CN113189126A - Method for detecting and analyzing tiny solid defects of float glass - Google Patents
Method for detecting and analyzing tiny solid defects of float glass Download PDFInfo
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- CN113189126A CN113189126A CN202110481422.5A CN202110481422A CN113189126A CN 113189126 A CN113189126 A CN 113189126A CN 202110481422 A CN202110481422 A CN 202110481422A CN 113189126 A CN113189126 A CN 113189126A
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- 230000007547 defect Effects 0.000 title claims abstract description 103
- 239000007787 solid Substances 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims abstract description 52
- 239000005329 float glass Substances 0.000 title claims abstract description 24
- 238000001514 detection method Methods 0.000 claims abstract description 73
- 238000001228 spectrum Methods 0.000 claims abstract description 25
- 238000010183 spectrum analysis Methods 0.000 claims abstract description 25
- 239000011521 glass Substances 0.000 claims abstract description 20
- 239000003153 chemical reaction reagent Substances 0.000 claims description 45
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 239000011707 mineral Substances 0.000 claims description 9
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 7
- 239000004327 boric acid Substances 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 abstract description 3
- 238000004451 qualitative analysis Methods 0.000 abstract description 3
- 238000004445 quantitative analysis Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 52
- 238000004458 analytical method Methods 0.000 description 10
- 238000004876 x-ray fluorescence Methods 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009614 chemical analysis method Methods 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 150000004760 silicates Chemical class 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005211 surface analysis Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
-
- 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
- G01N21/84—Systems specially adapted for particular applications
- G01N21/88—Investigating the presence of flaws or contamination
- G01N21/95—Investigating the presence of flaws or contamination characterised by the material or shape of the object to be examined
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
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- Life Sciences & Earth Sciences (AREA)
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Abstract
The application provides a method for detecting and analyzing tiny solid defects of float glass, which comprises the following steps: obtaining glass with solid defects, and peeling the solid defects from the glass; digesting the solid defects into a solution; dripping the solution onto first filter paper to form a detection sample; and carrying out spectral analysis on the detection sample to obtain a detection spectrum. In the method, the detection cost is low, and qualitative and quantitative analysis can be performed on the elements of the defects; meanwhile, the interference of the glass body on the defect measurement is effectively reduced, and the problem of inconvenience in defect detection in the glass is solved.
Description
Technical Field
The disclosure relates to the technical field of float glass defect detection, in particular to a method for detecting and analyzing tiny solid defects of float glass.
Background
In the production process of float glass, tiny solid defects are attached to the float glass due to various factors, so that the quality of a float glass product is influenced; the defects are generally formed by solid foreign matters in the external environment adhering to the glass. In the prior art, defects on the float glass are mainly detected and analyzed through electron probe analysis, polarization microscope analysis, chemical analysis method or spectrometer analysis so as to track the sources of the defects and reduce the generation of glass defects so as to improve the quality of float glass products.
However, for the electronic probe analysis, the investment cost is high, the instrument operation and maintenance cost is high, and the requirement on the operation environment (air cleanliness, environmental vibration and the like) is high; for the analysis of a polarizing microscope, the composition elements and the element content of the solid defects cannot be accurately judged; for chemical analysis methods, the method is generally only suitable for analysis scenes with large volume and large sample amount;
therefore, a method for detecting and analyzing tiny solid defects of float glass, which has relatively low detection cost and can detect the constituent elements and the element content of the solid defects, is needed.
Disclosure of Invention
In view of the above-mentioned drawbacks and deficiencies of the prior art, it would be desirable to provide a method for detecting and analyzing tiny solid defects in float glass to solve the above-mentioned problems.
The application provides a method for detecting and analyzing tiny solid defects of float glass, which comprises the following steps:
obtaining glass with solid defects, and peeling the solid defects from the glass;
digesting the solid defects into a solution;
dripping the solution onto first filter paper to form a detection sample;
and carrying out spectral analysis on the detection sample to obtain a detection spectrum.
According to the technical scheme provided by the embodiment of the application, the method for digesting the solid defects into the solution comprises the following steps:
determining the kind of the solid defects;
and selecting a chemical reagent according to the variety of the solid defects to treat the solid defects to form the solution.
According to the technical scheme provided by the embodiment of the application, the method further comprises the following steps after the detection sample is subjected to spectral analysis:
dripping the chemical reagent onto second filter paper to form a reagent sample;
carrying out spectral analysis on the reagent sample to obtain a reagent spectrum;
and determining the element types or element contents of the defects through the reagent spectrum and the detection spectrum.
