CN109738429A - The rapid detection method of alkali is analysed in a kind of glaze spraying vial - Google Patents
The rapid detection method of alkali is analysed in a kind of glaze spraying vial Download PDFInfo
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- CN109738429A CN109738429A CN201910036541.2A CN201910036541A CN109738429A CN 109738429 A CN109738429 A CN 109738429A CN 201910036541 A CN201910036541 A CN 201910036541A CN 109738429 A CN109738429 A CN 109738429A
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Abstract
The invention belongs to technical field of food safety detection, the rapid detection method of alkali is analysed in specially a kind of glaze spraying vial.Method includes the following steps: a. analysis alkali/crystallization solution preparation.Glaze spraying vial is taken, the distilled water of bottle volume 8-10% is then injected into bottle, then shaking glass bottle makes distilled water sufficiently infiltrate glass bottle inner wall 10-20s；B. alkali or the measurement of crystallization liquid pH value are analysed.Alkali/crystallization solution pH value is analysed using pH meter or phenolphthalein determination of color；C. the judgement of rate of decay.When analysis alkali/crystallization solution: pH value≤7.20 are determined as qualification；PH value 7.21~9.95 is judged to slightly analysing alkali；PH value 9.96~10.30 is determined as slight crystallization；PH value >=10.31 are determined as serious devitrification.This method has the advantages that easy to operate, high sensitivity, detection speed is fast, testing cost is low etc..
Description
Technical field
The invention belongs to technical field of food safety detection, the quick detection side of alkali is analysed in specially a kind of glaze spraying vial
Method.
Background technique
Vial is the main packing container of food, medicine, chemical industry.They have chemical stability good；It is easy to close
Envelope, air-tightness is good, transparent, can observe the case where containing object from the outside；Shelf characteric is good, any surface finish, goes out convenient for disinfection
Bacterium；It is handsome in appearance, it decorates rich and varied；There is certain mechanical strength, the external force being able to bear in the pressure in the bottle and transportational process
Effect；Feed distribution is wide, lower-price characteristic.
Glaze spraying is one of advanced ceramics glazing skill and technique, i.e., so that glaze slip atomization is sprayed onto billet surface with spray gun or sprayer.It cares for
Name Si Yi, glaze spraying vial are to carry out glaze spraying in traditional glass bottle surface, allow it both to keep vial cheap, chemistry is steady
Qualitative good feature, and there is texture and art atmosphere possessed by ceramics.Therefore, at present glaze spraying vial in the industry, especially
It is in field of food industry using more and more extensive.
Although glaze spraying vial appearance belongs to vial similar to ceramic bottle, essence.The originals such as the manufacture craft due to vial
Cause, glaze spraying vial during storage, can be by weathering by the effect of atmosphere.After glass weathering, destabilization, which studies, to be analyzed
(being known as analysis alkali or crystallization) forms misty, dotted, crystalloid transparent, translucent or opaque spot, spot in glass bottle inner wall
The phenomenon that block.When weathering is serious, glass surface forms bloom, or even generates glass bonding die phenomenon.For at present, rate of decay
Measuring method mainly has:
1. observing by the naked eye glass surface pattern and being classified, or the transparency point of glass surface is measured by turbidity
Grade, the not serious Shi Keyong ellipsometer of weathering measure the film thickness and refractive index on weathered glass surface.Though this serial determination method
It is so quick, but poor accuracy, and it is meaningless for glaze spraying vial, because glaze spraying glass, which has lost vial, to be had
Transparent characteristic；
2. the silicate glass containing alkali measures the glass surface generated alkali after weathering with atomic absorption spectrophotometer, this
Although method accuracy is high, detection process is complicated, and detection time is longer, and equipment requirement is high.
Therefore, it is badly in need of a kind of rapid detection method of the analysis alkali in the glaze spraying glass for being able to solve existing issue.
Summary of the invention
The purpose of the present invention is overcome the testing cost of existing glaze spraying vial analysis alkali detection technique is high, detection time is long,
The low defect of accuracy in detection, provides the rapid detection method that alkali is analysed in a kind of glaze spraying vial, this method have it is easy to operate,
High sensitivity detects the advantages such as speed is fast, testing cost is low.
