CN114486970A - X-ray fluorescence determination method for content of metal elements in toughened salt - Google Patents
X-ray fluorescence determination method for content of metal elements in toughened salt Download PDFInfo
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Abstract
The invention discloses an X-ray fluorescence measuring method for the content of metal elements in toughened salt, which relates to a detection method in the field of glass manufacturing, and the establishment method of a standard curve comprises the following steps: preparing a plurality of groups of standard samples with different concentrations by adopting standard samples of metal element components in toughened salt; mixing lithium tetraborate and silicon dioxide to prepare a mixed fluxing agent; mixing the standard sample with a mixed fluxing agent to prepare a mixed sample; melting the mixed sample at high temperature, and cooling to obtain a standard sample glass sheet; and carrying out X-ray fluorescence spectrum detection on the standard sample glass sheet, recording the content of metal element components in the toughened salt and the corresponding X-ray fluorescence intensity, and establishing a content-X-ray fluorescence intensity standard working curve. The method effectively reduces the dosage of the fluxing agent in the process of preparing the sample glass sheet of the toughened salt by utilizing the X-ray fluorescence spectrometry, successfully realizes the detection of the content of the metal elements in the toughened salt, and has high process efficiency and reliable result.
Description
Technical Field
The invention relates to a detection method in the field of glass manufacturing, in particular to an X-ray fluorescence measurement method for the content of metal elements in toughened salt.
Background
The tempering process is an important part of glass manufacturing. In the toughening process, if the proportion of the metal element components of the toughening salt does not meet the requirement, the mechanical strength of glass toughening is low, the pressure resistance is poor, and even glass self-explosion occurs, so that the timely detection of the content of each metal element component of the toughening salt is of great significance in glass production.
The main metal element components of the toughened salt comprise potassium nitrate, sodium nitrate, calcium nitrate and magnesium nitrate, and the conventional detection method is a chemical detection method at present. Wherein the potassium content is detected by adopting a tetraphenylboropotassium precipitation method, and the potassium, calcium and magnesium contents are detected by adopting an atomic absorption spectrum or a plasma emission spectrum method. The reagent required by the potassium tetraphenylborate precipitation method is expensive, the detection experiment waste liquid easily causes environmental pollution, the detection period is long, the requirement on the operation technical level of detection personnel is high, the detection steps are complicated, and the incomplete precipitation easily causes errors. When the atomic absorption spectrometry or the plasma emission spectrometry is used for detecting the contents of potassium, calcium and magnesium, a sample needs to be diluted to reach a detection limit, the dilution multiple is often up to 5000 times, and the detection result has larger error. The detection methods are difficult to meet the detection requirements of the field of glass manufacturing on the toughened salt.
In addition, the method utilizes the X-ray fluorescence spectrometry to measure the content of potassium and sodium elements in the industrial potassium nitrate, has simple sample treatment, no loss and no environmental pollution, and is a high-efficiency and high-reliability automatic measuring method. When the method is used, a sample to be detected and a fluxing agent are mixed and melted to obtain a mixed sample glass sheet for detection. The content of the fluxing agent used in the melting process is high, and when the content of the fluxing agent is less than 15 times of the mass of potassium nitrate, the molten glass sheet is easy to break and crystallize, and subsequent detection cannot be carried out. Meanwhile, the high content of the fluxing agent can increase the detection cost and reduce the detection accuracy. In addition, the method only detects the content of potassium and sodium.
Disclosure of Invention
The invention aims to provide an X-ray fluorescence measuring method for the content of metal elements in toughened salt, which can reduce the dosage content of a fluxing agent, and has the advantages of low detection cost and accurate detection result.
