CN113189215A - Air environment propellant heated CO2Quick automatic detection device of content - Google Patents
Air environment propellant heated CO2Quick automatic detection device of content Download PDFInfo
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- CN113189215A CN113189215A CN202110356553.0A CN202110356553A CN113189215A CN 113189215 A CN113189215 A CN 113189215A CN 202110356553 A CN202110356553 A CN 202110356553A CN 113189215 A CN113189215 A CN 113189215A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/66—Thermal conductivity detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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Abstract
The invention discloses CO generated after heating of propellant powder in air environment2Quick automatic checkout device of content. The device comprises a tank body, a cap, a cooling pipe, a heating furnace, a gas production device and a gas chromatograph. The propellant powder is filled into a tank body, a cap is screwed, and the propellant powder can be directly pumped for detection after being heated for 3 hours at 90 ℃. The gas in the tank flows through the cooling pipe and is injected into the gas chromatograph by the air extracting pump through the Shiviaoke quick joint, and CO in the gas can be detected2And (4) content. The device reduces the post-cooling time of sample heating and shortens the detection time; the automatic sample introduction reduces the manual operation error and increases the accuracy of the detection result.
Description
Technical Field
The invention belongs to the field of gas quantitative detection, mainly relates to a rapid and automatic detection device for the content of thermal decomposition gas of propellant powder, and particularly relates to the thermal decomposition of single-base propellant powderCO in gas2And (4) quickly and automatically detecting the content.
Background
The propellant powder is one of energy sources for firing gun shots, and plays a certain role in gun weapons.
The propellant has the characteristics of long-term storage and one-time use, and has to have better stability. The stability of the propellant is mainly chemical stability, which means the ability to delay decomposition and prevent automatic chemical changes during storage. The propellant contains nitrate compounds such as nitrocellulose, which contain nitrate groups and can be decomposed slowly by itself to obtain gaseous decomposition products (such as NO)2NO, water vapor and HNO3) Has catalytic action on the thermal decomposition of the nitrate ester compound, and can even improve the decomposition speed of the nitrate ester compound by tens of times.
The different gaseous decomposition products have different effects on the decomposition of nitrocellulose, NO2Can directly accelerate the oxidative decomposition (NO) of the nitrocellulose2The NO is oxidized with nitrocellulose to form NO, and the NO is further oxidized to form NO2) While NO2The inorganic acid generated with water can also accelerate the hydrolysis reaction of the nitrocellulose.
The decomposition of nitrate can be accelerated by increasing the temperature, for example, at (70-130 ℃) the decomposition speed of nitrocellulose is increased along with the increase of the temperature, and when the temperature is increased to more than 140 ℃, the decomposition of nitrocellulose becomes very violent. Therefore, the decomposition condition of the propellant containing the nitrate compound can be detected in a short time by adopting a method of raising the temperature, and the chemical stability information can be obtained.
Heating propellant at 90 deg.C for 3 hr, and detecting CO in decomposed gas2The chemical stability of the propellant can be evaluated. The current operating method is as follows: loading 10g propellant into a metal sample can, screwing a metal bottle cap (with a small hole at the top end of the sample can cap, sealing with a silica gel pad), placing into a 90 deg.C oven, timing half an hour later, taking out after 3 hours, cooling at room temperature for 30min, and injecting from the sample can with a syringe (sealed with oil to prevent air leakage)Extracting 1ml of gas, injecting into a gas chromatograph, and detecting CO in the gas2And (4) content. Each sample tank is repeatedly subjected to air suction testing for 2 times, and when the area difference between two peaks is not more than 5%, the testing result is effective; the indirect external standard calibration is carried out on the samples to be measured by using air, dry air is extracted by using an injector and injected into a chromatograph, the measurement is repeatedly carried out for 3 times, the difference of the area of the peaks of the adjacent 3 times is not more than 5%, and the average value of the 3 times of measurement is taken as the peak value of standard air (nitrogen and oxygen are one combined peak in a chromatogram); if CO is in the air2If the content is higher, two empty cups are filled at the same time for correction; decomposition of CO in gas2Volume content ═ CO2Chromatographic peak area 1.3 divided by calibrated air chromatographic peak area 100%, if CO in air2Higher levels should be removed from the results.
