CN107290375A - The method for determining calcirm-fluoride in fluorite, calcium carbonate, sulphur, iron and dioxide-containing silica - Google Patents
The method for determining calcirm-fluoride in fluorite, calcium carbonate, sulphur, iron and dioxide-containing silica Download PDFInfo
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- CN107290375A CN107290375A CN201710368846.4A CN201710368846A CN107290375A CN 107290375 A CN107290375 A CN 107290375A CN 201710368846 A CN201710368846 A CN 201710368846A CN 107290375 A CN107290375 A CN 107290375A
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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
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/366—Moulds; Demoulding
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Abstract
The invention discloses a kind of method for determining calcirm-fluoride in fluorite, calcium carbonate, sulphur, iron and dioxide-containing silica, several calibration samples, fluorite sample to be measured are prepared into pressed powder sample, the fluorescence intensity of F, Si, Ca, Fe, S element in press sheet compression is determined with X-ray fluorescence spectrometer, draw calibration curve, the fluorescence intensity and calibration curve of F, Si, Ca, Fe, S element in fluorite powder print to be measured are compared to the mass percentage content for calculating F, Si, Ca, Fe, S element, then calculate CaF2、CaCO3And SiO2Mass percentage content；Each element content in sample is consistent with chemical method analysis result, and error is all controlled within 0.6%, and precision, the degree of accuracy and stability can meet quality of production detection requirement.This method is that can avoid the loss of fluorine element, and the corrosion in fluorite melting process to platinum crucible can be avoided again.
Description
Technical field
The present invention relates to determine CaF in fluorite2、CaCO3, S, Fe and SiO2The method of content, it is specifically a kind of to utilize
The method that pressed powder sample preparation method determines calcirm-fluoride in fluorite, calcium carbonate, sulphur, iron and dioxide-containing silica.
Background technology
Fluorite（Fluorite）Also known as fluorite, fluorspar powder, Fluorspar Powder, are a kind of mineral, isometric system, and its main component is
Calcirm-fluoride（CaF2）.Ferrous metallurgical industry often makes flux of fluorite to improve slag fluidity, reduces foreign substance in molten steel, improves steel
Water quality.Each testing agency generally according to《The measure of GB/T5195.1-2006 fluorite Calcium Fluoride Contents》Specified in mode pair
Calcium Fluoride Content in fluorite detected, this method by determining total calcium and calcium carbonate content in fluorite, according to two calcium it
Difference seeks the contained Calcium Fluoride Content of calculation.Humid analysis complex operation, cycle are long.
The application due to X-ray fluorescence spectra in metallurgical analysis increases in recent years, and majority is determined using fluorite MTG YBCO bulk
Wherein each component；Using fuse piece method, the content of wherein calcirm-fluoride is determined by determining in fuse piece fluorine the intensity of spectral line.Because fluorine is
Light element, spectral line is weak, low intensity, and fluorite melts sample process fluorine and has loss, the measurement result degree of accuracy of MTG YBCO bulk detection method
It is not accurate enough, it is impossible to meet production requirement.And in application X-ray fluorescence spectra fuse piece method detection process, fluorite sample contains
There is reducing substances, platinum crucible can be corroded.
The content of the invention
It is an object of the invention to provide a kind of side for determining calcirm-fluoride in fluorite, calcium carbonate, sulphur, iron and dioxide-containing silica
Method, i.e., can avoid the loss of fluorine element, and the corrosion in fluorite melting process to platinum crucible can be avoided again.
