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

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。本方法采用样品中分别加入硝酸、双氧水及高氯酸，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）仪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：按照本实验方法测定无取向硅钢磷酸盐体系环保涂层液中二氧化硅含量，检测结果的相对标准偏差（RSD，n=12）在0.76%~1.08%之间，加标回收率在97.00%~104.0%之间。该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。

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

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.At this method,the sample was mixed with nitric acid,hydrogen peroxide and perchloric acid by electric heating plate for digestion,after the treated sample is dissolved in acid and filtered,the content of silicon dioxide in the precipitation is calculated by gravimetry,and the content of soluble silicon in the filtrate is determined by inductively coupled plasma atomic emission spectrometry (ICP-AES),then the content of silicon dioxide in the sample is the sum of the results determined by gravimetric method and inductively coupled plasma emission spectrometry.The determination of silicon dioxide in environment-friendly coating solution of phosphate system for non-oriented silicon steel by gravimetry and combined with inductively coupled plasma atomic emission spectrometry was established.The sample pretreatment digestion acid and temperature,detection of soluble silicon and its content,elemental interference being discussed.The results show that under the method,detected the silicon dioxide content in the phosphate system environmentally friendly coating solution of non-oriented silicon steel,the relative standard deviations(RSD,n=12) were 0.76% to 1.08%,and the recoveries were 97.00% to 104.0%.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.