The detection method is realized by the following technical scheme:
a method for establishing a standard curve in an X-ray fluorescence measuring method for the content of metal elements in a toughened salt comprises the following steps: preparing a plurality of groups of standard samples with different concentrations by adopting standard samples of metal element components in toughened salt; mixing lithium tetraborate and silicon dioxide to prepare a mixed fluxing agent; mixing the standard sample with a mixed fluxing agent to prepare a mixed sample; melting the mixed sample at high temperature, and cooling to obtain a standard sample glass sheet; and carrying out X-ray fluorescence spectrum detection on the standard sample glass sheet, recording the content of the metal element in the toughened salt and the corresponding X-ray fluorescence intensity, and establishing a content-X-ray fluorescence intensity standard working curve.
In one embodiment, the tempering salt composition is selected from the group consisting of potassium nitrate, sodium nitrate, calcium nitrate, and magnesium nitrate.
In one embodiment, in the mixed fluxing agent, the mass ratio of the lithium tetraborate to the silicon dioxide is 20-5: 1.
in one embodiment, in the mixed sample, the mass of the mixed fluxing agent and the mass of the standard sample are 30-8: 1.
in one embodiment, a release agent is applied to the surface of the mixed sample before high-temperature melting, wherein the release agent is lithium bromide.
In one embodiment, the parameters of the high-temperature molten sample include: standing for 120-160 s, standing for 100-150 s, primary swing time for 5-20 s, secondary swing time for 5-20 s, and melting temperature for 930-1200 ℃.
An X-ray fluorescence measuring method for the content of metal elements in toughened salt comprises the following steps: mixing lithium tetraborate and silicon dioxide to prepare a mixed fluxing agent; mixing the mixed fluxing agent with a to-be-detected toughened salt sample to prepare a mixed sample; adding a release agent, melting the mixed sample at a high temperature, and cooling to obtain a glass sheet of the sample to be detected; and carrying out X fluorescence spectrum detection on the sample glass sheet to be detected, and obtaining the content of the metal elements in the toughened salt to be detected according to the established standard curve.
In one embodiment, the metal element component in the tempered salt to be tested comprises one or more of potassium nitrate, sodium nitrate, calcium nitrate and magnesium nitrate.
In one embodiment, in the mixed fluxing agent, the mass ratio of the lithium tetraborate to the silicon dioxide is 20-5: 1.
in one embodiment, in the mixed sample, the mass ratio of the mixed fluxing agent to the toughened salt sample to be detected is 30-8: 1.
in one embodiment, a release agent is applied to the surface of the mixed sample before high-temperature melting, wherein the release agent is lithium bromide.
In one embodiment, the parameters of the high-temperature molten sample are as follows: standing for 120-160 s, standing for 100-150 s, primary swing time for 5-20 s, secondary swing time for 5-20 s, and melting temperature for 930-1200 ℃.
The invention has the beneficial effects that: according to the invention, by utilizing the X-ray fluorescence spectrometry, lithium tetraborate and silicon dioxide are used as mixed fluxing agents in the process of preparing the sample glass sheet of the toughened salt, so that the dosage of the fluxing agents is effectively reduced, the phenomena of breakage and crystallization of the sample glass sheet of the toughened salt when the dosage of the fluxing agents is low can be effectively prevented, the detection of the content of metal elements in the toughened salt is successfully realized, the detection process is efficient, the result is reliable, the sample treatment is simple, no loss is caused, and no environmental pollution is caused.
In addition, in the research, the method can simultaneously detect the contents of potassium, sodium, calcium and magnesium elements in the tempered salt.
Drawings
FIG. 1 is a standard curve of the metal element K of example 1;
FIG. 2 is a standard curve of the metal element Na of example 1;
FIG. 3 is a standard curve of the metal element Ca of example 1;
FIG. 4 is a standard curve of the metallic element Mg of example 1.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. The following is a preferred embodiment of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
In the present invention, "one or more" means any one, any two or more of the listed items.
In the present invention, the numerical intervals are regarded as continuous, and include the minimum and maximum values of the range and each value between the minimum and maximum values, unless otherwise specified. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range-describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein.
In the present invention, the percentage content refers to both mass percentage for solid-liquid mixing and solid-solid phase mixing and volume percentage for liquid-liquid phase mixing, unless otherwise specified.
