Method for detecting sulfides and sulfates in steel slag and slag-based full-solid-waste cementitious material

Abstract

The present application particularly relates to a detection method of sulfide and sulfate in steel slag and slag-based full solid waste cementitious material, and belongs to the technical field of analysis and detection. The peak intensity 2theta angle and mutual spectrum line overlapping coefficient of SKa1,2 spectrum line and SO3Ka1,2 spectrum line are determined through experiments. Then, the actual intensity of SKa1,2 spectrum line and SO3Ka1,2 spectrum line in the calibration sample is calculated by using the spectrum line overlapping coefficient. Finally, the working curve is established by using the actual intensity, and the content of sulfide (calculated by S) and sulfate (calculated by SO3) is calculated. The content of sulfide and sulfate in steel slag and slag-based full solid waste cementitious material is rapidly determined, and the detection period is greatly shortened under the premise of ensuring accuracy.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of analysis and detection, and particularly relates to a detection method of sulfides and sulfates in a steel slag and slag-based full-solid waste cementitious material. BACKGROUND

[0002] The raw material of the steel slag and slag-based full-solid waste cementitious material is steel slag, blast furnace slag and gypsum. The content of gypsum affects the setting time of the cementitious material and is a main index for measuring the quality of the cementitious material. At present, the most classic detection method for the determination of the content of sulfates in the cementitious material is the weight method, such as the barium sulfate weight method in GB / T 176-2017 "Cement Chemical Analysis Method". The method has high accuracy, but the operation steps are very cumbersome, the detection period is long, and at least two days are required.

[0003] In order to realize the rapid determination of the content of sulfates in the steel slag and slag-based full-solid waste cementitious material, GB / T 176-2017 simultaneously provides alternative methods such as the iodometric method, the coulometric titration method and the ion exchange method. The alternative methods can shorten the detection time, but there are problems such as difficulty in controlling the test conditions and complex interference, which affect the determination results.

[0004] The use of the X fluorescence spectrum method to determine the content of sulfates has advantages such as rapidness, accuracy and simple operation, but there are sulfides in the steel slag and slag-based full-solid waste cementitious material, and the content is high, which affects the determination of the content of sulfates. SUMMARY

[0005] The purpose of the present application is to provide a detection method of sulfides and sulfates in a steel slag and slag-based full-solid waste cementitious material, so as to solve the problem that there is no way to rapidly and accurately determine the sulfides and sulfates in the steel slag and slag-based full-solid waste cementitious material at present.

[0006] The embodiment of the present application provides a detection method of sulfides and sulfates in a steel slag and slag-based full-solid waste cementitious material, and the method comprises the following steps:

[0007] An overlapping coefficient between SKa1,2 and SO3Ka1,2 is obtained;

[0008] Sulfide working curves and sulfate working curves are obtained;

[0009] A to-be-measured sample is obtained;

[0010] The to-be-measured sample is determined by an X fluorescence spectrometer to obtain a determination intensity I S,测定 and a determination intensity

[0011] According to the overlapping coefficient between SKa1,2 and SO3Ka1,2, the determination intensity I S,测定measured intensity of SKa1,2 actual intensity I of SKa1,2 S,实际 actual intensity of SO3Ka1,2

[0012] actual intensity I of SKa1,2 S,实际 sulfide content according to the sulfide working curve and the actual intensity I of SKa1,2

[0013] sulfate content according to the sulfate working curve and the actual intensity of SO3Ka1,2

[0014] Optionally, the obtaining of the overlap coefficient between SKa1,2 and SO3Ka1,2 specifically comprises:

[0015] obtaining a first sample and a second sample, the sulfur in the first sample being in the form of sulfide, and the sulfur in the second sample being in the form of sulfate;

[0016] performing X fluorescence spectrum scanning analysis on the first sample and the second sample to obtain the 2θ angle of SKa1,2 and SO3Ka1,2;

[0017] performing multiple X fluorescence spectrum scanning analysis on the first sample and the second sample according to the 2θ angle of SKa1,2 and SO3Ka1,2 to obtain the overlap coefficient between SKa1,2 and SO3Ka1,2.

