CN112326584A - Method for detecting sulfur and carbon in steel - Google Patents

Method for detecting sulfur and carbon in steel Download PDF

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CN112326584A
CN112326584A CN202011117297.1A CN202011117297A CN112326584A CN 112326584 A CN112326584 A CN 112326584A CN 202011117297 A CN202011117297 A CN 202011117297A CN 112326584 A CN112326584 A CN 112326584A
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carbon
sulfur
steel
crucible
detecting
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武斌
赵广东
王亚朋
李明明
唐语
王立刚
王丽铭
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Bengang Steel Plates 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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Abstract

The invention relates to a method for detecting sulfur and carbon in steel, which comprises the following steps: detecting sample processing, namely drilling a steel sample with the gram weight of more than 0.1; treating the crucible, namely firing, cooling and drying the crucible in a muffle furnace; and (3) sulfur-carbon analysis: and (3) putting the steel sample into a crucible, adding a fluxing agent, and putting the steel sample into an infrared carbon-sulfur analyzer for sulfur-carbon analysis. The detection method is convenient to operate, can meet the analysis requirement of analyzing ultralow sulfur and carbon in steel, ensures the stability of blank values and improves the analysis precision.

Description

Method for detecting sulfur and carbon in steel
Technical Field
The invention relates to the technical field of analysis of carbon and sulfur in steel, in particular to a method for detecting sulfur and carbon in steel.
Background
With the increasing severity of the surplus of the domestic steel industry, the steel price is gradually lowered, and various large steel plants place products with optimized variety structures, high technology and high added value to the top, in recent years, the steel continuously develops high-added-value steel grades such as pipeline steel, high-strength steel, silicon steel, stainless steel and automobile plates, the technological process control requirements of the steel grades are strict, the analysis requirements on ultra-low carbon and sulfur in the steel are high, and the carbon and sulfur values of some steel grades are below 20ppm (1ppm is 0.0001%), so that the higher requirements for the analysis on the ultra-low carbon and sulfur are provided for people.
At present, in the prior art, a wet analyzer is generally adopted to analyze the carbon and sulfur content in steel or a high-frequency induction infrared absorption method is generally adopted to analyze the carbon and sulfur content in steel, wherein the analysis precision of the wet analyzer is far from meeting the requirement of analyzing ultra-low carbon and sulfur due to the limit of the principle of the wet analyzer, while the analysis precision can be achieved by adopting the high-frequency induction infrared absorption method, but a complete analysis method and control conditions are not available, and the operation is inconvenient.
Therefore, it is necessary to develop a method for detecting sulfur and carbon in steel, which is convenient to operate, can meet the analysis requirement of analyzing ultralow sulfur and carbon in steel, ensures the stability of blank values, and improves the analysis precision.
Disclosure of Invention
The present invention is directed to solving one of the technical problems of the prior art or the related art.
Therefore, the invention provides a method for detecting sulfur and carbon in steel.
In view of the above, the present invention provides a method for detecting sulfur and carbon in steel, including the following steps:
detecting sample processing, namely drilling a steel sample with the gram weight of more than 0.1;
treating a crucible, namely performing firing-cooling-drying treatment on the crucible in a muffle furnace;
and (3) sulfur-carbon analysis: and putting the steel sample into the crucible, adding a fluxing agent, and putting the steel sample into an infrared carbon-sulfur analyzer for sulfur-carbon analysis.
Further, the burning temperature in the muffle furnace is 1150-1250 ℃, and the burning time is 1.5-2.5 hours.
Further, the gram weight of the added fluxing agent is 1.5g to 2 g.
Further, before the fluxing agent is added, the fluxing agent is heated and then taken out for cooling for standby.
Further, the fluxing agent is placed into an oven to be heated to 280-320 ℃, and the temperature is kept for 50-70 min.
Further, taking the fluxing agent out of the oven, and placing the fluxing agent into a dryer for cooling.
Further, the flux is a tungsten flux.
Further, the parameters of the infrared carbon and sulfur analyzer during sulfur and carbon analysis are set as follows: the carrying parameter of carbon dioxide and sulfur dioxide gas emitted by the steel sample during high-temperature melting is 2800cc/min to 3200cc/min, and the gas parameter for providing power when the infrared sulfur-carbon instrument lifts and lowers the crucible is 800cc/min to 1200 cc/min.
The technical scheme provided by the embodiment of the invention can have the following beneficial effects:
the detection method is convenient to operate, can meet the analysis requirement of analyzing ultralow sulfur and carbon in steel, ensures the stability of blank values, and improves the analysis precision.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a schematic flow chart illustrating a method for detecting sulfur and carbon in steel according to an embodiment of the present invention.
Detailed Description
Reference will now be made in detail to the exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Rather, they are merely examples of apparatus and methods consistent with certain aspects of the invention, as detailed in the appended claims.
Examples
FIG. 1 is a schematic flow chart illustrating a method for detecting sulfur and carbon in steel according to an embodiment of the present invention.
As shown in fig. 1, the present embodiment provides a method for detecting sulfur and carbon in a steel material, including the following steps:
step 1, detecting sample processing, namely drilling a steel sample with the gram weight of more than 0.1;
