熔融制样-X射线荧光光谱法测定高碳铬铁中铬铁硅锰  

Determination of chromium,iron,silicon and manganese in high-carbon ferrochrome by X-ray fluorescence spectrometry with fusion sample preparation

作　　者：滕广清 侯钢铁 张改梅 鲍希波 TENG Guangqing;HOU Gangtie;ZHANG Gaimei;BAO Xibo(HBIS Group Hansteel Company Technology Center,Handan 056003,China)

机构地区：[1]河钢集团邯钢公司技术中心,河北邯郸056003

出　　处：《冶金分析》2024年第3期23-29,共7页Metallurgical Analysis

摘　　要：为解决高温熔融时铬铁试样中还原性物质对铂-金坩埚的侵蚀问题,实验确定在600~850℃条件下,以经碳烧失校正的试样、铬系合金专用氧化剂、无水偏硼酸锂混匀后,在石墨粉垫底陶瓷坩埚内程序升温氧化高碳铬铁试样,氧化后用六偏磷酸钠和无水偏硼酸锂作为熔剂,滴加1~3 mL 300 g/L溴化铵溶液作为脱模剂,在1050℃电热熔样炉中熔融20 min,制得玻璃样片,采用X射线荧光光谱法对玻璃样片进行测定。最终,建立了高碳铬铁中铬、铁、硅、锰含量的测定方法。硅和锰检测下限分别为44.51μg/g和22.62μg/g。精密度试验表明,高碳铬铁试样中铬、铁、硅、锰测定结果的相对标准偏差(RSD,n=12)分别为0.44%、0.51%、2.1%、4.8%;正确度试验表明,高碳铬铁合金标准样品中铬、铁、硅、锰的测定值与标准值间的误差,分别控制在GB/T 4699.2—2008、GB/T 5687.13—2021、GB/T 5687.2—2007和GB/T 5687.10—2006规定的允许差范围内。按照实验技术方案测定高碳铬铁中铬、铁、硅、锰含量,能够满足高碳铬铁试样的常规检测需求。In order to solve the corrosion problem of platinum crucible by the reducing substances in ferrochrome 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 chromium 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 oxidation,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 1050℃for 20 min to prepare the glass pellet,which was then determined by X-ray fluorescence 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 44.51μg/g and 22.62μg/g,respectively.The precision tests showed that the relative standard deviations(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 ferrochrome 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 samples.

关 键 词：熔融制样 X射线荧光光谱法(XRF) 高碳铬铁 铬 铁 硅 锰 陶瓷坩埚 预氧化 石墨粉 

分 类 号：O657.34[理学—分析化学] TF031[理学—化学]