CN113155879A - Method for measuring contents of silicon dioxide and calcium fluoride in fluorite - Google Patents
Method for measuring contents of silicon dioxide and calcium fluoride in fluorite Download PDFInfo
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- CN113155879A CN113155879A CN202110110972.6A CN202110110972A CN113155879A CN 113155879 A CN113155879 A CN 113155879A CN 202110110972 A CN202110110972 A CN 202110110972A CN 113155879 A CN113155879 A CN 113155879A
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Abstract
The invention provides a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite, which adopts an X fluorescence fuse method for measurement and specifically comprises the following steps: 1) drawing a standard curve; (2) sample pretreatment: weighing a fluorite sample to be detected, putting the fluorite sample into a glass beaker, adding acetic acid to dissolve and filtering; (3) fusing sheet: taking a platinum crucible, adding a flux and a viscosity reducer into the platinum crucible, putting the filter residue obtained by filtering in the step (2) and filter paper into the platinum crucible, putting the platinum crucible into a muffle furnace at 800 ℃ to ash the filter paper, and putting the filter paper into a sample melting furnace to melt a sample after the filter paper is ashed; adding a release agent before demolding, rotationally shaking, cooling and demolding to prepare a glass sheet for analysis; (4) the measurement was carried out by X-ray fluorescence spectrometer. The method provided by the invention can directly measure the contents of silicon dioxide and calcium fluoride in fluorite, the platinum crucible is not corroded in the sample melting stage, and the prepared sample wafer has high quality and high accuracy and precision.
Description
Technical Field
The invention relates to a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite, belonging to the technical field of physicochemical detection.
Background
In the ferrous metallurgy industry, fluorite is mainly used as a flux to improve the fluidity of slag, reduce inclusions in molten steel and improve the quality of the molten steel. The steel production enterprises need to perform chemical analysis on fluorite in the aspect of raw material quality control. According to the national standard GB/T5195.1-2006, the content of silicon dioxide and calcium fluoride is determined by adopting the traditional wet chemical analysis, the operation is complex, the number of steps is large, the data accuracy is easily influenced by errors in operation, and the accuracy and the stability of the analysis result are often influenced by the experience and the level of operators. Large modern analytical instruments such as an X-ray fluorescence spectrometer and the like are widely applied to metallurgical chemical analysis, and are gradually popularized and applied in the field of ferroalloy analysis in recent years, but fluorite not only contains silicon dioxide and calcium fluoride, but also contains a small amount of magnesium fluoride and calcium carbonate, and particularly fluorite used in the steel industry has poor quality and high calcium carbonate content.
Currently, there are two approaches to XRF methods for fluorite determination: first, a tablet press method XRF method is used for measuring silicon dioxide and calcium fluoride in fluorite, and a spectrum line for measuring a silicon element and a spectrum line for measuring a fluorine element are selected. The accuracy is not good due to the influence of mineral effect and granularity effect, and the interference of magnesium fluoride cannot be removed by measuring the content of calcium fluoride by measuring fluorine element. Secondly, measuring silicon dioxide and calcium fluoride in fluorite by a fuse-link method XRF method, selecting a spectral line for measuring silicon element and a spectral line for measuring fluorine element, wherein the measuring method of silicon dioxide has no problem, but fluorine element is volatile in the high-temperature melting process, the temperature rise speed, the temperature and the melting time must be strictly controlled in the process of preparing a molten sample, the requirement on a molten sample furnace is higher, the measurement of fluorine content is seriously influenced by carelessness, and the interference of magnesium fluoride on calcium fluoride cannot be removed; thirdly, measuring silicon dioxide and calcium fluoride in fluorite by a fuse link method XRF method, selecting a spectral line for measuring a silicon element and a spectral line for measuring a calcium element to obtain the content of the silicon dioxide and the total amount of the calcium fluoride and the calcium in the calcium carbonate, measuring the content of the calcium existing in the form of the calcium carbonate in the sample by other methods, subtracting the amount of the calcium in the calcium carbonate from the total amount of the calcium to obtain the amount of the calcium in the calcium fluoride, and converting the amount of the calcium fluoride, wherein the method is complex and tedious to operate.
