气相色谱法同时测定日化工业废水中16种防腐剂  

Simultaneous determination of 16 kinds of preservatives in waste water from daily chemical industry by gas chromatography

作　　者：李健华 黄锦波 LI Jianhua;HUANG Jinbo(Jiangmen Ecological Environment Monitoring Station,Guangdong Province,Jiangmen 529000,China;Jims(Guangzhou)Experimental Technology Co.,Ltd.,Guangzhou 510000,China)

机构地区：[1]广东省江门生态环境监测站,广东江门529000 [2]吉姆斯(广州)实验技术有限公司,广州510000

出　　处：《化学分析计量》2023年第6期74-79,共6页Chemical Analysis And Meterage

摘　　要：建立气相色谱法同时测定日化工业废水中16种防腐剂的含量。样品用甲醇溶解后,经0.22μm有机滤膜过滤,以DB-5毛细管柱(30 m×0.25 mm,0.25μm)为分离柱,柱温箱初始温度为110℃,载气流量为0.7 mL/min,采用氢火焰离子化检测器检测,利用色谱峰面积外标法定量。2-甲基-4-异噻唑啉-3-酮、苯氧乙醇、2,4-二氯苄醇、辛基异羟肟酸、对羟基苯乙酮、对羟基苯甲酸甲酯、乙基己基甘油、4-丁基间苯二酚、吡罗克酮乙醇胺盐的质量浓度在5~100μg/mL范围内,2.6-二叔丁基对甲酚、氯苯甘醚、苯乙基间苯二酚的质量浓度在1~100μg/mL范围内,对羟基苯甲酸正丙酯的质量浓度在2.0~100μg/mL范围内,3-碘-2-丙炔基-N-丁基氨基甲酸酯甲酸酯的质量浓度在10.0~100μg/mL范围内,单辛酸甘油酯、单癸酸甘油酯的质量浓度在15~100μg/mL范围内,与色谱峰面积具有良好的线性关系,相关系数均不小于0.998,检出限为1.12~15.12μg/mL。样品加标回收率为87.0%~109.6%,测定结果的相对标准偏差为0.3%~5.6%(n=6)。该方法操作简单,可用于测定日化行业废水中16种防腐剂。A gas chromatography method was established to simultaneously determine the contents of 16 kinds of preservatives in waste water from the daily chemical industry.After being dissolved in methanol,the sample was filtered through a 0.22μm organic filter membrane.A DB-5 capillary column(30 m×0.25 mm,0.25μm)was used as the separation column.The initial temperature of the column oven was 110℃and the flow rate of carrier gas was 0.7 mL/min.Hydrogen flame ionization detector was used for detection,and chromatography peak area external standard method was used for quantification.The chromatography peak area had a good linear relationship with the mass concentration of 2-Methyl-4-isothiazolin-3-one,phenoxyethanol,2,4-dichlorobenzyl alcohol,octyl hydroxamic acid,p-hydroelectrically,methylparaben,ethyl Hexylglycerol,4-butyl resorcinol,piroctone ethanolamine salt in the range of 5-100μg/mL,with which of 2.6-di-tert-butyl-p-cresol,chlorophyll,phenethyl resorcinol in the range of 1-100μg/mL,with which of n-propylparaben in the range of 2.0-100μg/mL,with which of 3-iodo-2-propynyl-N-butylcarbamate formate in the range of 10.0-100μg/mL,with which of monotonically acid glycerine and monochromatic acid glycerine in the range of 15-100μg/mL,the correlation coefficients were all not less than 0.998,and the detection limit was 1.12-15.12μg/mL.The spiked recoveries of the samples were 87.0%-109.6%,and the relative standard deviations of the determination results were 0.3%-5.6%(n=6).The method is simple to operate,which can be used for the determination of 16 kinds of preservatives in wastewater from the daily chemical industry.

关 键 词：气相色谱法 日化工业废水 防腐剂 

分 类 号：O657.7[理学—分析化学]