CN1262850C - Oil field tracing analysis and detection method using fluorobenzoic acid as tracer - Google Patents
Oil field tracing analysis and detection method using fluorobenzoic acid as tracer Download PDFInfo
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- CN1262850C CN1262850C CN 03146210 CN03146210A CN1262850C CN 1262850 C CN1262850 C CN 1262850C CN 03146210 CN03146210 CN 03146210 CN 03146210 A CN03146210 A CN 03146210A CN 1262850 C CN1262850 C CN 1262850C
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- 239000000700 radioactive tracer Substances 0.000 title claims abstract description 41
- 238000004458 analytical method Methods 0.000 title claims abstract description 13
- 238000001514 detection method Methods 0.000 title claims abstract description 13
- NSTREUWFTAOOKS-UHFFFAOYSA-N 2-fluorobenzoic acid Chemical compound OC(=O)C1=CC=CC=C1F NSTREUWFTAOOKS-UHFFFAOYSA-N 0.000 title abstract 2
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000005259 measurement Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 5
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims abstract description 4
- 239000003921 oil Substances 0.000 claims description 30
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 21
- 239000002253 acid Substances 0.000 claims description 17
- 238000012360 testing method Methods 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 9
- 238000002347 injection Methods 0.000 claims description 9
- 239000007924 injection Substances 0.000 claims description 9
- 238000001212 derivatisation Methods 0.000 claims description 8
- 239000012159 carrier gas Substances 0.000 claims description 7
- 241001597008 Nomeidae Species 0.000 claims description 5
- 239000003463 adsorbent Substances 0.000 claims description 5
- 238000005070 sampling Methods 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 238000012372 quality testing Methods 0.000 claims description 3
- XRKIHUXCUIFHAS-UHFFFAOYSA-N [4-(3-methoxy-3-oxopropyl)phenyl]boronic acid Chemical compound COC(=O)CCC1=CC=C(B(O)O)C=C1 XRKIHUXCUIFHAS-UHFFFAOYSA-N 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims description 2
- QNEFNFIKZWUAEQ-UHFFFAOYSA-N carbonic acid;potassium Chemical compound [K].OC(O)=O QNEFNFIKZWUAEQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims description 2
- 239000010779 crude oil Substances 0.000 claims description 2
- 238000012113 quantitative test Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- HGAZMNJKRQFZKS-UHFFFAOYSA-N chloroethene;ethenyl acetate Chemical compound ClC=C.CC(=O)OC=C HGAZMNJKRQFZKS-UHFFFAOYSA-N 0.000 claims 1
- 230000002596 correlated effect Effects 0.000 claims 1
- 230000008595 infiltration Effects 0.000 claims 1
- 238000001764 infiltration Methods 0.000 claims 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 abstract description 4
- 239000003129 oil well Substances 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- -1 fluorinated benzoic acid compound Chemical class 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract 1
- 238000009795 derivation Methods 0.000 abstract 1
- 238000004454 trace mineral analysis Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 244000005700 microbiome Species 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- LCALVNLSKDINOK-UHFFFAOYSA-N C(=O)O.FC=1C=CC=CC1 Chemical compound C(=O)O.FC=1C=CC=CC1 LCALVNLSKDINOK-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 239000012491 analyte Substances 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
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- 230000007613 environmental effect Effects 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- ZYJFGTCRTRQIAL-UHFFFAOYSA-N 1,2-difluorobenzene formic acid Chemical compound C(=O)O.FC1=C(C=CC=C1)F ZYJFGTCRTRQIAL-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960004365 benzoic acid Drugs 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000000451 chemical ionisation Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- OKIRSUTTZMRHLW-UHFFFAOYSA-N formic acid 1,2,3-trifluorobenzene Chemical compound C(=O)O.FC=1C(=C(C=CC1)F)F OKIRSUTTZMRHLW-UHFFFAOYSA-N 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002332 oil field water Substances 0.000 description 1
- XDEPVFFKOVDUNO-UHFFFAOYSA-N pentafluorobenzyl bromide Chemical compound FC1=C(F)C(F)=C(CBr)C(F)=C1F XDEPVFFKOVDUNO-UHFFFAOYSA-N 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
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Abstract
An oil field tracing and analysis detection method, in particular to a tracing and analysis detection method using a non-water-soluble reagent as an oil well tracer. The tracing method adopts fluorobenzoic acid (FBAs) as a tracing agent, adopts pretreatment means of samples such as filtration, derivation, solid phase extraction and the like during analysis and detection, and then adopts a gas chromatography-mass spectrometry combined technology to carry out trace analysis on the tracing agent. The method has the advantages of high detection precision, good recovery rate and high measurement sensitivity on FBAs, and can greatly reduce the using amount of the tracer, thereby reducing the using cost of the tracer, making the application of the fluorinated benzoic acid compound FBAs in high-temperature oil fields in China possible and making up the defects of the tracer in the high-temperature oil fields in China.
