CN113390813A - Method for measuring sulfur content in silicon-nitrogen alloy - Google Patents

Method for measuring sulfur content in silicon-nitrogen alloy Download PDF

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Publication number
CN113390813A
CN113390813A CN202110631598.4A CN202110631598A CN113390813A CN 113390813 A CN113390813 A CN 113390813A CN 202110631598 A CN202110631598 A CN 202110631598A CN 113390813 A CN113390813 A CN 113390813A
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sulfur content
sulfur
standard substance
sample
fluxing agent
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曾海梅
苏宁
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Wugang Group Kunming Iron and Steel Co Ltd
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Wugang Group Kunming Iron and Steel 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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  • 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)
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  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Investigating And Analyzing Materials By Characteristic Methods (AREA)

Abstract

The invention discloses a method for measuring sulfur content in a silicon-nitrogen alloy, which comprises the steps of pretreatment, preparation of spare parts for measurement, measurement of a sulfur content blank value, calibration of a high-frequency infrared carbon-sulfur analyzer and measurement of a sample. The method for detecting the sulfur dioxide content of the sample by using the infrared absorption method after the combustion of the high-frequency induction furnace changes the dosage and the adding sequence of the fluxing agent, ensures that the sulfur dioxide of the sample is completely released, is convenient to operate, greatly shortens the detection period, improves the detection efficiency, does not need to use a chemical reagent, reduces the pollution of the chemical reagent to the environment, and also reduces the physical injury of the chemical reagent to testers. The method for determining the sulfur content in the silicon nitrogen alloy has good stability, reproducibility and accuracy, and can meet the daily detection requirement of the sulfur content in the silicon nitrogen alloy.