step 2, treating the crucible, namely burning, cooling and drying the crucible in a muffle furnace;
and 3, sulfur and carbon analysis, namely putting the steel sample into a crucible, adding a fluxing agent, and putting into an infrared carbon and sulfur analyzer for sulfur and carbon analysis.
The detection method is convenient to operate, can meet the analysis requirement of analyzing ultralow sulfur and carbon in steel, and ensures the stability of a blank value and improves the analysis precision by processing the crucible, namely burning, cooling and drying the crucible in a muffle furnace.
Since the detection result of the fine steel chips having a grammage of 0.1 or less is very unstable and is usually high, a steel sample having a grammage of 0.1 or more is selected for sample processing, and when the sample is a thin automobile sheet, a flat drill is used for sampling, and the thin automobile sheet is not drilled through as much as possible.
Further, the burning temperature in the muffle furnace is 1150-1250 ℃, and the burning time is 1.5-2.5 hours.
In this example, the blank value analysis was performed using a crucible sulfur-carbon blank analysis.
The muffle furnace temperature was adjusted to 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃ respectively for testing, 10 crucibles were analyzed at each temperature for crucible carbon sulfur blank analysis, and the average of 10 crucible tests at each temperature was taken, and the results are shown in table 1.
TABLE 1 error comparison table of sulfur and carbon analysis at different temperatures
Figure BDA0002730751880000031
As can be seen from Table 1, the standard deviation of the blank value of carbon and sulfur in the crucible is the smallest when the burning is performed at 1200 ℃, so that the crucible is burned at 1200 ℃ for 2 hours in the embodiment.
It should be noted that too short a burning time cannot completely remove the carbon and sulfur impurities contained in the crucible, and too long a burning time increases the time of sulfur and carbon analysis and reduces the efficiency of sulfur and carbon analysis, so 2 hours are generally used
Further, the gram weight of the added fluxing agent is 1.5g to 2 g.
In this example, the sulfur-carbon content of the steel sample is less than 15ppm, and when the flux is added, a deviation of 3ppm is caused by adding 1.5g and 2g of flux (the carbon-sulfur content in the flux is respectively C. ltoreq.8 ppm, and S. ltoreq.8 ppm), respectively, so that when the flux with different gram weights is added during sulfur-carbon analysis, a deviation is caused in the analysis result, the detection result is affected, and when the gram weights of the flux added each time are the same, the error can be reduced.
Furthermore, before adding the fluxing agent, the fluxing agent is heated and then taken out for standby.
Wherein, the fluxing agent is put into an oven to be heated to 280 ℃ to 320 ℃, and the temperature is kept for 50min to 70 min.
Further, the flux is taken out of the oven and placed in a dryer for cooling.
The dried fluxing agent can reduce the moisture content, reduce the possibility of adsorbing carbon dioxide in the air and further reduce the carbon dioxide adsorbed in the analysis process, so that the blank value is reduced, and the analysis accuracy is reduced due to the fact that the blank value is too high, so that the accuracy of the obtained sulfur and carbon analysis is reduced, and therefore the blank value is controlled strictly and importantly.
Further, the flux is a tungsten flux.
The tungsten oxide is oxidized at a high temperature to generate tungsten trioxide, the tungsten trioxide belongs to an acidic oxide, the generation of the tungsten trioxide is beneficial to the release of carbon dioxide and sulfur dioxide, the melting point of the tungsten is 1473 ℃, the heat of fusion is low, the boiling point is greater than 1750 ℃, the tungsten trioxide has an important characteristic that the tungsten trioxide is obviously sublimated when the temperature is above 900 ℃, part of the tungsten trioxide is volatilized, the diffusion speed of carbon and sulfur is increased due to the overflow of the tungsten trioxide, the carbon and sulfur in a steel sample is fully oxidized, the volatilized tungsten trioxide is converted into a solid phase at 700-800 ℃, the ferric oxide still existing in a pipeline is covered, the catalytic conversion of sulfur dioxide into sulfur trioxide is prevented, the adsorption of the pipeline to sulfur is prevented, the reliability of a sulfur and carbon analysis result is ensured, in addition, the blank value of the tungsten is lower, and the tungsten oxide can be used for the analysis and detection of low carbon and low.
The detection method provided by the invention is mainly characterized in that the blank value of the crucible and the impurities brought by the fluxing agent are controlled, the precision of the detection result is improved by reducing the blank value of the crucible, and the accuracy of the detection result is improved by reducing the impurities brought by the fluxing agent, so that the purpose of accurately analyzing the ultra-low carbon sulfur sample is achieved.
It should be noted that the infrared carbon-sulfur analyzer used in this example is an american CS-600 infrared carbon-sulfur analyzer, the samples used are samples from steel research institute GBW01146 and shanghai steel research institute YSBS20123-2002, each sample is repeatedly tested 11 times, and the results are shown in table 2.
TABLE 2 GBW01146 and YSBS20123-2002 test results
Figure BDA0002730751880000041
As can be seen from the detection results in Table 2, the method can accurately detect the ultra-low carbon sulfur value and meet the regulations of national standards.
Comparative example
TABLE 3 comparison table of GBW01146 detection results by the method and the conventional method
Figure BDA0002730751880000051
As can be seen from Table 3, the relative standard deviation can be greatly reduced and the accuracy is better by using the method.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
It is to be understood that the present invention is not limited to what has been described above, and that various modifications and changes may be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.

