CN105548150A - Method for determining zirconium content in glass - Google Patents
Method for determining zirconium content in glass Download PDFInfo
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- CN105548150A CN105548150A CN201511022128.9A CN201511022128A CN105548150A CN 105548150 A CN105548150 A CN 105548150A CN 201511022128 A CN201511022128 A CN 201511022128A CN 105548150 A CN105548150 A CN 105548150A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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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
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Abstract
The invention relates to the field of glass processing and discloses a method for determining zirconium content in glass. The method comprises the following steps: (1) grinding to-be-determined glass into glass powder, successively adding water, perchloric acid and hydrofluoric acid into the glass powder, and then heating, thereby acquiring a glass solution; (2) maintaining constant volume of the glass solution with water, thereby acquiring a constant volume solution and determining the zirconium content in the constant volume solution; and (3) determining the zirconium content in the to-be-determined glass according to the volume of the constant volume solution and the determined zirconium content. The method provided by the invention has the advantages of simple operation, small matrix effect, high precision, high recovery rate, high efficiency, low detection limit, high result reliability and low cost. The method has important guiding significance in objectively reflecting the grade of the glass and the erosion condition of a tank furnace.
Description
Technical field
The present invention relates to glass processing field, particularly, relate to a kind of method measuring zirconium content in glass.
Background technology
In glass industry, the quality of fire resistive material for improve glass product seed output and quality, save fuel, extend melting furnaces serviceable life, reduce glass production cost and be significant.Along with the appearance of new quality refractory, strong impetus is played to glass industry modernization development.Aquarium kiln refractory is by aluminium-silicon (Al
2o
3-SiO
2) system is to aluminum-zirconium-silicon (Al
2o
3-ZrO
2-SiO
2) system, high alumina (Al
2o
3) System Development such as system and magnesia (MgO) goods, thus greatly facilitate the raising of tank furnace level.
Tank furnace temperature highest portion position and the position being subject to glass metal erosion the most serious, use electric smelting casting fused alumina zirconia (AZS) brick usually.
Zircon corundum brick is usually to contain ZrO
2amount number indicate different brick number.Formed primarily of two crystalline phases of α-corundum, baddeleyite and glassy phase in brick.Baddeleyite is except with except α-corundum eutectic, and all the other are free shape.Containing ZrO in brick
2more, the baddeleyite of free shape is more.The resistance to fouling of these two kinds of crystalline phases is all fine, and two kinds of crystalline phases are combined closely, and even structure is fine and close, and thus resistance to fouling is stronger.
First the Alteration of zircon corundum brick is that in melten glass brick and brick, unborn glassy phase is had an effect, diffusion dissolution gradually.Afterwards, the α-corundum in brick and monocline zircon slowly dissolve successively.Glass metal viscosity near brick surface increases, and defines erosion-resistant protective seam.Hand over reaction simultaneously and can produce α-corundum, nepheline, skeleton shape baddeleyite etc.Brick near the liquid level of usual pool wall top, the glass metal in its metamorphic layer obviously permeates to brick body, but α-corundum and baddeleyite eutectic are also connect by remaining glassy phase.At the brick of pool wall bottom, its surface is the glassy phase of α-corundum, the remaining body of baddeleyite and muddiness, produces nepheline matter liquid phase, dissolved a part of zircon, formed high viscosity metamorphic layer due to glassy phase in brick and glass metal reaction.When temperature reduces, the ZrO of dissolving
2secondary crystallization can be there is.Baddeleyite secondary crystallization mostly then is and nepheline crystallization coexists in the high viscosity layer of pool wall bottom.Along with the prolongation of service time, these two kinds of crystalline phases may be taken away by glass metal stream, then spread in glass metal further.More infusibilized baddeleyite, then may be partly dissolved and remain in glass metal and occur in finished product as calculus.
Therefore, in glass, the mensuration of zirconium content is particularly important for production, especially objectively can reflect the grade of glass and the erosion condition of tank furnace.
Zirconium content is in glass lower, and it is more difficult that it measures process, and what use was commonplace at present has soda melting ICP detection method, fluorescence detection.But these methods have respective drawback.Wherein, the shortcoming of soda melting ICP detection method: owing to have employed NaOH and sodium carbonate as flux, in glass specimen, the content of Zr element is natively very low, comparatively complicated plurality of reagents is used in sample handling processes, the severe jamming of matrix can be brought, cause ICP testing result confidence level to reduce.The shortcoming of fluorescence detection: the scope of fluoroscopic examination is percentage composition >1%, detecting reliability for trace element is lower, and fluorescence sample making course is complicated, sample needs to become to be applicable to the glass print of fluoroscopic examination through high-temperature fusion, this process is loaded down with trivial details, the time also longer, power cost is high.
