同位素稀释电感耦合等离子体质谱测定环境和生物样品中的镉

建立电感耦合等离子体质谱(ICP-MS)测定镉同位素比值的方法,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.     

氢化物发生电感耦合等离子体原子发射光谱同时测定土壤中十四种微量元素

近年来,已经有人用分光光度法,原子荧光光谱法,原子吸收法,X射线荧光光谱法,电感耦合等离子体质谱(ICP-MS)以及电感耦合等离子体原子发射光谱(ICP-AES)等方法测定土壤中某些重金属的含量,但这些方法各有一定局限性.本文利用自制新型雾化器与高盐雾室和PRODIGY型全谱直读电感耦合等离子体发射光谱仪相联,改制成氢化物发生器,操作灵活、方便,在一定优化条件下使Hg、Bi、As、Pb检出限降低了2—125倍,可以同时对氢化物和非氢化物进行检测,测定土壤标准样品可以获得满意的结果.     

ICP-MS测定《全国土壤污染状况详查》项目中14种元素

本文建立了电感耦合等离子体质谱(ICP-MS)同时测定土壤中14种元素的分析方法,14种元素的方法检出限均满足同类分析标准要求.使用本方法分析了10种土壤和沉积物标准物质,其测定值均在参考范围之内.应用该方法连续分析土壤标准物质4.5 h,14种元素的相对标准偏差(RSD)均小于5%,回收率在90%—107%.通过高基体进样系统(HMI)的使用,增强了ICP-MS对复杂基体的耐受性,大大延长了仪器的维护周期,实现了与火焰原子吸收分光光度法(FAAS)和电感耦合等离子体发射光谱法(ICP-OES)样品前处理方法的一致性.为提高土壤样品前处理效率,本文还探索了三酸"快速浸提法",并利用10种土壤标准物质验证了该方法的准确性.     

测定废弃线路板中重金属的酸消解方法比较

重金属含量一般采用原子吸收光谱仪(AAS)、电感耦合等离子体发射光谱仪(ICP-MS,ICP-AES)等方法测定.测定前需要对固体样品进行预处理.目前,常用的预处理方法有直接加热酸消解法、微波消解法和高压釜消解法等.而直接加热酸消解法是目前相对最常用的方法.     

中国大气颗粒物中重金属监测技术与方法综述

大气颗粒物中的重金属极易富集在细颗粒物中,并对人体带来危害。文章对中国大气颗粒物中重金属的监测技术方法进行梳理和汇总,从点位布设、样品采集、样品前处理、分析测试以及全过程的质量保证和质量控制等方面。探讨和分析颗粒物监测的各个环节应遵循的技术规范和相关方法。大气颗粒物的采样主要包括环境空气样品和无组织排放样品两大类,前处理方法包括全消解和酸浸提,而全消解中又包括酸消解法和碱熔法,消解方式包括电热板、马弗炉、高压密闭消解罐、微波消解等。测试方法主要包括分光光度法、X射线荧光光谱法(XRF)、原子吸收分光光度法(AAS)、原子荧光光谱法(AFS)、电感耦合等离子体发射光谱法(ICP-AES)、电感耦合等离子体质谱法(ICP-MS)等,根据不同的监测需求和仪器设备水平,选择不同的标准测试方法作为依据。在颗粒物重金属监测的全过程中,从布点、试剂空白、滤膜/滤筒空白的控制,到采样、前处理、实验室分析等各个环节,均需要考虑可能影响分析准确度的因素,建立起与监测方法同步的全程序质量保证和控制措施。完善大气颗粒物中重金属监测技术与方法体系,可为大气环境监测和管理部门的决策提供科学依据和技术支持,为源解析等颗粒物组分分析相关工作提供方法依据。     

