摘要
建立了同时测定染整助剂中18种氯代烃类有机溶剂的气相色谱-质谱(GC-MS)检测方法。加入适量氯化钠的染整助剂样品经正十四烷振荡提取后,以DB-624超高惰性毛细管柱(30 m×0.25 mm,1.4μm)为色谱柱进行分离分析,电子轰击(EI)离子源选择离子监测(SIM)模式进行质谱监测,外标法定量。结果显示,18种氯代烃类有机溶剂可在19 min内完成色谱分离分析,在0.2~100 mg/L质量浓度范围内线性关系良好,相关系数(r^2)均不低于0.999 2,检出限(LODs,S/N=3)和定量下限(LOQs,S/N=10)分别为0.033~0.063 mg/L和0.11~0.19 mg/L。在低、中、高3个加标浓度水平下,阴性样品荧光增白剂1#(液体)和柔软剂2#(固体)中18种氯代烃类有机溶剂的平均加标回收率分别为93.3%~104%和92.7%~104%,相对标准偏差(RSD,n=6)分别为3.5%~5.3%和3.2%~5.4%。对23种不同性能的染整助剂进行测定,在3种染整助剂中检出四氯乙烯。该方法灵敏度和准确度高,精密度好,适用于各种染整助剂中18种氯代烃类有机溶剂的测定,为染整助剂的质量监控提供了参考。
A method of gas chromatography-mass spectrometry(GC-MS) was developed for the simultaneous determination of 18 chlorinated hydrocarbon organic solvents in dyeing and finishing auxiliaries.The sample of dyeing and finishing auxiliaries with proper amount of sodium chloride was extracted by oscillation with n-tetradecane,then separated on a DB-624 IU column(30 m×0.25 mm,1.4 μm),and finally detected by GC-MS with EI source in SIM mode.External standard method was used for the quantitative determination.Results revealed that the 18 chlorinated hydrocarbon organic solvents could be separated within 19 min,and their calibration curves showed good linearity in the range of 0.2-100 mg/L with correlation coefficients(r^2) no less than 0.999 2.The limits of detection(LODs,S/N=3) and the limits of quantification(LOQs,S/N=10) were in the ranges of 0.033-0.063 mg/L and 0.11-0.19 mg/L,respectively.At three spiked levels of low,medium and high,the average recoveries for 18 analytes in fluorescent brightener 1#(liquid) and softener 2#(solid) were in the ranges of 93.3%-104% and 92.7%-104%,with their relative standard deviations(RSDs) of 3.5%-5.3% and 3.2%-5.4%(n=6),respectively.This method was applied in the determination of 23 dyeing and finishing auxiliaries with different properties,and tetrachloroethylene was detected in 3 dyeing and finishing auxiliaries.With the advantages of high sensitivity,good precision and accuracy,the method is suitable for the determination of chlorinated hydrocarbon organic solvents in all kinds of dyeing and finishing auxiliaries,and provides a good strategy for further quality control of dyeing and finishing auxiliaries.
作者
汤娟
周佳
钱凯
丁友超
TANG Juan;ZHOU Jia;QIAN Kai;DING You-chao(Nanjing Customs Industrial Products Testing Center,Nanjing 210001,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2020年第8期1023-1028,共6页
Journal of Instrumental Analysis
基金
国家重点研发计划项目(2018YFF0214803)
南京海关科研项目(2019KJ25)。
关键词
气相色谱-质谱
氯代烃类有机溶剂
染整助剂
gas chromatography-mass spectrometry(GC-MS)
chlorinated hydrocarbon organic solvents
dyeing and finishing auxiliaries
