纺织品中全氟辛酸和全氟辛烷磺酰基化合物的检测方法
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摘要
全氟辛烷磺酰基化合物(PFOS)和全氟辛酸及其盐(PFOA)作为纺织品、皮革、室内装饰装潢制品等防水、防油、抗污整理剂的主要活性成分,广泛应用于工业和消费品生产领域。PFOS和PFOA化学性质稳定,具有持久性、生物积累性和多种毒性,严重危害人类健康和其生存环境,已成为继有机氯农药、多氯联苯、二嗯英之后日益引起重视的一类新型持久性有机污染物,其污染问题受到全球的广泛关注。
为了遏制PFOS污染,欧洲议会及美国、加拿大、瑞典等发达国家的政府纷纷颁布法令法规,限制PFOS的使用。PFOS和PFOA的检测分析也成为了当今分析科学研究的热点。然而,目前对于纺织品中PFOA和PFOS的检测,国际上尚无统一的标准,我国也没有相应的国标及行标。以此为背景,本文对PFOA和PFOS快速、灵敏的定量分析方法进行了研究。
本论文根据纺织品中常用PFOS、PFOA类全氟化表面活性剂的成分,选择了3种常用的PFOS、PFOA单体(全氟辛磺酰胺、N-乙基全氟辛磺酰胺、全氟辛酸)作为研究对象,重点研究了纺织品中PFOS、PFOA的气相色谱分析测试方法。
在样品前处理方法研究方面,首先研究了测定PFOA衍生物以间接测定PFOA的可行性,通过研究衍生试剂配比、衍生反应温度、衍生时间和衍生试剂体积比等衍生条件对衍生效果的影响,确定了衍生实验的具体参数。
其次,对纺织品中PFOS和PFOA的萃取方法进行了研究。提出了两种适用的萃取方法即超声波辅助萃取法和微波辅助萃取法,通过萃取剂筛选实验、正交实验、单因子选择实验等方法实验确定了最佳萃取条件。
在检测方法方面,依据电子俘获检测器(ECD)对有机氟化物的较高响应,及仪器低廉的价格,选择了GC-ECD方法对三种PFOS、PFOA单体进行了气相色谱分析研究。通过优化仪器分析参数,实现了3种目标化合物的有效分离与与定量测定。
研究结果表明:本论文使用的检测方法加标回收率稳定在92.19～102.99%,检测限为0.00274～0.02319μg/g、RSD＜10%、保留时间较稳定、峰面积值变化小,重现性和精密度好,适于纺织品中PFOA、PFOS的检测分析。
Perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOA) and their salts have been widely used in industry as surfactants; they are used as water and oil repellants in the treatment of fabrics and leather and in the production of floor waxes and waxed paper. The chemical properties of PFOS and PFOA are stable which has persistent and bioaccumulative and a variety of toxic. It serious does harm to human health and their living environment. PFOS and PFOA have become a new type of persistent oranic pollutants which were paid increasing attention following oranochlorine pesticides, PCBs and dioxins. It has received extensive attention from all over the world.
In order to curb the pollution of PFOS, the European Union (EU) , the United States, Canada, Sweden and other developed countries have enacted laws and regulations. Detection and analysis of PFOS and PFOA has also become a hot spot of today's analysis secience. However, the testing standard of PFOS and PFOA in textiles has not developed yet. A method of simultaneous determination of PFOA and PFOS in textiles has been developed in this paper.
In this paper, three kinds of commonly used PFOS and PFOA monomer (perfluorooctane sulfonamide, N-ethyl perfluorooctane sulfonamide, perfluorooctanoic acid) were choosed as the object of study under the class perfluorocarbons surfactant composition of commonly used PFOS and PFOA in textiles. The gas chromatography analysis method of PFOS and PFOA in the textiles has been also focused.
In the first of sample pretreatment research, the feasibility of determinate FPOA has been analyzed by texting derivatives of PFOA. The specific parameters of derivative test was defined by studying derivatization temperature, derivatization time and volume ratio of derivatization reagent.
Secondly, the extraction method of PFOS and PFOA in the textiles has been studied. Two kinds of application extraction methods were proposed which were ultrasonic extraction and microwave extraction.The best extraction conditions were ensured through using extractant screening experiment, orthogonal design, and simple factor design experiments.
In the detection method research, GC-ECD method was chosed to study three kinds of PFOS and PFOA monomers by gas chromatography analysis which was based on electron capture detector (ECD) of higher response to organic fluoride and equipment at low prices. Finaly three kinds of target compounds have been separated effectively and determined quantitatively by optimizing the parameters of instrument.