Summary of the invention
The object of the invention is, in order to overcome above-mentioned defect of the prior art, to provide a kind of method measuring zirconium content in glass.
To achieve these goals, the invention provides a kind of method measuring zirconium content in glass, the method comprises:
(1) glass grinding to be measured is become glass dust, heat add water, perchloric acid and hydrofluorite successively in glass dust after, obtain glass dissolving liquid;
(2) glass dissolving liquid is used water constant volume, obtain constant volume liquid, and measure the zirconium content in constant volume liquid;
(3) zirconium content in glass to be measured is determined according to the volume of constant volume liquid and the zirconium content of mensuration.
Method of the present invention, simple to operate, matrix effect is little, precision is high, the recovery is high, detection limit is low, comparatively classic method efficiency is higher, credible result degree is high, cost is low, and has important directive significance to the erosion condition of the grade and tank furnace that objectively reflect glass.
According to one of the present invention preferred embodiment, (1) with the pure perchloric acid of top grade and the pure hydrofluoric acid dissolution glass dust of top grade, relatively large sample can be weighed, generally 1-3g can be reached, be 5-15 times of the sample dissolution amount (0.2g) of soda melting ICP detection method, thus greatly reduce the relative standard deviation of measurement result; (2) with perchloric acid and hydrofluoric acid dissolution glass dust, hydrofluorite is evaporated completely silicon dioxide, and perchloric acid can dissolve residue almost whole composition, and measurement result is true and reliable; (3) determine solution ICP-OES calibration curve method determination and analysis, eliminate Matrix effects, treat that test sample only needs one, save the time of sample preparation, measurement result confidence level comparatively classic method is high.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind of method measuring zirconium content in glass, the method comprises:
(1) glass grinding to be measured is become glass dust, heat add water, perchloric acid and hydrofluorite successively in glass dust after, obtain glass dissolving liquid;
(2) glass dissolving liquid is used water constant volume, obtain constant volume liquid, and measure the zirconium content in constant volume liquid;
(3) zirconium content in glass to be measured is determined according to the volume of constant volume liquid and the zirconium content of mensuration.
In method of the present invention, in order to dissolve glass dust more easily sooner, under preferable case, in step (1), the particle diameter of glass dust is not more than 10 μm.
In method of the present invention, in order to reduce introducing, the minimizing error at measurment of impurity in mensuration process, under preferable case, in step (1), the embodiment of grinding for grind in agate mortar.
In method of the present invention, for the addition of perchloric acid and hydrofluorite, there is no particular limitation, as long as glass dust can be dissolved completely.Measuring degree of accuracy to improve further, reducing error, under preferable case, water during mensuration is deionized water, and perchloric acid is the pure perchloric acid of top grade, and hydrofluorite is the pure hydrofluorite of top grade.It will be understood by those skilled in the art that the concentration >=70wt% of the pure perchloric acid of top grade, the concentration >=40wt% of the pure hydrofluorite of top grade.
In method of the present invention, under preferable case, in step (1), in 1g glass dust, the addition of deionized water is 1-2ml, and the addition of the pure perchloric acid of top grade is 4-10ml, and the addition of the pure hydrofluorite of top grade is 10-20ml.
In method of the present invention, for the condition heated, there is no particular limitation, as long as glass dust can be made to dissolve, obtain glass dissolving liquid, under preferable case, in step (1), the condition of heating comprises: temperature is 300-400 DEG C, and the time is 15-30min.Heating can be carried out on electric hot plate.
In method of the present invention, under preferable case, in step (2), add acid medium in glass dissolving liquid after, use water constant volume, obtain constant volume liquid.Further preferably, acid medium is salpeter solution, is further preferably >=the salpeter solution of 69wt%.For the addition of salpeter solution, there is no particular limitation, as long as make constant volume liquid for acid, preferably, in 100ml constant volume liquid, the addition of the salpeter solution of >=69wt% is 10ml.
In method of the present invention, under preferable case, in step (2), use the zirconium content in inductive coupling plasma emission spectrograph mensuration constant volume liquid.
For using inductive coupling plasma emission spectrograph to measure the method for the zirconium content in constant volume liquid, there is no particular limitation, the various methods can commonly used for this area, can be such as: first select the wavelength coverage of 200-800nm to carry out qualitative scanning to constant volume liquid, obtain the qualitative half-quantitative detection result of zr element, then according to the interval of zr element corresponding to qualitative half-quantitative detection result design standards curve and preparing standard solution, then calibration curve method is adopted to measure zirconium content.Concrete operating process is conventionally known to one of skill in the art, does not repeat them here.
