CN102221593A - Auxiliary method for detecting petroleum and coal resources - Google Patents
Auxiliary method for detecting petroleum and coal resources Download PDFInfo
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- CN102221593A CN102221593A CN2011100843901A CN201110084390A CN102221593A CN 102221593 A CN102221593 A CN 102221593A CN 2011100843901 A CN2011100843901 A CN 2011100843901A CN 201110084390 A CN201110084390 A CN 201110084390A CN 102221593 A CN102221593 A CN 102221593A
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Abstract
The invention discloses an auxiliary method for detecting petroleum and coal resources, belonging to technical field of energy resource detection. The method carries out gas chromatography-mass spectrometry analysis on a preprocessed collected water sample and analyzes the substance ingredients contained in the water sample; and if most of organic substances in the water sample are organic compositions in coal and petroleum, the places below the water sampling positions probably contain the petroleum and coal resources. The method has simple operation steps and is applicable to judge whether the area to be detected contains the coal resources.
Description
Technical field
The invention belongs to energy resources Detection Techniques field, be specifically related to a kind of method of auxiliary locate oil coal resources.
Background technology
Oil major pollutants in the ground water regime water are organic substances such as alkane, unsaturated hydro carbons, alkyl benzene, chlorinated hydrocarbon, chlorobenzene class, heterocyclic, condensed ring benzene class.If the underground oil coal resources that exist in an area, the composition of oil coal such as water-soluble toxicity hydrocarbon (as benzene, toluene, ethylbenzene and dimethylbenzene etc.) are because density is littler than water, can float on the underground water surface by migration in soil and trend, thereby form the float type pollution source of free state, polluted underground water.
In China oil gas field area, ground water regime is petroleum hydrocarbon contaminated very serious.Henan Shuan He water head site, along with the exploitation of oil gas field, water quality obviously has been subjected to pollution.Its shallow seated groundwater petroleum-type recall rate reaches 44%, and mid-deep strata water (about degree of depth 200m) recall rate is 78%.There is the petroleum content in 56% the well to exceed standard, reaches 0.4～2.7mg/L.Oil or coal constituent boiling point are lower, generally below 300 ℃, adopt GC-MS that the oil coal constituent is analyzed, the mass spectrum that obtains contains much information, and again it is carried out library searching, carries out the similarity coupling with spectrogram and judges, can accurately judge the mark that contains in the oil coal resources, therefore, use the GC-MS method that the underground water water sample is carried out organic pollutant category and analyze, but whether auxiliary judgment there is the existence of oil coal resources.
Summary of the invention
The method that the purpose of this invention is to provide a kind of auxiliary locate oil coal resources.
A kind of method of auxiliary locate oil coal resources is characterized in that, comprises the steps:
(1) pre-service
Gather water sample 50-160mL and join in the 250mL separating funnel, add 5～6g NaCl, jolting gently, dissolve fully until NaCl, add 60～80mL methylene chloride, liquid-liquid extraction 10min, leave standstill 10min, shift organic phase, regulate pH＞11, liquid-liquid extraction 10min, leave standstill 10min, regulate pH＜2, liquid-liquid extraction 10min, leave standstill 10min, merge organic phase; Rotary evaporation concentrates organic phase in 35 ℃～40 ℃ water-bath, when sample concentration to the 8～10mL left and right sides, evaporative flask is taken out from water-bath, rotary evaporation is at room temperature carried out, until sample volume is 2～3mL, shift concentrate to nitrogen and blow concentration tube, each swinging with the 1mL methylene chloride washed the rotary evaporation bottle, blowing solution until nitrogen is 9～10mL, heated sample in 35～45 ℃ of water-baths, and high purity nitrogen blows sample, when sample concentration to 2～3mL, with the centrifugal tube wall of the clean eluent methylene chloride of 1mL, be concentrated into below the 1mL, be settled to 1mL with methylene chloride at last;
(2) gas chromatography-mass spectrometry analysis
At first carry out gas chromatography, adjusting temperature of vaporization chamber is 250 ℃, split sampling, and split ratio is 30: 1; Post case initial temperature is 35 ℃, keeps 4min, rises to 300 ℃ with 4 ℃/min, keeps 3min; Press before the post and be 27.3kPa; Carry out mass spectrum then, the electron impact ion source temperature is 320 ℃ during mass spectrum, and interface temperature is 280 ℃, and electron-multiplier voltage is 1.02kV, and sweep velocity is 660amu/s, and sweep limit 55～400amu/s, solvent mute time 2.5min, sample size are 1 μ L;
(3) output GC-MS experimental result chromatogram;
(4) seek organism material in peak stronger in the chromatogram and the corresponding picture library thereof, if the organism material that shows belongs to the composition of oil coal resource basically, it is higher that then this area contains the possibility of oil coal resources.
