CN110987986A - Analysis method for inorganic matters in shaft plug of oil and gas well - Google Patents
Analysis method for inorganic matters in shaft plug of oil and gas well Download PDFInfo
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Abstract
The invention provides a method for analyzing inorganic matters in a shaft plug of an oil-gas well, which comprises the following steps: sequentially drying and dissolving the wellbore plug sample by acetone, and collecting acetone insoluble substances; carrying out X-ray diffraction analysis on the acetone insoluble substance to obtain an X-ray diffraction analysis result; performing fluorescence spectrum analysis on the acetone insoluble substance to obtain a fluorescence spectrum analysis result; and determining the composition and content of inorganic matters in the wellbore plugging according to the X-ray diffraction analysis result and the fluorescence spectrum analysis result. The method for analyzing inorganic matters in the shaft blockage of the oil-gas well can accurately and comprehensively measure the total proportion of the inorganic matters, the components of the inorganic matters and the content of each component in the shaft blockage, provides technical support for shaft blockage mechanism research, blockage removal process selection and blockage removal liquid optimization, and finally realizes low cost and high efficiency of blockage removal operation.
Description
Technical Field
The invention relates to an analysis method of inorganic matters in a shaft plug of an oil-gas well, in particular to a method for analyzing and determining the inorganic matter components and the content of the shaft plug, belonging to an experimental method in the aspect of well repair in the process of petroleum and natural gas development.
Background
Scale, formation sand, corrosion products and minerals such as barium sulfate are the major contributors to most wellbore plugging. The blockage of the shaft can cause great reduction of oil and gas yield, further influence the development of oil and gas fields and cause great economic loss, so that the prevention of the shaft blockage and the solution of the oil well blockage are important subjects facing various oil fields. The analysis of components and contents of the wellbore plugging is a premise for researching a wellbore plugging mechanism and a plugging removal mechanism, is a basis for solving the wellbore plugging problem, and is an important basis for optimizing a plugging removal process and selecting an appropriate plugging removal liquid.
To fully analyze the mineral composition and content of wellbore plugs having diversity, uncertainty, and unknown properties, a set of methods for analyzing the mineral composition and content of wellbore plugs must be developed. The current methods for analyzing the mineral composition and content of the plug mainly include titration, burning and X-ray diffraction analysis.
In the enterprise standard Q/SY TZ0231 < analysis method of main chemical components of inorganic salt scale in oil field > "established by Tarim oil field division of oil and gas Limited corporation of China, the content of common ions or elements is measured by titration method, and then the inorganic components and the content are deduced, but the problem of wrong or incomplete component deduction may occur.
The burning method is mainly carried out according to the national environmental protection standard HJ 761-2015 'method for measuring burning and reducing the amount of organic matters in solid wastes', although the burning method can avoid the interference of organic matters on an analysis result by removing the organic matters, the high-temperature burning easily causes the change of partial inorganic matters, thereby causing the inaccuracy of the analysis result.
The X-ray diffraction analysis method is mainly carried out according to the oil and gas industry standard SY/T5163-.
Thus, there is currently a lack of a methodology for accurately analyzing the mineral content and mineral content of wellbore plugs in oil and gas wells.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the method for analyzing the inorganic matters in the shaft blockage of the oil-gas well, which can accurately analyze the components and the content of the inorganic matters in the shaft blockage.
In order to achieve the above object, the present invention provides a method for analyzing inorganic substances in wellbore plugs of oil and gas wells, comprising the steps of:
sequentially drying and dissolving the wellbore plug sample by acetone, and collecting acetone insoluble substances;
carrying out X-ray diffraction analysis on the acetone insoluble substance to obtain an X-ray diffraction analysis result;
performing fluorescence spectrum analysis on the acetone insoluble substance to obtain a fluorescence spectrum analysis result;
and determining the composition and content of inorganic matters in the wellbore plugging according to the X-ray diffraction analysis result and the fluorescence spectrum analysis result.
According to the analysis method provided by the invention, acetone dissolution is adopted to replace a conventional burning method to remove organic matters in the wellbore blockage, so that the problem that the components of the blockage are changed due to reaction of partial inorganic matters generated by high-temperature burning can be avoided; the method is characterized in that the fluorescence spectrum analysis is used for measuring the elements and the element content of the whole inorganic matter in the shaft plug instead of the energy spectrum analysis, so that the result is representative and comprehensive, and the X-ray diffraction analysis result is further combined, so that the inorganic matter components and the content of the whole shaft plug can be accurately determined, and support can be provided for shaft plug mechanism research, plug removal process selection and plug removal liquid optimization.
