CN106770455A - A kind of new combustion heat determination method - Google Patents
A kind of new combustion heat determination method Download PDFInfo
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- CN106770455A CN106770455A CN201611105757.2A CN201611105757A CN106770455A CN 106770455 A CN106770455 A CN 106770455A CN 201611105757 A CN201611105757 A CN 201611105757A CN 106770455 A CN106770455 A CN 106770455A
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- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/22—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures
- G01N25/26—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures using combustion with oxygen under pressure, e.g. in bomb calorimeter
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Abstract
The invention discloses a kind of new combustion heat determination method, the method is comprised the following steps：Step one：Preheater apparatus, carry out baseline correction；Step 2：Dress sample；Testing sample is weighed, is put into sample cell, then sample cell is sealed in calorimeter；Step 3：Filled oxygen to calorimeter；Step 4：Calorimeter is installed；Reference and two calorimeters to be measured are delivered into two calorimetric rooms, sealed vol hot cell respectively；Step 5：Igniting；Certain electric current is set on DC power supply, the controlling switch of DC power supply is pressed, ignition point is completed；Step 6：Gathered data, calorimetric treatment.The combustion heat determined using this method, sensitivity is high, can detect microwatt level hot-fluid；Good stability, long-time baseline drift is no more than ± 0.1 Μ v；And easy grasp simple to operate, reproducible, amount of samples is small, is particularly suitable for measuring the measure of relatively valuable and explosive sample, therefore the non-constant width of experimental applications scope.
Description
Technical field
The present invention relates to thermoanalysis technology method field, more particularly to a kind of new combustion heat determination method.
Background technology
The combustion heat refers to that under standard pressure, during reaction temperature T, combustible complete oxidation is the specified product under equality of temperature
When enthalpy change.The combustion heat is a kind of important heat chemistry parameter, may determine that different compounds contain energy by combustion heat value
Size, while the formation mechanism of kinetics and compound can also be speculated.At present, the almost combustion heat of most of material
All it is to be determined by method of oxygen steel bomb, Oxygen bomb is the main tool of the method.The burning of method of oxygen steel bomb determination sample
Metal ignition wire is used when hot directly to ignite mode.
When determining the combustion heat of material using Oxygen bomb, first have to demarcate the energy equivalent of calorimeter.Typically
In the case of, be all use known combustion heat benzoic acid as standard substance, the benzoic acid for weighing certain mass is placed in oxygen bomb,
Being ignited by ignition wire makes it burn completely, causes the change of system temperature just can to obtain oxygen bomb amount according to burning liberated heat
Heat meter thermal capacitance.After demarcation, then a certain amount of test substance sample is placed in oxygen bomb, with the step as demarcating, finally determines combustion
The combustion heat of variation of ambient temperature and then acquisition testing sample before and after burning.
Method of oxygen steel bomb is the standard method of a kind of Accurate Determining substance combustion heat or biomass fermentation heat.But for combustion
Point sample higher, igniting is difficult successfully, and incomplete combustion, makes this method success rate low, complex operation；Even if low burn
The sample igniting of point is relatively easy, but because of heat exchange small between environment, makes the error of measure very big, and the method
Time consumption of experimental process it is long.Therefore, various improved methods on this basis occur therewith.In recent years, many was devoted to burning
The researcher of heat determination calorimetry has been carried out very big improvement with it is perfect, such as in temperature measuring, oxygenation mode, oxygen bomb
Interior oxygen pressure, the compressing tablet of sample, the installation of ignition wire and data processing etc. are leavened dough, and have made the degree of accuracy of this method notable
Improve.But energetic material is very easy to blast in combustion, with certain risk, the method is unsuitable for energetic material
The measure of the combustion heat.
For energetic material, the combustion heat is one of its indispensable thermodynamic data.By the combustion heat, can be to containing energy
The combustibility of material carries out out discussion, and determining whether can be as propellant or explosive additive etc..But the material containing energy
Material is very easy to blast in combustion, and method of oxygen steel bomb needs sample size larger, so has continuous mode certain
Danger, the measure for making it not be suitable for the energetic material combustion heat.So in the urgent need to a kind of method of new combustion heat determination,
The combustion heat of general compound can not only be determined, it is also possible to for determining the dangerous burning containing energy material of explosive, tool
Heat.
The content of the invention
In order to overcome defect of the prior art, there is provided a kind of new combustion heat determination method.
