CN105699365A - Method for measuring content of cerium in glass - Google Patents
Method for measuring content of cerium in glass Download PDFInfo
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Abstract
The invention relates to the field of glass processing, and discloses a method for measuring the content of cerium in glass. The method includes (1), grinding the to-be-measured glass to obtain glass powder, adding hydrofluoric acid into the glass powder, carrying out primary heat treatment on the glass powder to obtain products, adding perchloric acid into the products obtained by means of primary heat treatment, and carrying out secondary heat treatment on the products to obtain completely dissolved solution of the glass; (2), metering the completely dissolved solution of the glass by the aid of water to obtain constant-volume solution and measuring the content of cerium in the constant-volume solution; (3), determining the content of the cerium in the to-be-measured glass according to the volume of the constant-volume solution and the measured content of the cerium in the constant-volume solution. The method for measuring the content of the cerium in the glass has the advantages of easiness in operation, few matrix effects, high precision, standard recovery rate and result credibility, low detection limit and capability of completely meeting production requirements.
Description
Technical field
The present invention relates to glass processing field, measure the method for cerium content in glass in particular it relates to a kind of, especially measure the method for cerium (Ce) content in cover-plate glass。
Background technology
Research shows, cover-plate glass complicated component, and simple a kind of acid cannot be dissolved, even nitration mixture can not be dissolved simultaneously, wants to use inductive coupling plasma emission spectrograph to detect its low content composition, it appears particularly difficult。
Wherein, CeO2Cover-plate glass uses, it is possible to improve the acid and alkali-resistance erosion performance of cover-plate glass, but, CeO2Excessive other physical properties that also can reduce glass, therefore, measure in glass the CeO in especially cover-plate glass quickly and accurately2Content, particularly important for producing, help to ensure that the comprehensive physical performance of cover-plate glass, have important practical significance。
Summary of the invention
The invention aims to overcome drawbacks described above of the prior art, it is provided that a kind of measure the method for cerium content in glass。
To achieve these goals, the invention provides and a kind of measure the method for cerium content in glass, the method includes:
(1) glass grinding to be measured being become glass dust, add Fluohydric acid. and carry out the first heat treated in glass dust, add perchloric acid and carry out the second heat treated in the product then obtained to the first heat treated, what obtain glass is completely dissolved liquid；
(2) glass is completely dissolved liquid water constant volume, obtains constant volume liquid, and measure the cerium content in constant volume liquid；
(3) cerium content in glass to be measured is determined according to the volume of constant volume liquid and the cerium content of mensuration。
Preferably, in step (1), after Fluohydric acid. exhausts, in the product that described first heat treated obtains, add perchloric acid。
Preferably, in step (1), the condition of described first heat treated includes: temperature is 200-300 DEG C, more preferably 220-260 DEG C。
Preferably, in step (1), in 1g glass dust, the addition of Fluohydric acid. is 80-120ml, more preferably 90-100ml。
Preferably, in step (1), the condition of described second heat treated includes: temperature is 300-400 DEG C, more preferably 320-360 DEG C。
Preferably, in step (1), in 1g glass dust, the addition of perchloric acid is 20-40ml, more preferably 25-35ml。
Preferably, the particle diameter of glass dust is not more than 100 μm。
Preferably, in step (1), the embodiment of grinding for be ground in agate mortar。
Preferably, in step (1), described first heat treated and described second heat treated all carry out in platinum crucible。
Preferably, water during mensuration is deionized water, and perchloric acid is the pure perchloric acid of top grade, and Fluohydric acid. is the pure Fluohydric acid. of top grade。
Preferably, in step (2), inductive coupling plasma emission spectrograph is used to measure the cerium content in constant volume liquid。
Preferably, in step (3), through type I calculates the cerium content in glass to be measured:
W=C × V/m/1000 × 100% Formulas I
Wherein, W is the cerium content in glass to be measured, wt%；
C is the cerium content of constant volume liquid, mg/L；
V is the volume of constant volume liquid, L；
M is the quality of glass dust, g in step (1)。
Preferably, with the weight of glass for benchmark, described glass contains the SiO of 55-64wt%2, 10-18wt% Al2O3, 0-6wt% B2O3, 8-16wt% Na2The K of CaO, 0-12wt% of O, 0-4wt%2The ZrO of BaO, 0-4wt% of SrO, 0-2wt% of MgO, 0-2wt% of O, 0-10wt%2, 0-2wt% the CeO of ZnO and 0-1wt%2；
It is further preferred that with the weight of glass for benchmark, described glass contains the SiO of 56-60wt%2, 11-17wt% Al2O3, 0.1-5wt% B2O3, 10-15wt% Na2The K of CaO, 2-10wt% of O, 0.01-3wt%2The ZrO of BaO, 0.1-3.5wt% of SrO, 0.01-1wt% of MgO, 0.01-1wt% of O, 1-9wt%2, 0.01-1wt% the CeO of ZnO and 0.05-0.9wt%2。
The present invention measures the method for cerium content in glass, Fluohydric acid. and two kinds of acid of perchloric acid are adopted to be dissolved by glass dust step heating, adopt ICP-OES quantitative detecting analysis method simultaneously, the difficult problem successfully having solved low content composition detection in cover-plate glass not, and the method is simple to operate, matrix effect is little, precision is high, recovery of standard addition is high, detection limit low (detection limit can reach 0.01ppm (i.e. 0.01 μ g/mL)), analyze quick and precisely, credible result degree height。The method of the present invention, it is adaptable to all types of glass, is particularly suited for insoluble cover-plate glass。
Preferred embodiment, (1) adds the pure perchloric acid of top grade heating for dissolving cover-plate glass powder in two steps with the pure Fluohydric acid. of top grade to one according to the present invention, and weighing 0.1-0.5g glass dust can detect；(2) can dissolving whole composition with Fluohydric acid. and perchloric acid, testing result is true and reliable；(3) the ICP-OES quantitative detecting analysis method detection of constant volume liquid is analyzed, (essential element in cover-plate glass is silicon not to have matrix interference, other compositions are low content or trace, owing to overwhelming majority element silicon is waved away with the form of Silicon fluoride., therefore matrix effect can be ignored), treating that test sample only needs one, save the pre-treatment time, testing result is with a high credibility。
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently。
Detailed description of the invention
Hereinafter the specific embodiment of the present invention is described in detail。It should be appreciated that detailed description of the invention described herein is merely to illustrate and explains the present invention, it is not limited to the present invention。
End points and any value of scope disclosed in this article are not limited to this accurate scope or value, and these scopes or value should be understood to the value comprised close to these scopes or value。For numerical range, between the endpoint value of each scope, between endpoint value and the independent point value of each scope, and between independent point value can combination with one another and obtain one or more new numerical range, these numerical rangies should be considered specifically open in this article。
The invention provides and a kind of measure the method for cerium content in glass, the method includes:
(1) glass grinding to be measured being become glass dust, add Fluohydric acid. and carry out the first heat treated in glass dust, add perchloric acid and carry out the second heat treated in the product then obtained to the first heat treated, what obtain glass is completely dissolved liquid；
(2) glass is completely dissolved liquid water constant volume, obtains constant volume liquid, and measure the cerium content in constant volume liquid；
(3) cerium content in glass to be measured is determined according to the volume of constant volume liquid and the cerium content of mensuration。
In the method for the present invention, in order to faster dissolve glass dust more easily, it is preferable that in situation, in step (1), the particle diameter of glass dust is not more than 100 μm。
In the method for the present invention, in order to reduce the introducing of impurity in mensuration process, reduce evaluated error, it is preferable that in situation, in step (1), the embodiment of grinding for be ground in agate mortar。