Description
Technical field
The present invention relates to spike of a kind of oil field and analyzing detecting method thereof, be specifically related to a kind of non-spike and the analyzing detecting method thereof of dissolubility reagent that discharge water as the oil well tracer agent.
Background technology
At present, waterflooding is the China and the main mode of production in many national oil fields in the world.The spike test is used for determining that the movement underground rule of oilfield injection water and direction anisotropic property have historical for many years between well, the spike test is exactly to add specific tracer agent by the water injection well place to injecting water between the water drive well, producing well sampling analysis tracer concentration around, obtain tracer concentration curve over time, carry out analysis-by-synthesis then, and draw method about information such as remaining oil saturations between border, field, swept volume, directional flow, undesired injection well, injection fluid relative velocity and swept volume, well.As a kind of online, real-time follow-up means, the spike test can also be used for testing the oily measure of taking on the well group that increases during the evaluation test effectively between the water drive well, adopts adjustment etc. as water blockoff, profile control, notes.
In brief, spike test is a kind of under the responding curve of well state, under the situation that ordinary production and stratum not have to injure between well, in order to obtain the means of testing of inner fluid and oil reservoir information on a large scale.And tracer agent is uniquely can enter oil reservoir and carry out fluid and the material of oil reservoir information.
Oil field tracing method commonly used at present comprises use radioisotope tracer and the non-insoluble chemical agent that discharges water, and the latter comprises halogenide, thiocyanate, nitrate, alcohols and other chemical tracer.Analytical approach commonly used has liquid scintillation counter activity analysis detection method and the HPGe gamma energy spectrometer activity detection method that is directed to radiotracer, also have to be specifically designed to the non-chromatography of ions (IC), high performance liquid chromatograph (HPLC) or ultraviolet (UV) spectrum detection method of putting tracer agent, spectrophotometric method, titrimetry, neutron activation method are also more common.
Used tracer agent great majority all have its limitation in the tracing method at present commonly used.For the non-tracer agent of putting, the tracer agent that has is because be naturally occurring in most of oil-field brines, and the error of background concentration has influenced the accurate measurement result of tracer agent greatly; Have plenty of because fancy price has seriously limited its practical application; The shortcoming of other tracer agent is that its microbial stability and chemical stability is relatively poor, often is that the tracer agent post analysis that comes into operation detects not come out.Its reason is that oil reservoir itself is a huge reduction system, can make the tracer agent generation chemical change of unstable chemcial property.And a large amount of bacteriums and microorganism under the normal temperature in the oil field have tangible biological degradation to tracer agent.There are problems such as environmental protection and personnel protection again in radiotracer.Therefore, the use of tracer agent has been subjected to very big restriction, even dropped into use, does not also often reach its intended purposes.
Based on reasons such as safety and environmental protection, the spike of oil field, countries in the world develops to low toxicity, low-residual, high sensitivity, non-direction such as put.And, 100,000 mouthfuls of the nearly oil-water wells of China's onshore oil field, tracer technique has vast potential for future development between well.Especially, the oil reservoir in oil field, domestic northwest mostly is high-temperature oil reservoir, and existing oil field tracing method can not well solve oil field spike problem, and the domestic tracing method that also is not applicable to the high temperature oil field; In addition, therefore the formulation of development plan and adjust to need big quantitative analysis data in northwest high temperature oil field secondary recovery and the tertiary recovery process, develops how better tracing method and the high-sensitivity analysis method is necessary.
