Method for measuring sulfur content of low-sulfur alloy steel and application

Through the optimization treatment of carbon sulfur meter and flux, the interference coefficient is calculated and the mixture of pure iron flux and tungsten particles is used to help the flux, which solves the accuracy and stability of the sulfur content detection in alloy steel, and achieves efficient and accurate determination of the sulfur content of low sulfur alloy steel.

CN120352367APending Publication Date: 2025-07-22LESHAN CITY METROLOGY & TESTING INST

Patent Information

Application Number
CN202510838444.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-23
Publication Date
2025-07-22

AI Technical Summary

Technical Problem

The existing sulfur content detection methods in alloy steel are complex in operation and have poor accuracy, especially the low sulfur content detection accuracy, which affects product quality control.

Method used

The interference coefficient is calculated by combining the mean values of low-sulfur concentration, medium-sulfur concentration and high-sulfur concentration samples, and pure iron flux and tungsten particles are mixed to optimize the measurement process. Through the mixing and use of calibration curves and flux and the order of covering tungsten particles, the combustion is ensured and the detection accuracy and stability are improved.

Benefits of technology

The accurate determination of the sulfur content of low sulfur alloy steel is achieved, the test results are repetitive and stable, and the RSD value is low. It is suitable for sulfur content detection below 0.05%, solving the problems of low detection value and poor reproducibility.

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Abstract

The invention discloses a method for measuring the sulfur content of low-sulfur alloy steel and application, relates to the technical field of alloy steel detection, and solves the problems that an existing method for detecting the sulfur content of the alloy steel is complex in operation and poor in precision, and the detection accuracy of steel with the low sulfur content is poor. The determination method comprises the following steps: providing a carbon-sulfur instrument, a low-sulfur-concentration sample, a medium-sulfur-concentration sample and a high-sulfur-concentration sample, respectively putting the three samples into the carbon-sulfur instrument, and carrying out first treatment to obtain an average value I1, an average value I2 and an average value I3; calculating an interference coefficient RE through the average value I1, the average value I2 and the average value I3, and inputting the interference coefficient RE into the carbon-sulfur instrument to obtain a calibration curve; a sample needing to be detected is taken and subjected to second treatment to obtain a mixture, the mixture is put into a carbon and sulfur instrument, a calibration curve is selected, and measurement is started till the end. The measuring method is simple to operate and high in precision. The method has the advantages that discreteness is obviously reduced, detected results are good in repeatability and stability, and the RSD value is low.
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Description

Technical Field

[0001] The present invention relates to the technical field of alloy steel detection, and particularly to a method for determining the sulfur content of low-sulfur alloy steel and its application. Background Art

[0002] In the existing steel production process, the precise control of sulfur elements is crucial for product performance. Appropriate sulfides can improve the processing performance and magnetization performance of steel, but excessive sulfur content will damage the mechanical properties. Therefore, in the field of alloy steel preparation, controlling the sulfur content of alloy steel within a reasonable range is of great significance for the performance of steel.

[0003] Therefore, during the preparation and application processes, it is necessary to detect the sulfur content of alloy steel. Currently, the mainstream method for detecting ultra-low sulfur content is to use a high-frequency infrared carbon-sulfur analyzer for measurement. However, in actual applications, this method has problems such as low measured values, poor stability, and insufficient repeatability and reproducibility, which affect product quality control. Especially when measuring some steel samples with low sulfur content, problems often occur where the accuracy is insufficient and the detection results are inaccurate.

[0004] Although there are also methods such as the conductivity method, X-ray fluorescence spectrometry, turbidimetry, and inductively coupled plasma emission spectrometry in the prior art that can be used for sulfur detection, these methods generally have disadvantages such as complex operation and long time consumption, and it is difficult to meet the detection requirements of a large number of samples in enterprises.

[0005] Therefore, it is urgent to develop a sulfur content detection method with simple operation, high precision, high efficiency, and high sensitivity to improve the work efficiency and result reliability of detection personnel. Summary of the Invention

[0006] The purpose of the present invention is to provide a method for determining the sulfur content of low-sulfur alloy steel and its application, which has simple operation and high precision, in order to solve the problems of complex operation and poor accuracy in the existing methods for detecting the sulfur content of alloy steel, and poor detection accuracy for low-sulfur steel.

