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

Abstract

The present disclosure provides a method, apparatus and computer-readable medium for detecting the content of liquid content in a carrier liquid gel. Wherein, the method for detecting the content of liquid content in the carrier liquid gel includes: obtaining the thermogravimetric loss rate W _o of the gel matrix in the characteristic temperature range; obtaining the thermogravimetric loss rate W _PG of the liquid content in the characteristic temperature range; The thermogravimetric loss rate W of the carrier liquid gel with liquid content in the characteristic temperature range; calculate the content of liquid content C _PG in the carrier liquid gel according to the following formula:

Wherein, the characteristic temperature interval is set such that the difference between W _PG -W _o is ≥70%.

Description

Method and device for detecting liquid content in carrier liquid gel

technical field

The invention relates to the field of material detection, in particular to a method, a device and a computer-readable medium for detecting the content of liquid content in a carrier liquid gel.

Background technique

The application of filter stick aroma in cigarettes is increasing day by day, and aroma-loading gel is a new type of flavor carrier. The fragrance-carrying gel generally includes a gel matrix and a fragrance solution. The fragrance-carrying gel is obtained by fully mixing the fragrance solution with the molten gel matrix and then cooling and solidifying.

At present, the loading of the fragrance solution in the fragrance-carrying gel is generally characterized by the raw material weighing method, and there is currently no effective method for testing the content of the fragrance solution in the finished fragrance-carrying gel.

SUMMARY OF THE INVENTION

After extensive research, the inventor has proposed an innovative method for detecting the content of liquid content in the carrier liquid gel, which can accurately detect the content of the liquid content in the carrier liquid gel.

In some aspects, the present disclosure provides a method of detecting liquid content content in a carrier liquid gel, the carrier liquid gel containing a gel matrix and liquid content, the method comprising:

- Obtain the thermogravimetric loss rate W _o of the gel matrix in the characteristic temperature range;

- Obtain the thermogravimetric loss rate W _PG of the liquid content in the characteristic temperature range;

- Obtain the thermogravimetric loss rate W of the carrier liquid gel in the characteristic temperature range;

- Calculate the content of liquid content _CPG in the carrier gel according to the formula:

Wherein, the characteristic temperature interval is set such that the difference between W _PG -W _o is ≥70%.

In the above scheme, it is critical to set the characteristic temperature interval such that the difference between W _PG -W _o ≥ 70%, this key feature makes the measurement accuracy of the method of the present disclosure very high. The average deviation of the value from the preset value is 4% or less.

In some embodiments, the liquid content is a fragrance solution.

In some embodiments, the liquid content includes propylene glycol.

In some embodiments, the gel matrix contains one or more components: polyethylene glycol 1000, polyethylene glycol 2000, polyethylene glycol 3000, polyethylene glycol 4000, polyethylene glycol 5000, polyethylene glycol Ethylene glycol 6000, 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 _WPG > 80%.

In some embodiments, the thermogravimetric loss rate is determined under the following conditions:

Place 10-50 mg of sample in a thermogravimetric analyzer, and conduct thermogravimetric test under nitrogen atmosphere. The thermogravimetric test includes the following stages:

(1) The test temperature is raised from room temperature to T1;

(2) The test temperature is increased from T1 to T2, where T1 and T2 are the lower temperature limit and the upper temperature limit of the characteristic temperature interval, respectively, and the thermogravimetric loss rate of the sample in the characteristic temperature interval is obtained.

Step (1) is set so that the sample is sufficiently weightless in the temperature range below T1.

Step (2) is set so that the sample is sufficiently weightless in the characteristic temperature range.

In some embodiments, the liquid content is propylene glycol, and the characteristic temperature range is 90-250°C.

In some aspects, the present disclosure provides a device for detecting the content of liquid content in a carrier liquid gel, comprising:

memory; and

a processor coupled to the memory, the processor configured to perform the above-described method of measuring composite porosity based on instructions stored in the memory device;

Preferably, the device for detecting the content of 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 on which a computer program is stored, the program, when executed by a processor, implements the method for detecting the content of liquid content in a carrier gel as claimed in the preceding claims.

