CN107796863A - Method that is a kind of while determining various trace elements in reservoir cement - Google Patents
Method that is a kind of while determining various trace elements in reservoir cement Download PDFInfo
- Publication number
- CN107796863A CN107796863A CN201610751393.9A CN201610751393A CN107796863A CN 107796863 A CN107796863 A CN 107796863A CN 201610751393 A CN201610751393 A CN 201610751393A CN 107796863 A CN107796863 A CN 107796863A
- Authority
- CN
- China
- Prior art keywords
- sample
- reservoir
- degrading
- degrade
- cement
- 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
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/64—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pathology (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Immunology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Biomedical Technology (AREA)
- Engineering & Computer Science (AREA)
- Toxicology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention provides method that is a kind of while determining various trace elements in reservoir cement, it uses laser ablation inductively coupled plasma-mass spectrometry micro-region analysis technique, including reservoir cement sample preparation, remove reservoir cement sample and the pollutant on standard sample surface, instrument parameter optimization is carried out using standard sample, then the content of various trace elements in reservoir cement is determined by using line scanning or the single-point mode of degrading and carries out Data Management Analysis.Method provided by the invention can be in Accurate Determining reservoir cement various trace elements content, can be applied to depositional environment, diagenetic process and phase time research of reservoir, there is the advantages of measure element is more, detection limit is low, analysis precision is high.
Description
Technical field
The invention belongs to laser ablation-inductivity coupled plasma mass spectrometry micro-region analysis technique field, more particularly to one kind
Various trace elements in reservoir cement are determined using laser ablation-inductivity coupled plasma mass spectrometry micro-region analysis technique simultaneously
Method.
Background technology
Cement refers to the chemical precipitates for the diagenesis phase cementation being played between rock particles.Main cements are siliceous
(quartz, calcedony etc.), carbonate mineral (calcite, dolomite etc.), next to that irony (bloodstone, limonite etc.), sometimes may be used
See sulfate mineral (gypsum, anhydrite etc.), zeolite minerals (analcime, laumontite etc.), clay mineral (kaolinite, water cloud
Mother, chlorite etc.).Cement is the important record for showing rock Diagenetic History, analysis cement formation phase, forms environment pair
The control action of its reservoir properties, the pore evolution history and progress reservoir prediction for Study In Reservoir are significant, and glue
Tie thing structure with trace element composition be inverting Diagenesis fluids property in diagenesis research (such as temperature, pressure, pH value, from
Son is formed etc.) important means, but the micro- information in accurate analysis cement is then restricted by self-condition.
Relative to traditional method for dissolving whole sample comminution, microcell technology can be disclosed existing for inside sample itself
Inhomogeneity, more fully geochemistry support is provided for geologic interpretation, is mainly had for cement micro-zone analysis at present following
Two ways：
1st, off-line analysis
Off-line analysis technology typically uses Microcell sampling instrument, and current commercialized micro- drill sampling system carries real-time light
Imaging system is learned, very can easily and accurately choose sample object position.Sample is distinguished into sanding and polishing Cheng Guang up and down before sampling
Clean plane.Then sample is fixed on micro- brill operating desk.Sample position is chosen by micro imaging system, micro- brill is adjusted and inclines
Angle, start to sample after setting the running parameters such as sampling depth, rate of penetration.After sample collection, pass through Wet
Trace element and isotopics are determined after processing, measuring accuracy is higher, and analysis project is more.The number of sampling amount depends on
Post analysis project.But due to needing to be chemically treated, flow is cumbersome time-consuming, and experimental period is longer, while need strict
Control chemical process blank, and sample diameter (100-200 μm) and depth selection (100-200 μm) it is larger, spatial resolution compared with
It is low, then can not accurately it be drilled through for less cement.
2nd, on-line analysis
At present, on-line analysis technology mainly has three kinds of methods：ESEM, electron probe and laser ablation micro-zone analysis skill
Art.
