中国有色冶金

Rapid and accurate detection of silicon and zirconium content in silicon-zirconium alloy is of great significance for production. The silicon content was determined by referring to the industry standard “Method for determination of potassium fluosilicate Content in export ferrosilicon” (SN/T 1014.1—2001)，For silicon-zirconium alloys with high zirconium content, it is difficult to react completely, and the measured results are low. The inductively coupled plasma atomic emission spectrometry is more suitable for the determination of trace or trace zirconium. However, the mass fraction of zirconium in silicon zirconium alloy is greater than 10% and the content range is wide, which is not suitable for this method.In this study, the silicon-zirconium alloy was dissolved with sulfuric acid, nitric acid, hydrochloric acid and hydrofluoric acid, and then the silicon was converted into fluorosilicate, and then the potassium fluorosilicate was precipitated with saturated potassium nitrate solution, and dissolved and precipitated with hot water. The hydrofluoric acid was titrated with sodium hydroxide standard solution, so as to measure the silicon content indirectly. Zircon alloy is dissolved in acid solution, zirconium and amygdalic acid form zirconium amygdalic acid precipitation, filtration, burning into zirconia, weighing, indirect conversion of zirconia content by zirconia content. The relative standard deviation (n=6) of silicon and zirconium content was 0.13%~1.39%, and the standard recovery of accuracy test was 96.20%~104.60%. The results show that the method has good precision and accuracy, and can meet the determination requirements of silicon and zirconium in silicon-zirconium alloy.