CN102004084B - Method for measuring contents of ferrous ions and iron ions in glass - Google Patents
Method for measuring contents of ferrous ions and iron ions in glass Download PDFInfo
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- CN102004084B CN102004084B CN2010105479175A CN201010547917A CN102004084B CN 102004084 B CN102004084 B CN 102004084B CN 2010105479175 A CN2010105479175 A CN 2010105479175A CN 201010547917 A CN201010547917 A CN 201010547917A CN 102004084 B CN102004084 B CN 102004084B
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Abstract
The invention discloses a method for measuring contents of ferrous ions and iron ions in glass, comprising the following steps: measuring the absorption spectrum of a provided glass sheet within the waveband range of 350-1100nm by using an ultraviolet and visible spectrophotometer; dividing the absorbency data in the absorption spectrum by the thickness of the glass sheet to obtain the absorbency of glass sheet with unit thickness, thereby further obtaining the spectrum curve of relationship between the wavelength in the absorption spectrum and the absorbency of the thickness of the glass sheet; carrying out smoothing treatment and basic line correction on the spectrum curve successively; and carrying out area integration on the spectrum curve after line correction respectively within the waveband range of 370-400nm and within the waveband range of 520-1100nm, and calculating the contents of iron ions and ferrous ions according to corresponding integrated areas. By using the method, the contents of iron ions and ferrous ions can be measured simultaneously, the operation is simple and fast, data processing is simple and convenient, and the reliability and the repeatability are good, therefore, the method can meet on-line monitoring requirement of glass and is applicable to industrial popularization.
Description
Technical field
The present invention relates to ferrous ion (Fe in a kind of glass
2+) and ferric ion (Fe
3+) content assaying method.
Background technology
Iron (Fe) is the key factor that influences glass quality.Iron in the glass has ferrous ion (Fe
2+) and ferric ion (Fe
3+) two kinds of existence forms.Ferrous ion (Fe
2+) have very strong colorability, be the principal element that influences the glass whiteness.In addition, ferrous ion (Fe
2+) can influence the radiant heat transfer of glass, thus the Temperature Distribution of glass melt in the glass melter influenced.In addition, ferrous ion (Fe in the glass
2+) and ferric ion (Fe
3+) ratio reflected the redox state of glass melt.Therefore, ferrous ion (Fe in monitoring and the control glass
2+) content and ferrous ion (Fe
2+) and ferric ion (Fe
3+) ratio be to optimize the key factor of process of glass, to eliminating bubble in the glass, improving glass quality and have a very important role.
The assay method of ferrous ion and iron ion content is a wet chemical analytical method in the conventional glass, and its normal principle that adopts is: utilize hydrogen fluoride (HF) and sulfuric acid (H
2SO4) fine ground glass powder is dissolved into solution, the ferrous ion (Fe in the solution
2+) generating orange red complex compound with Phen, there is stable absorption in the place at the 510nm wave band; Ferric ion (Fe
3+) generating blood red complex compound with thiocyanate, there is stable absorption in the place at the 470nm wave band, can measure ferrous ion (Fe respectively through the colorimetric between orange red complex compound and the blood red complex compound
2+) and ferric ion (Fe
3+) content.Yet this wet chemical analytical method measurement operation time is long, ferrous ion (Fe
2+) and ferric ion (Fe
3+) content need to measure respectively and because ferrous ion (Fe
2+) instability in solution, so measuring Fe
2+Generally to carry out operations such as lucifuge (military gentle and quiet, Yan Ke during content; With the oxidation-reduction degree of spectrophotometric-photoreduction survey iron processes fast measuring glass, spun glass, 2004; (5): 11～13); Experimental implementation is complicated, requirement for experiment condition is high, and therefore the accuracy of experiment and degree of accuracy have a greatly reduced quality, and can not satisfy the requirement of monitoring the glass redox state in the glass production at any time.