It will be appreciated that the above analysis method is particularly suitable for the overall analysis of wellbore plugs, and therefore, it is preferable to take out sufficient wellbore plugs as samples at a time before the analysis, preferably after the wellbore plugs are taken out and mixed uniformly, so as to meet the requirements of subsequent treatment and testing, and ensure the representative and comprehensive analysis results. In the practice of the present invention, typically no less than 50g of wellbore plug samples are taken and subsequently processed and analyzed for testing.
During analysis, wellbore plug samples are first dried to remove sufficient water therefrom to facilitate subsequent acetone dissolution. In the practice of the invention, the wellbore plug sample is dried to constant weight at a temperature of 105 ± 3 ℃.
It can be understood that in order to facilitate acetone dissolution, to completely remove organic matter in the wellbore plugs, and to avoid the presence of organic matter from affecting the accuracy and reliability of subsequent X-ray diffraction analysis results, fluorescence spectroscopy analysis results, and the like, the wellbore plug samples can also be crushed to a particle size of less than 0.1 mm.
Typically, a wellbore plug sample is first dried, then the sample is comminuted to a particle size of less than 0.1mm, and finally acetone dissolution is performed. Of course, it is also possible to first crush the wellbore plug sample to a particle size of less than 0.1mm, then dry and finally perform acetone dissolution.
The crushing means used in the present invention is not particularly limited, and may be any conventional treatment means in the art, such as grinding to a desired particle size, and then mixing the particles of the wellbore plugging sample obtained after grinding uniformly for later use.
It can be understood that the acetone dissolution condition is reasonably controlled, which is beneficial to fully removing organic matters in the wellbore plugging sample. Generally, the volume mass ratio between the acetone and the dried wellbore plugging sample is controlled to be more than or equal to 5 mL: at least 5mL of acetone is used for 1g, i.e. for each 1g of the dried wellbore plug sample dissolved. After at least 8 hours, the acetone dissolution is considered complete.
In the specific implementation process of the invention, all dried and crushed particles are put into acetone, sealed to prevent the acetone from volatilizing, placed at normal temperature for more than 8h, shaken every 2h, filtered, collected and dried to constant weight to obtain acetone insoluble substances for later use.
It is understood that the mass ratio of acetone insolubles to the wellbore plug sample (after drying) can be considered as the total mass of minerals in the wellbore plug sample.
In the invention, the X-ray diffraction analysis can be specifically carried out by taking part of acetone insoluble substances for processing and analyzing with reference to the X-ray diffraction analysis method for clay minerals and common non-clay minerals in sedimentary rocks 2010, SY/T5163 standards in the oil and gas industry of the people's republic of China, so as to obtain the components and the contents of inorganic substances, particularly the components and the contents of minerals, in the shaft blockage.
In the invention, the fluorescence spectrum analysis can be specifically carried out by taking another part of acetone insoluble substances for treatment and analysis with reference to the wavelength dispersion X-ray fluorescence spectrometry for measuring inorganic elements in soil and sediments in the national environmental protection standard HJ780-2015 of the people's republic of China, so as to obtain the element types and the content of inorganic substances in the shaft plug.
The X-ray diffraction analysis and the fluorescence spectrum analysis may be performed separately or sequentially, and the present invention is not particularly limited herein.
And determining the composition and content of inorganic matters in the wellbore plugging according to the X-ray diffraction analysis result and the fluorescence spectrum analysis result. Specifically, the X-ray diffraction analysis result relates to the main mineral components and the content, and the fluorescence spectrum analysis result comprises the contents of main elements and trace elements. And comparing the main elements and the contents thereof in the fluorescence spectrum analysis result with the mineral components and the contents thereof in the X-ray diffraction analysis result, so as to accurately determine the components and the contents of the inorganic matters in the shaft blockage.
Besides, the sources of some elements can be presumed according to the analysis result of fluorescence spectrum, especially according to some special elements or trace elements. For example, in a specific embodiment, according to the fluorescence spectrum analysis result, a large amount of Fe elements and special elements, Cr, Mn, Ni, and Mo, are detected, and considering that the material of the oil pipe is 13 Cr. Thus, the inventors speculate that the iron-containing compounds in the wellbore plugs are likely to result from tubing corrosion.
