Department of Soil Pollution Control, Chinese Research Academy of Environmental Sciences, Beijing, 100012, China.
J Chromatogr A. 2010 Jan 15;1217(3):368-74. doi: 10.1016/j.chroma.2009.11.022. Epub 2009 Nov 14.
An analytical scheme to determine groups of petroleum hydrocarbon compounds in crude oil was developed and used for the qualitative and quantitative characterization of crude oil samples from the Shengli oilfield, the second largest oilfield in China. Crude oil samples were fractionated and analyzed by thin-layer chromatography with flame ionization detection (TLC-FID). Relative standard deviation (RSD) values for retention time, peak height and half peak width were less than 5.2% for all classes of compounds, based on nine independent replicates. The crude oil light fraction was further analyzed by GC-MS and the majority of identified compounds were methyl- or hydro-derivatives of long-chain hydrocarbons and aromatic compounds. The external standard method used in the present study can lower detection limits of petroleum hydrocarbon compound classes to 20.0 mg L(-1), and the crude oil concentration in the range of 30 and 35,000 mg L(-1) has a high linear correlation (r(2)>0.97, P<0.05) with peak area. A comparison between elution chromatography (EC) and TLC-FID regarding the recovery of petroleum hydrocarbon compounds was carried out with aged crude oil contaminated soils of 50, 80, 200 and 300 mg g(-1). The tested TLC-FID method showed a 10% higher recovery for total extractable materials than the reference EC method. The calibration factor was fraction-dependent and varied with the recovery rate of TLC/EC. Regarding the tested extraction procedures, accelerated solvent extraction (ASE) had a higher extraction efficiency for crude oil contaminated soils than Soxhlet and ultrasonic extractions.
建立了一种分析方案，用于确定原油中石油烃类化合物的组别，并用于定性和定量表征中国第二大油田——胜利油田的原油样品。采用薄层色谱-火焰离子化检测（TLC-FID）对原油样品进行分离和分析。基于 9 个独立重复实验，所有类别的化合物的保留时间、峰高和半峰宽的相对标准偏差（RSD）值均小于 5.2%。采用 GC-MS 对原油轻馏分进一步分析，鉴定出的大多数化合物为长链烃类和芳烃的甲基或氢衍生物。本研究中使用的外标法可将石油烃化合物类别的检测限降低至 20.0mg/L-1，且原油浓度在 30 至 35000mg/L-1 范围内与峰面积具有高度线性相关性（r²>0.97，P<0.05）。采用薄层色谱-火焰离子化检测（TLC-FID）和洗脱色谱（EC）对老化的 50、80、200 和 300mg/g-1 污染土壤中的石油烃化合物进行了回收率比较。与参考 EC 方法相比，经测试的 TLC-FID 方法对总可提取物质的回收率高出 10%。校准因子与馏分有关，且随 TLC/EC 的回收率而变化。就测试的提取程序而言，与索氏提取和超声提取相比，加速溶剂提取（ASE）对污染土壤中原油的提取效率更高。