Description

Method for measuring sulfur content in silicon-nitrogen alloy
Technical Field
The invention belongs to the technical field of chemical analysis, and relates to a method for measuring the sulfur content in a silicon-nitrogen alloy.
Background
The silicon-nitrogen alloy is a multielement nitrogen-fixing alloy prepared by combining abundant silicon resources and trace alloy elements for nitriding. Steel companies use a large amount of silicon-nitrogen alloy in the converter steelmaking process to improve the strength of steel. However, the sulfur content in the silicon nitrogen alloy needs to be kept below a certain value, and therefore, it is extremely important to measure the sulfur content in the silicon nitrogen alloy. At present, no report is found on a method for measuring sulfur in a silicon nitrogen alloy.
Disclosure of Invention
The invention aims to provide a method for accurately measuring the sulfur content in a silicon-nitrogen alloy.
The purpose of the invention is realized by the following technical scheme: the invention discloses a method for measuring sulfur content in a silicon-nitrogen alloy, which comprises the steps of pretreatment, preparation of spare parts for measurement, measurement of a sulfur content blank value, calibration of a high-frequency infrared carbon-sulfur analyzer and measurement of a sample, and specifically comprises the following steps:
1) pretreatment:
uniformly spreading 3-5 g/g at the bottom of the crucibleTest specimenCovering the sample to be tested on the pure iron fluxing agent;
at a ratio of 4 to 6g/gTest specimenIn an amount to cover the sample to be tested with a tin flux;
covering a tungsten particle fluxing agent on the tin fluxing agent according to the amount of 8-12 g/g of the sample;
2) preparation of measurement preparations:
the first standard substance is: GBW (E)010299, sulfur content 0.0014%; the first standard substance is: GBW01246, sulfur content 0.036%; the third standard substance is: GBW (E)010313, sulfur content 0.011%;
3) measuring a blank value of the sulfur content: determining blank values of carbon contents of the pure iron fluxing agent, the tin fluxing agent and the tungsten fluxing agent in the step 1 by using a high-frequency infrared carbon and sulfur analyzer, inputting the blank values into the high-frequency infrared carbon and sulfur analyzer, and automatically deducting the blank values when the high-frequency infrared carbon and sulfur analyzer is calibrated;
4) calibrating a high-frequency infrared carbon-sulfur analyzer: the sulfur content of the first standard substance is measured and compared to its standard value for calibrating the instrument. Respectively measuring the second standard substance and the third standard substance, respectively comparing the measured values with standard values, if the content difference value is not in an allowable range, repeating the step 4 until the difference value is in the allowable range to obtain the measured values of the sulfur content of the second standard substance and the sulfur content of the third standard substance, wherein the measured values of the sulfur content of the second standard substance and the sulfur content of the third standard substance are in the allowable difference range;
5) sample measurement
And (4) carrying out sulfur content on the sample to be detected prepared in the step (1) by using a high-frequency infrared carbon-sulfur analyzer according to the working conditions selected in the step (4).
The invention has the beneficial effects that:
1) the invention changes the dosage and adding sequence of the fluxing agent and uses the infrared absorption method after the combustion of the high-frequency induction furnace to determine the sulfur dioxide content of the sample, so that the sulfur dioxide of the sample is completely released, the operation is convenient, the detection period is greatly shortened, the detection efficiency is improved, meanwhile, the chemical reagent is not needed, the pollution of the chemical reagent to the environment is reduced, and the harm of the chemical reagent to the body of a tester is also reduced.
2) The method for determining the sulfur content in the silicon nitrogen alloy has good stability, reproducibility and accuracy, and can meet the daily detection requirement of the sulfur content in the silicon nitrogen alloy.
Detailed Description
The invention is further described below with reference to specific embodiments.
The invention discloses a method for measuring sulfur content in a silicon-nitrogen alloy, which comprises the steps of pretreatment, preparation of spare parts for measurement, measurement of a sulfur content blank value, calibration of a high-frequency infrared carbon-sulfur analyzer and measurement of a sample, and specifically comprises the following steps:
1) pretreatment:
uniformly spreading 3-5 g/g at the bottom of the crucibleTest specimenCovering the sample to be tested on the pure iron fluxing agent;
at a ratio of 4 to 6g/gTest specimenIn an amount to cover the sample to be tested with a tin flux;
covering a tungsten particle fluxing agent on the tin fluxing agent according to the amount of 8-12 g/g of the sample;
2) preparation of measurement preparations:
the first standard substance is: GBW (E)010299, sulfur content 0.0014%; the first standard substance is: GBW01246, sulfur content 0.036%; the third standard substance is: GBW (E)010313, sulfur content 0.011%;
