重量制备氮中氢气体标准物质的实验方法  

Experiment Method of Preparing Hydrogen in Nitrogen Calibration Gases though Gravimetric

作　　者：李春瑛[1] 韩桥[1] 叶华[2] 张新[1] 张国贤[2] 吴海[1] 吴梦一[3] 

机构地区：[1]中国计量科学研究院,北京100013 [2]原国家标准物质研究中心,北京100013 [3]北京化工大学,北京100029

出　　处：《现代科学仪器》2009年第2期78-81,共4页Modern Scientific Instruments

摘　　要：研究了重量法制备氮中氢气体标准物质的实验方法。采用中国计量科学研究院自行设计加工的气体充填装置制备了氮中氢气体标准物质,该装置低压系统真空度达到7×10^(-3)Pa;气体称量装置采用美国Mettler SB16001电子天平(16kg、0.1g)和上海第二天平仪器厂TG320B高精密天平(20kg、10 mg)称量组分及稀释气体的质量;采用美国Agilent公司6890型气相色谱仪脉冲放电氦离子化检测器(PDHID)对稀释气体中微量氢进行分析,该仪器对氢的检测限为4×10^(-9)。实验中选取其中氢含量低于0.01×10^(-6)的高纯氮气体,以满足配制1×10^(-6)及100×10^(-6)标准气体的需求。本项研究组分气体和稀释气体分析的扩展不确定度分别<0.002%,氮中氢系列气体标准物质重量制备的不确定度均小于1%。This article studied a test way of preparing standard gas of hydrogen in nitrogen by weight method. This method adopted the equipment filled with gas designed and processed by National Institute of Metrology to prepare standard gas of hydrogen in nitrogen, the attainable vacuum in low pressure system of which was 7 × 10^-3 Pa. The SB16001 electronic balance （16kg, 0. 1 g） produced by Metterler company of the United States was used for gas weighing installations and the TG320B high -precision instrument balance （20 kg, 10 mg） produced by Shanghai second balance company was used to weigh components and dilution gas. Micro hydrogen in dilution gas was analyzed by Agilent＇s 6890 gas chromatograph -pulse discharge helium ionization detector （PDHID）, the detection limit of which for hydrogen was up to 4 × 10^-9. In the experiment, high - purity nitrogen gas is selected in which hydrogen content less than 0.01 × 10^-6 to meet the demand of preparation of 1 × 10^-6 and 100 × 10^-6. In the study, the expanded uncertainty of composition gas and diluted gas is tess than 0. 002 percent respectively, the weigh preparing uncertainty of a series of standard gas about hydrogen in nitrogen is less than 1% respectively.

关 键 词：重量法 氯中氢 气体标准物质 不确定度 

分 类 号：TQ116.1[化学工程—无机化工]