CN110988021B - Heat value detection sample loading device and food self-heating bag detection method - Google Patents
Heat value detection sample loading device and food self-heating bag detection method Download PDFInfo
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Abstract
The invention relates to the field of material detection, in particular to a heat value detection sample loading device and a food self-heating bag detection method. Meanwhile, the detection method for applying the heat value detection device to the food self-heating bag is optimized and perfected, the bottlenecks that the existing detection method special for the food self-heating bag is lacked, the heat efficiency evaluation subjectivity is strong, and the industrial requirements are difficult to meet are broken through, and the special device, the quality evaluation scientific method and the technical support can be provided for the safe production and use of the self-heating food heating bag.
Description
Technical Field
The invention relates to the field of material detection, in particular to a heat value detection sample loading device and a food self-heating bag detection method.
Background
With the continuous improvement of consumption level and the acceleration of life rhythm, a plurality of products such as self-heating rice, self-heating chafing dish, self-heating vermicelli, self-heating noodles, self-heating spiral shell powder, self-heating cold dish and the like are derived from the current self-heating food. The heating bag is one of the necessary components of self-heating food, and plays an especially important role in the development of self-heating food.
However, when the quality of the heat-generating package is problematic, the heat-recovering effect of the self-heating food is affected, and a certain safety risk is brought about, so that it is urgently needed to develop a comprehensive detection method for the heat-generating package. In contrast, CN105699422A and CN108007968A both refer to methods for detecting heat-generating packs, but the methods mentioned above are greatly interfered by external factors, and professional and standard heat measurement is difficult to achieve.
Regarding the test of the heat generating capacity of the material, a more scientific and accurate method is generally accepted to determine the heat value of the material by using a heat value detection device, however, the device generally needs a long preheating and stabilizing process after sample loading. In the method for measuring the calorific value of the material by adopting a combustion method, the material is ignited by an ignition wire after the preheating is stable, so that the calorific value of the material is accurately measured. When the material to be detected (such as the heating bag mentioned above) heats on the principle of mixing with liquid to generate heat, the existing heat value detection device cannot be directly adopted for detection.
Disclosure of Invention
In order to solve the technical problem, the invention firstly provides a heat value detection sample loading device, which comprises a sample cup and an ignition wire, wherein the ignition wire is vertically higher than the bottom of the sample cup;
the bottom of the sample cup is provided with an opening, a bottom plate which completely covers the opening is arranged at the opening, and the bottom plate is movably connected to the bottom of the sample cup;
the free end of the bottom plate is connected with one end of a bottom plate limiting device, and the other end of the bottom plate limiting device is hung on the ignition wire, so that the bottom plate is buckled at the opening.
Preferably, the sample cup is not provided with a fixed cup bottom, and the bottom plate is used as a movable cup bottom of the sample cup.
Preferably, the ignition wire is positioned directly above the sample cup.
One skilled in the art may or may not provide a cup cover on the upper portion of the sample cup according to the detection requirement, and is not further limited herein.
In addition, the bottom plate limiting device in the invention can be made of metal materials such as springs and the like, and can also be made of flammable materials such as cotton threads and the like, and the limitation is not further made here.
The invention further provides a heat value detection device, wherein the reaction cartridge comprises a reaction cartridge and the heat value detection sample loading device which is higher than the bottom of the reaction cartridge in the vertical direction.
In order to make the exothermic agent to be detected fall into the reaction reagent completely, the exothermic agent should be prevented from sticking to the wall during the falling process as much as possible, and the relative positions of the heating value detection sample loading device and the reaction cartridge can be set by the person skilled in the art based on the principle.
Preferably, the opening at the bottom of the sample cup is oriented perpendicular to the bottom of the reaction cartridge.
The invention further provides the application of the heat value detection sample loading device or the heat value detection device in detecting the heat value of a material, wherein the material generates heat through a solid-liquid reaction.
