Method for measuring calcium, silicon and magnesium in quick lime by X-ray fluorescence with ignition loss correction

Abstract

The invention relates to the technical field of chemical detection, in particular to a method for measuring calcium, silicon and magnesium in quicklime through X-ray fluorescence with ignition loss correction, which comprises the following steps: preparing and drying a sample, burning the sample, calculating the amount of burning loss, fusing the sample, establishing an X-ray fluorescence detection method and setting detection conditions. The method comprises the following steps: establishing a working curve of X-ray fluorescence detection of quicklime, calibrating the working curve of X-ray fluorescence, carrying out ignition loss correction on a quicklime sample by an X-ray fluorescence method to obtain the content of the sample, and verifying the reliability of the working curve of X-ray fluorescence; before melting the glass sheet, the quick lime sample is fired, the ignition loss of the sample is calculated, the detection result is subjected to ignition loss correction calculation, the sample is subjected to glass melting sheet preparation, the content of calcium, silicon and magnesium is measured at one time by using the X-ray fluorescence spectrometry, chemical reagents and participated instruments are saved, the production cost is reduced, and the method is suitable for industrial production. The environmental pollution is reduced, and the production efficiency, accuracy and reliability are improved.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical detection, and particularly to a method for determining calcium, silicon and magnesium in quicklime by X-ray fluorescence with loss-on-ignition correction. Background Art

[0002] Quicklime is a widely used industrial raw material, and its uses include steelmaking, construction, agriculture, etc. Its main components are calcium oxide CaO, silicon dioxide SiO 2 and magnesium oxide MgO. It is characterized by being easy to absorb moisture in the air and containing a certain amount of loss-on-ignition component.

[0003] The existing technologies for detecting the contents of calcium, silicon and magnesium in quicklime: The national standard "GB / T5762-2024 Chemical analysis methods for limestone, quicklime and hydrated lime for building materials". This standard uses the EDTA titration method (for determining calcium oxide CaO), ammonium chloride NH 4 Cl gravimetric method (for determining silicon dioxide SiO 2 ) and atomic absorption spectrophotometry (for determining magnesium oxide MgO) to detect the main components in quicklime respectively. The above methods have a long detection period, use a lot of chemical reagents, require the participation of a variety of instruments, and one method can only detect one component, which requires a large amount of manpower and material resources.

[0004] Existing method 1: EDTA titration method (for determining calcium oxide CaO): In a strongly alkaline solution with a pH above 13, using triethanolamine as a masking agent, with a calcein-methyl thymol blue-phenolphthalein mixed indicator (abbreviated as CMP), titrating with an EDTA standard titration solution;

[0005] Existing method 2: Ammonium chloride gravimetric method (for determining silicon dioxide SiO 2 )): The sample is sintered with anhydrous sodium carbonate, dissolved in hydrochloric acid, evaporated to a paste, then solid ammonium chloride is added, evaporated to dryness to coagulate the silicic acid, filtered, calcined and weighed. After treatment with hydrofluoric acid, the lost mass is the content of gelatinous silicon dioxide, and adding the soluble silicon dioxide recovered by colorimetry in the filtrate is the total silicon dioxide content;

[0006] Existing method 3: Atomic absorption spectrometry (for determining magnesium oxide MgO): Preparing a solution by decomposing the sample with hydrofluoric acid-perchloric acid or sodium hydroxide fusion-hydrochloric acid decomposition. Taking a certain amount of the solution, using strontium salt to eliminate the interference of silicon, aluminum, titanium, etc. on magnesium, and measuring the absorbance of the solution at a wavelength of 285.2 nm in an air-acetylene flame.

[0007] Chinese Patent with publication number CN104359931A discloses a method for improving the qualified rate of fluorescence analysis of CaO in limestone. The method mainly requires the storage conditions of limestone standard samples and the maintenance operations of X-ray fluorescence spectrometers to ensure the precision of detection results. This method has certain reference value for quicklime samples with the main component of calcium oxide (CaO).

