CN108956569A - A kind of new method measuring paper surface pH - Google Patents
A kind of new method measuring paper surface pH Download PDFInfo
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- CN108956569A CN108956569A CN201810838425.8A CN201810838425A CN108956569A CN 108956569 A CN108956569 A CN 108956569A CN 201810838425 A CN201810838425 A CN 201810838425A CN 108956569 A CN108956569 A CN 108956569A
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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
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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Abstract
The invention belongs to technical field of nondestructive testing, disclose it is a kind of measure paper surface pH new method, include the following steps: S1, fluorescent marker chitosan preparation: the foundation of the relationship of S2, fluorescence intensity and paper surface pH value: the wherein linear relation of fluorescence intensity and paper surface pH are as follows: Y=3.075 × 106X‑9.413×106, wherein Y is fluorescence intensity, and X is the pH value of paper surface；The measurement of S3, paper surface pH value.Compared with prior art, the beneficial effect of the application is can fast, accurately to measure the pH value of paper surface on the basis of ensuring that paper is not impaired.
Description
Technical field
The invention belongs to technical field of nondestructive testing, in particular to a kind of new method for measuring paper surface pH.
Background technique
The pH value of paper surface, that is, paper surface hydrogen ion concentration height, learns pH value of paper and paper from actual use
It is related to open durability.Mainly the cellulose of paper surface is acted on by acidity and is degraded so that causing paper strength reduction, matter crisp
With color brightness reversion, that is, so-called aging phenomenon.Acid bigger, cellulose degradation speed is faster, and aging phenomenon is also more serious, thus
Shorten the service life of document.In addition pH value of paper also has an impact to paper printing, because of pH and ink absorption and ink dries
Dry process time is related, therefore measures paper surface pH value to the durability of research printing adaptability and paper with certain meaning
Justice.
The more common method of measurement paper surface has hot water or cold water extraction process, electrical measuring method, color ratio method and titration at present,
These methods all inevitably cause the damage that can not be repaired to paper when being measured paper surface pH value, and
The disadvantages of it is long that there are also elapsed times, and accuracy is not high.These methods are not applicable in terms of detecting books, folder, archaeology,
Being badly in need of one kind now has rapidly, accurately and not damages the detection method of the paper surface pH value of paper.
Summary of the invention
It is an object of the present invention to provide a kind of survey for the above problem existing for existing paper surface pH context of detection
Determine the new method of paper surface pH.
To achieve the goals above, the technical solution that the application uses are as follows: a kind of new method for measuring paper surface pH, packet
Include following steps:
S1, fluorescent marker chitosan preparation:
Firstly, Fluoresceincarboxylic acid, EDC and NHS are dissolved into acid citric acid-sodium citrate buffer, keep away
Light reacts 23h~25h, the Fluoresceincarboxylic acid solution activated under room temperature；The wherein substance of Fluoresceincarboxylic acid, EDC and NHS
The ratio between amount be Fluoresceincarboxylic acid: EDC:NHS=1:10:10；
Then, by the ratio of 0.025g/mL chitosan solution and the Fluoresceincarboxylic acid solution of above-mentioned activation 5:1 by volume
It is added in neutral phosphate buffer solution, is protected from light, 1h~3h is reacted under room temperature, obtains mixed solution；
Finally, high speed centrifugation, be washed with deionized obtained until cleaning solution unstressed configuration fluorescent marker chitosan it is molten
Liquid, for use；
The foundation of the relationship of S2, fluorescence intensity and paper surface pH value:
Firstly, adjusting the pH of the chitosan solution of fluorescent marker obtained in S1 to 4~6；
Then, the chitosan solution of fluorescent marker is added dropwise on the paper of known paper surface pH value, is formed after gel
Chitosan film, it is to be detected；
Finally, detecting the chitosan film on the paper of known paper surface pH value, fluorescence intensity is recorded, according to known paper
The fluorescence intensity that the pH value on surface and detection obtain, carries out linear fit with origin, obtains fluorescence intensity and paper surface pH
Linear relationship, linear relation is as follows:
Y=3.075 × 106X-9.413×106
Wherein, Y is fluorescence intensity, and X is the pH value of paper surface；
The measurement of S3, unknown paper sheet surface pH value
Firstly, the chitosan solution of fluorescent marker is added dropwise in sample paper surface, it is to be checked after gel is at chitosan film
It surveys；Wherein the sample paper is the paper of unknown paper sheet surface pH value；
It is then detected that the above-mentioned chitosan film on sample paper, records fluorescence intensity；
Finally, fluorescence intensity is brought into linear relation obtained in S2, the pH value of sample paper surface is obtained；Detection
After, remove the gel mould of sample paper surface.