The invention further provides a detection method of the food self-heating bag, which uses the heat value detection device to detect the heat value of the food self-heating bag; the method specifically comprises the following steps:
(1) placing a heating agent (solid) in the food self-heating bag into the sample cup, and placing a reaction reagent (liquid) into the reaction cartridge;
(2) after the heat value detection device is stable in heat balance, electrifying to fuse the ignition wire, so that the heating agent falls into the reaction reagent, and synchronously measuring by the heat value detection device; in the measuring process, the reaction cartridge cannot be filled with oxygen;
(3) and after the temperature of the oxygen bomb system is constant, measuring, and recording the heat value q.
In the measuring process, the reaction cartridge cannot be filled with oxygen, otherwise, the combustion reaction is easily caused; the oxygen bomb cap is screwed tightly, and air leakage or water leakage cannot occur.
Preferably, the reaction cartridge is filled with an inert gas (e.g., nitrogen) to further avoid combustion reactions, but care should be taken with a small fill to avoid excessive initial pressure in the bomb.
In order to avoid cross contamination between the exothermic agent to be measured and the cup bottom, non-woven fabrics can be padded on the cup bottom.
Although the detection method using the heat value detection device is provided only for the self-heating bag of the food, a person skilled in the art can replace a test object according to test requirements to obtain a corresponding detection method, and the detection method is not further limited herein.
Furthermore, the detection method is perfected on the basis, and the food self-heating bag can be detected more comprehensively and accurately when the detection is carried out by combining the following preferred scheme.
Preferably, the detection method further comprises: and (3) adopting a thermogravimetry-differential scanning calorimetry-mass spectrometry (TG/DSC-MS) technology to synchronously detect the exothermic process and gas generation components of the food self-heating bag.
Preferably, when the heat release process and the gas generation component of the food self-heating bag are detected, the method specifically comprises the following steps:
(1) setting the carrier gas of a thermal analyzer as high-purity nitrogen (preferably with the purity of 99.99%), the flow rate of a purge gas to be 45-55mL/min (preferably 50mL/min), the flow rate of a protective gas to be 20-30mL/min (preferably 25mL/min), and controlling the temperature range in the furnace to be room temperature (22-25 ℃);
(2) placing 5-10mg of the food self-heating bag heating agent in a crucible; adding 25-50mg of reaction reagent into a crucible;
(3) detecting the temperature change, the weight change, the heat flow value and the gas component of a reaction system along with the reaction;
(4) and finishing the detection when the weight change and the temperature change curve tend to be horizontal.
Preferably, when the main component of the heat generating agent is Al and/or Mg, the crucible type of the thermal analyzer is an alumina crucible.
The sample introduction time in the step (2) can be adjusted according to the requirements of instruments, for example, the sample introduction time is adjusted to be 25-35 s.
The food self-heating bag can generate hydrogen in the hydration reaction heat release process, and the hydrogen explosion limit is 4.0-75.6%, so that certain safety risk is realized. Therefore, it is necessary to quantitatively measure the hydrogen generated by the reaction of the food self-heating agent so as to measure the use safety performance of the food self-heating bag and provide data basis for safe use.
Preferably, the detection method further comprises: measuring the hydrogen production amount of the food self-heating bag; the method specifically comprises the following steps:
(1) weighing the heating agent of the food self-heating bag, marking as m, respectively adding the heating agent and the reaction reagent into a high-barrier packaging bag, and placing the high-barrier packaging bag at room temperature for reaction until the volume of the high-barrier packaging bag is stable to obtain a sample-carrying packaging bag;
(2) measuring the volume of the sample-carrying packaging bag by adopting a drainage method and marking as V1(ii) a Detecting the hydrogen concentration in the sample-carrying packaging bag by using a hydrogen detector, and recording the hydrogen concentration as p; discharging gas in the sample-carrying packaging bag, measuring the volume of residues in the bag and the high-barrier packaging bag by adopting a drainage method, and recording the volume as V2；
(3) The exothermic agent has a hydrogen generating capacity Q ═ V1-V2)*p/m。
In some embodiments, the operation of adding the heat generating agent and the reaction reagent into the high-barrier packaging bag respectively is specifically as follows: firstly, adding the heating agent into the high-barrier packaging bag, vacuumizing and sealing; then, the reaction reagent is injected into the bag by a syringe, and the injection needle hole is sealed to make the bag airtight.
