CN112326584A - Method for the detection of sulfur and carbon in steel - Google Patents
Method for the detection of sulfur and carbon in steel Download PDFInfo
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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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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 52
- 239000010959 steel Substances 0.000 title claims abstract description 52
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 41
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 41
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 40
- 239000011593 sulfur Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000001514 detection method Methods 0.000 title claims abstract description 17
- 238000004458 analytical method Methods 0.000 claims abstract description 37
- 230000004907 flux Effects 0.000 claims abstract description 19
- GJEAMHAFPYZYDE-UHFFFAOYSA-N [C].[S] Chemical compound [C].[S] GJEAMHAFPYZYDE-UHFFFAOYSA-N 0.000 claims abstract description 15
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000012545 processing Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 10
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000001569 carbon dioxide Substances 0.000 claims description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 239000010937 tungsten Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims 2
- 239000005864 Sulphur Substances 0.000 claims 1
- 238000005553 drilling Methods 0.000 abstract description 3
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 16
- 239000003795 chemical substances by application Substances 0.000 description 15
- 239000012535 impurity Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- 229910001930 tungsten oxide Inorganic materials 0.000 description 2
- 229910000976 Electrical steel Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating 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)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
本发明是关于一种钢材中硫碳的检测方法，该检测方法包括如下步骤：检测试样加工，钻取克重0.1以上的钢材试样；坩埚的处理，在马弗炉内对坩埚进行灼烧‑冷却‑干燥处理；硫碳分析：将钢材试样放入坩埚内，加入助熔剂后放入红外碳硫分析仪中进行硫碳分析。该检测方法，操作方便，能够达到分析钢材中超低硫碳的分析要求，保证空白值的稳定性，提高分析精度。
The invention relates to a method for detecting sulfur and carbon in steel, which comprises the following steps: processing a detection sample, drilling a steel sample with a gram weight of more than 0.1; processing a crucible, burning the crucible in a muffle furnace Burning-cooling-drying; sulfur-carbon analysis: put the steel sample into the crucible, add flux and put it into the infrared carbon-sulfur analyzer for sulfur-carbon analysis. The detection method is easy to operate, and can meet the analysis requirements of analyzing ultra-low sulfur carbon in steel, ensure the stability of blank values, and improve the analysis accuracy.
Description
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
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
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
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)
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011117297.1A CN112326584A (en) | 2020-10-19 | 2020-10-19 | Method for the detection of sulfur and carbon in steel |
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| CN202011117297.1A CN112326584A (en) | 2020-10-19 | 2020-10-19 | Method for the detection of sulfur and carbon in steel |
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Cited By (4)
| 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 of carbon content in alkali metals |
| 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 |
| CN119086479A (en) * | 2024-11-06 | 2024-12-06 | 季华实验室 | A method for determining sulfur content in sulfonated polyetheretherketone |
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Cited By (5)
| 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 |
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| CN119086479A (en) * | 2024-11-06 | 2024-12-06 | 季华实验室 | A method for determining sulfur content in sulfonated polyetheretherketone |
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