The present invention is realized by following proposal：
A kind of new combustion heat determination method, the method is comprised the following steps：
Step one：Preheater apparatus, carry out baseline correction；
Step 2：Dress sample；Testing sample is weighed, is put into sample cell, then sample cell is sealed in calorimeter；
Step 3：Filled oxygen to calorimeter；Oxygen cylinder is spun into the air inlet of calorimeter, gas cylinder is slowly opened, carried out
Inflation, inlet suction port of outwarding winding, inflation is completed；
Step 4：Calorimeter is installed；Reference and two calorimeters to be measured are delivered into two calorimetric rooms respectively, calorimetric is sealed
Room；
Step 5：Igniting；Certain electric current is set on DC power supply, the control of DC power supply is pressed
Switch, ignition point is completed；
Step 6：Gathered data, calorimetric treatment.
The step one includes step in detail below：
(1) power switch of measurement and control instrument is opened, computer main control software is then opened, tester is devoted oneself to work；
(2) heater switch of measurement and control instrument is opened, the temperature of control needed for setting；
(3) instrument is preheated, treats that baseline tends to be steady completely, stop preheating.
The step 6 includes step in detail below：
(1) measurement of thermoelectrical potential
Into voltage, by being shown after smoothing processing, being preserved, smoothing processing formula is the thermoelectrical potential data conversion that will be gathered：
Wherein ei, ej are the passage i-th, the j magnitude of voltage of sampling；
A is smoothing factor (positive integer), default value A=10；
(2) baseline correction
By selected base line measurement time T as the base line measurement sampling time, measure equation is：
Wherein, BEi is current baseline value, and baseline also directly can be considered appropriate numerical value, take E=by operator's input
Ej-BEi is referred to as base wavelet, shows E values, and the spectral line being made up of E；
(3) heat release power P is calculated
The computing formula of heat release power P is：P=E/S
S is instrumental sensitivity, is produced through demarcating, or author's input；
(4) thermal discharge is calculated
Reaction is set first and starts threshold value δ 1, and reaction terminates threshold value δ 2, δ 1>δ2>0,
As | E | >=δ 1, it is believed that reaction starts, and computer starts integrating
H is the calorimetric coefficient of instrument in formula, and A is the integral area of curve, and Q is the combustion heat of tested combustibility sample, and
The current thermal discharge having detected that is shown with once per second speed, thinks that reaction terminates when | E |≤δ 2, this calorimetric process
Terminate, the heat is shown in addition, system waits measurement next time.
The quality of the sample weighed needed for step 2 is 5-20 milligrams.
The reference that step 4 is related to and two calorimeters to be measured measure calorific value according to showing poor method by series system.
DC power supply in step 5 can be controlled to the duration of ignition, electric current and voltage.
Step 6 includes the process that spectral line is obtained, and its combustion heat is obtained by the area integral to spectral line.
Beneficial effects of the present invention are：
The combustion heat determined using this method, sensitivity is high, can detect microwatt level hot-fluid；Good stability, for a long time
Baseline drift is no more than ± 0.1 Μ v；And easy grasp simple to operate, reproducible, amount of samples is small, is particularly suitable for measurement
The measure of relatively valuable and explosive sample, therefore the non-constant width of experimental applications scope.
Brief description of the drawings
Fig. 1 is the structural representation of calorimeter of the invention；
Fig. 2 is a kind of Calorimetry system overall structure diagram of new combustion heat determination method of the invention.
Specific embodiment
The present invention is further described with specific embodiment below in conjunction with the accompanying drawings：
A kind of new combustion heat determination method, the method is comprised the following steps：
Step one：Preheater apparatus, carry out baseline correction；
Step 2：Dress sample；Testing sample is weighed, is put into sample cell, then sample cell is sealed in calorimeter；
Step 3：Filled oxygen to calorimeter；Oxygen cylinder is spun into the air inlet of calorimeter, gas cylinder is slowly opened, carried out
Inflation, inlet suction port of outwarding winding, inflation is completed；
Step 4：Calorimeter is installed；Reference and two calorimeters to be measured are delivered into two calorimetric rooms respectively, calorimetric is sealed
Room；
Step 5：Igniting；Certain electric current is set on DC power supply, the control of DC power supply is pressed
Switch, ignition point is completed；
Step 6：Gathered data, calorimetric treatment.
