基体改进剂在电感耦合等离子体质谱分析中的应用

基体改进剂在电感耦合等离子体质谱仪(ICP-MS)中的应用引起了人们很大的关注,对近年来化学改进剂在ICP-MS中的应用进展作了介绍,对各种改进剂的改进效果及机理进行阐述。     

浅析电感耦合等离子体质谱法测定水中镉的质量控制

电感耦合等离子体-质谱(ICP-MS)法测定水中镉在环境监测系统得到了广泛应用,本文主要从实验室内部控制和实验室外部控制两个角度来对电感耦合等离子体-质谱(ICP-MS)法测定镉的环境监测质量控制进行分析。     

电感耦合等离子体质谱技术在环境监测中的应用进展

电感耦合等离子体质谱技术(ICP-MS)是目前发展最快的痕量元素分析测试技术之一。由于该技术提供了极低的检出限、极宽的动态线性范围,干扰少、分析精密度高,可进行多元素同时快速分析,可与多种分离技术及样品前处理方法和进样方法相结合等优点,得到了迅速的发展。介绍了ICP-MS的基本原理及仪器构造、与其他分析测试技术的比较及发展趋势,并着重介绍了其在环境监测和环境科学研究领域的应用。     

环境样品中~(237)Np的ICP-MS分析研究进展

近年来,环境样品中237Np的准确测量受到越来越多的关注。随着质谱技术的发展,电感耦合等离子体质谱(ICP-MS)成为研究和测量环境样品中237Np的重要手段。文章从样品制备、定量方法、干扰降低、进样系统改进、与色谱联用等方面,对ICP-MS分析环境样品中237Np的研究进展作了评述。     

原子荧光法和电感耦合等离子体质谱法测定水中锑的比较

分别用原子荧光法(AFS)和电感耦合等离子体质谱法(ICP-MS)测定水中锑。AFS法和ICP-MS法均线性良好,相关系数分别为0.999 8和0.999 9,检出限分别为0.17和0.03μg/L,相对标准偏差均1.15%,加标回收率分别为96.6%~111.9%和95.4%~111.5%,2种方法均能很好地用于水中锑的测定。其中,ICP-MS法适合较清洁地表水和地下水样品中锑的分析,AFS法则对地表水、地下水和废水样品均适用。     

南极大气气溶胶中铅同位素比值的研究

通过对电感耦合等离子体质谱(ICP-MS)的工作条件和参数进行优化,建立了ICP-MS测定铅同位素比值的精确方法,测量了2007—2009年南极中山站采集到的气溶胶样品中208Pb/206Pb、207Pb/206Pb和206Pb/207Pb的比值。结果表明,南极大气气溶胶中铅同位素比值在逐年缓慢地发生线性变化,线性相关系数为0.996 2;气溶胶铅同位素示踪揭示南极附近国家(除南非)释放的铅可能成为南极大气中铅的重要来源。     

官厅水库重金属污染状况调查研究

为确保北京市饮用水源安全,2007年对官厅水库中重金属进行了筛选性调查.采用电感耦合等离子体质谱仪(ICP-MS),对官厅水库枯水期和丰水期水体中的金属元素含量进行了全面的分析.监测结果表明,水库在丰水期砷含量偏高,整体水质状况良好,重金属污染程度轻微.     

电感耦合等离子体质谱法测定地下水中痕量元素

采用电感耦合等离子体质谱法(ICP-MS)同时测定地下水中痕量元素。结果表明,ICP-MS可同时测定地下水中的16种元素,方法检出限为0.02~0.2μg/L,元素的精密度(RSD,n=5)为1.46%~4.36%,加标回收率为96.6%~105.6%,符合环境监测无机组份测试质量控制的要求。该方法应用于直接测定元素浓度范围在ng/L~mg/L级的实际地下水样品,具有样品前处理简单、干扰少、测定快速、元素同时分析、省时省力等优点。     

