氢化物发生辅助雾化火焰原子吸收法测定人发中的铅

使用氢化物发生辅助雾化的火焰原子吸收法,在K₃Fe(CN)₆-HCl体系中,测定了头发中铅的含量。对酸度、氧化剂及浓度、NaBH₄的浓度及流速对Pb测定的影响分别进行了研究。与传统雾化火焰原子吸收法相比,本方法测铅的灵敏度提高了13.4倍。方法的检出限为2.8 μg·L-1,精密度(RSD)为1.4%。用于测定人发中的Pb,回收率达96%～99%。     

原子吸收法测定背角无齿蚌中的重金属

测定太湖五里湖水域代表样点的背角无齿蚌 (Anodonta woodiana)体内 Zn、Cu、Cd、Pb、As5种重金属 ,Cu和 Zn选用火焰原子吸收法 ;Cd和 Pb选用石墨炉原子吸收法 ;As选用氢化物原子吸收法。对样品前处理方法和分析条件进行了探讨和优化。在优化的实验条件下用国标物质贻贝验证 ,获得较满意的准确度和精密度 ,方法可用于背角无齿蚌及其他水产类的重金属元素测定。     

一种简易火焰氢化法原子吸收测定矿石及金属铅中微量铋

氢化物-原子吸收法,是70年代发展起来的一种分析方法。此法可以灵敏地测定砷、锑、铋、锡、硒、碲等元素。但需用专门的装置,干扰较多,精度较差,不能满足较高含量的各种矿石、精矿样品的分析。近年来,国內研制一种简单、快速,不用特殊装置的双毛细管喷雾器、双喷雾器对吹的火焰氢化物-原子吸收法。灵敏度比一般的空气-乙炔火焰法提高一个数量级,并具有干扰少,精度高等特点。本文提出另一种更简易的方法。经实验证明,其效果与上述方法一样。由于容易制造很适合一般实验室使用。铋的灵敏度为0.015μg/ml,仪器精度可达0.2％,相对标准偏差≤2.0％。可测定矿石、钨、铜、铅、锌、镉精矿中0.00x％和金属铅中0.000x％的铋。     

基体改进效应用于石墨炉原子吸收法测定血清中硒

硒在生物体中既是一个必要的营养元素,又是一个毒性元素。人体血液中硒含量与人体健康密切相关。痕量元素硒的分析对生理、病理的研究及环境保护均具有重要意义。有关硒的测定,已有一些文献报导。以往多采用分光光度法,氢化物发生原子吸收法,分析前样品需要预处理,操作比较繁琐,且在消化过程中分析物易挥发损失。近年来,用非火焰原子吸收测定硒,具有灵敏度高,快速,简便的特点。     

硒的原子吸收分析进展

本文对1985年以来硒的原子吸收分析,从石墨炉法、氢化物法、氢化物-石墨炉法和火焰法四个方面的分析进展进行综合评述。     

原子捕获－火焰原子吸收光度法测定火药烟晕中微量铅和锑

本文采用双缝式原子捕获石英管在火焰原子吸收分光光度计上测定火药烟晕中微量铅和锑，研究了捕获的时间及乙炔的流量等测试条件。实验表明：本法提高了原子吸收分光光度法的灵敏度，铅提高４倍，锑提高了９倍。方法的回收率铅为９８．６～１０４％；锑为９８～１１０％。     

原子捕获—火焰原子吸收光度法测定火药烟晕中微量铅和锑

本文采用双缝式原子捕获石英管在火焰原子吸收分光光度计上测定火药烟晕中微量铅和锑，研究了捕获的时间及乙炔的流量等测试条件。实验表明，本文提高了原子吸收分光光度法的灵敏度，铅提高４倍，锑提高了９倍，方法的回收率铅为９８．６～１０４％，锑为９８～１１０％。     

氢化物-原子吸收法测定钢和生铁中痕量砷、锑、铅、锡、铋、硒、碲

本文提供了测定钢和生铁中砷、锑、铋、铅、硒、碲以及锡的分析方法,是以这些元素挥发性的氢化物放出,然后在无火焰电加热石英管中用原子吸收法测定之。通过位于石英管中部的侧管导入氢化物,在氮气流中热分解这些元素的氢化物,用一股横向氮气流可防止过量的氢气在管子的两端着火。本法的灵敏度比氩-氢-夹杂空气的火焰中分解法灵敏度提高一倍,因为在光路中原子云停留较长的时间,而且大大地降低了噪音水平。     

