The sample (1.000 0 g) of the high titanium vanadium slag was placed into a 250 mL beaker,and then the wall of the beaker was rinsed with 5 mL of water and the sample was dispersed.2.5 mL of HF,15 mL of HCl and 5 mL of HNO3 were added and the mixture was heated to boil to produce uniform large bubbles.5 mL of H2SO4 (1+1) solution was added,and then the solution was heated at high temperature to fumes of SO3 for 3-5 min.After cooling,15 mL of water was added and the solution was heated to boil.After cooling to room temperature,the solution was made its volume up to 100 mL with water.Inductively coupled plasma atomic emission spectrometry (ICP-AES) was used to determine 0.001％-3.0％ (w) chromium and 0.001％-0.300％ (w) of cobalt,nickel,gallium,scandium and zirconium in the above solution.Matrix matching and synchronous background correction were combined to eliminate the influence of matrix composition,and the analytical spectral lines,background correction region and the working parameters of spectrometer were selected.Detection limits (3s) of elements were in the range of 0.000 1％-0.000 2％,and values of RSDs (n=8) were all less than 25％.The samples were analyzed by the proposed metlhod,giving results in consistency with the results of ICP-MS.%高钛型钒渣样品1.000 0 g置于250 mL烧杯中,用水5 mL冲洗杯壁并分散样品,加入氢氟酸2.5 mL、盐酸15 mL和硝酸5 mL,加热煮沸反应至溶液产生均匀大气泡.加入硫酸(1+1)溶液5 mL,高温加热至产生三氧化硫浓白烟雾并保持3～5 min.冷却后,加入水15 mL煮沸,冷却至室温,用水定容至100mL.采用电感耦合等离子体原子发射光谱法(ICP-AES)测定所得溶液中0.001％～3.0％(质量分数)的铬和0.001％～0.300％(质量分数)的钴、镍、镓、钪、锆的含量.采用基体匹配和同步背景校正相结合方式消除基体组分影响,并且选择了待测元素的分析谱线、背景校正区域以及光谱仪工作参数等检测条件.各元素检出限(3s)为0.000 1％～0.000 2％,相对标准偏差(n=8)均小于25％.样品的本法测定结果与ICP-MS的测定结果一致.
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