[0008] Chinese Patent with publication number CN104897511A discloses a method for determining the effective components of desulfurized quicklime. The invention provides a method for determining the effective components of desulfurized quicklime, analyzes and determines the types and contents of decomposable effective components in the desulfurized quicklime sample, then conducts elemental analysis on the undecomposed sample to determine the content of the effective components contained in the undecomposed sample, so as to determine the content of the effective components in the desulfurized quicklime sample; the implementation and setting of the thermogravimetry-infrared detection method are mainly discussed in this method, and the X-ray fluorescence spectrometry is only an auxiliary detection method without detailed implementation description, so the reliability of the method cannot be proved.

[0009] Paper: Liu Jing et al., "Study on the Determination of 5 Components in Quicklime by X-ray Fluorescence Spectrometry", Light Metals 2018, 4: 54 - 56. This method uses the method of converting the loss on ignition of limestone to dry basis to draw the working curve, solves the problem of no standard sample for quicklime, and it is found through experiments that the precision of this method is good; but theoretical calculations show that: when the quicklime sample has a loss on ignition, the measured value calculated theoretically will be on the high side, and when the loss on ignition of the quicklime sample exceeds 10%, it is not suitable to use this method.

[0010] Paper: Qu Yuehua et al., "Determination of 5 Components in Limestone by Fusion Sampling - X-ray Fluorescence Spectrometry", Metallurgical Analysis 2013, 33(12): 29 - 33. This method uses standard samples and artificially prepared calibration samples to jointly draw the calibration curve, does not require burn loss correction for carbonates in limestone, directly melts limestone samples with lithium tetraborate anhydrous flux, and determines the contents of silicon, calcium, magnesium, iron, and aluminum elements in limestone by X-ray fluorescence spectrometry. The detection range of this method is limited to limestone samples with calcium oxide content in the range of 47% - 55% and loss on ignition in the range of 40% - 44%, and it cannot detect quicklime standard samples with higher calcium oxide content and unpredictable loss on ignition.

[0011] Paper: Wei Nan et al., "Application of X-ray Fluorescence Analysis Technology in Limestone Acceptance", Guangdong Chemical Industry, No. 4, 2019. This method improves the tablet pressing method, and realizes the rapid detection of calcium oxide (CaO) and magnesium oxide (MgO) components by making limestone into tablets for fluorescence. Considering that tablet pressing cannot eliminate the influence of mineral effect and particle size effect, the precision and accuracy of its detection results are inferior to those of the fusion method. Summary of the Invention

[0012] The present invention provides a method for determining calcium, silicon, and magnesium in quicklime by X-ray fluorescence with loss-on-ignition correction. A working curve for determining quicklime is established using a standard sample of limestone after calcination. The quicklime sample is calcined before melting into a glass disc, and the loss-on-ignition of the sample is calculated. The detection results are corrected for loss-on-ignition. The sample is made into a glass melt disc, and the contents of calcium, silicon, and magnesium are measured at one time using X-ray fluorescence spectrometry, saving chemical reagents and instruments for detection, reducing production costs, and reducing environmental pollution. The X-ray fluorescence method has a short sample processing time and a fast detection speed, which can improve working conditions and labor productivity. The sample processing method with loss-on-ignition correction can ensure the accuracy and reliability of the X-ray fluorescence detection results of quicklime samples, especially samples with a high loss-on-ignition.

[0013] To achieve the above object, the present invention is implemented by the following technical solutions:

[0014] A method for determining calcium, silicon, and magnesium in quicklime by X-ray fluorescence with loss-on-ignition correction, comprising the following steps:

[0015] S1. Sample preparation and drying;

[0016] S2. Sample calcination treatment and calculation of the loss on ignition;

[0017] S3. Sample disc melting;

[0018] S4. Establish an X-ray fluorescence detection method and set detection conditions;

[0019] S5. Establish a working curve for X-ray fluorescence detection of quicklime: According to the sample disc melt of the standard limestone sample after calcination, measure the fluorescence intensity of each component using the element spectral lines and detection conditions of each element, and establish a working curve for detecting calcium, silicon, and magnesium components according to the following formula,

[0020] W i =(BI i +A));