Hou Yinglan etc. have reported and have utilized original sheet glass to measure ferrous ion (Fe in the glass
2+) and ferric ion (Fe
3+) ratio new method (Hou Yinglan, Zhang Xianhua, Du Zhenyu, the research that concerns between the redox characteristic index variation of glass and glass microbubbles, glass, 2008,26 (2): 22～25), it sets up Fe according to the spectral absorption curve of iron oxide in glass
2+The linear relationship typical curve of the difference of concentration and 770nm wave band place and 1050nm wave band place absorbance, and Fe
3+Concentration and above-mentioned spectral absorption curve through after four differentiates in 360～420nm wavelength band the linear relationship typical curve of absorption maximum peak heights, measure the Fe in the glass sheet respectively
2+Content and Fe
3+Content, thus draw ferrous ion (Fe
2+) and ferric ion (Fe
3+) ratio.It is long that this glass sheet method has overcome in the above-mentioned traditional chemical analytic approach measurement operation time, Fe
2+And Fe
3+Content need to measure respectively and the mensuration process receives Fe
2+Unstable sex defective, simple and fast not only, and satisfy the requirement of monitoring the glass redox state in the glass production at any time.But, ferrous ion (Fe
2+) absorption all arranged in 400～1100nm wavelength band, and along with domestic and international market to the increasingly high requirement of deep processing glass (being generally white glass) quality, ferrous ion (Fe in the white glass
2+) content will be more and more lower, this moment infer Fe according to the difference of 770nm wave band place and 1050nm wave band place absorbance merely
2+Content may produce bigger error.
Therefore, be necessary to provide ferrous ion (Fe in a kind of improved glass
2+) and ferric ion (Fe
3+) content assaying method overcome the defective of prior art.
Summary of the invention
The purpose of this invention is to provide ferrous ion (Fe in a kind of glass
2+) and ferric ion (Fe
3+) content assaying method; Can not only overcome the defective of traditional chemical analytic approach, the measurement operation time is short, and the content of ferrous ion and ferric ion is measured simultaneously; The mensuration process does not receive that ferrous ion is instable to be influenced; Satisfy the requirement of monitoring the glass redox state in the glass production at any time, and can overcome the defective of the original sheet glass determination method of propositions such as Hou Yinglan, ferrous ion (Fe
2+) assay accuracy height.
To achieve these goals, the invention provides the content assaying method of ferrous ion and ferric ion in a kind of glass, comprise the steps:
Get original sheet glass, utilize ultraviolet-visible pectrophotometer to measure the absorption spectrum of original sheet glass in 350nm to 1100nm wavelength band;
Absorbance data in the absorption spectrum is obtained unit thickness glass sheet absorbance divided by the thickness of original sheet glass; And then the curve of spectrum of wavelength in the spectrum that is absorbed and unit thickness glass sheet absorbance relation; The curve of spectrum is successively carried out smoothing processing and baseline correction, to eliminate the influence of noise of instrument to test data;
The curve of spectrum after the baseline correction is carried out area integral in 370nm to 400nm wavelength band, the content of the absorption calculated by peak area ferric ion that obtains according to area integral, computing formula is: Fe
3+(wt%)=1.104 * S
370-400nm+ 2.906 * 10
-2, S wherein
370-400nmThe absorption peak area of representation unit thickness glass sheet absorption spectrum in 370nm to 400nm wavelength band;
The curve of spectrum after the baseline correction is carried out area integral in 520nm to 1100nm wavelength band, the content of the absorption calculated by peak area ferrous ion that obtains according to area integral, computing formula is: Fe
2+(wt%)=7.670 * 10
-3* S
520-1100nm+ 2.011 * 10
-2, S wherein
520-1100nmIt is the absorption peak area of unit thickness glass sheet absorption spectrum in 520nm to 1100nm wavelength band.
Compared with prior art, ferrous ion (Fe in the glass of the present invention
2+) and ferric ion (Fe
3+) content assaying method have following advantage:
1) adopt original sheet glass to measure, the running time is short, can survey ferrous ion (Fe simultaneously
2+) and ferric ion (Fe
3+) content, the mensuration process does not receive ferrous ion (Fe
2+) instable influence, so requirement for experiment condition is low, experimental implementation is simple, can satisfy the requirement of monitoring the glass redox state in the glass production at any time, has overcome all defect of traditional chemical analytic approach.
