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1.
Acar O  Türker AR  Kılıç Z 《Talanta》1999,49(1):135-142
Direct determination of Bi, In and Pb in sea water samples has been carried out by ETAAS with Zeeman background correction using molybdenum containing chemical modifiers and tartaric acid as a reducing agent. Maximum pyrolysis temperatures and the effect of mass ratios of the mixed modifier components on analytes have been investigated. Mo+Pd+TA or Mo+Pt+TA mixture was found to be powerful for the determination of 50 mug l(-1) of Bi, In and Pb spiked into synthetic and real sea waters. The accuracy and precision of the determination were thereby enhanced. The recoveries of analytes spiked were 94-103% with Mo+Pd+TA or Mo+Pt+TA and they are only 49-61% without modifier.  相似文献   

2.
Summary The determination of lead and cadmium in biological materials was carried out by potentiometric stripping analysis. Supporting electrolyte was a mixture of NaCl and HCl. In the presence of 4% lumatom in methanol, oxidation potentials of –0.46 V for Pb and –0.68 V for Cd were found (vs. SCE). The method was applied to different standard reference materials (leaves, needles, hair) and was also compared with the differential pulse anodic stripping technique. The latter presented considerable difficulties, in particular by the interference of oxygen.
Bestimmung von Blei und Cadmium in biologischem Material durch potentiometrische Stripping-Analyse
Zusammenfassung Als Trägerelektrolyt diente bei diesem Verfahren ein Gemisch von NaCl und HCl. In Gegenwart von 4% Lumatom in Methanol wurden Oxidationspotentiale von –0,46 V für Pb und –0,68 V für Cd (gegen SKE) erhalten. Die Methode wurde auf verschiedene Referenzmaterialien (Laub, Nadeln, Haar) angewendet und auch mit der Differentialpuls-Anodic Stripping-Analyse verglichen. Bei der letzteren ergaben sich größere Schwierigkeiten, hauptsächlich durch störenden Sauerstoff.
  相似文献   

3.
A method for direct determination of cadmium, chromium, copper and lead in sediments and soil samples by electrothermal atomic absorption spectrometry using Zr, Ir, etylenediamine acetic acid (EDTA), Zr + EDTA, Ir + EDTA, Zr + Ir and Zr + Ir + EDTA as chemical modifiers in 0.5% (v/v) Triton X-100 plus 0.2% (v/v) nitric acid mixture used as diluent was developed. The effects of mass and mass ratio of modifiers on analytes in sample solutions were studied. The optimum masses and mass ratios of modifiers: 20 microg of Zr, 4 microg of Ir, 100 microg of EDTA and 20 microg of Zr + 4 microg of Ir + 100 microg of EDTA, were used to enhance the analyte signals. Pyrolysis and atomization temperatures, atomization and background absorption profiles, characteristic masses, and detection limits of analytes in samples were compared in the presence or absence of a modifier. The detection limits and characteristic masses of analytes in a 0.5% (m/v) dissolved sample (dilution factor of 200 ml g(-1)) obtained with Zr + Ir + EDTA are 8.0 ng g(-1) and 1.2 pg for Cd, 61 ng g(-1) and 4.3 pg for Cr, 32 ng g(-1) and 23 pg for Cu, and 3.4 ng g(-1) and 19 pg for Pb, respectively. The Zr + Ir + EDTA modifier mixture was found to be preferable for the determination of analytes in sediment and soil-certified and standard reference materials. Depending on the sample type, the percent recoveries of analytes were increased from 81 to 103% by using the proposed modifier mixture; the results obtained are in good agreement with the certified values.  相似文献   

