Method for determining silicon dioxide in quartzite

Abstract

The invention relates to the technical field of detection methods, in particular to a method for determining silicon dioxide in quartzite, which comprises the following steps: preparing a test sample; establishing a standard curve; determining the SiO2 content of a sample to be detected; and establishing a correction point. The standard curve of the linear relation between the Si element emission peak intensity and the silicon dioxide content is constructed based on the X-ray fluorescence spectrum technology, and the silicon dioxide content in the to-be-detected sample can be rapidly obtained through the Si element emission peak intensity in the to-be-detected sample; and the calibration sample tablet is regularly introduced to dynamically calibrate the instrument, so that the problem of signal drift in long-term operation of the spectrograph is effectively solved, and the stability and the reliability of detection data are guaranteed. According to the method, the single-time detection time is shortened, the relative error and the relative standard deviation of the repeatability of the detection result are both smaller than 0.25%, and efficient and accurate technical guarantee is provided for quartz stone raw material quality control and copper smelting process optimization.

Description

Technical Field

[0001] The present invention relates to the technical field of detection methods, and in particular to a method for determining silicon dioxide in quartz stone. Background Art

[0002] In industrial production processes such as quartz raw material testing and copper smelting, accurate determination of silica content is crucial for furnace control, process optimization, and product quality control. The nonferrous industry standard for quartz analysis is YB / T4225-2010, which involves decomposing the sample with hydrofluoric acid and nitric acid, removing silicon and fluorine with sulfuric acid fumes, and then burning it at high temperature to constant weight. The silica content is determined by the difference in mass before and after the hydrofluoric acid treatment. This standard requires two burnings of the solid sample, both to a constant weight, resulting in a lengthy testing process and the use of a platinum crucible, which corrodes precious metal vessels and increases testing costs. Summary of the Invention

[0003] In order to solve the problems of high testing cost and long experimental process in the above-mentioned prior art, the present invention provides a method for determining silicon dioxide in quartz stone.

[0004] To achieve the above object, the technical solution of the present invention is as follows:

[0005] A method for determining silicon dioxide in quartz stone comprises the following steps:

[0006] S1. Preparation of test samples: Using starch as a binder, the starch and sample are placed in a grinding and sample preparation machine for grinding and mixing, the mixed sample is placed in a mold, and the sample is prepared into a sample tablet using a sample pressing machine;

[0007] S2. Establishing a standard curve: Prepare multiple standard sample tablets with determined SiO2 content values ​​according to step S1, place them in an X-ray fluorescence spectrometer, test them according to the characteristic spectrum of the Si element, and establish a standard curve; the abscissa of the standard curve is the SiO2 content, and the ordinate is the Si element emission peak intensity;

[0008] S3. Determination of SiO2 content in the sample to be tested: Prepare a sample to be tested pellet according to step S1, place it in an X-ray fluorescence spectrometer, and test it according to the characteristic spectrum of the Si element to obtain the element emission peak intensity of Si in the sample to be tested. Substitute the element emission peak intensity of Si in the sample to be tested into the standard curve obtained in step S2, and calculate the SiO2 content in the sample to be tested according to the standard curve;

[0009] S4. Calibration point establishment: Prepare a calibration sample pressed tablet with a determined SiO2 content value according to step S1, place it in the X-ray fluorescence spectrometer, and test it according to the characteristic spectrum of the Si element to obtain a calibration point corresponding to the SiO2 content value and the Si element emission peak intensity. Regularly use this calibration point to calibrate the test value of the X-ray fluorescence spectrometer.

[0010] Furthermore, in S1, the mass ratio of the sample to the binder is 8-10:1; the mass of the sample placed in the film mold for tableting is 5-6 g, and the particle size of the sample is less than 0.25 mm.

[0011] Furthermore, in S1, the grinding time is 45-60s, the pressure of the sample pressing machine is 30-35t, and the sample pressing time is 45-60s.

[0012] Furthermore, in S2, the number of prepared standard sample tablets is greater than or equal to 8, and the silicon dioxide content in the standard sample is 84-95%.

[0013] Furthermore, in S2-S4, the operating parameters of the X-ray fluorescence spectrometer are analysis line Kα, 2θ=109.08°, analysis crystal PE002, 300 μm collimator, current 100 mA, voltage 30 kV, and power 3000 kW.