ESEM (SEM) is a kind of microscopic appearance scanning electron microscopy between transmission electron microscope and light microscope
Sem observation means, directly it can carry out microcosmic imaging using the material performance of sample surfaces material.ESEM has higher put
Big multiple, continuously adjusted between ten thousand times of 20-200；With the very big depth of field, the visual field is big, is imaged rich in third dimension, can directly see
The fine structure on the uneven surface of various samples is examined, and the sample of ESEM is prepared simply.The resolution ratio of ESEM
Reach 1nm, by secondary electron image can be clearly observable the surface appearance features of Nano/micron mineral, micropore form
And distribution etc., and then be that the origin cause of formation and evaluating reservoir of rock etc. provide foundation, current ESEM is equipped with X-ray energy spectrometer
Device, observation and the Microanalysis of displaing micro tissue topography can be so carried out simultaneously.ESEM typically does sxemiquantitative point
Analysis, detection are limited to 10-4G/g, test elements are mainly macroelement.But ESEM can only be carried out to the material of sample surfaces
Imaging, observation analysis is unable to the material for being not presented at sample surfaces.
Laser ablation micro-region analysis technique is primarily referred to as laser ablation system connection inductivity coupled plasma mass spectrometry, its base
Present principles are that laser microbeam is focused on into sample surfaces to be allowed to corrode gasification, and sample particulate is delivered into electricity in plasma by carrier gas
From, then through mass spectrometer system progress mass filter, finally detect the ion of different charge-mass ratios respectively with receiver, can carry out polynary
Measure and isotopic ratio determine element simultaneously.Detection elements include macroelement, trace element and rare earth element, and detection is limited to
10-9-10-6G/g, analysis precision RSD 5%-10%.
Laser ablation micro-region analysis technique with it is in situ, in real time, quickly analysis advantage and higher sensitivity, preferably
Spatial resolution, multi element analysis and can provide application of the detectability of isotope ratio value information in rock micro-zone analysis and get over
Come more, but have no report using application of the laser ablation-Inductive coupling techniques in cement, not established a kind of will swash
Light degrades-the Inductive coupling techniques method that is applied to cement trace element analysis.
The content of the invention
In order to solve problem of the prior art, the present invention is micro- by using laser ablation-inductivity coupled plasma mass spectrometry
Area's analytical technology provides a kind of analysis method that can determine various trace elements in reservoir cement simultaneously.
In order to achieve the above object, the present invention adopts the following technical scheme that：
Method that is a kind of while determining various trace elements in reservoir cement, it uses laser ablation-inductive etc.
Gas ions mass spectrum micro-region analysis technique, comprises the following steps：1) reservoir cement sample preparation, 2) remove reservoir cement sample
With standard sample surface contaminant, 3) using standard sample carry out instrument parameter optimization, 4) using line scanning or single-point degrade
Mode determines the content of various trace elements in reservoir cement sample and carries out Data Management Analysis.
According to an embodiment of the invention, the detailed process of reservoir cement sample preparation is to incite somebody to action in the step 1)
It is (20-40) mm × (10-20) mm × (0.5-1.5) mm that cement reservoir rock sample, which cuts into length × width × height size, excellent
(30 ± 0.1) mm × (15 ± 0.1) mm × (1 ± 0.1) mm (length × width × height) thin slice is selected, then will be thin using epoxy resin
Piece is fixed on slide, polishing, is wiped sample surfaces with cotton ball soaked in alcohol.
According to an embodiment of the invention, sample and mark are removed by using dust technology cleaning in the step 2)
Quasi- sample surfaces pollutant, the concentration of the dust technology is preferably 0.5wt%-5wt%.
According to an embodiment of the invention, the instrument parameter optimization includes：With NBS (NIST)
Standard specimen NIST SRM610 or NIST SRM612 do instrument optimization, with US Geological Survey's standard sample carbonate standard specimen
MACS-3, basalt glass standard specimen BCR-2G, BHVO-2G and BIR-1G do external standard calibration curve.
According to an embodiment of the invention, selected during laser ablation-inductively coupled plasma micro-zone analysis
Make carrier gas with helium, argon gas is compensation gas, and to adjust sensitivity, the two is logical before inductively coupled plasma (ICP) is entered
Cross a T connector mixing.After instrument is lighted, stable 10-30min, preferably 20min, carrier gas and the optimization of compensation gas pass through stripping
Erosion NIST SRM610 make 7Li, 115In, and 232Th signals reach most strong；
According to an embodiment of the invention, to reduce the interference of oxide yield and monovalent ion, NIST is being degraded
During SRM610, ThO/Th ratio is less than 0.3%, Ca2+/Ca+Ratio less than 0.70%, 238U/232Th ratio be about 1.