[0007] The present invention specifically adopts the following technical solutions to achieve the above purpose: In a first aspect, the present invention provides a method for determining the sulfur content of low-sulfur alloy steel, including the following steps: S1. Provide a carbon-sulfur analyzer, a low-sulfur concentration sample, a medium-sulfur concentration sample, and a high-sulfur concentration sample. Respectively take the three samples and put them into the carbon-sulfur analyzer for the first treatment to obtain the average values I1, I2, and I3; S2. Calculate the interference coefficient RE through the average values I1, I2, and I3, and input it into the carbon-sulfur analyzer to obtain a calibration curve; S3. Take the sample to be detected, conduct a second treatment on it to obtain a mixture, put the mixture into a carbon-sulfur analyzer, select a calibration curve, and start the measurement until it ends.

[0008] Further, in the S1, the concentration ranges of the low-sulfur concentration sample, the medium-sulfur concentration sample, and the high-sulfur concentration sample are 0% to 0.01%, 0.01% to 0.03%, and 0.03% to 0.05% respectively in sequence.

[0009] Further, in the S1, the first treatment is to adjust the channel of the carbon-sulfur analyzer to the low-sulfur channel, first measure the mixed sample of the low-sulfur concentration sample and the medium-sulfur concentration sample for a preset number of times, and take the average value to obtain I1; measure the mixed sample of the medium-sulfur concentration sample and the high-sulfur concentration sample for a preset number of times, and take the average value to obtain I2; measure the mixed sample of the low-sulfur concentration sample and the high-sulfur concentration sample for a preset number of times, and take the average value to obtain I3.

[0010] Further, specifically in the S2, substitute the average values I1, I2, and I3 into the formula: RE = (I1 - I2) / I1 * 100% to obtain the interference coefficient RE.

[0011] Further, in the S3, the second treatment is to weigh a first preset amount of the sample, add a second preset amount of a flux and mix them, place tungsten grains on the upper layer of the sample, and evenly cover the sample to obtain a mixture.

[0012] Further, the first preset amount is 0.5 to 1 g.

[0013] Further, the second preset amount is 0.5 to 0.6 g.

[0014] Further, the flux is pure iron.

[0015] In the second aspect, the present invention also provides an application of the above method for measuring the sulfur content of a low-sulfur alloy steel, and the measurement method is applied to alloy steel.

[0016] Compared with the prior art, the advantages of the present invention are as follows: 1. The method for measuring the sulfur content of a low-sulfur alloy steel provided by the present invention first obtains a calibration curve through the average values of the low-sulfur concentration sample, the medium-sulfur concentration sample, and the high-sulfur concentration sample to obtain the interference coefficient. Secondly, the flux used in the measurement is improved, which can solve the problems of low measured value, poor reproducibility of the detected value, and low precision of the detection result in the detection of the sulfur content in the alloy. It has the advantages of significantly reduced discreteness, good repeatability and stability of the detected results, and a lower RSD value.

[0017] More importantly, the mainstream methods for detecting ultra-low sulfur content currently have problems such as low measured values, poor stability, and insufficient repeatability and reproducibility, which affect product quality control. Especially when measuring steel samples with relatively low sulfur content, the accuracy is often insufficient, resulting in poor accuracy of the test results. The present invention is particularly suitable for the determination of sulfur content in low-sulfur alloy steel, and can accurately determine samples with sulfur content below 0.05% (S < 0.05%), and the test results have good repeatability and stability.

[0018] Specifically, by selecting pure iron flux in the present invention, it can help generate high temperature and completely release various elements in the sample. Tungsten grains have a low price and a small blank value. When measuring samples with low-concentration sulfur content, they will not interfere with the measurement results. The combustion property of tungsten grains can increase the diffusion rate of sulfur and help the instrument capture sulfur elements that are fully burned to the greatest extent. In the experiment, mixing iron and tungsten as flux has good repeatability and stability.

[0019] At the same time, the present invention defines that the sample is first added to the flux for mixing, and then tungsten grains are placed on the upper layer to evenly cover the sample to obtain a mixture; through the mixed use of the flux and the regulation of the placement order, the combustion is sufficient, which helps the instrument better capture sulfur elements and further improves the accuracy of the determination result.

