【摘要】 建立了沉淀分离-EDTA滴定法与电感耦合等离子体光谱法(ICP-AES)相结合测定氧化钇稳定氧化锆(YSZ)样品中氧化锆含量的分析方法。考察了试样分解方法、锆的沉淀效果、盐酸用量(溶解氢氧化锆沉淀)、氧化锆测定方式、滴定酸度、滴定温度、共存物质等对测定结果的影响。结果表明,试样以过氧化钠熔融分解,用热水浸取过滤后,以6.0 mol/L盐酸溶解氢氧化锆沉淀,先以EDTA法测定溶液中氧化锆量,再以ICP-AES法测定滤纸上残留氧化锆量,两部分的合量即为试样中氧化锆的含量。氧化钇稳定氧化锆样品中共存物质不干扰氧化锆的测定。本法操作简单、测定快速,适用于氧化钇稳定氧化锆样品中氧化锆的测定,回收率在98%~101%之间,相对标准偏差(n=5)均小于0.5%,可用于日常分析。更多还原

【Abstract】 The analysis method of zirconia in yttria stabilized zirconia by precipitation separation—EDTA titration and inductively coupled plasma atomic emission spectrometry(ICP-AES) was established.The effects of sample decomposition,the precipitation effect of zirconium,HCl amount(dissolving Zr(OH)4),zirconia determination mode,titratable acidity,titratable temperature and coexisting substances were tested.The results have shown that samples were treated with sodium dioxide,dissolved with hot water,and then filtered through medium speed filter paper.The zirconium oxide content produced by dissolving Zr(OH)4 with 6.0 mol / L HCl was determined with EDTA at first,and then the residual zirconia content was determined with ICP-AES on the medium speed filter paper.Under optimum conditions,the coexisting foreign substances did not interfere with the analysis.This method was simple and fast,which has been used in yttria stabilized zirconia sample zirconia measurement.Recovery in 98% ~ 101% was obtained and the relative standard deviation(n = 5) is averagely less than 0.5%,which can be used for daily analysis.更多还原