CN109297923A - 纺织品中微量含氟整理剂的测定方法 - Google Patents
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Abstract
本发明公开了一种纺织品中微量含氟整理剂的测定方法，包括含氟织物整理剂的水解、全氟烷基类物质的初步定性、全氟烷基类物质的萃取、全氟烷基类物质的HPLC/MS/MS分析等步骤。本发明具有系统性、快速、安全高效。
Description
技术领域
本发明涉及一种纺织品中微量含氟整理剂的测定方法。
背景技术
化纤和纺织业在我国国民经济中一直占据着重要地位, 2015年中国化纤产量为4872万吨，同比增长12.5% ，占全球比重已超过60%，2015年，我国共进口化纤产品67.6万吨，化纤产品出口316.9万吨，棉纱、棉布、丝织品、化纤、服装的产量均居世界第一位。我国是纺织生产大国和出口大国，却非纺织强国，纺织品和服装产品的档次和质量不高，纺织品精加工技术落后。原因在于纺织品精加工技术需要高档纺织助剂和织物整理剂。
织物整理剂的整理目的是达到防油防水的效果。含氟织物整理剂不仅比任何防水剂具有更优良的防油防水性能，而且最大的特点是经含氟防油防水整理剂处理过的织物没有失去织物材料原有的透气性。与其他织物整理剂相比，含氟织物整理剂有以下显著特点：优异的拒水性和独特的拒油性，超低的表面张力，可以保持织物良好的手感和优异的透气性、透湿性，被广泛应用于高档纺织品种。
目前含氟织物整理剂主要分为以下几种类型：全氟羧酸型织物整理剂（也称为憎水憎油剂），全氟磺酸型织物整理剂，高分子氟碳织物整理剂。
全氟烷基羧酸型憎水憎油剂是指碳链不小于8个碳的全氟辛酸系列的含氟织物整理剂，例如：全氟辛酸铬络合物CF3(CF2)6CO2CrOH。全氟辛酸类化合物用PFOA表示。
全氟烷基磺酸型憎水憎油剂是指碳链不小于8个碳的全氟烷基磺酸络合物及其衍生物。可表示为CF3(CF2)nSO2R，其中n≥7，R可为：-OH，-NH2，-NHCH2CH3，-N(CH2CH3)2，例如：全氟辛烷磺酸(PFOS)—CF3(CF2)7SO3H。
高分子氟碳憎水憎油剂(聚合物型)其有效成分为具有不小于8个碳的全氟烷基(Rf)的丙烯酸或甲基丙烯酸酯的聚合物,Rf基作为侧基挂在主链上。
其憎水憎油性能的产生主要是由于这几种织物整理剂的含氟链段整齐排列在在织物表面，形成保护层，从而降低表面张力，提高界面性能。
氟链段在强碱溶液中可以水解进入溶液中，从而可以对含氟织物整理剂的活性成分进行定量和定性的检测分析。
PFOS、PFOA产品的广泛使用使它们通过多种途径进入环境，这类物质在环境中具有持久性、生物积累性和远距离迁移的能力，对人类健康和人类赖以生存的环境造成了极大危害。到目前为止，在水体、大气、海洋沉积物及人类和动物的血清、肝脏、肌肉等组织器官中PFOS和PFOA均有不同程度的分布，己成为全球性的污染问题。因此，美国环境保护局要求PFOA生产商以2000年的情况为基准，在2010年之前将产品中的PFOA释出量和含量减少95%，而在2015年之前彻底放弃使用长氟碳链（全氟碳原子数≥8）的含氟物质。 对于纺织行业，PFOS和PFOA的来源主要是含氟防水防油整理剂。因此，欧盟于2006年发布的法令中规定：出口欧盟的纺织品中，PFOS的含量必须小于1µg/m2；同样，对PFOA也提出了限制要求。同时指令提出PFOA及其盐与PFOS有相似的风险，出台关于PFOA及所有直链全氟辛基(C8)衍生物的禁令已成为趋势。现在已经有多家客户提出织物上的PFOA含量也要小于1µg/m2。
关于PFOS和PFOA的检测方法，由于其限量要求仅为1µg/m2因此对检测技术及检测设备的要求很高，国际上并无正式的检测方法出台，OEKO-TEX®100标准中也只是提到用甲醇萃取后，采用液相色谱—串联质谱的内部方法进行检测。相应地，浙江省于2009年6月3日发布了地方标准DB33/T749—2009 《纺织品、皮革中全氟辛烷磺酸盐（PFOS）和全氟辛酸盐（PFOA）的测定液相色谱—串联质谱法》，迈出了制定检测标准的第一步。然而，目前国内并没有检验织物中含氟整理剂的相关方法和标准。