[0018] Optionally, the first sample is a blast furnace slag sample with SO3 content less than 0.05%, and the second sample is a blast furnace slag sample after being calcined at 900-1000℃ for 32-40h

[0019] Optionally, the obtaining of the sulfide working curve and the sulfate working curve specifically comprises:

[0020] obtaining a plurality of calibration samples;

[0021] performing infrared carbon-sulfur analyzer measurement on the plurality of calibration samples to obtain the total sulfur content of each calibration sample;

[0022] performing barium sulfate gravimetric method measurement on the plurality of calibration samples to obtain the sulfate content of each calibration sample;

[0023] obtaining the sulfide content of each calibration sample through the total sulfur content and the sulfate content of each calibration sample;

[0024] performing X fluorescence spectrometer measurement on the plurality of calibration samples to obtain the measured intensity of SKa1,2 of each calibration sample and the measured intensity of SO3Ka1,2 of each calibration sample;

[0025] ​Based on the overlap coefficient between SKa1,2 and SO3Ka1,2, the measured intensity of SKa1,2 of each calibration sample and the measured intensity of SO3Ka1,2 of each calibration sample, the actual intensity of SKa1,2 and SO3Ka1,2 of each calibration sample are obtained.

[0026] Based on the sulfate content of each calibration sample and the actual strength of SO3Ka1,2 of each calibration sample, the sulfate working curve was obtained.

[0027] Based on the sulfide content of each calibration sample and the actual strength of SKa1,2 of each calibration sample, the sulfide working curve is obtained.

[0028] Optionally, the calibration sample is a blast furnace slag and steel slag-based solid waste cementitious material, and the sulfur in the blast furnace slag and steel slag-based solid waste cementitious material exists in the form of both sulfides and sulfates.

[0029] Optionally, obtaining the sample to be tested specifically includes:

[0030] Obtain the material to be tested.

[0031] The material to be tested is compressed into tablets to obtain the test sample.

[0032] Optionally, the particle size of the material to be tested is such that it passes through a 200-mesh sieve; the pressure for tablet preparation is 25t-30t; and the holding time for tablet preparation is 10s-20s.

[0033] Optionally, the method based on the overlap coefficient between SKa1,2 and SO3Ka1,2, and the measured intensity I of SKa1,2... S,测定 The intensity of SO3Ka1,2 was determined. The actual strength I of SKa1,2 was obtained. S,实际 The actual strength of SO3Ka1,2 middle,

[0034] The overlap coefficient between SKa1,2 and SO3Ka1,2 includes: the overlap coefficient of SKa1,2 with respect to SO3Ka1,2. The overlap coefficient between SO3Ka1,2 and SKa1,2

[0035] The actual strength I of SKa1,2 S,实际 The overlap coefficient between SKa1,2 and SO3Ka1,2, and the measured intensity I of SKa1,2 S,测定 The relationship satisfies:

[0036] The actual strength of SO3Ka1,2 the overlapping coefficient between SKa1,2 and SO3Ka1,2, the measured intensity of SO3Ka1,2 satisfy:

[0037] Optionally, the overlapping coefficient of SKa1,2 to SO3Ka1,2 the overlapping coefficient of SO3Ka1,2 to SKa1,2

[0038] Optionally, the detection range of the method includes a sulfide detection range and a sulfate detection range, the sulfide detection range is 0.4%-1.3%, and the sulfate detection range is 0.3%-4.0%.

