CN106770407A - A kind of fuse piece X-fluorescence assay method of the glass batch entirety uniformity - Google Patents
A kind of fuse piece X-fluorescence assay method of the glass batch entirety uniformity Download PDFInfo
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- 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
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Abstract
The invention discloses a kind of X-fluorescence assay method of the glass batch uniformity, comprise the following steps successively：According to batch constituent, a standard sample is prepared by the use of boric acid or starch as adhesive with raw material, standard sample is tabletted in being carried out under certain pressure and time on tablet press machine.Standard sample piece is used into fundamental parameters method (FP methods) in X fluorescence spectrometer, sensitivity coefficient standard curve is set up.Take 10 12 batch testing samples, the treatment same with standard sample tableting processes is tabletted, by chemical composition content of the gained print in each print of the sensitivity coefficient curve detection of establishing criteria sample in X fluorescence spectrometer, the RSD of chemical composition is calculated, and then calculates the uniformity of batch.Assay method of the invention avoids the complicated procedures of existing method, and with the shortcoming of the uniformity summary glass batch entirety uniformity of single component, it is easy, quick, comprehensive, efficient.
Description
Technical field
The invention belongs to glass manufacturing area, and in particular to a kind of fuse piece X-fluorescence of the glass batch entirety uniformity is surveyed
Determine method.
Background technology
In the production of glass industry, the outfit of batch is the important procedure during process of glass, and matter is obtained
The qualified batch of reason has conclusive effect to the quality and yield of glass.Batch mixture homogeneity is to weigh glass to match somebody with somebody
Close an important indicator of material quality.
It is domestic at present generally to use the mixture homogeneity that batch is detected containing titration or electrical conductivity method.The former is using chemistry
Method measure is acid-base titration, is that batch sample is dissolved in the water, and adds methyl orange indicator, former using acid-base titration
Reason, titrate test solution to be changed into orange from yellow with HCl standard liquids is terminal, is actually with the alkali in HCl titration batches
Na2CO3, taking three samples carries out parallel test, is compared with maximum with the minimum value for consuming hydrochloric acid volume, the ratio for drawing
Value is used as the uniformity.This method is only suitable for and contains Na2CO3Batch, be not suitable for electronic glass batch the uniformity survey
It is fixed, and Na can only be weighed2CO3A kind of uniformity of this material, is seemed excessively rather with the uniformity that this weighs whole batch
Take a part for the whole.
Electrical conductivity method, is that batch sample is dissolved in the water, and water-soluble salt is dissolved as ion, insertion electricity in making batch
Pole, makes ion be moved under electric field action, determines the electrical conductivity of solution, and the difference according to electrical conductivity calculates the size of the uniformity.
This method seems simple, and the scope of application is limited significantly actually, is only applicable to the batch containing the component that can be dissolved in water, is not suitable for
In the cloud test of the electronic glass batch without water-soluble inorganic salt, and can only be weighed as titration and be dissolved in water
Special component the uniformity, equally exist the not problem in science taken a part for the whole.
The content of the invention
It is cumbersome for glass batch uniformity detection method such as titration and electrical conductivity method analysis process general at present,
And the detection of the electronic glass batch uniformity for not being suitable for not containing soda ash and water-soluble inorganic salt, while existing method is deposited
With the unilateral situation for weighing batch uniformity of the uniformity of some specified chemical compositions, herein propose a kind of applied widely
General, sample treatment is simple, determines lossless quick, and computational science is simple, can comprehensively reflect the electronics glass of batch uniformity
The assay method of glass batch.
The technical scheme is that：
A kind of fuse piece X-fluorescence assay method of the glass batch entirety uniformity, including prepare glass batch standard sample
Product, the content and intensity of main component in the standard sample are registered with X fluorescence spectrometer, and set up the sensitive of each main component
Degree factor standard curve, each of batch sample to be measured is detected with X fluorescence spectrometer according to the sensitivity coefficient standard curve
The content of individual main component, calculates their RSD values, and then the calculation of thc Glass Batch entirety uniformity.