To reach above-mentioned purpose, the technical solution used in the present invention is：
Calcirm-fluoride in a kind of measure fluorite, calcium carbonate, sulphur, the method for iron and dioxide-containing silica, it comprises the following steps：
Step 1: choosing several fluorite calibration samples, 105 DEG C of drying 1h in dryer are respectively placed in, is placed in drier and is cooled to
Room temperature, is put into tungsten carbide vibration sample grinding machine and grinds, cross 100 mesh sieves, takes after appropriate calibration sample powder mixes with adhesive, puts
In tablet press machine mould, acid reagent is taken into 3.0g boric acid substrates after the sieving of 120 mesh, and uses boric acid fringing, fringing it is straight
Footpath is 0.3mm, the pressurize 30s under 30t pressure, is prepared into the smooth calibration print that thickness is 0.6mm；
Step 2: with X-ray fluorescence spectrometer to by step one handle each calibration sample in F, Si, Ca, Fe,
The intensity of S elements is measured, and obtains the fluorescence intensity of F, Si, Ca, Fe, S component in calibration sample；Respectively with each calibration sample
Each element mass percentage content is abscissa in product, using the fluorescence intensity of each element as ordinate, draws the glimmering of calibration sample
The light curve of spectrum, after overlap of spectral lines and basal image, carries out linear regression, obtains the calibration curve of each element；
Step 3: choosing fluorite sample to be measured, 105 DEG C of drying 1h, are placed in drier and are cooled to room temperature, be put into carbon in dryer
Change the powder that 100 mesh fineness are ground to form in tungsten vibration sample grinding machine, take the fluorite sample powder to be measured with calibrating print phase homogenous quantities
After being mixed with adhesive, it is placed in tablet press machine mould, acid reagent is taken into 3.0g boric acid substrates after the sieving of 120 mesh, is used in combination
Boric acid fringing, a diameter of 0.3mm of fringing, the pressurize 30s under 30t pressure are prepared into the smooth fluorite to be measured of 0.6mm thickness
Powder print；With fluorescence intensity of the X-ray fluorescence spectrometer to F, Si, Ca, Fe, S element in the last print of Fluorspar Powder to be measured
It is measured, is contrasted with the calibration curve of F, Si, Ca, Fe, S element in the calibration sample obtained by step 2, obtains to be measured
The mass percentage content of F, Si, Ca, Fe, S element in fluorite powder print；
Treated Step 4: being calculated according to F, Si element weight/mass percentage composition of the fluorite powder print to be measured obtained by step 3
Survey CaF in fluorite powder sample2、SiO2Mass percentage content, according to the gross mass degree and CaF of Ca elements2
Content calculates CaCO in fluorite powder sample to be measured indirectly3Mass percentage content.
It is preferred that, described adhesive is microcrystalline cellulose and stearic mixture, testing sample, microcrystalline cellulose, hard
The mass ratio of resin acid is 3:1:1.
CaF in fluorite sample to be measured in step 4 of the present invention2Mass percentage content calculation formula be：
（1）
Wherein coefficient 0.4867 is F elements in CaF2In shared molecular mass proportion；
CaCO in fluorite sample to be measured in step 4 of the present invention3Mass percentage content calculation formula be：
（2）
Wherein coefficient 0.4004 is Ca elements in CaCO3In shared molecular mass proportion；Coefficient 1.952 is CaF2Molecular weight/Ca
Element relative atomic mass calculates gained；
SiO in fluorite sample to be measured in step 4 of the present invention2Mass percentage content calculation formula be：
（3）
Wherein coefficient 0.4675 is Si elements in SiO2In shared molecular mass proportion.
Beneficial effects of the present invention are：
（1）Several calibration samples, fluorite sample to be measured are prepared into pressed powder sample by the present invention, with X-ray fluorescence spectra point
Analyzer determines the fluorescence intensity of F, Si, Ca, Fe, S element in press sheet compression, calibration curve is drawn, by fluorite powder print to be measured
In F, Si, Ca, Fe, S element fluorescence intensity and calibration curve be compared the quality for calculating F, Si, Ca, Fe, S element
Degree, then calculate CaF2、CaCO3And SiO2Mass percentage content；This method is that can avoid the damage of fluorine element
Lose, can avoid fluorite performance in the corrosion in fluorite melting process to platinum crucible, measurement process stable again, measurement data essence
Accuracy is high；
（2）The present invention is stronger using boric acid cohesive in sample powder tabletting, with low cost, easy sheet of characteristic, with boric acid
For substrate, boric acid fringing is used, prepared fluorite sample tabletting is more solid, it is easy to store.
