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Determination of chromium cobalt nickel gallium niobium scandium and zirconium in the blast furnace slag of vanadium titanium magnetite by inductively coupled plasma atomic emission spectrometry

机译:电感耦合等离子体原子发射光谱法测定钒钛磁铁高炉炉渣中钴镍镓铌钪和锆的测定

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In order to recover the precious metal elements in vanadium-titanium blast furnace slag, the analytical method that direct determination of the range from 0.001%~0.300% chromium, cobalt nickel, gallium, niobium, scandium and zirconium in the blast furnace slag of vanadium titanium magnetite by inductively coupled plasma atomic emission spectrometry was established. Sample digestion reagent consists of hydrofluoric acid, hydrochloric acid, nitric acid and sulfuric acid, and their ratio, dosage and reaction control condition are all optimized, so make sure that the blast furnace slag of vanadium titanium magnetite can be quickly completely digested. At the same time, the high content of silicon dioxide can be removed by volatilization to simplify the sample solution matrix composition, and because of the titanium ion and sulfate ion complex reaction generating oxygen titanium sulfate ion so as to solve the high concentration of titanium matrix easy hydrolysis problem in low acidity medium, thus it greatly reduce the acidity of sample solution to reduce the matrix effect. 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, then the test results are classified summary. The influence of substrate composition were eliminated by the matrix matching and synchronous background correction measures, and then the analytical lines, the background correction areas and working conditions of the spectrometer are all optimized according to the spectral interference test. The technical performance reached: calibration curve correlation coefficient of 0.998 or higher, detection limit of element is 0.0001%-0.0003% and the measuring elements content in lower 0.0003% ~ 0.0009%, RSD is less than 15% when the element content in the range from 0.001% to 0.05%, the actual sample testing results are consistent with ICP-MS.
机译:为了回收钒 - 钛高炉渣中的贵金属元素,分析方法直接测定钒高炉炉渣中的0.001%〜0.300%铬,钴镍,镓,铌,钪和锆的范围通过电感耦合等离子体原子发射光谱法建立了钛磁铁矿。样品消化试剂由氢氟酸,盐酸,硝酸和硫酸组成,它们的比例,剂量和反应控制条件全部优化,因此可以肯定可以快速完全消化钒钛磁铁矿的高炉炉渣。同时,可以通过挥发除去二氧化硅的高含量,以简化样品溶液基质组合物,并且由于钛离子和硫酸盐离子复合反应产生氧钛硫酸钛离子,以解决高浓度的钛基质低酸度介质中易于水解问题,从而大大降低了样品溶液的酸度,以降低基质效应。研究了光谱干扰和基质效应在高浓度的钛,铁,钒,铝,钙和镁共存基质系统中的影响,然后测试结果是分类概要。通过基质匹配和同步背景校正测量消除了基板组合物的影响,然后通过分析线,光谱仪的背景校正区域和工作条件根据光谱干扰测试进行优化。技术性能达到:校准曲线相关系数为0.998或更高,元素的检测极限为0.0001%-0.0003%,测量元素含量下降0.0003%〜0.0009%,RSD在范围内的元素含量时小于15%从0.001%到0.05%,实际样品测试结果与ICP-MS一致。

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