CN113092510A - X-fluorescence determination method for potassium nitrate as high-alumina glass raw material - Google Patents
X-fluorescence determination method for potassium nitrate as high-alumina glass raw material Download PDFInfo
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- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000011521 glass Substances 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000004323 potassium nitrate Substances 0.000 title claims abstract description 29
- 235000010333 potassium nitrate Nutrition 0.000 title claims abstract description 28
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 239000002994 raw material Substances 0.000 title claims abstract description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000001304 sample melting Methods 0.000 claims abstract description 31
- 238000002844 melting Methods 0.000 claims abstract description 20
- 230000008018 melting Effects 0.000 claims abstract description 20
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 40
- 239000011780 sodium chloride Substances 0.000 claims description 19
- 239000006184 cosolvent Substances 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- 238000004876 x-ray fluorescence Methods 0.000 claims description 8
- VGTPKLINSHNZRD-UHFFFAOYSA-N oxoborinic acid Chemical compound OB=O VGTPKLINSHNZRD-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- UKFWSNCTAHXBQN-UHFFFAOYSA-N ammonium iodide Chemical group [NH4+].[I-] UKFWSNCTAHXBQN-UHFFFAOYSA-N 0.000 claims description 2
- 238000009681 x-ray fluorescence measurement Methods 0.000 claims 3
- 238000005259 measurement Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 16
- 238000004458 analytical method Methods 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000010790 dilution Methods 0.000 abstract description 2
- 239000012895 dilution Substances 0.000 abstract description 2
- HZRMTWQRDMYLNW-UHFFFAOYSA-N lithium metaborate Chemical compound [Li+].[O-]B=O HZRMTWQRDMYLNW-UHFFFAOYSA-N 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 103
- 238000012795 verification Methods 0.000 description 22
- 238000006243 chemical reaction Methods 0.000 description 15
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 12
- 239000011734 sodium Substances 0.000 description 10
- 238000013461 design Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000003426 chemical strengthening reaction Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000013074 reference sample Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 235000016337 monopotassium tartrate Nutrition 0.000 description 1
- KYKNRZGSIGMXFH-ZVGUSBNCSA-M potassium bitartrate Chemical compound [K+].OC(=O)[C@H](O)[C@@H](O)C([O-])=O KYKNRZGSIGMXFH-ZVGUSBNCSA-M 0.000 description 1
- 229940081543 potassium bitartrate Drugs 0.000 description 1
- -1 potassium tetraphenylborate Chemical compound 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000003578 releasing effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000003221 volumetric titration Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses an X fluorescence determination method of potassium nitrate as a high-alumina glass raw material, belonging to a detection method in the field of glass manufacturing and sequentially comprising the following steps of: respectively and fully mixing a standard sample and a sample to be detected with a mixed fluxing agent (lithium tetraborate + lithium metaborate: 2:1-1:1) according to a certain dilution ratio (1:20-1:15), transferring to a platinum yellow crucible, adding a release agent, and respectively melting a standard sample glass sheet and a sample glass sheet to be detected by using a high-temperature sample melting furnace according to a set melting time temperature program; registering the strength and the component content of a standard sample glass sheet on an X fluorescence spectrometer, and drawing a standard working curve of components; and measuring the content of the sample to be measured by using the established standard working curve. The method is an automatic measuring method with high analysis efficiency and scientific and reliable analysis result.
Description
Technical Field
The invention belongs to a detection method in the field of glass manufacturing, and particularly relates to an X fluorescence determination method for potassium nitrate as a high-alumina glass raw material.
Background
Potassium nitrate is a very important raw material in the field of high-alumina glass manufacturing, is one of the composition components of high-alumina glass, and is a molten salt reagent for the subsequent chemical strengthening of glass. In order to ensure the accuracy of the ingredients and the reliability of chemical strengthening, the detection and analysis of the ingredient content must be scientific, accurate and reliable. KNO in industrial potassium nitrate3The content of (A) is required to be at least more than 99.4%.