Calculate the instrument of RSD values and unrestricted, the fuse piece X-fluorescence survey of the glass batch entirety uniformity of the invention
Determine a specific embodiment of method, the RSD values of chemical composition are calculated using computer EXCEl instruments.
One specific embodiment of the fuse piece X-fluorescence assay method of the glass batch entirety uniformity of the invention,
The sensitivity coefficient standard curve is to set up single standard sample strip using fundamental parameters method in X fluorescence spectrometer.
Fundamental parameters method is using a standard sample for principal component and content, in registering known in X fluorescence spectrometer
The content of composition, registers measurement intensity and theoretical strength, and sensitivity coefficient is the ratio of measurement intensity and theoretical strength, calculates spirit
Sensitivity coefficient curve (measurement intensity and theoretical strength than row relation), sensitivity coefficient curve is used to detect unknown sample
Component content, herein, the composition of unknown sample must be, it is known that and it is identical with standard sample composition, and content is close.
One specific embodiment of the fuse piece X-fluorescence assay method of the glass batch entirety uniformity of the invention,
With X fluorescence spectrometer is according to standard curve detection batch sample to be measured and calculates glass batch entirety to be measured uniformly
Degree, including these main components contain in calculating 3-15 parts of testing sample according to the sensitivity coefficient standard curve of each main component
Amount, and the corresponding RSD values of each main component of institute's test sample product are calculated, the average RSD values measure further according to surveyed composition treats test sample
The glass batch entirety uniformity of product.
Preferably, the glass batch that the average RSD values further according to surveyed composition determine testing sample is overall
Evenness is determined as the following formula：
Wherein, A1~An represents each main component respectively.
A specific embodiment of the invention, the main component includes Al2O3、SiO2, CaO, BaO, SrO and
B2O3。
The content of multiple compositions in same sample once can be simultaneously detected using the method for the present invention, and it is of the invention
The glass batch entirety uniformity that method determines testing sample is comprehensive multicomponent uniformity judges, it is to avoid with single
Composition is taken a part for the whole and judges the deviation brought.
One specific embodiment of the fuse piece X-fluorescence assay method of the glass batch entirety uniformity of the invention,
Testing sample quantity for detecting is 10-12 parts.The quantity of sample is more more more can accurately react uniformity situation, while more
The advantage of the inventive method can be manifested, compared to the acid-base method and electrical conductivity method of prior art, more convenient, required time is detected
Less.
One specific embodiment of the fuse piece X-fluorescence assay method of the glass batch entirety uniformity of the invention,
The preparation method of the standard sample and testing sample is：Take batch sample to be fully ground, weigh the cooperation feed powder after grinding
End adds mixing cosolvent in culture dish, and the sample is 1 with the mass ratio for mixing cosolvent:10, stir
After be transferred in platinum yellow crucible, releasing agent is uniformly added dropwise on its surface, by platinum yellow crucible be placed in constant temperature to 1100-1150 DEG C
Sample-melting stove burner hearth in, cover bell, start molten sample program, the time is 20-25min, is cooled down after the completion of founding, and obtains final product sample
Fuse piece.
It is preferred that NH of the releasing agent for 10-30%4I or NH4Br solution.
The sample preparation methods that a specific embodiment of the invention is used for：Take batch sample to be fully ground, will grind
Batch powder after mill with mix cosolvent according to 1:10 mass ratio is fully mixed in being listed in culture dish, meanwhile, sample with
The gross mass of cosolvent is controlled in 5g-8g, is transferred in platinum yellow crucible, and 3-8 drops NH is uniformly added dropwise at it4Or NH4Br
Releasing agent, is placed in platinum yellow crucible constant temperature and, to bell in the burner hearth of 1100 DEG C -1150 DEG C of sample-melting stove, is covered, starts molten
Sample program, cools down after the completion of founding, and obtains final product sample fuse piece.
Operating method of the invention can make appropriate order in the case where final result is not influenceed and exchange, and these should be regarded
It is equivalent technical solutions of the invention.
