应用GC-MS技术检测纺织品中的短链氯化石蜡方法研究
发布时间：2018-09-08 07:28
【摘要】：随着国际贸易日益繁荣,纺织品进出口安全问题倍受关注。近年来,一些进出口纺织品中不断被检测出禁用危害物质,其生态安全性问题引起纺织行业及其相关检测机构的极大关注。短链氯化石蜡因其具有阻燃性、低蒸气压、耐火性、低挥发性等特性,在纺织品中多被用于阻燃剂,但其又具有远距离环境迁移能力、持久性、生物蓄积性和生态毒性,长期接触会致畸、致癌、致突变,因此已被欧盟等列为禁止使用的持久性有机污染物,很多国家已限制或禁用。目前,关于纺织品中短链氯化石蜡的检测技术研究较少,且各实验室采用的检测仪器不同,无法进行有效性对比。本文建立了正己烷超声波萃取、正己烷活化弗罗里硅土柱净化的纺织品中短链氯化石蜡前处理方法;GC/MS选择离子扫描模式下的仪器检测方法;采用定性定量离子监控、手动积分方式、标准曲线定量分析方法。重点研究了不同含氯量的短链氯化石蜡定性定量分析方法,采用回收率和精密度、日间日内重现性、检测限和定量限对所建立的方法进行验证。本文所建立的检测方法为:以30mL正己烷为萃取剂,在50℃、500W的超声波条件下萃取35min后,收集萃取液,经弗罗里硅土柱净化(预先用4mL正己烷活化),以正己烷和二氯甲烷混合试剂(V/V,1:1)洗脱后,旋转蒸发再经N_2吹干,以1mL正己烷定容后经GC-MS检测。GC-MS检测条件为DB-5MS色谱柱、高纯N_2、进样口温度270℃、质谱端温度280℃、离子源温度240℃;不分流进样,进样量1μL、载气流量2.0ml/min;选择离子扫描模式、选择监测离子75、89、95、105;柱箱升温程序90℃保持1min后以40℃/min的升温速率升温至280℃,保持6min。定量方法为在定量监测离子下手动积分,经相应标准曲线定量。本文研究的检测方法线性良好,线性相关系数均达到0.990以上,回收率范围在92.11%~98.95%,相对标准偏差(RSD/%)均小于5%,日间日内重现性良好,日内相对标准偏差为4.90%~5.11%,日间相对标准偏差为6.01%~6.24%,检测限0.5mg/kg;定量限位3.5mg/kg。本文所建立的方法简便、快速、准确高效、灵敏度高,可用于纺织品中短链氯化石蜡的检测,为纺织品中短链氯化石蜡的检测提供了实用的技术手段。
[Abstract]:With the prosperity of international trade, the issue of textile import and export security has been paid more and more attention. In recent years, banned hazardous substances have been detected in some import and export textiles, and their ecological safety has attracted great attention of textile industry and related testing organizations. SCCPs are widely used as flame retardants in textiles because of their properties of flame retardancy, low vapor pressure, fire resistance and low volatility. However, SCCPs have long distance environmental transport, persistence, bioaccumulation and ecotoxicity. Long-term exposure to teratogenic, carcinogenic, mutagenic, has been banned by the European Union and other persistent organic pollutants, many countries have been restricted or banned. At present, there is little research on the detection technology of SCCPs in textiles, and the testing instruments used in each laboratory are different, so it is impossible to compare the validity of SCCPs. In this paper, an instrument method for the determination of SCCPs in textiles by ultrasonic extraction of n-hexane and purification with n-hexane activated Florisil column has been developed, in which GC / MS selected ion scanning mode, and qualitative and quantitative ion monitoring was used to monitor the SCCPs. Manual integration, standard curve quantitative analysis method. The methods of qualitative and quantitative analysis of SCCPs with different chlorine contents were studied. The recoveries, precision, intra-day reproducibility, detection limits and quantitative limits were used to verify the established methods. In this paper, the detection method is as follows: after extracting 35min with 30mL n-hexane as extractant and ultrasonic wave at 50 鈩，
本文编号：2229813
[Abstract]:With the prosperity of international trade, the issue of textile import and export security has been paid more and more attention. In recent years, banned hazardous substances have been detected in some import and export textiles, and their ecological safety has attracted great attention of textile industry and related testing organizations. SCCPs are widely used as flame retardants in textiles because of their properties of flame retardancy, low vapor pressure, fire resistance and low volatility. However, SCCPs have long distance environmental transport, persistence, bioaccumulation and ecotoxicity. Long-term exposure to teratogenic, carcinogenic, mutagenic, has been banned by the European Union and other persistent organic pollutants, many countries have been restricted or banned. At present, there is little research on the detection technology of SCCPs in textiles, and the testing instruments used in each laboratory are different, so it is impossible to compare the validity of SCCPs. In this paper, an instrument method for the determination of SCCPs in textiles by ultrasonic extraction of n-hexane and purification with n-hexane activated Florisil column has been developed, in which GC / MS selected ion scanning mode, and qualitative and quantitative ion monitoring was used to monitor the SCCPs. Manual integration, standard curve quantitative analysis method. The methods of qualitative and quantitative analysis of SCCPs with different chlorine contents were studied. The recoveries, precision, intra-day reproducibility, detection limits and quantitative limits were used to verify the established methods. In this paper, the detection method is as follows: after extracting 35min with 30mL n-hexane as extractant and ultrasonic wave at 50 鈩，
本文编号：2229813
本文链接：https://www.wllwen.com/kejilunwen/huaxue/2229813.html
教材专著
