氧弹燃烧-离子色谱法测定药用卤化丁基橡胶塞中的卤素含量
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摘要
目的:建立氧弹燃烧-离子色谱法测定药用卤化丁基橡胶塞中的氯、溴含量。方法:采用离子色谱Ion Pac AS11分析柱(4 mm×250 mm),Ion Pac AG11保护柱(4 mm×50 mm),以30 mmol·L~(-1)氢氧化钾溶液为淋洗液,流速1 mL·min~(-1),柱温30℃,电导检测器检测。结果:被测物氯离子和溴离子能得到很好的分离,空白对照无干扰,氯离子和溴离子质量浓度分别在0.05～20.0 mg·L~(-1)(r=0.999 3)和0.2～32.0 mg·L~(-1)(r=0.998 9)范围内与峰面积呈良好的线性关系,平均回收率(n=6)分别为105.2%和103.7%,检测下限分别为0.01和0.03 mg·L~(-1)。3批氯化丁基橡胶塞中氯离子含量为0.39%～0.54%,3批溴化丁基橡胶塞中溴离子含量为0.57%～0.75%。结论:该方法可应用于药用卤化丁基橡胶塞中氯和溴的含量测定。
Objective:To establish a method of oxygen bomb-ion chromatography for determination of chloride and bromide contents in halogenated butyl rubber stoppers. Methods:An ion chromatography method was developed,and an IonPacAS11 anion chromatography column(4.0 mm×250 mm)with an AG~(-1)1 guard column(4.0 mm×50 mm)was adopted,with the eluent of 30 mmol·L~(-1) potassium hydroxide solution. The flow rate was 1 mL· min~(-1) and the detector was conductivity detector. Results:Chloride ion and bromide ion were well separated. The calibration curves of chloride and bromide showed good linear relationships in the ranges of 0.05-20.0 mg·L~(-1)(r=0.999 3)and 0.2-32.0 mg·L~(-1)(r=0.998 9);the average recoveries(n=6)of chloride and bromide were 105.2% and 103.7%. The LODs of chloride and bromide were 0.01 mg·L~(-1) and 0.03 mg·L~(-1). The contents of chloride ion in three batches of chlorinated butyl rubber stoppers were 0.39%-0.54%. The contents of bromide ion in three batches of brominated butyl rubber stoppers were 0.57%-0.75%. Conclusion:The method can be used for the determination of chloride and bromide contents in halogenated butyl rubber stoppers.
Objective:To establish a method of oxygen bomb-ion chromatography for determination of chloride and bromide contents in halogenated butyl rubber stoppers. Methods:An ion chromatography method was developed,and an IonPacAS11 anion chromatography column(4.0 mm×250 mm)with an AG~(-1)1 guard column(4.0 mm×50 mm)was adopted,with the eluent of 30 mmol·L~(-1) potassium hydroxide solution. The flow rate was 1 mL· min~(-1) and the detector was conductivity detector. Results:Chloride ion and bromide ion were well separated. The calibration curves of chloride and bromide showed good linear relationships in the ranges of 0.05-20.0 mg·L~(-1)(r=0.999 3)and 0.2-32.0 mg·L~(-1)(r=0.998 9);the average recoveries(n=6)of chloride and bromide were 105.2% and 103.7%. The LODs of chloride and bromide were 0.01 mg·L~(-1) and 0.03 mg·L~(-1). The contents of chloride ion in three batches of chlorinated butyl rubber stoppers were 0.39%-0.54%. The contents of bromide ion in three batches of brominated butyl rubber stoppers were 0.57%-0.75%. Conclusion:The method can be used for the determination of chloride and bromide contents in halogenated butyl rubber stoppers.
