火焰原子吸收法同时测定土壤中铅和镉

原子吸收光谱法多元素同时测定技术至今还处在实验阶段。多元素原子吸收同时测定要求被测元素物理化学性质相似而又无光谱和化学的干扰。我们用Jarrell-Ash810型双光束双波道原子吸收分光光度计同时测定土壤中铅、镉,在已消化了的试样溶液中加入EDTA释放剂,抑制硅、铬、钼离子对铅、镉测定的干扰。双道测量精度:Pb2.67%,Cd10.0%,单道测量精度:Pb8.37%,Cd0.45%。     

多波长数据线性回归法在火焰原子吸收同时测定Fe,Pt中的应用

用火焰原子吸收法在２７１．９０３ｎｍ处测定Ｆｅ时Ｐｔ对其吸收线发生谱线重叠干扰，本实验用多波长数据线性回归法理想地校正了Ｐｔ２７１．９０４ｎｍ，对Ｆｅ的２７１．９０３ｎｍ干扰，实现了用Ｆｅ元素空心阴极灯同进测定Ｆｅ，Ｐｔ两种元素。     

原子吸收分光光度法测定矿石及金属镍、钴中的微量锌

矿石及有色金属中的微量锌,目前多采用氰化物掩蔽干扰元素,双硫腙萃取分光光度法测定。该法虽然准确、可靠,但操作手续繁琐,同时需使用剧毒的氰化物。其它分光光度法也往往存在着试剂空白和元素间干扰等不利因素。原子吸收分光光度法测定锌,早在1958年已有报导。由于方法具有灵敏度高、元素干扰少、操作简易、快速和准确等优点,因此近年来,得到了广泛的应用。但是,用原子吸收分光光度法测定矿石及金属镍、钴中微量锌的详细报导却较     

石墨炉原子吸收光谱法测定硫酸亚铁铵中痕量元素砷和铅

砷和铅是硫酸亚铁铵中的杂质元素,其含量对硫酸亚铁铵的纯度有影响,一般要求其质量分数不超过0.002%。如此低的含量,使用石墨炉原子吸收法测定较为合适。笔者采用日立公司的石墨炉原子吸收法同时测定溶液中痕量砷和铅,采用偏振塞曼扣除背景,结合光学快速升温技术及基体改进技术,消除了共存组分对痕量砷、铅测定的干扰,详细探     

水中矿物元素的ICP-MS分析

用ICP－MS对地下水、地表水和饮用水中的矿物元素进行了分析测定，实验证明用ICP－MS可以同时测定地下水，地表水和饮用水中矿物元素；该法灵敏度、精密度和准确度都能满足有关标准的要求，具有多元素同时分析，样品前处理简单，干扰少，测定快速，省事省力等优点。     

火焰原子吸收法中干扰效应的计算消除方法

本文研究了火焰原子吸收法中干扰效应的计算消除方法，提出用多项式作为表达待测元素和干扰元素之间相互关系的数学模型。本文旨在研究包括待测元素和干扰元素的两元体系中干扰效应的一些规律性，筛选出具有一定普遍性的数学模型。对某些双组份体系进行了实验，结果表明，用本文方法所得计算结果与实际浓度一致。     

ICP—AES法测定铝合金中硼锆铁铍镁钙锶

化学法测定铝合金中高硼一般采用酸碱中和容量法,基体需在碱性溶液中预先沉淀分离,手续繁琐,精度较差。碱土金属的测定多采用原子吸收法,但需加入一定量的抑制剂消除铝酸盐的负干扰,由于抑制剂的引入给测定带来了一系列的问题,如空白增大等,从而使同一溶液连续测定多元素变得复杂化。用ICP-AES法测定上述元素可直接在同一溶液中顺序测定,方法简便、快速,基体铝无干扰,尤其是测定碱上金属元素,本方法优于原子吸收法和其它化学方法,具有灵敏度高、精度好、测定范围广等特点。 本方法选择了七元素最佳分析线及仪器工作参数,试验考察了铝及有关元素的干扰以及溶液酸度的影响,做了七元素的工作曲线及合成样品的回收试验,分析了不同种类的铝合金样品,获得了满意的结果。     

火焰原子吸收法连续测定肥料中多元素

应用火焰原子吸收法连续测定肥料中Ｃｕ、Ｚｎ、Ｆｅ、Ｍｎ、Ｃａ、Ｍｇ，并对测定条件、干扰因素进行了综合考察。方法简便、快速、适用于多元素复合肥料生产控制分析和样品系统分析。     

