and Pb. The extraction with NMP yielded more extract than that with 1-MN, but it retained more organically associated major and trace metals in the extracts. In the extraction of WD coal with NMP, the acid pretreatment not only significantly enhanced the extraction yield but also significantly reduced the concentrations of alkaline earth elements such as Be, Ca, Mg, Sr, and Ba in the extract. In addition, the modes of occurrence of trace elements in the coals were discussed according to their extraction behaviors. 30 refs., 2 figs., 5 tabs.

Critical comparison of performances of inductively coupled plasma atomic emission spectrometry and neutron activation analysis for the determination of elements in human lungs

International Nuclear Information System (INIS)

Alimonti, A.; Coni, E.; Caroli, S.; Sabbioni, E.; Nicolaou, G.E.; Pietra, R.

1989-01-01

A study was carried out to assess the performance of inductively coupled plasma atomic emission spectrometry (ICP-AES) and neutron activation analysis (NAA) techniques for determining reference values for Al, Cd, Cr, Cu, Mg, Mn, V and Zn in human lungs of urban non-smoking subjects. Experimental data were subjected to the usual basic statistical tests to evaluate the respective merits of the two basically different analytical techniques. Both approaches, if used under carefully optimised experimental conditions, can yield reliable results affected only minimally by systematic and random errors. On the other hand, on a more routine basis, particular attention should be paid to elements such as Al, Cd and V which may pose some problems with both techniques. (author)

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

International Nuclear Information System (INIS)

Ho, Koon-Sing; Lui, Kwok-On; Lee, Kin-Ho; Chan, Wing-Tat

2013-01-01

empirical equation is formulated for the estimation of the position of complete vaporization of a particle in the ICP. The equation takes into account the particle properties (diameter, density, boiling point, and molecular weight of the constituents of the particle) and the ICP operating parameters (ICP forward power and central channel gas flow rate). The proportional constant and exponents of the variables in the equation were solved using literature values of ICP operating conditions for single-particle inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) measurements of 6 kinds of particles in 12 studies. The calculated position is a useful guide for the selection of sampling depth or observation height for ICP-MS and ICP-AES measurements of single particles as well as discrete particles in a flow, such as laser-ablated materials and airborne particulates. - Highlights: • Calibration curve constructed from ICPMS intensity and particle mass distributions • Degree of vaporization and analyte diffusion determine calibration curve linearity. • Single-particle ICPMS requires standard particle/solution droplet for calibration. • Empirical equation to estimate complete vaporization position of particle in ICP

Comparative study for toxic elements determination in air particulate reference material by INAA, CCT-ICP-MS, and ICP-MS

International Nuclear Information System (INIS)

Lim, J.M.; Lee, J.H.; Kim, K.H.; Moon, J.H.; Chung, Y.S.

2005-01-01

Although toxic elements are minor components in the atmospheric environment, they play a significant role as important marker for atmospheric science such as risk assessment, long-range transfer study, and source apportionment. Therefore, the techniques, which allow accurate and fast elemental analysis with a minimum pre-treatment, are very important. INAA has a main advantage of non-destruction of air particulate samples, while inductively Coupled plasma with mass spectrometry (ICP-MS) encounters the most significant difficulties in pre-treatment (digestion, fusion, and dilution) and polyatomic spectral interferences for interest toxic elements, Although INAA is still reference method, a number of factors (disadvantages of cost, complexity of the instruments, and scarcity of nuclear reactor) limit its applications. To date, the use of collision cell technology ICP-MS (CCT-ICP-MS) is recommended instead of typical ICP-MS for the analysis of the toxic elements; this is because CCT-ICP-MS technique prevents polyatomic spectral interferences despite of contamination and volatile effects. In this study, a number of toxic elements in reference material, NIST SRM 2783 (air particulate on filter media) were determined by INAA, CCT-ICP-MS, and ICP-MS. For both ICP methods, the filters were decomposed by microwave digestion with 5mL nitric acid. The analytical results by three methods were compared with certificated data; the INAA results showed the most accurate and precise data sets for all target elements among three methods. In detail, the deviation between analytical results and SRM's by INAA fell below 10% for all elements excluding As (14%), while those by CCT-ICP-MS were about 20%. For ICP-MS, the result does not agree with certificated data for several elements, because polyatomic spectral interference (due to 40 Ar 35 Cl, 40 Ar 23 Na, and 35 Cl 16 O) generate positive error of analytical result for As, Cu, and V. Based on our result, INAA is still one of the most

Nuclear techniques for the study of environmental pollution and control: experience and facilities at PINSTECH

International Nuclear Information System (INIS)

Rajput, M.U.; Butt, N.M.

2001-01-01

Environmental pollution is a worldwide problem. Developed countries have already gone in the clutches of pollution. Now the rapid industrialization and modernization process has also started in the developing countries. This is posing a serious threat to their own environment. One of the important factors in the pollution control measures is to investigate the levels of environmental pollution, from time to time, by effective and reliable methods. Nuclear techniques due to their high sensitivities play an important role in this regard. These techniques have the potential to determine the concentration of pollutants in trace level quantities (ppm and ppb) and for locating the possible pollution sources such as power plants, refineries, municipal waste, industries etc. Pakistan Institute of Nuclear Science and Technology (PINSTECH) has qualified and experienced scientists and has nearly all the major nuclear facilities that are needed for environmental research such as mass spectrometry, tracer techniques, neutron activation analysis (NAA), X-ray fluorescence spectrometry (XRFS), atomic absorption spectrometry (AAS), atomic emission spectrometry (AES), inductively coupled plasma-optical emission spectrometry (ICP-OES) etc. This paper discusses the importance of environmental pollution with a particular reference to the pollution aspects in Pakistan and the associated environmental research experience based on nuclear methods available at PINSTECH. 308 refs. (author)

Separation, preconcentration and estimation of rare earth and trace elements by inductively coupled plasma-atomic emission spectrometry (ICP-AES) in thorium matrices

International Nuclear Information System (INIS)

Chakraborty, Prithwish; Kumar Vijay; Durani, Smeer; Satyanarayana, K.

2007-01-01

A simple, sensitive and efficient method is developed for the separation of Rare earth elements (REEs) La-Lu, and Y and some trace elements Cd, Co, Cr, Cu, Ni,V, Zn from thorium matrix and their subsequent estimations by ICP-AES. In thorium-rich geological samples, the estimation of REE's by ICP-AES suffers from the spectral interferences due to the presence of excess of Th. In the proposed method, thorium is separated from the matrix by the solvent extraction. To optimize the separation, of REEs and trace elements from Th matrix, synthetic mixture solutions was prepared containing Th, REEs and trace elements maintaining different acidic conditions (1M, 2M, 4M, 6M, 8M and 10M HNO 3 and 2M, 4M, 6M and 8M HCl) and each solution was subjected to solvent extraction. The solvent extraction was carried out using a mixture of di-2-ethylhexyl phosphoric acid (in 30 % Toluene) and 1- pentanol in the ratio of 5:1. The aqueous phase containing the required elements was evaporated to dryness and an acidity of 5% HCl is maintained in final volume. Solutions were analysed by ICP-AES and the quantitative recovery of REEs and trace elements were obtained at 6M HNO 3 acidity. The developed method was applied to the certified standard reference material: IGS-36 and the values obtained were comparable with the certified values. The method was also applied to the real time monazite sample and the recovery was quantitative. Corrections have been applied for the REEs inter-elemental interferences in ICP-AES. (author)

Plutonium determination in urine by techniques of mass spectrometry

International Nuclear Information System (INIS)

Hernandez M, H.; Yllera de Ll, A.

2013-10-01

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 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 239 Pu). (author)

Atomic absorption spectrometry

International Nuclear Information System (INIS)

Haswell, S.J.

1991-01-01

Atomic absorption spectroscopy is now well established and widely used technique for the determination of trace and major elements in a wide range analyte types. There have been many advances in the atomic spectroscopy over the last decade and for this reason and to meet the demand, it was felt that there was a need for an updated book. Whilst interest in instrumental design has tended to dominate the minds of the spectrocopist, the analyst concerned with obtaining reliable and representative data, in diverse areas of application, has been diligently modifying and developing sample treatment and instrumental introduction techniques. Such methodology is de fundamental part of analysis and form the basis of the fourteen application chapters of this book. The text focuses in the main on AAS; however, the sample handling techniques described are in many cases equally applicable to ICP-OES and ICP-MS analysis. (author). refs.; figs.; tabs

Fe{sub 3}O{sub 4}/salicylic acid nanoparticles versatility in magnetic mediated vascular nanoblockage

Energy Technology Data Exchange (ETDEWEB)

Mîndrilă, I., E-mail: tutu0101@yahoo.com [University of Medicine and Pharmacy of Craiova, Faculty of Medicine (Romania); Buteică, S. A. [University of Medicine and Pharmacy of Craiova, Faculty of Pharmacy (Romania); Mihaiescu, D. E.; Badea, G.; Fudulu, A. [Politehnica University of Bucharest, Faculty of Applied Chemistry and Material Science (Romania); Mărgăritescu, D. N. [University of Medicine and Pharmacy of Craiova, Faculty of Medicine (Romania)

2016-01-15

An aqueous dispersion of Fe{sub 3}O{sub 4}/salicylic acid magnetic nanoparticles (SaMNPs) was synthesized by a modified Massart method, characterized by Inductively Coupled Plasma–Optic Emission Spectrometry (ICP-OES), High-Resolution Transmission Electron Microscopy (HRTEM) and Dynamic Light Scattering (DLS) methods, and tested on the chick chorioallantoic membrane (CAM) model to evaluate biocompatibility, biodistribution, intravascular time persistence, and ability to be magnetically target driven in order to block the blood supply into a tumor xenograft. ICP-OES, DLS, and HRTEM SaMNPs sample analyses showed a 0.356 mg/mL Fe concentration, a good stability in water (average Zeta potential of 39.3 mV), a hydrodynamic diameter around 52 nm and a core diameter in the 7–15 nm range for the Fe{sub 3}O{sub 4} nanoparticles. In vivo CAM assay showed that SaMNPs were biocompatible with the chick embryo, were fixed almost completely by the liver, had no embolic potential, and a threshold-dose-dependent intravascular magnetic targeting time. Study on the CAM tumor model showed that SaMNPs could be used for long-term magnetically mediated nanoblocking of the capillary networks and 70-µm smaller arterioles.

Regulatory quality control in the metal and semi metal environmental monitoring program at IPEN/CNEN-SP

International Nuclear Information System (INIS)

Faustino, Mainara G.; Silva, Doulgas Batista; Monteiro, Lucilena R.; Dantas, Elizabeth S.K.; Pires, Maria Aparecida F.; Cotrim, Marycel E.B.

2013-01-01

The CONAMA's Resolution 430 recently published in May 13 th of 2011, that completes and modifies the Resolution 357/2005, defined new quality standards to perform liquid effluent monitoring essays in order to allow the release in the public sewer system. This Resolution has established that the essay laboratories must be certified by Brazilian National Metrology, Normalization and Industrial Quality Institute - INMETRO and also count with an implemented quality control system. Thereby this publication affected directly IPEN's Environmental Monitoring Program of Stables Chemical Compound (PMA-Q), performed since 2007. In this program, 20 parameters related to the metallic and non-metallic chemical elements content are monitored by using sensitive analytical techniques such as graphite furnace atomic absorption spectrometry - GF-AAS or inductively coupled plasma spectrometry - ICP-OES. Therefore this paper presents improvements to determine the laboratory individual performance performed by GF-AAS and ICP-OES. To achieve the legislation compliance for these parameters, the following actions were implemented: the construction of control charts (internal quality control) and the participation of the laboratory in interlaboratory proficiency tests (external quality control). These actions are presented and discussed with the results of elements such as Arsenic and Lead that are analyzed through GF-AAS as well as Chromium, Cooper, Zinc, Iron and Nickel, that are analyzed through ICP-OES. These actions of quality control allowed the continuous monitoring of laboratory performance, the identification and resolution of analytic problems and interlaboratory differences, provide additional confidence to monitoring program. (author)

Surface modification of ceramic materials induced by irradiation of high power pulsed ICP

International Nuclear Information System (INIS)

Ishigaki, Takamasa; Okada, Nobuhiro; Ohashi, Naoki; Haneda, Hajime

2003-01-01

Newly developed pulse-modulated high-power inductively coupled plasma [ICP] is expected to offer the unique physico-chemical condition, such as the increased concentration of chemically reactive species, as well as the appropriate heat flux for materials processing. Two kinds of oxide materials, titanium and zinc oxide, were placed at the downstream of Ar-H 2 ICP and irradiated in the plasma of continuous [CN] and pulse-modulated [PM] modes. The CN-ICP irradiation at the position close to the plasma tail gave rise to the thermal reduction of oxides. In the PM-ICP irradiation, the degree of thermal reduction depended on the lower power level during pulse-off time, as well as the total electric power. Irradiation in PM-ICP led to the increased formation of oxygen vacancies in titanium dioxide. In the case of zinc oxide, the UV emission efficiency was improved by PM-ICP irradiation, while the green emission became predominant by CN-ICP irradiation at the appropriate position. Induced effects in the two oxides by PM-ICP would be related to the high concentration of hydrogen radicals in the plasma. (author)

Development of an on-line low gas pressure cell for laser ablation-ICP-mass spectrometry

International Nuclear Information System (INIS)

Hirata, Takafumi

2007-01-01

An on-line low gas pressure cell device has been developed for elemental analysis using laser ablation-ICP-mass spectrometry (LA-ICPMS). Ambient gas in the sample cell was evacuated by a constant-flow diaphragm pump, and the pressure of the sample cell was controlled by changing the flow rate of He-inlet gas. The degree of sample re-deposition around the ablation pit could be reduced when the pressure of the ambient gas was lower than 50 kPa. Produced sample aerosol was drawn and taken from the outlet of the diaphragm pump, and directly introduced into the ICP ion source. The flow rate of He gas controls not only the gas pressure in the sample cell, but also the transport efficiency of the sample particles from the cell to the ICP, and the gas flow rate must be optimized to maximize the signal intensity of the analytes. The flow rates of the He carrier and Ar makeup gas were tuned to maximize the signal intensity of the analytes, and in the case of 238 U from the NIST SRM610 glass material, the signal intensity could be maximized with gas flow rates of 0.4 L/min for He and 1.2 L/min for Ar. The resulting gas pressure in the cell was 30-35 kPa. Using the low gas pressure cell device, the stability in the signal intensities and the resulting precision in isotopic ratio measurements were evaluated. The signal intensity profile of 63 Cu obtained by laser ablation from a metallic sample (NIST SRM976) demonstrated that typical spikes in the transient signal, which can become a large source of analytical error, were no longer found. The resulting precision in the 65 Cu/ 63 Cu ratio measurements was 2-3% (n=10, 2SD), which was half on the level obtained by laser ablation under atmospheric pressure (6-10%). The newly developed low-pressure cell device provides easier optimization of the operational conditions, together with smaller degrees of sample re-deposition and better stability in the signal intensity, even from a metallic sample. (author)

Determination of mercury in hair: Comparison between gold amalgamation-atomic absorption spectrometry and mass spectrometry.

Science.gov (United States)

Domanico, Francesco; Forte, Giovanni; Majorani, Costanza; Senofonte, Oreste; Petrucci, Francesco; Pezzi, Vincenzo; Alimonti, Alessandro

2017-09-01

Mercury is a heavy metal that causes serious health problems in exposed subjects. The most toxic form, i.e., methylmercury (MeHg), is mostly excreted through human hair. Numerous analytical methods are available for total Hg analysis in human hair, including cold vapour atomic fluorescence spectrometry (CV-AFS), inductively coupled plasma mass spectrometry (ICP-MS) and thermal decomposition amalgamation atomic absorption spectrometry (TDA-AAS). The aim of the study was to compare the TDA-AAS with the ICP-MS in the Hg quantification in human hair. After the washing procedure to minimize the external contamination, from each hair sample two aliquots were taken; the first was used for direct analysis of Hg by TDA-AAS and the second was digested for Hg determination by the ICP-MS. Results indicated that the two data sets were fully comparable (median; TDA-AAS, 475ngg -1 ; ICP-MS, 437ngg -1 ) and were not statistically different (Mann-Whitney test; p=0.44). The two techniques presented results with a good coefficient of correlation (r=0.94) despite different operative ranges and method limits. Both techniques satisfied internal performance requirements and the parameters for method validation resulting sensitive, precise and reliable. Finally, the use of the TDA-AAS can be considered instead of the ICP-MS in hair analysis in order to reduce sample manipulation with minor risk of contamination, less time consuming due to the absence of the digestion step and cheaper analyses. Copyright © 2016 Elsevier GmbH. All rights reserved.

Method validation for determination of metals in Vitis labrusca L. grapevine leaf extracts by inductively coupled plasma mass spectrometry (ICP-MS

Directory of Open Access Journals (Sweden)

LIANE V.V. BOKOWSKI

Full Text Available ABSTRACT Vitis labrusca L. is the main species used for wine and juice production in Brazil. The grapevine leaves can be used both as functional foods and as cheapest sources for the extraction of phenolic compounds. Besides the antioxidant activity, grapevine leaves exhibited significant anti-inflammatory activity. Therefore, the aim of this study was to develop and validate an analytical methodology to determine the metals selenium (96Se, chromium (53Cr, nickel (62Ni, cadmium (111Cd and lead (206Pb in 30 samples of grapevine leaf extracts (Vitis labrusca, Bordo cultivar using inductively coupled plasma mass spectrometry (ICP-MS. To obtain the grapevine leaf extracts the samples were milled, weighed and digested in microwave oven with nitric acid. The method showed linearity, precision, accuracy and limits of quantification and detection acceptable for INMETRO protocol validation of analytical methods. Therefore, the method using ICP-MS was developed and validated to determine metals concentrations in grapevine leaves of Vitis labrusca L. and the proposed method could be applied in routine analytical laboratory.

Assessing the suitability of Norway spruce wood as an environmental archive for sulphur

International Nuclear Information System (INIS)

Barrelet, T.; Ulrich, A.; Rennenberg, H.; Zwicky, C.N.; Kraehenbuehl, U.

