CN112945793B - Method and device for detecting content of liquid content in carrier gel - Google Patents

Method and device for detecting content of liquid content in carrier gel Download PDF

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CN112945793B
CN112945793B CN202110339579.4A CN202110339579A CN112945793B CN 112945793 B CN112945793 B CN 112945793B CN 202110339579 A CN202110339579 A CN 202110339579A CN 112945793 B CN112945793 B CN 112945793B
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thermogravimetric
content
gel
liquid content
liquid
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CN112945793A (en
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余玉梅
刘雯
李巧灵
刘秀彩
梁晖
叶仲力
徐建荣
刘泽春
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China Tobacco Fujian Industrial Co Ltd
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    • G01N5/04Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder

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Abstract

The present disclosure provides a method, apparatus, and computer-readable medium for detecting the content of liquid contents in a carrier gel. The method for detecting the content of the liquid content in the carrier liquid gel comprises the following steps: obtaining the gel matrix at a characteristic temperatureThermal weight loss rate W of interval o (ii) a Obtaining the thermogravimetric loss rate W of the liquid content in a characteristic temperature interval PG (ii) a Acquiring the thermogravimetric loss rate W of the carrier gel containing the liquid content in a characteristic temperature interval; calculating the content C of the liquid content in the carrier gel according to the formula PG
Figure DDA0002998806410000011
Wherein the characteristic temperature interval is set so that W PG ‑W o The difference is more than or equal to 70 percent.