In the present invention, the percentage concentrations are, unless otherwise specified, the final concentrations. The final concentration refers to the ratio of the additive component in the system to which the component is added.
In the present invention, the temperature parameter is not particularly limited, and may be a constant temperature treatment or a treatment within a certain temperature range. The constant temperature process allows the temperature to fluctuate within the accuracy of the instrument control.
The invention provides a method for establishing a standard curve in an X-ray fluorescence measurement method for the content of metal elements in toughened salt, which comprises the following steps: preparing a plurality of groups of standard samples with different concentrations by adopting standard samples of metal element components in toughened salt; mixing lithium tetraborate and silicon dioxide to prepare a mixed fluxing agent; mixing the standard sample with a mixed fluxing agent to prepare a mixed sample; melting the mixed sample at high temperature, and cooling to obtain a standard sample glass sheet; and carrying out X-ray fluorescence spectrum detection on the standard sample glass sheet, recording the content of metal element components in the toughened salt and the corresponding X-ray fluorescence intensity, and establishing a content-X-ray fluorescence intensity standard working curve.
In one example, the tempering salt composition comprises a combination of one or more of potassium nitrate, sodium nitrate, calcium nitrate, and magnesium nitrate.
Further, in the mixed fluxing agent, the mass ratio of the lithium tetraborate to the silicon dioxide is 20-5: 1. the stabilizing agent silicon dioxide is added into the fluxing agent, so that the sample glass sheet of the toughened salt forms a stable silicate glass state, the intermolecular structure is more reasonable, the structure is more stable, the appearance is clearer, and the accuracy of an X-ray fluorescence detection result is more facilitated. Specifically, the mass ratio of lithium tetraborate to silica includes, but is not limited to: 20: 1. 18: 1. 15: 1. 10: 1. 5: 1.
further, in the mixed sample, the mass ratio of the mixed fluxing agent to the standard sample is 30-8: 1. thereby, the error of the X-ray fluorescence detection result can be further reduced. Meanwhile, the condition of thermal decomposition or violent splashing of the sample can be avoided in the reaction melting process. Specifically, the mass ratio of the mixed flux to the standard sample includes, but is not limited to: 30: 1. 25: 1. 20: 1. 15: 1. 10: 1. 8: 1.
further, prior to high temperature melting, a release agent is applied to the surface of the mixed sample.
Without limitation, the release agent comprises lithium bromide.
In one embodiment, the parameters of the high-temperature molten sample are as follows: standing for 120-160 s, standing for 100-150 s, primary swing time for 5-20 s, secondary swing time for 5-20 s, and melting temperature for 930-1200 ℃.
In one embodiment, the test parameters of the X-ray fluorescence spectrometer are: component K test parameters: a spectral line K-Ka, a voltage of 30kV, a current of 80mA, crystal LiF200, a detector FPC, a collimator of 0.4, an angle of 136.684 and a time of 24 s; component Na test parameters: a spectral line Na-Ka, a voltage of 30kV, a current of 80mA, crystal LiF200, a detector FPC, a collimator 1, an angle 45.591 and a time of 24 s; component Ca test parameters: spectral line Ca-Ka, voltage 30kV, current 80mA, crystal AX03, detector FPC, collimator 0.4, angle 113.086, time 40 s; component Mg test parameters: spectral line Mg-Ka, voltage 30kV, current 80mA, crystal AX03, detector FPC, collimator 1, angle 37.535, time 40 s.
The invention provides an X-ray fluorescence determination method for the content of metal elements in toughened salt, which comprises the following steps: mixing lithium tetraborate and silicon dioxide to prepare a mixed fluxing agent; mixing the mixed fluxing agent with a to-be-detected toughened salt sample to prepare a mixed sample; melting the mixed sample at high temperature, and cooling to obtain a glass sheet of the sample to be detected; and carrying out X-ray fluorescence spectrum detection on the sample glass sheet to be detected, and obtaining the content of the metal elements in the toughened salt sample to be detected according to the established standard curve.