2008-01-01

The aim of this study was to assess the suitability of Norway spruces (Picea abies L. Karst.) as an environmental archive for sulphur. For this purpose spruce trees were sampled in two distinct regions of Switzerland: the Alps and the Swiss Plateau, which differ significantly with respect to S immission. Wood samples were measured using two methods: LASER Ablation high resolution inductively coupled plasma mass spectrometry (LA-HR-ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES) after acid digestion. Independently corroborated by previous measurements of sulphur in peat bogs, the rise and fall of sulphur dioxide pollution in Switzerland appears to be reflected in spruce wood sulphur content. While the wood sulphur content profile of trees sampled in the Alps is relatively flat, the profiles of trees located on the Swiss Plateau display a characteristic sulphur peak. This corresponds to air pollution data in the different regions and indicates that the trees reacted on the changing S supply and recorded a pollution signal in the wood. - Norway spruce is a suitable archive for sulphur when physiological aspects and limitations are taken into account

Determination of Cr, Cu, Fe, Ni, Pb and Zn by ICP-OES in mushroom samples from Sakarya, Turkey

Directory of Open Access Journals (Sweden)

Esra Altıntığ

2017-06-01

Full Text Available Russula cyanoxantha, Russula delica, Lactarius salmonicolor, Lactarius deliciosus, Pleurotus eryngii, Pleurotus ostreatus, Agaricus bisporus, Suillus luteus, Pleurotus spp and Boletus edulis were collected from Sakarya-Turkey respectively. Also canned food in the form of the Pleurotus eryngii, Pleurotus ostreatus, and Lactarius salmonicolor mushrooms were used for the examination. Trace metal concentrations found in these mushrooms were determined inductively using coupled plasma optic emission spectrometry microwave processes. The results were obtained for (Cr 0.3-26.65, (Cu 17.38-132.75, (Fe 26.3-225.40, (Ni 2.57-39.28, (Pb 11.52-185.20, and (Zn 22.86-126.84 mg/kg. The accuracy of the method was checked by the standard reference material; tea leaves (INCY-TL-1 and tomato leaves (1573a.

Total-reflection X-ray fluorescence: An alternative tool for the analysis of magnetic ferrofluids

Energy Technology Data Exchange (ETDEWEB)

Fernandez-Ruiz, R. [Servicio Interdepartamental de Investigacion (SIdI), Facultad de Ciencias, Universidad Autonoma de Madrid, Cantoblanco, E-28049, Madrid (Spain)], E-mail: ramon.fernandez@uam.es; Costo, R.; Morales, M.P.; Bomati-Miguel, O.; Veintemillas-Verdaguer, S. [Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco, E-28049, Madrid (Spain)

2008-12-15

This work presents the first application of the total-reflection X-ray fluorescence (TXRF) to the compositional study of magnetic ferrofluids. With the aims of validating the best analytical conditions and also, limitations of the TXRF in the compositional study of these materials, an alternative empirical method, based in the use of angle-dependence TXRF (AD-TXRF) measurements, is proposed. Three kinds of ferromagnetic nanoparticles, with different morphologies, have been studied. The techniques of inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectroscopy (ICP-OES) have been used to validate the TXRF results. In contrast with the plasma techniques, the developed TXRF procedure need not of previous chemical acid digestion. Additionally, two procedures of magnetic nanoparticles synthesis, co-precipitation and laser-pyrolysis, have been checked for the contaminants trace metals Zn, Mn and Cr. It has been found that the method of laser-pyrolysis produces nanoparticles of higher purity.

Selenium speciation analysis of Misgurnus anguillicaudatus selenoprotein by HPLC-ICP-MS and HPLC-ESI-MS/MS

Science.gov (United States)

Analytical methods for selenium (Se) speciation were developed using high performance liquid chromatography (HPLC) coupled to either inductively coupled plasma mass spectrometry (ICP-MS) or electrospray ionization tandem mass spectrometry (ESI-MS/MS). Separations of selenomethionine (Se-Met) and sel...

Critical evaluation of analytical performance of atomic absorption spectrometry and inductively coupled plasma mass spectrometry for mercury determination

International Nuclear Information System (INIS)

Krata, A.; Bulska, E.

2005-01-01

The analytical performance of cold vapor atomic absorption spectrometry (CV AAS), graphite furnace atomic absorption spectrometry (GF AAS) and inductively coupled plasma mass spectrometry (ICP-MS) for mercury determination have been investigated with the use of two reference materials SRM 2710 Montana I Soil and BCR-144R (sewage sludge from domestic origin). The digestion conditions and their influence on determination of mercury have been studied. Samples were decomposed by microwave digestion in closed vessels with the use of HCl alone or mixture of HCl+HNO 3 +HF. The digestion solutions were analyzed by CV AAS using NaBH 4 as a reducing agent, by GF AAS with Pd or mixture of Pd/Rh as modifiers and by ICP-MS with Rh as internal standard. In the case of CV AAS, results were not dependent on digestion conditions. In the case of GF AAS and ICP-MS, results depended significantly on digestion conditions; in both cases, the use of the mixture of acids as defined above suppressed the signal of mercury. Therefore, in those cases, the microwave digestion with HCl is recommended. Detection limits of 0.003, 0.01 and 0.2 μg g -1 were achieved by ICP-MS, CV AAS and GF AAS, respectively

Results on the role of metastable Ar atoms in a 9-MHz high-power atmospheric ICP by using emission/absorption spectrometry

International Nuclear Information System (INIS)

Gunter, W.; Zeeman, P.B.; Visser, K.

1984-01-01

An investigation into the role of overpopulations of metastable argon levels as agents for causing non-local thermal equilibrium (LTE) in an inductively coupled plasma source (ICP), was carried out. Four argon transitions in the near infrared region were monitored through absorption measurements at two different observation heights in a 9-MHz high-power ICP. The lower states of the four transitions consist of two metastable (11.55 and 11.72 eV) and two radiating (11.62 and 11.83 eV) levels. Comparison of measured metastable level to radiating level absorbance ratios with calculated population ratios gave an indication whether overpopulations of certain levels existed. Results indicate no overpopulation of metastable states with respect to radiating states, arguing against their role as non-LTE mechanism agents. This conclusion is, however, preliminary, since the calculation of absolute population densities from absorbance measurements must still be carried out

Determination of neptunium in soil by ICP-MS

International Nuclear Information System (INIS)

Ayranov, M.; Kraehenbuehl, U.

2005-01-01

A fast and simple method for the determination of 237 Np in soil is presented. The borate fusion decreases the sample pre-treatment time and a TEVA extraction chromatography separates neptunium from uranium and the interfering matrix components. A comparison of the sensitivities of alpha spectrometry and sector field ICP-MS for determination of 237 Np is presented. (orig.)

Study of mineral and essential trace elements in milk and dairy products by inductively coupled plasma atomic emission spectrometry and neutron activation analysis

International Nuclear Information System (INIS)

Kira, Carmen Silvia

2002-01-01

The importance of food composition related to nutritional and toxicological contents has been emphasized in recent years. Some chemical elements are needed for cell metabolism, while excess or deficiency may be responsible for disorders. Milk is considered the most important food during the first months of life, nutritional needs of children being satisfied by milk and dairy products. These foods provide the main trace elements for the good growth of different tissues as well as the functioning of several enzymatic systems. Important deficiencies in mineral during this period can interfere with children's development. Determination of mineral and trace elements by using spectroscopic techniques generally involves a pretreatment of sample. Sample preparation is the most critical part of the analysis because of the long preparation time and the possibilities for contamination and losses of the analyte associated with this step. Different procedures of sample preparation (dry ashing digestion, wet digestion using an open focused microwave and a hot plate) were evaluated for determining Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P and Zn in milk and dairy products by the ICP OES technique. In this work the concentrations obtained for the elements determined by the ICP OES technique after using the different treatments of sample were compared to the results obtained by the INAA technique, that does not require dissolution of sample. The partial digestion with diluted hydrochloric acid was found to be suitable for determining Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P and Zn in milk samples and dairy products. (author)

Quantification of elemental mapping of heterogeneous geological sample by laser ablation inductively coupled plasma mass spectrometry

Czech Academy of Sciences Publication Activity Database

Vaculovič, T.; Breiter, Karel; Korbelová, Zuzana; Venclová, Natalie; Tomková, Kateřina; Jonášová, Šárka; Kanický, V.

2017-01-01

Roč. 133, JUL 2017 (2017), s. 200-207 ISSN 0026-265X R&D Projects: GA ČR GA14-13600S Institutional support: RVO:67985831 ; RVO:67985912 Keywords : LA-ICP-MS * induced breakdown spectroscopy * atomic emission spectrometry * in-situ analysis * trace-metals Subject RIV: CB - Analytical Chemistry, Separation; AC - Archeology, Anthropology, Ethnology (ARU-G) OBOR OECD: Analytical chemistry; Archaeology (ARU-G) Impact factor: 3.034, year: 2016

Monitoring of Cr, Cu, Pb, V and Zn in polluted soils by laser induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Dell'Aglio, Marcella; Gaudiuso, Rosalba; Senesi, Giorgio S; De Giacomo, Alessandro; Zaccone, Claudio; Miano, Teodoro M; De Pascale, Olga

2011-05-01

Laser Induced Breakdown Spectroscopy (LIBS) is a fast and multi-elemental analytical technique particularly suitable for the qualitative and quantitative analysis of heavy metals in solid samples, including environmental ones. Although LIBS is often recognised in the literature as a well-established analytical technique, results about quantitative analysis of elements in chemically complex matrices such as soils are quite contrasting. In this work, soil samples of various origins have been analyzed by LIBS and data compared to those obtained by Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). The emission intensities of one selected line for each of the five analytes (i.e., Cr, Cu, Pb, V, and Zn) were normalized to the background signal, and plotted as a function of the concentration values previously determined by ICP-OES. Data showed a good linearity for all calibration lines drawn, and the correlation between ICP-OES and LIBS was confirmed by the satisfactory agreement obtained between the corresponding values. Consequently, LIBS method can be used at least for metal monitoring in soils. In this respect, a simple method for the estimation of the soil pollution degree by heavy metals, based on the determination of an anthropogenic index, was proposed and determined for Cr and Zn.

Transition metal analysis. A comparison between ICP-AES and deuteron activation

International Nuclear Information System (INIS)

Pillay, A.E.; Williams, J.R.; Hassan, S.M.; Al-Hamdi, A.; El Mardi, M.O.

2002-01-01

The analytical capabilities of ICP-AES (ICP) and deuteron activation (associated with prompt gamma-rays and delayed X-rays) for the determination of certain transition metals, were investigated. The sensitivities of the three methods are given, and the general applicability of each technique is evaluated. In the case of ICP, numerical data were obtained from aqueous solutions containing digested plant material. These experimental results were assessed against minimum detectable limits attained in relevant solid matrices that were subjected to prompt gamma-ray and delayed X-ray spectrometry using 5 MeV 2 H + ions. The analytically useful lines originated mainly from (d,p) and (d,n) reactions. The potential of the three techniques for routine analysis is discussed and detailed methodologies are presented. (author)

On the application of ICP-MS techniques for measuring uranium and plutonium: a Nordic inter-laboratory comparison exercise

DEFF Research Database (Denmark)

Qiao, Jixin; Lagerkvist, Petra; Rodushkin, Ilia

2018-01-01

Inductively coupled plasma mass spectrometry (ICP-MS) techniques are widely used for determination of long-lived radionuclides and their isotopic ratios in the nuclear fields. Uranium (U) and Pu (Pu) isotopes have been determined by many researchers with ICP-MS due to its relatively high sensitiv...

A new major adze quarry from Nanakuli, O'ahu: implications for interaction studies in Hawai'i

International Nuclear Information System (INIS)

Weisler, M.I.; Collins, S.L.; Feng, Y.; Zhao, J.; Shipton, C.; Wei, S.

2013-01-01

A major new basalt adze quarry at Nanakuli Valley, Hawaiian Islands is described which now ranks as one of the two largest on O'ahu and aside from the Mauna Kea adze quarry complex on Hawai'i island and the Haleakala source on Maui, is one of the major quarries in the archipelago. We defined the approximate limits of the quarry complex, located the in situ geological source of the fine-grained basalt used for adze manufacture, report the petrographic and geochemical variability of the source rock, and describe the adze reduction strategies from analysis of adze blanks and preforms, as well as hammerstones and debitage. The geochemical variation of the nine source rocks and artefacts were defined by a comprehensive array of 10 fully quantitative major element concentrations, 43 trace element abundances, and high-precision Sr-Nd-Pb isotopic ratios obtained using the state-of-the-art Thermal Ionization Mass Spectrometry (TIMS, for Sr isotopes), Multi-Collector Inductively Coupled Plasma Mass Spectrometry (MC-ICP-MS, for Nd-Pb isotopes), quadrupole ICP-MS (for trace elements) and Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES, for major elements), respectively. A piece of branch coral was recovered from the surface of a rockshelter that provided a U-series date of possible quarry use in the mid-13th century. It is advocated that a comprehensive range of major and trace element concentrations and Sr-Nd-Pb isotopic ratios are required for geochemically characterising adze quarries to facilitate the long-term viability of sourcing studies. (author)

Exploration of robust operating conditions in inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Tromp, John W.; Pomares, Mario; Alvarez-Prieto, Manuel; Cole, Amanda; Ying Hai; Salin, Eric D.

2003-01-01

'Robust' conditions, as defined by Mermet and co-workers for inductively coupled plasma (ICP)-atomic emission spectrometry, minimize matrix effects on analyte signals, and are obtained by increasing power and reducing nebulizer gas flow. In ICP-mass spectrometry (MS), it is known that reduced nebulizer gas flow usually leads to more robust conditions such that matrix effects are reduced. In this work, robust conditions for ICP-MS have been determined by optimizing for accuracy in the determination of analytes in a multi-element solution with various interferents (Al, Ba, Cs, K, Na), by varying power, nebulizer gas flow, sample introduction rate and ion lens voltage. The goal of the work was to determine which operating parameters were the most important in reducing matrix effects, and whether different interferents yielded the same robust conditions. Reduction in nebulizer gas flow and in sample input rate led to a significantly decreased interference, while an increase in power seemed to have a lesser effect. Once the other parameters had been adjusted to their robust values, there was no additional improvement in accuracy attainable by adjusting the ion lens voltage. The robust conditions were universal, since, for all the interferents and analytes studied, the optimum was found at the same operating conditions. One drawback to the use of robust conditions was the slightly reduced sensitivity; however, in the context of 'intelligent' instruments, the concept of 'robust conditions' is useful in many cases

Microwave-assisted versus conventional decomposition procedures applied to a ceramic potsherd standard reference material by inductively coupled plasma atomic emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Papadopoulou, D.N.; Zachariadis, G.A.; Anthemidis, A.N.; Tsirliganis, N.C.; Stratis, J.A

2004-03-03

Inductively coupled plasma atomic emission spectrometry (ICP-AES) is a powerful, sensitive analytical technique with numerous applications in chemical characterization including that of ancient pottery, mainly due to its multi-element character, and the relatively short time required for the analysis. A critical step in characterization studies of ancient pottery is the selection of a suitable decomposition procedure for the ceramic matrix. The current work presents the results of a comparative study of six decomposition procedures applied on a standard ceramic potsherd reference material, SARM 69. The investigated decomposition procedures included three microwave-assisted decomposition procedures, one wet decomposition (WD) procedure by conventional heating, one combined microwave-assisted and conventional heating WD procedure, and one fusion procedure. Chemical analysis was carried out by ICP-AES. Five major (Si, Al, Fe, Ca, Mg), three minor (Mn, Ba, Ti) and two trace (Cu, Co) elements were determined and compared with their certified values. Quantitation was performed at two different spectral lines for each element and multi-element matrix-matched calibration standards were used. The recovery values for the six decomposition procedures ranged between 75 and 110% with a few notable exceptions. Data were processed statistically in order to evaluate the investigated decomposition procedures in terms of recovery, accuracy and precision, and eventually select the most appropriate one for ancient pottery analysis.

LA-ICP-MS Results: 3 Siple Dome A Glacial Age Archives, Version 1

Data.gov (United States)

National Aeronautics and Space Administration — This data set contains the results of Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) performed on an archive of the Siple Dome A ice core...

Chemical analysis of steel by optical emission spectrometry

International Nuclear Information System (INIS)

Hayakawa, M.O.; Kajita, T.; Jeszensky, G.

1981-01-01

The development of the chemical analysis for special steels by optical emission spectrometry direct reading method with computer, at the Siderurgica N.S. Aparecida S.A. is presented. Results are presented for the low alloy steels and high speed steel. Also, the contribution of this method to the special steel preparation is commented. (Author) [pt

Sweet chemistry: a green way for obtaining selenium nanoparticles active against cancer cells

International Nuclear Information System (INIS)

Vieira, Adriana P.; Stein, Erika M.; Ferreira, Ana Maria D.C.; Colepicolo, Pio; Andreguetti, Daniel X.; Cebrián-Torrejón, Gerardo; Doménech-Carbó, Antonio

2017-01-01

We present an environment friendly synthesis of selenium nanoparticles and the study of their cytotoxic activity against uterine sarcoma cancer and fibroblasts cells. Amorphous selenium (a-SeNPs) and trigonal selenium (t-SeNPs) were synthesized using D-fructose as the reducing agent and characterized by high-resolution transmission electron microscopy (HRTEM), energy dispersive X-ray spectroscopy (EDX), powder X-ray diffraction analysis (XRD), inductively coupled plasma optical emission spectrometry (ICP OES), dynamic light scattering (DLS) to obtain zeta potential values and cyclic voltammetry (CV). Particularly, a-SeNPs presented high toxicity toward the resistant cancer cell line MES-SA/Dx5 and its parental MES-SA line. However, they are not toxic against P4 fibroblast cells in comparative studies. (author)

Investigation Of The Effects Of Heavy Metal Pollution In Black Sea Seaside Caused From Vehicles By Using Verbascum Sinuatum L. (Scrophulariaceae

Directory of Open Access Journals (Sweden)

Neslihan Duru

2011-12-01

Full Text Available In this study, the heavy metal pollution caused by vehicle traffic was investigated in the leaves of Verbascum sinuatum L.(Scrophulariaceae collected from the Blacksea coast ranging between Samsun, Ordu, Giresun, Trabzon, Rize and Hopa. Sample collection procedure was made in 23 stations in the related route. Heavy metal concentrations in the leaf samples of each station were determined with Perkin Emler Optic Emission Spectrometry (ICP-OES. Heavy metal concentration in samples was showed an order as Lead (Pb ; Zinc (Zn ; Chromium (Cr ; Nickel (Ni ; Copper (Cu ; Cadmium (Cd. The results of this study showed that the heavy metal accumulation in samples increased with an increase in traffic and V. sinuatum used as a biological indicator of this accumulation.

