Estimation of Uncertainty Budgets in Analysis of Nickel by ICP-MS and High-Resolution Mass Spectrometry with a Glow Discharge

Moscow University Chemistry Bulletin - This paper estimates uncertainty budgets in determining the content of impurities of 15 elements (P, Mn, Fe, Cu, Zn, As, Se, Ag, Cd, Sn, Sb, Te, Tl, Pb, Bi)...     

The certification of the contents of Cd, Co, Cu, Fe, Hg, Ni, Pb, Zn, Sb, Se, Tl and Cr in a city waste incineration ash

Summary The analysis of ashes being of increasing importance, a reference material was prepared from fly ash of a city waste incinerator. The procedures of preparation, homogeneity and stability testing are described as well as the way of certification of elements of major importance: Cd, Co, Cr, Cu, Fe, Hg, Ni, Pb, Zn, Sb, Se and Tl.

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Zertifizierung der Gehalte an Cd, Co, Cu, Fe, Hg, Ni, Pb, Zn, Sb, Se, Tl und Cr in einer Stadtmüll-Verbrennungsasche

Zusammenfassung Da die Analyse von Aschen zunehmend an Bedeutung gewinnt, wurde von der Flugasche einer Stadtmüll-Verbrennungsanlage ein Referenzmaterial hergestellt. Die Methoden der Herstellung sowie der Homogenitätsund Stabilitätsprüfung werden beschrieben und die Art der Zertifizierung der Elemente von hauptsächlicher Bedeutung aufgezeigt (Cd, Co, Cr, Cu, Fe, Hg, Ni, Pb, Zn, Sb, Se, Tl).

     

Evaluation of a tungsten coil atomization-laser-induced fluorescence detection approach for trace elemental analysis

The analytical utility of a tungsten (W)-coil atomization-laser-induced fluorescence (LIF) approach has been evaluated for trace level measurements of elemental chromium (Cr), arsenic (As), selenium (Se), antimony (Sb), lead (Pb), tin (Sn), copper (Cu), thallium (Tl), indium (In), cadmium (Cd), zinc (Zn) and mercury (Hg). Measurements of As, Cr, In, Se, Sb, Pb, Tl, and Sn were performed by laser-induced fluorescence using a single dye laser operating near 460 nm whose output was converted by frequency doubling and stimulated Raman scattering to wavelengths ranging from 196 to 286 nm for atomic excitation. Absolute limits of detection (LODs) of 1, 0.3, 0.3, 0.2, 1, 6, 1, 0.2 and 0.8 pg and concentration LODs of 100, 30, 30, 20, 100, 600, 100, 20, and 80 pg/mL were achieved for As, Se, Sb, Sn, In, Cu, Cr, Pb and Tl, respectively. Determinations of Hg, Pb, Zn and Cd were performed using two-color excitation approaches and resulted in absolute LODs of 2, 30, 5 and 0.6 pg, respectively, and concentration LODs of 200, 3000, 500 and 60 pg/mL, respectively. The sensitivities achieved by the W-coil LIF approaches compare well with those reported by W-coil atomic absorption spectrometry, graphite furnace atomic absorption spectrometry, and graphite furnace electrothermal atomization-LIF approaches. The accuracy of the approach was verified through the analysis of a multielement reference solution containing Sb, Pb and Tl which each had certified performance acceptance limits of 19.6-20.4 μg/mL. The determined concentrations were 20.05 ± 2.60, 20.70 ± 2.27 and 20.60 ± 2.46 μg/mL, for Sb, Pb and Tl, respectively. The results demonstrate that W-coil LIF provides good analytical performance for trace analyses due to its high sensitivity, linearity, and capability to measure multiple elements using a single tunable laser and suggest that the development of portable W-coil LIF instrumentation using compact, solid-state lasers is feasible.     

Polarographic determination of Pb, Tl, Bi and Sb in ethylenediamine in presence of mannitol

Summary Pb, Tl, Bi and Sb yield well defined polarograms in 1 M ethylenediamine in presence of 3% mannitol, with half-wave potentials at – 0.71 V, – 0.51 V, – 0.60 V and – 1.10 V, respectively. Only Pb and Tl develop maxima which can be suppressed by 0.02% gelatin. Presence of mannitol prevents the precipitation of Pb, Bi, and Sb in the alkaline solution. Simultaneous determinations of Pb/Tl, Bi/Sb, and Pb/Sb can be carried out.

