原子发射光谱分析

本文是《分析试验室》期刊单年度定期评述中关于原子发射光谱分析的第三篇综述文章。文中对１９９３－１９９４年期间我国在ＡＥＳ领域所取得的主要进展作了简要的评述。评述内容包括基础理论、应用研究、仪器研制、新方法建立以及一般样品分析。研究领域主要涉及到电感耦合等离子体原子发射光谱法，微波等离子体原子发射光谱法，电弧和火花原子发射光谱法，辉发放电原子发射光谱法和亚稳态能量转移光谱法等。引用文献２１１篇。     

微波等离子体原子发射光谱法及其应用

本文评述了有关微波等离子体原子发射光谱法的一些最新进展，内容包括获得做波等离子体（ＭＷＰ）的装置，ＭＷＰ的放电特性，样品引入方法及实际应用。     

贵金属元素铂、铑、钯的分析进展

从光度法、电化学法、原子吸收法、中子活化法、电感耦合等离子体与原子发射光谱、质谱联用技术等各种方法,对国内外近几年来贵金属元素铂、铑、钯的测定方法进行综合评述,引用文献168篇。     

金属材料分析

评述了2007年10月至2009年12月期间国内在金属材料分析领域的现状及进展概况.内容包括重量分析法、滴定分析法、分光光度法和荧光光度法、催化动力学光度法、原子吸收光谱法和原子荧光光谱法、电感耦合等离子体原子发射光谱法和电感耦合等离子体质谱法、光电直读光谱法、X射线荧光光谱法、原位统计分析及电化学方法等其他分析方法、...     

硒的化学形态分析

对硒的化学形态分析的现状(1991-2006)进行了评述,主要涉及的分析方法有紫外-可见分光光度法、荧光光度法、氢化物发生(HG)原子荧光光谱法、HG原子吸收光谱法、电感耦合等离子体(ICP)原子发射光谱、气相色译原子吸收光谱联用、ICP-质谱与多种分析技术联用等(引用文献45篇).     

地质样品中总锡测定方法的研究进展

综述了地质样品中总锡分析方法(包括容量法、分光光度法、氢化物发生-原子荧光光谱法、原子吸收光谱法、极谱法、原子发射光谱法、电感耦合等离子体原子发射光谱法、电感耦合等离子体质谱法、X射线荧光光谱法)的研究进展。     

电感耦合等离子体原子发射光谱中进样技术的新进展

评述了电感耦合等离子体原子发射光谱中的进样技术的新近进展，引用近期文献１１８篇。     

电感耦合等离子体原子发射光谱法在环境分析中的应用

对1996—2010年间电感耦合等离子体原子发射光谱法在环境分析中的应用进展作了评述,主要涉及在大气和飞灰、水、土壤、污泥和植物等方面中的应用(引用文献23篇)。     

无机固体样品中硫的测定方法的研究进展

综述了无机固体样品中硫的高温燃烧热解(包括燃烧-红外吸收法、燃烧-碘量法、燃烧-库仑滴定法、燃烧-中和滴定法和燃烧-电导法等)、湿法消解(包括硫酸钡重量法、硫酸钡比浊法、电感耦合等离子体原子发射光谱法、电感耦合等离子体质谱法、原子吸收光谱法和离子色谱法等)和固体样品直接分析(包括火花源原子发射光谱法、辉光放电原子发射光谱法、X射线荧光光谱法等)等3类测定方法的研究进展(引用文献117篇)。     

电感耦合等离子体原子发射光谱(ICP-AES)技术的应用进展

概述了近年来电感耦合等离子体原子发射光谱技术的发展,并分别详细介绍了近年来电感耦合等离子体原子发射光谱法（ICP-AES）在金属材料、地矿、冶金、水质、环境、食品、农业、石油化工、生物、医药等不同领域的应用进展。最后对电感耦合等离子体原子发射光谱分析法的发展前景做了展望。     

Spectrochemical determination of trace uranium by an argon-stabilized U-shaped DC arc

An argon-stabilized U-shaped DC arc with the system for aerosol introduction was used for uranium determination. High uranium toxicity suggests the necessity of developing as sensitive methods as possible for U detection in various natural samples and complex matrices. By optimizing the operation conditions of U-shaped arc plasma and by applying an appropriate computer program that performs temporal integration of recorded signals, the measurement precision as well as the concentration sensitivity were improved, and the detection limit was lowered. Uranium detection limit, obtained by the application of U-shaped arc plasma during different integration times, decreases by increasing integration time. By increasing this time from 1 to 30 s, the detection limit was 37 times lower and the lowest detection limit is 0.07 μg/mL. The detection limit achieved by this method is comparable with the detection limits obtained by such methods as inductively coupled plasma-atomic emission spectroscopy (ICP-AES), direct coupled plasma-atomic emission spectroscopy (DCP-AES), and microwave induced plasma-atomic emission spectroscopy (MIP-AES). The text was submitted by the authors in English.     

Design and properties of a microwave boosted glow discharge lamp

The operation of a glow discharge lamp with integrated microwave resonator for the analysis of electrically conducting solid samples by atomic emission spectrometry is described. While the glow discharge in argon at a pressure of 300 Pa mainly serves for the production of free sample atoms by cathodic sputtering, a 40 W microwave discharge is applied for additional excitation of the ablated material. The construction of the lamp and the optimization of the working conditions are described. The intensities as well as the signal-to-background ratios of many analytical lines were found to be improved as compared to a conventional glow discharge lamp. The analytical performance is demonstrated by analysis results for steel samples. Detection limits for 13 elements in steel are between 0.05 and 1 μg/g. Because of the optically thin plasma the new lamp shows a large linear dynamic range.     