Sweet chemistry: a green way for obtaining selenium nanoparticles active against cancer cells

Energy Technology Data Exchange (ETDEWEB)

Vieira, Adriana P.; Stein, Erika M.; Ferreira, Ana Maria D.C.; Colepicolo, Pio, E-mail: apiresvieira@gmail.com [Universidade de São Paulo (USP), São Paulo-SP (Brazil); Andreguetti, Daniel X.; Cebrián-Torrejón, Gerardo; Doménech-Carbó, Antonio [Departament de Química Analítica, Facultat de Química, Universitat de València, Valencia (Spain)

2017-07-01

We present an environment friendly synthesis of selenium nanoparticles and the study of their cytotoxic activity against uterine sarcoma cancer and fibroblasts cells. Amorphous selenium (a-SeNPs) and trigonal selenium (t-SeNPs) were synthesized using D-fructose as the reducing agent and characterized by high-resolution transmission electron microscopy (HRTEM), energy dispersive X-ray spectroscopy (EDX), powder X-ray diffraction analysis (XRD), inductively coupled plasma optical emission spectrometry (ICP OES), dynamic light scattering (DLS) to obtain zeta potential values and cyclic voltammetry (CV). Particularly, a-SeNPs presented high toxicity toward the resistant cancer cell line MES-SA/Dx5 and its parental MES-SA line. However, they are not toxic against P4 fibroblast cells in comparative studies. (author)

Determination of the total drug-related chlorine and bromine contents in human blood plasma using high performance liquid chromatography-tandem ICP-mass spectrometry (HPLC-ICP-MS/MS).

Science.gov (United States)

Klencsár, Balázs; Bolea-Fernandez, Eduardo; Flórez, María R; Balcaen, Lieve; Cuyckens, Filip; Lynen, Frederic; Vanhaecke, Frank

2016-05-30

A fast, accurate and precise method for the separation and determination of the total contents of drug-related Cl and Br in human blood plasma, based on high performance liquid chromatography - inductively coupled plasma - tandem mass spectrometry (HPLC-ICP-MS/MS), has been developed. The novel approach was proved to be a suitable alternative to the presently used standard methodology (i.e. based on a radiolabelled version of the drug molecule and radiodetection), while eliminating the disadvantages of the latter. Interference-free determination of (35)Cl has been accomplished via ICP-MS/MS using H2 as reaction gas and monitoring the (35)ClH2(+) reaction product at mass-to-charge ratio of 37. Br could be measured "on mass" at a mass-to-charge of 79. HPLC was relied on for the separation of the drug-related entities from the substantial amount of inorganic Cl. The method developed was found to be sufficiently precise (repeatability 0.990) from the limit of quantification (0.05 and 0.01 mg/L for Cl and Br in blood plasma, respectively) to at least 5 and 1mg/L for Cl and Br, respectively. Quantification via either external or internal standard calibration provides reliable results for both elements. As a proof-of-concept, human blood plasma samples from a clinical study involving a newly developed Cl- and Br-containing active pharmaceutical ingredient were analysed and the total drug exposure was successfully described. Cross-validation was achieved by comparing the results obtained on Cl- and on Br-basis. Copyright © 2016 Elsevier B.V. All rights reserved.

CHAPTER 7. BERYLLIUM ANALYSIS BY NON-PLASMA BASED METHODS

Energy Technology Data Exchange (ETDEWEB)

Ekechukwu, A

2009-04-20

The most common method of analysis for beryllium is inductively coupled plasma atomic emission spectrometry (ICP-AES). This method, along with inductively coupled plasma mass spectrometry (ICP-MS), is discussed in Chapter 6. However, other methods exist and have been used for different applications. These methods include spectroscopic, chromatographic, colorimetric, and electrochemical. This chapter provides an overview of beryllium analysis methods other than plasma spectrometry (inductively coupled plasma atomic emission spectrometry or mass spectrometry). The basic methods, detection limits and interferences are described. Specific applications from the literature are also presented.

Quantitative analysis of phosphosilicate glass films on silicon wafers for calibration of x-ray fluorescence spectrometry standards

International Nuclear Information System (INIS)

Weissman, S.H.

1983-01-01

The phosphorus and silicon contents of phosphosilicate glass films deposited by chemical vapor deposition (CVD) on silicon wafers were determined. These films were prepared for use as x-ray fluorescence (XRF) spectrometry standards. The thin films were removed from the wafer by etching with dilute hydrofluoric acid, and the P and Si concentrations in solution were determined by inductively coupled plasma atomic emission spectroscopy (ICP). The calculated phosphorus concentration ranged from 2.2 to 12 wt %, with an uncertainty of 2.73 to 10.1 relative percent. Variation between the calculated weight loss (summation of P 2 O 5 and SiO 2 amounts as determined by ICP) and the measured weight loss (determined gravimetrically) averaged 4.9%. Results from the ICP method, Fourier transform-infrared spectroscopy (FT-IR), dispersive infrared spectroscopy, electron microprobe, and x-ray fluorescence spectroscopy for the same samples are compared

Application of factorial designs and Doehlert matrix in optimization of experimental variables associated with the preconcentration and determination of vanadium and copper in seawater by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Ferreira, Sergio L.C.; Queiroz, Adriana S.; Fernandes, Marcelo S.; Santos, Hilda C. dos

2002-01-01

In the present paper a procedure for preconcentration and determination of vanadium and copper in seawater using inductively coupled plasma optical emission spectrometry (ICP OES) is proposed, which is based on solid-phase extraction of vanadium (IV), vanadium (V) and copper (II) ions as 1-(2-pyridylazo)-2-naphthol (PAN) complexes by active carbon. The optimization process was carried out using two-level full factorials and Doehlert matrix designs. Four variables (PAN mass, pH, active carbon mass and shaking time) were regarded as factors in the optimization. Results of the two-level full factorial design 2 4 with 16 runs for vanadium extraction, based on the variance analysis (ANOVA), demonstrated that the factors pH and active carbon mass, besides the interaction (pHxactive carbon mass), are statistically significant. For copper, the ANOVA revealed that the factors PAN mass, pH and active carbon mass and the interactions (PAN massxpH) and (pHxactive carbon mass) are statistically significant. Doehlert designs were applied in order to determine the optimum conditions for extraction. The procedure proposed allowed the determination of vanadium and copper with detection limits (3σ/S) of 73 and 94 ng l -1 , respectively. The precision, calculated as relative standard deviation (R.S.D.), was 1.22 and 1.37% for 12.50 μg l -1 of vanadium and copper, respectively. The preconcentration factor was 80. The recovery achieved for determination of vanadium and copper in the presence of several cations demonstrated that this procedure improved the selectivity required for seawater analysis. The procedure was applied to the determination of vanadium and copper in seawater samples collected in Salvador City, Brazil. Results showed good agreement with other data reported in the literature

Application of isotope-dilution laser ablation ICP-MS for direct determination of Pu concentrations in soils at pg g(-1) levels.

Science.gov (United States)

Boulyga, Sergei F; Tibi, Markus; Heumann, Klaus G

2004-01-01

The methods available for determination of environmental contamination by plutonium at ultra-trace levels require labor-consuming sample preparation including matrix removal and plutonium extraction in both nuclear spectroscopy and mass spectrometry. In this work, laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was applied for direct analysis of Pu in soil and sediment samples. Application of a LINA-Spark-Atomizer system (a modified laser ablation system providing high ablation rates) coupled with a sector-field ICP-MS resulted in detection limits as low as 3x10(-13) g g(-1) for Pu isotopes in soil samples containing uranium at a concentration of a few microg g(-1). The isotope dilution (ID) technique was used for quantification, which compensated for matrix effects in LA-ICP-MS. Interferences by UH+ and PbO2+ ions and by the peak tail of 238U+ ions were reduced or separated by use of dry plasma conditions and a mass resolution of 4000, respectively. No other effects affecting measurement accuracy, except sample inhomogeneity, were revealed. Comparison of results obtained for three contaminated soil samples by use of alpha-spectrometry, ICP-MS with sample decomposition, and LA-ICP-IDMS showed, in general, satisfactory agreement of the different methods. The specific activity of (239+240)Pu (9.8 +/- 3.0 mBq g(-1)) calculated from LA-ICP-IDMS analysis of SRM NIST 4357 coincided well with the certified value of 10.4 +/- 0.2 mBq g(-1). However, the precision of LA-ICP-MS for determination of plutonium in inhomogeneous samples, i.e. if "hot" particles are present, is limited. As far as we are aware this paper reports the lowest detection limits and element concentrations yet measured in direct LA-ICP-MS analysis of environmental samples.

Application of isotope-dilution laser ablation ICP-MS for direct determination of Pu concentrations in soils at pg g-1 levels

International Nuclear Information System (INIS)

Boulyga, Sergei F.; Tibi, Markus; Heumann, Klaus G.

2004-01-01

The methods available for determination of environmental contamination by plutonium at ultra-trace levels require labor-consuming sample preparation including matrix removal and plutonium extraction in both nuclear spectroscopy and mass spectrometry. In this work, laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was applied for direct analysis of Pu in soil and sediment samples. Application of a LINA-Spark-Atomizer system (a modified laser ablation system providing high ablation rates) coupled with a sector-field ICP-MS resulted in detection limits as low as 3 x 10 -13 g g -1 for Pu isotopes in soil samples containing uranium at a concentration of a few μg g -1 . The isotope dilution (ID) technique was used for quantification, which compensated for matrix effects in LA-ICP-MS. Interferences by UH + and PbO 2 + ions and by the peak tail of 238 U + ions were reduced or separated by use of dry plasma conditions and a mass resolution of 4000, respectively. No other effects affecting measurement accuracy, except sample inhomogeneity, were revealed. Comparison of results obtained for three contaminated soil samples by use of α-spectrometry, ICP-MS with sample decomposition, and LA-ICP-IDMS showed, in general, satisfactory agreement of the different methods. The specific activity of 239+240 Pu (9.8±3.0 mBq g -1 ) calculated from LA-ICP-IDMS analysis of SRM NIST 4357 coincided well with the certified value of 10.4±0.2 mBq g -1 . However, the precision of LA-ICP-MS for determination of plutonium in inhomogeneous samples, i.e. if ''hot'' particles are present, is limited. As far as we are aware this paper reports the lowest detection limits and element concentrations yet measured in direct LA-ICP-MS analysis of environmental samples. (orig.)

Analysis of plutonium isotopes in marine samples by radiometric, ICP-MS and AMS techniques

International Nuclear Information System (INIS)

Lee, S.H.; Gastaud, J.; La Rosa, J.J.; Liong Wee Kwong, L.; Povinec, P.P.; Wyse, E.

2001-01-01

IAEA reference materials (radionuclides in the marine environment) collected in areas affected by nuclear reprocessing plants and nuclear weapons tests have been analysed by semiconductor alpha-spectrometry (SAS), liquid scintillation spectrometry (LSS) and mass spectrometric techniques (high resolution ICP-MS and AMS) with the aim of developing analytical procedures and to study the geochemical behavior of plutonium in the marine environment. The Pu results obtained by SAS, ICP-MS and AMS were in reasonably good agreement (R 2 = 0.99). The mean atom ratios of 240 Pu/ 239 Pu in IAEA reference materials, IAEA-134, 135 and 381 were (0.212±0.010), (0.211±0.004) and (0.242±0.004), respectively. IAEA-384 (Fangataufa Lagoon Sediment) gave a 240 Pu/ 239 Pu mean atom ratio of 0.051±0.001. The results of 241 Pu obtained buy ICP-MS and LSS also show reasonable agreement (R 2 = 0.91). Pu isotopic signatures were useful in tracing Pu origin and in interpreting biogeochemical processes involving Pu in the marine environment. (author)

Determination of iron in highly-saline matrices by FIA-ICP-MS

DEFF Research Database (Denmark)

Andersen, Jens Enevold Thaulov

Analysis of iron by inductively-coupled-plasma mass-spectrometry (ICP-MS) may be significantly improved by applying a protocol of flow-injection analysis. The iron species of the sample was preconcentrated by an ammonia buffer at pH = 9.2 on a filterless nylon-knotted reactor, and the adsorbed...... species were subsequently eluted by hydrochloric acid and analysed by ICP-MS. During the FIA step of preconcentration, a high degree of salinity did not influence the adsorption mechanism of iron, which may be related to formation of iron-hydroxide complexes at the sites of amide moieties of the nylon...

Formation and emission of PM10 in combustion of biofuels. Final report

International Nuclear Information System (INIS)

Johansson, Linda; Tullin, Claes; Leckner, Bo

2004-02-01

.g. soot). Submicron particles (particles less than 1 μm) dominated the emission, both with respect to mass and number. Analyses with EDX (Electron Dispersive X-ray), ICP-MS (Inductively Coupled Plasma Mass-Spectrometry), and IC (Ion-Chromatography) showed that the main components in the submicron particles were potassium, sulphur, chlorine, and oxygen. TOF-SIMS (Time-of-flight Secondary Ion Mass Spectrometry) analysis showed that potassium-sulphate followed by potassium chloride were the most dominant substances among alkali -sulphates -chlorides, and -carbonates. For morphology, many spherical particles around 0.1 μm were found. In the second part of the project, the formation of particles during bio-fuel combustion is studied by first measurements on metal release during biofuel combustion. Results from the first part of the project have shown that the particle emission is dominated by inorganic particles at favourable combustion conditions, and the second part is therefore focused on inorganic particles, in which metals are a part. The release of metals is studied to investigate the possibilities to influence formation of combustion particles, and consequently the particle emission. To be able to perform as many tests as possible and to include wide variations in combustion conditions, the second part of the project is carried out using a laboratory reactor. To obtain a time-resolved signal of the release of metals, a large number of single pellets were fired in a laboratory reactor and chemically analysed afterwards using ICP-OES (Inductively Coupled Plasma - Optical Emission Spectrometry). The combustion lapse was interrupted after devolatisation, and after 25 %, 50 %, and 75 % of the char burnout. To obtain a time resolved signal of the emission of unburnt particulate matter a photoelectric aerosol sensor was used as a soot indicator. The results of the initial tests show that the main part of the metals was released during char combustion, but a certain metal

Boletus edulis loaded with γ-Fe2O3 nanoparticles as a magnetic sorbent for preconcentration of Co(II) and Sn(II) prior to their determination by ICP-OES.

Science.gov (United States)

Ozdemir, Sadin; Serkan Yalcin, M; Kilinc, Ersin; Soylak, Mustafa

2017-12-20

The authors show that the fungus Boletus edulis loaded with γ-Fe 2 O 3 nanoparticles is a viable sorbent for magnetic solid phase extraction of trace levels of Co(II) and Sn(II). The surface structure of immobilized magnetized B. edulis was characterized by FT-IR, SEM and EDX. Experimental parameters were optimized. Following elution with 1 M HCl, the ions were quantified by ICP-OES. The limits of detection are 21 pg·mL -1 for Co(II), and 19 pg·mL -1 for Sn(II). The preconcentration factors are 100 for both ions. The sorption capacities of the sorbent are 35.8 mg·g -1 for Co(II) and 29.6 mg·g -1 for Sn(II). The method was applied to the analysis of certificated reference materials and gave ≥95% recoveries with low RSDs. It was also successfully applied to the quantification of Co(II) and Sn(II) in spiked environmental and food samples. Graphical abstract The fungus Boletus edulis loaded with γ-Fe 2 O 3 nanoparticles is a viable biosorbent for magnetic solid phase extraction (MSPE) of trace levels of Co(II) and Sn(II). The surface structure of immobilized magnetized B. edulis was characterized by FT-IR, SEM and EDX. Experimental parameters were optimized.

Designing of Synergistic Waste Mixtures for Multiphase Reactive Smelting

Directory of Open Access Journals (Sweden)

Vaso Manojlović

2016-06-01

Full Text Available Electric arc furnace (EAF dust, together with a mill scale and coke were smelted in a laboratory electric arc furnace. These metallurgical wastes consist of a many different phases and elements, making the reaction process complex. Thermo-chemical analysis of the reactions in metal, slag, and gas phases was done, and used for modeling of the mixture composition and energy consumption required for smelting. Modelling was performed with the software named RikiAlC. The crude ZnO, slag, and metal phase were analyzed using the atomic absorption spectrometry (AAS, the optical emission spectrometry with inductively coupled plasma (ICP-OES, the X-ray diffraction (XRD, the scanning electron microscopy (SEM equipped with energy dispersive spectrometry (EDS, and reflected and transmitted light microscopy. Also, in order to follow the behavior of this process the exhausted gases were monitored. The synergetic effects of the designed mixture may be recognized in minimizing energy consumption for the smelting process, improving the product yield efficiency, and reducing the negative environmental effects.

Analysis of zirconium alloys using inductively-coupled plasma emission spectrometry

International Nuclear Information System (INIS)

White, G.F.; Pickford, C.J.

1982-06-01

As part of an interlaboratory collaborative exercise, certain trace and minor elements have been determined in a proposed zircaloy reference material using inductively-coupled plasma emission spectrometry. A dissolution procedure involving hydrochloric and hydrofluoric acids was used for determination of Hf, Cr, Fe and Sn. Data have also been obtained for Ni, Cu and Mn. Use of a high resolution monochromator in a scanning mode was found necessary for measurement of the emission intensities in order to resolve the spectral lines of interest from the intense and complex emission from the zirconium matrix. (author)

Multielemental speciation analysis by advanced hyphenated technique - HPLC/ICP-MS: A review.

