Determination of Antimony in Waters by Electrothermal Atomic Absorption Spectrometry with Preconcentration on a Tantalum Wire

 A preconcentration method for antimony in waters involving adsorption on a tantalum wire, followed by electrothermal atomic absorption spectrometry with a tungsten tube atomizer is described. The best pH for the adsorption of antimony was 2. The optimal immersing time was 120 s. Under the optimal conditions, the detection limit for antimony by the tantalum wire preconcentration method was 50 pg/mL (3S/N) and the relative standard deviation was 9.4%. The effects of large amounts of concomitants on the preconcentration of antimony were evaluated. Even though 10³–10⁴ fold excess of matrix elements existed in water, the antimony response was not significantly affected by the matrix elements. The method with preconcentration on a tantalum wire was applied to the determination of antimony in waters and proved to be sensitive, simple, and convenient. This adsorption method can be utilized in in-situ sampling of ultra-trace antimony in environmental samples (water). Furthermore, after sampling it is easy to carry and store the tantalum wire without contamination for a long time. The technique developed was shown to be useful for the determination of Sb in waste waters at the 1–5 μg/L level. Received March 20, 2002; accepted June 26, 2002     

氢化物发生电热原子吸收法测定食品中微量锑铋

本文将电热氢化物原子吸收光谱技术应用于食品中微量锑铋测定,检出限可达ppb级。探讨了被测元素价态、预还原条件等因素对测定灵敏度的影响,并应用于罐头食品中微量锑铋分析。     

Determination of Inorganic and Total Arsenic in Wines by Hydride Generation Atomic Absorption Spectrometry

A method is described for the determination of inorganic arsenic species and total arsenic in wines by means of hydride generation atomic absorption spectrometry (HGAAS). Simple ethanol evaporation is the only pretreatment procedure proposed for wine samples prior to direct measurement of inorganic arsenic (AsIII) and As(V) species by HGAAS. The total arsenic content is determined after microwave digestion of the wine samples. The optimal parameters for the microwave digestion procedure and the next HGAAS measurement of arsenic are established. The detection limits achieved are 0.1µgL^–1 for inorganic and total arsenic determination. The relative standard deviation for both procedures and for ten independent determinations varied between 8 and 15% for arsenic species in the range of 1–30µgL^–1. The accuracy of the procedure for total arsenic determination was proved by comparative analysis using electrothermal atomic absorption spectrometry.     

微型氢化物原子吸收法测锑的研究及冶金样品中微量锑的测定

本文建立了一个微型氢化物发生原子吸收法测定微量锑的方法。用CyDTA 和8-羟基喹啉-草酸分别消除了钴和镍的干扰,采用峰面积测量模式,灵敏度22pg/1％。同时对镍的液相干扰机制做了一些探讨。     

Enhancement of Sensitivity for Antimony Determination in Atomic Absorption Spectrophotometry by Introducing Stibine into an Argon-Hydrogen Flame

Abstract

The sensitivity of antimony determination with atomic absorption spectrophotometry is enhanced to a large extent by introducing stibine gas into an argon-hydrogen flame. As a reducing agent, zinc tablet made from the zinc powder paste with water is successfully used for quantitative and rapid productions of stibine from antimony (III) solution. The sensitivity for 1% absorption of the signal is estimated to be about 0.004 ppm of antimony.     

原子吸收光谱和原子发射光谱法测定工业废水中的总铬

为了探讨原子吸收光谱法和原子发射光谱法测定工业废水中的总铬分析方法的异同,分别采用两种方法对工业废水中的总铬进行了对比分析,对样品前处理方法,方法的标准曲线、检出限、准确度、精密度、干扰及消除等进行了比较,并对两种方法的测定结果进行t检验。结果表明,两种方法具有良好的一致性。相对来说,原子发射光谱法各方面指标要优于原子吸收光谱法。     

铟氢化物发生原子吸收方法研究

本文对铟氢化物发生方法进行了探讨，所采用的方法使铟氢化物的发生效率明显提高。在电加热石英管原子化器中得到的测定灵敏度为０．００７μｇ／（１％吸收），比文献报道值提高了一个数量级。并讨论了铟氢化物的发生机理与原子化机理。     

The Simultaneous Arsenic,Antimony, and Selenium Determination in Water Samples by Batch Hydride Generation Atomic Absorption Spectrometry

The purpose of this paper is to present a procedure for the simultaneous determination of metalloids: arsenic, antimony, and selenium. Hydride generation was provided in a reaction vessel connected with the atomic absorption spectrometer (AAS) in a fast sequential mode. Two different types of water samples were used while developing the application: seawater and groundwater. The methodology of liquid samples analysis was developed with detection limits of 0.05, 0.03, and 0.06 ng · mL^?1 for arsenic, antimony, and selenium, respectively, in 10 mL samples. This methodology was used to determine arsenic, antimony, and selenium in natural water samples.     

