邻羟基苯基重氮氨基偶氮苯分光光度法测定地质样品中的痕量铊

１引言 铊是稀散元素，在制造电子元器件、化学、玻璃及半导体工业等领域有重要用途。铊也是剧毒元素，其毒性为氧化砷的３倍多。随着铊的使用日益增多，它的环境效应引起了人们的关注，因此铊的分析工作越来越重要。近年来，水相胶束增溶分光光度法测定铊的研究日趋增加。邻羟基苯基重氮氨基偶氯苯（Ｏ－ＨＤＡＡ）曾用于锌、银、镉、镍、钴等的光度分析。本文详细研究了在 Ｔｒｉｔｏｎ Ｘ－１００存在下，Ｏ－ＨＤＡＡ与铊的高灵敏显色反应。聚胺酯泡沫塑料对铊有很好的吸附性能，本文用于分离富集铊。建立了一个在水相体系中快速、准确…     

铊的环境污染与迁移转化

从铊的环境污染途径及其在环境中迁移转化等方面,分析了铊这一分散剧毒元素的表生地球化学行为,环境迁移,分散富集规律和特征,铊的环境污染研究方向和内容。     

镉试剂2B分光光度法测定地质样品中痕量铊

１引言 铊属高毒元素,且有积蓄性,列为优先监测的对象之一。在铊的分光光度分析法中,用得最普遍的是萃取光度法。大量使用有毒的有机溶剂将污染环境和损害健康。因此,水相胶束增溶分光光度法测定铭的研究日益增加。镉试剂及其衍生物作为铊的显色剂已有报道,但未见使用镉试剂２Ｂ的详文。本文详细研究了在Ｔｔｒｉｔｏｎ Ｘ－１００存在下,镉试剂２Ｂ与铊的显色反应。聚胺酯泡沫塑料对铊有很好的吸附性能,已用于原子吸收等方法测定铭,本文用于分离富集铊。建立了一个在水相体系快速、准确测定痕量铊的方法,成功地用于测定地质样品中…     

氧化石墨烯/硫杂杯芳烃复合材料富集分离-石墨炉原子吸收法测定痕量铊

自制了一种新型氧化石墨烯/硫杂杯芳烃复合材料,用扫描电镜、红外光谱、元素分析、热分析对合成产品进行表征,用于痕量铊的富集,提出了氧化石墨烯/硫杂杯芳烃复合材料分离预富集,石墨炉原子吸收光谱法测定痕量铊的一种新方法,探讨了溶液pH值、温度、洗脱条件及干扰离子对痕量铊分离富集的影响,结果发现该材料对Tl3+具有较大吸附量。在pH 8.0,温度为(23±1)℃条件下,铊可被该材料定量吸附,其吸附容量为73.1 mg/g。吸附的铊可被5.0 mL酸性硫脲(0.5 mol/L HCl+1.0 mol/L硫脲)完全洗脱,方法的线性范围为0.012~15μg/L,检出限(3σ)为0.008μg/L,对0.50μg/L Tl3+工作液测定的RSD(n=7)为2.3%,加标回收率为93.6%~104.1%。此法用于生物样品和环境水样中痕量铊的测定,结果满意。     

重金属铊在环境介质中的分布及其迁移行为

铊是剧毒重金属元素,它在自然界中是典型的稀有分散金属。环境介质中铊的自然本底值较低,但随着铊矿床的开发和铊资源的广泛应用,岩矿石中的铊在自然力或人为作用下向环境介质中迁移。综述了铊在岩（矿）石、土壤、水体、动植物和人体中的分布,以及在上述环境介质及大气中的迁移行为。研究表明,人类活动是导致环境介质中铊含量增加的主要原因。铊在环境介质中的迁移是反复循环的复杂过程,通过风化、溶解、淋滤、吸收、沉降、固结等方式在环境介质中循环往复,从而危害环境生态和人体健康。铊污染应引起人们的普遍重视。     

铊的光度分析及原子吸收光谱分析近况

本文综述了1980～1990年国内外铊的吸光光度、荧光光度及原子吸收光谱分析的发展概况.铊是稀散元素,在电子、化学、玻璃工业及医学等领域中有特殊用途,是制作电子器件的重要金属元素,铊的分析也成为工业分析的重要项目.但随着铊的使用日益增多,铊的环境效应引起了人们的关注.因为铊是人体非必需元素,具有累积性.属高毒类元素,因此,在生物、地质及各种环境样品中分析铊也显得更重要.至今,分析铊的方法既有经典的重量法及滴定法,也有光学、电化学、色谱、质谱和放射化学等仪器分析法.录自1980～1990年《CA》、《中国无机分析化学文摘》和《分析化学文摘》中有关铊分析的条目见表.从表统计可见,CA所载831篇文献中,吸光光度、荧光光度和AAS法共291篇,为文献总数35.0%,而在中文文摘中,该三类方法文献数为48篇,占文献总数49.5%.可见这三类方法在铊分析的普遍性和重要性.     