Glossary

If the following terms are used in this disclosure, they may have the following meanings.

The term polyethylene glycol X refers to polyethylene glycols having an average molecular weight in the range of X±10%. (X=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 tested and the change in temperature at a programmed temperature.

The term "carrier gel" refers to a stable system formed by a cross-linked network of polymeric materials (gel matrix) and liquid contents. The carrier gel has a certain shape in the stable state and does not flow. For the liquid carrier gel for cigarettes, it is solid at room temperature, which can solidify the aroma components and reduce the release loss of the aroma components. After the temperature rises to 40-70 °C, the gel can be converted into a liquid to realize the release of the aroma components.

The term "fragrance-loaded gel" is a "carrier gel" in which a fragrance solution is loaded.

Unless otherwise specified, % is 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 , where m ₁ and m ₂ are the mass of the sample at the first temperature of interest T ₁ and the second temperature of interest T ₂ (T ₂ >T ₁ ), respectively, m ₀ is the original mass of the sample before thermogravimetric testing.

beneficial effect

The technical solutions of the present disclosure may have one or more of the following advantages:

(1) The method is simple and easy to operate;

(2) The accuracy of the test results is high, and the average deviation is below 4%;

(3) It can be widely used in the detection and quality monitoring of the loading rate and batch stability of scented gel filter rods.

Description of drawings

Figure 1 is a histogram of the thermogravimetric loss rate of propylene glycol and gel matrix at different stages.

FIG. 2 is a flowchart of a method for detecting the content of liquid content in a carrier liquid gel according to some embodiments.

FIG. 3 is a device for detecting the content of liquid content in a carrier liquid gel according to some embodiments.

FIG. 4 is a device for detecting the content of liquid content in a carrier liquid gel according to further embodiments.

Detailed ways

The embodiments of the present invention will be described in detail below with reference to the examples, but those skilled in the art will understand that the following examples are only used to illustrate the present invention, and should not be regarded as limiting the scope of the present invention. If the specific conditions are not indicated in the examples, it is carried out according to the conventional conditions or the conditions suggested by the manufacturer. The reagents or instruments used without the manufacturer's indication are conventional products that can be obtained from the market.

1. Preparation of carrier gel

Mix polyethylene glycol 1000, polyethylene glycol 2000, and polyethylene glycol 7000 in a mass ratio of 7:8:5; pour the mixture into a sol tank, and set the water bath temperature of the sol tank to 60±5°C. Use the stirring equipment in the sol tank (rotation speed is set to 50r/min, stirring for 15-25min) to continuously stir the gel. After the gel is fully dissolved and uniform, the temperature of the water bath is lowered to 55°C to obtain a molten gel matrix.

Add liquid content (the liquid content in this example is propylene glycol) to the molten gel matrix, so that propylene glycol accounts for C ₀ % of the total mass of the final product (C ₀ =10, 20, 30, 40, 50), numbered S1 to S5. Continue stirring for 10-15min until the molten gel matrix and propylene glycol are fully mixed to obtain a carrier liquid gel.

Ethylene glycol and propylene glycol were provided by Wuxi Yatai United Chemical Co., Ltd.

2. Determination of characteristic temperature range

In order to select a suitable temperature range, thermogravimetric analysis of the gel matrix and propylene glycol was performed separately.

The thermogravimetric analysis instrument was NETZSCH STA449F3, and the thermogravimetric analysis conditions were: nitrogen atmosphere, gas flow rate 20 ml/min, and a sample loading amount of 20 mg.

The temperature program of thermogravimetric analysis includes the following stages (1) to (5) in sequence:

Stage 1: 30°C for 5min;

Stage 2: from 30 to 90 °C, the heating rate is 0.5K/min;

Stage 3: 90°C for 10min;

Stage 4: from 90 to 250 °C, the heating rate is 10K/min;

Stage 5: From 250 to 700°C, the temperature rise rate is 20K/min.

