微波等离子体炬原子发射光谱法测定原油中的钒  

Determination of vanadium in crude oil by microwave plasma torch atomic emission spectrometer

作　　者：张起凯[1] 张文秀[1] 李佳慧[1] 王婵[1] 

机构地区：[1]辽宁石油化工大学化学化工与环境学部,辽宁抚顺113001

出　　处：《化学研究与应用》2015年第7期1078-1081,共4页Chemical Research and Application

摘　　要：采用微波等离子体炬原子发射光谱法（MPT-AES）测定原油中的钒。详细考察了分析谱线、载气流量、工作气流量、氧屏蔽气流量和微波功率对钒发射强度的影响。实验结果表明：在分析谱线289.332nm,微波功率90W,载气流量1350m L·min^-1,工作气流量650m L·min^-1条件下,测得钒的检出限为56.2ng·m L^-1,钒含量在0-100μg·m L^-1范围符合线性关系。对原油中常见的共存元素影响进行考察,3倍的铜,10倍的镁、铁对钒的测定无影响;1倍的钙、镍、钠、锌、锰干扰钒的测定。测试体系对乙二胺四乙酸二钠有一定的允许量,适量的乙二胺四乙酸二钠溶液可大幅度提高共存元素的允许量。原油中钒测定结果的相对标准偏差不大于4.1%,加标回收实验的回收率为95.6%-104.3%。The determination of vanadium in crude oil use the method of MPT-AES. The effect to the emission intensity of vanadium of spectral lines,carrier gas flow rate,working gas flow,oxygen shielding gas flow rate is detailed analyzed. The results show that,in the condition that the analytical line is 289. 332 nm,microwave power is 90 W,carrier gas flow rate is1350 m L·min^-1,working gas flow is 650 m L·min^-1,the detection limit of vanadium is 56. 2ng·m L^-1. It meets linear relation when the content of vanadium within0 - 100μg·L^-1. Coexisting elements have little influence to the determine 3 times copper,10 times over magnesium,but all the other elements such as calcium,copper,iron,nickel,sodium,magnesium,zinc and manganese have influence to the test of vanadium. Adding the releasing agent of 0. 5%EDTA test solution can eliminate the interferences of coexisting elements copper,iron,nickel,sodium,magnesium,zinc and manganese excluding calcium in the determination of vanadium,the measured relative standard deviation was no more than4. 1%and the recovery of the experiment is 95. 6% - 104. 3%.

关 键 词：微波等离子体炬 原子发射光谱法 原油 钒 

分 类 号：O657.31[理学—分析化学]