CN109239105B - Millimeter wave method for identifying phase of glycerol monooleate - Google Patents
Millimeter wave method for identifying phase of glycerol monooleate Download PDFInfo
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- CN109239105B CN109239105B CN201811094082.5A CN201811094082A CN109239105B CN 109239105 B CN109239105 B CN 109239105B CN 201811094082 A CN201811094082 A CN 201811094082A CN 109239105 B CN109239105 B CN 109239105B
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- glycerol monooleate
- millimeter wave
- water content
- phase
- monooleate
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- RZRNAYUHWVFMIP-KTKRTIGZSA-N 1-oleoylglycerol Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(O)CO RZRNAYUHWVFMIP-KTKRTIGZSA-N 0.000 title claims abstract description 79
- RZRNAYUHWVFMIP-HXUWFJFHSA-N glycerol monolinoleate Natural products CCCCCCCCC=CCCCCCCCC(=O)OC[C@H](O)CO RZRNAYUHWVFMIP-HXUWFJFHSA-N 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 65
- 238000012360 testing method Methods 0.000 claims abstract description 34
- 230000005540 biological transmission Effects 0.000 claims abstract description 10
- 238000001028 reflection method Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000000263 2,3-dihydroxypropyl (Z)-octadec-9-enoate Substances 0.000 abstract description 10
- RZRNAYUHWVFMIP-GDCKJWNLSA-N 3-oleoyl-sn-glycerol Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@H](O)CO RZRNAYUHWVFMIP-GDCKJWNLSA-N 0.000 abstract description 10
- RZRNAYUHWVFMIP-UHFFFAOYSA-N monoelaidin Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(O)CO RZRNAYUHWVFMIP-UHFFFAOYSA-N 0.000 abstract description 10
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization 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
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- 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 Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
A millimeter wave method for identifying the phase of glycerol monooleate is disclosed: calibrating the millimeter wave test system to the rectangular waveguide port; filling millimeter wave rectangular waveguide slices with glycerol monooleate with known water content, and clamping the slices by using a waveguide port; testing the S parameter of the sheet, and extracting the complex dielectric constant of the glycerol monooleate by using a transmission reflection method; inputting the test result into a database; washing the sheet, replacing the sheet with glycerol monooleate with different water contents until the complex dielectric constants of the glycerol monooleate with different water contents are completely obtained, filling the sheet with the glycerol monooleate with unknown water content, clamping the sheet by using a waveguide port, testing S parameters, and extracting the complex dielectric constant of the glycerol monooleate by using a transmission reflection method; and comparing the obtained complex dielectric constant with data in a database to obtain the water content of the glyceryl monooleate, so as to obtain the phase and the structure of the glyceryl monooleate with unknown water content. The invention provides a basis for the application of the glycerol monooleate in industrial production.
Description
Technical Field
The invention relates to a macromolecular material structure identification. In particular to a millimeter wave method for identifying the phase of glycerol monooleate.
Background
In the past decades, glyceryl monooleate has found widespread use in areas such as drug delivery, emulsion stabilization, and protein crystallization. Glycerol monooleate has a variety of molecular structures, such as lamellar, tubular, spherical and more complex structures, which are defined as distinct phases. The glyceryl monooleate with different phases has different application values, so that the identification of the phases is of great significance in the actual industrial production.
It has been shown that the phase of glycerol monooleate is determined primarily by the water content. As shown in fig. 1, the horizontal axis of fig. 1 shows water content, and the vertical axis shows temperature. Lamellarcrystalline stands for lamellar crystals, Lamellar Liquid crystals for lamellar liquid crystals, Cubic-Pn3m stands for Cubic-Pn3m crystals, and Cubic-la3d stands for Cubic-la3d crystals.
Therefore, identification of moisture content is an important means of identifying phase. It is well known that millimeter waves have very large losses in water, which can be characterized by the imaginary part of the complex dielectric constant. Therefore, the water content of glycerol monooleate can be identified by testing the millimeter wave complex dielectric constant of the extracted glycerol monooleate.
Disclosure of Invention
The invention aims to solve the technical problem of providing a millimeter wave method for identifying the phase of glyceryl monooleate, which can determine the water content and the phase of the glyceryl monooleate.