The thermogravimetric loss rate of the propylene glycol/gel matrix was monitored separately at each stage from stage 1 to stage 5 and the results are shown in the table below.

Table 1

Figure 1 shows the thermogravimetric loss rates of propylene glycol and gel matrix at different stages.

From Table 1, it can be seen that in stage 4, that is, the stage of heating from 90 ° C to 250 ° C, the thermogravimetric loss rate W _PG % of propylene glycol is 84.02%, and the thermogravimetric loss rate W _PG % of the gel matrix is 4.78%, both. The difference is 79.25%, and this difference is ≥70%. Therefore, the temperature rising stage of 90-250° C. is selected as the characteristic temperature range used subsequently in this embodiment.

3. Determination of propylene glycol content in carrier liquid gel

The carrier liquid gel samples S1 to S5 prepared above were subjected to thermogravimetric analysis. The thermogravimetric analysis instrument was NETZSCH STA449F3. The thermogravimetric analysis conditions were: nitrogen atmosphere, gas flow rate 20ml/min, and a sample loading amount of 20mg.

The temperature program of thermogravimetric analysis includes the following stages (1) to (4) in sequence:

Stage 1: 30°C for 5min;

Stage 2: from 30 to 90 °C, the heating rate is 0.5K/min;

Stage 3: 90°C for 10min;

Stage 4: from 90 to 250 °C, the heating rate is 10K/min;

The thermogravimetric loss rate W% of the carrier liquid gel sample in the characteristic temperature range (ie, stage 4, 90-250°C) was collected.

Calculate the content of liquid content _CPG in the carrier gel according to the following formula:

The calculation results are shown in the table below.

Table 2

*Deviation = (|(predicted value - set value)/set value|

It can be seen from the above table that the average deviation between the predicted value of the propylene glycol content obtained by the measurement of the present 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 embodiment, those skilled in the art can understand that the liquid content of other components, such as the essence solution, such as the essence solution using propylene glycol as a solvent, can also The content of liquid content in the liquid-containing gel is obtained by the method of the present invention.

FIG. 2 is a flow chart of a method for detecting the content of liquid content in a carrier liquid gel. As shown in Figure 2, a method for detecting the content of liquid content in a carrier liquid gel includes:

S101 obtains the thermogravimetric loss rate W _o of the gel matrix in the characteristic temperature range;

S102 obtains the thermogravimetric loss rate _WPG of the liquid content in the characteristic temperature range;

S103 obtains the thermogravimetric loss rate W of the carrier liquid gel in the characteristic temperature range;

S104 calculates the content _CPG of the liquid content in the carrier liquid gel according to the following formula:

Wherein, the characteristic temperature interval is set such that the difference of W _{PG -WO} ≥ 70%.

FIG. 3 is a schematic diagram of some devices for detecting the content of liquid content in the carrier liquid gel.

As shown in FIG. 3 , the device 7 for detecting the content of liquid content in the carrier liquid gel in this embodiment includes: a memory 71 and a processor 72 coupled to the memory 71 , and the processor 72 is configured to be based on the storage in the memory 71 . , execute the method for detecting the content of liquid content in a carrier liquid gel in any one of the embodiments of the present disclosure.

Wherein, the memory 71 may include, for example, a system memory, a fixed non-volatile 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 other devices for detecting the content of liquid content in the carrier liquid gel.

As shown in FIG. 4 , the device 8 for detecting the content of liquid content in a carrier liquid gel in this embodiment includes: a memory 810 and a processor 820 coupled to the memory 810 , and the processor 820 is configured to be based on the storage in the memory 810 The instruction in any one of the foregoing embodiments is executed to detect the content of liquid content in the carrier liquid gel.

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 liquid content in the carrier liquid gel may further include an input and 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, for example, through a bus 860 . The input and output interface 830 provides a connection interface for input and output devices such as a display, a mouse, a keyboard, and a touch screen. Network interface 840 provides a connection interface for various networked devices. The storage interface 850 provides a connection interface for external storage devices such as SD cards and U disks.

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, etc.) having computer-usable program code embodied therein .

