CN104614279B - Method for determining content of gas in vitreous body by using density process - Google Patents

Method for determining content of gas in vitreous body by using density process Download PDF

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CN104614279B
CN104614279B CN201410843089.8A CN201410843089A CN104614279B CN 104614279 B CN104614279 B CN 104614279B CN 201410843089 A CN201410843089 A CN 201410843089A CN 104614279 B CN104614279 B CN 104614279B
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glass
sample
density
bubble
volume
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CN104614279A (en
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段秋桐
姜宏
赵会峰
有学军
周莉
杨剑
童云
代志祥
贺建雄
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Xinyi Glass (Hainan) Co.,Ltd.
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HAINAN AVIC SPECIAL GLASS MATERIALS CO Ltd
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Abstract

The invention belongs to the technical field of glass clarification quality evaluation and mainly relates to a method for determining the content of gas in a vitreous body by using a density process, which is used for evaluating the vitreous body clarification quality. The method comprises the following steps: determining the density of daily detected or common sodium calcium silicon glass required to be detected in a float glass production line by using a sedimentation method, indirectly reflecting the volume percentage of gas in the glass by using a linear equation, determining the density of one group of glass samples and the volume of the gas in the group of glass bubbles, building a relation curve between the density of the vitreous body and the volume of bubbles in the glass to calculate the volume of the bubbles in the vitreous body, and finally obtaining the volume percentage of the gas in the glass. The method is simple to operate, high in stability and reliable in result; serving as the reference for judging the clarification quality, the method is relatively high in reliability.

