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在样品比色皿-钨舟炉中进行炉内熔融后,通过电热蒸发电感耦合等离子体质谱法(ETV-ICP-MS)直接测定生物样品中的铅。

Direct determination of lead in biological samples by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) after furnace-fusion in the sample cuvette-tungsten boat furnace.

作者信息

Okamoto Y

机构信息

Department of Chemistry, Graduate School of Science, Hiroshima University, Higashihiroshima, Japan.

出版信息

Fresenius J Anal Chem. 2000 Jun;367(3):300-5. doi: 10.1007/s002160000336.

Abstract

The newly conceived electrothermal vaporization (ETV) system using a tungsten boat furnace (TBF) sample cuvette was designed for the direct analysis of solid samples with detection by inductively coupled plasma mass spectrometry (ICP-MS). Into this small sample cuvette, a solid mixture of the biological samples and diammonium hydrogenphosphate powder as a fusion flux was placed and situated on a TBF. Tetramethylammonium hydroxide solution was added to the mixture. After the on-furnace digestion had been completed, the analyte in the cuvette was vaporized and introduced into the ICP mass spectrometer. The solid samples were analyzed by using a calibration curve prepared from the aqueous standard solutions. The detection limit was estimated to be 5.1 pg of lead, which corresponds to 10.2 ng g(-1) of lead in solid samples when a prepared sample amount of 1.0 mg was applied. The relative standard deviation for 8 replicate measurements obtained with 100 pg of lead was calculated to be 6.5%. The analytical results for various biological samples are described.

摘要

新构思的采用钨舟炉(TBF)样品比色皿的电热蒸发(ETV)系统,设计用于通过电感耦合等离子体质谱法(ICP-MS)检测直接分析固体样品。在这个小样品比色皿中,放置生物样品与作为助熔剂的磷酸氢二铵粉末的固体混合物,并置于钨舟炉上。向混合物中加入氢氧化四甲铵溶液。炉内消解完成后,比色皿中的分析物被蒸发并引入ICP质谱仪。通过使用由水溶液标准溶液制备的校准曲线对固体样品进行分析。检测限估计为5.1 pg铅,当应用1.0 mg的制备样品量时,相当于固体样品中10.2 ng g⁻¹的铅。用100 pg铅进行8次重复测量得到的相对标准偏差经计算为6.5%。描述了各种生物样品的分析结果。

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