A specific embodiment of the invention, Al in the glass batch standard sample2O3、SiO2、CaO、BaO、
SrO and B2O3Weight percentage be respectively 15%, 58%, 7%, 5%, 6% and 9%.
A specific embodiment of the invention, the mixing cosolvent is：Anhydrous lithium metaborate and anhydrous tetraboric acid
Lithium is according to 1:2 mass ratioes row are fully mixed.
Beneficial effect：
(1) sample treatment of the inventive method is simple, completely lossless, and fuse piece is easy to preserve, and full-automation is realized in analysis, is carried
High efficiency.
(2) method for building up every time is not required to, curve can be reused, periodically need to be only corrected using the standard sample for preserving
The reliability of data can once be ensured.
(3) computational science is simple, can not only comprehensively reflect the uniformity of batch, and it is special specifically to reflect certain
Determine the uniformity of chemical constituent, it is applied widely, go for the uniformity detection of the glass batch of various species.
Specific embodiment
Embodiment 1
(1) instrument：X fluorescence spectrometer Shimadzu MXF-2400 and high temperature sample-melting stove TNRY-01A, vibromill
(2) batch standard sample is founded：
Prepare glass batch according to the Plays sample parameters data of table 1.
The standard sample glass batch parameter of table 1
| Items | Desired value |
| AL2O3(%) | 15 |
| SiO2(%) | 58 |
| CaO (%) | 7 |
| BaO (%) | 5 |
| SrO (%) | 6 |
| B2O3(%) | 9 |
| Mixing cosolvent (g) | 6 |
| Melt temperature DEG C | 1150 |
| Melting time min | 20 |
| Releasing agent 10%NH4I (drop) | 3 |
Fuse piece step is as follows：
1. the standard batch sample of known chemical constituent content in table 1 is taken, is fully ground in vibromill, it is standby；
2. 0.6g standard batch sample powder will be weighed in the standard batch powder sample after grinding in culture dish,
It is accurate again to add 6g mixing cosolvents, stirred with thin glass bar, then it is transferred to completely in platinum yellow crucible, in its table
Face is equably added dropwise 6 drop NH4I (10%) releasing agents；
3. platinum yellow crucible is placed in constant temperature and, to bell in the burner hearth of 1150 DEG C of sample-melting stove, is covered, starts molten sample journey
Sequence：Molten fritting time 120S, time of repose 10s, melting time 20min, 1150 DEG C of melt temperature, sample melting process enters automatically
OK；
5. after the completion of sample fusion, crucible is taken out, is cooled to room temperature, pour out fuse piece, be numbered with numbering, obtain final product standard sample, it is standby
With.
(3) foundation of standard curve
The standard sample piece that will be melted uses fundamental parameters method (FP methods), listing standard sample in X fluorescence spectrometer
Content and intensity, set up the sensitivity coefficient standard curve of component；
(4) set up analysis method is preserved, standard sample is sealed up for safekeeping, be stored in drier.In case regular calibration institute
The curve of foundation；
(5) detection of testing sample, takes 10-12 batch sample to be measured, is carried out with standard batch sample same
Polish process and fuse piece are processed, and room temperature is cooled to after being taken out after fuse piece EP (end of program), pour out sample strip, are numbered standby；
(6) the testing sample piece that will be melted is in the sensitivity coefficient curve inspection of establishing criteria sample in X fluorescence spectrometer
The chemical composition content surveyed in each print；
(7) the chemical composition testing result of all detection testing samples is collected and is input in EXCEL electrical forms, calculated
The corresponding RSD of each chemical composition of institute's test sample product.
Table 2
(8) the overall uniformity of batch is calculated using following equation
In formula, overall uniformity calculated value is more than 95%, and batch uniformity is qualified, if being less than 95%, you can to recognize
For batch uniformity is unqualified, meanwhile, if the RSD of certain chemical composition is more than 5%, it is believed that this kind of composition it is uniform
Property is poor.