[0021] wherein, W i is the content of the analyzed element i in the glass disc melt prepared from the standard limestone sample after calcination, %;

[0022] I i is the X-ray intensity of element i, kcps;

[0023] A and B are working curve coefficients;

[0024] At the same time, calculate the linear correlation coefficient of the working curve of each component;

[0025] S6. X-ray fluorescence working curve calibration: Standardize the instrument by measuring the fused tablets of limestone standard samples, correct the instrument drift, which is carried out every 24 h to 48 h or before measuring unknown samples;

[0026] S7. Carry out loss-on-ignition correction on quicklime samples by X-ray fluorescence method to obtain the sample content;

[0027] M i = M ical ×(1 - ωLOI);

[0028] where ω LOI is the loss-on-ignition of the test sample, expressed as %;

[0029] M ical is the mass fraction of component i detected by fluorescence method after the test sample is ignited, expressed as %;

[0030] M i is the mass fraction of component i before the test sample is ignited, expressed as %.

[0031] Furthermore, the test sample preparation and drying include crushing and grinding the test sample until it all passes through a square-hole sieve with a size of 120 μm to 150 μm, fully mixing it, sealing it as soon as possible, and without drying.

[0032] Furthermore, the test sample ignition treatment is to weigh the test sample, dry it and cool it to room temperature, and ignite the test sample at 1000 ± 50 °C for 0.5 h to 1 h or until constant weight.

[0033] Furthermore, for the test sample fused tablet, weigh the test sample after ignition, drying and cooling to room temperature, and mix it with lithium metaborate anhydrous Li 2 B 4 O 7 in a mass ratio of 1:10, place it in a platinum crucible, put the crucible into a high-frequency sample melting furnace, rotate and melt it at 1250 °C to 1300 °C for 6 min to 8 min, add the demolding agent ammonium iodide NH 4 I, take it out, shake it to drive out the bubbles, then place the crucible on a flat asbestos board, and after natural cooling, it will automatically peel off into a uniform round piece, which is numbered for measurement.

[0034] Furthermore, calculate the loss on ignition:

[0035]

[0036] where ω LOI is the loss-on-ignition of the test sample, expressed as %;

[0037] m 1 is the mass of the test sample and the ignition vessel before ignition, with the unit of gram g;

[0038] m 2is the mass of the sample and the crucible after ignition, in grams (g);

[0039] m 0 is the mass of the sample, in grams (g);

[0040] Similarly, the contents of calcium oxide (CaO), silicon dioxide (SiO 2 and magnesium oxide (MgO) in the ignited sample are calculated by the following formula due to loss on ignition:

[0041]

[0042] where M i is the mass fraction of component i in the sample before ignition, expressed as %;

[0043] M ical is the mass fraction of component i in the sample after ignition, expressed as %.

[0044] Compared with the prior art, the beneficial effects of the present invention are:

[0045] 1) The method is simple to operate and easy for other experimenters to learn;

[0046] 2) The instrument settings are simple and common, and easy for other laboratories to obtain;

[0047] 3) Compared with the national standard, the X-ray fluorescence method has stronger repeatability. The types of chemical reagents used are simpler, easier to obtain and in smaller amounts. The number of detection instruments involved is less, resulting in less environmental pollution and saving the procurement cost of instruments and chemical reagents;

[0048] 4) The X-ray fluorescence method has a short sample processing time and a fast detection speed, which can improve the working conditions and labor productivity; the three detected elements can be detected at one time, greatly improving the detection efficiency; the sample processing method with loss on ignition correction can ensure the accuracy and reliability of the X-ray fluorescence detection results of quicklime samples, especially samples with a high loss on ignition. BRIEF DESCRIPTION OF THE DRAWINGS

[0049] Figure 1 is the process flow chart of the method of the present invention.

[0050] Figure 2 is a schematic diagram of the working curve of the X-ray fluorescence method for detecting calcium oxide (CaO) in quicklime according to the present invention.

[0051] Figure 3 is a schematic diagram of the working curve of the X-ray fluorescence method for detecting magnesium oxide (MgO) in quicklime according to the present invention.