In the method for the present invention, in order to reduce the introducing of impurity in mensuration process, reduce evaluated error, it is preferable that in situation, in step (1), described first heat treated and described second heat treated all carry out in platinum crucible。
Process of the present invention it is preferred in situation, in step (1), after Fluohydric acid. exhausts, add perchloric acid in the product that described first heat treated obtains。It will be appreciated by persons skilled in the art that Fluohydric acid. exhausts and be meant to no liquid existence in platinum crucible when the first heat treated terminates。
Process of the present invention it is preferred in situation, in step (1), the condition of the first heat treated includes: temperature is 200-300 DEG C, more preferably 220-260 DEG C。For time of the first heat treated, there is no particular limitation, as long as can be exhausted by Fluohydric acid., for instance can be 20-40min。
In the method for the present invention, for the addition of Fluohydric acid., there is no particular limitation, as long as finally can be completely dissolved by glass dust。Under preferable case, in step (1), in 1g glass dust, the addition of Fluohydric acid. is 80-120ml, more preferably 90-100ml。
Process of the present invention it is preferred in situation, in step (1), the condition of the second heat treated includes: temperature is 300-400 DEG C, more preferably 320-360 DEG C。For time of the second heat treated, there is no particular limitation, as long as can be completely dissolved by glass dust, for instance can be 40-60min。
In the method for the present invention, for the addition of perchloric acid, there is no particular limitation, as long as finally can be completely dissolved by glass dust。Under preferable case, in step (1), in 1g glass dust, the addition of perchloric acid is 20-40ml, more preferably 25-35ml。It will be understood by those skilled in the art that the amount of Fluohydric acid. and the perchloric acid added in the inventive method is all excessive。
Process of the present invention it is preferred in situation, in order to improve mensuration degree of accuracy further, reduce error, it is preferable that in situation, water during mensuration is deionized water, and perchloric acid is the pure perchloric acid of top grade, and Fluohydric acid. is the pure Fluohydric acid. of top grade。Preferably, the concentration >=70wt% of the pure perchloric acid of top grade, the concentration >=40wt% of the pure Fluohydric acid. of top grade。
Process of the present invention it is preferred in situation, in step (2), use inductive coupling plasma emission spectrograph to measure the cerium content in constant volume liquid。
For using the method for the cerium content in inductive coupling plasma emission spectrograph mensuration constant volume liquid, there is no particular limitation, can be various methods commonly used in the art, can be such as: first select the wave-length coverage of 180-800nm that constant volume liquid is carried out qualitative scanning, obtain the qualitative half-quantitative detection result of Ce elements, then design interval the preparing standard solution of Ce elements corresponding to standard curve according to qualitative half-quantitative detection result, then adopt standard curve method to measure cerium content (during mensuration background correction)。Concrete operating process is conventionally known to one of skill in the art, does not repeat them here。
Process of the present invention it is preferred in situation, in step (3), through type I calculates the cerium content in glass to be measured:
W=C × V/m/1000 × 100% Formulas I
Wherein, W is the cerium content in glass to be measured, wt%；
C is the cerium content of constant volume liquid, mg/L；
V is the volume of constant volume liquid, L；
M is the quality of glass dust, g in step (1)。
The method of the present invention may be used for measuring the glass of all kinds, is particularly suited for cover-plate glass, it is preferable that in situation, and with the weight of glass for benchmark, described glass contains the SiO of 55-64wt%2, 10-18wt% Al2O3, 0-6wt% B2O3, 8-16wt% Na2The K of CaO, 0-12wt% of O, 0-4wt%2The ZrO of BaO, 0-4wt% of SrO, 0-2wt% of MgO, 0-2wt% of O, 0-10wt%2, 0-2wt% the CeO of ZnO and 0-1wt%2。Preferably, with the weight of glass for benchmark, described glass contains the SiO of 56-60wt%2, 11-17wt% Al2O3, 0.1-5wt% B2O3, 10-15wt% Na2The K of CaO, 2-10wt% of O, 0.01-3wt%2The ZrO of BaO, 0.1-3.5wt% of SrO, 0.01-1wt% of MgO, 0.01-1wt% of O, 1-9wt%2, 0.01-1wt% the CeO of ZnO and 0.05-0.9wt%2。
Embodiment
