微波消解-微波等离子体原子发射光谱法测定原油中6种元素含量

Determination of Six Elements in Crude Oil by Microwave Digestion-Microwave Plasma Atomic Emission Spectrometry

本研究建立了微波消解-微波等离子体原子发射光谱法测定原油中的镍(Ni)、钒(V)、铁(Fe)、钠(Na)、钾(K)、钙(Ca)的方法。对样品量、消解体系及消解温度控制进行了选择实验,确定0.2 g样品,6 mL硝酸+2 mL双氧水消解体系及消解程序;铁、钾、钠、钙、镍的检测浓度范围为0~2 mg/L;钒的检测浓度范围为0~5 mg/L;铁、钾、钠、钙方法检出限为5 mg/kg;钒、镍的方法检出限为2 mg/kg。方法的精密度为1.14%~5.13%,加标回收率范围为81.2%~109.6%,与标准方法对比结果无显著性差异,表明该检测方法能够满足口岸检测需求。

Nickel, vanadium, iron, sodium, potassium and calcium in crude oil were determined by microwave digestion-microwave plasma atomic emission spectrometry. For a comparison of the pretreatment conditions, 6 mL nitric acid+2 mL hydrogen peroxide digestion system was added to the crude oil sample that weight was 0.2 g. The determination of nickel, vanadium, iron, sodium,potassium and calcium in crude oil was carried out by microwave plasma atomic emission spectrometry. The detection concentration range of iron, potassium, sodium, calcium and nickel was 0 to 2 mg/L;The detection concentration range of vanadium was 0-5 mg/L;the detection limit of iron, potassium, sodium and calcium was 5 mg/kg;the detection limit of vanadium and nickel was 2 mg/kg.The precision of the method was 1.14%-5.13%, and the recovery of spiking was 81.2%-109.6%. There was no significant difference in results compared with the standard method, and the test method met the requirements of port testing.