Determination of Mercury and Arsenic in Oil-bearing Core by Soxhelt Extraction-Atomic Fluorescence Spectrometry
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摘要: 原油对测定含油岩心中的汞和砷有很大影响，目前去除原油等有机物的方法主要有高温烧制、强酸高温氧化等，要求反应温度较高，会造成汞和砷的损失而使测定结果偏低。本文采用索氏提取法，以氯仿作为提取剂在75℃下低温提取分离岩心中的原油，再用50%的王水溶解剩余样品，原子荧光光谱法测定汞和砷的含量。该方法对汞和砷的检出限分别为0.003mg/kg和0.10mg/kg，相对标准偏差分别为7.3%和5.1%，加标回收率均大于92.5%。与传统方法相比较，该方法避免了由于原油的疏水性造成样品与王水接触不充分、样品分解不完全和反应温度过高导致汞元素损失的问题，测定汞的相对标准偏差由33.0%降低至7.3%，测定砷的相对标准偏差由25.0%提高至5.1%，为含油岩心中其他元素的检测提供了借鉴。要点
(1) 在测定含油岩心中的汞和砷之前通过索氏提取法将原油分离。
(2) 原油被提取后样品可以更充分地与酸接触，其中的汞和砷被更加充分地溶解。
(3) 提取方法操作温度低，不会造成汞和砷的挥发。
(4) 通过原油的提取分离，方法的准确度和精密度得到很大提高。
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.
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Keywords:
- oil-bearing core /
- Hg /
- As /
- Soxhelt extraction /
- aqua regia /
- atomic fluorescence spectrometry
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图 1 经过提取和未经过提取的溶样效果对比
1—未经过索氏提取的样品SY-1溶液，2—经过索氏提取的样品SY-1溶液。
Figure 1. Comparison of sample dissolution effect between the extracted and unextracted samples
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图 2 不同提取时间汞和砷的测定结果
Figure 2. Analytical results of Hg and As at different extraction time
表 1 经过提取和未经过提取的汞和砷的测定结果对比
Table 1 Comparison of analytical results of Hg and As in the extracted and unextracted samples
样品编号 氯仿沥青含量(%) Hg测定值(mg/kg) As测定值(mg/kg) 未经过提取 经过提取 未经过提取 经过提取 SY-1 0.078 0.065 0.105 19.3 24.4 SY-2 0.134 0.044 0.114 16.4 26.5 SY-3 0.033 0.076 0.108 18.3 22.4 SY-4 0.254 0.049 0.128 12.3 31.5 
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表 2 不同溶剂提取原油的结果对比
Table 2 Comparison of crude oil extracted by different solvents
样品编号 氯仿
(g)相对提取率
(%)石油醚
(g)相对提取率
(%)正己烷
(g)相对提取率
(%)SY-1 0.0777 100 0.0748 96.3 0.0722 92.9 SY-2 0.1336 100 0.1242 93.0 0.1205 90.2 SY-3 0.0328 100 0.0302 92.1 0.0284 86.6 SY-4 0.2536 100 0.2311 91.1 0.2206 87.0
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表 3 精密度实验结果
Table 3 Precision tests of the method
样品处理 元素 分次测定值(mg/kg) RSD(%) 未经提取的SY-1 Hg 0.065 0.038 0.044 0.07
30.061 0.086 0.03533.0 As 15.3 11.4 14.2 18.7
17.0 20.1 9.6725.0 高氯酸处理的SY-1 Hg 0.089 0.082 0.068 0.073
0.089 0.094 0.07115.0 As 22.1 21.6 18.7 20.7
22.2 23.6 18.59.0 经过提取的SY-1 Hg 0.105 0.098 0.102 0.112
0.104 0.092 0.1147.3 As 24.4 26.5 23.2 23.5
25.6 24.1 25.95.1
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表 4 加标回收实验结果
Table 4 Spiked recovery tests of the method
实验序号 元素 样品浓度
(mg/kg)加标浓度
(mg/kg)测得浓度
(mg/kg)回收率
(%)1 Hg 0.105 0.200 0.296 95.5 As 24.4 50.0 72.4 96.0 2 Hg 0.105 0.100 0.199 94.0 As 24.4 25.0 48.1 94.8 3 Hg 0.105 0.040 0.142 92.5 As 24.4 10.0 33.8 94.0
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