铊污染及其生态健康效应

对铊污染及其生态效应，包括铊的地球化学特性、环境分布状况、生理毒性和人体慢性铊中毒的症状作了简要综述，分析了铊污染的来源，提出了铊污染的防治对策。     

萃取分离-电感耦合等离子体原子发射光谱法测定磷肥中铊

正近年来,有关重金属的环境污染和健康危害越来越受到社会广泛关注。铊是一种稀散的剧毒重金属元素,铊污染地区的土壤和水中铊含量较高,铊元素会在粮食作物中累积,长期食用高铊蔬菜和食物,会导致慢性铊中毒,如脱发、视神经萎缩甚至死亡~([1-4])。2014年公布的《全国土壤污染调查状况调查公报》显示:全国土壤环境状况总体不容乐观,耕地土壤环境质量堪忧,除工矿业导致部分地区重金属污染严重外,农业活动也是造成土壤污染的主要     

平台石墨炉原子吸收光谱法测定地表水中的铊

铊是一种典型的分散元素,被广泛应用于国防、航天、电子、通讯、卫生等领域,作为高新技术支撑材料的必需组成部分[1],铊的市场需求量与日俱增。同时,铊作为一种高毒性的重金属元素,被世界卫生组织(WHO)列为重点限制清单中的危险废物之一,具有极强的蓄积性,其毒性远超过镉、铜、铅等[2-9]。目前,铊已被我国列入优先控制的污染物名单中,是国家集中式生活饮用水、地表水源地特定项目和生活饮用水水质的非常规监测指标。     

攀钢冶炼废渣中重金属地球化学特征及其环境效应

为治理钢铁冶炼产生的废渣对环境造成的污染,通过对废矿渣堆以及周围土壤中重金属元素的地球化学特征分析,研究了它对附近环境造成破坏的影响因素及污染程度.结果表明:(1)冶炼废渣中重金属元素趋向于富集在比表面积大的颗粒上,易于进入大气中产生环境污染;(2)矿渣堆对环境的破坏以降尘为主要形式,与距离及地形因素呈一定相关;(3)...     

浊点萃取-紫外可见分光光度法测定痕量钴

浊点萃取(Cloud-Point Extraction,简称CPE)是近年来出现的一种新兴的液-液萃取技术,该法以表面活性剂胶束水溶液的溶解性和浊点现象为基础,通过改变实验参数如溶液pH值、离子强度、温度等引发相分离,将疏水性物质与亲水性物质分离,同时起到富集的作用.     

Electrochemical hydride generation of thallium

An electrochemical hydride generation (ECHG) technique was developed to improve the determination of thallium by atomic spectrometry. The technique is based on the catholyte variation system for production of thallium hydride. Using Pb-Sn alloy as cathode, a transient peak shaped signal was achieved and its height, the maximum absorbance value, was taken as an analytical parameter. Parameters that might affect the hydride generation efficiency were investigated and the analytical performance of the method under the optimized experimental conditions was assessed. The linear range was 1-250 ng mL⁻¹ for thallium and the relative standard deviation of the method was 4.2% (RSD, n = 7). The LOD for thallium was found to be 0.8 ng mL⁻¹, showing a significant improvement relative to conventional chemical hydride generation techniques. The proposed method was applied to the determination of thallium in unalloyed zinc standard reference material. This method offers high sensitivity, simplicity, rapidness, freeness from reagent and low acid consumption.     

Sample Preparation Techniques—An Important Part in Trace Element Analysis for Environmental Research and Monitoring

Abstract

For the determination of minute amounts of elements in environmental samples combined analytical procedures are frequently employed. The combination of suitable sample preparation techniques with adequate detection methods lead to powerful analytical procedures. Decomposition methods are an important part of combined procedures for the determination of trace elements in solid samples. After a short summary of the potential sources for systematic errors two new decomposition methods are described that are suitable for the ashing of organic environmental samples. In one method the organic sample is ashed in a high-frequency excited oxygen plasma. The second method is a high pressure decomposition that permits mineralization of the sample in sealed quartz vessels with nitric acid at temperatures up to 320°C.

