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Chemical modification for sulfur determination in human hair by high-resolution continuum source graphite furnace molecular absorption spectrometry
Spectrochimica Acta Part B: Atomic Spectroscopy ( IF 3.3 ) Pub Date : 2020-12-01 , DOI: 10.1016/j.sab.2020.106008
Vitor Cornaqui P. Marrocos , Rodrigo Araújo Gonçalves , Fábio G. Lepri , Tatiana D. Saint'Pierre

Abstract This paper presents the study of chemical modification for sulfur determination in human hair samples by high-resolution continuum source molecular absorption spectrometry in a graphite furnace (HR-CS GF MAS) via molecular absorption of CS. The thermal behavior of inorganic and organic S species was studied without and with the use of chemical modifiers. Without chemical modification, sulfur species were lost in the pyrolysis step, especially when using organic standards. The combination of a mixture of modifiers Pd + Mg (15 + 10 μg) in solution and W (800 μg) as a permanent modifier allowed the accurate determination of S in hair samples at 900 °C pyrolysis and 2400 °C vaporization temperatures, by using an inorganic sulfur standard for constructing the calibration curve. Accuracy was checked by the analysis of the certified reference material NSC DC73347a (human hair), with the recovery of the certified value better than 98%. The results obtained for 14 human hair samples by the proposed method were in agreement with those obtained by ICP OES, according to the paired t-test, with a 95% level of confidence.

中文翻译:

高分辨连续源石墨炉分子吸收光谱法测定人发中硫的化学修饰

摘要 本文介绍了通过石墨炉中高分辨率连续源分子吸收光谱法 (HR-CS GF MAS) 通过 CS 的分子吸收来测定人头发样品中硫的化学改性研究。在不使用和使用化学改性剂的情况下研究了无机和有机 S 物质的热行为。如果没有化学改性,硫物质会在热解步骤中丢失,尤其是在使用有机标准品时。将溶液中的改性剂 Pd + Mg (15 + 10 μg) 和作为永久性改性剂的 W (800 μg) 的混合物组合使用,可以在 900 °C 热解和 2400 °C 蒸发温度下准确测定头发样品中的 S,通过使用无机硫标准构建校准曲线。通过对有证标准物质 NSC DC73347a(人发)的分析来检查准确度,认证值的回收率优于 98%。根据配对 t 检验,通过所提出的方法获得的 14 个人发样本的结果与 ICP OES 获得的结果一致,置信水平为 95%。
更新日期:2020-12-01
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