CN111521639A - Combustion method for determining nitrogen content in alloy by Dumas combustion method - Google Patents
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 64
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 43
- 239000000956 alloy Substances 0.000 title claims abstract description 43
- 238000009841 combustion method Methods 0.000 title claims abstract description 42
- 241000698776 Duma Species 0.000 title claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 30
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 40
- 238000002485 combustion reaction Methods 0.000 claims description 26
- 229910052759 nickel Inorganic materials 0.000 claims description 20
- 229910052721 tungsten Inorganic materials 0.000 claims description 20
- 239000010937 tungsten Substances 0.000 claims description 20
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 16
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 15
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 10
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 8
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 238000004458 analytical method Methods 0.000 abstract description 20
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000009628 steelmaking Methods 0.000 abstract description 4
- 238000001514 detection method Methods 0.000 description 23
- 238000012360 testing method Methods 0.000 description 10
- 238000002844 melting Methods 0.000 description 9
- 230000008018 melting Effects 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 229910001199 N alloy Inorganic materials 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- -1 ferrovanadium nitride Chemical class 0.000 description 5
- 230000004907 flux Effects 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 229910000616 Ferromanganese Inorganic materials 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 239000011261 inert gas Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 2
- 229910000628 Ferrovanadium Inorganic materials 0.000 description 2
- MPCRDALPQLDDFX-UHFFFAOYSA-L Magnesium perchlorate Chemical compound [Mg+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O MPCRDALPQLDDFX-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000010425 asbestos Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 2
- JHOPGIQVBWUSNH-UHFFFAOYSA-N iron tungsten Chemical compound [Fe].[Fe].[W] JHOPGIQVBWUSNH-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 229910052895 riebeckite Inorganic materials 0.000 description 2
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical class [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- RRZKHZBOZDIQJG-UHFFFAOYSA-N azane;manganese Chemical compound N.[Mn] RRZKHZBOZDIQJG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000003631 expected effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910001337 iron nitride Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000033764 rhythmic process Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/22—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a combustion method for determining nitrogen content in alloy by a Dumas combustion method. According to the invention, a suitable fluxing agent is used in combination with a Dumas combustion method, so that a sample can be sufficiently combusted and dissolved at a lower temperature in a short time, nitrogen elements are sufficiently released, and the stability and accuracy of an analysis result are improved; by determining a proper adding mode of the fluxing agent, the nitrogen content analysis efficiency is improved; the invention has the advantages that: the method can rapidly and accurately measure the nitrogen in the alloy, better serve the steelmaking production, improve the working efficiency, reduce the production cost and increase the economic benefit.
Description
Technical Field
The invention relates to a combustion method for measuring nitrogen content in alloy, in particular to a combustion method for measuring nitrogen content in alloy by using a Dumas combustion method, and belongs to the field of methods for measuring nitrogen content combustion of alloy.
Background
The alloy is an important raw material used in the steelmaking process, the nitrogen content in the alloy directly influences the quality of a finished product, and accurate determination of the nitrogen content is very necessary. At present, when the nitrogen content is analyzed by adopting the traditional wet method, an acid is generally used for dissolving a sample, and then alkali distillation is carried out; or directly melting the sample with alkali, extracting nitrogen in the form of NH by using carrier gas, introducing the extracted nitrogen into a receiving cup containing absorption liquid, titrating the nitrogen by using dilute acid with known concentration, and finally calculating the nitrogen content. Although accurate results can be obtained, the analysis operation is complicated, the inspection period is long, and toxic and harmful gas and waste liquid are generated in the analysis process, which may cause harm to inspection personnel and environment. The method for measuring the nitrogen content in the alloy by the inert gas melting thermal conductivity method is widely applied in the prior art and has a national standard method, but the temperature in the inert gas melting thermal conductivity method is required to be increased to be higher than the melting point of the sample to melt the alloy sample, the temperature is about 3000 ℃, the load on an instrument is large (the heating and melting of the inert gas melting thermal conductivity method are physical changes), and when the temperature is instantly increased to be about three thousand ℃ by pulse heating, the sample is obviously splashed, and the detection stability is poor.
Most of the Dumas combustion method is only used for nitrogen detection in the fields of feed, food and the like at present, and the research on the detection of metallurgical raw materials by the Dumas combustion method is not seen yet. Therefore, how to adopt the Dumas combustion method to efficiently and accurately measure the nitrogen content in the alloy is the technical problem to be solved by the invention.
In the process of studying the problems, the inventor tries to measure the nitrogen content of the powder sample by using a LECO-FP628 nitrogen analyzer, but finds that the nitrogen in the high-melting-point alloy (such as ferrovanadium nitride, ferrosilicon nitride, manganese nitride and the like) can not be completely released in a short time in the detection process, and the stability of the analysis result and the detection efficiency are influenced.
