CN107831219A - The Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample - Google Patents
The Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample Download PDFInfo
- Publication number
- CN107831219A CN107831219A CN201710168858.2A CN201710168858A CN107831219A CN 107831219 A CN107831219 A CN 107831219A CN 201710168858 A CN201710168858 A CN 201710168858A CN 107831219 A CN107831219 A CN 107831219A
- Authority
- CN
- China
- Prior art keywords
- crude oil
- oil sample
- biomarker
- analysis method
- rapid identification
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The present invention provides a kind of Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample, and the Rapid identification analysis method of saturation hydrocarbon system row biomarker includes in the crude oil sample：Step 1, appropriate crude oil sample is weighed；Step 2, reagent is added into crude oil sample and obtains crude oil detection solution；Step 3, crude oil detection solution is loaded into sample bottle, is put into ultrasonic cleaner and fully vibrates；Step 4, sample bottle is put into centrifuge separation；Step 5, the crude oil detection solution after centrifugation is subjected to gaschromatographic mass spectrometry GC/MS analyses.The Rapid identification analysis method of saturation hydrocarbon system row biomarker simplifies operating procedure in the crude oil sample, reduces reagent dosage, shortens analysis process, can provide analyze data as early as possible.
Description
Technical field
The present invention relates to oil field development technical field, especially relates to saturation hydrocarbon system row biology mark in a kind of crude oil sample
The Rapid identification analysis method of will thing.
Background technology
With continually developing for oil, due to exploit, transport and the factor such as various petroleum pipeline agings perforation caused by it is former
Oily run, drip, leak phenomenon repeatedly occurs.Once generation crude oil leakage, due to lacking quickly and efficiently identification and analysis method, very
Hardly possible is timely, quickly determines oil spilling point, so as to cause to pollute continuous enlargement, causes huge economic loss.Therefore, when oil spilling is sent out
After life, in time, knowledge pollution source is correctly sentenced, be the quick premise for finding oil spilling point.Use at present analysis method detection according to
According to GB/T 18606 is seen, during analysis, crude oil sample will could carry out instrument after chromatographic column isolates different component
Analysis.The method is directed to for oil spilling identification, analytical cycle length be present, it is impossible to provides the weak point of analyze data in time.For
This we have invented a kind of Rapid identification analysis method of saturation hydrocarbon system row biomarker in new crude oil sample, solve with
Upper technical problem.
The content of the invention
It is an object of the invention to provide a kind of Rapid identification for being directed to saturation hydrocarbon system row biomarker in crude oil sample point
Analysis method, the saturated hydrocarbons series of biologic mark in crude oil can be quickly analyzed, be easy to provide analyze data in time.
The purpose of the present invention can be achieved by the following technical measures：Saturation hydrocarbon system row biomarker in crude oil sample
Rapid identification analysis method, the Rapid identification analysis method of saturation hydrocarbon system row biomarker includes in the crude oil sample：Step
1, weigh appropriate crude oil sample；Step 2, reagent is added into crude oil sample and obtains crude oil detection solution；Step 3, crude oil is examined
Survey solution and load sample bottle, be put into ultrasonic cleaner and fully vibrate；Step 4, sample bottle is put into centrifuge separation；
Step 5, the crude oil detection solution after centrifugation is subjected to gas chromatography-mass spectrum GC/MS analyses.
The purpose of the present invention can be also achieved by the following technical measures：
In step 1, the crude oil sample weighed is 15~20mg.
In step 1, the crude oil sample weighed is 18mg.
In step 2,1mL isooctane is added into crude oil sample and obtains crude oil detection solution.
In step 3, crude oil detection solution is loaded into sample bottle, is put into ultrasonic cleaner fully vibration 15 minutes.
In step 4, sample bottle is put into centrifuge, makes the detection solution of the crude oil after concussion with 4000 revs/min of centrifugations
10min。
In step 5, using quartz capillary column DB5-MS when carrying out gas chromatographic analysis, 60m*0.25mm*0.25 μm.
In step 5, when carrying out chromatography, 60 DEG C of initial temperature, after stopping 2min, with 4 DEG C/min temperature programmings to 300
DEG C, constant temperature 50min；Carrier gas is high-purity helium；Flow velocity 1.0mL/min, shunt mode：Do not shunt, 300 DEG C of injector temperature, enter
Sample amount：1μL.
In step 5, when carrying out gaseous-mass spectrography, the ion gun used is electron bombardment ionization source.
In step 5, when carrying out gaseous-mass spectrography, 230 DEG C of ion source temperature；Electron energy 70eV.；Scan mode is choosing
Select ion scan；Sweep speed is no more than 2s for each circulation.