2) taken into full account ferrous ion (Fe
2+) absorbing state in 400～1100nm wavelength band, the curve of spectrum after the baseline correction is carried out area integral in the 520-1100nm wavelength band, and then calculate ferrous ion (Fe
2+) content, Fe
2+The assay error is little, has overcome the defective of the original sheet glass determination method of propositions such as Hou Yinglan.
3) whole test analytic process is all accomplished by ultraviolet-visible pectrophotometer and data processing software such as MS Excel, Origin software; Not only eliminated personal error basically, greatly reduced accidental error, test data is accurate, good reproducibility; And data processing is quick; Whole process is no more than 12 minutes, and because the ultraviolet-visible pectrophotometer cost is low, it is general to use, so this assay method is convenient to the industry popularization.
Through following description and combine accompanying drawing, it is more clear that the present invention will become, and these accompanying drawings are used to explain enforcement of the present invention.
Description of drawings
Fig. 1 is ferrous ion (Fe in the glass of the present invention
2+) and ferric ion (Fe
3+) the process flow diagram of content assaying method.
Fig. 2 has showed ferrous ion (Fe in the glass shown in Figure 1
2+) and ferric ion (Fe
3+) content assaying method in the curve of spectrum behind the curve smoothing.
Fig. 3 has showed ferrous ion (Fe in the glass shown in Figure 1
2+) and ferric ion (Fe
3+) content assaying method in the curve of spectrum after the baseline correction.
Fig. 4 has showed ferrous ion (Fe in the glass shown in Figure 1
2+) and ferric ion (Fe
3+) content assaying method in ferric ion (Fe
3+) content and ferric ion (Fe
3+) relation of absorption peak integral area.
Fig. 5 has showed ferrous ion (Fe in the glass shown in Figure 1
2+) and ferric ion (Fe
3+) content assaying method in ferrous ion (Fe
2+) content and ferrous ion (Fe
2+) relation of absorption peak integral area.
Embodiment
With reference now to accompanying drawing, describe instance of the present invention, the similar elements label is represented similar elements in the accompanying drawing.
Ferrous ion (Fe in the glass of the present invention
2+) and ferric ion (Fe
3+) the inventor of content assaying method adopt pure chemical reagent to found the normal glass sample of a series of different iron contents, utilize total iron (∑ Fe) content in the spectrophotometric determination o-phenanthroline normal glass sample (with Fe
2O
3Expression, the wt% of unit), utilize ferric ion (Fe in the ammonium thiocyanate spectrophotometry normal glass sample
3+) content (with Fe
2O
3Expression, the wt% of unit), total iron (∑ Fe) content and ferric ion (Fe
3+) content subtract each other and obtain ferrous ion (Fe
2+) content (as shown in table 1).Through above-mentioned Phen AAS and ammonium thiocyanate AAS, obtained the ferrous ion (Fe of standard in the glass sample of different total iron contents
2+) content and ferric ion (Fe
3+) content.
The inventor with above-mentioned normal glass sample wear into twin polishing, transmittance reaches the glass sheet more than 95%, utilizes ultraviolet-visible pectrophotometer to measure the absorption spectrum of glass sheet in the 350-1100nm wavelength band.Utilize Origin8.0 software that the absorbance data in the absorption spectrum is obtained unit thickness glass sheet absorbance divided by the thickness (mm of unit) of glass sheet; And then the curve of spectrum of the wavelength in the spectrum that is absorbed and unit thickness glass sheet absorbance relation, the curve of spectrum is successively carried out curve smoothing (smoothing parameter selects 25) and baseline correction with the influence of elimination noise of instrument to test data.The curve of spectrum behind the curve smoothing is seen Fig. 2, and the curve of spectrum after the baseline correction is seen Fig. 3.
Through ferrous ion (Fe in the research different glass sample
2+) content and ferric ion (Fe
3+) find ferric ion (Fe in the glass behind the curve of spectrum of the glass sheet that content is corresponding with each glass sample
3+) content is relevant with the absorption peak area (be the curve of spectrum integral area 370～400nm wavelength band in) of unit thickness glass sheet in 370～400nm wavelength band, ferrous ion (Fe
2+) content is relevant with the absorption peak area (be the curve of spectrum integral area 520～1100nm wavelength band in) of unit thickness glass sheet in 520～1100nm wavelength band.The integral area of the curve of spectrum of above-mentioned each normal glass sample unit thickness glass sheet in 370～400nm wavelength band and in 520～1100nm wavelength band seen table 1.