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Polarographische Bestimmung von Pb, Tl, Bi und Sb in Äthylendiamin in Gegenwart von Mannit

Zusammenfassung Gut ausgebildete Polarogramme kann man von diesen Elementen in 1 M Äthylendiamin in Gegenwart von 3% Mannit erhalten. Die Halbstufenpotentiale liegen bei – 0,71 V (Pb), – 0,51 V (Tl), – 0,60 V (Bi) und – 1,10 V (Sb). Maxima, die im Falle von Pb und Tl gebildet werden, können durch 0,02% Gelatine unterdrückt werden. Durch Mannit wird die Fällung von Pb, Bi, und Sb in der alkalischen Lösung verhindert. Simultanbestimmungen von Pb/Tl, Bi/Sb und Pb/Sb sind möglich.

Our sincere thanks are due to Dr. G. B. Singh, Professor and Head, Department of Chemistry, B.H.U. for providing the necessary facilities.     

Determination of trace elements in coal and coal fly ash by joint-use of ICP-AES and atomic absorption spectrometry

Microwave-acid digestion (MW-AD) followed by inductively coupled plasma-atomic emission spectrometry (ICP-AES), graphite furnace atomic absorption spectrometry (GFAAS), and hydride generation atomic absorption spectrometry (HGAAS) were examined for the determination of various elements in coal and coal fly ash (CFA). Eight certified reference materials (four coal samples and four CFA samples) were tested. The 10 elements (As, Be, Cd, Co, Cr, Mn, Ni, Pb, Sb, and Se), which are described in the Clean Air Act Amendments (CAAA), were especially considered. For coal, the HF-free MW-AD followed by ICP-AES was successful in the determination of various elements except for As, Be, Cd, Sb, and Se. These elements (except for Sb) were well-determined by use of GFAAS (Be and Cd) and HGAAS (As and Se). For CFA, the addition of HF in the digestion acid mixture was needed for the determination of elements, except for As, Sb, and Se, for which the HF-free MW-AD was applicable. The use of GFAAS (Be and Cd) or HGAAS (Sb and Se) resulted in the successful determination of the elements for which ICP-AES did not work well. The protocol for the determination of the 10 elements in coal and CFA by MW-AD followed by the joint-use of ICP-AES, GFAAS, and HGAAS was established.     

Preconcentration of trace elements on a support impregnated with sodium diethyldithiocarbamate prior to their determination by inductively coupled plasma-atomic emission spectrometry

A procedure is developed for determination of As, Co, Se, Cr, Pb, Zn, Cu, Mn, Cd, Sb, and Sn in water by ICP-AES analysis of alcohol eluates after pre-concentration of the samples. The pre-concentration is performed on a sodium diethyldithiocarbamate supported soft polyurethane foam. The sorbed elements are subsequently eluted with 1-propanol and the alcohol eluates are analysed by ICP-AES. A eight-fold concentration is achieved. An increased sensitivity in the analysis of propanol-water (30:70, v/v) solution is established as compared with aqueous solutions. The strongest effect is observed for As, Se, Pb, Cr, Sn, and Cd-increasing is more than twice. For other elements the matrix influence is by a factor of 1.45 (Cu), 1.36 (Sb), 2.08 (Zn). The method is applied to the analysis of natural water samples.     

Preconcentration methods for the determination of trace elements in water by x-ray fluorescence spectrometry: Part 1. Response characteristics

Seven methods for the preconcentration of the elements Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Ag, Cd, Sb, Hg, Tl, and Pb in trace quantities from water have been evaluated. All the methods involved incorporation of the dissolved species into a solid resulting in large concentration factors and yielded samples well-suited to quantitation by either energy- or wavelength-dispersive x-ray fluorescence. On the basis of measurable criteria such as method sensitivity, linear range, and overall reproducibility, a scheme for ranking the seven methods is proposed. Application of such a rating scheme has enabled an objective, critical comparison of the available methods to be made on the basis of performance characteristics.     