火焰原子吸收分光光度法测大沂河水体的重金属含量

采用火焰原子吸收分光光度法测定了山东省曲阜市大沂河水体的重金属铜、铅、镉、锌含量。结果表明,大沂河水体中铜、铅、镉、锌的最高含量分别为0.018,0.230,0.176,0.490mg/L,其中铅和镉的含量超过国家Ⅴ类水标准。     

电热原子吸收光谱法测定水中总钼

建立电热原子吸收法测定水中总钼的含量。样品采用硝酸–过氧化氢消解,热解涂层石墨管减小记忆效应,塞曼背景校正消除背景噪声。检测了27种共存离子的干扰影响。经6家实验室对标准物质和实际样品检测验证,方法检出限为0.6μg/L,能够满足微量检测要求。钼测定结果相对误差最大值为–6.2%,实验室内相对标准偏差为4.5%~7.6%(n=6),实验室间相对标准偏差为4.3%~5.7%(n=6),加标回收率为91.8%~104.0%。该方法精密度和准确度满足我国地下水和废水监测技术规范的质控要求。     

原子吸收法测定碱性锌锰电池中铅的探讨

探讨了使用HCl-HF-HClO4分解体系，对碱性锌锰电池进行预处理，测定总铅含量的方法。     

氢化物－原子吸收光谱法测定六味地黄丸中砷和锑

本文建立了氢化物原子吸收光谱法测定六味地黄丸中砷和锑的方法。方法的相对标准偏差砷为１．３％、锑为１．６％，回收率在９０％～１１０％之间，检出限分别为砷０．０６ｎｇ／ｍＬ、锑０．１ｎｇ／ｍＬ。本方法可用于中成药中砷和锑的测定。     

冷原子吸收光谱法结合热解-原子吸收光谱法快速测定废水样中痕量无机汞和总有机汞

提出以冷原子吸收光谱法结合热解-原子吸收光潜法测定废水样中的痕量无机汞和总有机汞、水样经0．45μm膜过滤后不需消化处理,直接用冷原子吸收光谱法测定无机汞含量．用热解法测定总汞含量,二者之差为总有机汞含量。方法简便快速,干扰少．经加标回收实验验征,回收率为90％～103％．相对标准偏差(n=11)为3．8％。     

Determination of Antimony in Brass by On-line Hydride Generation Atomic Fluorescence Spectrometry Alkaline Solution

The hydride generation(HG) technique combined with atomic spectrometry as a detection system has become one of the most powerful analytical tools for the determination of elements, such as As, Sb, Bi, Se, Te,Ge, Sn and Pb. Normally, the hydride is generated by the reaction between an acidic sample solution with tetrahydroborate. However, when some inorganic ions such as the transition metal ions are present in the reaction matrix, interference arise. Some approaches for minimizing the interference have been suggested, including the addition of various reagents such as thiourea and iron(III) solution. Interfering metals can also be removed by precipitation. The procedure involved filtration before the solution was acidified. In order to reduce the steps of the process, hydride generation from alkaline solution was described for the determination of selenium in copper and nickel materials.     

火焰原子吸收分光光度法测定维血康颗粒中总铁

建立火焰原子吸收分光光度法测定维血康颗粒中总铁的含量,火焰类型选择空气–乙炔,测定波长为248.3 nm,测定时间为4.0 s,燃气流量为0.9 L/min,以氘灯作为背景校正。铁的质量浓度在2.4~28.8μg/mL范围内与吸光度呈良好的线性,线性相关系数r~2=0.999 8。6次测定结果的相对标准偏差小于1.0%,样品加样回收率为93.89%,方法检出限为0.011 3μg/mL。该方法具有准确度高,稳定性、重复性好等优点,可用于维血康颗粒中总铁含量的测定。     

氢化物发生-原子吸收光谱法测定萤石粉中砷

提出了以氢化物发生-原子吸收光谱法测定萤石粉中砷的方法,研究了酸介质、还原剂、载气流量等因素对测定的影响,并选择出最佳工作条件.砷的检出限为0.052μg·g-1,线性范围为0.10～6.00 μg·L-1,回收率在90.0%～102.0%之间,相对标准偏差为9.8%.     

原子吸收和原子荧光光谱分析

本文是《分析试验室》期刊定期评述中关于原子吸收光谱(AAS)及原子荧光光谱(AFS)分析的第10篇综述文章。文中对2002年12月～2004年11月期间我国在AAS/AFS领域所取得的主要进展进行评述。内容包括概述、仪器装置与数据处理、火焰原子吸收光谱法、电热原子吸收光谱法、化学蒸气发生技术以及原子荧光光谱法等。收集文献511篇。     

Determination of Antimony in Sediments by Zeeman-Corrected Electrothermal Atomic Absorption Spectrometry with Ultrasonic Slurry Sampling

A method was developed for the determination of antimony in slurried sediments (on the basis of samples of three Certified Reference Materials) by electrothermal atomic absorption spectrometry (ETAAS) with Zeeman-effect background correction. Slurried samples were prepared in 6% nitric acid containing 0.02% of Triton X-100. A mixed palladium/magnesium chemical matrix modifier, L'vov platform atomization and a temperature-time program with a relatively short (10 s) sample pyrolysis stage were used. The results of the determinations by this technique are in very close agreement with certified values and the repeatability of this analytical procedure expressed in terms of relative standard deviation was typically better than 9% at the slurry concentration of approx. 90 mg/2 mL. The characteristic mass of Sb (at the spectral line 231.1 nm) was 25.6 pg and the limit of detection (calculated for 100 mg/2 mL slurry) was about 0. 04 μg/g.     

平台石墨炉原子吸收法直接测定镍基合金中铅和锑

平台石墨炉原子吸收法直接测定镍基合金中铅和锑谢文兵，姚金玉，胡庆兰（中国科学院长春应用化学研究所长春１３００２２）关键词石墨炉原子吸收，镍合金，铅，锑，基体改进剂石墨炉原子吸收法是测定痕量元素最有效的方法之一。但是铅和锑都是易挥发元素，为了增强灰化过...     

天然水中痕量无机汞和有机汞的氢化物原子荧光光谱法分析

建立了天然水中溶解的痕量无机汞和有机汞的氢化物原子荧光光谱法分析方法,该方法经标准物质(PACS-1)和加标回收实验研究表明重现性好、准确度高。在此基础上,应用该方法分析了该校人工湖水中的无机汞和有机汞,发现无机汞和有机汞的含量均低于0.1 礸/L。