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采用溶胶-凝胶-硫化法,以甲基乙烯基硅橡胶和乙烯基封端硅橡胶为原料,制备硅橡胶吸附萃取搅拌棒(stir bar sorptive extraction,SBSE),一次涂层平均厚度150～250μm,涂层表面形貌规则,热分解温度300℃。使用寿命可达150次。采用热解析(ThermalDesorptionUnit,TDU)脱附-气相色谱分析,建立了水中痕量多环芳烃(polycyclicaromatichydrocarbons,PAHs)的分析方法,并考察了不同条件下搅拌棒对PAHs的萃取效率。结果表明:在样品体积为50mL,盐浓度25g/L,温度为25℃,搅拌速度为750rpm,萃取时间为90min时,各种PAHs的检测限(LOD)为2ng/L～8ng/L,各组分峰面积的相对标准偏差(RSD)在7.91%以下,该方法的线性范围为0.3μg/L～1.0×103μg/L。实际分析样品为流经城市的运河水,优化条件下PAHs的加标回收率在76.2%～102%之间。
SBSE was prepared by sol-gel-vulcanization method using methyl vinyl silicone rubber and vinyl terminated silicone rubber as raw materials. The average primary coating thickness was 150 ~ 250μm , Coating surface morphology rules, thermal decomposition temperature 300 ℃. Life of up to 150 times. The analytical method of polycyclic aromatic hydrocarbons (PAHs) in water was established by thermal desorption unit (TDU) desorption-gas chromatography (GC-MS). The extraction efficiency of PAHs under different conditions was also investigated. The results showed that the detection limits (LODs) of various PAHs ranged from 2ng / L to 8ng / L with the sample volume of 50mL, the salt concentration of 25g / L, the temperature of 25 ℃, the stirring speed of 750rpm and the extraction time of 90min. The relative standard deviation (RSD) of peak area of the components was below 7.91%. The linear range of this method was 0.3μg / L ~ 1.0 × 103μg / L. The actual sample was canal water flowing through the city. The spiked recoveries of PAHs ranged from 76.2% to 102%.