CN107367521A - Pass through the method for impurity in x-ray fluorescence spectrometry glass - Google Patents
Pass through the method for impurity in x-ray fluorescence spectrometry glass Download PDFInfo
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- CN107367521A CN107367521A CN201710514475.6A CN201710514475A CN107367521A CN 107367521 A CN107367521 A CN 107367521A CN 201710514475 A CN201710514475 A CN 201710514475A CN 107367521 A CN107367521 A CN 107367521A
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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
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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
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/652—Specific applications or type of materials impurities, foreign matter, trace amounts
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Abstract
The present invention relates to a kind of method of impurity in glass by x-ray fluorescence spectrometry, comprise the following steps：1) glass fibre standard items and glass fibre to be measured are taken, after the glass fibre standard items, glass fibre to be measured are first mixed evenly with mixed solvent respectively again, iodate ammonia is added dropwise again, obtain mixture, then in being warming up to 1100~1300 DEG C in 10 minutes, the mixture is melted 15~25 minutes into normal glass print and glass print to be measured then at 1100~1300 DEG C, the mixed solvent is the mixed solvent of lithium tetraborate and lithium metaborate, and the mass ratio of the lithium tetraborate and lithium metaborate is 35:65；2) the normal glass print and glass print to be detected are detected by Xray fluorescence spectrometer again, and linear relationship is determined according to intensity and content, made calibration curve, obtain the content of impurity in glass.The detection sensitivity of the method for the present invention is high, and repeatability is strong.
Description
Technical field
The present invention relates to a kind of method for determining impurity in ore, and in particular to one kind is surveyed by x ray fluorescence spectrometry
Determine the method for impurity in glass, belong to the chemical analysis method technical field of metallurgical industry.
Background technology
Glass fibre chemical composition is typically analyzed using wet chemical analysis method, complex operation, analysis time length etc. be present
Shortcoming.Glass fiber component is tested using Xray fluorescence spectrometer, how key solves the problems, such as standard substance, and country provides glass
Glass fibrous glass standard substance only has two：Each one of sodium silicate glass, borosilicate glass.
X-ray fluorescence spectra is analyzed and is widely used to the fields such as metallurgy, geology, chemical industry, environmental protection, biology at present, and by
Step is applied in the analysis of glass, but its degree of accuracy for measuring and precision are inadequate.
The content of the invention
The technical problem to be solved in the present invention is：To solve technical problem, there is provided a kind of x-ray fluorescence spectrometry glass
The method of impurity in glass, so as to greatly improve the analytical precision of XRF and the degree of accuracy.
The technical solution adopted for the present invention to solve the technical problems is：
The method that the present invention provides impurity in a kind of glass by x-ray fluorescence spectrometry, comprises the following steps：
1) glass fibre standard items and glass fibre to be measured are taken, then by the glass fibre standard items, glass fibre to be measured
After being first mixed evenly respectively with mixed solvent, then iodate ammonia is added dropwise, obtains standard items mixture and product to be tested mixture, so
After being warming up to 1100~1300 DEG C in 10 minutes, the standard items mixture and product to be tested are mixed then at 1100~1300 DEG C
Thing melts 15~25 minutes into normal glass print and glass print to be measured respectively, and the mixed solvent is lithium tetraborate and inclined boron
The mixed solvent of sour lithium, the mass ratio of the lithium tetraborate and lithium metaborate is 35:65；
2) the normal glass print and glass print to be detected are detected by Xray fluorescence spectrometer again, and
Linear relationship is determined according to intensity and content, calibration curve is made, obtains the content of impurity in glass.
Preferably, in step 1), normal glass print and glass print to be detected is made within 18 minutes in 1150 DEG C of meltings,
Can melt under this condition evenly so that Elemental redistribution is uniform, reduces absorption-enhancement effect of matrix, eliminates altogether
The absorption enhancement effect between element is deposited, so that testing result is more accurate.
Preferably, in step 1), before heating, in addition to by the mixture preheat 3~5min the step of, pass through
Preheating step is easier to be heated evenly mixture, so that Elemental redistribution is more uniformly distributed, Detection results are more accurate.
