CN111855268A - Processing method for analyzing test sample by using coring to drill oxygen, nitrogen and hydrogen - Google Patents
Processing method for analyzing test sample by using coring to drill oxygen, nitrogen and hydrogen Download PDFInfo
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- CN111855268A CN111855268A CN202010675461.4A CN202010675461A CN111855268A CN 111855268 A CN111855268 A CN 111855268A CN 202010675461 A CN202010675461 A CN 202010675461A CN 111855268 A CN111855268 A CN 111855268A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
- G01N1/08—Devices for withdrawing samples in the solid state, e.g. by cutting involving an extracting tool, e.g. core bit
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Abstract
The invention relates to a processing method for analyzing test samples by using core drilling to obtain oxygen, nitrogen and hydrogen, which comprises the following steps: fixing a sampling metal sample plate by using a clamp, wherein the thickness of the sampling metal sample plate is T; by a diameter phi1The drill bit pre-drills a hole at the sampling position on the front surface of the sampling metal sample plate, and the drilling depth is H1(ii) a Repeating the second step on the reverse side of the sampling metal sample plate, and pre-drilling holes at corresponding sampling positions, wherein the depth of the drilled holes is H2，H1And H2Satisfy T ═ H1+H2+ h, h is the sampling cylinder height; with an external diameter of phi2Inner diameter of phi3The hollow drill bit or the core drill bit is used for drilling and sampling at the pre-drilling position of the sampling metal sample plate. The processing method for analyzing the test sample by using the coring bit for oxygen, nitrogen and hydrogen has the advantages of simple operation, saving sample preparation time, reducing labor intensity and being simple and convenient in sample preparation when processing the O, N, H test sample.
Description
Technical Field
The invention relates to a processing method for analyzing a test sample by using a core drill to extract oxygen, nitrogen and hydrogen, belonging to the field of sample preparation and processing of the test sample.
Background
At present, in a laboratory, the processing methods of the column-shaped samples for oxygen, nitrogen and hydrogen analysis tests generally include the following methods:
1. the sample is processed into a rod-like shape by sawing, turning, etc. at a low speed, and then into a columnar sample by shearing. The sample is generally processed in such a manner that the sample is a rod-like product having a diameter of less than 10 mm. The disadvantages of this method are: when the sample is used for plates, the sample is processed into a rectangular strip shape by processing modes such as sawing and the like, and then the sample is lathed into a circle; when a sample with a large diameter is machined, the influence on the subsequent analysis detection value of the sample caused by the fact that the sample is overheated to turn blue needs to be prevented, so that the cutting amount of each cutting machining needs to be controlled, the cutting times are increased, and the machining time is too long.
2. When a sheet (plate) sample is subjected to sample processing, a sanding machine (disc) is adopted to polish platforms at two ends to remove an oxide layer, and then a punching manner of a punch is adopted to obtain a columnar sample. The disadvantages of this method are: if the sample is thick, the sample is ground to a certain thickness before punching, otherwise the punch is easy to damage, or the punched sample exceeds the upper limit of the thickness of the sample measured by the instrument due to the specification; when the hardness of the sample is high, the punch is easy to damage.
It is therefore desirable to devise a method of processing oxygen, nitrogen and hydrogen analysis test samples using core drilling to overcome the above problems.
Disclosure of Invention
The invention aims to overcome various defects of a processing method of a columnar sample for oxygen, nitrogen and hydrogen analysis tests in a laboratory at present, and provides a processing method for drilling oxygen, nitrogen and hydrogen analysis test samples by using a core.
