CN116519419A - Preparation method of in-situ analysis sample - Google Patents
Preparation method of in-situ analysis sample Download PDFInfo
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- CN116519419A CN116519419A CN202310621898.3A CN202310621898A CN116519419A CN 116519419 A CN116519419 A CN 116519419A CN 202310621898 A CN202310621898 A CN 202310621898A CN 116519419 A CN116519419 A CN 116519419A
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- 238000010249 in-situ analysis Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000002474 experimental method Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 239000000110 cooling liquid Substances 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 4
- 229920000742 Cotton Polymers 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 3
- 238000012613 in situ experiment Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 13
- 238000009826 distribution Methods 0.000 abstract description 10
- 229910000831 Steel Inorganic materials 0.000 abstract description 4
- 239000010959 steel Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000004458 analytical method Methods 0.000 description 9
- 230000005284 excitation Effects 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 238000005204 segregation Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000005464 sample preparation method Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- 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
-
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- 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
-
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a preparation method of an in-situ analysis sample, which relates to the technical field of steel production, and aims to ensure that the sample after being processed meets the test requirement, reduce the time consumed by repeated sample preparation and repeated experiments, and simultaneously ensure that the experimental result is more accurate and accords with the distribution rule of a component spectrogram of the sample so as to improve the experimental efficiency and the experimental precision.
Description
Technical Field
The invention relates to the technical field of steel production, in particular to a preparation method of an in-situ analysis sample.
Background
In-situ analysis is a technique for analyzing chemical components and structures of an original state of an analysis object, and can realize component analysis, segregation analysis, loose distribution analysis and qualitative and quantitative analysis of inclusions of a sample.
GB/T24213-2009 general rules of methods for analysis of metal in-situ statistical distribution recommends that a wire cutting or sawing machine is adopted to cut a sample to prepare a sample with proper size, then a milling machine is used to process the surface of the sample, and the milled surface of the sample is flat, clear in texture and kept clean. Or sample grinding equipment is arranged according to the requirement of analysis samples, the sample grinding material is alumina or zirconia, and the granularity is 0.25-0.40 mm. In-situ analyzer of model Opa-100 of steel in use at present, sample preparation requires cutting to proper position and size by band sawing machine, and the maximum dimension of sample processing is 100mm long by 90mm wide by (15-20 mm) thick, and the minimum dimension is 40mm long by 40mm wide by (15-20 mm) thick, or cylindrical section with diameter less than 100mm, and then grinding by grinding machine. In the grinding process, because overheating is prevented, certain cooling liquid needs to be released, a new surface is manually ground by adopting a belt sander after the processing is finished, the pollution on the surface is removed, and then in-situ analysis is carried out.
Grinding the sample requires that the surface of the sample must be smooth and that the periphery cannot be bumped, otherwise, gaps are left between the sample and the excitation holes, and the analysis data is inaccurate. The manual work is with the abrasive band machine grinds the sample and has certain degree of difficulty, and when the sample was too big overweight, when handheld sample was ground on the abrasive band machine, probably drops the sample because of holding, appears dangerous, or the sample is too big, and the uneven sample surface that leads to of abrasive process power. The samples ground by the abrasive belt are observed with naked eyes, the surfaces of the samples are smooth, but when the samples are placed on the excitation table, gaps are left between the samples and the excitation table, the experimental data show that the edges shown in fig. 3 are abnormally high, or the components shown in fig. 4 are distributed in a rainbow shape, and the requirements cannot be met. Therefore, a sample is usually subjected to repeated tests, so that the test time is prolonged, the test efficiency is reduced, and the test cost is increased.
Disclosure of Invention
Aiming at the technical problems and overcoming the defects of the prior art, the invention provides a preparation method of an in-situ analysis sample, which comprises the following steps:
(1) Cutting the sample to a proper position and size by a band sawing machine, and cutting a cross section with proper size and regular shape to ensure that the size and shape of the sample meet the experimental requirements;
(2) Grinding the surface to be subjected to in-situ experiments by adopting a grinder to enable the surface to be smooth and clear in texture; wiping off residual cooling liquid on the surface of the sample by clean cloth or absorbent cotton in time;
(3) Immersing the sample into a container containing absolute ethyl alcohol completely, vertically placing the experimental surface, and then cleaning by adopting an ultrasonic cleaner;
(4) Replacing absolute ethyl alcohol, repeating the step (3) for 1-2 times to ensure that the sample is sufficiently clean, and immediately drying the sample by a blower;
(5) Drying in an infrared oven to fully volatilize alcohol remained on the surface of the sample, and drying;
(6) And after the sample is cooled, taking out the sample, and carrying out in-situ analysis experiments, wherein if the experiments cannot be completed in time, the sample is required to be placed in a drying oven for storage.
The technical scheme of the invention is as follows:
the preparation method of the in-situ analysis sample comprises the following steps of (1), wherein the maximum dimension of sample processing is 100mm long by 90mm wide (15-20 mm) thick, and the diameter of a cylindrical sample is smaller than 100mm.
The preparation method of the in-situ analysis sample comprises the step (3) of cleaning for 10-20 min by adopting an ultrasonic cleaner.
The preparation method of the in-situ analysis sample comprises the following steps of (5) drying in an infrared oven for 30-60 min at the temperature below 50 ℃.
In the preparation method of the in-situ analysis sample, absolute ethyl alcohol is analytically pure.