Preferably, in step 1), the mixed solvent and the glass fibre standard items, the quality of glass fibre to be measured
Than for (12~15):1, mix under the ratio, obtained molten mixture good fluidity, reduce absorption-enhancing effect of matrix
Should.
Preferably, in step 1), the mixed solvent and the glass fibre standard items, the quality of glass fibre to be measured
Than for 13:1.
Preferably, the ammonium iodide is the ammonium iodide that concentration is 50%.
Preferably, in step 1), the mixture is melted 15~25 minutes into normal glass print and glass to be measured
After print, in addition to the step of the normal glass print and glass print to be measured are cooled down.
The beneficial effects of the invention are as follows：Using the lithium tetraborate and lithium metaborate mixed flux of proper ratio, fusing point is low, stream
Dynamic property is good, while passes through suitable dilution ratio so that its mobility is preferable, reduces absorption-enhancement effect of matrix so that
Elemental redistribution is uniform in manufactured glass print, eliminates the absorption enhancement effect between coexistence elements；It is and molten by rationally controlling
Melt temperature and melting time, avoid the too high metallic silicon of temperature from being reacted with crucible, produce side reaction so that the result measured is accurate
Really；Mixture is heated evenly by being preheated before melting, so that Elemental redistribution is more uniformly distributed, Detection results are more accurate.
Embodiment
Mode by the following examples, the application is further described.
Unless specifically stated otherwise, reagent used in following examples can be commercially available from regular channel.
Embodiment 1
1) preparation of testing sample：GBW03115 is weighed respectively as glass fibre standard items and glass fibre 1g to be measured,
12g mixed solvents are then respectively adding, mixed solvent is that mass ratio is 35:65 lithium tetraborate and lithium metaborate, then be added dropwise dense
The iodate ammonia for 50% is spent, obtains standard items mixture and product to be tested mixture, then in being warming up to 1100 DEG C in 10 minutes, then
Standard items mixture and product to be tested mixture are melted 25 minutes into normal glass print and glass to be detected respectively in 1100 DEG C
Print.
2) making of standard curve：
Condition test is carried out on Xray fluorescence spectrometer with the normal glass print prepared, to select instrument optimal
Analysis condition, and determine that linear relationship carries out linear regression according to intensity and content, produce calibration curve, and be stored in meter
In the quantitative analysis software of calculation machine.
3) in testing sample impurity test
Then the normal glass print and glass print to be detected are detected by Xray fluorescence spectrometer.
Embodiment 2
1) preparation of testing sample：GBW03115 is weighed respectively as glass fibre standard items and glass fibre 1g to be measured,
13g mixed solvents are then respectively adding, mixed solvent is that mass ratio is 35:65 lithium tetraborate and lithium metaborate, then be added dropwise dense
The iodate ammonia for 50% is spent, obtains standard items mixture and product to be tested mixture, then in being warming up to 1150 DEG C in 10 minutes, then
In 1300 DEG C by standard items mixture and product to be tested mixture melt respectively 15 minutes into.
2) making of standard curve：
Condition test is carried out on Xray fluorescence spectrometer with the normal glass print prepared, to select instrument optimal
Analysis condition, and determine that linear relationship carries out linear regression according to intensity and content, produce calibration curve, and be stored in meter
In the quantitative analysis software of calculation machine.
3) in testing sample impurity test
Then the normal glass print and glass print to be detected are detected by Xray fluorescence spectrometer.
Embodiment 3
1) preparation of testing sample：GBW03115 is weighed respectively as glass fibre standard items and glass fibre 1g to be measured,
15g mixed solvents are then respectively adding, mixed solvent is that mass ratio is 35:65 lithium tetraborate and lithium metaborate, then be added dropwise dense
The iodate ammonia for 50% is spent, obtains standard items mixture and product to be tested mixture, then in being warming up to 1100 DEG C in 10 minutes, then
Standard items mixture and product to be tested mixture are melted 25 minutes into normal glass print and glass to be detected respectively in 1100 DEG C
Print, then after being cooled to, be ready for testing.
2) making of standard curve：
Condition test is carried out on Xray fluorescence spectrometer with the normal glass print prepared, to select instrument optimal
Analysis condition, and determine that linear relationship carries out linear regression according to intensity and content, produce calibration curve, and be stored in meter
In the quantitative analysis software of calculation machine.