Brief description of the drawings
Fig. 1 is the fluorescence spectrum calibration curve of F elements in calibration sample；
Fig. 2 is the fluorescence spectrum calibration curve of Ga elements in calibration sample.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment the present invention is further detailed explanation.
Calcirm-fluoride in a kind of measure fluorite, calcium carbonate, sulphur, the method for iron and dioxide-containing silica, it comprises the following steps：
Step 1: choosing 8 fluorite calibration samples, 105 DEG C of drying 1h in dryer are respectively placed in, is placed in drier and is cooled to room
Temperature, is put into tungsten carbide vibration sample grinding machine and grinds, cross 100 mesh sieves, takes after appropriate calibration sample powder mixes with adhesive, is placed in
In tablet press machine mould, with 3.0g boric acid substrate (acid reagent by 120 mesh sieve), and use boric acid fringing, fringing it is a diameter of
0.3mm, the pressurize 30s under 30t pressure, are prepared into the smooth calibration print that thickness is 0.6mm；
The content of each element is as shown in table 1 in 8 fluorite calibration samples.
Table 1
Step 2: with X-ray fluorescence spectrometer to by step one handle each calibration sample in F, Si, Ca, Fe,
The intensity of S elements is measured, and obtains the fluorescence intensity of F, Si, Ca, Fe, S component in calibration sample；Respectively with each calibration sample
Each element mass percentage content is abscissa in product, using the fluorescence intensity of each element as ordinate, draws the glimmering of calibration sample
The light curve of spectrum, after overlap of spectral lines and basal image, carries out linear regression, obtains the calibration curve of each element；
Wherein F elements, Ga elements fluorescence spectrum calibration curve as shown in Figure 1 and Figure 2.
The measuring condition of X-ray fluorescence spectrometer is as shown in table 2.
Table 2
Step 3: choosing fluorite sample to be measured, 105 DEG C of drying 1h, are placed in drier and are cooled to room temperature, be put into carbon in dryer
Change the powder that 100 mesh fineness are ground to form in tungsten vibration sample grinding machine, take the fluorite sample powder to be measured with calibrating print phase homogenous quantities
After being mixed with adhesive, it is placed in tablet press machine mould, with 3.0g boric acid substrate (acid reagent sieves by 120 mesh), and uses boron
Sour fringing, a diameter of 0.3mm of fringing, the pressurize 30s under 30t pressure are prepared into the smooth Fluorspar Powder to be measured of 0.6mm thickness
Last print；The fluorescence intensity of F, Si, Ca, Fe, S element in the last print of Fluorspar Powder to be measured is entered with X-ray fluorescence spectrometer
Row is determined, and is contrasted with the calibration curve of F, Si, Ca, Fe, S element in the calibration sample obtained by step 2, obtains firefly to be measured
The mass percentage content of F, Si, Ca, Fe, S element in stone powder print；
Treated Step 4: being calculated according to F, Si element weight/mass percentage composition of the fluorite powder print to be measured obtained by step 3
Survey CaF in fluorite powder sample2、SiO2Mass percentage content, according to the gross mass degree and CaF of Ca elements2
Content calculates CaCO in fluorite powder sample to be measured indirectly3Mass percentage content.
It is preferred that, described adhesive is microcrystalline cellulose and stearic mixture, testing sample, microcrystalline cellulose, hard
The mass ratio of resin acid is 3:1:1.
CaF in fluorite sample to be measured in step 4 of the present invention2Mass percentage content calculation formula be：
（1）
Wherein coefficient 0.4867 is F elements in CaF2In shared molecular mass proportion；
CaCO in fluorite sample to be measured in step 4 of the present invention3Mass percentage content calculation formula be：
（2）
Wherein coefficient 0.4004 is Ca elements in CaCO3In shared molecular mass proportion；Coefficient 1.952 is CaF2Molecular weight/Ca
Element relative atomic mass calculates gained；
SiO in fluorite sample to be measured in step 4 of the present invention2Mass percentage content calculation formula be：
（3）
Wherein coefficient 0.4675 is Si elements in SiO2In shared molecular mass proportion.