[0014] Compared with the prior art, the present invention has the following beneficial effects:

[0015] The present invention provides a method for determining silicon dioxide in quartz stone, which uses starch as a binder, and the binder is a hydrocarbon, which will not cause interference during the test process. Based on X-ray fluorescence spectroscopy technology, a standard curve of the linear relationship between the emission peak intensity of the Si element and the silicon dioxide content is constructed, which can quickly obtain the silicon dioxide content in the sample to be tested through the emission peak intensity of the Si element in the sample to be tested; regularly introducing calibration sample tablets to dynamically calibrate the instrument, effectively solving the signal drift problem in the long-term operation of the spectrometer, and ensuring the stability and reliability of the test data. This method has a short single detection time, a simple detection process, and a low detection cost, and the repeatability relative error and relative standard deviation of the test results are both less than 0.25%, providing efficient and accurate technical guarantees for the quality control of quartz stone raw materials and the optimization of copper smelting processes. DETAILED DESCRIPTION

[0016] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below through specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0017] A method for determining silicon dioxide in quartz stone comprises the following steps:

[0018] S1. Preparation of test samples: Using starch as a binder, the starch and sample are placed in a grinding and sample preparation machine for grinding and mixing, the mixed sample is placed in a mold, and the sample is prepared into a sample tablet using a sample pressing machine;

[0019] S2. Establishing a standard curve: Prepare multiple standard sample tablets with determined SiO2 content values ​​according to step S1, place them in an X-ray fluorescence spectrometer, test them according to the characteristic spectrum of the Si element, and establish a standard curve; the abscissa of the standard curve is the SiO2 content, and the ordinate is the Si element emission peak intensity;

[0020] S3. Determination of SiO2 content in the sample to be tested: Prepare a sample to be tested pellet according to step S1, place it in an X-ray fluorescence spectrometer, and test it according to the characteristic spectrum of the Si element to obtain the element emission peak intensity of Si in the sample to be tested. Substitute the element emission peak intensity of Si in the sample to be tested into the standard curve obtained in step S2, and calculate the SiO2 content in the sample to be tested according to the standard curve;

[0021] S4. Calibration point establishment: Prepare a calibration sample pressed tablet with a determined SiO2 content value according to step S1, place it in the X-ray fluorescence spectrometer, and test it according to the characteristic spectrum of the Si element to obtain a calibration point corresponding to the SiO2 content value and the Si element emission peak intensity. Regularly use this calibration point to calibrate the test value of the X-ray fluorescence spectrometer.

[0022] In one embodiment of the present invention, in S1, the mass ratio of the sample to the binder is 8-10:1; the mass of the sample placed in the mold for tableting is 5-6 g, and the particle size of the sample is less than 0.25 mm.

[0023] In one embodiment of the present invention, in S1, the grinding time is 45-60s, the pressure of the sample pressing machine is 30-35t, and the sample pressing time is 45-60s.

[0024] In one embodiment of the present invention, in S2, the number of prepared standard sample tablets is greater than or equal to 8, and the silicon dioxide content in the standard sample is 84-95%.

[0025] In one embodiment of the present invention, in S2-S4, the operating parameters of the X-ray fluorescence spectrometer are analysis line Kα, 2θ=109.08°, analysis crystal PE002, 300μm collimator, current 100mA, voltage 30kV, and power 3000kW.

[0026] Example 1: Tablet sample quality selection

[0027] Starch was used as a binder. The starch and sample were ground and mixed in a grinding machine. Samples of varying weights were weighed and placed in a mold. The samples were then pressed into tablets using a pressing machine. Experimental data for samples of varying weights, tablet state, and sample thickness are shown in Table 1.

[0028] Table 1

[0029] Sample mass (g) Sample compression status Sample pressing thickness (mm) 3 The sample is pressed out of the pit and separated from the membrane, and cannot be formed into a sheet 3 4 The sample is separated from the film, has cracks, and cannot be formed into a sheet 3.5 5 The sample is pressed smoothly and can be sliced 4.5 6 The sample is pressed smoothly and can be sliced 5 7 The sample tablet is slightly sludged and can be sliced 5

[0030] As can be seen from Table 1, the sample mass required to prepare the sample tablets is 5-6 g.

