摘要
采用顶空自动进样器进样,利用DB-1色谱柱分离、电子捕获检测器检测,通过基质匹配校正法建立标准曲线,外标法定量,建立了一种基于静态顶空-气相色谱法(HS-GC)测定棉、毛纺织品中二氯甲烷等9种氯化溶剂残留量的方法,探讨了顶空进样的平衡温度、平衡时间对测试结果的影响,以及该方法的准确度、精密度和检出限。结果表明:顶空进样平衡温度为60℃、平衡时间为15 min较为合适;基质空白样中添加浓度为1.0 mg/kg的9种氯化溶剂标准混合溶液进行测试,9种氯化溶剂的检出限为0.002~0.190 mg/kg;在0.5~20.0 mg/kg的加标水平下进行测试,9种氯化溶剂的加标回收率为77.7%~114.1%,相对标准偏差为1.02%~8.76%;该方法准确性好,灵敏度高,适用于棉、毛纺织品中氯化溶剂的定性定量分析。
A method based on static headspace gas chromatography(HS-GC)was developed for the determination of nine kinds of residual chlorinated solvents such as dichloromethane in cotton and wool textiles by quantitative analysis of external standard method according to standard curves established by matrix matching correction method using headspace automatic sampler,DB-1 chromatographic column and electron capture detector.The influence of equilibrium temperature and time of headspace injection on test results,as well as the accuracy,precision and detection limit of this method,was explored.The results showed that a rational headspace injection equilibrium temperature and time was 60℃and 15 min,respectively;the detection limit of the nine chlorinated solvents was 0.002-0.190 mg/kg when nine kinds of standard mixed solutions of chlorinated solvents with a concentration of 1.0 mg/kg were added to the matrix blank sample for testing;the standard addition recovery rate of nine kinds of chlorinated solvents was 77.7%-114.1%and the relative standard deviation was 1.02%-8.76%when the standard addition level was 0.5-20.0 mg/kg;and this method is suitable for qualitative and quantitative analysis of chlorinated solvents in cotton and wool textiles due to its good accuracy and high sensitivity.
作者
田姝
赵金晶
李海
任一佳
徐建云
TIAN Shu;ZHAO Jinjing;LI Hai;REN Yijia;XU Jianyun(Jiangsu Textile Products Quality Supervision and Inspection Institute,Nanjing 210007)
出处
《合成纤维工业》
CAS
2024年第3期91-95,共5页
China Synthetic Fiber Industry
基金
江苏省市场监督管理局科技项目(KJ2022017、KJ2023022)。
关键词
棉毛纺织品
氯化溶剂
残留量
顶空气相色谱法
cotton and wool textiles
chlorinated solvent
residual content
headspace gas chromatography