For both methods the ratio of sample weight to decomposition reagents is comparatively high. This makes these methods in combination with adequate detection methods suitable for the determination of elements at very low concentrations.

X-ray fluorescence spectrometry combined with adequate preconcentration methods is very well suited for the simultaneous determination of trace elements. Following a critical evaluation of various preconcentration techniques the analytical characteristics of filter paper with immobilized complexing agents are described. Particular emphasis is given to filter papers with dithiocarbamates as chelating group.     

激光剥蚀串联电感耦合等离子体质谱在环境分析中的应用进展

激光剥蚀串联电感耦合等离子体质谱法(LA-ICP-MS)是一种功能强大的化学元素检测方法,它具有样品前处理简单、多元素同时测定、高通量、高灵敏度、宽线性范围以及原位分析等优点。同时,激光剥蚀可以与多接收器电感耦合等离子体质谱仪(MC-ICP-MS)串联用于稳定同位素组成测定,不仅避免了繁琐的样品前处理,同时还可应用于固体样品的微区原位同位素分析,揭示微观尺度上稳定同位素组成的变化。LA-ICP-MS已广泛应用于地质、考古等领域,其在环境科学领域应用相对起步较晚,但近年来发展迅速。该文总结了近年来LA-ICP-MS的环境分析方法开发及其在环境科学中的应用进展,并对其未来发展趋势进行了展望。     

Speciation analysis of thallium using electrothermal AAS following on-line pre-concentration in a microcolumn filled with multiwalled carbon nanotubes

The enrichment ability of carbon nanotubes (CNTs) was investigated and a new method established for the determination of trace thallium species in environmental samples using electrothermal atomization-atomic absorption spectrometry (ETAAS). The CNTs were employed as sorbent substrate in a continuous flow system coupled to ETAAS. Parameters influencing the recoveries of thallium were optimized. Under optimal conditions, the detection limit and precision of the method were 0.009 µg L^?1 and 3.9%, respectively. The method was applied to the determination of thallium in real environmental samples and the recoveries were in the range from 96 to 100%. This system was able to separate thallium (I) from the matrix, which allowed its selective determination. The total thallium content was then determined by reducing Tl(III) with hydroxylamine. All these experimental results indicated that this new procedure can be applied to the determination of trace thallium in drinking water samples.     

全氟/多氟化合物分析方法的研究进展

随着全氟和多氟化合物（perfluoroalkyl and polyfluoroalkyl substances,PFASs）被列入《斯德哥尔摩公约》的持久性有机污染物名录,各国对于该类物质的关注逐步升高。该类物质在环境中的广泛检出,使得其环境行为研究不断扩展和加深。目前,针对不同类型PFASs的样品前处理方式与检测方法也在不断发展中,而从中选择最合适的前处理和分析方法是开展PFASs环境科学、管理和污染控制研究的前提。该文针对传统PFASs及其异构体、PFASs前体物和新型PFASs等的样品前处理方法、色谱-质谱分析方法进行归纳总结,认识其现状和问题,并在此基础上对其发展进行了展望。     

Enantiomeric fraction determination of chiral drugs in environmental samples using chiral liquid chromatography and mass spectrometry

When it was recognized that chiral drug residues have stereospecific toxicity towards environmental organisms the attention given to enantiomeric fraction determination of chiral drugs in the environment increased. Among various analytical techniques, chiral liquid chromatography (LC) coupled with mass spectrometry (MS) has been widely used due to its simplicity, wide applicability and high sensitivity. In this review, we aim to provide a comprehensive overview and comparison of the types of chiral stationary phases, elution modes and MS detection techniques employed and address the advances and limitations. The impact of the mobile phase composition on enantioseparation and MS detection are discussed based on the different methods developed. In addition, diverse applications for the enantiomeric fraction determination of chiral drugs in environmental matrices using chiral LC and MS are discussed in depth.     

