氢化物发生及其在分析检测领域的应用

论述了氢化物发生的条件和普遍性及其在分析检测领域的应用,这些领域包括试样分解,分离富集,容量分析、比色分析、原子荧光光谱、原子吸收光谱、电感耦合等离子体原子发射光谱、电感耦合等离子体质谱等分析测试技术。     

生态地球化学评价湿沉降和悬浮物样品分析方法体系研究

探讨生态地球化学评价湿沉降、悬浮物样品分析体系中,进行多元素含量测定的分析测试新方法及样品的制备技术。根据待测元素的不同,分别采用微波消解、酸溶、碱熔等方法进行样品制备,使用原子荧光光谱法、离子选择电极法、电感耦合等离子体发射光谱法、电感耦合等离子体质谱法等进行样品的测定。文章系统地建立了生态地球化学评价湿沉降、悬浮物样品的多元素分析体系,利用建立的方法对不同种类的国家标准物质进行测定,结果令人满意。     

无机多元素现代仪器分析技术

本文重点介绍地质领域目前广泛应用的无机多元素现代仪器分析技术,包括电感耦合等离子体原子发射光谱(ICP-AES)、电感耦合等离子体质谱(ICP-MS)、X射线荧光光谱(XRF)、原子吸收光谱(AAS)、原子荧光光谱(AFS)、电子探针分析技术和共享平台的建立、激光剥蚀等离子体质谱(LA-ICP-MS)微区原位分析技术以...     

环境样品中钼的测定方法进展

根据多年来国内对钼的测定方法的研究报道,对环境样品中钼的主要测定方法进行总结,常用方法有分光光度法、催化极谱法、原子吸收分光光度法、ICP—AES法及ICP-MS等,分析了它们的优缺点,有利于选择适宜的测定方法。     

斯里兰卡曼泰遗址出土青花瓷的化学成分分析及产地初探

利用X射线荧光光谱、同步辐射X射线荧光光谱、中子活化、电感耦合等离子体原子发射光谱等多种技术手段分析了斯里兰卡曼泰遗址出土的7枚青花瓷残片的结构和成分。通过遗址出土部分青花瓷样品和中国各地瓷器样品的瓷胎元素含量聚类分析,初步判断其中的4枚青花瓷残片产自中国景德镇,而其余3枚样品的出处尚不能确定,需作进一步研究。     

生态地球化学土壤样品元素形态分析方法研究

对生态地球化学土壤样品,采用振荡提取法提取样品中离子交换态(包括水溶态)、碳酸盐结合态、腐殖酸结合态、铁锰氧化物结合态、强有机质结合态(包括部分硫化物);采用等离子体发射光谱法测定其中Cd、Co、Cr、Cu、Mn、Mo、Ni、Pb、Zn,原子荧光光谱法测定As、Hg、Sb、Se。方法的质量参数满足生态地球化学土壤样品评价形态分析的需要。     

Elemental Concentrations in Japanese Silicate Rock Standards JA-1, JR-1 and JB-2

Data on three Japanese geochemical reference samples (JR-1, JA-1, and JB-2) are presented. Ten major and thirty-five trace element concentrations were determined using x-ray fluorescence, instrumental thermal neutron activation, thermal neutron capture prompt gamma-ray spectrometry, delayed neutron assay, automated thermal neutron activation analysis, inductively coupled plasma emission, atomic absorption, and ion selective electrode. Good agreement between the various methods and with recent literature values were obtained using error weighted mean concentrations for the samples.     

Characteristics of distribution and chemical speciation of heavy metals in environmental mediums around Jinchang mining city,Northwest China

