粉末压片制样-X射线荧光光谱法测定二氧化锆材料中二氧化锆的含量  

Determination of Zirconium Dioxide in Zirconium Dioxide Material by X-Ray Fluorescence Spectrometry after Sample Preparation with Powder Tableting

作　　者：周双清[1] 徐建平[1] 李明昌 ZHOU Shuangqing;XU Jianping;LI Mingchang(The State Key Laboratory of Refractories and Metallurgy,Wuhan University of Science and Technology,Wuhan 430081,China;Anhui Changjiang Iron and Steel Co.,Ltd.,Maanshan 243100,China)

机构地区：[1]武汉科技大学省部共建耐火材料与冶金国家重点实验室,武汉430081 [2]安徽长江钢铁股份有限公司,马鞍山243100

出　　处：《理化检验（化学分册）》2022年第8期902-908,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：以题示方法测定二氧化锆材料中二氧化锆含量,并研究了取样量以及谱线重叠对二氧化锆测定的影响。将样品研磨成粒径小于75μm的粉末,于105℃加热2 h。将2 g硼酸作为衬底置于压样机压腔中,铺平,称取不少于2.00 g样品粉末均匀覆盖在硼酸上,在压力410 kN,保压时间20 s的条件下,压制成外径为40 mm的样片,按仪器工作条件测定。结果表明:取样量为1.00 g时,样片厚度低于临界厚度(167 nm),且样片辐射面厚薄不均,二氧化锆测定值偏低;取样量不小于2.00 g时,虽然样品分析层密度降低,二氧化锆测定值降低,但是其影响可用归一法校正消除;二氧化锆样品中的锆元素会在钼、铈和钕元素分析谱线处会产生较强的谱线重叠干扰,可通过调整钼、铈和钕的谱线重叠校正系数消除。方法用于4个实际样品和二氧化锆标准物质GBW 06602的分析,测定值的相对标准偏差(n=5)不大于0.15%;和熔融制样-X射线荧光光谱法结果比对,两种方法的测定值基本一致,标准物质的测定值均在认定值的不确定度范围内。Zirconium dioxide in zirconium dioxide material was determined by the title method,and effects of sample amount and spectral line overlapping interference on the determination of zirconium dioxide were studied.The samples were ground into powder with particle size less than 75μm,and heated at 105℃for 2 h.Boric acid(2 g)was placed into the pressure chamber of tabletting machine as the substrate,flattened,and covered evenly with not less than 2.00 g of sample powder,and the sample tablet with outer diameter of 40 mm was pressed under 410 kN for 20 s,and detected according to the working conditions of the instrument.As found by results,when the sample amount was 1.00 g,the sample thickness was lower than the critical thickness(167 nm),and the radiation surface thickness of the sample was uneven,and the determined value of zirconium dioxide was low;when the sample amount was not less than 2.00 g,the density of the analytical layer was decreased,and the determined value of zirconium dioxide was decreased,and the effect could be corrected by the normalization method.Zirconium in the zirconium dioxide sample could produce strong spectral line overlapping interference at the analytical spectral lines of molybdenum,cerium and neodymium,and the interference could be eliminated by adjusting the spectral line overlapping correction coefficients of molybdenum,cerium and neodymium.The proposed method was used for the analysis of 4 actual samples and zirconium dioxide standard substance GBW 06602,and RSDs(n=5)of the determined values were not more than 0.15%.Compared with the results found by X-ray fluorescence spectrometry with fusion sample preparation,the determined values of the 2 methods were basically consistent,and the determined values of the standard substance were within the uncertainty range of the certified value.

关 键 词：粉末压片法 X射线荧光光谱法 UniQuant软件 归一法 重叠干扰校正 二氧化锆 

分 类 号：O657.34[理学—分析化学]