The invention provides a processing method for analyzing test samples of oxygen, nitrogen and hydrogen by using a core drill, which aims at a sample with an oxide layer on the front and back sampling surfaces of a sampling metal sample plate and comprises the following steps:
the method comprises the following steps: fixing a sampling metal sample plate by using a clamp, wherein the thickness of the sampling metal sample plate is T;
step two: by a diameter phi1The drill bit pre-drills a hole at the sampling position on the front surface of the sampling metal sample plate, and the drilling depth is H1；
Step three: repeating the second step on the reverse side of the sampling metal sample plate, and pre-drilling holes at corresponding sampling positions, wherein the depth of the drilled holes is H2，H1And H2Satisfy T ═ H1+H2+ h, h is the height of the sampling cylinder, and the sampling on the front and back of the sampling metal sample plate is already carried out in the process of twice drilling by the drill bitRemoving the oxide layer at the position;
step four: with an external diameter of phi 2Inner diameter of phi3The hollow drill bit or the core drill bit is used for drilling and sampling at the pre-drilling position of the sampling metal sample plate.
Further, steps two and three may be replaced with a counter-drilling method: adopt two diameters to be phi x's drill bit, on the sample position that the positive and negative two sides of sample metal specimen board corresponds, in the while with same parameter speed predrilling, the degree of depth of drilling is H, and drilling depth H satisfies T ═ H + H + H.
Further, in the first to fourth steps, when the drill bit and the hollow drill bit or the core drill bit are used for drilling, liquid nitrogen is gasified and then sprayed to the drilling part for cooling, and hydrogen is prevented from overflowing from metal due to overheating of the drilling hole.
Further, the inner diameter Φ of the hollow bit or core bit3I.e. the diameter of the sampling cylinder, the diameter phi of the drill bit1Not less than the outer diameter phi of a hollow or core drill bit2The height h of the sampling cylinder is directly calculated according to the requirements of the analytical instrument: according to the requirements of analytical instrument, sample mass m and drill diameter phi1Outside diameter phi of hollow bit or core bit2Inside diameter phi3；
Wherein rho is the density of the sample material, and pi is the circumferential ratio.
Further, in the process of drilling and sampling, the drill bit and the hollow drill bit or the core drill bit can be sequentially arranged on the same machine tool to drill and sample the same sample, and can also be respectively arranged on two machine tools to pre-drill and sample the two samples simultaneously.
The invention also provides a processing method for analyzing and testing samples by using core drilling to obtain oxygen, nitrogen and hydrogen, which aims at the samples of which at least one of the front and back surfaces of the sampling metal sample plate does not have an oxide layer and comprises the following steps:
the method comprises the following steps: fixing a sampling metal sample plate by using a clamp, wherein the thickness of the sampling metal sample plate is T;
step two: setting the front surface of the sampling metal sample plate as one surface without an oxide layer and the back surface with or without an oxide layer, wherein the diameter phi is used1The drill bit pre-drills a hole at the sampling position on the reverse side of the sampling metal sample plate, the depth of the drilled hole is H, H is T-H, and H is the height of a sampling cylinder;
step three: with an external diameter of phi2Inner diameter of phi3The hollow drill bit or the core drill bit is used for drilling and sampling at the position of the pre-drilled hole on the front surface of the sampling metal sample plate.
Further, steps two and three may be replaced with: the method comprises the steps of pre-drilling a hole at the front sampling position of a sampling metal sample plate by using a hollow drill bit or a core drill bit, and drilling a through hole at the back sampling position of the sampling metal sample plate by using the drill bit for sampling.
Furthermore, when the drill bit and the hollow drill bit or the core drill bit are used for drilling, liquid nitrogen is gasified and then sprayed to the drilling part for cooling, so that hydrogen is prevented from overflowing from metal due to overheating of the drilling hole.
Further, the inner diameter Φ of the hollow bit or core bit3I.e. the diameter of the sampling cylinder, the diameter phi of the drill bit1Not less than the outside diameter phi of a hollow or core drill bit2The height h of the sampling cylinder is directly calculated according to the requirements of the analytical instrument: according to the requirements of analytical instrument, sample mass m and drill diameter phi1Outside diameter phi of hollow bit or core bit2Inside diameter phi3；
Wherein rho is the density of the sample material, and pi is the circumferential ratio.
