CN114280100A - Method for detecting nitrogen content in manganese metal - Google Patents
Method for detecting nitrogen content in manganese metal Download PDFInfo
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- CN114280100A CN114280100A CN202111646045.2A CN202111646045A CN114280100A CN 114280100 A CN114280100 A CN 114280100A CN 202111646045 A CN202111646045 A CN 202111646045A CN 114280100 A CN114280100 A CN 114280100A
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- Prior art keywords
- nitrogen content
- nickel
- manganese metal
- sample
- nitrogen
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 39
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 38
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 35
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 76
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 38
- 239000002775 capsule Substances 0.000 claims abstract description 15
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 7
- 238000001514 detection method Methods 0.000 claims description 13
- 238000004458 analytical method Methods 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000012159 carrier gas Substances 0.000 claims description 4
- 238000007872 degassing Methods 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 239000011572 manganese Substances 0.000 claims description 4
- 230000010354 integration Effects 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 238000007689 inspection Methods 0.000 claims 1
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 6
- 238000004821 distillation Methods 0.000 abstract description 4
- 239000011261 inert gas Substances 0.000 abstract description 4
- 238000002835 absorbance Methods 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 3
- 238000011161 development Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 2
- 229910000831 Steel Inorganic materials 0.000 description 7
- 239000010959 steel Substances 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VRZJGENLTNRAIG-UHFFFAOYSA-N 4-[4-(dimethylamino)phenyl]iminonaphthalen-1-one Chemical compound C1=CC(N(C)C)=CC=C1N=C1C2=CC=CC=C2C(=O)C=C1 VRZJGENLTNRAIG-UHFFFAOYSA-N 0.000 description 1
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910021652 non-ferrous alloy Inorganic materials 0.000 description 1
- 238000011022 operating instruction Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides a method for detecting nitrogen content in manganese metal, which comprises the following steps: A) putting a manganese metal sample into a nickel bag, exhausting air from the obtained nickel bag and sealing the nickel bag; B) and B) placing the nickel capsule obtained in the step A) in a nitrogen-oxygen analyzer to detect the nitrogen content. The application provides a method for measuring the nitrogen content in manganese metal by a pulse heating-inert gas melting-thermal conductivity method, the method does not need to use acid and alkali reagents and a distillation instrument to process samples, and the sample processing operation is simple and convenient and does not take time; meanwhile, reagent development is not needed in the testing process, a spectrophotometer is not needed to be used for measuring absorbance, and the sample is simple and convenient to detect and convenient to control quality.
Description
Technical Field
The invention relates to the technical field of detection and assay, in particular to a method for detecting nitrogen content in manganese metal.
Background
The manganese metal plays an important role in smelting high-grade alloy steel and non-ferrous alloy, can be used as a manganese element additive or deoxidize, but the nitrogen content in molten steel can be correspondingly increased by adding the manganese metal, steel with high nitrogen content is placed for a long time, the performance becomes brittle (aging), when the nitrogen content in the steel is high, the surface turns blue when the steel is heated to the temperature range of 250-450 ℃, the strength of the steel is increased, and the impact toughness is reduced (blue brittleness), so that part of steel mills bring the nitrogen content in the manganese metal into raw material acceptance indexes.
At present, other methods for measuring the nitrogen content in domestic manganese-free metal comprise a distillation-neutralization titration method of alloy and nitrided alloy, but the distillation-neutralization titration method has the problems of complicated steps, long time consumption and complicated operation.
Disclosure of Invention
The invention aims to provide a method for detecting the nitrogen content in manganese metal, which can accurately detect the nitrogen content in manganese and has the advantages of simple operation and short time.
In view of this, the present application provides a method for detecting nitrogen content in manganese metal, including the following steps:
A) putting a manganese metal sample into a nickel bag, exhausting air from the obtained nickel bag and sealing the nickel bag;
B) and B) placing the nickel capsule obtained in the step A) in a nitrogen-oxygen analyzer to detect the nitrogen content.
Preferably, the particle size of the manganese metal sample is less than 0.125 mm.
Preferably, phi x h of the nickel capsule is (5-7) mm x (9-12) mm.
Preferably, the tool for sealing is nipper pliers.
Preferably, the detection temperature is 20-30 ℃.
Preferably, the detection conditions are specifically as follows: the integration time is 60s, the carrier gas flow is 3.0L/min, the comparison level is 1.0 percent, the crucible degassing power is 7.00KW, and the sample analysis power is 5.50 KW.
The application provides a method for detecting nitrogen content in manganese metal, which comprises the following steps: A) placing a manganese metal sample in a nickel bag, exhausting air from the opening of the obtained nickel bag and sealing the opening; B) and B) placing the nickel capsule obtained in the step A) in a nitrogen-oxygen analyzer to detect the nitrogen content. The application provides a method for measuring the nitrogen content in manganese metal by a pulse heating-inert gas melting-thermal conductivity method, the method does not need to use acid and alkali reagents and a distillation instrument to process samples, and the sample processing operation is simple and convenient and does not take time; meanwhile, reagent development is not needed in the testing process, a spectrophotometer is not needed to be used for measuring absorbance, and the sample is simple and convenient to detect and convenient to control quality. In conclusion, compared with the existing method, the method for detecting the nitrogen content in the manganese metal is simple and convenient, short in time consumption, good in determination precision and high in accuracy.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
In view of the fact that no instrument detection method for detecting the nitrogen content in the metal manganese exists in the prior art, the method for detecting the nitrogen content in the metal manganese is provided, the method uses a pulse heating-inert gas melting-thermal conductivity method to measure the nitrogen content in the metal manganese, and the method has the advantages of being accurate and fast. Specifically, the embodiment of the invention discloses a method for detecting the nitrogen content in manganese metal, which comprises the following steps:
A) putting a manganese metal sample into a nickel bag, exhausting air from the obtained nickel bag and sealing the nickel bag;
B) and B) placing the nickel capsule obtained in the step A) in a nitrogen-oxygen analyzer to detect the nitrogen content.