石英缝管原子捕集-火焰原子吸收光谱法测定化探样品中的铅

采用石英缝管原子捕集技术,可实现原子高效捕集和瞬间释放,使火焰原子吸收法测定铅的灵敏度比常规FAAS测定铅的灵敏度提高三至四倍。精密度与火焰原子吸收法相同。通过实验,建立了石英缝管原子捕集-火焰原子吸收光谱法测定化探样品中铅的分析方法,方法的检出限（CL）可达3.82μg/g,精密度（RSD）可达1.72%,应用于化探样品中铅的测定效果令人满意。     

单缝石英管火焰原子吸收法测定大米中微量铜

本文根据文献报道使用单缝石英管火焰原子吸收法提高火焰原子法的灵敏度,对大米中微量铜的测定进行研究。方法简单、快速,文献尚未见报道。由实验得到了比较满意的分析结果,回收率为96～102%。变异系数为1.9%,灵敏度可提高3倍。     

Flame Furnace Atomic Absorption Spectrometry: A Review

Abstract

Flame atomic absorption spectrometry (FAAS) is one of the most widespread traditional analytical techniques for trace element determination, but it often suffers from poor sensitivity due to the low nebulization efficiency and the short residence time of free atoms in the flame. On the basis of conventional FAAS, flame furnace atomic absorption spectrometry (FF-AAS) is developed with a tube (flame furnace) placed on top of the FAAS burner for the atomization. Sample is introduced via beam injection (BIFF-AAS) or thermospray (TS-FF-AAS). Due to the total sample introduction and prolonged residence time of free atoms in the flame furnace, marked sensitivity improvement is obtained for volatile and semivolatile elements over conventional FAAS. TS-FF-AAS can be employed as an element-selective detector for GC, HPLC, or CE for studying of metal speciation analysis and metallomics. In addition, three newly developed sample introduction methods, including ultrasonic nebulization, hydride generation, and pneumatic nebulization, are discussed. The analytical figures of merit and practical applications of FF-AAS in analytical atomic spectrometry are reviewed in this article.     

Atomic Absorption Spectrometry of Silver with Absorption Tube Having Nebulization Chamber

In the atomic absorption spectrometry with the long absorption tube using a hydrogen-air flame, only the total consumption type of the burners, e.g., Beckman¹ or ring burners², have been used for the input of a sample solution to the flame. The use of the indirect input method with nebulization chamber has never been attempted, though, by use of a commercially available apparatus with nebulization chamber, the large increase of the sensitivity has been easily obtained by heating the chamber and nebulizing air^3–5.     

Determination of Cu,Zn, and Se in microvolumes of liquid biological samples

Cu, Zn, and Se were successfully determined in a few microliters (<100 μl) of biological samples using discrete injection atomic absorption spectrometry. Different factors were investigated in order to obtain a biological sample volume which is valid for analysis. Among them are the effect of microsampling volume variations (starting from 40 to 200 μl), nebulization efficiency, detection limits, precision, and finally the calibration and sensitivity of the proposed method. It was found that 60 μl of the biological sample was adequate for the quantitative analysis with reasonable precision. The advantages of the proposed method are not only rapidity, simplicity, sensitivity, and good precision, but also, contrary to conventional flame atomic absorption spectrometry, the capability of analyzing microvolumes of samples.     

富氧空气-乙炔火焰原子吸收光谱法测定地质样品中痕量铍

研究了用富氧空气-乙炔火焰原子吸收光谱法测定铍的分析方法。当空气流量为6.0 L·min-1,氧气流量为4.2 L·min-1,乙炔流量为7.4 L·min-1时铍有较高的吸光度。在2.5%的8-羟基喹啉介质中,能较好地消除基体干扰且有一定的增感作用。方法的检测限为0.006 μg·mL-1,测定精密度RSD为4.69％,测定地质标准物质中铍的结果与鉴定值吻合。     