[0020] In addition, due to its special material, the ceramic boiler is extremely easy to absorb moisture, sulfur dioxide and other gases on its surface. However, during the detection process, the burned moisture will vaporize and carry away sulfur dioxide, which reduces the conversion rate of sulfur dioxide to a certain extent and causes the measured value of sulfur element to be low. Therefore, by pre-treating the ceramic crucible in the present invention, the accuracy of this determination method can be further enhanced.

[0021] 3. The application of the method for determining the sulfur content of low-sulfur alloy steel provided by the present invention has a wide application space because the determination method is simple and easy to control. Brief Description of the Drawings

[0022] Figure 1 It is a schematic diagram of the method for determining the sulfur content of a low-sulfur alloy steel according to the present invention.

[0023] To make the objectives, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are some but not all of the embodiments of the present invention.

[0024] Therefore, the following detailed description of the provided embodiments of the present invention is not intended to limit the scope of the claimed present invention, but merely represents selected embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the scope of protection of the present invention. Specific Embodiments

[0025] In a first aspect, the present invention provides a method for determining the sulfur content of a low-sulfur alloy steel. Please refer to Figure 1 , which includes the following steps: S1. Provide a carbon-sulfur analyzer, a low-sulfur concentration sample, a medium-sulfur concentration sample, and a high-sulfur concentration sample. Put the three samples into the carbon-sulfur analyzer respectively and perform a first treatment to obtain an average value I1, an average value I2, and an average value I3; S2. Calculate the interference coefficient RE through the average values I1, I2, and I3, and input it into the carbon-sulfur analyzer to obtain a calibration curve; S3. Take the sample to be detected, perform a second treatment on it to obtain a mixture, put the mixture into the carbon-sulfur analyzer, select the calibration curve, and start the measurement until it ends.

[0026] It can be understood that the determination method of the present invention first obtains a calibration curve through the average values of the low-sulfur concentration sample, the medium-sulfur concentration sample, and the high-sulfur concentration sample to obtain the interference coefficient. Secondly, the flux used in the measurement is improved, which can solve the problems of low measured value, poor reproducibility of the detected value, and low precision of the detection result in the detection of sulfur content in alloys.

[0027] In some embodiments of the present invention, in S1, the concentration ranges of the low-sulfur concentration sample, the medium-sulfur concentration sample, and the high-sulfur concentration sample are 0% to 0.01%, 0.01% to 0.03%, and 0.03% to 0.05% respectively.

[0028] Specifically, the low-sulfur concentration sample, the medium-sulfur concentration sample, and the high-sulfur concentration sample are respectively: GBW(E)010330a (s = 0.0055%), GBW01122 (s = 0.010%), and GBW01246 (s = 0.036%).

[0029] In some embodiments of the present invention, in S1, it also includes pre-treating the ceramic crucible. Use crucible tongs to push the crucible into the combustion tube, burn the crucible for 20 minutes, wait for the equipment to heat up to 1300 °C, keep it at a constant temperature for 2 to 4 hours, and use crucible tongs to take the crucible and place it on the cooling plate.

[0030] It can be understood that due to its special material, the ceramic boiler is extremely easy to absorb gases such as moisture and sulfur dioxide on its surface. However, during the detection process, the burned moisture will vaporize and carry away sulfur dioxide, which reduces the conversion rate of sulfur dioxide to a certain extent and causes the measured value of sulfur element to be low. Therefore, by pre-treating the ceramic crucible, the accuracy of the present determination method can be further enhanced.

[0031] In some embodiments of the present invention, in S1, the first treatment is to adjust the channel of the carbon and sulfur analyzer to the low sulfur channel, first measure a mixed sample of a low sulfur concentration sample and a medium sulfur concentration sample a preset number of times, and take the average value to obtain I1; measure a mixed sample of a medium sulfur concentration sample and a high sulfur concentration sample a preset number of times, and take the average value to obtain I2; measure a mixed sample of a low sulfur concentration sample and a high sulfur concentration sample a preset number of times, and take the average value to obtain I3.

[0032] In some embodiments of the present invention, specifically in S2, substitute the average values I1, I2, and I3 into the formula: RE = (I1 - I2) / I1 * 100%, to obtain the interference coefficient RE.

[0033] In some embodiments of the present invention, in S3, the second treatment is to weigh a first preset amount of the sample, add a second preset amount of the flux and mix them, place tungsten grains on the upper layer of the sample, and evenly cover the sample to obtain a mixture.