Description

Method and device for detecting content of liquid content in carrier liquid gel
Technical Field
The invention relates to the field of material detection, in particular to a method and a device for detecting the content of liquid contents in carrier gel and a computer readable medium.
Background
The application of the cigarette filter stick carrying fragrance in cigarettes is increasing day by day, and the fragrance carrying gel is a novel essence carrier. The fragrance-carrying gel generally comprises a gel matrix and a essence solution, and is obtained by fully mixing the essence solution with the molten gel matrix and then cooling and solidifying.
At present, the loading capacity of the fragrance solution in the fragrance-carrying gel is generally characterized by adopting a raw material weighing method, and an effective method for testing the content of the essence solution in the finished fragrance-carrying gel is lacked.
Disclosure of Invention
Through a great deal of research, the inventor provides an innovative method for detecting the content of the liquid content in the carrier gel, and the method can accurately detect the content of the liquid content in the carrier gel.
In some aspects, the present disclosure provides a method of detecting the amount of liquid content in a carrier gel, the carrier gel containing a gel matrix and liquid content, the method comprising:
-obtaining the thermogravimetric loss rate W of the gel matrix in a characteristic temperature interval o
-obtaining the thermogravimetric loss rate W of the liquid content in a characteristic temperature interval PG
-obtaining the thermogravimetric loss rate W of the carrier gel in a characteristic temperature interval;
-calculating the content C of the liquid content of the carrier gel according to the following formula PG
Figure BDA0002998806390000011
Wherein the characteristic temperature interval is set so that W PG -W o The difference is more than or equal to 70 percent.
In the above aspect, the characteristic temperature interval is set so that W PG -W o The difference of > 70% is critical, and this critical feature makes the method of the present disclosure highly accurate, for example, the average deviation of the test value from the preset value is below 4% as demonstrated in the examples.
In some embodiments, the liquid content is a perfume solution.
In some embodiments, the liquid content comprises propylene glycol.
In some embodiments, the gel matrix contains one or more ingredients: polyethylene glycol 1000, polyethylene glycol 2000, polyethylene glycol 3000, polyethylene glycol 4000, polyethylene glycol 5000, polyethylene glycol 6000 and polyethylene glycol 7000.
In some embodiments, the characteristic temperature interval is set such that W o ≤10%。
In some embodiments, the characteristic temperature interval is set such that W PG ≥80%。
In some embodiments, the thermogravimetric loss rate is determined under the following conditions:
placing 10-50 mg of sample in a thermogravimetric analyzer, and carrying out a thermogravimetric test under a nitrogen atmosphere, wherein the thermogravimetric test comprises the following stages:
(1) the test temperature was raised from room temperature to T1;
(2) the test temperature is increased from T1 to T2, wherein T1 and T2 are respectively the lower temperature limit and the upper temperature limit of the characteristic temperature interval, and the thermogravimetric loss rate of the sample in the characteristic temperature interval is obtained.
Step (1) is arranged to substantially weightless the sample in the temperature interval below T1.
Step (2) is arranged to substantially weightless the sample in the characteristic temperature interval.
In some embodiments, the liquid content is propylene glycol and the characteristic temperature range is 90 to 250 ℃.
In some aspects, the present disclosure provides a device for detecting the content of liquid contents in a carrier gel, comprising:
a memory; and
a processor coupled to the memory, the processor configured to perform the method of measuring porosity of a composite material described above based on instructions stored in the memory device;
preferably, the device for detecting the content of the liquid content in the carrier liquid gel further comprises a thermogravimetric analyzer, and the thermogravimetric analyzer outputs the thermogravimetric loss rate to the storage.
In some aspects, the present disclosure provides a computer-readable storage medium having stored thereon a computer program which, when executed by a processor, implements the method of detecting the liquid content of a carrier gel of claim above.
Description of the terms
The present disclosure, if the following terms are used, may have the following meanings.
The term polyethylene glycol X refers to polyethylene glycol having an average molecular weight in the range of X ± 10%. (1000, 2000, 3000.)
The term "thermogravimetric analysis" refers to a thermal analysis technique that measures the relationship between the mass of a sample to be measured and the change in temperature at a programmed temperature.
The term "carrier gel" refers to a stable system of a cross-linked network of polymeric material (gel matrix) with liquid contents. The carrier gel has a shape and does not flow in a stable state. The carrier liquid gel for the cigarette is solid at normal temperature, can solidify the fragrance components to reduce the release loss of the fragrance components, and can be converted into liquid after the temperature is increased to 40-70 ℃ to realize the release of the fragrance components.
The term "fragrance-bearing gel" is a "carrier gel" in which a fragrance solution is loaded.
Unless otherwise specified,% are mass%.
"thermogravimetric loss rate" refers to the mass loss of a sample during a thermogravimetric test.
Thermogravimetric loss rate (m) 2 -m 1 )/m 0 ,m 1 And m 2 Respectively a first temperature of interest T 1 And a second temperature of interest T 2 Mass of sample (T) 2 >T 1 ),m 0 Is the original mass of the sample before thermogravimetric testing.
Advantageous effects
The technical scheme of the disclosure can have one or more of the following advantages:
(1) the method is simple and easy to operate;
(2) the accuracy of the test result is high, and the average deviation is below 4%;
(3) the method can be popularized and applied to detection and quality monitoring of the loading rate and batch stability of the aroma-carrying gel filter stick.
Drawings
FIG. 1 is a graph of thermogravimetric loss rates of propylene glycol and gel matrix at different stages.
FIG. 2 is a flow chart of a method of detecting the amount of liquid content in a carrier gel according to some embodiments.
FIG. 3 illustrates an apparatus for measuring the amount of liquid contents in a carrier gel according to some embodiments.
Fig. 4 is a schematic diagram of an apparatus for detecting the amount of liquid contents in a carrier gel according to further embodiments.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
1. Preparation of a Carrier gel
Mixing polyethylene glycol 1000, polyethylene glycol 2000 and polyethylene glycol 7000 according to the mass ratio of 7: 8: 5; pouring the mixture into a sol tank, and setting the water bath temperature of the sol tank to be 60 +/-5 ℃. Continuously stirring the gel by using stirring equipment (the rotating speed is set to be 50r/min, and the stirring time is 15-25min) in the sol tank, and after the gel is fully dissolved and uniform, adjusting the water bath temperature to be 55 ℃ to obtain the molten gel matrix.
The liquid content (propylene glycol in this example) is added to the molten gel matrix such that propylene glycol represents the total mass C of the final product 0 %(C 0 10, 20, 30, 40, 50), numbers S1 to S5. And continuously stirring for 10-15min until the molten gel matrix and the propylene glycol are fully and uniformly mixed to obtain the carrier gel.
Ethylene glycol and propylene glycol were provided by Staita chemical Co., Ltd.
2. Determination of a characteristic temperature interval
In order to select the appropriate temperature interval, thermogravimetric analysis was performed on the gel matrix and propylene glycol, respectively.
The thermogravimetric analysis instrument is relaxation-resistant STA449F3, and the thermogravimetric analysis conditions are as follows: nitrogen atmosphere, gas flow rate 20ml/min, one sample load 20 mg.