Summary of the invention
The objective of the invention is to disclose and a kind ofly can be used for high temperature oil field, the accurate spike of effect and analyzing detecting method thereof.
The object of the present invention is achieved like this, and a kind of oil field tracing method uses fluorinated acid (FBAs) as tracer agent.
Do to show that the analyzing detecting method of oil field tracer agent comprises pre-treatment and two stages of analyzing and testing with fluorinated acid.In pretreatment stage, earlier with the sample filtering of obtaining, add internal standard compound matter then and regulate pH value, again sample is crossed post, wash-out, carry out derivatization treatment then, at last that sample concentration is to be measured in the acetonitrile.
In the analyzing and testing stage, about condition and parameter are set to:
GC input mode: adopt column sample injection or split sampling not
Sample injection time: 35～70s
The selection of capillary column: low polarity capillary column in the employing
Column temperature and flow rate of carrier gas control mode: the pillar temperature-rise period is for to rise to 140 ℃ from 60 ℃ of speed with 30～50 ℃/min, and the speed with 10～30 ℃/min rises to 280 ℃, constant temperature 1～2min again; Carrier gas stream is current constant mode, and speed is 0.8～2ml/min;
Injector temperature: 200～260 ℃
Quality testing mode: select ion scan mode (SIM)
Interface temperature: 200～260 ℃
EI source temperature: 200～250 ℃
The image data time: the zero-time of determining image data is 1～2min
At last, adopt a characteristic ion peak of target compound to carry out quantitative test.
The present invention with the fluorinated acid class as the oil field tracer agent, be because the fluorinated acid class has following character: the dynamic behavior of phenyl-monofluoride formic acid is almost completely consistent with HTO, thermodynamic stability and chemical stability are all fine, at high temperature not with reservoir fluid generation chemical reaction, also not by material absorption in the oil reservoir, its partition factor in oil and salt solution shows that also it has possessed most of condition that the oil field water-soluble tracer should possess.Some difluoro-benzene formic acid and trifluoro-benzene formic acid also possess most of condition of oil field tracer agent.Certainly, the fluorinated acid class also has certain limitation, can be degraded by microorganisms at normal temperatures, but when result of study shows their (70-175 ℃) uses at high temperature, the energy of bacterium and microorganism is very low, and it is degraded to lose to ignore and does not remember, therefore, the spike test is carried out in the high temperature oil field, more suitable with the fluorinated acid compounds.
Description of drawings
Fig. 1 tracer agent thermodynamic stability
Fig. 2 tracer agent chemical stability
Partition factor in Fig. 3 tracer agent oil/salt solution
The working curve of the 2-FBA that Fig. 4 and embodiment 1 corresponding method is measured
Embodiment
At first equally put in oil well and sampling with other non-tracer agent of putting fluorinated acid, and then obtain relevant data through pre-treatment and analysis to measure.
1. the pre-treatment of sample:
(1) sample filtering.Filtering removal with 0.45 μ m filtering membrane contains the tiny solid material and drips shape crude oil.
(2) add internal standard compound matter and regulate the sample pH value value.Select the 4-trifluoromethylbenzoic acid as interior mark, addition is advisable with the concentration (150,250) of 200ng/ml, then the pH value is transferred to 1.5 (1,2), makes it consistent with the media environment of extraction column, is beneficial to the extraction of analyte.
(3) adsorbent of crosslinked polystyrene as solid-phase extraction column selected in the Solid-Phase Extraction of measured object and desorb.Concrete extraction step is
1. activation: earlier soak into extraction column, cross post with the acetonitrile drip washing of certain volume again, and then with the hydrochloric acid of a certain amount of (about 25ml) adsorbent to be equilibrated to PH be 1.5 (1,2) with acetonitrile.Before carrying out in next one step, the pillar upper end will keep the liquid of certain volume, in order to avoid the pillar drying causes leakage.
