CN108152101A - One thermal conductivity method of inert gas fusion measures nitrogen content sample-smelting method in ferrovanadium nitride - Google Patents
One thermal conductivity method of inert gas fusion measures nitrogen content sample-smelting method in ferrovanadium nitride Download PDFInfo
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- CN108152101A CN108152101A CN201711387995.1A CN201711387995A CN108152101A CN 108152101 A CN108152101 A CN 108152101A CN 201711387995 A CN201711387995 A CN 201711387995A CN 108152101 A CN108152101 A CN 108152101A
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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Abstract
The invention discloses a kind of one thermal conductivity methods of inert gas fusion to measure nitrogen content sample-smelting method in ferrovanadium nitride, uses suitable fluxing agent so that sample can fully dissolve, and nitrogen fully discharges, and improve the stability of analysis result；Suitable fluxing agent addition sequence is determined, improves analysis efficiency；The advantage of the invention is that：Nitrogen in ferrovanadium nitride can be fast and accurately measured, is preferably STEELMAKING PRODUCTION service, improves work efficiency, reduce production cost, increase economic benefit.
Description
Technical field
The present invention relates to a kind of method for measuring nitrogen content in ferrovanadium nitride and melting sample, specifically a kind of inert gas fusions one
Thermal conductivity method measures nitrogen content sample-smelting method in ferrovanadium nitride, belongs to the method field that nitrogen content in ferrovanadium nitride melts sample that measures.
Background technology
Ferrovanadium nitride is a kind of novel steel-making additive, adds people's ferrovanadium nitride that can play by force into steel in steelmaking process
Change precipitation, crystal grain thinning, increase the effects that yield strength of micro alloyed steel, content of nitrogen in vanadium-nitrogen alloy is the important finger of the product
Mark, its content of Accurate Determining are very necessary.My company's U.S.'s power can ONH836 gas analyzers, available for measuring powder sample
High content nitrogen, and using gas analyzer measure VN alloy in nitrogen had corresponding national standard（GBT 24583.2-
2009）, however, it was found that the fluxing agent used in national standard can not discharge nitrogen therein completely, if easy during the too small melting of crucible
Overflow sample.Measurement result is unstable, impact analysis result accuracy and stability.
In the reason of finding to influence experiment stability through analysis mainly sample caused by nitrogen release not exclusively, sample is melted at present
Method sample cannot melt completely causes in sample nitrogen release incomplete, about sample-smelting method be mainly fluxing agent and add in
The selection of sequence.Paper publishing is more on various publications, and the fluxing agent collocation mode of use also has very much, but sent out through actual tests
It is poor now to measure stability, usually primary experiment needs or so 4 hours, wastes more time and consumptive material.However, experiment consumption
When longer steel-making influence rhythm of production when quickly producing urgent experiment.Therefore, it finds suitable sample-smelting method and improves analysis efficiency
It is very urgent with accuracy.
Through consulting related data flux selection, there are following several methods：
1. use stannum fluxing agent and nickel fluxing agent（National standard method uses tin capsule and nickel basket）, by being limited by crucible volume, sample
Product reaction is excessively violent, easily sprays crucible, causes unstable result；
2. most papers can see melting effect using stannum fluxing agent and pure iron fluxing agent by the complete crucible sample of observation analysis
Fruit is bad.Analysis result is unstable.
Invention content
To solve the above-mentioned problems, the present invention devises a kind of one thermal conductivity method of inert gas fusion and measures nitrogen content in ferrovanadium nitride
Sample-smelting method can fast and accurately measure nitrogen in ferrovanadium nitride, be preferably STEELMAKING PRODUCTION service, improve work efficiency,
Production cost is reduced, increases economic benefit.
The technical scheme is that：
One thermal conductivity method of inert gas fusion measures nitrogen content sample-smelting method in ferrovanadium nitride, and concrete operation method is：
Fluxing agent is being added in crucible, molten sample is carried out as fluxing agent using tungsten fluxing agent, stannum fluxing agent and pure iron fluxing agent,
The fluxing agent addition is in the following ways：
Sample tin capsule is wrapped up, being put into 0.0200-0.0400g samples, 0.3g pure iron fluxing agents, 0.3g tungsten after crucible degassing helps
Flux is analyzed；
It is tested using national certified reference material, data analysis is accurate.Sample is spherical after the completion of analysis, illustrates that N is released
It discharges complete.
Since ferrovanadium nitride fusing point is higher（2360℃）Pure iron+pure tungsten+tin is selected when high frequency-infrared analysis of carbon and sulfur method measures
Fluxing agent carries out molten sample.
The addition sequence of the fluxing agent is：Tungsten fluxing agent-tin capsule-pure iron.
Using national certified reference material, analysis result is stablized.
Experiment finds that the stability that fluxing agent, sample addition sequence detect instrument has a significant impact, and sequence adds in not
Right, nitrogen release is incomplete in sample, and analysis result stability is poor（Standard sample, which need to analyze 15-20, can analyze stabilization）.
