CN102830082A - Preparation method of stokehold steel-making gas specimen as well as method for analyzing gas content - Google Patents
Preparation method of stokehold steel-making gas specimen as well as method for analyzing gas content Download PDFInfo
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- CN102830082A CN102830082A CN2012102744977A CN201210274497A CN102830082A CN 102830082 A CN102830082 A CN 102830082A CN 2012102744977 A CN2012102744977 A CN 2012102744977A CN 201210274497 A CN201210274497 A CN 201210274497A CN 102830082 A CN102830082 A CN 102830082A
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Abstract
The invention discloses a preparation method of a stokehold steel-making gas specimen as well as a method for analyzing gas content. The preparation method comprises the following process steps: (1) grinding a specimen: manufacturing the gas analysis specimen into a cylinder shape of Phi 6-8MM, then grinding by a sand belt until the outer layer oxidation iron skin is completely grinded completely, and the temperature of the gas analysis specimen is controlled to be lower than 50 DEG C during the grinding process; (2) cutting the sample: cutting the grinded gas analysis specimen, controlling the cutting length to be within 3-5mm; and controlling the cutting quality to be within 0.6-1.3g; and (3) processing the specimen: removing the surface residual oxide of the cut gas analysis sample by a cleaning agent, and drying, thereby obtaining the gas specimen. The method solves the difficulties of long analysis time, low analysis accuracy and high analysis inspection process investment, can be implemented by utilizing the existing inspection equipment, and has the characteristics of low analysis cot, and high accuracy and reproducibility, and is simple in operation, and easy to master.
Description
Technical field
The invention belongs to a kind of chemical analysis field, the especially a kind of preparation method of stokehold steel-making gas sample and the method for lab for analysis of gas content.
Background technology
Along with improving constantly of steel-smelting technology level, stokehold steel-making progressively to maximization, automation direction development, is had higher requirement to the data analysis in the steelmaking process.For example progressively applying of Handan Iron and Steel Co newly developed area " one-touch " robotization steel-smelting technology proposed high requirement to the stokehold check data, particularly in smelting the exploitation high value added product, the gas content in the steel controlled the key point that becomes steel-making quality height.Because steel-making rhythm in stokehold is fast, it is not only soon but also accurate that the analysis of gas content is required.Consider that present new product development develops to low-cost direction, therefore, how quick and precisely to check gas content to become the difficult problem of stokehold gas analysis again at low cost.At present; Adopt thickness appearance before the advanced both at home and abroad converter, carry tube appearance and carry out the gas content analysis; But these two kinds of method sampling costs are expensive; Inspection cost is also high, especially need utilize specialized apparatus to prepare gas sample at test stage, not only cost an arm and a leg and also the specimen preparation cost also higher.And the way of steel-making enterprise is used lathe car system exactly usually; This method requires that sample flatness reaches 97% or more, sample needs that crop truncates, the clamping sample needs firmly, the lathe rotating speed is less than specimen temperature≤50 in 700r/min, the preparation process ℃ etc.; The requirement that these are almost harsh; Cause the sample difficulty of processing to increase, the post personnel can't fine grasp and control and analysis time longer.
Summary of the invention
The technical matters that the present invention will solve provides a kind of preparation method who processes the stokehold steel-making gas sample simple, that analysis speed is fast; The present invention also provides the method for utilizing this gas sample lab for analysis of gas content.
For solving the problems of the technologies described above; The technical scheme that the present invention taked is: (1) sample grinds: the gas analysis sample is processed the cylindrical of Ф 6-8mm; Grind with the abrasive band then; Clean until the complete grinding of outer oxide iron sheet, the temperature that grinds pilot-gas analytic sample in the process is less than 50 ℃;
(2) sample cuts: the gas analysis sample after will grinding cuts, and cuts length and is controlled between the 3-5mm, cuts quality control between 0.6-1.3g;
(3) sample preparation: the gas analysis sample that will cut is drying to obtain gas sample after removing the oxide of remained on surface with clean-out system.
The material in abrasive band is corundum, zirconia or silit in the step according to the invention (1), and the granularity in abrasive band is the 36-70 order.The material in said abrasive band is preferably corundum, and the granularity in abrasive band is preferably 46 orders.
Step according to the invention (1) grinds in the process, and the abrasive band rotating speed is controlled at 200-400r/min.Said abrasive band rotating speed preferably is controlled at 250r/min.
Step according to the invention (1) grinds in the process, the air cooling while grinding.
In the step according to the invention (3), the gas analysis sample is put into the beaker that fills clean-out system and is soaked to remove the oxide of remained on surface; Described clean-out system is the potpourri of alcohol and acetone.Said clean-out system is preferably alcohol: the potpourri of acetone=8:2.