As shown in figure 1, calorimeter used in the present invention is to show differential thermal flowmeter, it is described to show that differential thermal flowmeter is main by two lists
One heat-flow meter composition, thermocouple has almost been discontented with around the calorimetric chamber wall 1 of the heat-flow meter, constitutes thermoelectric pile 2, often
One one end of thermocouple 3 is contacted with calorimetric chamber wall, and the other end 4 is contacted with soaking block 5, soaking block 5 be a thermal capacity compared with
Big metal derby, is not influenceed at a temperature of control by reaction heat, and liberated heat makes thermocouple two ends the temperature difference occur during burning,
So that there is the heat transfer that Newtonian cooling law is carried out, hot-fluid is produced.Then further according to poor method is shown, main control software is measured
The curve integration that thermoelectrical potential is changed over time can be in the hope of sample combustion institute liberated heat.
The step one includes step in detail below：
(1) power switch of measurement and control instrument is opened, computer main control software is then opened, tester is devoted oneself to work；
(2) heater switch of measurement and control instrument is opened, the temperature of control needed for setting；
(3) instrument is preheated, treats that baseline tends to be steady completely, stop preheating.
The step 6 includes step in detail below：
(1) measurement of thermoelectrical potential
Into voltage, by being shown after smoothing processing, being preserved, smoothing processing formula is the thermoelectrical potential data conversion that will be gathered：
Wherein ei, ej are the passage i-th, the j magnitude of voltage of sampling；
A is smoothing factor (positive integer), default value A=10；
(2) baseline correction
By selected base line measurement time T as the base line measurement sampling time, measure equation is：
Wherein, BEi is current baseline value, and baseline also directly can be considered appropriate numerical value, take E=by operator's input
Ej-BEi is referred to as base wavelet, shows E values, and the spectral line being made up of E；
(3) heat release power P is calculated
The computing formula of heat release power P is：P=E/S
S is instrumental sensitivity, is produced through demarcating, or author's input；
(4) thermal discharge is calculated
Reaction is set first and starts threshold value δ 1, and reaction terminates threshold value δ 2, δ 1>δ2>0,
As | E | >=δ 1, it is believed that reaction starts, and computer starts integrating
H is the calorimetric coefficient of instrument in formula, and A is the integral area of curve, and Q is the combustion heat of tested combustibility sample, and
The current thermal discharge having detected that is shown with once per second speed, thinks that reaction terminates when | E |≤δ 2, this calorimetric process
Terminate, the heat is shown in addition, system waits measurement next time.
The quality of the sample weighed needed for step 2 is 5-20 milligrams.
The reference that step 4 is related to and two calorimeters to be measured measure calorific value according to showing poor method by series system.
DC power supply in step 5 can be controlled to the duration of ignition, electric current and voltage.
Step 6 includes the process that spectral line is obtained, and its combustion heat is obtained by the area integral to spectral line.
A kind of Calorimetry system overall structure diagram of new combustion heat determination method of the present invention is as shown in Figure 2.Using
When, calorimeter of the invention is installed additional sample postpositive in the inside of calorimeter main body 6, the power supply for opening temperature control system 9 is opened
Close and the main control software of computer system 7, steady temperature is set, calorimeter is preheated, treat that the baseline on software interface is complete
Tend to be steady, stop preheating；If set low temperature, can by heat-insulation system 11 temperature is controlled with it is constant；Weigh to be measured
Sample, is put into sample cell；Sample cell is sealed in calorimeter；
Oxygen cylinder is spun into the air inlet of calorimeter, gas cylinder is slowly opened, is inflated, be filled with to 1.5~2.0MPa
When, inlet suction port of outwarding winding, inflation is completed；Will be equipped with testing sample and two calorimeters without sample are put into calorimeter main body 6
Two calorimetric rooms in, then by calorimetric room seal；
Certain electric current is set on current control system 10, controlling switch is pressed, igniting makes sample combustion；In use
Calorimetry system of the invention is controlled with using rear cooperation vacuum system 8.
Although having done more detailed elaboration to technical scheme and having enumerated, it will be appreciated that for ability
For field technique personnel, modification is made to above-described embodiment or equivalent alternative solution is used, this is to those skilled in the art
It is it is clear that these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the present invention for member
Claimed scope.
Claims (7)
1. a kind of new combustion heat determination method, it is characterised in that the method is comprised the following steps：
Step one：Preheater apparatus, carry out baseline correction；
Step 2：Dress sample；Testing sample is weighed, is put into sample cell, then sample cell is sealed in calorimeter；
Step 3：Filled oxygen to calorimeter；Oxygen cylinder is spun into the air inlet of calorimeter, gas cylinder is slowly opened, is inflated,
Outward winding inlet suction port, inflation is completed；
Step 4：Calorimeter is installed；Reference and two calorimeters to be measured are delivered into two calorimetric rooms, sealed vol hot cell respectively；
Step 5：Igniting；Certain electric current is set on DC power supply, and the control for pressing DC power supply is opened
Close, ignition point is completed；
Step 6：Gathered data, calorimetric treatment.
