Determination of Copper,Cadmium, Zinc And Lead In ArgeŞ River In Romania During Four Seasons By Inductively Coupled Plasma Atomic Emission Spectrometry And Anodic Stripping Voltammetry

ABSTRACT

The paper represents a continued study of selected heavy metals concentration in the Arge? River, the fifth river in length from Romania.

For the determination of metal ion concentration in Arge? river was used Atomic Absorption Spectrometry for sodium, potassium and magnesium; Direct Coupled Plasma Atomic Emission Spectrometry for calcium; Inductively Coupled Plasma Atomic Emission Spectrometry for copper, cadmium, zinc, aluminium, lead, titanium, zirconium, chromium, molybdenum, manganese, iron and nickel.

Copper, cadmium, zinc and lead concentration were determined by ICP–AES and ASV and results were reliable.

By comparison of the results a good agreement between these two techniques is observed.     

Electrochemical Analysis of Mercury Using a Kryptofix Carbon‐Paste Electrode

Abstract

Successful applications of different analytical procedures to determine quantitatively mercury in aqueous media can be found in recent literature. Fundamentally it has made use of Cold Vapour Atomic Absorption Spectrometry (CV‐AAS), X‐Ray Fluorescence or UV Spectrophotometry, Inductively Coupled Plasma Atomic Emission Spectrometry (ICP‐AES), or Inductively Coupled Plasma Mass Spectrometry (ICP‐MS), which are the techniques commonly used for trace measurement of heavy metal in the laboratory. In this paper a new and alternative methodology to determine quantitatively mercury in aqueous media is reported. A kryptofix carbon‐paste electrode has been used to determine voltammetrically mercury. The detection limit for mercury was evaluated to be 0.12 µg/l.     

Trends in Preconcentration Procedures for Metal Determination Using Atomic Spectrometry Techniques

 Methods for metal preconcentration are often described in the literature. However, purposes are often different, depending on whether the methods are applied in environmental, clinical or technological fields. The respective method needs to be efficient, give high sensitivity, and ideally also is selective which is useful when used in combination with atomic spectroscopy. This review presents the actual tendencies in metal preconcentration using techniques such as Flame Atomic Absorption Spectrometry (FAAS), Electrothermal Atomic Absorption Spectrometry (ETAAS), Hydride Generation Atomic Absorption Spectrometry (HGAAS), Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Procedures based on related to electrochemical, coprecipitation/precipitation, liquid–liquid and solid–liquid extraction and atom trapping mechanisms are presented. Correspondence: Department of Analytical Chemistry, Universidade Estadual de Campinas – UNICAMP, P.O. Box 6154, 13083-970 Campinas, Brazil. e-mail: zezzi@iqm.unicamp.br Received December 20, 2001; accepted October 11, 2002     

Classical analysis including trace-matrix separation versus solid state mass spectrometry: A comparative study for the analysis of high purity Mo,W and Cr

The applicability of GDMS, SIMS, SSMS, NAA and TMS with AAS, ICP-OES and ICP-MS end determination for routine bulk ultratrace analysis of high purity refractory metals was investigated. Due to the heterogeneous distribution of trace elements in the sub-ppm range, sample consumption and analysis time have a tremendous influence on quantification with procedures of low sample consumption. As an example, GDMS, which is commonly used for ultrapure material certification by most of the manufacturers in Europe and the USA, exhibits discrepancies by more than one order of magnitude for repetitive analyses of a series of trace components in the same sample. Furthermore, results of different laboratories using the same instrument are frequently not comparable. Due to easy standardization and large sample consumption TMS procedures combined with FAAS, GFAAS, ICP-AES and ICP-MS as methods of end determination exhibit better precision and accuracy than GDMS and SIMS. Detection limits are comparably low or even better in case of ICP-MS end determination. TMS procedures are less expensive and less time consuming than highly sophisticated analytical techniques like GDMS, SIMS or NAA. Additionally, they can be easily applied by experienced personnel in a well equipped industrial analytical laboratory.List of Acronyms Used AAS Atomic Absorption Spectrometry - FAAS Flame Atomic Absorption Spectrometry - GDMB Gesellschaft Deutscher Metallhütten- und Bergleute - GDMS Glow Discharge Mass Spectrometry - GFAAS Graphite Furnace Atomic Absorption Spectrometry - ICP-AES Inductively Coupled Plasma Atomic Emission Spectrometry - ICP-MS Inductively Coupled Plasma Mass Spectrometry - IDMS Isotope Dilution Mass Spectrometry - NAA Neutron Activation Analysis - SIMS Secondary Ion Mass Spectrometry - SSMS Spark Source Mass Spectrometry - TMS Trace-Matrix Separation - VLSI Very Large Scale Integration - XRFS X-Ray fluorescence Spectroscopy Dedicated to Professor Günther Tölg on the occasion of his 60th birthday     

