CN107421908A - A kind of method of carbon in method of high frequency IR-absorption final slag modifier - Google Patents

A kind of method of carbon in method of high frequency IR-absorption final slag modifier Download PDF

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Publication number
CN107421908A
CN107421908A CN201710624797.6A CN201710624797A CN107421908A CN 107421908 A CN107421908 A CN 107421908A CN 201710624797 A CN201710624797 A CN 201710624797A CN 107421908 A CN107421908 A CN 107421908A
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Prior art keywords
carbon
final slag
slag modifier
high frequency
sample
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CN201710624797.6A
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张育新
谢永宏
许鸿英
耿艳霞
王占荣
贺红侠
王洁源
田月华
詹娟
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Xuanhua Iron and Steel Group Co Ltd
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Xuanhua Iron and Steel Group Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Refinement Of Pig-Iron, Manufacture Of Cast Iron, And Steel Manufacture Other Than In Revolving Furnaces (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The invention discloses a kind of method of carbon in method of high frequency IR-absorption final slag modifier, methods described utilizes high frequency-infrared carbon sulphur instrument, establishes calibration curve using lime stone standard sample, carbon in final slag modifier is analyzed;Fluxing agent is added during the analysis, the fluxing agent is pure iron, tungsten particle, any one or a few mixture of tin grain.Analysis method of the present invention is fast and convenient, and demand is fast and accurately analyzed in adaptation;Efficiently solve no final slag modifier standard sample and can not directly establish the problem of carbon sulphur instrument calibration curve;Effectively protect high frequency-infrared carbon sulphur instrument without prejudice by reducing sample weighting amount, reduce the volatilization of dust in melting process, reduce influence of the dust adsorption to analysis result stability.