Meanwhile, the comparison of the analysis results is actually a process for verifying the accuracy of the analysis results according to the X-ray diffraction analysis results and the fluorescence spectrum analysis results. If the mineral components and their contents are matched with the results of the main elements and their contents, the accuracy and reliability of the analysis results can be determined.
In order to further ensure the accuracy and reliability of the analysis result, the method also comprises the step of verifying the determined components and contents of the inorganic matters.
As described above, the comparison between the above-mentioned fluorescence spectrum analysis result and the X-ray diffraction analysis result also belongs to a process of verifying the composition and content of the determined inorganic substance. In addition, the components and the content of the determined inorganic substances can be comprehensively verified according to the cause analysis of the wellbore blockage, the actual production experience and the like, so that the accuracy and the reliability of the analysis result are ensured.
In the specific implementation process of the invention, the verification step specifically comprises:
determining the mass ratio of acid soluble matters in inorganic matters in the wellbore plugging sample according to the X-ray diffraction analysis result;
adopting hydrochloric acid to erode acetone insoluble substances, and determining the acid solubility of inorganic substances in the wellbore plug sample;
comparing the mass ratio of the acid soluble substance in the inorganic substance with the acid solubility of the inorganic substance.
It is understood that since hydrochloric acid is used for measuring the acid solubility, the acid-soluble substance in the inorganic substance actually means a mineral that can be dissolved in hydrochloric acid. Accordingly, the mass ratio of the acid-soluble substance in the inorganic substance is the sum of the mass ratios of the minerals soluble in hydrochloric acid.
The acid solubility of the inorganic substance can be determined by specifically referring to a determination method and a calculation method of an acid insoluble substance in the oil and gas industry standard SY/T5559-1992 Universal test method for treating agents for drilling fluids of the people's republic of China, and the mass content of the acid insoluble substance is determined by dissolving the acetone insoluble substance with hydrochloric acid, so that the mass content of the acid insoluble substance, namely the acid solubility of the inorganic substance is obtained:
the acid solubility (acid-soluble content) of the inorganic substance is 100% to the mass content of the acid-insoluble substance.
In the specific implementation process of the invention, hydrochloric acid with the mass concentration of 5-8% is adopted to erode the acetone insoluble substance, and the volume mass ratio between the hydrochloric acid and the acetone insoluble substance is controlled to be more than or equal to 10 mL: 1g (at least 10mL of hydrochloric acid aqueous solution is needed for each 1g of dried insoluble substances after corrosion); the temperature of the corrosion is 90 +/-5 ℃, and the time is not less than 1 hour.
After the hydrochloric acid etching is completed, the part which is not etched by the hydrochloric acid is filtered and collected, dried and weighed, thereby obtaining the acid dissolution rate of the inorganic substance in the wellbore plugging sample.
Further, it is also possible to first pulverize the acetone-insoluble substance to a particle size of not more than 0.425mm before the dissolution by hydrochloric acid. Typically, the acetone insoluble material is ground to a powder and passed through a 40 mesh screen.
Comparing the acid solubility of the inorganic substances with the mass content of the acid soluble substances, if the acid solubility and the mass content of the acid soluble substances are the same or have small difference, the result of determining the composition and the content of the inorganic substances in the wellbore plugging object is accurate and reliable, and the representative sample of the taken plugging object is also verified.
The above-described use of hydrochloric acid to erode acetone insolubles is also a practical process for preliminary test analysis of wellbore plug samples. In the specific implementation process of the invention, part of acetone insoluble substances are generally taken to carry out hydrochloric acid corrosion, the acid dissolution rate of inorganic substances is qualitatively judged, then the wellbore plugging substance sample is quantitatively analyzed by microscopic means (X-ray diffraction analysis and fluorescence spectrum analysis), finally, the components and the content of the inorganic substances are determined by combining various test results, and the accuracy and the reliability of the analysis results are ensured.
In general, when the ratio of the mass of the acid-soluble substance in the inorganic substance to the change rate of the acid-soluble rate of the inorganic substance is 20% or less, the results of the determined composition and content of the inorganic substance are considered to be accurate. That is, when the acid solubility of the inorganic substance is represented by a and the mass ratio of the acid-soluble substance in the inorganic substance is represented by B, the analysis result is considered to be accurate and reliable if the following conditions are satisfied.