电感耦合等离子体质谱法测定尘土样品中贵金属元素的研究

建立了用电感耦合等离子体质谱法(ICP-MS)测定尘土样品中贵金属元素Au、Pt、Pd、Ir、Ru、Rh的方法.样品用王水微波消解后,试液直接用ICP-MS同时测定上述6种贵金属元素.以Sc、Y、In作为内标物质,补偿了基体效应;选择适当的待测元素同位素克服了质谱干扰;确定了最佳测定条件.结果表明,6种贵金属元素的检出限为0.004～0.006 μg/L,线性关系良好,相关系数r≥0.999 2,回收率为83%～97%,RSD＜3.6%.该法准确、快速、简便,已成功地应用于尘土样品中微量贵金属元素的测定.     

三重四极杆电感耦合等离子体质谱法测定水中痕量磷的方法建立及在新安江水库的应用

建立了三重四极杆电感耦合等离子体质谱法（ICP-MS/MS）测定地表水中痕量总磷、溶解态磷、颗粒态磷的方法，确定了ICP-MS/MS测定水中磷的仪器参数及氧气流量。研究了该方法检测水中磷元素的检出限、精密度、正确度，探索了浊度、色度及砷、铬、硫的存在对ICP-MS/MS测磷的影响。结果表明，采用高纯氧气反应ICP-MS/MS法可对地表水中的各形态痕量磷进行质量浓度检测，该方法的检出限可达0.24 μg/L，磷元素在1.00～1 000 μg/L 质量浓度范围内具有良好的线性，相关系数为0.999 5，加标回收率为 92%～103%。该方法检测速度快，抗浊度、色度及共存元素（砷、铬、硫）干扰的能力强。对新安江水库4个季度的总磷、溶解态磷、颗粒态磷进行测定，结果表明，水库总磷平均质量浓度为10～20 μg/L，ρ（溶解态磷）/ρ（总磷）为42.4%～50.9%。该方法可以满足地表水中痕量磷的快速测定及形态分析。     

等离子发射光谱-质谱(ICP-MS)直接用于饮用水中的砷、锑、硒测定研究

用等离子发射光谱和等离子发射光谱-质谱作比较,等离子发射光谱-质谱用于饮用水As、Sb、Se的测量时需考虑校正系数,通过不确定度分析,确定了ICP-MS测定方法不确定度大小,得出结论:不要氢化物发生器,不加EDTA作为掩蔽剂,也可以直接用于实际.     

Methodologies for determination of antimony in terrestrial environmental samples

Methodologies for the environmental analysis of total antimony and aqueous chemical speciation are critically reviewed, including preparation techniques for aqueous and solid matrices and the determination of solid state partitioning and recommendations are given for future research directions. Concentrations of total antimony commonly present in aqueous and solid environmental samples are readily determined using present day analytical techniques. This has resulted primarily from technological advances in microwave digestion for solid matrices and the development of plasma based analyte detection systems. ICP-AES and ICP-MS techniques are both utilised for the environmental analysis of total antimony concentrations. However, ICP-MS is increasingly favoured as a result of reduced spectral interferences and the potential for analyte detection in the pg mL(-1) range. Determination of aqueous antimony speciation presents a number of complex analytical challenges and highly selective separation and identification techniques are required prior to detection. The majority of published techniques including common applications of hydride generation are insufficiently selective for the determination of intrinsic chemical speciation and often only oxidation state data are obtained. The recent in-line applications of HPLC-ICP-MS offer the potential for highly selective separations of aqueous antimony species and determination of detailed chemical speciation data. However, considerable development work is required to optimise chromatographic separations and identify uncharacterised species resident in environmental systems. Analytical techniques to aid the determination of antimony's associations with solid environmental matrices include the application of chemical extraction procedures and leaching experiments. To date, this area of analytical research has received little attention and further studies are required to elucidate this aspect of antimony's environmental chemistry.     