Description

A kind of method of carbon in method of high frequency IR-absorption final slag modifier
Technical field
The invention belongs to material composition analysis determining technology field, and in particular to a kind of method of high frequency IR-absorption finishing slag The method of carbon in modification agent.
Background technology
During pneumatic steelmaking, add final slag modifier after, can play residue adjustment effect, improve slag in carbon, content of magnesium, and with end Slag is chemically reacted, and changes slag phase, and high molten protective layer is formed to furnace wall by splashing slag, reaches the purpose of protection furnace lining, prolongs Long converter service life.The height of carbon content directly affects its fusing time in converter finishing slag in finishing slag transformation of the way agent, therefore Carbon element content has great importance to steel-making link slag splashing in Accurate Determining final slag modifier.
The analysis method of carbon has a lot, such as gas volumetric method, non-aqueous titration, conductance method, but determines above Square law device is complicated, and operation is lengthy and tedious, and analytical cycle length, intensity of workers is high, and a variety ofization are needed to use during analysis Learning reagent causes environmental pollution, and certain danger be present, it is impossible to meets not only quick but also accurate analysis of modernization requirement.
High frequency-infrared carbon sulphur instrument is the equipment of domestic and international relatively advanced specialty analysis carbon-sulfure elements at present, has operation letter Just the advantages that, analysis is quick, measure content range is wide, precision is high, its carbon analysis precision:Sample size≤0.002% (m/m), n-1≤0.00003% (m/m);Sample size > 0.002% (m/m), n-1≤0.0001% (m/m) orCV≤0.5%.
The standard sample of current final slag modifier no on the market establishes calibration curve available for high frequency-infrared carbon sulphur instrument, and Carbon content is higher in final slag modifier, generally >=6.0%, and when high frequency-infrared carbon sulphur instrument uses standard sample weighting amount 0.1g carbon survey It is 0-6% to measure scope, and modification agent density is small, and dust is big, be also easy to produce during analysis a large amount of dust be attached to metal filter screen and In analysis channel, instrument is polluted, causes analysis result inaccurate, to sum up, it is necessary to finds a kind of rationally reliable standard sample and uses In establishing calibration curve, explore optimum analysis condition and realize carbon element content in method of high frequency IR-absorption final slag modifier.
The content of the invention
The technical problem to be solved in the present invention is to provide carbon in a kind of method of high frequency IR-absorption final slag modifier Method, realize the quick measure of carbon in final slag modifier.
In order to solve the above technical problems, the present invention adopts the technical scheme that:A kind of method of high frequency IR-absorption finishing slag The method of carbon in modification agent, methods described utilize high frequency-infrared carbon sulphur instrument, and it is bent to establish calibration using lime stone standard sample Line, carbon in final slag modifier is analyzed;Fluxing agent is added during the analysis, the fluxing agent is pure iron, tungsten Any one or a few mixture in grain, tin grain.
The measurement range of carbon is 0-6% when high frequency-infrared carbon sulphur instrument of the present invention uses standard sample weighting amount 0.1g, and modification agent is close Spend small, dust is big, and a large amount of dust is also easy to produce during analysis and is attached in metal filter screen and analysis channel, pollutes instrument, leads Cause analysis result inaccurate, so sample weighting amount is set to 0.05 ± 0.0001g by this method.
Pure iron addition is 6 times of sample final slag modifier quality in fluxing agent of the present invention.
Tungsten particle addition is 30 times of sample final slag modifier quality in fluxing agent of the present invention.
Tin grain addition is 6 times of sample final slag modifier quality in fluxing agent of the present invention.
Fluxing agent order of addition of the present invention is pure iron, tungsten particle, tin grain;The sample final slag modifier is after pure iron Addition.
The method of the invention establishes calibration curve using the method for two-point calibration.
The sample of the invention that does every time is first measured to monitoring sample before, and monitoring sample is changed using lime stone standard sample After calculation parallel determination is carried out on the basis of carbon content at least twice, it is desirable to difference≤0.1% of measurement result, to determine that working curve can To carry out normal assay work.
The principle of the invention and mentality of designing:
Generally >=6%, when high-frequency induction infrared C-S analyzer uses standard sample weighting amount 1g, it measures model to the carbon content of final slag modifier Enclose:ω(C)=0.001~6.000%, therefore the present invention realizes that sample detects using the method for reducing sample weighting amount, due to modification agent Density is smaller, and dust is larger, and a large amount of dust is also easy to produce during analysis and is attached in metal filter screen and analysis channel, pollution Instrument, cause analysis result inaccurate, weigh 0.05g samples in the process of the present invention and tested, analysis curve is shown in Fig. 1, can See that absworption peak is obvious, curve smoothing, meet analysis demand.
Because final slag modifier belongs to non-magnetic material, it is necessary to add magnetisable material and ensure good conductive magnetic properties side Combustion-supporting burning, promote gas release complete, tested in the present invention using tungsten particle+tin grain+pure iron compound additive.When tungsten particle adds Curve is analyzed when dosage is less than 1.3g and jagged peaks occurs, gas release is uneven, and analysis result is unstable;Tin grain addition is less than Sample can not be melted fully during 0.25g, and bath surface has residue, but because tin aoxidizes generation SnO2Belong to basic anhydride, add Enter excessively, the release of carbon sulphur gas can be influenceed, cause Lower result;Test result fluctuation is larger when pure iron addition is less than 0.3g, Add excessive and can cause to waste, increase analysis cost.Test and show when sample weighting amount is 0.05g, fluxing agent addition tungsten particle 1.5g, tin grain 0.3g, pure iron 0.3g, best results are melted, and it is rebasing with pure iron, final slag modifier sample is added, tungsten particle is covered The order on sample top, being eventually adding tin grain is covered, the bath surface after burning is bright and clean, bubble-free, and slag is smooth, and analysis peak is bent Line is smooth, and gas release is complete, and analysis result is stable.