[0034] In some embodiments of the present invention, the first preset amount is 0.5 - 1 g.

[0035] In some embodiments of the present invention, the second preset amount is 0.5 - 0.6 g.

[0036] In some embodiments of the present invention, the amount of tungsten grains used is 0.3 g.

[0037] It can be understood that when the weighed sample mass is too large, incomplete combustion of the sample will occur, resulting in a trailing release curve and incomplete release of sulfur dioxide, causing the measured value to be low. When the weighed value is too small, the instrument will capture insufficient sulfur element content, resulting in a large error in the integral calculation of the measurement result, a weak detection signal, and poor precision of the detection result. Therefore, the present invention controls a reasonable first preset amount to make the measured value result have high reproducibility.

[0038] In some embodiments of the present invention, the flux is pure iron.

[0039] When using a high-frequency infrared carbon and sulfur analyzer to measure the sulfur content in low sulfur alloy steel, selecting a suitable flux is crucial for ensuring combustion efficiency, improving detection stability and repeatability. Using iron + tungsten as the combustion flux in the present invention can significantly improve the sulfur release kinetics, making the detected results have good repeatability and stability, and having superiority.

[0040] The dual role of iron + tungsten as the combustion flux significantly improves the accuracy and repeatability of the high-frequency infrared method for measuring low sulfur alloy steel.

[0041] It is understandable that the amount of flux used has a great influence on the measurement reproducibility. Excessive flux will generate a large amount of dust, resulting in a large number of bubbles in the combustion sample. The mixed slag will cause blockage of the instrument and equipment, deviate greatly in the infrared absorption spectrum, resulting in poor reproducibility of the detection value and affecting the detection accuracy.

[0042] There are usually three types of fluxes commonly used for the combustion of alloy samples: tungsten granules, tin granules, and pure iron. The price of tin granules is relatively high compared to the former two, which is not friendly to the cost control of enterprises. Its chemical combustion properties will cause the measured value of sulfur mass fraction to be on the low side.

[0043] In the present invention, by selecting pure iron flux, it can help generate high temperature and completely release various elements in the sample. Tungsten granules have a low price and a small blank value. When measuring samples with low sulfur content, they will not interfere with the measurement results. The combustion property of tungsten granules can increase the diffusion rate of sulfur and help the instrument capture the fully combusted sulfur element to the greatest extent. And mixing iron and tungsten fluxes has good repeatability and stability.

[0044] At the same time, the present invention limits that the sample is first added to the flux and mixed, and then tungsten granules are placed on the upper layer to evenly cover the sample to obtain a mixture; through the mixed use of the flux and the regulation of the placement order, the combustion is made sufficient, which helps the instrument better capture the sulfur element and further improves the accuracy of the measurement result.

[0045] In some embodiments of the present invention, the carbon sulfur analyzer setting program is operated, and the sulfur content in the standard is deducted by the automatic blank correction method of the instrument.

[0046] Since the analysis accuracy of sulfur element determination is affected by the blank value of the instrument, and at the same time, in the operation and setting program, the sulfur content in the standard is deducted by the automatic blank correction method of the instrument, which uses the functions equipped with the existing carbon sulfur analyzer. During long-term operation, the infrared light source decays or the detector sensitivity decreases. In the case of high measurement results or unstable numerical values, automatic calibration is performed to eliminate them.

[0047] In the case where the blank value is much smaller than the sulfur content fraction, it will not affect the measurement result. And it can improve the accuracy of the measurement result.

[0048] In some embodiments of the present invention, the specific operation of S3 is to operate the carbon sulfur analyzer to obtain the content of sulfur element according to the following formula: s = ( As b m b / A b m )- s o In the formula:s—— Mass fraction of sulfur element in the sample; % m —— Mass of the sample, g m b —— Mass of the steel reference sample taken, g; A —— Absorbance of the sample; A b —— Corrected absorbance of the steel reference sample; s b —— Standard value of the mass fraction of sulfur element in the steel reference sample, %; s o —— Measured value of the mass fraction of sulfur element during blank correction, %.