[0039] One or more technical solutions in the embodiments of the present application have at least the following technical effects or advantages:

[0040] The method for detecting sulfides and sulfates in the steel slag and slag-based full-solid waste cementing material provided by the embodiments of the present application determines the peak intensity 2θ angle and the spectral line overlapping coefficient of the SKa1,2 spectral line and the SO3Ka1,2 spectral line through experiments; then, the spectral line overlapping coefficient is used to calculate the actual intensity of the SKa1,2 spectral line and the SO3Ka1,2 spectral line in the calibration sample; finally, the actual intensity is used to establish a working curve, and the content of sulfides (calculated in terms of S) and sulfates (calculated in terms of SO3) is calculated; the rapid determination of the content of sulfides and sulfates in the steel slag and slag-based full-solid waste cementing material is realized, and the detection period is greatly shortened under the premise of ensuring accuracy.

[0041] The above description is only a summary of the technical solutions of the present application, in order to more clearly understand the technical means of the present application, the embodiments of the present application can be implemented according to the content of the specification, and in order to make the above and other purposes, characteristics and advantages of the present application more obvious and easy to understand, the following specific embodiments of the present application are described. BRIEF DESCRIPTION OF DRAWINGS

[0042] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following will briefly introduce the drawings needed in the embodiment description. Obviously, the drawings in the following description are some embodiments of the present application, and those skilled in the art can also obtain other drawings according to these drawings without creating any creative labor.

[0043] Figure 1 is a flow chart of the method provided by the embodiments of the present application;

[0044] Figure 2 is a working curve of sulfides provided by the embodiments of the present application;

[0045] Figure 3is a working curve of the sulfate provided by the embodiment of the present application. DETAILED DESCRIPTION

[0046] The advantages and various effects of the present application will be more clearly presented hereinafter with specific embodiments and examples. Those skilled in the art should understand that these specific embodiments and examples are used to illustrate the present application, rather than limit the present application.

[0047] Throughout the specification, unless otherwise specifically indicated, the terms used herein are to be understood as having the meanings commonly used in the art. Therefore, unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the present application belongs. If there is a conflict, the present specification takes precedence.

[0048] Unless otherwise specifically indicated, various raw materials, reagents, instruments and equipment used in the present application can be purchased from the market or can be prepared by existing methods.

[0049] The technical solution of the embodiments of the present application is to solve the above technical problems, and the general idea is as follows:

[0050] The applicant found in the process of invention that there is a certain energy level difference between the SKa1,2 spectrum line of sulfur in sulfide and the SO3Ka1,2 spectrum line of sulfur in sulfate. When performing X fluorescence spectrum analysis, if a GE111 crystal is used for spectrometry, the 2θ angles corresponding to the peak intensities of the two are different by about 0.1°, and the resolution of the X fluorescence spectrometer is not enough to distinguish the two.

[0051] According to a typical embodiment of the present application, a method for detecting sulfide and sulfate in a steel slag and slag-based full-solid waste cementitious material is provided, which comprises: first, determining the peak intensity 2θ angle and the mutual spectrum line overlap coefficient of SKa1,2 spectrum line and SO3Ka1,2 spectrum line through experiments; then, calculating the actual intensity of SKa1,2 spectrum line and SO3Ka1,2 spectrum line in the calibration sample using the spectrum line overlap coefficient; finally, establishing a working curve using the actual intensity, and calculating the content of sulfide (calculated as S) and sulfate (calculated as SO3).

[0052] Specifically, the method comprises:

[0053] S1. obtaining the overlap coefficient between SKa1,2 and SO3Ka1,2;

[0054] In some embodiments, the obtaining of the overlap coefficient between SKa1,2 and SO3Ka1,2 specifically comprises:

[0055] S1.1. obtaining a first sample and a second sample, sulfur in the first sample existing in the form of sulfide, and sulfur in the second sample existing in the form of sulfate;

[0056] S1.2. performing X fluorescence spectrum scanning analysis on the first sample and the second sample to obtain 2theta angles of SKa1,2 and SO3Ka1,2;

[0057] S1.3. performing multiple X fluorescence spectrum scanning analysis on the first sample and the second sample according to the 2theta angles of SKa1,2 and SO3Ka1,2 to obtain an overlapping coefficient between SKa1,2 and SO3Ka1,2.