Because final slag modifier is typically that dolomite and anchracite duff preparation are compounded after flotation magnesite mine tailing is light-burned , its material composition is close with lime stone, so the present invention establishes high frequency-infrared analysis of carbon and sulfur song using lime stone standard sample Line, the CaO indicated using lime stone standard sample, content of MgO are calculated the mass fraction of C content, used using scaled data The method of one standard sample two-point calibration establishes calibration curve, and can fast and accurately determine finishing slag according to this calibration curve changes Carbon element content in matter agent.
Calculate the formula of C content in lime stone standard sample:
C%=(12×CaO%)/56.077+(12×MgO%)/40.304
In formula:
CaO% --- CaO content in standard sample;
56.077 --- CaO relative molecular mass;
MgO% --- MgO content in standard sample;
40.304 --- MgO relative molecular mass.
The numbering and conversion situation for the lime stone standard sample that this method uses are as shown in table 1.
The standard sample scaled value of table 1
First above-mentioned standard sample is measured before making sample every time, the difference of the data of standard sample parallel determination twice exists It is normal within 0.1%, illustrates that data stabilization is reliable;Sample to be tested is analyzed according to the method described above, produces carbon in final slag modifier Constituent content.
It is using beneficial effect caused by above-mentioned technical proposal:1st, analysis method of the present invention is fast and convenient, adapts to fast Fast accurately analysis demand.2nd, the present invention efficiently solves no final slag modifier standard sample and can not directly establish carbon sulphur instrument The problem of calibration curve.3rd, the present invention effectively protects high frequency-infrared carbon sulphur instrument without prejudice by reducing sample weighting amount, reduces melting During dust volatilization, reduce influence of the dust adsorption to analysis result stability.
Brief description of the drawings
Fig. 1 is carbon peak shape figure when using 0.05g sample weighting amounts in experimentation;
Fig. 2 is the carbon peak shape figure that the method for embodiment 3 analyzes lime stone YSBC28701-93.
Embodiment
Because final slag modifier belongs to non-magnetic material, it is necessary to add magnetisable material and ensure good conductive magnetic properties side Combustion-supporting burning, promote gas release complete, carried out respectively with pure iron, tungsten particle, tin grain and their mixed flux in experimentation Check experiment, it the results are shown in Table 2.
The melting effect of the variety classes fluxing agent of table 2 compares
When proving to combine using pure iron+tungsten particle+tin grain by testing, final slag modifier best results are melted, release profiles are smooth, Without conditions of streaking, so carrying out subsequent experimental using tungsten particle+tin grain+pure iron compound additive in the present invention.
With reference to specific embodiment, the present invention is further detailed explanation.
Embodiment 1
The method of carbon, comprises the following steps in the present embodiment method of high frequency IR-absorption final slag modifier:
1)Weigh 0.2g pure iron fluxing agents and be laid in crucible bottom, then weigh 0.05g standard samples(Lime stone YSBC28701- 93)It is placed on it, 1.0g tungsten powders are weighed afterwards and are covered on sample, are finally weighed 0.2g tin grains and are placed on the superiors;
2)By step 1)In install fluxing agent and the crucible of sample is placed on the tripod of high frequency-infrared carbon sulphur instrument, what is set It is measured under analysis condition:
Analysis condition sets and is shown in Table 3:
The final slag modifier condition determination 1 of table 3
3)Lime stone YSBC28701-93 and two final slag modifier sample repeat steps 1 are taken respectively)、2)Carry out parallel survey three times It is fixed, record measurement result and compared with standard value, the results are shown in Table 4:
The analysis result of 4 embodiment of table 1
Sample does not melt fully as seen from the above table, and detection signal is unstable, and data deviation is larger.
Embodiment 2
The method of carbon, comprises the following steps in the present embodiment method of high frequency IR-absorption final slag modifier:
1)Weigh 0.3g pure iron fluxing agents and be laid in crucible bottom, then weigh 0.05g standard samples(Lime stone YSBC28701- 93)It is placed on it, 1.3g tungsten powders are weighed afterwards and are covered on sample, are finally weighed 0.2g tin grains and are placed on the superiors;
2)By step 1)In install fluxing agent and the crucible of sample is placed on the tripod of high frequency-infrared carbon sulphur instrument, what is set It is measured under analysis condition:
Analysis condition sets and is shown in Table 5:
The final slag modifier condition determination 2 of table 5
3)Lime stone YSBC28701-93 and two final slag modifier sample repeat steps 1 are taken respectively)、2)Carry out parallel survey three times It is fixed, record measurement result and compared with standard value, the results are shown in Table 6:
The analysis result of 6 embodiment of table 2
Sample melting effect is unstable as seen from the above table, and analysis result precision, the degree of accuracy are undesirable.
Embodiment 3
The method of carbon, comprises the following steps in the present embodiment method of high frequency IR-absorption final slag modifier:
1)Weigh 0.3g pure iron fluxing agents and be laid in crucible bottom, then weigh 0.05g standard samples(Lime stone YSBC28701- 93)It is placed on it, 1.5g tungsten powders are weighed afterwards and are covered on sample, are finally weighed 0.3g tin grains and are placed on the superiors;
2)By step 1)In install fluxing agent and the crucible of sample is placed on the tripod of high frequency-infrared carbon sulphur instrument, what is set It is measured under analysis condition:
Analysis condition sets and is shown in Table 7:
The final slag modifier condition determination 3 of table 7
3)Lime stone YSBC28701-93 and two final slag modifier samples are taken respectively as test substance, repeat step 1)、2) Parallel determination three times is carried out, records measurement result and compared with standard value, as a result as shown in table 8:
The analysis result of 8 embodiment of table 3
Sample melting is abundant as seen from the above table, and analysis result is stable.
Standard sample lime stone is utilized using the instrument parameter and fluxing agent dosage set in example 3(YSBC28701-93) Calibration curve is established, utilizes lime stone( BWH0120-5W)Curve is monitored, analyzes final slag modifier sample, curve release is smooth, Peak shape is smoothly stable without hangover, analysis result.
Above example is only to illustrative and not limiting technical scheme, although with reference to above-described embodiment to this hair It is bright to be described in detail, it will be understood by those within the art that:Still the present invention can be modified or be waited With replacing, any modification or partial replacement without departing from the spirit and scope of the present invention, it all should cover the power in the present invention Among sharp claimed range.

