高能偏振能量色散X射线荧光光谱法分析古陶瓷  

Application of High Energy Polarized Energy Dispersion-XRFS to Analysis of Ancient Ceramics

作　　者：盛成[1] 卓尚军[1] 吉昂[1] 申如香[1] 

机构地区：[1]中国科学院上海硅酸盐研究所古陶瓷科学研究国家文物局重点科研基地,上海200050

出　　处：《理化检验（化学分册）》2012年第6期629-633,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家重点基础研究发展计划973计划项目(2012CB720900)

摘　　要：以国家地质标准样品制作工作曲线,用粉末压片法制样,高能偏振能量色散X射线荧光光谱法测定古陶瓷中包括15种稀土元素在内的56种元素,通过对6个陶瓷胎标准样品分析,结果表明:钪、钒、锰、铬、锌、镓、锗、铷、锶、钇、锆、铌、镉、锡、铯、钡、镧、铈、镨、钕、钆、钬、铒、铥、镱、镥、钍、铀等28种痕量元素测定值均在参考值的不确定度3～4倍范围,其他痕量元素如镍、铜、钼、锑、钐、铕、铽、铪、铅、铋等10种元素合格率为50%～83%。钠、镁、钾、钙、铁的氧化物和钛等6个项目均在允许误差范围内。氯、硫、磷的合格率均为66.6%。二氧化硅和三氧化二铝测定值和波长色散X射线荧光光谱熔融法测定结果相比,绝对误差分别在0.95%～4.46%和0.60%～1.66%之间。Fifty six elements including t5 rare earth elements in ancient ceramics were determined by high energy polarized energy dispersion （HEPED）-XRFS. The sample was prepared by technique of pressed powder pellets using China national geological certified reference materials for preparation of working standard curves. The proposed method was applied to the analysis of 6 standard samples of ceramics body. As shown by the analytical results, the determined values of Sc, V, Mn, Cr, Zn, Ga, Ge, Rb, Sr, Y, Zr, Nb, Cd, Sn, Cs, Ba, La, Ce, Pr, Nd, Gd, Ho, Er, Tm, Yb, Lu, Th and U were in conformity with the certified values having their uncertainties in the range of 3 to 4 times of certainties of the certified values; among the determined values of the 10 trace elements, i. e. , Ni, Cu, Mo, Sb, Sm, Eu, Tb, Hf, Pb and Bi, 50% to 83% were accepted; values of Ti and oxides of Na, Mg, K, Ca, Fe and Ti obtained were within the tolerances of these elements; 66. 6% of the determined values of C1, S and P were accepted; absolute errors between the determined values of SiO2 and AlcOa found by this method and by WDXRFS method （with sample preparation by fusion） were in the ranges of 0. 95%-4.46% and 0. 60%-1.66% respectively.

关 键 词：高能偏振能量色散X射线荧光光谱法 定量分析 古陶瓷 

分 类 号：O657.34[理学—分析化学]