Various modes are arranged in pairs or groups, and find most suitable addition sequence.
The present invention uses the abundant sample dissolution of suitable fluxing agent so that nitrogen discharges completely, steady so as to obtain comparison
Fixed intensity and then it is converted into stable data.
The advantage of the invention is that：Use suitable fluxing agent so that sample can fully dissolve, and nitrogen is fully released
It puts, improves the stability of analysis result；Suitable fluxing agent addition sequence is determined, improves analysis efficiency.
With reference to specific embodiment, the invention will be further described.
Specific embodiment
The preferred embodiment of the present invention is illustrated below, it should be understood that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1
One thermal conductivity method of inert gas fusion measures nitrogen content sample-smelting method in ferrovanadium nitride, and concrete operation method is：
Fluxing agent is being added in crucible, molten sample is carried out as fluxing agent using tungsten fluxing agent, stannum fluxing agent and pure iron fluxing agent,
The fluxing agent addition uses three kinds of modes：
（1）Sample tin capsule is wrapped up, sample is put into after crucible degassing（0.02-0.04g is accurate to 0.0001g）, 0.3g pure iron
Fluxing agent, 0.3g tungsten fluxing agents, are analyzed；
（2）Sample tin capsule is wrapped up, sample is put into after crucible degassing（0.02-0.04g is accurate to 0.0001g）, 0.1g pure iron
Fluxing agent, 0.1g tungsten fluxing agents, are analyzed；
（3）Sample tin capsule is wrapped up, sample is put into after crucible degassing（0.02-0.04g is accurate to 0.0001g）, 0.5g pure iron
Fluxing agent, 0.5g tungsten fluxing agents, are analyzed.
It is tested using national certified reference material, first way data analysis is accurate.Sample is in after the completion of analysis
Spherical shape illustrates that N releases are complete.Other two kinds of analysis mode accuracy are poor and N element release is incomplete, sample after the completion of analysis
Product do not melt completely, are as a result not sufficiently stable.
Since ferrovanadium nitride fusing point is higher（2360℃）Pure iron+pure tungsten+tin is selected when high frequency-infrared analysis of carbon and sulfur method measures
Fluxing agent carries out molten sample.
The addition sequence of the fluxing agent is：1 tin capsule-pure iron-tungsten fluxing agent, 2 tin capsules-tungsten fluxing agent-pure iron, 3
Pure iron-tin capsule-tungsten fluxing agent, 4 pure iron-tungsten fluxing agent-tin capsule, 5 tungsten fluxing agents-tin capsule-pure iron, 6 tungsten fluxing agents-
One kind in pure iron -6 kinds of tin capsule combination.
Using national certified reference material, each analysis mode is measured 3 times, is found by experiment that, the 5th kind of addition sequence point
Result is analysed to stablize.
Various equipment employed in the present invention, are the conventional equipment used in the production technology of this field, and each equipment
Operation, parameter etc. carried out according to routine operation, have no special feature.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify to the technical solution recorded in foregoing embodiments or carry out equivalent replacement to which part technical characteristic.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (2)
1. one thermal conductivity method of inert gas fusion measures nitrogen content sample-smelting method in ferrovanadium nitride, which is characterized in that concrete operation method is：
Fluxing agent is being added in crucible, molten sample is carried out as fluxing agent using tungsten fluxing agent, stannum fluxing agent and pure iron fluxing agent,
The fluxing agent addition is in the following ways：
Sample tin capsule is wrapped up, being put into 0.0200-0.0400g samples, 0.3g pure iron fluxing agents, 0.3g tungsten after crucible degassing helps
Flux is analyzed；
Since ferrovanadium nitride fusing point is higher（2360℃）Select pure iron+pure tungsten+tin fluxing when high frequency-infrared analysis of carbon and sulfur method measures
Agent carries out molten sample.
2. one thermal conductivity method of inert gas fusion according to claim 1 measures nitrogen content sample-smelting method in ferrovanadium nitride, feature
It is：The addition sequence of the fluxing agent is：Tungsten fluxing agent-tin capsule-pure iron.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111521639A (en) * | 2020-05-13 | 2020-08-11 | 中天钢铁集团有限公司 | Combustion method for determining nitrogen content in alloy by Dumas combustion method |
| CN111948344A (en) * | 2020-08-11 | 2020-11-17 | 河南省金太阳精密铸业股份有限公司 | Method for analyzing and determining nitrogen content in silicon carbide |
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| CN111521639A (en) * | 2020-05-13 | 2020-08-11 | 中天钢铁集团有限公司 | Combustion method for determining nitrogen content in alloy by Dumas combustion method |
| CN111948344A (en) * | 2020-08-11 | 2020-11-17 | 河南省金太阳精密铸业股份有限公司 | Method for analyzing and determining nitrogen content in silicon carbide |
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Application publication date: 20180612 |