[0049] Second, the present invention also provides an application of the above method for determining the sulfur content of low-sulfur alloy steel, and the determination method is applied to alloy steel. It can be understood that due to the simplicity and easy control of the determination method, the application space of the method for determining the sulfur content of low-sulfur alloy steel of the present invention is extensive.

[0050] Example 1 This example provides a method for determining the sulfur content of low-sulfur alloy steel. The instrument used is a COREY-320 high-frequency infrared carbon-sulfur analyzer, which has a high usage rate in the steel industry and representative practical scenarios. The steps of the method are as follows: (1) Establish a working calibration curve for measuring low-concentration sulfur content Use standard samples GBW(E)010330a (s = 0.0055%), GBW01122 (s = 0.010%), and GBW01246 (s = 0.036%) as test standard samples. Adjust the instrument channel to the low-sulfur channel. The three concentrations are A, B, and C respectively. First, measure the A + B mixed sample 3 times and take the average value I1. Then measure the C sample, and then measure the B + C mixed sample 3 times and take the average value I2. Similarly, measure the average value I3 of the A + C mixed sample.

[0051] Calculate the interference coefficient RE of these three samples, eliminate the mutual interference between different low-concentration coefficient sulfur contents, and then use the three standard substances for curve verification respectively. Conduct data analysis and fit the regression equation to establish a linear model Y = aX + b, and establish a standard working curve of the interference coefficient of the sulfur mass fraction (0.0055% - 0.036%) based on the data results.

[0052] RE b =(I1 - I2) / I1 * 100% (interference coefficient) (2) Treatment of the ceramic crucible Use a special crucible tongs to push the crucible into the combustion tube, and burn the crucible for 20 minutes. Wait for the equipment to heat up to 1300 °C and keep it at a constant temperature for 2 - 4 hours. Then use the special crucible tongs to take out the crucible and place it on the cooling tray.

[0053] (3)Sample treatment Weigh 0.5 - 1 g of the measurement sample, then add 0.5 - 1 g of pure iron fluxing agent. Place an appropriate amount (1 spoonful) of tungsten grains on the upper layer of the measurement sample to evenly cover the sample. Put the final mixture into the carbon-sulfur analyzer, set the analysis time to 40 s, select the corresponding channel for analysis and measurement, and obtain the sulfur element content according to formula (1): Formula (1): s = (Asbmb / Ab m)-so In the formula: s — mass fraction of sulfur element in the sample; %, m — mass of the sample, g mb — mass of the steel standard sample weighed, g; A — absorbance of the sample; Ab — corrected absorbance of the steel standard sample; sb — standard value of the mass fraction of sulfur element in the steel standard sample, %; so — measured value of the mass fraction of sulfur element during blank correction, %.

[0054] Example 2 In this example, a method for determining the sulfur content of low-sulfur alloy steel is provided. It includes the following steps: S1. Provide a carbon-sulfur analyzer: COREY-320 high-frequency infrared carbon-sulfur analyzer, low-sulfur concentration sample, medium-sulfur concentration sample, and high-sulfur concentration sample. Put the three samples into the carbon-sulfur analyzer respectively and perform the first treatment to obtain the average values I1, I2, and I3; the low-sulfur concentration sample, the medium-sulfur concentration sample, and the high-sulfur concentration sample are GBW(E)010330a, GBW01122, and GBW01246 respectively. The first treatment is to adjust the channel of the carbon-sulfur analyzer to the low-sulfur channel. First, measure the mixed sample of the low-sulfur concentration sample and the medium-sulfur concentration sample a preset number of times and take the average to get I1; measure the mixed sample of the medium-sulfur concentration sample and the high-sulfur concentration sample a preset number of times and take the average to get I2; measure the mixed sample of the low-sulfur concentration sample and the high-sulfur concentration sample a preset number of times and take the average to get I3.

[0055] S2. Calculate the interference coefficient RE through the average values I1, I2, and I3, and input it into the carbon-sulfur analyzer to obtain the calibration curve; substitute the average values I1, I2, and I3 into the formula: RE = (I1 - I2) / I1 * 100%, and obtain the interference coefficient RE.

[0056] S3. Take the sample to be detected, conduct a second treatment on it to obtain a mixture, put the mixture into a carbon-sulfur analyzer, select a calibration curve, and start the determination until it ends. The second treatment is to weigh a first preset amount of the sample, add a second preset amount of a flux and mix them, place tungsten grains on the upper layer of the sample, and evenly cover the sample to obtain a mixture; the first preset amount is 0.5 - 1 g. The second preset amount is 0.5 - 1 g. The flux is pure iron.

