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首页> 外文期刊>Analytical methods >Fast chemical fingerprinting analysis for biodiesel/ diesel blends using commercial solid phase extraction (SPE) cartridge and gas chromatography-mass spectrometry (GC-MS)
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Fast chemical fingerprinting analysis for biodiesel/ diesel blends using commercial solid phase extraction (SPE) cartridge and gas chromatography-mass spectrometry (GC-MS)

机译:使用商业固相萃取(SPE)柱和气相色谱-质谱(GC-MS)对生物柴油/柴油混合物进行快速化学指纹分析

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摘要

Commercially available solid phase extraction (SPE) cartridges were combined with GC-MS forfast cleanup and fractionation of biodiesel/diesel samples in oil fingerprinting analysis. Several commercially available SPE cartridges (e.g., silica gel/cyanopropyl (SiO2/C3-CN) and extractable petroleum hydrocarbons (EPH) fractionation cartridges), were employed for the fractionation of biodiesel/diesel blends into aliphatic, aromatic hydrocarbons, and fatty acid methyl esters (FAMEs). The SiO2/C3-CN (1 g/0.5 g) SPE cartridge could not separate biodiesel from petroleum hydrocarbons effectively, however, the 5 g EPH SPE cartridge successfully separated blended samples into aliphatic, aromatic and FAME fractions by eluting with 15 mL of hexane, 15 mL of dichloromethylene (DCM)/hexane (1:1, v/v), and 18 mL of DCM, respectively. No cross-elution was observed among aliphatic, aromatic and FAME fractions when the loading mass of blends was less than 8 mg. The relative standard deviations (RSD) for five replicate SPE-GC-MS analyses of 5 mg of diesel blended with 20% biodiesel (volume/volume) and soybean oil ranged from 3.4% to 33.2%, 4.3% to 18.7% and 5.4% to 29.2% for selected alkane, polycydic aromatic hydrocarbons (PAHs) and FAMEs, respectively. The final recovery rates of surrogates for aliphatic, aromatic and FAME fractions ranged from 82.5 to 91.1%. This developed method was successfully used for the fingerprinting analysis of three simulated blend samples. The concentration profiles of target compounds and the blended level are both comparable to those obtained by the conventional silica gel column-GC-MS method.
机译:将市售的固相萃取(SPE)柱与GC-MS结合使用,可以在油指纹分析中快速净化和分离生物柴油/柴油样品。使用了几种市售的SPE柱(例如硅胶/氰基丙基(SiO2 / C3-CN)和可萃取石油烃(EPH)分馏柱),将生物柴油/柴油混合物分馏成脂肪族,芳族烃和脂肪酸甲基酯(FAME)。 SiO2 / C3-CN(1 g / 0.5 g)SPE柱无法有效地从石油烃中分离出生物柴油,但是5 g EPH SPE柱通过用15 mL己烷洗脱成功地将混合样品分离为脂肪族,芳族和FAME馏分分别为15毫升的二氯亚甲基(DCM)/己烷(1:1,v / v)和18毫升的DCM。当共混物的负载质量小于8mg时,在脂族,芳族和FAME级分之间没有观察到交叉洗脱。对5 mg柴油与20%生物柴油(体积/体积)和豆油混合进行的五次重复SPE-GC-MS分析的相对标准偏差(RSD)为3.4%至33.2%,4.3%至18.7%和5.4%对于选定的烷烃,多环芳烃(PAH)和FAME,分别降低到29.2%。脂族,芳族和FAME馏分的代用品的最终回收率在82.5%至91.1%之间。该开发的方法已成功用于三种模拟混合物样品的指纹分析。目标化合物的浓度曲线和混合水平均与常规硅胶柱-GC-MS方法获得的浓度曲线相当。

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