Determination of fluorine, chlorine, bromine and iodine by barrier discharge radiofrequency helium plasma.

A determination method of fluorine (F), chlorine (Cl), bromine (Br) and iodine (I) by a barrier discharge radiofrequency helium plasma-atomic emission spectroscopy was developed. A borosilicate glass was wrapped by two copper film electrodes, one of which was earthed, and the other was supplied with a radiofrequency high voltage (98 kHz, 3.2 kV), resulting in a discharge inside of the tube. An optical emission from the discharge tube was introduced to a charge-coupled device (CCD)-spectrometer through an optical fiber, and was monitored in the wavelength range of 730-960 nm. The emission lines of F (733.2 nm, 739.9 nm), Cl (833.3 nm, 837.6 nm, 858.6 nm, 894.8 nm, 912.1 nm, etc.), Br (827.2 nm, 882.5 nm, 889.8 nm, 926.5 nm, etc.) and I (905.8 nm) were observed. The linearity of the calibration was determined for F and Cl over the range of 1-10 microg, and for Br of 0.1-1 microg. The relative emission intensity was in the order of Br > I > Cl >F.     

Zn3(OH)2V2O7·2H2O纳米片的水热制备

采用硝酸锌、五氧化二钒和氢氧化钠作为反应物,通过一个简单的CTAB辅助的水热方法制备了Zn3(OH)2V2O7·2H2O纳米片.运用XRD,ICP-AES,FTIR,HRTEM,EDS,FE-SEM对产物的晶相和形貌进行了表征.结果表明CTAB在控制产物的形貌、尺寸分布和自组装过程中起着关键作用.同时我们研究了产物的晶体生长行为和自组装过程.     

MeAPO-5分子筛的合成及其在肉桂醇选择氧化反应中的催化性能

采用水热法合成了一系列杂原子磷铝分子筛MeAPO-5(Me=Co,Fe,Cu,Zn,Mn),并利用X射线衍射(XRD),热重-差热分析(TG-DTA),电感耦合等离子体原子发射光谱(ICP-AES)和漫反射紫外-可见光谱(DRUV-Vis)等技术对分子筛的结构,化学组成以及金属离子的存在状态进行了表征.结果表明,合成的纯相MeAPO-5分子筛具有较高的结晶度,金属杂原子种类显著影响其在MeAPO-5分子筛中的存在状态,取代度及合成样品的结晶度.Co2+,Fe3+,Zn2+和Mn2+较易进入分子筛骨架,而Cu2+较难进入.通过考察MeAPO-5分子筛在肉桂醇氧化反应中的催化性能,发现CoAPO-5分子筛具有良好的选择氧化催化性能,1,4-二氧六环是较好的溶剂,调变反应温度可以有效调控产物的选择性.     

Spectrochemical Determination of Some Elements in Zinc Samples Using Glow Discharge Lamp

Abstract

Results in spectrochemical analysis with optical emission spectroscopy(OES) are affected by matrix. Analysis of zinc samples are difficult with other emission excitation sources as arc and spark, since zinc is a volatile element. For this reason, metallic zinc samples and its low alloys were analysed by using a glow discharge lamp in this work. Interelement effects were also investigated in the determination of Al, Cu and Mg in the samples.     

Microwave sputtering of conductors and insulators for optical emission and mass spectrometry

A microwave-powered slab-line cavity was used to excite a discharge in low pressure argon or neon and to demonstrate the sputtering of conducting and non-conducting samples by a microwave excited discharge. Both optical emission spectroscopy and mass spectrometry were used as detection systems. The dependence of the signals on gas pressure and net microwave power was investigated.     

Microwave sputtering of conductors and insulators for optical emission and mass spectrometry

A microwave-powered slab-line cavity was used to excite a discharge in low pressure argon or neon and to demonstrate the sputtering of conducting and non-conducting samples by a microwave excited discharge. Both optical emission spectroscopy and mass spectrometry were used as detection systems. The dependence of the signals on gas pressure and net microwave power was investigated.     

Microwave digestion of sediment, soils and urban particulate matter for trace metal analysis

A microwave digestion technique was developed to determine the content of nine heavy metals in sediments and soils. The digests were subsequently analysed by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The metals determined were Ca, Mg, Fe, Mn, Zn, Cr, Cd, Cu, Pb and V. The digestion was achieved by using an acid mixture of HNO₃, HF and distilled H₂O. The experimental study was conducted using four standard reference materials (SRMs): sewage sludge (LGC6136), marine sediment (PACS-1), urban particulate matter (NIST 1648) and coal carbonisation site soil (LGC6138). Two different programs were examined to determine which was optimal for the digestion of real environmental samples. The accuracy and precision of the two digestion programs for the analysis of the SRMs were compared. From the results obtained, the microwave program providing a maximum of power of 650 W and a cycle time of 51 min resulted in the best analytical performance. The experimental results obtained were in good agreement with the certified values and demonstrated that the proposed method is precise and accurate.