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1.
样品用硝酸-盐酸分解,采用扣除背景的方式消除高含量的锌对低含量镉测定的影响。优化了镉测定的仪器条件,建立了粗锌中镉含量的测定方法。用于测定粗锌中镉,结果的相对标准偏差(RSD,n=11)为0.95%~6.3%。按照实验方法对粗锌样品进行加标回收实验,加标回收率为98.0%~102%。与ICP-AES法测定结果基本一致,能满足日常对粗锌中镉含量的测定要求。 相似文献
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采用火焰原子荧光法(FAFS)和电感耦合等离子体质谱法(ICP-MS)测定铅锌矿中的镉. 通过对比研究,两种方法的校准曲线相关系数良好(
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A procedure for the direct determination of zinc, cadmium and copper in air and water has been developed. The possible interference effects of numerous anions and cations have been investigated. Few interferences were found, and these were eliminated by the addition of EDTA. The sensitivities found were 2 p.p.b. for cadmium, 8 p.p.b. for copper and 2 p.p.b. for zinc. 相似文献
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Summary A convenient electroanalytical technique for the simultaneous determination of lead, cadmium, copper and zinc in human blood and teeth is described. The method is based on differential pulse anodic stripping voltammetry at the static mercury drop electrode (SMDE). Optimum conditions for the anodic stripping of Pb, Cd, Cu and Zn were determined using ammonium acetate and dilute nitric acid (pH 2) as electrolytes. Interferences from other metals were not observed and the estimations were reproducible within a standard deviation of±4%. Low blank values and high sensitivity of the method allowed the determinations at sub-ppb levels with an electrolysis time of 1–3 min. The accuracy of the method has been tested by comparison with the results obtained by mass spectrometry and atomic absorption spectrometry. The results and findings are discussed in brief.
Bestimmung von Blei, Cadmium, Kupfer und Zink in menschlichen Geweben mit Hilfe der Differentialpuls-Anodic Stripping Voltammetrie
Zusammenfassung Eine vorteilhafte elektroanalytische Methode zur Bestimmung von Pb, Cd, Cu und Zn in menschlichem Blut und in Zähnen wird beschrieben. Das Verfahren beruht auf der Differentialpuls-Anodic Stripping Voltammetrie an der statischen Quecksilbertropfelektrode. Mit Hilfe von Ammoniumacetat und verdünnter Salpetersäure (pH 2) als Trägerelektrolyten wurden die optimalen Bedingungen ausgearbeitet. Störungen durch andere Metalle wurden nicht beobachtet. Die Standardabweichung betrug ±4%. Infolge der niedrigen Blindwerte und der hohen Empfindlichkeit konnten Bestimmungen im Sub-ppb-Bereich mit Elektrolysezeiten von 1–3 min durchgeführt werden. Die Genauigkeit der Methode wurde durch Vergleich mit massenspektrometrischen und AAS-Untersuchungen bewiesen. Die Ergebnisse werden kurz diskutiert.相似文献
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The reliability of the voltammetric determination of the cadmium and copper content (at pH 1.0), inherent to metallothionein (MT) isolated from the digestive gland of Mytilus galloprovincialis, was investigated. An artifact signal enhancement of copper, caused by the cupric-thionein complex adsorption at the mercury electrode, was established. This artifact was removed by UV-digestion of the sample for 15–20 h prior to analysis. A similar artifact was not detected for cadmium, because at this pH the cadmium-thionein complex has dissociated, and cadmium exists in the ionic form. Therefore, the voltammetric analysis of the cadmium content can be performed directly at pH 1.0, without prior UV-digestion of the sample. 相似文献
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The reliability of the voltammetric determination of the cadmium and copper content (at pH 1.0), inherent to metallothionein
(MT) isolated from the digestive gland of Mytilus galloprovincialis, was investigated. An artifact signal enhancement of copper, caused by the cupric-thionein complex adsorption at the mercury
electrode, was established. This artifact was removed by UV-digestion of the sample for 15–20 h prior to analysis. A similar
artifact was not detected for cadmium, because at this pH the cadmium-thionein complex has dissociated, and cadmium exists
in the ionic form. Therefore, the voltammetric analysis of the cadmium content can be performed directly at pH 1.0, without
prior UV-digestion of the sample.
