微波消解-电感耦合等离子体原子发射光谱法测定废脱硝催化剂中钨和钛

Determination of tungsten and titanium in waste denitration catalyst by microwave digestion-inductively coupled plasma atomic emission spectrometry

选择酒石酸-氢氟酸-硝酸体系并利用微波消解处理样品,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定钨和钛,建立了微波消解-电感耦合等离子体原子发射光谱法测定废脱硝催化剂中钨和钛的方法。试验考察了消解体系及用量,优化了微波消解程序。结果表明,钨和钛的质量浓度分别为0.05~5mg/L和0.01~10mg/L与其相应的发射强度呈线性关系,相关系数分别为0.999 5、0.999 8,检出限分别为0.002%、0.000 2%。废脱硝催化剂中铁、铝、钙、镁、钒和钼等元素对钨和钛的测定无影响。方法用于废脱硝催化剂样品中钨和钛的测定,结果的相对标准偏差(RSD,n=6)均小于3%,并与原子吸收光谱法(AAS)测定值一致。

The waste denitration catalyst sample was treated by microwave digestion in tartaric acidhydrofluoric acid-nitric acid system.The content of tungsten and titanium was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The determination method of tungsten and titanium in waste denitration catalyst by ICP-AES was established after microwave digestion.The digestion system and the dosage were investigated to optimize the microwave digestion procedures.The results showed that the mass concentration of tungsten and titanium in range of 0.05-5 mg/L and 0.01-10 mg/L was linear to the corresponding emission intensity,respectively.The correlation coefficient was 0.999 5 and 0.999 8,and the detection limit was 0.002% and 0.000 2%,respectively.The coexisting elements in waste denitration catalyst including iron,aluminum,calcium,magnesium,vanadium and molybdenum had no influence on the determination of tungsten and titanium.The proposed method was applied to the determination of tungsten and titanium in waste denitration catalyst sample.The relative standard deviations(RSD,n=6)were less than 3%.The found results were consistent with those obtained by atomic absorption spectrometry(AAS).