Analysis shows that the reason influencing the test stability is mainly caused by incomplete nitrogen release in a sample, a combustion method without adding a fluxing agent enables the sample not to be completely combusted in a short time, so that the nitrogen release in the sample is incomplete, the combustion method mainly refers to the addition of the fluxing agent, a plurality of papers are published on various publications, and a plurality of fluxing agent collocation modes are adopted, but the test stability is found to be poor through practical tests, about 2 hours is usually needed in one test, and more time and consumables are wasted. However, the long time-consuming test seriously affects the production rhythm when the steel-making rapid production is subjected to the emergency test.
Therefore, it is not easy to find a proper combustion method for determining the nitrogen content in the alloy by the dumas combustion method to improve the analysis efficiency and accuracy.
Disclosure of Invention
In order to solve the problems in the background art, the invention designs the combustion method for determining the nitrogen content in the alloy by the Dumas combustion method, the method can rapidly and accurately determine the nitrogen in the alloy, and has the advantages of short detection period, low detection temperature, high automation degree and stable and accurate retrieval result, so that the method can better serve for steelmaking production, the working efficiency is improved, the production cost is reduced, and the economic benefit is increased.
In order to achieve the purpose, the invention adopts the technical scheme that:
the combustion method for determining the nitrogen content in the alloy by the Dumas combustion method comprises the following specific operation methods:
(1) wrapping a nitrogenous alloy sample by using a tin sheet, and putting a nickel fluxing agent and a tungsten fluxing agent into the tin sheet;
(2) and (3) placing the substance wrapped by the tin sheet into a sample injector of an LECO-FP628 nitrogen analyzer, introducing pure oxygen (the flow of the pure oxygen is 300-450 mL/min), burning the nitrogen-containing alloy sample in a pure oxygen environment, and measuring the nitrogen content in the alloy by adopting a conventional Dumas burning method after burning.
Further, the subsequent conventional Dumas combustion method detection method comprises the following steps: the mixed gas containing nitrogen oxide generated after combustion is collected in the gas mixing cavity, gas is taken through the quantitative gas measuring cavity, redundant oxygen is removed from the quantitative gas through the pure copper column, the nitrogen oxide is completely converted into nitrogen through the nitrogen catalyst, water and carbon dioxide are removed through the magnesium perchlorate and the alkali asbestos, and only residual N is left in the residual sampling gas2And the carrier gas (He) is brought into a thermal conductivity cell for TCD detection. The above-mentioned steps are well known in the art, and conditions thereof are not particularly limited.
Further, nickel particles-tungsten simple substance is adopted as fluxing agent.
Preferably, the tin flakes: nickel: tungsten: the mass ratio of the sample is 5:1:1: 0.4-0.6;
preferably, the grain size of the alloy sample is not more than 0.074 mm.
The method can be applied to the determination of the alloy with 0.8 to 29 wt.% of nitrogen content which is common at present. The combustion temperature and the combustion time of different alloys are slightly different, and can be adjusted according to actual conditions, so that the purpose of full combustion and release can be achieved. The combustion and dissolution temperature is 900-1000 ℃, and the combustion and dissolution time is 240-330 s.
Further comprises the following steps: vanadium nitride, ferrovanadium nitride, ferromanganese nitride, ferrosilicon nitride and nitrogen alloy cored wire.
Wherein, when the sample is vanadium-nitrogen alloy (nitrogen content is 13.14% -16.64%), the combustion temperature is as follows: at 950 ℃, the nitrogen can be fully combusted and released by heating for 270s of combustion time.
When the sample is the nitrogen alloy cored wire (the nitrogen content is 26-28%), the combustion temperature is 1000 ℃, the combustion time is 330s, and nitrogen is fully combusted and released.
When the sample is nitrided ferromanganese alloy (the nitrogen content is 7% -8%), the combustion temperature is 950 ℃, and the combustion time is set to 240s, so that nitrogen is fully combusted and released.
The determination of heating combustion dissolution in the alloy by the Dumas combustion method is a chemical change, namely, the oxidation-reduction reaction of an alloy sample and oxygen is carried out, nitrogen elements in the sample react with oxygen elements to generate nitrogen-oxygen compounds for release, and the nitrogen compounds are completely reduced into nitrogen through a nitrogen catalyst for detection. Compared with a physical melting method of an inert gas melting thermal conduction method, the method has different reaction principles, and can finish accurate and stable determination at a lower temperature in a shorter time.
