电感耦合等离子体原子发射光谱法测定金属饰品中铅、镉、铬、汞、锑、砷、硒、钡、镍溶出量

金属饰品样品用硝酸(20+80)溶液浸泡过夜,采用电感耦合等离子体原子发射光谱法测定金属饰品中铅、镉、铬、汞、锑、砷、硒、钡和镍的溶出量。选择波长为216.9,228.8,267.7,194.2,206.8,189.0,196.0,455.4,216.6nm的9条谱线依次作为测定铅、镉、铬、汞、锑、砷、硒、钡和镍的分析线。铅、镉、铬、锑、砷、硒、钡和镍的质量浓度与其发射强度在10.0mg·L-1以内、汞在2.0mg·L-1以内呈线性关系,检出限(3s)在0.002～0.05mg·L-1之间。方法用于金属饰品的分析,回收率在95.4%～103.0%之间,测定值的相对标准偏差(n=11)在0.68%～2.0%之间。     

icp-ms法同时测定卷烟纸中元素铬、镍、铜、砷、硒、镉、铅

电感耦合等离子体质谱(icp-ms);卷烟纸;微波消解     

The fate of As, Pb, Cd, Cr and Mn in a coal during pyrolysis

Transformation of As, Pb, Cd, Cr, and Mn in Chinese Datong coal during pyrolysis was studied. Experiments were carried out in a fixed-bed quartz reactor with a heating rate of 20 °C min⁻¹. Effects of the final temperature (300–1000 °C) and atmosphere (N₂ and H₂ at 0.1 MPa) were examined. Chemical form distribution of the elements in the coal and coal-derived chars (obtained at 1000 °C under N₂ and H₂) was investigated. As, Pb, Cr, Cd, and Mn in the coal and the chars were classified into five chemical forms (ion exchangeable, bound to carbonates, bound to Fe–Mn oxides, bound to organic matter, and in the residue) by a sequential dissolution method. Results show that As, Pb, and Cd are more volatile and tend to enrich in the volatile phase in the pyrolysis. Cr and Mn are relative non-volatile and tend to enrich in the solid phase. H₂ atmosphere promotes the release of the elements. The elements in all the five chemical forms undergo transformation in pyrolysis, and As, Pb, Cr and Cd show similar behavior.     

Determination of As,Cd, Cu,Hg and Pb in biological samples by modern electrothermal atomic absorption spectrometry

Pollution from heavy metals has increased in recent decades and has become an important concern for environmental agencies. Arsenic, cadmium, copper, mercury and lead are among the trace elements that have the greatest impact and carry the highest risk to human health. Electrothermal atomic absorption spectrometry (ETAAS) has long been used for trace element analyses and over the past few years, the main constraints of atomic absorption spectrometry (AAS) methods, namely matrix interferences that provoked high background absorption and interferences, have been reduced. The use of new, more efficient modifiers and in situ trapping methods for stabilization and pre-concentration of these analytes, progress in control of atomization temperatures, new designs of atomizers and advances in methods to correct background spectral interferences have permitted an improvement in sensitivity, an increase in detection power, reduction in sample manipulation, and increase in the reproducibility of the results. These advances have enhanced the utility of Electrothermal atomic absorption spectrometry (ETAAS) for trace element determination at μg L⁻¹ levels, especially in difficult matrices, giving rise to greater reproducibility, lower economic cost and ease of sample pre-treatment compared to other methods. Moreover, the recent introduction of high resolution continuum source Electrothermal atomic absorption spectrometry (HR-CS-ETAAS) has facilitated direct solid sampling, reducing background noise and opening the possibility of achieving even more rapid quantitation of some elements. The incorporation of flow injection analysis (FIA) systems for automation of sample pre-treatment, as well as chemical vapor generation renders (ETAAS) into a feasible option for detection of As and Hg in environmental and food control studies wherein large numbers of samples can be rapidly analyzed. A relatively inexpensive approach with low sample consumption provide additional advantages of this technique that reaches figures of merit equivalent to Inductively coupled plasma mass spectrometry (ICP-MS). Herein is presented an overview of recent advances and applications of (ETAAS) for the determination of As, Cd, Cu, Hg and Pb in biological samples drawn from studies over the last decade.     