According to the invention, firstly, a sample is subjected to chemical treatment, calcium carbonate and magnesium carbonate in the sample are removed, so that silicon dioxide and calcium fluoride in the fluorite sample are completely reserved, then the fluorite sample is melted into a qualified glass sample, silicon and calcium in the sample are tested in an XRF mode, and accurate results of the silicon dioxide and the calcium fluoride can be directly obtained.
Disclosure of Invention
The invention aims to provide a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite by adopting an X fluorescence fuse link method, which can directly measure the contents of the silicon dioxide and the calcium fluoride without measuring the content of calcium carbonate, ensures that a platinum crucible is not corroded, ensures that the accuracy and precision of a measurement result meet the requirements, and improves the analysis efficiency.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite adopts an X fluorescence fuse method for measurement, and specifically comprises the following steps:
(1) drawing a standard curve
Preparing a plurality of standard samples with different contents of silicon dioxide and calcium fluoride by using fluorite standard substances, spectrally pure reagent silicon dioxide and calcium carbonate; when the standard sample contains the fluorite standard substance, dissolving the fluorite standard substance by acetic acid and filtering to remove calcium carbonate in the fluorite standard substance;
taking a platinum crucible, adding a fusing agent and a viscosity reducer into the platinum crucible, then adding a standard sample, and placing the standard sample in a sample melting furnace for melting; adding a release agent before demolding, rotationally shaking, cooling and demolding to prepare a glass sheet for analysis;
testing the intensity value of the main element in the standard sample by using an X-ray fluorescence spectrometer, and drawing a working curve by using the content of silicon dioxide or calcium fluoride as a horizontal coordinate and the intensity value as a vertical coordinate;
(2) sample pretreatment
Weighing a fluorite sample to be detected, putting the fluorite sample into a glass beaker, adding acetic acid to dissolve and filtering;
(3) fusing sheet:
taking a platinum crucible, adding a flux and a viscosity reducer into the platinum crucible, putting the filter residue obtained by filtering in the step (2) and filter paper into the platinum crucible, putting the platinum crucible into a muffle furnace at 800 ℃ to ash the filter paper, and putting the filter paper into a sample melting furnace to melt a sample after the filter paper is ashed; adding a release agent before demolding, rotationally shaking, cooling and demolding to prepare a glass sheet for analysis;
(4) measurement of
And (3) measuring the intensity values of the silicon dioxide and the calcium fluoride in the sample under the same test conditions as the standard sample by using an X-ray fluorescence spectrometer, and then reading the content of the silicon dioxide and the calcium fluoride in the sample according to a standard curve.
The invention relates to a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite, which comprises the following steps: the standard sample and the sample to be detected have the same matrix type, and the granularity needs to reach 200 meshes.
The invention relates to a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite, which comprises the following steps: the sample weighing amount of the standard sample and the sample in the step (1) and the step (2) is 0.2-1.0 g.
The invention relates to a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite, which comprises the following steps: the specific operation of dissolving the fluorite standard substance or dissolving the sample to be tested by acetic acid in the step (1) and the step (2) is as follows: placing a fluorite standard substance or a sample to be tested in a beaker, adding 20ml of dilute acetic acid with the concentration of 10%, and heating to keep micro-boiling for 30 minutes; adding 20ml of water into the beaker, heating, shaking up, filtering with medium-speed quantitative filter paper, and repeatedly washing the filter residue and the filter paper for more than 3 times.
The invention relates to a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite, which comprises the following steps: the flux in the step (1) and the step (3) is pure anhydrous lithium tetraborate, or a mixed flux of lithium tetraborate and lithium metaborate with a mass ratio of 67:33, or a mixed flux of lithium tetraborate, lithium metaborate and lithium fluoride with a mass ratio of 65:25:10, or a mixed flux formed by the fluxes in any proportion, and the addition amount of the flux is 10-20 times of that of a standard sample or a sample to be tested.
The invention relates to a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite, which comprises the following steps: the viscosity reducer in the step (1) and the step (3) can be potassium bromide, lithium bromide, potassium iodide or lithium iodide, the addition amount of the viscosity reducer is based on proper melt fluidity, and the old and new degree of a platinum crucible and the melt viscosity at the melt temperature are considered. Generally 0.2-0.5g of viscosity reducer can meet the requirement.