Further, in the process of drilling and sampling, the drill bit and the hollow drill bit or the core drill bit can be sequentially arranged on the same machine tool to drill and sample the same sample, and can also be respectively arranged on two machine tools to pre-drill and sample the two samples simultaneously.
The invention has the following beneficial effects: the processing method for analyzing the test sample by using the coring bit for oxygen, nitrogen and hydrogen has the advantages of simple operation, saving sample preparation time, reducing the labor intensity of sample preparation and enabling the sample preparation to be more concise and convenient when processing the O, N, H test sample.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of a first step in a process of sampling a sample with an oxide layer on the front and back sides of a sampling metal sample plate according to the method for processing a sample for analyzing oxygen, nitrogen and hydrogen by using a core drill;
FIG. 2 is a schematic diagram of a second step in the process of sampling a sample with an oxide layer on the front and back sides of a sampling metal sample plate according to the method for processing a sample for oxygen, nitrogen and hydrogen analysis test by core drilling provided by the invention;
FIG. 3 is a schematic diagram of a fourth step in the process of sampling a sample with an oxide layer on the front and back sides of a sampling metal sample plate according to the method for processing oxygen, nitrogen and hydrogen analysis test samples by core drilling provided by the invention;
FIG. 4 is a schematic diagram of a method for processing oxygen, nitrogen and hydrogen analysis test samples by core drilling, which is provided by the invention, and the method is used for drilling in a sample with an oxide layer on the front and back surfaces of a sampling metal sample plate;
FIG. 5 is a schematic view of a first step in a method for processing a sample for oxygen, nitrogen and hydrogen analysis by core drilling according to the present invention, wherein the sample does not have an oxide layer on at least one of front and back surfaces of a metal sample plate to be sampled;
FIG. 6 is a schematic view of a second step in the process of sampling a sample for oxygen, nitrogen and hydrogen analysis by core drilling according to the present invention, wherein the sample does not have an oxide layer on at least one of the front and back surfaces of the sampled metal sample plate;
FIG. 7 is a schematic view of a third step in the process of analyzing a test sample by core drilling for oxygen, nitrogen and hydrogen according to the present invention, wherein the sample does not have an oxide layer on at least one of the front and back surfaces of the metal sample plate;
FIG. 8 is a schematic view showing a hollow drill or a core drill followed by a drill in a sample having no oxide layer on at least one of the front and back surfaces of a metal sample plate to be sampled according to the method for analyzing a test sample for oxygen, nitrogen or hydrogen by core drilling of the present invention.
Detailed Description
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 only a part of the embodiments of the present invention, and not all of the embodiments. 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.
The invention provides a processing method for analyzing and testing samples of oxygen, nitrogen and hydrogen by using a core drill, which aims at sampling a sample with an oxide layer on the front and back surfaces of a sampling metal sample plate and comprises the following steps:
the method comprises the following steps: a sampling metal sample plate is fixed by a clamp, and the thickness of the sampling metal sample plate is T. Referring to fig. 1, fig. 1 is a schematic diagram of step one.
Step two: by a diameter phi1The drill bit pre-drills a hole at the sampling position on the front surface of the sampling metal sample plate, and the drilling depth is H1. Referring to fig. 2, fig. 2 is a schematic diagram of step two.
Step three: repeating the second step on the reverse side of the sampling metal sample plate, and pre-drilling holes at corresponding sampling positions, wherein the depth of the drilled holes is H2，H1And H2Satisfy T ═ H1+H2And h is the height of the sampling cylinder, and the oxide layers at the sampling positions on the front and back surfaces of the sampling metal sample plate are removed in the process of drilling twice by the drill bit.
Step (ii) ofFourthly, the method comprises the following steps: with an external diameter of phi2Inner diameter of phi3The hollow drill bit or the core drill bit is used for drilling and sampling at the pre-drilling position of the sampling metal sample plate. Referring to fig. 3, fig. 3 is a schematic diagram of step four.