According to an embodiment of the invention, the line scanning, which is degraded, to be comprised the following steps：
1. degrade in advance：In order to remove sample surfaces pollution, using laser spot beam first, denuding process is for 120-180 μm
80-120 μm/s condition of degrading is entered line scan to target area sample and degraded in advance, and detector is not examined during pre- degrade
Survey, purging 50-70s is carried out after the completion of degrading；
2. line scanning is degraded：Done in the duct degraded in advance per 0.8-1.2mm and once focus into line scan and degrade, line is swept
Retouch and degrade 35-45 μm of laser spot beam, 3-7 μm of denuding process/s, in order to ensure that laser preferably focuses on sample surfaces,
Degrade the small duct of 5 tandem arrays altogether, before degrading every time, all block laser first and carry out blank counts 10-20s, connect
Into line scan and degrade；
3. remove residue：After sample degrades, continue to purge 40-80s, ensure that residual does not influence next in sample room
Sample determines.
According to an embodiment of the invention, the single-point, which degrades, to be comprised the following steps：
1. degrade in advance：In order to remove sample surfaces pollution, using laser spot beam first, denuding process is for 120-180 μm
80-120 μm/s condition of degrading is entered line scan to target area sample and degraded in advance, and detector is not examined during pre- degrade
Survey；
2. single-point degrades：Laser spot beam diameter is 30-50 μm in single-point denudation, during laser sampling, is hidden first
Keep off laser beam and carry out blank counts 15-35s, then point position each to sample carries out continuously degrading 40-60s, finally stops degrading,
Continue to count 15-35s, each bulk analysis time 70-130s for putting position when cleaning sampling system with helium purge,；
3. remove residue：After sample degrades, continue to purge 60s, ensure that residual does not influence next sample in sample room
Product determine.
Preferably, degrade online or single-point degraded in test process, often determine 5 samples after, with MACS-3, BCR-2G,
BHVO-2G and BIR-1G does an external standard calibration curve.
Beneficial effects of the present invention：
Determined simultaneously based on laser ablation-inductivity coupled plasma mass spectrometry micro-region analysis technique the invention provides one kind
The analysis method of various trace elements in reservoir cement.5-300 μm of aperture is degraded, reservoir rock matrix is avoided and tradition is molten
Pollution and interference of the quadrat method to object element, more reliable micro- information is obtained with smaller less sample, relative to
The methods of ESEM, electron probe, measure element is more, detection limit is low, analysis precision is high, passes through the micro- information of acquisition
The depositional environment, diagenesis process and phase time of reservoir can be disclosed, technical support is provided for oil-gas exploration and development.
Brief description of the drawings
Fig. 1 is reservoir cement trace element coatings by situ flow chart of the present invention.
Embodiment
The present invention is described in detail with reference to embodiments, but the present invention is not limited by following embodiments.
Embodiment 1
Method that is a kind of while determining various trace elements in reservoir cement, it uses laser ablation-inductive etc.
Gas ions mass spectrum micro-region analysis technique, comprises the following steps：
1) reservoir cement sample preparation：Reservoir cement rock sample is cut into the thin of 20mm × 10mm × 0.5mm
Piece, thin slice is fixed on slide using epoxy resin, then polishes, is wiped sample surfaces using cotton ball soaked in alcohol；
2) reservoir cement sample and standard sample surface contaminant are removed：Before sample test is carried out, concentration
For 0.5wt% dust technology by testing sample and standard sample carry out be cleaned by ultrasonic remove surface pollutant；
3) instrument parameter optimization is carried out using standard sample：Marked in the present embodiment from NBS (NIST)
Sample NIST SRM610 carry out instrument optimization, with US Geological Survey standard sample carbonate standard specimen MACS-3, basalt glass
Standard specimen BCR-2G, BHVO-2G and BIR-1G do external standard calibration curve；
After instrument is lighted, 10min stable first, carrier gas, argon gas are made using helium during laser ablation of the present invention
To compensate gas, with adjust sensitivity, helium and argon gas before inductively coupled plasma (ICP) is entered it is T-shaped by one
Joint mixes, and carrier gas and the optimization of compensation gas make 7Li, 115In by degrading NIST SRM610, and 232Th signals reach most strong；
To reduce the interference of oxide yield and monovalent ion, when degrading NISTSRM610, ThO/Th ratio is less than 0.3%, Ca2 +/Ca+Ratio less than 0.70%, 238U/232Th ratio be about 1.
