用溶剂沉淀-气相色谱-微量池电子捕获法测定橡胶制品中得克隆阻燃剂含量  

Determination of content of dechlorane plus flame retardant in rubber products by solvent precipitation and gas chromatography-micro cell electron capture method

作　　者：余建龙 霍炜江 彭志铿 刘志文 李全忠 YU Jian-long;HUO Wei-jiang;PENG Zhi-keng;LIU Zhi-wen;LI Quan-zhong(Guangzhou Customs District Technology Center,Guangzhou 510623,China)

机构地区：[1]广州海关技术中心,广州510623

出　　处：《合成橡胶工业》2025年第2期97-100,共4页China Synthetic Rubber Industry

基　　金：国际标准科研项目资助子项目(ISO/TS 21826:2020);广州海关科技资助项目(2022 GZCK 11)。通讯联系人。

摘　　要：采用溶剂沉淀-气相色谱-微量池电子捕获法检测橡胶制品中得克隆(DP)阻燃剂的含量,使用二氯甲烷、丙酮、四氢呋喃和乙酸乙酯对3种橡胶制品中DP的提取效果进行了考察。结果表明,四氢呋喃对丁苯橡胶、硅橡胶和天然橡胶的溶解及对DP的提取效果较好。使用100%二甲基聚硅氧烷、(5%-苯基)-甲基聚硅氧烷和聚乙二醇3种不同极性的毛细色谱柱对DP进行分离,结果显示(5%-苯基)-甲基聚硅氧烷色谱柱对DP顺反异构体的分离度良好,灵敏度高。通过加入乙腈对提取液中聚合物分子进行沉淀,结果表明图谱的信噪比和试验的精密度均有所改善。DP在质量浓度50~2000μg/L范围内与色谱峰面积呈良好线性关系,其检出限为50μg/L。DP在空白基质中的加标回收率为85.7%~102.0%,相对标准偏差为2.9%~4.8%。该方法准确、高效,适用于橡胶制品中阻燃剂DP的分析检测。The content of dechlorane plus(DP)flame retardant in rubber products was detected by solvent precipitation and gas chromatography-micro cell electron capture method.The extraction efficiency of DP from three rubber samples was investigated using dichloromethane,acetone,tetrahydrofuran,and ethyl acetate.The results showed that tetrahydrofuran had better solubility in styrene-butadiene rubber,silicone rubber,and natural rubber,as well as better extraction effect on DP.The separation of DP was carried out using capillary chromatography columns with different polarities of 100%dimethyl polysiloxane,(5%-phenyl)-methyl polysiloxane,and polyethylene glycol.The results showed that the(5%-phenyl)-methyl polysiloxane column had good separation efficiency and high sensitivity for the cis-and trans-isomers of DP.By adding acetonitrile for solvent precipitation of polymer molecules in the extraction solution,the results showed that the signal-to-noise ratio of the spectrum and precision of the experiment were improved.DP showed a good linear relationship with the chromatographic peak area within the concentration range of 50-2000μg/L,with a detection limit of 50μg/L.The spiked recovery rate of DP in blank matrix was 85.7%-102.0%,with a relative standard deviation range of 2.9%-4.8%.This method was accurate,efficient,and suitable for the analysis and detection of flame retardant DP in rubber products.

关 键 词：气相色谱-微量池电子捕获 溶剂沉淀 橡胶制品 得克隆 阻燃剂 加标回收率 相对标准偏差 

分 类 号：TQ330.7[化学工程—橡胶工业]