Table 1
In Origin8.0 software, with absorption peak area (integral area) S of the curve of spectrum in 370～400nm wavelength band
370～400nmBe X axle, Fe
3+Content is the Y axle, utilizes Fit Linear order to carry out linear fit, obtains ferric ion (Fe in the glass as shown in Figure 4
3+) content and the absorption peak area S of the curve of spectrum in 370～400nm wavelength band
370～400nmLinear relationship, the corresponding linear regression equation is:
Fe
3+(wt％)＝1.104×S
370-400nm+2.906×10
-2 (1)
Square R of this dependence among equations coefficient
2=0.9973, absorption peak area and the Fe of the curve of spectrum in 370～400nm wavelength band is described
3+The linear dependence of content is very good.Therefore utilize absorption peak area and the equation (1) of the curve of spectrum in 370～400nm wavelength band to calculate Fe
3+Content good reliability, accuracy height.
In Origin8.0 software, with absorption peak area (integral area) S of the curve of spectrum in 520～1100nm wavelength band
520～1100nmBe X axle, Fe
2+Content is the Y axle, utilizes Fit Linear order to carry out linear fit, obtains ferrous ion (Fe in the glass as shown in Figure 5
2+) content and the absorption peak area S of the curve of spectrum in 520～1100nm wavelength band
520～1100nmLinear relationship, the corresponding linear regression equation is:
Fe
2+(wt％)＝7.670×10
-3×S
520-1100nm+2.011×10
-2 (2)
Square R of this dependence among equations coefficient
2=0.9966, absorption peak area and the Fe of the curve of spectrum in 520～1100nm wavelength band is described
2+The linear dependence of content is very good, therefore utilizes absorption peak area and the equation (2) of the curve of spectrum in 520～1100nm wavelength band to calculate Fe
2+Content good reliability, accuracy height.
Can find out that by Fig. 4 and Fig. 5 the linear dependence of two curves is all fine, related coefficient square all approach 1, both compare and can obtain ferrous ion (Fe
2+) and ferric ion (Fe
3+) ratio.
In sum, ferrous ion (Fe in the glass of the present invention
2+) and ferric ion (Fe
3+) content assaying method comprise the steps:
Step S1 gets glass sheet, utilizes ultraviolet-visible pectrophotometer to measure the absorption spectrum of glass sheet in 350～1100nm wavelength band;
Step S2; Absorbance data in the absorption spectrum is obtained unit thickness glass sheet absorbance divided by the thickness of glass sheet; And then the curve of spectrum of wavelength in the spectrum that is absorbed and unit thickness glass sheet absorbance relation; The curve of spectrum is successively carried out smoothing processing and baseline correction, to eliminate the influence of noise of instrument to test data;
Step S3 carries out area integral to the curve of spectrum after the baseline correction in 370nm to 400nm wavelength band, the absorption peak area that obtains according to area integral passes through the content that formula (1) calculates ferric ion;
Step S4 carries out area integral to the curve of spectrum after the baseline correction in 520nm to 1100nm wavelength band, the absorption peak area that obtains according to area integral calculates ferrous ion content through formula (2).
Pass through two instances to ferrous ion (Fe in this glass according to above-mentioned principle below
2+) and ferric ion (Fe
3+) content assaying method be elaborated.