The temperature program for thermogravimetric analysis comprises the following stages (1) to (5) carried out in sequence:
stage 1: maintaining at 30 deg.C for 5 min;
and (2) stage: heating from 30 ℃ to 90 ℃, wherein the heating rate is 0.5K/min;
and (3) stage: maintaining at 90 deg.C for 10 min;
and (4) stage: heating from 90 ℃ to 250 ℃, wherein the heating rate is 10K/min;
and (5) stage: the temperature is increased from 250 ℃ to 700 ℃, and the heating rate is 20K/min.
The thermogravimetric loss rate of the propylene glycol/gel matrix was monitored separately at each of stages 1 to 5, with the results shown in the following table.
TABLE 1
Figure BDA0002998806390000051
Figure 1 shows the thermogravimetric loss rate of propylene glycol and gel matrix at different stages.
As can be seen from Table 1, in stage 4, i.e., the temperature increased from 90 ℃ to 250 ℃, the thermogravimetric loss W of propylene glycol was observed PG % of 84.02%, thermal weight loss W of gel matrix PG % is 4.78%, the difference is 79.25%, and the difference is more than or equal to 70%. Therefore, the temperature rise stage of 90-250 ℃ is selected as the characteristic temperature interval for subsequent use in the embodiment.
3. Determination of the propylene glycol content of a carrier gel
Thermogravimetric analysis is carried out on the prepared carrier gel samples S1-S5, wherein a thermogravimetric analysis instrument is relaxation-resistant STA449F3, and the thermogravimetric analysis conditions are as follows: nitrogen atmosphere, gas flow rate 20ml/min, one sample load 20 mg.
The temperature program for thermogravimetric analysis comprises the following stages (1) to (4) carried out in sequence:
stage 1: maintaining at 30 deg.C for 5 min;
and (2) stage: heating from 30 ℃ to 90 ℃, wherein the heating rate is 0.5K/min;
and (3) stage: maintaining at 90 deg.C for 10 min;
and (4) stage: heating from 90 ℃ to 250 ℃, wherein the heating rate is 10K/min;
and collecting the thermogravimetric loss rate W% of the carrier liquid gel sample in a characteristic temperature interval (namely, stage 4, 90-250 ℃).
Calculating the carrier fluid gel according toContent of medium-liquid content C PG
Figure BDA0002998806390000052
The calculation results are shown in the following table.
TABLE 2
Figure BDA0002998806390000053
Figure BDA0002998806390000061
Calculation of deviation (| (predicted value-set value)/set value-
As can be seen from the above table, the average deviation of the predicted propylene glycol content value obtained by the measurement of the invention and the set value is not more than 4%.
It should be noted that, although propylene glycol is used as the liquid content in the above examples, it is understood by those skilled in the art that the content of the liquid content in the liquid-containing gel can also be obtained by the method of the present invention through the liquid content of other components, such as a perfume solution, for example, a perfume solution using propylene glycol as a solvent.
FIG. 2 is a flow chart of a method for detecting the amount of liquid content in a carrier gel. As shown in fig. 2, a method for detecting the content of liquid contents in carrier gel comprises:
s101, acquiring the thermogravimetric loss rate W of the gel matrix in a characteristic temperature interval o
S102, acquiring the thermogravimetric loss rate W of the liquid content in a characteristic temperature interval PG
S103, acquiring the thermogravimetric loss rate W of the carrier liquid gel in a characteristic temperature interval;
s104, calculating the content C of the liquid content in the carrier liquid gel according to the following formula PG
Figure BDA0002998806390000062
Wherein the characteristic temperature interval is set so that W PG -W O The difference value of the two is more than or equal to 70 percent.
FIG. 3 shows a schematic of some devices for measuring the amount of liquid contents in a carrier gel.
As shown in fig. 3, the apparatus 7 for detecting the content of the liquid content in the carrier liquid gel of this embodiment includes: a memory 71 and a processor 72 coupled to the memory 71, the processor 72 being configured to perform a method of detecting the content of a liquid content in a carrier fluid gel according to any one of the embodiments of the present disclosure, based on instructions stored in the memory 71.
The memory 71 may include, for example, a system memory, a fixed nonvolatile storage medium, and the like. The system memory stores, for example, an operating system, an application program, a Boot Loader (Boot Loader), a database, and other programs.
FIG. 4 is a schematic diagram of still another apparatus for detecting the amount of liquid contents in a carrier gel.
As shown in fig. 4, the apparatus 8 for detecting the content of the liquid content in the carrier liquid gel of this embodiment includes: a memory 810 and a processor 820 coupled to the memory 810, the processor 820 being configured to perform the method of detecting the content of the liquid content in the carrier gel according to any of the embodiments described above based on instructions stored in the memory 810.
Memory 810 may include, for example, system memory, fixed non-volatile storage media, and the like. The system memory stores, for example, an operating system, an application program, a Boot Loader (Boot Loader), and other programs.
The device 8 for detecting the content of the liquid content in the carrier gel may further include an input/output interface 830, a network interface 840, a storage interface 850, and the like. These interfaces 830, 840, 850, and the memory 810 and the processor 820 may be connected by a bus 860, for example. The input/output interface 830 provides a connection interface for input/output devices such as a display, a mouse, a keyboard, and a touch screen. Network interface 840 provides a connection interface for a variety of networking devices. The storage interface 850 provides a connection interface for external storage devices such as an SD card and a usb disk.
As will be appreciated by one skilled in the art, embodiments of the present disclosure may be provided as a method, system, or computer program product. Accordingly, the present disclosure may take the form of an entirely hardware embodiment, an entirely software embodiment or an embodiment combining software and hardware aspects. Furthermore, the present disclosure may take the form of a computer program product embodied on one or more computer-usable non-transitory storage media (including, but not limited to, disk storage, CD-ROM, optical storage, and so forth) having computer-usable program code embodied therein.
Thus far, a method of detecting the amount of liquid content in a carrier gel, an apparatus for detecting the amount of liquid content in a carrier gel, and a computer-readable storage medium according to the present disclosure have been described in detail. Some details well known in the art have not been described in order to avoid obscuring the concepts of the present disclosure. It will be fully apparent to those skilled in the art from the foregoing description how to practice the presently disclosed embodiments.
The method and system of the present disclosure may be implemented in a number of ways. For example, the methods and systems of the present disclosure may be implemented by software, hardware, firmware, or any combination of software, hardware, and firmware. The above-described order for the steps of the method is for illustration only, and the steps of the method of the present disclosure are not limited to the order specifically described above unless specifically stated otherwise. Further, in some embodiments, the present disclosure may also be embodied as programs recorded in a recording medium, the programs including machine-readable instructions for implementing the methods according to the present disclosure. Thus, the present disclosure also covers a recording medium storing a program for executing the method according to the present disclosure.
Although some specific embodiments of the present disclosure have been described in detail by way of example, it should be understood by those skilled in the art that the foregoing examples are for purposes of illustration only and are not intended to limit the scope of the present disclosure. It will be appreciated by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the present disclosure. The scope of the present disclosure is defined by the appended claims.