[0052] Figure 4 is a schematic diagram of the working curve of the X-ray fluorescence method for detecting silicon dioxide (SiO 2 in quicklime according to the present invention. Detailed implementation manners

[0053] The following further explains the detailed implementation manners of the present invention in conjunction with the accompanying drawings:

[0054] See Figure 1 , which is the method flow chart of the present invention. A method for determining calcium, silicon, and magnesium in quicklime by X-ray fluorescence with loss-on-ignition correction includes the following steps:

[0055] S1. Specimen preparation and drying:

[0056] Crush and grind the specimen, and it should all pass through a 150μm square-hole sieve for sieving, mix well. The above steps should be carried out as quickly as possible, seal and store the specimen to prevent moisture absorption, and no drying is required.

[0057] S2. Specimen ignition treatment and calculation of loss on ignition:

[0058] Weigh 1.0000 g (accurate to 0.0001 g) of the specimen dried and cooled to room temperature and place it in a square porcelain dish, then put it into a high-temperature muffle furnace and ignite it at 1000°C ± 50°C for 1 h or until constant weight;

[0059] Take out the specimen from the high-temperature furnace, put it into a desiccator to cool to room temperature and weigh it, and calculate the loss on ignition of the specimen according to the following formula:

[0060]

[0061] Among them, ω LOI is the loss on ignition of the specimen, expressed in %;

[0062] m 1 is the mass of the specimen and the ignition vessel before ignition, with the unit of gram g;

[0063] m 2 is the mass of the specimen and the ignition vessel after ignition, with the unit of gram g;

[0064] m 0 is the mass of the specimen, with the unit of gram g;

[0065] Similarly, the contents of calcium oxide CaO, silicon oxide SiO 2 and magnesium oxide MgO in the ignited specimen are calculated according to the following formula due to loss on ignition:

[0066]

[0067] Among them, M i is the mass fraction of component i before ignition of the specimen, expressed in %;

[0068] M ical is the mass fraction of component i after ignition of the specimen, expressed in %.

[0069] S3. Specimen fusion slice:

[0070] Weigh 0.4000 g (accurate to 0.0001 g) of the specimen that has been burned, dried, and cooled to room temperature, and 4.0000 g (accurate to 0.0001 g) of anhydrous lithium tetraborate Li 2 B 4 O 7 Place them in a platinum crucible, put the crucible into a high-frequency sample melting furnace, rotate and melt at 1250 °C for 8 minutes, add the demolding agent ammonium iodide NH 4 I. After taking it out and shaking to drive out the bubbles, place the crucible on a flat asbestos board. After natural cooling, it will automatically peel off into a uniform glass disc. After numbering, it is ready for measurement.

[0071] S4. Establish an X-ray fluorescence detection method and set detection conditions:

[0072] Turn on the X-ray fluorescence spectrometer and establish a method for detecting calcium, silicon, and magnesium elements in quicklime by X-ray fluorescence;

[0073] Put the prepared glass fusion slice into the fluorescence spectrometer, make optical and electrical selections for the measurement channels of each component, and the measured element spectral lines and measurement conditions are shown in Table 1:

[0074] Table 1: Measured element spectral lines and measurement conditions

[0075]

[0076]

[0077] S5. Establish a working curve for X-ray fluorescence detection of quicklime:

[0078] According to the instrument operation manual, draw a working curve. The measurement conditions for detecting calcium, silicon, and magnesium elements in quicklime are listed in Table 1. Since the main component of quicklime is calcium oxide CaO, its chemical properties are very active and it is extremely easy to absorb water and carbon dioxide CO in the air 2 , so there is currently no standard sample of quicklime. The method to solve this problem is to use a limestone standard sample with relatively stable chemical properties, burn it at high temperature to release carbon dioxide CO 2 , and obtain quicklime with only calcium oxide CaO;

[0079] Process several limestone standard samples with concentration gradients into glass fusion slices according to steps S2 and S3. And based on the standard values and loss on ignition of each component of these limestone standard samples, calculate the corresponding mass content of quicklime according to formula (1) and formula (2). The working curve for X-ray fluorescence detection of quicklime can be drawn with the glass fusion slices made from this standard sample and used as a calibration control sample;

