【摘要】：隨著國際貿(mào)易日益繁榮,紡織品進出口安全問題倍受關(guān)注。近年來,一些進出口紡織品中不斷被檢測出禁用危害物質(zhì),其生態(tài)安全性問題引起紡織行業(yè)及其相關(guān)檢測機構(gòu)的極大關(guān)注。短鏈氯化石蠟因其具有阻燃性、低蒸氣壓、耐火性、低揮發(fā)性等特性,在紡織品中多被用于阻燃劑,但其又具有遠(yuǎn)距離環(huán)境遷移能力、持久性、生物蓄積性和生態(tài)毒性,長期接觸會致畸、致癌、致突變,因此已被歐盟等列為禁止使用的持久性有機污染物,很多國家已限制或禁用。目前,關(guān)于紡織品中短鏈氯化石蠟的檢測技術(shù)研究較少,且各實驗室采用的檢測儀器不同,無法進行有效性對比。本文建立了正己烷超聲波萃取、正己烷活化弗羅里硅土柱凈化的紡織品中短鏈氯化石蠟前處理方法;GC/MS選擇離子掃描模式下的儀器檢測方法;采用定性定量離子監(jiān)控、手動積分方式、標(biāo)準(zhǔn)曲線定量分析方法。重點研究了不同含氯量的短鏈氯化石蠟定性定量分析方法,采用回收率和精密度、日間日內(nèi)重現(xiàn)性、檢測限和定量限對所建立的方法進行驗證。本文所建立的檢測方法為:以30mL正己烷為萃取劑,在50℃、500W的超聲波條件下萃取35min后,收集萃取液,經(jīng)弗羅里硅土柱凈化(預(yù)先用4mL正己烷活化),以正己烷和二氯甲烷混合試劑(V/V,1:1)洗脫后,旋轉(zhuǎn)蒸發(fā)再經(jīng)N_2吹干,以1mL正己烷定容后經(jīng)GC-MS檢測。GC-MS檢測條件為DB-5MS色譜柱、高純N_2、進樣口溫度270℃、質(zhì)譜端溫度280℃、離子源溫度240℃;不分流進樣,進樣量1μL、載氣流量2.0ml/min;選擇離子掃描模式、選擇監(jiān)測離子75、89、95、105;柱箱升溫程序90℃保持1min后以40℃/min的升溫速率升溫至280℃,保持6min。定量方法為在定量監(jiān)測離子下手動積分,經(jīng)相應(yīng)標(biāo)準(zhǔn)曲線定量。本文研究的檢測方法線性良好,線性相關(guān)系數(shù)均達到0.990以上,回收率范圍在92.11%~98.95%,相對標(biāo)準(zhǔn)偏差(RSD/%)均小于5%,日間日內(nèi)重現(xiàn)性良好,日內(nèi)相對標(biāo)準(zhǔn)偏差為4.90%~5.11%,日間相對標(biāo)準(zhǔn)偏差為6.01%~6.24%,檢測限0.5mg/kg;定量限位3.5mg/kg。本文所建立的方法簡便、快速、準(zhǔn)確高效、靈敏度高,可用于紡織品中短鏈氯化石蠟的檢測,為紡織品中短鏈氯化石蠟的檢測提供了實用的技術(shù)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，

本文編號：2229813