In step 5, the ion of selection is M/Z57, M/Z66, M/Z69, M/Z71, M/Z82, M/Z83, M/Z85, M/Z97,
M/Z98、M/Z109、M/Z123、M/Z125、M/Z163、M/Z177、M/Z183、M/Z191、M/Z205、M/Z217、M/Z218、
M/Z219、M/Z221、M/Z231、M/Z232、M/Z245、M/Z259。
The Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample in the present invention, crude oil sample can
To be handled without chromatographic column, it is possible to carry out Instrumental Analysis, simplify operating procedure, reduce reagent dosage, shorten point
Flow is analysed, analyze data can be provided as early as possible.
Brief description of the drawings
Fig. 1 be the present invention crude oil sample in saturation hydrocarbon system row biomarker Rapid identification analysis method it is one specific
The flow chart of embodiment；
Fig. 2 is that GC/MS analyzes total ion current figure in a specific embodiment of the invention；
Fig. 3 is that GC/MS analyzes M/Z217 mass chromatograms in a specific embodiment of the invention；
Fig. 4 is that GC/MS analyzes M/Z191 mass chromatograms in a specific embodiment of the invention.
Embodiment
For enable the present invention above and other objects, features and advantages become apparent, it is cited below particularly go out preferable implementation
Example, and coordinate shown in accompanying drawing, it is described in detail below.
As shown in figure 1, Fig. 1 is the Rapid identification analysis side of saturation hydrocarbon system row biomarker in crude oil sample of the invention
The flow chart of method.
In step 101, appropriate amount of sample is weighed.Weigh crude oil sample about 15~20mg.
In step 102, reagent is added into crude oil sample and obtains crude oil detection solution.
In step 103, crude oil detection solution is loaded into sample bottle, is put into ultrasonic cleaner and fully vibrates.
In step 104, sample bottle is put into centrifuge separation.
In step 105, crude oil detection solution is subjected to gas chromatography-mass spectrum GC/MS analyses.In one embodiment, GC/MS
Analysis condition is：
1. chromatographic condition：Quartz capillary column DB5-MS, 60m*0.25mm*0.25 μm；60 DEG C of initial temperature, stop 2min
Afterwards, with 4 DEG C/min temperature programmings to 300 DEG C, constant temperature 50min；Carrier gas is high-purity helium；Flow velocity 1.0mL/min, shunt mode：
Do not shunt, 300 DEG C of injector temperature, sample size：1μL；
2. Mass Spectrometry Conditions：Ion gun is electron bombardment ionization source (EI), 230 DEG C of ion source temperature；Electron energy 70eV.；Scanning
Mode is selection ion scan (SIM)；Sweep speed is no more than 2s for each circulation；The ion of selection is M/Z57, M/Z66, M/
Z69、M/Z71、M/Z82、M/Z83、M/Z85、M/Z97、M/Z98、M/Z109、M/Z123、M/Z125、M/Z163、M/Z177、M/
Z183、M/Z191、M/Z205、M/Z217、M/Z218、M/Z219、M/Z221、M/Z231、M/Z232、M/Z245、M/Z259。
In the specific embodiment of the application present invention, comprise the following steps：
In step 1, crude oil sample 18mg is weighed.
In step 2,1mL isooctane (analysis is pure) is added into crude oil sample and obtains crude oil detection solution.
In step 3, crude oil detection solution is loaded into sample bottle, is put into ultrasonic cleaner fully vibration 15 minutes.
In step 4, sample bottle is put into centrifuge, makes mixed liquor with 4000 revs/min of centrifugation 10min.
In step 5, crude oil detection solution is subjected to gas chromatography-mass spectrum GC/MS analyses.GC/MS analysis conditions are：
1. chromatographic condition：Quartz capillary column DB5-MS, 60m*0.25mm*0.25 μm；60 DEG C of initial temperature, stop 2min
Afterwards, with 4 DEG C/min temperature programmings to 300 DEG C, constant temperature 50min；Carrier gas is high-purity helium；Flow velocity 1.0mL/min, shunt mode：
Do not shunt, 300 DEG C of injector temperature, sample size：1μL；
2. Mass Spectrometry Conditions：Ion gun is electron bombardment ionization source (EI), 230 DEG C of ion source temperature；Electron energy 70eV.；Scanning
Mode is selection ion scan (SIM)；Sweep speed is no more than 2s for each circulation.The ion of selection is M/Z57, M/Z66, M/
Z69、M/Z71、M/Z82、M/Z83、M/Z85、M/Z97、M/Z98、M/Z109、M/Z123、M/Z125、M/Z163、M/Z177、M/
Z183、M/Z191、M/Z205、M/Z217、M/Z218、M/Z219、M/Z221、M/Z231、M/Z232、M/Z245、M/Z259。
Fig. 2 is that GC/MS analyzes total ion current figure in a specific embodiment of the invention, figure it is seen that n-alkane
Series and pristane and phytane can detect.