[0058] In this embodiment,

[0059] The sample 1 is a blast furnace slag sample in which sulfur exists in the form of sulfide (total sulfur content is 1.30%), and the SO3 content of the blast furnace slag sample is determined by the barium sulfate gravimetric method in GB / T 176-2017, and the determination result is required to be less than 0.05%.

[0060] The sample 2 is a blast furnace slag sample after ignition in which sulfur exists in the form of sulfate (total sulfur content is 0.97%), about 7g of the blast furnace slag sample is weighed and laid flat in a ceramic dish, and is ignited at 900℃-1000℃ for 32h-40h to oxidize all the sulfide into sulfate.

[0061] The sample 1 and the sample 2 are subjected to X fluorescence spectrum scanning analysis to determine the 2theta angles of the peak values of the SKa1,2 spectrum line and the SO3Ka1,2 spectrum line and the overlapping coefficient therebetween, and the scanning analysis conditions are shown in Table 1.

[0062] Table 1 Scanning conditions of X fluorescence spectrometer

[0063]

[0064] The sample 1 and the sample 2 are subjected to X fluorescence spectrum scanning analysis by using the scanning conditions in Table 1, and it is obtained that the peak value 2theta angle of the SKa1,2 spectrum line is 110.71°, and the peak value 2theta angle of the SO3Ka1,2 spectrum line is 110.62°.

[0065] Table 2 Analysis conditions of X fluorescence spectrometer

[0066]

[0067] The sample 1 and the sample 2 are subjected to 3 times of determination by using the analysis conditions in Table 2, and the overlapping coefficient between SKa1,2 and SO3Ka1,2 is calculated by using the mean value of the spectrum line intensity of the two, and the results are shown in Table 3.

[0068] Table 3 Calculation results of overlapping coefficient

[0069]

[0070] S2. obtaining a sulfide working curve and a sulfate working curve;

[0071] In some embodiments, the obtaining a sulfide working curve and a sulfate working curve specifically comprises:

[0072] S2.1. obtaining a plurality of calibration samples;

[0073] S2.2. subjecting the plurality of calibration samples to infrared carbon-sulfur analyzer determination to obtain total sulfur content of each calibration sample;

[0074] S2.3. subjecting the plurality of calibration samples to barium sulfate gravimetric determination to obtain sulfate content of each calibration sample;

[0075] S2.4. obtaining sulfide content of each calibration sample from the total sulfur content and the sulfate content of each calibration sample;

[0076] S2.5. subjecting the plurality of calibration samples to X-ray fluorescence spectrometer determination to obtain measured intensity of SKa1,2of each calibration sample and measured intensity of SO3Ka1,2of each calibration sample;

[0077] S2.6. obtaining actual intensity of SKa1,2of each calibration sample and actual intensity of SO3Ka1,2of each calibration sample according to the overlap coefficient between SKa1,2and SO3Ka1,2, the measured intensity of SKa1,2of each calibration sample and the measured intensity of SO3Ka1,2of each calibration sample;

[0078] S2.7. obtaining a sulfate working curve according to the sulfate content of each calibration sample and the actual intensity of SO3Ka1,2of each calibration sample;

[0079] S2.8. obtaining a sulfide working curve according to the sulfide content of each calibration sample and the actual intensity of SKa1,2of each calibration sample.

[0080] In this embodiment, 11 blast furnace slag and steel slag mineral slag-based full solid waste cementitious materials were selected as calibration samples, the total sulfur content therein was determined using a high-frequency infrared carbon-sulfur analyzer, the sulfate (calculated as SO3) content therein was determined using a barium sulfate gravimetric method, and the sulfide (calculated as S) content was indirectly calculated. The calibration sample value determination results are shown in Table 4.