The following disadvantages are available in practical application:
(1) after the sample tank is heated, the sample tank needs to be cooled for 30min, and the gas can be extracted by the injector only after the gas pressure in the tank is reduced, so that the whole detection time is long;
(2) gas is extracted from the tank manually and injected into the chromatograph, so that gas leakage is easy to occur in the operation process, and the accuracy of the detection result is influenced; the air extraction operation has higher requirements on the proficiency of personnel, the accuracy of the gas volume is greatly influenced by human factors, and the fluctuation of the detection result is increased.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides CO after the propellant powder in the air environment is heated2The device for quickly and automatically detecting the content comprises a tank body 1, a cap 2, a cooling pipe 3, a heating furnace 4, a gas production device 5 and a gas chromatograph 6;
the tank body 1 is a barrel, the wall thickness of the tank body 1 is 2mm, the outer diameter is 30mm, the outer height is 80mm, the upper end part of the outer surface of the tank body 1 is a first external thread area, the height of the first external thread area is 10mm, and the tank body 1 is made of 316 stainless steel;
the outer diameter of the cap 2 is 36mm, the outer height of the cap is 12mm, the inner depth of the cap is 10mm, a second internal thread area with the height of 9mm is arranged on the cap 2 from the bottom end to the top, the second internal thread area is matched with the threads of the first external thread area of the tank body 1, and an air hole with the diameter of 1mm is formed in the center of the circle on the upper surface of the cap 2; the uppermost end in the cap 2 is provided with a second sealing ring, and the outer diameter, the inner diameter and the thickness of the second sealing ring are 30mm, 26mm and 1.5mm respectively; the second sealing gasket is made of silicon rubber, and the rest materials are 316 stainless steel;
the cap 2 is positioned right above the tank body 1;
the cooling pipe 3 is in a spring shape and consists of 4 spring rings with the maximum outer diameter of 20mm, and the spacing between the spring rings is 3 mm; the cooling pipe 3 is made of 316 stainless steel;
the cooling pipe 3 is positioned right above the cap 2, one end of the cooling pipe is welded at the center of the upper surface of the cap 2, the inside of the cooling pipe 3 is communicated with the air hole 8 of the cap 2, and the other end of the cooling pipe 3 is partially sealed at the pipe orifice by a Shiviaoke quick joint A;
the heating furnace 4 is a cylinder, heating holes are uniformly distributed on the upper plane of the heating furnace 4 along the circumference, the depth of each heating hole is 70mm, and the diameter of each heating hole is 31 mm;
the tank body 1 is positioned right above the heating hole of the heating furnace 4;
the gas production device 5 consists of a left part, a middle part and a right part, the left part of the gas production device 5 is a gas production pipe Vivialack quick connector B part, the middle part of the gas production device 5 is a quantitative pipe, and the right part of the gas production device 5 is an air extraction pump; the gas production pipe is made of polytetrafluoroethylene; the left end of the gas production pipe of the gas production device 5 is sealed by a Shiweioke quick connector B part, and the Shiweioke quick connector B part is matched with the Shiweioke quick connector A part of the cooling pipe 5; the right end of the gas production pipe is connected with an air pump through a quantitative pipe, and the volume of the quantitative pipe is 0.5 mL;
a quantitative tube and an air pump in the gas production device 5 are arranged inside the gas chromatograph 6, and a gas production tube is positioned outside the gas chromatograph 6; the gas production device 5 is not connected with the tank body 1, the cap 2, the cooling pipe 3 and the heating furnace 4;
the gas chromatograph 6 comprises a chromatographic column, a thermal conductivity detector and a workstation; starting a work station air pump, feeding a sample by a quantitative tube, adjusting the temperature of a chromatographic column, adjusting the temperature of a thermal conductivity detector, and recording the area of a chromatographic peak;
the gas chromatograph 6 is not connected with the tank body 1, the cap 2, the cooling pipe 3 and the heating furnace 4;
the above-mentionedAir environment propellant heated CO2The use method of the rapid automatic content detection device comprises the following steps:
step 7, emitting CO in the reaction gas of the medicine sample2Volume content is CO in gas in reaction tank containing propellant2Volume content-CO in empty retort gas2Volume content;
CO after heated propellant powder in air environment2The rapid automatic detection device for the content is characterized in that the reaction tank is directly pumped out for detection without being taken out of the heating furnace 4 after being heated for 3 hours at 90 ℃.
CO after heated propellant powder in air environment2The rapid automatic detection device for the content is characterized in that the reaction tank is taken out of the heating furnace 4 after being heated for 3 hours at 90 ℃, placed at room temperature and exhausted within 6 hours for detection
The invention mainly focuses on the following problems and carries out corresponding technical design when overcoming the defects of the prior method:
(1) the condensing device is added, so that the gas entering the chromatograph for detection can be rapidly cooled
The cooling pipe 3 is spring-shaped and consists of 4 spring rings with the maximum outer diameter of 20mm, and the spacing between the spring rings is 3 mm. The spring-like part can not only cool the hot gas passing through the cooling pipe, but also make the whole condensation part compact in volume, and after the reaction tank is assembled, the reaction tank is guaranteed to have better stability. One end of the cooling pipe is welded with the cover of the reaction tank from the outside, and the other end of the cooling pipe is connected with the part A of the Shiweiroc quick connector; the Shiviaroc quick connector A has a sealing function, and gas in the reaction tank cannot leak from the cooling pipe.