In one example, the sample component of the tempered salt to be tested comprises a combination of one or more of potassium nitrate, sodium nitrate, calcium nitrate and magnesium nitrate.
Further, in the mixed fluxing agent, the mass ratio of the lithium tetraborate to the silicon dioxide is 20-5: 1. the stabilizing agent silicon dioxide is added into the fluxing agent, so that the sample glass sheet of the toughened salt forms a stable silicate glass state, the intermolecular structure is more reasonable, the structure is more stable, the appearance is clearer, and the accuracy of an X-ray fluorescence detection result is more facilitated. Specifically, the mass ratio of lithium tetraborate to silica includes, but is not limited to: 20: 1. 18: 1. 15: 1. 10: 1. 5: 1.
further, in the mixed sample, the mass of the mixed fluxing agent and the toughened salt sample to be detected is 30-8: 1. thereby, the error of the X-ray fluorescence detection result can be further reduced. Meanwhile, the condition of thermal decomposition or violent splashing of the sample can be avoided in the reaction melting process. Specifically, the mass ratio of the mixed flux to the tempered salt sample to be tested includes, but is not limited to: 30: 1. 25: 1. 20: 1. 15: 1. 10: 1. 8: 1.
further, prior to high temperature melting, a release agent is applied to the surface of the mixed sample.
Without limitation, the release agent comprises lithium bromide.
In one embodiment, the high temperature melt setting parameters are: standing for 120-160 s, standing for 100-150 s, primary swing time for 5-20 s, secondary swing time for 5-20 s, and melting temperature for 930-1200 ℃.
In one embodiment, the test parameters of the X-ray fluorescence spectrometer are: component K test parameters: a spectral line K-Ka, a voltage of 30kV, a current of 80mA, crystal LiF200, a detector FPC, a collimator of 0.4, an angle of 136.684 and a time of 24 s; component Na test parameters: a spectral line Na-Ka, a voltage of 30kV, a current of 80mA, crystal LiF200, a detector FPC, a collimator 1, an angle 45.591 and a time of 24 s; component Ca test parameters: spectral line Ca-Ka, voltage 30kV, current 80mA, crystal AX03, detector FPC, collimator 0.4, angle 113.086, time 40 s; component Mg test parameters: spectral line Mg-Ka, voltage 30kV, current 80mA, crystal AX03, detector FPC, collimator 1, angle 37.535, time 40 s.
The following are specific examples.
The X-ray fluorescence spectrometer used in the embodiment of the present invention is an ARL performance' X4200 type X-ray fluorescence spectrometer manufactured by seimer feishale science and technology (china).
Example 1
1. Drying commercially available lithium tetraborate (GR), silicon dioxide (more than or equal to 99.99%), potassium nitrate (GR), sodium nitrate (GR), calcium nitrate (AR) and magnesium nitrate (GR) at 110 ℃ for later use;
2. mixing the potassium nitrate, the sodium nitrate, the calcium nitrate and the magnesium nitrate in the step 1 together to prepare standard samples, and preparing 5.05g of standard series samples No. 1, No. 2, No. 3, No. 4, No. 5 and No. 6 respectively, wherein the preparation parameters of the standard samples are shown in Table 1;
table 1: standard sample set of formulation parameters Table for example 1
3. Lithium tetraborate and silica were mixed in a 10: 1, fully and uniformly mixing in a corundum crucible mortar to form a mixed fluxing agent;
4. accurately weighing 7.7000g of the mixed fluxing agent in the step 3 and 5.5000g of the standard sample 1# in the step 2, placing the weighed materials in a platinum yellow crucible, and uniformly stirring the weighed materials;
5. dripping 300 mu L of 300g/L lithium bromide release agent on the surface of the sample in the step 4;
6. placing the platinum yellow crucible in a high-temperature sample melting machine for melting samples, wherein the sample melting parameters of the high-temperature sample melting machine are shown in a toughened salt sample melting parameter setting table in a table 2; after the sample is melted by a high-temperature sample melting machine, taking out the platinum yellow crucible, naturally cooling and demolding to obtain a standard sample glass sheet No. 1;
table 2: example 1 sample melting program parameter setting Table
7. And repeating the steps 4-6 to obtain 2#, 3#, 4#, 5#, and 6# standard sample glass sheets respectively. Calculating to obtain the contents of potassium, sodium, calcium and magnesium in each standard sample as shown in table 3;
table 3: table for conversion data of component content of glass sheet for reference sample in example 1
8. Recording the component content of the standard sample glass sheet on an X-ray fluorescence spectrometer, and testing the corresponding intensity, wherein the measurement conditions of the X-ray fluorescence spectrometer are shown in Table 4;
table 4: measuring condition table of X-ray fluorescence spectrometer
9. According to the content of the standard sample glass sheet component and the corresponding intensity data obtained by the X-ray fluorescence spectrometer, a content-X-ray fluorescence intensity standard working curve is established, and the result is shown in figures 1-4.