To verify the degree of accuracy of the method for the invention, the accuracy of this method is verified from 5 fluorite production samples,
As shown in table 3, contrasted from chemical score and this method, the accuracy of experimental data is good, as a result meet national standard permission
Deviation.
Table 3
Meanwhile, in order to verify the precision of the method for the invention, same sample has been carried out continuous 10 times identical molten sample and
CaF in MTG YBCO bulk method detection fluorite2、CaCO3, S, Fe and SiO2The operation of content.Investigated from the precision of experimental data
The stability of this method.By the as shown by data of table 4, CaF2、CaCO3, S, Fe and SiO2The relative standard deviation of content is all smaller
Within the scope of, illustrate that this method is reliable and stable.
Table 4
In summary, several calibration samples, fluorite sample to be measured are prepared into pressed powder sample by the present invention, use XRF
Spectroanalysis instrument determines the fluorescence intensity of F, Si, Ca, Fe, S element in press sheet compression, calibration curve is drawn, by Fluorspar Powder to be measured
The fluorescence intensity and calibration curve of F, Si, Ca, Fe, S element in last print, which are compared, calculates F, Si, Ca, Fe, S element
Mass percentage content, then calculate CaF2、CaCO3And SiO2Mass percentage content；Each element content in sample with
Chemical method analysis result is consistent, and error is all controlled within 0.6%, and precision, the degree of accuracy and stability can meet the quality of production
Detection is required.This method is that can avoid the loss of fluorine element, and the corruption in fluorite melting process to platinum crucible can be avoided again
Erosion.
Claims (2)
1. a kind of method for determining calcirm-fluoride in fluorite, calcium carbonate, sulphur, iron and dioxide-containing silica, it comprises the following steps：
Step 1: choosing several fluorite calibration samples, 105 DEG C of drying 1h in dryer are respectively placed in, is placed in drier and is cooled to
Room temperature, is put into tungsten carbide vibration sample grinding machine and grinds, cross 100 mesh sieves, takes after appropriate calibration sample powder mixes with adhesive, puts
In tablet press machine mould, acid reagent is taken into 3.0g boric acid substrates after the sieving of 120 mesh, and uses boric acid fringing, in 30t pressure
Lower pressurize 30s, it is calibration print smooth 0.6mm to be prepared into thickness；
Step 2: with X-ray fluorescence spectrometer to by step one handle each calibration sample in F, Si, Ca, Fe,
The intensity of S elements is measured, and obtains the fluorescence intensity of F, Si, Ca, Fe, S component in calibration sample；Respectively with each calibration sample
Each element mass percentage content is abscissa in product, using the fluorescence intensity of each element as ordinate, draws the glimmering of calibration sample
The light curve of spectrum, after overlap of spectral lines and basal image, carries out linear regression, obtains the calibration curve of each element；
Step 3: choosing fluorite sample to be measured, 105 DEG C of drying 1h, are placed in drier and are cooled to room temperature, be put into carbon in dryer
Change the powder that 100 mesh fineness are ground to form in tungsten vibration sample grinding machine, take the fluorite sample powder to be measured with calibrating print phase homogenous quantities
After being mixed with adhesive, it is placed in tablet press machine mould, acid reagent is taken into 3.0g boric acid substrates after the sieving of 120 mesh, is used in combination
Boric acid fringing, the pressurize 30s under 30t pressure is prepared into the smooth fluorite powder print to be measured of 0.6mm thickness；It is glimmering with X-ray
Light spectroanalysis instrument is measured to the fluorescence intensity of F, Si, Ca, Fe, S element in the last print of Fluorspar Powder to be measured, with step 2 institute
Calibration sample in the calibration curve of F, Si, Ca, Fe, S element contrasted, obtain F in fluorite powder print to be measured, Si,
The mass percentage content of Ca, Fe, S element；
Treated Step 4: being calculated according to F, Si element weight/mass percentage composition of the fluorite powder print to be measured obtained by step 3
Survey CaF in fluorite powder sample2、SiO2Mass percentage content, according to the gross mass degree and CaF of Ca elements2
Content calculates CaCO in fluorite powder sample to be measured indirectly3Mass percentage content.