4) content of various trace elements in line sweep measuring reservoir cement sample is used, is comprised the following steps that：
1. degrade in advance：In order to remove sample surfaces pollution, laser spot beam is used as 120 μm, and denuding process is 80 μm/s's
Degrade condition line scan is entered to target area sample and degrade in advance, detector does not detect during pre- degrade, after the completion of degrading
Carry out purging 50s；
2. line scans：Done in the duct degraded in advance per 0.8mm and once focus into line scan and degrade, line scanning is degraded sharp
35 μm of hot spot beam, 4 μm/s of denuding process, in order to ensure that laser preferably focuses on sample surfaces, degrade 5 head altogether
The small duct of tail linking, before degrading every time, laser is all blocked first and carries out blank counts 10s, then enters line scan and degrades；
3. remove residue：After each sample degrades, continue to purge 40s, under the influence of ensureing that residual is not in sample room
Individual sample measure.
After often determining 5 samples, an external standard calibration curve is done with MACS-3, BCR-2G, BHVO-2G and BIR-1G.
Embodiment 2-4
Using the method in embodiment 1, change the size of thin slice and the mass concentration of dust technology, as shown in table 1
Table 1
| Lamina dimensions (length × width × height) | Concentration of nitric acid | |
| Embodiment 2 | 40mm×15mm×1.5mm | 5wt% |
| Embodiment 3 | 30mm×15mm×1mm | 2wt% |
| Embodiment 4 | 30.1mm×15.1mm×1.1mm | 2.5wt% |
Embodiment 5
Using the method for embodiment 3, change the parameter setting in line scanning process, line scanning process is：
1. degrade in advance：In order to remove sample surfaces pollution, laser spot beam is used as 180 μm, and denuding process is 120 μm/s's
Degrade condition line scan is entered to target area sample and degrade in advance, detector does not detect during pre- degrade, after the completion of degrading
Carry out purging 70s；
2. line scans：Done in the duct degraded in advance per 1.2mm and once focus into line scan and degrade, line scanning is degraded sharp
45 μm of hot spot beam, 6 μm/s of denuding process, in order to ensure that laser preferably focuses on sample surfaces, degrade 5 head altogether
The small duct of tail linking, before degrading every time, laser is all blocked first and carries out blank counts 20s, then enters line scan and degrades；
3. remove residue：After each sample degrades, continue to purge 80s, under the influence of ensureing that residual is not in sample room
Individual sample measure.
After often determining 5 samples, an external standard calibration curve is done with MACS-3, BCR-2G, BHVO-2G and BIR-1G.
Embodiment 6
Using the method for embodiment 3, change the parameter setting in line scanning process, line scanning process is：
1. degrade in advance：In order to remove sample surfaces pollution, laser spot beam is used as 150 μm, and denuding process is 100 μm/s's
Degrade condition line scan is entered to target area sample and degrade in advance, detector does not detect during pre- degrade, after the completion of degrading
Carry out purging 60s；
2. line scans：Done in the duct degraded in advance per 1mm and once focus into line scan and degrade, laser is degraded in line scanning
40 μm of spot beam, 5 μm/s of denuding process, in order to ensure that laser preferably focuses on sample surfaces, degrade 5 head and the tail altogether
The small duct of linking, before degrading every time, laser is all blocked first and carries out blank counts 15s, then enters line scan and degrades；
3. remove residue：After each sample degrades, continue to purge 60s, under the influence of ensureing that residual is not in sample room
Individual sample measure.
After often determining 5 samples, an external standard calibration curve is done with MACS-3, BCR-2G, BHVO-2G and BIR-1G.
Embodiment 7
Method that is a kind of while determining various trace elements in reservoir cement, it uses laser ablation-inductive etc.
