CN110108737A - Rock natural section sample carbonate characterizing method - Google Patents
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- CN110108737A CN110108737A CN201910374284.3A CN201910374284A CN110108737A CN 110108737 A CN110108737 A CN 110108737A CN 201910374284 A CN201910374284 A CN 201910374284A CN 110108737 A CN110108737 A CN 110108737A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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Abstract
The present invention provides a kind of rock natural section sample carbonate characterizing method, which includes: step 1, chooses being partially placed into vacuum oven for energy representative sample feature；Step 2, the parameter of vacuum oven is set；Step 3, the sample of height 3mm~5mm is removed on the direction of vertical sample bed plane；Step 4, sample is stained in sample stake；Step 5, the sample stake that sample has been stained in step 4 is dried；Step 6, sample is focused, observed and identified, determine the type and distribution of carbonate, and estimate carbonate content.The rock natural section sample carbonate characterizing method can analyze and identify the type and distribution of carbonate with high-efficiency environment friendly, provide more acurrate reliable analysis data for petroleum exploration and development.
Description
Technical field
The present invention relates to In Oil Field Exploration And Development technical fields, especially relate to a kind of rock natural section sample carbonate
Characterizing method.
Background technique
Carbonate mineral is distributed more widely in oil and gas reservoir rock, either sedimentary rock or magmatic rock.Carbon in rock
Hydrochlorate some is distributed with graininess, and some is with the distribution of chink state.The method of conventional analysis identification carbonate has slice method
(SY/T 5368-2017), Electronic Speculum topography (SY/T 5162-2014) and acid extracting (SY/T 6867-2012) etc..But it
All must first go through Soxhlet extractor using the organic solvents such as benzene will crude oil in rock extract it is clean after just can be carried out into one
The operation processing of step, therefore not environmentally (toxic solvent is waved for analysis process long (extracting about 7 day time of one batch), process
Hair).In addition, slice method is also needed to identify carbonate using mineral photosensitiveness by way of thin-section staining and be named to mineral.Electricity
Mirror topography is mineral to be observed by mineral shape, but be difficult to determine mineral distributing position.It is wanted position has been determined
It could be named to mineral after measuring contained element by X-ray energy spectrometer.And acid extracting measurement content then assumes that institute in rock
Carbonate containing is all calcium carbonate to calculate its carbonate content, but carbonate type is many in fact, for example there are also white clouds
Stone, ankerite, siderite, smithsonite (ZnCO3), cerussite (PbCO3) etc..It is therefore desirable to look for a kind of more Efficient Ring
The method of guarantor determines the distribution even information such as content of carbonate.
When backscattered electron is beam bombardment sample in scanning electron microscope, reflected by the atomic nucleus of mineral element, through a high position
The electronics that back scattering probe is received and is imaged.The average atomic number high-positive correlation of back scattering picture and mineral, can reflect mine
Object pattern, moreover it is possible to reflect mineralogical composition, be the concentrated expression of pattern and ingredient.Rock sample backscattering analysis carbonate before
It has to extract by crude oil, polish and just can be carried out analysis with polishing treatment, working efficiency is low.
The method of traditional analysis identification carbonate has slice method (SY/T 5368-2017), Electronic Speculum topography (SY/T
5162-2014) and acid extracting (SY/T 6867-2012) etc..But they all must first go through Soxhlet extractor and have using benzene etc.
Solvent will just can be carried out further operation processing, therefore the long (extracting one of analysis process after the crude oil extracting completely in rock
The about 7 day time of a batch), process not environmentally (volatilization of toxic solvent).In addition, slice method also needs the side by thin-section staining
Formula identifies carbonate using mineral photosensitiveness and names to mineral.Electronic Speculum topography is that mineral are observed by mineral shape, still
It is difficult to determine mineral distributing position.It could be to mine after element contained by being measured by X-ray energy spectrometer position has been determined
Object is named.And acid extracting measurement content then assumes that institute's carbonate containing is all calcium carbonate to calculate its carbonate content in rock,
But carbonate type is many in fact, for example there are also dolomite, ankerite, siderite, smithsonite (ZnCO3), zinc powder
Mine (PbCO3) etc..