Instance one
The first step: getting thickness is the float glass sheet of 3.96mm, utilizes ultrasonic cleaner that it is cleaned, with the glass sheet oven dry that cleans up;
Second step: utilize ultraviolet-visible pectrophotometer to measure the absorption spectrum of glass sheet in 350～1100nm wavelength band, the data of absorption spectrum are saved as excel spreadsheet lattice file (expansion .xls by name);
The 3rd step: utilize data processing software such as MS Excel, Origin etc. to open the electronic form file (this patent is that example describes with Origin) in second step, wavelength is put into the X row, absorbance data is put into the Y row.Selected absorbance column data; Utilize set column values function that absorbance data is obtained unit thickness glass sheet absorbance divided by the thickness of glass sheet; Utilize the Plot-line order to draw, obtain the curve of spectrum of wavelength and unit thickness glass sheet absorbance relation, utilize the smoothing order that the curve of spectrum is carried out smoothing processing then; Smoothing parameter is 25, at last the curve of spectrum after level and smooth is carried out baseline correction;
The 4th step: utilize the integrate order respectively the curve of spectrum after the baseline correction to be carried out area integral in 370～400nm wavelength band He in 520～1100nm wavelength band, obtain ferric ion (Fe
3+) integral area (absorption peak area) be S
370～400nm=0.02708, obtain ferrous ion (Fe
2+) integral area (absorption peak area) be S
S20～1100nm=4.882;
The 5th step:, get Fe with the 4th step gained data difference substitution formula (1) and (2)
2+(wt%)=0.05756, Fe
3+(wt%)=0.05897, ∑ Fe (wt%)=Fe
2+(wt%)+Fe
3+(wt%)=0.1165, Fe
2+/ Fe
3+=0.9761.
Instance two
The first step: getting thickness is the high ferro glass sheet of 1.58mm, utilizes ultrasonic cleaner that it is cleaned, with the glass sheet oven dry that cleans up;
Second step: utilize ultraviolet-visible pectrophotometer to measure the absorption spectrum of glass sheet in 350～1100nm wavelength band, the data of absorption spectrum are saved as excel spreadsheet lattice file (expansion .xls by name);
The 3rd step: utilize data processing software such as MS Excel, Origin etc. to open the electronic form file (this patent is that example describes with Origin) in second step, wavelength is put into the X row, absorbance data is put into the Y row.Selected absorbance column data; Utilize set column values function that absorbance data is obtained unit thickness glass sheet absorbance divided by the thickness of glass sheet; Utilize the Plot-line order to draw, obtain the curve of spectrum of wavelength and unit thickness glass sheet absorbance relation, utilize the smoothing order that curve is carried out smoothing processing then; Smoothing parameter is 25, at last the curve after level and smooth is carried out baseline correction;
The 4th step: utilize the integrate order respectively the curve of spectrum after the baseline correction to be carried out area integral in 370～400nm wavelength band He in 520～1100nm wavelength band, obtain ferric ion (Fe
3+) integral area (absorption peak area) be S
370～400nM=0.2408 obtains ferrous ion (Fe
2+) integral area (absorption peak area) be S
520～1100nm=37.800;
The 5th step:, obtain Fe with the 4th step gained data difference substitution formula (1) and (2)
3+(wt%)=0.2950, Fe
2+(wt%)=0.3100, ∑ Fe (wt%)=Fe
2+(wt%)+Fe
3+(wt%)=0.6050, Fe
2+/ Fe
3+=1.051.
By on can know ferrous ion (Fe in the glass of the present invention
2+) and ferric ion (Fe
3+) content assaying method have following advantage:
1) adopt original sheet glass to measure, the running time is short, can survey ferrous ion (Fe simultaneously
2+) and ferric ion (Fe
3+) content, the mensuration process does not receive ferrous ion (Fe
2+) instable influence, so requirement for experiment condition is low, experimental implementation is simple, can satisfy the requirement of monitoring the glass redox state in the glass production at any time, has overcome all defect of traditional chemical analytic approach.
2) taken into full account ferrous ion (Fe
2+) absorbing state in 400～1100nm wavelength band, the curve of spectrum after the baseline correction is carried out area integral in 520～1100nm wavelength band, and then calculate ferrous ion (Fe
2+) content, Fe
2+The assay error is little, has overcome the defective of the original sheet glass determination method of propositions such as Hou Yinglan.
3) whole test analytic process is all accomplished by ultraviolet-visible pectrophotometer and data processing software such as MS Excel, Origin software; Not only eliminated personal error basically, greatly reduced accidental error, test data is accurate, good reproducibility; And data processing is quick; Whole process is no more than 12 minutes, because the ultraviolet-visible pectrophotometer cost is low, it is general to use, so this assay method is convenient to the industry popularization.
Invention has been described more than to combine most preferred embodiment, but the present invention is not limited to the embodiment of above announcement, and should contain various modification, equivalent combinations of carrying out according to essence of the present invention.
