首页|X射线荧光光谱法测定复式碳化物中的主组分

X射线荧光光谱法测定复式碳化物中的主组分

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采用传统化学方法测定复式碳化钨中的主组分时操作步骤繁多,分析时间长且检测结果不稳定.本文采用四硼酸锂-偏硼酸锂混合试剂为溶剂、溴化锂为脱模剂进行熔融制样,系统考察了试样的预氧化时间、试样与溶剂质量比、脱模剂用量对检测结果的影响,得出了制样的最佳条件:预氧化时间60min,试样与溶剂质量比为1:25,脱模剂用量为1.0ml.自制 20个Ti、Ta、W氧化物不同梯度的标准样品,用理论α系数校正基体效应,建立X射线荧光光谱分析标准曲线,校准曲线的线性相关系数均大于0.999.分别选用CK29和CK32样品进行精密度考察,测定复式碳化物中各组分的相对标准偏差(RSD,n=11)均小于1%,结果表明采用本实验方法测定复式碳化物中的组分结果准确可靠.
Determination of main components in compound carbides by X-ray fluorescence spectrometry
There are many operation steps,long analysis time and unstable results when traditional chemical methods are used to determine the main components in compound tungsten carbide.In this paper,the mixed flux of lithium tetraborate and lithium metaborate was used as solvent and lithium bromide as release agent for melting sample preparation.The effects of pre oxidation time,mass ratio of sample to solvent,and amount of release agent on the detection method were investigated.The optimal conditions for sample preparation were obtained:pre oxidation time 60min,mass ratio of sample to solvent 1:25,and amount of release agent 1.0ml.20 standard samples of Ti,Ta,W oxides with different gradients were prepared α The coefficient is used to correct the matrix effect,and the standard curve of X-ray fluorescence spectrum analysis is established.The linear correlation coefficients of the calibration curves are greater than 0.991.CK29 and CK32 samples were selected for precision inspection,and the relative standard deviation(RSD,n=11)of each component in the compound carbide was less than 1%.The results showed that the method was accurate and reliable.

X-ray fluorescence spectrometrymelting sample preparationWTiTa

何红梅、唐彦渊、钟志强

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崇义章源钨业股份有限公司,江西 赣州 341300

X射线荧光光谱法 熔融制样 Ti Ta W

2024

世界有色金属
有色金属技术经济研究院

世界有色金属

影响因子:0.138
ISSN:1002-5065
年,卷(期):2024.(8)
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