电感耦合等离子体-发射光谱法（ICP-AES）快速测定饮用水中8种微量元素

用电感耦合等离子体-发射光谱法（ICP-AES）同时快速测定饮用水中微量的铜、铅、锌、铁、锰、镉、铬、砷,具有快速、简便、灵敏度高等优点,精密度为1．2％～8．2％（RSD,n=5）．回收率为90％～110％．     

Ultrasound-assisted emulsification of cosmetic samples prior to elemental analysis by different atomic spectrometric techniques

In this work, ultrasound-assisted emulsification with a probe system is proposed as a rapid and simple sample treatment for atomic spectrometric determinations (Electrothermal Atomic Absorption Spectrometry, Inductively Coupled Plasma Optical Emission Spectrometry, Flame Atomic Absorption Spectrometry and Cold Vapour Atomic Absorption Spectrometry) of trace elements (As, Cd, Cr, Cu, Hg, Mg, Mn, Ni, Sr and Zn) in cosmetic samples such as shampoos, gel (hair gel), crèmes (body milk, hair conditioner) and oil (body oil). The type of dispersion medium, the sample mass-to-dispersion medium volume ratio, as well as the parameters related to the ultrasound-assisted emulsification (sonication amplitude and treatment time) were exhaustively studied. Only 1 min of ultrasonic shaking and a dispersion medium containing 0.5% (w/v) of SDS + 3% (v/v) of HNO₃ or HCl allows obtaining a stable emulsion at least for 3 months. Thermal programs, nebulization of emulsions, speed of pumps and concentration of reagents used in cold vapour generation were optimized. Calibration using aqueous standards was feasible in all cases. Calibration by the standard addition method and recovery studies was also applied for validation. Microwave-assisted digestion and Inductively Coupled Plasma Mass Spectrometry were used for comparison purposes. Relative standard deviations from analysis of five independent emulsions were less than 9% in all cases.     

微波消解电感耦合等离子体发射光谱法测定塑料中铅和镉

采用微波消解技术溶样，ICP-AES法测定了塑料中的铅和镉。通过对消解试剂和微波温度程序的研究，建立了塑料样品的微波消解方法。该方法与传统马弗炉高温灰化消解方法比较，具有准确、简便、快速、省试剂、污染少、消解完全等优点。方法回收率为93％～106％，相对标准偏差(n=7)均小于2％。实际样品对比分析结果表明，方法具有良好的准确度，适于多种塑料材料中铅和镉的快速分析。     

Determination of Thallium in Antarctic Snow by Means of Laser Induced Atomic Fluorescence and High Resolution Inductively Coupled Plasma Mass Spectrometry

Abstract

Measurements of thallium levels in Antarctic snow samples collected in an area surrounding the Italian Station at Terra Nova Bay in different campaigns have been performed without preconcentration by means of Laser Induced Atomic Fluorescence Spectroscopy (LIAF) as well as by High Resolution Inductively Coupled Plasma Mass Spectrometry (HR ICP-MS).

The data obtained by both methods compare favourably and are of the order of tenths of pg/g. The data is discussed taking into account the effect of the marine aerosol and the crustal contribution to the thallium content in samples.     

The Simultaneous Determination of Trace Dy,Eu, Gd and Sm in Nuclear Grade Uranium Oxide by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES)

A method for the simultaneous determination of trace Dy, Eu, Gd and Sm in nuclear grade uranium oxide by Inductively Coupled Plasma Atomic Emission Spectrometry has been developed. The process of uranium extraction and ICP/AES optimization are investigated. The detection limits of Dy, Eu, Gd and Sm are 0.003, 0.002, 0.006 and 0.010 μg/ml respectively, and more than 90% recovery can be obtained.     

