CN106990129B - The analysis method of constituent content in high-pressure digestion-x-ray fluorescent spectrometry measurement glass powder - Google Patents
The analysis method of constituent content in high-pressure digestion-x-ray fluorescent spectrometry measurement glass powder Download PDFInfo
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- CN106990129B CN106990129B CN201710343497.0A CN201710343497A CN106990129B CN 106990129 B CN106990129 B CN 106990129B CN 201710343497 A CN201710343497 A CN 201710343497A CN 106990129 B CN106990129 B CN 106990129B
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- B30B—PRESSES IN GENERAL
- B30B11/00—Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses
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Abstract
The invention discloses a kind of high-pressure digestion-x-ray fluorescent spectrometry measurement glass powder constituent content analysis methods.The boron content of glass powder raw material is that the chemical method dissolved using high-pressure digestion and nitration mixture is measured in the present invention, simultaneously, the zinc, antimony, bismuth intensity of the artificial synthesized sample preparation of fixed boron content are measured using x-ray fluorescence spectrometry instrument, intensity is established to the standard curve of content to release the content of the zinc, antimony, bismuth in glass powder raw material under corresponding boron content.
Description
Technical field
The invention belongs to analysis technical fields, specifically contain a kind of high-pressure digestion-x-ray fluorescent spectrometry measurement glass
The analysis method of constituent content in powder, the boron content in this method in glass powder are substantially bent using the dissolution measurement of high-pressure digestion method
Line does standard curve acquisition using standard addition method and x-ray Fluorescence Spectrometer data measured.
Background technique
As x-ray fluorescence analysis is also known as X-ray secondary emission spectrum analysis.The genealogy of law using simple x-ray photon or
Atom in other microcosmic particles excitation test substances, be allowed to generate secondary characteristic X-ray (X-ray fluorescence) and carry out substance at
The method of analysis and chemical state research.
First wavelength was made by H. expense Reed graceful (H.Friedmann) and L.S. Bai Kesi (L.S.Birks) in 1948
Dispersive x-ray fluorescence analyzer, until the sixties, this law was established in the status of analysis field.
Modern X-ray fluorescence spectrum analyzer consists of the following components: X-ray emitter (X-ray tube, high voltage power supply
And stablize constant-current stabilizer), spectral detection system (analyzing crystal, collimator and detector), numeration record system (impulse radiation point
Parser, calibration meter, timer, integrator, logger).The characteristic X-ray spectrum that different elements have wavelength different, and each spectral line
Fluorescence intensity be in again certain relationship with the concentration of element, the wavelength and intensity for measuring elemental characteristic X-ray spectral line to be measured can
To carry out qualitative and quantitative analysis.
Summary of the invention
Goal of the invention: in order to solve the deficiencies in the prior art, the present invention provides a kind of high-pressure digestion-x-ray fluorescence light
Spectrometry measures the analysis method of constituent content in glass powder.
Technical solution: a kind of high-pressure digestion-x-ray fluorescent spectrometry measures the analysis method of constituent content in glass powder,
Include the following steps:
1) 5g glass powder is placed in high-pressure digestion tank, and two kinds of acid of HCl, HF (proportion is 1:1 or 1:1.5) is added,
Mixed solution is put into baking oven, oven temperature is set as 110 DEG C~150 DEG C, and the time is 3h~7h；The glass that will be completely dissolved afterwards
For glass powder solution liquid relief to the volumetric flask constant volume of 50ml, the solution after pipetting 20ml constant volume is 2% with mass concentration to conical flask
NaOH solution is titrated to solution and sports light red, calculates boron content using relational expression；
2) the powder several groups that zinc oxide, antimony oxide, bismuth oxide and boric acid gross mass are 6g are weighed, wherein boron content is distinguished
It is fixed as 0%, 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%.It is identical fixation in boron content
In the case where value, zinc oxide, antimony oxide, bismuth oxide solid powder are again with any 3 kinds of proportional arrangements.
3) configured zinc oxide, antimony oxide, bismuth oxide and boric acid mixed-powder are poured into plant pulverizer mixed grinding,
It grinds 20 seconds and stops 90 seconds, repetitive operation 3 times, until powder is sufficiently mixed.