[0080] According to the glass fusion slices of the limestone standard sample prepared after calcination, measure the fluorescence intensity of each component using the element spectral lines and measurement conditions in Table 1, and establish a working curve for detecting calcium, silicon, and magnesium components according to formula (3):

[0081] W i =(BI i +A)(3);

[0082] Among them, W i is the content of the analyzed element i in the glass fusion slice of the limestone standard sample prepared after calcination, %;

[0083] I i is the X-ray intensity of element i, kcps;

[0084] A and B are the working curve coefficients;

[0085] At the same time, calculate the linear correlation coefficient of the working curve of each component.

[0086] S6. Calibration of the X-ray fluorescence working curve:

[0087] By measuring the glass fusion slices of the limestone standard sample, standardize the instrument and correct the instrument drift; perform this operation every 24 hours or before measuring unknown samples.

[0088] S7. Loss on ignition correction of quicklime samples by X-ray fluorescence method:

[0089] Process the quicklime sample into a glass melt slice according to steps S2 and S3, calculate its loss on ignition according to formula (1), detect the content of each component of the glass melt slice using the X-ray fluorescence working curve, and finally perform loss on ignition correction on it according to formula (4) to obtain the sample content:

[0090] M i =M ical ×(1 - ω LOI )(4);

[0091] Among them, ω LOI is the loss on ignition of the sample, expressed as %;

[0092] M ical is the mass fraction of component i detected by fluorescence method after the sample is calcined, expressed as %;

[0093] M i is the mass fraction of component i before the sample is calcined, expressed as %.

[0094] S8. Verify the reliability of the X-ray fluorescence working curve:

[0095] The limestone standard samples and random quicklime samples that are not involved in establishing the method are detected by this method, and are also processed into glass fusion slices according to steps S2 and S3. The loss on ignition correction is performed on the test results according to formula (4). If the corrected results are consistent with the standard values or the results of other testing methods such as the EDTA volumetric method, gravimetric method, and atomic absorption method, it proves that this method is reliable and meets the requirements of chemical inspection.

[0096] Considering that quicklime samples have a certain loss on ignition due to moisture absorption and oxidation, and currently the main sample processing method for X-ray fluorescence spectrometry is the fused glass disc method, which requires a fixed solute-solvent ratio (usually 1:10 or 1:5). If direct high-temperature fusion is performed on quicklime samples, it will cause the solute-solvent ratio to decrease. Therefore, in this method, the quicklime samples need to be calcined before melting into glass discs, and the loss on ignition of the samples is calculated, and the loss on ignition correction calculation is performed on the test results.

[0097] This detection method saves chemical reagents and instruments used in detection, reduces production costs, improves labor productivity. The previous work of multiple people and multiple instruments has been simplified to be completed by one person and one instrument. Moreover, the detection efficiency is high, the speed is fast, the reagents used are simple and easy to obtain and the dosage is smaller, reducing environmental pollution. The improved sample processing method can ensure the accuracy and reliability of the test results.

[0098] The following examples are implemented on the premise of the technical solution of the present invention, and the detailed implementation manners and specific operation processes are given, but the protection scope of the present invention is not limited to the following examples. The methods used in the following examples are all conventional methods unless otherwise specified.

[0099] Example 1:

[0100] A working curve is established using limestone standard samples;

[0101] Select limestone standard samples 8601, YSBC28711-93, GBW07214a, BH0119-3Wa, YSB14771-96, YSBC28721a-2013, and their loss on ignition and standard values of each component are shown in Table 2:

[0102] Table 2: Standard values and loss on ignition of limestone standard samples participating in establishing the working curve

[0103]

[0104]

[0105] The above limestone standard samples are processed into glass fusion slices according to steps S2 and S3, and the content of each component in the glass fusion slices is calculated according to the loss on ignition of each standard sample using formula (2), as shown in Table 3:

[0106] Table 3: Component contents in the glass chips of the limestone standard samples for establishing the working curve

[0107]

[0108] Put the glass fusion chips made from the above limestone standard samples into the fluorescence spectrometer. Under the spectral lines and instrument conditions listed in Table 1, establish the working curve for detecting quicklime according to formula (3), as Figure 2 、 3 、4;

[0109] See Table 4. The calibration parameters and linear ranges of the working curves for detecting each component of quicklime by fluorescence method are as follows:

[0110] Table 4: Calibration parameters and linear ranges of the working curves for detecting each component of quicklime by fluorescence method

[0111]

[0112] It can be seen that the correlation coefficients of the working curves for each component by the tablet pressing method are all close to 1.0000, and the linear condition of the working curve is good.