At present, the commonly used analysis method for detecting potassium nitrate mainly comprises a chemical method: potassium tetraphenylborate gravimetric method, potassium bitartrate volumetric titration analysis method. The reagents required by the two analysis methods are expensive, the waste liquid of the analysis experiment is easy to cause environmental pollution, meanwhile, the requirements on the operation technical level of an analyst are quite high, the analysis steps are quite complicated, the precipitation is quite easy to be incomplete due to slight carelessness, or the titration is not accurate, and the requirements on the analysis accuracy of the high-content potassium nitrate in the field of glass manufacturing are difficult to meet.
Disclosure of Invention
The technical problem solved by the invention is as follows: provided is a highly efficient and highly reliable automated measurement method which is simple in sample processing, free from loss and environmental pollution, and capable of simultaneously measuring a main component and an impurity component in potassium nitrate.
The technical scheme adopted by the invention is as follows:
an X fluorescence determination method for potassium nitrate as a raw material of high-alumina glass specifically comprises the following steps:
step 1: adopting a commercially available potassium nitrate purity standard sample as a standard sample, or adding a commercially available sodium chloride standard substance into the commercially available potassium nitrate purity standard sample to prepare a standard sample;
step 2: uniformly mixing lithium tetraborate and metaboric acid to obtain a mixed cosolvent;
and step 3: placing the standard sample in the step 1 and the mixed cosolvent in the step 2 in a culture dish, and uniformly stirring to form a mixed sample;
and 4, step 4: transferring the mixed sample of the culture dish in the step 3 into a platinum yellow crucible, and dropwise adding 1-3 drops of a release agent on the surface of the platinum yellow crucible;
and 5: placing the platinum yellow crucible in the step 4 into a high-temperature sample melting furnace for sample melting; after the sample is melted by a high-temperature sample melting furnace, taking out the platinum yellow crucible, naturally cooling and demolding to obtain a standard sample glass sheet;
step 6: registering the component content and the corresponding strength of the standard sample glass sheet melted in the step 5 on an X fluorescence spectrometer;
and 7: repeating the steps 1-6 to obtain a plurality of groups of standard sample glass sheets, and establishing a content-strength standard working curve;
and 8: and (5) repeating the step 2-5 on the sample to be detected to obtain a sample glass sheet to be detected, detecting the intensity of the sample glass sheet to be detected on an X-ray fluorescence spectrometer, and detecting the content according to the standard working curve established in the step 7.
Preferably, the ratio of the lithium tetraborate to the metaboric acid in the cosolvent in the step 2 is 1:1-2: 1.
Preferably, in the step 3, the ratio of the standard sample to the mixed cosolvent is 1:15-1: 20.
Preferably, the parameters of the high-temperature sample melting furnace in the step 4 are as follows: standing for pre-melting time of 100-150S, and standing for 5-10S; the swing melting time is 15-20min, and the melting temperature is 980-1100 ℃.
Preferably, the thickness of the standard sample glass sheet in the step 5 is 1-3mm, and the total mass of the sample is 8-10 g.
Preferably, the thickness of the standard sample glass sheet in the step 5 is 2mm, and the total mass of the sample is 8.4-9.6 g.
Preferably, the release agent is NH4I aqueous solution or NH4Any of aqueous solutions of Br.
Preferably, the NH is4I aqueous solution or NH4The mass fraction of the solute in the Br aqueous solution is 30%.
The invention has the beneficial effects that:
(1) the required reagent is easy to obtain, the mixing auxiliary agent adopts scientific proportion, the fluidity of a sample in a molten state can be ensured, the uniformity of the sample is convenient to realize, the use of a release agent is matched, the forming and releasing effect of the sample glass sheet is ensured, and the absorption effect on X rays is effectively reduced.
(2) And the proper sample fluxing agent dilution proportion and sample melting procedure are adopted, so that the complete and thorough melting of the sample can be ensured, and the proper sensitivity of component analysis is ensured.
(3) The method has the advantages that the sample is easy to process, automatic sample melting is achieved in one step, step-by-step melting is not needed, sample loss and sample melting quality difference are avoided, full automation of analysis is achieved, human errors are reduced, and through experimental verification, the method can guarantee precision and accuracy of data, and analysis efficiency is improved.
(4) The method is not required to be established every time, the standard curve can be recycled, and the reliability of the data can be ensured only by regularly using the stored standard sample for correction. Before detecting the potassium nitrate sample to be detected each time, the sample to be detected only needs to be melted into a glass sheet, and the standard curve established before can be directly used on a machine for detection.