4) well-mixed powder is put into the center die of tablet press machine, 5g addition is uniformly poured into edge mold
Object presses manual handle back and forth, until dwell pressure stops when being 20-30Pa, is removed from the molds after 5-20min in flakes, in flakes
For round sheet object (radius 2cm, thick 0.5cm),；The tablet being pressed into is directly placed into x-ray fluorescence spectrometry instrument, is detected
The intensity of element；The intensity and content measured according to it do standard curve.
5) glass powder solution remaining in (1) is placed in tetrafluoroethene beaker, beaker is placed directly within x-ray fluorescence spectrum
In instrument, click starts, and measures the intensity of the multiple elements of zinc in glass powder, antimony, bismuth；
6) boron content and element-intensities that will test out, which are put into the standard curve measured, finds its correspondence content.
As optimization: the tablet press machine be Manual tablet pressing machine (tablet press machine is single-punch tablet press, it is cheap, easy to operate,
Structure is simple.Mainly contain handwheel, lead screw, column, mold, piston, pressure gauge, manual handle etc.).
As optimization: the zinc oxide, antimony oxide, bismuth oxide and boric acid powder are intended to the pre- place for being dried and grinding
Reason.It is put into baking oven specific steps are as follows: powder is placed in culture dish, and 3 hour postpositions are dried at 150 DEG C
It is spare in drying bottle.4 kinds of powder are successively poured into plant pulverizer mixed grinding again, grinds 20 seconds and stops 90 seconds, repeat to grasp
Make 3 times.
As optimization: the additive is by drying and to grind pretreated solid boric acid binder, concrete operations
Steps are as follows: powder being placed in culture dish, is put into baking oven, 3 hours of drying are placed on standby in drying bottle at 150 DEG C
With.Powder is poured into the grinding of plant pulverizer again, grinds 20 seconds and stops 90 seconds, repetitive operation 3 times.Its main function be substrate and
Fringing.
The utility model has the advantages that the boron content of glass powder raw material is the chemistry dissolved using high-pressure digestion and nitration mixture in the present invention
Method is measured, meanwhile, the zinc, antimony, bismuth intensity of the artificial synthesized sample preparation of fixed boron content are measured using x-ray fluorescence spectrometry instrument,
The standard curve of intensity and content is established to release glass powder raw material wherein content of zinc, antimony, bismuth under the boron content, is had
Quick accurate advantage, it is excellent to have that spectral line is simple, analysis speed is fast, measurement element is more, can be carried out Simultaneous multi element analysis etc.
Point is that (other two methods are neutron activation to one of widely applied three big analysis means in current Atmospheric particulates elemental analysis
Analysis and proton fluorescence analysis).
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, so that the technology of this field
Personnel can better understand advantages and features of the invention, to make apparent boundary to protection scope of the present invention
It is fixed.Embodiment described in the invention is only a part of the embodiment of the present invention, instead of all the embodiments, based on the present invention
In embodiment, those of ordinary skill in the art's every other implementation obtained without making creative work
Example, shall fall within the protection scope of the present invention.
The present invention will be described in detail combined with specific embodiments below.
Specific embodiment one:
The analysis method of constituent content in a kind of high-pressure digestion-x-ray fluorescent spectrometry measurement glass powder, including walk as follows
It is rapid:
1) 5g glass powder is placed in high-pressure digestion tank, and two kinds of acid of HCl, HF (proportion is 1:1 or 1:1.5) is added,
Mixed solution is put into baking oven, oven temperature is set as 110 DEG C~150 DEG C, and the time is 3h~7h；The glass that will be completely dissolved afterwards
For glass powder solution liquid relief to the volumetric flask constant volume of 50ml, the solution after pipetting 20ml constant volume is 2% with mass concentration to conical flask
NaOH solution is titrated to solution and sports light red, calculates boron content using relational expression；
2) the powder several groups that zinc oxide, antimony oxide, bismuth oxide and boric acid gross mass are 6g are weighed, wherein boron content is fixed
It is 20%.Under this boron content, zinc oxide, antimony oxide, bismuth oxide solid powder content are respectively 10%, 30%, 40%；
30%, 40%, 10%；40%, 10%, 30%.