2. a kind of new combustion heat determination method according to claim 1, it is characterised in that the step one includes following
Specific steps：
(1) power switch of measurement and control instrument is opened, computer main control software is then opened, tester is devoted oneself to work；
(2) heater switch of measurement and control instrument is opened, the temperature of control needed for setting；
(3) instrument is preheated, treats that baseline tends to be steady completely, stop preheating.
3. a kind of new combustion heat determination method according to claim 1, it is characterised in that the step 6 includes following
Specific steps：
(1) measurement of thermoelectrical potential
Into voltage, by being shown after smoothing processing, being preserved, smoothing processing formula is the thermoelectrical potential data conversion that will be gathered：
Wherein ei, ej are the passage i-th, the j magnitude of voltage of sampling；
A is smoothing factor (positive integer), default value A=10；
(2) baseline correction
By selected base line measurement time T as the base line measurement sampling time, measure equation is：
Wherein, BEi is current baseline value, and baseline also directly can be considered appropriate numerical value, take E=ej-BEi by operator's input
Referred to as base wavelet, shows E values, and the spectral line being made up of E；
(3) heat release power P is calculated
The computing formula of heat release power P is：P=E/S
S is instrumental sensitivity, is produced through demarcating, or author's input；
(4) thermal discharge is calculated
Reaction is set first and starts threshold value δ 1, and reaction terminates threshold value δ 2, δ 1>δ2>0,
As | E | >=δ 1, it is believed that reaction starts, and computer starts integrating
H is the calorimetric coefficient of instrument in formula, and A is the integral area of curve, and Q is the combustion heat of tested combustibility sample, and with every
Second first time rate shows the current thermal discharge having detected that, thinks that reaction terminates when | E |≤δ 2, this calorimetric process knot
Beam, the heat is shown that system waits measurement next time in addition.
4. a kind of new combustion heat determination method according to claim 1, it is characterised in that：Weighed needed for step 2
The quality of sample is 5-20 milligrams.
5. a kind of new combustion heat determination method according to claim 1, it is characterised in that：Reference that step 4 is related to
Two calorimeters to be measured measure calorific value according to showing poor method by series system.
6. a kind of new combustion heat determination method according to claim 1, it is characterised in that：Dc source in step 5
Supply can be controlled to the duration of ignition, electric current and voltage.
7. a kind of new combustion heat determination method according to claim 1, it is characterised in that：Step 6 includes that spectral line is obtained
The process for obtaining, its combustion heat is obtained by the area integral to spectral line.
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Cited By (6)
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| CN107247074A (en) * | 2017-06-20 | 2017-10-13 | 江苏和顺环保有限公司 | The assay method of low heat value industry dangerous waste combustion heat value |
| CN107884437A (en) * | 2017-12-13 | 2018-04-06 | 中国科学院大连化学物理研究所 | It is a kind of to vary convenient and good airproof performance calorimeter sample cell |
| CN111780895A (en) * | 2020-07-06 | 2020-10-16 | 中国原子能科学研究院 | Heat measuring device |
| CN112782223A (en) * | 2020-12-31 | 2021-05-11 | 西南科技大学 | Calorimetric system of combustion heat tester |
| CN112782224A (en) * | 2020-12-31 | 2021-05-11 | 西南科技大学 | Method and device for measuring combustion heat of material |
| CN114018978A (en) * | 2021-10-09 | 2022-02-08 | 广西电网有限责任公司电力科学研究院 | Method for quantifying micro-plastic in environment based on micro-combustion calorimetry |
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| CN107247074A (en) * | 2017-06-20 | 2017-10-13 | 江苏和顺环保有限公司 | The assay method of low heat value industry dangerous waste combustion heat value |
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| CN112782223A (en) * | 2020-12-31 | 2021-05-11 | 西南科技大学 | Calorimetric system of combustion heat tester |
| CN112782224A (en) * | 2020-12-31 | 2021-05-11 | 西南科技大学 | Method and device for measuring combustion heat of material |
| CN114018978A (en) * | 2021-10-09 | 2022-02-08 | 广西电网有限责任公司电力科学研究院 | Method for quantifying micro-plastic in environment based on micro-combustion calorimetry |
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