植物类中药材及饮片中18种重金属及有害元素研究

建立植物类中药材及饮片中铅、镉、总砷、总汞、铜、锑、锡、铬、镍、钡、锰、铊、银、铍、镝、铝、硒、钼共18种重金属及有害元素含量的检测方法和限量。样品经微波消解处理后,采用电感耦合等离子体质谱法(ICP-MS)对100批植物类中药材中的重金属及有害元素进行测定和方法研究。各元素线性关系良好,相关系数(r)均大于0.999 5,方法检出限为0.000 22~0.023 0 mg/kg,回收率为90.2%~108.7%,相对标准偏差为1.8%~4.9%。该方法准确、简便、灵敏,可为植物类中药材中重金属及有害元素的检测与控制提供方法参考。     

The application of discontinuous,countercurrent, liquid-liquid extraction to the study of the distribution of metal ions between hydrochloric acid and methyl isobutyl ketone

Summary The extraction of the elements Ti, V, Cr, Mn, Fe, Co, Ni, Zn, Ga, As, Nb, Mo, Ru, Rh, Pd, Ag, Cd, In, Sn, Sb, La, W, Re, Os, Ir, Pt, Au, Hg, Tl, Pb and Bi from hydrochloric acid into methyl isobutyl ketone has been studied as a function of hydrochloric acid concentration. The results are presented in graphical form. The data were obtained by studying the distribution patterns of the elements after equilibration on a Craig countercurrent liquid-liquid extraction apparatus.

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Zusammenfassung Die Extraktion der Elemente Ti, V, Cr, Mn, Fe, Co, Ni, Zn, Ga, As, Nb, Mo, Ru, Rh, Pd, Ag, Cd, In, Sn, Sb, La, W, Re, Os, Ir, Pt, Au, Hg, Tl, Pb und Bi mit Methylisobutylketon aus salzsaurer Lösung als Funktion der Säurekonzentration wurde studiert. Die Ergebnisse wurden aus den Spitzen der Verteilungskurven nach Einstellung des Gleichgewichts in einem diskontinuierlichen Gegenstrom-flüssig-flüssig-Extraktionsapparat berechnet.

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Résumé On a étudié l'extraction des éléments Ti, V, Cr, Mn, Fe, Co, Ni, Zn, Ga, As, Nb, Mo, Ru, Rh, Pd, Ag, Cd, In, Sn, Sb, La, W, Re, Os, Ir, Pt, Au, Hg, Tl, Pb et Bi en solution chlorhydrique par la méthylisobutylcétone. On présente les résultats sous forme graphique. Les données ont été obtenues en étudiant les diagrammes de distribution des éléments après équilibrage sur un appareil Craig à extraction à contre-courant liquide-liquide.

     

乳化辅助微波消解-ICP-ORS-MS快速测定霜膏类化妆品中17种微量元素

采用乳化剂和硝酸体系微波消解样品,带八极杆碰撞/反应池(ORS)的电感耦合等离子体质谱(ICP-MS)法同时测定了霜膏类化妆品中铍、硼、铝、钛、铬、锌、砷、硒、银、镉、锡、锑、碘、钕、汞、铊和铅等17种微量元素.通过优化样品前处理和ICP-MS操作条件,降低了质谱干扰,各元素的检出限(3σ)在0.003 ～0.058 ...     

Determination of Se,Pb, and Sb by atomic fluorescence spectrometry using a new flameless,dielectric barrier discharge atomizer

A flameless atomizer for atomic fluorescence spectrometry (AFS), based on an atmospheric pressure dielectric barrier discharge, has been developed for the atomization of hydride-forming elements, such as Se, Sb and Pb. The atomizer (8 mm o.d, 35 mm length) was operated at a power less than 50 W. The discharge was sustained with argon at the flow rate of 0.85 L min^− 1 after optimization. The characteristics of the atomizer and the effects of different parameters (power, gas flow rate, and KBH₄ concentration) are investigated. The most attractive feature of this atomizer is its low operation temperature (~ 52 °C, detected at the outlet of the atomizer by a thermocouple), allowing both the radiation source and the detector to be placed in close proximity with the atomizer. The analytical performance of the atomizer has been evaluated, and detection limits for Se, Sb and Pb obtained with the present technique were 0.08, 0.11 and 0.27 μg L^− 1, respectively. The accuracy of the system was verified by the determination of Se, Sb and Pb in reference material of spinage GBW 10015. The concentrations of Se, Sb, and Pb determined by the present technique agreed well with the reference values (Se: 92 ± 24 mg kg^− 1, Sb: 43 ± 14 mg kg^− 1, Pb: 11.1 ± 0.9 mg kg^− 1). This detector is very promising for field elements detection with portable AFS.     

