重量法-电感耦合等离子体原子发射光谱法联用测定无取向硅钢磷酸盐体系环保涂层液中二氧化硅含量  

Determination of Silicon Dioxide Content in Environment-Friendly Coating Solution of Non-oriented Silicon Steel Phosphate System by Gravimetry Combined with Inductively Coupled Plasma Atomic Emission Spectrometry

作　　者：董礼男 张继明 赵希文 朱春要 DONG Linan;ZHANG Jiming;ZHAO Xiwen;ZHU Chunyao(Institute of Research of Iron and Steel,Jiangsu Province/Sha-Steel,Zhangjiagang,Jiangsu 215625,China)

机构地区：[1]江苏省(沙钢)钢铁研究院,江苏张家港215625

出　　处：《中国无机分析化学》2024年第5期600-606,共7页Chinese Journal of Inorganic Analytical Chemistry

摘　　要：二氧化硅是无取向硅钢环保涂层液的核心成分,其含量直接影响硅钢涂层的固化工艺及涂层产品的磁性能。因此为保证涂覆过程的顺利进行,对涂层液中二氧化硅含量的检测是十分必要的。通过在样品中分别加入硝酸、过氧化氢及高氯酸,置于电热板上进行消解处理,处理后的样品经酸溶、过滤步骤,以重量法计算沉淀中二氧化硅的含量,采用电感耦合等离子体原子发射光谱(ICP-AES)法测定滤液中可溶性硅含量,则样品中二氧化硅含量为重量法和电感耦合等离子体原子发射光谱法测定结果的合量。从而建立了重量法-电感耦合等离子体原子发射光谱法联用测定无取向硅钢磷酸盐体系环保涂层液中二氧化硅含量的方法。讨论了样品前处理用消解酸及消解温度、滤液中可溶性硅及含量、ICP-AES仪器检测时的元素干扰。结果表明,检测结果的相对标准偏差(RSD,n=12)在0.76%~1.1%,加标回收率在97.0%~104%。方法可广泛应用于各检测部门对无取向硅钢磷酸盐体系环保涂层液中二氧化硅含量的监控。Silicon dioxide is the core component of environmental-friendly coating solution of phosphate system for non-oriented silicon steel,and its content directly affects the curing process and the magnetic properties of coating products.Therefore,in order to ensure the quality of coating products,it is necessary to detect the silicon dioxide content in the coating solution.The sample was mixed with nitric acid,hydrogen peroxide and perchloric acid separately and then placed it on an electric heating plate for digestion.After the treated sample undergoes acid dissolution and filtration steps,the content of silicon dioxide in the precipitation was calculated by gravimetry,and the content of soluble silicon in the filtrate was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).Therefore,the content of silicon dioxide in the sample was the sum of the results determined by gravimetric method and ICP-AES.Thus,a method was established for silicon dioxide content determination in environment-friendly coating solution of phosphate system for non-oriented silicon steel by gravimetry combined with ICP-AES was established.The sample pretreatment digestion acid and temperature,soluble silicon and its content in the filtrate,and elemental interference during ICP-AES instrument detection were discussed.The results showed that the relative standard deviations(RSD,n=12)were 0.76% to 1.1%,and the recoveries were 97.0% to 104%.This method can be widely applied in various testing departments to monitor the silicon dioxide content in environment-friendly coating solution of phosphate system for non-oriented silicon steel.

关 键 词：重量法 电感耦合等离子体原子发射光谱法(ICP-AES) 无取向硅钢 磷酸盐体系 环保涂层液 二氧化硅 

分 类 号：O657.31[理学—分析化学]