The invention relates to a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite, which comprises the following steps: the release agent in the step (1) and the step (3) is ammonium iodide, and the addition amount of the release agent is 0.2-0.5 g.
The invention relates to a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite, which comprises the following steps: in the step (1) and the step (3), the sample melting temperature of the sample melt is 1050-.
The invention relates to a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite, which comprises the following steps: in the step (1) and the step (3), the specific conditions of the sample melting are as follows: the sample melting temperature is 1050 ℃, the heat preservation time is 700s, the swing speed is 100 percent, and the swing angle is 45 degrees.
The invention relates to a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite, which comprises the following steps: the working parameters of the X-ray fluorescence spectrometer are as follows:
CaF2: the test spectral line is Ca-Kalpha, the detector is selected to be FPC, the voltage of a light pipe is 30kV, the current of the light pipe is 80mA, the spectroscopic crystal LiF is 200, the collimator is 0.60, the PHD range is 40-100, and the counting time is 20 s.
SiO2: the test spectral line is Si-K alpha, the detector is selected to be FPC, the voltage of a light pipe is 30kV, the current of the light pipe is 80mA, the spectroscopic crystal PET is 0.60, the PHD range is 40-100, and the counting time is 20 s.
The invention provides a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite through a large number of tests and repeated demonstration, and adopts a series of measures such as weak organic acid sample dissolution, filtering and washing, melting condition optimization, X fluorescence analysis and the like, thereby achieving the purposes of good repeatability and high accuracy of sample analysis, not corroding a platinum crucible, and the analysis result of the sample reaches the precision requirement in the related national chemical analysis standard.
Through a large number of tests, the concentration of acetic acid is preferably 20ml and 10%, the volume of the acetic acid can ensure that the acetic acid is not evaporated to dryness in the process of dissolving a sample, and carbonate in the sample can be completely dissolved. The sample melting temperature in the sample melting operation is preferably over 1050 ℃, the filter paper wrapping filter residues can be removed by carbonization and combustion in the sample melting process, the sample piece is prevented from being cracked due to scum with carbon components on the sample piece, and the sample piece can be ensured to be uniform by determined heat preservation and swinging time. The quality of the finally formed sample wafer is high, the platinum crucible is not corroded in the melting process, and no residue is left on the inner wall of the platinum crucible finally.
The key innovative technology of the invention is as follows: 1) in the sample treatment process, the carbonate in the sample is dissolved by acetic acid and removed in a filtering mode, so that calcium in the sample can represent calcium fluoride, the content of calcium carbonate in the sample does not need to be analyzed, and the analysis operation is reduced. 2) The sample wafer is melted at the temperature of not less than 1050 ℃, the filter paper is burnt and removed in the sample melting process, the finally obtained sample wafer has no carbon slag, the glass wafer can be manufactured with high quality, the platinum crucible has no corrosion risk, the method has high efficiency and the operation is simple and convenient.
Compared with the existing chemical analysis technology, the method has the advantages that the sample is only melted and filtered once, and the fuse piece can be used for testing by the X-ray fluorescence spectrometer to directly obtain the content of silicon dioxide and calcium fluoride once, so that the complexity of the analysis process is effectively reduced, and errors caused by different operators in mastering titration end points are also reduced. The whole analysis period is short, the operation steps are few, the rapid, accurate and environment-friendly measurement requirements are met, the risk that the platinum crucible is corroded is avoided, and the analysis result of the sample meets the precision requirement in the related national chemical analysis standard.
The invention has the beneficial effects that:
the invention innovatively discloses a method for measuring the contents of silicon dioxide and calcium fluoride in fluorite, and utilizes an X fluorescence fuse technology to optimize a sample treatment process, so that the method has no corrosion risk of a platinum crucible, ensures that the accuracy and precision of a measurement result meet requirements, and has high efficiency; according to the invention, the glass fuse piece which can be used for X fluorescence spectrum analysis is prepared by borate high-temperature melting, the quality of the glass sample piece is ensured by adjusting the adding time of the release agent, and the determination of the contents of silicon dioxide and calcium fluoride in fluorite can be rapidly and accurately completed by an X fluorescence fuse piece method; the method can replace the currently and generally used chemical analysis method, has the advantages of short analysis period, few operation steps, accurate and reliable analysis result and the like, and can be popularized and applied to fluorite acceptance of all steel enterprises in the metallurgical industry and the like.