(5) The application range is wide.
Drawings
FIG. 1 shows Na in example 12O standard curve;
FIG. 2 shows K in example 12O standard curve;
FIG. 3 is KNO of example 13A standard curve;
FIG. 4 is a Cl standard curve for example 1;
FIG. 5 shows Na in example 22O standard curve;
FIG. 6 shows K in example 22O standard curve;
FIG. 7 is KNO of example 23A standard curve;
FIG. 8 is a Cl standard curve for example 2;
FIG. 9 shows Na in example 32O standard curve;
FIG. 10 shows K in example 32O standard curve;
FIG. 11 is KNO of example 33A standard curve;
FIG. 12 is a Cl standard curve for example 3.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments for the purpose of making the objects, technical solutions and advantages of the present invention more apparent, but it should not be construed that the scope of the above-described subject matter of the present invention is limited to the following examples. Various substitutions and alterations can be made without departing from the technical idea of the invention as described above, according to the common technical knowledge and conventional means in the field, and the scope of the invention is covered.
The X-fluorescence spectrometer Shimadzu MXF-2400 was used in the X-fluorescence test in the present invention.
Example 1
Step 1: adding a commercially available potassium nitrate purity standard sample into a commercially available sodium chloride standard substance to prepare a standard sample, and respectively preparing 100g of standard series samples No. 1, No. 2, No. 3 and No. 4, wherein the preparation parameters of the standard sample are shown in Table 1;
table 1 table of formulation parameters for the standard sample series of example 1
Step 2: mixing lithium tetraborate and metaboric acid according to the proportion of 1:1 as a mixed cosolvent after being uniformly mixed;
and step 3: respectively weighing 0.4g of the standard sample No. 1 in the step 1 and 8g of the mixed cosolvent in the step 2, placing the weighed mixed cosolvent in a culture dish, and uniformly stirring to form a mixed sample, wherein the total amount of the mixed sample is 8.4 g;
and 4, step 4: transferring the mixed sample of the culture dish in the step 3 into a platinum yellow crucible, and dropwise adding 1 drop of release agent NH on the surface of the mixed sample4Br aqueous solution;
and 5: placing the platinum yellow crucible in the step 4 into a high-temperature sample melting furnace for sample melting, wherein the sample melting parameters of the high-temperature sample melting furnace are shown in a sample melting procedure parameter table in a table 2; after the sample melting is finished by a high-temperature sample melting furnace, taking out the platinum yellow crucible, naturally cooling and demolding to obtain a standard sample glass sheet No. 1;
table 2 example 1 melting procedure parameter table
| Standing premelting time | Rest time | Time of swing fusion | Melting temperature |
| 150S | 5S | 20min | 980℃ |
Step 6: registering the component content and testing the corresponding strength of the standard sample glass sheet No. 1 melted in the step 5 on an X fluorescence spectrometer; after melting the sample, the K is registered on an X-ray fluorescence spectrometer2O、Na2O, Cl content and corresponding intensity; wherein K2The content of O is KNO3Converted to form Na2O, Cl is converted from NaCl; wherein the conversion coefficient of K is as follows: m (K)2O)/2M(KNO3)(ii) a Wherein the conversion coefficient of Na is as follows: m (Na)2O)/2M (NaCl) with the conversion factor of Cl: m (Cl)/M (NaCl);
and 7: repeating the steps 2-6, respectively obtaining the content and the corresponding strength of each component of the standard sample glass sheets 2#, 3#, 4#, wherein the corresponding conversion relation is as shown in table 3, obtaining the component content of a plurality of groups of standard sample glass sheets according to the table 3, obtaining the corresponding strength data by an X fluorescence spectrometer, establishing a content-strength standard working curve, and obtaining K2O standard working curve, Na2An O standard working curve and a Cl standard working curve, as shown in figures 1, 2 and 4; and obtaining KNO by conversion3Standard operating curve, fig. 3.