3) in testing sample impurity test
Then the normal glass print and glass print to be detected are detected by Xray fluorescence spectrometer.
Embodiment 4
Detected according to the same manner as in Example 2, it is different be before being warming up to 1150 DEG C in 10 minutes, in addition to
The step of mixture is preheated 4 minutes.
The measurement result of the weight percent content of each impurity element of standard items in embodiment 1-4 such as table 1 below institute
Show：
Table 1
| AL2O3 | Fe2O3 | MgO | CaO | TiO2 | |
| Embodiment 1 | 30.15 | 0.89 | 0.31 | 0.71 | 1.29 |
| Embodiment 2 | 30.62 | 0.93 | 0.35 | 0.76 | 1.34 |
| Embodiment 3 | 30.25 | 0.92 | 0.29 | 0.73 | 1.28 |
| Embodiment 4 | 30.65 | 0.95 | 0.33 | 0.77 | 1.35 |
Result above shows that the degree of accuracy of detection method of the invention is high, and repeatability is strong.
For example following tables of measurement result of the weight percent content of each impurity element of ore to be detected in embodiment 1-4
Shown in 2：
Table 2
| AL2O3 | Fe2O3 | MgO | CaO | TiO2 | |
| Embodiment 1 | 8.29 | 0.32 | 2.35 | 15.12 | 1.55 |
| Embodiment 2 | 8.31 | 0.35 | 2.38 | 15.21 | 1.58 |
| Embodiment 3 | 8.24 | 0.33 | 2.31 | 15.16 | 1.52 |
| Embodiment 4 | 8.33 | 0.37 | 2.41 | 15.24 | 1.53 |
| Average value | 8.2925 | 0.3425 | 2.3625 | 15.1825 | 1.545 |
| SD | 0.0386 | 0.0222 | 0.0427 | 0.0532 | 0.0265 |
| RSD | 0.465 | 6.48 | 1.81 | 0.35 | 1.72 |
Result above shows, its standard deviation (SD) and relative standard deviation (RSD) in rational scope, this method
It is high to detect accuracy.
In addition, determined by chemical analysis method in the normal glass print and glass print to be detected in embodiment 1-4
Impurity, the results showed that the result in the measurement result and chemical analysis method of embodiment 2 and 4 is more closely, the survey of embodiment 4
It is more close to determine result.
It is complete by above-mentioned description, relevant staff using the above-mentioned desirable embodiment according to the present invention as enlightenment
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property scope is not limited to the content on specification, it is necessary to determines its technical scope according to right.
Claims (7)
1. the method for impurity, comprises the following steps in a kind of glass by x-ray fluorescence spectrometry：
1) glass fibre standard items and glass fibre to be measured are taken, then the glass fibre standard items, glass fibre to be measured are distinguished
After being first mixed evenly with mixed solvent, then iodate ammonia is added dropwise, obtains mixture, then in be warming up to 1100 in 10 minutes~
1300 DEG C, the standard items mixture and product to be tested mixture are melted 15~25 minutes into mark respectively then at 1100~1300 DEG C
Quasi- glass print and glass print to be measured, the mixed solvent are the mixed solvent of lithium tetraborate and lithium metaborate, four boron
The mass ratio of sour lithium and lithium metaborate is 35:65；
2) the normal glass print and glass print to be detected are detected by Xray fluorescence spectrometer again, and according to
Intensity determines linear relationship with content, makes calibration curve, obtains the content of impurity in glass.
2. the method for impurity in the glass according to claim 1 by x-ray fluorescence spectrometry, it is characterised in that
In step 1), normal glass print and glass print to be detected is made within 18 minutes in 1150 DEG C of meltings.
3. the method for impurity, its feature exist in the glass according to claim 1 or 2 by x-ray fluorescence spectrometry
In, in step 1), before heating, in addition to by the mixture preheat 3~5min the step of.