Heavy metal contamination was the main environmental problem around the Jinchang Ni–Cu mine area of Gansu, Northwest China. The concentration of heavy metals (Cr, Cu, Ni, Pb, and Zn) in various environmental mediums around the Jinchang Ni–Cu mine area were analyzed using atomic absorption spectrometry (AAS). The different chemical speciation of heavy metals was extracted using BCR (European Community Bureau of Reference) sequential extraction procedure, and the concentration of chemical speciation of each heavy metal was measured by inductively coupled plasma-atomic emission spectrometry. The results showed that Cu and Ni were the most important heavy metal pollutants in various mediums including cultivated soils, dust on slagheap surfaces, tailings, and sediments in waste water drains. In the tailings and sediments, the concentrations of Ni were obviously higher than those of Cu, whereas, in the soil and dust, the concentrations of Cu were higher than those of Ni. Analysis of chemical speciation indicated that Cr and Zn were mainly in residual fraction; Cu was mainly in oxidizable fraction; Ni was mainly in reducible fraction and acid soluble fraction; and Pb was mainly in reducible fraction and residual fraction. The extent of contamination of various environmental mediums was different because the heavy metals were derived from different sources. Furthermore, the mobility of various heavy metals was different because of the different distribution of chemical speciation.     

Heavy metals content and distribution in the surface sediments of the Guangzhou section of the Pearl River,Southern China

The long-term industrialization and urbanization of Guangzhou city may lead to heavy metal contamination of its aquatic sediment. Nevertheless, only few studies have been published on the distribution and contamination assessment of heavy metals in this urban river sediment. Thus, the major objective of this study was to quantitatively assess contamination of heavy metals and their chemical partitioning in the sediments of the Guangzhou section of the Pearl River (GSPR). Surface sediment samples were collected at 10 sites in the main river and 12 sites in the creeks of the GSPR. The total content of Cd was determined by graphite furnace atomic adsorption spectrometry (GF-AAS), and content of Cr, Cu, Pb and Zn was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The chemical partitioning of these heavy metals in the sediments of the main river was determined by the sequential selective extraction (SSE) method. Results indicated that the average total concentrations of Cd, Cr, Pb, Cu and Zn in the sediments of the main river were 1.44, 63.7, 95.5, 253.6 and 370.0 mg/kg, respectively, whereas they were 2.10, 125.5, 110.1, 433.7 and 401.9 mg/kg in the sediments of the creeks. The sediment at M4 and C9 sites was heavily contaminated with about 8 and 11 of toxic unit, respectively. Cr, Cu, Pb and Zn were mostly bound to organic matter and in the residual phase, whereas Cd was mostly associated with the soluble and exchangeable phase and the residual phase. The mobility and bioavailability of Cd, Zn and Cr in the sediments of the main river were relatively higher than Cu and Pb, due to higher levels in the soluble and exchangeable fraction and the carbonate fraction. The potential acute toxicity in the sediments of the main river and creeks was mainly caused by Cu contamination, accounting for 21.7–37.1% and 16.9–46.3% of the total toxicity, respectively, followed by Zn and Pb. Adverse biological effects induced by heavy metals would be expected in the sediments of the GSPR. Therefore, the sediments of the GSPR, especially at M4 and C9 sites, need to be remediated to maintain aquatic ecosystem health.     

Chemical availability of arsenic and heavy metals in sediments from abandoned cinnabar mine tailings

The understanding of the solid-phase speciation of arsenic in soils and sediments is important in the evaluations of its potential mobility and availability in the environment. The spoil heaps of abandoned mercury mines contain waste materials with high arsenic and heavy metals concentrations. The weathering of these tailings can cause their mobilization to the surroundings. In this work, the mobility and availability of arsenic and some heavy metals were evaluated in sediments from two heavily polluted mercury mining districts in Asturias (NW Spain). For this purpose, a slightly modified version of the Bureau Community of Reference sequential extraction scheme was applied to sediments. The total contents in the operationally defined fractions were analysed by inductively coupled plasma-atomic emission spectrometry. Extremely high total arsenic concentrations were found in all sediments ranging from 4,000 to 24,800 mg kg^?1. High easily mobilizable arsenic contents were found in the first mining area, related to the solubilization of Ca-bearing phases, supported by extracts analyses, X-ray diffraction results and the positive correlation found among the As and Ca fractionations. Ni and Zn were the most mobile among heavy metals, being Cr the least mobile, suggesting an anthropogenic origin due to the metallurgical processes, transport or dispersion generated from neighbour spoil heaps. In the second mining area, the bulk of As was concentrated in the residual phase, as well as Cr, Cu, Fe, Pb, Ti, indicating a mineralogical origin and the low availability of these elements. The strong correlations established between As and Fe and Ti distributions support the hypothesis that As is mainly associated to structural mineral phases in these sediments.     