火焰原子吸收法间接测定混凝土外加剂中的微量Cl-

火焰原子吸收法以其灵敏度高、选择性好等优点而广泛应用于各种基体中微量金属元素的测定 ,而不用于直接测定Cl- 。本文提出了采用火焰原子吸收法间接测定混凝土外加剂中微量Cl- 的方法 ,在待测液中加入过量的Ag 标液 ,通过测定与Cl- 定量反应后剩余的Ag 量从而换算出Cl- 的含量 ,本法进行了测定最佳酸度试验、精密度试验、在样品中加入Cl- 标准溶液回收试验 ,回收率为 96 %～ 10 4 %。经过实际样品测定 ,证明该方法具有样品预处理手续简单、测定周期短、干扰小等优点 ,最适合于测定基体较为复杂的混凝土外加剂中的微量Cl- 。称取样品 0 0 5～ 2g ,溶解后 ,用硝酸调节酸度 ,加入与之对应的Ag 标准溶液 ,放置 2h过滤后即可测定 ,所用仪器为澳大利亚GBC90 2型原子吸收光谱仪。     

Increasing the sensitivity of atomic absorption determination of iron

We have studied the effect of the nature and concentration of surfactants on the atomic absorption of iron. We show that using sodium dodecylbenzenesulfonate as the modifier in flame atomic absorption determination of iron in real samples makes it possible to make the measurements in a low-temperature flame (propane-butane-air type) with increased sensitivity and selectivity and also a lower detection limit for iron. We have developed a procedure for atomic absorption determination of iron in food products using sodium dodecylbenzenesulfonate as the modifier. The detection limit for iron is C_min = 0.008 μg/cm³. Report given at the International Congress of Analytical Sciences, ICAS-2006, 20–30 June 2006, Moscow, Russia __________ Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 74, No. 2, pp. 263–266, March–April, 2007.     

FAAS和HG-AFS研究野生葛根中微量元素的溶出特性

采用HNO₃-HCIO₄消解体系,应用火焰原子吸收光谱法（FAAS）和氢化物发生-原子荧光光谱法（HG-AFS）测定了洞口县野生葛根中Zn、Fe、Cu、Mn等15种微量元素的含量,方法对试样中各元素测定的相对标准偏差（RSD）为1.07%—4.29%,加标回收率为90.00%—104.00%,方法快速、准确、灵敏度高,适用于葛根中微量元素含量的测定。同时考察了微波提取、超声提取和传统煎煮法对野生葛根中15种微量元素的溶出情况。结果表明:野生葛根溶出液中含量较多元素的顺序为:Zn>Cu>Mn>Se>Fe,其余元素的含量均很少;野生葛根中Zn、Cu、Mn和Se的水溶性强,其溶出率比Fe高很多。     

在线流动注射N1923萃淋树脂预富集火焰原子吸收法测定痕量金

研究了富集酸度、进样体积、洗脱流速、富集时间、洗脱液的浓度和酸度、共存离子的影响 ,建立了N1 92 3萃淋树脂富集在线流动注射火焰原子吸收法测定痕量金的新方法。富集倍率为 32倍 ,检测限为 1 μg·L- 1 。用于电镀金废液的在线测定 ,方法灵敏度高、操纵简便、结果较好。     

Improved Performance of On-line Atom Trapping in Flame Furnace Atomic Absorption Spectrometry by Chemical Vapor Generation: Determination of Cadmium in High-Salinity Water Samples

ABSTRACT

On-line atom trapping inside a nickel flame furnace using chemical vapor generation for sample introduction was proposed for the determination of trace cadmium by flame atomic absorption spectrometry (AAS). Cadmium volatile species was generated upon reaction with potassium borohydride and then flushed into a flame furnace for on-line trapping by a flow of nitrogen carrier gas. The middle part of the flame furnace, where the carrier gas impacts, is cooled by the gas flow, and this provides a fine strategy for on-line atom trapping for the purpose of preconcentration. A stainless steel plate is put on the top of the flame burner in the middle to form a flame-free zone, which also greatly lowers the temperature of the flame furnace and facilitates the atom-trapping process. Due to the introduction of chemical vapor generation, matrix effect was greatly alleviated compared with direct pneumatic nebulization for on-line atom trapping in flame furnace AAS. With trapping time of 35 s, the current approach achieved an excellent limit of detection of 20 ng L^?1. The proposed method was successfully applied for the quantification of cadmium in high-salinity samples.