Ultraviolet photolysis assisted mineralization and determination of trace levels of Cr, Cd, Cu, Sn, and Pb in isosulfan blue by ICP-MS

Isosulfan blue dye is used in sentinel node mapping technique to evaluate breast cancer patients where determination of different trace elements is required. A UV-photolysis assisted mineralization of isosulfan blue is described here for the determination of trace elements (Cr, Cd, Cu, Sn and Pb) by Inductively Coupled Plasma Mass Spectrometry (ICP-MS). In the present study advanced oxidation processes such as UV, UV/H₂O₂, and UV/H₂O₂/HNO₃ have been assessed and compared for the degradation and mineralization of isosulfan blue dye. The extent of mineralization was determined on the basis of total organic carbon (TOC) measurement. The adopted procedure (UV/HNO₃/H₂O₂) provided very low TOC content (0.5%), corresponding to a mineralization efficiency of > 99%. With the present procedure, the use of dynamic reaction cell (DRC) or collision cell was not required for chromium determination which suffers interference from the presence of carbon. Method detection limits were 0.0028, 0.0021, 0.016, 0.007, and 0.005 μg g^? 1 for Cr, Cd, Cu, Sn and Pb respectively. The values obtained by the proposed method were cross-validated by those obtained by ETAAS analysis. The expanded uncertainties in the measurement at 95% confidence level (coverage factor 2) are in the range of 13.7–25.8%.     

ICP-MS法测定中成药中微量砷铅镉和汞

对药品中毒性较大的有害元素指标进行严格限量控制是国际通用法规的重要规定。目前,已报道的光学分析方法归纳起来有：原子吸收光谱法、电感耦合等离子体原子发射光谱法、分光光度法、荧光分析法、化学发光法。在诸多方法中ICP-AES由于检出限低,精密度高、基体效应小、线性范围宽和多元素同时测定等优点,已在中草药微量元素分析中得到广泛应用。而ICP-MS比ICP-AES检出限改善了2-3个数量级,在中药微量分析中的应用开始受到人们的重视。本文利用微波消解ICP-MS法对几种中药及中成药中的As、Pb、Cd、Hg进行了测定,结果满意。     

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.     

电感耦合等离子体质谱法(ICP-MS)测定化妆品中铍、镉、铊、铬、砷、碲、钕、铅

建立了化妆品中铍、铬、砷、镉、碲、钕、铊、铅8种有害元素的测定方法,样品采用微波消解,以钇、锂、铟、铋为测定的内标元素,用电感耦合等离子体质谱法测定,结果表明,各元素和内标元素在一定浓度范围内的质量数比值均与浓度呈良好的线性关系,线性方程的相关系数均大于0.999 8,平均加标回收率为95%~104%,相对标准偏差(RSD)均小于3%。方法灵敏度高,准确,可为化妆品中上述元素的限量检查提供参考。     

电感耦合等离子体原子发射光谱法同时测定仿真饰品中砷、钡、镉、钴、铬、汞、镍、铅、锑和硒迁移量

仿真饰品样品用模拟人体环境的酸性汗液萃取60min后,采用电感耦合等离子体原子发射光谱法测定其中砷、钡、镉、钴、铬、汞、镍、铅、锑和硒的迁移量。试验选择波长为193.759,233.527,214.438,228.616,267.716,194.227,232.003,220.353,206.833,196.090nm的10条谱线依次作为测定砷、钡、镉、钴、铬、汞、镍、铅、锑和硒的分析线。方法的检出限(3sb/k)在0.002～0.06mg.L-1之间,测定下限(15sb/k)在0.01～0.3mg.L-1之间。方法用于仿真饰品的分析,回收率在88.0%～100%之间,测定值的相对标准偏差(n=7)在3.1%～9.8%之间。     