[0113] Example 2:

[0114] Verify the accuracy of this method;

[0115] Select limestone standard samples 8602, YSBC16703-01, YSBC28710-93, YSBC28705-93, YSBC28706-93 and make them into glass fusion tablets according to steps S2 and S3, and calculate their loss on ignition. Then use the working curve established by this method to detect the calcium oxide CaO, silicon dioxide SiO 2 and magnesium oxide MgO components in the glass chips. The detection values are shown in Table 5:

[0116] Table 5: Fluorescence detection results of the standard sample glass fusion tablets

[0117]

[0118]

[0119] Make loss on ignition correction for the fluorescence detection results of the standard samples in Table 5 according to formula (4) based on their loss on ignition, obtain the component contents before loss on ignition, and compare with the standard values to judge the accuracy of the method. The results are shown in Tables 6, 7, and 8. Comparison of the fluorescence method for detecting standard samples with the standard values:

[0120] Table 6: Accuracy of detecting calcium oxide CaO in the standard sample

[0121]

[0122] Table 7: Silicon Oxide SiO in the Test Standard Sample 2 Accuracy

[0123]

[0124] Table 8: Accuracy of Magnesium Oxide MgO in the Test Standard Sample

[0125]

[0126] As can be seen from Tables 6, 7, and 8, the results of testing the limestone standard sample by this method are highly consistent with the standard values and do not exceed the tolerance, meeting the requirements of chemical testing.

[0127] Example 3:

[0128] Verify the precision of this method;

[0129] Select limestone standard samples 8601, GBW07214a, YSB14771-96, and YSBC28721a-2013, and prepare them into glass fusion tablets according to steps S2 and S3, and calculate their loss on ignition. Then, use the working curve established by this method to detect calcium oxide CaO, silicon dioxide SiO 2 and magnesium oxide MgO components in the glass 10 times each, and calculate the repeatability limit of the measurement results of each component. The results are shown in Tables 9, 10, and 11 (for convenience, all the test results in the tables are the contents of each component before loss on ignition calculated after loss on ignition correction by formula (4)):

[0130] Table 9: Precision of Calcium Oxide CaO by X-ray Fluorescence Method

[0131]

[0132] Table 10: Silicon Dioxide SiO by X-ray Fluorescence Method 2 Precision

[0133]

[0134] Table 11: Precision of Magnesium Oxide MgO by X-ray Fluorescence Method

[0135]

[0136]

[0137] Note: The test values here are all the results after loss on ignition correction, so there will be a difference from the test range specified in Table 4. The test results before loss on ignition correction are all within the test range of Table 4;

[0138] As can be seen from Table 11, the repeatability limits of the test results of each component by fluorescence method do not exceed the tolerance, meeting the requirements of chemical testing.

[0139] Comparative example:

[0140] Detect random quicklime samples;

[0141] For random quicklime samples HB24070008, HB24080615, HB24100053, HB24110013, HB25010017, make glass fusion tablets according to steps S2 and S3 and calculate their loss on ignition. Then use the working curve established by this method to detect the calcium oxide CaO, silicon dioxide SiO 2 and magnesium oxide MgO components in the glass. Finally, perform loss on ignition correction on the test results according to the loss on ignition using formula (4) to obtain the component content before loss on ignition, and compare it with the results of other test methods. See Tables 12, 13, and 14 for the comparison of the test results of random limestone samples by fluorescence method with those of other test methods:

[0142] Table 12: Accuracy of detecting calcium oxide CaO in random samples

[0143]

[0144] Table 13: Accuracy of detecting silicon dioxide SiO 2 in random samples

[0145]

[0146]

[0147] Table 14: Accuracy of detecting magnesium oxide MgO in random samples

[0148]

[0149] Note: When the magnesium oxide MgO content is greater than 2.5%, the other test method for result comparison with the fluorescence method is the volumetric method.

