微波消解–电感耦合等离子体原子发射光谱法测定钨矿石中钨

Determination of tungsten in tungsten ore by inductively coupled plasma atomic emission spectrometry with microwave digestion

建立微波消解–电感耦合等离子体原子发射光谱测定钨矿石中钨的方法。以氢氧化钠溶液为消解试剂,按设定的消解条件对样品进行消解,消解完成后,加入盐酸和酒石酸,定容于25 mL,用电感耦合等离子体原子发射光谱法测定钨含量。钨的质量浓度在0~50 mg/L范围内与光谱强度线性关系良好,相关系数为0.9998,方法检出限为0.0024%。用所建方法对5个标准物质样品进行测定,测定值与标称值的相对偏差为–1.33%~2.73%,测定结果的相对标准偏差不大于3.07%(n=5)。该方法简便快速,准确可靠,绿色环保,适应于钨矿石中钨的测定。

A method for the determination of tungsten in tungsten ore by microwave digestion–inductively coupled plasma atomic emission spectrometry was established.The sample was digested with sodium hydroxide solution under programmed temperature elevation mode.After digestion,hydrochloric acid and tartaric acid were added before diluted to 25 mL,the tungsten content was determined by inductively coupled plasma atomic emission spectrometry.The mass concentration of tungsten had a good linear relationship with the spectral intensity in the range of 0–50 mg/L with the correlation coefficient of 0.9998,and the detection limit was 0.0024%.The method was applied to the determination of 5 reference materials,the relative deviation between the measured value and the certified value was–1.33%–2.73%,and the relative standard deviation of the determination results was less than 3.07%(n=5).The method is simple,rapid,accurate,reliable and green environmental protection,which is suitable for the determination of tungsten in tungsten ores.