2. the method according to claim 1 for determining calcirm-fluoride in fluorite, calcium carbonate, sulphur, iron and dioxide-containing silica, its
It is characterised by：Described adhesive is microcrystalline cellulose and stearic mixture, testing sample, microcrystalline cellulose, stearic
Mass ratio is 3:1:1.
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Cited By (9)
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| CN109324074A (en) * | 2018-10-30 | 2019-02-12 | 湖南航天磁电有限责任公司 | The method of x-ray fluorescence spectrometry strontium permanent-magnet ferrite component content |
| CN110376234A (en) * | 2019-07-10 | 2019-10-25 | 大唐东北电力试验研究院有限公司 | A kind of method of X-fluorescence energy disperse spectroscopy measurement content of calcium oxide in limestone |
| CN110609051A (en) * | 2019-08-14 | 2019-12-24 | 天津力神电池股份有限公司 | Method for detecting content of silicon-based material in lithium battery negative plate |
| CN111239169A (en) * | 2020-03-18 | 2020-06-05 | 重庆天泰铝业有限公司 | Method for analyzing electrolyte of aluminum electrolysis cell by oxygen measurement method and sampling device thereof |
| CN112415034A (en) * | 2020-10-09 | 2021-02-26 | 湖南省生态环境监测中心 | XRF (X-ray fluorescence) measurement and analysis method of solid waste |
| CN112748141A (en) * | 2020-12-28 | 2021-05-04 | 漳州旗滨玻璃有限公司 | Method for detecting selenium element in soda-lime-silica glass |
| CN112924437A (en) * | 2019-12-06 | 2021-06-08 | 核工业西南物理研究院 | Laser-induced breakdown spectroscopy absolute quantitative analysis method |
| CN113155879A (en) * | 2021-01-27 | 2021-07-23 | 邯郸钢铁集团有限责任公司 | Method for measuring contents of silicon dioxide and calcium fluoride in fluorite |
| CN113702411A (en) * | 2021-09-16 | 2021-11-26 | 福建贝思科电子材料股份有限公司 | Method for measuring molar ratio of calcium to zirconium in calcium zirconate |
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| CN112924437B (en) * | 2019-12-06 | 2023-02-21 | 核工业西南物理研究院 | Laser-induced breakdown spectroscopy absolute quantitative analysis method |
| CN111239169A (en) * | 2020-03-18 | 2020-06-05 | 重庆天泰铝业有限公司 | Method for analyzing electrolyte of aluminum electrolysis cell by oxygen measurement method and sampling device thereof |
| CN111239169B (en) * | 2020-03-18 | 2023-04-18 | 重庆天泰铝业有限公司 | Method for analyzing electrolyte of aluminum electrolysis cell by oxygen measurement method and sampling device thereof |
| CN112415034A (en) * | 2020-10-09 | 2021-02-26 | 湖南省生态环境监测中心 | XRF (X-ray fluorescence) measurement and analysis method of solid waste |
| CN112748141A (en) * | 2020-12-28 | 2021-05-04 | 漳州旗滨玻璃有限公司 | Method for detecting selenium element in soda-lime-silica glass |
| CN113155879A (en) * | 2021-01-27 | 2021-07-23 | 邯郸钢铁集团有限责任公司 | Method for measuring contents of silicon dioxide and calcium fluoride in fluorite |
| CN113702411A (en) * | 2021-09-16 | 2021-11-26 | 福建贝思科电子材料股份有限公司 | Method for measuring molar ratio of calcium to zirconium in calcium zirconate |
| CN113702411B (en) * | 2021-09-16 | 2022-12-16 | 福建贝思科电子材料股份有限公司 | Method for determining molar ratio of calcium to zirconium in calcium zirconate |
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Application publication date: 20171024 |