CN114486970B - X-ray fluorescence determination method for metal element content in tempered salt - Google Patents
X-ray fluorescence determination method for metal element content in tempered salt Download PDFInfo
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Abstract
The invention discloses an X-ray fluorescence measurement method for metal element content in toughened salt, which relates to a detection method in the glass manufacturing field, wherein 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 tempered 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 tempered salt and the corresponding X-ray fluorescence intensity, and establishing a content-X-ray fluorescence intensity standard working curve. The invention utilizes the X-ray fluorescence spectrometry to effectively reduce the consumption of the fluxing agent in the process of preparing the sample glass sheet of the toughened salt, successfully realizes the detection of the content of the metal element in the toughened salt, has high efficiency in the process and reliable results.
Description
Technical Field
The invention relates to a detection method in the glass manufacturing field, in particular to an X-ray fluorescence measurement method for the content of metal elements in tempered salt.
Background
The tempering process is an important part of glass manufacturing. In the tempering process, if the proportion of the metal element components of the tempered salt does not meet the requirement, the mechanical strength and the pressure resistance of the tempered glass are low, and even the glass is subject to self-explosion, so that the timely detection of the content of each metal element component of the tempered salt is of great significance in the glass production.
The main metal elements of the toughened salt comprise potassium nitrate, sodium nitrate, calcium nitrate and magnesium nitrate, and the traditional detection method is a chemical detection method at present. Wherein the potassium content is detected by adopting a tetraphenylboron potassium precipitation method, and the potassium, calcium and magnesium contents are detected by adopting an atomic absorption spectrum or a plasma emission spectrum method. The tetraphenylboron potassium precipitation method has the advantages of expensive reagents, easy environmental pollution caused by detection of experimental waste liquid, long detection period, high requirements on the operation technical level of detection personnel, complicated detection steps and easy incomplete precipitation errors. When the atomic absorption spectrum or the plasma emission spectrum method is used for detecting the content of potassium, calcium and magnesium, the sample is required to be diluted to reach the detection limit, the dilution times are often up to 5000 times, and the error of the detection result is larger. The detection method is difficult to meet the detection requirement of toughened salt in the glass manufacturing field.
In addition, the method for measuring the content of potassium and sodium elements in the industrial potassium nitrate by utilizing an X-ray fluorescence spectrometry is simple in sample treatment, free of loss and environmental pollution, and is an automatic measuring method with high efficiency and high reliability. When the method is used, the sample to be detected and the fluxing agent are required to be mixed first, and the mixed sample glass sheet for detection is obtained after melting. The content of the fluxing agent used in the melting process is higher, and when the content of the fluxing agent is less than 15 times of the mass of the potassium nitrate, the molten glass sheet is easy to break and devitrify, and subsequent detection cannot be carried out. Meanwhile, the high flux content 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 measurement method for the content of metal elements in toughened salt, which can reduce the dosage content of fluxing agent, has 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 measurement method for metal element content in tempered salt, comprising the following steps: preparing a plurality of groups of standard samples with different concentrations by adopting standard samples of metal element components in tempered 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 tempered salt and the corresponding X-ray fluorescence intensity, and establishing a content-X-ray fluorescence intensity standard working curve.
In one embodiment, the tempered salt component is selected from 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 of the mixed fluxing agent and the standard sample is 30-8: 1.
in one embodiment, a release agent, which is lithium bromide, is applied to the surface of the mixed sample prior to high temperature melting.
In one embodiment, the parameters of the high temperature melt sample include: the standing pre-melting time is 120-160 s, the standing pause time is 100-150 s, the primary swing time is 5-20 s, the secondary swing time is 5-20 s, and the melting temperature is 930-1200 ℃.
An X-ray fluorescence measurement method for the content of metal elements in tempered salt comprises the following steps: mixing lithium tetraborate and silicon dioxide to prepare a mixed fluxing agent; mixing the mixed fluxing agent with a toughened salt sample to be tested to prepare a mixed sample; adding a release agent, melting the mixed sample at a high temperature, and cooling to obtain a sample glass sheet to be tested; and carrying out X fluorescence spectrum detection on the glass sheet of the sample to be detected, and obtaining the content of the metal element 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 measured includes 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 tested is 30-8: 1.
in one embodiment, a release agent, which is lithium bromide, is applied to the surface of the mixed sample prior to high temperature melting.
