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顶空气相色谱法测定棉毛纺织品中氯化溶剂残留量

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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.
Determination of residual chlorinated solvents in cotton and wool textiles by headspace gas chromatography
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 ra-tional 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 concen-tration of 1.0 mg/kg were added to the matrix blank sample for testing;the standard addition recovery rate of nine kinds of chlori-nated 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.

cotton and wool textileschlorinated solventresidual contentheadspace gas chromatography

田姝、赵金晶、李海、任一佳、徐建云

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江苏省纺织产品质量监督检验研究院,江苏 南京 210007

棉毛纺织品 氯化溶剂 残留量 顶空气相色谱法

江苏省市场监督管理局科技项目江苏省市场监督管理局科技项目

KJ2022017KJ2023022

2024

合成纤维工业
中国石化集团巴陵石油化工有限责任公司 中国石化集团公司合成纤维科技情报中心站

合成纤维工业

CSTPCD
影响因子:0.417
ISSN:1001-0041
年,卷(期):2024.47(3)