CN110763647A - Method for determining partition paper extract by using infrared spectroscopy - Google Patents
Method for determining partition paper extract by using infrared spectroscopy Download PDFInfo
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- CN110763647A CN110763647A CN201911140076.3A CN201911140076A CN110763647A CN 110763647 A CN110763647 A CN 110763647A CN 201911140076 A CN201911140076 A CN 201911140076A CN 110763647 A CN110763647 A CN 110763647A
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- 239000000284 extract Substances 0.000 title claims abstract description 38
- 238000005192 partition Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000004566 IR spectroscopy Methods 0.000 title claims abstract description 13
- 125000006850 spacer group Chemical group 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 10
- 238000001228 spectrum Methods 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 238000010521 absorption reaction Methods 0.000 claims abstract description 5
- 125000000524 functional group Chemical group 0.000 claims abstract description 5
- 239000012535 impurity Substances 0.000 claims abstract description 5
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 11
- 239000000498 cooling water Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 239000004570 mortar (masonry) Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 230000035807 sensation Effects 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 4
- 239000008399 tap water Substances 0.000 claims description 4
- 235000020679 tap water Nutrition 0.000 claims description 4
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 6
- 239000011521 glass Substances 0.000 description 12
- 239000000758 substrate Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920001621 AMOLED Polymers 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000005102 attenuated total reflection Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 125000004355 nitrogen functional group Chemical group 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- G01N2021/3572—Preparation of samples, e.g. salt matrices
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention provides a method for determining a spacer paper extract by using an infrared spectroscopy, which comprises the following steps of preparing the spacer paper extract through the spacer paper extract; tabletting, namely pressing a KBr sheet; step three, testing, namely utilizing an infrared spectrometer to perform background scanning to obtain a current air background image; uniformly coating a piece of partition paper extract on a reflecting surface of a KBr sheet, repeatedly coating and drying, then placing the KBr sheet on a measuring clamp for fixing, scanning to obtain an infrared absorption spectrogram with an air background subtracted, selecting a marked peak value on the sample image, continuously testing a plurality of samples, identifying each scanned spectrogram peak value, then searching and checking with a spectrum library, further judging the relative difference value of the batch of partition paper corresponding to the functional group by counting the height of the corresponding peak value, and analyzing to obtain the impurity content of the partition paper extract. The method has the advantages of simple detection step operation, high precision and high efficiency, can meet the daily detection control requirements, and is convenient to popularize and use.
Description
Technical Field
The invention relates to a method for measuring spacing paper for glass transportation, in particular to a method for measuring an extract of the spacing paper by using an infrared spectroscopy.
Background
Under the high-speed development of the internet of things and the internet, the display screen is used as the most important medium for human-computer interaction, and the market scale of the display screen is continuously enlarged along with the increase of the number of terminal devices and the display area. From the existing liquid crystal panel industry, whether the TFT-LCD or the AMOLED, the glass substrate is an important material required by the production thereof. Depending on the display technology and the application scenario, additional layers of glass or multiple layers of glass may be required. Since the glass substrate is an important component constituting the liquid crystal display device and is one of the key basic materials of the liquid crystal display industry, the quality requirements of the glass substrate are becoming more and more strict.
The quality problems of the glass substrate mainly include surface scratches, internal defects, surface oil stains, and the like, wherein the most serious problem is the surface oil stains. In order to solve the problem, the quality of the paper which is clamped between the glass and the glass in the transportation process after the glass is processed is very important. How to ensure that the spacer paper does not cause oily pollution on the surface of the glass by testing the spacer paper extract is an important problem for improving the quality of the glass substrate.
The current common measurement methods for the partition paper extract are as follows: quantitative test is carried out by utilizing Fourier transform attenuated total reflection infrared spectroscopy, and the liquid ATR accessory is required, is expensive and is not beneficial to popularization; the test by using a liquid and KBr mixed tabletting method is adopted, and the KBr sheet is often unsuccessfully prepared due to high moisture content, so that the detection cannot be carried out.
Disclosure of Invention
In order to solve the problems of the prior art, the present invention aims to provide a method for measuring a separation paper extract by using infrared spectroscopy. The method adopted by the invention does not need to add an ATR accessory of liquid, can ensure the light transmittance of the KBr sheet, and is convenient for detection.