According to the technical scheme provided by the embodiment of the application, the method for determining the types of the solid defects comprises the following steps: by visual observation or by microscopic observation.
According to the technical scheme provided by the embodiment of the application, the specific method for treating the solid defects by selecting the chemical reagent according to the types of the solid defects comprises the following steps:
and when the type of the solid defects is judged to be silicate or mineral: obtaining sodium carbonate and boric acid, mixing the sodium carbonate and the boric acid with the solid defects, sintering and cooling, adding dilute hydrochloric acid and water, and heating and dissolving to form the solution;
and when the type of the solid defects is judged to be metal: and (2) acquiring perchloric acid and hydrofluoric acid, mixing the perchloric acid, the hydrofluoric acid and the solid defects, heating, evaporating to dryness, cooling, adding dilute hydrochloric acid and water, and heating to dissolve to form the solution.
According to the technical scheme provided by the embodiment of the application, the method for carrying out spectrum analysis on the detection sample comprises the following steps: and carrying out spectral analysis on the detection sample by using a spectrometer.
According to the technical scheme provided by the embodiment of the application, the method for performing spectral analysis on the detection sample by using the spectrometer specifically comprises the following steps:
and when the type of the solid defects is judged to be silicate or mineral: acquiring a detection spectrum of the detection sample through semi-quantitative scanning on the spectrograph;
and when the type of the solid defects is judged to be metal: and acquiring a detection spectrum of the detection sample through 2 theta angle scanning on the spectrometer.
According to the technical scheme provided by the embodiment of the application, the specific method for forming the reagent sample comprises the following steps: dripping the chemical reagent into the middle position of the second filter paper and drying to form sample spots; and repeatedly dripping and drying until the chemical reagent is used up.
According to the technical scheme provided by the embodiment of the application, the specific method for forming the detection sample comprises the following steps: dripping the solution into the middle position of the first filter paper and drying to form sample spots; the dropwise addition and drying were repeated until the solution was used up.
According to the technical scheme provided by the embodiment of the application, the sampling diameter of the first filter paper is 29 mm.
The beneficial effect of this application lies in: based on the technical scheme provided by the application, the solid defects are prepared into the solution through the steps, and the solution is dripped onto the first filter paper to form the detection sample, so that the elements to be detected can be uniformly distributed on the first filter paper, the detection sample is converted into a flat thin layer sample from a three-dimensional irregular shape, the conventional analysis requirements of a detection instrument are met, and the detection spectrum is obtained through performing spectral analysis on the detection sample, so that the types and the content of the elements contained in the defects can be obtained;
in the method, the detection cost is low, and qualitative and quantitative analysis can be performed on the elements of the defects; meanwhile, the interference of the glass body on the defect measurement is effectively reduced, and the problem of inconvenience in defect detection in the glass is solved.
Drawings
Other features, objects and advantages of the present application will become more apparent upon reading of the following detailed description of non-limiting embodiments thereof, made with reference to the accompanying drawings in which:
FIG. 1 is a flow chart of a method for detecting and analyzing tiny solid defects of float glass provided by the present application.
FIG. 2 is a flowchart of the overall method for setting the step of eliminating the chemical interference after step S400 shown in FIG. 1.
Detailed Description
The present application will be described in further detail with reference to the following drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and not restrictive of the invention. It should be noted that, for convenience of description, only the portions related to the present invention are shown in the drawings.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.
Please refer to fig. 1, which is a method for detecting and analyzing micro solid defects of a float glass provided by the present application, comprising the following steps:
s100: obtaining glass with solid defects, and peeling the solid defects from the glass;
specifically, the solid defects are physically removed from the glass;
s200: digesting the solid defects into a solution;
s300: dripping the solution onto first filter paper to form a detection sample;
specifically, the specific method for forming the detection sample comprises the following steps: dripping the solution into the middle position of the first filter paper and drying to form sample spots; the dropwise addition and drying were repeated until the solution was used up. Preferably, the first filter paper is a circular filter paper with a diameter of 4cm, and the sampling area (i.e. spot area) of the first filter paper is a circular area with a diameter of 29 mm.
S400: and carrying out spectral analysis on the detection sample to obtain a detection spectrum.