In one embodiment, the parameters of the high temperature melt sample are: the standing pre-melting time is 120-160 s, the standing pause time is 100-150 s, the primary swing time is 5-20 s, the secondary swing time is 5-20 s, and the melting temperature is 930-1200 ℃.
The invention has the beneficial effects that: according to the invention, the lithium tetraborate and the silicon dioxide are used as the mixed fluxing agent in the process of preparing the sample glass sheet of the toughened salt by utilizing an X-ray fluorescence spectrometry, so that the consumption of the fluxing agent is effectively reduced, the phenomena of fracture and crystallization of the sample glass sheet of the toughened salt when the consumption of the fluxing agent 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, and the loss and the pollution are avoided.
In addition, the method can be used for simultaneously detecting the contents of potassium, sodium, calcium and magnesium elements in the toughened 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 metal element Mg of example 1.
Detailed Description
The present invention will be described more fully hereinafter in order to facilitate an understanding of the present invention. Preferred embodiments of the present invention are given below. 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 herein in the description of the invention 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 ranges are referred to as continuous, and include the minimum and maximum values of the ranges, 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 description 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 include any and all subranges subsumed therein.
In the present invention, the percentages refer to mass percentages for both solid-liquid and solid-solid phase mixtures and volume percentages for liquid-liquid phase mixtures unless otherwise specified.
In the present invention, the percentage concentrations referred to refer to the final concentrations unless otherwise specified. The final concentration refers to the ratio of the additive component in the system after the component is added.
In the present invention, the temperature parameter is not particularly limited, and it is permissible to perform the constant temperature treatment or to perform the treatment within a predetermined 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 metal element content in tempered 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 tempered 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 tempered salt and the corresponding X-ray fluorescence intensity, and establishing a content-X-ray fluorescence intensity standard working curve.
In one example, the tempered 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 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 silicon dioxide 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 conditions of thermal decomposition or severe splashing of the sample can be avoided in the reaction melting process. Specifically, the mass ratio of the mixed fluxing agent to the standard sample includes, but is not limited to: 30: 1. 25: 1. 20: 1. 15: 1. 10: 1. 8:1.
further, a release agent is applied prior to the surface of the mixed sample prior to high temperature melting.
Without limitation, the release agent comprises lithium bromide.
In one embodiment, the parameters of the high temperature melt are: the standing pre-melting time is 120-160 s, the standing pause time is 100-150 s, the primary swing time is 5-20 s, the secondary swing time is 5-20 s, and the melting temperature is 930-1200 ℃.
In one embodiment, the test parameters of the X-ray fluorescence spectrometer are: component K test parameters: spectral line K-Ka, voltage 30kV, current 80mA, crystal LiF200, detector FPC, collimator 0.4, angle 136.684, time 24s; component Na test parameters: spectral line Na-Ka, voltage 30kV, current 80mA, crystal LiF200, detector FPC, collimator 1, angle 45.591 and time 24s; component Ca test parameters: spectral line Ca-Ka, voltage 30kV, current 80mA, crystal AX03, detector FPC, collimator 0.4, angle 113.086 and time 40s; component Mg test parameters: spectral line Mg-Ka, voltage 30kV, current 80mA, crystal AX03, detector FPC, collimator 1, angle 37.535 and time 40s.
The invention provides an X-ray fluorescence measurement method for the content of metal elements in tempered 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 toughened salt sample to be tested to prepare a mixed sample; melting the mixed sample at a high temperature, and cooling to obtain a glass sheet of a sample to be detected; and carrying out X fluorescence spectrum detection on the glass sheet of the sample to be detected, and obtaining the content of the metal element in the toughened salt sample to be detected according to the established standard curve.
In one example, the sample composition 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 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 silicon dioxide 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 conditions of thermal decomposition or severe splashing of the sample can be avoided in the reaction melting process. Specifically, the mass ratio of the mixed fluxing agent to the toughened salt sample to be tested includes but is not limited to: 30: 1. 25: 1. 20: 1. 15: 1. 10: 1. 8:1.
further, a release agent is applied prior to the surface of the mixed sample prior to high temperature melting.
Without limitation, the release agent comprises lithium bromide.
In one embodiment, the high temperature melt sample set parameters are: the standing pre-melting time is 120-160 s, the standing pause time is 100-150 s, the primary swing time is 5-20 s, the secondary swing time is 5-20 s, and the melting temperature is 930-1200 ℃.
