| 高温燃烧－水蒸气吸收－离子色谱法测定纺织品中的有机卤化物 |
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| 基金项目:海关总署科研项目（2019HK079）；海关技术规范制订项目（2020B221） |
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| 中文摘要:建立了高温燃烧－水蒸气吸收－离子色谱同时测定纺织品中有机氟、有机氯、有机溴和有机碘的分析方法。首先采用振荡方式去除纺织品中的无机卤化物得到试样，之后通过设计一种新型的高温燃烧吸收装置，采用程序升温方式对试样进行高温氧化燃烧、裂解及气化，产生的游离态卤素和卤化氢等气体被水蒸气吸收并完全转化为无机卤素阴离子，冷凝收集后用离子色谱分离测定，外标法定量。实验优化了称样量、燃烧方式、燃烧气及其流速、水蒸发量以及冷凝液收集方式等前处理条件，并对离子色谱分析条件进行优化。结果表明，氟、氯、溴、碘离子在0.02～10 mg/L范围内呈线性关系，相关系数（r2）均大于0.999；方法定量下限分别为：有机氟、有机氯1.0 mg/kg，有机溴2.5 mg/kg，有机碘5.0 mg/kg。以棉和涤纶2种不同种类的阴性纺织样品作为基质，在5、50、200 mg/kg 3个加标水平下，测得有机卤化物在棉和涤纶中的平均回收率分别为86.6%～100%和85.4%～99.6%，相对标准偏差（RSD，n = 7）分别为2.3%～5.6%和1.9%～5.7%，表明方法具有良好的准确度和精密度。将该方法应用于实际纺织样品的测定，检出了不同含量的有机氟、有机氯和有机溴化合物。该方法克服了传统燃烧法存在的燃烧和吸收不完全、回收率低的问题，准确度和灵敏度高、重复性好，适用于纺织品中有机卤化物的检测，为我国纺织品中有机卤化物检测标准的制订和质量安全监控提供了参考。 |
| 中文关键词:有机卤化物 离子色谱 纺织品 高温燃烧 水蒸气吸收 |
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| Determination of Organic Halides in Textiles by Ion Chromatography Method with High Temperature Combustion and Water Vapor Absorption |
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| Abstract:A new method was developed for the simultaneous determination of organic fluorine，organic chlorine，organic bromine and organic iodine compounds in textiles by ion chromatography with high temperature combustion and water vapor absorption．The samples were firstly oscillated to remove the inorganic halides in textiles，then burned，cracked and gasified with a new type of high temperature combustion absorption device in temperature programmed heating mode．The produced free halogen and hydrogen halide gases were absorbed with water vapor，and completely transformed into inorganic halogen anions．After condensation and collection，they were separated and determined by ion chromatography and quantified by external standard method．In the experiment，the pre-treatment conditions were optimized，including the sample weight，the combustion method，the combustion gas and its flow rate，the water evaporation and the condensate collection method．In addition，the analytical conditions for ion chromatography such as column，column temperature and the flow rate of eluent were also optimized．The results showed that the method was linear in the concentration range of 0.02－10 mg/L for the standard solutions of fluorine，chlorine，bromine and iodine ions，and the correlation coefficients（r2） were greater than 0.999．The limits of quantitation were both 1.0 mg/kg for organic fluorine and organic chlorine，2.5 mg/kg for organic bromine and 5.0 mg/kg for organic iodine．The negative textile samples of cotton and polyester were used as the sample matrixes，and typical organic halides were selected for the standard addition and recovery．The average recoveries for organic halides in cotton and polyester at spiked levels of 5，50，200 mg/kg were in the ranges of 86.6%－100% and 85.4%－99.6%，with their relative standard deviations（RSD，n = 7） of 2.3%－5.6% and 1.9%－5.7%，respectively，indicating that the method had good recovery and precision．This method was used in the determination of different contents of organic fluorine，organic chlorine and organic bromine in actual textile samples with good repeatability．The established method overcomes the problems of incomplete combustion and absorption，and low recovery existing in conventional combustion methods．With the advantages of high accuracy，sensitivity and good repeatability，the method is suitable for the determination of organic halides in textiles，and provides a reference for the establishment of standard and the quality and safety control of textiles in China． |
| Key Words:organic halides ion chromatography textiles high temperature combustion water vapor absorption |
| 引用本文：曹丽华,丁友超,张秀,顾从英,周佳,钱凯,汤娟.高温燃烧－水蒸气吸收－离子色谱法测定纺织品中的有机卤化物[J].分析测试学报,2022,41(2):234-241. |
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