ICP-MS测定化妆品中铍、镉、铊、铬、砷、碲、钕、铅

目的：建立化妆品中铍、镉、铊、铬、砷、碲、钕、铅8种有害元素的测定方法。方法：采用电感耦合等离子体质谱法,样品采用微波消解,以钇、锂、铟、铋为内标作定量分析。结果：各元素和内标元素在一定浓度范围内的质量数比值均与浓度呈良好的线性关系,线性方程的相关系数均大于0.9998,平均回收率为95%~104%,相对标准偏差(RSD)均小于3%。结论：该方法灵敏度高,准确,可为化妆品中上述元素的限量检查提供参考。     

ICP-AES测定南红玛瑙中剧毒元素As、Cd、Cr、Pb、Sb含量的研究

文章研究报道了电感耦合等离子体发射光谱法测定南红玛瑙中As、Cd、Cr、Pb、Sb元素含量的分析方法。通过对前处理方法的确定、分析线的选择、基体干扰方面的研究,确定了分析条件,并对比研究了标准曲线法与标准加入法在测定方面的异同。标准加入法与标准曲线法的测定结果相近,但标准曲线法的测定结果总是比标准加入法的测定结果小。在标准加入法中,各元素加标回收率在93.6％～103％之间,测定值的相对标准偏差(RSD_n=6)小于10％;在标准曲线法中,各元素加标回收率在90.2％～103％之间,各元素的相对标准偏差(RSD _n=6)也均小于10％。基体效应对标准曲线法测定存在一定的影响,但不十分明显。标准加入法可以很好地减轻基体效应的干扰,但不可大批量测定样品。因此,在分析控制质量要求允许范围内,可采用标准曲线法对南红玛瑙中剧毒元素As、Cd、Cr、Pb、Sb的含量进行测定。     

原子吸收光谱法测定大承气颗粒剂中砷铅镉铬汞的含量

采用原子吸收光谱法测定了大承气颗粒剂及其原料药材中砷、铅、镉、铬和汞的含量，并参照食品中重金属的限量规定进行了比较。结果表明，大承气颗粒剂及其原料药材中的砷、铅、镉、铬和汞均低于限量标准，成品中重金属的含量均低于原料药材中的平均含量，这为大承气颗粒剂生产中的质量控制提供了依据。     

原子吸收光谱法测定益寿回春口服液中砷铅镉铬汞的含量

采用原子吸收光谱法测定了益寿回春口服液中砷、铅、镉、铬和汞的含量，并参照食品中重金属的限量规定进行了比较。结果表明，益寿回春口服液中的砷、铅、镉、铬和汞均低于限量标准，为该产品的质量控制提供了依据。     

Determination of Cr,Mn, Fe,Cu, Zn,As, Se,Cd, Hg and Pb in Ginseng by Inductively Coupled Plasma Mass Spectroscopy

Inductively coupled plasma mass spectroscopy (ICP-MS) has become an established technique of multi-element trace analysis, and it has been used for the analysis for the variety of samples,especially the samples of traditional Chinese medicine.     

Determination of As,Cd, Cr,Cu, Hg,Sb and Se concentrations by radiochemical neutron activation analysis in different Brazilian regional diets

The present paper describes radiochemical separation procedures developed for the determination of seven elements: As, Cd, Cr, Cu, Hg, Sb and Se in different Brazilian regional diets. In the case of the elements As, Hg, Sb and Se, the procedure was based on retention in inorganic exchanger TDO (tin dioxide) and determination of Hg by extraction with Ni(DDC)₂. For determination of Cd, Cr, Cu and Se the procedure chosen was based on retention in inorganic exchanger HMD (hydrated managese dioxide) and extraction of Cu and Cd as diethyldithiocarbamate compounds. The accuracy and precision of the methods studied were tested by means of analyses of different reference materials. Due to the lack of data on trace element levels in Brazilian foodstuffs and diets, these methods were applied to determination of these elements in different Brazilian regional diets. These diets were supplied by the Food and Experimental Nutrition Department of the Faculty of Pharmaceutical Science, University of São Paulo. The daily dietary intake values for these diets are presented for As, Cd, Cr, Cu, Hg, Sb and Se.     