[0081] Table 4 Calibration sample value determination results

[0082]

[0083] About 7 g of the calibration sample with particle size greater than 200 mesh is placed in a steel ring padded with boric acid, and is pressed for 10 s to 20 s under a pressure of 25 t to 30 t to prepare a powder tablet for measurement.

[0084] The intensities of the calibration samples SKa1,2 and SO3Ka1,2 are measured according to the analysis conditions in Table 2, and the actual intensities of the two are calculated according to the formula and The working curve is plotted with the actual intensities and the corresponding calibration results, and the working curve is fitted by a second order line, with the X axis representing the content (%) and the Y axis representing the actual intensity (Kcps).

[0085] S3. Obtain a sample to be measured;

[0086] In some embodiments, the obtaining of the sample to be measured specifically comprises:

[0087] S3.1. Obtain a material to be measured,

[0088] In this embodiment, the particle size of the material to be measured is greater than 200 mesh.

[0089] S3.2. Tablet the material to be measured to obtain a sample to be measured.

[0090] In this embodiment, the pressure for tabletting the sample to be measured is 25 t to 30 t, and the holding pressure time for tabletting the sample to be measured is 10 s to 20 s.

[0091] S4. Measure the sample to be measured by an X-ray fluorescence spectrometer to obtain the measured intensity I S,测定 and the measured intensity of SO3Ka1,2

[0092] S5. According to the overlapping coefficient between SKa1,2 and SO3Ka1,2, the measured intensity I S,测定 and the measured intensity of SO3Ka1,2 the actual intensity I S,实际 and the actual intensity of SO3Ka1,2

[0093] In some embodiments, the actual intensity I S,测定 and the actual intensity of SO3Ka1,2 the actual intensity I S,实际 and the actual intensity of SO3Ka1,2 In the above,

[0094] The overlap coefficient between the SKa1,2 and the SO3Ka1,2 includes: the overlap coefficient of the SKa1,2 to the SO3Ka1,2 and the overlap coefficient of the SO3Ka1,2 to the SKa1,2

[0095] The actual intensity I of the SKa1,2 S,实际 and the overlap coefficient between the SKa1,2 and the SO3Ka1,2, the measured intensity I of the SKa1,2 S,测定 The relationship satisfies:

[0096] The actual intensity of the SO3Ka1,2 and the overlap coefficient between the SKa1,2 and the SO3Ka1,2, the measured intensity of the SO3Ka1,2 The relationship satisfies: Wherein, the overlap coefficient of the SKa1,2 to the SO3Ka1,2 The overlap coefficient of the SO3Ka1,2 to the SKa1,2

[0097] S6. According to the sulfide working curve and the actual intensity I of the SKa1,2 S,实际 , the content of sulfide is obtained;

[0098] S7. According to the sulfate working curve and the actual intensity of the SO3Ka1,2 The content of sulfate is obtained.

[0099] It should be noted that the present method is suitable for the determination of the content of sulfide (calculated as S) and sulfate (calculated as SO3) in steel slag and slag-based full solid waste cementitious materials, the determination range of sulfide is 0.4% to 1.3%, and the determination range of sulfate is 0.3% to 4.0%.

[0100] The detection method of sulfide and sulfate in steel slag and slag-based full solid waste cementitious materials of the present application will be described in detail below in combination with examples, control examples and experimental data.

[0101] Examples

[0102] A detection method of sulfide and sulfate in a steel slag and slag-based full solid waste cementitious material, the method comprising:

[0103] Step 1: Prepare the steel slag and slag-based full solid waste cementitious material sample according to the requirements of GB / T 176-2017, and the sample is passed through a 200 mesh sieve.

[0104] Step 2: Take about 7g of the sample with a particle size greater than 200 mesh, place it in a steel ring padded with boric acid, and keep it under a pressure of 25t to 30t for 10s to 20s to prepare a powder tablet for measurement.