Fig. 3 is that GC/MS analyzes M/Z217 mass chromatograms in a specific embodiment of the invention, from figure 3, it can be seen that weight
Row's gonane series and C27, C28 and C29 rule gonane series can detect.Detection foundation is shown in the matter of 18606 gas-chromatographies of GB/T one
Spectrometry determines biomarker in sediment and crude oil.
Fig. 4 is that GC/MS analyzes M/Z191 mass chromatograms in a specific embodiment of the invention, from fig. 4, it can be seen that three
Cyclic terpene methane series row, Ts and Tm, C29 norhopane, C30 hopances, C31~C35 homohopanes series and gamma wax alkane can detect, and detect
Foundation is shown in biomarker in the gas chromatography and mass spectromentry methods of GB/T 18606 measure sediment and crude oil.
Claims (11)
1. the Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample, it is characterised in that the crude oil sample
The Rapid identification analysis method of middle saturation hydrocarbon system row biomarker includes：
Step 1, appropriate crude oil sample is weighed；
Step 2, reagent is added into crude oil sample and obtains crude oil detection solution；
Step 3, crude oil detection solution is loaded into sample bottle, is put into ultrasonic cleaner and fully vibrates；
Step 4, sample bottle is put into centrifuge separation；
Step 5, the crude oil detection solution after centrifugation is subjected to gas chromatography-mass spectrum GC/MS analyses.
2. the Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample according to claim 1, its
It is characterised by, in step 1, the crude oil sample weighed is 15~20mg.
3. the Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample according to claim 1, its
It is characterised by, in step 1, the crude oil sample weighed is 18mg.
4. the Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample according to claim 1, its
It is characterised by, in step 2,1mL isooctane is added into crude oil sample and obtains crude oil detection solution.
5. the Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample according to claim 1, its
It is characterised by, in step 3, crude oil detection solution is loaded into sample bottle, is put into ultrasonic cleaner fully vibration 15 minutes.
6. the Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample according to claim 1, its
It is characterised by, in step 4, sample bottle is put into centrifuge, makes the detection solution of the crude oil after concussion with 4000 revs/min of centrifugations
10min。
7. the Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample according to claim 1, its
It is characterised by, in step 5, using quartz capillary column DB5-MS when carrying out gas chromatographic analysis, 60m*0.25mm*0.25 μm.
8. the Rapid identification analysis method of crude oil sample according to claim 1, it is characterised in that in step 5, carry out color
During spectrum analysis, 60 DEG C of initial temperature, after stopping 2min, with 4 DEG C/min temperature programmings to 300 DEG C, constant temperature 50min；Carrier gas is height
Pure helium；Flow velocity 1.0mL/min, shunt mode：Do not shunt, 300 DEG C of injector temperature, sample size：1μL.
9. the Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample according to claim 1, its
It is characterised by, in step 5, when carrying out gaseous-mass spectrography, the ion gun used is electron bombardment ionization source.
10. the Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample according to claim 1, its
It is characterised by, in step 5, when carrying out gaseous-mass spectrography, 230 DEG C of ion source temperature；Electron energy 70eV.；Scan mode is
Select ion scan；Sweep speed is no more than 2s for each circulation.
11. the Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample according to claim 10,
Characterized in that, in step 5, the ion of selection is M/Z57, M/Z66, M/Z69, M/Z71, M/Z82, M/Z83, M/Z85, M/
Z97、M/Z98、M/Z109、M/Z123、M/Z125、M/Z163、M/Z177、M/Z183、M/Z191、M/Z205、M/Z217、M/
Z218、M/Z219、M/Z221、M/Z231、M/Z232、M/Z245、M/Z259。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710168858.2A CN107831219A (en) | 2017-03-20 | 2017-03-20 | The Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710168858.2A CN107831219A (en) | 2017-03-20 | 2017-03-20 | The Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107831219A true CN107831219A (en) | 2018-03-23 |
Family
ID=61643082
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710168858.2A Pending CN107831219A (en) | 2017-03-20 | 2017-03-20 | The Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107831219A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111157648A (en) * | 2020-01-03 | 2020-05-15 | 中国石油化工股份有限公司 | Rapid quantitative analysis method for saturated hydrocarbon gas chromatography in crude oil sample |