The invention has the following beneficial effects:
(1) the invention provides a heat value detection sample loading device and a corresponding heat value detection device aiming at a material which releases heat through a solid-liquid reaction, and realizes accurate detection of the material.
(2) The invention optimizes and perfects the detection method for applying the heat value detection device to the food self-heating bag, breaks through the bottlenecks that the current detection method special for the food self-heating bag is lack, the heat efficiency evaluation subjectivity is strong, and the industrial requirement is difficult to meet, and can provide a special device, a quality evaluation scientific method and a technical support for the safe production and use of the self-heating food heating bag.
Drawings
FIG. 1 is a schematic view of a heat value detection sample loading apparatus in example 1;
FIG. 2 is a TG-DSC sync pattern of F1-F10 samples;
FIG. 3 is a TG/DSC-MS simultaneous analysis chart of F9 sample;
FIG. 4 shows the results of hydrogen production measurements for the F1-F10 samples.
In fig. 1: 1. a sample cup; 2. an ignition wire; 3. a base plate; 4. bottom plate stop device.
Detailed Description
The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention.
The examples do not specify particular techniques or conditions, and are to be construed in accordance with the description of the art in the literature or with the specification of the product. The reagents or instruments used are conventional products available from regular distributors, not indicated by the manufacturer.
Example 1
The embodiment provides a heat value detection sample loading device (shown in a schematic diagram in figure 1), which comprises a sample cup 1 and an ignition wire 2 positioned right above the sample cup 1;
the bottom of the sample cup 1 is not provided with a fixed cup bottom, the bottom of the sample cup 1 is movably connected with a bottom plate 3, and the bottom plate 3 is used as a movable cup bottom of the sample cup 1;
one end of a bottom plate limiting device 4 is connected to the free end of the bottom plate 3, and the other end of the bottom plate limiting device 4 is hung on the ignition wire 2, so that the bottom plate 3 is buckled at the bottom of the sample cup 1.
The embodiment further provides a heat value detection device, which comprises a reaction cartridge and the above-mentioned heat value detection sample loading device which is vertically higher than the bottom of the reaction cartridge, wherein the opening at the bottom of the sample cup 1 faces to the bottom which is vertical to the reaction cartridge.
Example 2
This example provides a method for detecting a heat generating agent sample derived from a self-heating bag for food, which is F1 to F10.
1. Detecting the calorific value of the food self-heating bag, and specifically comprising the following steps:
(1) placing a heat generating agent in the sample cup, and placing water in the reaction cartridge;
(2) after the heat value detection device is stable in heat balance, electrifying to fuse the ignition wire, so that the heating agent falls into water, and synchronously measuring by the heat value detection device; in the measuring process, a small amount of nitrogen is filled in the reaction bomb;
(3) after the temperature of the oxygen bomb system is constant, the heat value q is recorded after the measurement is finished, and the result is shown in the following table 1.
TABLE 1
| Sample (I) | Calorific value q (unit: kJ/g) |
| F1 | 3.50 |
| F2 | 6.04 |
| F3 | 5.25 |
| F4 | 3.34 |
| F5 | 3.66 |
| F6 | 4.61 |
| F7 | 2.39 |
| F8 | 6.04 |
| F9 | 1.91 |
| F10 | 6.36 |
2. The method adopts a thermogravimetry-differential scanning calorimetry-mass spectrometry (TG/DSC-MS) technology to synchronously detect the exothermic process and gas production components of the food self-heating bag, and specifically comprises the following steps:
(1) setting the carrier gas of a thermal analyzer as high-purity nitrogen (with the purity of 99.99%), the flow rate of a purging gas to be 50mL/min, the flow rate of a protective gas to be 25mL/min, and controlling the temperature range in the furnace to be room temperature;
(2) placing 8mg of the food self-heating bag of the heating agent in a crucible; adding 45mg of ultrapure water into the crucible, and sampling for 30 s;
(3) detecting the temperature change, the weight change, the heat flow value and the gas composition of a reaction system along with the reaction;
(4) when the weight change and temperature change curves tend to be horizontal, ending the detection, wherein the detection result is shown in fig. 2-3, and fig. 2 is a TG-DSC synchronous analysis chart of the F1-F10 sample; FIG. 3 is a TG/DSC-MS simultaneous analysis chart of F9 sample.