[0105] Step 3: The samples were determined by using X fluorescence spectrometer according to the analysis conditions in Table 2 to obtain the determination intensity of samples SKa1,2 and SO3Ka1,2.

[0106] Step 4: The actual intensity of samples SKa1,2 and SO3Ka1,2 was calculated by using formula and .

[0107] Step 5: The content of sulfide (calculated as S) and sulfate (calculated as SO3) in the sample was calculated according to the established working curve.

[0108] Comparative Example 1

[0109] Barium sulfate gravimetric method and high-frequency infrared absorption method in GB / T 176-2017

[0110] Experimental Example

[0111] The method provided by the embodiment and the comparative example was respectively used to determine three steel slag and slag-based full solid waste cementitious material samples (i.e., cement 1#, cement 2# and cement 3#) produced by Shougang, and the determination results are shown in Table 5 and Table 6.

[0112] Table 5 Determination results of sulfate (calculated as SO3) of full solid waste cementitious material produced by Shougang

[0113]

[0114] Table 6 Determination results of sulfide (calculated as S) of full solid waste cementitious material produced by Shougang

[0115]

[0116]

[0117] *Note: This calculated value is equal to the average value of total sulfur determined by the infrared absorption method minus the average value of sulfate (calculated as S) determined by the barium sulfate gravimetric method.

[0118] As shown in Table 5, the precision of sulfate determination by the method of the present application is better than that of the barium sulfate gravimetric method in GB / T 176-2017; the average error of sulfate determination is within 0.2%, while the reproducibility R of the chemical analysis method provided by GB / T 176-2017 is 0.2%, indicating that the accuracy of sulfate determination by the method of the present application can meet the analysis requirements.

[0119] From table 6, it can be obtained that the precision of determining sulfide by the method of the present application is equivalent to the precision of determining sulfide by the chemical analysis method provided by GB / T 176-2017, SD=0.011%; the average error of sulfide is within 0.05%, while the reproducibility of determining sulfide by the chemical analysis method provided by GB / T 176-2017 is R=0.05%, which indicates that the accuracy of determining sulfide by the method of the present application can also meet the analysis requirements.

[0120] The one or more technical solutions in the embodiments of the present application have at least the following technical effects or advantages:

[0121] The method provided by the embodiments of the present application shortens the analysis period to within 1h, and can simultaneously detect the content of sulfide and sulfate in the sample, greatly improving the analysis efficiency.

[0122] Finally, it should be noted that the terms "comprising", "containing" or any other variant thereof are intended to cover non-exclusive inclusion, so that the process, method, article or equipment including a series of elements not only includes those elements, but also includes other elements not explicitly listed or inherent to such process, method, article or equipment.

[0123] Although the preferred embodiments of the present application have been described, those skilled in the art can make further changes and modifications to the embodiments once they know the basic inventive concept. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications falling within the scope of the present application.

[0124] Obviously, those skilled in the art can make various modifications and variations to the present application without departing from the spirit and scope of the present application. Thus, if these modifications and variations of the present application fall within the scope of the claims of the present application and their equivalent technologies, the present application also intends to include these modifications and variations.