3) configured zinc oxide, antimony oxide, bismuth oxide and boric acid mixed-powder are poured into plant pulverizer mixed grinding,
It grinds 20 seconds and stops 90 seconds, repetitive operation 3 times, until powder is sufficiently mixed.
4) well-mixed powder is put into the center die of tablet press machine, 5g addition is uniformly poured into edge mold
Object presses manual handle back and forth, until dwell pressure stops when being 20-30Pa, is removed from the molds after 5-20min in flakes, in flakes
For round sheet object (radius 2cm, thick 0.5cm),；The tablet being pressed into is directly placed into x-ray fluorescence spectrometry instrument, is detected
The intensity of element；The intensity and content measured according to it do standard curve.
5) glass powder solution remaining in (1) is placed in tetrafluoroethene beaker, beaker is placed directly within x-ray fluorescence spectrum
In instrument, click starts, and measures the intensity of the multiple elements of zinc in glass powder, antimony, bismuth；
6) boron content and element-intensities that will test out, which are put into the standard curve measured, finds its correspondence content.
Specific embodiment two:
The analysis method of constituent content in a kind of high-pressure digestion-x-ray fluorescent spectrometry measurement glass powder, including walk as follows
It is rapid:
1) 5g glass powder is placed in high-pressure digestion tank, and two kinds of acid of HCl, HF (proportion is 1:1 or 1:1.5) is added,
Mixed solution is put into baking oven, oven temperature is set as 110 DEG C~150 DEG C, and the time is 3h~7h；The glass that will be completely dissolved afterwards
For glass powder solution liquid relief to the volumetric flask constant volume of 50ml, the solution after pipetting 20ml constant volume is 2% with mass concentration to conical flask
NaOH solution is titrated to solution and sports light red, calculates boron content using relational expression；
2) the powder several groups that zinc oxide, antimony oxide, bismuth oxide and boric acid gross mass are 6g are weighed, wherein boron content is fixed
It is 30%.Under this boron content, zinc oxide, antimony oxide, bismuth oxide solid powder content are respectively 10%, 20%, 40%；
20%, 40%, 10%；40%, 10%, 20%.
3) configured zinc oxide, antimony oxide, bismuth oxide and boric acid mixed-powder are poured into plant pulverizer mixed grinding,
It grinds 20 seconds and stops 90 seconds, repetitive operation 3 times, until powder is sufficiently mixed.
4) well-mixed powder is put into the center die of tablet press machine, 5g addition is uniformly poured into edge mold
Object presses manual handle back and forth, until dwell pressure stops when being 20-30Pa, is removed from the molds after 5-20min in flakes, in flakes
For round sheet object (radius 2cm, thick 0.5cm),；The tablet being pressed into is directly placed into x-ray fluorescence spectrometry instrument, is detected
The intensity of element；The intensity and content measured according to it do standard curve.
5) glass powder solution remaining in (1) is placed in tetrafluoroethene beaker, beaker is placed directly within x-ray fluorescence spectrum
In instrument, click starts, and measures the intensity of the multiple elements of zinc in glass powder, antimony, bismuth；
6) boron content and element-intensities that will test out, which are put into the standard curve measured, finds its correspondence content.
Specific embodiment three:
The analysis method of constituent content in a kind of high-pressure digestion-x-ray fluorescent spectrometry measurement glass powder, including walk as follows
It is rapid:
1) 5g glass powder is placed in high-pressure digestion tank, and two kinds of acid of HCl, HF (proportion is 1:1 or 1:1.5) is added,
Mixed solution is put into baking oven, oven temperature is set as 110 DEG C~150 DEG C, and the time is 3h~7h；The glass that will be completely dissolved afterwards
For glass powder solution liquid relief to the volumetric flask constant volume of 50ml, the solution after pipetting 20ml constant volume is 2% with mass concentration to conical flask
NaOH solution is titrated to solution and sports light red, calculates boron content using relational expression；
2) the powder several groups that zinc oxide, antimony oxide, bismuth oxide and boric acid gross mass are 6g are weighed, wherein boron content is fixed
It is 40%.Under this boron content, zinc oxide, antimony oxide, bismuth oxide solid powder content are respectively 10%, 30%, 20%；
30%, 20%, 10%；20%, 10%, 30%.
