摘要
建立了顶空气相色谱(HS-GC)同时测定树脂工艺品中7种残留苯系物BTEX(苯、甲苯、乙苯、对二甲苯、间二甲苯、邻二甲苯、苯乙烯)的方法。对溶剂种类、萃取温度、萃取时间及HG-GC分离测定条件进行优化。结果表明,在顶空温度为130℃、平衡时间为60 min、粉碎样品粒径低于2 mm、选择DB-WAX色谱柱的条件下,可获得良好的分离效果和定量结果。7种残留苯系物在0.1~500μg范围内具有良好的线性关系(r2>0.999)。方法的定量下限(LOQ,S/N=10)在0.1~0.4μg.g-1之间,加标回收率为93%~114%,相对标准偏差(RSDs,n=6)为0.7%~4.8%。所建立的方法快速、准确,适用于树脂工艺品中苯系物的测定。
A method was developed for the simultaneous determination of 7 residual benzene series(BTEX),including benzene,toluene,ethylbenzene,p-xylene,m-xylene,o-xylene and styrene,in resin crafts by headspace gas chromatography(HG-GC).The extraction conditions,including solvent type,extraction temperature and time,were investigated,and the chromatographic conditions for HS-GC,including headspace bases,equilibrium temperature and time,sample granularity,were optimized.The results showed that 7 residual benzene series were preferably separated and good quantitative analyses were achieved under the headspace equilibrium temperature at 130 ℃ for 60 min,where the diameter of sample particle was smaller than 2mm and the DB-WAX capillary operation was chosen.Under the optimal conditions,the calibration curves were linear in the range of 0.1-500 μg with correlation coeficients higher than 0.999.The limits of quantitation(LOQs,S/N=10) of this method were between 0.1 μg·g-1 and 0.4 μg·g-1.The recoveries at three spiked levels ranged from 93% to 114% with relative standard deviations(RSDs) of 0.7%-4.8%.The established method was rapid and accurate,and was suitable for the analysis of benzene series in resin crafts.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第5期570-574,580,共6页
Journal of Instrumental Analysis
基金
国家质检总局科研项目(2012IK124)
国家公益性行业科研专项经费"双打"研究专项项目(2012104020)
关键词
顶空
气相色谱
树脂工艺品
苯系物
headspace
gas chromatography
resin crafts
benzene series