Hereinafter will be described the present invention by embodiment, but and be not so limited the present invention。In following example, if no special instructions, each material and reagent all can pass through commercially available, and each method is this area conventional method。
The pure perchloric acid of top grade is purchased from Solution on Chemical Reagents in Shanghai company limited of traditional Chinese medicines group, and concentration is 70wt%。
The pure Fluohydric acid. of top grade is purchased from Solution on Chemical Reagents in Shanghai company limited of traditional Chinese medicines group, and concentration is 40wt%。
Inductive coupling plasma emission spectrograph is purchased from JY company of France。
Precision electronic balance is purchased from prunus mume (sieb.) sieb.et zucc. Teller-Tuo benefit instrument company, and absolute precision scale division value is 0.1mg。
Each standard solution (such as cerium single element Standard Stock solutions) is purchased from Zhen Zhun bio tech ltd, Shanghai。
The composition of glass sample used in embodiment: with the weight of glass for benchmark, glass contains the SiO of 57.5wt%2, 12.5wt% Al2O3, 0.1wt% B2O3, 12wt% Na2The K of CaO, 5wt% of O, 0.1wt%2The ZrO of BaO, 3wt% of SrO, 0.5wt% of MgO, 1wt% of O, 7wt%2, 0.8wt% the CeO of ZnO and 0.5wt%2, namely the content of Ce elements is about 0.407wt%。
Embodiment 1
The present embodiment is for illustrating that the present invention's measures the method for cerium content in glass。
(1) from zero defect, glass sample indefectible, cleaning, drying, cut 35g with diamant, put into the glass dust grinding to form 3-8 μm in agate mortar, put into valve bag mix homogeneously。
(2) in valve bag, take out 10g glass dust, put in the tared dish of cleaning, drying, after 110 DEG C of drying in oven 2h, put into exsiccator be cooled to 25 DEG C, standby。
(3) the 0.1000g glass dust dried accurately is weighed by precision electronic balance, it is placed in the platinum crucible of cleaning, drying, then in platinum crucible, add the pure Fluohydric acid. of 9ml top grade, platinum crucible is placed on resistance furnace at 250 DEG C and heats 25min, by completely depleted for pure for top grade Fluohydric acid., in platinum crucible, then add the pure perchloric acid of 2.5ml top grade, resistance furnace heats at 350 DEG C 50min, being completely dissolved by glass dust, what obtain glass dust is completely dissolved liquid。
(4) it is completely dissolved after liquid is cooled to 25 DEG C until glass dust, the liquid that is completely dissolved of glass dust is transferred in 50ml politef volumetric flask, then platinum crucible is cleaned with deionized water, and cleanout fluid is transferred in aforementioned 50ml politef volumetric flask, use deionized water constant volume, obtain constant volume liquid。
(5) blank experiment is done: test according to step (3)-(4), the difference is that, step is added without glass dust in (3) in platinum crucible, obtains blank constant volume liquid。
(6) cerium content in constant volume liquid is measured with ICP-OES: start ICP-OES main frame, cooling-water machine and recirculated water, open high-purity argon gas, instrument condition is set: RF power is 1300W, plasma gas flow rate is 12L/min, atomization gas flow is 0.8L/min, assisted gas flow is 0L/min, and cooling gas flow is 2L/min。Lighting plasma flame, point is stablized 10min after catching fire and is tested。First carry out instrumental correction, seek zero order light and carry out the correction of reference line。Secondly constant volume liquid is carried out qualitative and half-quantitative analysis by chosen wavelength range 180-800nm, and the qualitative half-quantitative detection result of the Ce elements obtaining qualitative scanning is: the line wavelength of Ce elements is 413.380nm, and concentration is 8.31mg/L。The interval of Ce elements corresponding to standard curve is designed according to aforementioned qualitative semi-quantitative results, and preparing standard solution, wherein, deionized water, standard solution 1, standard solution 2, standard solution 3 cerium content respectively 0ppm, 4.0ppm, 8.0ppm, 12.0ppm, reset testing conditions: the detection line wavelength of Ce elements is 413.380nm, RF power to be 1200kW, assisted gas flow be 0.5L/min, the time of integration are 10s, atomization gas flow to be 0.55L/min, pump speed be 50r/min, pump stabilization time are 0s。After mensuration, obtaining standard curve: I=9.26+2780.51*C, wherein, C is cerium content, and I is intensity。The cerium content obtaining constant volume liquid after utilizing this standard curve and deducting blank constant volume liquid is 8.12mg/L。