The analysis process described above is essentially a test and analysis performed around the entire wellbore plug. Further, the analysis method of the present invention may further include a step of performing a test analysis on a local inorganic matter, and particularly, based on the overall analysis result, when the inventors consider that performing a further local analysis on certain regions can be advantageous to determine the cause of the wellbore plugging and even the mechanism of the plugging formation, the detection and analysis of certain local regions may also be performed. For example, in one embodiment, the X-ray diffraction analysis reveals a lot of minerals containing iron compounds, the fluorescence spectroscopy also detects Fe, and the visual inspection of the wellbore obstruction reveals a lot of red substances suspected of containing iron compounds, which can be further analyzed.
Specifically, the local analysis may include: scanning electron microscopy analysis was performed on a portion of the wellbore plug sample. For example, in the above embodiment, the local red substance can be analyzed by scanning electron microscopy.
Specifically, the scanning electron microscope analysis can refer to the oil and gas industry standard SY/T5162-.
Adopt scanning electron microscope, can observe the microscopic form on local sample surface, not only can judge the main mineral composition of local sample in view of the above, can be used for the source of preliminary judgement pit shaft stopper moreover: reservoir production, working fluid carry-in, or production in the wellbore.
Furthermore, the energy spectrum analysis can be carried out on the local part of the sample of the wellbore plugging material to obtain the element type and the content of the local sample, so that the element of the local sample and the content of the main element can be confirmed by combining the analysis result of the scanning electron microscope.
Specifically, the energy spectrum analysis can refer to the oil and gas industry standard SY/T6189-.
In addition, according to the element type and content of the local surface of the sample, mutual verification can be performed with the whole analysis result of the sample, which is not repeated.
By carrying out overall analysis on the shaft blockage and combining the local analysis, the overall situation and the local situation of inorganic matters in the shaft blockage are further accurately and comprehensively measured, so that support is better provided for shaft blockage mechanism research, blockage removal process selection and blockage removal liquid optimization.
The invention establishes an analysis method of inorganic matters in the shaft blockage of the oil-gas well, and finally can accurately and comprehensively measure the total proportion of the inorganic matters, the components of the inorganic matters and the content of each component in the shaft blockage by adopting acetone to dissolve a sample and combining X-ray diffraction analysis and fluorescence spectrum analysis, thereby providing technical support for shaft blockage mechanism research, blockage removal process selection and blockage removal liquid optimization, and finally realizing the low cost and high efficiency of blockage removal operation.
Drawings
FIG. 1 is an X-ray diffraction pattern of sample # 1 in example 1 of the present invention;
FIG. 2 is an X-ray diffraction pattern of sample # 2 of example 1 of the present invention;
FIG. 3 is an SEM photograph of a partial sample No. 1 in example 1 of the present invention;
FIG. 4 is a spectrum of a local sample No. 1 in example 1 of the present invention;
FIG. 5 is an SEM photograph of a partial sample No. 2 in example 1 of the present invention;
FIG. 6 is a spectrum of a local sample No. 2 in example 1 of the present invention;
FIG. 7 is an SEM photograph of a partial sample No. 3 in example 1 of the present invention;
FIG. 8 is a spectrum of a local sample No. 3 in example 1 of the present invention;
FIG. 9 is an SEM photograph of a partial sample No. 4 in example 1 of the present invention;
FIG. 10 is a spectrum of a local sample No. 4 in example 1 of the present invention;
FIG. 11 is an SEM photograph of a partial sample No. 5 in example 1 of the present invention;
FIG. 12 is a spectrum of a local sample No. 5 in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The present example provides a method for analyzing the mineral composition and content of a wellbore blockage, including bulk mineral analysis and localized analysis. The wellbore plug sample is from a wellbore plug of an X-well in a kriging block of a Tarim oilfield.
1. Bulk analysis of inorganic materials in plugs:
(1) sampling and processing
Taking out the shaft plug, weighing the total mass of the shaft plug to be 300g, uniformly mixing the shaft plug, taking out 50g of the shaft plug as a shaft plug sample, drying the shaft plug sample at the temperature of about 105 ℃ to constant weight, weighing the shaft plug to be 48.4g, grinding to ensure that the particle size is less than 0.1mm, and uniformly mixing.
