A Comparison of Methods for the Determination of Available Trace Metals in Sea Water

Abstract

Two methods for the determination of available trace metals CCd, Pb, and Cu) in sea water are compared. One method employs anodic stripping voltammetry at controlled pH (8.1, 5.3, and 2); the other method involves sample pretreatment with Chelex-100 resin before ASV analysis. Differences in the results are discussed in terms of the definition of available metal and differences in the analytical methods.     

Determination of Trace Metals in Antarctic Sediments from Terra Nova Bay - Ross Sea

Abstract

Trace metals (Cu, Pb, Zn, Cd, Cr, Ni, Co, Mn) and iron concentration were determined in several sediments collected in the Antarctica (Terra Nova Bay—Ross Sea). Samples were analyzed by inductively coupled plasma (ICP-AES) after selective and total extraction. The results are in good agreement with the data previously collected in the same area.     

菊花茶中重金属和微量元素溶出特性研究

为了探究菊花茶和茶汤中重金属及微量元素含量,指导菊花茶的饮用,本研究对浙江主要菊花茶品种皇菊和金丝皇菊的重金属和微量元素含量及其溶出特性进行了分析。通过ICP-MS和ICP-OES测定Cd、Cr、Cu、Pb、Zn、Ni、As七种重金属和K、Na、Ca、Mg、Se、Fe和Mn七种微量元素的含量,并参照传统泡茶方式对不同浸泡时间及不同浸泡次数条件下的皇菊和金丝皇菊中重金属和微量元素的溶出特性进行研究。结果发现,两种菊花中Cd含量均超标,但茶汤中的Cd与其他重金属符合生活饮用水标准,随着浸泡时间延长,菊花中重金属和微量元素的溶出率逐渐增加,Cd的总溶出率仅9.9%-11.8%,Cr、Pb的总溶出率也在10%以下,但Cu、Zn、Ni、As溶出率较高,在45.0%-71.6%之间,微量元素的溶出率在1.7%-84.0%之间,其中K、Na、Se元素的溶出率较高,最高分别达到了84.0%、72.9%、78.0%;随着浸泡次数增加,菊花中重金属和微量元素的溶出率逐渐降低,在第一次浸泡后,菊花中Cd、Cr、Pb的溶出率较低,分别在0.3%-8.0%, Cd、Cr、Pb的初次溶出量占溶出总量50%-100%,Cu、Zn、Ni、As在第一次浸泡后,溶出量占总量的28%-63%,第一次浸泡后,菊花中的K和Se的溶出率较高,达到30.6%-65.8%,Na、Ca、Mg、Mn的溶出率在5.8%-29.4%。微量元素第一次浸泡溶出量占溶出总量的41%- 100%。两种菊花中,金丝皇菊第一次浸泡溶出的重金属和微量元素比例均较高。通过延长浸泡时间可增加茶汤中重金属和微量元素的溶出,弃去初泡水的方式,虽然去除了过半含量的重金属,但同时也损失了大量微量元素,建议泡茶时延长浸泡时间。     

Nafion Coated Silver Amalgam Electrode for Determination of Trace Metals by Anodic Stripping Voltammetry

This paper describes characterization and application of Nafion coated solid silver amalgam electrodes to prevent surface fouling of surfactants in determination of trace metals by differential pulse anodic stripping voltammetry (DPASV). Polymer films of different thickness were tested using Nafion solutions in the range 0.25%–1%. Optimum thickness was archived using a 0.5% Nafion solution, resulting in both increased response and stability over time compared to uncoated electrodes. The influence of model surface active macromolecules was studied using triton X‐100, sodium dodecyl sulfate, dodecyl pyridinium chloride and bovine serum albumin as representatives for surfactants. The resistance to surfactants makes the studied Nafion coated solid silver amalgam electrodes an interesting alternative for practical use in environmental monitoring.     

Detection of Trace Heavy Metals Ions by Arrays of Titania Nanotubes Annealed in Nitrogen

Redox response of trace heavy metals ions(THMIs) has better performance on highly ordered vertically oriented titania nanotube arrays(TNA) annealed in nitrogen. Experimental data showed that different THMIs possess different reaction peak shapes and charge and discharge capacities. Therefore, the TNA will become an important tool used for environmental protection and facilitating the rapid determination of THMIs. THMIs of 5×10-4 mol/L concentration were measured at a scan rate of 100 mV/s. The analytical ut...     

Bismuth‐Coated Iridium Microwire Electrode for the Determination of Trace Metals by Anodic Stripping Voltammetry

This work reports the utility of an iridium microwire plated in situ with a bismuth film for the simultaneous determination of Pb(II) and Cd(II) by square‐wave anodic stripping voltammetry (SWASV). The experimental variables (concentration of the bismuth plating solution, preconcentration potential, accumulation time) were investigated. The limit of detection was 1 µg L^?1 for Pb(II) and 1.5 µg L^?1 for Cd(II) (at 300 s of preconcentration) and the % relative standard deviations were lower than 4.9 % and 5.5 %, respectively, at the 20 µg L^?1 level (n=8). In addition, a study was made of coating the iridium‐based bismuth‐film microsensor with a film of Nafion for operation in the presence of surfactants. Finally, the electrode was applied to the determination of Pb(II) and Cd(II) in wastewater and tapwater samples.     