3. Measuring the gas production rate of the food self-heating bag; the method specifically comprises the following steps:
(1) weighing 1.0g of the heating agent of the food self-heating bag, marking as m, firstly adding the heating agent into the high-barrier packaging bag, vacuumizing and sealing; then injecting distilled water of which the amount is 5 times that of a self-heating agent into the vacuum packaging bag by using a 10mL injector, sealing the injection needle hole by using an adhesive tape to seal the injection needle hole to ensure that the injection needle hole is airtight, placing the packaging bag at room temperature for reacting for 1 hour till the reaction is complete, generating gas by the reaction to ensure that the vacuum packaging bag expands, and stabilizing the volume until the volume is not changed any more to obtain a carrier packaging bag;
(2) the volume of the carrier packaging bag is measured by adopting a drainage method,is marked as V1；
Detecting the hydrogen concentration in the carrier gas bag by using a probe of a hydrogen detector (MS400-H2-RD1), pricking the detector with a gas-pumping pillow into the packaging bag, recording the change of the hydrogen concentration in the inner bag within 2min, and recording the concentration once every 2s by using the instrument. After the recording is finished, taking a concentration value within a time range of 30s before and after the highest concentration, and taking an average value, namely the hydrogen concentration in the carrier gas packaging bag, and recording as p;
discharging the gas in the carrier gas packaging bag, carrying out vacuum sealing on the packaging bag and the reaction residues, measuring the volumes of the residues in the packaging bag and the high-barrier packaging bag by adopting a drainage method, and marking as V2；
(3) The hydrogen production capacity Q of the exothermic agent is (V)1-V2) P/m, hydrogen production measured for each sample is shown in figure 4.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (8)
1. The heat value detection device is characterized by comprising a reaction cartridge and a heat value detection sample loading device which is higher than the bottom of the reaction cartridge in the vertical direction, wherein the opening at the bottom of a sample cup faces to the bottom which is vertical to the reaction cartridge;
wherein the calorific value detection sample loading device comprises a sample cup and an ignition wire which is higher than the bottom of the sample cup in the vertical direction;
the bottom of the sample cup is provided with an opening, a bottom plate which completely covers the opening is arranged at the opening, and the bottom plate is movably connected to the bottom of the sample cup;
one end of a bottom plate limiting device is connected to the free end of the bottom plate, and the other end of the bottom plate limiting device is hung on the ignition wire, so that the bottom plate is buckled at the opening;
the heat value detection device is used for detecting the heat value of the food self-heating bag; the method specifically comprises the following steps:
(1) placing the exothermic agent in the food self-heating bag into the sample cup, and placing a reaction reagent into the reaction cartridge;
(2) after the heat value detection device is stable in heat balance, electrifying to fuse the ignition wire, so that the heating agent falls into the reaction reagent, and synchronously measuring by the heat value detection device; in the measuring process, filling inert gas into the reaction bomb;
(3) and after the temperature of the oxygen bomb system is constant, recording the calorific value q after the measurement is finished.
2. The calorific value detector of claim 1, wherein said sample cup is not provided with a fixed bottom, and said bottom plate is a movable bottom of said sample cup.
3. The calorific value detection device of claim 1 or 2, wherein the ignition wire is located directly above the sample cup.
4. Use of a calorific value detection device according to any one of claims 1 to 3 in detecting the calorific value of a material which generates heat by a solid-liquid reaction.
5. A detection method of a food self-heating pack is characterized in that the heat value of the food self-heating pack is detected by using the heat value detection device of any one of claims 1-3;
the method specifically comprises the following steps:
(1) placing a heating agent in the food self-heating bag into the sample cup, and placing a reaction reagent into the reaction cartridge;
(2) after the heat value detection device is stable in heat balance, electrifying to fuse the ignition wire, so that the heating agent falls into the reaction reagent, and synchronously measuring by the heat value detection device; in the measuring process, filling inert gas into the reaction bomb;
(3) and after the temperature of the oxygen bomb system is constant, measuring, and recording the heat value q.
