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一种新型多火焰光度检测器中线性硫响应模式的特性。

Properties of a novel linear sulfur response mode in a multiple flame photometric detector.

机构信息

Department of Chemistry, University of Calgary, Calgary, AB, Canada T2N 1N4.

Department of Chemistry, University of Calgary, Calgary, AB, Canada T2N 1N4.

出版信息

J Chromatogr A. 2014 Jan 24;1326:103-9. doi: 10.1016/j.chroma.2013.12.050. Epub 2013 Dec 25.

Abstract

A new linear sulfur response mode was established in the multiple flame photometric detector (mFPD) by monitoring HSO* emission in the red spectral region above 600nm. Optimal conditions for this mode were found by using a 750nm interference filter and oxygen flows to the worker flames of this device that were about 10mL/min larger than those used for monitoring quadratic S2* emission. By employing these parameters, this mode provided a linear response over about 4 orders of magnitude, with a detection limit near 5.8×10(-11)gS/s and a selectivity of sulfur over carbon of about 3.5×10(3). Specifically, the minimum detectable masses for 10 different sulfur analytes investigated ranged from 0.4 to 3.6ng for peak half-widths spanning 4-6s. The response toward ten different sulfur compounds was examined and produced an average reproducibility of 1.7% RSD (n=10) and an average equimolarity value of 1.0±0.1. In contrast to this, a conventional single flame S2* mode comparatively yielded respective values of 6.7% RSD (n=10) and 1.1±0.4. HSO* emission in the mFPD was also found to be relatively much less affected by response quenching due to hydrocarbons compared to a conventional single flame S2* emission mode. Results indicate that this new alternative linear mFPD response mode could be beneficial for sulfur monitoring applications.

摘要

一种新的线性硫响应模式在多火焰光度检测器(mFPD)中建立,通过监测 600nm 以上的红色光谱区域中的 HSO发射。通过使用 750nm 干涉滤光片和向该装置的工作火焰供应约 10mL/min 大于用于监测二次 S2发射的氧气流,找到了该模式的最佳条件。通过采用这些参数,该模式在约 4 个数量级范围内提供了线性响应,检测限接近 5.8×10(-11)gS/s,硫对碳的选择性约为 3.5×10(3)。具体而言,对于跨度为 4-6s 的 10 种不同硫分析物进行调查,检测到的最小可检测质量范围从 0.4 到 3.6ng。对十种不同的硫化合物的响应进行了检查,平均重现性为 1.7%RSD(n=10),平均等摩尔值为 1.0±0.1。相比之下,传统的单火焰 S2模式分别产生 6.7%RSD(n=10)和 1.1±0.4 的值。与传统的单火焰 S2发射模式相比,mFPD 中的 HSO*发射也被发现相对较少受到由于碳氢化合物导致的响应猝灭的影响。结果表明,这种新的替代线性 mFPD 响应模式可能有益于硫监测应用。

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