Comparison of different multielement techniques for analysis of mosses used as biomonitors

Mosses are used as biomonitors on a regular basis to study trends in the atmospheric deposition of trace elements in Norway. In this paper the analytical scheme used so far, based on a combination of instrumental neutron activation analysis and atomic absorption spectrometry (INAA/AAS) is compared with inductively coupled plasma emission spectrometry (ICP-ES) and inductively coupled plasma mass spectrometry (ICP-MS). ICP-ES provided satisfactory data for nearly 20 elements, but detection limits were inadequate for some elements of importance. For ICP-MS quantitative data were obtained for 33 elements including the heavy metals of key interest in air pollution studies. In most cases where comparison was possible the ICP-MS data compared favourably with data obtained by the reference scheme or by ICP-ES. On the basis of this study ICP-MS is considered to be an equivalent alternative to INAA/AAS in multielement studies using mosses as biomonitors. In addition ICP-MS offers some promise for the study of elements such as Be, Ga, Mo, Te, Tl, and Bi, for which very little information exists regarding their behaviour as air pollutants.     

Development of a simple extraction cell with bi-directional continuous flow coupled on-line to ICP-MS for assessment of elemental associations in solid samples

A continuous-flow system comprising a novel, custom-built extraction module and hyphenated with inductively coupled plasma-mass spectrometric (ICP-MS) detection is proposed for assessing metal mobilities and geochemical associations in soil compartments as based on using the three step BCR (now the Measurements and Testing Programme of the European Commission) sequential extraction scheme. Employing a peristaltic pump as liquid driver, alternate directional flows of the extractants are used to overcome compression of the solid particles within the extraction unit to ensure a steady partitioning flow rate and thus to maintain constant operationally defined extraction conditions. The proposed flow set-up is proven to allow for trouble-free handling of soil samples up to 1 g and flow rates < or =10 mL min(-1). The miniaturized extraction system was coupled to ICP-MS through a flow injection interface in order to discretely introduce appropriate extract volumes to the detector at a given time and with a given dilution factor. The proposed hyphenated method demonstrates excellent performance for on-line monitoring of major and trace elements (Ca, Mn, Fe, Ni, Pb, Zn and Cd) released when applying the various extracting reagents as addressed in the BCR scheme, that is, 0.11 M CH(3)COOH, 0.1 NH(2)OH.HCl and 30% H(2)O(2), even when a well recognized matrix-sensitive detector, such as ICP-MS, is used. As a result of the enhanced temporal resolution of the ongoing extraction, insights into the breaking down of phases and into the kinetics of the metal release are obtained. With the simultaneous multielement detection capability of ICP-MS, the dynamic fractionation system presents itself as an efficient front-end for evaluation of actual elemental association by interelement comparison of metals leached concurrently during the extraction time. Thus, the intimate elemental association between Cd and Zn in contaminated soils could be assessed.     

异丙醇增感电感耦合等离子体质谱法直接测定土壤和沉积物中硒

提出了沸水浴混合酸法消解,以异丙醇为增感剂,电感耦合等离子体质谱直接测定土壤和沉积物中硒的方法。实验表明2mol/L硝酸-4mol/L盐酸混酸能有效溶出土壤和沉积物中各种形态的硒。相对于1%硝酸基体,4%(V/V)异丙醇基体中硒的ICP-MS响应值提高了12.1倍;而且4%(V/V)异丙醇基体可有效抑制硒的质谱干扰。ICP发射功率和雾化气流速是影响异丙醇在ICP-MS测定过程增敏效应的主要因素。以78硒为测定同位素,方法检出限为0.005mg/kg,实际样品测定精密度均小于5%。用于测定土壤和沉积物国家标准样品并对其消解液进行加标回收实验,结果令人满意。     

ICP-MS碰撞池技术消除复杂水样中硒的基体干扰

通过测定深圳某河流水样中的主要成分，确定ICP—MS碰撞模式测定se的主要基体干扰，并对碰撞气流量进行条件优化和水样基体干扰消除试验，确定当氦气流量为3．0L／min时，测定77Se的干扰能基本被消除。该方法测定实际水样的结果与原子荧光法的测定值无显著差异。