[0057] Experimental Example 1 Exploration of discreteness 1.1 Specific verification method In this experimental example, based on Example 1 and Example 2, operate the carbon-sulfur analyzer to verify the analysis results of the linear curve and the interference coefficient curve.

[0058] The model of the carbon-sulfur analyzer is: COREY-320 high-frequency infrared carbon-sulfur analyzer.

[0059] The analysis results are shown in Table 1.

[0060] 1.2 Verification results Table 1. Verification table of the analysis results of the linear curve and the interference coefficient curve Unit %

[0061] 1.2 Result analysis Referring to the results in Table 1, the deviation value of the measured value using the linear curve is relatively large compared with the national standard value, and the discreteness of the measured value is significantly reduced after using the interference coefficient curve.

[0062] Experimental Example 2 Exploration of the influence of different weighed sample masses on the detection results 2.1 Experimental design In this experimental example, explore the influence of different weighed sample masses on the detection results.

[0063] Select alloy steel samples with less sulfur content: Select GBW01245 ( s =0.020%) for sample mass verification. The measurement method uses the measurement methods in Example 1 and Example 2.

[0064] And set four experimental groups (Experimental Groups 1 - 4), and all select GBW01245 ( s =0.020%) as the weighed samples.

[0065] The detection methods of the four experimental groups of Experimental Groups 1 - 4 are all carried out according to the operations in Example 1 and Example 2, and are kept consistent. The difference lies in the weighed sample masses, which are 0.1, 0.3, 0.5, and 1.0 g respectively.

[0066] The measurement results of the four experimental groups of Experimental Groups 1 - 4 are shown in Table 2 respectively.

[0067] 2.2 Test Results Table 2. Determination Results of Weighed Sample Mass and Sulfur Content

[0068] 2.3 Analysis of Test Results According to the experimental results in Table 2, for the groups in Experimental Groups 3 and 4 where the weighed sample mass is 0.5 - 1.0 g, the error between the measured value of the mass fraction and the standard value is relatively small.

[0069] However, for Experimental Groups 1 and 2 where the weighed sample mass is less than 0.5 g, the measurement repeatability significantly deteriorates, resulting in poor reproducibility of the test results.

[0070] Therefore, in the present invention, the weighed sample mass is selected as (0.5 - 1.0) g, which has good reproducibility.

[0071] Test Example 3 explores the influence of different fluxes on the test results 3.1 Test Design In this test example, the influence of different fluxes on the test results is explored.

[0072] Select alloy steel samples with less sulfur content: Select GBW01245 ( s = 0.020%) for flux verification. The measurement method used is the measurement method in Example 1.

[0073] And set four experimental groups (Experimental Groups 1 - 4), all of which select GBW01245 ( s = 0.020%) as the weighed sample.

[0074] The detection methods of the four experimental groups of Experimental Groups 1 - 4 are all carried out according to the operations of Example 1 and Example 2, and are kept consistent. The difference lies in the fluxes used, which are iron, tungsten, iron + tungsten, and tin respectively.

[0075] The measurement results of the four experimental groups of Experimental Groups 1 - 4 are shown in Table 3 respectively.

[0076] 3.2 Test Results Table 3. Determination Results of Sulfur Mass Fraction in Samples with Different Fluxes

[0077] 3.3 Analysis of Test Results Referring to the measurement results of Experimental Groups 1 - 4 in Table 3 and making a comparison, it can be seen that for Experimental Groups 1 and 4 using fluxes of pure iron and pure tin, the measured results have relatively large errors, both above 0.01.

[0078] However, the error of Experimental Group 2 using pure tungsten as the flux is relatively not large.

[0079] For Experimental Group 3 that selects iron + tungsten as the combustion flux defined by the present invention, the error is the smallest and the RSD value is the lowest.

[0080] Test Example 4 explores the precision of the method of the present invention. 4.1 Experimental Design In this test example, the operation time of the calibration blank mode is adjusted to eliminate the tailing phenomenon during the use of the instrument and improve the measurement precision. And the precision of the method of the present invention is explored.

