摘要
建立了以波长色散x射线荧光光谱仪直接测定羰化反应液及催化剂中铑含量的定量分析方法,采用甲苯为溶剂的铑催化剂溶液做校准曲线标准样品,铑质量分数测量范围为10-1000μg/g,在总测量时间为20s时,其检出限为2.2μg/g。15次的平行重复测试结果,相对标准偏差为0.94%。溶液厚度实验说明,当溶液的厚度超过14.7mm时可视为达到无限厚。并将不同样品同时进行了XRF测试和原子吸收法测量,结果一致。
The concentration of rhodium in OXO synthesis reaction solution and catalysts were directly determined by wavelength dispersive X-ray fluorescence spectrometry. Rhodium catalysts solved in toluene were used as calibration standards and the concentration of rhodium ranged from 10 to 1000μg/g were measured. The LLD of the method is lower than 2.2μg/g when the measurement time of 20 seconds was used. Repeatability results for 15 times showed that RSD of this method was only 0.94%. The effect of sample thickness on rhodium intensity was examined. The results indicated that thickness of the solution should be more than 14.7mm. With the comparison of X-ray fluorescence (XRF) and flame atomic absorption spectrophotometry (FAAS), the analysis accuracy of XRF is consistent with that of FAAS.
出处
《分析试验室》
CAS
CSCD
北大核心
2009年第5期80-82,共3页
Chinese Journal of Analysis Laboratory