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高分辨连续光源火焰原子吸收光谱法测定煤样中硫的实用方法。

A practical method for the determination of sulphur in coal samples by high-resolution continuum source flame atomic absorption spectrometry.

机构信息

Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469 Maslak, Istanbul, Turkey.

出版信息

Talanta. 2011 Oct 15;85(5):2662-5. doi: 10.1016/j.talanta.2011.08.038. Epub 2011 Aug 26.

DOI:10.1016/j.talanta.2011.08.038
PMID:21962699
Abstract

Sulphur in coal was determined using a high-resolution continuum source flame atomic absorption spectrophotometer (HR-CS-FAAS) with actylene/air flame. The C-S absorption band at 258.056 nm was found the most suitable analytical line with respect to sensitivity and spectral interferences. The instrumental parameters were optimized. The coal samples were dried and dissolved using microwave-assisted digestion technique. The validity of the method was tested using standard reference material and certified values were found in the limits of 95% confidence level. Since the concentrations of matrix elements of coal other than carbon are low enough not to cause any spectral interferences, the linear calibration method was applied in all quantifications without any problem. The calibration standards were prepared in sulphuric acid. The method was accurate, fast, simple and sensitive. The limit of detection (LOD, 3δ, N=10) and the limit of quantification (LOQ, 10δ, N=10) were found to be 0.01 and 0.03% (w/w), respectively. The sulphur concentrations of various kinds of the coal samples received around Turkey were determined. The sulphur contents of the coal samples were ranged from ≤ LOQ to 1.2%.

摘要

采用乙炔/空气火焰的高分辨连续光源火焰原子吸收分光光度法(HR-CS-FAAS)测定煤中的硫。在灵敏度和光谱干扰方面,258.056nm 处的 C-S 吸收带被认为是最适合的分析线。优化了仪器参数。煤样采用微波辅助消解技术进行干燥和溶解。使用标准参考物质验证了方法的有效性,在 95%置信水平的范围内发现了认证值。由于除碳以外的煤基质元素的浓度足够低,不会引起任何光谱干扰,因此无需任何问题即可在所有定量分析中应用线性校准方法。校准标准在硫酸中制备。该方法准确、快速、简单、灵敏。检测限(LOD,3δ,N=10)和定量限(LOQ,10δ,N=10)分别为 0.01%和 0.03%(w/w)。测定了土耳其各地收到的各种煤样中的硫浓度。煤样中的硫含量范围为≤检出限到 1.2%。

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