2. go up sample: the sample of handling well is passed through extraction column with certain flow velocity.
3. dry post bed: passed through the post bed 10-15 minute with nitrogen, with the pillar drying.
4. wash-out: with the acetonitrile of Sq with the fluorinated acid wash-out.
5. concentrate: the heating cabinet that the sample behind the wash-out is put under the nitrogen protection is dried, again residue is dissolved in the acetonitrile about 200-300 μ l.
(4) derivatization treatment.
Make derivative reagent with PFBBr (1-bromo-2,3,4,5,6-phenyl-pentafluoride/2,3,4,5,6-five fluorobenzyl bromides), in the sample compound that needs are analyzed, introduce elements such as halogen, to carry out the highly sensitive analysis of selectivity with ECD or chemical ionization source by derivatization.The amount of derivative reagent is by the 200-1000 of derivant total amount doubly, and derivatization reaction is made catalyzer with solid carbonic acid potassium.
2. derivant is carried out the gas chromatography mass spectrometry method and carry out analyzing and testing, its actual conditions is as follows:
1. GC input mode: adopt column sample injection or split sampling not
2. the selection of capillary column: the DB-1701 type capillary column of low polarity in the employing
3. column temperature and flow rate of carrier gas control mode: the pillar temperature-rise period is for (30 ℃/min, 40 ℃/min) speed rises to 140 ℃ from 60 ℃ with 50 ℃/min, (10 ℃/min, 30 ℃/min) speed rises to 280 ℃, constant temperature 1min (1.5min, 2min) with 25 ℃/min again; Carrier gas stream is current constant mode 1.5ml/min (0.8ml/min, 2ml/min)
4. injector temperature: 200 ℃ (230 ℃, 260 ℃)
5. quality testing mode: select ion scan mode (SIM).
6. interface temperature: 200 ℃ (240 ℃, 260 ℃)
7. EI source temperature: 200 ℃ (220 ℃, 250 ℃)
8. image data time: the zero-time of determining image data is 2min (1min, 1.5min), so that than solvent slow 0.5～1min clipping time.Before this, the filament no power is avoided big solvent peak to enter the ion chamber and is made the disintegration of filament.
9. the selection of mark compound characteristic quasi-molecular ions in: mark compound one characteristic ion is measured in selected, so that carry out the correction of analyte concentration.It is 173 that this method adopts m/z.
The measurement effect of this method:
The working curve of the representative 2-fluobenzoic acid of the fluobenzoic acid class tracer agent that employing the present invention measures is seen accompanying drawing 4, and is as follows in detail:
| The lowest detection amount (〉=2S/N) | 0.002μg/L |
| The curve concentration range | 0.01～2μg/L |
| Cross over the concentration multiple | 200 times |
| R^2 | ≥0.9995 |
(note: above-mentioned concentration is the actual concentrations of tracer agent in oil-field water)
Embodiment 2.
Corresponding with embodiment 1, other condition is constant, and when correlation parameters such as pH value, temperature, carrier gas stream flow velocity and time all adopted first value in the bracket, measurement effect is: the lowest detection degree was 0.004 μ g/L; The curve width range is 0.02～4 μ g/L; Crossing over the concentration multiple is 200; R^2 〉=0.999.
Embodiment 3.
Corresponding with embodiment 1, when correlation parameter adopted in the bracket second class value, measurement effect is as follows: the lowest detection degree was 0.002 μ g/L; The curve width range is 0.01～2 μ g/L; Crossing over the concentration multiple is 200; R^2 〉=0.999.
Originally be operated in and adopt the 2-fluobenzoic acid to analyze in the fluobenzoic acid class, very representative.Because the molecular volume minimum of phenyl-monofluoride formic acid, and the interaction force between the adsorbent is also the most weak, and because the 2-fluobenzoic acid has the F atom to exist on the ortho position, steric effect is arranged in the derivatization process, by comparison, derive under the similarity condition ortho position of 2-FBA replaces than position and contraposition between 3-FBA, 4-FBA and replaces difficulty.In addition, there is document to prove: to wear the volume minimum in the leakage of the benzoic acid that is replaced by the F atom on the ortho position on same solid-phase extraction column, that is to say that adsorbent is to its adsorption capacity minimum, therefore, under the identical concentration, 2-FBA does not take place to leak and wears, and other fluorinated acid can not take place to leak yet to be worn.This work has solved the trace measurement of 2-FBA, and measurement lower limit reaches and be better than the effect of expectation fully, haves laid a good foundation as tracer agent for the fluorinated acid that further employing is different.