The beneficial effects of the invention are as follows: the number of times of in-situ analysis of anti-copy samples is obviously reduced, the experimental efficiency is improved, the experimental cost is reduced, and spectrogram and data errors caused by poor sample preparation are reduced. The sample experimental surface is vertically placed, and the purpose is to ensure that impurities cannot be attached to the experimental surface after ultrasonic oscillation is carried out on the surface of the sample. Before improvement, a belt sander is adopted to grind a sample surface of a handheld sample, the analysis surface is uneven due to uneven force, a mechanical arm clamps the sample and can not keep the sample completely attached to an experiment table, argon overflows in the excitation process, stability in the excitation process is reduced, abnormal element components (higher or lower) of a part area C, P, S, mn and the like can be caused, and repeated sample grinding is needed to perform experiments until the analysis result of the sample is consistent with the low-power segregation distribution condition of the sample; after improvement, the surface of the sample is smooth and clean, the surface finish can reach more than 6, the sample is attached to the test bed, and the excitation state is stable. The data result is good, and repeated manual grinding of the sample is not needed.
Drawings
FIG. 1 is a low-power inspection diagram of an embodiment;
FIG. 2 is a two-dimensional distribution diagram of Mn element of the original manual sample grinding test result;
FIG. 3 is a three-dimensional distribution diagram of Mn element of the original manual sample grinding test result;
FIG. 4 is a two-dimensional distribution diagram of Mn element of the test result after the sample preparation method is improved;
FIG. 5 is a three-dimensional distribution diagram of Mn element as a result of the test after the improvement of the sample preparation method.
Description of the embodiments
The preparation method of the in-situ analysis sample provided by the embodiment comprises the following steps:
(1) Taking Q345 steel grade after low-power observation, wherein the sample size is 70cm x 70cm, and polishing by a grinder to make the sample smooth and clear in texture; wiping off residual cooling liquid on the surface of the sample by using clean cloth in time;
(2) Grinding the surface to be subjected to in-situ experiments by adopting a grinder to enable the surface to be smooth and clear in texture; wiping off the cooling liquid participated in on the surface of the sample by using clean absorbent cotton;
(3) Immersing the sample completely in a container containing absolute ethyl alcohol (analytically pure), vertically placing the experimental surface, and then cleaning for 10min by adopting an ultrasonic cleaner;
(4) Replacing clean absolute ethyl alcohol (analytically pure), repeating the step (3) for 2 times to ensure that the sample is sufficiently clean, and immediately drying the sample by a blower;
(5) And (5) baking for 40min in an infrared oven to fully volatilize the residual alcohol on the surface of the sample and drying.
(6) And taking out the sample after the sample is cooled, and carrying out in-situ analysis experiments.
As can be seen from FIG. 1, the sample has a clearer segregation band, and the rest parts are uniform. From the two-dimensional contour map (fig. 2-5) of the Mn element of the sample, it can be seen that the left component of the Mn element scanning region is significantly lower than other positions, and is in a stripe-like distribution, the other positions are distributed uniformly, and from the Mn element distribution map, there is a significant difference in local positions (upper right of the two-dimensional contour map) before and after improvement. The reason is that uneven force is applied to the test surface of the sample when the sample is manually ground by the belt sander, so that the mechanical arm clamps the sample and cannot keep the sample completely attached to the test surface, and the components of a part of the area are abnormal (higher or lower). Furthermore, the results of the test sample show rainbow-like patterns or anomalies with more pronounced local content. This problem is significantly solved after the improvement of the method according to the invention (see fig. 4, 5).
In addition to the embodiments described above, other embodiments of the invention are possible. All technical schemes formed by equivalent substitution or equivalent transformation fall within the protection scope of the invention.
Claims (5)
1. A method for preparing an in-situ analysis sample, which is characterized by comprising the following steps: the method comprises the following steps:
(1) Cutting the sample to a proper position and size by a band sawing machine, and cutting a cross section with proper size and regular shape to ensure that the size and shape of the sample meet the experimental requirements;
(2) Grinding the surface to be subjected to in-situ experiments by adopting a grinder to enable the surface to be smooth and clear in texture; wiping off residual cooling liquid on the surface of the sample by clean cloth or absorbent cotton in time;
(3) Immersing the sample into a container containing absolute ethyl alcohol completely, vertically placing the experimental surface, and then cleaning by adopting an ultrasonic cleaner;
(4) Replacing absolute ethyl alcohol, repeating the step (3) for 1-2 times to ensure that the sample is sufficiently clean, and immediately drying the sample by a blower;
(5) Drying in an infrared oven to fully volatilize alcohol remained on the surface of the sample, and drying;
(6) And after the sample is cooled, taking out the sample, and carrying out in-situ analysis experiments, wherein if the experiments cannot be completed in time, the sample is required to be placed in a drying oven for storage.
2. The method for preparing an in situ analysis sample according to claim 1, wherein: and (3) in the step (1), the maximum dimension of sample processing is 100mm long by 90mm wide (15-20 mm) thick, and the diameter of a cylindrical sample is less than 100mm.
3. The method for preparing an in situ analysis sample according to claim 1, wherein: and (3) cleaning for 10-20 min by adopting an ultrasonic cleaner.
4. The method for preparing an in situ analysis sample according to claim 1, wherein: and (5) baking in an infrared oven for 30-60 min at the temperature below 50 ℃.
5. The method for preparing an in situ analysis sample according to claim 1, wherein: the absolute ethanol is analytically pure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310621898.3A CN116519419A (en) | 2023-05-30 | 2023-05-30 | Preparation method of in-situ analysis sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310621898.3A CN116519419A (en) | 2023-05-30 | 2023-05-30 | Preparation method of in-situ analysis sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116519419A true CN116519419A (en) | 2023-08-01 |
Family
ID=87403028
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310621898.3A Pending CN116519419A (en) | 2023-05-30 | 2023-05-30 | Preparation method of in-situ analysis sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116519419A (en) |
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2023
- 2023-05-30 CN CN202310621898.3A patent/CN116519419A/en active Pending
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