In method of the present invention, under preferable case, in step (3), through type I calculates the zirconium content in glass to be measured:
W=C × V/m formula I
Wherein, W is the zirconium content in glass to be measured,
C is the zirconium content of constant volume liquid,
V is the volume of constant volume liquid,
M is the quality of carrying out the glass dust heated.
Embodiment
Below will be described the present invention by embodiment, but therefore not limit the present invention.In following examples, if no special instructions, each material and reagent are all by 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 hydrofluorite 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, and model is 2000-2.
Precision electronic balance is purchased from plum Teller-Tuo benefit instrument company, and model is Ms-s, and absolute precision scale division value is 0.1mg.
The standard solution (as zirconium single element Standard Stock solutions) of Criterion curve is purchased from Zhen Zhun bio tech ltd, Shanghai.
Embodiment 1
The present embodiment is for illustration of the method for zirconium content in mensuration glass of the present invention.
(1) from zero defect, glass sample that is indefectible, cleaning, drying (purchased from Shijiazhuang rising sun New Photoelectricity Technology Co., Ltd), 35g is cut with glass cutter, put into the glass dust that agate mortar grinds to form 3-8 μm, put into valve bag and mix.
(2) in valve bag, take out 15g glass dust, put into the measuring cup of cleaning, drying, after 110 DEG C of drying in oven 2h, put into exsiccator cool, for subsequent use.
(3) accurately take by precision electronic balance the glass dust that 1.0000g dried, and be placed in the platinum ware of cleaning, drying, then 1ml deionized water is first added moistening, add the pure perchloric acid of 5ml top grade and the pure hydrofluorite of 15ml top grade more successively, electric hot plate be heated to 400 DEG C and keep this temperature 20min, obtaining glass dissolving liquid.
(4) after glass dissolving liquid is cooled to 25 DEG C, glass dissolving liquid is transferred in 100ml teflon volumetric flask, then washed with de-ionized water platinum ware ware wall is used, and cleaning fluid is transferred in aforementioned 100ml teflon volumetric flask, use deionized water constant volume after adding the salpeter solution of 10ml69wt%, obtain constant volume liquid.
(5) blank assay is done: test according to step (3)-(4), unlike, step does not add glass dust in (3) in platinum ware, obtains blank constant volume liquid.
(6) measure the zirconium content in constant volume liquid with ICP-OES: start ICP-OES main frame, recirculated water and ventilation, open high-purity argon gas, instrument condition is set.After pipette is inserted deionized water, start operating key and peristaltic pump is rotated, by starting igniting after two minutes, stablizing 15min after point catches fire and testing.First carry out instrumental correction, seek zero order light and carry out the correction of reference line.Secondly chosen wavelength range 200-800nm carries out qualitative and half-quantitative analysis to constant volume liquid, obtains the qualitative half-quantitative detection result of the zr element of qualitative scanning.According to the interval of zr element corresponding to qualitative semi-quantitative results design standards curve, and preparing standard solution, wherein, the zirconium content of deionized water, standard solution 1, standard solution 2, standard solution 3 is respectively 0ppm, 0.2ppm, 0.4ppm, 0.6ppm, obtain typical curve: I=900.4+29056*C, wherein, C is zirconium content, and I is intensity.Utilize this typical curve and obtain the zirconium content of constant volume liquid for 0.45ppm after deducting blank constant volume liquid.
(7) through type I calculates the zirconium content in glass sample is 0.045 ‰, wherein:
W=C × V/m formula I
W is the zirconium content in glass to be measured,
C is the zirconium content of constant volume liquid,
V is the volume of constant volume liquid,
M is the quality of carrying out the glass dust heated.
(8) accuracy analysis
Recovery of standard addition is adopted to evaluate the accuracy of the method: to obtain glass dissolving liquid according to step (1)-(3), after glass dissolving liquid is cooled to 25 DEG C, glass dissolving liquid is transferred in 100ml teflon volumetric flask, then washed with de-ionized water platinum ware ware wall is used, and cleaning fluid is transferred in aforementioned 100ml teflon volumetric flask, add the salpeter solution of 10ml69wt%, add the zirconium single element Standard Stock solutions of 0.45ppm again, scale is settled to deionized water, measure final zirconium content, table 1 is recovery of standard addition result.
Table 1
| Element | Background values (ug/ml) | Addition (ug/ml) | Measured value (ug/ml) | Recovery of standard addition % |
| Zr | 0.45 | 0.45 | 0.89 | 98.89％ |
As seen from the results in Table 1, recovery of standard addition >95%, illustrates that the accuracy of the method is very high.