不同酸化体系测定中国不同地区土壤重金属的比较研究

本文采用硝酸-氢氟酸-盐酸-过氧化氢(5∶1∶1∶1)的消解体系和硝酸-过氧化氢(6∶2)消解体系,均通过微波消解法和电感耦合等离子体质谱法(ICP-MS)测定土壤中的铬、镍、铜、锌、砷、镉、铅等7种元素.分析了来自全国不同地区的9种土壤与水系沉积物的质控样品,研究了全量微波消解酸体系对土壤中7种重金属测定的影响.结果表明,对于Cr和Pb元素,硝酸-过氧化氢消解体系可溶态元素的结果显著低于元素全量的结果,未加入氢氟酸,难以将硅晶格中的Cr和Pb析出.对于As元素,硝酸-氢氟酸-盐酸-过氧化氢消解体系的回收率略有偏高,推测其原因为盐酸引入的氯离子对ICP-MS的测定产生了质谱型干扰,因此消解体系应尽量避免引入氯.对于Ni、Cu和Zn的结果,硝酸-过氧化氢消解体系的回收率在75%—110%的范围,两种消解体系结果的偏差较小,硝酸-过氧化氢法测定的可溶态元素的结果可以较好的反映元素全量的水平.对比不同地区土壤的结果发现,除水系沉积物和砖红壤中的Pb及砖红壤中的Cr,土壤中部分Cr和Pb难以被硝酸-过氧化氢体系消解出来,在环境中处于稳定的状态,因此采用硝酸-过氧化氢体系能更准确地评估Cr和Pb对环境的危害.     

离子色谱在砷化物形态分析中的应用

砷的分析方法最初有光度法、原子吸收光谱法和极谱法等，但这些方法仅能用于总砷，不能用于砷的形态分析．因而又发展了电感耦合等离子体质谱法(ICP-MS)、离子色谱法(IC)、气相色谱法、气相色谱-原子吸收光谱联用、液相色谱-质谱联用、离子色谱-电感耦合等离子体质谱、离子色谱-原子吸收／发射光谱联用技术等．由于砷化物在水中多以离子形式存在，采用离子色谱法能同时分析不同形态的砷离子．同时，采用电感耦合等离子体质谱及原子吸收光谱测定砷化物具有较高的灵敏度，因此，离子色谱及离子色谱与电感耦合等离子体质谱、原子吸收／发射光谱的联用技术在砷化物的形态分析中得到了较多的应用^[1-8]。     

电感耦合等离子体质谱法直接测定酱油中的铅

采用电感耦合等离子体质谱(ICP-MS)法直接测定酱油样品中的痕量铅,样品无需前处理与稀释,直接进行测定.外标法绘制工作曲线、在线内标法校准基体效应,方法简便、快速.根据所建立的方法,对实验室间比对实验的酱油考察样品进行了分析,测定值与参考值吻合,相对标准偏差为2.5%.用加标回收实验评价了该方法的准确性,回收率为94.2%-102%,结果令人满意.     

超级微波消解-ICP-MS法测定人工沉香中的11种无机元素

本文采用超级微波消解对样品进行前处理,以钪、锗、铑、铟、铼和铋作为内标物消除基体干扰,碰撞/反应池技术消除质谱干扰的方式测定了人工沉香中的铝、铬、锰、铁、铜、锌、砷、镉、钡、汞和铅.建立超级微波消解-电感耦合等离子体质谱(ICP-MS)法测定人工沉香中的11种无机元素,并收集两种结香方法10批人工沉香样品进行测定.结果表明,所测元素在相应的测定范围内线性关系良好,相关系数为0.9991—0.9999,方法检出限为0.001—3 mg·kg~(-1),相对标准偏差为1.4%—5.5%,加标回收率为85.6%—109%,标准物质的测定结果与认定值相符.     

微波消解ICP-MS法测定空气颗粒物中54种元素

正目前我国环境空气颗粒物中元素测定的标准方法为原子荧光法和原子吸收分光光度法,电感耦合等离子体质谱法(ICP-MS)作为新发展起来的无机元素分析测试技术,能够弥补上述方法的局限性,具有检出限低、线性范围宽、灵敏度高、快速简便、一次可测定多种元素等优点.本文将微波消解技术与电感耦合等离子体质谱法结合,快速准确地测定颗粒物中54种元素,并用该方法对京津冀     

Extraction of arsenic species in soils using microwave-assisted extraction detected by ion chromatography coupled to inductively coupled plasma mass spectrometry

We have developed a novel microwave-assisted extraction method for determining the arsenic (As) speciation in soils that is based on extraction with phosphate solutions, including orthophosphoric acid, ammonium dihydrogen orthophosphate, and ammonium hydrogen orthophosphate. The highest extracting efficiency was obtained with 1 M ortho-phosphoric acid solution as the extractant, and this efficiency is associated with the pH of the extractant. Total As content and As species in the soil extracts were determined by inductively coupled plasma mass spectrometry (ICP-MS) alone and by the combined ion chromatography (IC) with ICP-MS, respectively. The proposed extraction procedure was applied to National Institute of Standards and Technology (NIST) standard reference material (SRM) 2711 (Montana soil) as well as to environmental soil samples collected from the agricultural lands of Bangladesh. As(V) was detected in all the soil samples, and As(III) was detected in nine soils of the 20. These results of extractable As testing indicate that the extraction of As species mainly depends on the composition of the soils. The As speciation results also indicate that As adsorption is highly dependent on the iron, aluminum, and manganese concentrations in the soil. The stability of As species in the extracts was also studied.     