端视ICP-AES法同时测定玩具涂料中可溶性铅、镉、汞、砷、铬、锑、硒和钡

采用端视电感耦合等离子体原子发射光谱(ICP-AES)法同时测定玩具涂料中可溶性铅、镉、汞、砷、铬、锑、硒和钡.对仪器的工作参数和被测元素的分析谱线进行了优化和选择.铅、镉、汞、砷、铬、锑、硒和钡的检出限分别为0.006、0.0009、0.012、0.023、0.000 8、0.013、0.030和0.0006 mg/L.定量下限分别为0.99、0.15、2.0、3.8、0.14、2.2、5.0和0.10 mg/kg.相对标准偏差为0.76%～2.72%(n=8),加标回收率为96.0%～104.0%.该法适用于玩具涂料中铅、镉、汞、砷、铬、锑、硒和钡的快速测定.     

Determination of Hg,Cd, Mn,Pb and Sn in seafood by solid sampling Zeeman atomic absorption spectrometry

Direct solid sampling Zeeman atomic absorption spectrometric methods were developed and applied to the determination of mercury, cadmium, manganese, lead and tin in seafood. All elements but mercury were measured by a third generation Zeeman atomic absorption spectrometry combined with an automatic solid sampler. In 3-field- and dynamic mode the calibrations concentration range was substantially extended and high amounts of analyte were detectable without laborious dilution of solid samples. The measurements were based on calibrations using certified reference materials of organic matrices. In case solid certified reference materials were not available calibration by aqueous standard solutions was proved to be an alternative. No matrix effects were observed under the optimized conditions. Results obtained were in good agreement with the certified values. Solid sampling Zeeman atomic absorption spectrometry proved to be a reliable, rapid and low-cost method for the control of trace elements in seafood.     

电感耦合等离子体质谱法测定海洋贝类中镉、铬、铜和铅

采用微波消解法处理海洋贝类样品,用电感耦合等离子体质谱法测定样品中镉、铬、铜和铅等4种重金属元素的含量。选择111 Cd、53 Cr、63 Cu和208 Pb等待测元素的同位素克服了质谱干扰。4种元素分别在一定的质量浓度范围内呈线性,检出限(3s)在0.005～0.17μg.L-1之间。镉、铬、铜和铅的回收率分别为94.7%,102.1%,101.9%,105.3%;测定值的相对标准偏差(n=7)分别为4.3%,3.8%,1.5%,6.0%。     

Determination of traces of silver in human scalp hair slurries by electrothermal atomic absorption spectrometry

A simple and rapid method for the determination of traces of silver in human hair by slurry sampling and electrothermal atomic absorption spectrometry was optimized. Hair pulverization and the particle size reduction were achieved using a vibrational zirconia mill ball for 20 min. Palladium nitrate, magnesium nitrate and palladium-magnesium nitrate were investigated as chemical modifiers to thermally stabilize silver. Glycerol was used as wetting agent to stabilize the hair slurries. A limit of detection of 21.6 g kg^–1 was obtained for the use of palladium nitrate as best chemical modifier. The repeatibility of the overall procedure (slurry preparation and atomic absorption spectrometric determination) corresponding to eleven measurements was 14.3%. Matrix effect was significant and so, the standard addition method was used to determine silver in hair samples from healthy people. The levels found varied between 0.10 and 1.62 mg kg^–1.