So far, the method for detecting the content of liquid content in the carrier gel, the device for detecting the content of the liquid content in the carrier gel, and the computer-readable storage medium according to the present disclosure have been described in detail. Some details that are well known in the art are not described in order to avoid obscuring the concept of the present disclosure. Those skilled in the art can fully understand how to implement the technical solutions disclosed herein based on the above description.

The methods and systems of the present disclosure may be implemented in many ways. For example, the methods and systems of the present disclosure may be implemented in software, hardware, firmware, or any combination of software, hardware, and firmware. The above-described order of steps for 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. Furthermore, in some embodiments, the present disclosure can also be implemented as programs recorded in a recording medium, the programs including machine-readable instructions for implementing 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.

While some specific embodiments of the present disclosure have been described in detail by way of examples, those skilled in the art will appreciate that the above examples are provided for illustration only, and are not intended to limit the scope of the present disclosure. Those skilled in the art will appreciate 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 for detecting the content of liquid content in a carrier liquid gel, the carrier liquid gel contains a gel matrix and a liquid content, the method comprising: - Obtain the thermogravimetric loss rate W _o of the gel matrix in the characteristic temperature range; - obtaining the thermogravimetric loss rate W _PG of the liquid content in the characteristic temperature range; - obtaining the thermogravimetric loss rate W of the carrier liquid gel in the characteristic temperature range; - Calculate the content of liquid content _CPG in the carrier gel according to the formula:

Wherein, the characteristic temperature interval is set so that the difference between W _PG -W _o ≥ 70%; Wherein, the thermogravimetric loss rate is measured and obtained under the following conditions: Place 10-50 mg of sample in a thermogravimetric analyzer, and conduct thermogravimetric test under nitrogen atmosphere. The thermogravimetric test includes the following stages: (1) The test temperature is raised from room temperature to T ₁ ; (2) The test temperature is increased from T ₁ to T ₂ , where T ₁ and T ₂ are the lower temperature limit and the upper temperature limit of the characteristic temperature interval, respectively, and the thermogravimetric loss rate of the sample in the characteristic temperature interval is obtained. 2. The method of claim 1, wherein the liquid content is a fragrance solution. 3. The method of claim 1, wherein the liquid content comprises propylene glycol. 4. The method according to claim 1, wherein the gel matrix contains one or more components: polyethylene glycol 1000, polyethylene glycol 2000, polyethylene glycol 3000, polyethylene glycol 4000, Macrogol 5000, Macrogol 6000, Macrogol 7000. 5. The method of claim 1, wherein the characteristic temperature interval is set such that W _o ≤ 10%. 6. The method of claim 1, wherein the characteristic temperature interval is set such that _WPG > 80%. 7. The method of claim 1, wherein the liquid content is propylene glycol, and the characteristic temperature range is 90-250°C. 8. The method according to claim 1, wherein, the thermogravimetric loss rate is measured and obtained under the following conditions: placing a 10-50 mg sample in a thermogravimetric analyzer, carrying out a thermogravimetric test under a nitrogen atmosphere, and the thermogravimetric test Includes the following stages: Stage 1: 30°C for 5min; Stage 2: from 30 to 90 °C, the heating rate is 0.5K/min; Stage 3: 90°C for 10min; Stage 4: From 90 to 250°C, the temperature rise rate is 10K/min. 9. A device for detecting the content of liquid content in a carrier liquid gel, comprising: memory; and A processor coupled to the memory, the processor configured to perform the detection of liquid content in a liquid carrier gel according to any one of claims 1-8 based on instructions stored in the memory device Methods. 10 . The device according to claim 9 , wherein the device for detecting the content of liquid content in the carrier liquid gel further comprises a thermogravimetric analyzer, and the thermogravimetric analyzer outputs the sample thermogravimetric loss rate to the storage. 11 . 11. A computer-readable storage medium having a computer program stored thereon, and when the program is executed by a processor, implements the method for detecting the content of liquid content in a liquid carrier gel according to any one of claims 1-8.

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