ASD—ICP—MS联合快速测定土壤中部分金属元素

土壤环境质量例行监测正在全国展开,如何准确快速分析土壤中的金属含量成为当务之急。采用HNO3-HCl-HF—HClO4体系在全自动消解仪（ASD）上对土壤进行前处理,以50．0μg／L的铑作内标,电感耦合等离子体-质谱仪同时测定《土壤环境质量标准》的7种元素：Cd、As、Cu、Ph、Cr、Zn、Ni。各元素的方法检出限为0．003～0．40mg／kg,相对标准偏差小于6．0％,土壤标样的测定值与标准值吻合。该方法简便快捷、灵敏度高、重现性好,为大批量土壤重金属元素含量的快速测定提供了可靠地消解-分析方法。     

Metals and organic pollutants in snow surrounding an iron factory

To estimate air pollution snow samples were collected in March 2001 at six sites in the vicinity of the Kostomuksha factory in Karelia. Seventy-two chemical elements and more than 200 individual organic compounds were identified by inductively coupled plasma mass spectrometry (ICP-MS) and gas chromatography mass spectrometry (GC-MS). It was found that the levels of Li, B, Al, Fe, Ni, Cu, Zn, Hg, Mn, Mo as well as hydrocarbons, phthalates and phenols exceeded the existing maximum allowable concentrations. A list of toxicants emitted with the factory exhausts and a list of priority pollutants for Kostomuksha were compiled. The impact of the exhausts of the Kostomuksha factory on the environment in Finland is relatively small. Electronic Publication     

Assessment of potentially toxic elements in Swiss chard and sediments of Akaki River,Ethiopia

For the determination of 15 potentially toxic elements (V, Cr, Fe, Mn, Co, Ni, Cu, Zn, As, Se, Ag, Cd, Sn, Hg, and Pb) in plant and sediment samples of the Akaki River, Ethiopia, inductively coupled plasma–mass spectrometry, inductively coupled plasma–optical emission spectrometry, and a RA-915+ mercury analyzer were applied. Sediment and plant samples were mineralized using a closed-vessel microwave-assisted digestion system. The elemental concentrations varied considerably in plant and sediment samples. The minimum concentration was observed for known toxic elements (As, Hg, and Cd) while the highest concentration was observed for the elements of relatively low toxicity Zn, Mn, and Fe. The concentration of Cr, Fe, Pb, Zn, and As in Swiss chard surpassed the maximum permissible levels at specific sites. At some of the sites, the sediment quality guidelines are surpassed for Cu, Zn, and Pb.     

电感耦合等离子体质谱法测定饮料中的铀

建立了电感耦合等离子体质谱法(ICP-MS)测定饮料中的铀.对不同基质的饮料进行了前处理方法的摸索,从精密度和回收率考察了方法的准确性,相对标准偏差(RSD)为1.67%-8.21%(n=6),加标回收率为96.0%-109.0%,方法检出限为0.010μg·l~(-1),方法准确可靠.     

Identification and apportionment of sources of lead in human tissue

A brief review of the use of stable lead isotope ratio measurements to identify and apportion sources of lead in human tissue is followed by examples of the use of inductively coupled plasma source mass spectrometry for such studies. Inductively coupled plasma source mass spectrometry (ICP-MS) has only recently been used for measurements of coupled ratios in body tissues and fluids and in environmental sources of lead. Generally, the inaccuracy of these measurements is about −0.2% and the imprecision less than 0.5%. This analytical performance is sufficient to detect the much larger changes in²⁰⁶Pb:²⁰⁷Pb ratios of −2% or higher, seen in environmental lead exposure and in childhood lead poisoning. Measurements of lead isotope ratios by ICP-MS have been used to identify specific sources of childhood lead poisoning and to indicate the relative importance of environmental sources, such as drinking water and lead from petrol. Populations in the United Kingdom with low lead uptake usually have²⁰⁶:Pb²⁰⁷Pb ratios in body tissues within the range 1.13 ± 0.01. Significant deviations from this range have been seen in response to increased uptake from lead in: drinking water in parts of Scotland (source ratio ∼1.18 and petrol lead in inner London (source ratio ∼1.07). The dominant source for some Scottish subjects with high concentrations of lead in blood or in teeth was water, which contributed approximately 60% to body lead. Petrol lead was shown to be a significant contributor (30–40%) to the body lead of inner London children.     