Example 2
The standard sample No. 2 is detected by the method of the invention and compared with the detection result of a chemical method.
1. Lithium tetraborate and silica were mixed in a 10: 1, fully and uniformly mixing in a corundum crucible mortar to form a mixed fluxing agent;
2. accurately weighing 5.5000g of standard sample No. 2 and 7.7000g of mixed fluxing agent in the step 2 of the embodiment 1, placing the standard sample No. 2 and the mixed fluxing agent in a platinum yellow crucible, and uniformly stirring;
3. dripping 300 mu L of 300g/L of lithium bromide release agent on the surface of the sample in the step 2;
4. placing the platinum yellow crucible in a high-temperature sample melting machine for melting samples, wherein the sample melting parameters of the high-temperature sample melting machine are shown in a toughened salt sample melting parameter setting table of a table 5; after the sample is melted by a high-temperature sample melting machine, taking out the platinum yellow crucible, naturally cooling and demolding to obtain a standard sample glass sheet No. 2;
table 5: sample melting program parameter setting table
5. Placing a sample glass sheet 2# to be tested in a sample box of the X-ray fluorescence spectrometer, starting a quantitative analysis program, and testing corresponding intensity, wherein the measurement conditions of the X-ray fluorescence spectrometer are shown in a table 6;
table 6: measuring condition table of X-ray fluorescence spectrometer
6. The content of each element to be measured was automatically calculated by a computer based on the standard working curve of content-strength established in example 1, and the results of comparison of the results with those of the conventional chemical method are shown in Table 7. The detection results in Table 7 show that the error of the results of the detection methods of the invention and the chemical method is in a reasonable range, which indicates that the method of the invention is stable and reliable.
Table 7: the method of the invention is compared with the detection result of the conventional chemical method
Example 3
And (5) detecting a tempered salt sample in a chemical tempering furnace.
1. Taking about 50g of toughened salt in a chemical toughening furnace, after a toughened salt sample is cooled, placing the sample in a corundum crucible, grinding the sample to be less than 0.01 mu m, transferring the sample to a weighing bottle, drying the sample for 2 hours at 110 ℃, taking out the sample, and naturally cooling the sample for later use;
2. lithium tetraborate and silica were mixed as 10: 1, fully and uniformly mixing in a corundum crucible mortar to form a mixed fluxing agent;
3. accurately weighing 5.5000g of the toughened salt sample in the step 1 and 7.7000g of the mixed fluxing agent, placing the samples in a platinum yellow crucible, and uniformly stirring;
4. dripping 300 mu L of 300g/L of lithium bromide release agent on the surface of the sample in the step 3;
5. placing the platinum yellow crucible in a high-temperature sample melting machine for melting samples, wherein the sample melting parameters of the high-temperature sample melting machine are shown in a table 8 for setting the tempered salt sample melting parameters; after sample melting is finished by a high-temperature sample melting machine, taking out the platinum yellow crucible, naturally cooling and demolding to obtain a toughened salt sample glass sheet to be detected;
table 8: sample melting program parameter setting table
6. Placing a sample glass sheet to be tested in a sample box of the X-ray fluorescence spectrometer, starting a quantitative analysis program, and testing corresponding intensity, wherein the measurement conditions of the X-ray fluorescence spectrometer are shown in a table 9;
table 9: measuring condition table of X-ray fluorescence spectrometer
7. According to the standard working curve of content-X-ray fluorescence intensity established in the embodiment 1, the content of each element to be detected is automatically calculated by a computer, and the comparison result between the detection result and the design theoretical value is shown in Table 10, wherein the calculation mode of the design theoretical value is as follows: potassium nitrate in the toughened salt: sodium nitrate: calcium nitrate: the theoretical mass ratio of the magnesium nitrate is 100: 100: 1: 1, conversion to potassium: sodium: calcium: the percentage content of magnesium metal elements is respectively 19.14%, 13.39%, 0.0084% and 0.0081%. From table 10, it can be seen that the error between the detection result and the theoretical value of the present invention is within a reasonable range, which indicates that the method of the present invention is stable and reliable.