3) configured zinc oxide, antimony oxide, bismuth oxide and boric acid mixed-powder are poured into plant pulverizer mixed grinding,
It grinds 20 seconds and stops 90 seconds, repetitive operation 3 times, until powder is sufficiently mixed.
4) well-mixed powder is put into the center die of tablet press machine, 5g addition is uniformly poured into edge mold
Object presses manual handle back and forth, until dwell pressure stops when being 20-30Pa, is removed from the molds after 5-20min in flakes, in flakes
For round sheet object (radius 2cm, thick 0.5cm),；The tablet being pressed into is directly placed into x-ray fluorescence spectrometry instrument, is detected
The intensity of element；The intensity and content measured according to it do standard curve.
5) glass powder solution remaining in (1) is placed in tetrafluoroethene beaker, beaker is placed directly within x-ray fluorescence spectrum
In instrument, click starts, and measures the intensity of the multiple elements of zinc in glass powder, antimony, bismuth；
6) boron content and element-intensities that will test out, which are put into the standard curve measured, finds its correspondence content.
The tablet press machine is Manual tablet pressing machine, cheap, easy to operate, structure is simple.Mainly contain handwheel, lead screw,
Column, mold, piston, pressure gauge, manual handle etc..
The zinc oxide, antimony oxide, bismuth oxide and boric acid powder are intended to the pretreatment for being dried and grinding.It is specifically grasped
Steps are as follows for work: powder being placed in culture dish, is put into baking oven, 3 hours of drying are placed on standby in drying bottle at 150 DEG C
With.4 kinds of powder are successively poured into plant pulverizer mixed grinding again, grinds 20 seconds and stops 90 seconds, repetitive operation 3 times.
The additive be by dry and grind pretreated solid boric acid binder, specific steps are as follows:
Powder is placed in culture dish, is put into baking oven, 3 hours of drying are placed on spare in drying bottle at 150 DEG C.Again by powder
The grinding of plant pulverizer is poured into, grinds 20 seconds and stops 90 seconds, repetitive operation 3 times.Its main function is substrate and fringing.
The boron content of glass powder raw material is that the chemical method dissolved using high-pressure digestion and nitration mixture is measured in the present invention,
Meanwhile the zinc, antimony, bismuth intensity of the artificial synthesized sample preparation of fixed boron content are measured using x-ray fluorescence spectrometry instrument, establish intensity
With the standard curve of content to release glass powder raw material wherein content of zinc, antimony, bismuth under the boron content, there is quick essence
True advantage has many advantages, such as that spectral line is simple, analysis speed is fast, measurement element is more, can be carried out Simultaneous multi element analysis, is current
(other two methods are neutron activation analysis and proton to one of widely applied three big analysis means in Atmospheric particulates elemental analysis
Fluorescence analysis).
Claims (4)
1. the analysis method of constituent content in a kind of high-pressure digestion-x-ray fluorescent spectrometry measurement glass powder, it is characterised in that:
Include the following steps:
(1) 5g glass powder is placed in high-pressure digestion tank, and two kinds of acid of HCl, HF is added, matched as HCl:HF=1:1 or 1:
1.5, mixed solution is put into baking oven, oven temperature is set as 110 DEG C~150 DEG C, and the time is 3h~7h；After will be completely dissolved
Glass powder solution liquid relief to the volumetric flask constant volume of 50ml, the solution after pipetting 20ml constant volume is with mass concentration to conical flask
2% NaOH solution is titrated to solution and sports light red, calculates boron content using relational expression；
(2) powder that zinc oxide, antimony oxide, bismuth oxide and boric acid gross mass are 6g is weighed, wherein the boron content in boric acid is (1)
Detection；In the case where boron content is same fixed value, zinc oxide, antimony oxide, bismuth oxide solid powder are compared again with any 3 kinds
Example configuration；
(3) configured zinc oxide, antimony oxide, bismuth oxide and boric acid mixed-powder are poured into plant pulverizer mixed grinding, ground
It grinds 20 seconds and stops 90 seconds, repetitive operation 3 times, until powder is sufficiently mixed；
(4) well-mixed powder is put into the center die of tablet press machine, 5g additive is uniformly poured into edge mold, come
It returns and presses manual handle, until dwell pressure stops when being 20-30Pa, be removed from the molds after 5-20min in flakes, be in flakes circle
Tablet, radius 2cm, thick 0.5cm；The tablet being pressed into is directly placed into x-ray fluorescence spectrometry instrument, detection elements it is strong
Degree；The intensity and content measured according to it do standard curve；
(5) 30ml glass powder solution remaining in (1) is placed in tetrafluoroethene beaker, beaker is placed directly within x-ray fluorescence
In spectrometer, click starts, and measures the intensity of zinc in glass powder, antimony, bismuth element；
(6) boron content and element-intensities that will test out, which are put into the standard curve measured, finds its correspondence content.
