基于固相萃取联合顶空进样气相色谱技术的变压器油中甲醇含量检测研究
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摘要
近年来,变压器油中的甲醇含量已经成为一种新的变压器固体绝缘老化程度指标。本研究结合固相萃取和顶空进样的前处理技术,利用固相萃取对样品进行吸附浓缩,然后采用顶空进样技术解吸附并进样,再采用气相色谱对变压器油中微量甲醇进行测定。结果表明:当固相萃取的样品量为20 mL,顶空进样器的平衡温度为90℃,加热时间为25 min时测定效果最佳。绝缘油中甲醇浓度为0.98～18.62 mg/L时,甲醇的浓度与其色谱峰面积具有良好的线性关系,线性拟合优度为0.998 2,相对标准偏差(RSD)为5.51%,能够满足实际应用的要求。
In recent years, the methanol content in transformer oil has been a new ageing degree indicator of solid insulation in power transformer. The solid phase extraction and the pretreatment technology of headspace sampling were combined in this paper. The sample was adsorbed and concentrated using solid phase extraction, and then was desorbed and injected using headspace sampling technology. Finally,the trace amount of methanol in transformer insulating oil was measured by gas chromatography. The results show that when the sample amount of solid phase extraction is 20 mL, the equilibrium temperature of headspace sampler is 90 ℃, and the heating time is 25 min, the test effect is the best. When the methanol concentration in insulating oil is 0.98～18.62 mg/L, there is a good linear relation between the methanol concentration and the chromatographic peak area, the linear goodness of fit is 0.998 2, and the relative standard deviation(RSD) is 5.51%, which can meet the requirements of practical application.
In recent years, the methanol content in transformer oil has been a new ageing degree indicator of solid insulation in power transformer. The solid phase extraction and the pretreatment technology of headspace sampling were combined in this paper. The sample was adsorbed and concentrated using solid phase extraction, and then was desorbed and injected using headspace sampling technology. Finally,the trace amount of methanol in transformer insulating oil was measured by gas chromatography. The results show that when the sample amount of solid phase extraction is 20 mL, the equilibrium temperature of headspace sampler is 90 ℃, and the heating time is 25 min, the test effect is the best. When the methanol concentration in insulating oil is 0.98～18.62 mg/L, there is a good linear relation between the methanol concentration and the chromatographic peak area, the linear goodness of fit is 0.998 2, and the relative standard deviation(RSD) is 5.51%, which can meet the requirements of practical application.
引文
[1]张欲晓,李胜利,王梦君,等.变压器绝缘纸的聚合度变化规律[J].高电压技术,2011,37(10):2458-2463.
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[3]漆薇.变压器油中溶解糠醛拉曼光谱检测表面增强方法研究[D].重庆:重庆大学,2016.
[4]张欲晓,李胜利,喻培元,等.一种光谱法检测油中糠醛的初步研究[J].高压电器,2014,50(8):47-52.
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[9]王灵红,广家权,王少磊,等.品红亚硫酸法测定甲醇显色反应温度的确定[J].酿酒科技,2016(7):70-71.
[10]欧阳爱国,黄志鸿,刘燕德.近红外光谱法对甲醇柴油中甲醇含量测定[J].光谱学与光谱分析,2017,37(4):1118-1122.
[11]陈玉锋,庄志萍,魏林博,等.激光拉曼光谱内标法直接测定甲醇含量[J].理化检验-化学分册,2015,51(4):558-559.
[12]PONTES H,PINHO P G D,CASAL S,et al.GC determination of acetone,acetaldehyde,ethanol,and methanol in biological matrices and cell culture[J].Journal of Chromatographic Science,2009,47(4):272-278.
[13]吴锋,张欢,王永军,等.芝麻香型白酒甲醇含量的测定研究[J].酿酒,2014(6):55-57.
[14]田富饶,吴景武,刘冬,等.毛细管柱-顶空气相色谱法测定化妆品中的甲醇[J].光谱实验室,2013,30(6):3205-3208.
[15]李长秀,孔翠萍.顶空气相色谱法测定生物柴油中的微量甲醇[J].石油化工,2012,41(10):1196-1200.
[16]林海,李春雄,林静,等.顶空-气相色谱法测定B-100生物柴油中游离甲醇含量[J].分析测试技术与仪器,2015,21(3):153-157.
[17]崔诚,巩泽龙,张龙庄,等.顶空-气相色谱法测定甲醇柴油中甲醇的含量[J].石油化工,2016,45(11):1386-1389.
[18]P?OTKAWASYLKA J,MAR?M,SZCZEPA?SKA N,et al.New polymeric materials for solid phase extraction[J].Critical Reviews in Analytical Chemistry,2017,47(5):373-383.
[19]相雷雷,宋洋,卞永荣,等.土壤中10种多溴联苯醚的加速溶剂-固相萃取净化方法优化研究[J].分析化学,2016,44(5):671-677.