Claims (11)

1. A method of detecting the amount of liquid content in a carrier gel comprising a gel matrix and liquid content, the method comprising:
-obtaining the thermogravimetric loss W of the gel matrix in a characteristic temperature interval o
-obtaining the thermogravimetric loss rate W of the liquid content in the characteristic temperature interval PG
-obtaining the thermogravimetric loss W of the carrier gel in said characteristic temperature interval;
-calculating the content C of the liquid content of the carrier gel according to the following formula PG
Figure FDA0003730553150000011
Wherein the characteristic temperature interval is set so that W PG -W o The difference value is more than or equal to 70 percent;
wherein the thermogravimetric loss rate is obtained by measuring under the following conditions:
placing 10-50 mg of sample in a thermogravimetric analyzer, and carrying out a thermogravimetric test under a nitrogen atmosphere, wherein the thermogravimetric test comprises the following stages:
(1) the test temperature is raised from room temperature to T 1
(2) Test temperature from T 1 Is raised to T 2 Wherein T is 1 And T 2 Respectively obtaining the thermogravimetric loss rate of the sample in the characteristic temperature interval by the lower temperature limit and the upper temperature limit of the characteristic temperature interval.
2. The method of claim 1, wherein the liquid content is a perfume solution.
3. The method of claim 1, wherein the liquid content comprises propylene glycol.
4. The method of claim 1, wherein the gel matrix contains one or more ingredients: polyethylene glycol 1000, polyethylene glycol 2000, polyethylene glycol 3000, polyethylene glycol 4000, polyethylene glycol 5000, polyethylene glycol 6000 and polyethylene glycol 7000.
5. The method according to claim 1, wherein the characteristic temperature interval is set such that W o ≤10%。
6. The method according to claim 1, wherein the characteristic temperature interval is set such that W PG ≥80%。
7. The method of claim 1, wherein the liquid content is propylene glycol and the characteristic temperature range is 90-250 ℃.
8. The method of claim 1, wherein the thermogravimetric loss ratio is determined under the following conditions: placing 10-50 mg of sample in a thermogravimetric analyzer, and carrying out a thermogravimetric test under a nitrogen atmosphere, wherein the thermogravimetric test comprises the following stages:
stage 1: maintaining at 30 deg.C for 5 min;
and (2) stage: heating from 30 ℃ to 90 ℃, wherein the heating rate is 0.5K/min;
and (3) stage: maintaining at 90 deg.C for 10 min;
and (4) stage: the temperature is increased from 90 ℃ to 250 ℃, and the heating rate is 10K/min.
9. An apparatus for detecting the amount of liquid content in a carrier gel, comprising:
a memory; and
a processor coupled to the memory, the processor being configured to perform the method of detecting the content of liquid contents in a carrier gel of any one of claims 1-8 based on instructions stored in the memory device.
10. The apparatus of claim 9, wherein said means for detecting the liquid content of the carrier liquid gel further comprises a thermogravimetric analyzer, said thermogravimetric analyzer outputting the thermogravimetric loss of the sample to the reservoir.
11. A computer-readable storage medium, on which a computer program is stored which, when being executed by a processor, carries out the method for detecting the content of a liquid content in a carrier gel according to any one of claims 1 to 8.
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