4.
Pereira LA  Amorim I  da Silva JB 《Talanta》2006,68(3):771-775
A procedure for the determination of cadmium, chromium, and lead in marine sediment slurries by electrothermal atomic absorption spectrometry is proposed. Slurry was prepared by mixing 10 mg of ground sample with particle size smaller than 50 μm completed to the weight of 1.0 g with a 3% nitric acid and 10% hydrogen peroxide solution. The slurry was maintained homogeneous with an aquarium air pump. For cadmium, the best results were obtained using iridium permanent with optimum pyrolysis and atomization temperatures of 400 and 1300 °C, respectively, a characteristic mass, mo (1% absorption), of 2.3 pg (recommended 1 pg). Without modifier use, zirconium, ruthenium, and rhodium mo were 3.4, 4.1, 4.6, and 4.8 pg, respectively. For chromium, the most sensitive condition was obtained with zirconium permanent with optimum pyrolysis and atomization temperatures of 1500 and 2500 °C, mo of 6.6 pg (recommended 5.5 pg); and without modifier use, rhodium, iridium, and ruthenium mo were 5.3, 8.8, 8.8, and 8.9 pg, respectively. For lead, the best modifier was also zirconium, mo of 8.3 pg for the optimum pyrolysis and atomization temperatures of 600 and 1400 °C, respectively, (recommended mo of 9.0 pg). For iridium, ruthenium, without modifier, and rhodium, mo were 14.7, 15.5, 16.5, and 16.5 pg, respectively. For all the modifiers selected in each case, the peaks were symmetrical with r2 higher than 0.99. Being analyzed (n = 10), two marine sediment reference materials (PACS-2 and MESS-2 from NRCC), the determined values, μg l−1, and certified values in brackets, were 2.17 ± 0.05 (2.11 ± 0.15) and 0.25 ± 0.03 (0.24 ± 0.01) for cadmium in PACS-2 and MESS-2, respectively. For chromium in PACS-2 and MESS-2 the values were 94.7 ± 5.6 (90.7 ± 4.6) and 102.3 ± 10.7 (106 ± 8), respectively. Finally, for lead in PACS-2 and MESS-2, the results obtained were 184 ± 7 (183 ± 8) and of 25.2 ± 0.40 (21.9 ± 1.2), respectively. For cadmium and lead in both samples and chromium in PACS-2, calibration was accomplished with aqueous calibration curves. For chromium in MESS-2, only with the standard addition technique results were in agreement with the certified ones. The limits of detection (k = 3, n = 10) obtained with the diluents were 0.1, 3.4, and 3.6 μg l−1 for cadmium, chromium, and lead, respectively.  相似文献   

5.
Procedures for the electrothermal atomic absorption spectrometric determination of lead and cadmium in urine, serum and blood are developed. For serum and blood, the samples are diluted by incorporating 0.015% (w/v) Triton X-100 and 0.1% (w/v) ammonium dihydrogenphosphate to the solutions, which are then introduced directly into the furnace. A solution containing 15% (w/v) hydrogen peroxide and 0.65% (w/v) nitric acid is also introduced into the atomizer by means of a separate injection. Zeeman-based correction is recommended. Both conventional and fast-heating programs are discussed. Calibration is carried out using the standard additions method. The reliability of the procedures is checked by analyzing three certified reference materials and by recovery studies.  相似文献   

6.
Legotte PA  Rosa WC  Sutton DC 《Talanta》1980,27(1):39-44
A method for determining cadmium and lead in urine and other biological samples by graphite-furnace atomic-absorption spectrometry is reported. Samples were analysed after wet or dry ashing and without extraction or matrix-modification techniques, in laminar-flow clean-room; negligible blank contributions were found. Matrix interference effects were observed only for lead and were resolved by the method of standard additions. Five NBS biological reference materials were used as internal quality-control standards. The urinary levels for non-exposed volunteers ranged from 0.16 +/- 0.01 to 1.65 +/- 0.20 and from 6 +/- 1 to 31 +/- 6 ng/ml for cadmium and lead, respectively; this corresponds to 0.15 +/- 0.02 to 2.01 +/- 0.16 and 7 +/- 1 to 31 +/- 3 mug/day. The average relative standard deviation for 60 urine samples was 10% for cadmium and 13% for lead.  相似文献   

7.
A method for the determination of cadmium in slurries of marine sediment using palladium and phosphate as chemical modifier has been optimized. To stabilize the marine sediment slurry, Triton X-100 at 0.1% was used. To obtain a complete pyrolysis of the slurry sample two mineralization steps were used, the first at 480 °C and the second at 600 °C and 700 °C for phosphate and palladium, respectively. The precision and accuracy of the method have been studied by analyzing the Reference Material PACS-1 (marine sediment) of National Research Council Canada. The detection limits (LOD) were 11.9 g kg–1 for phosphate and 42.0 g kg–1 when palladium was used. These methods have been applied to the determination of cadmium in marine sediment samples from the Galicia coast and the results of both methods were compared; no significant differences were found between the two procedures.  相似文献   