Arrangement of ad-atoms of various kinds on substrates: Part II. Iridium and rhodium

The number of iridium sites and that of rhodium sites occupied by a foreign atom was determined with the aid of the pulse technique. In the case of iridium the foreign atoms included are Cu, Ag, Cd, Hg, In, Tl, Pb, Se, Te, As and Bi. The approximate value is 1 for the first two, 2 for the next five and 2.5–2.7 for the others. In the case of rhodium substrate, the foreign atoms included are Cu, Ag, Cd, Hg, In, Tl, Ge, Pb, As, Sb, Se, Te, and Bi. The approximate value is 1 for the first two, 2 for the next six, 2.4–2.6 for the next four and 3.0 for the last one. Silver and copper ad-atoms are closely packed both on the iridium and rhodium surface, but the ad-atoms of the other elements are arranged on the surfaces leaving empty sites for geometrical reasons, even when the monolayer is apparently complete.     

微波消解-ICP-OES法测定汽车涂料中8种重金属

建立微波消解-电感耦合等离子体发射光谱(ICP-OES)测定汽车涂料中Pb,Cr,Se,Ba,Sb,As,Cd,Hg含量的方法。以HNO_3-H_2O_2(体积比为4∶1)混合酸消解样品,各元素分析谱线:Pb 220.353 nm,Cr 267.716 nm,Se196.090 nm,Ba 233.527 nm,Sb 217.581 nm,As 189.042 nm,Cd 228.802 nm,Hg 184.950 nm。8种元素测定结果的相对标准偏差为2.02%~12.94%(n=6);对白色、蓝色、红色汽车漆样品进行加标回收试验,Pb,Cr,Se,Ba,As,Cd,Hg,的加标回收率为81.26%~99.79%,Sb的回收率为62.43%~87.61%。该方法快速、简便,精密度、准确度较高,可用于汽车涂料中重金属含量的监控。     

Determination of traces of As,Cd, Cr,Hg, Mn,Ni, Sb,Se, Sn and Pb in human hair by triple quadrupole ICP-MS

With the wide range of metallic contaminants discharged in the environment, studying the human health requires a growing number of elements to be monitored in biological samples. Hair analysis has been suggested as a suitable tool for biomonitoring environmental and occupational exposure to toxic elements. This study describes a method for the determination of 10 trace elements in hair samples using ICP-QQQ-MS. Combining the power of the MS/MS high-energy Helium mode with the MS/MS O₂ mass-shift mode, the method offers great analytical performances with detection limits reaching 0.0014 µg g^?1 for As, 0.0016 µg g^?1 for Cd, 0.012 µg g^?1 for Cr, 0.0035 µg g^?1 for Hg, 0.0055 µg g^?1 for Mn, 0.10 µg g^?1 for Ni, 0.0012 µg g^?1 for Sb, 0.0083 µg g^?1 for Sn, 0.011 µg g^?1 for Se and Pb. The accuracy of the method was tested on a human hair ERM® certified reference material. Percent recoveries varied from 91.3% and 106.9% being always in the acceptance range of 90–110%. For all analysed elements, RSD% of repeatability ranged between 0.6% and 9.0% and those of intermediate precision did not exceed the limit of 20% being always lower than 10% (except for As). The proposed method was applied for the determination of trace elements in hair samples from 20 unexposed subjects. The geometric mean levels were as follows: Cr 0.28 µg g^?1, Mn 0.30 µg g^?1, Sn 1.04µg g^?1, Sb 0.07 µg g^?1, Hg 0.42 µg g^?1, As 0.02 µg g^?1, Cd 0.03 µg g^?1, Ni 0.51 µg g^?1, Se 0.45 µg g^?1 and Pb 1.83 µg g^?1. Element concentrations were in the same range with the reported data. The reported results may be useful for environmental exposure assessment or comparisons studies when establishing reference values of trace elements in exposed population.     