[0150] As can be seen from Tables 12, 13, and 14, regardless of the high or low loss on ignition of the quicklime samples (the loss on ignition of samples HB24070008 and HB24080615 reaches about 15%), the measurement results of the X-ray fluorescence method are highly consistent with those of other test methods and do not exceed the allowable error, indicating the practicality of this method.

Claims

1. A method for determining calcium, silicon and magnesium in quicklime by X-ray fluorescence with loss on ignition correction, characterized in that: The steps include: S1. Sample preparation and drying; S2. Burning treatment of samples and calculation of burning loss; S3, sample melt; S4. Establishing X-ray fluorescence detection method and setting detection conditions; S5. Establishing a working curve for X-ray fluorescence detection of quicklime: Based on the limestone standard sample obtained after burning, the fluorescence intensity of each component is measured by the element spectrum of each element and the detection conditions, and a working curve for detecting calcium, silicon and magnesium components is established according to the following formula: W i =(BI i +A)); Among them, W i is the content of element i in the glass frit obtained by burning the limestone standard sample, %; I i is the X-ray intensity of element i, kcps; A and B are working curve coefficients; At the same time, the linear correlation coefficient of the working curve of each component is calculated; S6. X-ray fluorescence working curve calibration: Standardize the instrument operation and correct the instrument drift by measuring the limestone standard sample fused piece, every 24h to 48h or before measuring the unknown sample; S7, X-ray fluorescence method is used to correct the burning loss of quicklime sample and obtain the sample content; M i =M ical ×(1-ω LOI ); Among them, ω LOI is the loss on ignition of the sample, expressed in %; M ical is the mass fraction of component i detected by fluorescence method after the sample is burned, expressed in %; M i It is the mass fraction of component i before the sample is burned, expressed in %.

2. The method for determining calcium, silicon and magnesium in quicklime by X-ray fluorescence with loss on ignition correction according to claim 1, characterized in that: The sample preparation and drying include crushing and grinding the sample until it can all pass through a 120 μm-150 μm square hole sieve, fully mixing, and sealing as soon as possible without drying.

3. The method for determining calcium, silicon and magnesium in quicklime by X-ray fluorescence with loss on ignition correction according to claim 1, characterized in that: The sample burning treatment is to weigh the sample, dry and cool it to room temperature, and burn the sample at 1000±50°C for 0.5h to 1h or until constant weight.

4. The method for determining calcium, silicon and magnesium in quicklime by X-ray fluorescence with loss on ignition correction according to claim 3, characterized in that: The sample melt is weighed, dried and cooled to room temperature after calcination, and placed in a platinum crucible with anhydrous lithium tetraborate Li2B4O7 in a mass ratio of 1:10, the crucible is placed in a high-frequency melting furnace and rotated to melt at 1250°C to 1300°C for 6min to 8min, and a demolding agent ammonium iodide NH4I is added. After taking out and shaking to drive away bubbles, the crucible is placed on a flat asbestos board, and after natural cooling, it is automatically peeled off into uniform discs, which are numbered for measurement.

5. The method for determining calcium, silicon and magnesium in quicklime by X-ray fluorescence with loss on ignition correction according to claim 1, characterized in that: The calculation of loss on ignition: Among them, ω LOI is the loss on ignition of the sample, expressed in %; m1 is the mass of the sample and the burning vessel before burning, in grams; m2 is the mass of the sample and the burning vessel after burning, in grams; m0 is the mass of the sample, in grams; Similarly, the contents of calcium oxide (CaO), silicon oxide (SiO2) and magnesium oxide (MgO) in the sample after burning are lost due to burning, and are calculated as follows: Among them, M i is the mass fraction of component i before the sample is burned, expressed in %; M ical It is the mass fraction of component i after the sample is burned, expressed in %.

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