[0031] Example 2: Standard curve establishment

[0032] S1. Preparation of test samples: Using starch as a binder, the starch and sample are placed in a grinding and sample preparation machine for grinding and mixing, the mixed sample is placed in a mold, and the sample is prepared into a sample tablet using a sample pressing machine;

[0033] S2. Standard Curve Creation: 11 standard sample tablets with defined SiO2 content values ​​were prepared according to step S1. These tablets were placed in an X-ray fluorescence spectrometer and tested according to the characteristic Si element spectrum to create a standard curve. The abscissa of the standard curve represents the SiO2 content, and the ordinate represents the Si element emission peak intensity. Table 2 shows the SiO2 content in the standard samples.

[0034] Table 2

[0035] Standard sample number <![CDATA[SiO2 content (%)]]> <![CDATA[1 # ]]> 84.06 <![CDATA[2 # ]]> 85.77 <![CDATA[3 # ]]> 88.88 <![CDATA[4 # ]]> 90.05 <![CDATA[5 # ]]> 91.35 <![CDATA[6 # ]]> 91.86 <![CDATA[7 # ]]> 93.25 <![CDATA[8 # ]]> 93.70 <![CDATA[9 # ]]> 94.46 <![CDATA[10 # ]]> 95.45 <![CDATA[11 # ]]> 95.67

[0036] Example 3: Accuracy Test

[0037] S1. Preparation of test samples: Using starch as a binder, the starch and sample are placed in a grinding and sample preparation machine for grinding and mixing, the mixed sample is placed in a mold, and the sample is prepared into a sample tablet using a sample pressing machine;

[0038] S2. Establishing a standard curve: Select the 11 standard samples in Example 2, prepare standard sample tablets with determined SiO2 content values ​​according to step S1, place them in an X-ray fluorescence spectrometer, test them according to the characteristic spectrum of the Si element, and establish a standard curve; the abscissa of the standard curve is the SiO2 content, and the ordinate is the Si element emission peak intensity;

[0039] S3. Determination of SiO2 content in the sample to be tested: Select 3 # , 6 # and 8 #The standard sample was used as the test sample. The test sample pellet was prepared according to step S1 and placed in an X-ray fluorescence spectrometer. The test was performed according to the characteristic spectrum of the Si element. Eleven parallel measurements were performed to obtain the elemental emission peak intensity of Si in the test sample. The elemental emission peak intensity of Si in the test sample was then incorporated into the calibration curve obtained in step S2. The SiO2 content in the test sample was then calculated based on the calibration curve. Table 3 shows the test value, standard value, relative error, and relative standard deviation of the test sample.

[0040] Table 3

[0041]

[0042] As shown in Table 3, the relative error and relative standard deviation of SiO2 tested by the present invention are both less than 0.25%, with good precision, meeting the detection requirements of the sample.

[0043] Example 4: Actual sample testing

[0044] S1. Preparation of test samples: Using starch as a binder, the starch and sample are placed in a grinding and sample preparation machine for grinding and mixing, the mixed sample is placed in a mold, and the sample is prepared into a sample tablet using a sample pressing machine;

[0045] S2. Establishing a standard curve: Prepare multiple standard sample tablets with determined SiO2 content values ​​according to step S1, place them in an X-ray fluorescence spectrometer, test them according to the characteristic spectrum of the Si element, and establish a standard curve; the abscissa of the standard curve is the SiO2 content, and the ordinate is the Si element emission peak intensity;

[0046] S3. Determination of SiO2 content in the sample to be tested: Prepare a sample pellet according to step S1, place it in an X-ray fluorescence spectrometer, and test it according to the characteristic spectrum of the Si element to obtain the elemental emission peak intensity of Si in the sample to be tested. This elemental emission peak intensity of Si in the sample to be tested is then inserted into the standard curve obtained in step S2. The SiO2 content in the sample to be tested can then be calculated based on the standard curve. Table 4 shows the difference between the test values ​​obtained by this method and those obtained by other companies.

