Method for detecting silicon dioxide, calcium oxide and magnesium oxide in fly ash
The detection method combining glass fusion method and X-ray fluorescence spectrometry solves the problems of slow detection speed and insufficient sample in existing technologies for silica, calcium oxide and magnesium oxide in dust, and achieves rapid and accurate detection results.
Patent Information
- Application Number
- CN202511637594.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-10
- Publication Date
- 2026-02-03
AI Technical Summary
Existing technologies for detecting silica, calcium oxide, and magnesium oxide in dust collectors suffer from method mismatch, resulting in slow analysis speeds and a lack of standard samples, which affects detection efficiency and accuracy.
The glass fusion method combined with X-ray fluorescence spectrometry was used to prepare glass slides by high-temperature calcination of dust removal ash. The X-ray fluorescence intensity of silicon, calcium, and magnesium was measured using X-ray fluorescence spectrometry, and the elemental content was calculated by combining the calibration curves.
It enables rapid and accurate detection of the content of silicon dioxide, calcium oxide, and magnesium oxide in dust collector ash, simplifies the operation process, and meets production needs.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the technical field of detection and analysis of the content of silicon dioxide, calcium oxide and magnesium oxide in dust ash, and particularly relates to a detection method for silicon dioxide, calcium oxide and magnesium oxide in dust ash. BACKGROUND
[0002] Dust ash can be used as a substitute for iron ore and sintered ore and is added into sintered ore for recycling. In ironmaking production, the content of calcium oxide, magnesium oxide, total iron, potassium, sodium, zinc and other items in gravity ash, cyclone ash, bag dust and other dust ash needs to be determined periodically, and the detection results are increasingly valued by ironmaking plants. For the determination of silicon dioxide, calcium oxide and magnesium oxide in dust ash, mainly the methods such as spectrophotometry, volumetry and ICP spectrometry are used for determination, and there are problems such as mismatch between the method and the content of the measured substance, the need for multiple methods for joint determination, slow analysis speed, and few standard samples of dust ash on the market, which brings inconvenience to daily detection.
[0003] The present application is aimed at the characteristics of on-site dust ash, and determines SiO2, CaO and MgO therein. The sample is carbon-free by high-temperature calcination, and is prepared into a glass sheet by melting. The analysis principle and performance of the X-ray fluorescence spectrometer are fully mastered, and dust ash quality control samples are self-made to draw a calibration curve. The determination of SiO2, CaO and MgO in dust ash is completed by determining the X-ray fluorescence intensity of silicon, calcium and magnesium of the molten glass sheet. The method is simple in operation, short in process, accurate in result, and can more scientifically guide production. SUMMARY
[0004] The purpose of the present application is a detection method for determining silicon dioxide, calcium oxide and magnesium oxide in dust ash by glass melting sheet method-X-ray fluorescence spectrometer. The analysis method is simple and easy to master, the analysis speed is fast, and the on-site production needs are met.
[0005] To solve the above technical problems, the present application adopts the following technical solutions:
[0006] The present application is a detection method for determining silicon dioxide, calcium oxide and magnesium oxide in dust ash, comprising the following steps:
[0007] (1) 0.9g-1.1g of dust ash sample is weighed, placed in an ash dish and flattened, and is calcined at 650℃±10℃ for 2h to remove carbon, and the burning loss rate k is calculated;
[0008] (2) 7.000g of mixed flux is weighed to 0.0005g, and is placed in a porcelain crucible or glass dish; then 0.500g of the calcined sample is accurately weighed and placed in the porcelain crucible or glass dish, and is accurately weighed to 0.0002g, and is fully stirred with a glass rod, and is then transferred into a yellow-white gold crucible, and 1-2mL of ammonium iodide solution is dropped;
[0009] (3) In the melting furnace at 1050±10℃, the melting time is 110-130s for pre-melting, 690-750s for swinging, and the sample is cooled and demolded to prepare the glass sheet to be measured;
[0010] (4) The prepared glass sheet sample to be measured is placed in the sample box of the X fluorescence spectrometer, and the X-ray fluorescence intensity of silicon, calcium and magnesium is measured under the set instrument analysis parameters, and the content is obtained by linear regression, multiplied by the burn loss rate, and the content of each element in the sample is obtained.