Detailed Description
The method mainly provides a method for stably and reproducibly measuring the contents of silicon dioxide and calcium fluoride in fluorite, and the basic principle is that acetic acid reacts with calcium carbonate in a sample to generate water-soluble calcium acetate, calcium existing in the sample in the form of calcium carbonate is removed in a filtering mode, and then the treated sample and a flux are melted to prepare a glass sample wafer for X fluorescence test. And (3) adding a release agent at a proper time in the process of melting the sample wafer to ensure the final release quality, and finally analyzing chemical components by using an X-ray fluorescence spectrometer. The method has the advantages of simple, rapid, safe and reliable process, no corrosion to the platinum crucible in the whole sample processing process, no sample residue on the platinum crucible after demoulding, no interference to the manufacture of the next sample wafer, accurate analysis result and better precision.
(1) Drawing a standard curve
1.1 preparation of Standard samples
Drying a fluorite standard substance, spectrally pure reagents of silicon dioxide and calcium carbonate for one hour at 105 ℃, and then putting the dried fluorite standard substance, spectrally pure reagents of silicon dioxide and calcium carbonate into a dryer for cooling for later use; accurately weighing fluorite standard substances, silicon dioxide and calcium carbonate according to the table 1, and preparing standard samples with different silicon dioxide and calcium contents (calcium is converted into calcium fluoride); .
TABLE 1 Fluorite Standard specimen Table
1.2 Standard sample pretreatment
The fluorite standard substance contains carbonate, and is removed by adopting a mode of dissolving acetic acid and filtering, and the specific operation is as follows:
label 1, label 2, label 3: putting the weighed fluorite standard substance into a 100ml glass beaker, adding 20ml of 10% acetic acid solution, heating to boil, and keeping slight boiling for 30 minutes; adding 20ml of water into the beaker, heating, slightly cooling, filtering with medium-speed quantitative filter paper, and washing the filter paper and filter residue with warm water for more than 3 times;
label 7, label 8, label 9: putting the weighed fluorite standard substance into a 100ml glass beaker, adding 20ml of 10% acetic acid solution, heating to boil, and keeping slight boiling for 30 minutes; adding 20ml of water into a beaker, heating, slightly cooling, filtering with medium-speed quantitative filter paper, washing the filter paper and filter residue with warm water for more than 3 times, and adding a corresponding amount of calcium carbonate into the filter residue;
1.3, melt sheet:
Sample melting conditions are as follows: the temperature is 1050 ℃, the heat preservation time is 720s, the swing speed is 100 percent, and the swing angle is 45 degrees; adding a release agent ammonium iodide into a platinum crucible, wherein the adding amount of the ammonium iodide is 0.2-0.5g, continuously rotating and swinging for 120s without accurate weighing, taking out the platinum crucible, standing, cooling to room temperature, and demolding to finish manufacturing of a glass sample wafer;
1.4, drawing a working curve: according to the working curve establishing step of the X-ray fluorescence spectrometer, a Ca-K a spectral line and a Si-K a spectral line are selected, analysis conditions are compiled, standard values of silicon dioxide and calcium fluoride in each standard sample are input, a standardization task is established, the glass sheets are sequentially placed into an analysis station to measure the strength values of required elements, the measured strength values and the standard values are established into a primary working curve, and the linear correlation coefficients of all the elements meet the analysis requirements;
working curve of silica: w = 0.7237I-0.3738R =0.9992
Working curve of calcium fluoride: w = 0.4539I-0.1663R =0.9984
(2) Sample pretreatment: processing a sample until the granularity reaches 200 meshes, accurately weighing 0.5000g of the sample, putting the sample into a 100ml glass beaker, adding 20ml of 10% acetic acid solution, heating to boil, and keeping slight boiling for 30 minutes; adding 20ml of water into the beaker, heating, slightly cooling, filtering with medium-speed quantitative filter paper, and washing the filter paper and filter residue with warm water for more than 3 times.