The cooling pipe is fixed on the cover, and in order to keep the cooling pipe at room temperature all the time, the heating mode of the reaction tank is changed from the original oven to the heating furnace. According to the stacking height of the propellant powder sample in the reaction tank, the size of the heating hole of the heating furnace is determined, so that the sample can be completely in a heating environment of 90 ℃, and the cooling pipe can be prevented from being heated.
(2) The manual sampling is changed into the automatic sampling, the air leakage probability is reduced, and the gas volume accuracy is high
The Shivaloke quick joint A part is matched with the Shivaloke quick joint B part, when the Shivaloke quick joint A part is not connected with the Shivaloke quick joint B part, the A part has sealing performance and seals the port of the cooling pipe, so that after the tank body 1 and the cap 2 are screwed, the tank body 1, the cap 2 and the cooling pipe 3 form a closed space, and gas in the space is not communicated with the atmosphere. Only after the portion B of the swagelok quick coupling is inserted into the portion a of the swagelok quick coupling does the portion a of the swagelok quick coupling no longer have a sealing function and become a passage. At the moment, the air pump works, gas in the reaction tank enters the quantitative pipe through the condenser pipe and the gas production pipe, and then is automatically injected into the chromatographic column for separation and detected by the thermal conductivity detector.
(3) The change related to the rapid automatic detection can not reduce the detection limit, the accuracy and the precision of the detection result
The air pump is arranged in the gas chromatograph, the gas chromatograph workstation controls the air pump to pump air, gas in the reaction tank enters the gas production pipe and the air pump through the condensation pipe, and the initial section gas is mixed with the original air in the gas production pipe, so that the initial section gas is not equal to the gas in the reaction tank, and the intermediate section gas is taken and sent into the quantitative pipe and then automatically injected into the chromatograph to be detected. Compared with the original sample tank, the gas extraction device has the advantages that the cooling pipe and the gas extraction pipe are additionally arranged, and in addition, only middle-section gas can be adopted, so that the gas quantity extracted from the reaction tank by the gas extraction pump is larger and is far larger than the gas quantity entering the chromatogram specified by the original method.
The air extraction amount of the original method is 1mL, which is considered that the error of manual air extraction and sample injection operation is large, so that the larger the air extraction amount is, the smaller the influence of the error of the manual air extraction and sample injection operation on the detection result is. If automatic air suction and sample injection are adopted, the error caused by the automatic air suction and sample injection can be obviously reduced, and the detection air quantity can be correspondingly reduced. But because of decomposition of CO in the gas2The content is low, so the detection gas amount cannot be too small, otherwise the detection limit is too high. In the original manual sampling detection method, the air suction test is repeated for 2 times for each sample tank, and when the area difference between two peaks is not more than 5 percent, the determination result is effectiveWhen the method is used for automatic air extraction and sample injection, if the requirement of 2 times of air extraction test is met, the detection air quantity is extremely possibly too small. Namely, the requirements of 'effective criterion of original determination result' and 'detection limit can not be reduced' can not be met at the same time.
The deep analysis shows that: when the original manual detection is changed into the automatic detection of the invention, the detection limit can not be reduced firstly, and the part of the original determination result effective criterion can be reestablished. And comprehensively considering, and finally determining the detection gas amount to be 0.5 mL. On the basis, the effective criterion of the measured result is reestablished.
A testing cap is designed, the testing cap is provided with a ventilation hole more than the cap of the invention, the inner diameter of the ventilation hole is 0.1mm, and the ventilation hole is positioned at the position 5mm from the center of the testing cap (the ventilation hole is plugged by Vaseline). A reaction vessel was assembled with a test cap instead of the cap of the present invention, and 10g of propellant was charged into the reaction vessel. According to the method of the invention, after the gas in the reaction tank assembled by the testing cap is pumped out, the tank is in a negative pressure state, and the air at the ambient temperature enters the tank through the vent hole (the vaseline is pumped into the reaction tank by the negative pressure). Due to CO in the environment2The content of CO is lower than that of decomposed gas in the tank2Content, so gas in the reaction tank is extracted for multiple times for detection, CO2The content of the carbon dioxide is gradually reduced until the CO in the environment is approached2And (4) content.
