CN108132328A - A kind of hydrazine gas detection method - Google Patents
A kind of hydrazine gas detection method Download PDFInfo
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- CN108132328A CN108132328A CN201611087751.7A CN201611087751A CN108132328A CN 108132328 A CN108132328 A CN 108132328A CN 201611087751 A CN201611087751 A CN 201611087751A CN 108132328 A CN108132328 A CN 108132328A
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- hydrazine
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
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Abstract
The present invention relates to a kind of hydrazine gas detection methods, air containing hydrazine is pre-processed first, and sets a series of decomposition environment, realizes the catalytic decomposition of hydrazine, by detecting the density of hydrogen of hydrazine decomposition product, finally the content of hydrazine steam is calculated with reference to the resolution ratio and temperature of hydrazine steam;The present invention carries out hydrazine Concentration Testing using completely new method, solves the problems, such as that current hydrazine detection method selectivity is not high, and can realize that on-line continuous measures.
Description
Technical field
The present invention relates to a kind of hydrazine gas detection method, particularly a kind of hydrazine gas using hydrazine catalytic decomposition mode detects
Method.
Background technology
Hydrazine is widely used as the propellant of spacecraft, has moderate toxicity, is potential carcinogen.Repeated exposure is in hydrazine atmosphere
In, the liver kidney of people can be damaged;It is exposed in high concentration atmosphere, spasm can be made one, so that it is dead.Hydrazine is due to low boiling point, vapour pressure
Height easily forms explosive mixture in air, causes an explosion accident.National regulation is in Hydrazine fuel air of workplace
Maximum permissible concentration is 0.13mg/m3.But during the use of hydrazine, due to run, drip, leak of propellant etc., operation
Hydrazine vapor concentration often occurs exceeded in place, and very big harm is brought to operating personnel.It therefore must be to the hydrazine of Work places
Vapor concentration is detected, with the health and safety of support personnel.The method of monitoring Detection of Trace Hydrazine in Air vapor concentration mainly has:Chemistry
Luminescence method, chemical sensor method, solid absorbent/spectrophotometry, chromatography, mass spectrography, detection tube method and personnel dosimeter
Deng.
Chemoluminescence method, chemical sensor method, solid absorbent/spectrophotometry, shortcoming are that selection is poor.Chromatography,
Mass spectrography, volume are too big complicated for operation and expensive.Detection tube method and personnel dosimeter can not realize continuous measurement and error
Also it is larger.
For the deficiency of current hydrazine detection method, a kind of high selectivity is invented, can continuously be measured, inexpensive hydrazine detection side
Method is very important.
Invention content
The present invention in order to solve hydrazine detection selectivity, continuous measurement capability, cost problem and propose it is a kind of catalysis point
Solution formula hydrazine detection method, first pre-processes air containing hydrazine, and sets a series of decomposition environment, realizes the catalysis point of hydrazine
Solution, by detecting the density of hydrogen of hydrazine decomposition product, finally calculates containing for hydrazine steam with reference to the resolution ratio and temperature of hydrazine steam
Amount.The present invention utilizes " hydrazine catalytic decomposition principle ", hydrazine is made to be decomposed into hydrogen and nitrogen, using the more ripe selectivity of technology only
One detection limits broader optics hydrogen detection technique, realizes the detection of hydrazine.
To achieve these goals, used technical solution is the present invention:A kind of hydrazine gas-detecting device, including sequence
Air intake duct, air processing unit, catalytic bed, air pump, hydrogen detection unit, microprocessor, the catalytic bed temperature controller of connection;
The air intake duct is connect with air processing unit arrival end;
The air processing unit port of export is connect with catalytic bed arrival end, and catalytic bed temperature-measuring port is inserted into catalytic bed temperature controller
Thermocouple, catalytic bed outer surface heater strip connect with catalytic bed temperature controller with conducting wire;The catalytic bed port of export enters with air pump
Mouth end is connected with pipeline;
Air pump control terminal is connect with microprocessor, and the air pump port of export is connect with hydrogen detection unit by pipeline;
Hydrogen detection unit signal output end is connect with microprocessor, output end of microprocessor and catalytic bed temperature controller
Control terminal connects.
The air processing unit is hollow container, and silica wool, drier are sequentially arranged with from entrance to outlet.
The drier be with the nonreactive drier of hydrazine, including CaO particles.