Wherein, step two and step three can be replaced by drilling the method: using two diameters of phi1The drill bit of (1) on the sample position that sample metal sample board tow sides correspond, simultaneously with the same parameter speed pre-drilling, the degree of depth of drilling is H, and drilling depth H satisfies T ═ H + H + H. Referring to fig. 4, fig. 4 is a schematic diagram of a drilling method.
In the first to the fourth steps, when the drill bit and the hollow drill bit or the core drill bit are used for drilling, liquid nitrogen is gasified and then sprayed to the drilling part for cooling, so that hydrogen is prevented from overflowing from metal due to overheating of the drilling hole.
Hollow or core drill bit inner diameter phi3I.e. the diameter of the sampling cylinder, the diameter phi of the drill bit1Not less than the outer diameter phi of a hollow or core drill bit2The height h of the sampling cylinder is directly calculated according to the requirements of the analytical instrument: according to the requirements of analytical instrument, sample mass m and drill diameter phi1Outside diameter phi of hollow bit or core bit2Inside diameter phi3；
Wherein rho is the density of the sample material, and pi is the circumferential ratio.
In the present embodiment, it is preferable that: the mass m of the sample is 1g, and the diameter phi of the drill bit1Is selected to be 12-13mm, and the outer diameter phi of a hollow drill bit or a core drill bit2Is selected to be 12mm and the inner diameter phi3And is selected to be 6 mm.
In the process of drilling and sampling, the drill bit and the hollow drill bit or the coring drill bit can be sequentially arranged on the same machine tool to drill and sample the same sample, and can also be respectively arranged on two machine tools to pre-drill and sample the two samples simultaneously.
The invention also provides a processing method for analyzing and testing samples by using core drilling to obtain oxygen, nitrogen and hydrogen, which aims at the samples of which at least one of the front and back surfaces of the sampling metal sample plate does not have an oxide layer and comprises the following steps:
the method comprises the following steps: a sampling metal sample plate is fixed by a clamp, and the thickness of the sampling metal sample plate is T. Please refer to fig. 5, in which fig. 5 is a schematic diagram of step one.
Step two: setting the front surface of the sampling metal sample plate as one surface without an oxide layer and the back surface with or without an oxide layer, wherein the diameter phi is used1The drill bit pre-drills a hole at the sampling position on the reverse side of the sampling metal sample plate, the depth of the drilled hole is H, H is T-H, and H is the height of a sampling cylinder; referring to fig. 6, fig. 6 is a schematic diagram of step two.
Step three: with an external diameter of phi2Inner diameter of phi3The hollow drill bit or the core drill bit is used for drilling and sampling at the position of the pre-drilled hole on the front surface of the sampling metal sample plate. Referring to fig. 7, fig. 7 is a schematic diagram of step three.
Wherein, the second and third steps can be replaced by: the method comprises the steps of pre-drilling a hole at the front sampling position of a sampling metal sample plate by using a hollow drill bit or a core drill bit, and drilling a through hole at the back sampling position of the sampling metal sample plate by using the drill bit for sampling. Referring to fig. 8, fig. 8 is a schematic view of a core bit or coring bit followed by a drill bit.
When the drill bit and the hollow drill bit or the core drill bit are used for drilling, liquid nitrogen is gasified and then sprayed to the drilling part for cooling, so that hydrogen is prevented from overflowing from metal due to overheating of the drilling hole.
Hollow or core drill bit inner diameter phi3I.e. the diameter of the sampling cylinder, the diameter phi of the drill bit 1Not less than the outside diameter phi of a hollow or core drill bit2The height h of the sampling cylinder is directly calculated according to the requirements of the analytical instrument: according to the requirements of analytical instrument, sample mass m and drill diameter phi1Outside diameter phi of hollow bit or core bit2Inside diameter phi3；
Wherein rho is the density of the sample material, and pi is the circumferential ratio.
In the present embodiment, it is preferable that: the mass m of the sample is 1g, and the diameter phi of the drill bit1Is selected to be 12-13mm, and the outer diameter phi of a hollow drill bit or a core drill bit2Is selected to be 12mm and the inner diameter phi3And is selected to be 6 mm.
