摘要
在粉末压片-X射线荧光光谱法中采用粘结性强、腐蚀性低、价格低廉的有机纤维素粉末替换硼酸衬层,解决硼酸衬层在样品分析过程中受热挥发造成仪器金属部件、滤光片、准直器硼酸粉尘累积。添加微晶纤维素粉改善矿石粉末的粘结效果,提高制备待测样片物理性能,降低仪器维护保养成本,提高仪器运行稳定性和检测结果的准确性。通过研究羟甲基纤维素、羟乙基纤维素、羟丙基甲基纤维素等三种有机纤维素作为衬层的机械强度、热稳定性,采用微晶纤维粉改善砂岩型铀矿样品制片过程中会出现样品分层和裂纹的问题,对比替换衬层,添加辅助粘结剂前后样品测试结果的变化。结果表明,采用羟甲基纤维素作为衬层,添加0.5 g微晶纤维素测定砂岩型铀矿中9种主次元素的精密度(RSD,n=11)为0.34%~4.8%,测铀准确度为0.93%~2.8%,测钍准确度为0.80%~2.8%,其他主量元素相对误差为0.060%~5.5%。相较于硼酸衬层和未添加辅助粘结剂样品的测定值,应用格拉布斯法检验各元素统计量G均在1.2%~1.4%,实验数据无离群值和可疑值。采用羟甲基纤维素作为衬层可用于砂岩型铀矿中主次元素的测定,降低了样品分析过程中产生粉末,避免了对仪器金属部件的腐蚀影响,添加微晶纤维素0.5 g改善了矿石粘结性能,提升实验制备样片的稳定性和达标率。
Boric acid lining was replaced by organic cellulose powder with strong adhesion,low corrodibility and low price in powder lamination X-ray fluorescence spectrometry to solve the boric acid dust accumulation in instrument metal parts,filter and collimator caused by volatilization of boric acid lining during sample analysis.The addition of microcrystalline cellulose powder can improve the bonding effect of the ore powder,improve the physical properties of the sample to be tested,reduce the maintenance cost of the instrument,and improve the stability of the instrument and the accuracy of the test results.The mechanical strength and thermal stability of three kinds of organic cellulose such as hydroxymethyl cellulose,hydroxyethyl cellulose and hydroxypropyl methyl cellulose as lining layers were studied.Microcrystalline fiber powder was used to improve the problems of sample delamination and cracks during the preparation of sandstone type uranium ore samples.The changes of sample test results before and after replacing lining layers and adding auxiliary binder were compared.The precision(RSD,n=11)of 9 primary and secondary elements in sandstone uranium ore was 0.34%-4.8%,the accuracy of uranium was 0.93%-2.8%,and the accuracy of thorium was 0.80%-2.8%with the addition of 0.5 g microcrystalline cellulose as lining layer.The relative error of other major elements was 0.060%-5.5%.Compared with the values of boric acid lining and samples without auxiliary binder,the Grubbs method was used,and the statistical G of each element was between 1.2%-1.4%.There were no outliers and suspicious values in the experimental data.The use of hydroxymethyl cellulose as lining layer can be used for the determination of primary and secondary elements in sandstone type uranium ore,which reduces the powder generation in the sample analysis process and avoids the corrosion effect on the instrument metal parts.The addition of 0.5 g microcrystalline cellulose can improve the bonding property of the ore and improve the stability and standard rate of the sample prepared by the experiment.
作者
乔浩
王明力
邓长生
王斌堂
李鹏飞
QIAO Hao;WANG Mingli;DENG Changsheng;WANG Bintang;LI Pengfei(Geology Party No.216,CNNC,Urumqi,Xinjiang 830011,China)
出处
《中国无机分析化学》
CAS
北大核心
2024年第4期443-449,共7页
Chinese Journal of Inorganic Analytical Chemistry
基金
核工二一六大队2022年QC项目(QC216-2022-07)。
关键词
有机纤维素
粉末压片
X射线荧光光谱法
砂岩型铀矿
格拉布斯法
organic cellulose
powder lamination
X-ray fluorescence spectrometry
sandstone type uranium ore
Grubbs