The catalytic bed is hollow tube, and catalyst for preparing hydrogen, outer tube wall winding heater strip is catalytically decomposed in inside filling hydrazine;Outer tube
Wall is equipped with groove or temperature-measuring port, for probeing into thermocouple;
A kind of hydrazine gas-detecting device, further includes display unit and alarm unit, is connect with microprocessor.
A kind of hydrazine gas detection method, includes the following steps:
When the catalytic bed temperature of catalytic bed temperature controller feedback is more than operating temperature ratings, air intake duct is with specified speed
Rate sucks the air for being mixed with hydrazine gas;
The air for being mixed with hydrazine gas being inhaled into is filtered out by the silica wool of air processing unit in air first
Then dust carries out removal moisture drying by CaO particles;
Filtered dried gas enters catalytic bed, and hydrazine decomposes in air;
Gas after decomposition enters hydrogen detection unit, detects hydrogen content;
The content of Detection of Trace Hydrazine in Air is obtained according to the detection limit of catalytic bed temperature, the setting resolution ratio of hydrazine, hydrogen.
The operating temperature ratings are 35 DEG C.
The nominal rated speed is 5mL/s.
The resolution ratio is completely decomposed into hydrogen and the hydrazine of nitrogen and the percentage of total hydrazine amount for hydrazine.
The detection limit according to catalytic bed temperature, the design resolution ratio of hydrazine, hydrogen show that the content of Detection of Trace Hydrazine in Air passes through
Following formula obtains:
CHydrazine=K*CHydrogen*(Vt*(T0+273)/(Tt+273))/2;
CHydrazineFor Detection of Trace Hydrazine in Air concentration;K is resolution ratio;CHydrogenThe concentration of hydrogen is detected for hydrogen detection unit;VtIt is specified
Rate;T0For environment temperature;TtFor catalytic bed temperature.
The invention has the advantages that and advantage:
1. the configuration of the present invention is simple, stabilization, detection limit for width;
2. carrying out hydrazine Concentration Testing using completely new method, solve the problems, such as that current hydrazine detection method selectivity is not high.
3. equipment can realize that on-line continuous measures.
4. the relatively general hydrazine detection device of the present invention greatly reduced system complexity and cost.
Description of the drawings
Fig. 1 is the system flow chart of hydrazine gas-detecting device.
Wherein, 1 air intake duct, 2 air processing units, 3 catalytic beds, 4 air pumps, 5 hydrogen detection units, 6 catalytic bed temperature controls
Device processed, 7 microprocessors, 8 display units, 9 alarm units.
Fig. 2 is the structure diagram of hydrazine gas-detecting device.
Wherein, 201 air intake ducts, 202 air processing units, 203 catalytic beds, 204 air pumps, 205 hydrogen detection units, 206
Temperature controller, 207 microprocessors, 208 microprocessor pwm output terminals, 209 display units, 210 alarm units.
Fig. 3 is the catalytic bed structure diagram of catalytic decomposition formula hydrazine device for fast detecting.
Fig. 4 is the control flow chart of catalytic decomposition formula hydrazine device for fast detecting.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and embodiments.
As shown in Figure 1, a kind of hydrazine gas-detecting device, including air intake duct, air processing unit, catalytic bed, air pump, hydrogen
Detection unit, catalytic bed temperature controller, microprocessor, display unit, alarm unit;
Air intake duct is connect with air processing unit arrival end with ferrule fitting;The air processing unit port of export enters with catalytic bed
Mouthful end flanged joint, catalytic bed temperature-measuring port are inserted into the thermocouple of catalytic bed temperature controller, catalytic bed outer surface heater strip with
Catalytic bed temperature controller is connected with conducting wire;The catalytic bed port of export is connect with air pump arrival end with pipeline;Air pump control terminal with it is micro-
Processor is connected with conducting wire, and the air pump port of export is connect with hydrogen detection unit by pipeline;Hydrogen detection unit signal output end
It is connect with microprocessor by conducting wire, output end of microprocessor is connect with catalytic bed temperature controller control terminal by conducting wire, micro-
Processor output terminal is connect with display unit control terminal by conducting wire, and output end of microprocessor is with alarm unit control terminal by leading
Line connects;
The air processing unit is hollow container, and first half loads the latter half of filling of silica wool and includes CaO solid particles
Inside with the nonreactive drier of hydrazine;
The catalytic bed is hollow tube, and catalyst for preparing hydrogen is catalytically decomposed in inside filling hydrazine, and outer wall winding heater strip has thermometric
Probe into groove;
The hydrogen detection unit is the Optical Hydrogen detector with signal processing function and signal output function;
The display unit can carry out the device that numeric literal is shown including LCD display etc.;
The alarm unit is to include the sound-light alarms equipment such as buzzer;
A kind of hydrazine gas detection method, step are:
1. catalytic bed temperature is maintained not less than operating temperature ratings after booting detection environment temperature;
2. the air for being mixed with hydrazine gas is sucked by air intake duct with nominal rated speed;
3. the silica wool that the air for being mixed with hydrazine gas being inhaled into initially enters air processing unit is filtered out in air
Dust, subsequently into air processing unit calcium oxide particle carry out removal moisture drying;
4. entering catalytic bed at the gas after filtration drying enters catalytic bed, hydrazine decomposes in air;
5. gas enters hydrogen detection unit after decomposing, hydrogen content is detected;
6. Detection of Trace Hydrazine in Air is calculated by computational methods according to the detection limit of operating temperature, the design resolution ratio of hydrazine, hydrogen
Content.