Gas ions mass spectrum micro-region analysis technique, using the method for embodiment 3, mode is degraded in change, using using the simple scan side of degrading
The content of various trace elements in formula measure reservoir cement sample, single-point, which degrades, to be comprised the following steps that：
1. degrade in advance：In order to remove sample surfaces pollution, laser spot beam is used first as 150 μm, denuding process is 100 μ
M/s condition of degrading is entered line scan to target area sample and degraded in advance, and detector does not detect during pre- degrade；
2. single-point degrades：Laser spot beam diameter is 40 μm in single-point denudation, during laser sampling, is blocked first sharp
Light beam carries out blank counts 25s, and then point position each to sample carries out continuously degrading 50s, finally stops degrading, uses helium purge
Continue to count 25s, each bulk analysis time 100s for putting position when cleaning sampling system,；
3. remove residue：After each sample degrades, continue to purge 60s, under the influence of ensureing that residual is not in sample room
Individual sample measure.
After often determining 5 samples, an external standard calibration curve is done with MACS-3, BCR-2G, BHVO-2G and BIR-1G.
Embodiment 8
Using the method for embodiment 7, change the parameter setting in single-point denudation, single-point denudation is：
1. degrade in advance：In order to remove sample surfaces pollution, laser spot beam is used first as 180 μm, denuding process is 120 μ
M/s condition of degrading is entered line scan to target area sample and degraded in advance, and detector does not detect during pre- degrade；
2. single-point degrades：Laser spot beam diameter is 60 μm in single-point denudation, during laser sampling, is blocked first sharp
Light beam carries out blank counts 35s, and then point position each to sample carries out continuously degrading 60s, finally stops degrading, uses helium purge
Continue to count 35s, each bulk analysis time 130s for putting position when cleaning sampling system,；
3. remove residue：After each sample degrades, continue to purge 80s, under the influence of ensureing that residual is not in sample room
Individual sample measure.
After often determining 5 samples, an external standard calibration curve is done with MACS-3, BCR-2G, BHVO-2G and BIR-1G.
Embodiment 9
Using the method for embodiment 7, change the parameter setting in single-point denudation, single-point denudation is：
1. degrade in advance：In order to remove sample surfaces pollution, laser spot beam is used first as 150 μm, denuding process is 100 μ
M/s condition of degrading is entered line scan to target area sample and degraded in advance, and detector does not detect during pre- degrade；
2. single-point degrades：Laser spot beam diameter is 40 μm in single-point denudation, during laser sampling, is blocked first sharp
Light beam carries out blank counts 25s, and then point position each to sample carries out continuously degrading 50s, finally stops degrading, uses helium purge
Continue to count 25s, each bulk analysis time 100s for putting position when cleaning sampling system,；
3. remove residue：After each sample degrades, continue to purge 60s, under the influence of ensureing that residual is not in sample room
Individual sample measure.
After often determining 5 samples, an external standard calibration curve is done with MACS-3, BCR-2G, BHVO-2G and BIR-1G.
Claims (9)
1. method that is a kind of while determining various trace elements in reservoir cement, it is characterised in that using laser ablation-inductance
Coupled plasma mass spectrometry micro-region analysis technique, comprises the following steps：1) it is cementing reservoir cement sample preparation, 2) to remove reservoir
Thing sample and standard sample surface contaminant, 3) instrument parameter optimization is carried out using standard sample, 4) using line scanning or single
The point mode of degrading determines the content of various trace elements in reservoir cement sample and carries out Data Management Analysis.
2. according to the method for claim 1, it is characterised in that the sample preparation of reservoir cement is specific in the step 1)
Process is that cement reservoir rock sample is cut into length × width × height size is (20-40) mm × (10-20) mm × (0.5-
1.5) mm, preferably (30 ± 0.1) mm × (15 ± 0.1) mm × (1 ± 0.1) mm thin slice, then using epoxy resin by thin slice
It is fixed on slide, polishes, wiped sample surfaces with cotton ball soaked in alcohol.
3. method according to claim 1 or 2, it is characterised in that in the step 2), come by using dust technology cleaning
Sample and standard sample surface contaminant are removed, the concentration of the dust technology is preferably 0.5%-5%.
4. according to the method any one of claim 1-3, it is characterised in that the instrument parameter optimization includes：With U.S.
State Standard Bureau of state standard specimen NIST SRM610 or NIST SRM612 does instrument optimization, with US Geological Survey's standard sample carbon
Hydrochlorate standard specimen MACS-3, basalt glass standard specimen BCR-2G, BHVO-2G and BIR-1G do external standard calibration curve.
5. according to the method any one of claim 1-4, it is characterised in that in laser ablation-inductively coupled plasma
Make carrier gas from helium during body micro-zone analysis, argon gas is compensation gas, and the two leads to before inductively coupled plasma is entered
Cross a T connector mixing.