Table 10: comparison table of detection result and theoretical value of toughened salt sample
Example 4
Determination of Potassium nitrate and sodium nitrate toughened salts
1. Mixing potassium nitrate and sodium nitrate in a ratio of 1: 1, drying and cooling at 110 ℃ for later use, and obtaining toughened salt A;
2. lithium tetraborate and silica were mixed in a 20: 1, fully and uniformly mixing in a corundum crucible mortar to form a mixed fluxing agent;
3. accurately weighing 10.0000g of mixed fluxing agent in the step 2 and 1.0000g of toughened salt in the step 1, placing the weighed materials in a platinum yellow crucible, and uniformly stirring the materials;
4. dripping 300 mu L of 300g/L of lithium bromide release agent on the surface of the sample in the step 3;
5. placing the platinum yellow crucible in a high-temperature sample melting machine for sample melting, wherein the sample melting parameters of the high-temperature sample melting machine are shown in a toughened salt sample melting parameter setting table in table 2 in example 1; after the sample is melted by a high-temperature sample melting machine, taking out the platinum yellow crucible, and naturally cooling and demolding to obtain a sample glass sheet with the effect shown in Table 11;
6. detection of a toughened salt sample to be tested
And detecting the melted sample glass sheet to be detected on an X-ray fluorescence spectrometer according to the established standard working curve.
Example 5
The procedure of example 5 was substantially the same as that of example 4, except that: in the step 2, the mass ratio of the lithium tetraborate to the silicon dioxide is 10: 1, the effect of the sample glass sheet obtained is shown in Table 11.
Example 6
The method of operation of example 6 is substantially the same as that of example 4, except that: in the step 2, the mass ratio of the lithium tetraborate to the silicon dioxide is 5: 1, the effect of the sample glass sheet obtained is shown in Table 11.
Comparative example 1
The procedure of comparative example 1 was substantially the same as that of example 4 except that: in the step 2, the fluxing agent is a traditional fluxing agent which is a mixture of lithium tetraborate and lithium metaborate in a mass ratio of 67:33, and the effects and detection results of the obtained sample glass sheets are shown in table 11.
Table 11: melting effect comparison table
From the above table 11, it can be seen that the quality of the molten sample pieces in examples 4 to 6 is significantly higher than that in comparative example 1, which shows that the X-ray fluorescence measurement method for the content of the metal elements in the toughened salt according to the present invention has a better effect. Specifically, from the experimental results of example 4 and comparative example 1 (the ratio of the flux to the tempered salt to be measured is 10: 1, and only the flux component is different), it can be seen that the quality of the molten sample glass sheet can be significantly improved by adding the mixed flux of the present invention, while the molten glass sheet in comparative example 1 has the phenomena of breakage and devitrification, and the subsequent X-ray fluorescence measurement cannot be performed.