8.
The development of 3 different ultrasonic-based sample treatment methods, ultrasonic probe-assisted acid extraction, ultrasonic-assisted acid slurry, and ultrasonic-assisted acid pseudodigestion is presented. These methods were compared for the determination of Cd and Pb by electrothermal atomic absorption spectrometry in biological samples (blood and scalp hair) and validated by using certified materials BCR 397 human hair and BCR 185R bovine liver. The sample amounts chosen to perform the analysis were 100 mg and 0.5 mL for solids (human hair and bovine liver) and blood samples, respectively. An acid digestion induced by microwave energy was used to obtain the total metal concentrations and for comparative purposes. The best results were obtained with the ultrasonic-assisted acid pseudodigestion, with which it was possible to perform accurate and precise determination of the Cd and Pb contents in 2 certified reference materials and biological samples of 50 normal males of ages 25-40 years. The precision of the methods, together with their efficiency, rapidity, low cost, and environmental acceptability, make them good alternatives for the determination of trace metals from biological samples. The precision of the methods for accuracy evaluation, resulting in good agreement according to the t-test for a 95% confidence level, and the relative standard deviations were lower than 10% (n=10) for all determinations.  相似文献   

9.
应用同位素稀释电感耦合等离子体质谱(ID—ICP—MS)对环境和生物样品茶叶、湖沉积物和人发标准物质中的镉进行测定研究。对电感耦合等离子体质谱(ICP—MS)的工作条件和参数进行了最优化。讨论了多原子离子和同量异位素对镉同位素比值的影响,通过天然镉标准溶液对质量歧视进行了校正,并优化同位素稀释剂的加入量。将该方法应用于茶叶、人发和沉积物标准物质的测定。  相似文献   

10.
Acar O 《Talanta》2005,65(3):672-677
Cadmium, copper and lead in soils, sediments and spiked sea water samples have been determined by electrothermal atomic absorption spectrometry (ETAAS) with Zeeman effect background corrector using NH4NO3, Sc, Pd, Sc + NH4NO3, Pd + NH4NO3, Sc + Pd and Sc + Pd + NH4NO3 as chemical modifiers. A comprehensive comparison was made among the modifiers and without modifier in terms of pyrolysis and atomization temperatures, atomization and background absorption profiles, characteristic masses, detection limits and accuracy of the determinations. Sc + Pd + NH4NO3 modifier mixture was found to be preferable for the determination of analytes in soil and sediment certified and standard reference materials, and sea water samples because it increased the pyrolysis temperature up to 900 °C for Cd, 1350 °C for Cu and 1300 °C for Pb. Optimum masses of mixed modifier components found are 20 μg Sc + 4 μg Pd + 8 μg NH4NO3. Characteristic masses of Cd, Cu and Pb obtained are 0.6, 5.3 and 15.8 pg, respectively. The detection limits of Cd, Cu and Pb were found to be 0.08, 0.57 and 0.83 μg l−1, respectively. Depending on the solid sample type, the percent recoveries were increased up to 103% for Cd, Cu and Pb by using the proposed modifier mixture. The accuracy of the determination of analytes in the sea water samples was also increased.  相似文献   

11.
An interference-free routine method for the determination of vanadium in alkaline sludge by ETAAS has been developed. Chromium nitrate was used as a chemical modifier. The limits of detection and quantification are 0.56 and 1.9 ng V, respectively. The relative standard deviation is±1.5% for 101.8 μg/g vanadium.  相似文献   

