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中国无机分析化学:2018,8(6):58-63
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电感耦合等离子体原子发射光谱测定钒钛高炉渣中钪镓铬镍钴
梅毅
(成都市公安局刑警支队技术处化验室)
Determination of scandium gallium chromium nickel cobalt in the blast furnace slag of vanadium titanium magnetite by inductively coupled plasma atomic emission spectrometry
Mei Yi
(Chengdu Public Security Bureau Criminal Police Detachment Technical Office Laboratory)
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投稿时间:2018-06-26    修订日期:2018-07-19
中文摘要: 建立电感耦合等离子体原子发射光谱法(ICP-AES)同时测定钒钛高炉渣中0005%~0.3%的贵金属元素钪、镓、钴和0.0005%~0.6%铬、镍的检测方法。样品前处理方法采用氢氟酸、盐酸、硝酸和硫酸消解钒钛高炉渣,高温加热至硫酸分解产生三氧化硫浓白烟为此,直接以水稀释定容制备样品溶液,不仅快速完全消解高钛基样品,而且通过挥发除去高含量二氧化硅基体和反应残余的氢氟酸,减少溶液共存组分有效降低基体效应影响以及避免腐蚀检测仪器;而且依靠残余硫酸根与高钛基体络合生成硫酸氧钛离子,解决了高浓度钛基体在低酸度介质中易水解问题,无需补充加入大剂量酸以限制钛水解,直接以水稀释制备样品溶液,从而降低溶液酸度减少酸度效应影响。方法重点试验考察了钒钛高炉渣中钒钛铁钙镁铝等共存介质下基体效应、光谱干扰等干扰影响因素,优选了元素的分析谱线、背景校正区域以及光谱仪工作参数等检测条件,采用基体匹配和同步背景校正法消除基体效应影响。验证表明方法的技术性能指标:校准曲线相关系数>0.999,背景等效浓度0.0001%~0.0002%,元素检出限0.0001%~0.0002%,检测范围内RSD<15%,回收率90%~114%
中文关键词: ICP-AES  钒钛高炉渣            
Abstract:The analytical method that direct determination of the range from 0.0005%~0.300% scandium, gallium, cobalt and 0.0005%~0.600% chromium, nickel in the blast furnace slag of vanadium titanium magnetite by inductively coupled plasma atomic emission spectrometry was established. The blast furnace slag is digested with hydrofluoric acid, hydrochloric acid, nitric acid and sulfuric acid, it is heated at high temperature until sulfuric acid is decomposed to produce sulfur trioxide white smoke, and then the sample solution is prepared by directly diluting to volume with water. The method rapidly and completely dissipated the high titanium sample, and the high content of the silica matrix and the residual hydrofluoric acid were removed by volatilization, thus reducing the solution coexisting components and effectively reducing the matrix effect and avoiding corrosion detection instruments. At the same time, the high titanium matrix is complexed with sulfate to form titanium oxysulphate ion, which solves the problem of high-concentration titanium matrix easily hydrolyzed in low acidity media. Therefore, there is no need to add a large dose of acid to limit the hydrolysis of titanium, and the sample solution can be diluted directly with water to reduce the acidity of the solution and reduce the effect of acidity. That the influence of the spectral interferences and matrix effects in the high concentrations of titanium, iron, vanadium, aluminum, calcium and magnesium coexistence matrix system had been studied, and then the detection conditions of the elements such as analytical lines, background correction areas, and spectrometer operating parameters are optimized. The influence of substrate composition were eliminated by the matrix matching and synchronous background correction measures. The technical performance reached: the calibration curve correlation coefficient is >0.999, the background equivalent concentration is 0.0001% to 0.0002%, the element detection limit is 0.0001% to 0.0002%, and the RSD is <15% within the detection range, the recoveries were 90% ~ 114%.
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梅毅.电感耦合等离子体原子发射光谱测定钒钛高炉渣中钪镓铬镍钴[J].中国无机分析化学,2018,8(6):58-63.
Mei Yi.Determination of scandium gallium chromium nickel cobalt in the blast furnace slag of vanadium titanium magnetite by inductively coupled plasma atomic emission spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2018,8(6):58-63.

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