原子吸收法测定高含量铅

高含量铅的测定通常采用容量法。多金属矿石中的高含量铅,则要经过冗长的分离手续,最后以络合滴定法完成测定。原子吸收法(AAS)由于具有干扰少、简便、快速、准确等优点,已广泛应用于低含量元素的测定。近年来国内应用原子吸收法测定高含量无素的实用分析方法已有报导。     

ICP-AES法测定方铅矿中多元素的方法研究

采用电感耦合等离子体原子发射光谱法(ICP-AES)进行方铅矿中多元素同时测定.通过对方铅矿样品化学处理试验建立了HCl-NH4Cl-HNO3的溶矿体系.本体系采用基体匹配、背景系数和元素干扰系数校正及元素内标法确定了最佳综合实验测试条件.本实验建立的ICP-AES法同时测定方铅矿中镉、钴、铜、铁、铟、铅、锌7种元素的方法,本方法测量相对误差RE (n=8)为1.50%～7.50%,相对标准偏差RSD (n=8)为1.7%～5.7%.经国家一级标准物质GBW 07269分析验证可以满足方铅矿单矿物样品的分析要求.     

探针-石墨炉原子吸收光谱法测定岩石矿物中的金

本文采用自制探针系统对探针-石墨炉原子吸收光谱法测金的性能,探针系统的制作,探针的处理,探针原子化法的检测限,灵敏度及抗干扰能力进行了详细的研究,探针原子化的各项指标均优于常规的管壁原子化法。采用本法可不必分离基体物质,直接测定地质样品中的金,所得结果与萃取原子吸收法的结果相吻合。     

Atomic-absorption spectrophotometric determination of antimony, arsenic, bismuth, tellurium, thallium and vanadium in sewage sludge

Electrothermal atomic-absorption spectrophotometry (AAS), by use of a graphite furnace, in conjunction with sample pretreatment by homogenization, was evaluated as a rapid method for the determination of bismuth, thallium and vanadium in sewage sludge. This method was compared with use of flame, electrothermal and hydride-generation (for bismuth) AAS in conjunction with conventional acid digestion and dry-ashing pretreatments and was found to be applicable to this type of sample. Comparisons were also made between flame and hydride-generation AAS in conjunction with an acid digestion pretreatment for the determination of antimony, arsenic and tellurium in sewage sludge. The hydride-generation technique was considered the better for waste-water samples because of its greater sensitivity.     

Improvements in thermospray flame furnace atomic absorption spectrometry

In thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) a nickel atomization tube is placed in the acetylene/air flame on a holder built onto a standard AAS burner head. The liquid to be analyzed is transported by a low or high-pressure pump through a very hot, simple, inexpensive ceramic capillary tip acting as a flame-heated thermospray into the flame furnace. This results in complete sample introduction and increases the residence time of the sample in the absorption volume. This leads for 17 elements to a 3-110-fold improvement in the power of detection compared to conventional flame AAS. The absolute detection limits (3s values, N=25) lie between 0.2 μg l⁻¹ (Zn) and 310 μg l⁻¹ (Se) according to the element. The R.S.D. (N=15) is 1.4-5.5% according to the element and applied concentration. TS-FF-AAS can easily be incorporated on any standard flame AAS instrument and can be automated with a standard autosampler.     

在线螯合树脂富集火焰原子吸收光谱法测定天然水体中铜和锌

对螯合树脂富集——火焰原子吸收光谱法测定天然水体中痕量铜和锌的在线富集条件、干扰因素等进行研究,在线富集倍数达到两个数量级,在灵敏度与石墨炉原子吸收光谱法相当情况下,提高了测定准确度。     

High-performance flow atomic spectrometry: New nebulization techniques,on-line speciation and on-line sample pretreatment

An interface-free combination of HPLC separation techniques and methods for element determination by atomic spectrometry can be achieved by hydraulic high-pressure nebulization (HHPN). With high-temperature HHPN (300 ( degrees )C) super heated liquids can be nebulized providing aerosol yields of up to 90% in flame AAS. This new nebulization method combines the advantages of HHPN and thermospray techniques (very small aerosol droplets, high aerosol yield, nebulization of saturated salt solutions).     

