Abstract：Conventional pressed powder sample preparation is a simple, efficient and environmentally friendly technique. However, when it is applied for the preparation of cobalt-rich crust samples, there are some problems, for example, the surface is rough and the powders easily fall off. The application of high-pressure powder pelleting preparation for cobalt-rich crust samples was explored in experiments. The analysis method of twenty components (Na2O, MgO, Al2O3, SiO2, P2O5, K2O, CaO, TiO2, Mn, Fe, Co, Ni, Cu, Zn, V, Sr, Zr, Ba, Pb and Y) in cobalt-rich crust samples by X-ray fluorescence spectrometry (XRF) was established. High-pressure sample preparation system was used, and the sample preparation effect and analysis performance of pressed pellets under different pressures (300 kN and 600 kN) were discussed. The results showed that the powder pellet pressed at 600 kN was dense and smooth without cracks and powder dropping. The reproducibility of sample preparation and the precision of determination were greatly improved. Certified reference materials of crusts and nodules, crust samples certified by other methods were applied to prepare the calibration curves. The actual samples were determined for 12 times, and the limits of detection were between 2.45 μg/g and 2 026 μg/g. The results of precision test indicated that the relative standard deviations (RSD, n=7) were between 0.22% and 0.91%. The proposed method was applied for the analysis of actual cobalt-rich crust samples. The found results were consistent with those obtained by other methods. The proposed method could meet the requirements of accurate determination of multiple components in cobalt-rich crust samples.
林庆文,杨俊,刘玉纯.波长色散-X射线荧光光谱法测定土地质量地球化学评估样品中24种主次痕量元素[J].理化检验(化学分册),2019,55(5):565-570.LIN Qingwen,YANG Jun,LIU Yuchun.Determination of 24 major,minor and trace elements in samples for land quality geochemical assessment by wavelength dispersive X-ray fluorescence spectrometry[J].Physical Testing and Chemical Analysis (Part B: Chemical Analysis),2019,55(5):565-570.
[2]
曾江萍,郑智慷,张楠,等.粉末压片制样-X 射线荧光光谱法测定锂云母中铷、铯及主量组分[J].冶金分析,2019,39(10):73-77.ZENG Jiangping,ZHENG Zhikang,ZHANG Nan,et al.Determination of rubidium,cesium and major components in lithium mica by X-ray fluorescence spectrometry with pressed powder pellet[J].Metallurgical Analysis,2019,39(10):73-77.
[3]
郑小敏,於利慧.熔融制样-X射线荧光光谱法测定酸溶性钛渣中主次量成分[J].冶金分析,2019,39(11):16-23.ZHENG Xiaomin,YU Lihui.Determination of major and minor components in acid-soluble titanium slag by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2019,39(11):16-23.
[4]
张勤,于兆水,李小莉,等.X射线荧光光谱高压制样方法和技术研究[J].光谱学与光谱分析,2013,33(12):3402-3407.ZHANG Qin,YU Zhaoshui,LI Xiaoli,et al.Study on high pressure sample preparation method for pressed powder pellet and its application in X-ray fluorescence spectrum analysis[J].Spectroscopy and Spectral Analysis,2013,33(12):3402-3407.
[5]
李小莉,安树清,于兆水,等.高压制样X-射线荧光光谱法测定煤样品中17种元素和灰分[J].分析化学,2014,42(2):283-287.LI Xiaoli,AN Shuqing,YU Zhaoshui,et al.Determination multi-elements and ash in coal sample by X-ray fluorescence spectrometer with high pressure pelletised sample[J].Chinese Journal of Analytical Chemistry,2014,42(2):283-287.
[6]
LI Xiaoli,AN Shuqing,LIU Yaxuan,et al.Investigation of a high-pressure pressed powder pellet technique for the analysis of coal by wavelength dispersive X-ray fluorescence spectroscopy[J].Applied Radiation and Isotopes,2018,132:170-177.
[7]
于兆水,张勤,李小莉,等.高压粉末制样波长色散X射线荧光光谱法测定生物样品中23种元素[J].岩矿测试,2014,33(6):844-848.YU Zhaoshui,ZHANG Qin,LI Xiaoli,et al.Determination of 23 elements in biological samples by wavelength dispersion X-ray fluorescence spectrometry with high pressure powder pelleting preparation[J].Rock and Mineral Analysis,2014,33(6):844-848.
[8]
于兆水,陈海杰,张雪梅,等.高压粉末制样-偏振能量色散X射线荧光光谱法测定生物样品中24种元素[J].理化检验(化学分册),2015,51(11):1594-1597.YU Zhaoshui,CHEN Haijie,ZHANG Xuemei,et al.Determination of 24 elements in biological samples by polarized energy dispersive X-ray fluorescence spectrometry[J].Physical Testing and Chemical Analysis (Part B: Chemical Analysis),2015,51(11):1594-1597.
[9]
韦振权,何高文,邓希光,等.大洋富钴结壳资源调查与研究进展[J].中国地质,2017,44(3):460-472.WEI Zhenquan,HE Gaowen,DENG Xiguang,et al.The progress in the study and survey of oceanic cobalt-rich crust resources[J].Geology in China,2017,44(3): 460-472.
[10]
高晶晶,刘季花,张辉,等.太平洋海山富钴结壳中铂族元素赋存状态与富集机理[J].海洋学报,2019,41(8):115-124.GAO Jingjing,LIU Jihua,ZHANG Hui,et al.Occurrence phase and enrichment mechanism of platinum group elements in the Pacific cobalt-rich crusts[J].Haiyang Xuebao,2019,41(8):115-124.
[11]
赵宏樵,曾江宁,俞元挺,等.富钴结壳主要成分的X荧光快速测定[J].海洋学研究,2005,23(2):17-23.ZHAO Hongqiao,ZENG Jiangning,YU Yuanting,et al.An XRFS method for rapidly analyzing main elements in cobalt-enriched crusts[J].Journal of Marine Sciences,2005,23(2):17-23.
[12]
李强,张学华.手持式X 射线荧光光谱仪测定富钴结壳样品中锰铁钴镍铜锌[J].岩矿测试,2013,32(5):724-728.LI Qiang,ZHANG Xuehua.Determination of Mn,Fe,Co,Ni,Cu and Zn in cobalt-rich crusts by portable X-ray fluorescence spectrometer[J].Rock and Mineral Analysis,2013,32(5):724-728.
[13]
李强,张学华.粉末压片-X射线荧光光谱法快速分析多金属结核和富钴结壳中22种组分[J].冶金分析,2014,34(1):28-33.LI Qiang,ZHANG Xuehua.Rapid determination of twenty-two components in polymetallic nodule and cobalt-rich crusts by X-ray fluorescence spectrometry with pressed powder pellet[J].Metallurgical Analysis,2014,34(1):28-33.
