气相色谱法测定环境水体中总石油烃
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摘要
用气相色谱法测定环境水体中挥发性石油烃(VPHC)时,采集水样40mL,调节其酸度至pH<2.0,冷却至4℃后直接上机,用吹扫捕集进样。测定可萃取石油烃(EPHC),则采集水样后取500mL,用二氯甲烷萃取2次,每次用二氯甲烷15mL。合并萃取液,吹氮浓缩至1.0mL以下,用二氯甲烷定容至1.0mL,上机分析。以上两项分析均采用DB-5毛细管色谱柱分离和以火焰离子检测器(FID)测定。在上述两项测定中分别用石油标准溶液和柴油标准品制备标准溶液。测定VPHC时以保留时间在3.439~15.418min之间的C_6H_(14)至C_(10)H_(22)所有色谱峰总面积为纵坐标,以质量浓度为横坐标绘制标准曲线。测定EPHC,则以保留时间在9.027~40.479min之间的C_(10)H_(28)至C_(28)H_(58)所有色谱峰总面积对其相对质量浓度绘制标准曲线。测得的线性范围为:VPHC 0.018~0.25mg·L~(-1)和0.13~2.5mg·L~(-1);EPHC 23.7~474mg·L~(-1),两者的检出限依次为0.003,0.024 mg·L~(-1)。精密度与加标回收试验结果为:相对标准偏差(n=6)均不大于10%,回收率在89.0%~103%之间。
For GC-determination of volatile petroleum hydrocarbons(VPHC)in environmental water,40 mL of the water sample,after adjusting its acidity to pH<2.0 and cooling to 4 ℃,was used directly for GC analysis,and the purging and trapping technique for sample introduction was adopted.In the GC-determination of extractable petroleum hydrocarbons(EPHC),500 mL of the water sample,was extracted twice with 15 mL of CH_2 Cl2 in each extraction.The extracts were combined and evaporated to less than 1.0 mL by N2-blowing.CH_2 Cl2 was added to make its volume to 1.0 mL and it was used for GC-analysis.DB-5 capillary chromatographic column was used for GC-separation of both the VPHC and EPHC,and the FID was used for determination in both cases.The gasoline standard solution and diesel standard sample were used as primary standards in the above 2 analytical items respectively.In preparation of standard curves,values of total peak areas of the chromatographic peaks of compounds of C_6H_(14) to C_(10)H_(22) appeared in the retention time interval of 3.439 to 15.418 min(for VPHC),and of the chromatographic peaks of compounds of C_(10)H_(28) to C_(28)H_(58) appeared in the retention time interval of 9.027 to 40.479 min(for EPHC)were taken as the ordinate and values of their mass concentrations were taken as the abscissa.The linearity ranges found were between 0.018 to 0.25 mg·L~(-1) and 0.13 to 2.5 mg·L~(-1) for VPHC and between 23.7 to 474 mg·L~(-1) for EPHC,with detection limits of 0.003 mg·L~(-1) and 0.024 mg·L~(-1) for the 2 items respectively.Tests for precision and recovery by standard addition method were performed,giving results of RSDs(n=6)all≤10%,and recovery in the range of 89.0% to 103%.
For GC-determination of volatile petroleum hydrocarbons(VPHC)in environmental water,40 mL of the water sample,after adjusting its acidity to pH<2.0 and cooling to 4 ℃,was used directly for GC analysis,and the purging and trapping technique for sample introduction was adopted.In the GC-determination of extractable petroleum hydrocarbons(EPHC),500 mL of the water sample,was extracted twice with 15 mL of CH_2 Cl2 in each extraction.The extracts were combined and evaporated to less than 1.0 mL by N2-blowing.CH_2 Cl2 was added to make its volume to 1.0 mL and it was used for GC-analysis.DB-5 capillary chromatographic column was used for GC-separation of both the VPHC and EPHC,and the FID was used for determination in both cases.The gasoline standard solution and diesel standard sample were used as primary standards in the above 2 analytical items respectively.In preparation of standard curves,values of total peak areas of the chromatographic peaks of compounds of C_6H_(14) to C_(10)H_(22) appeared in the retention time interval of 3.439 to 15.418 min(for VPHC),and of the chromatographic peaks of compounds of C_(10)H_(28) to C_(28)H_(58) appeared in the retention time interval of 9.027 to 40.479 min(for EPHC)were taken as the ordinate and values of their mass concentrations were taken as the abscissa.The linearity ranges found were between 0.018 to 0.25 mg·L~(-1) and 0.13 to 2.5 mg·L~(-1) for VPHC and between 23.7 to 474 mg·L~(-1) for EPHC,with detection limits of 0.003 mg·L~(-1) and 0.024 mg·L~(-1) for the 2 items respectively.Tests for precision and recovery by standard addition method were performed,giving results of RSDs(n=6)all≤10%,and recovery in the range of 89.0% to 103%.
引文
[1]李国刚,付强,吕怡兵.突发性环境污染事故应急监测案例[M].北京:中国环境科学出版社,2010.
[2]张厚福.石油地质学[M].北京:石油工业出版社,1999.
[3]曹云者,施烈焰,李丽和,等.石油烃污染场地环境风险评价与风险管理[J].生态毒理学报,2007,2(3):265-272.
[4]TANG S L,ZHANG Y,ZHONG S,et al.A novel infrared specrophotometric method for the rapid determination of petroleum hydrocarbons,and animal and vegetable oils in water[J].Chinese Chemical Letters,2012,23(1):109-112.
[5]王永刚,倪宁峰.红外光谱法测定废水中石油类[J].理化检验-化学分册,2005,41(5):347-348.