6. The detection method according to claim 5, further comprising: and detecting the heat release process and gas generation components of the food self-heating bag synchronously by adopting a thermogravimetry-differential scanning calorimetry-mass spectrometry combined technology.
7. The detection method according to claim 6, wherein when the exothermic process and the gas generating components of the food self-heating bag are detected, the method specifically comprises the following steps:
(1) setting the carrier gas of a thermal analyzer as high-purity nitrogen, wherein the flow rate of the purge gas is 45-55mL/min, the flow rate of the protective gas is 20-30mL/min, and the temperature range in the furnace is controlled at room temperature;
(2) placing 5-10mg of the food self-heating bag heating agent in a crucible; adding 25-50mg of reaction reagent into a crucible;
(3) detecting the temperature change, the weight change, the heat flow value and the gas component of a reaction system along with the reaction;
(4) and finishing the detection when the weight change and the temperature change curve tend to be horizontal.
8. The detection method according to any one of claims 5 to 7, further comprising: quantitatively measuring the hydrogen production amount of the food self-heating bag; the method specifically comprises the following steps:
(1) weighing the heating agent of the food self-heating bag, marking as m, respectively adding the heating agent and the reaction reagent into a high-barrier packaging bag, and placing the high-barrier packaging bag at room temperature for reaction until the volume of the high-barrier packaging bag is stable to obtain a sample-carrying packaging bag;
(2) measuring the volume of the sample-carrying packaging bag by adopting a drainage method and marking as V1(ii) a Detecting the hydrogen concentration in the sample-carrying packaging bag by using a hydrogen detector, and recording the hydrogen concentration as p; discharging gas in the sample-loading packaging bag, measuring the volume of residues in the bag and the high-barrier packaging bag by adopting a drainage method, and marking as V2；
(3) The exothermic agent has a hydrogen generating capacity Q ═ V1-V2)*p/m。
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| JP2001052848A (en) * | 1999-08-11 | 2001-02-23 | Hitachi Hometec Ltd | Electromagnetic induction heating device |
| CN1900706A (en) * | 2006-06-07 | 2007-01-24 | 西北工业大学 | Detector for boron containing lean oxygen propellant heat value |
| CN105699422A (en) * | 2016-04-01 | 2016-06-22 | 宁夏中航郑飞塞外香清真食品有限公司 | Heating efficiency detection method of heating packet and heating efficiency detection device of heating packet |
| CN209132194U (en) * | 2018-09-29 | 2019-07-19 | 湖南三德科技股份有限公司 | It is a kind of can automatic clamping and placing crucible oxygen bomb |
| CN209130923U (en) * | 2018-09-29 | 2019-07-19 | 湖南三德科技股份有限公司 | A kind of calorimeter fire rod and calorimeter |
| CN110261435A (en) * | 2019-06-05 | 2019-09-20 | 中国建筑科学研究院有限公司 | Method for measuring combustion heat value of thermosetting composite polystyrene board |
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2019
- 2019-11-19 CN CN201911133426.3A patent/CN110988021B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001052848A (en) * | 1999-08-11 | 2001-02-23 | Hitachi Hometec Ltd | Electromagnetic induction heating device |
| CN1900706A (en) * | 2006-06-07 | 2007-01-24 | 西北工业大学 | Detector for boron containing lean oxygen propellant heat value |
| CN105699422A (en) * | 2016-04-01 | 2016-06-22 | 宁夏中航郑飞塞外香清真食品有限公司 | Heating efficiency detection method of heating packet and heating efficiency detection device of heating packet |
| CN209132194U (en) * | 2018-09-29 | 2019-07-19 | 湖南三德科技股份有限公司 | It is a kind of can automatic clamping and placing crucible oxygen bomb |
| CN209130923U (en) * | 2018-09-29 | 2019-07-19 | 湖南三德科技股份有限公司 | A kind of calorimeter fire rod and calorimeter |
| CN110261435A (en) * | 2019-06-05 | 2019-09-20 | 中国建筑科学研究院有限公司 | Method for measuring combustion heat value of thermosetting composite polystyrene board |
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