The research result indicated that the recoveries of spiked samples were 92.19～102.99% and the detection limits of method were 0.00274～0.02319μg/g and the precisions were less than 10%. In addition, the peak area value has been changed little and the retention time is stable. It illustrated the method was sensitive, rapid, low cost and high recovery and could be used to the determination for the trace amount of PFOA and PFOS in textiles.
为了遏制PFOS污染,欧洲议会及美国、加拿大、瑞典等发达国家的政府纷纷颁布法令法规,限制PFOS的使用。PFOS和PFOA的检测分析也成为了当今分析科学研究的热点。然而,目前对于纺织品中PFOA和PFOS的检测,国际上尚无统一的标准,我国也没有相应的国标及行标。以此为背景,本文对PFOA和PFOS快速、灵敏的定量分析方法进行了研究。
本论文根据纺织品中常用PFOS、PFOA类全氟化表面活性剂的成分,选择了3种常用的PFOS、PFOA单体(全氟辛磺酰胺、N-乙基全氟辛磺酰胺、全氟辛酸)作为研究对象,重点研究了纺织品中PFOS、PFOA的气相色谱分析测试方法。
在样品前处理方法研究方面,首先研究了测定PFOA衍生物以间接测定PFOA的可行性,通过研究衍生试剂配比、衍生反应温度、衍生时间和衍生试剂体积比等衍生条件对衍生效果的影响,确定了衍生实验的具体参数。
其次,对纺织品中PFOS和PFOA的萃取方法进行了研究。提出了两种适用的萃取方法即超声波辅助萃取法和微波辅助萃取法,通过萃取剂筛选实验、正交实验、单因子选择实验等方法实验确定了最佳萃取条件。
在检测方法方面,依据电子俘获检测器(ECD)对有机氟化物的较高响应,及仪器低廉的价格,选择了GC-ECD方法对三种PFOS、PFOA单体进行了气相色谱分析研究。通过优化仪器分析参数,实现了3种目标化合物的有效分离与与定量测定。
研究结果表明:本论文使用的检测方法加标回收率稳定在92.19～102.99%,检测限为0.00274～0.02319μg/g、RSD＜10%、保留时间较稳定、峰面积值变化小,重现性和精密度好,适于纺织品中PFOA、PFOS的检测分析。
Perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOA) and their salts have been widely used in industry as surfactants; they are used as water and oil repellants in the treatment of fabrics and leather and in the production of floor waxes and waxed paper. The chemical properties of PFOS and PFOA are stable which has persistent and bioaccumulative and a variety of toxic. It serious does harm to human health and their living environment. PFOS and PFOA have become a new type of persistent oranic pollutants which were paid increasing attention following oranochlorine pesticides, PCBs and dioxins. It has received extensive attention from all over the world.
In order to curb the pollution of PFOS, the European Union (EU) , the United States, Canada, Sweden and other developed countries have enacted laws and regulations. Detection and analysis of PFOS and PFOA has also become a hot spot of today's analysis secience. However, the testing standard of PFOS and PFOA in textiles has not developed yet. A method of simultaneous determination of PFOA and PFOS in textiles has been developed in this paper.
In this paper, three kinds of commonly used PFOS and PFOA monomer (perfluorooctane sulfonamide, N-ethyl perfluorooctane sulfonamide, perfluorooctanoic acid) were choosed as the object of study under the class perfluorocarbons surfactant composition of commonly used PFOS and PFOA in textiles. The gas chromatography analysis method of PFOS and PFOA in the textiles has been also focused.
In the first of sample pretreatment research, the feasibility of determinate FPOA has been analyzed by texting derivatives of PFOA. The specific parameters of derivative test was defined by studying derivatization temperature, derivatization time and volume ratio of derivatization reagent.
Secondly, the extraction method of PFOS and PFOA in the textiles has been studied. Two kinds of application extraction methods were proposed which were ultrasonic extraction and microwave extraction.The best extraction conditions were ensured through using extractant screening experiment, orthogonal design, and simple factor design experiments.
In the detection method research, GC-ECD method was chosed to study three kinds of PFOS and PFOA monomers by gas chromatography analysis which was based on electron capture detector (ECD) of higher response to organic fluoride and equipment at low prices. Finaly three kinds of target compounds have been separated effectively and determined quantitatively by optimizing the parameters of instrument.
The research result indicated that the recoveries of spiked samples were 92.19～102.99% and the detection limits of method were 0.00274～0.02319μg/g and the precisions were less than 10%. In addition, the peak area value has been changed little and the retention time is stable. It illustrated the method was sensitive, rapid, low cost and high recovery and could be used to the determination for the trace amount of PFOA and PFOS in textiles.
引文
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