环境监测用5种氯代烯烃混合气体标准样品研制

介绍了1μmol/mol氮气中5种氯代烯气体标准样品的研制方法。这5种氯代烯包括氯乙烯、1,1-二氯乙烯、顺1,2-二氯乙烯、三氯乙烯、四氯乙烯,其中氯乙烯常温下为气态,其他4种为液态,并且沸点低,将这几种氯代烯制备成气体标准样品存在制备精度低、气液转换不完全等困难。经研究,采用2步称量法制备5种氯代烯气体标准样品,重复制备的相对标准偏差小于1.6%。建立了5种氯代烯标准气体瓶内均匀性的实验方法,并通过考察样品量值伴随样品压力的变化来评价样品的均匀性。结果显示,5种氯代烯标准气体是均匀的,最低使用压力为1 MPa。依照ISO 15000.3来考察样品的时间稳定性,样品有效期为12个月。相对扩展不确定度为3%(置信度为95%)。

Development of a Standard Reference Material Containing 5 Chlorinated Hydrocarbons for Environmental Monitoring

The development of reference material of the mixed gas of five hydrochloric hydrocarbons was described. Vinyl chloride is gas, 1, 1-Dichloroethylene cis-1,2-Dichloroethene, Trichloroethylene, Trichloroethylene, Tetrachloroethylene are liquid at room temperature, and so it is difficult to prepare an accurate a standard Reference Material containing 5 Chlorinated hydrocarbons. This research adopts two-step weighting method to prepare the standard gas of five hydrochloric hydrocarbons, and the relative standard deviation of preparation repeatability is less than 1.6%. The experimental method of within-bottle homogeneity of 5 chlorinated hydrocarbon gas standards was developed, and whether the trend for the values varying with the sample pressure changed was used to investigate the sample homogeneity. Based on experimental results, 5 volatile chlorinated hydrocarbons standard gas is homogeneous, and the minimum pressure was determined as 1MPa.The experiment design and data evaluation of long-stability is according to ISO Guide 35 (Reference materials-General and statistical principles for certification). Individual Sample was measured as time elapses over a period of 12 months under identical conditions. The analytical data showed no instability was observed and all 5 chlorinated hydrocarbons in treated aluminum gas cylinders was stable for as long as 12 months. The relative expanded uncertainty is 3%(confidence coefficient is 95%).