Science.gov (United States)

Marcinkowska, Monika; Barałkiewicz, Danuta

2016-12-01

Speciation analysis has become an invaluable tool in human health risk assessment, environmental monitoring or food quality control. Another step is to develop reliable multielemental speciation methodologies, to reduce costs, waste and time needed for the analysis. Separation and detection of species of several elements in a single analytical run can be accomplished by high performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry (HPLC/ICP-MS). Our review assembles articles concerning multielemental speciation determination of: As, Se, Cr, Sb, I, Br, Pb, Hg, V, Mo, Te, Tl, Cd and W in environmental, biological, food and clinical samples analyzed with HPLC/ICP-MS. It addresses the procedures in terms of following issues: sample collection and pretreatment, selection of optimal conditions for elements species separation by HPLC and determination using ICP-MS as well as metrological approach. The presented work is the first review article concerning multielemental speciation analysis by advanced hyphenated technique HPLC/ICP-MS. Copyright © 2016 Elsevier B.V. All rights reserved.

In vitro permeation of platinum through African and Caucasian skin.

Science.gov (United States)

Franken, A; Eloff, F C; du Plessis, J; Badenhorst, C J; Du Plessis, J L

2015-02-03

The majority of the South African workforce are Africans, therefore potential racial differences should be considered in risk and exposure assessments in the workplace. Literature suggests African skin to be a superior barrier against permeation and irritants. Previous in vitro studies on metals only included skin from Caucasian donors, whereas this study compared the permeation of platinum through African and Caucasian skin. A donor solution of 0.3 mg/ml of potassium tetrachloroplatinate (K₂PtCl₄) dissolved in synthetic sweat was applied to the vertical Franz diffusion cells with full thickness abdominal skin. Skin from three female African and three female Caucasian donors were included (n=21). The receptor solution was removed at various intervals during the 24 h experiment, and analysed with high resolution inductively coupled plasma-mass spectrometry (ICP-MS). Skin was digested and analysed by inductively coupled plasma-optical emission spectrometry (ICP-OES). Significantly higher permeation of platinum through intact African skin (p=0.044), as well as a significantly higher mass of platinum retention in African skin in comparison with Caucasian skin (p=0.002) occurred. Significant inter-donor variation was found in both racial groups (pskin and further investigation is necessary to explain the higher permeation through African skin. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Determination of trace elements in petroleum products by inductively coupled plasma techniques: A critical review

International Nuclear Information System (INIS)

Sánchez, Raquel; Todolí, José Luis; Lienemann, Charles-Philippe; Mermet, Jean-Michel

2013-01-01

The fundamentals, applications and latter developments of petroleum products analysis through inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are revisited in the present bibliographic survey. Sample preparation procedures for the direct analysis of fuels by using liquid sample introduction systems are critically reviewed and compared. The most employed methods are sample dilution, emulsion or micro-emulsion preparation and sample decomposition. The first one is the most widely employed due to its simplicity. Once the sample has been prepared, an organic matrix is usually present. The performance of the sample introduction system (i.e., nebulizer and spray chamber) depends strongly upon the nature and properties of the solution finally obtained. Many different devices have been assayed and the obtained results are shown. Additionally, samples can be introduced into the plasma by using an electrothermal vaporization (ETV) device or a laser ablation system (LA). The recent results published in the literature showing the feasibility, advantages and drawbacks of latter alternatives are also described. Therefore, the main goal of the review is the discussion of the different approaches developed for the analysis of crude oil and its derivates by inductively coupled plasma (ICP) techniques. - Highlights: • Analysis of petroleum products by inductively coupled plasma techniques is revisited. • Fundamental studies are included together with reports dealing with applications. • Conventional and non-conventional sample introduction methods are considered. • Sample preparation methods are critically compared and described

Determination of trace amounts of rare-earth elements in highly pure neodymium oxide by sector field inductively coupled plasma mass spectrometry (ICP-SFMS) and high-performance liquid chromatography (HPLC) techniques

Science.gov (United States)

Pedreira, W. R.; Sarkis, J. E. S.; da Silva Queiroz, C. A.; Rodrigues, C.; Tomiyoshi, I. A.; Abrão, A.

2003-02-01

Recently rare-earth elements (REE) have received much attention in fields of geochemistry and industry. Rapid and accurate determinations of them are increasingly required as industrial demands expand. Sector field inductively coupled plasma mass spectrometry (ICP-SFMS) with high-performance liquid chromatography (HPLC) has been applied to the determination of REE. HR ICP-MS was used as an element-selective detector for HPLC in highly pure materials. The separation of REE with HPLC helped to avoid erroneous analytical results due to spectral interferences. Sixteen elements (Sc, Y and 14 lanthanides) were determined selectively with the HPLC/ICP-SFMS system using a concentration gradient methods. The detection limits with the HPLC/ICP-SFMS system were about 0.5-10 pg mL-1. The percentage recovery ranged from 90% to 100% for different REE. The %RSD of the methods varying between 2.5% and 4.5% for a set of five (n=5) replicates was found for the IPEN's material and for the certificate reference sample. Determination of trace REEs in two highly pure neodymium oxides samples (IPEN and Johnson Matthey Company) were performed. In short, the IPEN's materials which are highly pure (>99.9%) were successfully analyzed without spectral interferences.

Determination of trace amounts of rare-earth elements in highly pure neodymium oxide by sector field inductively coupled plasma mass spectrometry (ICP-SFMS) and high-performance liquid chromatography (HPLC) techniques

International Nuclear Information System (INIS)

Pedreira, W.R.; Sarkis, J.E.S.; Silva Queiroz, C.A. da; Rodrigues, C.; Tomiyoshi, I.A.; Abrao, A.

2003-01-01

Recently rare-earth elements (REE) have received much attention in fields of geochemistry and industry. Rapid and accurate determinations of them are increasingly required as industrial demands expand. Sector field inductively coupled plasma mass spectrometry (ICP-SFMS) with high-performance liquid chromatography (HPLC) has been applied to the determination of REE. HR ICP-MS was used as an element-selective detector for HPLC in highly pure materials. The separation of REE with HPLC helped to avoid erroneous analytical results due to spectral interferences. Sixteen elements (Sc, Y and 14 lanthanides) were determined selectively with the HPLC/ICP-SFMS system using a concentration gradient methods. The detection limits with the HPLC/ICP-SFMS system were about 0.5-10 pg mL -1 . The percentage recovery ranged from 90% to 100% for different REE. The %RSD of the methods varying between 2.5% and 4.5% for a set of five (n=5) replicates was found for the IPEN's material and for the certificate reference sample. Determination of trace REEs in two highly pure neodymium oxides samples (IPEN and Johnson Matthey Company) were performed. In short, the IPEN's materials which are highly pure (>99.9%) were successfully analyzed without spectral interferences

Determination of some inorganic metals in edible vegetable oils by inductively coupled plasma atomic emission spectroscopy (ICP-AES

Directory of Open Access Journals (Sweden)

Musa Özcan, M.

2008-09-01

Full Text Available Seventeen edible vegetable oils were analyzed spectrometrically for their metal (Cu, Fe, Mn, Co, Cr, Pb, Cd, Ni, and Zn contents. Toxic metals in edible vegetable oils were determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES. The highest metal concentrations were measured as 0.0850, 0.0352, 0.0220, 0.0040, 0.0010, 0.0074, 0.0045, 0.0254 and 0.2870 mg/kg for copper in almond oil, for iron in corn oil-(c, for manganese in soybean oil, for cobalt in sunflower oil-(b and almond oil, for chromium in almond oil, for lead in virgin olive oil, for cadmium in sunflower oil-(e, for nickel almond oil and for zinc in almond oil respectively. The method for determining toxic metals in edible vegetable oils by using ICP-AES is discussed. The metals were extracted from low quantities of oil (2-3 g with a 10% nitric acid solution. The extracted metal in acid solution can be injected into the ICPAES. The proposed method is simple and allows the metals to be determined in edible vegetable oils with a precision estimated below 10% relative standard deviation (RSD for Cu, 5% for Fe, 15% for Mn, 8% for Co, 10% for Cr, 20% for Pb, 5% for Cd, 16% for Ni and 11% for Zn.En este estudio se analizó espectrométricamente el contenido en metales (Cu, Fe, Mn, Co, Cr, Pb, Cd, Ni, and Zn de 17 aceites vegetales comestibles mediante ICP-AES. Las concentaciones más elevadas se encontraron para el cobre en el aceite de almendra (0.0850 mg/kg, para el hierro en el aceite de maiz(c,(0.0352 mg/kg, para el manganeso en el aceite de soja (0.0220 mg/kg, para el cobalto en el aceite de girasol (b (0.0040 mg/kg, para el cromo en el aceite de almendra (0.0010 mg/kg, para el plomo en el aceite de oliva virgen (0.0074 mg/kg, para el cadmio en el aceite de girasol (e (0.0045 mg/kg, para el niquel en el aceite de almendra (0.0254 mg/kg y para el zincen el aceite de almendra (0.2870 mg/kg. Los metales se extrajeron a partir de bajas cantidades de aceite (2-3 g, con

Inductively coupled plasma source mass spectrometry

International Nuclear Information System (INIS)

Price Russ, G. III

1993-01-01

Inductively coupled plasma source mass spectrometry (ICP-MS) is a relatively new (5 y commercial availability) technique for simultaneously determining the concentration and isotopic composition of a large number of elements at trace levels. The principle advantages of ICP-MS are the ability to measure essentially all the metallic elements at concentrations as low as 1 part in 10 12 by weight, to analyse aqueous samples directly, to determine the isotopic composition of essentially all the metallic elements, and to analyse samples rapidly (minutes). The history of the development of ICP-MS and discussions of a variety of applications have been discussed in detail in Date and Gray (1988). Koppenaal (1988, 1990) has reviewed the ICP-MS literature. In that ICP-MS is a relatively new and still evolving technique, this chapter will discuss potential capability more than proven performance. (author). 24 refs

Mass and emission spectrometry in the Analytical Chemistry Division of Oak Ridge National Laboratory

Energy Technology Data Exchange (ETDEWEB)

Smith, D.H. (ed.)

1978-11-01

The capabilities of the Mass and Emission Spectrometry Section of the Analytical Chemistry Division of Oak Ridge National Laboratory are described. Many different areas of mass spectrometric expertise are represented in the section: gas analysis, high abundance sensitivity measurements, high- and low-resolution organic analyses, spark source trace constituent analysis, and ion microprobe analysis of surfaces. These capabilities are complemented by emission spectrometry. The instruments are described along with a few applications, some of which are unique.

Mass and emission spectrometry in the Analytical Chemistry Division of Oak Ridge National Laboratory

International Nuclear Information System (INIS)

Smith, D.H.

1978-11-01

The capabilities of the Mass and Emission Spectrometry Section of the Analytical Chemistry Division of Oak Ridge National Laboratory are described. Many different areas of mass spectrometric expertise are represented in the section: gas analysis, high abundance sensitivity measurements, high- and low-resolution organic analyses, spark source trace constituent analysis, and ion microprobe analysis of surfaces. These capabilities are complemented by emission spectrometry. The instruments are described along with a few applications, some of which are unique

Using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) to characterize copper, zinc and mercury along grizzly bear hair providing estimate of diet

International Nuclear Information System (INIS)

Noël, Marie; Christensen, Jennie R.; Spence, Jody; Robbins, Charles T.

2015-01-01

We enhanced an existing technique, laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), to function as a non-lethal tool in the temporal characterization of trace element exposure in wild mammals. Mercury (Hg), copper (Cu), cadmium (Cd), lead (Pb), iron (Fe) and zinc (Zn) were analyzed along the hair of captive and wild grizzly bears (Ursus arctos horribilis). Laser parameters were optimized (consecutive 2000 μm line scans along the middle line of the hair at a speed of 50 μm/s; spot size = 30 μm) for consistent ablation of the hair. A pressed pellet of reference material DOLT-2 and sulfur were used as external and internal standards, respectively. Our newly adapted method passed the quality control tests with strong correlations between trace element concentrations obtained using LA-ICP-MS and those obtained with regular solution-ICP-MS (r 2 = 0.92, 0.98, 0.63, 0.57, 0.99 and 0.90 for Hg, Fe, Cu, Zn, Cd and Pb, respectively). Cross-correlation analyses revealed good reproducibility between trace element patterns obtained from hair collected from the same bear. One exception was Cd for which external contamination was observed resulting in poor reproducibility. In order to validate the method, we used LA-ICP-MS on the hair of five captive grizzly bears fed known and varying amounts of cutthroat trout over a period of 33 days. Trace element patterns along the hair revealed strong Hg, Cu and Zn signals coinciding with fish consumption. Accordingly, significant correlations between Hg, Cu, and Zn in the hair and Hg, Cu, and Zn intake were evident and we were able to develop accumulation models for each of these elements. While the use of LA-ICP-MS for the monitoring of trace elements in wildlife is in its infancy, this study highlights the robustness and applicability of this newly adapted method. - Highlights: • LA-ICP-MS provides temporal trace metal exposure information for wild grizzly bears. • Cu and Zn temporal exposures provide

Using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) to characterize copper, zinc and mercury along grizzly bear hair providing estimate of diet

Energy Technology Data Exchange (ETDEWEB)

Noël, Marie, E-mail: marie.noel@stantec.com [Stantec Consulting Ltd. 2042 Mills Road, Unit 11, Sidney BC V8L 4X2 (Canada); Christensen, Jennie R., E-mail: jennie.christensen@stantec.com [Stantec Consulting Ltd. 2042 Mills Road, Unit 11, Sidney BC V8L 4X2 (Canada); Spence, Jody, E-mail: jodys@uvic.ca [School of Earth and Ocean Sciences, Bob Wright Centre A405, University of Victoria, PO BOX 3065 STN CSC, Victoria, BC V8W 3V6 (Canada); Robbins, Charles T., E-mail: ctrobbins@wsu.edu [School of the Environment and School of Biological Sciences, Washington State University, Pullman, WA 99164-4236 (United States)

2015-10-01

We enhanced an existing technique, laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), to function as a non-lethal tool in the temporal characterization of trace element exposure in wild mammals. Mercury (Hg), copper (Cu), cadmium (Cd), lead (Pb), iron (Fe) and zinc (Zn) were analyzed along the hair of captive and wild grizzly bears (Ursus arctos horribilis). Laser parameters were optimized (consecutive 2000 μm line scans along the middle line of the hair at a speed of 50 μm/s; spot size = 30 μm) for consistent ablation of the hair. A pressed pellet of reference material DOLT-2 and sulfur were used as external and internal standards, respectively. Our newly adapted method passed the quality control tests with strong correlations between trace element concentrations obtained using LA-ICP-MS and those obtained with regular solution-ICP-MS (r{sup 2} = 0.92, 0.98, 0.63, 0.57, 0.99 and 0.90 for Hg, Fe, Cu, Zn, Cd and Pb, respectively). Cross-correlation analyses revealed good reproducibility between trace element patterns obtained from hair collected from the same bear. One exception was Cd for which external contamination was observed resulting in poor reproducibility. In order to validate the method, we used LA-ICP-MS on the hair of five captive grizzly bears fed known and varying amounts of cutthroat trout over a period of 33 days. Trace element patterns along the hair revealed strong Hg, Cu and Zn signals coinciding with fish consumption. Accordingly, significant correlations between Hg, Cu, and Zn in the hair and Hg, Cu, and Zn intake were evident and we were able to develop accumulation models for each of these elements. While the use of LA-ICP-MS for the monitoring of trace elements in wildlife is in its infancy, this study highlights the robustness and applicability of this newly adapted method. - Highlights: • LA-ICP-MS provides temporal trace metal exposure information for wild grizzly bears. • Cu and Zn temporal exposures provide

Analysis of zirconium and nickel based alloys and zirconium oxides by relative and internal monostandard neutron activation analysis methods

International Nuclear Information System (INIS)

Shinde, Amol D.; Acharya, Raghunath; Reddy, Annareddy V. R.

2017-01-01

The chemical characterization of metallic alloys and oxides is conventionally carried out by wet chemical analytical methods and/or instrumental methods. Instrumental neutron activation analysis (INAA) is capable of analyzing samples nondestructively. As a part of a chemical quality control exercise, Zircaloys 2 and 4, nimonic alloy, and zirconium oxide samples were analyzed by two INAA methods. The samples of alloys and oxides were also analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES) and direct current Arc OES methods, respectively, for quality assurance purposes. The samples are important in various fields including nuclear technology. Samples were neutron irradiated using nuclear reactors, and the radioactive assay was carried out using high-resolution gamma-ray spectrometry. Major to trace mass fractions were determined using both relative and internal monostandard (IM) NAA methods as well as OES methods. In the case of alloys, compositional analyses as well as concentrations of some trace elements were determined, whereas in the case of zirconium oxides, six trace elements were determined. For method validation, British Chemical Standard (BCS)-certified reference material 310/1 (a nimonic alloy) was analyzed using both relative INAA and IM-NAA methods. The results showed that IM-NAA and relative INAA methods can be used for nondestructive chemical quality control of alloys and oxide samples

Analysis of zirconium and nickel based alloys and zirconium oxides by relative and internal monostandard neutron activation analysis methods

Energy Technology Data Exchange (ETDEWEB)

Shinde, Amol D.; Acharya, Raghunath; Reddy, Annareddy V. R. [Bhabha Atomic Research Centre, Mumbai (India)

2017-04-15

The chemical characterization of metallic alloys and oxides is conventionally carried out by wet chemical analytical methods and/or instrumental methods. Instrumental neutron activation analysis (INAA) is capable of analyzing samples nondestructively. As a part of a chemical quality control exercise, Zircaloys 2 and 4, nimonic alloy, and zirconium oxide samples were analyzed by two INAA methods. The samples of alloys and oxides were also analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES) and direct current Arc OES methods, respectively, for quality assurance purposes. The samples are important in various fields including nuclear technology. Samples were neutron irradiated using nuclear reactors, and the radioactive assay was carried out using high-resolution gamma-ray spectrometry. Major to trace mass fractions were determined using both relative and internal monostandard (IM) NAA methods as well as OES methods. In the case of alloys, compositional analyses as well as concentrations of some trace elements were determined, whereas in the case of zirconium oxides, six trace elements were determined. For method validation, British Chemical Standard (BCS)-certified reference material 310/1 (a nimonic alloy) was analyzed using both relative INAA and IM-NAA methods. The results showed that IM-NAA and relative INAA methods can be used for nondestructive chemical quality control of alloys and oxide samples.

