Pandey Sudhir Kumar, Kim Ki-Hyun
Department of Earth & Environmental Sciences, Atmospheric Environment Laboratory, Sejong University, Seoul 143-747, Republic of Korea.
Anal Chim Acta. 2008 May 19;615(2):165-73. doi: 10.1016/j.aca.2008.03.055. Epub 2008 Apr 4.
In this study, the fundamental aspects of gas chromatography with a pulsed flame photometric detector were investigated through the calibration of gaseous reduced sulfur compounds based on the direct injection method. Gaseous standards of five reduced sulfur compounds (hydrogen sulfide, methane thiol, dimethyl sulfide, carbon disulfide, and dimethyl disulfide) were calibrated as a function of injection volume and concentration level. The results were evaluated by means of two contrasting calibration approaches: fixed standard concentration method (variable volumetric injection of standard gases prepared at a given concentration) and fixed standard volume method (injection of multiple standards with varying concentrations at a given volume). The optimum detection limit values of reduced sulfur compounds, when estimated at 100microL of injection volume, ranged from 2.37pg (carbon disulfide) to 4.89pg (dimethyl sulfide). Although these detection limit values improved gradually with decreasing injection volume, the minimum detectable concentration (e.g., in nmolmol(-1) scale) remained constant due to a balance by the sample volume reduction. The linearity property of pulsed flame photometric detector also appeared to vary dynamically with changes in its sensitivity. According to this study, the performance of pulsed flame photometric detector, when tested by direct injection method, is highly reliable to precisely describe the behavior of reduced sulfur compounds above approximately 20nmolmol(-1).
在本研究中,通过基于直接进样法对气态还原态硫化合物进行校准,研究了配备脉冲火焰光度检测器的气相色谱的基本特性。对五种还原态硫化合物(硫化氢、甲硫醇、二甲基硫醚、二硫化碳和二甲基二硫醚)的气态标准品进行校准,作为进样体积和浓度水平的函数。通过两种对比校准方法对结果进行评估:固定标准浓度法(可变体积进样给定浓度下制备的标准气体)和固定标准体积法(在给定体积下进样多种不同浓度的标准品)。当进样体积为100微升时,还原态硫化合物的最佳检测限值范围为2.37皮克(二硫化碳)至4.89皮克(二甲基硫醚)。尽管这些检测限值随着进样体积的减小而逐渐改善,但由于样品体积减小带来的平衡作用,最低可检测浓度(例如,以纳摩尔每摩尔为单位)保持不变。脉冲火焰光度检测器的线性特性似乎也会随着其灵敏度的变化而动态变化。根据本研究,当通过直接进样法进行测试时,脉冲火焰光度检测器的性能对于精确描述高于约20纳摩尔每摩尔的还原态硫化合物的行为具有高度可靠性。