Claims (8)

1. The method for detecting the sulfur and carbon in the steel is characterized by comprising the following steps:
detecting sample processing, namely drilling a steel sample with the gram weight of more than 0.1;
treating a crucible, namely performing firing-cooling-drying treatment on the crucible in a muffle furnace;
and (3) sulfur and carbon analysis, namely putting the steel sample into the crucible, adding a fluxing agent, and putting the crucible into an infrared carbon and sulfur analyzer for sulfur and carbon analysis.
2. The method of claim 1, wherein the crucible treatment is performed at a firing temperature of 1150 ℃ to 1250 ℃ for 1.5 to 2.5 hours.
3. A method of detecting sulphur and carbon in a steel product as claimed in claim 1, wherein the grammage of the flux added is in the range of 1.5 to 2 g.
4. A method of detecting sulfur and carbon in a steel product as claimed in claim 1 wherein said flux is heated and then cooled for future use before said flux is added.
5. The method for detecting sulfur and carbon in steel according to claim 4, wherein the fluxing agent is placed in an oven and heated to 280-320 ℃, and the temperature is kept for 50-70 min.
6. The method of detecting sulfur and carbon in a steel product as set forth in claim 5, wherein the flux is taken out from the oven and cooled in a dryer.
7. The method of detecting sulfur and carbon in a steel product as claimed in any one of claims 4 to 6, characterized in that said flux is a tungsten flux.
8. The method of detecting sulfur and carbon in a steel product according to claim 1, wherein the parameters for the sulfur and carbon analysis in said infrared carbon-sulfur analyzer are set to: the carrying parameter of carbon dioxide and sulfur dioxide gas emitted by the steel sample during high-temperature melting is 2800cc/min to 3200cc/min, and the gas parameter for providing power when the infrared sulfur-carbon instrument lifts and lowers the crucible is 800cc/min to 1200 cc/min.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114414726A (en) * 2022-01-10 2022-04-29 中国原子能科学研究院 Detection device and detection method for carbon content in alkali metal
CN116359166A (en) * 2023-05-31 2023-06-30 北京一控系统技术有限公司 Method for detecting sulfur-carbon content in steel
CN113686806B (en) * 2021-09-24 2024-04-02 广东韶钢松山股份有限公司 Method for detecting carbon and sulfur content in spring

