CN104181078A - Method and device for testing content of easily-volatile matters in explosive - Google Patents
Method and device for testing content of easily-volatile matters in explosive Download PDFInfo
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- CN104181078A CN104181078A CN201410440576.XA CN201410440576A CN104181078A CN 104181078 A CN104181078 A CN 104181078A CN 201410440576 A CN201410440576 A CN 201410440576A CN 104181078 A CN104181078 A CN 104181078A
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Abstract
The invention discloses a method for testing the content of easily-volatile matters in explosive, and provides a device improved based on a microcalorimeter correspondingly, wherein the device is formed by arranging a presser sensor used for measuring the real-time pressure in a sample cell on the sample cell of the microcalorimeter and arranging a reading device, a searching device and a comparing device on a control system of the microcalorimeter. In testing, the explosive is put into the sample cell firstly, and after vacuumization is carried out, the device provided by the invention is started, parameters including the start temperature, the temperature rise amplitude, the reaction judgment sensitivity, the constant temperature time, the waiting time, the reaction termination conditions and the like of the microcalorimeter are set, the pressure change and the temperature rise rate change in the sample cell are recorded, and then the content of the volatile matters is obtained by an ideal gas state equation. According to the invention, by analyzing the relationship between the gas discharge quantity and the heat flux change, the content of the easily-volatile matters in the explosive can be effectively tested.
Description
Technical field
Embodiments of the present invention relate to instrumental analysis field, and more specifically, embodiments of the present invention relate to the assay method of volatile matter adsorbance in a kind of explosive.
Background technology
Explosive in metastable state, along with environment temperature of living in raises, can carry out thermal decomposition with given pace in normal temperature environment, discharges the relatively low gaseous product of molecular weight, and quality reduces thereupon simultaneously, and is accompanied by the variation of heat.Utilize the variation of these character, can the thermal decomposition process of explosive and phenomenological kinetic property be studied and be followed the trail of.Wherein, eudiometry, is about to explosive and puts into the method for the variation of confined space measurement gas product pressure, is one of classical means of research explosive thermal decomposition.Conventional eudiometry mainly comprises Bu Shi pressure application and vacuum stability (VST) method.Bu Shi pressure application is to carry out under vacuum isothermal condition, by the METHOD FOR CONTINUOUS DETERMINATION gas pressure change that certain explosive thermal decomposition produces in different time, and be converted under standard state (0 ℃, 101.325kPa) every gram of sample thermal decomposition produces the volume of gas, thereby obtains decomposition kinetics curve.Similar with Bu Shi pressure application principle, vacuum stability (VST) method is that sample is placed under uniform temperature, certain hour and certain vacuum degree condition and is heated, gas discharge quantity by contrast various sample judges the thermal decomposition speed of explosive, its in practical engineering application usually used as the macro approach of rapid screening high explosive.
But due to the impact of preparation method and process conditions, in explosive sample, conventionally can adsorb and have a small amount of organic solvent, moisture and other volatile matters.When carrying out Bu Shi pressure application and the test of vacuum stability method, the organic solvent of these absorption, moisture and other volatile matters can evaporate or distil for gaseous state, thereby make the discharge quantity of the explosive thermal decomposition that records more higher than actual discharge quantity, follow-up thermal decomposition rate calculations and decomposition kinetics analysis are impacted.Therefore when carrying out Bu Shi pressure application and the test of vacuum stability method, conventionally need in baking oven, under uniform temperature, carry out sample pretreatment a period of time, and extracting vacuum, to remove to greatest extent solvent, moisture and other volatile matters in sample, reduce their impacts on test findings.However, sample pre-treatments and extracting vacuum can not be disposed the volatile matter adsorbing in explosive completely, the remaining trace absorption volatile matter of part still can discharge in Bu Shi pressure application and vacuum stability test process, affects the accuracy of experimental result.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, a kind of improved microcalorimeter is provided and measures the embodiment of the method for volatile matter content in explosive, by the method to the explosive volatile matter amount that the relation analysis between changes of heat flux and discharge quantity obtains adsorbing in explosive in isothermal environment.
