Determination of titanium,tungsten,cobalt,niobium,nickel,molybdenum in Ti(C,N) based cermets by X-ray fluorescence spectrometry with fusion sample preparation
JIANG Jia-lu
China National R&D Center for Tungsten Technology,Xiamen Tungsten Co.,Ltd.,Technology Center,Xiamen 361009,China
Abstract：There are rare reports about the determination of Ti (C, N) in cermets by X-ray fluorescence spectrometry(XRF). Ti (C, N) based cermets sample was pretreated through acid dissolution and low temperature drying, and then prepared by fusion sample preparation method. Artificially-prepared oxide standard sample was used for establishing calibration curve of X-ray fluorescence spectrometric analysis, so that rapid qualitative determination for Ti, W, Co, Nb, Ni, Mo of cermets was achieved with internal standard method. Two pretreatment methods of pre-oxidation and acid dissolution were compared in the experiment, which found that the mass-loss of W and Mo during high temperature fusion could be avoided by acid dissolving, drying, and smelting. With 7.72 g of mixed flux [m(Li2B4O7)∶m(LiBO2)=67∶33], 0.7 g of auxiliary oxidant NH4NO3, 8 drops of 150 g/L release agent LiBr solution, uniform fuse piece could be produced at the fusion temperature of 1 100 ℃ and the fusion time of 190 s. Two groups of samples (0.12-0.25 g, 0.08-0.23 g) were weighed for contrast test. Through varying sample mass to enlarge matrix effect, the influence of the parameters on the test results could be directly observed, so that the optimum parameters could be selected with the least experiment times. Using Ta as internal standard, the precision could be improved significantly without normalizing the results. For Co and Ni, Ta-Lα spectral line was better for correction; for W and Nb, Ta-Lβ1 spectral line was better. Results precision was tested with samples prepared by internal and non-internal standard methods. The results showed that the relative standard deviation of internal standard method was RSD<1.0%, while that of non-internal standard method was RSD<2.5%. Ti (C,N)-based cermets samples of different formula were used for testing trueness, and the measured values are consistent with the reference values.
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