CN108872127A - A kind of nano-cellulose film measurement of water ratio method based on Subtractive Infrared Spectroscopy - Google Patents
A kind of nano-cellulose film measurement of water ratio method based on Subtractive Infrared Spectroscopy Download PDFInfo
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- CN108872127A CN108872127A CN201810391274.6A CN201810391274A CN108872127A CN 108872127 A CN108872127 A CN 108872127A CN 201810391274 A CN201810391274 A CN 201810391274A CN 108872127 A CN108872127 A CN 108872127A
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- 229920002678 cellulose Polymers 0.000 title claims abstract description 94
- 239000001913 cellulose Substances 0.000 title claims abstract description 94
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000005259 measurement Methods 0.000 title claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000004566 IR spectroscopy Methods 0.000 title claims abstract description 18
- 238000012417 linear regression Methods 0.000 claims abstract description 5
- 235000011194 food seasoning agent Nutrition 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 241000208340 Araliaceae Species 0.000 claims 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims 1
- 235000003140 Panax quinquefolius Nutrition 0.000 claims 1
- 238000002474 experimental method Methods 0.000 claims 1
- 235000008434 ginseng Nutrition 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000009659 non-destructive testing Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 abstract 8
- 239000010409 thin film Substances 0.000 abstract 1
- 238000000691 measurement method Methods 0.000 description 5
- 239000002159 nanocrystal Substances 0.000 description 5
- 108010002217 Calcifying Nanoparticles Proteins 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 229920000298 Cellophane Polymers 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000000721 bacterilogical effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000126 substance Substances 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
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3554—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for determining moisture content
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- Spectroscopy & Molecular Physics (AREA)
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- Life Sciences & Earth Sciences (AREA)
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The nano-cellulose film measurement of water ratio method based on Subtractive Infrared Spectroscopy that the invention discloses a kind of chooses the sample that nano-cellulose film to be measured is made under basic pattern and different humidity；Measure the infrared spectrogram H of basic pattern respectively using infrared spectrometer0With the infrared spectrogram H of nano-cellulose film sample under different humidityS；With the infrared spectrogram H of nano-cellulose film sample under different humiditySSubtract the infrared spectrogram H of basic pattern0, obtain Infrared Difference spectrogram HS‑0；Acquire 1600-1800cm in Infrared Difference spectrogram‑1Area A in rangeS‑0；Utilize the moisture content MC of nano-cellulose film sample under dry method measurement different humidityS；By moisture content MCSWith area AS‑0The nano-cellulose film measurement of water ratio model based on Subtractive Infrared Spectroscopy is constructed using least square method linear regression.The model can be used for the batch measurement of nano-cellulose film moisture content to be measured, and each sample time-consuming 1s substantially reduces the detection time of nano-cellulose film moisture content.The present invention has the advantages that detection is quick, sample is less-in-demand, is a kind of non-destructive testing technology, can be applied to nano-cellulose thin film testing field.
Description
Technical field
This patent is related to nano-cellulose membrane quality measurement field more particularly to a kind of receiving based on Subtractive Infrared Spectroscopy
Rice cellophane measurement of water ratio method.
Background technique
Nano-cellulose film has many advantages, such as that tensile strength is big, bacteriological filtration performance is good, biodegradable, high-crystallinity,
Middle moisture content is one of the important physical of nano-cellulose film, is had with cellulose membrane mechanical property and its practical utilize
Close relationship.The traditional classical method for measuring nano-cellulose film moisture content is seasoning.Seasoning also known as gravimetric method, this
Method accuracy is high, but inconvenient, takes a long time.Exactly these obvious limitations, constrain the practical application of the measurement method
Range and application scenarios.
Infrared spectroscopy is used as " molecular fingerprint ", is widely used in substance chemistry composition research.Nineteen forty-seven First in the world
Dual-beam automatically records infrared spectrophotometer appearance.Thereafter, infrared spectroscopy is technically constantly progressive.The seventies later period,
Interference-type Fourier transform infrared spectroscopy becomes increasingly popular, it has, and test sample dosage is few, detection time is short, accuracy is high, spectrum
The advantages that chart database is comprehensively, identification and analysis result is reliable, apparatus structure is simple.Therewith, infrared spectroscopy just becomes modern analysis
The most frequently used and indispensable tool in chemistry.It introduces based on the above background, infrared spectroscopy is hopeful to be applied to nano-cellulose
The rapid survey of moisture content in film.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, provide it is a kind of quickly, sample dosage it is few
The measurement method of nano-cellulose film moisture content.