In one embodiment, the test parameters of the X-ray fluorescence spectrometer are: component K test parameters: spectral line K-Ka, voltage 30kV, current 80mA, crystal LiF200, detector FPC, collimator 0.4, angle 136.684, time 24s; component Na test parameters: spectral line Na-Ka, voltage 30kV, current 80mA, crystal LiF200, detector FPC, collimator 1, angle 45.591 and time 24s; component Ca test parameters: spectral line Ca-Ka, voltage 30kV, current 80mA, crystal AX03, detector FPC, collimator 0.4, angle 113.086 and time 40s; component Mg test parameters: spectral line Mg-Ka, voltage 30kV, current 80mA, crystal AX03, detector FPC, collimator 1, angle 37.535 and time 40s.
The following are specific examples.
The X-ray fluorescence spectrometer used in the embodiment of the invention is an ARL Performance' X4200 type X-ray fluorescence spectrometer manufactured by Simer Feishi technologies (China).
Example 1
1. 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) are dried at 110 ℃ for standby;
2. mixing potassium nitrate, sodium nitrate, calcium nitrate and magnesium nitrate in the step 1 together to prepare standard samples, and respectively preparing 5.05g standard series samples No. 1, no. 2, no. 3, no. 4, no. 5 and No. 6, wherein the preparation parameters of the standard samples are shown in Table 1;
table 1: series of formulation parameters table for Standard sample of example 1
3. Lithium tetraborate and silica were mixed according to 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#5.5000g in the step 2, placing the mixture in a platinum yellow crucible, and uniformly stirring;
5. dropwise adding 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 melter for sample melting, wherein sample melting parameters of the high-temperature sample melter are shown in a toughened salt sample melting parameter setting table in Table 2; after finishing sample melting through a high-temperature sample melting machine, taking out the platinum yellow crucible, and naturally cooling and demoulding to obtain a standard sample glass sheet 1#;
table 2: example 1 melt sample procedure parameter set table
7. And (5) repeating the steps 4-6 to obtain standard sample glass sheets No. 2, no. 3, no. 4, no. 5 and No. 6 respectively. The contents of potassium, sodium, calcium and magnesium in each standard sample are calculated as shown in Table 3;
table 3: table for correspondence of standard sample glass sheet component content conversion data in example 1
8. Recording component content of a standard sample glass sheet on an X-ray fluorescence spectrometer, and testing corresponding intensity, wherein the measurement conditions of the X-ray fluorescence spectrometer are shown in table 4;
table 4: measurement condition table of X-ray fluorescence spectrometer
9. And establishing a content-X-ray fluorescence intensity standard working curve according to the content of the glass sheet component of the standard sample and corresponding intensity data obtained by an X-ray fluorescence spectrometer, wherein the results are shown in figures 1-4.
Example 2
1. Lithium tetraborate and silica were mixed according to 10:1, fully and uniformly mixing in a corundum crucible mortar to form a mixed fluxing agent;
2. accurately weighing 5.5000g of the standard sample 2# in the step 2 of the example 1 and 7.7000g of the mixed fluxing agent, placing the mixture into a platinum yellow crucible, and uniformly stirring;
3. dropwise adding 300 mu L of 300g/L 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 melter for sample melting, wherein sample melting parameters of the high-temperature sample melter are shown in a toughened salt sample melting parameter setting table in Table 5; after finishing sample melting through a high-temperature sample melting machine, taking out the platinum yellow crucible, and naturally cooling and demoulding to obtain a standard sample glass sheet No. 2;
table 5: fusion sample program parameter setting table
5. Placing a glass sheet 2# of a sample to be detected in a sample box of an X-ray fluorescence spectrometer, starting a quantitative analysis program, and testing the corresponding intensity, wherein the measurement conditions of the X-ray fluorescence spectrometer are shown in Table 6;
table 6: measurement condition table of X-ray fluorescence spectrometer
6. According to the content-intensity standard working curve established in example 1, the content of each element to be measured was automatically calculated by a computer, and the comparison result of the detection result with the conventional chemical method is shown in Table 7. From the detection results in table 7, it can be seen that the result errors of the two detection methods of the invention and the chemical method are within a reasonable range, which proves that the method of the invention is stable and reliable.
Table 7: comparing the method with the detection result of the conventional chemical method
Example 3
And detecting a tempered salt sample in the chemical tempering furnace.