Coupling of ultrasonic nebulization to flame furnace atomic absorption spectrometry—new possibilities for trace element determination

The use of ultrasonic nebulization (USN) with desolvation system for sample introduction in flame atomic absorption spectrometry (F AAS) and flame furnace atomic absorption spectrometry (FF AAS) with a nickel tube is described. Polytetrafluorethylene (PTFE) adaptors were built to replace the pneumatic nebulizer for USN-F AAS measurements. For USN-FF AAS analysis, an alumina injector allowed the direct introduction of the dry aerosol into the nickel tube. The analytical performance of both systems is shown for Ag, Bi, Cd, Cr, Cu, Mn, Pb, Sb, Se, Tl and Zn. The results demonstrate that a sensitivity gain of up to 39 times can be achieved using USN-FF AAS, mainly due to the increase in residence time and to the absence of dilution of the analyte by the flame gases, as the atomization takes place inside the nickel tube. However, elements that require higher atomization temperatures, such as Cr and Mn, are more efficiently determined using USN-F AAS. To evaluate the accuracy of the proposed methods for the determination of trace elements, five certified reference samples were analyzed, and good agreement was, in general, achieved between certified and determined values at a 95% confidence level. The relative standard deviation was frequently below 5%, demonstrating good precision, particularly for USN-FF AAS. In this sense, coupling of USN with F AAS and especially with FF AAS has proved to be simple, safe, with high precision and good accuracy, also maintaining some of the most important features of F AAS, such as the high analytical frequency and the low running cost.     

Eine mikromethode der flammen-atomabsorptions- und emissionsspektrometrie (platinschlaufen-methode)—II: Die bestimmung von As,Bi, Cd,Hg, Pb,Sb, Se,Te, Tl,Zn/Li,Na, K,Cs, Sr,Ba

This paper described the continuation of the work of Part I dealing with a microanalytical method in which the sample is introduced into a flame using an electrically heated platinum loop. This device is used in connection with an atomic absorption (AA) spectrometer. The detection limits are one to two orders of magnitude better than those of conventional flame AAS. The reproducibility depends on the element and is in general 3–5% (relative standard deviation) for concentrations in the $\text{ng}\text{ml}$ range. The platinum loop method can be also applied for flame emission analysis of small amounts of sample or the determination of low concentrations (alkalis). This application gives access to determinations in the lower ng or the pg range (detection limit of lithium: 0.6 pg).     

Determination of barium in sulphide ores, concentrates and other geological samples by flame atomic-absorption spectrometry

A rapid, precise and selective analytical method has been developed for estimation of barium in geological samples by flame atomic-absorption spectrometry. The method consists of precipitation of barium sulphate with ammonium sulphate, followed by dissolution of the sulphates in EDTA at pH 10. The barium in this solution is measured by AAS with a nitrous oxide-acetylene flame. Appreciable amounts of lead, calcium and strontium can be tolerated in the method, which has been applied for estimation of barium in sulphide ores and concentrates of lead, zinc and copper, and is feasible for estimation of barium from 20.0 ppm to the per cent level in such geological samples.     

Indirect determination of free cyanide in industrial waste effluent by atomic absorption spectrometry

An indirect method is described for the determination of free cyanide in industrial waste effluent samples by atomic absorption spectrometry (AAS). In an alkaline medium, cyanide forms a stable complex species [Cu(BPTC)(CN)] (BPTC = 2-benzoylpyridine thiosemicarbazone), which can be extracted into a mixture of isobutyl methyl ketone-isopentyl alcohol (7 + 1) with an efficiency of greater than 98.5%. The extract can be analysed directly for copper (and hence indirectly for cyanide) by flame AAS. The calibration graph is linear up to 5.7 micrograms of cyanide per millilitre of solvent mixture and the limit of detection is 4.8 ng ml-1. A large number of foreign ions were found not to interfere with the proposed method.     

Silberhalogenide als Spurenfänger für Chelatkomplexe

The power of detection of flame AAS for trace elements decreases considerably in presence of manganese. For the purity control of manganese and manganese compounds, therefore, it is necessary to separate the traces from the main component of the samples. For that purpose the traces were complexed by 1,10-phenanthroline and coprecipitated by silver iodide as trace collector. To receive a trace solution of 10 ml being free of manganese the filtered AgI was boiled with HNO₃. The enriched elements (Fe, Co, Ni, Cu, Zn, Cd, Pb, Bi and Tl) were determined by flame AAS. Using samples of 5 to 10 g of manganese or manganese compounds of different stages of oxidation the limits of detection of the various elements were found to be in a range between 0.01 and 1 ppm. By evaporation of the trace solution down to 1 ml and determination of the traces by the “injection method” of flame AAS limits of detection are obtained between 0.007 and 0.1 ppm.