Determination of Mercury and Arsenic in Oil-bearing Core by Soxhelt Extraction-Atomic Fluorescence Spectrometry

Ning-qiang QIAO; Zhi-wei XUE; Gang-feng WANG; Dan LUO

doi:10.15898/j.cnki.11-2131/td.201812030128

Rock and Mineral Analysis > 2019 > 38(4): 461-467. > DOI: 10.15898/j.cnki.11-2131/td.201812030128

Ning-qiang QIAO, Zhi-wei XUE, Gang-feng WANG, Dan LUO. Determination of Mercury and Arsenic in Oil-bearing Core by Soxhelt Extraction-Atomic Fluorescence Spectrometry[J]. Rock and Mineral Analysis, 2019, 38(4): 461-467. DOI: 10.15898/j.cnki.11-2131/td.201812030128

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Determination of Mercury and Arsenic in Oil-bearing Core by Soxhelt Extraction-Atomic Fluorescence Spectrometry

No. 203 Research Institute, China National Nuclear Corporation, Xianyang 712000, China

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Received Date: December 02, 2018
Revised Date: March 07, 2019
Accepted Date: April 08, 2019
Published Date: June 30, 2019

Abstract

HIGHLIGHTS
(1) Crude oil was separated by Soxhlet extraction before the determination of Hg and As in oil-bearing cores.

(2) Post-extraction samples can be fully exposed to acid, resulting in complete dissolution of Hg and As.

(3) Volatization of Hg and As did not occur, even though the extraction method was operated at a low temperature.

(4) A significant improvement of method accuracy and precision through the extraction and separation of crude oil.

ABSTRACT

BACKGROUNDCrude oil had a great influence on the determination of mercury and arsenic in oil-bearing cores by atomic fluorescence spectrometry. At present, the main methods of removing organic matter such as crude oil are high-temperature firing and high-temperature oxidation with strong acid. In these methods, high reaction temperature will cause loss of mercury and arsenic, resulting in lower results.
OBJECTIVESTo develop a separation method with low operating temperature.
METHODSMercury and arsenic in oil-bearing cores were determined by atomic fluorescence spectrometry with Soxhlet extraction at a low temperature for this method of 75℃ and the remaining part was decomposed by 50% aqua regia.
RESULTSThe detection limits were 0.003mg/kg and 0.10mg/kg for mercury and arsenic, respectively. The relative standard deviations were 7.3% and 5.1%, respectively. The relative standard deviation of mercury decreased from 33.0% to 7.3%, and the relative standard deviation of arsenic decreased from 25.0% to 5.1%. The recoveries of standard addition were greater than 92.5%.
CONCLUSIONSCompared with traditional methods, this method avoided the problems of insufficient contact between samples and aqua regia due to the hydrophobicity of crude oil, incomplete decomposition of samples and mercury loss due to excessive reaction temperature. The proposed method provides a reference for the determination of other elements in oil-bearing cores.
- oil-bearing core,
- Hg,
- As,
- Soxhelt extraction,
- aqua regia,
- atomic fluorescence spectrometry

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Determination of Mercury and Arsenic in Oil-bearing Core by Soxhelt Extraction-Atomic Fluorescence Spectrometry

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