ICP MS ニヨル カンキョウ シリョウチュウ ノ コンセキ ゲンソ ノ ソクテイ 1 ICP MS ソウチ ノ サイテキ ジョウケン オヨビ ソノ ブンセキ セイド

OpenAIRE

"猶原,順/大西,諭/佐藤,昭彦[他]"; "ナオハラ,ジュン/オオニシ,サトシ/サトウ,アキヒコ"; "Naohara,Jun/Oonishi,Satoshi/Satou,Akihiko"

1992-01-01

"For determination of trace elements in environmental sample by inductively coupled plasma mass spectrometry (ICP-MS), the optimum condition of ICP-MS was determined and the stability of ICP-MS and the precision of elements concentration were investigated. The optimum condition was the sampling depth : 13 mm and RF-power : 1.2 KW. The stability of ICP-MS was indicated little drift of ionic strength after plasma lighting, however, ICP-MS was stabilized after 40 minutes. The coefficient variati...

The calibration of XRF polyethylene reference materials with k 0-NAA and ICP-AES

International Nuclear Information System (INIS)

Swagten, Josefien; Bossus, Daniel; Vanwersch, Hanny

2006-01-01

Due to the lack of commercially available polyethylene reference materials for the calibration of X-ray fluorescence spectrometers (XRF), DSM Resolve, in cooperation with PANalytical, prepared and calibrated such a set of standards in 2005. The reference materials were prepared based on the addition of additives to virgin polyethylene. The mentioned additives are added to improve the performance of the polymers. The elements present in additives are tracers for the used additives. The reference materials contain the following elements: F, Na, Mg, Al, Si, P, S, Ca, Ti and Zn in the concentration range of 5 mg/kg for Ti, up to 600 mg/kg for Mg. The calibration of the reference materials, including a blank, was performed using inductively coupled plasma atomic emission spectrometry (ICP-AES) and Neutron Activation Analysis (k 0 -NAA). ICP-AES was used to determine the elements Na, Mg, Al, P, Ca, Ti and Zn whereas k 0 -NAA was used for F, Na, Mg, Al, Ca, Ti and Zn. Over the complete concentration range, a good agreement of the results was found between the both techniques. This project has shown that within DSM Resolve, it is possible to develop and to calibrate homogenous reference materials for XRF

Curve resolution and figures of merit estimation for determination of trace elements in geological materials by inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Lorber, A.; Harel, A.; Goldbart, Z.; Brenner, I.B.

1987-01-01

In geochemical analysis using inductively coupled plasma atomic emission spectrometry (ICP-AES), spectral interferences and background enhancement in response to sample concomitants are the main cause of deterioration of the limit of detection (LOD) and inaccuracy of the determination at the trace and minor element levels. In this account, the authors describe the chemometric procedure of curve resolution for compensating for these sources of error. A newly developed method for calculating figures of merit is used to evaluate the correction procedure, test the statistical significance of the determined concentration, and determine LODs for each sample. The technique involves scanning the vicinity of the spectral line of the analyte. With prior knowledge of potential spectral interferences, deconvolution of the overlapped response is possible. Analytical data for a wide range of geological standard reference materials demonstrate the effectiveness of the chemometric techniques. Separation of 0.002 nm spectral coincidence, employing a 0.02 nm resolution spectrometer, is demonstrated

Thallium and manganese complexes involved in the luminescence emission of potassium-bearing aluminosilicates

Energy Technology Data Exchange (ETDEWEB)

Gomez-Gonzalez, Miguel A., E-mail: miguel.gomez@mncn.csic.es [Museo Nacional de Ciencias Naturales, CSIC, Jose Gutierrez Abascal 2, Madrid E-28006 (Spain); Garcia-Guinea, Javier, E-mail: guinea@mncn.csic.es [Museo Nacional de Ciencias Naturales, CSIC, Jose Gutierrez Abascal 2, Madrid E-28006 (Spain); Garrido, Fernando, E-mail: fernando.garrido@mncn.csic.es [Museo Nacional de Ciencias Naturales, CSIC, Jose Gutierrez Abascal 2, Madrid E-28006 (Spain); Townsend, Peter D., E-mail: pdtownsend@gmail.com [School of Science and Technology, University of Sussex, Brighton BN1 9QH (United Kingdom); Marco, Jose-Francisco, E-mail: jfmarco@iqfr.csic.es [Instituto de Química-Física Rocasolano, CSIC, Calle Serrano 119, Madrid E-28006 (Spain)

2015-03-15

The luminescence emission at 285 nm in natural K-feldspar has been studied by Russian groups and associated with thallium ions in structural positions of K{sup +} sites as artificially thallium-doped feldspars display the same emission band. Here attention is focussed on spectra of CL emission bands centered near 285 and 560 nm from paragenetic adularia, moscovite and quartz micro-inclusions. With accesorial thallium they show clear resemblances to each other. Associated sedimentary and hydrothermal aluminosilicate samples collected from Guadalix (Madrid, Spain) were analyzed with a wide range of experimental techniques including Environmental Scanning Electron Microscopy (ESEM) with an attached X-Ray Energy-Dispersive Spectrometer (EDS) and a cathodoluminescence probe (CL) and Electron Probe Microanalysis (EPMA), X-Ray Fluorescence Spectrometry (XRF), Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES), Differential and Thermogravimetric Analyses (DTA-TG), radioluminescence (RL), Mössbauer spectroscopy and X-Ray Photoelectron Spectrometry (XPS). The luminescence emission bands at 285 and 560 nm seem to be associated with hydrous thallium–manganese complexes bonded to potassium-bearing aluminosilicates since various minerals such as K-feldspar, moscovite and quartz micro-inclusions display similar CL spectra, accesorial thallium and hydroxyl groups. The presence of iron introduces a brown color which is attributed to submicroscopic iron oxides detectable in the optical and chemical microanalysis, but this does not contribute to the luminescence emission. The XPS Mn 2p spectrum of the adularia sample at room temperature is composed of a spin–orbit doublet plus clear shake-up satellite structure ∼4 eV above the main photoemision lines and is consistent with Mn{sup 2+} in good agreement with the observed luminescence emission at 560 nm for aluminosilicates produced by a {sup 4}T1({sup 4}G)→{sup 6}A1({sup 6}S) transition in tetrahedrally

Concerns about Quadrupole ICP-MS Lead Isotopic Data and Interpretations in the Environment and Health Fields

Directory of Open Access Journals (Sweden)

Brian Gulson

2018-04-01

Full Text Available There has been a massive increase in recent years of the use of lead (Pb isotopes in attempts to better understand sources and pathways of Pb in the environment and in man or experimental animals. Unfortunately, there have been many cases where the quality of the isotopic data, especially that obtained by quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS, are questionable, resulting in questionable identification of potential sources, which, in turn, impacts study interpretation and conclusions. We present several cases where the isotopic data have compromised interpretation because of the use of only the major isotopes 208Pb/206Pb and 207Pb/206Pb, or their graphing in other combinations. We also present some examples comparing high precision data from thermal ionization (TIMS or multi-collector plasma mass spectrometry (MC-ICP-MS to illustrate the deficiency in the Q-ICP-MS data. In addition, we present cases where Pb isotopic ratios measured on Q-ICP-MS are virtually impossible for terrestrial samples. We also evaluate the Pb isotopic data for rat studies, which had concluded that Pb isotopic fractionation occurs between different organs and suggest that this notion of biological fractionation of Pb as an explanation for isotopic differences is not valid. Overall, the brief review of these case studies shows that Q-ICP-MS as commonly practiced is not a suitable technique for precise and accurate Pb isotopic analysis in the environment and health fields.

Concerns about Quadrupole ICP-MS Lead Isotopic Data and Interpretations in the Environment and Health Fields.

Science.gov (United States)

Gulson, Brian; Kamenov, George D; Manton, William; Rabinowitz, Michael

2018-04-11

There has been a massive increase in recent years of the use of lead (Pb) isotopes in attempts to better understand sources and pathways of Pb in the environment and in man or experimental animals. Unfortunately, there have been many cases where the quality of the isotopic data, especially that obtained by quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS), are questionable, resulting in questionable identification of potential sources, which, in turn, impacts study interpretation and conclusions. We present several cases where the isotopic data have compromised interpretation because of the use of only the major isotopes 208 Pb/ 206 Pb and 207 Pb/ 206 Pb, or their graphing in other combinations. We also present some examples comparing high precision data from thermal ionization (TIMS) or multi-collector plasma mass spectrometry (MC-ICP-MS) to illustrate the deficiency in the Q-ICP-MS data. In addition, we present cases where Pb isotopic ratios measured on Q-ICP-MS are virtually impossible for terrestrial samples. We also evaluate the Pb isotopic data for rat studies, which had concluded that Pb isotopic fractionation occurs between different organs and suggest that this notion of biological fractionation of Pb as an explanation for isotopic differences is not valid. Overall, the brief review of these case studies shows that Q-ICP-MS as commonly practiced is not a suitable technique for precise and accurate Pb isotopic analysis in the environment and health fields.

Non-Aqueous Sol-Gel Synthesis of FePt Nanoparticles in the Absence of In Situ Stabilizers

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Tobias Preller

2018-05-01

Full Text Available The synthesis of FePt nanocrystals is typically performed in an organic solvent at rather high temperatures, demanding the addition of the in situ stabilizers oleic acid and oleylamine to produce monomodal particles with well-defined morphologies. Replacing frequently-used solvents with organic media bearing functional moieties, the use of the stabilizers can be completely circumvented. In addition, various morphologies and sizes of the nanocrystals can be achieved by the choice of organic solvent. The kinetics of particle growth and the change in the magnetic behavior of the superparamagnetic FePt nanocrystals during the synthesis with a set of different solvents, as well as the resulting morphologies and stoichiometries of the nanoparticles were determined by powder X-ray diffraction (PXRD, small-angle X-ray scattering (SAXS, transmission electron microscopy (TEM, inductively coupled plasma optical emission spectroscopy (ICP-OES/mass spectrometry (ICP-MS, and superconducting quantum interference device (SQUID measurements. Furthermore, annealing of the as-prepared FePt nanoparticles led to the ordered L10 phase and, thus, to hard magnetic materials with varying saturation magnetizations and magnetic coercivities.

Chromium Speciation Analysis by Ion Chromatography Coupled ...

African Journals Online (AJOL)

Two methods coupling ion chromatography with inductively coupled plasma - optical emission spectroscopy (ICP-OES) were developed for the simultaneous separation and determination of Cr(III) and Cr(VI) species. In the first method, anion chromatography with sodium bicarbonate/carbonate solution as the eluent was ...

Spectrochemical pure cerium dioxide preparation and its quality control by inductively coupled plasma and mass spectrometry (ICP/MS)

International Nuclear Information System (INIS)

Da Silva Queiroz, C.A.; De Souza, J.E.; Abrao, A.

1998-01-01

Full text: A simple and economic procedure for the purification until 500 g CeO 2 batch is presented. The purified material will be used as spectrochemical standard. It is obtained by association of the fractional precipitation technique in the system REC 3 /H 2 O 2 /NH 4 OH to enrich the cerium up to 90% and then refined by ion exchange up to 99.9% CeO2. The 99,9% CeO 2 warranty control of purity was accomplished by inductively coupled plasma and mass spectrometry (ICP/ MS) and compared with activation analysis data, exhibiting impurities traces of same values of the international spec pure standard. The following results (average values) for the contaminant rare earths are (ppm):La(36), Pr(19), Nd(161), Sm(11), Eu(5,3),Gd(113),Tb(89),Dy(2),Ho(0.05),Er(1), Tm(0), Yb(11), Lu (19) and Y(2.1), respectively

Establishment of methodology for determination of 93Zr in radioactive wastes by Liquid Scintillation Counting (LSC) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

International Nuclear Information System (INIS)

Oliveira, Thiago Cesar de

2014-01-01

The zirconium-93 is a long-lived pure β-particle-emitting radionuclide produced from 235 U fission and from neutron activation of the stable isotope 92 Zr and thus occurring as one of the radionuclides found in nuclear reactors. Due to its long half life, 93 Zr is one of the radionuclides of interest for the performance of assessment studies of waste storage or disposal. Measurement of 93 Zr is difficult owing to its trace level concentration and its low activity in nuclear wastes and further because its certified standards are not frequently available. The aim of this work was to develop a selective radiochemical separation methodology for the determination of 93 Zr in nuclear waste and analyze it by Liquid Scintillation Counting (LSC) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS). To set up the radiochemical separation procedure for zirconium, a tracer solution of 95 Zr and its 724 keV γ-ray measurements by γ- spectrometry were used in order to follow the behavior of zirconium during the radiochemical separation. For the LSC technique a 55 Fe solution, which is one of the major interfering measures zirconium, was used to verify the decontamination factor during the separation process. The efficiency detection for 63 Ni was used to determination of 93 Zr activity in the matrices analyzed. The limit of detection of the 0.05 Bq 1 −1 was obtained for 63 Ni standard solutions by using a sample:cocktail ratio of 3:17 mL for Optiphase Hisafe 3 cocktail. For the ICP-MS technique a zirconium stable solution was used to verify the zirconium behavior and recovery during radiochemical separation and a solution of Ba, Co, Eu, Fe, Mn, Nb, Sr and Y was used to verify the decontamination factor during the separation process. A standard solution 93 Nb as isotope for determining the 93 Zr by ICP-MS was used for calibration and analysis. The detection limit of 0.039 ppb was obtained for the standard solution of zirconium. Then, the protocol was applied to low level

Spectroscopic analysis of high protein nigella seeds (Kalonji) using laser-induced breakdown spectroscopy and inductively coupled plasma/optical emission spectroscopy

Science.gov (United States)

Rehan, Imran; Khan, M. Zubair; Ali, Irfan; Rehan, Kamran; Sultana, Sabiha; Shah, Sher

2018-03-01

The spectroscopic analysis of high protein nigella seeds (also called Kalonji) was performed using pulsed nanosecond laser-induced breakdown spectroscopy (LIBS) at 532 nm. The emission spectrum of Kalonji recorded with an LIBS spectrometer exposed the presence of various elements like Al, B, Ba, Ca, Cr, K, P, Mg, Mn, Na, Ni, S, Si, Cu, Fe, Ti, Sn, Sr, and Zn. The plasma parameters (electron temperature and electron density) were estimated using Ca-I spectral lines and their behavior were studied against laser irradiance. The electron temperature and electron density was observed to show an increasing trend in the range of 5802-7849 K, and (1.2-3.9) × 1017 cm- 3, respectively, in the studied irradiance range of (1.2-12.6) × 109 W/cm2. Furthermore, the effect of varying laser energy on the integrated signal intensities was also studied. The quantitative analysis of the detected elements was performed via the calibration curves drawn for all the observed elements through typical samples made in the known concentration in the Kalonji matrix, and by setting the concentration of P as the calibration. The validity of our LIBS findings was verified via comparison of the results with the concentration of every element find in Kalonji using the standard analytical tool like ICP/OES. The results acquired using LIBS and ICP/OES were found in fine harmony. Moreover, limit of detection was measured for toxic metals only.

Metals recovery of spent household batteries using a hydrometallurgical process

International Nuclear Information System (INIS)

Souza, K.P.; Tenorio, J.A.S.

2010-01-01

The objective of the work is to study a method for metals recovery from a sample composed by a mixture of the main types of spent household batteries. Segregation of the main metals is investigated using a treatment route consisting of the following steps: manual identified and dismantling, grinding, electric furnace reduction, acid leaching and selective precipitation with sodium hydroxide with and without hydrogen peroxide. Before and after precipitations the solutions had been analyzed by Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP/OES) and the precipitated analyzed by Scanning Electron Microscopy (SEM) with Spectrometry of Energy Dispersion Spectroscopy (EDS). The results had indicated that the great majority of metals had been precipitated in pHs studied, also had co-precipitation or simultaneous precipitation of metals in some pHs. (author)

Metals recovery of spent household batteries using a hydrometallurgical process; Recuperacao de metais de sucatas de pilhas e baterias pos-consumo utilizando processamento hidrometalurgico

Energy Technology Data Exchange (ETDEWEB)

Souza, K.P.; Tenorio, J.A.S., E-mail: kprovazi@gmail.co [Universidade de Sao Paulo (USP), SP (Brazil). Dept. de Engenharia Metalurgica e de Materiais

2010-07-01

The objective of the work is to study a method for metals recovery from a sample composed by a mixture of the main types of spent household batteries. Segregation of the main metals is investigated using a treatment route consisting of the following steps: manual identified and dismantling, grinding, electric furnace reduction, acid leaching and selective precipitation with sodium hydroxide with and without hydrogen peroxide. Before and after precipitations the solutions had been analyzed by Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP/OES) and the precipitated analyzed by Scanning Electron Microscopy (SEM) with Spectrometry of Energy Dispersion Spectroscopy (EDS). The results had indicated that the great majority of metals had been precipitated in pHs studied, also had co-precipitation or simultaneous precipitation of metals in some pHs. (author)

A Preliminary study of Sr/Ca thermometry in Chang Islands, Gulf of Thailand

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Wararat Sirianansakul

2014-10-01

Full Text Available Variations in ratios of strontium-to-calcium (Sr/Ca for two Porites sp. coral specimens collected from Wai (PW and Loa Ya (PLY islands, part of Chang islands, Gulf of Thailand, were determined. Inductively coupled plasma optimal emission spectrometry (ICP-OES was used to analyze this ratio, which demonstrates annual cycles and the data is assumed to reflect the sea surface temperature (SST. Comparing the ratios with SST data, following Sr/Ca–SST relationships were determined PW: Sr/Ca (mmol/mol = 11.56–0.070×SST, PLY: Sr/Ca (mmol/mol = 11.89–0.081×SST. Our correlations are different from those previously reported; a discrepancy that may involve differences in analytical methods employed and abnormally low sea surface salinity (SSS (<30 psu in the Gulf of Thailand.