Mapping of lead,magnesium and copper accumulation in plant tissues by laser-induced breakdown spectroscopy and laser-ablation inductively coupled plasma mass spectrometry

Laser-Induced Breakdown Spectroscopy (LIBS) and Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) were utilized for mapping the accumulation of Pb, Mg and Cu with a resolution up to 200 μm in a up to cm × cm area of sunflower (Helianthus annuus L.) leaves. The results obtained by LIBS and LA-ICP-MS are compared with the outcomes from Atomic Absorption Spectrometry (AAS) and Thin-Layer Chromatography (TLC). It is shown that laser-ablation based analytical methods can substitute or supplement these techniques mainly in the cases when a fast multi-elemental mapping of a large sample area is needed.     

Direct Multielement Determination of Selected Elements in Rat Urine by Inductively Coupled Plasma Atomic Emission Spectroscopy

Abstract

A method has been developed for the direct determination of dissolved elements in samples of rat urine of less than 2 ml, by Inductively Coupled Plasma Atomic Emission Spectroscopy. The method is capable of measuring copper, iron, magnesium, manganese, phosphorus and zinc.     

ICP-AES法同时测定玻璃组份中的Ca、Mg、Ti、Fe、Pb、Cd、Al、Si、B、Zn、Cu元素

建立了一种用电感耦合等离子发射光谱(ICP-AES)法测定玻璃成份的简便、快速、准确、精密度好的方法．研究了样品的处理、标准样品的配制、谱线干扰等问题,并采用和基体匹配的方法消除基体的影响,进行了标准样品的分析、对照、精密度等试验,均取得了满意的结果．     

Neptunium determination by inductively coupled plasma mass spectrometry (ICP-MS)

The determination of neptunium-237 (²³⁷Np) traditionally has been performed by alpha spectrometry or neutron activation analysis. These methods are labor intensive and require several days for completion. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a possible alternative for²³⁷Np determinations. This paper describes the analytical method developed for samples that have significant levels of uranium present. The lower reporting limits achievable by ICP-MS are competitive with the counting methods, but the real advantage for this laboratory lies in the lower cost and faster turnaround time provided by ICP-MS.     

大型分析仪器几例故障分析及维修

介绍了实验室几种大型分析仪器：X荧光光谱仪、ICP直读光谱仪、原子吸收光谱仪、原子荧光光度计的几例故障分析及维修。     

A simple solution to expanding available reference materials for Laser Ablation Inductively Coupled Plasma Mass Spectrometry analysis: Applications to sedimentary materials

Analytical data on sediments are of great importance in understanding and documenting environmental issues. For laboratories interested in in-situ chemical analysis of sediments by LA-ICP-MS, a major issue is the lack of appropriate matrix matched sediment reference materials. Those available were largely designed for partial extractions which generally do not reflect the total elemental compositions. In this work we provide a comprehensive study on chemical compositions of seven currently available sediment reference materials (Lake sediments: LKSD-1, LKSD-2, LKSD-3, Stream sediments: STSD-2, STSD-3, and Marine sediments: PACS-2, MESS-3) as determined by Solution Nebulization Inductively Coupled Plasma Mass Spectrometry (SN-ICP-MS) and Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) after digestion in a mixture of concentrated HNO₃ and HF acids. We also report a simple method to prepare these sediment reference materials and more generally appropriate sediment cores for LA-ICP-MS analysis using epoxy resin. This sample preparation method maintains sediment integrity for high spatial resolution analysis which is required for tracing changes in environmental conditions over short time periods. This work also demonstrates the application of fs-LA-ICP-MS as a tool for direct, rapid and high spatial resolution analysis of sediments.     