3) measuring a blank value of the sulfur content: determining blank values of carbon contents of the pure iron fluxing agent, the tin fluxing agent and the tungsten fluxing agent in the step 1 by using a high-frequency infrared carbon and sulfur analyzer, inputting the blank values into the high-frequency infrared carbon and sulfur analyzer, and automatically deducting the blank values when the high-frequency infrared carbon and sulfur analyzer is calibrated;
4) calibrating a high-frequency infrared carbon-sulfur analyzer: the sulfur content of the first standard substance is measured and compared to its standard value for calibrating the instrument. Respectively measuring the second standard substance and the third standard substance, respectively comparing the measured values with standard values, if the content difference value is not in an allowable range, repeating the step 4 until the difference value is in the allowable range to obtain the measured values of the sulfur content of the second standard substance and the sulfur content of the third standard substance, wherein the measured values of the sulfur content of the second standard substance and the sulfur content of the third standard substance are in the allowable difference range;
5) sample measurement
And (4) carrying out sulfur content on the sample to be detected prepared in the step (1) by using a high-frequency infrared carbon-sulfur analyzer according to the working conditions selected in the step (4).
The working conditions of the high-frequency infrared carbon and sulfur analyzer are as follows: a cut-off level 7; the temperature of the combustion furnace is 1300 ℃; the number of integration times is 1; minimum analysis time 32 s; the maximum analysis time was 50 s.
The tin particle fluxing agent is a commercially available tin fluxing agent with tin of more than 99.95 percent.
The pure iron fluxing agent is a commercial pure iron fluxing agent with iron content of more than 99.90%.
The tungsten particle fluxing agent is a commercially available pure tungsten fluxing agent with tungsten content of more than 99.95%.
Example 1
Placing the special ceramic crucible for carbon and sulfur analysis in a high-temperature furnace, firing at 1000 ℃ for 40min, taking out the crucible, placing the crucible in a clean heat-resistant disc, cooling for 2 min-3 min, and finally storing the crucible in a dryer;
taking out the ceramic crucible, adding 0.30g of tin particle fluxing agent, 0.50g of pure iron fluxing agent and 10g of tungsten particle fluxing agent into the ceramic crucible, measuring and analyzing by an infrared absorption method after combustion in a high-frequency induction furnace, repeatedly measuring for three times, taking an average value to obtain an average blank value, inputting the average blank value, and automatically calibrating the blank value by an instrument.
Selecting 3 ceramic crucibles in the step 1A as the first standard substance, and respectively adding 0.30g of tin particle fluxing agent;
the sulphur content of the first standard substance was determined according to the selected operating conditions (cut-off level 7; furnace temperature 1300 ℃; number of integrations 1; shortest analysis time 32 s; longest analysis time 50s), with a measured value of 0.0018, compared to its standard value of 0.0014 and the instrument was calibrated. The second and third standard substances were measured to be 0.038 and 0.014, respectively, and the content difference was within the allowable range as compared with the standard value.
Example 2
3g of pure iron fluxing agent is evenly laid at the bottom of the crucible, 1g of a sample to be tested is weighed to cover the pure iron fluxing agent, 5g of tin fluxing agent is covered on the sample to be tested, 10g of tungsten particle fluxing agent is covered on the tin fluxing agent, and finally the crucible is placed in a high-frequency infrared carbon-sulfur analyzer to measure the sulfur content according to the working conditions selected in the embodiment 1, so that the sulfur content value is 0.013%.
Example 3
5g of pure iron fluxing agent is evenly laid at the bottom of the crucible, 1g of a sample to be tested is weighed to cover the pure iron fluxing agent, 4g of tin fluxing agent is covered on the sample to be tested, 8g of tungsten particle fluxing agent is covered on the tin fluxing agent, and finally the crucible is placed in a high-frequency infrared carbon-sulfur analyzer to measure the sulfur content according to the working conditions selected in the embodiment 1, so that the sulfur content value is 0.013%.
Example 4
4g of pure iron fluxing agent is evenly laid at the bottom of the crucible, 1g of a sample to be tested is weighed to cover the pure iron fluxing agent, 6g of tin fluxing agent is covered on the sample to be tested, 12g of tungsten particle fluxing agent is covered on the tin fluxing agent, and finally the crucible is placed in a high-frequency infrared carbon-sulfur analyzer to measure the sulfur content according to the working conditions selected in the embodiment 1, so that the sulfur content value is 0.013%.
Example 5
5g of pure iron fluxing agent is evenly laid at the bottom of the crucible, 1g of a sample to be tested is weighed to cover the pure iron fluxing agent, 5g of tin fluxing agent is covered on the sample to be tested, 9g of tungsten particle fluxing agent is covered on the tin fluxing agent, and finally the crucible is placed in a high-frequency infrared carbon-sulfur analyzer to measure the sulfur content according to the working conditions selected in the embodiment 1, so that the sulfur content value is 0.013%.