Specifically, the detection spectrum can be obtained by performing spectral analysis on the detection sample through an X-ray fluorescence spectrometer. After the detection spectrum is obtained, qualitative and quantitative analysis can be carried out on the element types of the defects, and the element types and the element content can be obtained.
Specifically, the solution is dropped into the first filter paper and then dried to form the detection sample.
The working principle is as follows: through the steps, the solid defects are prepared into the solution, the solution is dripped onto the first filter paper to form the detection sample, so that the elements to be detected can be uniformly distributed on the first filter paper, the detection sample is converted from a three-dimensional irregular shape into a flat thin layer sample, the conventional analysis requirements of a detection instrument are met, and the types and the content of the elements contained in the defects can be obtained by performing spectral analysis on the detection sample to obtain the detection spectrum.
By the method, the defects are separated from the glass and independently sampled, so that the interference of the glass body on the defect measurement is effectively reduced, the fluorescence yield of elements is improved, and the problem of inconvenience in defect detection in the glass is solved; meanwhile, the method is also beneficial to reducing the detection cost, so that the X-ray fluorescence spectrometer without the micro-area detection function or the Map function can also carry out defect detection and analysis.
In a preferred embodiment of step S200, as shown in fig. 2, the method for resolving the solid defects into the solution specifically includes:
s201: determining the kind of the solid defects;
specifically, the method for determining the type of the solid defect comprises the following steps: by visual observation or by microscopic observation; the categories of the solid defects include: silicates, minerals, and metals; wherein, the boundaries of the metal solid defects and the glass are clearer, and the boundaries of the silicate or mineral solid and the glass are more fuzzy; when the solid defects are relatively large or the types of the solid defects are easy to judge, the detection judgment can be carried out through naked eyes, and when the solid defects are relatively small or the types of the solid defects are difficult to judge, the auxiliary detection judgment can be carried out through a microscope.
S202: and selecting a chemical reagent according to the variety of the solid defects to treat the solid defects to form the solution.
Specifically, the specific method for treating the solid defects by selecting the chemical reagent according to the types of the solid defects comprises the following steps:
and when the type of the solid defects is judged to be silicate or mineral: obtaining sodium carbonate and boric acid, mixing the sodium carbonate and the boric acid with the solid defects, sintering and cooling, adding dilute hydrochloric acid and water, and heating and dissolving to form the solution; specifically, the sintering temperature of the sodium carbonate and the boric acid may be set to 1000 ℃.
And when the type of the solid defects is judged to be metal: and (2) acquiring perchloric acid and hydrofluoric acid, mixing the perchloric acid, the hydrofluoric acid and the solid defects, heating, evaporating to dryness, cooling, adding dilute hydrochloric acid and water, and heating to dissolve to form the solution.
By the method, the digestion method can be flexibly selected according to the variety of the solid defects, and the targeted pretreatment is realized.
In a preferred embodiment, as shown in fig. 2, after performing the spectral analysis (i.e., step S400) on the test sample, the method further includes a chemical reagent interference elimination step, where the chemical reagent interference elimination step includes:
s500: dripping the chemical reagent onto second filter paper to form a reagent sample;
specifically, in order to ensure consistency, the second filter paper and the first filter paper are equal in size and material; the chemical reagent in the reagent sample and the chemical reagent in the detection sample are the same in type and use amount.
Specifically, the specific method for forming the reagent sample comprises the following steps: dripping the chemical reagent into the middle position of the second filter paper and drying to form sample spots; and repeatedly dripping and drying until the chemical reagent is used up.
S501: carrying out spectral analysis on the reagent sample to obtain a reagent spectrum;
s502: and determining the element types or element contents of the defects through the reagent spectrum and the detection spectrum.
Through the steps, by setting a sample blank, namely, dropping a chemical reagent on the second filter paper to form a reagent sample, carrying out spectral analysis on the reagent sample and obtaining a reagent spectrum; therefore, the element types and contents in the chemical reagent can be obtained. The element types and element contents in the defects can be accurately obtained by performing difference operation processing on the element contents in the detection sample and the element contents in the chemical reagent, so that the influence of the chemical reagent on the detection result is eliminated, and the detection result is more accurate.