The technical scheme adopted by the invention for solving the problems is as follows: a method for determining a separation paper extract by infrared spectroscopy comprises the following steps:
preparing a spacer paper extract, cutting a certain amount of spacer paper, assembling an extractor, placing a sample and a reagent correspondingly, and then opening a tap water valve and an electric furnace switch for heating; observing and controlling the water inlet and outlet speed of a condensation water pipe, repeatedly condensing and volatilizing dichloromethane in the extracting solution for many times, and obtaining a partition paper extract after volatilizing;
tabletting, namely putting a proper amount of KBr crystals into an agate mortar for full grinding until no granular sensation exists when sample powder is scratched by a grinding pestle, putting the ground sample into a weighing bottle, drying the sample in an oven, and transferring the sample into a dryer for storage for later use; weighing dried KBr powder, putting the powder into a sample cell of a sample press, pressing by using a tablet press, taking out a KBr sheet, flattening the surface, and packaging by using a self-sealing bag to prevent the KBr sheet from being polluted;
step three, testing, namely utilizing an infrared spectrometer to perform background scanning to obtain a current air background image; uniformly coating a piece of partition paper extract on a reflecting surface of a KBr sheet, repeatedly coating and drying, then placing the KBr sheet on a measuring clamp for fixing, scanning to obtain an infrared absorption spectrogram with an air background subtracted, selecting a marked peak value on the sample image, continuously testing a plurality of samples, identifying each scanned spectrogram peak value, then searching and checking with a spectrum library, further judging the relative difference value of the batch of partition paper corresponding to the functional group by counting the height of the corresponding peak value, and analyzing to obtain the impurity content of the partition paper extract.
Further, the scanning start wavenumber is 4000 cm-1The wave number at the end of scanning was 450 cm-1Resolution of 4cm-1Data interval of 1.93cm-1The number of scans was set to 16.
Further, in the second step, the temperature in the oven is set to be 105 ℃, and the drying time is 4 hours.
Further, in the second step, the pressure of the tablet press is set to 40 tons, and the pressing time is 30 seconds.
Further, in the first step, the structure of the assembled extractor is as follows: the flask is positioned at the bottom, the stirring magnetons are positioned in the flask, dichloromethane is contained in the flask, the bottom of the flask is placed on an electric furnace for heating, a sleeve is arranged on the opening of the flask, and the other end of the sleeve is connected with a condensing tube through an adapter; one side of the sleeve is connected with the siphon pipe, the other side of the sleeve is connected with the steam bypass pipe, and two ends of the steam bypass pipe are connected to the lower part and the upper part of the sleeve; the lower part of the condensing pipe is provided with a cooling water inlet, and the upper part of the condensing pipe is provided with a cooling water outlet; the sample is located within the cannula.
The beneficial technical effects of the invention are as follows: the detection steps are simple to operate, high in precision and high in efficiency, can meet the requirement of daily detection management and control, and are convenient to popularize and use.
Drawings
The technical scheme of the invention is described in detail in the following with reference to the accompanying drawings
FIG. 1 is a schematic diagram of the assembly of the extract of the present invention.
In the figure: 1. stirring magneton, 2, flask, 3, steam bypass pipe, 4, siphon pipe, 5, sleeve, 6, adapter, 7, condenser pipe, 8, cooling water inlet, 9 and cooling water outlet.
Detailed Description
Example 1
A method for determining a separation paper extract by infrared spectroscopy comprises the following steps:
preparing a spacer paper extract, cutting a certain amount of spacer paper, assembling an extractor, placing a sample and a reagent correspondingly, and then opening a tap water valve and an electric furnace switch for heating; observing and controlling the water inlet and outlet speed of a condensation water pipe, repeatedly condensing and volatilizing dichloromethane in the extracting solution for many times, and obtaining a partition paper extract after volatilizing;
tabletting, namely putting a proper amount of KBr crystals into an agate mortar for full grinding until no granular sensation exists when sample powder is scratched by a grinding pestle, putting the ground sample into a weighing bottle, drying the sample in an oven, and transferring the sample into a dryer for storage for later use; weighing dried KBr powder, putting the powder into a sample cell of a sample press, pressing by using a tablet press, taking out a KBr sheet, flattening the surface, and packaging by using a self-sealing bag to prevent the KBr sheet from being polluted;
step three, testing, namely utilizing an infrared spectrometer to perform background scanning to obtain a current air background image; uniformly coating a piece of partition paper extract on a reflecting surface of a KBr sheet, repeatedly coating and drying, then placing the KBr sheet on a measuring clamp for fixing, scanning to obtain an infrared absorption spectrogram with an air background subtracted, selecting a marked peak value on the sample image, continuously testing a plurality of samples, identifying each scanned spectrogram peak value, then searching and checking with a spectrum library, further judging the relative difference value of the batch of partition paper corresponding to the functional group by counting the height of the corresponding peak value, and analyzing to obtain the impurity content of the partition paper extract.