| CN112798698A (en) * | 2020-11-30 | 2021-05-14 | 潍坊学院 | Oil fingerprint identification method for selecting biomarkers based on difference degree of main components |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101936973A (en) * | 2009-06-30 | 2011-01-05 | 中国石油化工股份有限公司石油化工科学研究院 | Method for rapidly classifying hydrocarbon oil with combined gas-phase chromatography-mass spectrometryer |
| CN101413931B (en) * | 2008-11-25 | 2011-07-27 | 大庆油田有限责任公司 | Biomarker gas chromatograph-high resolved flight time mass spectrographic analysis method in crude oil or sediment |
| CN102608235B (en) * | 2012-04-06 | 2013-11-13 | 中国石油天然气股份有限公司 | Method for analyzing biomarkers in natural gas |
-
2017
- 2017-03-20 CN CN201710168858.2A patent/CN107831219A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101413931B (en) * | 2008-11-25 | 2011-07-27 | 大庆油田有限责任公司 | Biomarker gas chromatograph-high resolved flight time mass spectrographic analysis method in crude oil or sediment |
| CN101936973A (en) * | 2009-06-30 | 2011-01-05 | 中国石油化工股份有限公司石油化工科学研究院 | Method for rapidly classifying hydrocarbon oil with combined gas-phase chromatography-mass spectrometryer |
| CN102608235B (en) * | 2012-04-06 | 2013-11-13 | 中国石油天然气股份有限公司 | Method for analyzing biomarkers in natural gas |
Non-Patent Citations (2)
| Title |
|---|
| ZHENDI WANG等: "Fractionation of a Light Crude Oil and Identification and Quantitation of Aliphatic, Aromatic, and Biomarker Compounds by GC-FID and GC-MS, Part II", 《JOURNAL OF CHROMATOGRAPHIC SCIENCE》 * |
| 徐真等: "冀中地区文安油田原油非均质性及其意义", 《石油与天然气地质》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111157648A (en) * | 2020-01-03 | 2020-05-15 | 中国石油化工股份有限公司 | Rapid quantitative analysis method for saturated hydrocarbon gas chromatography in crude oil sample |
| CN112798698A (en) * | 2020-11-30 | 2021-05-14 | 潍坊学院 | Oil fingerprint identification method for selecting biomarkers based on difference degree of main components |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Qigui et al. | Quantitative characterization of shale oil in different occurrence states and its application | |
| Swinnerton et al. | Determination of the C1 to C4 hydrocarbons in sea water by gas chromatography | |
| Hill et al. | Modeling of gas generation from the Barnett shale, Fort Worth Basin, Texas | |
| Li et al. | Experimental investigation of shale oil recovery from Qianjiang core samples by the CO 2 huff-n-puff EOR method | |
| Liu et al. | Thermochemical sulphate reduction (TSR) versus maturation and their effects on hydrogen stable isotopes of very dry alkane gases | |
| US20180134964A1 (en) | Pyrolysis to determine hydrocarbon expulsion efficiency of hydrocarbon source rock | |
| CN102253136A (en) | Method for analyzing carbon isotopes of micro single hydrocarbons in natural gas | |
| CN107831219A (en) | The Rapid identification analysis method of saturation hydrocarbon system row biomarker in crude oil sample | |
| Zhu et al. | Origin of diamondoid and sulphur compounds in the Tazhong Ordovician condensate, Tarim Basin, China: Implications for hydrocarbon exploration in deep-buried strata | |
| CN102608235B (en) | Method for analyzing biomarkers in natural gas | |
| CN105548377B (en) | A kind of method and device for judging crude oil output layer | |
| CN106996966B (en) | A kind of device and method of online quickly analysis oil component | |
| Wang et al. | Origin of deep sour natural gas in the Ordovician carbonate reservoir of the Tazhong Uplift, Tarim Basin, northwest China: Insights from gas geochemistry and formation water | |
| CN104133242B (en) | A kind of method for sentencing the oil-gas possibility for knowing underlying strata construction | |
| CN105975761B (en) | A kind of method and device of determining Oil-gas Accumulation Types | |
| US20050082473A1 (en) | Mobile system for in situ acquisition of carbon isotope data on natural gas | |
| CN105866293A (en) | Method for identifying coal-formed gas and oil type gas by combining He and N2 and application of method | |
| CN104749303A (en) | Mud shale thermal release C5-C14 hydrocarbon preparation and online chromatographic analysis method | |
| CN109387577B (en) | Analysis device for analyzing gaseous hydrocarbon isotope in fluid inclusion | |
| CN111157648A (en) | Rapid quantitative analysis method for saturated hydrocarbon gas chromatography in crude oil sample | |
| CN103760004B (en) | Solvent desorption device and method | |
| Ghosh et al. | Analysis of siloxanes in hydrocarbon mixtures using comprehensive two-dimensional gas chromatography | |
| CN107831220A (en) | The Rapid identification analysis method of aromatic hydrocarbons series of biologic mark in crude oil sample | |
| CN102809558B (en) | Method for measuring polycyclic aromatic hydrocarbons (PAHs) of sea water in flow injection chemiluminescence way | |
| CN206362695U (en) | Double light path modulation detection system in a kind of infrared spectrum gas detection logging |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180323 |
|
| RJ01 | Rejection of invention patent application after publication |