(3) Fusing sheet: adding a mixed flux prepared from 7 g of lithium tetraborate, 2 g of lithium tetraborate, lithium metaborate and lithium fluoride according to the mass ratio of 65:25:10 into a platinum crucible, folding the filter paper with the filter residue in the step (2) to a small volume, putting the filter paper into the platinum crucible, adding 0.2 g of potassium bromide, and putting the filter paper in a muffle furnace at 800 ℃ for ashing the filter paper. After ashing is finished, putting the sample into a sample melting machine for melting samples, wherein the sample melting conditions are as follows: the temperature is 1050 ℃, the heat preservation time is 720s, the swing speed is 100 percent, and the swing angle is 45 degrees; adding a release agent ammonium iodide into a platinum crucible, wherein the adding amount of the ammonium iodide is 0.2-0.5g, continuously rotating and swinging for 120s without accurate weighing, taking out the platinum crucible, standing, cooling to room temperature, and demolding to finish manufacturing of a glass sample wafer;
(4) and (3) determination: putting the melted sample into an X-ray fluorescence spectrometer, calling the drawn standard working curve to measure the sampleTesting to obtain SiO of corresponding sample2And CaF2And (4) content value.
And (3) precision test: randomly selecting a fluorite sample sent by a supplier, repeatedly melting 10 glass sheets according to the sample melting step, selecting the established working curve, and reading an analysis result, which is shown in the following table 2.
TABLE 2 precision test results of measuring silicon dioxide and calcium fluoride in fluorite by X fluorescence fuse method
As can be seen from Table 2, the novel method of the present invention has high stability and good precision of the test results.
And (3) accuracy test: randomly selecting 10 fluorite samples from suppliers from the site, and carrying out chemical analysis on the 10 samples by adopting national standards (the analysis result is shown in a method I in a table 3); the analysis was carried out by the method of the present invention (see method II in Table 3).
TABLE 3 comparison results
As can be seen from Table 3, the sample results obtained by the present invention are consistent with the results obtained by chemical methods and have high accuracy.
In conclusion, the method for determining the contents of silicon dioxide and calcium fluoride in fluorite provided by the invention is simple to operate, environment-friendly and safe, carbonate in a sample is dissolved by adopting acetic acid, carbon in filter paper can be completely removed through subsequent ashing and melting stages through filtering separation, and the quality of the sample wafer is ensured through reasonable adding time and adding amount of the release agent. The interference of magnesium fluoride and calcium carbonate in the sample is eliminated in the processing process of the sample, the risk of corroding a platinum crucible is avoided in the process of melting the sample, the current commonly used chemical analysis method can be replaced, the analysis accuracy and precision are good, and the analysis efficiency is high.
Claims (10)
1. A method for measuring the content of silicon dioxide and calcium fluoride in fluorite is characterized in that: the method adopts an X fluorescence fuse method for determination, and specifically comprises the following steps:
(1) drawing a standard curve
Preparing a plurality of standard samples with different contents of silicon dioxide and calcium by using fluorite standard substances, spectral pure reagent silicon dioxide and other calcium carbonate; when the standard sample contains the fluorite standard substance, dissolving the fluorite standard substance by acetic acid and filtering to remove calcium carbonate in the fluorite standard substance;
taking a platinum crucible, adding a fusing agent and a viscosity reducer into the platinum crucible, then adding a standard sample, and placing the standard sample in a sample melting furnace for melting; adding a release agent before demolding, rotationally shaking, cooling and demolding to prepare a glass sheet for analysis;
testing the intensity value of the main element in the standard sample by using an X-ray fluorescence spectrometer, and drawing a working curve by using the content of silicon dioxide or calcium fluoride as a horizontal coordinate and the intensity value as a vertical coordinate;
(2) sample pretreatment
Weighing a fluorite sample to be detected, putting the fluorite sample into a glass beaker, adding acetic acid to dissolve and filtering;
(3) fusing sheet:
taking a platinum crucible, adding a flux and a viscosity reducer into the platinum crucible, putting the filter residue obtained by filtering in the step (2) and filter paper into the platinum crucible, putting the platinum crucible into a muffle furnace at 800 ℃ to ash the filter paper, and putting the filter paper into a sample melting furnace to melt a sample after the filter paper is ashed; adding a release agent before demolding, rotationally shaking, cooling and demolding to prepare a glass sheet for analysis;
(4) measurement of
And (3) measuring the intensity values of the silicon dioxide and the calcium fluoride in the sample under the same test conditions as the standard sample by using an X-ray fluorescence spectrometer, and then reading the content of the silicon dioxide and the calcium fluoride in the sample according to a standard curve.
