熔融制样-X射线荧光光谱法测定氮化硅锰中主次组分

Silicon-manganese nitride is a new type of raw material for nitriding in steelmaking. At present, the contents of silicon, manganese, phosphorus and iron are usually analyzed by wet chemical method. The experimental procedures are relatively time-consuming and the operation is relatively tedious. The determination method of silicon, manganese, phosphorus and iron in silicon-manganese nitride by X-ray fluorescence (XRF) was established using lithium carbonate as oxidant, lithium tetraborate as flux and ammonium bromide as release agent. The influence of loss on ignition (LOI) was considered during the preparation of calibration curve. The linear range of calibration curve was extended by adding pure materials (such as SiO₂ and Fe₂O₃) into the standard sample of ferromanganese-silicon. Experiments showed that the prepared glass beads had smooth surface without gas pores under the following conditions: the dilution ratio was 1:20; the mixture was fused in a melting furnace at 1 150 ℃ for 8 min. Meanwhile, there were no residues for carbon and nitrogen. The precision results showed that the relative standard deviations (RSD, n=10) of Si, Mn, P and Fe were between 0.36% and 2.3%. Three samples were determined according to the experimental method, and the found results were consistent with those obtained by wet chemical method in national standard method.