In order to protect environment, working efficiency is improved, rock characteristic is preferably characterized, it is naturally disconnected that we have invented a kind of rocks
Face sample carbonate characterizing method.
Summary of the invention
The object of the present invention is to provide types and distribution that one kind can analyze and identify carbonate with high-efficiency environment friendly, are stone
Exploration activity exploitation provides the rock natural section sample carbonate characterizing method of more acurrate reliable analysis data.
The purpose of the present invention can be achieved by the following technical measures: rock natural section sample carbonate characterizing method,
The rock natural section sample carbonate characterizing method includes: step 1, and the vacuum that is partially placed into for choosing energy representative sample feature is done
In dry case；Step 2, the parameter of vacuum oven is set；Step 3, removed on the direction of vertical sample bed plane height 3mm~
The sample of 5mm；Step 4, sample is stained in sample stake；Step 5, the sample stake that sample has been stained in step 4 is dried；Step
Rapid 6, sample is focused, observe and is identified, determines the type and distribution of carbonate, and estimates carbonate content.
The purpose of the present invention can be also achieved by the following technical measures:
In step 1, sample is having a size of 12mm × 10mm × 10mm, and wherein the direction of size 12mm will be with sample bed plane
In parallel.
In step 2, vacuum oven temperature parameter is set as 25 ± 1 DEG C, pressure parameter 1Pa, and time parameter is not
Less than 2 hours.
In step 3, the sample of height 3mm~5mm is removed with diagonal cutting pliers on the direction of vertical sample bed plane, and is made
Sample section it is smooth, the differences in height of sample surfaces is no more than 1mm.
In step 4, it is mixed into uniform paste with the white glue with vinyl of 1:1 and graphite powder, forms graphite latex；It will be real
It tests observation up, sample is stained in sample stake with the graphite latex modulated.
In steps of 5, it after the sample stake that sample has been stained in step 4 being dried 5 hours at normal temperature, is set according still further to step 2
Fixed method is dried.
Step 5 further includes, and by the sample prepared includes that sample stake is put into scanning electron microscope after the completion of dry, sets Electronic Speculum
Experiment parameter: acceleration voltage 10kV, sample chamber pressure are 60Pa, and electron beam operating distance is 8mm.
In step 6, sample is focused, observe and is identified with the signal of Electronic Speculum back scattering probe acquisition, determine carbon
The type and distribution of hydrochlorate.
Rock natural section sample carbonate characterizing method in the present invention, can provide a mesh for geological work personnel
Right carbonate type and distribution can preferably hold sample characteristic.The rock natural section sample carbonate characterizing method can
The type and distribution of carbonate are analyzed and identified with high-efficiency environment friendly, provide more acurrate reliable analysis number for petroleum exploration and development
According to.
Detailed description of the invention
Fig. 1 is the schematic diagram of dolomite and calcite back scattering picture in a specific embodiment of the invention；
Fig. 2 is the X rays topographs of calcite and the comparison diagram of back scattering picture in a specific embodiment of the invention；
Fig. 3 is the schematic diagram of carbonate mineral X rays topographs in a specific embodiment of the invention；
Fig. 4 is the schematic diagram of the carbonate back scattering picture of Fig. 3 in a specific embodiment of the invention；
Fig. 5 is the flow chart of a specific embodiment of rock natural section sample carbonate characterizing method of the invention.
Specific embodiment
To enable above and other objects, features and advantages of the invention to be clearer and more comprehensible, preferably implementation is cited below particularly out
Example, and cooperate shown in attached drawing, it is described in detail below.
As shown in figure 5, Fig. 5 is the structure chart of rock natural section sample carbonate characterizing method of the invention.