Assessment of trace elements characteristics and human health risk of exposure to ambient PM2.5 in Hangzhou,China

A method for simultaneously determining the trace elements in particulate matter (PM) (PM2.5) by inductively coupled plasma mass spectrometry was established. The PM2.5-loaded filter samples were digested under the optimised conditions including a mixture of HNO₃–HCl–HF with ultrasonication proceeding at 70°C for 2 h. Recoveries of 90.83–103.33% were achieved for 20 elements (Co, Sr, Ag, Cd, Sb, La, Ce, Sm, W etc.) in NIST standard reference material 1648a (urban PM). PM2.5 samples were collected at urban site in Hangzhou from August 2015 to November 2015. PM2.5 concentrations of 15% sampling days exceeded the daily limitation and the mean concentrations of PM2.5 from August to November reached the 66.4% of the limitation. PM2.5 concentrations in summer were higher than that in autumn. The concentration of Zn was highest, following with Al, Pb, Mn, Cu and As. Significant enrichment was observed in Mn, Zn, Pb, Ag, V, Ni, Cu, As, Se, Hg, Co, Cd and W, which was probably induced by vehicular exhaust, oil and residual fuel combustion and industrial emissions. The daily mass concentrations of PM2.5 and elements fluctuated significantly. Rainfall could significantly reduce the concentration of Ti, Mn, Cu, Zn, As, Se, Hg, Sr, Ag, Cd, Sb, La, Ce, Sm and Pb, and the risk levels of carcinogenic elements and non-carcinogenic elements in rain day were significantly lower (43.7–81.4%) than those in non-rain day. The risk levels of Co, Cd and As could lead to adverse health outcomes through the respiratory system, which should deserve more attention, while the risk levels of Ni and non-carcinogenic elements (Hg, Mn, Cu, Zn, Pb, V) were under average risk acceptance.     

A pilot study for the production of a certified reference material for trace elements in honey

In the context of the general mandate of the European Union Community Reference Laboratory (CRL) for residues in living animals and their products established at the Istituto Superiore di Sanità, a pilot study was undertaken to assess the possibility of producing a new certified reference material (CRM) for trace elements in a matrix of honey. The elements considered were As, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Sn, V and Zn. Their determination was performed by inductively coupled plasma (ICP)-based techniques. Data obtained with different ICP techniques were generally in good agreement. In light of these results, the next step was the effective production of a candidate CRM in a honey matrix. In the preliminary phase, two different types of honey, i.e., Eucalyptus (solid and sticky) and Robinia (viscous and sticky), were pretreated at the Institute for Reference Materials and Measurements, Joint Research Centre, European Commission (EC-JRC-IRMM) in order to produce the materials candidate for the certification process. Approximately 600 ampoules were thus produced for the Robinia honey and 450 ampoules for the Eucalyptus honey, each ampoule containing 5 g of an aqueous solution of honey (with 20% and 30% high purity water, respectively) and sealed under inert gas (Ar). A ring test to determine the levels of the chemical elements and a long-term study to evaluate the stability of the samples is in progress. Tentative figures for the analytes of interest are (in ng g⁻¹): Robinia, As, 1.28±0.09; Cd, 0.59±0.08; Cr, 2.36±0.21; Cu, 57.6±3.2; Fe, 209±9; Mn, 90.8±3; Ni, 18.1±0.6; Pb, 23±1.5; Sn, 8.10±0.35; V, 1.19±0.37; and Zn, 178±4; Eucalyptus, As, 3.18±0.21; Cd, 0.70±0.08; Cr, 2.73±0.22; Cu, 141±6; Fe, 926±16; Mn, 1905±81; Ni, 7.77±0.4; Pb, 138±4; Sn, 7.97±0.16; V, 3.47±0.15; and Zn, 405±9.     

Determination of trace elements in marine plankton by inductively coupled plasma mass spectrometry (ICP-MS)