The tungsten fluxing agent and the nickel particles are fluxing agents, and the adding amount of the fluxing agents is controlled in the Dumas combustion method, so that a sample can be completely combusted in a short time, the measurement result is stable, the national certified standard substances are used for verification, the analysis result is stable, and the detection precision is high. And if no fluxing agent is added, the nitrogen in the high-melting-point sample is not completely released in a short time, and the stability of the analysis result is poor.
The tungsten particles in the fluxing agent can be oxidized in pure oxygen to generate tungsten trioxide, so that the stable combustion effect can be achieved, a sample can be stably combusted in a pure oxygen environment, heat generated after the tungsten particles cover the sample and are beneficial to full combustion and melting of the sample, and release of nitrogen oxide is facilitated, so that an experimental result is stabilized.
The invention has the advantages that:
the method adopts a Dumas combustion method to measure the nitrogen content in the alloy for the first time, and finds and obtains a sample with a proper grain size (not more than 0.074mm), sample weighing, combustion time, combustion temperature, fluxing agent, proper fluxing agent combination and addition amount, so that the sample can be fully combusted, nitrogen elements are fully released, the stability of an analysis result is obviously improved, and the analysis efficiency is improved. Therefore, compared with the method, the method of the invention not only obviously reduces the heating temperature and shortens the comprehensive detection time, but also improves the precision and the stability. Provides reference for the application of the Dumas combustion method in the metallurgical raw material inspection.
Detailed Description
The present invention will be further described with reference to the following specific examples.
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
The national certified standard sample GBW (E)010299 is used for carrying out verification detection, wherein the standard value of the nitrogen content is 14.57%.
Blank experiment: measuring the blank value of the fluxing agent (nickel particles-tungsten) for 11 times to determine a detection limit and a measurement lower limit, wherein the standard deviation of the finally obtained blank value is 0.002%, and the standard deviation of the detection limit calculation method according to the blank value of 3 times is 0.006%; the lower limit of detection was 0.02% as the standard deviation of 10-fold blank.
The combustion method for determining the nitrogen content in the alloy by the Dumas combustion method comprises the following specific operation methods: adding the standard sample and the fluxing agent into a tin sheet, wherein a tungsten fluxing agent and a nickel fluxing agent are used as a combined fluxing agent for combustion, and the adding amount of the fluxing agent adopts the following mode:
mode 1
(1) Wrapping 0.0500g (to the nearest 0.0001g) of the standard sample with a tin sheet;
(2) placing a sample wrapped by a tin sheet (0.5g) in a sample injector of an LECO-FP628 nitrogen analyzer, placing the sample in a pure oxygen environment for combustion, wherein the oxygen flow is 300mL/min, the heating temperature is heated to 950 ℃, the heating combustion time is 270s, after combustion and dissolution, taking gas through a quantitative gas measuring cavity, removing redundant oxygen through a pure copper column, converting nitrogen oxide into nitrogen through a nitrogen catalyst, removing water and carbon dioxide through magnesium perchlorate and alkali asbestos, and carrying the nitrogen gas into a thermal conductivity cell TCD for detection.
Mode 2
Wrapping a sample, a nickel fluxing agent and a tungsten fluxing agent by using tin sheets (0.5g), wherein the mass of the sample is 0.0500g (accurate to 0.0001g), the mass of the nickel fluxing agent is 0.1g, and the mass of the tungsten fluxing agent is 0.1 g; the subsequent detection and analysis method is the same as mode 1.
Mode 3
Wrapping a sample, a nickel fluxing agent and a tungsten fluxing agent by using tin sheets (0.5g), wherein the mass of the sample is 0.0500g (accurate to 0.0001g), the mass of the nickel fluxing agent is 0.2g, and the mass of the tungsten fluxing agent is 0.2 g; the subsequent detection and analysis method is the same as mode 1.
Mode 4
Wrapping a sample, a nickel fluxing agent and a tungsten fluxing agent by using tin sheets (0.5g), wherein the mass of the sample is 0.0500g (accurate to 0.0001g), the mass of the nickel fluxing agent is 0.3g, and the mass of the tungsten fluxing agent is 0.3 g; the subsequent detection and analysis method is the same as mode 1.
The results of the 4 addition modes are shown in Table 1.
TABLE 1
As can be seen from Table 1, the results obtained by the second analysis method are closest to the standard values and have high stability. The accuracy of the first analysis mode is poor, the N element is not completely released, a sample is not completely combusted after the analysis is completed, and the result is not stable enough. In the other two analysis methods, the amount of the added flux is too large, which easily causes splashing, and results in unstable measurement results.
