粉末压片-X-射线荧光光谱法分析砂岩型铀矿制样中粘结剂用量的探讨  

Analysis of Binder Content in Sandstone Type Uranium Ore SamplePreparation by Powder Tablet-X-ray Fluorescence Spectrometry

作　　者：方蓬达 张莉娟 陈彭 马骏驰 孙浩 邓华 金硕 吕学峰 FANG Pengda;ZHANG Lijuan;CHEN Peng;MA Junchi;SUN Hao;DENG Hua;JIN Shuo;LYU Xuefeng(Langfang General Survey of Natural Resources Center,China Geological Survey,Langfang,Hebei 065000,China)

机构地区：[1]中国地质调查局廊坊自然资源综合调查中心,河北廊坊065000

出　　处：《中国无机分析化学》2024年第4期450-456,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：松嫩平原西北缘扎兰屯-扎赉特地区黑土地地表基质调查项目(DD20220856)。

摘　　要：由于砂岩型铀矿的成矿特性,样品粉末的内聚力小,采用直接压片法有时难以成型,样片表面常见裂纹,上机测量易碎裂。混合压片法适应性强,制样成功率高,但常见的问题是样品经粘结剂稀释会影响元素的检出限及结果的准确性。通过对粉末压片-X射线荧光光谱法测定砂岩型铀矿地质样品时前期制样中添加粘结剂的比例进行研究,按照不同比例在铀矿石标准物质GBW04101、GBW04102中添加粘结剂,在扫描电子显微镜下观察到随着粘结剂用量的增加,样片表面的光滑度及致密度都呈上升趋势,在X-射线荧光光谱仪上对主量元素进行测定后发现X射线强度在粘结剂添加量大于0.2 g时明显下降,经与GBW04101、GBW04102标准值进行对比后,优选出粘结剂与样品的最佳比例为1∶20,在此比例下制成的样片光滑平整,不易碎裂,用粉末压片-X射线荧光光谱法进行测定,标准物质测定结果的相对误差为0.56%~6.76%,相对标准偏差(RSD,n=12)为0.013%~7.7%,均达到了《地质矿产实验室测试质量管理规范》DZ/T 0130—2006的要求。为粉末压片-X射线荧光光谱法分析砂岩型铀矿地质样品提供了可靠的实验参考依据。Due to the mineralization characteristics of sandstone type uranium deposits,the cohesive force of sample powder is small,and it is sometimes difficult to form by direct compression method.The surface of the sample is often cracked,and it is easy to break when measured on the machine.The mixed compression method has strong adaptability and a high success rate in sample preparation,but a common problem that diluting the sample with adhesive can affect the detection limit of elements and the accuracy of the results.In this paper,the proportion of binder added in the early sample preparation for the determination of sandstone type uranium ore geological samples by powder tablet pressing X-ray fluorescence spectrometry was studied.In the test,different proportions binders were added to the uranium ore standards GBW04101 and GBW04102.Scanning electron microscope observed that the smoothness and density of the sample surface increased with the increase of binder dosage.After measuring the main elements on the X-ray fluorescence spectrometer,it was found that the X-ray intensity decreased significantly when the amount of binder was greater than 0.2 g.After comparing the standard values of GBW04102,the optimal ratio of binder to sample was 1∶20.The sample prepared under this ratio was smooth and flat and not easy to break,which was determined by powder tablet pressing X-ray fluorescence spectrometry.The relative error of the determination results of reference materials was 0.56%-6.76%,and the relative standard deviation(RSD,n=12)was 0.013%-7.7%,meeting the requirements of quality management specification for laboratory testing of geology and mineral resources(DZ/T 0130—2006).This paper provides a reliable experimental reference for the analysis of geological samples of sandstone type uranium deposits by powder tablet pressing X-ray fluorescence spectrometry.

关 键 词：砂岩型铀矿 粉末压片法 粘结剂 X射线荧光光谱仪 

分 类 号：O657.39[理学—分析化学] O657.34[理学—化学]