[0011] Further, the mixed flux is specifically LiB4O7:LiBO2=67:33.
[0012] Further, the particle size of the fly ash sample in step (1) is 0.075mm.
[0013] Further, the sample after calcination is weighed to the constant weight, and the burn loss rate is calculated, and the burn loss rate k=the mass of the sample after calcination / the mass of the sample before calcination.
[0014] Further, the surface of the glass sheet sample to be measured in step (3) is free of bubbles, cracks and crystallization.
[0015] Further, the X fluorescence spectrometer in step (4) is an X fluorescence spectrometer provided with a scanning channel or a fixed channel of silicon, calcium and magnesium.
[0016] Further, the calibration work curve in step (4) is obtained by using steps (1)-(4), selecting five standard samples with content gradient, and selecting the same type of fly ash control sample, and drawing the calibration work curve of the content of the analyzed elements in the standard sample and the control sample and the X-ray fluorescence intensity, so as to obtain the content of the analyzed elements in the sample to be measured.
[0017] Further, the content of silicon dioxide, calcium oxide and magnesium oxide in the fly ash is calculated by the calibration work curve; according to the drawn calibration work curve, the content of silicon dioxide, calcium oxide and magnesium oxide in the fly ash is obtained, and the content of each component is multiplied by the burn loss rate to obtain the final result of silicon dioxide, calcium oxide and magnesium oxide in the fly ash to be measured.
[0018] Compared with the prior art, the beneficial technical effects of the present application are:
[0019] (1) Before the fly ash sample is melted, the carbon is removed by calcining at 650℃±10℃ for 2h, and the burn loss rate is calculated, so that the carbon can be removed at a suitable temperature and time, and the sample is not easy to be melted due to too high temperature.
[0020] (2) In drawing the calibration work curve, the standard sample and the self-made quality control sample are combined to draw the curve, the matrix effect is reduced, and the problem of lack of on-site fly ash standard sample is solved.
[0021] (3) The glass fusion piece-X fluorescence spectrum method is used to accurately determine the contents of silicon dioxide, calcium oxide and magnesium oxide in fly ash, and the determination range can meet the on-site requirements. DETAILED DESCRIPTION
[0022] The technical solutions of the present application are further described below in combination with examples, so that those skilled in the art can further understand the present application, and the present application is not limited by the rights.
[0023] Example 1: A detection method for silicon dioxide, calcium oxide and magnesium oxide in fly ash, the actual operation is as follows:
[0024] 1. 0.9g-1.1g of fly ash sample (particle size 0.075mm) was weighed in a crucible that had been calcined to constant weight, and was calcined in a muffle furnace at 650±10℃ for 2h. After cooling, it was weighed and the loss on ignition was calculated. Loss on ignition = mass of sample after ignition / mass of sample before ignition.
[0025] 2. 7.000g of mixed flux (Li B4O7:LiBO2=67:33) was accurately weighed to 0.0005g and placed in a porcelain crucible (glass dish). Then 0.5000g of the calcined sample was accurately weighed and placed in the porcelain crucible (glass dish). A glass rod was used to mix thoroughly, and then it was transferred to a yellow-white gold crucible. 1-2mL of ammonium iodide (50%) was added dropwise.
[0026] 3. The fusion piece was melted in a 1050℃ melting furnace. The melting time was pre-melting for 120s, swinging for 720s, and standing for 10s. After the melting was completed, the melting furnace was opened, the yellow-white gold crucible was taken out, the molten material was shaken evenly, and then it was placed to cool and demolded.
[0027] 4. The prepared glass piece without air bubbles, cracks or crystals was placed in an X-ray fluorescence spectrometer sample box with a scanning channel or a silicon, calcium and magnesium fixed channel. The X-ray fluorescence intensity was measured under the set instrument analysis parameters.
[0028] 5. According to different content gradients, 12 standard samples and 6 different types of fly ash control samples were selected. According to steps 1, 2, 3 and 4, the measured silicon, calcium and magnesium X-ray fluorescence intensity was taken as the ordinate, and the contents of silicon dioxide, calcium oxide and magnesium oxide were taken as the abscissa. The calibration work curve was drawn, and the calculation formula was obtained.