润肤霜类化妆品中金属元素的测定及砷形态初探

采用电感耦合等离子体质谱(ICP-MS)测定化妆品中的金属元素铝、铬、镍、铜、锌、砷、硒、镉、锡、锑、钡、镧、铈、镨、钕、钐、汞、铅的总量,并结合液相色谱(HPLC)-ICPMS联用技术考察了化妆品中的砷形态.研究表明,金属指标不合格的化妆品多为汞含量超标;此外,化妆品中的砷多以无机砷形式存在.     

Geochemistry,mineralogy, solid-phase fractionation and oral bioaccessibility of lead in urban soils of Lisbon

An urban survey of Lisbon, the largest city in Portugal, was carried out to investigate its environmental burden, emphasizing metallic elements and their public health impacts. This paper examines the geochemistry of lead (Pb) and its influence on human health data. A total of 51 soil samples were collected from urban recreational areas used by children to play outdoors. The semi-quantitative analysis of Pb was carried out by inductively coupled plasma mass spectrometry after an acid digestion. X-ray diffraction was used to characterize the soil mineralogy. The solid-phase distribution of Pb in the urban soils was investigated on a subset of 7 soils, out of a total of 51 samples, using a non-specific sequential extraction method coupled with chemometric analysis. Oral bioaccessibility measurements were obtained using the Unified BARGE Method developed by the Bioaccessibility Research Group of Europe. The objectives of the study are as follows: (1) investigation of Pb solid-phase distribution; (2) interpretation of Pb oral bioaccessibility measurements; (3) integration of metal geochemistry with human health data; and (4) understanding the influence of geochemistry and mineralogy on oral bioaccessibility. The results show that the bioaccessible fraction of Pb is lower when major metal fractions are associated with less soluble soil phases such as Fe oxyhydroxides, and more increased when the metal is in the highly soluble carbonate phase. However, there is some evidence that the proportion of carbonates in the soil environment is also a key control over the oral bioaccessibility of Pb, irrespective of its solid-phase fractionation.     

Earthworms and in vitro physiologically-based extraction tests: complementary tools for a holistic approach towards understanding risk at arsenic-contaminated sites

The relationship of the total arsenic content of a soil and its bioaccumulation by earthworms (Lumbricus rubellus and Dendrodrilus rubidus) to the arsenic fraction bioaccessible to humans, measured using an in vitro physiologically-based extraction test (PBET), was investigated. Soil and earthworm samples were collected at 24 sites at the former arsenic mine at the Devon Great Consols (DGC) in southwest England (UK), along with an uncontaminated site in Nottingham, UK, for comparison. Analysis of soil and earthworm total arsenic via inductively coupled plasma mass spectrometry (ICP-MS) was performed following a mixed acid digestion. Arsenic concentrations in the soil were elevated (204–9,025 mg kg⁻¹) at DGC. The arsenic bioaccumulation factor (BAF) for both earthworm species was found to correlate positively with the human bioaccessible fraction (HBF), although the correlation was only significant (P ≤ 0.05) for L. rubellus. The potential use of both in vitro PBETs and earthworms as complementary tools is explored as a holistic and multidisciplinary approach towards understanding risk at contaminated sites. Arsenic resistant earthworm species such as the L. rubellus populations at DGC are presented as a valuable tool for understanding risk at highly contaminated sites.     

Nano-capillary electrophoresis for environmental analysis

Many analytical techniques have been used to monitor environmental pollutants. But most techniques are not capable to detect pollutants at nanogram levels. Hence, under such conditions, absence of pollutants is often assumed, whereas pollutants are in fact present at low but undetectable concentrations. Detection at low levels may be done by nano-capillary electrophoresis, also named microchip electrophoresis. Here, we review the analysis of pollutants by nano-capillary electrophoresis. We present instrumentations, applications, optimizations and separation mechanisms. We discuss the analysis of metal ions, pesticides, polycyclic aromatic hydrocarbons, explosives, viruses, bacteria and other contaminants. Detectors include ultraviolet–visible, fluorescent, conductivity, atomic absorption spectroscopy, refractive index, atomic fluorescence spectrometry, atomic emission spectroscopy, inductively coupled plasma, inductively coupled plasma–mass spectrometry, mass spectrometry, time-of-flight mass spectrometry and nuclear magnetic resonance. Detection limits ranged from nanogram to picogram levels.