For solving above-mentioned technical matters, one embodiment of the present invention by the following technical solutions:
A kind of device of measuring volatile matter content in explosive, comprise microcalorimeter, it is characterized in that described device is to install for measuring the pressure transducer of real-time pressure in sample cell on the sample cell of microcalorimeter, and arrange and form as lower device in the control system of microcalorimeter:
Reading device
Be connected with the control system signal of microcalorimeter, for in the temperature of sample cell, rise to the default initial temperature of microcalorimeter or by intensification stride, heat up after temperature time read microcalorimeter stand-by period, when the stand-by period of microcalorimeter expires, transmit enabling signal to searcher;
Searcher
Receive the enabling signal of reading device, then in the default constant temperature time of microcalorimeter, search for the sample cell heating rate signal that microcalorimeter detects and pass to comparison means;
Comparison means
In the default constant temperature time of microcalorimeter, receive the sample cell heating rate signal searching of searcher, and react default with microcalorimeter judges that susceptibility and reaction terminating condition compare, when the absolute value of susceptibility is judged in the absolute value < reaction that sample cell heating rate does not reach reaction terminating condition and perseverance has sample cell heating rate in this constant temperature time, after this constant temperature time finishes, to microcalorimeter, send the signal heating up by intensification stride; When sample cell heating rate does not reach reaction terminating condition and occur that in this constant temperature time the absolute value of susceptibility is judged in the absolute value of sample cell heating rate >=reaction, after this constant temperature time finishes, to the control system of microcalorimeter, send the signal of repetition constant temperature time; When sample cell heating rate reaches reaction terminating condition, to the control system transmission termination test signal of microcalorimeter.
A method that adopts volatile matter content in said apparatus test explosive, it comprises the steps:
(1) explosive that contains in right amount volatile matter is joined in the sample cell of microcalorimeter, then sample cell is vacuumized;
(2) in the control system of microcalorimeter, set initial temperature, stand-by period, constant temperature time, intensification stride, reaction judgement susceptibility and reaction terminating condition;
(3) sample cell is warmed up to initial temperature;
(4) waiting temperature balance;
(5) after equalized temperature, search for temperature, hot-fluid, pressure and the sample cell heating rate under the same time, by sample cell heating rate and reaction terminating condition and react and judge that susceptibility compares;
(6) when the absolute value of susceptibility is judged in the absolute value < reaction that sample cell heating rate does not reach reaction terminating condition and perseverance has sample cell heating rate in this constant temperature time, after this constant temperature time finishes,, microcalorimeter heats up to sample cell by intensification stride;
(7) then repeating step (4), (5), (6), when sample cell heating rate does not reach reaction terminating condition and occur that in this constant temperature time the absolute value of susceptibility is judged in the absolute value of sample cell heating rate >=reaction, after this constant temperature time finishes, again enter next constant temperature time section, then repeating step (5), (6), until sample cell heating rate end of test while reaching reaction terminating condition;
(8) then take pressure, hot-fluid, the temperature of step (5) gained is ordinate, and its corresponding time is horizontal ordinate, makes pressure/hot-fluid/temperature-time curve;
(9), when the pressure of step (8) gained pressure/hot-fluid/temperature-time curve in the same time period before end of test and hot-fluid are definite value, the corresponding pressure of pressure/hot-fluid/temperature-time curve in this time period of take is p
1, temperature is T;
(10) by the Al adding in the empty sample cell of microcalorimeter with explosive charge same volume
2o
3, after extracting vacuum, being increased the temperature to T, the force value of measuring is now p
2, with p=p
1-p
2, and to take the volume of sample cell be V, ideal gas constant is R, utilizes the Ideal-Gas Equation pV=nRT through calculating the amount of substance n of the volatile matter in explosive.
Further technical scheme is that described explosive keeps stable chemical nature when the volatilization temperature less than or equal to volatile matter.
Further technical scheme is, described initial temperature is lower than the decomposition temperature of volatilization temperature and the explosive of volatile matter in explosive.If initial temperature is higher than the volatilization temperature of volatile matter in explosive, some volatile matter will vapor away before test certainly, thereby can not test the volatile matter of this part volatilization, causes test result inaccurate.In like manner, if initial temperature is higher than the decomposition temperature of explosive, with regard to the amount of can not testing volatile matter.
According to one embodiment of the present invention, described intensification stride is set as 0.2～5 ℃.Intensification stride is set must be suitable, if intensification stride is excessive, may causes the temperature being directly warmed up to higher than explosive decomposition, and volatilization temperature is masked at the intersegmental volatile matter of two temperatures; If intensification stride is too small, can cause the test duration long.