Weighing 10.0487g of mono-pine propellant powder, placing into a reaction tank (equipped with a cap containing a vent hole), heating at 90 deg.C for 3 hr by the method of the invention, continuously detecting gas in the tank, wherein the gas chromatogram of the thermolysis of the propellant powder is shown in FIG. 1, and detecting CO for 6 times2The content of CO in air was 0.264%, 0.191%, 0.150%, 0.124%, 0.109%, 0.101% (no subtraction of CO in air from the test results)2Content(s). It can be seen that CO2The content is rapidly reduced and approaches to CO in the air2Content (CO in laboratory air)2Content 0.06%). This is because the propellant generates CO when heated2When the gas in the tank is pumped away by the air pump, no new CO is available in a short time2Generating, the air at normal temperature enters the tank through the vent hole, and finally the CO in the tank2Stable approach to skyCO in gas2And (4) content.
Another empty reaction tank (provided with a cap with a vent hole and without a propellant sample) is heated at 90 ℃ for 3 hours by the method of the invention, the gas in the empty reaction tank is continuously detected for 6 times totally, and CO is detected2The chromatographic peak areas are 65207, 64867, 65195, 65535, 65681 and 66191 respectively, the chromatographic peak areas of oxygen and air are 84485027, 83299734, 83292731, 83856192, 83662190 and 83461735 respectively, and the calculated CO can be obtained2The content is 0.059%, 0.060%, 0.061%. It is shown that the detection data of the invention is very stable when the composition of the gas to be detected is unchanged. Prove that in the thermal decomposition test of the mono-pine propellant, CO is generated2The content is continuously reduced because the gas in the reaction tank changes.
Therefore, even if the detection gas amount is 0.5mL, the gas in each reaction tank can be detected only by sampling 1 time.
In the original method, "each sample tank is repeatedly pumped and tested for 2 times, when the area difference between two peaks is not more than 5%, the determination result is effective", mainly aiming at the manual pumping and sample injection detection, the artificial error is large, and the sample injection operation repeatability of each sample tank is regulated for limiting the influence of the error on the detection result. In the above empty retort test: CO 22In the chromatographic peak area detection results, the minimum area of 6 chromatographic peaks is 64867, the maximum area is 66191, and the difference of the two peak areas is 2.0%; the oxygen and nitrogen chromatographic peak areas were 83292731 at the minimum and 84485027 at the maximum, with a 1.4% difference in peak areas. CO 22The chromatographic peak area difference value and the oxygen and nitrogen chromatographic peak area difference value all meet the requirement that the air extraction test is repeated for 2 times for each sample tank, and when the difference between the two peak areas is not more than 5 percent, the measurement result is effective, which indicates that the method has the advantages of automatic air extraction and sample injection, very good repeatability and CO in the gas in the empty reaction tank2The chromatographic peak area, the oxygen and nitrogen chromatographic peak areas can all represent the stability of the state of the instrument.
Taking into account some CO in laboratory air2May be too low, and therefore the stability of the instrument state as characterized by the oxygen and nitrogen chromatographic peak areas is determined, so "determineThe new criterion of valid result is determined as follows: "detect the gas in 2 empty unheated retort, when the chromatographic peak area difference of oxygen and nitrogen gas that 2 times detected is not more than 5%, judge the instrument state is stable, can begin to detect propellant decomposition gas.
The beneficial effects of the invention are shown in the following aspects:
(1) through the arrangement of a built-in pump, a Shiviaoke quick connector, a quantitative pipe and the like, gas is extracted from a tank and injected into a chromatograph, no gas leakage exists in the operation process, the accuracy and the repeatability of the volume of the extracted gas have no human influence factors, and the repeatability of a detection result is good;
(2) after the sample tank is heated, the cooling pipe connected with the reaction tank can rapidly cool the gas in the pumped tank and reduce the pressure, the detection can be carried out without cooling for 30min, the detection efficiency is improved, and the whole detection time is shortened.
Drawings
FIG. 1 is a schematic view of the apparatus. 1. The device comprises a tank body, 2, a cap, 3, a cooling pipe, 4, a heating furnace, 5, a gas production device and 6 and a gas chromatograph.
FIG. 2 is a chromatogram of propellant decomposition gas and air.
Detailed Description
The invention is described in further detail below with reference to the drawings and preferred embodiments.
Example 1
12/1-32 single-base propellant powder heated CO is detected by the patent2And (4) content.