Claims

1. A method for detecting sulfides and sulfates in a steel slag and slag-based full-solid-waste cementitious material, characterized by, The method comprises: obtaining an overlapping coefficient between SKa1,2 and SO3Ka1,2; obtaining a sulfide working curve and a sulfate working curve; obtaining a sample to be tested; The sample to be measured is subjected to X fluorescence spectrometer to obtain the measured intensity I of SKa1,2 S,测定 and the measured intensity of SO3Ka1,2 According to the overlap coefficient between SKa1 2 and SO3Ka1 2, the measured intensity I of SKa1 2 S,测定 and the measured intensity of SO3Ka1 2 the actual intensity I of SKa1 2 S,实际 and the actual intensity of SO3Ka1 2 According to the sulfide working curve and the actual intensity I of SKa1,2 S,实际 , the content of sulfide is obtained; According to the sulfate working curve and the actual intensity of SO3Ka1,2 The content of sulfate is obtained; The method comprises: obtaining a first sample and a second sample, wherein the sulfur in the first sample exists in the form of sulfide, and the sulfur in the second sample exists in the form of sulfate; performing X fluorescence spectrum scanning analysis on the first sample and the second sample to obtain 2θ angles of SKa1,2 and SO3Ka1,2; performing multiple X fluorescence spectrum scanning analysis on the first sample and the second sample according to the 2θ angles of SKa1,2 and SO3Ka1,2 to obtain an overlapping coefficient between SKa1,2 and SO3Ka1,2; The first sample is a blast furnace slag sample with a SO3 content less than 0.05%, and the second sample is a blast furnace slag sample after being calcined at 900-1000℃ for 32-40h. the measured intensity I of SKa1,2 S,测定 and the measured intensity of SO3Ka1,2 the actual intensity I of SKa1,2 S,实际 and the actual intensity of SO3Ka1,2 in which, The overlap coefficients between the SKa1 2and the SO3Ka1 2include: an overlap coefficient of the SKa1 2against the SO3Ka1 2 and an overlap coefficient of the SO3Ka1 2against the SKa1 2 the actual intensity I of SKa1 2 S,实际 the overlap coefficient between SKa1 2 and SO3Ka1 2, the measured intensity I of SKa1 2 S,测定 the relationship is satisfied: the actual intensity of SO3Ka1 2 the relationship between the overlap coefficient between SKa1 2 and SO3Ka1 2 and the measured intensity of SO3Ka1 2 the relationship between the overlap coefficient between SKa1 2 and SO3Ka1 2 and the measured intensity of SO3Ka1 2 the overlap coefficient of SO3Ka1 2 to SKa1 2 the overlap coefficient of SO3Ka1 2 to SKa1 2 The detection range of the method comprises a sulfide detection range and a sulfate detection range, wherein the sulfide detection range is 0.4%-1.3%, and the sulfate detection range is 0.3%-4.0%.

2. The method according to claim 1, characterized in that, The method comprises: obtaining a plurality of calibration samples; performing infrared carbon-sulfur analyzer determination on the plurality of calibration samples to obtain total sulfur contents of the calibration samples; performing barium sulfate gravimetric method determination on the plurality of calibration samples to obtain sulfate contents of the calibration samples; obtaining sulfide contents of the calibration samples through the total sulfur contents and the sulfate contents of the calibration samples; performing X fluorescence spectrometer determination on the plurality of calibration samples to obtain determination intensities of SKa1,2 of the calibration samples and determination intensities of SO3Ka1,2 of the calibration samples; obtaining actual intensities of SKa1,2 of the calibration samples and actual intensities of SO3Ka1,2 of the calibration samples according to the overlapping coefficient between SKa1,2 and SO3Ka1,2, the determination intensities of SKa1,2 of the calibration samples, and the determination intensities of SO3Ka1,2 of the calibration samples; obtaining a sulfate working curve according to the sulfate contents of the calibration samples and the actual intensities of SO3Ka1,2 of the calibration samples; obtaining a sulfide working curve according to the sulfide contents of the calibration samples and the actual intensities of SKa1,2 of the calibration samples.

3. The method according to claim 2, characterized in that, The calibration samples are blast furnace slag and steel slag and mineral slag-based full solid waste cementitious materials, and the sulfur in the blast furnace slag and steel slag and mineral slag-based full solid waste cementitious materials exists in the forms of sulfide and sulfate.

4. The method according to claim 1, characterized in that, The method comprises: obtaining a material to be tested, performing tabletting to obtain a sample to be tested.

5. The method according to claim 4, characterized in that, The particle size of the material to be tested is greater than 200 mesh, the pressure of the tabletting is 25-30t, and the pressure holding time of the tabletting is 10-20s.

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