Description

A kind of method that densimetry determines gas content in vitreous body
Technical field
The invention belongs to glass clarifying technical field of quality evaluation, relates generally to a kind of densimetry and determines gas in vitreous body The method of content, for evaluating the quality of vitreous body clear quality.
Background technology
China just becomes the maximum country of glass production in the world from last century the nineties, and current production rate has reached More than the 50% of Gross World Product.There are at present 200 a plurality of float lines in China, and Dou You research and development departments of each glass factory are responsible for right The exploitation and simulation experiment of glass new product.Port simulates melting experiment to most basic in the good and bad basis for estimation of glass quality Condition be accomplished by detect port fusion cast glass sample in air bubble content number.Air bubble content is fewer to represent glass clarifying more It is good.The glass sample founded out during port simulation melting experiment is generally all containing many air bubble contents than industrial production line.
Current detection method is that glass specimen is observed using stereomicroscope or polarizing microscope, calculates glass The number of microbubble in sample, concrete grammar is that three kens, Cong Zhongguan are arbitrarily chosen on observed same glass specimen Examine the number of bubble.Bubble number what is observed in three kens is added, so as to judge glass formula or melting conditions Impact of the change to glass quality.There is following defect in the method:1. the bubble in simulation experiment glass sample is mostly distributed not Uniformly, the region for observing number of bubbles by personal subjective selection has subjective error.2. bubble is most in simulation experiment glass sample Small and dense collection, also easily to the wrong number of bubble number generation in glass blocks when human eye is observed by microscope.3. pair fusing The number of number of bubbles in the space of cubic unit centimetre is generally chosen when sample bubble number is observed how much to judge glass clarifying The quality of quality, and bubble overlaps a thickness direction mostly in fusion cast glass sample, human eye there is also subjectivity in observation Leakage number error.4. Air Bubble Size is different, single to judge that glass clarifying quality is inaccurate with number.4 points of the above is all current microscope The significant deficiency of sight glass bubble number.There are a large amount of subjective error when air bubble content is observed, this is to evaluating glass smelting The quality of quality also result in inevitable error.
This project is intended to overcome the shortcoming of above microscope observational method, and using the density for determining glass sample glass is reflected indirectly The overall content of gas in glass, so as to judge glass sample in gas content number, the quality of glass clarifying quality is made Objective evaluation.The invention provides a kind of test side of gas content in glass sample for glass industry research worker and manufacturing enterprise Method, simple to operate, good stability, reliable results.There is higher credibility as the foundation for judging clear quality.
The content of the invention
The purpose of the present invention is to propose to a kind of method that densimetry determines gas content in vitreous body, the method is using sedimentation The density that method determines the common soda-lime-silica glass of floatation glass production line routine testing or required detection is indirect by linear equation Reflect the percent by volume of gas in glass, by gas in the density and this group of glass blister that determine one group of glass sample Volume, the volume of bubble in setting up the density of vitreous body and the relation curve of Bubbles in Glass volume to calculate vitreous body, Finally give gas volume percentage ratio in glass.The method is simple to operate, good stability, reliable results.As judgement clarification matter The foundation of amount has higher credibility.
The present invention adopts following technical proposals to complete foregoing invention purpose:
A kind of method that densimetry determines gas content in vitreous body, methods described is applied to sodium silico-calcium white plate glass Glass, described method of testing comprises the steps:
1)Take one group of inside of the same batch of production line and make print to be measured, one group of glass specimen containing bubble glass sample of remaining silent No less than 10 pieces of samples;Print to be measured is cut into into 0.5mm3 ~0.7mm3Coupon, all surface requires polishing;Gas Bubble should retain in coupon after dicing;
2)Band bubble sample is measured using optical microscope, obtains the spheroid half of bubble in each piece of glass specimen Footpath, the shaft length of spheroid three;Using spheroid volume computing formula:With spheroid volume computing formulaCount respectively Calculate gas content in the volume i.e. bubble of bubble in vitreous body;Count respectively if it there are two kinds of form bubbles simultaneously in vitreous body Calculate to be summed up after volume and obtain total gas volume;
3)First sample in one group is put in Density Measuring Instrument test tube, the standard specimen of sample and known density floats over liquid simultaneously Surface;Density Measuring Instrument heating is opened, illuminator is opened in stirring;The temperature of record examination liquid in pipe is started simultaneously at, 0.01 is accurate to ℃;
4)Heating rate is 0.4 DEG C/min in initial 2 DEG C of intensification, and heating rate is 0.1 DEG C/min after 2 DEG C of intensification;Heat up Period need to not stop shaking test tube, it is to avoid sample and standard specimen are because surface tension of liquid factor " viscous " is in liquid surface;
5)Keep the heating rate of 0.1 DEG C/min persistently overheating, until standard specimen and sample at the uniform velocity sank by the graticule time-division Ji Lu not the temperature of standard specimen and sample when passing through graticule;