[0029] 6. According to the drawn calibration working curve, the content of silicon dioxide, calcium oxide and magnesium oxide in the fly ash is obtained, and the final result is multiplied by the burning loss rate to obtain the content of silicon dioxide, calcium oxide and magnesium oxide in the fly ash sample to be measured.
[0030] 7. The standard sample and the fly ash sample are analyzed, and the results are close to the standard value and the chemical method. The content of silicon dioxide, calcium oxide and magnesium oxide in the fly ash is determined by the patent, and the result is accurate. The specific detection data is shown in Tables 1 and 2.
[0031] Table 1 Analysis results of iron-containing dust and sludge standard sample
[0032]
[0033] Table 2 Comparison results between methods
[0034]
[0035] The above-described embodiments are only preferred modes of the present application and do not limit the scope of the present application. Various modifications and improvements to the technical solutions of the present application made by those skilled in the art without departing from the design spirit of the present application shall fall within the protection scope of the present application defined by the claims.
Claims
1. A method for detecting silica, calcium oxide, and magnesium oxide in dust collector ash, characterized in that, Includes the following steps: (1) Weigh 0.9g~1.1g of dust sample, spread it in a ash dish, and burn it at 650℃±10℃ for 2h to remove carbon, and calculate the burn-off rate k; (2) Weigh 7.000g of mixed flux, accurate to 0.0005g, and place it in a porcelain crucible or glass dish; then accurately weigh 0.500g of the ignited sample and place it in a porcelain crucible or glass dish, accurate to 0.0002g. Stir it thoroughly with a glass rod, then transfer it to a gold crucible and add 1-2mL of ammonium iodide solution. (3) Melt the sheet in a melting furnace at 1050±10℃. The melting time is 110-130s for pre-melting and 690-750s for shaking. After standing, open the melting furnace, take out the gold crucible, shake the melt evenly, let it cool, demold it, and prepare the glass sheet to be tested. (4) The prepared glass slide sample to be tested is placed in the X-ray fluorescence spectrometer sample box for measurement. Under the set instrument analysis parameters, the X-ray fluorescence intensity of silicon, calcium and magnesium is measured according to the established dust ash calibration working curve. The content is obtained by linear regression and multiplied by the burn-off rate to obtain the content of each element in the sample.
2. The method for detecting silicon dioxide, calcium oxide, and magnesium oxide in dust collector ash according to claim 1, characterized in that, The specific mixed flux is: LiB4O7:LiBO2 = 67:
33.
3. The method for detecting silicon dioxide, calcium oxide, and magnesium oxide in dust collector ash according to claim 1, characterized in that, The particle size of the dust sample mentioned in step (1) is 0.075 mm.
4. The method for detecting silicon dioxide, calcium oxide, and magnesium oxide in dust collector ash according to claim 1, characterized in that, The sample after ignition must reach a constant weight, and the burn loss rate must be calculated. The burn loss rate k = mass of the sample after ignition / mass of the sample before ignition.
5. The method for detecting silicon dioxide, calcium oxide, and magnesium oxide in dust collector ash according to claim 1, characterized in that, The glass sample to be tested in step (3) must be free of bubbles, cracks and crystals on its surface.
6. The method for detecting silica, calcium oxide, and magnesium oxide in dust collector ash according to claim 1, characterized in that, The X-ray fluorescence spectrometer mentioned in step (4) is an X-ray fluorescence spectrometer equipped with a scanning channel or a fixed channel for silicon, calcium, or magnesium.
7. The method for detecting silicon dioxide, calcium oxide, and magnesium oxide in dust collector ash according to claim 1, characterized in that, The calibration curve described in step (4) is obtained by using steps (1)-(4), selecting five standard samples with content gradients, and selecting control samples of the same type of dust ash, plotting the relationship between the content of the analytical element in the standard samples and control samples and the X-ray fluorescence intensity to obtain the content of the analytical element in the sample to be tested.
8. The method for detecting silica, calcium oxide, and magnesium oxide in dust collector ash according to claim 1, characterized in that, The content of silicon dioxide, calcium oxide, and magnesium oxide in the dust is calculated by using a calibration working curve. Based on the drawn calibration working curve, the content of silicon dioxide, calcium oxide, and magnesium oxide in the dust is obtained. The content of each component multiplied by the burn-off rate is the final result of silicon dioxide, calcium oxide, and magnesium oxide in the dust to be tested.