悬浮液直接进样ICP–OES法测定高纯氧化铝中的铁、钛、硅、铬

采用悬浮液直接进样电感耦合等离子体发射光谱法(ICP–OES)测定高纯氢氧化铝中铁、钛、硅、铬的含量。悬浮液用电磁搅拌器搅拌,均匀地分散在溶液中,通过仪器蠕动泵进入雾化室,均匀无阻地导入ICP光源。Fe,Ti,Si,Cr的分析谱线分别为259.940,336.112,251.611,205.552 nm;RF功率为1 300W,等离子体气流量为13.0 L/min,雾化器气体流量为0.60 L/min,辅助气流量为1.00 L/min。Fe,Ti,Si,Cr的质量浓度分别在0.0~30.0,0.0~15.0,0.0~90.0,0.0~15.0μg/m L范围内与信号强度呈良好的线性,线性相关系数均大于0.999,方法的检出限为0.027 6~0.993 9μg/m L,测量结果的相对标准偏差为0.65%~6.84%(n=11),回收率为95.0%~104.8%。该法抗干扰能力强、线性范围宽,适用于高纯氢氧化铝中铁、钛、硅、铬含量的分析。

Determination of Iron,Titanium, Silicon,Chromium in High Purity Alumina by Suspension Sampling Inductively Coupled Plasma Emission Spectrometry

Iron,titanium,silicon,chromium in high purity aluminum hydroxide were determined by direct suspension inductively coupled plasma emission spectrometry.After being stired with electromagnetic stirrer,dispersed in solution,suspension was pumped in the spray chamber by peristaltic pump,uniform access to import ICP light source.The analysis spectral lines of Fe,Ti,Si,Cr were 259.940,336.112,251.611,205.552 nm,respcctively.Instrument working parameters were as the follows:ICP power was 1 300 W,plasma gas flow rate was 13.0 L/min,nebulizer gas velocity was 0.60 L/min,and auxiliary gas flow rate was 1.00 L/min.The concentration ofFe,Ti,Si,Cr was linear with signal strength in the range of 0.0-30.0,0.0-15.0,0.0-90.0,0.0-15.0 μ g/mL,repectively.The relative standard deviation of detection results was 0.65％-6.84％(n=11),and the recovery was 95.0％-104.8％.The method has strong anti-interference ability and wide linear range,it is suitable for the analysis of iron,titanium,silicon,chromium content in high purity aluminum hydroxide.