碱熔-氟硅酸钾滴定法测定复合脱氧剂中硅  

Determination of silicon in complex deoxidizer by alkali fusion-potassium fluosilicate titration

作　　者：张丽伟 高立红[1,2] 权龙海 徐艳艳 王晓佳 ZHANG Liwei;GAO Lihong;QUAN Longhai;XU Yanyan;WANG Xiaojia(Baotou Research Institute of Rare Earths,Baotou 014030,China;Ruike National Engineering Research Center for Rare Earth Metallurgy and Functional Materials,Baotou 014030,China)

机构地区：[1]包头稀土研究院,内蒙古包头014030 [2]稀土冶金及功能材料国家工程研究中心,内蒙古包头014030

出　　处：《冶金分析》2024年第4期73-78,共6页Metallurgical Analysis

摘　　要：快速、准确测定炼钢用复合脱氧剂(成分复杂)中硅含量对于有效控制炼钢技术和产品质量具有重要意义。样品分解采用混合熔剂氢氧化钾和过氧化钠进行碱熔,碱熔温度850℃,碱熔时间为15 min,加入15 mL硝酸、50 mL热水浸取熔融物,加过氧化氢掩蔽钛元素,加入氟化钾生成氟硅酸钾沉淀。经过15 min陈化,向过滤后沉淀中加入热水,分解成氢氟酸,用氢氧化钠标准溶液进行滴定,建立了碱熔-氟硅酸钾滴定法测定复合脱氧剂中硅的方法。按照实验方法测定4个复合脱氧剂中硅,结果的相对标准偏差(RSD,n=6)为0.15%~0.25%;加标回收率为99.3%~99.7%。The rapid and accurate determination of silicon content in complex deoxidizer for steelmaking(the components are complicated)is of great significance for the effective control of steelmaking technology and product quality.The sample was decomposed by alkali fusion with mixed flux of potassium hydroxide and sodium peroxide.The alkali fusion temperature was 850℃,and the fusion time was 15 min.The molten material was leached with 15 mL of HNO_(3) and 50 mL of hot water.Hydrogen peroxide was added to mask titanium.Potassium fluosilicate precipitation was formed by adding potassium fluoride.After aging for 15 min,hot water was added in the precipitation.Hydrofluoric acid was generated and titrated with sodium hydroxide standard solution.The method for the determination of silicon in complex deoxidizer by alkali fusion-potassium fluosilicate titration was established.The contents of silicon in four samples of complex deoxidizer were determined according to the experimental method.The relative standard deviations(RSD,n=6)were between 0.15% and 0.25%,and the recoveries were between 99.3% and 99.7%.

关 键 词：复合脱氧剂 氟硅酸钾 滴定法 碱熔融 硅 

分 类 号：O655.2[理学—分析化学] TF713.5[理学—化学]