电感耦合等离子体质谱测试硫化物中的微量元素

采用多种酸组合消解方法消解硫化物样品,最终选取A:HNO3密闭消解法;B:HCI+HF与HNO3两步消解法对硫化物标准物质GBW07267(黄铁矿)、GBW07268(黄铜矿),GBW07270(闪锌矿)及硫化物标准物质WMS-1a(块状硫化物)样品进行消解,采用ICP-MS测试了39种微量元素.结果表明,HNO3密闭...     

Preparation of a reference mussel tissue material for polycyclic aromatic hydrocarbons and trace metals determination

Due to high cost of certified reference materials (CRMs), reference materials (RMs) are preferred to check the method performance in environmental analysis. In this work, a laboratory reference material (LRM) was prepared and characterised to carry out the quality control in monitoring analysis of eight polycyclic aromatic hydrocarbons (PAHs) and nine trace metals in mussel tissue. Mussels were collected in a naturally polluted area. Before the reference material was bottled, the mussel tissue was stabilised by freeze-drying, ground and sieved. For the material characterisation, several statistical tests were applied to check the homogeneity of the analytes in the tissue, and a stability test was performed to study the effect of the storage temperature in the analyte concentration. Other characteristics such as specific density, moisture and lipid contents as well as particle size distribution of the material were determined. Although the LRM had a homogeneous distribution for all PAHs and almost all metals, the stability study showed different results at both storage temperatures studied. For both PAHs and trace metals, the material was suitable to assure the quality control of the analysis.     

液体阴极辉光放电原子发射光谱法分析硅酸钇镥中痕量杂质元素

采用液体阴极辉光放电原子发射光谱( Solution-cathode glow discharge-atomic emission spectrometry, SCGD-AES)法测定了硅酸钇镥(Lutetium-Yttrium Orthosilicate, LYSO)闪烁晶体材料中痕量元素 Ca,Fe, K, Li, Mg和Na。最佳实验条件是溶液pH为1的HNO3,直流电压为1080 V,溶液流速为2.0 mL/min。本方法对LYSO基体的耐盐量为10 g/L。硅酸钇镥晶体使用HNO3, HF, HClO4溶解后经SCGD-AES分析测定,结果同电感耦合等离子体发射光谱( Inductively coupled plasma-atomic emission spectroscopy, ICP-AES)和电感耦合等离子体质谱( Inductively coupled plasma-mass spectroscopy, ICP-MS)分析结果比对,具有较好的一致性。在运用SCGD-AES对LYSO的测定中,未观察到Lu、Y元素的激发谱线,因此测定LYSO中痕量元素时测定的光谱干扰少,Ca, Fe, K, Li, Mg和Na的检出限分别为：1.0,3.0,0.02,0.01,0.02和1.0 mg/kg。     

土壤中重金属元素检测的质量认证

探讨了土壤中重金属检测能力验证的质量控制措施,为确保能力验证结果的准确性及不断提高实验室的检测技术水平提供参考.     

孕期及非孕期黄褐斑患者几种微量元素对比观察

检测了５０例孕期黄褐斑患者、４９地期无黄褐斑妇女、４８例未孕黄褐斑患者及５１例未孕无黄褐斑者的Ｚｎ、Ｃｕ、Ｆｅ、Ｍｇ水平，发现孕期及非孕期黄褐斑患者轿清Ｃｕ水平升高：而孕期患者血清Ｚｎ较孕期非患者高，其血清Ｆｅ较未孕非患者高，孕期患者血清镁较未孕非患者低；提示血清Ｃｕ水平升高可能在黄褐斑的发生中具有一定作用，而血清Ｚｎ、Ｆｅ可能与妊娠其黄褐斑的发病。     

XRF检验标准物质中痕量元素的匀性

本文讨论了用Ｘ射线荧光光谱检验标准物质中痕量元素的均匀性时，可根据峰和背景强度确定能否用ＸＲＦ进行检验，以及相应于一定精度度要求的浓度下限（可检浓度），并以大米和岩石标准物质为例，计算了Ｃ－的可检浓度。还指出，作为均匀性检验量应采用浓度或净强度，尤其是对于痕量元素，最后说明了样品基体对可检浓度和最小样品量的影响。     

Determination of polybrominated diphenyl ethers in environmental standard reference materials