7. evaluation is directly displayed by display unit, if numerical value is more than alarming value, alarm unit alarm.
The environment temperature is detection device ambient temperature;
The operating temperature ratings are 35 DEG C;
The nominal rated speed is 5mL/s.
The resolution ratio is completely decomposed into hydrogen and the hydrazine of nitrogen and the percentage of total hydrazine amount for hydrazine;
The computational methods are:CHydrazine=K*CHydrogen*(Vt*(T0+273)/(Tt+273))/2;
CHydrazineFor Detection of Trace Hydrazine in Air concentration;K is resolution ratio;CHydrogenThe concentration of hydrogen is detected for hydrogen detection unit;VtIt is specified
Rate;T0For environment temperature;TtFor operating temperature.
1. such as Fig. 2:This example is controlled by air intake duct, air processing unit, catalytic bed, air pump, hydrogen detection unit, temperature
Device, microprocessor, display unit, alarm unit composition.
2. such as Fig. 3:Air intake duct uses diameter 6mm long 10mm spiral shape stainless steel tubes;Air processing unit is by outer diameter 30mm
Internal diameter 28mm long 100mm stainless steels cylinders and both ends band φ 6 connector compositions, the interior filling silica wool of stainless steel cylinder first half, after
Half portion fills calcium oxide particle;
3. catalytic bed length according to catalyst performance it is unusual using 100ppm standard hydrazine air mixers with 5ml/s's
After draft speed is by catalytic bed, gas enter ammonia indicator it is non-discolouring when bed a length of resolution ratio 100% when catalytic bed ruler
Very little relationship;This example catalytic bed is made of outer diameter 40mm internal diameter 36mm long 120mm stainless steels cylinders and both ends band 6 connectors of φ, is urged
Change and 1 holes of φ are opened at bed entrance 5mm, cylinder interior filling hydrazine catalytic decomposition catalyst, hydrazine resolution ratio is 100%;
4. air pump is speed of evacuation 5ml/s direct current air pumps, entrance has 6 connectors of φ;Hydrogen detection unit is Optical Hydrogen
Sensor;Catalytic bed heater strip power is 5w, and temperature controller thermocouple corresponds to pick-up specification as 0-300 DEG C of corresponding 0-5V;It is micro-
Processor uses LPC1768 embedded microcontrollers;Display unit uses 12864 liquid crystal displays;Alarm unit uses voice
Buzzer.
5. air intake duct is connect with air processing unit inlet with 6 connectors of φ, air processing unit outlet and air pump entrance
It is connected with 6 stainless steel tubes of φ, air pump outlet is connect with hydrogen detection unit with 6 stainless steel tubes of φ, and hydrogen detection unit serial ports is defeated
Go out and connect with microprocessor LPC1768-UART pins, heater strip uniform winding is on catalytic bed barrel, the heat of temperature controller
Galvanic couple is inserted into 1 apertures of catalytic bed φ, insertion depth 20mm, and temperature controller input termination microprocessor LPC1768-I/O draws
On foot, display unit is connect with alarm unit input terminal by conducting wire with for processor I/O pins.
6. such as Fig. 4:The workflow of the device is booting detection room temperature T0Catalytic bed temperature is maintained not less than minimum afterwards
Determine 35 DEG C of operating temperature;
7. the air for being mixed with hydrazine gas is sucked by air intake duct with nominal rated speed 5ml/s;
8. the silica wool that the air for being mixed with hydrazine gas being inhaled into initially enters air processing unit is filtered out in air
Dust, subsequently into air processing unit calcium oxide particle carry out removal moisture drying;
9. enter catalytic bed catalytic decomposition at the gas after filtration drying;
10. gas enters hydrogen detection unit after decomposing, hydrogen content is detected;
11. according to environment temperature, catalytic bed temperature, the design resolution ratio of hydrazine, hydrogen detection limit calculated by computational methods
Go out the content of Detection of Trace Hydrazine in Air, this example hydrazine resolution ratio is 100%.