Step 101, being partially placed into vacuum oven for energy representative sample feature is chosen；
Step 102, vacuum oven temperature parameter is set as 25 ± 1 DEG C, and pressure parameter is 1Pa or so, and time parameter is
No less than 2 hours；
Step 103, the sample for removing height about 5mm with diagonal cutting pliers on the direction of vertical sample bed plane, guarantees as far as possible
Sample section it is smooth, the difference in height of sample surfaces is preferably not more than 1mm；
Step 104, it is mixed into uniform paste with the white glue with vinyl of 1:1 and graphite powder, we term it graphite latexes.
Germicidal efficacy is face-up, sample is stained in sample stake with the graphite latex modulated；
Step 105, after the sample stake that sample has been stained in step 104 being dried 5 hours at normal temperature, according still further to step 102
The method of setting is dried.Put it into scanning electron microscope after the completion of dry, set electron microscope experiment parameter: acceleration voltage as
10kV, sample chamber pressure are 60Pa, and electron beam operating distance is 8mm；
Step 106, sample is focused, observe and is identified with the signal of Electronic Speculum back scattering probe acquisition, determine carbonic acid
The type and distribution of salt, and estimate carbonate content.
In an application specific embodiment of the invention, comprising the following steps:
Step 1, selection can representative sample feature be partially placed into vacuum oven, specific size about 12mm ×
10mm × 10mm, wherein the direction of size 12mm is parallel with sample bed plane.
Step 2, vacuum oven temperature parameter is set as 25 DEG C, pressure parameter 1Pa, and time parameter is 2 hours；
Step 3, the sample for cutting height 3mm~5mm with diagonal cutting pliers on the direction of vertical sample bed plane, guarantees as far as possible
Sample section it is smooth, the difference in height of sample surfaces is preferably not more than 1mm；
Step 4, white glue with vinyl and graphite powder are uniformly mixed according to the ratio of 1:1, we and referred to as graphite latex, then
Sample is sticked in sample stake with graphite latex.The method set after drying 5 hours according still further to step 2 under room temperature is dried；
Step 5, the sample after drying is put into scanning electron microscope.Set electron microscope experiment parameter: acceleration voltage 10kV, sample
Product chamber pressure is 60Pa, and electron beam operating distance is 8mm；
Step 6, observation identification is carried out to sample with Electronic Speculum back scattering picture and taken pictures, according to the gray scale sequence of table 1, determine carbon
The type and distribution of hydrochlorate.Average atomic number is smaller, and gray scale is lower；It is on the contrary then higher.
1 carbonate average atomic number table of table
| Title | Molecular formula | Molecular weight | Average atomic number |
| Dolomite | CaMg(CO3)2 | 184 | 10.9 |
| Calcite | CaCO3 | 100 | 12.6 |
| Ankerite | Ca(Fe,Mg)(CO3)2 | 200 | 12.9 |
| Siderite | FeCO3 | 116 | 16.5 |
| Smithsonite | ZnCO3 | 125 | 19.2 |
| Cerussite | PbCO3 | 267 | 65.3 |
In order to better understand back scattering as the advantages of, image instance below can provide one well help.
Fig. 1 is the back scattering picture of dolomite and calcite, according to back scattering as the characteristics of, in conjunction with dolomite and calcite
Average atomic number is easy to distinguish one from the other dolomite and calcite distribution situation from image.
Fig. 2 is the X rays topographs of calcite and the comparison diagram of back scattering picture.In X rays topographs, we can not identify calcite
Distribution situation, or even do not know either with or without calcite.And in back scattering picture, the side's of observing solution that we can be apparent
Stone understands the distribution of calcite, even through the available calcite content of visual estimation.
Fig. 3 is the X rays topographs of various carbonate.In image, identification carbonic acid salt distribution is highly difficult, even if you, which know, has
The distribution of carbonate, it is also necessary to just can determine that it is any carbonate mineral by X-ray energy spectrometer assaying element.