Received: 4 August 1997 / Revised: 12 November 1997 / Accepted: 16 November 1997 相似文献
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This study was performed to determine the concentrations of cadmium, lead, copper and zinc in the edible muscle of pelagic (Scomberomorus commerson, Chirocentrus dorab, Sphyraena jello, Rachycentron conadum, Thunus tonggol, and Tenualosa ilisha) and demersal (Nemipterus japonicas, Epinephelus coioides, Platycephalus indicus, Psettodes erumei, Pomadasys argenteus, and Acanthopagrus latus) fish species from the Persian Gulf during winter and summer. The samples were analyzed by the derivative potentiometric stripping technique; and the results were expressed as μg/g of wet weight. The obtained range of metals in fish species was 0.024–0.111 μg/g for cadmium, 0.057–0.471 μg/g for lead, 0.799–4.790 μg/g for copper and 3.226–11.390 μg/g for zinc. The study revealed that seasonal variation influenced the concentration of metals in the samples. The highest concentration of cadmium, lead, copper and zinc was found in Platycephalus indicus (0.147 μg/g), Acanthopagrus latus (0.534 μg/g), Psettodes erumei (5.294 μg/g) and Psettodes erumei (13.528 μg/g) in winter, respectively. Moreover, demersal fish species had higher cadmium, lead and zinc concentrations, but lower copper content than pelagic ones. Our study demonstrated that the estimated daily and weekly intakes of lead, copper and zinc, and estimated monthly intake of cadmium via consumption of fish flesh were below the PTDI, PTWI and PTMI values established by FAO/WHO. 相似文献
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A method for the simultaneous spectrophotometric determination of cadmium, copper and zinc based on the formation of their complexes with 1,5-bis(di-2-pyridylmethylene)thiocarbonohydrazide is proposed. The absorption curves of these complexes overlap severely in the scanning range 380–480 nm. The analyte concentrations are calculated by a least squares fit of the pure spectra to the mixture spectra. A linear determination range of 0.1–1.7 μg/ml for cadmium, 0.1–1.3 μg/ml for copper and 0.2–1.2 μg/ml for zinc were obtained. The effect of interference was studied. The method has been applied to the determination of these metal ions in various type of materials. 相似文献
11.
Differential pulse anodic stripping voltamrnetry and a hanging mercury drop electrode are used for the determination of copper, lead, cadmium and zinc in Norwegian teeth and pure hydroxyapatite. Special attention is given to the choice of decomposition procedure and the determination of the blank values. A complete dissolution of the tooth material and satisfactory blank values can be obtained by using decomposition with nitric acid in a Teflon bomb. 相似文献
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Summary A preconcentration technique involving anion-exchange in thiocyanate media has been developed for the determination of traces of bio-significant and biofunctional elements. The procedure is applied to the analyses of NBS standard reference materials as well as environmental reference materials of NIES (The National Institute of Environmental Studies, Japan Environmental Agency). The results are quoted for vanadium, cobalt, copper, zinc, and cadmium. 相似文献
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研究了湿法冶炼产出的析出锌,经过冲床冲压脱模、马弗炉高温熔化、模具浇铸成型、车床切削等过程,于直读光谱仪上测定析出锌中铅、铜、铁、镉、锡、铝含量的方法.通过实验确认了仪器的工作条件、熔样器皿、熔样温度、析出锌取样位置,并对熔样铸锭后铅、铜、铁、镉、锡、铝的偏析情况进行了分析,铅最大偏差达到30%,经玻璃棒搅动后保温,铅... 相似文献
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Water samples from the Arctic Sea were analyzed by the potentiometric stripping technique. Lead(II) and cadmium(II) were determined after pre-electrolysis for 32 min at—1.1 V vs. Ag/AgCl, the detection limits being 0.06 and 0.04 nM, respectively. Zinc(II) was determined after the addition of gallium(III) by pre-electrolysis for 16 min at —1.4 V vs. Ag/AgCl, the detection limit being 0.25 nM. Problems in the determination of copper(II) at the very low concentrations found in oceanic waters are outlined. The average zinc(II), cadmium(II) and lead(II) concentrations in eight different samples were 2.5, 0.16 and 0.10 nM as determined by potentiometric stripping analysis and 1.9, 0.16 and 0.09 nM as determined by solvent extraction/atomic absorption spectrometry. The advantages of this computerized technique for the analysis of sea water are discussed. 相似文献