The composition of described oil coal resource is alkane, unsaturated hydro carbons, alkyl benzene, chlorinated hydrocarbon, chlorobenzene class, heterocyclic, condensed ring benzene class.
Embodiment
The present invention will be further described below in conjunction with specific embodiment.
Instrument and reagent that following examples adopt are: GC/MS gas chromatography mass spectrometer, Rotary Evaporators, separating funnel, pH meter, methylene chloride (chromatographically pure), sodium chloride (top grade is pure).
Embodiment 1
The method of auxiliary locate oil coal resources, carry out according to following steps:
(1) pre-service
Gather water sample 50mL and join in the 250mL separating funnel, add 5gNaCl, jolting gently, dissolve fully until NaCl, add the 60mL methylene chloride, liquid-liquid extraction 10min, leave standstill 10min, shift organic phase, regulate pH=11.5, liquid-liquid extraction 10min, leave standstill 10min, regulate pH=1.5, liquid-liquid extraction 10min, leave standstill 10min, merge organic phase; Rotary evaporation concentrates organic phase in 35 ℃ water-bath, when sample concentration during to 8mL, evaporative flask is taken out from water-bath, rotary evaporation is at room temperature carried out, until sample volume is 2mL, shift concentrate to nitrogen and blow concentration tube, each swinging with the 1mL methylene chloride washed the rotary evaporation bottle, blowing solution until nitrogen is 9mL, heated sample in 35 ℃ of water-baths, and high purity nitrogen blows sample, when sample concentration arrives 2mL, with the centrifugal tube wall of the clean eluent methylene chloride of 1mL, be concentrated into below the 1mL, be settled to 1mL with methylene chloride at last;
(2) gas chromatography-mass spectrometry analysis
At first carry out gas chromatography, adjusting temperature of vaporization chamber is 250 ℃, split sampling, and split ratio is 30: 1; Post case initial temperature is 35 ℃, keeps 4min, rises to 300 ℃ with 4 ℃/min, keeps 3min; Press before the post and be 27.3kPa; Carry out mass spectrum then, the electron impact ion source temperature is 320 ℃ during mass spectrum, and interface temperature is 280 ℃, and electron-multiplier voltage is 1.02kV, and sweep velocity is 660amu/s, and sweep limit 55amu/s, solvent mute time 2.5min, sample size are 1 μ L;
(3) output GC-MS experimental result chromatogram;
(4) seek organism material in peak stronger in the chromatogram and the corresponding picture library thereof, if the organism material that shows belongs to the composition of oil coal resource basically, it is higher that then this area contains the possibility of oil coal resources.