Described reaction judges that susceptibility is set as-0.02 ℃/min～-0.005 ℃/min.Reaction judges that susceptibility arranges improper the carrying out that is unfavorable for test process, causes the test duration long when excessive, and when too small, some volatile matter signal is covered, and causes test result inaccurate.
The described stand-by period is set as 5～15min.
Described constant temperature time is set as 15～30min.
Described reaction terminating condition is heating rate >=0.05 ℃/min.
Compared with prior art, one of beneficial effect of the present invention is: preparation method of the present invention can obtain the volatile content in explosive accurately, thereby when measuring the thermal decomposition discharge quantity of explosive, eliminate the impact of volatile matter, make follow-up thermal decomposition rate calculations and decomposition kinetics analysis result more accurate; Device provided by the invention can be quick, real-time the variation of detected pressures, temperature and heat flow value, by the data that detect, can make pressure/hot-fluid/temperature-time curve, in this curve, a period of time internal pressure before end of test and hot-fluid are definite value, utilize temperature and the pressure after overcorrect now can calculate fast the volatile matter amount of explosive by the Ideal-Gas Equation, simple to operate, for the follow-up test of explosive provides basis, for accuracy and the thermoanalytical validity of follow-up test data are given security.
Accompanying drawing explanation
Fig. 1 is that the sample cell of apparatus of the present invention improves structural representation.
Fig. 2 is the curve synoptic diagram that the present invention records.
Fig. 3 is the pressure that records of the present invention and the curve comparison schematic diagram of hot-fluid.
Fig. 4 is that improvement structure and the signal of apparatus of the present invention in microcalorimeter control system moves towards schematic diagram.
Fig. 5 is the present invention's stride schematic diagram that heats up.
Fig. 6 is the actual intensification stride figure detecting of the present invention.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
As shown in Figure 1, the measurement mechanism that the present invention adopts is improved microcalorimeter, can adopt the BT2.15 microcalorimeter of French Sai Talamu company to improve, first a pressure transducer 101 is installed on sample cell 103, to realize the real-time measurement to the pressure in sample cell, because microcalorimeter itself can detect by thermopair 102 hot-fluid and the temperature of sample cell, therefore, after setting pressure sensor 101, device of the present invention both can detect real-time pressure, can detect real-time hot-fluid and temperature again.Sample cell 103 is for splendid attire explosive 104.Except above-mentioned improvement, the present invention also improves the control system of microcalorimeter, and improved structure as shown in Figure 4, comprises reading device, searcher, comparison means; Fig. 4 has shown the signal transitive relation between each device, below by Fig. 4, illustrates that relation and signal between device all parts of the present invention flow to.Use before device of the present invention, first the explosive of need being measured packs in sample cell, set on computers initial temperature, stand-by period, constant temperature time, intensification stride, the operational factors such as susceptibility and reaction terminating condition are judged in reaction, then starting microcalorimeter starts working, first microcalorimeter can be warmed up to initial temperature by sample cell within the stand-by period, reading device meeting read waiting time, treat that the stand-by period expires, namely the temperature of sample cell is initial temperature stable equilibrium, at this moment reading device can send a signal to searcher, searcher receives after the signal of reading device, start function of search, the sample cell heating rate signal that search microcalorimeter detects also passes to comparison means, comparison means judges that by sample cell heating rate and the reaction of setting susceptibility (such as being-0.02 ℃/min) and reaction terminating condition (such as being 0.05 ℃/min) compare, if sample cell heating rate is for reaching reaction terminating condition, and the absolute value of susceptibility is judged in its absolute value < reaction, comparison means sends the signal of " heating up by intensification stride " to the control system of microcalorimeter, the sample cell of microcalorimeter starts again to heat and enters the next stand-by period, if sample cell heating rate does not reach reaction terminating condition, and the absolute value of susceptibility is judged in its absolute value >=reaction, comparison means sends the signal of " next constant temperature time " to the control system of microcalorimeter, the sample cell of microcalorimeter enters next constant temperature time, and reading device, searcher, decision maker repeat again above-mentioned work until sample cell heating rate reaches the end condition of setting, when if sample cell heating rate reaches the end condition of setting, comparison means sends the signal of " stopping heating " to the control system of microcalorimeter, in whole process, microcalorimeter can detect and record hot-fluid, the temperature and pressure of sample cell, and computing machine is understood the parameters such as automatic writing time, temperature, heating rate, pressure and hot-fluid.
