A simple dilution method for the direct determination of trace nickel in crude oil with a miniaturized electrothermal atomic absorption spectrometer,Journal of Analytical Atomic Spectrometry

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A simple dilution method for the direct determination of trace nickel in crude oil with a miniaturized electrothermal atomic absorption spectrometer
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2020-09-01 , DOI: 10.1039/d0ja00081g
Kai Li _{1,

2,

3,

4} , Xi Wu _{1,

2,

3,

4} , Zhiming Chen _{4,

5,

6,

7} , Jin Luo _{3,

4,

8} , Xiandeng Hou _{1,

2,

3,

4,

9} , Xiaoming Jiang _{1,

2,

3,

4}

Affiliation

A simple procedure for the direct determination of trace nickel in crude oil samples has been proposed using a miniaturized electrothermal atomic absorption spectrometer (ETAAS). Prior to the analysis, crude oil in cyclohexane without any complicated or lengthy sample digestion was employed to suit a potential field analysis. A proper aliquot of the oil-based standard stock solution of Ni or crude oil was diluted in 20 mL cyclohexane, followed by 30 min ultrasonication and 60 min shaking. A tiny aliquot (20 μL) of the diluted sample solution was directly pipetted onto a tungsten coil (W-coil) atomizer of the miniaturized ETAAS (Fig. S1). With the heating program of the W-coil, the sample solvent and matrix were first removed, and the nickel was subsequently atomized for the AAS detection using palladium as a chemical modifier. Under optimized drying conditions, ashing and atomization currents, gas flow rate and atomizer height, a limit of detection (LOD) of 10 μg kg⁻¹ was achieved, which satisfies the demands of field analysis for petroleum exploration. The accuracy of the proposed method for the determination of Ni in real crude oil samples was assessed by comparing the analytical data with those obtained via ICP-OES after microwave digestion, and the reproducibility was also investigated by analyzing 50 crude oil samples. The statistical results indicated that this is potentially useful for the field analysis of Ni in crude oil.

中文翻译：

小型电热原子吸收光谱仪直接测定原油中痕量镍的简单稀释方法

已经提出了使用小型化的电热原子吸收光谱仪（ETAAS）直接测定原油样品中痕量镍的简单方法。在分析之前，采用环己烷中的原油，无需进行任何复杂或冗长的样品消化，即可进行潜在的现场分析。将镍或原油的油基标准储备溶液的等分试样在20 mL环己烷中稀释，然后超声30分钟，振摇60分钟。将一小部分（20μL）稀释的样品溶液直接移液到微型ETAAS的钨卷（W线圈）雾化器上（图S1）。通过W线圈的加热程序，首先去除样品溶剂和基体，然后将镍雾化，使用钯作为化学改性剂进行AAS检测。达到^-1，满足石油勘探的现场分析要求。通过将分析数据与微波消解后通过ICP-OES获得的分析数据进行比较，评估了所建议的测定实际原油样品中Ni的方法的准确性，并且还通过分析50个原油样品来研究了重现性。统计结果表明，这可能对原油中镍的现场分析有用。

更新日期：2020-11-03

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