Under the same instrument working condition, three other different flux combination methods (A nickel particle-tungsten flux, B pure iron-tungsten flux, C nickel particle-pure iron) are adopted for testing, and each analysis method is used for measuring 5 times, and specifically comprises the following steps:
method A
Nickel particle-tungsten fluxing agent adding mode
And (3) wrapping the sample, the nickel fluxing agent and the tungsten fluxing agent by using tin sheets, wherein the using amount and the detection operation are the same as those in the mode 2.
Method B
Adopts the mode of adding pure iron-tungsten fluxing agent
The sample (0.0500 g), pure iron (0.1 g) and tungsten flux (0.1 g) were wrapped with tin foil, and the rest of the operation and detection were carried out in the same manner as in mode 2.
Method C
Adding mode of nickel particles and pure iron
The sample (0.0500 g), pure iron (0.1 g) and nickel (0.1 g) were wrapped with tin foil, and the remaining operation and detection method were the same as in mode 2.
The results of the 3 addition modes are shown in Table 2.
TABLE 2
The results in Table 2 show that the fluxing agent in the method A has good fluxing effect, the goodness of fit between the measured value and the standard value of the sample is high, and the stability of the method is satisfactory.
Subsequently, the vanadium-nitrogen alloy real sample was subjected to 10 parallel measurements in the mode 2, and the relative standard deviation (RSD, n is 10) of the measured values was 0.42% to 0.50%, and the Standard Deviation (SD) was 0.060% to 0.071%. Through a large number of experiments, the key technical problems of sample weighing, burning time, working conditions and the like in the vanadium-nitrogen alloy test by the Dumas combustion method are well solved.
In order to further illustrate that the Dumas combustion method can also be used for measuring the nitrogen content in other alloys and achieve the expected effect, the invention takes ferromanganese nitride and a nitrogen alloy core-spun yarn as examples, and the nitrogen content of the ferromanganese nitride and the nitrogen alloy core-spun yarn are greatly different, so that the method of the invention can be applied to common nitrogen-containing alloys.
Wherein, the actual sample of the manganese iron nitride with the nitrogen content of 7-8% is measured, and the burning time is set to be 240s, and the burning temperature is set to be 950 ℃; the remaining amounts used and the operating conditions were the same as in mode 2. The measurement results were compared with the results of manual wet tests.
And (3) measuring an actual sample with the nitrogen content of 26-28% of the nitrogen alloy cored wire, setting the combustion time to be 330s and the combustion temperature to be 1000 ℃, and keeping the rest working conditions the same as the mode 2. The measurement results were compared with the results of manual wet tests.
TABLE 3
As can be seen from the results in Table 3, the nitrogen measurements obtained by the Dumas combustion method for the two alloy samples are substantially identical to the results of the manual wet analysis, and the standard deviation and the relative standard deviation of the Dumas combustion method are satisfactory. Therefore, the Dumas combustion method can be used for measuring the nitrogen content of the conventional alloy, and has good stability and high accuracy.
The various devices adopted in the invention are conventional devices used in the production process in the field, and the operation, parameters and the like of each device are carried out according to the conventional operations without special points.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The combustion method for determining the nitrogen content in the alloy by the Dumas combustion method is characterized in that a nitrogen-containing alloy sample and a fluxing agent are wrapped by a tin sheet, the wrapped nitrogen-containing alloy sample and the fluxing agent are placed in a nitrogen analyzer, pure oxygen is introduced, the wrapped nitrogen-containing alloy sample is combusted and dissolved for a period of time in a pure oxygen environment, the nitrogen oxide gas is fully combusted and released by the nitrogen-containing alloy sample, and the nitrogen content in the alloy is determined by the Dumas combustion method subsequently.
2. The combustion method for determining the nitrogen content in the alloy by the dumas combustion method as claimed in claim 1, characterized in that: the fluxing agent is nickel particles and tungsten particles.
3. The combustion method for determining the nitrogen content in the alloy by the dumas combustion method as claimed in claim 1, characterized in that: the method is suitable for measuring the alloy with the nitrogen content of 0.8-29 percent.
4. The combustion method for determining the nitrogen content in an alloy according to claim 2, characterized in that: the mass ratio of the tin sheet to the nickel particles to the tungsten fluxing agent to the nitrogen-containing sample is 5:1:1: 0.4-0.6.
5. The combustion method for determining the nitrogen content in an alloy according to claim 2, characterized in that: the combustion temperature is 900-1000 ℃, and the combustion time is 240-330 s.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114280100A (en) * | 2021-12-29 | 2022-04-05 | 攀钢集团西昌钢钒有限公司 | Method for detecting nitrogen content in manganese metal |
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