[0047] Table 4

[0048] Sample number Test data of this method (%) Test data of Beijing Institute of Mining (%) Difference (%) SYS-1 92.37 92.05 0.35 SYS-2 89.59 89.44 0.15 SYS-3 91.87 91.90 -0.03 SYS-4 94.36 94.60 -0.24

[0049] As shown in Table 5, the difference between the test results of this method and those of other companies is within a reasonable range, and the test results of this method can be widely recognized.

[0050] The present invention provides a method for determining silicon dioxide in quartz stone, which uses starch as a binder, and the binder is a hydrocarbon, which will not cause interference during the test process. Based on X-ray fluorescence spectroscopy technology, a standard curve of the linear relationship between the emission peak intensity of the Si element and the silicon dioxide content is constructed, which can quickly obtain the silicon dioxide content in the sample to be tested through the emission peak intensity of the Si element in the sample to be tested; regularly introducing calibration sample tablets to dynamically calibrate the instrument, effectively solving the signal drift problem in the long-term operation of the spectrometer, and ensuring the stability and reliability of the test data. This method has a short single detection time, a simple detection process, and a low detection cost, and the repeatability relative error and relative standard deviation of the test results are both less than 0.25%, providing efficient and accurate technical guarantees for the quality control of quartz stone raw materials and the optimization of copper smelting processes.

[0051] Some exemplary embodiments of the present invention are described above. It will be understood that the above embodiments are only used to explain the present invention and do not constitute a limitation on the scope of protection of the present invention. The features in these embodiments can be recombined in an appropriate manner, and the solutions obtained thereby are still within the scope of protection claimed by the present invention. Based on the above embodiments, all other embodiments obtained by those skilled in the art without making creative work, that is, all modifications, equivalent substitutions and improvements made within the spirit and principles of this application, fall within the scope of protection claimed by the present invention.

Claims

1. A method for determining silicon dioxide in quartz stone, characterized in that: The following steps are involved: S1. Preparation of test samples: Using starch as a binder, the starch and sample are placed in a grinding and sample preparation machine for grinding and mixing, the mixed sample is placed in a mold, and the sample is prepared into a sample tablet using a sample pressing machine; S2. Establishing a standard curve: Prepare multiple standard sample tablets with determined SiO2 content values ​​according to step S1, place them in an X-ray fluorescence spectrometer, test them according to the characteristic spectrum of the Si element, and establish a standard curve; the abscissa of the standard curve is the SiO2 content, and the ordinate is the Si element emission peak intensity; S3. Determination of SiO2 content in the sample to be tested: Prepare a sample to be tested pellet according to step S1, place it in an X-ray fluorescence spectrometer, and test it according to the characteristic spectrum of the Si element to obtain the element emission peak intensity of Si in the sample to be tested. Substitute the element emission peak intensity of Si in the sample to be tested into the standard curve obtained in step S2, and calculate the SiO2 content in the sample to be tested according to the standard curve; S4. Calibration point establishment: Prepare a calibration sample pressed tablet with a determined SiO2 content value according to step S1, place it in the X-ray fluorescence spectrometer, and test it according to the characteristic spectrum of the Si element to obtain a calibration point corresponding to the SiO2 content value and the Si element emission peak intensity. Regularly use this calibration point to calibrate the test value of the X-ray fluorescence spectrometer.

2. The method for determining silicon dioxide in quartz stone according to claim 1, wherein: In S1, the mass ratio of the sample to the binder is 8-10:1; the mass of the sample placed in the film mold for tableting is 5-6 g, and the particle size of the sample is less than 0.25 mm.

3. The method for determining silicon dioxide in quartz stone according to claim 1, wherein In S1, the grinding time is 45-60s, the pressure of the sample press is 30-35t, and the sample pressing time is 45-60s.

4. The method for determining silicon dioxide in quartz stone according to claim 1, wherein: In S2, the number of prepared standard sample tablets is greater than or equal to 8, and the silicon dioxide content in the standard sample is 84-95%.

5. The method for determining silicon dioxide in quartz stone according to claim 1, wherein: In S2-S4, the operating parameters of the X-ray fluorescence spectrometer are analysis line Kα, 2θ=109.08°, analysis crystal PE002, 300 μm collimator, current 100 mA, voltage 30 kV, and power 3000 kW.

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