Fig. 5 is the present invention's stride schematic diagram that heats up, but is not the figure really detecting, and the intensification stride figure really detecting as shown in Figure 6.The intensification stride step that heats up, take ℃ is linear module, the existence of intensification stride should make temperature become in Fig. 5 shown in A part in theory, but because intensification has certain speed, so be usually expressed as in Fig. 5 shown in B part, and in order to prevent the generation of the situations such as temperature overshot, heating rate is not constant conventionally, but PID is programme controlled in microcalorimeter, so actual temperature shows as in Fig. 5 shown in C part.Popular says, intensification stride is exactly two temperature gaps between adjacent temperature constant state.
Fig. 2 is pressure/hot-fluid/temperature-time curve, adopts method provided by the invention to obtain.
Fig. 3 is the comparison curves of pressure and hot-fluid, in fact be corresponding with pressure-time curve, hot-fluid-time curve in Fig. 2 pressure/hot-fluid/temperature-time curve, the effect of Fig. 3 be to highlight final stage before end of test at one time scope remain pressure-time curve and the hot-fluid-time curve of horizontal linear, as shown in dotted line frame 301, illustrate that section keeps constant between pressure and hot-fluid are at this moment.The temperature of Fig. 3 dotted line frame 301 interior correspondences of take is that T, corresponding pressure are p
1, deduct base measuring pressure p
2(p
2by the Al adding in sample cell with explosive charge same volume
2o
3, after extracting vacuum, increased the temperature to T, the force value measuring) and the pressure p that obtains, utilize the Ideal-Gas Equation pV=nRT can calculate the amount n of volatile matter, the volume that wherein V is sample cell, R is ideal gas constant.Because the volatilization process of volatile matter is endothermic process, and the decomposable process of energetic material is exothermic process, by being heat absorption to occur or heat release just can be distinguished the volatilization process of volatile matter or the decomposable process of energetic material in test process.And in energetic material, explosive keeps stable chemical nature when the volatilization temperature less than or equal to volatile matter, the volatilization temperature of the volatile matter of absorption conventionally will be far below the decomposition temperature of energetic material, in measuring energetic material, in the process of the amount of volatile matter volatilization, there will be hardly mutually covering of endothermic signal and heat release signal, therefore can accurately obtain the amount of the volatile matter that adsorbs in energetic material.
Below by specific embodiment, set forth the inventive method.
Embodiment 1
1gHMX base PBX explosive is joined in the sample cell of measuring the device (hereinafter to be referred as improved microcalorimeter) of volatile matter content in explosive, sample cell is vacuumized, in the control system of improved microcalorimeter, setting initial temperature is 20 ℃, stand-by period is 5min, constant temperature time 30min, 1 ℃ of intensification stride, reaction judges that susceptibility-0.005 ℃/min and reaction terminating condition are as heating rate >=0.05 ℃/min, starter gear heating, sample cell is warmed up to then waiting temperature balance of 20 ℃ of initial temperatures, after equalized temperature, search for the temperature under the same time, hot-fluid, pressure and sample cell heating rate, by sample cell heating rate and reaction terminating condition and react and judge that susceptibility compares, when 0.05 ℃/min of sample cell heating rate < does not reach reaction terminating condition and in this constant temperature time during the 0.005 ℃/min of the absolute value < absolute value of susceptibility (reaction judge) of sample cell heating rate, after this constant temperature time finishes, improved microcalorimeter heats up to sample cell by the intensification stride of 1 ℃, then repeat waiting temperature balance, by sample cell heating rate and reaction terminating condition and react the step of judging that susceptibility compares, while occurring that 0.05 ℃/min of sample cell heating rate < does not reach reaction terminating condition and occur the absolute value >=0.005 ℃/min of sample cell heating rate in this constant temperature time, after this constant temperature time finishes, again enter next constant temperature time section, then the step that repeats comparison and heat up by intensification stride until sample cell heating rate >=0.05 ℃/min reach reaction terminating condition instrument test and enter termination phase.