3D printing for cyclonic spray chambers in ICP spectrometry

OpenAIRE

Geertsen , Valérie; Barruet , Elodie; Tache , Olivier

2015-01-01

International audience; Additive manufacturing (AM) or 3D-printing is an increasingly widespread technique which is often described as a source for rapid prototyping whereas it is a manufacturing process in itself. It is a new tool for instrumental research laboratories which can now easily manufacture by themselves a large variety of devices. This article describes its application to ICP introduction system spray chambers. We undertake to print and study cyclone spray chambers by combining a...

Tissue gadolinium deposition in renally impaired rats exposed to different gadolinium-based MRI contrast agents: evaluation with inductively coupled plasma mass spectrometry (ICP-MS).

Science.gov (United States)

Sato, Tomohiro; Ito, Katsuyoshi; Tamada, Tsutomu; Kanki, Akihiko; Watanabe, Shigeru; Nishimura, Hirotake; Tanimoto, Daigo; Higashi, Hiroki; Yamamoto, Akira

2013-10-01

To quantify tissue gadolinium (Gd) deposition in renally impaired rats exposed to Gd-EOB-DTPA and other Gd-based MRI contrast agents by means of inductively coupled plasma mass spectrometry (ICP-MS), and to compare the differences in distribution among major organs as possible triggers for nephrogenic systemic fibrosis (NSF). A total of 15 renally impaired rats were injected with Gd-EOB-DTPA, Gd-DTPA-BMA and Gd-HP-DO3A. Gd contents of skin, liver, kidney, lung, heart, spleen, diaphragm and femoral muscle were measured by inductively coupled plasma mass spectrometry (ICP-MS). Histological assessment was also conducted. Tissue Gd deposition in all organs was significantly higher (P=0.005~0.009) in the Gd-DTPA-BMA group than in the Gd-HP-DO3A and Gd-EOB-DTPA groups. In the Gd-DTPA-BMA group, Gd was predominantly deposited in kidney (1306±605.7μg/g), followed by skin, liver, lung, spleen, femoral muscle, diaphragm and heart. Comparing Gd-HP-DO3A and Gd-EOB-DTPA groups, Gd depositions in the kidney, liver and lung were significantly lower (P=0.009~0.011) in the Gd-EOB-DTPA group than in the Gd-HP-DO3A group although no significant differences were seen for any other organs. Gd-EOB-DTPA is a stable and safe Gd-based contrast agent (GBCA) showing lower Gd deposition in major organs in renally impaired rats, compared with other GBCAs. This fact suggests that the risk of NSF onset would be low in the use of Gd-EOB-DTPA. Copyright © 2013 Elsevier Inc. All rights reserved.

Single-cell analysis by ICP-MS/MS as a fast tool for cellular bioavailability studies of arsenite.

Science.gov (United States)

Meyer, S; López-Serrano, A; Mitze, H; Jakubowski, N; Schwerdtle, T

2018-01-24

Single-cell inductively coupled plasma mass spectrometry (SC-ICP-MS) has become a powerful and fast tool to evaluate the elemental composition at a single-cell level. In this study, the cellular bioavailability of arsenite (incubation of 25 and 50 μM for 0-48 h) has been successfully assessed by SC-ICP-MS/MS for the first time directly after re-suspending the cells in water. This procedure avoids the normally arising cell membrane permeabilization caused by cell fixation methods (e.g. methanol fixation). The reliability and feasibility of this SC-ICP-MS/MS approach with a limit of detection of 0.35 fg per cell was validated by conventional bulk ICP-MS/MS analysis after cell digestion and parallel measurement of sulfur and phosphorus.

Assessment and modifications of digestion procedures to determine trace elements in urine of hypertensive and diabetes mellitus patients

Directory of Open Access Journals (Sweden)

Awad Abdalla Momen

2013-01-01

Full Text Available Context: There is accumulating evidence that the metabolism of several trace elements like Cr, Cu, Pb, Cd, Co, Mn and Zn might have specific roles in the pathogenesis and progress of many diseases like hypertension (HTN and diabetes mellitus (DM. Objectives: To provide a fast, efficient, sensitive, and reliable analytical procedure for trace element determination in urine samples of HTN and DM patients using inductively coupled plasma optical emission spectrometry (ICP-OES. Setting and Design: The ICP-OES operating conditions were optimised and carefully selected in order to maximise the sensitivity, precision and accuracy. Factors affecting analytical and biological variability of the concentrations under study were discussed and carefully optimised. Materials and Methods: Different digestion procedures with acids and oxidising reagents were tested. The suitable procedure ICP-OES was selected, carefully modified and applied. The validity and accuracy of the different elements were determined by spiking of samples with known amounts of multi-element standard solution. Statistical Analysis: Student t-test and analysis of variance (ANOVA test were used for analysis. Microsoft Excel was used to assess the significance of the difference between variables. The concentrations obtained were expressed as mean value ± standard deviation (P = 0.05. Results: The results of this study showed that the mean concentrations of Cd, Zn, Pb, Cu, Cr and Mn in urine from both HTN (study group A and DM (study group B patients were higher than the corresponding values observed in the control group. However, while the mean value of Co was low as compared to the control group, the differences found were not significant (P = 0.05. Conclusion: The method used had excellent sensitivity, multi-element data could be obtained with very short acquisition time. The elements Cr, Cd, Pb and Zn might have specific roles in the pathogenesis and progress of HTN and DM. Further

Characterization of edible seaweed harvested on the Galician coast (northwestern Spain) using pattern recognition techniques and major and trace element data.

Science.gov (United States)

Romarís-Hortas, Vanessa; García-Sartal, Cristina; Barciela-Alonso, María Carmen; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Pilar

2010-02-10

Major and trace elements in North Atlantic seaweed originating from Galicia (northwestern Spain) were determined by using inductively coupled plasma-optical emission spectrometry (ICP-OES) (Ba, Ca, Cu, K, Mg, Mn, Na, Sr, and Zn), inductively coupled plasma-mass spectrometry (ICP-MS) (Br and I) and hydride generation-atomic fluorescence spectrometry (HG-AFS) (As). Pattern recognition techniques were then used to classify the edible seaweed according to their type (red, brown, and green seaweed) and also their variety (Wakame, Fucus, Sea Spaghetti, Kombu, Dulse, Nori, and Sea Lettuce). Principal component analysis (PCA) and cluster analysis (CA) were used as exploratory techniques, and linear discriminant analysis (LDA) and soft independent modeling of class analogy (SIMCA) were used as classification procedures. In total, t12 elements were determined in a range of 35 edible seaweed samples (20 brown seaweed, 10 red seaweed, 4 green seaweed, and 1 canned seaweed). Natural groupings of the samples (brown, red, and green types) were observed using PCA and CA (squared Euclidean distance between objects and Ward method as clustering procedure). The application of LDA gave correct assignation percentages of 100% for brown, red, and green types at a significance level of 5%. However, a satisfactory classification (recognition and prediction) using SIMCA was obtained only for red seaweed (100% of cases correctly classified), whereas percentages of 89 and 80% were obtained for brown seaweed for recognition (training set) and prediction (testing set), respectively.

Geochemistry of environmentally sensitive trace elements in Permian coals from the Huainan coalfield, Anhui, China

Science.gov (United States)

Chen, J.; Liu, Gaisheng; Jiang, M.; Chou, C.-L.; Li, H.; Wu, B.; Zheng, Lingyun; Jiang, D.

2011-01-01

To study the geochemical characteristics of 11 environmentally sensitive trace elements in the coals of the Permian Period from the Huainan coalfield, Anhui province, China, borehole samples of 336 coals, two partings, and four roof and floor mudstones were collected from mineable coal seams. Major elements and selected trace elements were determined by inductively coupled plasma optical emission spectrometry (ICP-OES), inductively coupled plasma mass spectrometry (ICP-MS), and hydride generation atomic absorption spectrometry (HAAS). The depositional environment, abundances, distribution, and modes of occurrence of trace elements were investigated. Results show that clay and carbonate minerals are the principal inorganic constituents in the coals. A lower deltaic plain, where fluvial channel systems developed successively, was the likely depositional environment of the Permian coals in the Huainan coalfield. All major elements have wider variation ranges than those of Chinese coals except for Mg and Fe. The contents of Cr, Co, Ni, and Se are higher than their averages for Chinese coals and world coals. Vertical variations of trace elements in different formations are not significant except for B and Ba. Certain roof and partings are distinctly higher in trace elements than underlying coal bench samples. The modes of occurrence of trace elements vary in different coal seams as a result of different coal-forming environments. Vanadium, Cr, and Th are associated with aluminosilicate minerals, Ba with carbonate minerals, and Cu, Zn, As, Se, and Pb mainly with sulfide minerals. ?? 2011 Elsevier B.V.

Application of isotope-dilution laser ablation ICP-MS for direct determination of Pu concentrations in soils at pg g{sup -1} levels

Energy Technology Data Exchange (ETDEWEB)

Boulyga, Sergei F.; Tibi, Markus; Heumann, Klaus G. [Institute of Inorganic Chemistry and Analytical Chemistry, Johannes Gutenberg-University Mainz, Duesbergweg 10-14, 55099, Mainz (Germany)

2004-01-01

The methods available for determination of environmental contamination by plutonium at ultra-trace levels require labor-consuming sample preparation including matrix removal and plutonium extraction in both nuclear spectroscopy and mass spectrometry. In this work, laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was applied for direct analysis of Pu in soil and sediment samples. Application of a LINA-Spark-Atomizer system (a modified laser ablation system providing high ablation rates) coupled with a sector-field ICP-MS resulted in detection limits as low as 3 x 10{sup -13} g g{sup -1} for Pu isotopes in soil samples containing uranium at a concentration of a few {mu}g g{sup -1}. The isotope dilution (ID) technique was used for quantification, which compensated for matrix effects in LA-ICP-MS. Interferences by UH{sup +} and PbO{sub 2}{sup +} ions and by the peak tail of {sup 238}U{sup +} ions were reduced or separated by use of dry plasma conditions and a mass resolution of 4000, respectively. No other effects affecting measurement accuracy, except sample inhomogeneity, were revealed. Comparison of results obtained for three contaminated soil samples by use of {alpha}-spectrometry, ICP-MS with sample decomposition, and LA-ICP-IDMS showed, in general, satisfactory agreement of the different methods. The specific activity of {sup 239+240}Pu (9.8{+-}3.0 mBq g{sup -1}) calculated from LA-ICP-IDMS analysis of SRM NIST 4357 coincided well with the certified value of 10.4{+-}0.2 mBq g{sup -1}. However, the precision of LA-ICP-MS for determination of plutonium in inhomogeneous samples, i.e. if ''hot'' particles are present, is limited. As far as we are aware this paper reports the lowest detection limits and element concentrations yet measured in direct LA-ICP-MS analysis of environmental samples. (orig.)

[Determination of Total Iron and Fe2+ in Basalt].

Science.gov (United States)

Liu, Jian-xun; Chen, Mei-rong; Jian, Zheng-guo; Wu, Gang; Wu, Zhi-shen

2015-08-01

Basalt is the raw material of basalt fiber. The content of FeO and Fe2O3 has a great impact on the properties of basalt fibers. ICP-OES and dichromate method were used to test total Fe and Fe(2+) in basalt. Suitable instrument parameters and analysis lines of Fe were chosen for ICP-OES. The relative standard deviation (RSD) of ICP-OES is 2.2%, and the recovery is in the range of 98%~101%. The method shows simple, rapid and highly accurate for determination of total Fe and Fe(2+) in basalt. The RSD of ICP-OES and dichromate method is 0.42% and 1.4%, respectively.

Determination of Metal Levels in Shamma (Smokeless Tobacco) with Inductively Coupled Plasma Mass Spectrometry (ICP-MS) in Najran, Saudi Arabia

Science.gov (United States)

Brima, Eid Ibrahim

2016-10-01

Objective: The use of Shamma (smokeless tobacco) by certain groups is giving rise to health problems, including cancer, in parts of Saudi Arabia. Our objective was to determine metals levels in Shamma using inductively coupled plasma mass spectrometry (ICP-MS). Methods: Thirty-three samples of Shamma (smokeless tobacco) were collected, comprising four types: brown Shamma (n = 14.0), red Shamma (n = 9.0), white Shamma (n = 4.0), and yellow Shamma (n = 6.0). All samples were collected randomly from Shamma users in the city of Najran. Levels of 11 elements (Al, As, Cd, Co, Cr, Cu, Li, Mn, Ni, Pb, and Zn) were determined by ICP-MS. Results: A mixed standard (20 ppb) of all elements was used for quality control, and average recoveries ranged from 74.7% to 112.2%. The highest average concentrations were found in the following order: Al (598.8–812.2 μg/g), Mn (51.0–80.6 μg/g), and Ni (23.2–53.3 μg/g) in all four Shamma types. The lowest concentrations were for As (0.7–1.0 μg/g) and Cd (0.0–0.06 μg/g). Conclusions: The colour of each Shamma type reflects additives mixed into the tobacco. Cr and Cu were showed significant differences (P awareness about the safety and health effects of Shamma, which is clearly a source of oral exposure to metals. Creative Commons Attribution License

Road Environments: Impact of Metals on Human Health in Heavily Congested Cities of Poland.

Science.gov (United States)

Adamiec, Ewa

2017-06-29

Road dust as a by-product of exhaust and non-exhaust emissions can be a major cause of systemic oxidative stress and multiple disorders. Substantial amounts of road dust are repeatedly resuspended, in particular at traffic lights and junctions where more braking is involved, causing potential threat to pedestrians, especially children. In order to determine the degree of contamination in the heavily traffic-congested cities of Poland, a total of 148 samples of road dust (RD), sludge from storm drains (SL) and roadside soil (RS) were collected. Sixteen metals were analysed using inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectroscopy (ICP-OES) and atomic absorption spectroscopy (AAS) in all samples. Chemical evaluation followed by Principal Component Analysis (PCA) revealed that road environments have been severely contaminated with traffic-related elements. Concentration of copper in all road-environment samples is even higher, exceeding even up to 15 times its average concentrations established for the surrounding soils. Non-carcinogenic health risk assessment revealed that the hazard index (HI) for children in all road-environment samples exceeds the safe level of 1. Therefore, greater attention should be paid to potential health risks caused by the ingestion of traffic-related particles during outdoor activities.

Air pollution studies using PIXE and ICP methods

International Nuclear Information System (INIS)

Stihi, Claudia; Bancuta, Anca; Popescu, I V; Virgolici, M; Cimpoca, V; Gugiu, M; Vlaicu, Gh

2006-01-01

In the present work the moss biomonitoring technique and the combination of two analytical techniques - Particle Induced X-ray Emission (PIXE) and Inductively Coupled Plasma (ICP) - were applied for assessing environmental situation from the point of view of air polluting along the transect from north to south of the Dambovita County. PIXE analysis at the Tandem Accelerator FN-8 of the National Institute of Nuclear Physics - Horia Hulubei of Magurele, Bucharest, allowed determination of P, S, Cl, K, Ca, Mn, Fe, Ni, Cu, Zn, As, Sr, Cd and Pb in samples. ICP analyses were made using a Baird ICP2070 - Sequential Plasma Spectrometer in Targoviste and we determined in samples the concentration of Li, B, Na, and Mg together with Cd and Pb. The obtained results will permit to determine the regional extent of heavy metals and toxic elements atmospheric pollution and to identify specially affected areas and local sources of

Redox speciation of final repository relevant elements using separation methods in combination with ICP mass spectrometry

International Nuclear Information System (INIS)

Graser, Carl-Heinrich

2015-01-01

The long-term safety assessment for nuclear waste repositories requires a detailed understanding of the chemistry of actinide elements in the geosphere. The development of advanced analytical tools is required to gain detailed insights into actinide redox speciation in a given system. The mobility of radionuclides is mostly determined by the geochemical conditions which control the redox state of radionuclides. Besides the longlived radionuclides plutonium (Pu) and neptunium (Np), which are key elements in high level nuclear waste, iron (Fe) represents a main component in natural systems controlling redox related geochemical processes. Analytical techniques for determining oxidation state distribution for redox sensitive radionuclides and other metal ions often have a lack of sensitivity. The detection limits of these methods (i.e. UV/vis, TRLFS, XANES) are in general in the range of ≥ 10 -6 mol.L -1 . As a consequence ultrasensitive new analytical techniques are required. Capillary electrophoresis (CE) and ion chromatography (IC) are powerful separation methods for metal ions. In the course of this thesis different speciation method for iron, neptunium and plutonium were optimized. With the optimized setup redox speciation analysis of these elements in different samples were done. Furthermore CE hyphenated to inductively coupled plasma sector field mass spectrometry (CE - ICP - SF - MS) was used to measure the redox speciation of Pu (III, IV, V, VI), Np (IV, V, VI) and Fe (II, III) at concentrations lower than 10 -7 mol.L -1 . CE coupling and separation parameters such as sample gas pressure, make up flow rate, capillary position, auxiliary gas flow, as well as the electrolyte system were optimized to obtain the maximum sensitivity. The methodes detection limits are 10 -12 mol.L -1 for Np and Pu. The various oxidation state species of Pu and Np in different samples were separated by application of an acetate based electrolyte system. The separation of Fe (II

Analysis of I-Br-Cl in single fluid inclusions by LA-ICP-MS

Science.gov (United States)

Giehl, C.; Fusswinkel, T.; Beermann, O.; Garbe-Schönberg, D.; Scholten, L.; Wagner, T.