Embodiment 2
The method of auxiliary locate oil coal resources, carry out according to following steps:
(1) pre-service
Gather water sample 100mL and join in the 250mL separating funnel, add 5.5gNaCl, jolting gently, dissolve fully until NaCl, add the 70mL methylene chloride, liquid-liquid extraction 10min, leave standstill 10min, shift organic phase, regulate pH=12, liquid-liquid extraction 10min, leave standstill 10min, regulate pH=1, liquid-liquid extraction 10min, leave standstill 10min, merge organic phase; Rotary evaporation concentrates organic phase in 38 ℃ water-bath, when sample concentration during to the 9mL left and right sides, evaporative flask is taken out from water-bath, rotary evaporation is at room temperature carried out, until sample volume is 2.5mL, shift concentrate to nitrogen and blow concentration tube, each swinging with the 1mL methylene chloride washed the rotary evaporation bottle, blowing solution until nitrogen is 9.5mL, heated sample in 40 ℃ of water-baths, and high purity nitrogen blows sample, when sample concentration arrives 2.5mL, with the centrifugal tube wall of the clean eluent methylene chloride of 1mL, be concentrated into below the 1mL, be settled to 1mL with methylene chloride at last;
(2) gas chromatography-mass spectrometry analysis
At first carry out gas chromatography, adjusting temperature of vaporization chamber is 250 ℃, split sampling, and split ratio is 30: 1; Post case initial temperature is 35 ℃, keeps 4min, rises to 300 ℃ with 4 ℃/min, keeps 3min; Press before the post and be 27.3kPa; Carry out mass spectrum then, the electron impact ion source temperature is 320 ℃ during mass spectrum, and interface temperature is 280 ℃, and electron-multiplier voltage is 1.02kV, and sweep velocity is 660amu/s, and sweep limit 200amu/s, solvent mute time 2.5min, sample size are 1 μ L;
(3) output GC-MS experimental result chromatogram;
(4) seek organism material in peak stronger in the chromatogram and the corresponding picture library thereof, if the organism material that shows belongs to the composition of oil coal resource basically, it is higher that then this area contains the possibility of oil coal resources.
Embodiment 3
The method of auxiliary locate oil coal resources, carry out according to following steps:
(1) pre-service
Gather water sample 160mL and join in the 250mL separating funnel, add 6gNaCl, jolting gently, dissolve fully until NaCl, add the 80mL methylene chloride, liquid-liquid extraction 10min, leave standstill 10min, shift organic phase, regulate pH=12.5, liquid-liquid extraction 10min, leave standstill 10min, regulate pH=0.5, liquid-liquid extraction 10min, leave standstill 10min, merge organic phase; Rotary evaporation concentrates organic phase in 40 ℃ water-bath, when sample concentration during to the 10mL left and right sides, evaporative flask is taken out from water-bath, rotary evaporation is at room temperature carried out, until sample volume is 3mL, shift concentrate to nitrogen and blow concentration tube, each swinging with the 1mL methylene chloride washed the rotary evaporation bottle, blowing solution until nitrogen is 10mL, heated sample in 45 ℃ of water-baths, and high purity nitrogen blows sample, when sample concentration arrives 3mL, with the centrifugal tube wall of the clean eluent methylene chloride of 1mL, be concentrated into below the 1mL, be settled to 1mL with methylene chloride at last;
(2) gas chromatography-mass spectrometry analysis
At first carry out gas chromatography, adjusting temperature of vaporization chamber is 250 ℃, split sampling, and split ratio is 30: 1; Post case initial temperature is 35 ℃, keeps 4min, rises to 300 ℃ with 4 ℃/min, keeps 3min; Press before the post and be 27.3kPa; Carry out mass spectrum then, the electron impact ion source temperature is 320 ℃ during mass spectrum, and interface temperature is 280 ℃, and electron-multiplier voltage is 1.02kV, and sweep velocity is 660amu/s, and sweep limit 400amu/s, solvent mute time 2.5min, sample size are 1 μ L;
(3) output GC-MS experimental result chromatogram;
(4) seek organism material in peak stronger in the chromatogram and the corresponding picture library thereof, if the organism material that shows belongs to the composition of oil coal resource basically, it is higher that then this area contains the possibility of oil coal resources.