In a preferred embodiment, the method for performing the spectral analysis on the detection sample comprises: and carrying out spectral analysis on the detection sample by using a spectrometer. In particular, the spectrometer can be an X-ray fluorescence spectrometer. The X-ray fluorescence spectrum analysis is a surface-near surface analysis technology, namely, the thickness of a sample close to the micron level of the surface represents the whole sample, and the information of each element in the sample can be truly reflected.
In a preferred embodiment, the method for performing spectrum analysis on the detection sample by using the spectrometer specifically includes:
and when the type of the solid defects is judged to be silicate or mineral: acquiring a detection spectrum of the detection sample through semi-quantitative scanning on the spectrograph;
and when the type of the solid defects is judged to be metal: and acquiring a detection spectrum of the detection sample through 2 theta angle scanning on the spectrometer.
Specifically, the semi-quantitative scanning detection range is wide, and the method is suitable for detecting samples with more element types, such as silicates or minerals; the 2 theta angle scanning has strong pertinence and is suitable for detecting samples with few types of elements, such as metals. For example, when the content of the detected heavy metal elements such as chromium and nickel or the element is trace ppm, the 2 theta scanning can be used for carrying out targeted element analysis, and the detection process is convenient and quick.
Specifically, when the reagent sample is subjected to spectral analysis, a reagent spectrum of the reagent sample can be obtained by semi-quantitative scanning.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Claims (9)
1. A method for detecting and analyzing tiny solid defects of float glass is characterized by comprising the following steps: the method comprises the following steps:
obtaining glass with solid defects, and peeling the solid defects from the glass;
digesting the solid defects into a solution;
dripping the solution onto first filter paper to form a detection sample;
and carrying out spectral analysis on the detection sample to obtain a detection spectrum.
2. The method for detecting and analyzing micro solid defects of a float glass according to claim 1, wherein: the method for digesting the solid defects into the solution comprises the following steps:
determining the kind of the solid defects;
and selecting a chemical reagent according to the variety of the solid defects to treat the solid defects to form the solution.
3. The method for detecting and analyzing micro solid defects of a float glass according to claim 2, wherein: the method also comprises the following steps after the detection sample is subjected to spectral analysis:
dripping the chemical reagent onto second filter paper to form a reagent sample;
carrying out spectral analysis on the reagent sample to obtain a reagent spectrum;
and determining the element types or element contents of the defects through the reagent spectrum and the detection spectrum.
4. The method for detecting and analyzing micro solid defects of a float glass according to claim 2, wherein: the specific method for treating the solid defects by selecting the chemical reagent according to the types of the solid defects comprises the following steps:
and when the type of the solid defects is judged to be silicate or mineral: obtaining sodium carbonate and boric acid, mixing the sodium carbonate and the boric acid with the solid defects, sintering and cooling, adding dilute hydrochloric acid and water, and heating and dissolving to form the solution;
and when the type of the solid defects is judged to be metal: and (2) acquiring perchloric acid and hydrofluoric acid, mixing the perchloric acid, the hydrofluoric acid and the solid defects, heating, evaporating to dryness, cooling, adding dilute hydrochloric acid and water, and heating to dissolve to form the solution.
5. The method for detecting and analyzing micro solid defects of a float glass according to claim 2, wherein: the method for carrying out spectrum analysis on the detection sample comprises the following steps: and carrying out spectral analysis on the detection sample by using a spectrometer.
6. The method for detecting and analyzing micro solid defects of a float glass according to claim 5, wherein: the method for performing spectral analysis on the detection sample by using the spectrometer specifically comprises the following steps:
and when the type of the solid defects is judged to be silicate or mineral: acquiring a detection spectrum of the detection sample through semi-quantitative scanning on the spectrograph;
and when the type of the solid defects is judged to be metal: and acquiring a detection spectrum of the detection sample through 2 theta angle scanning on the spectrometer.
7. The method for detecting and analyzing micro solid defects of a float glass according to claim 3, wherein: the specific method for forming the reagent sample comprises the following steps: dripping the chemical reagent into the middle position of the second filter paper and drying to form sample spots; and repeatedly dripping and drying until the chemical reagent is used up.
8. The method for detecting and analyzing micro solid defects of a float glass according to any one of claims 1 to 7, wherein: the specific method for forming the detection sample comprises the following steps: dripping the solution into the middle position of the first filter paper and drying to form sample spots; the dropwise addition and drying were repeated until the solution was used up.
9. The method for detecting and analyzing micro solid defects of a float glass according to claim 8, wherein: the first filter paper had a sample diameter of 29 mm.
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