引文
[1]国家药包材标准[S].2015:227,230National Drug Packaging Standard[S].2015:227,230
[2]张文英.离子色谱测定氧弹燃烧吸收液中卤素离子[C]//第十二届全国离子色谱学术报告会论文集.厦门:中国仪器仪表学会分析仪器学会,2008ZHANG WY.Determination of chlorine and bromine by oxygen bomb-ion chromatography[C]//Proceedings of the Twelfth National Symposium on Ion Chromatography.Xiamen:Analytical Instrument Branch of China Instrument and Control Society,2008
[3]邓江华,昌慧娟,王进,等.氧弹燃烧-自动电位滴定法测定橡胶中卤素含量[J].弹性体,2010,20(5):70DENG JH,CHANG HJ,WANG J,et al.Determination of halogen in rubber by oxygen bomb-potentiometric titration[J].China Elastom,2014,61(3):184
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[5]GB/T 9872-1998氧瓶燃烧法测定橡胶和橡胶制品中溴和氯的含量[S].1998GB/T 9872-1998 Rubber and Rubber Products-Determination of Bromine and Chlorine Content-Oxygen Flask Combustion Technique[S].1998
[6]GB/T 3050-2000无机化工产品中氯化物含量测定的通用方法-电位滴定法[S].2000GB/T 3050-2000 Inorganic Chemical Products for Industrial Use-General Method for Determination of Chloride ContentPotentiometric Method[S].2000
[7]施秀杰,衷明华.氧瓶燃烧-离子色谱法测定固体样品中无机元素的样品处理方法[J].江西化工,2014(2):108SHI XJ,ZHONG MH.Sample pretreatment of inorganic elements in solid samples in oxygen bomb-ion chromatography[J].Jiangxi Chem Ind,2014(2):108
[8]范云场,朱岩.离子色谱分析中样品前处理技术[J].色谱,2007,25(5):633FAN YC,ZHU Y.Sample pretreatment in ion chromatography[J].J Chromatogr,2007,25(5):633
[9]任飞,邬蓓蕾,叶佳楣,等.氧弹燃烧-离子色谱法测定原油中氯和溴[J].理化检验(化学分册),2012,48(11):1350REN F,WU PL,YE JM,et al.Determination of chlorine and bromine in crude oil by oxygen bomb-ion chromatography[J].Phys Test Chem Anal Part B:Chem Anal,2012,48(11):1350
[10]陶振卫,张娇,姚文全,等.氧弹燃烧-ICP-OES测定塑料中的氯和溴[J].广州化工,2011,39(18):106TAO ZW,ZHANG J,YAO WQ,et al.Determination of chlorine and bromine in plastics by oxygen bomb-ICP-OES[J].Guangzhou Chem Ind,2011,39(18):106
[11]高振,丁利,刘大壮,等.改良氧瓶燃烧-离子色谱法测定氯化聚丙烯中的氯含量[J].化工时刊,2007,21(8):42GAO Z,DING L,LIU DZ,et al.Determination of chloride content in chlorinated polypropylene by improved oxygen flask combustion-ion chromatography[J].Chem Ind Times,2007,21(8):42
[12]邓江华,谭帅霞,昌慧娟,等.氧弹燃烧-离子色谱法测定橡胶中的氯、溴含量[J].橡胶工业,2012,59(7):437DENG JH,TAN SX,CHANG HJ,et al.Determination of chlorine and bromine in rubber by oxygen bomb-ion chromatography[J].Chin Rub Ind,2012,59(7):437
[13]邓江华,谭帅霞,昌慧娟,等.氧弹燃烧-离子色谱法测定天然橡胶中的氮含量[J].橡胶工业,201 4,61(3):184DENG JH,TAN SX,CHANG HJ,et al.Determination of chlorine and bromine in natural rubber by oxygen bomb-ion chromatography[J].Chin Rub Ind,2014,61(3):184
[14]曾凤娟,鲁万卿,魏金桥,等.溴化氯丁橡胶中溴含量的测定[J].广东化工,2015,42(20):130ZENG FJ,LU WQ,WEI JQ,et al.Determination of bromine content in the brominated chloroprene rubber[J].Guangdong Chem Ind,2015,42(20):130
[15]刘建权,赵峰华,刘璟,等.氧弹燃烧-离子色谱法测定煤中氯含量[J].分析化学,2009,37(8):1152LIU JQ,ZHAO FH,LIU J,et al.Determination of chlorine in coal by oxygen bomb-ion ch romatography[J].Chin J Anal Chem,2009,37(8):1152
[16]王培,王颖,贾丽,等.氧弹燃烧-离子色谱法测定涂料中氯和溴的含量[J].化学分析计量,2013,22(3):63WANG P,WANG Y,JIA L,et al.Determination of chlorine and bromine in pai nt by oxygen bomb-ion chromatography[J].Chem Anal Meter,2013,22(3):63(本文于2018年9月2日修改回)