Further, in the S1, the pH of citric acid-sodium citrate buffer is 4~6.
Further, the pH of the chitosan solution of fluorescent marker is adjusted in S2 using acetum.
Further, the pH of the chitosan solution of fluorescent marker is 6 in the S2.
Further, the Fluoresceincarboxylic acid is one of 6- Fluoresceincarboxylic acid or 5-carboxyfluorescein.
Further, the process that the gel mould of sample paper surface is removed in the S3 is as follows:
The sodium tetraborate solution that about 200 μ L concentration are 0.05g/mL is added dropwise at paper film forming, is come into full contact with to the two
Afterwards, the white flock precipitate that chitosan and sodium tetraborate are formed is scraped off, gently to remove the gel mould of sample paper surface.
Further, the chitosan film of ultraviolet transmission reflective analysis instrument detection paper surface is utilized in the S2 and S3
Fluorescence intensity.
Compared with prior art, the beneficial effects of the present invention are: the pH on unknown paper sheet surface accurately, can be measured promptly
Value；And when testing paper surface pH value, paper will not be damaged.
Detailed description of the invention
Fig. 1 is the linear relationship chart of fluorescence intensity of the present invention Yu paper surface pH；
Fig. 2 is variation diagram of the carboxylic ammonia coupled product fluorescence intensity of the present invention with pH；
Before (a) is secondhand book paper membrane removal in Fig. 3；It (b) is after secondhand book paper membrane removal；It (c) is before filter paper membrane removal；It (d) is that filter paper removes
After film.
Specific embodiment
Technological means of the invention, creation characteristic, achieving the goal is easy to understand with effect in order to make, below in conjunction with
Technical solution of the present invention is clearly and completely described in specific embodiments of the present invention.
A specific embodiment of the invention, which adopts the following technical solutions, to be achieved.
Embodiment 1
A kind of new method measuring paper surface pH, includes the following steps:
S1, fluorescent marker chitosan preparation:
Firstly, the citric acid-sodium citrate buffering that Fluoresceincarboxylic acid, EDC and NHS are dissolved into acid (pH=5) is molten
It in liquid, is protected from light, reacts 23h under room temperature, the Fluoresceincarboxylic acid solution activated；The wherein object of Fluoresceincarboxylic acid, EDC and NHS
The ratio between amount of matter is Fluoresceincarboxylic acid: EDC:NHS=1:10:10；
Then, by the ratio of 0.025g/mL chitosan solution and the Fluoresceincarboxylic acid solution of above-mentioned activation 5:1 by volume
It is added in neutral phosphate buffer solution, is protected from light, reacts 1h under room temperature, obtain mixed solution；
Finally, high speed centrifugation, be washed with deionized obtained until cleaning solution unstressed configuration fluorescent marker chitosan it is molten
Liquid, for use；
The foundation of the relationship of S2, fluorescence intensity and paper surface pH value:
Firstly, adjusting the pH of the chitosan solution of fluorescent marker obtained in S1 to 4；
Then, the chitosan solution of fluorescent marker is added dropwise on the paper of known paper surface pH value, is formed after gel
Chitosan film, it is to be detected；
Finally, (365nm is the excitation of the chitosan film of fluorescent marker at 365nm wavelength using ultraviolet reflectance analyzer
Wavelength) chitosan film on the paper of known paper surface pH value is detected, and analyze to obtain by ImageJ image analysis software
Fluorescence intensity, and record, according to the fluorescence intensity that the pH value of known paper surface and detection obtain, Linear Quasi is carried out with origin
It closes, obtains the linear relationship of fluorescence intensity Yu paper surface pH, linear relation is as follows:
Y=3.075 × 106X-9.413×106
Wherein, Y is fluorescence intensity, and X is the pH value of paper surface；
The measurement of S3, unknown paper sheet surface pH value
Firstly, the chitosan solution of fluorescent marker is added dropwise in sample paper surface, after gel is at chitosan film later, to
Detection；Wherein the sample paper is the paper of unknown paper sheet surface pH value；
It is then detected that the above-mentioned chitosan film on sample paper, records fluorescence intensity；
Finally, fluorescence intensity is brought into linear relation obtained in S2, the pH value of sample paper surface is obtained；Detection
After, remove the gel mould of sample paper surface.