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《Spectrochimica Acta Part B: Atomic Spectroscopy》2002,57(8):1333-1338
A method was standardized for the dissolution of hair samples and analysis was carried out by inductively coupled plasma atomic emission spectrometry (ICP-AES). Hair samples were brought into solution by using a mixture of nitric acid and hydrogen peroxide. Various parameters that influence the sample preparation, namely temperature, digestion time and ratio of acid mixture were studied and standardized. The optimized method has been employed to digest standard reference materials and hair samples of residents of India, collected from different age groups and sex, and analyzed for Fe, Co, Ni, Mn, Zn, Cu, Cd and Pb. The values agree for most of the metals with the data reported for human hair samples of residents of India. The NIES CRM Human Hair No. 5 and IAEA Reference Hair HH-1 certified reference materials were used in order to verify the accuracy of the method and the results were in excellent agreement with the certified values. 相似文献
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《Spectrochimica Acta Part B: Atomic Spectroscopy》1999,54(10):1463-1468
The concentration of copper in traditional homemade alcoholic distillates produced in Venezuela (Cocuy de Penca) were determined by total reflection X-ray fluorescence (TXRF) using vanadium as internal standard. The results were compared to those obtained by flame atomic absorption spectrometry (FAAS). Three preparative methods of addition of vanadium were compared: classical internal standard addition, ‘layer on layer’ internal standard addition and in situ addition of internal standard. The TXRF procedures were accurate and the precision was comparable to that obtained by the FAAS technique. Copper levels were above the maximum allowed limits for similar beverages. Zinc and iron in commercial and homemade distilled beverages were also analyzed by TXRF with in situ addition of internal standard demonstrating the usefulness of this technique for trace metal determination in distillates. 相似文献
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Ferricyan can be determined in the presence of copper, silver and cadmium by addition of potassium ferrocyanide, filtration of the ferrocyanides of copper, silver and cadmium formed in this reaction, and titration of the potassium ferricyanide contained in the filtrate. In the case of silver, the ferricyan can also be determined without filtration by addition of potassium iodide and titration of the ferricyanide. In the case of zinc, potassium, ferrocyanide is added and without filtration the ferricyanide titrated. 相似文献
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Arc-nebulization (a thermal nebulization technique) is used to form an aerosol of cadmium, lead and zinc. An open arc chamber of simple operation and an ejector of high efficiency are described which are adaptable for use with any flame atomic absorption spectrometer. Limits of detection better by one or two orders of magnitude than those achieved by conventional flame a.a.s. methods were obtained viz., 43 ng Pb, 5 ng Cd, 7 ng Zn (equivalent to 0.7, 0.08 and 0.11 ppm, respectively, in copper). Calibration with matrix-free solutions was possible for lead and cadmium but not for zinc. The spectral interference of copper on absorbance at the most sensitive zinc line (213.856nm) and the efficiency of arc nebulization of cadmium are also discussed. 相似文献
20.
张晨 《中国无机分析化学》2020,10(6):18-22
针对银精矿样品复杂,难消解的特点,研究了不同酸溶法和碱熔法对样品的消解情况,建立了硝酸,盐酸,氢氟酸,高氯酸消解银精矿的方法。根据元素灵敏度和抗干扰性,选定各元素的测定波长。通过酸溶样和碱熔样测定结果比对,验证了方法准确性。建立了四酸消解-电感耦合等离子体光谱法测定银精矿中铜、铅、锌、砷、镉、钙、镁、锰含量的方法,元素的线性相关系数均在0.9999以上。通过共存元素干扰实验,确定了银精矿中高含量元素(铜、铅、锌、铁、锑、铋等)对测定元素结果没有影响。方法检出限:Cu 0.0063 mg/L, Pb 0.0159 mg/L ,Zn 0.0090 mg/L,As 0.0192 mg/L, Cd 0.0093 mg/L ,Ca 0.0084 mg/L, Mg 0.0075 mg/L, Mn 0.0081 mg/L。测定下限:Cu 0.0105mg/L,Pb 0.0265 mg/L, Zn 0.0150 mg/L, As 0.0320 mg/L, Cd 0.0155 mg/L, Ca 0.0140 mg/L, Mg 0.0125 mg/L,Mn 0.0135 mg/L。3个样品的相对标准偏差在0.87%~3.56%之间,加标回收率在95.00%~103.56%之间。方法流程短,操作简单,快速,灵敏度和再现性高,结果准确可靠,可以满足银精矿中铜、铅、锌、砷、镉、钙、镁、锰含量的测定。 相似文献