微波消解-微波等离子体炬原子发射光谱法测定原油和渣油中的铁、镍、铜和钠

Determination of Iron, Nickel, Copper, Sodium in Crude Oil and Residue Oil by Microwave Digestion-Microwave Plasma Torch Atomic Emission Spectrometry

采用微波消解技术消解原油和渣油,利用微波等离子体炬原子发射光谱法测定原油和渣油中的Fe、Ni、Cu、Na。考察了原油和渣油的最佳消解条件、各元素测定条件及共存元素对测定的影响。方法对Fe、Ni、Cu和Na元素的检出限分别为22、42、2.0和1.0μg/L;线性范围分别为0.1～100、0.15～50、0.01～5.0和0.006～2.0mg/L,应用该方法测定实际样品中Fe、Ni、Cu和Na的相对标准偏差分别为3.9%、3.6%、5.5%和3.4%。微波消解样品的测定结果与常规干法灰化法的测定结果相吻合。本方法省时、省酸、简便、快速,没有环境污染,具有一定的实际应用价值。

The microwave digestion procedures were developed for crude oil and residue oil. Microwave plasma torch atomic emission spectrometry (MPT-AES) was used to determine the iron, nickel, copper, sodium in crude oil and residue oil. Optimal condition for determination ( analytical wavelength, microwave power, flow rate of carrier gas, flow rate of supporting gas and acid concentrations) were chosen. The effect of concomitant elements on determination of iron, nickel, copper, sodium were studied. The detection limits were 22, 42, 2.0 and 1.0 mu g/L for iron, nickel, copper, sodium, respectively. The linear range were 0.1 similar to 100, 0.15 similar to 50, 0.01 similar to 5.0 and 0.006 similar to 2.0 mg/L, respectively. The relative standard deviation for the determination of samples were less than 3.9%, 3.6%, 5.5.% , 3.4% respectively. The determination results of microwave digestion were identical with those obtained with routine dry-ash method. The results show that the method is simple, rapid, accurate, save reagent, less environment contamination and of great application value.