As shown in figure 1, an air environment propellant is heated to CO2The device for quickly and automatically detecting the content comprises a tank body 1, a cap 2, a cooling pipe 3, a heating furnace 4, a gas production device 5 and a gas chromatograph 6;
the tank body 1 is a barrel, the wall thickness of the tank body 1 is 2mm, the outer diameter is 30mm, the outer height is 80mm, the upper end part of the outer surface of the tank body 1 is a first external thread area, the height of the first external thread area is 10mm, and the tank body 1 is made of 316 stainless steel;
the outer diameter of the cap 2 is 36mm, the outer height of the cap is 12mm, the inner depth of the cap is 10mm, a second internal thread area with the height of 9mm is arranged from the bottom end to the top of the cap 2, the second internal thread area is matched with the threads of the first external thread area of the tank body 1, and an air hole with the diameter of 1mm is arranged at the center of the circle on the upper surface of the cap 2); the uppermost end in the cap 2 is provided with a second sealing ring, and the outer diameter, the inner diameter and the thickness of the second sealing ring are 30mm, 26mm and 1.5mm respectively; the second sealing gasket is made of silicon rubber, and the rest materials are 316 stainless steel;
the cap 2 is positioned right above the tank body 1;
the cooling pipe 3 is in a spring shape and consists of 4 spring rings with the maximum outer diameter of 20mm, and the spacing between the spring rings is 3 mm; the cooling pipe 3 is made of 316 stainless steel;
the cooling pipe 3 is positioned right above the cap 2, one end of the cooling pipe is welded at the center of the upper surface of the cap 2, the inside of the cooling pipe 3 is communicated with the air hole 8 of the cap 2, and the other end of the cooling pipe 3 is partially sealed at the pipe orifice by a Shiviaoke quick joint A;
the heating furnace 4 is a cylinder, heating holes are uniformly distributed on the upper plane of the heating furnace 4 along the circumference, the depth of each heating hole is 70mm, and the diameter of each heating hole is 31 mm;
the tank body 1 is positioned right above the heating hole of the heating furnace 4;
the gas production device 5 consists of a left part, a middle part and a right part, the left part of the gas production device 5 is a gas production pipe Vivialack quick connector B part, the middle part of the gas production device 5 is a quantitative pipe, and the right part of the gas production device 5 is an air extraction pump; the gas production pipe is made of polytetrafluoroethylene; the left end of the gas production pipe of the gas production device 5 is sealed by a Shiweioke quick connector B part, and the Shiweioke quick connector B part is matched with the Shiweioke quick connector A part of the cooling pipe 3; the right end of the gas production pipe is connected with an air pump through a quantitative pipe, and the volume of the quantitative pipe is 0.5 mL;
a quantitative tube and an air pump in the gas production device 5 are arranged inside the gas chromatograph 6, and a gas production tube is positioned outside the gas chromatograph 6; the gas production device 5 is not connected with the tank body 1, the cap 2, the cooling pipe 3 and the heating furnace 4;
the gas chromatograph 6 comprises a chromatographic column, a thermal conductivity detector and a workstation; starting a work station air pump, feeding a sample by a quantitative tube, adjusting the temperature of a chromatographic column, adjusting the temperature of a thermal conductivity detector, and recording the area of a chromatographic peak;
the gas chromatograph 6 is not connected with the tank body 1, the cap 2, the cooling pipe 3 and the heating furnace 4;
CO after the propellant powder in air environment is heated2The use method of the rapid automatic content detection device comprises the following steps:
step 7, emitting CO in the reaction gas of the medicine sample2Volume content is CO in gas in reaction tank containing propellant2Volumetric content-CO in heated empty retort gas2Volume content;
This example detects 12/1-32 CO after heating of a single-base propellant2The content, the detection result is 0.13%, 0.14%. The detection results of manual air suction detection by the original method are 0.11 percent and 0.16 percent. As can be seen from the detection results, in the original method, because the air is extracted manually, the influence of human factors on the detection results is large, and therefore the fluctuation of the detection results is large. The large fluctuation of the detection result means that the repeatability of the detection result is poor and the precision is low, and the high precision is the premise of high precision in the detection work, which shows that the detection result of the invention has higher reliability in the aspect of precision.
Example 2
The method is used for detecting the CO after the monoamine single-base propellant is heated2And (4) content.
