新会出入境检验检疫局
扫 描 看 全 文
邓爱华, 庞晋山, 彭晓俊, 等. 气相色谱/双柱双检测器测定塑料制品中10种有机锡[J]. 分析测试学报, 2015,34(1):35-42.
Determination of 10 Organotin Compounds in Plastic Products by Gas Chromatography Coupled with Dual Columns and Dual Detectors[J]. 2015,34(1):35-42.
将不同材质塑料样品用四氢呋喃溶解,再用甲醇沉淀杂质大分子后高速离心过滤,各有机锡在乙酸-乙酸钠缓冲溶液中与四乙基硼酸钠反应生成有机锡的乙基化衍生物,经正己烷萃取后进行气相色谱定性、定量分析,并对衍生化条件(如衍生时间、酸度、衍生试剂)进行优化。用双柱-质谱和火焰光度双检测器/气相色谱法测定了PVC,PC,PS,AS及ABS不同塑料样品中的二甲基锡、三甲基锡、二乙基锡、一丁基锡、二丁基锡、四丁基锡、二辛基锡、三环己基锡、二苯基锡和三苯基锡共10种有机锡化合物。采用外标法定量,在0.01~10 mg?L-1浓度范围内,各有机锡化合物均呈良好线性,其相关系数(r)均大于0.999。测得PVC,PS,ABS不同塑料样品中10种有机锡的回收率为75.1%~110.1%,相对标准偏差(n=6)小于10%,检出限为0.005~0.037 mg/kg。该方法重复性好,操作简单,灵敏度高,能广泛应用于各种塑料制品中多种有机锡的检测。
Different plastic samples were dissolved completely in tetrahydrofuran(THF),the impurities of high molecular weight were precipitated with methanol and separated by high speed centrifugation and filtration.The target organotin compounds were derivatized with sodium tetraethylborate in acetic acid and sodium acetate buffer solution.The ethyl derivatives of organotin compounds were extracted with n-hexane and then qualitatively and quantitatively analyzed by gas chromatography.The derivatization conditions such as derivatization time,pH value,derivatization reagent were optimized.10 organotin compounds(dimethyltin,trimethyltin,diethyltin,n butyltin,dibutyltin,tetrabutyltin,di n-octyltin,tricyclohexyltin,diphenyltin and triphenyltin) in plastic samples of PVC,PC,PS,AS and ABS were determined by gas chromatography coupled with dual column and dual detectors of mass spectrometry and flame photometric detector.10 mixed organotin compounds ranging from 0.01 to 10 mg/L were tested by the external standard method.The experimental results indicated that the correlation coefficients of calibration curves(r) for the organotin compounds were over 0.999.The average spiked recoveries were in the range of 75.1%-110.1% with relative standard deviations less than 10% in ABS,PS and PVC plastic samples,and the detection limits for 10 organotin compounds were in the range of 0.005-0.037 mg/kg.The method showed good extraction efficiency,high sensitivity and good reproducibility,and was suitable for the determination of organotin compounds in different plastic products.
双柱双检测器气相色谱有机锡化合物质谱火焰光度检测器塑料制品
gas chromatography with dual columns and dual detectorsorganotin compoundsmass spectrometry(MS)flame photometric detector(FPD)plastic products
0
浏览量
562
下载量
9
CSCD
关联资源
相关文章
相关作者
相关机构