19种氯代烃混合标准气体的研制  

Development of a 19 chlorinated hydrocarbon gas standard mixture for environmental measurement

作　　者：李宁[1] 杜健[1] 王倩[1] 范洁[1] 钱萌[1] 倪才倩 田文[1] 

机构地区：[1]环境保护部标准样品研究所,北京100029

出　　处：《分析试验室》2013年第12期92-96,共5页Chinese Journal of Analysis Laboratory

基　　金：环保公益性科研专项(200909014;201309013)资助

摘　　要：研究了常温下19种氯代烃混合标准气体的气瓶筛选、制备方法、瓶内均匀性和稳定性等。应用自主研发的挥发性有机物气化装置,采用称量法制备了19种氯代烃标准气体,其制备重复性的相对标准偏差小于1.4%。样品采用GC-FID法测定。经气瓶筛选研究发现,19种氯代烃标准气体可以选用国产涂层气瓶,大大降低了原材料成本。依据ISO Guild 35评价样品的时间稳定性,结果显示19种氯代烃可以稳定保存12个月。19种氯代烃的浓度水平为1μmol/mol,相对扩展不确定度为5%,最低使用压力为2MPa,使用有限期为一年,为环境空气中挥发性氯代烃的测定提供实物标准支持。Cylinder selection, preparation method, within bottle homogeneity and stability studies for the 19 chlorinated hydrocarbons gas standard mixtures were studied. 19 chlorinated hydrocarbon gas standard mixtures were prepared by gravimetric method using home-made volatile organic compounds gasifying apparatus, and the relative standard deviation of preparation repeatability was less than 1.4%. Those gas standard mixtures were determined using gas chromatography with a hydrogen flame ionization detector. Cylinder selection study indicated that the chlorinated hydrocarbon gas standard mixtures could be papered by domestic treated cylinder, which significantly decreased the cost of raw materials. The experiment design and data evaluation of long- stability were performed according to ISO Guide 35 （Reference materials-General and statistical principles for certification）. Individual sample was measured as time elapsed over a period of 12 months under identical conditions. The analytical data showed that no instability was observed and all 19 chlorinated hydrocarbons in treated aluminum gas cylinders were stable for as long as 12 months. The uncertainties for the certified values of 19 chlorinated hydrocarbons in the gas standards included uncertainties of the certified value, uncertainties of unhomogeneity and instability. The determination results showed that the 19 chlorinated hydrocarbons at a level of 1 μmol/mol with relative expanded uncertainties of 5% were homogeneous in cylinders and stable as long as 12 months. This study supplied the standard support for the determination of volatile chlorinated hydrocarbons in ambient air.

关 键 词：氯代烃 标准气体 制备方法 稳定性 不确定度 

分 类 号：O657.7[理学—分析化学]