GGR Biennial Review: Atomic Absorption,Inductively Coupled Plasma-Atomic Emission Spectrometry,Neutron Activation Analysis and X-Ray Fluorescence Spectrometry Review for 2008–2009

This review describes developments major and in trace element determination using atomic absorption spectroscopy (AAS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), instrumental neutron activation analysis (INAA), and X-ray fluorescence (XRF) spectrometry that were reported in 2008 and 2009. Publication levels were comparable to those of previous years, except for XRF which showed an increase in the number of articles published in the past 2 years. In terms of number of publications and impact, the most active field was AAS, while INAA was the least active. As expected for well-established and mature methods, novel developments for all four analytical techniques were relatively sparse. For AAS, the most notable publications concerned developments in sample introduction, particularly focussing on solid samples, increasing analyte sensitivity, and higher sample throughput. For ICP-AES, publication of developments in sample introduction, remediation of matrix effects and calibration continues. Compared with past years, there was a clear focus on sample preconcentration methods, but very few publications reporting new hyphenated speciation methods. For INAA, there were several publications exploring the accuracy and robustness of the method, as well as the requirements for INAA to meet criteria for a primary method of measurement. Two other related techniques, delayed neutron activation analysis, and prompt gamma activation analysis, were also described. Hyphenated XRF techniques showed interesting developments in enabling XRF and XRD analysis on the same spot, and further work characterising and calibrating three-dimensional micro-XRF shows promising results for investigating sample heterogeneity.     

废雷尼镍催化剂的组成分析

运用红外光谱、X射线粉末衍射、等离子体发射光谱、X射线光电子能谱、扫描电镜、元素分析等多种仪器分析手段,对一种废雷尼镍催化剂的组成进行全面分析,该废催化剂中镍元素的含量较高,具有较高的回收利用价值;通过实验得到其中组分镍、铝、钙、铁、钼、铜、硅的定量信息和部分定性信息,建立了废雷尼镍催化剂中镍回收利用的技术方案。     

高钙碳酸盐地质样品中铜镍的测定

用电感耦合等离子体质谱法和电感耦合等离子体发射光谱法测定高钙碳酸盐样品中的铜和镍。通过试验分析了高钙碳酸盐样品中钙对铜、镍测定的影响,并确定其影响因子,提出两套检测高钙碳酸盐样品中铜、镍的方案。方法经国家标准物质验证,测定值与标准值相符;相对标准偏差(RSD,n=10)两元素均小于2%。     

电感耦合等离子体发射光谱法测定重晶石矿石中BaSO4和Sr

采用电感耦合等离子体发射光谱法同时测定重晶石矿石中Ba、Sr,再将Ba换算成BaSO₄.研究了基体对Sr测定的影响及消除.Ba、Sr相对标准偏差（RSD,n=12）分别为0.74%、3.3%.本方法简便、快速,准确.     

泡塑吸附-电感耦合等离子体发射光谱法测定矿石中的金

试样在650℃烧制、王水溶解、泡塑振荡吸附、硫脲解脱,用电感耦合等离子体发射光谱法测定矿石中的金量,克服了原子吸收光谱法对低含量金测定稳定性和精密度差、对高含量金测定分取误差大和返工率高等不足,缩短了分析时间。方法经国家一级标准物质分析验证,结果与标准值相符。对二级标准物质测定的方法精密度(RSD,n=12)为6.45%。方法检出限为0.138μg/g,线性范围宽,适用于矿石中0.2μg/g以上金的测定。     

江西德兴矿集区水系沉积物重金属污染的时空对比

对比研究矿山开采一定时段内区域环境污染的时空变化特征,对于动态监测矿山开采对区域环境质量的影响情况、污染趋势等,具有重要的科学意义和实际价值。本文在利用2004年野外采集与测试分析的330个水系沉积物样品重金属含量数据基础上,充分利用矿山开采早期(1989)的1:20万乐平幅(As、Hg、Cd、Cr、Zn、Cu、Pb)水系沉积物地球化学图,通过数据预处理,分别对样品采集点重金属元素含量的统计分析和地质累积指数法评价的基础上,采用GIS的三维空间分析功能,对比研究德兴地区水系沉积物重金属污染时空变化。研究结果表明,十几年来,矿山开采对区域水系沉积物已造成了严重的污染,主要集中分布在是德兴铅锌和铜钼矿区德兴河与大坞河流域及其周边地区、乐安河下游沿岸局部地区、西北煤矿区以及乐安河下游乐平附近的煤矿区。     