2. The method of claim 1, wherein the silica and calcium fluoride content of fluorite is determined by: the standard sample and the sample to be detected have the same matrix type, and the granularity needs to reach 200 meshes.
3. The method of claim 1, wherein the silica and calcium fluoride content of fluorite is determined by: the sample weighing amount of the standard sample and the sample in the step (1) and the step (2) is 0.2-1.0 g.
4. The method of claim 1, wherein the silica and calcium fluoride content of fluorite is determined by: the specific operation of dissolving the fluorite standard substance or dissolving the sample to be tested by acetic acid in the step (1) and the step (2) is as follows: placing a fluorite standard substance or a sample to be tested in a beaker, adding 20ml of dilute acetic acid with the concentration of 10%, and heating to keep micro-boiling for 30 minutes; adding 20ml of water into the beaker, heating, shaking up, filtering with medium-speed quantitative filter paper, and repeatedly washing the filter residue and the filter paper for more than 3 times.
5. The method of claim 1, wherein the silica and calcium fluoride content of fluorite is determined by: the flux in the step (1) and the step (3) is pure anhydrous lithium tetraborate, or a mixed flux of lithium tetraborate and lithium metaborate with a mass ratio of 67:33, or a mixed flux of lithium tetraborate, lithium metaborate and lithium fluoride with a mass ratio of 65:25:10, or a mixed flux formed by the fluxes in any proportion, and the addition amount of the flux is 10-20 times of that of a standard sample or a sample to be tested.
6. The method of claim 1, wherein the silica and calcium fluoride content of fluorite is determined by: the viscosity reducer in the step (1) and the step (3) can be potassium bromide, lithium bromide, potassium iodide or lithium iodide, the addition amount of the viscosity reducer is based on proper melt fluidity, and 0.2-0.5g of the viscosity reducer can meet the requirement in consideration of the old and new degree of a platinum crucible and the viscosity of a melt at a molten sample temperature.
7. The method of claim 1, wherein the silica and calcium fluoride content of fluorite is determined by: the release agent in the step (1) and the step (3) is ammonium iodide, and the addition amount of the release agent is 0.2-0.5 g.
8. The method of claim 1, wherein the silica and calcium fluoride content of fluorite is determined by: in the step (1) and the step (3), the sample melting temperature of the sample melt is 1050-.
9. The method of claim 1, wherein the silica and calcium fluoride content of fluorite is determined by: in the step (1) and the step (3), the specific conditions of the sample melting are as follows: the sample melting temperature is 1050 ℃, the heat preservation time is 700s, the swing speed is 100 percent, and the swing angle is 45 degrees.
10. The method of claim 1, wherein the silica and calcium fluoride content of fluorite is determined by: the working parameters of the X-ray fluorescence spectrometer are as follows:
CaF2: testing a spectral line Ca-Kalpha, selecting a detector FPC, a light tube voltage 30kV, a light tube current 80mA, a spectroscopic crystal LiF200, a collimator 0.60, a PHD range 40-100 and a counting time 20 s;
SiO2: the test spectral line is Si-K alpha, the detector is selected to be FPC, the voltage of a light pipe is 30kV, the current of the light pipe is 80mA, the spectroscopic crystal PET is 0.60, the PHD range is 40-100, and the counting time is 20 s.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113702411A (en) * | 2021-09-16 | 2021-11-26 | 福建贝思科电子材料股份有限公司 | Method for measuring molar ratio of calcium to zirconium in calcium zirconate |
| CN113702411B (en) * | 2021-09-16 | 2022-12-16 | 福建贝思科电子材料股份有限公司 | Method for determining molar ratio of calcium to zirconium in calcium zirconate |
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