As shown in fig. 1, the structure of the assembled extractor is: the flask 2 is positioned at the bottom, the stirring magneton 1 is positioned in the flask 2, dichloromethane is contained in the flask 2, the bottom of the flask is placed on an electric furnace for heating, a sleeve 5 is arranged on the mouth of the flask 2, and the other end of the sleeve 5 is connected with a condensation pipe 7 through an adapter 6; one side of the sleeve 5 is connected with the siphon 4, the other side of the sleeve is connected with the steam bypass pipe 3, and two ends of the steam bypass pipe 3 are connected with the lower part and the upper part of the sleeve 5; the lower part of the condensation pipe 7 is provided with a cooling water inlet 8, and the upper part is provided with a cooling water outlet 9; the sample is located within the cannula 5.
Example 2
The embodiment adopts the same batch of partition paper of the same manufacturer, namely selects 180526 batches of partition paper with the batch number of manufacturer A, and is implemented according to the following steps:
1. preparation of the spacer paper extract
(1) Cutting 10g of partition paper, assembling the Soxhlet extractor strictly according to the structure shown in figure 1, placing a sample and a reagent correspondingly, and then opening a tap water valve and an electric furnace switch for heating;
(2) observing and controlling the water inlet and outlet speed of the condensation water pipe, repeatedly condensing and volatilizing the dichloromethane in the extracting solution for many times, and finally obtaining the partition paper extract after volatilizing.
2. Tabletting
(1) An appropriate amount of KBr crystals (spectrally pure) is taken and put into an agate mortar for sufficient grinding until no grain sensation is observed after the sample powder is scratched by a grinding pestle. And then the ground sample is put into a weighing bottle, a cover is covered (a seam is left), the sample is dried for 4 hours in an oven at 105 ℃, and then the sample is transferred into a dryer for storage for standby.
(2) 2.4 g of dried KBr powder is weighed and put into a sample cell of a sample press, the sample cell is pressed for 30 seconds by a tablet press under the pressure of 40 tons, and a KBr sheet is taken out, has a flat and semitransparent surface and is packaged by a self-sealing bag to prevent pollution.
3. Testing
(1) Opening a computer and an infrared Spectrum power supply, clicking a Spectrum shortcut icon on a desktop, selecting a user name administeror, and clicking to confirm that a Spectrum interface is entered;
(2) clicking a button for setting basic functions of the instrument to edit parameters, selecting wave number in abscissa unit and T% in ordinate unit, wherein the scanning starting wave number is 4000 cm-1The wave number at the end of scanning was 450 cm-1Resolution of 4cm-1Data interval of 1.93cm-1Setting the number of scanning times to be 16 times in the accumulation amount;
(3) selecting a background in a scanning type, clicking to scan, and obtaining an air background image on a spectrum interface after scanning is finished for ten seconds;
(4) uniformly coating a reflecting surface (one surface corresponding to a light source) of a KBr sheet with a partition paper extract, carefully drying the KBr sheet by using a blower, repeatedly coating and drying for 8 times, opening an instrument cover, putting the KBr sheet on a clamp for fixing, covering the clamp with the cover, editing a sample name in a sample ID, selecting a sample in a scanning type, clicking a scanning button, and obtaining an infrared absorption spectrogram with an air background subtracted on a spectrum interface after ten seconds. Clicking the view, selecting a marked peak value, and automatically marking the peak value on the sample graph;
(5) continuously testing 5 samples, identifying each scanning spectrogram peak value through instrument software processing, searching and checking with a spectrum library, and further judging the relative difference value of the batch of spacing paper corresponding to the functional group by counting the height of the corresponding peak value to obtain:
TABLE 1 peak height of NH2 groups for the same batch of products
Example 3
In this embodiment, different batches of partition paper of the same manufacturer are adopted, that is, batches of partition paper with lot numbers of manufacturers a 180111, 180214, 180419, 180526, and 180609 are selected, and implemented according to the same steps in embodiment 2, so as to obtain:
TABLE 2 peak heights of NH2 groups for different batches of product
From the above measurements of the samples (Table 1 and Table 2), it can be seen that NH2 groups are 3180cm between the same batch of spacer paper extracts from the same manufacturer-1The difference of the peak heights is not large, and the difference of samples of different batches of the same manufacturer is relatively large, which shows that the infrared spectrum tabletting method is used for testing the partition paper extract, so that the product quality of partition paper of different batches is compared, the sample treatment can be conveniently carried out, the impurity content of the partition paper extract is rapidly analyzed, and whether the extract contains nitrogen functional groups or not can be rapidly known.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and their concepts should be equivalent or changed within the technical scope of the present invention.