4. the method for impurity, its feature exist in the glass according to claim 1 or 2 by x-ray fluorescence spectrometry
In, in step 1), the mixed solvent and the glass fibre standard items, glass fibre to be measured mass ratio for (12~
15):1。
5. the method for impurity, its feature exist in the glass according to claim 1 or 2 by x-ray fluorescence spectrometry
In in step 1), the mass ratio of the mixed solvent and the glass fibre standard items, glass fibre to be measured is 13:1.
6. the method for impurity in the glass according to claim 5 by x-ray fluorescence spectrometry, it is characterised in that
The ammonium iodide is the ammonium iodide that concentration is 50%.
7. the method for impurity, its feature exist in the glass according to claim 1 or 2 by x-ray fluorescence spectrometry
In, in step 1), the mixture is melted 15~25 minutes into after normal glass print and glass print to be measured, in addition to
The step of normal glass print and glass print to be measured are cooled down.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710514475.6A CN107367521A (en) | 2017-06-29 | 2017-06-29 | Pass through the method for impurity in x-ray fluorescence spectrometry glass |
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| CN201710514475.6A CN107367521A (en) | 2017-06-29 | 2017-06-29 | Pass through the method for impurity in x-ray fluorescence spectrometry glass |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108982563A (en) * | 2018-08-03 | 2018-12-11 | 武汉科技大学 | Method for preparing glass sheet for XRF analysis of release aid effect |
| CN112345570A (en) * | 2020-10-27 | 2021-02-09 | 南京玻璃纤维研究设计院有限公司 | Method for measuring components of glass fibers |
| CN113189126A (en) * | 2021-04-30 | 2021-07-30 | 河北南玻玻璃有限公司 | Method for detecting and analyzing tiny solid defects of float glass |
| CN113702412A (en) * | 2021-09-23 | 2021-11-26 | 河南旭阳光电科技有限公司 | Method for controlling mechanical iron impurity level in glass production process |
| CN114460117A (en) * | 2022-03-16 | 2022-05-10 | 清远南玻节能新材料有限公司 | Method for detecting component content of aluminum hydroxide product |
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| CN104280415A (en) * | 2013-10-31 | 2015-01-14 | 东旭集团有限公司 | Method for accurately detecting components of raw glass sheets |
| CN105651799A (en) * | 2015-12-29 | 2016-06-08 | 郑州旭飞光电科技有限公司 | X fluorescence detection method of impurity content in quartz sand |
| CN105651745A (en) * | 2015-12-29 | 2016-06-08 | 郑州旭飞光电科技有限公司 | Fluorescence detection method of zirconia content in TFT glass |
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| CN103529067A (en) * | 2013-10-29 | 2014-01-22 | 吉林建龙钢铁有限责任公司 | Detection reagents and method for detecting iron ores by X fluorescent spectrometry |
| CN104280415A (en) * | 2013-10-31 | 2015-01-14 | 东旭集团有限公司 | Method for accurately detecting components of raw glass sheets |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108982563A (en) * | 2018-08-03 | 2018-12-11 | 武汉科技大学 | Method for preparing glass sheet for XRF analysis of release aid effect |
| CN108982563B (en) * | 2018-08-03 | 2021-02-19 | 武汉科技大学 | Method for preparing glass sheet for XRF analysis of release aid effect |
| CN112345570A (en) * | 2020-10-27 | 2021-02-09 | 南京玻璃纤维研究设计院有限公司 | Method for measuring components of glass fibers |
| CN113189126A (en) * | 2021-04-30 | 2021-07-30 | 河北南玻玻璃有限公司 | Method for detecting and analyzing tiny solid defects of float glass |
| CN113702412A (en) * | 2021-09-23 | 2021-11-26 | 河南旭阳光电科技有限公司 | Method for controlling mechanical iron impurity level in glass production process |
| CN113702412B (en) * | 2021-09-23 | 2023-12-15 | 河南旭阳光电科技有限公司 | Method for controlling mechanical iron impurity level in glass production process |
| CN114460117A (en) * | 2022-03-16 | 2022-05-10 | 清远南玻节能新材料有限公司 | Method for detecting component content of aluminum hydroxide product |
| CN114460117B (en) * | 2022-03-16 | 2023-06-06 | 清远南玻节能新材料有限公司 | Method for detecting component content of aluminum hydroxide product |
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