(9) Precision Analyze
Accurately take by precision electronic balance the glass dust that in step (2), 1.0000g has been dried, carry out 11 parallel analysiss (sample number into spectrum is corresponding 1#-11# respectively) to same sample, 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, and precision is high, with a high credibility; The data (0.46ppm) that the sample detection subsidiary with producer is reported compare, and relative deviation is 2.17%.Therefore, can find out, method relative standard deviation (less than 5%) of the present invention is very little, illustrates that the precision of the method for zirconium content in mensuration glass of the present invention is high, can meet the demand of producing completely.In addition, method of the present invention obtains checking in production line, has certain directive significance to production.
Comparative example 1
Comparative example 1 is for illustration of the method adopting soda melting ICP detection method to measure zirconium content in glass.
According to the method for embodiment 1, unlike, step (3) is: the NaOH melting on alcohol blast burner first 1g being placed in silver crucible, cools and add 0.2g glass dust and 2g NaOH after whole melting, again on alcohol blast burner, melt to whole dissolving, cooling.
The zirconium content of the constant volume liquid measured in step (6) is 0.68ppm.
In step (8), recovery of standard addition is 94.53%.
In step (9), Precision Analyze result is as shown in table 3.
Table 3
From table 3 data, the assay method of comparative example 1, discreteness is poor, and precision is low, and confidence level has much room for improvement; The data (0.46ppm) that the sample detection subsidiary with producer is reported compare, relative deviation is 47.8%, simultaneously that embodiment 1 is known with each results contrast of comparative example 1, method of the present invention, precision is high, the recovery is high, efficiency is high, credible result degree is high, cost is low, and has important directive significance to the erosion condition of the grade and tank furnace that objectively reflect glass.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out combination in any between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. measure a method for zirconium content in glass, it is characterized in that, the method comprises:
(1) glass grinding to be measured is become glass dust, heat add water, perchloric acid and hydrofluorite successively in glass dust after, obtain glass dissolving liquid;
(2) glass dissolving liquid is used water constant volume, obtain constant volume liquid, and measure the zirconium content in constant volume liquid;
(3) zirconium content in glass to be measured is determined according to the volume of constant volume liquid and the zirconium content of mensuration.
2. method according to claim 1, wherein, in step (1), the particle diameter of glass dust is not more than 10 μm.
3. method according to claim 2, wherein, in step (1), the embodiment of grinding for grind in agate mortar.
4. method according to claim 1, wherein, water during mensuration is deionized water, and perchloric acid is the pure perchloric acid of top grade, and hydrofluorite is the pure hydrofluorite of top grade.
5. method according to claim 4, wherein, in step (1), in 1g glass dust, the addition of deionized water is 1-2ml, and the addition of the pure perchloric acid of top grade is 4-10ml, and the addition of the pure hydrofluorite of top grade is 10-20ml.
6. method according to claim 1, wherein, in step (1), the condition of heating comprises: temperature is 300-400 DEG C, and the time is 15-30min.
7. method according to claim 1, wherein, in step (2), uses water constant volume in glass dissolving liquid, obtains constant volume liquid after adding acid medium.
8. method according to claim 7, wherein, described acid medium is salpeter solution.
9. the method according to claim 7 or 8, wherein, in step (2), uses the zirconium content in inductive coupling plasma emission spectrograph mensuration constant volume liquid.
10. method according to claim 1, wherein, in step (3), through type I calculates the zirconium content in glass to be measured:
W=C × V/m formula I
Wherein, W is the zirconium content in glass to be measured,
C is the zirconium content of constant volume liquid,
V is the volume of constant volume liquid,
M is the quality of carrying out the glass dust heated.
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| CN106525561A (en) * | 2016-11-03 | 2017-03-22 | 芜湖东旭光电科技有限公司 | Method for determining content of platinum and rhodium in glass |
| CN109856120A (en) * | 2019-01-09 | 2019-06-07 | 成都光明光电股份有限公司 | The measurement method of glass ingredient content |
| CN110243810A (en) * | 2019-07-01 | 2019-09-17 | 中国第一汽车股份有限公司 | The test method of zirconium content in a kind of metal material surface conversion film |
| CN110261198A (en) * | 2019-07-01 | 2019-09-20 | 中国第一汽车股份有限公司 | The preparation method and its quantitative approach of the standard test panel containing zirconium in a kind of metal material surface conversion film |
| CN113189126A (en) * | 2021-04-30 | 2021-07-30 | 河北南玻玻璃有限公司 | Method for detecting and analyzing tiny solid defects of float glass |
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| CN106092685A (en) * | 2016-06-12 | 2016-11-09 | 蚌埠中恒新材料科技有限责任公司 | A kind of sample treatment of inductively coupled plasma spectroscopic assay electric-melting zirconia |
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| CN113189126A (en) * | 2021-04-30 | 2021-07-30 | 河北南玻玻璃有限公司 | Method for detecting and analyzing tiny solid defects of float glass |
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