A comparison between ICP-MS and AFS detection for arsenic speciation in environmental samples

Performances of two atomic detectors, Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) and Atomic Fluorescence Spectrometry (AFS) have been compared for arsenic speciation in environmental samples. Instrumental couplings, based on the use of high performance liquid chromatography (HPLC), hydride generation (HG), and the two atomic detectors were used for the speciation of arsenite, arsenate, dimethylarsinic acid and monomethylarsonic acid. Optionally, arsenobetaine was also determined using on-line ultraviolet (UV) photooxidation. The detection limits ranging from 0.1 to 0.3 mug l(-1) (as As) and the precision >10% RSD obtained with HPLC-(UV)-HG-AFS were comparable with those obtained with HPLC-(UV)-HG-ICP-MS. Both instrumental coupling were applied to the NRCC-TORT-1 and several environmental samples, such as seawater, freshwater, sediments, bivalves and bird eggs, taken from two areas with different degrees of pollution. No influence of the sample matrix was observed on the results using external calibration and standard additions methods, for both coupled techniques.     

金属组学：高通量分析技术进展与展望

金属组学是系统研究一种细胞、组织或完整生物体内全部金属原子的分布、含量、化学种态及其功能的新兴综合学科,它的提出受到人们越来越多的关注。本文综述了金属组学的研究方法,并对各种方法的特点和局限性做了比较说明．ICP-MS与NAA技术可实现多元素同时定量分析,同步辐射微束CT及μRF,EDX,PIXE,SIMS及LA-ICP—MS亦可实现金属组分布研究．金属组学研究目前正处于发展初期,仍有许多困难特别是分析仪器及方法方面的问题有待解决．已有的金属组形态及结构分析工作大多数采用的是较低效率的分析方法,一些正在发展中的关键技术平台,如HTXAS可真正实现高通量的形态或结构分析．此外,生物信息学有望成为金属组学研究的重要工具之一．     

电感耦合等离子体原子发射光谱(ICP-AES)法测定Ti50Si合金中的钛元素

研究了ICP-AES测定Ti50Si合金中钛含量的方法。采用氢氟酸、硝酸溶解试样,优化了射频发生器(RF)功率、雾化压力、辅助气流量以及泵速等仪器参数,通过实验分析了溶液酸度、分析谱线的影响,确定了最佳实验条件。测定了2份Ti50Si样品,相对标准偏差小于0.64%(n=11),与硫酸高铁铵滴定法测定结果一致,证明了方法有较高的准确度和实用性。     

Speciation of Se,Fe and Zn in Human Milk Whey: The use of Instrumental Neutron Activation Analysis (INAA) to corroborate element profiles measured with Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

In human milk trace elements normally exist in a form which can easily be absorbed by the newborn infant. For investigations of the bioavailability of trace elements it is necessary to carry out a speciation analysis of the elements of interest. An independent analytical method has been used for the quality control of the shape of the element profiles obtained from the speciation analysis of Se, Fe and Zn in individual samples of human milk whey after chromatographic separation. For the element detection in the untreated milk fractions Instrumental Neutron Activation Analysis (INAA) was chosen as the reference method. Element distribution patterns have been obtained with Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) using on-line digestion of the fraction, reduction and hydride formation of Se ("T"-mode). Prior results are compared with those obtained by means of element detection in the untreated fractions ("U"-mode) with ICP-AES. The elution profiles of Se, Fe and Zn in human milk whey obtained by means of ICP-AES detection using the "T"-mode show good agreement with the distribution patterns obtained with INAA. Recoveries of 103% for Fe, 86% for Zn and 87% for Se were obtained. The element distribution patterns of Fe and Zn obtained with ICP-AES speciation using the "T"-mode also show good agreement with those obtained by means of ICP-AES using the "U"-mode.     

Determination of Trace Metals in Air Particulate Matters by Graphite Furnace - Capacitively Coupled Plasma - Atomic Emission Spectrometry

In Graphite Furnace - Capacitively Coupled Plasma - Atomic Emission Spectrometry, an atmospheric pressure radio frequency helium plasma is sustained inside a graphite furnace containing a coaxially placed graphite rod antenna. Sample vaporizaiton/atomization can be separated from the excitation step. This technique combines the advantages of highly sensitive GF-AAS and the efficient plasma source for sample decomposition. Thus, it will provide a suitable technique to determine both total trace metals and different speciation of metals existing in various forms with different thermal properties. The information obtained will be useful to assess the health impact and to apportion major sources of air particulate matters.