Heshka Nicole E, Choy Joanne M, Chen Jinwen
Natural Resources Canada, CanmetENERGY, 1 Oil Patch Drive, Devon, Alberta, T9G 1A8, Canada.
Natural Resources Canada, CanmetENERGY, 1 Oil Patch Drive, Devon, Alberta, T9G 1A8, Canada.
J Chromatogr A. 2017 Dec 29;1530:241-246. doi: 10.1016/j.chroma.2017.11.007. Epub 2017 Nov 4.
A modification to American Society for Testing and Materials (ASTM) method D5623 is proposed to enable successful and repeatable analysis of heavy crude oil samples. A two-dimensional gas chromatography configuration was implemented, with separation of sulphur compounds occurring on two columns. A Deans switch is used to enable heart-cutting of volatile sulphur compounds onto a DB-Sulfur stationary phase, and separation occurs concurrently with the backflushing of the primary column. The use of a sulphur-selective detector increases selectivity, and 22 volatile sulphur species are quantified in less than 15min, which is almost half the time of the original ASTM method. Samples ranging from light distillation cuts to whole crudes (boiling from 100°C to >750°C) were analyzed with minimal sample preparation. The calculated limit of detection was 0.7mg/kg, repeatability was 3% relative standard deviation (RSD), and a linear range of 1-250mg/kg was obtained, with an R value of 0.994 or better, depending on the compound.
建议对美国材料与试验协会（ASTM）的D5623方法进行修改，以便能够成功且可重复地分析重质原油样品。采用了二维气相色谱配置，在两根柱上对含硫化合物进行分离。使用迪恩斯切换器将挥发性含硫化合物中心切割至DB - 硫固定相上，分离过程与主柱的反吹同时进行。使用硫选择性检测器提高了选择性，在不到15分钟的时间内对22种挥发性含硫物质进行了定量分析，这几乎是原始ASTM方法时间的一半。对从轻馏分切割到全原油（沸点从100°C到>750°C）的样品进行分析，样品制备最少。计算得出的检测限为0.7mg/kg，重复性为3%相对标准偏差（RSD），获得了1 - 250mg/kg的线性范围，R值为0.994或更高，具体取决于化合物。