In order to solve the above technical problems, technical solution proposed by the present invention is：
A kind of nano-cellulose film measurement of water ratio method based on Subtractive Infrared Spectroscopy, includes the following steps：
1) basic pattern is prepared：Selected nano-cellulose film sample is placed in an oven, and first drying 2 is small under 60 DEG C of low temperature
When, 103 ± 2 DEG C, 8~10h of continuous drying are adjusted the temperature to later, during which, are weighed once every 1h, until finally weighing twice
Difference be no more than 0.3%；
2) the nano-cellulose film sample under different humidity is prepared：Selected nano-cellulose film is put into constant temperature perseverance
Wet tank adjusts humidity, balances 5h, and the nano-cellulose film sample under different humidity is made；
3) under dry method measurement different humidity nano-cellulose film sample moisture content：Utilize seasoning determination step 2)
The moisture content MC of nano-cellulose film sample under middle different humidityS；
4) Infrared Difference spectrogram is measured：Utilize infrared spectrometer distinguish determination step 1) in basic pattern infrared spectrogram H0And step
It is rapid 2) under different humidity nano-cellulose film sample infrared spectrogram HS；It is tried with nano-cellulose film under different humidity
The infrared spectrogram H of sampleSSubtract the infrared spectrogram H of basic pattern0, obtain Infrared Difference spectrogram HS-0；Acquire 1600- in Infrared Difference spectrogram
1800cm-1Area A in rangeS-0；
5) the nano-cellulose film measurement of water ratio model based on Subtractive Infrared Spectroscopy is constructed：By DIFFERENT WET in step 3)
The moisture content MC of nano-cellulose film sample under degreeSWith area A in step 4)S-0It is obtained using least square method linear regression
To equation：MCS=k × AS-0, to calculate nano-cellulose film moisture content；MC in equationSIt is aqueous for nano-cellulose film
Rate, AS-0For 1600-1800cm in Infrared Difference spectrogram-1Area in range, k are different nano-cellulose film measurement of water ratio
Parameter；
6) moisture content is measured：Using the regression equation measured in step 5), nano-cellulose film examination to be measured is measured in batches
Sample moisture content.
As a further improvement of the above technical scheme：
Nano-cellulose film sample to be measured is that thickness is lower than 5 microns, and area is greater than the micro sample of 1 square micron.
In step 6) after obtaining regression equation, the time of single nano-cellulose film sample moisture content to be measured is measured
Only need 1s.
Compared with existing measurement method, it is an advantage of the invention that：
The surveyed nano-cellulose film sample of the present invention is that thickness is lower than 5 microns, and area is greater than 1 micron of micro sample,
Sample size needed for greatly reducing measurement of water-content coefficient in the process；Meanwhile the time of measuring of nano-cellulose film moisture content being contracted
Short is 1s, the measure batch suitable for sample.That the present invention overcomes original measurement methods is inconvenient, take a long time, sample needs
The big disadvantage of the amount of asking has the advantages that detection is quick, sample is less-in-demand, is a non-destructive testing technology, can be used for fiber
Plain film film evaluates field.
Detailed description of the invention
Fig. 1 is the Infrared Difference spectrogram of cellulose nano-fibrous film used in this patent modeling.
Fig. 2 is the regression equation that cellulose nano-fibrous film sample obtains used in this patent.
Specific embodiment
To facilitate the understanding of the present invention, it is more careful to make below in conjunction with Figure of description and preferred embodiment to the present invention
Description, but the protection scope of the present invention is not limited to the following specific embodiments.
A kind of nano-cellulose film measurement of water ratio method based on Subtractive Infrared Spectroscopy, includes the following steps：
1) basic pattern is prepared：Selected nano-cellulose film sample is placed in an oven, and temperature is adjusted to 103 ± 2 DEG C, continues
10h is dried, during which, is weighed once every 2h, until the difference of last weighing twice is no more than 0.3%；
2) the nano-cellulose film sample under different humidity is prepared：Selected nano-cellulose film is put into constant temperature perseverance
Wet tank adjusts humidity, balances 5h, and the nano-cellulose film sample under different humidity is made；
3) under dry method measurement different humidity nano-cellulose film sample moisture content：Utilize seasoning determination step 2)
The moisture content MC of nano-cellulose film sample under middle different humidityS；
4) Infrared Difference spectrogram is measured：Utilize infrared spectrometer distinguish determination step 1) in basic pattern infrared spectrogram H0And step
It is rapid 2) under different humidity nano-cellulose film sample infrared spectrogram HS；It is tried with nano-cellulose film under different humidity
The infrared spectrogram H of sampleSSubtract the infrared spectrogram H of basic pattern0, obtain Infrared Difference spectrogram HS-0；Acquire 1600- in Infrared Difference spectrogram
1800cm-1Area A in rangeS-0；
5) the nano-cellulose film measurement of water ratio model based on Subtractive Infrared Spectroscopy is constructed：By DIFFERENT WET in step 3)
The moisture content MC of nano-cellulose film sample under degreeSWith area A in step 4)S-0It is obtained using least square method linear regression
To equation：MCS=k × AS-0, to calculate nano-cellulose film moisture content；MC in equationSIt is aqueous for nano-cellulose film
Rate, AS-0For 1600-1800cm in Infrared Difference spectrogram-1Area in range, k are different nano-cellulose film measurement of water ratio
Parameter；
6) moisture content is measured：Using the regression equation measured in step 5), nano-cellulose film examination to be measured is measured in batches
Sample, single nano-cellulose film sample measurement only need 1s.