Recent Developments in Trace Element Analysis by ICP-AES and ICP-MS with Particular Reference to Geological and Environmental Samples

This review describes recent developments in trace element analysis using inductively coupled plasma-atomic emission spectrometry (ICP-AES) and inductively coupled plasma-mass spectrometry (ICP-MS). It aims to focus on the application of ICP techniques to geological and environmental samples. Therefore, fundamental studies in ICP-MS and ICP-AES instrumentation have largely been ignored. Whereas the majority of literature reviewed related to ICP-MS, indicating that ICP-MS is now the preferred technique for all geological analysis, there is still a steady development of ICP-AES to environmental applications. It is clear that true flexibility in elemental analysis can only be achieved by combining the advantages of both ICP-AES and ICP-MS. Two particular groups of elements (long-lived radionuclide and the platinum-group elements) stood out as warranting dedicated sections describing analytical developments these areas.     

基于污染指数法和GIS技术评价江西德兴矿区土壤重金属污染

以江西德兴大型矿区为例,进行大尺度的土壤环境调查和重金属污染评价。系统采集该区域919个土壤样品,在应用X荧光光谱仪和电感耦合等离子原子发射光谱仪为主体的分析配套方案分析土壤样品中重金属含量的基础上,采用单因子污染指数法和综合污染指数法,分别从原始含量、污染指数以及基于GIS的污染空间分析3个方面进行该矿区的土壤重金属污染评价。结果表明,矿山开采对该区的土壤环境造成了不同程度的As、Cd、Zn、Cu重金属污染。污染区域主要分布在德兴铜钼和铅锌矿区、乐安河下游乐平附近的煤矿区以及南部电化学厂附近。     

电感耦合等离子体发射光谱法快速测定钼铁合金中的钼

用电感耦合等离子体发射光谱法测定钼铁中的钼,优化了仪器操作条件,克服了常规重量法测定钼铁中钼步骤繁琐、耗时长、工作量大的不足。方法简便易行,快速准确,分析误差在化学分析允许的误差范围内,能替代原有的化学分析方法,基本满足生产和科研的要求。     

Enrichment of heavy metals in coal gangue by puff balls and mechanism research

Coal gangue with/without wild puff balls growing on or covering up were analyzed by means of inductively coupled plasma atomic emission spectrometry （ICP-AES） and atomic fluorescence spectrometry （AFS） to detect the contents of heavy metal elements in the plants. Seven heavy metals were chosen to do the experiments, which showed that the puffballs have strong enrichment capacity for heavy metals （As, Pb, Mn and Ni）. The highest enrichment level was Mn, 220.3 mg/kg （dry weight） for puffball fruiting bodies, and the highest As, Cr and Pb enrichment levels for puffball mycelium were 111,265.3 and 86 mg/kg, respectively. Cd, Mn and Ni could transfer from puffball mycelium to its fruiting bodies, while As, Cr, Pb and Co mainly accumulated in the mycelium. The contents of five organic acids （tartaric acid, glycolic acid, lactic acid, citric acid and malic acid） in puffballs were determined with high performance liquid chromatography. With water, ethanol and ethyl acetate as solvents, the puffball extracts performed dissolution reactions with coal gangue, in which the water extract （containing a large amount of organic acids） was most effective in releasing heavy metals, especially As, Pb, Cr, Mn, Co and Ni from coal gangue. As a pioneer species, puff balls absorbed the hazardous trace elements in coal gangue matrix to reduce its eco-toxicity, on the other hand, it raised the pH value of coal gangue, improving the vegetation growing conditions for coal gangue matrix to a certain extent and laying the foundation for ecological restoration of coal gangue dumps.