Other samples press step 3), step 4), step 5)Carry out, obtain each sample by temperature during graticule, And record;
6)The computing formula for determining glass density using sink and float method calculates the density of each piece of sample;
ρXB+(TS-TB)×(-0.00175)
ρX=sample to be tested density, g/cm3
ρB=standard sample density, 2.5003g/cm3
TSTemperature when=sample sinks, DEG C;
TBTemperature when=standard specimen sinks, DEG C;
7)The gas volume of one group of glass specimen and the data of density have been drawn by said method, relation has been drawn bent Line, draws linear relationship of the bubble gas volume with glass density and linear equation;
8)Determine the gas volume hundred in the common soda-lime-silica glass of floatation glass production line routine testing or required detection Divide ratio:
A. by the step of said method 3)- step 6)Obtain the density of detected glass specimen;
B. measurement detects the overall volume of glass specimen;
C. by above-mentioned steps 7)In the linear equation that draws calculate and detect bubble gas volume in glass specimen;
D. gas volume percentage in glass is drawn divided by detected glass specimen overall volume with gas volume in bubble Than.
A kind of method of testing for evaluating glass clarifying quality good or not proposed by the present invention, using densimetry to inside glass gas Body content is characterized, and realizes the quantification to glass clarifying quality good or not;By measuring a large amount of gas with various content glass Density, the gas content in setting up standard working curve to calculate vitreous body, with the high spy of simple to operate, measuring accuracy Point.
Description of the drawings
Fig. 1 is the fitting operations curve of gas volume and density in vitreous body.
Specific embodiment
The present invention is illustrated with reference to the drawings and specific embodiments:
1)Take the plate glass that one group of ten pieces of inside glass contains bubble of remaining silent and make print to be measured, print to be measured is cut into 0.5mm3Coupon, all surface requires polishing, and bubble should retain in coupon after dicing;
2)Band bubble sample is measured using optical microscope.The radius of acquisition spheroid bubble, the three of spheroid bubble Shaft length;Half r=118.576um of 2 spheroid bubble as samples;The 8 axle radius a of spheroid three=473.521um, b as samples =406.868um, c=466.875um. utilize spheroid volume computing formulaWith spheroid volume computing formulaPoint The volume for not calculating spheroid bubble in the vitreous body of sample 2 is:6.98×10-12m3;And ellipsoid bromhidrosis in the vitreous body of sample 8 Foam is accumulated:3.766×10-10m3;Calculate respectively if it there are two kinds of form bubbles simultaneously in vitreous body and summed up after volume Obtain total gas volume;
3)One of sample is put in Density Measuring Instrument test tube, sample and standard specimen float over liquid surface simultaneously.Open density Instrument is heated, stirring, opens illuminator;The initial temperature of liquid when recording each sample in vitro is started simultaneously at, is accurate to 0.01℃;
4)Heating rate is 0.4 DEG C/min in initial 2 DEG C of intensification, and heating rate is 0.1 DEG C/min after 2 DEG C of intensification.Heat up Period need to not stop shaking test tube, it is to avoid sample and standard specimen are because surface tension of liquid factor " viscous " is in liquid surface;
5)Keep heating rate persistently overheating, record standard specimen and sample at the uniform velocity sink and by solution temperature during graticule;
Other samples press step 3), step 4), step 5)Carry out, obtain each sample by temperature during graticule, And record;
Wherein, it is 30.72 DEG C that standard specimen at the uniform velocity sinks by the solution temperature of mark line;
6) computing formula for determining glass density using sink and float method calculates respectively the density of each piece of sample.
ρXB+(TS-TB)*(-0.00175)
ρX=sample to be tested density, g/cm3
ρB=standard sample density, 2.5003g/cm3
TSTemperature when=sample sinks, DEG C;
TBTemperature when=standard specimen sinks, DEG C;
It is 29.46 DEG C as the 2nd piece of glass specimen sinks by solution temperature during graticule, the density of the 2nd piece of glass specimen For:
ρX=2.5003+(29.46-30.72)•(-0.00175)=2.5025g/cm3
It is 31.85 DEG C as the 8th piece of glass specimen sinks by solution temperature during graticule, the density of the 8th piece of glass specimen For:
ρX=2.5003+(31.85-30.72)•(-0.00175)=2.4983g/cm3
7) glass specimen of ten gas with various contents, experimental result such as table 1, by what is measured are measured using said method Gas volume and glass specimen density drawing curve are shown in Fig. 1 in bubble, and by linear regression gas volume in bubble is drawn With the linear relationship equation of density:Y=228.50785-91.31368•X;Wherein, Y is gas volume in bubble, and X is density;Close Coefficients R2=0.99, dependency is good, illustrates working curve reliability.
8)In determining the common soda-lime-silica glass of floatation glass production line routine testing or required detection according to the method described above Gas volume percentage ratio:
For example:By the step of said method 3)- step 6)Obtain density 2.4984g/cm of detected glass specimen3
Measurement detects that the length, width and height of glass specimen are respectively 5.12mm × 5.14mm × 6.36mm, glass specimen entirety body Product is 1.6737 × 10-7m3
By above-mentioned steps 7)In the linear equation that draws calculate and detect bubble gas volume in sample;Y=228.50785- 91.31368 •2.4984g/cm3, Y=3.698 × 10-10m3, that is, the gas volume of bubble is 3.698 × 10 in detected sample-10m3
D. with gas volume in bubble divided by detected glass specimen overall volume, show that gas contains rate in vitreous body(Body Product percentage ratio).
In vitreous body gas containing rate==0.221%。
The gas with various content glass density of table 1 tests table

