Applications of Accelerated Solvent Extraction in Preparation of Poly-nuclear Aromatic Hydrocarbons in Oil and Gas Geochemical Exploration Samples
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摘要: 油气化探样品测定芳烃物质的提取方法通常采用振荡提取，在实际的样品测试过程中，这种前处理方法效率较低，得到的提取液用于分析测定的结果重现性较差。本文对油气化探样品稠环芳烃的提取方法进行改进，采用加速溶剂萃取技术，对实际样品进行试验，考察了压力、静态萃取时间和萃取温度对稠环芳烃萃取效率的影响，确定最佳的萃取条件为：萃取压力8.3 MPa，静态时间5 min，萃取温度80 ℃。对比了加速溶剂萃取与传统振荡提取应用于油气化探样品前处理的提取效率，证实了加速溶剂萃取技术可以显著提高萃取效率，稠环芳烃的荧光强度提高60.5%~152.6%，方法的稳定性好，测定结果的精密度高，相对标准偏差(RSD, n=7)低于4%。加速溶剂萃取技术优于传统振荡法，更能满足油气化探样品分析测试的准确度与精密度要求，可以应用于油气化探样品前处理过程。Abstract: The method of oscillations-extraction was used to obtain target compounds for the analysis of geochemical exploration of oil and gas. The efficiency and precision of the results were unsatisfactory for practical samples when using this method. In order to improve the conventional method, accelerated solvent extraction technology was used to prepare poly-nuclear aromatic hydrocarbons samples. The experimental conditions (pressure, static extraction time and extraction temperature) are discussed and optimized with an extraction pressure of 8.3 MPa, extraction temperature of 80℃ and heating time of 5 min. Under the optimized experimental conditions, a comparison of the extraction efficiency of the accelerated solvent extraction with the conventional oscillation method was performed. The extraction efficiencies of 3 different samples were improved from 60.5% to 152.6%, and the satisfactory precision and stability were obtained with RSDs (n=7) of less than 4%. Accelerated Solvent Extraction technology is superior to traditional methods and gives more satisfactory results in accuracy and precision requirements. It can be applied to oil and gas geochemical exploration samples by pre-treatment processing.
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表 1 不同压力条件下测量的荧光强度
Table 1. The fluorescence intensity under different extraction pressure
压力
p/MPa320 nm 360 nm 405 nm 荧光强度平均值 RSD/% 荧光强度平均值 RSD/% 荧光强度平均值 RSD/% 6.9 375.93 3.39 208.74 6.34 47.01 7.61 8.3 382.39 0.84 203.17 1.38 50.46 2.21 10.3 381.92 1.65 205.67 1.01 53.72 3.36 
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表 2 不同静态时间条件下测量的荧光强度
Table 2. The fluorescence intensitiy under different static extraction time
静态时间
t/min320 nm 360 nm 405 nm 荧光强度平均值 RSD/% 荧光强度平均值 RSD/% 荧光强度平均值 RSD/% 3 369.65 3.06 193.06 2.76 47.68 5.31 5 381.28 1.25 204.20 1.02 52.91 4.04 7 380.16 1.41 207.59 1.45 54.66 1.88 10 384.66 0.92 208.98 1.21 60.46 2.70
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表 3 不同温度条件下测量的荧光强度
Table 3. The fluorescence intensity under different temperature
温度
θ/℃320 nm 360 nm 405 nm 荧光强度平均值 RSD/% 荧光强度平均值 RSD/% 荧光强度平均值 RSD/% 40 300.26 2.99 137.79 1.74 35.14 5.84 70 366.25 3.13 197.24 1.60 52.22 3.96 100 395.75 1.17 214.47 1.57 54.74 1.49
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表 4 振荡提取和ASE提取方法测量的荧光强度
Table 4. The fluorescence intensities under the oscillations-extraction and ASE
提取方法 发射波长
λ/nm样品1 样品2 样品3 荧光强度平均值 RSD/% 荧光强度平均值 RSD/% 荧光强度平均值 RSD/% 振荡提取 320 128.15 4.62 239.48 5.21 356.87 4.51 360 54.23 4.84 107.58 4.32 174.53 4.29 405 8.51 5.65 21.11 5.25 36.22 3.78 ASE提取 320 213.32 2.82 384.57 1.89 576.24 2.10 360 117.54 2.14 206.38 1.28 321.17 1.56 405 19.83 1.83 53.32 1.03 81.07 1.22
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