In the step according to the invention (3), the gas analysis sample after the cleaning is placed on the filter paper dry 5-10 second before air-cooler.
The method of steel-making lab for analysis of gas content in stokehold of the present invention adopts above-mentioned gas sample, and its procedure is: utilize gas analyzer analysis correction standard specimen, obtain the linear regression analysis curve; Select for use this analytic curve to carry out the mensuration of gas sample then,, calculate the content of gas in the sample according to the corresponding relation of intensity and concentration in thermal conduction principle and the infrared absorption principle.
Adopt the beneficial effect that technique scheme produced to be: to the invention solves the difficult problem that stokehold steel-making gas content analysis time is long, analysis precision is low, the analytical control technology investment is high; Gas content that not only can rapid and accurate determination stokehold molten steel and inspection process investment easy low, simple to operate; Can support for the stokehold STEELMAKING PRODUCTION provides data promptly and accurately, thereby strong analysis backing is provided for smelting high value added products such as exploitation Automobile Plate, pipe line steel.The present invention utilizes existing inspection machine to implement, have simple to operate, be easy to grasp, analysis cost is low, accuracy and the higher characteristics of repeatability.
Embodiment
Below in conjunction with specific embodiment the present invention is done further detailed explanation.
The preparation method of this stokehold steel-making gas sample and the method for lab for analysis of gas content utilize oxygen nitrogen hydrogen analyser to measure.Emphasis of this method and difficult point are taking of analytic sample and prepare link that it is the key point of impact analysis precision and accuracy.At first; Utilize the vacuum gas ST that the gas analysis sample is got in the stokehold and process the cylindrical sample of diameter between 6-8mm; Deliver to the laboratory through air sample transporting system behind the chilling; The laboratory judges from outward appearance whether gaseous sample exists defective such as pore, crackle, sand holes etc. after receiving the gas analysis sample, and the processing that (the low removal that influence oxide layer of flatness) carried out necessity to its flatness is to reach the requirement of sample preparation technology to flatness; Secondly, grind after utilizing anchor clamps clamping gas analysis sample, pay special attention to grind Material Selection, grinding material can be corundum (Al
2O
3), zirconia (ZrO
2), silit (SiC) etc., be preferably corundum, the granularity of material is the 36-70 order; Be preferably 46 orders, the abrasive band rotating speed is controlled at 200-400r/min, is preferably 250r/min; The rotational speed in abrasive band is most important to the preparation of gas analysis sample, and rotating speed is too fast to be prone to cause specimen surface heating (escape of hydrogen in the gas sample ℃ will be caused in gas analysis sample surfaces>=50), grinds time lengthening excessively slowly; In the process of grinding, carry out air cooling while grind, with pilot-gas analytic sample surface temperature effectively; The dynamics of exerting oneself is difficult for excessive, otherwise heating easily causes the loss of hydrogen in the gaseous sample; The upset while grinding is till the complete grinding of outer oxide iron sheet is clean (the iron scale grinding totally will not influence oxygen content in the gas analysis sample); Then, utilize the gas shearing equipment that the gas analysis sample that grinds is sheared, before shearing, shearing knife edge is carried out wiping with alcohol swab; The oxidizing substance that it is surperficial is removed; Adjustment cuts length, cuts length and generally is controlled between the 3-5mm, preferably selects 3mm; Quality control is preferably selected 1.0g between 0.6-1.3g; Long overweight or too short kicking the beam, the one, the gas sample delivery device of gas analyzer is worked the mischief, the 2nd, bring deviation to analysis; Cut the defectives such as whether pore, sand holes, crackle are arranged that detect by an unaided eye again after the end; Again then, be exactly processing to the gas analysis sample, adopt clean-out system to clean the main residual oxidizing substance of gas analysis sample surfaces of removing; Require clean-out system to volatilize easily, the analysis to gas content does not have any impact, and surrounding environment is not caused damage yet; The gas analysis sample that cuts is put in the beaker of the clean-out system that fills voluntarily configuration (potpourri of alcohol and acetone is mainly removed the oxide of remained on surface), 5-10 is after second in immersion; Take out with clean tweezers and to be placed on the filter paper that dry 5-10 can analyze second before air-cooler,, need place it in the exsiccator and preserve if can not analyze at once; The clean-out system that this method adopts is the potpourri of alcohol: acetone=9:1-7:3 by volume; Be preferably alcohol: the potpourri of acetone=8:2, get advantage between the two, the acetone price is more expensive; Belong to poisonous and harmful substance again; To inhibition, the anesthetic action of central nervous system, high concentration contacts the infringement that possibly occur liver, kidney and pancreas to one or two people, and low concentration can reduce cleaning performance.50,100,150,200ppm etc. at last, the correction standard specimen that utilizes gas analyzer to analyze different content (for example:, depend on sample and constituent content) carries out series of analysis, and each content analysis 3 to 5 times obtains the linear regression analysis curve; Select for use this analytic curve to carry out the mensuration of gas sample then,, calculate the content of gas in the gas sample according to the corresponding relation of intensity and concentration in thermal conduction principle and the infrared absorption principle.