Fig. 4 is the back scattering picture of Fig. 3.It, can by the ingredient difference of carbonate in the back scattering picture then different feature of gray scale
Easily to identify and identify carbonate mine species and distribution situation.For example, in Fig. 4, it is corresponding flat according to image grayscale
The principle of equal atomic number, can therefrom identify dolomite (D), calcite (Cal), ankerite (Ak) and water chestnut from low to high
Iron ore (Ic).
Claims (8)
1. rock natural section sample carbonate characterizing method, which is characterized in that rock natural section sample carbonate characterization
Method includes:
Step 1, being partially placed into vacuum oven for energy representative sample feature is chosen；
Step 2, the parameter of vacuum oven is set；
Step 3, the sample of height 3mm~5mm is removed on the direction of vertical sample bed plane；
Step 4, sample is stained in sample stake；
Step 5, the sample stake that sample has been stained in step 4 is dried；
Step 6, sample is focused, observed and identified, determine the type and distribution of carbonate, and estimate that carbonate contains
Amount.
2. rock natural section sample carbonate characterizing method according to claim 1, which is characterized in that in step 1,
Sample is having a size of 12mm × 10mm × 10mm, and wherein the direction of size 12mm is parallel with sample bed plane.
3. rock natural section sample carbonate characterizing method according to claim 1, which is characterized in that in step 2,
Vacuum oven temperature parameter is set as 25 ± 1 DEG C, pressure parameter 1Pa, time parameter is no less than 2 hours.
4. rock natural section sample carbonate characterizing method according to claim 1, which is characterized in that in step 3,
The sample of height 3mm~5mm is removed with diagonal cutting pliers on the direction of vertical sample bed plane, and makes the smooth of sample section, sample
The difference in height on product surface is no more than 1mm.
5. rock natural section sample carbonate characterizing method according to claim 1, which is characterized in that in step 4,
It is mixed into uniform paste with the white glue with vinyl of 1:1 and graphite powder, forms graphite latex；Germicidal efficacy is face-up, with tune
The graphite latex made is stained on sample in sample stake.
6. rock natural section sample carbonate characterizing method according to claim 1, which is characterized in that in steps of 5,
After the sample stake for being stained with sample in step 4 is dried 5 hours at normal temperature, the method set according still further to step 2 is dried.
7. rock natural section sample carbonate characterizing method according to claim 6, which is characterized in that step 5 is also wrapped
It includes, by the sample prepared includes that sample stake is put into scanning electron microscope after the completion of dry, set electron microscope experiment parameter: acceleration voltage
For 10kV, sample chamber pressure is 60Pa, and electron beam operating distance is 8mm.
8. rock natural section sample carbonate characterizing method according to claim 7, which is characterized in that in step 6,
Sample is focused, observe and is identified with the signal of Electronic Speculum back scattering probe acquisition, determines the type and distribution shape of carbonate
State.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116468724A (en) * | 2023-06-08 | 2023-07-21 | 四川亿欣新材料有限公司 | Method for testing content of calcium carbonate based on optical sensing technology |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108318515A (en) * | 2018-01-09 | 2018-07-24 | 南京大学 | A kind of individual particle mineral facies automatic identification and quantitative analysis method based on sem energy spectrum analysis |
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- 2019-05-07 CN CN201910374284.3A patent/CN110108737A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108318515A (en) * | 2018-01-09 | 2018-07-24 | 南京大学 | A kind of individual particle mineral facies automatic identification and quantitative analysis method based on sem energy spectrum analysis |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116468724A (en) * | 2023-06-08 | 2023-07-21 | 四川亿欣新材料有限公司 | Method for testing content of calcium carbonate based on optical sensing technology |
| CN116468724B (en) * | 2023-06-08 | 2023-08-29 | 四川亿欣新材料有限公司 | Method for testing content of calcium carbonate based on optical sensing technology |
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Application publication date: 20190809 |