Claims (8)

1. a kind of method of carbon in method of high frequency IR-absorption final slag modifier, it is characterised in that methods described utilizes High frequency-infrared carbon sulphur instrument, establishes calibration curve using lime stone standard sample, carbon in final slag modifier is analyzed;Institute State and fluxing agent is added during analyzing, the fluxing agent is any one or a few mixture in pure iron, tungsten particle, tin grain.
2. the method for carbon in a kind of method of high frequency IR-absorption final slag modifier according to claim 1, it is special Sign is that the final slag modifier sample weighting amount is 0.05 ± 0.0001g.
3. the method for carbon in a kind of method of high frequency IR-absorption final slag modifier according to claim 1, it is special Sign is, pure iron addition is 6 times of sample final slag modifier quality in the fluxing agent.
4. the method for carbon in a kind of method of high frequency IR-absorption final slag modifier according to claim 1, it is special Sign is, tungsten particle addition is 30 times of sample final slag modifier quality in the fluxing agent.
5. the method for carbon in a kind of method of high frequency IR-absorption final slag modifier according to claim 1, it is special Sign is, tin grain addition is 6 times of sample final slag modifier quality in the fluxing agent.
6. carbon in a kind of method of high frequency IR-absorption final slag modifier according to claim 1-5 any one Method, it is characterised in that the fluxing agent order of addition is pure iron, tungsten particle, tin grain;The sample final slag modifier pure iron it After add.
7. carbon in a kind of method of high frequency IR-absorption final slag modifier according to claim 1-5 any one Method, it is characterised in that methods described establishes calibration curve using the method for two-point calibration.
8. carbon in a kind of method of high frequency IR-absorption final slag modifier according to claim 1-5 any one Method, it is characterised in that be first measured before making sample every time to monitoring sample, monitoring sample uses lime stone standard sample After conversion parallel determination is carried out on the basis of carbon content at least twice, it is desirable to difference≤0.1% of measurement result, to determine working curve Normal assay work can be carried out.
CN201710624797.6A 2017-07-27 2017-07-27 A kind of method of carbon in method of high frequency IR-absorption final slag modifier Withdrawn CN107421908A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108152101A (en) * 2017-12-20 2018-06-12 新疆昆玉钢铁有限公司 One thermal conductivity method of inert gas fusion measures nitrogen content sample-smelting method in ferrovanadium nitride
CN110296953A (en) * 2019-06-20 2019-10-01 江阴兴澄特种钢铁有限公司 A kind of method that infrared absorption method surveys carbon content in high carbon ferro-chrome
CN111366552A (en) * 2020-03-06 2020-07-03 中国地质科学院郑州矿产综合利用研究所 Method for measuring fixed carbon content in flake graphite ore flotation process sample
CN113267463A (en) * 2021-04-21 2021-08-17 宣化钢铁集团有限责任公司 Method for measuring content of sulfur element in cold-pressed ball

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
贺红侠: "终渣改质剂碳元素分析方法的研究", 《河北冶金》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108152101A (en) * 2017-12-20 2018-06-12 新疆昆玉钢铁有限公司 One thermal conductivity method of inert gas fusion measures nitrogen content sample-smelting method in ferrovanadium nitride
CN110296953A (en) * 2019-06-20 2019-10-01 江阴兴澄特种钢铁有限公司 A kind of method that infrared absorption method surveys carbon content in high carbon ferro-chrome
CN111366552A (en) * 2020-03-06 2020-07-03 中国地质科学院郑州矿产综合利用研究所 Method for measuring fixed carbon content in flake graphite ore flotation process sample
CN113267463A (en) * 2021-04-21 2021-08-17 宣化钢铁集团有限责任公司 Method for measuring content of sulfur element in cold-pressed ball

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Application publication date: 20171201