6. according to the method any one of claim 1-5, it is characterised in that step 3) the instrument parameter optimization bag
Include：After instrument is lighted, stable 10-30 minutes, carrier gas and the optimization of compensation gas make 7Li, 115In by degrading NIST SRM610,
232Th signals reach most strong.
7. according to the method for claim 6, it is characterised in that when degrading NIST SRM610, ThO/Th ratio is less than
0.3%, Ca2+/Ca+Ratio less than 0.70%, 238U/232Th ratio be about 1.
8. according to the method any one of claim 1-7, it is characterised in that the line scanning is degraded including following step
Suddenly：
1. degrade in advance：In order to remove sample surfaces pollution, laser spot beam is used first as 120-180 μm, denuding process 80-
120 μm/s condition of degrading is entered line scan to target area sample and degraded in advance, and detector does not detect during pre- degrade, and shells
Purging 50-70s is carried out after the completion of erosion；
2. line scanning is degraded：Done in the duct degraded in advance per 0.8-1.2mm and once focus into line scan and degrade, line scanning stripping
Lose 35-45 μm of laser spot beam, 3-7 μm of denuding process/s, degrade the small ducts of 5 tandem arrays altogether, before degrading every time, all
Laser is blocked first and carries out blank counts 10-20s, is then entered line scan and is degraded；
3. remove residue：After each sample degrades, continue to purge 40-80s, ensure that residual does not influence next in sample room
Sample determines；
After often determining 5 samples, an external standard calibration curve is done with MACS-3, BCR-2G, BHVO-2G and BIR-1G.
9. according to the method any one of claim 1-8, it is characterised in that the single-point, which degrades, to be comprised the following steps：
1. degrade in advance：In order to remove sample surfaces pollution, laser spot beam is used first as 120-180 μm, denuding process 80-
120 μm/s condition of degrading is entered line scan to target area sample and degraded in advance, and detector does not detect during pre- degrade；
2. single-point degrades：Laser spot beam diameter is 30-50 μm in single-point denudation, during laser sampling, is blocked first sharp
Light beam carries out blank counts 15-35s, and then point position each to sample carries out continuously degrading 40-60s, finally stops degrading, uses helium
Air-blowing is cleared away to be continued to count 15-35s, each bulk analysis time 70-130s for putting position when washing sampling system, and each sample has degraded
Bi Hou, continue to purge 40-80s, remaining in guarantee sample room, which does not influence next sample, degrades；
3. remove residue：After each sample degrades, continue to purge 40-80s, ensure that residual does not influence next in sample room
Sample determines；
After often determining 5 samples, an external standard calibration curve is done with MACS-3, BCR-2G, BHVO-2G and BIR-1G.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610751393.9A CN107796863A (en) | 2016-08-29 | 2016-08-29 | Method that is a kind of while determining various trace elements in reservoir cement |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610751393.9A CN107796863A (en) | 2016-08-29 | 2016-08-29 | Method that is a kind of while determining various trace elements in reservoir cement |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107796863A true CN107796863A (en) | 2018-03-13 |
Family
ID=61528781
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610751393.9A Pending CN107796863A (en) | 2016-08-29 | 2016-08-29 | Method that is a kind of while determining various trace elements in reservoir cement |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107796863A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110793991A (en) * | 2019-10-12 | 2020-02-14 | 国家地质实验测试中心 | Analytical method for occurrence state of Re in sedimentary rock |
| CN110806405A (en) * | 2019-10-16 | 2020-02-18 | 中国地质大学（武汉） | Method for determining hydrothermal activity age of carbonate reservoir |
| CN112577903A (en) * | 2020-11-26 | 2021-03-30 | 中国石油天然气股份有限公司 | Method for determining scanning parameters of carbonate rock trace element laser surface scanning |
| CN112858627A (en) * | 2020-12-25 | 2021-05-28 | 核工业北京地质研究院 | Method for determining uranium deposit cause by using rare earth element characteristics of uranium minerals |
