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采用端盖石墨管电热原子吸收光谱法同时测定尿液中的镉和铅

Multielement determination of cadmium and lead in urine by simultaneous electrothermal atomic absorption spectrometry with an end-capped graphite tube.

作者信息

Correia Paulo R M, Nomura Cassiana S, Oliveira Pedro V

机构信息

Instituto de Química, Universidade de São Paulo, C. P. 26077, CEP 05513-970, São Paulo, SP, Brasil.

出版信息

Anal Sci. 2003 Nov;19(11):1519-23. doi: 10.2116/analsci.19.1519.

Abstract

A method for the multielement determination of cadmium and lead in urine is proposed by simultaneous electrothermal atomic absorption spectrometry (SIMAAS) with an end-capped transversely heated graphite atomizer (EC-THGA). The best conditions for cadmium and lead determination were obtained in the presence of NH4H2PO4 as a chemical modifier, using 500 degrees C and 1800 degrees C as the pyrolysis and atomization temperatures, respectively. Urine samples were diluted 1 + 4 directly in autosampler cups with a mixture of 0.125% (w/v) Triton X-100 + 2.5% (v/v) HNO3 + 0.31% (w/v) NH4H2PO4. The optimized heating program was carried out in 57 s, and the instrument calibration was done with aqueous reference solutions. The use of EC-THGA increased the sensitivity of cadmium and lead by 14% and 25%, respectively. The detection limits (n = 20, 3delta) were 0.03 microg L(-1) (0.36 pg) for cadmium and 0.57 microg L(-1) (6.8 pg) for lead. The performance of EC-THGA was acceptable up to 500 heating cycles. The reliability of the entire procedure was checked with the analysis of a lyophilized urine certified reference material. The found concentrations were in agreement with the recommended values (95% confidence level).

摘要

本文提出了一种采用带端盖的横向加热石墨原子化器(EC - THGA)的同步电热原子吸收光谱法(SIMAAS)对尿液中的镉和铅进行多元素测定的方法。在以磷酸二氢铵(NH4H2PO4)作为化学改进剂的情况下,分别采用500℃和1800℃作为镉和铅测定的灰化温度和原子化温度,从而获得了最佳测定条件。尿液样品直接在自动进样器杯中用含有0.125%(w/v) Triton X - 100 + 2.5%(v/v)硝酸 + 0.31%(w/v)磷酸二氢铵的混合溶液按1 + 4进行稀释。优化后的加热程序在57秒内完成,仪器校准采用水基标准溶液。使用EC - THGA使镉和铅的灵敏度分别提高了14%和25%。镉的检测限(n = 20,3δ)为0.03 μg L-1(0.36 pg);铅的检测限为0.57 μg L-1(6.8 pg)。在高达500次加热循环的情况下,EC - THGA的性能是可接受的。通过对冻干尿液有证标准物质的分析来检验整个程序的可靠性。测定结果与推荐值相符(95%置信水平)。

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