(2) Dissolving with acetone
Taking all the particles obtained by grinding and uniformly mixing the dried wellbore plugging sample in the step (1), putting the particles into acetone, and sealing, wherein the ratio of the volume of the acetone to the mass of the dried wellbore plugging sample is 5 mL: 1g, standing at room temperature (about 25 ℃) for more than 8 hours, shaking once every 2 hours, filtering to obtain a solid part insoluble in acetone, drying to constant weight, and weighing 46.06g of acetone insoluble substances.
The total proportion of inorganic material in the wellbore plug was calculated as (46.06 g/48.4 g) x 100% ═ 95.17%.
(3) Hydrochloric acid corrosion
And (3) taking out 20g of acetone insoluble substances in the step (2), crushing, sieving by a 40-mesh sieve to obtain 11.42g of sample powder with the particle size of less than or equal to 0.425mm, weighing 2 parts of sample powder with the mass of 5g, then respectively corroding by 50mL of hydrochloric acid with the mass fraction of 8%, controlling the temperature to be 90 ℃ and the time to be 2 hours, filtering, taking solid parts which are not corroded by the hydrochloric acid, drying, and measuring that the mass of the two samples is 1.35g and 1.38g respectively.
The acid solubility of the minerals in the two samples was calculated to be (5g-1.35g) ÷ 5g × 100% ═ 73.0%, and (5g-1.38g) ÷ 5g × 100% ═ 72.4%, and the average acid solubility of the minerals in the wellbore plugs was calculated to be (73.0+72.4) ÷ 2 ═ 72.7%, and reported as a.
(4) X-ray diffraction analysis
And (3) taking 2g of acetone insoluble substances in the step (2), processing and analyzing the samples by referring to SY/T5163-.
TABLE 1 results of X-ray diffraction analysis
Referring to figures 1 and 2 and table 1, the major mineral of the wellbore plugging is carbonate (CaCO)3、MgCO3、Ca(Fe,Mg,Mn)(CO3)2Iron-containing compound (Fe)3O4、Fe2O3、FeCO3FeO (OH), and amphibole, the sum of the acid soluble (hydrochloric acid) in the inorganic matter is 74.5% on average, and is denoted as B.
(5) Fluorescence spectroscopy
Taking about 6g of acetone insoluble substances in the step (2), treating and analyzing the sample by referring to HJ780-2015 'determination wavelength dispersion X-ray fluorescence spectrometry for inorganic elements in soil and sediments', testing twice in parallel, respectively marking as a 1# sample and a 2# sample, and testing results are detailed in Table 2.
TABLE 2 results of fluorescence spectrum analysis
| Numbering | Ca | Fe | Na | K | Cl | Mg | P |
| 1# | 15.66 | 12.73 | 7.58 | 3.73 | 3.93 | 1.04 | 0.5 |
| 2# | 15.55 | 12.69 | 7.75 | 3.74 | 3.93 | 1.05 | 0.34 |
| Average | 15.61 | 12.71 | 7.67 | 3.74 | 3.93 | 1.05 | 0.42 |
| Numbering | Si | Cr | Sr | S | Al | Ba | Mn |
| 1# | 0.34 | 0.45 | 0.37 | 0.16 | 0.14 | 0.19 | 0.15 |
| 2# | 0.34 | 0.45 | 0.36 | 0.16 | 0.14 | 0.19 | 0.15 |
| Average | 0.34 | 0.45 | 0.36 | 0.16 | 0.14 | 0.19 | 0.15 |
| Numbering | Ni | Mo | Cu | Zn | V | Zr | Ti |
| 1# | 0.12 | 0.06 | 0.06 | 0.037 | 0.012 | 0.008 | 0.004 |
| 2# | 0.12 | 0.05 | 0.06 | 0.040 | 0.013 | 0.009 | 0.003 |
| Average | 0.12 | 0.05 | 0.06 | 0.039 | 0.012 | 0.009 | 0.004 |
| Numbering | Pb | Co | Sn | Pu | Se | Ge | Rb |
| 1# | 0.006 | 0.003 | 0.001 | 0.0009 | 0.0004 | 0.0004 | 0.0005 |
| 2# | 0.007 | 0.003 | 0.000 | 0.0005 | 0 | 0 | 0.0004 |
| Average | 0.007 | 0.003 | 0.001 | 0.0007 | 0.0002 | 0.0002 | 0.0005 |
| Numbering | Sc | Am | Ga | Cs | Y | ||
| 1# | 0.0003 | 0.0003 | 0.0002 | 0.0013 | 0.00009 | ||
| 2# | 0 | 0 | 0 | 0 | 0 | ||
| Average | 0.0002 | 0.0002 | 0.0001 | 0.0007 | 0.00005 |
As can be seen from Table 2, the main elements of the inorganic substances in the wellbore plugging are Ca and Fe, and the iron-containing compounds are judged to possibly come to the oil pipe corrosion (the oil pipe material of the X well is 13Cr) mainly according to the special elements of Cr, Mn, Ni and Mo.