In the process heating at improved microcalorimeter, the pressure in sample cell, temperature and changes of heat flux situation are carried out to real-time synchronization record, obtain pressure-time curve, temperature-time curve and hot-fluid-time curve.Volatile matter volatilizees completely substantially and energetic material starts to decompose hot-fluid, pressure in front curve and is definite value, pressure p after calibration is 3.18Pa, temperature T is 77 ℃, sample cell volume V is 12.5mL, ideal gas constant R=8.314J/ (molK), calculates amount of substance n=1.37 * 10 of the volatile matter in explosive by equation pV=nRT
-8mol.
Embodiment 2
1gTATB explosive is joined in the sample cell of improved microcalorimeter, sample cell is vacuumized, in the control system of improved microcalorimeter, set initial temperature and be 25 ℃, stand-by period and be 15min, constant temperature time 15min, 5 ℃ of intensification strides, reaction and judge that susceptibility-0.02 ℃/min and reaction terminating condition are as heating rate >=0.05 ℃/min, starter gear heating, it is identical with embodiment 1 with the process judged that equipment heats, and the data of only judging are used the data of the present embodiment.While heating rate >=0.05 ℃/min being detected, instrument test enters termination phase, even if the present embodiment improved microcalorimeter when heating rate just surpasses 0.05 ℃/min enters termination phase.
In the process heating at improved microcalorimeter, the pressure in sample cell, temperature and changes of heat flux situation are carried out to real-time synchronization record, obtain pressure-time curve, temperature-time curve and hot-fluid-time curve.Volatile matter volatilizees completely substantially and energetic material starts to decompose hot-fluid, pressure in front curve and is definite value, pressure p after calibration is 5.81Pa, temperature T is 80 ℃, sample cell volume V is 12.5mL, ideal gas constant R=8.314J/ (molK), calculates amount of substance n=2.47 * 10 of the volatile matter in explosive by equation pV=nRT
-8mol.
Embodiment 3
2gPETN explosive is joined in the sample cell of improved microcalorimeter, sample cell is vacuumized, in the control system of improved microcalorimeter, set initial temperature and be 21 ℃, stand-by period and be 10min, constant temperature time 25min, 0.2 ℃ of intensification stride, reaction and judge that susceptibility-0.02 ℃/min and reaction terminating condition are as heating rate >=0.05 ℃/min, it is identical with embodiment 1 with the process judged that equipment heats, and the data of only judging are used the data of the present embodiment.While heating rate >=0.05 ℃/min being detected, instrument test enters termination phase, even if the present embodiment improved microcalorimeter when heating rate just surpasses 0.05 ℃/min enters termination phase.
In the process heating at improved microcalorimeter, the pressure in sample cell, temperature and changes of heat flux situation are carried out to real-time synchronization record, obtain pressure-time curve, temperature-time curve and hot-fluid-time curve.Volatile matter volatilizees completely substantially and energetic material starts to decompose hot-fluid, pressure in front curve and is definite value, pressure p after calibration is 10.82Pa, temperature T is 78.2 ℃, sample cell volume V is 12.5mL, ideal gas constant R=8.314J/ (molK), calculates amount of substance n=4.63 * 10 of the volatile matter in explosive by equation pV=nRT
-8mol.
Although with reference to a plurality of explanatory embodiment of the present invention, invention has been described here, but, should be appreciated that, those skilled in the art can design a lot of other modification and embodiments, and these are revised and within embodiment will drop on the disclosed principle scope and spirit of the application.More particularly, in the scope of, accompanying drawing open in the application and claim, can carry out multiple modification and improvement to the building block of subject combination layout and/or layout.Except modification that building block and/or layout are carried out with improving, to those skilled in the art, other purposes will be also obvious.