1. Taking about 50g of toughened salt in a chemical toughening furnace, placing a cooled toughened salt sample in a corundum crucible, grinding to less than 0.01 mu m, transferring to a weighing bottle, drying at 110 ℃ for 2h, taking out, and naturally cooling for later use;
2. lithium tetraborate and silica were mixed according to 10:1, fully and uniformly mixing in a corundum crucible mortar to form a mixed fluxing agent;
3. accurately weighing 5.5000g of the tempered salt sample and 7.7000g of the mixed fluxing agent in the step 1, placing the tempered salt sample and the mixed fluxing agent in a platinum yellow crucible, and uniformly stirring;
4. dropwise adding 300 mu L of 300g/L 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 melter for sample melting, wherein sample melting parameters of the high-temperature sample melter are shown in a toughened salt sample melting parameter setting table in Table 8; after finishing sample melting through a high-temperature sample melting machine, taking out the platinum yellow crucible, naturally cooling and demoulding to obtain a toughened salt sample glass sheet to be tested;
table 8: fusion sample program parameter setting table
6. Placing a glass sheet of a sample to be tested in a sample box of an X-ray fluorescence spectrometer, starting a quantitative analysis program, and testing the corresponding intensity, wherein the measurement conditions of the X-ray fluorescence spectrometer are shown in Table 9;
table 9: measurement condition table of X-ray fluorescence spectrometer
7. According to the content-X-ray fluorescence intensity standard working curve established in example 1, the content of each element to be measured 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 tempered salt: sodium nitrate: calcium nitrate: the theoretical mass ratio of magnesium nitrate is 100:100:1:1, converted to potassium: sodium: calcium: the percentages of magnesium metal elements are 19.14%, 13.39%, 0.0084% and 0.0081%, respectively. From table 10, it can be seen that the errors of the detection result and the theoretical value of the invention are within a reasonable range, which indicates that the method of the invention is stable and reliable.
Table 10: comparison table of detection results and theoretical values of tempered salt samples
Example 4
Determination of potassium nitrate and sodium nitrate tempered salts
1. Potassium nitrate and sodium nitrate were combined in 1: mixing evenly in a mass ratio, and drying and cooling at 110 ℃ for later use, namely toughened salt A;
2. lithium tetraborate and silica were mixed according to 20:1, fully and uniformly mixing in a corundum crucible mortar to form a mixed fluxing agent;
3. accurately weighing 10.0000g of the mixed fluxing agent in the step 2 and 1.0000g of the toughened salt in the step 1, placing the materials in a platinum yellow crucible, and uniformly stirring;
4. dropwise adding 300 mu L of 300g/L 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 melter for sample melting, wherein sample melting parameters of the high-temperature sample melter are shown in a table 2 toughened salt sample melting parameter setting table in the embodiment 1; after the sample melting is finished through a high-temperature sample melting machine, taking out the platinum yellow crucible, naturally cooling and demoulding to obtain a sample glass sheet, wherein the effect of the sample glass sheet is shown in Table 11;
6. detection of tempered salt sample to be detected
And detecting the melted glass sheet of the sample to be detected on an X-ray fluorescence spectrometer according to the established standard working curve.
Example 5
The operating method of example 5 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 10:1, the effect of the sample glass sheet is shown in Table 11.
Example 6
The operating method 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 is shown in Table 11.
Comparative example 1
The operation method 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, the traditional fluxing agent is a mixture of lithium tetraborate and lithium metaborate in a mass ratio of 67:33, and the effect and the detection result of the sample glass sheet are shown in Table 11.
Table 11: comparison table of melting effect
As is clear from Table 11, the molten sample pieces of examples 4 to 6 were all significantly higher in mass than comparative example 1, indicating that the X-ray fluorescence measurement method of the metal element content in the tempered salt of the present invention was more effective. Specifically, from the experimental results of example 4 and comparative example 1 (the ratio of the fluxing agent to the toughened salt to be measured is 10:1, and only the fluxing agent components are different), it can be seen that the addition of the mixed fluxing agent in the invention can significantly improve the quality of the molten sample glass sheet, while the molten glass sheet in comparative example 1 has fracture and crystallization phenomena, 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 and silicon dioxide in the mixed fluxing agent is 20:1 to 5:1, the glass sheet of the molten sample has clear appearance and stable quality, and is suitable for the subsequent X-ray fluorescence measurement of the content of metal elements in the tempered salt.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (4)
1. A method for establishing a standard curve in an X-ray fluorescence measurement method for metal element content in tempered salt, which 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 tempered 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; performing X-ray fluorescence spectrum detection on the standard sample glass sheet, recording the content of metal element components in the tempered salt and the corresponding X-ray fluorescence intensity, and establishing a content-X-ray fluorescence intensity standard working curve;
the metal element component in the toughened salt is selected from one or a combination of more of potassium nitrate, sodium nitrate, calcium nitrate and magnesium nitrate;
in the mixed fluxing agent, the mass ratio of the lithium tetraborate to the silicon dioxide is 20-5: 1, a step of;
in the mixed sample, the mass ratio of the mixed fluxing agent to the standard sample is 30-8: 1, a step of;
and before high-temperature sample melting, a release agent is applied to the surface of the mixed sample, wherein the release agent is lithium bromide or ammonium iodide.