[2]张文英.离子色谱测定氧弹燃烧吸收液中卤素离子[C]//第十二届全国离子色谱学术报告会论文集.厦门:中国仪器仪表学会分析仪器学会,2008ZHANG WY.Determination of chlorine and bromine by oxygen bomb-ion chromatography[C]//Proceedings of the Twelfth National Symposium on Ion Chromatography.Xiamen:Analytical Instrument Branch of China Instrument and Control Society,2008
[3]邓江华,昌慧娟,王进,等.氧弹燃烧-自动电位滴定法测定橡胶中卤素含量[J].弹性体,2010,20(5):70DENG JH,CHANG HJ,WANG J,et al.Determination of halogen in rubber by oxygen bomb-potentiometric titration[J].China Elastom,2014,61(3):184
[4]EN14582-2002废弃物特性描述-卤素和硫含量-密闭系统内氧气燃烧法和测定法[S].2002EN14582-2002 Characterization of Waste-Halogen and Sulfur Content-Oxygen Burning Method and Determination Method in Closed System[S].2002
[5]GB/T 9872-1998氧瓶燃烧法测定橡胶和橡胶制品中溴和氯的含量[S].1998GB/T 9872-1998 Rubber and Rubber Products-Determination of Bromine and Chlorine Content-Oxygen Flask Combustion Technique[S].1998
[6]GB/T 3050-2000无机化工产品中氯化物含量测定的通用方法-电位滴定法[S].2000GB/T 3050-2000 Inorganic Chemical Products for Industrial Use-General Method for Determination of Chloride ContentPotentiometric Method[S].2000
[7]施秀杰,衷明华.氧瓶燃烧-离子色谱法测定固体样品中无机元素的样品处理方法[J].江西化工,2014(2):108SHI XJ,ZHONG MH.Sample pretreatment of inorganic elements in solid samples in oxygen bomb-ion chromatography[J].Jiangxi Chem Ind,2014(2):108
[8]范云场,朱岩.离子色谱分析中样品前处理技术[J].色谱,2007,25(5):633FAN YC,ZHU Y.Sample pretreatment in ion chromatography[J].J Chromatogr,2007,25(5):633
[9]任飞,邬蓓蕾,叶佳楣,等.氧弹燃烧-离子色谱法测定原油中氯和溴[J].理化检验(化学分册),2012,48(11):1350REN F,WU PL,YE JM,et al.Determination of chlorine and bromine in crude oil by oxygen bomb-ion chromatography[J].Phys Test Chem Anal Part B:Chem Anal,2012,48(11):1350
[10]陶振卫,张娇,姚文全,等.氧弹燃烧-ICP-OES测定塑料中的氯和溴[J].广州化工,2011,39(18):106TAO ZW,ZHANG J,YAO WQ,et al.Determination of chlorine and bromine in plastics by oxygen bomb-ICP-OES[J].Guangzhou Chem Ind,2011,39(18):106
[11]高振,丁利,刘大壮,等.改良氧瓶燃烧-离子色谱法测定氯化聚丙烯中的氯含量[J].化工时刊,2007,21(8):42GAO Z,DING L,LIU DZ,et al.Determination of chloride content in chlorinated polypropylene by improved oxygen flask combustion-ion chromatography[J].Chem Ind Times,2007,21(8):42
[12]邓江华,谭帅霞,昌慧娟,等.氧弹燃烧-离子色谱法测定橡胶中的氯、溴含量[J].橡胶工业,2012,59(7):437DENG JH,TAN SX,CHANG HJ,et al.Determination of chlorine and bromine in rubber by oxygen bomb-ion chromatography[J].Chin Rub Ind,2012,59(7):437
[13]邓江华,谭帅霞,昌慧娟,等.氧弹燃烧-离子色谱法测定天然橡胶中的氮含量[J].橡胶工业,201 4,61(3):184DENG JH,TAN SX,CHANG HJ,et al.Determination of chlorine and bromine in natural rubber by oxygen bomb-ion chromatography[J].Chin Rub Ind,2014,61(3):184
[14]曾凤娟,鲁万卿,魏金桥,等.溴化氯丁橡胶中溴含量的测定[J].广东化工,2015,42(20):130ZENG FJ,LU WQ,WEI JQ,et al.Determination of bromine content in the brominated chloroprene rubber[J].Guangdong Chem Ind,2015,42(20):130
[15]刘建权,赵峰华,刘璟,等.氧弹燃烧-离子色谱法测定煤中氯含量[J].分析化学,2009,37(8):1152LIU JQ,ZHAO FH,LIU J,et al.Determination of chlorine in coal by oxygen bomb-ion ch romatography[J].Chin J Anal Chem,2009,37(8):1152
[16]王培,王颖,贾丽,等.氧弹燃烧-离子色谱法测定涂料中氯和溴的含量[J].化学分析计量,2013,22(3):63WANG P,WANG Y,JIA L,et al.Determination of chlorine and bromine in pai nt by oxygen bomb-ion chromatography[J].Chem Anal Meter,2013,22(3):63(本文于2018年9月2日修改回)