Above-mentioned nano-cellulose film sample is micro sample, and thickness is lower than 10 microns, and area is greater than 1 square micron.
With 3 kinds of different nano-cellulose films, (cellulose nano-fibrous, Cellulose nanocrystal, bacteria nano are fine below
Dimension element) illustrate measurement method of the invention for measurement of water ratio：
Embodiment 1
(1) cellulose nano-fibrous film is made into growth 5mm × 4 μ m in size of wide 5mm × thickness sample, is put into baking oven,
It is first dried 2 hours under 60 DEG C of low temperature, adjusts the temperature to 103 ± 2 DEG C, 8~10h of continuous drying later, therebetween, try to claim every 1h
Once, until finally the difference of weighing is minimum (being no more than 0.3%) twice, basic pattern is made；
(2) cellulose nano-fibrous film sample is placed in climatic chamber, it is 10%, 20%, 30% that humidity, which is made,
40%, 50%, 60%, 70%, 80% and 90% cellulose nano-fibrous film sample；
(3) the aqueous of the cellulose nano-fibrous film sample under different humidity obtained in seasoning measurement (2) is utilized
Rate MC10%, MC20%, MC30%, MC40%, MC50%, MC60%, MC70%, MC80%, MC90%；
(4) the infrared spectrogram H of basic pattern in (1) is measured using infrared spectrometer0%(2) sample under different humidity in
Infrared spectrogram H10%, H20%, H30%, H40%, H50%, H60%, H70%, H80%, H90%；With cellulose nano-fibrous thin under different humidity
The infrared spectrogram of film sample subtracts the infrared spectrogram of basic pattern, obtains Infrared Difference spectrogram H10%-0%, H20%-0%, H30%-0%,
H40%-0%, H50%-0%, H60%-0%, H70%-0%, H80%-0%, H90%-0%, as shown in Figure 1；Acquire 1600- in Infrared Difference spectrogram
1800cm-1Area A in range10%-0%, A20%-0%, A30%-0%, A40%-0%, A50%-0%, A60%-0%, A70%-0%, A80%-0%,
A90%-0%；
(5) by the moisture content MC of film sample cellulose nano-fibrous under different humiditySWith area AS-0Utilize least square
Method linear regression obtains equation：MCS=0.0305 × AS-0, as shown in Figure 2.
By moisture content MCSWith Infrared Difference Spectrum area AS-0Building Subtractive Infrared Spectroscopy measures cellulose nano-fibrous film and contains
When water rate model, the related coefficient of model is greater than 0.95, as shown in Fig. 2, obtaining satisfied precision of prediction.Obtained humidity at random
For 15% cellulose nano-fibrous film, using the above method, measuring moisture content is 0.0519, and dry method measurement is aqueous
Rate is 0.051, and calculating relative error is 1.76%.As a result explanation can rapidly and accurately measure fiber using method of the invention
Plain nano-fiber film sample moisture content.Individual sample time-consuming is only 1s.
Embodiment 2
Using method in embodiment 1, Cellulose nanocrystal film sample moisture content is measured, obtains regression equation：
MCS=MCS=0.0262 × AS-0.When measure batch Cellulose nanocrystal film sample, each Specimen Determination used time is only needed 1 second.
The Cellulose nanocrystal film sample that random obtained humidity is 15%, using the above method, measuring moisture content is 0.0430, and is done
The moisture content that dry method measures is 0.042, and calculating relative error is 2.38%.As a result explanation can be quick using the method for this patent
Accurately measurement Cellulose nanocrystal film sample moisture content.