TABLE 3 TABLE 1 Table for data of conversion of component content of glass sheet for reference sample
| |
1# | 2# | 3# | 4# |
| KNO3 | 98.96 | 99.63 | 99.96 | 99.36 |
| K2O | 46.09967 | 46.41178 | 46.56551 | 46.28600 |
| NaCl | 1.00 | 0.33 | 0 | 0.6 |
| Na2O | 0.530 | 0.175 | 0 | 0.318 |
| Cl | 0.607 | 0.200 | 0 | 0.364 |
And 8: verifying the standard curve and the method reliability, namely, fully mixing a commercially available potassium nitrate purity standard sample and a commercially available sodium chloride standard substance according to a certain proportion to prepare a verification sample, obtaining a verification sample glass sheet by the verification sample according to the steps 2-5, detecting the intensity of each component of the verification sample glass sheet on an X fluorescence spectrometer, and detecting the component content of the verification sample by using the obtained intensity values corresponding to each component according to the corresponding standard working curve established in the step 7, wherein the specific design standard value and detection value of the verification sample are shown in a table 4;
table 4 example 1 verification of design standard value and comparison table of detection value of sample
| Composition (I) | Design Standard value (%) | Detection value (%) |
| KNO3 | 99.16 | 99.17 |
| NaCL | 0.80 | 0.78 |
| K2O | 46.19 | 46.22 |
| Na2O | 0.424 | 0.432 |
| Cl | 0.485 | 0.491 |
The data in the above table illustrate that the reliability of the method can be guaranteed.
And step 9: detection of a 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 2
Step 1: adding a commercially available potassium nitrate purity standard sample into a commercially available sodium chloride standard substance to prepare a standard sample, and respectively preparing 100g of standard series samples No. 1, No. 2, No. 3 and No. 4, wherein the preparation parameters of the standard sample are shown in Table 5;
table 5 table of formulation parameters for the standard sample set of example 2
Step 2: mixing lithium tetraborate and metaboric acid according to the ratio of 2:1 as a mixed cosolvent after being uniformly mixed;
and step 3: respectively weighing 0.6g of the standard sample No. 1 in the step 1 and 9g of the mixed cosolvent in the step 2, placing the weighed materials in a culture dish, and uniformly stirring to form a mixed sample, wherein 9.6g of the mixed sample is totally obtained;
and 4, step 4: transferring the mixed sample of the culture dish in the step 3 into a platinum yellow crucible, and dropwise adding 3 drops of a release agent NH on the surface of the mixed sample4I, water solution;
and 5: placing the platinum yellow crucible in the step 4 into a high-temperature sample melting furnace for sample melting, wherein the sample melting parameters of the high-temperature sample melting furnace are shown in a sample melting program parameter table of a table 6; after the sample melting is finished by a high-temperature sample melting furnace, taking out the platinum yellow crucible, naturally cooling and demolding to obtain a standard sample glass sheet No. 1;
TABLE 6 EXAMPLE 2 melting procedure parameter Table
| Standing stillPremelting time | Rest time | Time of swing fusion | Melting temperature |
| 100S | 10S | 15min | 1100℃ |
Step 6: registering the component content and testing the corresponding strength of the standard sample glass sheet No. 1 melted in the step 5 on an X fluorescence spectrometer; after melting the sample, the K is registered on an X-ray fluorescence spectrometer2O、Na2O, Cl content and corresponding intensity; wherein K2The content of O is KNO3Converted to form Na2O, Cl is converted from NaCl; wherein the conversion coefficient of K is as follows: m (K)2O)/2M(KNO3)(ii) a Wherein the conversion coefficient of Na is as follows: m (Na)2O)/2M (NaCl) with the conversion factor of Cl: m (Cl)/M (NaCl);
and 7: repeating the steps 2-6, respectively obtaining the content and the corresponding strength of each component of the standard sample glass sheets 2#, 3#, 4#, wherein the corresponding conversion relation is shown in table 7, obtaining the component content of a plurality of groups of standard sample glass sheets according to the table 7, obtaining corresponding strength data by an X fluorescence spectrometer, establishing a content-strength standard working curve, and obtaining K2O standard working curve, Na2O standard working curve, Cl standard working curve, as in fig. 5, 6, 8; and obtaining KNO by conversion3The standard operating curve, as shown in figure 7,
TABLE 7 TABLE 2 Table for data on conversion of component content of glass sheet for standard sample
And 8: verifying the standard curve and the method reliability, namely, fully mixing a commercially available potassium nitrate purity standard sample and a commercially available sodium chloride standard substance according to a certain proportion to prepare a verification sample, obtaining a verification sample glass sheet by the verification sample according to the steps 2-5, detecting the intensity of each component of the verification sample glass sheet on an X fluorescence spectrometer, and detecting the component content of the verification sample by using the obtained intensity values corresponding to each component according to the corresponding standard working curve established in the step 7, wherein the specific design standard value and detection value of the verification sample are shown in a table 8;
table 8 example 2 verification of design standard value and comparison table of detection value of sample
| Composition (I) | Design Standard value (%) | Detection value (%) |
| KNO3 | 98.86 | 98.82 |
| NaCl | 1.100 | 1.104 |
| K2O | 46.15 | 46.17 |
| Na2O | 0.583 | 0.579 |
| Cl | 0.667 | 0.670 |
The data in the above table illustrate that the reliability of the method can be guaranteed.