Rapid Methods in Analytical Chemistry

This article presents the most recent research in analytical chemistry concerning the development of rapid methodologies covering the period from 2009 up until today. In this context, different useful analytical methods have been developed based mainly on typical techniques such as gas chromatography, liquid chromatography, mass spectrometry, electrophoresis, electroanalytical chemistry, and biosensors. The analytical features of these methods have allowed the analysis of samples of different natures, such as environmental, food, pharmaceutical, and biological type, in which wide classes of analytes are promptly determined. The main advantages of these methods are included and discussed in this review regarding novelty, rapidity, sensitivity, selectivity, and costs. It is concluded that the development of rapid methods is still a growing trend in analytical chemistry and that gas- and liquid-chromatography mainly coupled to different modes of mass spectrometry are the most common analytical techniques applied today. Regarding the matrices analyzed, most of the methods have been developed for food analysis, followed by biological and environmental matrices.     

Inorganic trace analysis by mass spectrometry

Mass spectrometric methods for the trace analysis of inorganic materials with their ability to provide a very sensitive multielemental analysis have been established for the determination of trace and ultratrace elements in high-purity materials (metals, semiconductors and insulators), in different technical samples (e.g. alloys, pure chemicals, ceramics, thin films, ion-implanted semiconductors), in environmental samples (waters, soils, biological and medical materials) and geological samples. Whereas such techniques as spark source mass spectrometry (SSMS), laser ionization mass spectrometry (LIMS), laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), glow discharge mass spectrometry (GDMS), secondary ion mass spectrometry (SIMS) and inductively coupled plasma mass spectrometry (ICP-MS) have multielemental capability, other methods such as thermal ionization mass spectrometry (TIMS), accelerator mass spectrometry (AMS) and resonance ionization mass spectrometry (RIMS) have been used for sensitive mono- or oligoelemental ultratrace analysis (and precise determination of isotopic ratios) in solid samples. The limits of detection for chemical elements using these mass spectrometric techniques are in the low ng g⁻¹ concentration range. The quantification of the analytical results of mass spectrometric methods is sometimes difficult due to a lack of matrix-fitted multielement standard reference materials (SRMs) for many solid samples. Therefore, owing to the simple quantification procedure of the aqueous solution, inductively coupled plasma mass spectrometry (ICP-MS) is being increasingly used for the characterization of solid samples after sample dissolution. ICP-MS is often combined with special sample introduction equipment (e.g. flow injection, hydride generation, high performance liquid chromatography (HPLC) or electrothermal vaporization) or an off-line matrix separation and enrichment of trace impurities (especially for characterization of high-purity materials and environmental samples) is used in order to improve the detection limits of trace elements. Furthermore, the determination of chemical elements in the trace and ultratrace concentration range is often difficult and can be disturbed through mass interferences of analyte ions by molecular ions at the same nominal mass. By applying double-focusing sector field mass spectrometry at the required mass resolution—by the mass spectrometric separation of molecular ions from the analyte ions—it is often possible to overcome these interference problems. Commercial instrumental equipment, the capability (detection limits, accuracy, precision) and the analytical application fields of mass spectrometric methods for the determination of trace and ultratrace elements and for surface analysis are discussed.     

Spectral and non-spectral interferences in the determination of thallium in environmental materials using electrothermal atomization and vaporization techniques—a case study

The literature on the determination of Tl in environmental samples using electrothermal atomization (ETA) and vaporization (ETV) techniques has been reviewed with special attention devoted to potential interferences and their control. Chloride interference, which is due to the formation of the volatile monochloride in the condensed phase, is the most frequently observed problem. Due to its high dissociation energy (88 kcal/mol), TlCl is difficult to dissociate in the gas phase and is easily lost. The best means of controlling this interference in ETA is atomization under isothermal conditions according to the stabilized temperature platform furnace concept, and the use of reduced palladium as a modifier. An alternative approach appears to be the ‘fast furnace’ concept, wherein both the use of a modifier and the pyrolysis stage are omitted. This concept requires an efficient background correction system, and high-resolution continuum-source atomic absorption spectrometry (HR-CS AAS) appears to offer the best results. This chloride interference can also cause significant problems when ETV techniques are used. Among the spectral interferences found in the determination of thallium are those due to Pd, the most efficient modifier, and Fe, which is frequently found at high concentrations in environmental samples. Both interferences are due to nearby atomic lines, and are observed only when deuterium background correction and relatively high atomization temperatures are used. A more serious spectral interference is that due to the molecular absorption spectrum of SO₂, which has a maximum around the Tl line and exhibits a pronounced rotational fine structure. HR-CS AAS again showed the best performance in coping with this interference.