Embodiment 2
A kind of new method measuring paper surface pH, includes the following steps:
S1, fluorescent marker chitosan preparation:
Firstly, the citric acid-sodium citrate buffering that Fluoresceincarboxylic acid, EDC and NHS are dissolved into acid (pH=4) is molten
It in liquid, is protected from light, reacts 25h under room temperature, the Fluoresceincarboxylic acid solution activated；The wherein object of Fluoresceincarboxylic acid, EDC and NHS
The ratio between amount of matter is Fluoresceincarboxylic acid: EDC:NHS=1:10:10；
Then, by the ratio of 0.025g/mL chitosan solution and the Fluoresceincarboxylic acid solution of above-mentioned activation 5:1 by volume
It is added in neutral phosphate buffer solution, is protected from light, reacts 3h under room temperature, obtain mixed solution；
Finally, high speed centrifugation, be washed with deionized obtained until cleaning solution unstressed configuration fluorescent marker chitosan it is molten
Liquid, for use；
The foundation of the relationship of S2, fluorescence intensity and paper surface pH value:
Firstly, the pH of the chitosan solution of fluorescent marker obtained in S1 is adjusted to 5 using acetum；
Then, the chitosan solution of fluorescent marker is added dropwise on the paper of known paper surface pH value, is formed after gel
Chitosan film, it is to be detected；
Finally, (365nm is the excitation of the chitosan film of fluorescent marker at 365nm wavelength using ultraviolet reflectance analyzer
Wavelength) chitosan film on the paper of known paper surface pH value is detected, and analyze to obtain by ImageJ image analysis software
Fluorescence intensity, and record, according to the fluorescence intensity that the pH value of known paper surface and detection obtain, Linear Quasi is carried out with origin
It closes, obtains the linear relationship of fluorescence intensity Yu paper surface pH, linear relation is as follows:
Y=3.075 × 106X-9.413×106
Wherein, Y is fluorescence intensity, and X is the pH value of paper surface；
The measurement of S3, unknown paper sheet surface pH value
Firstly, the chitosan solution of fluorescent marker is added dropwise in sample paper surface, after gel is at chitosan film later, to
Detection；Wherein the sample paper is the paper of unknown paper sheet surface pH value；
It is then detected that the above-mentioned chitosan film on sample paper, records fluorescence intensity；
Finally, fluorescence intensity is brought into linear relation obtained in S2, the pH value of sample paper surface is obtained；Detection
After, remove the gel mould of sample paper surface.
Embodiment 3
A kind of new method measuring paper surface pH, includes the following steps:
S1, fluorescent marker chitosan preparation:
Firstly, the citric acid-sodium citrate buffering that Fluoresceincarboxylic acid, EDC and NHS are dissolved into acid (pH=6) is molten
It in liquid, is protected from light, the Fluoresceincarboxylic acid solution activated for 24 hours is reacted under room temperature；The wherein object of Fluoresceincarboxylic acid, EDC and NHS
The ratio between amount of matter is Fluoresceincarboxylic acid: EDC:NHS=1:10:10；EDC can greatly improve condensation reaction effect under NHS effect
Rate, carboxyl is reacted with EDC first generates intermediate, and NHS generates ester with intermediate again.