2. the analysis side of constituent content in high-pressure digestion according to claim 1-x-ray fluorescent spectrometry measurement glass powder
Method, it is characterised in that: the tablet press machine be Manual tablet pressing machine, mainly contain handwheel, lead screw, column, mold, piston, pressure gauge,
Manual handle.
3. the analysis side of constituent content in high-pressure digestion according to claim 1-x-ray fluorescent spectrometry measurement glass powder
Method, it is characterised in that: the zinc oxide, antimony oxide, bismuth oxide and boric acid powder are intended to the pretreatment for being dried and grinding；Its
Specific steps are as follows: powder is placed in culture dish, it is put into baking oven, 3 hours of drying are placed on drying at 150 DEG C
It is spare in bottle；4 kinds of powder are successively poured into plant pulverizer mixed grinding again, grinds 20 seconds and stops 90 seconds, repetitive operation 3 times.
4. the analysis side of constituent content in high-pressure digestion according to claim 1-x-ray fluorescent spectrometry measurement glass powder
Method, it is characterised in that: the additive is by drying and to grind pretreated solid boric acid binder, concrete operation step
It is as follows: powder being placed in culture dish, is put into baking oven, 3 hours of drying are placed on spare in drying bottle at 150 DEG C；Again
Powder is poured into the grinding of plant pulverizer, grinds 20 seconds and stops 90 seconds, repetitive operation 3 times, main function is substrate and fringing.
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| CN101713751A (en) * | 2009-12-07 | 2010-05-26 | 巨石集团有限公司 | Method for detecting chemical components of alkali-free glass by mixing X-ray fluorescence spectrometry with compression method |
| CN103323479A (en) * | 2013-06-18 | 2013-09-25 | 芜湖东旭光电科技有限公司 | Glass mixed batch uniformity determination method |
| CN104237277A (en) * | 2014-08-29 | 2014-12-24 | 无锡英普林纳米科技有限公司 | Method for analyzing minor elements in geological sample by utilizing X-fluorescent spectrum |
| CN104267054A (en) * | 2014-08-29 | 2015-01-07 | 无锡英普林纳米科技有限公司 | Method for analyzing main elements in geological sample by utilizing X-fluorescence spectrum |
| CN105572295A (en) * | 2016-02-04 | 2016-05-11 | 东旭（营口）光电显示有限公司 | Method of determining content of boron oxide in glass |
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2017
- 2017-05-16 CN CN201710343497.0A patent/CN106990129B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101713751A (en) * | 2009-12-07 | 2010-05-26 | 巨石集团有限公司 | Method for detecting chemical components of alkali-free glass by mixing X-ray fluorescence spectrometry with compression method |
| CN103323479A (en) * | 2013-06-18 | 2013-09-25 | 芜湖东旭光电科技有限公司 | Glass mixed batch uniformity determination method |
| CN104237277A (en) * | 2014-08-29 | 2014-12-24 | 无锡英普林纳米科技有限公司 | Method for analyzing minor elements in geological sample by utilizing X-fluorescent spectrum |
| CN104267054A (en) * | 2014-08-29 | 2015-01-07 | 无锡英普林纳米科技有限公司 | Method for analyzing main elements in geological sample by utilizing X-fluorescence spectrum |
| CN105572295A (en) * | 2016-02-04 | 2016-05-11 | 东旭（营口）光电显示有限公司 | Method of determining content of boron oxide in glass |
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