12.
Direct analysis of solid samples employing a laboratory assembled electrothermal atomic absorption spectrometer is demonstrated to be a feasible approach for determination of trace elements in plant tissue and hair samples for special applications in plant physiology and biomedical research. As an example, the kinetics of Cr uptake by cabbage and its distribution have been measured as a function of chromium speciation in the nutrient solution. Further, longitudinal concentration gradients of Cr, Pb and Cd have been measured in hair of various population groups exposed to different levels of these elements in ambient and/or occupational environments. The techniques are validated for the determination of these trace elements by neutron activation analysis, dissolution atomic absorption spectrometry and by analysis of certified reference materials. Slurry sample introduction is found appropriate for routine trace element determination and in homogeneity testing. Direct sample introduction is indispensable in the analysis of very small (< 1 mg) tissue biopsy samples in the determination of trace element distributions.  相似文献   

13.
A comparative study on the efficiency of some tungsten containing chemical modifiers such as W, W+Pd, W+Rh, W+Pt and W+Ru for thermal stabilization of Bi, In, Pb and Sb has been performed systematically by a Zeeman electrothermal atomization atomic absorption spectrometer (ETAAS). The addition of tartaric acid (TA) as a reducing agent additionally to the mixed modifiers was studied. A mixture of W+Pd+TA was found to be a powerful mixed modifier for the determination of Bi, In, Pb and Sb. Pretreatment temperatures could be increased up to 1250–1500° C using this mixed modifier. The use of the mixed modifier results in an enhanced accuracy and precision of the method and recovery rates above 97% for all samples. The W+Pd+TA mixed modifier was applied to the determination of Bi and Pb in dissolved geological reference samples. Received: 14 March 1996 / Revised: 3 June 1996 / Accepted: 30 June 1996  相似文献   

14.
A comparative study on the efficiency of some tungsten containing chemical modifiers such as W, W+Pd, W+Rh, W+Pt and W+Ru for thermal stabilization of Bi, In, Pb and Sb has been performed systematically by a Zeeman electrothermal atomization atomic absorption spectrometer (ETAAS). The addition of tartaric acid (TA) as a reducing agent additionally to the mixed modifiers was studied. A mixture of W+Pd+TA was found to be a powerful mixed modifier for the determination of Bi, In, Pb and Sb. Pretreatment temperatures could be increased up to 1250–1500° C using this mixed modifier. The use of the mixed modifier results in an enhanced accuracy and precision of the method and recovery rates above 97% for all samples. The W+Pd+TA mixed modifier was applied to the determination of Bi and Pb in dissolved geological reference samples. Received: 14 March 1996 / Revised: 3 June 1996 / Accepted: 30 June 1996  相似文献   

15.
A radiochemical procedure for simultaneous determination of lead (203Pb), thallium (202TI) and cadmium (115Cd115mIn) after fast neutron activation, based on ion-exchange separation from bromide medium and additional purification steps for Pb and Tl is described. Radioactive tracers210Pb and109Cd were used for determination of the chemical yields of Pb and Cd; for Tl it was determined gravimetrically. Two standard reference materials, BCR CRM No. 146 Sewage Sludge and NIST SRM 1633a Coal Fly Ash were analyzed and satisfactory agreement with certified values was obtained.  相似文献   

16.
Robles LC  Aller AJ 《Talanta》1995,42(11):1731-1744
The retention of cadmium by the bacteria Escherichia coli and Pseudomonas putida was optimized in order to develop a rapid and selective preconcentration method for cadmium from biological and environmental samples prior to determination by electrothermal atomic absorption spectrometry. Living and lyophilized cells for both bacteria were used, but the method using dead cells shows better analytical capabilities. Cadmium from aqueous solutions is easily retained on the outer membrane of both bacteria in the pH range 4-10, although the selected working pHs for E. coli and P. putida were 5 and 9, respectively. Cadmium retained by the bacteria was dispersed in 3.5 M nitric acid and the slurry was introduced directly into the graphite tube. The best sensitivity and detection limit were obtained for E. coli (0.03 ng ml(-1) and 0.04 ng ml(-1) respectively, in the absence of any chemical modifier). A strong spectral interference from nickel chloride was found and methods to overcome it were developed. The proposed extraction procedure was tested by the determination of cadmium in different standard biological and environmental samples.  相似文献   