Then, 0.025g/mL chitosan solution and the Fluoresceincarboxylic acid solution of above-mentioned activation are added in the ratio of 5:1
In the phosphate buffer solution of neutral (pH=7~7.4), it is protected from light, reacts 2h under room temperature, obtain mixed solution；
Finally, high speed centrifugation, be washed with deionized obtained until cleaning solution unstressed configuration fluorescent marker chitosan it is molten
Liquid, for use；
The foundation of the relationship of S2, fluorescence intensity and paper surface pH value:
Firstly, the pH of the chitosan solution of fluorescent marker obtained above is adjusted to 6, for use with acetum；
Then, the chitosan solution of fluorescent marker is added dropwise to the paper in pH=4, pH=5, pH=6, pH=7 and pH=8
Surface, it is to be detected after chitosan gel rubber film；
Finally, (365nm is the excitation of the chitosan film of fluorescent marker at 365nm wavelength using ultraviolet reflectance analyzer
Wavelength) chitosan film of the above-mentioned fluorescent marker formed on the paper of known paper surface pH value is detected, and pass through ImageJ
Image analysis software is analyzed to obtain fluorescence intensity level, and records, as a result such as table 1.
The fluorescence intensity of paper surface pH value known to table 1
According to the fluorescence intensity that the pH value of paper surface in table 1 and detection obtain, linear fit is carried out with origin, is obtained
The linear relationship of fluorescence intensity and paper surface pH, as shown in Figure 1, linear relation is as follows:
Y=3.075 × 106X-9.413×106
Wherein, Y is fluorescence intensity, and X is the pH value of paper surface；
The measurement of S3, unknown paper sheet surface pH value
Firstly, the chitosan solution of fluorescent marker is added dropwise after sample paper surface, gel film forming, it is to be detected；Wherein
The sample paper is the paper of unknown paper sheet surface pH value；
Then, the shell of the fluorescent marker on above-mentioned sample paper is detected at 365nm wavelength using ultraviolet reflectance analyzer
Glycan film, and fluorescence intensity level is obtained by the analysis of ImageJ image analysis software, and record；
Finally, fluorescence intensity is brought into linear relation obtained in S2, the pH value of sample paper surface is obtained；Detection
After, remove the gel mould of sample paper surface.
Except the process of the gel mould of sample paper surface is as follows:
The sodium tetraborate solution that about 200 μ L concentration are 0.05g/mL is added dropwise at paper film forming, is come into full contact with to the two
Afterwards, the white flock precipitate that chitosan and sodium tetraborate are formed is scraped off, gently to remove the gel mould of sample paper surface.
Such as the fluorescence intensity through test sample paper is 1058903, brings Y=3.075 × 10 into for 10589036X-
9.413×106In, obtain 1058903=3.075 × 106X-9.413×106, X value, the i.e. pH value of paper surface is calculated
It is 3.4.We can accurately obtain the pH value of sample paper surface in this way.
As a preferred embodiment of the present embodiment, Fluoresceincarboxylic acid is in 6- Fluoresceincarboxylic acid or 5-carboxyfluorescein
It is a kind of.
The test that we also carry out the membrance casting condition of the chitosan gel rubber of fluorescent marker, the chitosan of fluorescent marker is molten
The pH of liquid is respectively adjusted to pH=5, pH=6 and pH=7；Then by the chitosan solution of the fluorescent marker of above-mentioned three kinds of differences pH
It is added drop-wise to gel on filter paper respectively to form a film, finds following result:
(1) chitosan solution of both of pH=5 and pH=6 fluorescent markers can gel film forming, and it is obvious to form a film；pH
Under the conditions of=6, the most easy gel film forming of chitosan solution.
(2) chitosan gel rubber of this fluorescent marker of pH=7 can not form a film, and have white flock precipitate.
The fluorescence intensity carried out again to the chitosan gel rubber of the fluorescent marker of above-mentioned three kinds of differences pH simultaneously is tested, discovery knot
Fruit is as shown in Fig. 2, be the fluorescence mark of pH=7 at 517nm (fluorescence emission wavelengths of the chitosan gel rubber of fluorescent marker) in wavelength
For the chitosan gel rubber of note almost without there is peak value, this just illustrates the chitosan gel rubber of the fluorescent marker of this pH=7 in paper
Surface does not form a film.
In addition, after removing the chitosan gel rubber film of fluorescent marker, paper surface is still kept completely, paper after detection
It opens and is not destroyed, as shown in Figure 3.
