Determination of Mo, Zn, Cd, Ti, Ni, V, Fe, Mn, Cr and Co in crude oil using inductively coupled plasma optical emission spectrometry and sample introduction as detergentless microemulsions
Determination of Mo, Zn, Cd, Ti, Ni, V, Fe, Mn, Cr and Co in crude oil using inductively coupled plasma optical emission spectrometry and sample introduction as detergentless microemulsions
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DOI：
10.1016/j.microc.2006.01.005
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发表时间：
2006-04
影响因子：
4.8
通讯作者：
R. Souza;André L.S. Meliande;C. L. Silveira;R. Aucélio
中科院分区：
文献类型：
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作者：
R. Souza;André L.S. Meliande;C. L. Silveira;R. Aucélio
优化了原油样品制备无洗涤剂微乳的工艺，并将其应用于ICP OES法测定Mo、Zn、Cd、Si、Ti、Ni、V、Fe、Mn、Cr和Co。丙烷-1-醇作为助溶剂，形成了一种含有原油和水的均匀稳定的体系。微乳液的最佳组成为原油/丙烷-1-醇/水/浓硝酸，6/70/20/4 w/w/w/w。这个简单的样品制备程序连同有效的样品导入（使用Meinhard K3雾化器和涡旋式旋风喷雾室）允许使用用分析物无机标准制备的校准曲线对分析物进行快速定量。在本例中，Sc作为校正信号波动和矩阵效应的内标。在雾化器气体流中使用氧气，以尽量减少碳的积累和背景。所有元素的检出限均在ng g−1范围内。以SRM NIST 1634c残余燃料油为标准品，回收率在97.9% ~ 103.8%之间。该方法还应用于两种原油样品，结果与酸分解法的结果吻合较好。所得精密度（n=3）在5%以下，结果表明该方法适用于微量元素含量较低的油样。
A procedure to prepare crude oil samples as detergentless microemulsions was optimized and applied for the determination of Mo, Zn, Cd, Si, Ti, Ni, V, Fe, Mn, Cr and Co by ICP OES. Propan-1-ol was used as a co-solvent allowing the formation of a homogeneous and stable system containing crude oil and water. The optimum composition of the microemulsion was crude oil/propan-1-ol/water/concentrated nitric acid, 6/70/20/4 w/w/w/w. This simple sample preparation procedure together with an efficient sample introduction (using a Meinhard K3 nebulizer and a twister cyclonic spray chamber) allowed a fast quantification of the analytes using calibration curves prepared with analyte inorganic standards. In this case, Sc was used as internal standard for correction of signal fluctuations and matrix effects. Oxygen was used in the nebulizer gas flow in order to minimize carbon building up and background. Limits of detection in the ng g−1range were achieved for all elements. The methodology was tested through the analysis of one standard reference material (SRM NIST 1634c, Residual Fuel Oil) with recoveries between 97.9% and 103.8%. The method was also applied to two crude oil samples and the results were in good agreement with those obtained using the acid decomposition procedure. The precision (n=3) obtained was below 5% and the results indicated that the method is well suited for oil samples containing low concentrations of trace elements.