微波消解-ICP法测定石油焦气化炉渣中7种金属的含量

Determination of 7 Metals in Petroleum Coke Gasification Slag by Microwave Digestion-ICP

石油焦气化炉渣是在石油焦制氢的过程中产生的,其化学成分复杂,难以处理。准确测定其含量,可为后期炉渣的处置及资源化再利用提供重要的数据参考。石油焦气化炉渣在生成的过程中会形成玻璃体结构,为此本文采用碱熔+酸溶的消解方法,建立了微波消解-电感耦合等离子体发射光谱法测定石油焦气化炉渣中的铝、铁、镍、钒、钙、钾、镁等元素的方法。考察了微波消解体系和消解条件,最终确定,0.3g样品用10m L、20%NaOH溶液在180℃下消解20min后,再用10m L盐酸消解1次,待测元素可消解完全,且测定结果与X射线荧光法的结果一致。该方法的RSD小于5%,回收率为94.2%~103.4%。

The coke gasification slag was produced in the process of hydrogen production from petroleum coke,and its chemical composition was complex and difficult to deal with.Petroleum coke gasification slag would form a glassy structure in the process of generation,so a microwave ablation-inductively coupled plasma emission spectrometry method was established for the determination of Al,Fe,Ni,V,Ca,K and Mg in petroleum coke gasification slag by the ablation method of alkali fusion+acid dissolution.The microwave digestion system and digestion conditions were investigated and obtained:0.3g sample was digested with 10 mL,20%NaOH solution at 180℃for 20 min,and then digested with 10mL hydrochloric acid(AR),the RSD was less than 5%and the recovery was 94.2%~103.4%.