A method has been developed for the determination of 23 elements in marine plankton in which inductively coupled plasma (ICP) source mass spectrometry (MS) was used to quantify the elements in the solution after digestion in a mixture of hydrofluoric and nitric acids in sealed PTFE vessels in a microwave field. The procedure was validated by the analysis of a standard reference soil (SRM 2709 San Joaquin Soil) and a standard reference fresh water plankton (CRM 414). The method was applied to the analysis of several marine plankton samples grown under controlled conditions including several whose growth media had been enriched with selenium. Matrix induced signal suppressions and instrumental drift were corrected by internal standardization. The suitabilities of germanium, indium, rhodium, scandium and yttrium as internal standard elements were evaluated. Neither scandium nor yttrium could be used due to the presence of these elements in the samples, germanium was used for the determination of As, Co, Cu, Fe, Ni, Se, Si and Zn, indium was used for Al, Ba, Ca, Eu, Sr, and Tl, and rhodium was used for Cd, Cr, Hg, Mg, Pb, Sb, Sn, and V. For Al, Ca, Cr, Cu, Fe, Mg, Mn, Ni, Si, Sr, V, and Zn internal standardization did not completely compensate for the suppressive effect of the heavier elements and the solutions were diluted. However, for As, Ba, Cd, Co, Eu, Hg, Pb, Sb, Se, Sn and Tl, it was possible to obtain accurate results despite the 35–¶40% suppression in the signals. Isobaric overlap was only a problem in the cases of ⁴²Ca and ⁷⁸Se; ⁴⁴Ca and ⁷⁷Se, respectively, were used. Memory effects were only observed with Hg for which a nitric acid-sodium chloride solution was the most effective wash-out solution. The marine plankton samples were able to tolerate a higher concentration of Hg as the selenium concentration increased.     

Determination of As, Ge, Hg, Pb, Sb, Se and Sn in coal slurries by CVG-ETV-ICP-MS using external or isotopic dilution calibration

A method for the multi-elemental determination of As, Ge, Hg, Pb, Sb, Se and Sn in coal reference materials by slurry sampling chemical vapor generation (CVG) using external calibration and isotopic dilution (ID) calibration and detection by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) is proposed. As, Ge, Sb, Se and Sn were determined using the external calibration, while, Hg, Pb, Se and Sn were determined by isotopic dilution. About 50–250 mg of sample was mixed with an acid solution, containing aqua regia and HCl, in an ultrasonic bath. For the isotopic dilution calibration, the enriched isotopes ²⁰¹Hg, ²⁰⁶Pb, ⁷⁷Se and ¹¹⁹Sn were added to the slurry in an adequate amount in order to produce an altered isotopic ratio close to 1. The vapor produced by the reaction of the sample slurry with the reducing agent was transported to the vaporizer and trapped in a Ir-treated graphite tube at 200 °C, before vaporization at 2100 °C and transportation of the vapor to the plasma. The accuracy of the method was assured by the analysis of four certified reference coal samples, using external calibration with aqueous solutions, prepared in the same medium and subjected to the same CVG and trapping procedure as the slurries and also by isotopic dilution calibration. The obtained concentrations were in agreement with the certified values, using the t-Student test for a confidence level of 95%. The detection limits (3 s; n = 5) of isotopic dilution, in ng g^− 1, were: 0.4 for Hg, 900 for Pb, 0.3 for Se and 0.2 for Sn. For external calibration, the detection limits, in ng g^− 1, were: 1.6 for As, 0.1 for Ge, 0.3 for Sb, 0.9 for Se and 7.5 for Sn. The relative standard deviations generally were lower than 14%, adequate for slurry analysis.     

Capabilities of double focussing magnetic sector-ICP-MS for the determination of trace elements in body fluids (blood, blood serum, urine) at the example of control materials

The capability of double focussing magnetic sector inductively coupled plasma mass spectrometry (HR-ICP-MS) for the determination of trace elements in different body fluids was investigated in commercially available control materials. The elements included in this study were: Al, As, Cd, Cr, Co, Cu, Hg, Mn, Ni, Pb, Sb, Se, Tl and Zn. Sample preparation, instrument stability and the results, which are in very good agreement to the given values, are presented and discussed. Received: 27 August 1997 / Revised: 19 November 1997 / Accepted: 23 November 1997     

Capabilities of double focussing magnetic sector-ICP-MS for the determination of trace elements in body fluids (blood, blood serum, urine) at the example of control materials

The capability of double focussing magnetic sector inductively coupled plasma mass spectrometry (HR-ICP-MS) for the determination of trace elements in different body fluids was investigated in commercially available control materials. The elements included in this study were: Al, As, Cd, Cr, Co, Cu, Hg, Mn, Ni, Pb, Sb, Se, Tl and Zn. Sample preparation, instrument stability and the results, which are in very good agreement to the given values, are presented and discussed. Received: 27 August 1997 / Revised: 19 November 1997 / Accepted: 23 November 1997