| CN113720897A (en) * | 2021-08-13 | 2021-11-30 | 中冶南方都市环保工程技术股份有限公司 | Method for accurately measuring chemical components of film-shaped structure in situ and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105334150A (en) * | 2015-11-24 | 2016-02-17 | 中国石油大学(北京) | Method for determining diagenetic process and porosity evolution process of foreland basin sandstone reservoir |
-
2016
- 2016-08-29 CN CN201610751393.9A patent/CN107796863A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105334150A (en) * | 2015-11-24 | 2016-02-17 | 中国石油大学(北京) | Method for determining diagenetic process and porosity evolution process of foreland basin sandstone reservoir |
Non-Patent Citations (2)
| Title |
|---|
| 汪正: "《原子光谱分析基础与应用》", 31 January 2015, 上海科学技术出版社 * |
| 陈璐: "碳酸岩样品微量元素LA-ICP-MS微区原位准确分析方法研究", 《CNKI硕士论文全文数据库》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110793991A (en) * | 2019-10-12 | 2020-02-14 | 国家地质实验测试中心 | Analytical method for occurrence state of Re in sedimentary rock |
| CN110793991B (en) * | 2019-10-12 | 2022-05-27 | 国家地质实验测试中心 | Analytical method for occurrence state of Re in sedimentary rock |
| CN110806405A (en) * | 2019-10-16 | 2020-02-18 | 中国地质大学（武汉） | Method for determining hydrothermal activity age of carbonate reservoir |
| CN112577903A (en) * | 2020-11-26 | 2021-03-30 | 中国石油天然气股份有限公司 | Method for determining scanning parameters of carbonate rock trace element laser surface scanning |
| CN112858627A (en) * | 2020-12-25 | 2021-05-28 | 核工业北京地质研究院 | Method for determining uranium deposit cause by using rare earth element characteristics of uranium minerals |
| CN113720897A (en) * | 2021-08-13 | 2021-11-30 | 中冶南方都市环保工程技术股份有限公司 | Method for accurately measuring chemical components of film-shaped structure in situ and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107796863A (en) | Method that is a kind of while determining various trace elements in reservoir cement | |
| US9488605B2 (en) | Confocal XRF-CT system for mining analysis | |
| US9922811B2 (en) | Laser ablation cell | |
| CN111398403B (en) | Method for simultaneously determining forsterite value and trace elements in olivine | |
| CN105649615A (en) | Method for testing tight oil occurrence state of reservoir stratum through CT quantitative and three-dimensional visualization | |
| CN112927762B (en) | Method for determining high-precision age of micron-sized Xie stone | |
| CN103454300A (en) | Electronic probe line analysis quantitative test method of ultra-light element carbon | |
| CN113624830A (en) | In-situ micro-area calcite U-Pb dating method | |
| CN109060859B (en) | Analysis method for initial value of Os of sedimentary rock | |
| CN114383909A (en) | In-situ micro-area element analysis standard sample, preparation method and application | |
| CN113340852B (en) | Laser scattering detection device for processing damage of fiber reinforced ceramic matrix composite | |
| CN105807330A (en) | Method for rapidly recognizing mineral volume content of shale formation | |
| CN108761047A (en) | The detection method of long bubble in overflow down draw formed glass | |
| CN114894829B (en) | Electronic probe analysis method for testing F and Cl of olivine trace elements | |
| Baron | Measurement of fibers | |
| CN116203117B (en) | In-situ microcell garnet Lu-Hf annual determining method | |
| CN107941891A (en) | A kind of method of C-O isotopes in on-line period measure microcell carbonate | |
| CN115096639B (en) | Micro-area sampling and micro-analysis method for rock | |
| CN102890113A (en) | Method for abating mercury memory effect in ICP-MS (inductively coupled plasma-mass spectrometry) detection | |
| CN207488294U (en) | A kind of test sample positioning device on glass blister analyzer | |
| Liu et al. | Speleothem annual layers revealed by seasonal SIMS δ 18 O measurements | |
| CN112525976B (en) | Method for simultaneously analyzing water content, oxygen isotope and hydrogen isotope in water-containing mineral based on large-scale ion probe | |
| Sylvester | Trends in analytical developments and earth science applications in LA‐ICP‐MS and LA‐MC‐ICP‐MS for 2004 and 2005 | |
| CN105372275A (en) | Calibration method of martensite-austenite island in steel plate | |
| CN110208300B (en) | Method for defining fluid inclusion in ore-forming period of hydrothermal uranium ore based on scanning electron microscope |
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: 20180313 |
|
| RJ01 | Rejection of invention patent application after publication |