In conclusion the present processes can fast, accurately measure paper on the basis of ensuring that paper is not impaired
Open the pH value on surface.
Disclosed above is only presently preferred embodiments of the present invention, and still, the embodiment of the present invention is not limited to this, Ren Heben
What the technical staff in field can think variation should all fall into protection scope of the present invention.
Claims (7)
1. a kind of new method for measuring paper surface pH, which comprises the steps of:
S1, fluorescent marker chitosan preparation:
Firstly, Fluoresceincarboxylic acid, EDC and NHS are dissolved into acid citric acid-sodium citrate buffer, it is protected from light, often
Temperature is lower to react 23h~25h, the Fluoresceincarboxylic acid solution activated；Wherein the amount of the substance of Fluoresceincarboxylic acid, EDC and NHS it
Than for Fluoresceincarboxylic acid: EDC:NHS=1:10:10；
Then, by 0.025g/mL chitosan solution and the Fluoresceincarboxylic acid solution of above-mentioned activation by volume 5:1 ratio be added
It into neutral phosphate buffer solution, is protected from light, 1h~3h is reacted under room temperature, obtains mixed solution；
Finally, high speed centrifugation, is washed with deionized the chitosan solution that fluorescent marker is obtained until cleaning solution unstressed configuration,
For use；
The foundation of the relationship of S2, fluorescence intensity and paper surface pH value:
Firstly, adjusting the pH of the chitosan solution of fluorescent marker obtained in S1 to 4~6；
Then, the chitosan solution of fluorescent marker is added dropwise on the paper of known paper surface pH value, it is poly- forms shell after gel
Sugared film, it is to be detected；
Finally, detecting the chitosan film on the paper of known paper surface pH value, fluorescence intensity is recorded, according to known paper surface
PH value and the obtained fluorescence intensity of detection, carry out linear fit with origin, obtain the line of fluorescence intensity Yu paper surface pH
Sexual intercourse, linear relation are as follows:
Y=3.075 × 106X-9.413×106
Wherein, Y is fluorescence intensity, and X is the pH value of paper surface；
The measurement of S3, unknown paper sheet surface pH value
Firstly, the chitosan solution of fluorescent marker is added dropwise in sample paper surface, it is to be checked after gel is at chitosan film later
It surveys；Wherein the sample paper is the paper of unknown paper sheet surface pH value；
It is then detected that the above-mentioned chitosan film on sample paper, records fluorescence intensity；
Finally, fluorescence intensity is brought into linear relation obtained in S2, the pH value of sample paper surface is obtained；Detection terminates
Afterwards, the gel mould of sample paper surface is removed.
2. a kind of new method for measuring paper surface pH as described in claim 1, which is characterized in that in the S1, citric acid-
The pH of sodium citrate buffer is 4~6.
3. a kind of new method for measuring paper surface pH as described in claim 1, which is characterized in that use acetic acid in the S2
Solution adjusts the pH of the chitosan solution of fluorescent marker.
4. a kind of new method for measuring paper surface pH as claimed in claim 3, which is characterized in that the shell of the fluorescent marker
The pH of glycan solution is 6.
5. a kind of new method for measuring paper surface pH as described in claim 1, which is characterized in that the Fluoresceincarboxylic acid is
One of 6- Fluoresceincarboxylic acid or 5-carboxyfluorescein.
6. a kind of new method for measuring paper surface pH as described in claim 1, which is characterized in that remove sample in the S3
The process of the gel mould of paper surface is as follows:
The sodium tetraborate solution that concentration is 0.05g/mL is added dropwise at paper film forming and scrapes off chitosan after the two comes into full contact with
The white flock precipitate formed with sodium tetraborate, to remove the gel mould of sample paper surface.
7. a kind of new method for measuring paper surface pH as described in claim 1, which is characterized in that sharp in the S2 and S3
With the fluorescence intensity of the chitosan film of ultraviolet transmission reflective analysis instrument detection paper surface.
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| CN113484288A (en) * | 2021-05-17 | 2021-10-08 | 上海交通大学 | Weak acid and weak base concentration measuring method based on laser-induced fluorescence of fluorescein sodium |
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| Publication number | Publication date |
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| CN108956569B (en) | 2021-02-05 |
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