And step 9: detection of a 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 3
Step 1: adding a commercially available potassium nitrate purity standard sample into a commercially available sodium chloride standard substance to prepare a standard sample, and respectively preparing 100g of standard series samples No. 1, No. 2, No. 3 and No. 4, wherein the preparation parameters of the standard sample are shown in Table 1;
table 9 table of formulation parameters for the standard sample set of example 3
Step 2: mixing lithium tetraborate and metaboric acid according to the weight ratio of 1.5: 1 as a mixed cosolvent after being uniformly mixed;
and step 3: respectively weighing 0.5g of the standard sample No. 1 in the step 1 and 8.5g of the mixed cosolvent in the step 2, placing the weighed mixed cosolvent in a culture dish, and uniformly stirring to form a mixed sample, wherein 9g of the mixed sample is obtained;
and 4, step 4: transferring the mixed sample of the culture dish in the step 3 into a platinum yellow crucible, and dropwise adding 2 drops of a release agent NH on the surface of the mixed sample4I, water solution;
and 5: placing the platinum yellow crucible in the step 4 into a high-temperature sample melting furnace for sample melting, wherein the sample melting parameters of the high-temperature sample melting furnace are shown in a sample melting procedure parameter table in a table 2; after the sample melting is finished by a high-temperature sample melting furnace, taking out the platinum yellow crucible, naturally cooling and demolding to obtain a standard sample glass sheet No. 1;
TABLE 10 EXAMPLE 3 melting procedure parameters Table
| Standing premelting time | Rest time | Time of swing fusion | Melting temperature |
| 120S | 7S | 18min | 1000℃ |
Step 6: registering the component content and testing the corresponding strength of the standard sample glass sheet No. 1 melted in the step 5 on an X fluorescence spectrometer; after melting the sample, the K is registered on an X-ray fluorescence spectrometer2O、Na2O, Cl content and corresponding intensity; wherein K2The content of O is KNO3Converted to form Na2O, Cl is converted from NaCl; wherein the conversion coefficient of K is as follows: m (K)2O)/2M(KNO3)(ii) a Wherein the conversion coefficient of Na is as follows: m (Na)2O)/2M (NaCl) with the conversion factor of Cl: m (Cl)/M (NaCl);
and 7: repeating the steps 2-6, respectively obtaining the content and the corresponding strength of each component of the standard sample glass sheets 2#, 3#, 4#, wherein the corresponding conversion relation is shown in table 11, and a plurality of groups of standard samples are obtained according to the table 11The component content of the product glass sheet, and the X fluorescence spectrometer obtain corresponding intensity data, establish a content-intensity standard working curve and obtain K2O standard working curve, Na2O standard working curve, Cl standard working curve, e.g., 9, 10, 12; and obtaining KNO by conversion3The standard operating curve, as shown in figure 11,
TABLE 11 TABLE 3 Table for data on conversion of component content of glass sheet of reference sample
And 8: verifying the standard curve and the method reliability, namely, fully mixing a commercially available potassium nitrate purity standard sample and a commercially available sodium chloride standard substance according to a certain proportion to prepare a verification sample, obtaining a verification sample glass sheet by the verification sample according to the steps 2-5, detecting the intensity of each component of the verification sample glass sheet on an X fluorescence spectrometer, and detecting the component content of the verification sample by using the obtained intensity values corresponding to each component according to the corresponding standard working curve established in the step 7, wherein the specific design standard value and detection value of the verification sample are shown in a table 12;
table 12 example 3 verification sample design standard value and detection value comparison table
| Composition (I) | Design Standard value (%) | Detection value (%) |
| KNO3 | 99.70 | 99.71 |
| NaCL | 0.260 | 0.264 |
| K2O | 46.33 | 46.30 |
| Na2O | 0.138 | 0.140 |
| Cl | 0.158 | 0.156 |
The above table data illustrates that the reliability of the method can be guaranteed
And 8: detection of a 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.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. The invention extends to any novel feature or any novel combination of features disclosed in this specification and any novel method or process steps or any novel combination of features disclosed.