As shown in figure 1, an air environment propellant is heated to CO2The device for quickly and automatically detecting the content comprises a tank body 1, a cap 2, a cooling pipe 3, a heating furnace 4, a gas production device 5 and a gas chromatograph 6;
the tank body 1 is a barrel, the wall thickness of the tank body 1 is 2mm, the outer diameter is 30mm, the outer height is 80mm, the upper end part of the outer surface of the tank body 1 is a first external thread area, the height of the first external thread area is 10mm, and the tank body 1 is made of 316 stainless steel;
the outer diameter of the cap 2 is 36mm, the outer height of the cap is 12mm, the inner depth of the cap is 10mm, a second internal thread area with the height of 9mm is arranged from the bottom end to the top of the cap 2, the second internal thread area is matched with the threads of the first external thread area of the tank body 1, and an air hole with the diameter of 1mm is arranged at the center of the circle on the upper surface of the cap 2); the uppermost end in the cap 2 is provided with a second sealing ring, and the outer diameter, the inner diameter and the thickness of the second sealing ring are 30mm, 26mm and 1.5mm respectively; the second sealing gasket is made of silicon rubber, and the rest materials are 316 stainless steel;
the cap 2 is positioned right above the tank body 1;
the cooling pipe 3 is in a spring shape and consists of 4 spring rings with the maximum outer diameter of 20mm, and the spacing between the spring rings is 3 mm; the cooling pipe 3 is made of 316 stainless steel;
the cooling pipe 3 is positioned right above the cap 2, one end of the cooling pipe is welded at the center of the upper surface of the cap 2, the inside of the cooling pipe 3 is communicated with the air hole 8 of the cap 2, and the other end of the cooling pipe 3 is partially sealed at the pipe orifice by a Shiviaoke quick joint A;
the heating furnace 4 is a cylinder, heating holes are uniformly distributed on the upper plane of the heating furnace 4 along the circumference, the depth of each heating hole is 70mm, and the diameter of each heating hole is 31 mm;
the tank body 1 is positioned right above the heating hole of the heating furnace 4;
the gas production device 5 consists of a left part, a middle part and a right part, the left part of the gas production device 5 is a gas production pipe Vivialack quick connector B part, the middle part of the gas production device 5 is a quantitative pipe, and the right part of the gas production device 5 is an air extraction pump; the gas production pipe is made of polytetrafluoroethylene; the left end of the gas production pipe of the gas production device 5 is sealed by a Shiweioke quick connector B part, and the Shiweioke quick connector B part is matched with the Shiweioke quick connector A part of the cooling pipe 3; the right end of the gas production pipe is connected with an air pump through a quantitative pipe, and the volume of the quantitative pipe is 0.5 mL;
a quantitative tube and an air pump in the gas production device 5 are arranged inside the gas chromatograph 6, and a gas production tube is positioned outside the gas chromatograph 6; the gas production device 5 is not connected with the tank body 1, the cap 2, the cooling pipe 3 and the heating furnace 4;
the gas chromatograph 6 comprises a chromatographic column, a thermal conductivity detector and a workstation; starting a work station air pump, feeding a sample by a quantitative tube, adjusting the temperature of a chromatographic column, adjusting the temperature of a thermal conductivity detector, and recording the area of a chromatographic peak;
the gas chromatograph 6 is not connected with the tank body 1, the cap 2, the cooling pipe 3 and the heating furnace 4;
CO after the propellant powder in air environment is heated2The use method of the rapid automatic content detection device comprises the following steps:
step 7, CO in the propellant reaction gas in each reaction tank2Volume content is CO in gas in reaction tank containing propellant2Volumetric content-CO in heated empty retort gas2Volume content;
This example detects CO after heating of monoamine Mono-based propellant2The content is as follows: the sample is not taken out of the heating furnace 4, and the detection results of direct detection are 0.053% and 0.055%; taking out from the heating furnace 4, standing at room temperature for 30min, and detecting results are 0.054% and 0.055%. The detection result shows that the detection result of the uncooled reaction tank after heating is consistent with the detection result after cooling, which shows that the cooling pipe of the device can rapidly cool the gas to be detected, so that the heated reaction tank can be directly detected without being placed for 30min at room temperature for cooling. The invention has the advantage of shorter detection time because no after-cooling time is needed.
Example 3
Use this patent to detect single pine list base propellant powder CO after being heated2And (4) content.
As shown in figure 1, an air environment propellant is heated to CO2The device for quickly and automatically detecting the content comprises a tank body 1, a cap 2, a cooling pipe 3, a heating furnace 4, a gas production device 5 and a gas chromatograph 6;
the tank body 1 is a barrel, the wall thickness of the tank body 1 is 2mm, the outer diameter is 30mm, the outer height is 80mm, the upper end part of the outer surface of the tank body 1 is a first external thread area, the height of the first external thread area is 10mm, and the tank body 1 is made of 316 stainless steel;