[20]刘玲玲,武彦文,李冰宁,等.固相萃取-大体积进样-气相色谱法定量分析油茶籽油中的矿物油[J].分析化学,2016,44(9):1419-1424.
[21]MOKHTARI B,POURABDOLLAH K.SPME-GC determination of methanol as a hydrate inhibitor in crude oil[J].Talanta,2011,87(1):118-125.
[22]何仲强,林晓佳,陈树东,等.固相萃取-同位素稀释-气相色谱-质谱法检测婴幼儿配方米粉中的五种甾醇[J].现代食品科技,2018(1):209-215.
[23]吴丽洒,赵明月,葛畅,等.固相萃取-GC/MS法同时测定卷烟主流烟气中的16种多环芳烃[J].烟草科技,2018,51(4):46-52.
[2]PRADHAN M K.Assessment of the status of insulation during thermal stress accelerated experiments on transformer prototypes[J].IEEE Transactions on Dielectrics and Electrical Insulation,2006,13(1):227-237.
[3]漆薇.变压器油中溶解糠醛拉曼光谱检测表面增强方法研究[D].重庆:重庆大学,2016.
[4]张欲晓,李胜利,喻培元,等.一种光谱法检测油中糠醛的初步研究[J].高压电器,2014,50(8):47-52.
[5]CHEIM L,PLATTS D,PREVOST T,et al.Furan analysis for liquid power transformers[J].IEEE Electrical Insulation Magazine,2012,28(2):8-21.
[6]JALBERT J,DUCHESNE S,RODRIGUEZCELIS E,et al.Robust and sensitive analysis of methanol and ethanol from cellulose degradation in mineral oils[J].Journal of Chromatography A,2012,1256(18):240-245.
[7]BURSOVáM,HLO?EK T,?ABALA R.Simultaneous determination of methanol,ethanol and formic acid in serum and urine by headspace GC-FID[J].Journal of Analytical Toxicology,2015,39(9):741-745.
[8]BRUZZONITI M C,MAINA R,CARLO R M D,et al.GC methods for the determination of methanol and ethanol in insulating mineral oils as markers of cellulose degradation in power transformers[J].Chromatographia,2014,77(15-16):1081-1089.
[9]王灵红,广家权,王少磊,等.品红亚硫酸法测定甲醇显色反应温度的确定[J].酿酒科技,2016(7):70-71.
[10]欧阳爱国,黄志鸿,刘燕德.近红外光谱法对甲醇柴油中甲醇含量测定[J].光谱学与光谱分析,2017,37(4):1118-1122.
[11]陈玉锋,庄志萍,魏林博,等.激光拉曼光谱内标法直接测定甲醇含量[J].理化检验-化学分册,2015,51(4):558-559.
[12]PONTES H,PINHO P G D,CASAL S,et al.GC determination of acetone,acetaldehyde,ethanol,and methanol in biological matrices and cell culture[J].Journal of Chromatographic Science,2009,47(4):272-278.
[13]吴锋,张欢,王永军,等.芝麻香型白酒甲醇含量的测定研究[J].酿酒,2014(6):55-57.
[14]田富饶,吴景武,刘冬,等.毛细管柱-顶空气相色谱法测定化妆品中的甲醇[J].光谱实验室,2013,30(6):3205-3208.
[15]李长秀,孔翠萍.顶空气相色谱法测定生物柴油中的微量甲醇[J].石油化工,2012,41(10):1196-1200.
[16]林海,李春雄,林静,等.顶空-气相色谱法测定B-100生物柴油中游离甲醇含量[J].分析测试技术与仪器,2015,21(3):153-157.
[17]崔诚,巩泽龙,张龙庄,等.顶空-气相色谱法测定甲醇柴油中甲醇的含量[J].石油化工,2016,45(11):1386-1389.
[18]P?OTKAWASYLKA J,MAR?M,SZCZEPA?SKA N,et al.New polymeric materials for solid phase extraction[J].Critical Reviews in Analytical Chemistry,2017,47(5):373-383.
[19]相雷雷,宋洋,卞永荣,等.土壤中10种多溴联苯醚的加速溶剂-固相萃取净化方法优化研究[J].分析化学,2016,44(5):671-677.
[20]刘玲玲,武彦文,李冰宁,等.固相萃取-大体积进样-气相色谱法定量分析油茶籽油中的矿物油[J].分析化学,2016,44(9):1419-1424.
[21]MOKHTARI B,POURABDOLLAH K.SPME-GC determination of methanol as a hydrate inhibitor in crude oil[J].Talanta,2011,87(1):118-125.
[22]何仲强,林晓佳,陈树东,等.固相萃取-同位素稀释-气相色谱-质谱法检测婴幼儿配方米粉中的五种甾醇[J].现代食品科技,2018(1):209-215.
[23]吴丽洒,赵明月,葛畅,等.固相萃取-GC/MS法同时测定卷烟主流烟气中的16种多环芳烃[J].烟草科技,2018,51(4):46-52.