12. since gas is by the effective unit time flow of heating and micro hydrazine decomposition caused heat release gas in detection process
V0=Vt*(T0+273)/(Tt+ 273) wherein VtEnter flows per unit time, T for pumping0For environment temperature, TtFor current catalytic bed
Interior temperature is considered as gas Current Temperatures;
13. formula is catalytically decomposed according to hydrazine completely:N2H4 → N2 (g)+2H2 (g) hydrazines are 1 with hydrogen molar ratio:2;
14. it is C to obtain hydrazine concentration calculation formulaHydrazine=K*CHydrogen*(Vt*(T0+273)/(Tt+ 273))/215. evaluation leads to
Display unit is crossed to directly display, if numerical value is more than alarming value, alarm unit alarm.
Claims (5)
1. a kind of hydrazine gas detection method, it is characterised in that include the following steps:
When the catalytic bed temperature of catalytic bed temperature controller feedback is more than operating temperature ratings, air intake duct is inhaled with nominal rated speed
Enter to be mixed with the air of hydrazine gas;
The air for being mixed with hydrazine gas being inhaled into filters out the dust in air by the silica wool of air processing unit first,
Then removal moisture drying is carried out by CaO particles;
Filtered dried gas enters catalytic bed, and hydrazine decomposes in air;
Gas after decomposition enters hydrogen detection unit, detects hydrogen content;
The content of Detection of Trace Hydrazine in Air is obtained according to the detection limit of catalytic bed temperature, the setting resolution ratio of hydrazine, hydrogen.
2. a kind of hydrazine gas detection method according to claim 1, it is characterised in that the operating temperature ratings are 35 DEG C.
3. a kind of hydrazine gas detection method according to claim 1, it is characterised in that the nominal rated speed is 5mL/s.
4. a kind of hydrazine gas detection method according to claim 1, it is characterised in that the resolution ratio is decomposed completely for hydrazine
For the hydrazine of hydrogen and nitrogen and the percentage of total hydrazine amount.
5. a kind of hydrazine gas detection method according to claim 1, it is characterised in that described according to catalytic bed temperature, hydrazine
Design resolution ratio, the detection limit of hydrogen show that the content of Detection of Trace Hydrazine in Air is obtained by following formula:
CHydrazine=K*CHydrogen*(Vt*(T0+273)/(Tt+273))/2;
CHydrazineFor Detection of Trace Hydrazine in Air concentration;K is resolution ratio;CHydrogenThe concentration of hydrogen is detected for hydrogen detection unit;VtFor nominal rated speed;
T0For environment temperature;TtFor catalytic bed temperature.
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CN201611087751.7A CN108132328A (en) | 2016-12-01 | 2016-12-01 | A kind of hydrazine gas detection method |
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Citations (3)
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CN105136698A (en) * | 2015-08-24 | 2015-12-09 | 天津师范大学 | Volatile compound determination method and apparatus thereof |
CN105195159A (en) * | 2015-10-13 | 2015-12-30 | 天津工业大学 | Catalyst for decomposing hydrazine hydrate to prepare hydrogen and preparation method of catalyst |
CN105618065A (en) * | 2014-11-07 | 2016-06-01 | 中国科学院大连化学物理研究所 | Applications of catalyst in hydrogen production through hydrazine decomposition |
-
2016
- 2016-12-01 CN CN201611087751.7A patent/CN108132328A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105618065A (en) * | 2014-11-07 | 2016-06-01 | 中国科学院大连化学物理研究所 | Applications of catalyst in hydrogen production through hydrazine decomposition |
CN105136698A (en) * | 2015-08-24 | 2015-12-09 | 天津师范大学 | Volatile compound determination method and apparatus thereof |
CN105195159A (en) * | 2015-10-13 | 2015-12-30 | 天津工业大学 | Catalyst for decomposing hydrazine hydrate to prepare hydrogen and preparation method of catalyst |
Non-Patent Citations (2)
Title |
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刘志娟等: "肼类火箭推进剂气体检测技术", 《低温与特气》 * |
孙军等: "活性炭担载碳化钨催化剂在肼分解反应中的应用", 《中国化学会第三属全国化学推进钠学术会议•论文集》 * |
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