the outer diameter of the cap 2 is 36mm, the outer height of the cap is 12mm, the inner depth of the cap is 10mm, a second internal thread area with the height of 9mm is arranged from the bottom end to the top of the cap 2, the second internal thread area is matched with the threads of the first external thread area of the tank body 1, and an air hole with the diameter of 1mm is arranged at the center of the circle on the upper surface of the cap 2); the uppermost end in the cap 2 is provided with a second sealing ring, and the outer diameter, the inner diameter and the thickness of the second sealing ring are 30mm, 26mm and 1.5mm respectively; the second sealing gasket is made of silicon rubber, and the rest materials are 316 stainless steel;
the cap 2 is positioned right above the tank body 1;
the cooling pipe 3 is in a spring shape and consists of 4 spring rings with the maximum outer diameter of 20mm, and the spacing between the spring rings is 3 mm; the cooling pipe 3 is made of 316 stainless steel;
the cooling pipe 3 is positioned right above the cap 2, one end of the cooling pipe is welded at the center of the upper surface of the cap 2, the inside of the cooling pipe 3 is communicated with the air hole 8 of the cap 2, and the other end of the cooling pipe 3 is partially sealed at the pipe orifice by a Shiviaoke quick joint A;
the heating furnace 4 is a cylinder, heating holes are uniformly distributed on the upper plane of the heating furnace 4 along the circumference, the depth of each heating hole is 70mm, and the diameter of each heating hole is 31 mm;
the tank body 1 is positioned right above the heating hole of the heating furnace 4;
the gas production device 5 consists of a left part, a middle part and a right part, the left part of the gas production device 5 is a gas production pipe Vivialack quick connector B part, the middle part of the gas production device 5 is a quantitative pipe, and the right part of the gas production device 5 is an air extraction pump; the gas production pipe is made of polytetrafluoroethylene; the left end of the gas production pipe of the gas production device 5 is sealed by a Shiweioke quick connector B part, and the Shiweioke quick connector B part is matched with the Shiweioke quick connector A part of the cooling pipe 3; the right end of the gas production pipe is connected with an air pump through a quantitative pipe, and the volume of the quantitative pipe is 0.5 mL;
a quantitative tube and an air pump in the gas production device 5 are arranged inside the gas chromatograph 6, and a gas production tube is positioned outside the gas chromatograph 6; the gas production device 5 is not connected with the tank body 1, the cap 2, the cooling pipe 3 and the heating furnace 4;
the gas chromatograph 6 comprises a chromatographic column, a thermal conductivity detector and a workstation; starting a work station air pump, feeding a sample by a quantitative tube, adjusting the temperature of a chromatographic column, adjusting the temperature of a thermal conductivity detector, and recording the area of a chromatographic peak;
the gas chromatograph 6 is not connected with the tank body 1, the cap 2, the cooling pipe 3 and the heating furnace 4;
CO after the propellant powder in air environment is heated2The use method of the rapid automatic content detection device comprises the following steps:
step 7, emitting CO in the reaction gas of the medicine sample2Volume content is CO in gas in reaction tank containing propellant2Volumetric content-CO in heated empty retort gas2Volume content.
Heated CO of mono-pine mono-base propellant2The detection results of the contents of the extract after being placed at room temperature for 0, 1, 2, 3, 4 and 6 hours are respectively 0.029%, 0.027%, 0.030%, 0.026%, 0.028% and 0.030%. The detection results show that: the reaction tank has good sealing effect, and can be placed at room temperature for no more than 6h after being taken out of the heating furnace, and the detection result cannot be changed.
Claims (3)
1. Air environment propellant heated CO2The device for quickly and automatically detecting the content comprises a tank body (1), a cap (2), a cooling pipe (3), a heating furnace (4), a gas production device (5) and a gas chromatograph (6);
the tank body (1) is a barrel body, the wall thickness of the tank body (1) is 2mm, the outer diameter is 30mm, the outer height is 80mm, the upper end part of the outer surface of the tank body (1) is a first external thread area, the height of the first external thread area is 10mm, and the tank body (1) is made of 316 stainless steel;
the outer diameter of the cap (2) is 36mm, the outer height of the cap is 12mm, the inner depth of the cap is 10mm, a second internal thread area with the height of 9mm is arranged from the bottom end of the cap (2) to the top, the second internal thread area is matched with the thread of the first external thread area of the tank body (1), and an air hole with the diameter of 1mm is formed in the circle center of the upper surface of the cap (2); the uppermost end in the cap (2) is provided with a second sealing ring, and the outer diameter, the inner diameter and the thickness of the second sealing ring are 30mm, 26mm and 1.5mm respectively; the second sealing gasket is made of silicon rubber, and the rest materials are 316 stainless steel;
the cap (2) is positioned right above the tank body (1);
the cooling pipe (3) is in a spring shape and consists of 4 spring rings with the maximum outer diameter of 20mm, and the spacing between the spring rings is 3 mm; the cooling pipe (3) is made of 316 stainless steel;
the cooling pipe (3) is positioned right above the cap (2), one end of the cooling pipe is welded at the center of the circle of the upper surface of the cap (2), the inside of the cooling pipe (3) is communicated with the air hole (8) of the cover (2), and the other end of the cooling pipe (3) is partially sealed at the pipe orifice by a Shiviaoke quick coupling A;
the heating furnace (4) is a cylinder, heating holes are uniformly distributed on the upper plane of the heating furnace (4) along the circumference, the depth of each heating hole is 70mm, and the diameter of each heating hole is 31 mm;
