ABSTRACT
A rapid multi-element analysis method for clay mineral samples was described. This method utilized a polarized wave-length dispersive X-ray fluorescence spectrometer--Axios PW4400, which had a maximum tube power of 4 000 watts. The method was developed for the determination of As, Mn, Co, Cu, Cr, Dy, Ga, Mo, P, Pb, Rb, S, Sr, Ni, ,Cs, Ta, Th, Ti, U, V, Y, Zn, Zr, MgO, K2O, Na2O, CaO, Fe2O3, Al2O3, SiO2 and so on. Thirty elements in clay mineral species were measured by X-ray fluorescence spectrometry with pressed powder pellets. Spectral interferences, in particular the indirect interferences of each element, were studied. A method to distinguish the interference between each other periodic elements in element periodic table was put forward. The measuring conditions and existence were mainly investigated, and the selected background position as well as corrected spectral overlap for the trace elements were also discussed. It was found that the indirect spectral overlap line was the same important as direct spectral overlap line. Due to inducing the effect of indirect spectral overlap, some elements jlike Bi, Sn, W which do not need analysis were also added to the elements channel. The relative standard deviation (RSD) was in the range of 0.01% to 5.45% except three elements Mo, Cs and Ta. The detection limits, precisions and accuracies for most elements using this method can meet the requirements of sample analysis in clay mineral species.
ABSTRACT
In the present paper a method for the determination of strontium, barium, calcium, magnesium, silicon, iron, aluminum and sulfur in the product of strontium carbonate by X-ray fluorescence spectrometry with pressed powder sample preparation was developed, and the standard samples were synthesized by high purity reagent. As the contents of strontium in the product of strontium carbonate were very high, the phenomenon of spectrum-peak-saturated occurred and the count rate was overflowed according to the measuring condition which was automatically given by the software system of X-ray fluorescence spectrometry. As a result, the deviation of the measurement is greater. According to analyzing the measuring condition of strontium, a method was given for reducing the count rate by reducing the measuring power of strontium, thus achieving the goal of measurement. When sulfate was measured with pressed powder sample, the results were enhanced with the increase in measuring number. In light of this situation, a method was proposed to solve the problem. As the self-forming characteristic of the product of strontium carbonate was not so well, it was very difficult to press the sample successfully. So, the condition of squash method involving the kinds of the adhesives, the mixing technique with powder sample and the pressing-time technique was discussed. During making the sample, it was found that the effects of pellet formation were better if the time could be delayed by 120 seconds. Matrix effect was corrected by alpha coefficient method, the accuracy of the method was evaluated by analysis of synthetic sample. Detection limits of 0.623-107.6 mg x g(-1) were obtained. The results were in good agreement with certified values with precision of < 2.5% RSD.