Claims (8)
1. The X fluorescence determination method for the high-alumina glass raw material potassium nitrate is characterized by comprising the following steps:
step 1: adopting a commercially available potassium nitrate purity standard sample as a standard sample, or adding a commercially available sodium chloride standard substance into the commercially available potassium nitrate purity standard sample to prepare a standard sample;
step 2: uniformly mixing lithium tetraborate and metaboric acid to obtain a mixed cosolvent;
and step 3: placing the standard sample in the step 1 and the mixed cosolvent in the step 2 in a culture dish, and uniformly stirring to form a mixed sample;
and 4, step 4: transferring the mixed sample of the culture dish in the step 3 into a platinum yellow crucible, and dropwise adding 1-3 drops of a release agent on the surface of the platinum yellow crucible;
and 5: placing the platinum yellow crucible in the step 4 into a high-temperature sample melting furnace for sample melting; after the sample is melted by a high-temperature sample melting furnace, taking out the platinum yellow crucible, naturally cooling and demolding to obtain a standard sample glass sheet;
step 6: registering the component content and the corresponding strength of the standard sample glass sheet melted in the step 5 on an X fluorescence spectrometer;
and 7: repeating the steps 1-6 to obtain a plurality of groups of standard sample glass sheets, and establishing a content-strength standard working curve;
and 8: and (5) repeating the step 2-5 on the sample to be detected to obtain a sample glass sheet to be detected, detecting the intensity of the sample glass sheet to be detected on an X-ray fluorescence spectrometer, and detecting the content according to the standard working curve established in the step 7.
2. The method for measuring the X fluorescence of the potassium nitrate as the raw material of the high-alumina glass according to claim 1, wherein the ratio of the lithium tetraborate to the metaboric acid in the cosolvent in the step 2 is 1:1-2: 1.
3. The method for measuring the X fluorescence of the raw material potassium nitrate in the high-alumina glass as claimed in claim 1, wherein in the step 3, the ratio of the standard sample to the mixed cosolvent is 1:15-1: 20.
4. The method for measuring the X fluorescence of the potassium nitrate as the raw material of the high-alumina glass according to claim 1, wherein the parameters of the high-temperature melting furnace in the step 4 are as follows: standing for pre-melting time of 100-150S, and standing for 5-10S; the swing melting time is 15-20min, and the melting temperature is 980-1100 ℃.
5. The method for X-ray fluorescence measurement of potassium nitrate as a raw material of high-alumina glass according to claim 1, wherein the thickness of the glass sheet of the standard sample in the step 5 is 1-3mm, and the total mass of the sample is 8-10 g.
6. The method for X-ray fluorescence measurement of potassium nitrate as a raw material of high-alumina glass according to claim 1, wherein the thickness of the glass sheet of the standard sample in the step 5 is 2mm, and the total mass of the sample is 8.4-9.6 g.
7. The method for X-ray fluorescence measurement of potassium nitrate as a raw material for high-alumina glass according to claim 1, wherein the release agent is NH4I aqueous solution or NH4Any of aqueous solutions of Br.
8. The method according to claim 7, wherein the NH is measured by X-fluorescence measurement of potassium nitrate as a raw material of high-alumina glass4I aqueous solution or NH4The mass fraction of the solute in the Br aqueous solution is 30%.
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