[6]VERSHININ V I,PETROV S V.The estimation of total petroleum hydrocarbons content in waste water by IR spectrometry with multivariate calibrations[J].Talanta,2015,148(1/3):163-169.
[7]FARMAKI E,KALOUDIS T,DIMITROU K,et al.Validation of a FT-IR method for the determination of oils and grease in water using tetrachloroethylene as the extraction solvent[J].Desalination,2007,210(1/3):52-60.
[8]WANG S J,GUO G L,YAN Z G,et al.The development of a method for the qualitative and quantitative determination of petroleum hydrocarbon components using thin-layer chromatography with flame ionization detection[J].Journal of Chromatography A,2010,1217(3):368-374.
[9]SAARI E,PERAMAKI P,JALONEN J.Evaluating the impact of GC operating settings on GC-FID performance for total petroleum hydrocarbon(TPH)determination[J].Microchemical Journal,2010,94(1):73-78.
[10]张欢燕,王臻,周守毅.环境中总石油烃的气相色谱分析测定[J].环境监控与预警,2013,5(2):24-27.
[11]周艳红,李凌波.废水中萃取性石油烃的测定[J].石油炼制与化工,2013,5(2):24-27.
[12]高翔,肖寒,魏新明,等.气相色谱法测定作业场所空气中的溶剂汽油[J].理化检验-化学分册,2016,52(4):469-471.
[13]HJ 637-2012水质石油类和动植物油的测定红外光谱法[S].
[14]EPA Method 418.1-1978 Determination of petroleum hydrocarbons by spectrophotometric infrared[S].
[15]ASTM Method D 3921-96-2003 Standard test method for oil and grease and petroleum hydrocarbons in water[S].
[16]APHA Method 5520C-2000 Standard methods for the examination of water and wastewater[S].
[17]EPA Method 8015D-2003 Nonhalogenated organics using GC/FID[S].
[18]ISO 9377-2-2000 Water quality-determination of hydrocarbon oil index-method using solvent extraction and gas chromatography[S].
[19]LESAGE S,HAO X,KENT S N.Distinguishing natural hydrocarbons from anthropogenic contamination in groundwater[J].Ground Water,2010,35(1):149-160.
[20]李发生.石油烃污染场地土壤指导限值构建方法[M].北京:科学出版社,2014.
[21]GB 31570-2015石油炼制工业污染物排放标准[S].
[22]GB 31571-2015石油化学工业污染物排放标准[S].
[23]GB 3838-2002地表水环境质量标准[S].
[2]张厚福.石油地质学[M].北京:石油工业出版社,1999.
[3]曹云者,施烈焰,李丽和,等.石油烃污染场地环境风险评价与风险管理[J].生态毒理学报,2007,2(3):265-272.
[4]TANG S L,ZHANG Y,ZHONG S,et al.A novel infrared specrophotometric method for the rapid determination of petroleum hydrocarbons,and animal and vegetable oils in water[J].Chinese Chemical Letters,2012,23(1):109-112.
[5]王永刚,倪宁峰.红外光谱法测定废水中石油类[J].理化检验-化学分册,2005,41(5):347-348.
[6]VERSHININ V I,PETROV S V.The estimation of total petroleum hydrocarbons content in waste water by IR spectrometry with multivariate calibrations[J].Talanta,2015,148(1/3):163-169.
[7]FARMAKI E,KALOUDIS T,DIMITROU K,et al.Validation of a FT-IR method for the determination of oils and grease in water using tetrachloroethylene as the extraction solvent[J].Desalination,2007,210(1/3):52-60.
[8]WANG S J,GUO G L,YAN Z G,et al.The development of a method for the qualitative and quantitative determination of petroleum hydrocarbon components using thin-layer chromatography with flame ionization detection[J].Journal of Chromatography A,2010,1217(3):368-374.
[9]SAARI E,PERAMAKI P,JALONEN J.Evaluating the impact of GC operating settings on GC-FID performance for total petroleum hydrocarbon(TPH)determination[J].Microchemical Journal,2010,94(1):73-78.
[10]张欢燕,王臻,周守毅.环境中总石油烃的气相色谱分析测定[J].环境监控与预警,2013,5(2):24-27.
[11]周艳红,李凌波.废水中萃取性石油烃的测定[J].石油炼制与化工,2013,5(2):24-27.
[12]高翔,肖寒,魏新明,等.气相色谱法测定作业场所空气中的溶剂汽油[J].理化检验-化学分册,2016,52(4):469-471.
[13]HJ 637-2012水质石油类和动植物油的测定红外光谱法[S].
[14]EPA Method 418.1-1978 Determination of petroleum hydrocarbons by spectrophotometric infrared[S].
[15]ASTM Method D 3921-96-2003 Standard test method for oil and grease and petroleum hydrocarbons in water[S].
[16]APHA Method 5520C-2000 Standard methods for the examination of water and wastewater[S].
[17]EPA Method 8015D-2003 Nonhalogenated organics using GC/FID[S].
[18]ISO 9377-2-2000 Water quality-determination of hydrocarbon oil index-method using solvent extraction and gas chromatography[S].
[19]LESAGE S,HAO X,KENT S N.Distinguishing natural hydrocarbons from anthropogenic contamination in groundwater[J].Ground Water,2010,35(1):149-160.
[20]李发生.石油烃污染场地土壤指导限值构建方法[M].北京:科学出版社,2014.
[21]GB 31570-2015石油炼制工业污染物排放标准[S].
[22]GB 31571-2015石油化学工业污染物排放标准[S].
[23]GB 3838-2002地表水环境质量标准[S].
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