微波消解-火焰原子吸收光谱法测定磷矿石中铅

来源期刊：冶金分析2010年第10期

论文作者：刘国文 王旭刚 崔东胜 龚福忠

文章页码：54 - 57

关键词：磷矿石； 微波消解； 铅； 火焰原子吸收光谱法

Key words：phosphate ore； microwave digestion； lead； flame atomic absorption spectrometry

摘    要：采用微波消解技术对磷矿石样品进行预处理,确定了溶样酸介质及其用量、微波消解压力、时间等关键因素,建立了火焰原子吸收光谱法测定磷矿石中铅的方法。实验结果表明,在盐酸、硝酸、硫酸、王水等四种溶样介质中,以王水的溶样效果最好,其适宜用量为每克样品5 mL。采用3步的微波消解程序,消解压力/消解时间依次为:0.3 MPa/60 s,0.5 MPa/360s,1.0 MPa/180 s。与传统酸溶法相比,微波消解的溶样时间短,试样溶解完全。方法的检出限为0.036μg/mL。对磷矿石样品进行分析,相对标准偏差(RSD)在4.1%~6.6%之间,加标回收率为94%~108%。

Abstract: The phosphate ore samples were pretreated by microwave digestion technique.The key factors such as acid medium,dosage,and the pressure and time of microwave digestion were investigated.Consequently,a determination method of lead in phosphate ore by flame atomic absorption spectrometry was established.The results indicated that in four acid mediums(hydrochloric acid,nitric acid,sulfuric acid and aqua regia),the sample dissolving effect in aqua regia was the best. Its proper dosage is 5 mL per grammes.The three-step microwave digestion procedure were adopted with digestion pressure and time: 0.3 Mpa/60 s,0.5 Mpa/360 s,1.0 Mpa/180 s. Compared with traditional acid solution method,the dissolving time of microwave digestion was short,and the sample dissolution was complete. The detection limit of method was 0.036 μg/mL.The proposed method was applied to the determination of phosphate ore samples.The relative standard deviation(RSD) was 4.1%-6.6%,and the recovery of standard addition was 94%-108%.