To achieve the goals above, the specific technical proposal of the invention is:
The rapid detection method of alkali is analysed in a kind of glaze spraying vial, specifically includes the following steps:
A. alkali/crystallization solution preparation is analysed.Glaze spraying vial is taken, the distillation of bottle volume 8-10% is then injected into bottle
Water, then shaking glass bottle makes distilled water sufficiently infiltrate glass bottle inner wall 10-20s；
B. alkali or the measurement of crystallization liquid pH value are analysed.Alkali/crystallization solution is analysed using pH meter or phenolphthalein determination of color
PH value；
C. the judgement of rate of decay.When analysis alkali/crystallization liquid pH value is lower than
Solution pH value≤7.20, are determined as chromatography-less alkali；
Solution pH value 7.21~9.95 is judged to slightly analysing alkali；
Solution pH value 9.96~10.30 is determined as slight crystallization；
Solution pH value >=10.31, are determined as serious devitrification.
The positive effect of the present invention is embodied in:
(1) compared to other detection methods, this method is easy to operate, and detection speed is fast.
(2) high sensitivity, detect it is more accurate, convenient for food etc. production it is filling before detection, reduce testing cost and
Operation difficulty.
(3) alkali degree is analysed inside range estimation vial under 2400 power microscopes with by will pass through after the broken bottle of glaze spraying vial
Visual method result fit like a glove.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, right With reference to embodiment
The present invention is described in further detail, but the range that this should not be interpreted as to the above-mentioned theme of the present invention is only limitted to following implementations
Example.Without departing from the idea case in the present invention described above, it according to ordinary skill knowledge and customary means, makes various
Replacement and change, should all be included within the scope of the invention.
The detection method that alkali is analysed in traditional glaze spraying vial, generallys use atomic spectrophotometer measuring method, the measurement
Method is as follows:
1) one, glass bottle sample, is taken, cylindrical surface is cut into having a size of 25mm × 25mm size with cutting machine；
2) it, after dry under infrared lamp, is placed in 500m1 beaker, is impregnated half an hour with 30m1 deionized water, and stir and turn over
Turn glass several times, to keep each part of glass slice that can contact with deionized water, the alkali of precipitation is all dissolved in water.
3), take out glass slice, leachate in beaker moved into 100m1 volumetric flask, then with deionized water by sample and
Beaker flushes three times respectively, and flows into whole flushing liquors in volumetric flask, and 5m1 is added and rushes slow agent, is diluted to scale.Buffer is
The CsCl solution of 3m1 2000ppm is added in the leachate of every 50ml for CsCl solution.It is different according to the kind that alkali is precipitated, it uses
Different reference solutions, Na2O NaC1 (spectroscopic pure), K2O matches the stoste of 1000ppm with KC1 (spectroscopic pure), then is diluted to
The standard solution of 50ppm.
4) according to the difference that numerical quantity is precipitated when, measuring, it is configured to the reference solution of 0.2,04,0.6,0,8ppm respectively,
Make standard curve.
5) R in leachate, is measured with atomic absorption spectrophotometer2After O concentration, the analysis alkali of unit area can be conversed
It measures (S):
S=CV/A
S-per surface generated alkali (R2Oμg/cm2)
C-Steep cencentration (ppm)
V-leachate volume (ml)
Full surface area (the cm of A-weathered glass2)。
Generated alkali corresponds to the criterion of rate of decay are as follows:
Generated alkali range (μ g/cm2):
Generated alkali≤0.40, chromatography-less alkali
Generated alkali 0.41~0.60, slightly analyses alkali
Generated alkali 0.61~0.95, slight crystallization
Generated alkali >=0.96, serious devitrification.
Embodiment 1:
The quick detection of alkali is analysed in glaze spraying vial, the specific steps are as follows:
A. alkali/crystallization solution preparation is analysed.Same producer is extracted, with glaze spraying vial 20 of batch, appoints and takes 10 points
Injection accounts for the distilled water of bottle volume 8% not into bottle, then shakes glass bottle 20s, distilled water is made sufficiently to infiltrate glass bottle inner wall；So
Distilled water is poured out afterwards, obtains analysis alkali/crystallization liquid；
B. alkali/crystallization liquid pH value measurement is analysed.It is measured in this 10 using pH meter and is poured out in each glaze spraying vial
Analysis alkali/crystallization solution, measuring their pH value is respectively 6.0；
C. the judgement of rate of decay.According to solution ph≤7.20, the glaze spraying vial chromatography-less alkali of this 10 extractions is determined.
Other 10 glaze spraying vials of extraction are detected with atomic spectrophotometer measuring method, most afterwards through counting
It calculates, generated alkali is 0.28 μ g/cm2, the judgement result of the result and this method fits like a glove.
