| As agricultural production material of potassium manure, sylvine is one of the scarce bulk strategic mineral resources in China. And the demand of breakthrough in sylvine mine exploration is urgent. Most of China’s domestic potash deposits locates in remote areas of western and southern mountain areas, and these sparsely populated areas, long distances, make it take not only a lot of time, but also the consumption of human, material and financial resources from sample collection to obtain analytical data. At the same time, most of these areas are plateau areas, where the field work cycle is short. Some problems that need to be on-site decision-making can’t get timely data support, which greatly affect the efficiency and effectiveness of the prospecting work. Therefore, it is urgent to study and develop the rapid analysis technique.The usual analytical method of potassium salt mainly including Inductively Coupled Plasma Mass Spectrometry, Atomic Emission Spectrometry, Atomic Absorption Spectroscopy, Flame Spectrometry and so on. And those large-scale instrument are all need support and requirement such as the gas, carrier gas and combustion-supporting gas. Some traditional analytical chemistry method of potassium salt include gravimetric method, volumetric method, electrochemical method etc. But its operation is complicated and the method have long determining period. Thus, the above analytical methods can’t suitable for on-site rapid analysis.Energy dispersive X-ray fluorescence(EDXRF) spectroscopy has a lot of advantages such as compact structure, small volume, great adaptability of environment, multielement analysis, high sensitivity, high speed, can direct analyze solid samples and liquid samples and so on, and it has been successfully applied in the resources exploration. A new analytical techniques, solution cathode atmospheric glow discharge(SCGD) spectrum, will remedy the defect that XRF can’t analyse the Li. And the instrument that combined with charge coupled device(CCD) would be portable. In this paper, based on EDXRF and SCGD-CCD, the on-site analytical method has been developed and applied to analyse K、Br、Rb、Sr in potassium drilling fluid development and application. And the rapid analysis method of Li in spodumene samples has been studied and developed.1) For satisfying the demand of rapidly analysed indicator elements including K、Br、R、 Sr in potassium drilling fluid, the analytical method of K、Br、Rb、Sr in liquid samples has been established with the energy dispersive X-ray fluorescence(EDXRF) Spectro XEPOS spectrometry instruments. The correlation coefficient of the standard curve of four elements were greater than 0.9982, the linear ranges of K are about 50-4000μg/mL, the linear ranges of Rb are about 2-150μg/mL, linear ranges of Br and Sr are both 1～200μg/mL, the relative standard deviation of method greater than 1.28%, the recoveries are 86.58% ～98.06%. And the method is suitable for analysed brine or drilling fluid sample. The analytical method were utilized for on-site analysis of drilling fluid sample from sylvite well that were depth of 200m-800m in Jiangling. The results of the sample measurement are basically consistent with the data that were ICP-AES measured. The filtration and motionless stand for obtaining supernatant liquor of mud were compared and the compared results indicates that both treatment of drilling fluid can get consistent analytical results. The concentration change of four elements in the mud samples and the corresponding depth debris samples were compared and the experimental data show that drilling mud can effectively reflect the trend of the composition of rock to providing technical support for drilling decisions.2) The analytical method of Li、K、Br、Rb、Cs has been established with portable solution cathode atmospheric glow discharge charge coupled device(SCGD-CCD) that was researched and developed by project group. The paper discussed the influence of instrument parameter such as integral time and gains etc and determined the optimal experimental conditions. The correlation coefficient of the standard curve of four elements were greater than 0.9973, the detection limit of K、Li are about 0.03μg/mL, the detection limit of Rb about 0.57μg/mL, the detection limit of Cs about 0.55μg/mL. We have detected Li and K in spodumene samples that dissolved by ammonium bifluoride and found the results were seriously affected by matrix effect of sample solution. And the accuracy of analysis results have been greatly improved by using the standard addition method and have consistency with ICP-AES data. At present, no literatures that solution cathode atmospheric glow discharge charge spectrometry analyzed spodumene samples have been report. The analytical method can be applied to analyze spodumene samples in the field and can extend to analyze Li in brine samples analysis. |
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