Determination of chromium,iron,silicon and manganese in high-carbon ferrochrome by X-ray fluorescence spectrometry with fusion sample preparation
In order to solve the corrosion problem of platinum crucible by the reducing substances in ferro-chrome sample during high temperature fusion,the following experiment conditions were adopted:under the temperature of 600-850 ℃,the sample with carbon loss correction,the special oxidizing agent for chro-mium alloy and anhydrous lithium metaborate were mixed,and the high-carbon ferrochrome sample was oxidized in the ceramic crucible with graphite powder as the base by temperature programming;after oxi-dation,sodium hexametaphosphate and anhydrous lithium metaborate were used as the flux,and 1-3 mL of 300 g/L ammonium bromide solution were added as the release agent;the mixture was melted in electric melting furnace at 1 050 ℃ for 20 min to prepare the glass pellet,which was then determined by X-ray flu-orescence spectrometry.Consequently,a determination method of chromium,iron,silicon and manganese in high-carbon ferrochrome was established.The lower limits of determination for silicon and manganese were 44.51 μg/g and 22.62 μg/g,respectively.The precision tests showed that the relative standard devi-ations(RSD,n=12)of determination results for chromium,iron,silicon and manganese were 0.44％,0.51％,2.1％and 4.8％,respectively.The trueness tests showed that the errors between the measured values of chromium,iron,silicon and manganese in certified reference materials of high carbon ferro-chrome and the standard values could be controlled within the allowable deviation ranges specified in GB/T 4699.2-2008,GB/T 5687.13-2021,GB/T 5687.2-2007 and GB/T 5687.10-2006,respectively.According to the proposed technical scheme,the determination results of chromium,iron,silicon,and manganese in high carbon ferrochrome could meet the routine detection requirements of high-carbon ferrochrome sam-ples.
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