[0081] 4.2 Experimental Design and Results Select a blank sample of sulfur element to measure the blank value of the sulfur element sample, and the results are shown in Table 4.

[0082] Table 4. Blank value of sulfur element sample (n = 10) %

[0083] Referring to the corresponding operations in Example 1 and Example 2, use this method to select the sample standard GBW01245 (s = 0.020%) and conduct 12 parallel measurements. The measurement results are shown in Table 5.

[0084] Table 5. Results of precision measurement %

[0085] 4.3 Analysis of Test Results According to the data in Table 4 and Table 5, using the method of the present invention, whether measuring the sulfur element content of blank samples or standard samples, the obtained measured values are very stable and the RSD values are relatively low. This shows that the method of the present invention has high precision and superiority.

[0086] To sum up, through the measurement of discreteness in Test Example 1, the exploration of the influence of different weighed sample masses on the test results in Test Example 2, the exploration of the influence of different fluxes on the test results in Test Example 3, and the exploration of the precision of the method of the present invention in Test Example 4, it shows that a method for measuring the sulfur content of low-sulfur alloy steel provided by the present invention can solve problems such as low measured values, poor reproducibility of detected values, and low precision of test results in the detection of sulfur content in alloys. It has the advantages of significantly reduced discreteness, good repeatability and stability of detected results, and relatively low RSD values.

[0087] The above embodiments are only one implementation manner of the present invention, and its description is relatively specific and detailed, but it should not be construed as a limitation to the scope of the present invention patent. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present invention, several deformations and improvements can still be made, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the present invention patent should be subject to the appended claims.

Claims

1. A method for determining the sulfur content of a low-sulfur alloy steel, characterized in that, Including the following steps: S1. Provide a carbon-sulfur analyzer, low-sulfur concentration samples, medium-sulfur concentration samples, and high-sulfur concentration samples. Put the three types of samples into the carbon-sulfur analyzer respectively and conduct the first treatment to obtain the average values I1, I2, and I3. S2. Calculate the interference coefficient RE through the average values I1, I2, and I3, and input it into the carbon-sulfur analyzer to obtain the calibration curve. S3. Take the sample to be detected, conduct the second treatment to obtain a mixture, put the mixture into the carbon-sulfur analyzer, select the calibration curve, and start the measurement until it ends.

2. The method for determining the sulfur content of a low-sulfur alloy steel according to claim 1, characterized in that, In S1, the concentration ranges of the low-sulfur concentration sample, the medium-sulfur concentration sample, and the high-sulfur concentration sample are 0% - 0.01%, 0.01% - 0.03%, and 0.03% - 0.05% respectively in sequence.

3. The method for determining the sulfur content of a low-sulfur alloy steel according to claim 1, wherein In S1, the first treatment is to adjust the channel of the carbon-sulfur analyzer to the low-sulfur channel. First, measure the mixed sample of the low-sulfur concentration sample and the medium-sulfur concentration sample for a preset number of times and take the average to obtain I1; measure the mixed sample of the medium-sulfur concentration sample and the high-sulfur concentration sample for a preset number of times and take the average to obtain I2; measure the mixed sample of the low-sulfur concentration sample and the high-sulfur concentration sample for a preset number of times and take the average to obtain I3.

4. The method for determining the sulfur content of a low-sulfur alloy steel according to claim 1, characterized in that, Specifically in S2, substitute the average values I1, I2, and I3 into the formula: RE = (I1 - I2) / I1 * 100% to obtain the interference coefficient RE.

5. The method for determining the sulfur content of a low-sulfur alloy steel according to claim 1, wherein, In S3, the second treatment is to weigh a first preset amount of the sample, add a second preset amount of the flux and mix them, place tungsten grains on the upper layer of the sample, and evenly cover the sample to obtain a mixture.

6. The method for determining the sulfur content of a low-sulfur alloy steel according to claim 5, wherein The first preset amount is 0.5 - 1 g.

7. The method for determining the sulfur content of a low-sulfur alloy steel according to claim 5, characterized in that The second preset amount is 0.5 - 0.6 g.

8. A method for determining the sulfur content of a low-sulfur alloy steel according to claim 5, characterized in that, The flux is pure iron.

9. Use of a method for determining the sulfur content of a low-sulfur alloy steel according to any one of claims 1-8, characterized in that, The determination method is applied to alloy steel.

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