2017-12-01

Halogens are excellent tracers of hydrothermal fluid sources and in-situ LA-ICP-MS analysis of Cl and Br in single fluid inclusions has provided fundamentally new insight into hydrothermal fluid flow and ore formation. There is mounting evidence that enrichment and depletion of Br relative to Cl may be caused by a number of processes beyond seawater evaporation and halite dissolution which cannot be discriminated on the basis of Br/Cl ratios alone. Expanding the analytical capabilities of fluid inclusion LA-ICP-MS analysis to include iodine would allow to discern between selective and coupled enrichment processes of Cl, Br and I, even in geologically complex samples that are inaccessible to bulk extraction techniques. We present iodine concentration data determined by LA-ICP-MS analysis of synthetic fluid inclusions, using the Sca17 scapolite reference material for external standardization (Seo et al., 2011). Iodine concentrations in Sca17 were determined using the Durango apatite standard. Four starting solutions containing I (0.3, 1.5, 27, 78 µg/g), Br (941, 1403, 2868, 4275 µg/g), Na (30.7, 94.7 mg/g), and Cl (50, 137 mg/g) (analyzed by ICP-OES and ICP-MS at CAU Kiel) were prepared by dissolving reagent grade chemical powders in ultra-pure water. Spherical inclusions (up to 40 µm) were synthesized from the starting solutions in pre-cracked, HF-treated synthetic quartz crystals which were placed in gold capsules and equilibrated at 600°C, 100/200 MPa in cold seal pressure vessels. Fluid inclusion LA-ICP-MS analysis (University of Helsinki) yielded average I concentrations in excellent agreement with the starting solutions (27.3 µg/g ± 14 %RSD for the 27 µg/g solution and 77.6 µg/g ± 8.3 %RSD for the 78 µg/g solution). Average Br and I concentrations deviate less than 10 % from solution concentration values. For the low I concentration solutions, the synthetic inclusions were too small to detect I. Thus, given suitable standard materials and sufficient

Metal and trace element sediment assessment from Guarapiranga reservoir, Alto Tiete Basin, Sao Paulo, SP, Brazil; Avaliacao da concentracao de metais e elementos traco em amostras de sedimento do reservatorio Guarapiranga, Sao Paulo, SP, Brasil

Energy Technology Data Exchange (ETDEWEB)

Guimaraes, Guilherme Moura

2011-07-01

The Guarapiranga Reservoir, located in Sao Paulo metropolitan region, Brazil, is responsible for supplying about 20% of the entire population's water needs of this region or approximately 3.7 million people. However, this system has shown significant degradation in water quality, due to untreated domestic sewage and industrial effluents. In this study sediment samples were collected at five points along the reservoir and total concentration of some major (Fe, K and Na), trace (As, Ba, Br, Co, Cr, Cs, Hf, Hg, Rb, Sb, Sc, Ta, Tb, Th, U, V and Zn) and rare earth (Ce, Eu, La, Lu, Nd, Sm, Tb and Yb) elements were determined by instrumental neutron activation analysis (INAA). By inductively coupled plasma optical emission spectrometry (ICP OES) the concentrations of Al, Ba, Be, Ca, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, Pb, Ti, V e Zn were determined after digestion procedure following US EPA 3051 methodology. The concentrations of metals Cd and Pb were determined by graphite furnace atomic absorption spectrometry (GFAAS) and total Hg by cold vapor atomic absorption spectrometry (CVAAS). Methodology validation according to precision and accuracy was performed by reference materials analyses for the three different analytical techniques used. Multielemental results obtained by INAA were compared to NASC (North American Shale Composite), Upper Continental Crust (UCC) and soil from Guarapiranga park values. The Enrichment Factor (EF) and Geo accumulation Index (Igeo) were also evaluated for these data. Metal concentration results by ICP OES and AAS in the samples were compared to the TEL and PEL oriented values established by the Canadian Council of Ministers of the Environment and also adopted by CETESB (Environmental Protection Agency of the Sao Paulo State). The results were also compared to regional reference values (VRR) of limnic sediments from the Alto Tiete Basin. From these data an assessment of metal and trace element accumulated in the sediments from the

Metal and trace element sediment assessment from Guarapiranga reservoir, Alto Tiete Basin, Sao Paulo, SP, Brazil

International Nuclear Information System (INIS)

Guimaraes, Guilherme Moura

2011-01-01

The Guarapiranga Reservoir, located in Sao Paulo metropolitan region, Brazil, is responsible for supplying about 20% of the entire population's water needs of this region or approximately 3.7 million people. However, this system has shown significant degradation in water quality, due to untreated domestic sewage and industrial effluents. In this study sediment samples were collected at five points along the reservoir and total concentration of some major (Fe, K and Na), trace (As, Ba, Br, Co, Cr, Cs, Hf, Hg, Rb, Sb, Sc, Ta, Tb, Th, U, V and Zn) and rare earth (Ce, Eu, La, Lu, Nd, Sm, Tb and Yb) elements were determined by instrumental neutron activation analysis (INAA). By inductively coupled plasma optical emission spectrometry (ICP OES) the concentrations of Al, Ba, Be, Ca, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, Pb, Ti, V e Zn were determined after digestion procedure following US EPA 3051 methodology. The concentrations of metals Cd and Pb were determined by graphite furnace atomic absorption spectrometry (GFAAS) and total Hg by cold vapor atomic absorption spectrometry (CVAAS). Methodology validation according to precision and accuracy was performed by reference materials analyses for the three different analytical techniques used. Multielemental results obtained by INAA were compared to NASC (North American Shale Composite), Upper Continental Crust (UCC) and soil from Guarapiranga park values. The Enrichment Factor (EF) and Geo accumulation Index (Igeo) were also evaluated for these data. Metal concentration results by ICP OES and AAS in the samples were compared to the TEL and PEL oriented values established by the Canadian Council of Ministers of the Environment and also adopted by CETESB (Environmental Protection Agency of the Sao Paulo State). The results were also compared to regional reference values (VRR) of limnic sediments from the Alto Tiete Basin. From these data an assessment of metal and trace element accumulated in the sediments from the

Metal and trace element sediment assessment from Guarapiranga reservoir, Alto Tiete Basin, Sao Paulo, SP, Brazil; Avaliacao da concentracao de metais e elementos traco em amostras de sedimento do reservatorio Guarapiranga, Sao Paulo, SP, Brasil

Energy Technology Data Exchange (ETDEWEB)

Guimaraes, Guilherme Moura

2011-07-01

The Guarapiranga Reservoir, located in Sao Paulo metropolitan region, Brazil, is responsible for supplying about 20% of the entire population's water needs of this region or approximately 3.7 million people. However, this system has shown significant degradation in water quality, due to untreated domestic sewage and industrial effluents. In this study sediment samples were collected at five points along the reservoir and total concentration of some major (Fe, K and Na), trace (As, Ba, Br, Co, Cr, Cs, Hf, Hg, Rb, Sb, Sc, Ta, Tb, Th, U, V and Zn) and rare earth (Ce, Eu, La, Lu, Nd, Sm, Tb and Yb) elements were determined by instrumental neutron activation analysis (INAA). By inductively coupled plasma optical emission spectrometry (ICP OES) the concentrations of Al, Ba, Be, Ca, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, Pb, Ti, V e Zn were determined after digestion procedure following US EPA 3051 methodology. The concentrations of metals Cd and Pb were determined by graphite furnace atomic absorption spectrometry (GFAAS) and total Hg by cold vapor atomic absorption spectrometry (CVAAS). Methodology validation according to precision and accuracy was performed by reference materials analyses for the three different analytical techniques used. Multielemental results obtained by INAA were compared to NASC (North American Shale Composite), Upper Continental Crust (UCC) and soil from Guarapiranga park values. The Enrichment Factor (EF) and Geo accumulation Index (Igeo) were also evaluated for these data. Metal concentration results by ICP OES and AAS in the samples were compared to the TEL and PEL oriented values established by the Canadian Council of Ministers of the Environment and also adopted by CETESB (Environmental Protection Agency of the Sao Paulo State). The results were also compared to regional reference values (VRR) of limnic sediments from the Alto Tiete Basin. From these data an assessment of metal and trace element accumulated in the sediments from the

Removal of Uranium from Aqueous Solutions using Ammonium ...

African Journals Online (AJOL)

NICOLAAS

content was determined by Inductively Coupled Plasma Optical Emission Specroscopy (ICP-OES). The removal of uranium ... systems and may influence the surface properties of such adsorbents. .... The high silica content of the natural zeolite makes it more ..... average drop of 24.94 %) due to competition for binding sites.

Detection and characterisation of aluminium-containing nanoparticles in Chinese noodles by single particle ICP-MS.

Science.gov (United States)

Loeschner, Katrin; Correia, Manuel; López Chaves, Carlos; Rokkjær, Inge; Sloth, Jens J

2018-01-01

This study investigated Chinese noodles for the presence of aluminium-containing nanoparticles by using inductively coupled plasma mass spectrometry in single particle mode (spICP-MS) after enzymatic digestion by α-amylase. The aluminium concentrations in the noodle samples, determined by conventional ICP-MS without or with the use of hydrofluoric acid for digestion, were 5.4 ± 1.9 µg/g and 10.1 ± 2.2 µg/g (N = 21), respectively. Aluminium-containing nanoparticles were detected by spICP-MS in all 21 samples. Depending on the assumed particle composition, Al 2 O 3 or Al 2 O 3 ∙2SiO 2 ∙2H 2 O, the median particle diameters were either below or above 100 nm, respectively. The minimum detectable particle diameter by spICP-MS was between 54 and 83 nm. The mass recovery of aluminium in the form of particles was between 5% and 18%. The presented work reports for the first time the detection of Al-containing particles in food by spICP-MS.

PIXE analysis of human stones: comparison with data from ICP-AES

International Nuclear Information System (INIS)

Pougnet, M.A.B.; Peisach, M.; Pineda, C.A.; Rodgers, A.L.

1987-01-01

25 human stone samples previously analyzed by inductively coupled plasma atomic emission spectroscopy (ICP-AES) and the IAEA Animal Bone Standard Reference Material were used to evaluate trace element analysis by PIXE. Bombardment with 4 MeV protons was used for the determination of Mn, Fe, Cu, Pb, Br, Rb, Sr and Ca. PIXE and ICP-AES data gave correlation factors better than 0.97 for the elements Ca, Fe, Zn, Sr and Pb. (author) 9 refs.; 5 figs

ICP-MS and elemental tags for the life sciences

Energy Technology Data Exchange (ETDEWEB)

Giesen, Charlotte

2012-08-07

Inductively coupled plasma mass spectrometry (ICP-MS) has been applied for the analysis of biomolecules due to its high sensitivity, wide linear dynamic range, and multielement capabilities. However, outside the elemental MS community the potential of this technique, e.g. for life sciences applications, is not yet fully exploited. Thus, the development of ICP-MS-based (immuno) assays for a wide range of medical (cancer diagnostics, cisplatin toxicity studies), biochemical (DNA microarray, single cell analysis), and environmental (analysis of comestible goods) applications was accomplished by utilization of chemical labels. Laser ablation (LA)-ICP-MS was employed for the direct analysis of solid samples like microarrays and thin tissue sections. An immunoassay was developed for ochratoxin A (OTA) determination in wine, and ICP-MS detection was compared to conventional photometry by gold nanoparticle tagging and horseradish peroxidase, respectively. Detection limits of the assay were optimized to 0.003 {mu}g L{sup -1}, and the quantification range was 0.01-1 {mu}g L{sup -1} for both methods. For LA-ICP-MS-based DNA microarray detection, gold nanoparticle tags were specifically introduced via a streptavidin-biotin linkage. In immunohistochemistry (IHC), up to 20 tumor markers are routinely evaluated for one patient and thus, a common analysis results in a series of time consuming staining procedures. Hence, LA-ICP-MS was elaborated as a detection tool for a novel, multiplexed IHC analysis of tissue sections. Different lanthanides were employed for the simultaneous detection of up to three tumor markers (Her 2, CK 7, and MUC 1) in a breast cancer tissue. Additionally, iodine was employed as a labeling reagent, and a new LA-ICP-MS method for single cell and cell nucleus imaging was developed at 4 {mu}m laser spot size. Iodine was also applied as a new internal standard for tissue samples. Moreover, Pt-protein complexes separated by an optimized 1D and 2D gel

Fully automated gamma spectrometry gauge observing possible radioactive contamination of melting-shop samples

International Nuclear Information System (INIS)

Kroos, J.; Westkaemper, G.; Stein, J.

1999-01-01

At Salzgitter AG, several monitoring systems have been installed to check the scrap transport by rail and by car. At the moment, the scrap transport by ship is reloaded onto wagons for monitoring afterwards. In the future, a detection system will be mounted onto a crane for a direct check on scrap upon the departure of ship. Furthermore, at Salzgitter AG Central Chemical Laboratory, a fully automated gamma spectrometry gauge is installed in order to observe a possible radioactive contamination of the products. The gamma spectrometer is integrated into the automated OE spectrometry line for testing melting shop samples after performing the OE spectrometry. With this technique the specific activity of selected nuclides and dose rate will be determined. The activity observation is part of the release procedure. The corresponding measurement data are stored in a database for quality management reasons. (author)

ICP-MS: suitable method to study the metals distribution in estuarine regions; ICP-MS metodo adequado para o estudo da distribuicao de metais em regioes estuarinas

Energy Technology Data Exchange (ETDEWEB)

Vasconcelos, Danilo C.; Oliveira, Arno H. [Minas Gerais Univ., Belo Horizonte, MG (Brazil). Dept. de Engenharia Nuclear]. E-mail: danilochagas@yahoo.com.br; heeren@nuclear.ufmg.br; Santos, Silvio J. dos; Brito, Veronica F.O.; Severo, Maria Isabel G. [Universidade Estadual de Santa Cruz, Ilheus, BA (Brazil). Dept. de Ciencias Biologicas

2005-07-01

Anthropogenic inputs of pollutants such as heavy metals into the marine environment have increased their levels to large extents within past a few decades. These pollutants tend to accumulate in the bottom sediments. As a result, ecosystems such as seaports or other industrialized coastal areas that have chronic inputs of metals have highly contaminated sediments. This characteristic has led to concerns over the ecological effects that may be associated with sediment quality. Of particular concern are toxic effects and the potential for bioaccumulation of metals in biota exposed to the sediments. The bivalves Crassostrea rhizophorae, Lucina pectinata and Mytella falcata have been used as biomonitors of trace metal contamination in two estuaries from Ilheus city, Bahia state, in Brazil. Bivalves, sediment and water samples were collected in March 2004 in Acuipe and Rio do Engenho mangroves. The proposed technique to analyze the studied matrices was the inductively coupled plasma mass spectrometry (ICP-MS). The results suggested that the studied molluscs are bioaccumulators of metals and showed the Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) as an adequate technique to determine a large range of inorganic elements, because its high sensibility and low detection limits. (author)

Atomic fluorescence spectrometry with the inductively coupled plasma

International Nuclear Information System (INIS)

Omenetto, N.; Winefordner, J.D.

1987-01-01

Atomic fluorescence spectrometry (AFS) is based on the radiational activation of atoms and ions produced in a suitable atomizer (ionizer) and the subsequent measurement of the resulting radiational deactivation, called fluorescence. Atomic fluorescence spectrometry has been of considerable interest to researchers in atomic spectrometry because of its use for both analytical and diagnostic purposes. Unfortunately, the analytical applications of AFS have suffered from the lack of commercial instrumentation until the recent marketing of the Baird multiple-element, hollow cathode lamp-excited inductively coupled plasma system. This chapter is concerned strictly with the use of the inductively coupled plasma (ICP) as a cell and as a source for AFS. Many of the major references concerning the ICP in analytical AFS are categorized in Table 9.1, along with several reviews and diagnostical studies. For more detailed discussions of the fundamental aspects of AFS, the reader is referred to previous reviews

A novel quantification strategy of transferrin and albumin in human serum by species-unspecific isotope dilution laser ablation inductively coupled plasma mass spectrometry (ICP-MS)

Energy Technology Data Exchange (ETDEWEB)

Feng, Liuxing, E-mail: fenglx@nim.ac.cn; Zhang, Dan; Wang, Jun; Shen, Dairui; Li, Hongmei

2015-07-16

Highlights: • Species-unspecific ID-PAGE-LA-ICP-MS was used to quantify Alb and Tf in human serum. • Addition methods of species-unspecific {sup 34}S spike were evaluated. • Isotope change conditions were investigated to reach satisfactory “isotope equilibration”. • Human serum CRM (ERM-DA470k/IFCC) was used to validate the new arrangements. • The developed method offers potential for accurate quantification of protein by ID-PAGE-LA-ICP-MS. - Abstract: Species-specific (SS) isotope dilution analysis with gel electrophoresis (GE)-laser ablation (LA)-ICP-MS is a promising technique for the quantification of particular metal-binding proteins in biological samples. However, unavailable isotopically enriched spike and metal losses in GE separation are main limitations for SS-isotope dilution PAGE-LA-ICP-MS. In this study, we report for the first time the absolute quantification of transferrin (Tf) and albumin (Alb) in human serum by non-denaturing (native) GE combined with species-unspecific isotope dilution mass spectrometry (IDMS). In order to achieve a homogeneous distribution of both protein and isotope-enriched spike (simulated isotope equilibration), immersing the protein strips with {sup 34}S spike solution after gel electrophoresis was demonstrated to be an effective way of spike addition. Furthermore, effects of immersion time and {sup 34}S spike concentration were investigated to obtain optimal conditions of the post-electrophoresis isotope dilution method. The relative mass of spike and ablated sample (m{sub sp}/m{sub sam}) in IDMS equation was calculated by standard Tf and Alb proteins, which could be applied to the quantification of Tf and Alb in ERM-DA470k/IFCC for method confirmation. The results were in agreement with the certified value with good precision and small uncertainty (1.5–3%). In this method, species-specific spike protein is not necessary and the integrity of the heteroatom-protein could be maintained in sample preparation

A novel quantification strategy of transferrin and albumin in human serum by species-unspecific isotope dilution laser ablation inductively coupled plasma mass spectrometry (ICP-MS)

International Nuclear Information System (INIS)

Feng, Liuxing; Zhang, Dan; Wang, Jun; Shen, Dairui; Li, Hongmei

2015-01-01

Highlights: • Species-unspecific ID-PAGE-LA-ICP-MS was used to quantify Alb and Tf in human serum. • Addition methods of species-unspecific 34 S spike were evaluated. • Isotope change conditions were investigated to reach satisfactory “isotope equilibration”. • Human serum CRM (ERM-DA470k/IFCC) was used to validate the new arrangements. • The developed method offers potential for accurate quantification of protein by ID-PAGE-LA-ICP-MS. - Abstract: Species-specific (SS) isotope dilution analysis with gel electrophoresis (GE)-laser ablation (LA)-ICP-MS is a promising technique for the quantification of particular metal-binding proteins in biological samples. However, unavailable isotopically enriched spike and metal losses in GE separation are main limitations for SS-isotope dilution PAGE-LA-ICP-MS. In this study, we report for the first time the absolute quantification of transferrin (Tf) and albumin (Alb) in human serum by non-denaturing (native) GE combined with species-unspecific isotope dilution mass spectrometry (IDMS). In order to achieve a homogeneous distribution of both protein and isotope-enriched spike (simulated isotope equilibration), immersing the protein strips with 34 S spike solution after gel electrophoresis was demonstrated to be an effective way of spike addition. Furthermore, effects of immersion time and 34 S spike concentration were investigated to obtain optimal conditions of the post-electrophoresis isotope dilution method. The relative mass of spike and ablated sample (m sp /m sam ) in IDMS equation was calculated by standard Tf and Alb proteins, which could be applied to the quantification of Tf and Alb in ERM-DA470k/IFCC for method confirmation. The results were in agreement with the certified value with good precision and small uncertainty (1.5–3%). In this method, species-specific spike protein is not necessary and the integrity of the heteroatom-protein could be maintained in sample preparation process. Moreover, the

Determination of phosphorus in small amounts of protein samples by ICP-MS.