Embodiment 3
Using method in embodiment 1, Nano bacteria cellulose film sample moisture content is measured, obtains recurrence side
Journey：MCS=0.0397 × AS-0.When measure batch Nano bacteria cellulose film sample, each Specimen Determination used time is only needed 1 second.
The Nano bacteria cellulose film sample that random obtained humidity is 15%, using the above method, measuring moisture content is 0.0675, and
The moisture content that seasoning measures is 0.066, and calculating relative error is 2.27%.As a result explanation can be fast using the method for this patent
Fast accurately measurement Nano bacteria cellulose film moisture content.
Claims (3)
1. a kind of experimental procedure of the nano-cellulose film measurement of water ratio method based on Subtractive Infrared Spectroscopy：
1) basic pattern is prepared：Selected nano-cellulose film sample is placed in an oven, is first dried 2 hours under 60 DEG C of low temperature,
103 ± 2 DEG C, 8~10h of continuous drying are adjusted the temperature to later, during which, are weighed once every 1h, until finally weighing it twice
Difference is no more than 0.3%, and basic pattern is made；
2) the nano-cellulose film sample under different humidity is prepared：Selected nano-cellulose film is put into constant temperature and humidity
Case adjusts humidity, balances 5h, and the nano-cellulose film sample under different humidity is made；
3) under dry method measurement different humidity nano-cellulose film sample moisture content：Utilize seasoning determination step 2) in not
With the moisture content MC of the nano-cellulose film sample under humiditys；
4) Infrared Difference spectrogram is measured：Utilize infrared spectrometer distinguish determination step 1) in basic pattern infrared spectrogram H0With step 2)
The infrared spectrogram H of nano-cellulose film sample under middle different humidityS；With nano-cellulose film sample under different humidity
Infrared spectrogram HSSubtract the infrared spectrogram H of basic pattern0, obtain Infrared Difference spectrogram HS-0；Acquire 1600- in Infrared Difference spectrogram
1800cm-1Area A in rangeS-0；
5) the nano-cellulose film measurement of water ratio model based on Subtractive Infrared Spectroscopy is constructed：It will be under different humidity in step 3)
Nano-cellulose film sample moisture content MCSWith area A in step 4)S-0Utilize the least square method linear regression side of obtaining
Journey：MCS=k × AS-0, to calculate nano-cellulose film moisture content；MC in equationSFor nano-cellulose film moisture content,
AW-0For 1600-1800cm in Infrared Difference spectrogram-1Area in range, k are the ginseng of different nano-cellulose film measurement of water ratio
Number；
6) moisture content is measured：Using regression equation obtained in step 5), nano-cellulose film sample to be measured is measured in batches and is contained
Water rate.
2. the nano-cellulose film measurement of water ratio method according to claim 1 based on Subtractive Infrared Spectroscopy, special
Sign is：The nano-cellulose film sample to be measured is that thickness is lower than 10 microns, and area is greater than the micro examination of 1 square micron
Sample.
3. the nano-cellulose film measurement of water ratio method according to claim 1 based on Subtractive Infrared Spectroscopy, special
Sign is：In step 6) after obtaining regression equation, when batch measures nano-cellulose film sample, individual sample is measured only
Need 1s.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111610117A (en) * | 2020-05-13 | 2020-09-01 | 江苏鑫源烟草薄片有限公司 | Method for rapidly measuring moisture content of sheet for heating cigarette |
| CN114166822A (en) * | 2021-12-03 | 2022-03-11 | 中南林业科技大学 | Method for measuring water content of wood cell wall based on Raman difference spectrum technology |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104390932A (en) * | 2014-11-12 | 2015-03-04 | 中南林业科技大学 | Method for detecting moisture content of wood on basis of infrared differential spectrum technology |
| CN107462549A (en) * | 2017-08-23 | 2017-12-12 | 东北林业大学 | A kind of forest dead fuel moisture content on-line measurement device and its measuring method |
-
2018
- 2018-04-27 CN CN201810391274.6A patent/CN108872127A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104390932A (en) * | 2014-11-12 | 2015-03-04 | 中南林业科技大学 | Method for detecting moisture content of wood on basis of infrared differential spectrum technology |
| CN107462549A (en) * | 2017-08-23 | 2017-12-12 | 东北林业大学 | A kind of forest dead fuel moisture content on-line measurement device and its measuring method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111610117A (en) * | 2020-05-13 | 2020-09-01 | 江苏鑫源烟草薄片有限公司 | Method for rapidly measuring moisture content of sheet for heating cigarette |
| CN114166822A (en) * | 2021-12-03 | 2022-03-11 | 中南林业科技大学 | Method for measuring water content of wood cell wall based on Raman difference spectrum technology |
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