摘要：选择商品化的13X分子筛颗粒作为微孔孔容和孔径标准物质候选材料,利用交叉缩分方法对标准物质样品进行分装;从分装后的标准物质样品中随机抽取样品来检验其均匀性、稳定性;采用国际公认的氩气物理吸附方法,通过与欧洲经济共同体IRMM标准物质BCR-704比较测量的方式对标准物质样品进行定值。结果表明,经均匀性、稳定性检验,所研制的微孔孔容和孔径标准物质GBW(E)130366具有良好的均匀性和稳定性(至少12个月);微孔孔容和孔径分别为0.242 cm³/g和0.668 nm;与国内外同类标准物质相比,GBW(E)130366填补了国内空白,其相对不确定度(3.3%和2.8%)达到国际同类标准物质的先进水平。

关键词：标准物质；微孔孔容；微孔孔径；Saito-Foley 方法；氩气吸附

Abstract：The commercial 13X molecular sieve particles were used as the candidate of certified reference materials(CRM) for micropore volume and diameter and subpackaged by means of cross riffling method.Homogeneity and stability tests were carried out by exacting samples randomly from CRM.Using the internationally recognized argon physical adsorption method,the micropore was certified by comparison with CRM BCR-704.The results show that by homogeneity and stability tests CRM GBW(E)130366 is homogeneous and stable for at least 12 months,respectively.The micropore volume and diameter are 0.242 cm³/g and 0.668 nm.Compared with the similar CRM in the world,it shows that the developed CRM GBW(E)130366 for micropore volume and diameter fills the domestic blanks and its uncertainty(3.3% and 2.8%) comes up to the advanced world level.

Keywords：certified reference materials；micropore volume；micropore diameter；Saito-Foley method；Ar adsorption