休闲渔具油漆涂层中的短链氯化石蜡测定方法及测量不确定度分析  

Determination of Short Chain Chlorinated Paraffins in Paint Coating of Fishing Tackle and Evaluation of Uncertainly in Measurement

作　　者：侯德坤 李书胜 牛凤英 杨建民 肖亮 Hou Dekun;Li Shusheng;Niu Fengying;Yang Jianmin;Xiao Liang(Weihai Institute for Product Quality Inspection,Weihai 264210,China;National Center for Fishing Tackle Quality Inspection,Weihai 264210,China)

机构地区：[1]威海市产品质量监督检验所,山东威海264210 [2]国家渔具质量监督检验中心,山东威海264210

出　　处：《山东化工》2021年第3期119-122,125,共5页Shandong Chemical Industry

基　　金：山东省质量技术监督局科研项目(2017KY29Z02)。

摘　　要：建立了加速溶剂萃取弗罗里硅土-酸性硅胶复合柱净化气相色谱串联质谱法测定渔具油漆涂层中短链氯化石蜡的方法,利用design-expert设计正交实验对萃取、净化条件进行了优化,方法检出限为0.09 mg/kg,加标回收率为91.2%~96.4%,相对标准偏差为3.1%~3.6%,满足短链氯化石蜡的检测要求。对方法的测量不确定度进行了分析,在置信概率为95%时,该方法测定短链氯化石蜡残留的扩展不确定度为±0.022 mg/kg。A method for the determination of short chain chlorinated paraffins(SCCPs)in paint coating of fishing tackle based on accelerated solvent extraction and florisil-acid silica gel column cleanup coupled with GC-MS analysis was developed.An orthogonal experiment designed by software design-expert was used to optimize the extraction conditions,the influence of elution solvents to recoveries were also discussed.The results showed that the LODs of method was 0.09 mg/kg,the recoveries of SCCPs in paint coating ranged from 91.2%to 96.4%,with relative standard deviation in range of 3.1%~3.6%,indicated that the method was desirable for SCCPs analysis.The uncertainty components were calculated on the basis of this mathematical model,when the confidence probability was 95%,the extended uncertainty in measurement of SCCPs residue in paint coating by GS-MS was±0.022 mg/kg.

关 键 词：短链氯化石蜡 加速溶剂萃取 油漆涂层 不确定度 

分 类 号：O657.63[理学—分析化学]