Claims (1)
1. the content assaying method of ferrous ion and ferric ion in the glass comprises the steps:
Get glass sheet, utilize ultraviolet-visible pectrophotometer to measure the absorption spectrum of glass sheet in 350nm to 1100nm wavelength band;
Absorbance data in the absorption spectrum is obtained unit thickness glass sheet absorbance divided by the thickness of glass sheet; And then the curve of spectrum of wavelength in the spectrum that is absorbed and unit thickness glass sheet absorbance relation, the curve of spectrum is successively carried out smoothing processing and baseline correction;
The curve of spectrum after the baseline correction is carried out area integral in 370nm to 400nm wavelength band, the content of the absorption calculated by peak area ferric ion that obtains according to area integral, computing formula is: Fe
3+(wt%)=1.104 * S
370～400nm+ 2.906 * 10
-2, Fe wherein
3+Content with Fe
2O
3Meter, S
370～400nmThe absorption peak area of representation unit thickness glass sheet absorption spectrum in 370nm to 400nm wavelength band;
The curve of spectrum after the baseline correction is carried out area integral in 520nm to 1100nm wavelength band, the content of the absorption calculated by peak area ferrous ion that obtains according to area integral, computing formula is: Fe
2+(wt%)=7.670 * 10
-3* S
520～1100nm+ 2.011 * 10
-2, Fe wherein
2+Content with Fe
2O
3Meter, S
520～1100nmIt is the absorption peak area of unit thickness glass sheet absorption spectrum in 520nm to 1100nm wavelength band.
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|---|---|---|---|
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|---|---|---|---|
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| CN102004084B true CN102004084B (en) | 2012-07-04 |
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| CN102288605A (en) * | 2011-08-25 | 2011-12-21 | 浙江天能电池(江苏)有限公司 | Method for rapidly determining iron content in concentrated sulphuric acid |
| FI125514B (en) * | 2012-05-25 | 2015-11-13 | Valmet Automation Oy | Apparatus and method for measuring a web containing cellulose and optionally lignin |
| CN103267737B (en) * | 2013-05-13 | 2015-06-17 | 浙江省质量检测科学研究院 | Quick detecting method of mass content of trace iron in photovoltaic glass |
| CN106198461A (en) * | 2016-08-16 | 2016-12-07 | 海南中航特玻科技有限公司 | Cr in test coloured glass2o3, the method for CoO content |
| CN108872114A (en) * | 2018-07-24 | 2018-11-23 | 彩虹显示器件股份有限公司 | A method of quick and precisely monitoring glass oxidation-reduction quality |
| CN110118739B (en) * | 2019-06-05 | 2021-09-10 | 四川虹科创新科技有限公司 | Method for measuring content of ferrous iron and ferric iron in glass |
| CN111562226B (en) * | 2020-04-10 | 2021-10-15 | 中国科学院西安光学精密机械研究所 | Method and system for analyzing total nitrogen and total phosphorus in seawater based on characteristic peak area of absorption spectrum |
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| CN1712932A (en) * | 2004-06-25 | 2005-12-28 | 中国洛阳浮法玻璃集团有限责任公司 | Test for Fe2+ and Fe3+ content in glass |
| CN1712933A (en) * | 2004-06-25 | 2005-12-28 | 中国洛阳浮法玻璃集团有限责任公司 | Test for Fe2+ and Fe3+ content in thin/super-thin glass |
| CN1813181A (en) * | 2003-06-24 | 2006-08-02 | 康宁股份有限公司 | Methods for quantifying the oxidation state of glass |
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| CN1813181A (en) * | 2003-06-24 | 2006-08-02 | 康宁股份有限公司 | Methods for quantifying the oxidation state of glass |
| CN1712932A (en) * | 2004-06-25 | 2005-12-28 | 中国洛阳浮法玻璃集团有限责任公司 | Test for Fe2+ and Fe3+ content in glass |
| CN1712933A (en) * | 2004-06-25 | 2005-12-28 | 中国洛阳浮法玻璃集团有限责任公司 | Test for Fe2+ and Fe3+ content in thin/super-thin glass |
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