In the provided detection method, firstly, a manganese metal sample is placed in a nickel bag, and then the obtained nickel bag is evacuated and sealed. In the application, the granularity of the manganese metal sample is less than 0.125mm, and phi x h of the nickel capsule is (5-7) mm x (9-12) mm; in a specific embodiment, φ × h of the nickel capsule is 6mm × 10 mm. This application adopts sharp-nosed pliers to compress tightly the nickel bag mouth and exhaust gas, adjusts at any time when compressing tightly the nickel bag mouth to avoid the too big card appearance that leads to of nickel bag diameter.
After the sample is obtained, the application preferentially calibrates the nitrogen-oxygen analyzer, and then detects the content of nitrogen in the sample for the obtained nickel capsule. The detection of the nitrogen content in the manganese metal is a detection method that a combustion sample is heated by a pulse heating furnace under inert gas, and the nitrogen content in the sample is measured by a thermal conductivity detector; in the present application, the model of the nitrogen oxygen analyzer is EMGA-820, and the detection conditions are specifically as follows: the integration time is 60s, the carrier gas flow is 3.0L/min, the comparison level is 1.0 percent, the crucible degassing power is 7.00KW, and the sample analysis power is 5.50 KW.
Compared with the existing method for detecting the content of nitrogen in the alloy, the method does not need to use acid and alkali reagents and a distillation instrument to process samples, and is simple and convenient to operate and free of time consumption; reagent color development is not needed, a spectrophotometer is used for measuring absorbance, sample detection is simple and convenient, and quality control is convenient. In conclusion, compared with the existing method, the method for measuring the nitrogen content in the manganese metal provided by the invention is simple and convenient to operate, short in time consumption, good in measurement precision and high in accuracy.
In order to further understand the present invention, the following examples are provided to describe the method for detecting the nitrogen content in manganese metal in detail, and the scope of the present invention is not limited by the following examples.
(1) Weighing sample
Weighing a 0.1g +/-0.1 mg manganese metal sample (less than 0.125mm) in a nickel capsule (phi multiplied by h is approximately equal to 6mm multiplied by 10mm), using a tool (such as a sharp nose pliers) to compress the mouth of the nickel capsule and discharge air, adjusting at any time when compressing the mouth of the nickel capsule, and avoiding the sample clamping caused by overlarge diameter of the nickel capsule;
(2) measurement of
A. Oxygen nitrogen meter calibration
Weigh 0.1g alloy standard sample in the nickel bag, use tools (like sharp-nosed pliers) compress tightly the nickel bag mouth and exhaust air, adjust at any time when compressing tightly the tweezers bag mouth, avoid the too big card appearance that leads to of nickel bag diameter, place the nickel bag on the oxygen nitrogen appearance (equipment model EMGA-820), specific condition: integrating time is 60s, carrier gas flow is 3.0L/min, the comparison level is 1.0%, crucible degassing power is 7.00KW, sample analysis power is 5.50KW, operating is carried out according to instrument operating instructions, and the instrument is calibrated;
B. determination of nitrogen content
Placing the weighed sample and the closed nickel capsule on an oxygen nitrogen instrument after calibration for automatic analysis, wherein the measurement result is shown in table 1;
TABLE 1 determination of nitrogen content in manganese metal by the method of the present invention
Note: range-max-min, RSD: relative standard deviation.
(3) Comparative test
In consideration of the content range of the manganese metal, the nitrogen content in the manganese metal is measured by adopting the existing national standard GB/T223.37-1989 method for measuring the nitrogen content of steel and alloy by distillation and separation indophenol blue spectrophotometry, and the measurement result is shown in the table 2;
table 2 comparison of the nitrogen content determined by the conventional method and the nitrogen content determined by the present invention
From the comparative results in table 2, the precision of the present invention is significantly better than the prior art methods.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. A method for detecting the nitrogen content in metal manganese comprises the following steps:
A) putting a manganese metal sample into a nickel bag, exhausting air from the obtained nickel bag and sealing the nickel bag;
B) and B) placing the nickel capsule obtained in the step A) in a nitrogen-oxygen analyzer to detect the nitrogen content.
2. The detection method according to claim 1, wherein the particle size of the manganese metal sample is < 0.125 mm.
3. The method of claim 1, wherein φ xh of the nickel capsules is (5-7) mm x (9-12) mm.
4. The inspection method of claim 1, wherein the sealing tool is a nipper pliers.
5. The method according to claim 1, wherein the temperature of the detection is 20 to 30 ℃.
6. The detection method according to claim 1, wherein the detection conditions are specifically: the integration time is 60s, the carrier gas flow is 3.0L/min, the comparison level is 1.0 percent, the crucible degassing power is 7.00KW, and the sample analysis power is 5.50 KW.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111646045.2A CN114280100B (en) | 2021-12-29 | 2021-12-29 | Method for detecting nitrogen content in manganese metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111646045.2A CN114280100B (en) | 2021-12-29 | 2021-12-29 | Method for detecting nitrogen content in manganese metal |
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| Publication Number | Publication Date |
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| CN114280100A true CN114280100A (en) | 2022-04-05 |
| CN114280100B CN114280100B (en) | 2024-09-17 |
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