(7) cerium content that through type I calculates in glass sample is 0.406wt%, wherein:
W=C × V/m/1000 × 100% Formulas I
W is the cerium content in glass to be measured, wt%；
C is the cerium content of constant volume liquid, mg/L；
V is the volume of constant volume liquid, L；
M is the quality of glass dust, g in step (3)。
(8) spectral line interference analysis
Prepare standard solution (50 μ g/mL) and Ce, Al, K, Na, Ca mixed solution (each concentration of element is 50 μ g/mL) of Ce element respectively, measure the intensity of spectral line of Ce element respectively, find Ce element spectral line intensity unchanged, illustrate other elements to Ce element without matrix interference。
(9) detection limit analysis
Utilize above-mentioned standard working curve, Ce concentration in 11 deionized waters of continuous detecting, calculate standard deviation (SD), then be multiplied by 3 and be detection limit。After measured, the detection of Ce elements is limited to 0.01ppm。
(10) accuracy analysis
It is separately added into a certain amount of spectroscopic pure CeO in the glass sample that above-mentioned testing result cerium content is 0.406wt%2(particle diameter 3-8 μm), makes addition spectroscopic pure CeO2After glass dust in Ce content it is known that
It is specifically shown in table 1:
Table 1
| Element | Background values (wt%) | Addition (wt%) | Measured value (wt%) | Recovery of standard addition % |
| Ce | 0.406 | 0.2 | 0.601 | 99.17 |
| Ce | 0.406 | 0.4 | 0.811 | 100.62 |
As seen from the results in Table 1, recovery of standard addition, between 99.17%-100.62%, illustrates that the accuracy of the method is significantly high。
(11) Precision Analyze
The glass dust that in step (2), 0.1000g has been dried is accurately weighed by precision electronic balance, according to step (3)-(7), same sample is additionally carried out 11 parallel analysis (sample number into spectrum is corresponding 1#-11# respectively), and measurement result is as shown in table 2。
Table 2
From table 2 data, the assay method of the embodiment of the present invention 1, discreteness is good, precision is high, with a high credibility, relative standard deviation (less than 5%) is only small, illustrates that the present invention's measures the method for cerium content in glass, matrix effect is little, precision is high, recovery of standard addition is high, detection limit is low, credible result degree high, is entirely capable of meeting the demand of production。Additionally, the method for the present invention has obtained checking in production line, the control of cover-plate glass physical property is had great importance。
Embodiment 2
Method according to embodiment 1, the difference is that, in step (3), the method being completely dissolved liquid obtaining glass dust is: accurately weigh the 0.1000g glass dust dried by precision electronic balance, it is placed in the platinum crucible of cleaning, drying, then in platinum crucible, add the pure Fluohydric acid. of 9.5ml top grade, platinum crucible is placed on resistance furnace at 220 DEG C and heats 40min, by completely depleted for pure for top grade Fluohydric acid., then in platinum crucible, add the pure perchloric acid of 3ml top grade, resistance furnace heats at 320 DEG C 60min, glass dust is completely dissolved, what obtain glass dust is completely dissolved liquid。
After measured, the cerium content of constant volume liquid is 8.13mg/L, is computed, and the cerium content in glass sample is 0.4065wt%。
Embodiment 3
Method according to embodiment 1, the difference is that, in step (3), the method being completely dissolved liquid obtaining glass dust is: accurately weigh the 0.1000g glass dust dried by precision electronic balance, it is placed in the platinum crucible of cleaning, drying, then in platinum crucible, add the pure Fluohydric acid. of 10ml top grade, platinum crucible is placed on resistance furnace at 260 DEG C and heats 20min, by completely depleted for pure for top grade Fluohydric acid., then in platinum crucible, add the pure perchloric acid of 3.5ml top grade, resistance furnace heats at 360 DEG C 40min, glass dust is completely dissolved, what obtain glass dust is completely dissolved liquid。
After measured, the cerium content of constant volume liquid is 8.14mg/L, is computed, and the cerium content in glass sample is 0.407wt%。
The method of cerium content in glass that measures of the present invention, simple to operate, matrix effect is little, precision is high, recovery of standard addition is high, detection limit is low, credible result degree high, is entirely capable of meeting the demand of production。