Science.gov (United States)

Becker, J Sabine; Boulyga, Sergei F; Pickhardt, Carola; Becker, J; Buddrus, Stefan; Przybylski, Michael

2003-02-01

Inductively coupled plasma mass spectrometry (ICP-MS) is used for phosphorus determination in protein samples. A small amount of solid protein sample (down to 1 micro g) or digest (1-10 micro L) protein solution was denatured in nitric acid and hydrogen peroxide by closed-microvessel microwave digestion. Phosphorus determination was performed with an optimized analytical method using a double-focusing sector field inductively coupled plasma mass spectrometer (ICP-SFMS) and quadrupole-based ICP-MS (ICP-QMS). For quality control of phosphorus determination a certified reference material (CRM), single cell proteins (BCR 273) with a high phosphorus content of 26.8+/-0.4 mg g(-1), was analyzed. For studies on phosphorus determination in proteins while reducing the sample amount as low as possible the homogeneity of CRM BCR 273 was investigated. Relative standard deviation and measurement accuracy in ICP-QMS was within 2%, 3.5%, 11% and 12% when using CRM BCR 273 sample weights of 40 mg, 5 mg, 1 mg and 0.3 mg, respectively. The lowest possible sample weight for an accurate phosphorus analysis in protein samples by ICP-MS is discussed. The analytical method developed was applied for the analysis of homogeneous protein samples in very low amounts [1-100 micro g of solid protein sample, e.g. beta-casein or down to 1 micro L of protein or digest in solution (e.g., tau protein)]. A further reduction of the diluted protein solution volume was achieved by the application of flow injection in ICP-SFMS, which is discussed with reference to real protein digests after protein separation using 2D gel electrophoresis.The detection limits for phosphorus in biological samples were determined by ICP-SFMS down to the ng g(-1) level. The present work discusses the figure of merit for the determination of phosphorus in a small amount of protein sample with ICP-SFMS in comparison to ICP-QMS.

Exploiting dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS) for sequential determination of trace elements in blood using a dilute-and-shoot procedure

International Nuclear Information System (INIS)

Lemos Batista, Bruno; Lisboa Rodrigues, Jairo; Andrade Nunes, Juliana; Oliveira Souza, Vanessa Cristina de; Barbosa, Fernando

2009-01-01

Inductively coupled plasma mass spectrometry with quadrupole (q-ICP-MS) and dynamic reaction cell (DRC-ICP-MS) were evaluated for sequential determination of As, Cd, Co, Cr, Cu, Mn, Pb, Se, Tl, V and Zn in blood. The method requires as little as 100 μL of blood. Prior to analysis, samples (100 μL) were diluted 1:50 in a solution containing 0.01% (v/v) Triton X-100 and 0.5% (v/v) nitric acid. The use of the DRC was only mandatory for Cr, Cu, V and Zn. For the other elements the equipment may be operated in a standard mode (q-ICP-MS). Ammonia was used as reaction gas. Selection of best flow rate of ammonium gas and optimization of the quadrupole dynamic band-pass tuning parameter (RPq) were carried out, using a ovine base blood for Cr and V and a synthetic matrix solution (SMS) for Zn and Cu diluted 1:50 and spiked to contain 1 μg L -1 of each element. Method detection limits (3 s) for 75 As, 114 Cd, 59 Co, 51 Cr, 63 Cu 55 Mn, 208 Pb, 82 Se, 205 Tl, 51 V, and 64 Zn were 14.0, 3.0, 11.0, 7.0, 280, 9.0, 3.0, 264, 0.7, 6.0 and 800 ng L -1 , respectively. Method validation was accomplished by the analysis of blood Reference Materials produced by the L'Institut National de Sante Publique du Quebec (Canada).

Application of high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) for determination of chromium compounds in the air at the workplace.

Science.gov (United States)

Stanislawska, Magdalena; Janasik, Beata; Wasowicz, Wojciech

2013-12-15

The toxicity and bioavailability of chromium species are highly dependable on the form or species, therefore determination of total chromium is insufficient for a complete toxicological evaluation and risk assessment. An analytical method for determination of soluble and insoluble Cr (III) and Cr (VI) compounds in welding fume at workplace air has been developed. The total chromium (Cr) was determined by using quadruple inductively coupled plasma mass spectrometry (ICP-MS) equipped with a dynamic reaction cell (DRC(®)). Soluble trivalent and hexavalent chromium compounds were determined by high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). A high-speed, reversed-phase CR C8 column (PerkinElmer, Inc., Shelton, CT, USA) was used for the speciation of soluble Cr (III) and soluble Cr (VI). The separation was accomplished by interaction of the chromium species with the different components of the mobile phase. Cr (III) formed a complex with EDTA, i.e. retained on the column, while Cr (VI) existed in the solutions as dichromate. Alkaline extraction (2% KOH and 3% Na2CO3) and anion exchange column (PRP-X100, PEEK, Hamilton) were used for the separation of the total Cr (VI). The results of the determination of Cr (VI) were confirmed by the analysis of the certified reference material BCR CRM 545 (Cr (VI) in welding dust). The results obtained for the certified material (40.2±0.6 g kg(-1)) and the values recorded in the examined samples (40.7±0.6 g kg(-1)) were highly consistent. This analytical method was applied for the determination of chromium in the samples in the workplace air collected onto glass (Whatman, Ø 37 mm) and membrane filters (Sartorius, 0.8 μm, Ø 37 mm). High performance liquid chromatography with inductively coupled plasma mass spectrometry is a remarkably powerful and versatile technique for determination of chromium species in welding fume at workplace air. Crown Copyright © 2013 Published by

Standard practice for analysis of aqueous leachates from nuclear waste materials using inductively coupled plasma-atomic emission spectrometry

CERN Document Server

American Society for Testing and Materials. Philadelphia

2010-01-01

1.1 This practice is applicable to the determination of low concentration and trace elements in aqueous leachate solutions produced by the leaching of nuclear waste materials, using inductively coupled plasma-atomic emission spectroscopy (ICP-AES). 1.2 The nuclear waste material may be a simulated (non-radioactive) solid waste form or an actual solid radioactive waste material. 1.3 The leachate may be deionized water or any natural or simulated leachate solution containing less than 1 % total dissolved solids. 1.4 This practice should be used by analysts experienced in the use of ICP-AES, the interpretation of spectral and non-spectral interferences, and procedures for their correction. 1.5 No detailed operating instructions are provided because of differences among various makes and models of suitable ICP-AES instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument. This test method does not address comparative accuracy of different devices...

Isotopic analysis of calcium in blood plasma and bone from mouse samples by multiple collector-ICP-mass spectrometry

International Nuclear Information System (INIS)

Hirata, Takafumi; Tanoshima, Mina; Suga, Akinobu; Tanaka, Yu-ki; Nagata, Yuichi; Shinohara, Atsuko; Chiba, Momoko

2008-01-01

The biological processing of Ca produces significant stable isotope fractionation. The level of isotopic fractionation can provide key information about the variation in dietary consumption or Ca metabolism. To investigate this, we measured the 43 Ca/ 42 Ca and 44 Ca/ 42 Ca ratios for bone and blood plasma samples collected from mice of various ages using multiple collector-ICP-mass spectrometry (MC-ICP-MS). The 44 Ca/ 42 Ca ratio in bones was significantly (0.44 - 0.84 per mille) lower than the corresponding ratios in the diet, suggesting that Ca was isotopically fractionated during Ca metabolism for bone formation. The resulting 44 Ca/ 42 Ca ratios for blood plasma showed almost identical, or slightly higher, values (0.03 - 0.2 per mille) than found in a corresponding diet. This indicates that a significant amount of Ca in the blood plasma was from dietary sources. Unlike that discovered for Fe, there were not significant differences in the measured 44 Ca/ 42 Ca ratios between female and male specimens (for either bone or blood plasma samples). Similarity, the 44 Ca/ 42 Ca ratios suggests that there were no significant differences in Ca dietary consumption or Ca metabolism between female and male specimens. In contrast, the 44 Ca/ 42 Ca ratios of blood plasma from mother mice during the lactation period were significantly higher than those for all other adult specimens. This suggests that Ca supplied to infants through lactation was isotopically lighter, and the preferential supply of isotropically lighter Ca resulted in isotopically heavier Ca in blood plasma of mother mice during the lactation period. The data obtained here clearly demonstrate that the Ca isotopic ratio has a potential to become a new tool for evaluating changes in dietary consumption, or Ca metabolism of animals. (author)

The use of inductively coupled plasma mass spectrometry (ICP-MS) for the determination of toxic and essential elements in different types of food samples

Science.gov (United States)

Voica, C.; Dehelean, A.; Kovacs, M. H.

2012-02-01

Food is the primary source of essential elements for humans and it is an important source of exposure to toxic elements. In this context, levels of essential and toxic elements must be determined routinely in consumed food products. The content of trace elements (As, Pb, Cu, Cd, Zn, Sn, Hg) in different types of food samples (e.g. rice, bread, sugar, cheese, milk, butter, wheat, coffee, chocolate, biscuits pasta, etc.) was determined, using inductively coupled plasma mass spectrometry (ICP-MS). Trace element contents in some foods were higher than maximum permissible levels of toxic metals in human food (Cd in bread, Zn in cheese, Cu in coffee, Hg in carrots and peppers).

Characterization of PCBs from computers and mobile phones, and the proposal of newly developed materials for substitution of gold, lead and arsenic.

Science.gov (United States)

Dervišević, Irma; Minić, Duško; Kamberović, Željko; Ćosović, Vladan; Ristić, Mirjana

2013-06-01

In this paper, we have analyzed parts of printed circuit board (PCB) and liquid crystal display (LCD) screens of mobile phones and computers, quantitative and qualitative chemical compositions of individual components, and complete PCBs were determined. Differential thermal analysis (DTA) and differential scanning calorimetry (DSC) methods were used to determine the temperatures of phase transformations, whereas qualitative and quantitative compositions of the samples were determined by X-ray fluorescence spectrometry (XRF), inductively coupled plasma optical emission spectrometry (ICP-OES), and scanning electron microscopy (SEM)-energy dispersive X-ray spectrometry (EDS) analyses. The microstructure of samples was studied by optical microscopy. Based on results of the analysis, a procedure for recycling PCBs is proposed. The emphasis was on the effects that can be achieved in the recycling process by extraction of some parts before the melting process. In addition, newly developed materials can be an adequate substitute for some of the dangerous and harmful materials, such as lead and arsenic are proposed, which is in accordance with the European Union (EU) Restriction of the use of certain hazardous substances (RoHS) directive as well as some alternative materials for use in the electronics industry instead of gold and gold alloys.

Polonium (²¹⁰Po), uranium (²³⁴U, ²³⁸U) isotopes and trace metals in mosses from Sobieszewo Island, northern Poland.

Science.gov (United States)

Boryło, Alicja; Nowicki, Waldemar; Olszewski, Grzegorz; Skwarzec, Bogdan

2012-01-01

The activity of polonium (210)Po and uranium (234)U, (238)U radionuclides, as well as trace metals in mosses, collected from Sobieszewo Island area (northern Poland), were determined using the alpha spectrometry, AAS (atomic absorption spectrometry) and OES-ICP (atomic emission spectrometry with inductively coupled plasma). The concentrations of mercury (directly from the solid sample) were determined by the cold vapor technique of CV AAS. The obtained results revealed that the concentrations of (210)Po, (234)U, and (238)U in the two analyzed kinds of mosses: schrebers big red stem moss (Pleurozium schreberi) and broom moss (Dicranum scoparium) were similar. The higher polonium concentrations were found in broom moss (Dicranum scoparium), but uranium concentrations were relatively low for both species of analyzed mosses. Among the analyzed trace metals the highest concentration in mosses was recorded for iron, while the lowest for nickel, cadmium and mercury. The obtained studies showed that the sources of polonium and uranium isotopes, as well as trace metals in analyzed mosses are air city contaminations transported from Gdańsk and from existing in the vicinity the phosphogypsum waste heap in Wiślinka (near Gdańsk).

Ultra-sensitive radionuclide spectrometry. Radiometrics and mass spectrometry synergy

International Nuclear Information System (INIS)

Povinec, P.P.

2005-01-01

Recent developments in radiometrics and mass spectrometry techniques for ultra-sensitive analysis of radionuclides in the marine environment are reviewed. In the radiometrics sector the dominant development has been the utilization of large HPGe detectors in underground laboratories with anti-cosmic or anti-Compton shielding for the analysis of short and medium-lived radionuclides in the environment. In the mass spectrometry sector, applications of inductively coupled plasma mass spectrometry (ICP-MS) and accelerator mass spectrometry (AMS) for the analysis of long-lived radionuclides in the environment are the most important recent achievements. The recent developments do not only considerably decrease the detection limits for several radionuclides (up to several orders of magnitude), but they also enable to decrease sample volumes so that sampling, e.g., of the water column can be much easier and more effective. A comparison of radiometrics and mass spectrometry results for the analysis of radionuclides in the marine environment shows a reasonable agreement - within quoted uncertainties, for wide range of activities and different sample matrices analyzed. (author)

Analysis of iron-base alloys by low-wattage glow discharge emission spectrometry

International Nuclear Information System (INIS)

Wagatsuma, K.; Hirokawa, K.

1984-01-01

Several iron-base alloys were investigated by low-wattage glow discharge emission spectrometry. The emission intensity principally depended on the sputtering parameters of constituent elements in the alloy. However, in the case of chromium, stable and firm oxides formed on the surface influencing the yield of ejected atoms. This paper discusses the relation between the sputtering parameters in Fe-Ni, Fe-Cr, and Fe-Co alloys and their relative emission intensities. Additionally, quantitative analysis was performed for some ternary iron-base alloys and commercial stainless steels with the calibration factors of binary alloy systems

Measurement of isotopic composition of lanthanides in reprocessing process solutions by high-performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC/ICP-MS)

International Nuclear Information System (INIS)

Okano, Masanori; Jitsukata, Shu; Kuno, Takehiko; Yamada, Keiji

2011-01-01

Isotopic compositions of fission products in process solutions and wastes in a reprocessing plant are valuable to proceed safety study of the solutions and research/development concerning treatment/disposal of the wastes. The amount of neodymium-148 is a reliable indication to evaluate irradiation history. The isotopic compositions of samarium and gadolinium in high radioactive wastes are referred to as essential data to evaluate environmental impact in geological repositories. However, pretreatment of analysis must be done with complicated chemical separation such as solvent extraction and ion exchange. The actual measurement data of isotopic compositions of lanthanides comparable to the one of actinides in spent fuel reprocessing process has not been obtained enough. Rapid and high sensitive analytical technique based on high-performance liquid chromatography (HPLC) with an inductively coupled plasma mass spectrometry (ICP-MS) has been developed for the measurement of isotopic compositions of lanthanides in spent fuel reprocessing solutions. HPLC/ICP-MS measurement system was customized for a glove-box to be applied to the radioactive solutions. The cation exchange chromatographic columns (Shim-pack IC-C1) and injection valve (20μL) were located inside of the glove-box except the chromatographic pump. The elements of lanthanide group were separated by a gradient program of HPLC with α-hydroxyisobutyric acid. Isotopic compositions of lanthanides in eluate was sequentially analyzed by a quadruple ICP-MS. Optimization of parameter of HPLC and ICP-MS measurement system was examined with standard solutions containing 14 lanthanide elements. The elements of lanthanides were separated by HPLC and detected by ICP-MS within 25 minutes. The detection limits of Nd-146, Sm-147 and Gd-157 were 0.37 μg L -1 , 0.69 μg L -1 and 0.47 μg L -1 , respectively. The analytical precision of the above three isotopes was better than 10% for standard solutions of 100 μg L -1 with

ICP27-dependent resistance of herpes simplex virus type 1 to leptomycin B is associated with enhanced nuclear localization of ICP4 and ICP0

International Nuclear Information System (INIS)

Lengyel, Joy; Strain, Anna K.; Perkins, Keith D.; Rice, Stephen A.

2006-01-01

It was previously shown that herpes simplex virus type 1 (HSV-1) is sensitive to leptomycin B (LMB), an inhibitor of nuclear export factor CRM1, and that a single methionine to threonine change at residue 50 (M50T) of viral immediate-early (IE) protein ICP27 can confer LMB resistance. In this work, we show that deletion of residues 21-63 from ICP27 can also confer LMB resistance. We further show that neither the M50T mutation nor the presence of LMB affects the nuclear shuttling activity of ICP27, suggesting that another function of ICP27 determines LMB resistance. A possible clue to this function emerged when it was discovered that LMB treatment of HSV-1-infected cells dramatically enhances the cytoplasmic accumulation of two other IE proteins, ICP0 and ICP4. This effect is completely dependent on ICP27 and is reversed in cells infected with LMB-resistant mutants. Moreover, LMB-resistant mutations in ICP27 enhance the nuclear localization of ICP0 and ICP4 even in the absence of LMB, and this effect can be discerned in transfected cells. Thus, the same amino (N)-terminal region of ICP27 that determines sensitivity to LMB also enhances ICP27's previously documented ability to promote the cytoplasmic accumulation of ICP4 and ICP0. We speculate that ICP27's effects on ICP4 and ICP0 may contribute to HSV-1 LMB sensitivity