ANALYSIS OF AROMATICS AND THEIR DERIVATIVES IN OIL-GAS GEOCHEMICAL SAMPLES BY ULTRAVIOLET SPECTROPHOTOMETRY
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摘要:
应用紫外分光光度法分析芳烃及芳烃衍生物，以苯、萘、菲3种物质作为代表性物质，选用正己烷为溶剂，在5个特征波长下测试物质的吸光强度.检出限为12.9×10-9~20.5×10-9，空白加标准确度为98.9%~101.4%，精密度为3.73%~4.51%，实际样品的加标回收分析基本满足要求.在分析测试方法上做了优化，对环境污染小，对人体毒害低，安全性高，既缩减了成本又提高了效率.该方法的准确度精密度高，简便易行，可满足地质行业分析测试的要求，适用于油气化探样品中芳烃类的大批量集中分析测试.
Abstract:The ultraviolet spectrophotometry is used to analyze aromatics and their derivatives. Taking benzene, naphthalene and phenanthrene as representative substances, n-hexane as solvent, the photon absorbing intensity of the substances is measured at 5 characteristic wavelengths. The results show the detection limit of 12.9×10-9-20.5×10-9, accuracy of standard-addition in blank 98.9%-101.4% and precision 3.73%-4.51%, and the standard recovery analysis of practical samples basically meets the requirements. The analysis testing method is optimized, with low pollution to environment, low toxicity to human body and high safety, which both reduces cost and improves efficiency. The method is simple and feasible, with high accuracy and precision, and can meet the requirements for analysis and testing of geological industry, suitable for mass analysis testing of aromatics in oil-gas geochemical samples.
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表 1 苯、萘、菲3种物质工作曲线的相关数据
Table 1. Relevant data of working curves for benzene, naphthalene and phenanthrene
序号 浓度/(μg/L) 吸光度值(A) 苯 萘 菲 209 nm 220 nm 260 nm 275 nm 296 nm 1 0 0 0 0 0 0 2 50 0.0029 0.0539 0.0018 0.0539 0.00175 3 100 0.0054 0.0897 0.0034 0.0897 0.0034 4 200 0.0112 0.1794 0.007 0.1794 0.007 5 500 0.0281 0.439 0.0175 0.439 0.0175 6 800 0.045 0.6674 0.0267 0.6674 0.0267 7 1000 0.0545 0.8412 0.0344 0.8412 0.0344 相关系数r2 0.9995 0.9994 0.9994 0.999 0.9995 线性方程 y=6×10-5x+0.0001 y=0.0008x+0.009 y=3×10-5x+7×10-5 y=7×10-5x+0.0006 y=1×10-5x+2×10-5 
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表 2 检出限分析
Table 2. Detection limit analysis
物质名称 波长/nm 加标浓度/(μg/L) 芳烃含量测定值/10-9 平均值/(μg/L) 标准偏差/(s) 在土壤中的检出限/10-9 1 2 3 4 5 6 7 苯 209 100 103.1 104.2 97.6 94.9 105.9 103.7 105.0 102.1 4.1 19.4 萘 220 100 102.8 99.6 101.3 103.5 103.8 98.4 96.2 100.8 2.9 13.4 260 100 105.4 96.5 102.8 105.8 103.5 99.1 97.5 101.5 3.8 17.8 菲 275 100 107.9 103.2 97.6 99.4 94.6 103.4 101.8 101.1 4.4 20.5 296 100 96.4 103.6 98.4 101.4 98.0 103.0 101.4 100.3 2.7 12.9
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表 3 准确度和精密度分析
Table 3. Accuracy and precision analysis
物质名称 波长/nm 加标浓度/(μg/L) 芳烃含量测定值/10-9 平均值/(μg/L) 回收率/% RSD/% 1 2 3 4 5 6 7 苯 209 500 526.7 496.0 534.7 516.0 475.3 482.7 491.3 503.2 100.6 4.5 萘 220 500 478.7 502.2 485.7 522.0 482.7 476.2 515.0 494.6 98.9 3.7 260 500 515.2 516.4 507.9 472.1 495.6 508.5 534.2 507.1 101.4 3.8 菲 275 500 493.0 515.0 465.0 525.0 508.0 495.0 481.0 497.4 99.5 4.1 296 500 519.0 525.0 531.0 488.0 491.0 512.0 483.0 507.0 101.4 3.8
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表 4 实际样品分析
Table 4. Analysis of practical samples
样品号 1号 2号 3号 波长/nm 209 220 260 275 296 209 220 260 275 296 209 220 260 275 296 原含量/10-9 222.0 4.5 8.0 12.9 22.5 540.0 64.5 213.0 57.9 450.0 1023 261.0 763.0 270.0 1665 加标浓度I/10-9 15 60 270 测定值/10-9 237.8 21.4 25.3 27.1 38.4 605.0 130.3 276.0 115.6 509.4 1281 514.3 1068 523.1 2000 回收量/10-9 15.8 16.9 17.3 14.2 15.9 65.0 65.8 63.0 57.7 59.4 257.6 253.3 305.3 253.1 335.1 回收率/% 105.3 112.7 115.3 95.0 106.0 108.3 109.7 105.0 96.2 99.0 95.4 93.8 113.1 93.7 124.1 加标浓度II/10-9 30 210 750 测定值/10-9 250.3 36.8 34.9 39.8 49.7 734.1 257.2 416.7 259.4 642.5 1681 966.1 1450 1103 2756 回收量/10-9 28.3 32.3 26.9 26.9 27.2 194.1 192.7 203.7 201.5 192.5 657.6 705.1 687 833.1 1091 回收率/% 94.3 107.7 89.7 89.8 90.7 92.4 91.8 97.0 96.0 91.7 87.7 94.0 91.6 111.1 145.5 加标浓度III/10-9 210 480 1200 测定值/10-9 456.2 224.8 206.5 240.3 256.4 1006 578.6 685.6 514.0 882.4 1897 1292 1652 1265 3654 回收量/10-9 234.2 220.3 198.5 227.4 233.9 465.6 514.1 472.6 456.1 432.4 873.5 1031 889.3 995.4 1989 回收率/% 111.5 104.9 94.5 108.3 111.4 97.0 107.1 98.5 95.0 90.1 72.8 85.9 74.1 83.0 165.8
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