2. The method for establishing a standard curve in an X-ray fluorescence measurement method of a metal element content in a tempered salt according to claim 1, wherein the parameters of the high temperature melting sample include: the pre-melting time is 120-160 s, the standing pause time is 100-150 s, the primary swing time is 5-20 s, the secondary swing time is 5-20 s, and the melting temperature is 930-1200 ℃.
3. An X-ray fluorescence measurement method for the content of metal elements in tempered 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 toughened salt sample to be tested to prepare a mixed sample; melting the mixed sample at a high temperature, and cooling to obtain a glass sheet of a sample to be detected; performing X fluorescence spectrum detection on the glass sheet of the sample to be detected, and obtaining the content of metal elements in the tempered salt sample to be detected according to the standard curve established by the method of any one of claims 1-2;
the metal element components in the toughened salt to be detected comprise one or a combination of more of potassium nitrate, sodium nitrate, calcium nitrate and magnesium nitrate;
in the mixed fluxing agent, the mass ratio of the lithium tetraborate to the silicon dioxide is 20-5: 1, a step of;
in the mixed sample, the mass ratio of the mixed fluxing agent to the toughened salt sample to be detected is 30-8: 1, a step of;
and before high-temperature melting, a release agent is applied to the surface of the mixed sample, wherein the release agent is lithium bromide.
4. The method for establishing a content of a metal element in a tempered salt according to claim 3, wherein the high temperature melting parameters include: the pre-melting time is 120-160 s, the standing pause time is 100-150 s, the primary swing time is 5-20 s, the secondary swing time is 5-20 s, and the melting temperature is 930-1200 ℃.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590255A (en) * | 2012-02-29 | 2012-07-18 | 成都中光电科技有限公司 | Method for detecting main content of glass raw material |
| CN104280367A (en) * | 2013-10-31 | 2015-01-14 | 东旭集团有限公司 | Method for efficiently and accurately detecting content of silicon dioxide in quartz sand |
| CN112179930A (en) * | 2020-08-26 | 2021-01-05 | 中铝郑州有色金属研究院有限公司 | Method for measuring contents of nine substances in high-sulfur bauxite by X-ray fluorescence spectrometry |
| CN113092510A (en) * | 2021-03-18 | 2021-07-09 | 成都中光电科技有限公司 | X-fluorescence determination method for potassium nitrate as high-alumina glass raw material |
| CN113800766A (en) * | 2021-03-05 | 2021-12-17 | 赣州海发中空玻璃工程有限公司 | Toughened special glass and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590255A (en) * | 2012-02-29 | 2012-07-18 | 成都中光电科技有限公司 | Method for detecting main content of glass raw material |
| CN104280367A (en) * | 2013-10-31 | 2015-01-14 | 东旭集团有限公司 | Method for efficiently and accurately detecting content of silicon dioxide in quartz sand |
| CN112179930A (en) * | 2020-08-26 | 2021-01-05 | 中铝郑州有色金属研究院有限公司 | Method for measuring contents of nine substances in high-sulfur bauxite by X-ray fluorescence spectrometry |
| CN113800766A (en) * | 2021-03-05 | 2021-12-17 | 赣州海发中空玻璃工程有限公司 | Toughened special glass and preparation method thereof |
| CN113092510A (en) * | 2021-03-18 | 2021-07-09 | 成都中光电科技有限公司 | X-fluorescence determination method for potassium nitrate as high-alumina glass raw material |
Non-Patent Citations (1)
| Title |
|---|
| 李韶梅 ; 杜彩霞 ; 张慧娟 ; .X射线荧光光谱法测定萤石中氟化钙、二氧化硅、氧化铝、全铁的含量.理化检验(化学分册).2011,第47卷(第10期),第1162-1164页. * |
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