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采用直接固体进样和石墨炉中 CS 分子的高分辨率连续光源分子吸收光谱法测定煤中的硫。

Determination of sulfur in coal using direct solid sampling and high-resolution continuum source molecular absorption spectrometry of the CS molecule in a graphite furnace.

机构信息

Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC, Brazil.

出版信息

Talanta. 2013 Mar 15;106:368-74. doi: 10.1016/j.talanta.2013.01.004. Epub 2013 Jan 29.

Abstract

An analytical method has been developed for the determination of sulfur in coal using direct solid sample analysis in a graphite tube furnace and high-resolution continuum source molecular absorption spectrometry (HR-CS GF MAS). The molecular absorbance of the carbon monosulfide molecule (CS), which is formed in the vaporization stage, has been measured using the rotational line at 258.033 nm. Several chemical modifiers were tested and Ru, applied as permanent modifier was chosen, because it exhibited the best performance. The optimum pyrolysis and vaporization temperatures were found to be 500 °C and 2200 °C, respectively. Aqueous standard solutions prepared from l-cysteine were used for calibration, as the linear regression obtained for this standard was not significantly different from that for a certified coal reference material (CRM) according to a Student t-test. The results obtained for sulfur in three coal CRM and six additional samples also showed no significant difference for the two calibration techniques according to the same statistical test. The sulfur concentration in the coal samples was found between 3.5 mg g(-1) and 33.7 mg g(-1) with a typical repeatability around 10%. The limit of detection for the direct analysis of solid coal samples was better than 0.1 μg S.

摘要

已开发出一种使用石墨管炉和高分辨率连续光源分子吸收光谱法(HR-CS GF MAS)直接对固体煤样进行分析的方法,用于测定煤中的硫。在蒸发阶段形成的一硫化碳(CS)分子的分子吸收在 258.033nm 的旋转线上进行测量。测试了几种化学改性剂,选择了 Ru 作为永久性改性剂,因为它表现出最佳的性能。发现最佳的热解和蒸发温度分别为 500°C 和 2200°C。使用 L-半胱氨酸的水溶液标准溶液进行校准,因为根据学生 t 检验,此标准的线性回归与经过认证的煤标准物质(CRM)的线性回归没有显着差异。根据相同的统计检验,对三种煤 CRM 和六个附加样品中的硫进行的测定结果也表明,两种校准技术之间没有显着差异。煤样品中的硫浓度在 3.5mg g(-1)至 33.7mg g(-1)之间,典型的重复性约为 10%。直接分析固体煤样的检出限优于 0.1μg S。

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