含氟织物整理剂在织物使用过程中会发生水解，活性物质—长链全氟烷基衍生物进入人体和环境中最终转化为PFOA和PFOS，对人体和环境产生持久性危害。欧盟已对以PFOS及其衍生物为原料的相关制品提出禁令，但世界上多数国家仍允许此类产品的使用。我国纺织品产量和进出口数量巨大，此类产品广泛存在于民众的生产和生活中。同时为了应对贸易壁垒对我国纺织业造成进一步的危害，我国正积极采取应对措施，所以，建立含氟织物整理剂的检验、检测方法和条件，建立具有系统性、快速、安全高效的成份分析方法有重要意义。
发明内容
本发明的目的在于提供一种方便、快捷、效果好的纺织品中微量含氟整理剂的测定方法。
本发明的技术解决方案是：
一种纺织品中微量含氟整理剂的测定方法，其特征是：包括下列步骤：
（1）含氟织物整理剂的水解：
选取一定面积涂覆含氟整理剂的织物，表面清洗干净，在浓度为0.1mol/L的氢氧化钠溶液中沸腾回流30分钟，冷却；取出织物置于新配置的浓度为0.1mol/L的氢氧化钠溶液中二次沸腾回流30分钟；如此沸腾回流共三次；
（2）全氟烷基类物质的初步定性：
选取甲苯或二甲苯，使用液液萃取的方法在超声和微波的辅助下对水解脱落的全氟烷基物质进行萃取，分离有机相，并进行旋蒸处理，将处理后的样品进行红外光谱或拉曼光谱的光谱学分析，通过对特定官能团光谱学特征的分析初步判断活性物质的种类；
（3）全氟烷基类物质的萃取：
用匀浆法、振荡法、超声波辅助提取法或微波辅助萃取方法，选用甲苯或二甲苯进行提取；提取液通过液液萃取、固相萃取、固相微量萃取或凝胶渗透色谱法进行净化处理，去除其中的干扰物，制成适合仪器分析的样品；
（4）全氟烷基类物质的HPLC/MS/MS分析：
用高效液相-质谱联用的方法对含氟织物整理剂的活性物质进行检测分析，对织物中含氟整理剂进行定性、定量分析。
本发明具有系统性、快速、安全高效。
下面结合实施例对本发明作进一步说明。
具体实施方式
一种纺织品中微量含氟整理剂的测定方法，包括下列步骤：
（1）含氟织物整理剂的水解：
选取一定面积涂覆含氟整理剂的织物，表面清洗干净，在浓度为0.1mol/L的氢氧化钠溶液中沸腾回流30分钟，冷却；取出织物置于新配置的浓度为0.1mol/L的氢氧化钠溶液中二次沸腾回流30分钟；如此沸腾回流共三次；
（2）全氟烷基类物质的初步定性：
选取甲苯或二甲苯，使用液液萃取的方法在超声和微波的辅助下对水解脱落的全氟烷基物质进行萃取，分离有机相，并进行旋蒸处理，将处理后的样品进行红外光谱或拉曼光谱的光谱学分析，通过对特定官能团光谱学特征的分析初步判断活性物质的种类；
（3）全氟烷基类物质的萃取：
用匀浆法、振荡法、超声波辅助提取法或微波辅助萃取方法，选用甲苯或二甲苯进行提取；提取液通过液液萃取、固相萃取、固相微量萃取或凝胶渗透色谱法进行净化处理，去除其中的干扰物，制成适合仪器分析的样品；
（4）全氟烷基类物质的HPLC/MS/MS分析：
用高效液相-质谱联用的方法对含氟织物整理剂的活性物质进行检测分析，对织物中含氟整理剂进行定性、定量分析。
Claims (1)
1.一种纺织品中微量含氟整理剂的测定方法，其特征是：包括下列步骤：
（1）含氟织物整理剂的水解：
选取一定面积涂覆含氟整理剂的织物，表面清洗干净，在浓度为0.1mol/L的氢氧化钠溶液中沸腾回流30分钟，冷却；取出织物置于新配置的浓度为0.1mol/L的氢氧化钠溶液中二次沸腾回流30分钟；如此沸腾回流共三次；
（2）全氟烷基类物质的初步定性：
选取甲苯或二甲苯，使用液液萃取的方法在超声和微波的辅助下对水解脱落的全氟烷基物质进行萃取，分离有机相，并进行旋蒸处理，将处理后的样品进行红外光谱或拉曼光谱的光谱学分析，通过对特定官能团光谱学特征的分析初步判断活性物质的种类；
（3）全氟烷基类物质的萃取：
用匀浆法、振荡法、超声波辅助提取法或微波辅助萃取方法，选用甲苯或二甲苯进行提取；提取液通过液液萃取、固相萃取、固相微量萃取或凝胶渗透色谱法进行净化处理，去除其中的干扰物，制成适合仪器分析的样品；
（4）全氟烷基类物质的HPLC/MS/MS分析：
用高效液相-质谱联用的方法对含氟织物整理剂的活性物质进行检测分析，对织物中含氟整理剂进行定性、定量分析。
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