微波消解-微波等离子体原子发射光谱法测定石煤钒矿中钒

Microwave digestion microwave plasma atomic emission spectrometry Vanadium in stone coal vanadium ore

建立一种石煤钒矿试样经硝酸-氢氟酸-高氯酸三酸体系微波消解,微波等离子体原子发射光谱法(MP-AES)测定石煤钒矿中钒的方法。通过考察微波消解用酸试验条件,分析谱线和共存元素Al、Fe、K、Ca和Mg对测定钒的影响。结果表明:选用5.0 mL硝酸,3.0 mL氢氟酸,2.0 mL高氯酸进行试样处理,溶液清澈,钒溶出效果好;选择437.923 nm次灵敏度分析谱线,光谱干扰少;共存元素Al、Fe、K、Ca和Mg分别在浓度85μg/m L、35μg/mL、40μg/mL、35μg/mL和30μg/mL以下对测定钒基本无影响。钒在0.10～2.50%范围内的质量与相应的发射强度呈线性关系,线性相关系数为0.9999,检出限为0.6μg/g。该方法用于测定石煤钒矿中钒含量相对标准偏差RSD(n=10)均小于2%,具有较高的精密度和准确度。

The sample was treated in Nitric acid-Hydrofluoric acid-Perchloric acid system by microwave digestion, a method for the determination of vanadium in stone coal vanadium ores by microwave plasma atomic emission spectrometry （ MP-AES ） was established. The acid test conditions , Analysis of the influence of line and coexisting elements A1, Fe, K, Ca and Mg for microwave digestion were investigated on the determination of vanadium. The results show that the sample solution was clear and dissolving well with 5.0 mL Nitric acid, 3.0 mLHydrofluoric acid and 2.0mLPerchloric acid, the spectral line of 437.923 nm sensitivity analysis was selected with little spectral interference and the coexistence elements Al, Fe, K, Ca and Mg had no effect on the determination of vanadium in the following concentrations： 85 g/mL, 35 g/mL, 40 g/mL, 35 g/mLand 30 g/mL. The mass of vanadium in range of 0.00018-2.50% was linear to corresponding emission intensity with linear correlation coefficient of 0.9999, respectively .The linear correlation coefficient of vanadium between 0.10 and 2.50% was 0.99999, and the detection limit was 0.6 ptg/g. The method is appiled to the determination of vanadium in stone coal vanadium mine with relative standard deviation RSD （ n=10 ） less than 2%, which has high precision and accuracy.