Claims (9)
1. a device of measuring volatile matter content in explosive, comprise microcalorimeter, it is characterized in that described device is to install for measuring the pressure transducer of real-time pressure in sample cell on the sample cell of microcalorimeter, and arrange and form as lower device in the control system of microcalorimeter:
Reading device
Be connected with the control system signal of microcalorimeter, for in the temperature of sample cell, rise to the default initial temperature of microcalorimeter or by intensification stride, heat up after temperature time read microcalorimeter stand-by period, when the stand-by period of microcalorimeter expires, transmit enabling signal to searcher;
Searcher
Receive the enabling signal of reading device, then in the default constant temperature time of microcalorimeter, search for the sample cell heating rate signal that microcalorimeter detects and pass to comparison means;
Comparison means
In the default constant temperature time of microcalorimeter, receive the sample cell heating rate signal searching of searcher, and react default with microcalorimeter judges that susceptibility and reaction terminating condition compare, when the absolute value of susceptibility is judged in the absolute value < reaction that sample cell heating rate does not reach reaction terminating condition and perseverance has sample cell heating rate in this constant temperature time, after this constant temperature time finishes, to microcalorimeter, send the signal heating up by intensification stride; When sample cell heating rate does not reach reaction terminating condition and occur that in this constant temperature time the absolute value of susceptibility is judged in the absolute value of sample cell heating rate >=reaction, after this constant temperature time finishes, to the control system of microcalorimeter, send the signal of repetition constant temperature time; When sample cell heating rate reaches reaction terminating condition, to the control system transmission termination test signal of microcalorimeter.
2. a method that adopts volatile matter content in device to test explosive as claimed in claim 1, is characterized in that it comprises the steps:
(1) explosive that contains in right amount volatile matter is joined in the sample cell of microcalorimeter, then sample cell is vacuumized;
(2) in the control system of microcalorimeter, set initial temperature, stand-by period, constant temperature time, intensification stride, reaction judgement susceptibility and reaction terminating condition;
(3) sample cell is warmed up to initial temperature;
(4) waiting temperature balance;
(5) after equalized temperature, search for temperature, hot-fluid, pressure and the sample cell heating rate under the same time, by sample cell heating rate and reaction terminating condition and react and judge that susceptibility compares;
(6) when the absolute value of susceptibility is judged in the absolute value < reaction that sample cell heating rate does not reach reaction terminating condition and perseverance has sample cell heating rate in this constant temperature time, after this constant temperature time finishes, microcalorimeter heats up to sample cell by intensification stride;
(7) then repeating step (4), (5), (6), when sample cell heating rate does not reach reaction terminating condition and occur that in this constant temperature time the absolute value of susceptibility is judged in the absolute value of sample cell heating rate >=reaction, after this constant temperature time finishes, again enter next constant temperature time section, then repeating step (5), (6), until sample cell heating rate end of test while reaching reaction terminating condition;
(8) then take pressure, hot-fluid, the temperature of step (5) gained is ordinate, and its corresponding time is horizontal ordinate, makes pressure/hot-fluid/temperature-time curve;
(9), when the pressure of step (8) gained pressure/hot-fluid/temperature-time curve in the same time period before end of test and hot-fluid are definite value, the corresponding pressure of pressure/hot-fluid/temperature-time curve in this time period of take is p
1, temperature is T;
(10) by the Al adding in the empty sample cell of microcalorimeter with explosive charge same volume
2o
3, after extracting vacuum, being increased the temperature to T, the force value of measuring is now p
2, with p=p
1-p
2, and to take the volume of sample cell be V, ideal gas constant is R, utilizes the Ideal-Gas Equation pV=nRT through calculating the amount of substance n of the volatile matter in explosive.
3. the method for volatile matter content in test explosive according to claim 2, is characterized in that described explosive keeps stable chemical nature when the volatilization temperature less than or equal to volatile matter.
4. the method for volatile matter content in test explosive according to claim 2, is characterized in that described initial temperature is lower than the decomposition temperature of volatilization temperature and the explosive of volatile matter in explosive.
5. the method for volatile matter content in test explosive according to claim 2, is characterized in that described intensification stride is set as 0.2～5 ℃.
6. the method for volatile matter content in test explosive according to claim 2, is characterized in that described reaction judges that susceptibility is set as-0.02 ℃/min～-0.005 ℃/min.
7. the method for volatile matter content in test explosive according to claim 2, is characterized in that the described stand-by period is set as 5～15min.
8. the method for volatile matter content in test explosive according to claim 1, is characterized in that described constant temperature time is set as 15～30min.
9. the method for volatile matter content in test explosive according to claim 1, is characterized in that described reaction terminating condition is heating rate >=0.05 ℃/min.
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| CN110907496A (en) * | 2019-12-10 | 2020-03-24 | 福州大学 | Experimental device and test method for inducing explosive auto-explosion of sulfide ore |
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