Embodiment 2:
The quick detection of alkali is analysed in glaze spraying vial, the specific steps are as follows:
A. alkali/crystallization solution preparation is analysed.Same producer is extracted, with glaze spraying vial 25 of batch, appoints and takes 10 points
Injection accounts for the distilled water of bottle volume 8% not into bottle, then shakes glass bottle 20s, distilled water is made sufficiently to infiltrate glass bottle inner wall；So
Distilled water is poured out afterwards, obtains analysis alkali/crystallization liquid；
B. alkali/crystallization liquid pH value measurement is analysed.Each glaze spraying vial in this 10 is extracted using pH meter measurement to fall
Analysis alkali/crystallization solution out, and the pH value for measuring them is 9.0；
C. the judgement of rate of decay.According to solution ph in 7.21~9.95 ranges, the glaze spraying of this 10 extractions is determined
Vial is slight analysis alkali.
5 glaze spraying vials in remaining 15 glaze spraying vials are examined with atomic spectrophotometer measuring method
It surveys, is finally computed, generated alkali is 0.52 μ g/cm2, for slight analysis alkali, the judgement result of the result and this method is kissed completely
It closes.
Comparative example 1:
Do not detect also 10 glaze spraying vials are carried out analysing alkali in glaze spraying vial using the method for embodiment 2
Quickly detection, specific steps are identical, only change the loadings of distilled water, and the volume for making distilled water account for bottle is adjusted to 5%,
Measuring their alkali/crystallization solution pH value is respectively 7.16, and criterion according to the present invention is determined as chromatography-less alkali；But according to
The generated alkali of atomic spectrophotometer method measurement is judged to slightly analysing alkali, and two results are deviated.
Embodiment 3:
The quick detection of alkali is analysed in glaze spraying vial, the specific steps are as follows:
A. alkali/crystallization solution preparation is analysed.Appoint and take same production man, with glaze spraying vial 30 of batch, appoints and take 10 points
Injection accounts for the distilled water of bottle volume 8% not into bottle, then shakes glass bottle 20s, distilled water is made sufficiently to infiltrate glass bottle inner wall；So
Distilled water is poured out afterwards, obtains analysis alkali/crystallization liquid；
B. alkali/crystallization liquid pH value measurement is analysed.Each glaze spraying vial in this 10 is extracted using pH meter measurement to fall
Analysis alkali/crystallization solution out, and the pH value for measuring them is 10.10；
C. the judgement of rate of decay.It is to determine this 10 glaze spraying vials in 9.96~10.30 ranges according to solution ph
It is slight crystallization.
5 glaze spraying vials in remaining 20 glaze spraying vials are examined with atomic spectrophotometer measuring method
It surveys, is finally computed, generated alkali is 0.83 μ g/cm2, for slight crystallization, the judgement result of the result and this method is kissed completely
It closes.
Comparative example 2:
To not carry out also appointing in the 15 glaze spraying vials detected takes 5 glaze spraying vials using in embodiment 3
Method carries out the quick detection that alkali is analysed in glaze spraying vial, and specific steps are identical, only change the loadings of distilled water, make to steam
Distilled water accounts for bottle volume 16%, and measuring their alkali/crystallization solution pH value is 9.82, and criterion is slight according to the present invention
Alkali is analysed, result and atomic spectrophotometer measuring method, which determine the result come, deviation.
Comparative example 3:
Arbitrary extracting 5 in do not detect also 10 glaze spraying vials is sprayed only with the method in embodiment 3
The quick detection of alkali is analysed in glaze vial, specific steps are identical, only the time of change infiltration glass bottle inner wall, time 10s,
Measuring their alkali/crystallization solution pH value is respectively 9.89, is as a result had partially according to our criterion for slight analysis alkali
Difference.
Comparative example 4:
It will not carry out the other 5 glaze spraying vials detected also and glaze spraying vial carried out using the method in embodiment 3
The quick detection of middle analysis alkali, specific steps are identical, only change the time of infiltration glass bottle inner wall, and time 30s measures them
Alkali/crystallization solution pH value is respectively 10.69, and criterion is serious devitrification according to the present invention, is as a result deviated.
Embodiment 4:
The quick detection of alkali is analysed in glaze spraying vial, the specific steps are as follows:
A. alkali/crystallization solution preparation is analysed.Same production man is extracted, with glaze spraying vial 20 of batch, appoints and takes 10 points
The distilled water of bottle volume 8% Zhu Ru not be accounted for, glass bottle 20s is then shaken, distilled water is made sufficiently to infiltrate glass bottle inner wall；Then it will steam
Distilled water is poured out, and analysis alkali/crystallization liquid is obtained；
B. alkali/crystallization liquid pH value measurement is analysed.Each glaze spraying vial in this 10 is extracted using pH meter measurement to fall
Analysis alkali/crystallization solution out, and the pH value equal 10.42 for measuring them.
