气相色谱-质谱联用法测定PAE湿强剂中氯丙醇残留量  

Determination of 1,3-Dichloro-2-propanol and 3-Chloro-1,2-propanediol Glycol in PAE by Gas Chromatography-mass Spectrometry

作　　者：杜显生 贾春红 郭欣 DU Xian-sheng;JIA Chun-hong;GUO Xin(Mudanjiang Hengfeng Paper Co.,Ltd.,Mudanjiang 157013,China)

机构地区：[1]牡丹江恒丰纸业股份有限公司,黑龙江牡丹江157013

出　　处：《造纸化学品》2021年第4期12-16,共5页Paper Chemicals

摘　　要：建立了以气相色谱-质谱联用法对聚酰胺环氧氯丙烷(PAE)湿强剂中1,3-二氯-2-丙醇和3-氯-1,2-丙二醇残留量的测定方法。采用乙醚对PAE湿强剂中氯丙醇进行振荡溶解,并以一定比例的稀释后,经七氟丁酰基咪唑常温衍生化,加入饱和氯化钠溶液盐析除杂,再通过气相色谱-质谱联用仪选择离子扫描分析,内标法定量。结果表明:1,3-二氯-2-丙醇和3-氯-1,2-丙二醇标准溶液质量浓度为0~400μg/L范围内线性关系较好,线性系数R 2分别为0.9994和0.9996;方法的加标回收率分别为92.7%和104.0%;精密度偏差分别为2.9%和2.4%。该方法具有操作简单、定量准确等优点,可完全满足PAE湿强剂中1,3-二氯-2-丙醇和3-氯-1,2-丙二醇残留量的测试要求。A method was developed for the determination of 1,3-dichloro-2-propanol and 3-chloro-1,2-propanediol residues in wet strength agent PAE by gas chromatography-mass spectrometry.The chloropropanol in the wet strength agent was dissolved by ethyl ether,diluted in a certain proportion,derivatized by heptafluorobutyryl imidazole at room temperature.And then the saturated sodium chloride solution was added to salt out and remove the impurities.Finally,ion scanning analysis was selected by gas chromatography-mass spectrometry(GC-MS),and internal standard method was used for quantitative analysis.The results showed that the linear relationships of 1,3-dichloro-2-propanol and 3-chloro-1,2-propanediol standard solutions were good within the concentration range of 0~400μg/L,the R 2 were 0.9994 and 0.9996 respectively;and the recoveries of the method were 92.7%and 104.0%,respectively;the precision deviations were 2.9%and 2.4%,respectively.The method has the advantages of simple operation and accurate quantification,and can completely meet the requirements for the determination of 1,3-dichloro-2-propanol and 3-chloro-1,2-propanediol residues in PAE wet strength agent.

关 键 词：聚酰胺环氧氯丙烷 湿强剂 气相色谱-质谱联用法 1 3-二氯-2-丙醇 3-氯-1 2-丙二醇 

分 类 号：O657[理学—分析化学]