In the process of drilling and sampling, the drill bit and the hollow drill bit or the coring drill bit can be sequentially arranged on the same machine tool to drill and sample the same sample, and can also be respectively arranged on two machine tools to pre-drill and sample the two samples simultaneously.
The embodiment of the invention has the following beneficial effects: the processing method for analyzing the test sample by using the coring bit for oxygen, nitrogen and hydrogen has the advantages of simple operation, saving sample preparation time, reducing the labor intensity of sample preparation and enabling the sample preparation to be more concise and convenient when processing the O, N, H test sample.
Details not described in this specification are within the skill of the art that are well known to those skilled in the art. The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A processing method for analyzing test samples by using coring to drill oxygen, nitrogen and hydrogen is characterized in that: the method is used for sampling a sample with an oxide layer on the front and back sampling surfaces of a sampling metal sample plate, and comprises the following steps:
the method comprises the following steps: fixing a sampling metal sample plate by using a clamp, wherein the thickness of the sampling metal sample plate is T;
step two: by a diameter phi1The drill bit pre-drills a hole at the sampling position on the front surface of the sampling metal sample plate, and the drilling depth is H1；
Step three: repeating the second step on the reverse side of the sampling metal sample plate, and pre-drilling holes at corresponding sampling positions, wherein the depth of each drilled hole is H2，H1And H2Satisfy T ═ H1+H2+ h, h is the height of the sampling cylinder, and the oxide layers at the sampling positions on the front and back surfaces of the sampling metal sample plate are removed in the process of twice drilling by the drill bit;
step four: with an external diameter of phi2Inner diameter of phi3The hollow drill bit or the core drill bit is used for drilling and sampling at the pre-drilling position of the sampling metal sample plate.
2. The method of processing oxygen, nitrogen, hydrogen analysis test samples by core drilling as claimed in claim 1, wherein: the second and third steps can be replaced by a drilling method: using two diameters of phi1The drill bit of (1) on the sample position that sample metal sample board tow sides correspond, simultaneously with the same parameter speed pre-drilling, the degree of depth of drilling is H, and drilling depth H satisfies T ═ H + H + H.
3. The method of processing oxygen, nitrogen, hydrogen analysis test samples by core drilling as claimed in claim 1 or 2, wherein: in the first to the fourth steps, when the drill bit and the hollow drill bit or the core drill bit are used for drilling, liquid nitrogen is gasified and then sprayed to the drilling part for cooling, so that hydrogen is prevented from overflowing from metal due to overheating of the drilling hole.
4. The method of processing oxygen, nitrogen, hydrogen analysis test samples by core drilling as claimed in claim 1 or 2, wherein: hollow or core drill bit inner diameter phi3I.e. the diameter of the sampling cylinder, the diameter phi of the drill bit1Not less than the outer diameter phi of a hollow or core drill bit2The height h of the sampling cylinder is directly calculated according to the requirements of the analytical instrument: according to the requirements of analytical instrument, sample mass m and drill diameter phi1Outside diameter phi of hollow bit or core bit2Inside diameter phi3；
Wherein rho is the density of the sample material, and pi is the circumferential ratio.
5. The method of processing oxygen, nitrogen, hydrogen analysis test samples by core drilling as claimed in claim 4, wherein: in the process of drilling and sampling, the drill bit and the hollow drill bit or the coring drill bit can be sequentially arranged on the same machine tool to drill and sample the same sample, and can also be respectively arranged on two machine tools to pre-drill and sample the two samples simultaneously.