The preferred embodiment of the present invention described in detail above; but, the present invention is not limited to the detail in above-mentioned embodiment, in the technology concept of the present invention; technical scheme can being carried out multiple simple variant, these simple variant belong to protection scope of the present invention。
It is further to note that, each concrete technical characteristic described in above-mentioned detailed description of the invention, in reconcilable situation, it is possible to be combined by any suitable mode, in order to avoid unnecessary repetition, various possible compound modes are no longer illustrated by the present invention separately。
Additionally, can also carry out combination in any between the various different embodiment of the present invention, as long as it is without prejudice to the thought of the present invention, it should be considered as content disclosed in this invention equally。
Claims (11)
1. one kind measures the method for cerium content in glass, it is characterised in that the method includes:
(1) glass grinding to be measured being become glass dust, add Fluohydric acid. and carry out the first heat treated in glass dust, add perchloric acid and carry out the second heat treated in the product then obtained to the first heat treated, what obtain glass is completely dissolved liquid；
(2) glass is completely dissolved liquid water constant volume, obtains constant volume liquid, and measure the cerium content in constant volume liquid；
(3) cerium content in glass to be measured is determined according to the volume of constant volume liquid and the cerium content of mensuration。
2. method according to claim 1, it is characterised in that in step (1), after Fluohydric acid. exhausts, adds perchloric acid in the product that described first heat treated obtains。
3. method according to claim 1 and 2, it is characterised in that in step (1), the condition of described first heat treated includes: temperature is 200-300 DEG C, it is preferred to 220-260 DEG C。
4. method according to claim 1 and 2, it is characterised in that in step (1), in 1g glass dust, the addition of Fluohydric acid. is 80-120ml, it is preferred to 90-100ml。
5. method according to claim 1 and 2, it is characterised in that in step (1), the condition of described second heat treated includes: temperature is 300-400 DEG C, it is preferred to 320-360 DEG C。
6. method according to claim 1 and 2, it is characterised in that in step (1), in 1g glass dust, the addition of perchloric acid is 20-40ml, it is preferred to 25-35ml。
7. method according to claim 1 and 2, it is characterised in that the particle diameter of glass dust is not more than 100 μm；
Preferably, in step (1), the embodiment of grinding for be ground in agate mortar；
Preferably, in step (1), described first heat treated and described second heat treated all carry out in platinum crucible。
8. the method according to any one in claim 1-7, it is characterised in that water during mensuration is deionized water, perchloric acid is the pure perchloric acid of top grade, and Fluohydric acid. is the pure Fluohydric acid. of top grade。
9. method according to claim 1 and 2, it is characterised in that in step (2), uses inductive coupling plasma emission spectrograph to measure the cerium content in constant volume liquid。
10. method according to claim 1 and 2, it is characterised in that in step (3), through type I calculates the cerium content in glass to be measured:
W=C × V/m/1000 × 100% Formulas I
Wherein, W is the cerium content in glass to be measured, wt%；
C is the cerium content of constant volume liquid, mg/L；
V is the volume of constant volume liquid, L；
M is the quality of glass dust, g in step (1)。
11. the method according to any one in claim 1-10, it is characterised in that with the weight of glass for benchmark, described glass contains the SiO of 55-64wt%2, 10-18wt% Al2O3, 0-6wt% B2O3, 8-16wt% Na2The K of CaO, 0-12wt% of O, 0-4wt%2The ZrO of BaO, 0-4wt% of SrO, 0-2wt% of MgO, 0-2wt% of O, 0-10wt%2, 0-2wt% the CeO of ZnO and 0-1wt%2；
Preferably, with the weight of glass for benchmark, described glass contains the SiO of 56-60wt%2, 11-17wt% Al2O3, 0.1-5wt% B2O3, 10-15wt% Na2The K of CaO, 2-10wt% of O, 0.01-3wt%2The ZrO of BaO, 0.1-3.5wt% of SrO, 0.01-1wt% of MgO, 0.01-1wt% of O, 1-9wt%2, 0.01-1wt% the CeO of ZnO and 0.05-0.9wt%2。
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| CN113945598A (en) * | 2021-09-07 | 2022-01-18 | 河北光兴半导体技术有限公司 | Evaluation method of glass strengthening ion exchange efficiency |
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