As in table 2, the overall uniformity of the present embodiment glass batch is：96.72%, more than 95%, the uniformity is qualified,
Meanwhile, RSD (B2O3) it is more than 5%, B2O3Uniformity it is poor.
Claims (9)
1. the fuse piece X-fluorescence assay method of a kind of glass batch entirety uniformity, including glass batch standard sample is prepared,
The content and intensity of main component in the standard sample are registered with X fluorescence spectrometer, and sets up the sensitivity of each main component
Factor standard curve, detects testing sample and waits to be measured according to the sensitivity coefficient standard curve determination with X fluorescence spectrometer
The content of each main component of material sample is closed, the corresponding RSD values of each main component is calculated, and then calculate the overall uniform of batch
Degree.
2. the fuse piece X-fluorescence assay method of the glass batch according to claim 1 entirety uniformity, it is characterised in that
Single standard sample strip is used into fundamental parameters method in X fluorescence spectrometer, sensitivity coefficient standard curve is set up.
3. the fuse piece X-fluorescence assay method of the glass batch according to claim 1 entirety uniformity, it is characterised in that
Testing sample and the calculation of thc Glass Batch entirety uniformity, including basis are detected according to the standard curve with X fluorescence spectrometer
The content of these main components in 3-15 parts of testing sample of sensitivity coefficient standard curve determination of each main component, and calculate institute
The corresponding RSD values of each main component of test sample product, the average RSD values further according to surveyed composition determine the glass batch of testing sample
The overall uniformity of material.
4. the fuse piece X-fluorescence assay method of the glass batch entirety uniformity according to claim 3, its feature exists
In the glass batch entirety uniformity that the average RSD values further according to surveyed composition determine testing sample is determined as the following formula：
Wherein, A1~An represents each main component respectively.
5. the fuse piece X-fluorescence assay method of the glass batch according to claim 1 entirety uniformity, it is characterised in that
The main component includes Al2O3、SiO2, CaO, BaO, SrO and B2O3。
6. the fuse piece X-fluorescence assay method of the glass batch according to claim 3 entirety uniformity, it is characterised in that
Testing sample quantity for detecting is 10-12 parts.
7. the fuse piece X-fluorescence assay method of the glass batch according to claim 1 entirety uniformity, it is characterised in that
The preparation method of the standard sample and testing sample is：Take batch sample to be fully ground, weigh the cooperation feed powder after grinding
End adds mixing cosolvent in culture dish, and the sample is 1 with the mass ratio for mixing cosolvent:10, stir
After be transferred in platinum yellow crucible, releasing agent is uniformly added dropwise on its surface, by platinum yellow crucible be placed in constant temperature to 1100-1150 DEG C
Sample-melting stove burner hearth in, cover bell, start molten sample program, the melting time is 20-25min, is cooled down after the completion of founding, and is obtained final product
Sample fuse piece.
8. the fuse piece X-fluorescence assay method of the glass batch according to claim 7 entirety uniformity, it is characterised in that
The releasing agent is the NH of 10-30%4I or NH4Br solution.
9. the fuse piece X-fluorescence assay method of the glass batch according to claim 7 entirety uniformity, it is characterised in that
The mixing cosolvent is by anhydrous lithium metaborate and anhydrous lithium tetraborate according to 1:2 mass ratioes are fully uniformly mixed so as to obtain.
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| CN108181244A (en) * | 2017-11-30 | 2018-06-19 | 彩虹（合肥）液晶玻璃有限公司 | A kind of method for measuring TFT-LCD liquid crystal substrate glass batch uniformities |
| CN111707514A (en) * | 2020-06-17 | 2020-09-25 | 河北视窗玻璃有限公司 | Method for evaluating uniformity of glass batch |
| CN113748333A (en) * | 2019-09-26 | 2021-12-03 | 株式会社理学 | Fluorescent X-ray analyzer |
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| CN111707514A (en) * | 2020-06-17 | 2020-09-25 | 河北视窗玻璃有限公司 | Method for evaluating uniformity of glass batch |
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