Claims (6)
1. make the oil field tracer analysis detection method of tracer agent with fluorinated acid for one kind, comprise two stages of pre-treatment and analyzing and testing, concrete steps are as follows:
(1), removes solid matter and drip shape crude oil with the spike sample filtering;
(2) add the 4-trifluoromethylbenzoic acid in the sample after filtering as interior mark compound, and pH value is transferred to 1～2;
(3) sample is extracted on extraction column and concentrates in the acetonitrile;
(4) sample is made derivatization treatment;
(5) carry out the derivant Measurement and analysis with the gas chromatography mass spectrometry method, correlated condition and parameter are selected as follows:
GC input mode: adopt column sample injection or split sampling not
Sample injection time: 35～70s
The selection of capillary column: low polarity capillary column in the employing
Column temperature and flow rate of carrier gas control mode: the pillar temperature-rise period is for to rise to 140 ℃ from 60 ℃ of speed with 30～50 ℃/min, and the speed with 10～30 ℃/min rises to 280 ℃, constant temperature 1～2min again; Carrier gas stream is current constant mode, and speed is 0.8～2ml/min;
Injector temperature: 200～260 ℃;
Quality testing mode: select ion scan mode SIM;
Interface temperature: 200～260 ℃;
EI source temperature: 200～250 ℃;
The image data time: the zero-time of determining image data is 1～2min;
At last, adopt a characteristic ion peak of target compound to carry out quantitative test.
2. analyzing detecting method as claimed in claim 1 is characterized in that: select for use crosslinked tygon to make the solid absorption material of extraction column.
3. analyzing detecting method as claimed in claim 1 is characterized in that: during extraction, earlier with acetonitrile infiltration, drip washing extraction column, the adsorbent pH value is transferred to 1～2 scope again.
4. analyzing detecting method as claimed in claim 1 is characterized in that: with 1-bromo-2,3,4,5, the 6-phenyl-pentafluoride was made derivative reagent when sample was made derivatization treatment, and its use amount is by the 200-1000 of derivant total amount doubly.
5. analyzing detecting method as claimed in claim 4 is characterized in that: when sample carries out derivatization treatment, make catalyzer with solid carbonic acid potassium.
6. analyzing detecting method as claimed in claim 1 is characterized in that: when carrying out the derivant Measurement and analysis with the gas chromatography mass spectrometry method, select DB-1701 type capillary column for use.
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| CN 03146210 CN1262850C (en) | 2003-07-04 | 2003-07-04 | Oil field tracing analysis and detection method using fluorobenzoic acid as tracer |
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| CN 03146210 CN1262850C (en) | 2003-07-04 | 2003-07-04 | Oil field tracing analysis and detection method using fluorobenzoic acid as tracer |
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| AU2012318521B2 (en) * | 2011-10-06 | 2015-12-03 | Landmark Graphics Corporation | Systems and methods for subsurface oil recovery optimization |
| CN102650207A (en) * | 2012-05-09 | 2012-08-29 | 中国石油天然气股份有限公司 | Interwell layered tracing monitoring method |
| CN103901149B (en) * | 2014-04-18 | 2015-07-29 | 中国海洋石油总公司 | The detection method of 2,3,4,5-tetrafluorobenzoic aid tracer agents in oil field extracted water |
| CN112682031B (en) * | 2019-10-18 | 2024-06-28 | 中国石油化工股份有限公司 | Oil field interwell tracer, tracing method and fracturing fluid |
| CN116577434A (en) * | 2023-05-26 | 2023-08-11 | 西南大学 | Rapid detection method for water-soluble tracer of multistage fracturing horizontal well |
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