光谱学与光谱分析, 2011, 31 (9): 2574, 网络出版: 2011-11-09  

X射线荧光光谱分析样品烧增量的影响及校正

The Influence of the Gain on Ignition and Correction in X-Ray Fluorescence Spectrometry
作者单位
1 宁波出入境检验检疫局, 浙江 宁波315012
2 德国布鲁克AXS公司北京代表处, 北京10008
摘要
研究采用熔融法制备矿石样品时出现的烧增量问题, 建立新的校正方法。 硫化物矿的烧增量有百分之几十, 它改变基体组成, 造成基体校正的错误, 新方法先将具有烧增量的样品转换成具有烧失量的新样品, 然后用差减法校正烧失量, 用理论影响系数法校正基体效应, 求得新样品的结果, 最后再换算回原样的结果。 此方法以铜精矿为实验对象, 比较差减法和重量法测烧增量的差异, 计算当两者相差较大时对被测元素的影响, 并且发现稀释比越大烧增量误差对被测元素的影响越小。 经过烧增量校正后的铜精矿方法Cu, Fe和S等主成分的校准曲线标准偏差达到了0.14%, 0.074%和0.14%, 明显优于经验影响系数法校正后的结果0.21%, 0.15%和0.19%, 准确性通过标准物质的验证结果良好。
Abstract
Research on the gain on ignition question for preparing ore with fusion sample preparation technique was done, and a new correction method was worked out. After fusion sample preparation, sulphide ore would have a lot of sulfate, which would change the sample matrix dramatically, and the matrix effect was corrected with errors. In this paper, a new solution to measuring gain on ignition was put forward, and it was committed step that the sample having gain on ignition was redefined by sample having loss on ignition. Through conversion, the gain on ignition was corrected by subtraction method, and the matrix effect was corrected by theoretical influence coefficients. The analysis results of redefinition samples were converted into the primal samples lastly. The project took copper concentrates as the experimental object, it was found that the gain on ignition of this method was obviously different from the gravimetric method, but through influence evaluation, this error had little effect on test results, and may be reduced by flux. After correction of the gain on ignition, the standard deviation of the elements calibration curves for Cu, Fe and S were less than 0.14%, 0.074% and 0.14% respectively, which were obviousely superior to 0.21%, 0.15% and 0.19%. The results got from this method were in satisfactory agreement with certified values.

王谦, 应晓浒, 张建波. X射线荧光光谱分析样品烧增量的影响及校正[J]. 光谱学与光谱分析, 2011, 31(9): 2574. WANG Qian, YING Xiao-hu, ZHANG Jian-bo. The Influence of the Gain on Ignition and Correction in X-Ray Fluorescence Spectrometry[J]. Spectroscopy and Spectral Analysis, 2011, 31(9): 2574.

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