6. A processing method for analyzing test samples by using coring to drill oxygen, nitrogen and hydrogen is characterized in that: the method is used for sampling the samples without the oxide layer on at least one of the front and back surfaces of the sampling metal sample plate, and comprises the following steps:
the method comprises the following steps: fixing a sampling metal sample plate by using a clamp, wherein the thickness of the sampling metal sample plate is T;
step two: setting the front surface of the sampling metal sample plate as one surface without an oxide layer and the back surface with or without an oxide layer, wherein the diameter phi is used1The drill bit pre-drills a hole at the sampling position on the reverse side of the sampling metal sample plate, the depth of the drilled hole is H, H is T-H, and H is the height of a sampling cylinder;
step three: with an external diameter of phi2Inner diameter of phi3The hollow drill bit or the core drill bit is used for drilling and sampling at the position of the pre-drilled hole on the front surface of the sampling metal sample plate.
7. The method of processing oxygen, nitrogen, hydrogen analysis test samples by core drilling as claimed in claim 6, wherein: steps two and three may be replaced with: the method comprises the steps of pre-drilling a hole at the front sampling position of a sampling metal sample plate by using a hollow drill bit or a core drill bit, and drilling a through hole at the back sampling position of the sampling metal sample plate by using the drill bit for sampling.
8. The method of processing oxygen, nitrogen, hydrogen analysis test samples by core drilling as claimed in claim 7, wherein: when the drill bit and the hollow drill bit or the core drill bit are used for drilling, liquid nitrogen is gasified and then sprayed to the drilling part for cooling, so that hydrogen is prevented from overflowing from metal due to overheating of the drilling hole.
9. The method of processing oxygen, nitrogen, hydrogen analysis test samples by core drilling as claimed in claim 8, wherein: hollow or core drill bit inner diameter phi3I.e. the diameter of the sampling cylinder, the diameter phi of the drill bit1Not less than the outside diameter phi of a hollow or core drill bit2The height h of the sampling cylinder is directly calculated according to the requirements of the analytical instrument: according to the requirements of analytical instrument, sample mass m and drill diameter phi1Outside diameter phi of hollow bit or core bit2Inside diameter phi3；
Wherein rho is the density of the sample material, and pi is the circumferential ratio.
10. The method of processing oxygen, nitrogen, hydrogen analysis test samples by core drilling as claimed in claim 9, wherein: in the process of drilling and sampling, the drill bit and the hollow drill bit or the coring drill bit can be sequentially arranged on the same machine tool to drill and sample the same sample, and can also be respectively arranged on two machine tools to pre-drill and sample the two samples simultaneously.
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| JP2017166836A (en) * | 2016-03-14 | 2017-09-21 | パンパシフィック・カッパー株式会社 | Device and method for sampling of specimen for analysis |
| CN107764658A (en) * | 2017-11-23 | 2018-03-06 | 中南大学 | Simulating two-dimensional loads the experimental rig and method of liquid nitrogen cooling roadway excavation off-load |
| CN210603974U (en) * | 2019-06-05 | 2020-05-22 | 四川省乐山市科百瑞新材料有限公司 | Automatic sampling device of rare earth metal ingot |
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2020
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0862105A (en) * | 1994-08-18 | 1996-03-08 | Kawasaki Steel Corp | Method and apparatus for conditioning metal sample |
| CN101419135A (en) * | 2007-10-26 | 2009-04-29 | 首钢总公司 | Sampling method for analyzing slab hydrogen content distribution and chisel bit thereof |
| CN203443841U (en) * | 2013-09-12 | 2014-02-19 | 武汉华科新材料有限公司 | Crucible support for electrothermal smelter |
| CN104316345A (en) * | 2014-09-25 | 2015-01-28 | 江西稀有稀土金属钨业集团有限公司 | Multi-component rare earth raw material sampling method |
| JP2017166836A (en) * | 2016-03-14 | 2017-09-21 | パンパシフィック・カッパー株式会社 | Device and method for sampling of specimen for analysis |
| CN107764658A (en) * | 2017-11-23 | 2018-03-06 | 中南大学 | Simulating two-dimensional loads the experimental rig and method of liquid nitrogen cooling roadway excavation off-load |
| CN210603974U (en) * | 2019-06-05 | 2020-05-22 | 四川省乐山市科百瑞新材料有限公司 | Automatic sampling device of rare earth metal ingot |
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