Claims (5)
1. A method for determining a separation paper extract by using an infrared spectroscopy is characterized by comprising the following steps:
preparing a spacer paper extract, cutting a certain amount of spacer paper, assembling an extractor, placing a sample and a reagent correspondingly, and then opening a tap water valve and an electric furnace switch for heating; observing and controlling the water inlet and outlet speed of a condensation water pipe, repeatedly condensing and volatilizing dichloromethane in the extracting solution for many times, and obtaining a partition paper extract after volatilizing;
tabletting, namely putting a proper amount of KBr crystals into an agate mortar for full grinding until no granular sensation exists when sample powder is scratched by a grinding pestle, putting the ground sample into a weighing bottle, drying the sample in an oven, and transferring the sample into a dryer for storage for later use; weighing dried KBr powder, putting the powder into a sample cell of a sample press, pressing by using a tablet press, taking out a KBr sheet, flattening the surface, and packaging by using a self-sealing bag to prevent the KBr sheet from being polluted;
step three, testing, namely utilizing an infrared spectrometer to perform background scanning to obtain a current air background image; uniformly coating a piece of partition paper extract on a reflecting surface of a KBr sheet, repeatedly coating and drying, then placing the KBr sheet on a measuring clamp for fixing, scanning to obtain an infrared absorption spectrogram with an air background subtracted, selecting a marked peak value on the sample image, continuously testing a plurality of samples, identifying each scanned spectrogram peak value, then searching and checking with a spectrum library, further judging the relative difference value of the batch of partition paper corresponding to the functional group by counting the height of the corresponding peak value, and analyzing to obtain the impurity content of the partition paper extract.
2. The method of determining a interleaving paper extract using infrared spectroscopy as claimed in claim 1, wherein: in the third step, the scanning starting wave number is 4000 cm-1The wave number at the end of scanning was 450 cm-1Resolution of 4cm-1Data interval of 1.93cm-1The number of scans was set to 16.
3. The method of determining a interleaving paper extract using infrared spectroscopy as claimed in claim 1, wherein: in the second step, the temperature in the oven is set to be 105 ℃, and the drying time is 4 hours.
4. The method of determining a interleaving paper extract using infrared spectroscopy as claimed in claim 1, wherein: in the second step, the pressure of the tablet press is set to 40 tons, and the pressing time is 30 seconds.
5. The method of determining a interleaving paper extract using infrared spectroscopy as claimed in claim 1, wherein: in the first step, the structure of the assembly extractor is as follows: the flask is positioned at the bottom, the stirring magnetons are positioned in the flask, dichloromethane is contained in the flask, the bottom of the flask is placed on an electric furnace for heating, a sleeve is arranged on the opening of the flask, and the other end of the sleeve is connected with a condensing tube through an adapter; one side of the sleeve is connected with the siphon pipe, the other side of the sleeve is connected with the steam bypass pipe, and two ends of the steam bypass pipe are connected to the lower part and the upper part of the sleeve; the lower part of the condensing pipe is provided with a cooling water inlet, and the upper part of the condensing pipe is provided with a cooling water outlet; the sample is located within the cannula.
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| CN201911140076.3A CN110763647A (en) | 2019-11-20 | 2019-11-20 | Method for determining partition paper extract by using infrared spectroscopy |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103837490A (en) * | 2014-03-12 | 2014-06-04 | 大连民族学院 | Method for detecting oil steam based on infrared spectroscopic analysis |
| CN105044015A (en) * | 2015-06-29 | 2015-11-11 | 郑州翱翔医药科技股份有限公司 | Method for testing content of silicone oil on surface of rubber plug by infrared spectroscopy tabletting method |
-
2019
- 2019-11-20 CN CN201911140076.3A patent/CN110763647A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103837490A (en) * | 2014-03-12 | 2014-06-04 | 大连民族学院 | Method for detecting oil steam based on infrared spectroscopic analysis |
| CN105044015A (en) * | 2015-06-29 | 2015-11-11 | 郑州翱翔医药科技股份有限公司 | Method for testing content of silicone oil on surface of rubber plug by infrared spectroscopy tabletting method |
Non-Patent Citations (2)
| Title |
|---|
| 翟爱华 等: "《粮油及其制品检验》", 31 August 2014, 中国轻工业出版社 * |
| 马佩选 等: "《葡萄酒分析与检验》", 28 February 2017, 中国轻工业出版社 * |
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Application publication date: 20200207 |