Embodiment 1: the preparation method of this stokehold steel-making gas sample and the method for lab for analysis of gas content adopt following step.
(1) sample grinds: the gas analysis sample is processed the cylindrical of Ф 7mm, and using granularity then is that 46 purpose emergy bands grind, and the abrasive band rotating speed is controlled at 250r/min, and is clean until the complete grinding of outer oxide iron sheet; Grind in the process, the air cooling while grinding, the temperature of pilot-gas analytic sample is less than 50 ℃; Grind in the process, abrasive band granularity and abrasive band rotating speed to the influence of the time of grinding shown in table 1, table 2;
(2) sample cuts: the gas analysis sample after will grinding cuts, and cuts length and is controlled at 3mm, cuts quality control at 1.0g;
(3) sample preparation: the gas analysis sample that will cut is put into the beaker of the clean-out system that fills voluntarily configuration, soaks 10 seconds, and clean-out system is the potpourri of alcohol: acetone=8:2 by volume; Take out with clean tweezers and to be placed on the filter paper before air-cooler dry 10 seconds, promptly get gas sample; The clean-out system allocation ratio is as shown in table 3 to the impact effect of analysis result.
(4) mensuration of gas content in the sample: utilize gas analyzer (for example: 50,100,150,200ppm etc. to analyze different content; Depend on sample and constituent content) the correction standard specimen carry out series of analysis; Each content analysis 3 to 5 times obtains the linear regression analysis curve; Select for use this analytic curve to carry out the mensuration of testing sample then,, calculate the content of gas in the sample according to the corresponding relation of intensity and concentration in thermal conduction principle and the infrared absorption principle.Utilize gas analyzer to create analytical approach: select analysis time, comparison level, analysis power, degassing power and the Measuring Time etc. of oxygen, nitrogen, three kinds of elements of hydrogen to analyze parameter, as shown in table 4.
Embodiment 2: the preparation method of this stokehold steel-making gas sample and the method for lab for analysis of gas content adopt following step.
(1) sample grinds: the gas analysis sample is processed the cylindrical of Ф 8mm, and using granularity then is that 36 purpose emergy bands grind, and the abrasive band rotating speed is controlled at 400r/min, and is clean until the complete grinding of outer oxide iron sheet; Grind in the process, the air cooling while grinding, the temperature of pilot-gas analytic sample is less than 50 ℃;
(2) sample cuts: the gas analysis sample after will grinding cuts, and cuts length and is controlled at 4mm, cuts quality control at 1.3g;
(3) sample preparation: the gas analysis sample that will cut is put into the beaker that fills the clean-out system that disposes voluntarily and is cleaned, and clean-out system is the potpourri of alcohol: acetone=9:1; Take out the back drying with clean tweezers, promptly get gas sample;
(4) utilize gas analyzer analysis correction standard specimen, obtain the linear regression analysis curve; Select for use this analytic curve to carry out the mensuration of gas sample then,, calculate the content of gas in the sample according to the corresponding relation of intensity and concentration in thermal conduction principle and the infrared absorption principle.
Embodiment 3: the preparation method of this stokehold steel-making gas sample and the method for lab for analysis of gas content adopt following step.
(1) sample grinds: the gas analysis sample is processed the cylindrical of Ф 6mm, and using granularity then is that 70 purpose emergy bands grind, and the abrasive band rotating speed is controlled at 200r/min, and is clean until the complete grinding of outer oxide iron sheet; The temperature that grinds pilot-gas analytic sample in the process is less than 50 ℃;
(2) sample cuts: the gas analysis sample after will grinding cuts, and cuts length and is controlled at 5mm, cuts quality control at 0.6g;
(3) sample preparation: the gas analysis sample that will cut is put into the beaker that fills the clean-out system that disposes voluntarily and is cleaned, and clean-out system is the potpourri of alcohol: acetone=7:3; Take out the back drying with clean tweezers, promptly get gas sample;
(4) utilize gas analyzer analysis correction standard specimen, obtain the linear regression analysis curve; Select for use this analytic curve to carry out the mensuration of gas sample then,, calculate the content of gas in the sample according to the corresponding relation of intensity and concentration in thermal conduction principle and the infrared absorption principle.