From the experimental results of examples 4 to 6, it can be seen that when the ratio of lithium tetraborate to silica in the mixed flux is 20: 1-5: 1, the molten sample glass sheet is clear in appearance and stable in quality, and is suitable for the subsequent X-ray fluorescence measurement of the content of metal elements in the toughened salt.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (12)
1. A method for establishing a standard curve in an X-ray fluorescence measuring method for the content of metal elements in a tempered salt is characterized by comprising the following steps: preparing a plurality of groups of standard samples with different concentrations by adopting standard samples of metal element components in toughened salt; mixing lithium tetraborate and silicon dioxide to prepare a mixed fluxing agent; mixing the standard sample with a mixed fluxing agent to prepare a mixed sample; melting the mixed sample at high temperature, and cooling to obtain a standard sample glass sheet; and carrying out X-ray fluorescence spectrum detection on the standard sample glass sheet, recording the content of metal element components in the toughened salt and the corresponding X-ray fluorescence intensity, and establishing a content-X-ray fluorescence intensity standard working curve.
2. The method of establishing a calibration curve for a method of X-ray fluorometry of metal content in a tempering salt of claim 1, wherein the metal component in the tempering salt is selected from the group consisting of potassium nitrate, sodium nitrate, calcium nitrate and magnesium nitrate.
3. The method for establishing a standard curve in an X-ray fluorescence measuring method for the content of metal elements in a tempered salt according to claim 1, wherein the mass ratio of the lithium tetraborate to the silicon dioxide in the mixed flux is 20-5: 1.
4. the method for establishing the standard curve in the X-ray fluorescence measuring method for the content of the metal elements in the tempered salt according to claim 1, wherein the mass ratio of the mixed fluxing agent to the standard sample in the mixed sample is 30-8: 1.
5. the method for establishing a calibration curve in an X-ray fluorescence measuring method for the content of metal elements in a tempered salt according to any one of claims 1 to 4, wherein a release agent is applied to the surface of the mixed sample before high-temperature melting, and the release agent is lithium bromide or ammonium iodide.
6. The method for establishing a standard curve in the X-ray fluorescence measuring method for the content of metal elements in a tempered salt according to any one of claims 1 to 4, wherein the parameters of the high-temperature melt sample comprise: standing for 120-160 s, standing for 100-150 s, primary swing time for 5-20 s, secondary swing time for 5-20 s, and melting temperature for 930-1200 ℃.
7. An X-ray fluorescence measuring method for the content of metal elements in a toughened salt is characterized by comprising the following steps: mixing lithium tetraborate and silicon dioxide to prepare a mixed fluxing agent; mixing the mixed fluxing agent with a to-be-detected toughened salt sample to prepare a mixed sample; melting the mixed sample at high temperature, and cooling to obtain a glass sheet of the sample to be detected; and (3) carrying out X fluorescence spectrum detection on the sample glass sheet to be detected, and obtaining the content of the metal elements in the tempered salt sample to be detected according to the standard curve established by the method of any one of claims 1-6.
8. The X-ray fluorescence measurement method for establishing the content of metal elements in a tempered salt according to claim 7, wherein the metal element components in the tempered salt to be measured comprise one or a combination of more of potassium nitrate, sodium nitrate, calcium nitrate and magnesium nitrate.
9. The method for X-ray fluorescence measurement of establishing the content of metal elements in a tempered salt according to claim 7, wherein the mass ratio of the lithium tetraborate to the silicon dioxide in the mixed flux is 20-5: 1.
10. the X-ray fluorescence measuring method for establishing the content of metal elements in the tempered salt according to claim 7, wherein in the mixed sample, the mass ratio of the mixed fluxing agent to the tempered salt sample to be measured is 30-8: 1.
11. the method according to any one of claims 7 to 10, wherein a release agent is applied to the surface of the mixed sample before the sample is melted at a high temperature, wherein the release agent is lithium bromide.
12. The method according to any one of claims 7 to 10, wherein the high temperature melting parameters comprise: standing for 120-160 s, standing for 100-150 s, primary swing time for 5-20 s, secondary swing time for 5-20 s, and melting temperature for 930-1200 ℃.
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