Standard reference materials (SRMs) are valuable tools in developing and validating analytical methods to improve quality assurance standards. The National Institute of Standards and Technology (NIST) has a long history of providing environmental SRMs with certified concentrations of organic and inorganic contaminants. Here we report on new certified and reference concentrations for 27 polybrominated diphenyl ether (PBDE) congeners in seven different SRMs: cod-liver oil, whale blubber, fish tissue (two materials), mussel tissue and sediment (two materials). PBDEs were measured in these SRMs, with the lowest concentrations measured in mussel tissue (SRM 1974b) and the highest in sediment collected from the New York/New Jersey Waterway (SRM 1944). Comparing the relative PBDE congener concentrations within the samples, we found the biota SRMs contained primarily tetrabrominated and pentabrominated diphenyl ethers, whereas the sediment SRMs contained primarily decabromodiphenyl ether (BDE 209). The cod-liver oil (SRM 1588b) and whale blubber (SRM 1945) materials were also found to contain measurable concentrations of two methoxylated PBDEs (MeO-BDEs). Certified and reference concentrations are reported for 12 PBDE congeners measured in the biota SRMs and reference values are available for two MeO-BDEs. Results from a sediment interlaboratory comparison PBDE exercise are available for the two sediment SRMs (1941b and 1944).     

An overview of laboratory performance studies conducted by the IAEA for marine pollution studies of metals and organic contaminants

Aspects of the International Atomic Energy Agency (IAEA) Analytical Quality Control Services (AQCS) for marine environmental studies are discussed, focusing on recent laboratory performance studies (LPS) and the production of reference materials for trace metals and organic compounds in various marine matrices. The IAEA has organized seventeen global interlaboratory studies for a range of organic contaminants. Of note has been the inclusion of numerous polychlorinated biphenyl congeners (PCBs) and some sterols of anthropogenic origin. Concurrently, there have been eleven worldwide intercomparison exercises for trace metals in the marine environment, most of which included methylmercury. Although such interlaboratory studies can help improve performance in individual laboratories and regional laboratory networks, the results reveal that problems remain in the determination of some metals and many organic contaminants.     

Systematic Errors in the Determination of Trace Metals by GFAAS Technique,Part I

The behaviour of solutions containing 7 metals in trace range (pH=2) prepared in borosilicate glass and polyethylene containers and transferred into commercial polyethylene–polypropylene and home-made quartz autosampler cups for measurements were studied using graphite furnace atomic absorption spectrometry. The different interactions between metal solution and vessel material were observed for the metals studied. The most significant losses of chromium and nickel occurred on a polyethylene surface, while the highest absorbance signals were registered from quartz containers. Higher absorbance signals from quartz containers were also obtained for cadmium and copper solutions. Contrary to these results, the absorbance signals for lead solutions were lowest when measured from quartz vessels. The container material had no influence on the analytical signals of cobalt and manganese.Received January 15, 2003; accepted April 15, 2003 published online August 22, 2003     

人中白钙含量及微量元素的测定

报道了人中白的钙及微量元素含量测定结果。     

丙烯中微量硫的测定

本文采用燃烧方法将不同形式的可燃性硫转化为SO2，在硝酸介质中用H2O2将SO2氧化为SO4^2-，并用离子色谱法测定。结果表明，该法样品处理简单，干扰离子少，灵敏度高，能较准确测定出丙烯中的微量硫。     

An Electrochemical Investigation of Complexation of Pb(II) by a Well‐Characterized Fulvic Acid in Model Systems – Effect of Competition with Major Cations and Trace Metals

Effect of competition of major cations, Ca²⁺, Mg²⁺, and trace metals, Cu²⁺, Ni²⁺ and Zn²⁺, on the stability of the Pb(II)‐fulvic acid (FA) complexes in model systems at constant pH and ionic strength was investigated by square‐wave anodic stripping voltammetry (SWASV). The results show that the trace metals compete with the target trace metal, Pb(II), for binding sites of the FA even when they are present in the same concentration as that of Pb(II), whereas the major cations compete with Pb(II) only when they are present in massive excess.     

悬浮液进样-液体阴极辉光放电原子发射光谱法测定高纯氮化硅粉体中微量杂质元素

针对高纯氮化硅粉体中的9种微量杂质元素(Al、Ca、Co、Fe、K、Mg、Mn、Na、Ni),建立了悬浮液进样-液体阴极辉光放电原子发射光谱定量分析方法.考察了制备稳定悬浮液对样品颗粒度的要求,并通过六通阀将悬浮液引入液体阴极辉光放电原子发射光谱装置检测.本方法采用水溶液标准进行定量分析,无需对悬浮液的pH值进行精确调节,能够保持液体阴极辉光等离子体的稳定性.研究了仪器装置的操作电压、载液流速、光电倍增管积分时间等因素对检出限的影响.优化后得到的最佳实验条件为操作电压1080 V,载液流速1.2 mL/min,光电倍增管积分时间800 ms.利用六通阀进样系统对原有的液体阴极辉光放电原子发射光谱装置进行改进,从而实现悬浮液直接进样检测.用此装置对氮化硅实际样品进行检测,得到各种元素的检出限在0.2~53 mg/kg之间,RSD在1.1%~5.0%之间.通过对氮化硅标准参考物质ERM-ED101进行分析,其测定结果与高温高压消解-电感耦合等离子体发射光谱法一致,并与标准参考值吻合,表明此方法可用于氮化硅粉体的悬浮液直接进样检测,结果准确可靠,灵敏度高,具备应用价值.