The technical scheme adopted by the invention is as follows: a millimeter wave method for identifying the phase of glycerol monooleate comprises the following steps:
1) calibrating the millimeter wave test system to the rectangular waveguide port;
2) filling the millimeter wave rectangular waveguide sheet with glycerol monooleate with known water content, and clamping the millimeter wave rectangular waveguide sheet filled with the glycerol monooleate by using the calibrated waveguide port;
3) testing the S parameter of the filling of the glycerol monooleate slices;
4) extracting the complex dielectric constant of the glycerol monooleate by using a transmission reflection method according to the S parameter;
5) inputting the test result into a test database;
6) washing away the glycerol monooleate in the millimeter wave rectangular waveguide sheet by using deionized water, replacing the glycerol monooleate with different water contents, repeating the steps 2) to 5) until the complex dielectric constants of the set number of glycerol monooleate with different water contents are obtained, and entering the next step;
7) filling the millimeter wave rectangular waveguide sheet with glycerol monooleate with unknown water content, clamping the millimeter wave rectangular waveguide sheet filled with the glycerol monooleate with unknown water content by using a calibrated waveguide port, testing S parameters, and extracting the complex dielectric constant of the glycerol monooleate by using a transmission reflection method according to the S parameters;
8) and comparing the obtained complex dielectric constant with data in a test database to obtain the water content of the glycerol monooleate with unknown water content, and obtaining the phase and the structure of the glycerol monooleate with unknown water content according to the relation between the water content and the phase.
The millimeter waves in the step 1) are millimeter waves in the frequency ranges of 90-140GHz, 140-220 GHz and 220-330 GHz.
Step 5), testing the coverage range of the water content of the database: 0 to 75 percent.
According to the millimeter wave method for identifying the phase of the glyceryl monooleate, the characteristic that the millimeter wave has large loss in water is applied for the first time, the water content of the glyceryl monooleate is identified, the phase of the glyceryl monooleate is identified by combining the relation between the water content and the phase, the structure is further identified, and a basis is provided for the application of the glyceryl monooleate to industrial production.
Drawings
FIG. 1 is a graph of water content versus phase for glycerol monooleate;
FIG. 2 is a flow chart of a millimeter wave method for identifying the phase of glycerol monooleate of the present invention;
FIG. 3a is S11Amplitude and phase maps;
FIG. 3b is S21Amplitude and phase maps;
FIG. 4 is a graph of complex dielectric constant extracted according to an embodiment of the present invention.
Detailed Description
The millimeter wave method for identifying the phase of glycerol monooleate according to the invention is described in detail below with reference to the following embodiments and the accompanying drawings.
As shown in fig. 2, the millimeter wave method for identifying the phase of glycerol monooleate of the present invention includes the following steps:
1) calibrating a millimeter wave test system to a rectangular waveguide port, wherein the millimeter waves are millimeter waves in the frequency ranges of 90-140GHz, 140-220 GHz and 220-330 GHz;
2) filling millimeter wave rectangular waveguide slices with glycerol monooleate with known water content, wherein the glycerol monooleate is colloid and has a plastic shape, so that rectangular waveguide ports are convenient to fill, and then clamping the millimeter wave rectangular waveguide slices filled with the glycerol monooleate by using the calibrated waveguide ports;
3) testing the S parameter of the filling of the glycerol monooleate slices;
4) extracting the complex dielectric constant of the glycerol monooleate by using a transmission reflection method according to the S parameter;
5) inputting the test result into a test database, wherein the water content coverage range of the test database is as follows: 0% -75%;
6) washing away the glycerol monooleate in the millimeter wave rectangular waveguide sheet by using deionized water, replacing the glycerol monooleate with different water contents, repeating the steps 2) to 5) until the complex dielectric constants of the set number of glycerol monooleate with different water contents are obtained, and entering the next step;
7) filling the millimeter wave rectangular waveguide sheet with glycerol monooleate with unknown water content, clamping the millimeter wave rectangular waveguide sheet filled with the glycerol monooleate with unknown water content by using a calibrated waveguide port, testing S parameters, and extracting the complex dielectric constant of the glycerol monooleate by using a transmission reflection method according to the S parameters;
8) and comparing the obtained complex dielectric constant with data in a test database to obtain the water content of the glycerol monooleate with unknown water content, and obtaining the phase and the structure of the glycerol monooleate with unknown water content according to the relation between the water content and the phase.