C. the judgement of rate of decay.According to solution ph >=10.31, determine that this 10 glaze spraying vials extracted are tight
Weight crystallization.
Remaining 10 glaze spraying vials are detected with atomic spectrophotometer measuring method, are finally computed,
Generated alkali is 1.03 μ g/cm2, for serious devitrification, the judgement result of the result and this method fits like a glove.
Test one: the judgement test of alkali/crystallization detection method accuracy rate is analysed in glaze spraying vial:
Analysis alkali/crystallization inspection in the glaze spraying vial in the application is respectively adopted in 90 glass samples of arbitrary extracting
Survey method and ocular estimate (after the broken bottle of glaze spraying vial, pass through to estimate under 2400 power microscopes and analyse alkali degree inside vial) into
Row comparative analysis, specific sample lot number and result see the table below:
1 the method for the present invention of table and ocular estimate testing result contrast table
As seen from the above table, it is high that alkali/crystallization detection method accuracy rate is analysed in glaze spraying vial, it is feasible, and by by glaze spraying
It is fitted like a glove after the broken bottle of vial by estimating the visual method result of analysis alkali degree inside vial under 2400 power microscopes.
Example described above is only the preferred embodiment of this patent, but the protection scope of this patent is not limited thereto.
It should be pointed out that for those skilled in the art, under the premise of not departing from this patent principle, specially according to this
The technical solution and its inventional idea of benefit, can also make several improvements and modifications, these improvements and modifications also should be regarded as this specially
Within the protection scope of benefit.
Claims (3)
1. analysing the rapid detection method of alkali in a kind of glaze spraying vial, it is characterised in that the following steps are included:
A. it analyses alkali/crystallization solution preparation: taking glaze spraying vial, the distilled water of a constant volume is then injected into bottle, shake glass bottle
Distilled water is set sufficiently to infiltrate glass bottle inner wall；
B. alkali or the measurement of crystallization liquid pH value are analysed: alkali/crystallization solution pH value is analysed using pH meter or phenolphthalein determination of color；
C. the judgement of rate of decay: when analysis alkali/crystallization liquid pH value is lower than
Solution ph≤7.20 are determined as qualification；
Solution ph 7.21~9.95 is judged to slightly analysing alkali；
Solution ph 9.96~10.30 is determined as slight crystallization；
Solution ph >=10.31 are determined as serious devitrification.
2. analysing the rapid detection method of alkali in glaze spraying vial as described in claim 1, it is characterised in that: the additional amount of distilled water
For the 8-10% of bottle volume.
3. analysing the rapid detection method of alkali in glaze spraying vial as described in claim 1, it is characterised in that: the time of concussion glass bottle
For 10-20s.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1312866A (en) * | 1998-08-13 | 2001-09-12 | 汉高两合股份公司 | Automatic regulation and control of cleansing baths |
| CN205099577U (en) * | 2015-11-06 | 2016-03-23 | 安徽古井贡酒股份有限公司 | Glaze spraying equipment is trailed in step to glass bottle |
| CN106323857A (en) * | 2016-09-27 | 2017-01-11 | 南京玻璃纤维研究设计院有限公司 | Measuring device and measuring method of glass fiber water resistance |
| CN207646081U (en) * | 2017-11-01 | 2018-07-24 | 泸县浙川玻璃有限公司 | A kind of vial glaze spraying system |
-
2019
- 2019-01-15 CN CN201910036541.2A patent/CN109738429A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1312866A (en) * | 1998-08-13 | 2001-09-12 | 汉高两合股份公司 | Automatic regulation and control of cleansing baths |
| CN205099577U (en) * | 2015-11-06 | 2016-03-23 | 安徽古井贡酒股份有限公司 | Glaze spraying equipment is trailed in step to glass bottle |
| CN106323857A (en) * | 2016-09-27 | 2017-01-11 | 南京玻璃纤维研究设计院有限公司 | Measuring device and measuring method of glass fiber water resistance |
| CN207646081U (en) * | 2017-11-01 | 2018-07-24 | 泸县浙川玻璃有限公司 | A kind of vial glaze spraying system |
Non-Patent Citations (5)
| Title |
|---|
| 中国食品药品检定研究院 编写: "《国家药包材标准》", 31 December 2015, 中国医药科技出版社 * |
| 宋玉华 等: "搪玻璃瓷面色泽异常的探讨", 《中国搪瓷》 * |
| 王承遇 等: "硅酸盐玻璃的风化", 《硅酸盐学报》 * |
| 蒋荃 等: "影响玻璃防霉粉防霉效果的几个因素的研究", 《中国建材科技》 * |
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