Claims (2)
1. the method for auxiliary locate oil coal resources is characterized in that, comprises the steps:
(1) pre-service
Gather water sample 50-160mL and join in the 250mL separating funnel, add 5～6gNaCl, jolting gently, dissolve fully until NaCl, add 60～80mL methylene chloride, liquid-liquid extraction 10min, leave standstill 10min, shift organic phase, regulate pH＞11, liquid-liquid extraction 10min, leave standstill 10min, regulate pH＜2, liquid-liquid extraction 10min, leave standstill 10min, merge organic phase; Rotary evaporation concentrates organic phase in 35 ℃～40 ℃ water-bath, when sample concentration to the 8～10mL left and right sides, evaporative flask is taken out from water-bath, rotary evaporation is at room temperature carried out, until sample volume is 2～3mL, shift concentrate to nitrogen and blow concentration tube, each swinging with the 1mL methylene chloride washed the rotary evaporation bottle, blowing solution until nitrogen is 9～10mL, heated sample in 35～45 ℃ of water-baths, and high purity nitrogen blows sample, when sample concentration to 2～3mL, with the centrifugal tube wall of the clean eluent methylene chloride of 1mL, be concentrated into below the 1mL, be settled to 1mL with methylene chloride at last;
(2) gas chromatography-mass spectrometry analysis
At first carry out gas chromatography, adjusting temperature of vaporization chamber is 250 ℃, split sampling, and split ratio is 30: 1; Post case initial temperature is 35 ℃, keeps 4min, rises to 300 ℃ with 4 ℃/min, keeps 3min; Press before the post and be 27.3kPa; Carry out mass spectrum then, the electron impact ion source temperature is 320 ℃ during mass spectrum, and interface temperature is 280 ℃, and electron-multiplier voltage is 1.02kV, and sweep velocity is 660amu/s, and sweep limit 55～400amu/s, solvent mute time 2.5min, sample size are 1 μ L;
(3) output GC-MS experimental result chromatogram;
(4) seek organism material in peak stronger in the chromatogram and the corresponding picture library thereof, if the organism material that shows belongs to the composition of oil coal resource basically, it is higher that then this area contains the possibility of oil coal resources.
2. according to the method for the described a kind of auxiliary locate oil coal resources of claim 1, it is characterized in that the composition of described oil coal resource is alkane, unsaturated hydro carbons, alkyl benzene, chlorinated hydrocarbon, chlorobenzene class, heterocyclic, condensed ring benzene class.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105486768A (en) * | 2015-12-08 | 2016-04-13 | 中国石油大学(北京) | Defining method of hydrocarbon expulsion source rock |
| CN111624266A (en) * | 2020-04-29 | 2020-09-04 | 中国石油天然气股份有限公司 | Method for extracting petroleum biomarkers in formation water of dry gas well |
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| CN101097211A (en) * | 2006-06-28 | 2008-01-02 | 宝山钢铁股份有限公司 | Method for detecting molecular weight of strong-polarity organic matters in coking wastewater biochemical treatment discharge liquid |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101097211A (en) * | 2006-06-28 | 2008-01-02 | 宝山钢铁股份有限公司 | Method for detecting molecular weight of strong-polarity organic matters in coking wastewater biochemical treatment discharge liquid |
| CN1936586A (en) * | 2006-09-15 | 2007-03-28 | 北京工业大学 | Method for fully analyzing air (oxygen) oxidation cyclohexaane reaction mixture |
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| 吕振波等: "烷基苯生产中循环烷烃的液-固吸附色谱预分离和气相色谱／质谱分析", 《色谱》, vol. 18, no. 6, 30 November 2000 (2000-11-30), pages 559 - 562 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105486768A (en) * | 2015-12-08 | 2016-04-13 | 中国石油大学(北京) | Defining method of hydrocarbon expulsion source rock |
| CN111624266A (en) * | 2020-04-29 | 2020-09-04 | 中国石油天然气股份有限公司 | Method for extracting petroleum biomarkers in formation water of dry gas well |
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Inventor after: Yang Shengjie Inventor after: Cang Nanzhi Inventor after: Li Fenjie Inventor before: Yang Shengjie Inventor before: Cang Nanzhi Inventor before: Li Fenjie |
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