In order to verify the feasibility of this method, a series of precision tests, accuracy test have been done under these conditions.The precision test is analyzed 10 times to same gaseous sample continuously, calculating mean value and relative standard deviation, and wherein number of times 1-4 adopts the condition of embodiment 1; Number of times 5-7 adopts embodiment 2; Number of times 8-10 adopts embodiment 3; Accuracy test is chosen some gas analysis samples, measures with method among the embodiment 1, and gained result and car system method are compared, and test figure is seen table 5, table 6.
Show that through above test figure this method utilizes precision, the accuracy of the method that the abrasive band grinds can satisfy stokehold gas content analytical technology requirement.
Claims (10)
1. the preparation method of stokehold steel-making gas sample is characterized in that it adopts following processing step:
(1) sample grinds: the gas analysis sample is processed the cylindrical of Ф 6-8mm, grind with the abrasive band then, clean until the complete grinding of outer oxide iron sheet, the temperature that grinds pilot-gas analytic sample in the process is less than 50 ℃;
(2) sample cuts: the gas analysis sample after will grinding cuts, and cuts length and is controlled between the 3-5mm, cuts quality control between 0.6-1.3g;
(3) sample preparation: the gas analysis sample that will cut is drying to obtain gas sample after removing the oxide of remained on surface with clean-out system.
2. the preparation method of steel-making gas sample in stokehold according to claim 1, it is characterized in that: the material in abrasive band is corundum, zirconia or silit in the said step (1), and the granularity in abrasive band is the 36-70 order.
3. the preparation method of steel-making gas sample in stokehold according to claim 2, it is characterized in that: the material in said abrasive band is a corundum, the granularity in abrasive band is 46 orders.
4. the preparation method of steel-making gas sample in stokehold according to claim 1, it is characterized in that: said step (1) grinds in the process, and the abrasive band rotating speed is controlled at 200-400r/min.
5. the preparation method of steel-making gas sample in stokehold according to claim 4, it is characterized in that: said abrasive band rotating speed is controlled at 250r/min.
6. according to the preparation method of described any one stokehold steel-making gas sample of claim 1-5, it is characterized in that: said step (1) grinds in the process, the air cooling while grinding.
7. the preparation method of steel-making gas sample in stokehold according to claim 1 is characterized in that: in the said step (3), the gas analysis sample is put into the beaker that fills clean-out system and is soaked to remove the oxide of remained on surface; Described clean-out system is the potpourri of alcohol: acetone=9:1-7:3 by volume.
8. the preparation method of steel-making gas sample in stokehold according to claim 7, it is characterized in that: said clean-out system is the potpourri of alcohol: acetone=8:2.
9. the preparation method of stokehold according to claim 1 steel-making gas sample is characterized in that: in the said step (3), the gas analysis sample after the cleaning is placed on the filter paper dry 5-10 second before air-cooler.
10. the method for stokehold steel-making lab for analysis of gas content, it adopts described any one gas sample of claim 1-9, it is characterized in that: utilize gas analyzer analysis correction standard specimen, obtain the linear regression analysis curve; Select for use this analytic curve to carry out the mensuration of gas sample then,, calculate the content of gas in the sample according to the corresponding relation of intensity and concentration in thermal conduction principle and the infrared absorption principle.
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Cited By (3)
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| CN105067399A (en) * | 2015-07-21 | 2015-11-18 | 北京首钢股份有限公司 | Method for making internal control standard sample |
| CN108693133A (en) * | 2018-08-10 | 2018-10-23 | 北京科技大学 | A kind of method of oxygen content in measurement potassium steel |
| CN111474024A (en) * | 2020-04-09 | 2020-07-31 | 北京首钢股份有限公司 | Rapid sample preparation method for low-oxygen and low-nitrogen analysis sample in front of steel-making furnace and product thereof |
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2012
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| JPH09152391A (en) * | 1995-11-29 | 1997-06-10 | Nippon Steel Corp | Method for working specimen for analyzing component in steel |
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Cited By (3)
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| CN105067399A (en) * | 2015-07-21 | 2015-11-18 | 北京首钢股份有限公司 | Method for making internal control standard sample |
| CN108693133A (en) * | 2018-08-10 | 2018-10-23 | 北京科技大学 | A kind of method of oxygen content in measurement potassium steel |
| CN111474024A (en) * | 2020-04-09 | 2020-07-31 | 北京首钢股份有限公司 | Rapid sample preparation method for low-oxygen and low-nitrogen analysis sample in front of steel-making furnace and product thereof |
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Application publication date: 20121219 |