In the frequency range of 90-140GHz, the glycerol monooleate with the water content of 30%, 35% and 45% is taken as three glycerol monooleate with unknown water content, so as to find out the water content of the glycerol monooleate with three water contents, and thus the millimeter wave method for identifying the phase of the glycerol monooleate is verified.
1. Calibrating a 90-140GHz millimeter wave test system to a rectangular waveguide port;
2. filling 1 kind of glycerol monooleate with known water content in a millimeter wave rectangular waveguide slice, and clamping the millimeter wave rectangular waveguide slice by using a calibrated waveguide port;
3. testing the S parameter of the millimeter wave rectangular waveguide filled with the glycerol monooleate;
4. extracting the complex dielectric constant of the glycerol monooleate by using a transmission reflection method according to the S parameter;
5. recording the test result into a test database (the coverage range of the water content of the database is 0-75%);
6. washing away the glycerol monooleate in the millimeter wave rectangular waveguide sheet by using deionized water, replacing the glycerol monooleate with different water contents, repeating the steps 2, 3, 4 and 5 until the complex dielectric constants of the set number of glycerol monooleate with different water contents are obtained, and entering the next step;
7. respectively filling the slices with 30%, 35% and 45% water content glycerol monooleate, respectively testing the S parameters (see fig. 3a and 3b), and respectively extracting the complex dielectric constants (see fig. 4) of the glycerol monooleate with three water contents by using a transmission reflection method according to the S parameters of the glycerol monooleate with three water contents;
8. and comparing the complex dielectric constants of the glycerol monooleate with three water contents with the data of a test database to obtain the water contents of the glycerol monooleate with the three water contents of 30%, 35% and 45%, and identifying the phase and the structure of the glycerol monooleate by combining the relationship between the water contents and the phase. The identification result is true and effective.
In conclusion, the glycerol monooleate with different water contents can be effectively identified by testing and extracting the 90-140GHz complex dielectric constant of the glycerol monooleate. Combining this property, the phase and structure of glycerol monooleate can be identified from the test database.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (3)
1. A millimeter wave method for identifying the phase of glycerol monooleate is characterized by comprising the following steps:
1) the millimeter wave test system is connected with the rectangular waveguide port in a calibration mode;
2) filling the millimeter wave rectangular waveguide sheet with glycerol monooleate with known water content, and clamping the millimeter wave rectangular waveguide sheet filled with the glycerol monooleate by using the calibrated waveguide port;
3) testing the S parameter of the filling of the glycerol monooleate slices;
4) extracting the complex dielectric constant of the glycerol monooleate by using a transmission reflection method according to the S parameter;
5) inputting the test result into a test database;
6) washing away the glycerol monooleate in the millimeter wave rectangular waveguide sheet by using deionized water, replacing the glycerol monooleate with different water contents, repeating the steps 2) to 5) until the complex dielectric constants of the set number of glycerol monooleate with different water contents are obtained, and entering the next step;
7) filling the millimeter wave rectangular waveguide sheet with glycerol monooleate with unknown water content, clamping the millimeter wave rectangular waveguide sheet filled with the glycerol monooleate with unknown water content by using a calibrated waveguide port, testing S parameters, and extracting the complex dielectric constant of the glycerol monooleate by using a transmission reflection method according to the S parameters;
8) and comparing the obtained complex dielectric constant with data in a test database to obtain the water content of the glycerol monooleate with unknown water content, and obtaining the phase and the structure of the glycerol monooleate with unknown water content according to the relation between the water content and the phase.
2. The millimeter wave method for identifying the phase of glycerol monooleate as claimed in claim 1, wherein the millimeter waves in the step 1) are millimeter waves in the frequency ranges of 90-140GHz, 140-220 GHz and 220-330 GHz.
3. The millimeter wave method for identifying the phase of glycerol monooleate according to claim 1, wherein the test database of step 5) has a water content coverage range of: 0 to 75 percent.
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