Claims (6)

1. The method for measuring the sulfur content in the silicon-nitrogen alloy is characterized by comprising the steps of pretreatment, preparation of spare parts for measurement, measurement of a sulfur content blank value, calibration of a high-frequency infrared carbon-sulfur analyzer and measurement of a sample, and specifically comprises the following steps:
1) pretreatment:
uniformly spreading 3-5 g/g at the bottom of the crucibleTest specimenCovering the sample to be tested on the pure iron fluxing agent;
at a ratio of 4 to 6g/gTest specimenIn an amount to cover the sample to be tested with a tin flux;
covering a tungsten particle fluxing agent on the tin fluxing agent according to the amount of 8-12 g/g of the sample;
2) preparation of measurement preparations:
the first standard substance is: GBW (E)010299, sulfur content 0.0014%; the first standard substance is: GBW01246, sulfur content 0.036%; the third standard substance is: GBW (E)010313, sulfur content 0.011%;
3) measuring a blank value of the sulfur content: determining blank values of carbon contents of the pure iron fluxing agent, the tin fluxing agent and the tungsten fluxing agent in the step 1 by using a high-frequency infrared carbon and sulfur analyzer, inputting the blank values into the high-frequency infrared carbon and sulfur analyzer, and automatically deducting the blank values when the high-frequency infrared carbon and sulfur analyzer is calibrated;
4) calibrating a high-frequency infrared carbon-sulfur analyzer: measuring the sulfur content of the first standard substance, and comparing the sulfur content with a standard value to calibrate the instrument; respectively measuring the second standard substance and the third standard substance, respectively comparing the measured values with standard values, if the content difference value is not in an allowable range, repeating the step 4 until the difference value is in the allowable range to obtain the measured values of the sulfur content of the second standard substance and the sulfur content of the third standard substance, wherein the measured values of the sulfur content of the second standard substance and the sulfur content of the third standard substance are in the allowable difference range;
5) and (3) sample measurement:
and (4) carrying out sulfur content on the sample to be detected prepared in the step (1) by using a high-frequency infrared carbon-sulfur analyzer according to the working conditions selected in the step (4).
2. The method for measuring the sulfur content in the silicon nitrogen alloy according to claim 1, wherein the operating conditions of the high-frequency infrared carbon-sulfur analyzer are as follows: a cut-off level 7; the temperature of the combustion furnace is 1300 ℃; the number of integration times is 1; minimum analysis time 32 s; the maximum analysis time was 50 s.
3. The method for measuring the sulfur content in silicon nitride alloy as defined in claim 1, wherein in step 1, the crucible is burned at 900-1100 ℃ for 30-50min in a high temperature furnace before use, the crucible is taken out, placed in a clean heat-resistant plate, cooled for 2-3 min, and finally stored in a dryer.
4. The method of determining sulfur content in a silicon nitride alloy according to claim 1, wherein the tin particle flux is a commercially available tin flux with >99.95% tin.
5. The method for determining sulfur content in a silicon nitride alloy according to claim 1, wherein the pure iron flux is a commercially available pure iron flux with iron > 99.90%.
6. The method for determining the sulfur content in a silicon nitride alloy according to claim 1, wherein the tungsten particle flux is a commercially available pure tungsten flux with tungsten > 99.95%.
CN202110631598.4A 2021-06-07 2021-06-07 Method for measuring sulfur content in silicon-nitrogen alloy Pending CN113390813A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114235734A (en) * 2021-10-25 2022-03-25 攀钢集团攀枝花钢铁研究院有限公司 Method for determining high-sulfur content in pyrite

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CN101975760A (en) * 2010-10-08 2011-02-16 中国航空工业集团公司北京航空材料研究院 Method for measuring sulfur content in powdered high-temperature alloy
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
CN103245633A (en) * 2013-05-16 2013-08-14 内蒙古包钢钢联股份有限公司 Method of measuring carbon and sulfur contents in rare earth aluminum alloy through different reference material calibration infrared absorption method
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
CN104964945A (en) * 2015-06-12 2015-10-07 内蒙古包钢钢联股份有限公司 Method for measuring content of carbon in vanadium-nitrogen alloy

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101975760A (en) * 2010-10-08 2011-02-16 中国航空工业集团公司北京航空材料研究院 Method for measuring sulfur content in powdered high-temperature alloy
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
CN103245633A (en) * 2013-05-16 2013-08-14 内蒙古包钢钢联股份有限公司 Method of measuring carbon and sulfur contents in rare earth aluminum alloy through different reference material calibration infrared absorption method
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
CN104964945A (en) * 2015-06-12 2015-10-07 内蒙古包钢钢联股份有限公司 Method for measuring content of carbon in vanadium-nitrogen alloy

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114235734A (en) * 2021-10-25 2022-03-25 攀钢集团攀枝花钢铁研究院有限公司 Method for determining high-sulfur content in pyrite
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