Claims (1)

1. a kind of method that densimetry determines gas content in vitreous body, methods described is applied to sodium silico-calcium white plate glass, Described method of testing comprises the steps:
1)Take one group of inside of the same batch of production line and make print to be measured containing bubble glass sample of remaining silent, one group of glass specimen is many In 10 pieces of samples;Print to be measured is cut into into 0.5mm3 ~0.7mm3Coupon, all surface requires polishing;Bubble should In retaining coupon after dicing;
2)Band bubble sample is measured using optical microscope, obtains the radius of sphericity of bubble in each piece of glass specimen, it is ellipse The shaft length of spheroid three;Using spheroid volume computing formula:With spheroid volume computing formulaGlass is calculated respectively The volume of bubble is gas content in bubble in glass body;Volume is calculated respectively if it there are two kinds of form bubbles simultaneously in vitreous body After sum up and obtain total gas volume;
3)First piece of sample in one group of sample is put in Density Measuring Instrument test tube, the standard specimen of sample and known density floats over liquid simultaneously Body surface face;Density Measuring Instrument heating is opened, illuminator is opened in stirring;The temperature of record examination liquid in pipe is started simultaneously at, is accurate to 0.01℃;
4)Heating rate is 0.4 DEG C/min in initial 2 DEG C of intensification, and heating rate is 0.1 DEG C/min after 2 DEG C of intensification;During intensification Shaking test tube need to not be stopped, it is to avoid sample and standard specimen are because surface tension of liquid factor " viscous " is in liquid surface;
5)Keep the heating rate of 0.1 DEG C/min persistently overheating, remember respectively when standard specimen and sample at the uniform velocity sink by graticule Record standard specimen and sample pass through temperature during graticule;
Other samples press step 3), step 4), step 5)Carry out, obtain each sample by temperature during graticule, and remember Record;
6)The computing formula for determining glass density using sink and float method calculates the density of each piece of sample;
ρXB+(TS-TB)×(-0.00175)
ρX=sample to be tested density, g/cm3
ρB=standard sample density, 2.5003g/cm3
TSTemperature when=sample sinks, DEG C;
TBTemperature when=standard specimen sinks, DEG C;
7)The gas volume of one group of glass specimen and the data of density are drawn by said method, relation curve has been drawn, has been obtained Go out linear relationship of the bubble gas volume with glass density and linear equation;
8)Determine the gas volume percentage ratio in the common soda-lime-silica glass of floatation glass production line routine testing or required detection:
A. by the step of said method 3)- step 6)Obtain the density of detected glass specimen;
B. measurement detects the overall volume of glass specimen;
C. by above-mentioned steps 7)In the linear equation that draws calculate and detect bubble gas volume in glass specimen;
D. gas volume percentage ratio in glass is drawn divided by detected glass specimen overall volume with gas volume in bubble.
CN201410843089.8A 2014-12-30 2014-12-30 Method for determining content of gas in vitreous body by using density process Active CN104614279B (en)

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CN110514554A (en) * 2019-10-12 2019-11-29 杭州之江新材料有限公司 A kind of method of quick inspection hot setting adhesive deaeration effect
CN112858097B (en) * 2019-11-26 2023-08-29 隆基绿能科技股份有限公司 Method, equipment and storage medium for detecting inclusion content of quartz sand

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CN103884645A (en) * 2012-12-24 2014-06-25 中国制浆造纸研究院 Method for testing gas content in paint

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Publication number Priority date Publication date Assignee Title
JP2000338040A (en) * 1999-05-25 2000-12-08 Nippon Telegr & Teleph Corp <Ntt> Method and apparatus for gas concentration analysis
CN103884645A (en) * 2012-12-24 2014-06-25 中国制浆造纸研究院 Method for testing gas content in paint

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Address after: 571924 Fuyin Road, Laocheng Economic Development Zone, Chengmai County, Hainan Province

Patentee after: Xinyi Glass (Hainan) Co.,Ltd.

Address before: South 1st ring road, Laocheng Economic Development Zone, Chengmai County, Hainan Province

Patentee before: HAINAN AVIC SPECIAL GLASS MATERIALS Co.,Ltd.