17.
Molybdenum, Ir, Ru, Mo-Ir, Mo-Ru thermally coated on to platforms inserted in pyrolytic graphite tubes as permanent modifiers and Pd + Mg(NO3)2 conventional modifier mixture have been employed for the determination of cadmium and lead in dissolved sediments and soil samples by electrothermal atomic absorption spectrometry (ETAAS). Optimum masses and mass ratios of permanent modifiers for the analysis of Cd and Pb in sample solutions have been investigated. The 280 μg of Mo, 200 μg of Ir, 200 μg of Ru, 280 μg of Mo + 200 μg of Ir or 280 μg of Mo + 200 μg of Ru has been found as efficient as 5 μg of Pd + 3 μg of Mg(NO3)2 for increasing thermal stabilization of analytes and for decreasing the most serious interferences. Pyrolysis and atomization temperatures, atomization and background signal shapes, characteristic masses and detection limits of analytes in dissolved samples with or without permanent and conventional modifiers have been compared. The detection limits and characteristic masses obtained with Mo-Ir coated platform are 0.01 μg g−1 and 1.1 pg for Cd and 0.09 μg g−1 and 19 pg for Pb, respectively. Long-term stabilities for analytes in samples with Mo, Mo-Ir, Mo-Ru and Pd + Mg(NO3)2 have been studied. Cadmium and lead contents have been determined in certified and standard reference materials by using optimum conditions investigated and the results obtained with Mo-Ir or Mo-Ru were in agreement with the values of certified reference materials.  相似文献   

18.
Three chemical modifiers ((NH(4))(2)HPO(4), NH(4)H(2)PO(4), and Pd as Pd(NO(3))(2)) were evaluated for the determination of Cd in acid-digested solutions of hair and blood using electrothermal atomic absorption spectrometry in a tungsten coil atomizer (TCA). All modifiers caused some thermal stabilization of Cd when compared to the behavior observed in nitric acid medium. The best effects were observed in 15 mug ml(-)(1) Pd medium; the characteristic mass of Cd was 0.3 pg and the method detection limits were 0.009 mug g(-)(1) in hair and 0.2 mug l(-)(1) in blood. In addition to a slight thermal stabilization effect, Pd also increased the sensitivity for Cd by ca. 40% and the tungsten coil lifetime by 20% (i.e. from 300 to 360 heating cycles), reduced background signals, and eliminated condensed phase interferences caused by concomitants. The accuracy (3.2% as mean relative error in the Pd modifier) was checked for the determination of Cd in acid-digested solutions of certified reference materials of human hair and blood and by recoveries of Cd in spiked hair and blood samples by both TCA and a graphite furnace procedure. All results obtained in chemical modifiers are in agreement at a 95% confidence level.  相似文献   

19.
Pedro R. Aranda 《Talanta》2008,77(2):663-666
Cloud point extraction (CPE) has been used for the preconcentration of cadmium, after the formation of a complex with 2-(5-bromo-2-pyridylazo)-5-(diethylamino)-phenol (5-Br-PADAP), and further determination by graphite furnace atomic absorption spectrometry (ETAAS) using polyethyleneglicolmono-p-nonyphenylether (PONPE 7.5) as surfactant. The chemical variables that affect the cloud point extraction were optimized. The separation of the two phases was easily accomplished by cooling the mixture in order to make more viscous the surfactant-rich phase. In order to establish the optimum conditions for the determination of Cd by ETAAS, Pd + Mg, Pt, Ir, Rh and Ru were studied as chemical modifiers. The best thermal stabilization was obtained with Pd + Mg, with a maximum pyrolysis temperature of 1100 °C. Under the optimum conditions i.e., pH 9.0, [5-Br-PADAP] = 2.0 × 10−5 mol L−1, [PONPE 7.5] = 0.02% (w/v), an enhancement factor of 22-fold was reached. The lower limit of detection (LOD) obtained under the optimal conditions was 0.008 μg L−1. The precision for 10 replicate determinations at 0.2 μg L−1 Cd was 3.5% relative standard deviation (R.S.D.). The calibration graph using the preconcentration method was linear with a correlation coefficient of 0.9984 at levels close to the detection limit up to at least 1.0 μg L−1. The method was successfully applied to the determination of cadmium in urine samples and in a water standard reference material.  相似文献   

20.
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