the tank body (1) is positioned right above the heating hole of the heating furnace (4);
the gas production device (5) consists of a left part, a middle part and a right part, the left part of the gas production device (5) is a gas production pipe Vivialack quick joint B part, the middle part of the gas production device (5) is a quantitative pipe, and the right part of the gas production device (5) is an air pump; the gas production pipe is made of polytetrafluoroethylene; the left end of the gas production pipe of the gas production device (5) is sealed by a Shiweioke quick joint B part, and the Shiweioke quick joint B part is matched with the Shiweioke quick joint A part of the cooling pipe (3); the right end of the gas production pipe is connected with an air pump through a quantitative pipe, and the volume of the quantitative pipe is 0.5 mL;
a quantitative tube and an air pump in the gas production device (5) are arranged in the gas chromatograph (6), and a gas production tube is positioned outside the gas chromatograph (6); the gas production device (5) is not connected with the tank body (1), the cap (2), the cooling pipe (3) and the heating furnace (4);
the gas chromatograph (6) comprises a chromatographic column, a thermal conductivity detector and a workstation; starting a work station air pump, feeding a sample by a quantitative tube, adjusting the temperature of a chromatographic column, adjusting the temperature of a thermal conductivity detector, and recording the area of a chromatographic peak;
the gas chromatograph (6) is not connected with the tank body (1), the cap (2), the cooling pipe (3) and the heating furnace (4);
CO after the propellant powder in air environment is heated2The use method of the rapid automatic content detection device comprises the following steps:
step 1, processing 30 g of propellant powder into blocks with length, width and height not greater than 8 mm;
step 2, placing the tank body (1) on a workbench with an upward opening, loading 10g of block propellant powder, screwing down the cap (2), and assembling the reaction tank; each propellant sample needs to be assembled into 2 sample tanks containing propellant samples as parallel samples; assembling 3 empty reaction tanks without propellant;
step 3, heating the heating furnace (4) to 90 ℃, after the temperature is stable, putting 1 empty reaction tank and the reaction tank filled with propellant powder into 3 heating holes of the heating furnace (4) one by one, emptying the reaction tanks firstly, and then putting the reaction tanks filled with the propellant powder, wherein each reaction tank is put in at an interval of 10 min; after each reaction tank is placed for 20min, the heating time is recorded; the remaining 2 empty reaction tanks were not heated;
step 4, starting the gas chromatograph (6), and setting the temperature of the detector to be 250 ℃ and the temperature of the chromatographic column to be 80 ℃; after the instrument is stabilized, pumping air to detect 2 empty reaction tanks which are not heated; inserting the Shivaloke quick joint B part of the gas production device (5) into the Shivaloke quick joint A part of the cooling pipe (3), and communicating a gas production pipe of the gas production device (5) with an internal gas circuit of the cooling pipe (3); a gas chromatograph (6) workstation controls an air pump, and air in the reaction tank is pumped into a quantitative pipe of an air extraction device (5) from a cooling pipe (3) and then injected into chromatographic column separation, a thermal conductivity detector detects and records the chromatographic peak areas of oxygen and nitrogen; comparing the peak areas of the oxygen and nitrogen chromatograms of the 2 empty reaction tanks, and judging that the state of the instrument is stable when the difference of the 2 peak areas is not more than 5 percent, so that the detection can be carried out;
step 5, heating the reaction tank at 90 ℃ for 3 hours, and then starting air extraction detection; inserting the Shivaloke quick joint B part of the gas production device (5) into the Shivaloke quick joint A part of the cooling pipe (3), and communicating a gas production pipe of the gas production device (5) with an internal gas circuit of the cooling pipe (3); a gas chromatograph (6) workstation controls an air pump, and air in the reaction tank is pumped into a quantitative pipe of an air extraction device (5) from a cooling pipe (3) and then injected into a chromatographic column for separation, a thermal conductivity detector for detection and chromatographic peak area recording; detecting the gas in the 3 heated reaction tanks according to the same step;
step 6, CO in the gas of the reaction tank2Volume content ═ CO2Chromatographic peak area ÷ 1.3) ÷ nitrogen and oxygen chromatographic peak area × 100%;
step 7, emitting CO in the reaction gas of the medicine sample2Volume content is CO in gas in reaction tank containing propellant2Volumetric content-CO in heated empty retort gas2Volume content;
step 8, 2 parallel sample samples of propellant powder and CO in reaction gas2The volume contents are not arithmetically averaged and are reported together as the detection result.
2. The air environment propellant powder of claim 1, wherein the CO is heated2The rapid automatic detection device for the content is characterized in that the reaction tank is directly pumped for detection without being taken out from the heating furnace (4) after being heated for 3 hours at 90 ℃.
3. The air environment propellant powder of claim 1, wherein the CO is heated2The rapid automatic detection device for the content is characterized in that a reaction tank is heated at 90 ℃ for 3 hours, taken out from a heating furnace (4), placed at room temperature, and subjected to air extraction detection within 6 hours.
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