电感耦合等离子体原子发射光谱(ICP-AES)法测定铸造用硅砂中的Fe_2O_3、Al_2O_3、CaO、MgO、TiO_2、K_2O、Na_2O
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摘要
建立了电感耦合等离子体原子发射光谱(ICP-AES)法测定铸造用硅砂中Fe_2O_3、Al_2O_3、CaO、MgO、TiO_2、K_2O、Na_2O的方法。研究了溶样方法的选择优化,采用硝酸、氢氟酸溶样,冒高氯酸处理,通过元素分析线的选择,基体和共存元素影响的消除,在最佳的仪器分析条件下得出了方法的线性范围、相关系数及检出限。用硅砂3个梯度含量的标准物质的分析结果评价方法的准确度和精密度。方法的检出限Fe为0.012μg/mL、Al为0.032μg/mL、Ca为0.27μg/mL、Mg为0.003 2μg/mL、Ti为0.002 1μg/mL、K为0.16μg/mL,Na为0.000 44μg/mL。5次数据的相对标准偏差说明方法稳定性较好。方法适用于铸造用硅砂中Fe_2O_3、Al_2O_3、CaO、MgO、TiO_2、K_2O、Na_2O含量的测定。
A method for the determination of iron oxide,aluminum oxide,calcium oxide,magnesium oxide,titanium oxide,potassium oxide and sodium oxide in foundry silica sand by inductively coupled plasma atomic emission spectrometry was established.The selection and optimization of the dissolution method were studied.The linear range of the method,correlation coefficient and detection limit was determined under the optimal instrumental analysis,using nitric acid,hydrofluoric acid treatment,perchloric acid treatment,elemental analysis line selection,matrix and coexisting elements.The accuracy and precision of the method were evaluated by using the analytical results of three grades of silica sand.The detection limit of iron Fe is 0.012μg/mL,Al is 0.032μg/mL,Ca is 0.27μg/mL,Mg is 0.003 2μg/mL,Ti is 0.002 1μg/mL,K is 0.16μg/mL,Na is 0.000 44μg/mL.The relative standard deviation of the data of 5 times indicates that the method has good stability.The method is suitable for the determination of the content of iron oxide,aluminum oxide,calcium oxide,magnesium oxide,titanium oxide,potassium oxide and sodium oxide in the silica sand for casting.
A method for the determination of iron oxide,aluminum oxide,calcium oxide,magnesium oxide,titanium oxide,potassium oxide and sodium oxide in foundry silica sand by inductively coupled plasma atomic emission spectrometry was established.The selection and optimization of the dissolution method were studied.The linear range of the method,correlation coefficient and detection limit was determined under the optimal instrumental analysis,using nitric acid,hydrofluoric acid treatment,perchloric acid treatment,elemental analysis line selection,matrix and coexisting elements.The accuracy and precision of the method were evaluated by using the analytical results of three grades of silica sand.The detection limit of iron Fe is 0.012μg/mL,Al is 0.032μg/mL,Ca is 0.27μg/mL,Mg is 0.003 2μg/mL,Ti is 0.002 1μg/mL,K is 0.16μg/mL,Na is 0.000 44μg/mL.The relative standard deviation of the data of 5 times indicates that the method has good stability.The method is suitable for the determination of the content of iron oxide,aluminum oxide,calcium oxide,magnesium oxide,titanium oxide,potassium oxide and sodium oxide in the silica sand for casting.
引文
[1]中国国家标准化管理委员会.铸造用硅砂化学分析方法:GB/T 7143-2010[S].北京:中国标准出版社,2010.
[2]李欣.铬天青S分光光度法分析硅砂铝含量[J].化工中间体(Chemical Intermediates),2015,11(04):73-75.
[3]杨斌,胡向平,何蓉.电感耦合等离子体原子发射光谱(ICP-AES)法测定H-ZF类光学玻璃中锑含量[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2018,8(6):21-24.
[4]杨雪梅.X射线荧光光谱法测定硅砂中杂质元素[J].理化检验(化学分册)(Physical Testing and Chemical Analysis Part B(Chemical Analysis)),2008,44(6):538-539.
[5]刘亚亮.应用六西格玛方法对B公司进行可靠性试验项目的研究[D].北京:中国科学院大学,2014.
[2]李欣.铬天青S分光光度法分析硅砂铝含量[J].化工中间体(Chemical Intermediates),2015,11(04):73-75.
[3]杨斌,胡向平,何蓉.电感耦合等离子体原子发射光谱(ICP-AES)法测定H-ZF类光学玻璃中锑含量[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2018,8(6):21-24.
[4]杨雪梅.X射线荧光光谱法测定硅砂中杂质元素[J].理化检验(化学分册)(Physical Testing and Chemical Analysis Part B(Chemical Analysis)),2008,44(6):538-539.
[5]刘亚亮.应用六西格玛方法对B公司进行可靠性试验项目的研究[D].北京:中国科学院大学,2014.