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0367168A (en) * 1989-08-04 1991-03-22 Nippon Steel Corp Analysis of trace carbon, sulfur, phosphorus in metallic sample and equipment therefor
JPH08327625A (en) * 1995-06-05 1996-12-13 Nippon Steel Corp Method and equipment for analyzing carbon, sulfur and phosphorus in metal sample
CN103196863A (en) * 2013-03-21 2013-07-10 内蒙古包钢钢联股份有限公司 Method for determining contents of carbon and sulfur in iron alloy by using infrared absorption method with calibration of different reference materials
CN104458631A (en) * 2013-09-22 2015-03-25 贵州航天精工制造有限公司 Method for determining carbon and sulfur in material through repeatedly using crucible
CN104458637A (en) * 2014-12-16 2015-03-25 内蒙古包钢钢联股份有限公司 Method for testing ultra-low carbon and sulphur content in plain carbon steel-low alloy steel
CN104483286A (en) * 2014-12-16 2015-04-01 内蒙古包钢钢联股份有限公司 Method for determining contents of carbon and sulfur in iron-containing dust mud
WO2015124254A1 (en) * 2014-02-18 2015-08-27 Elementar Analysensysteme Gmbh Analyzer and a method for analyzing carbon (c) and sulfur (s) in metals

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0367168A (en) * 1989-08-04 1991-03-22 Nippon Steel Corp Analysis of trace carbon, sulfur, phosphorus in metallic sample and equipment therefor
JPH08327625A (en) * 1995-06-05 1996-12-13 Nippon Steel Corp Method and equipment for analyzing carbon, sulfur and phosphorus in metal sample
CN103196863A (en) * 2013-03-21 2013-07-10 内蒙古包钢钢联股份有限公司 Method for determining contents of carbon and sulfur in iron alloy by using infrared absorption method with calibration of different reference materials
CN104458631A (en) * 2013-09-22 2015-03-25 贵州航天精工制造有限公司 Method for determining carbon and sulfur in material through repeatedly using crucible
WO2015124254A1 (en) * 2014-02-18 2015-08-27 Elementar Analysensysteme Gmbh Analyzer and a method for analyzing carbon (c) and sulfur (s) in metals
CN104458637A (en) * 2014-12-16 2015-03-25 内蒙古包钢钢联股份有限公司 Method for testing ultra-low carbon and sulphur content in plain carbon steel-low alloy steel
CN104483286A (en) * 2014-12-16 2015-04-01 内蒙古包钢钢联股份有限公司 Method for determining contents of carbon and sulfur in iron-containing dust mud

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
汪本林 等: ""红外线吸收光谱法测定金属材料中碳硫元素的原理及注意事项"", 《化学分析计量》 *
赵冬梅 等: ""国际比对钢中碳硫含量的测定"", 《化学分析计量》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113686806B (en) * 2021-09-24 2024-04-02 广东韶钢松山股份有限公司 Method for detecting carbon and sulfur content in spring
CN114414726A (en) * 2022-01-10 2022-04-29 中国原子能科学研究院 Detection device and detection method for carbon content in alkali metal
CN116359166A (en) * 2023-05-31 2023-06-30 北京一控系统技术有限公司 Method for detecting sulfur-carbon content in steel
CN116359166B (en) * 2023-05-31 2023-08-11 北京一控系统技术有限公司 Method for detecting sulfur-carbon content in steel

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Application publication date: 20210205