(6) Verification analysis
Calculated, (B-a) ÷ a × 100% ═ 75.5% -72.5% ÷ 72.5% × 100% ═ 4.13%, clearly 4.13% was less than 20%.
And the main mineral (CaCO) in the step (4)3And iron-containing compound) and the main elements (Ca and Fe) in the step (5) are compared, so that the analysis result of the inorganic matter component and the content in the wellbore plugging is accurate and reliable.
According to the results in the step (4) and the step (5), the composition and content of inorganic matters in the wellbore plugging can be determined, and the specific contents can be seen in table 1 and table 2.
2. Local analysis of mineral in wellbore plugs
Since a large amount of minerals containing iron compounds are found in the overall analysis of the wellbore plug, red substances suspected of containing iron compounds are observed outside a portion of the plug particles. Then, further performing scanning electron microscope analysis on the local red substance, and referring to SY/T6189-.
According to table 3, fig. 3 to fig. 12, the main elements of this red partial sample were Fe (46.4%) and O (25.3%), so that it could be confirmed that the sample was partially mainly iron-containing compound.
TABLE 3 results of energy spectrum analysis
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (10)
1. A method for analyzing minerals in wellbore plugs of oil and gas wells, comprising the steps of:
sequentially drying and dissolving the wellbore plug sample by acetone, and collecting acetone insoluble substances;
carrying out X-ray diffraction analysis on the acetone insoluble substance to obtain an X-ray diffraction analysis result;
performing fluorescence spectrum analysis on the acetone insoluble substance to obtain a fluorescence spectrum analysis result;
and determining the composition and content of inorganic matters in the wellbore plugging according to the X-ray diffraction analysis result and the fluorescence spectrum analysis result.
2. The analytical method of claim 1, further comprising: crushing the wellbore plug sample to a particle size of less than 0.1 mm.
3. The analytical method according to claim 1 or 2, wherein the volume-to-mass ratio of acetone to the dried wellbore plug sample is controlled to be greater than or equal to 5 mL: 1g, and the acetone dissolution time is not less than 8 hours.
4. The assay of any one of claims 1-3, further comprising the step of verifying the determined composition and content of the inorganic species.
5. The analytical method of claim 4, wherein the step of verifying comprises:
adopting hydrochloric acid to erode the acetone insoluble substance, and determining the acid solubility of inorganic substances in the wellbore plug sample;
determining the mass ratio of acid soluble matters in inorganic matters in the wellbore plugging sample according to the X-ray diffraction analysis result;
the acid solubility of the inorganic substance and the mass ratio of the acid-soluble substance in the inorganic substance were compared.
6. The analysis method according to claim 5, wherein the ratio of the mass of the acid-soluble substance in the inorganic substance to the rate of change in the acid-soluble rate of the inorganic substance is 20% or less, and the results of the determined composition and content of the inorganic substance are considered to be accurate.
7. The analytical method according to claim 5 or 6, wherein the hydrochloric acid has a mass concentration of 5% to 8%, and the volume-to-mass ratio between the hydrochloric acid and the acetone-insoluble substance is 10mL or more: 1g, wherein the corrosion temperature is 90 +/-5 ℃, and the time is not less than 1 hour.
8. The assay of any one of claims 5-7, further comprising, prior to being eroded by hydrochloric acid: pulverizing the dried insoluble substance to a particle size of not more than 0.425 mm.
9. The assay of any one of claims 1-8, further comprising: scanning electron microscopy analysis is performed on a portion of the wellbore plug sample.
10. The analytical method of claim 9, further comprising: performing a power spectrum analysis on a portion of the wellbore plug sample.
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| CN112378936A (en) * | 2020-10-28 | 2021-02-19 | 中国石油化工股份有限公司 | Analysis method for corrosion unknown composition of oil refining device |
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| CN112378936A (en) * | 2020-10-28 | 2021-02-19 | 中国石油化工股份有限公司 | Analysis method for corrosion unknown composition of oil refining device |
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