CN105136661A - Oxygen and nitrogen analyzer - Google Patents
Oxygen and nitrogen analyzer Download PDFInfo
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- CN105136661A CN105136661A CN201510598174.7A CN201510598174A CN105136661A CN 105136661 A CN105136661 A CN 105136661A CN 201510598174 A CN201510598174 A CN 201510598174A CN 105136661 A CN105136661 A CN 105136661A
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Abstract
The invention relates to an oxygen and nitrogen analyzer. The oxygen and nitrogen analyzer comprises a gas stripping unit and a detecting unit, wherein the gas stripping unit comprises a carrier gas pressure gauge, a purification furnace, a carrier gas purification tube, a gas analysis reducing valve, a gas analysis pressure gauge, a flushing adjusting valve, a six-way valve, a pulse heating furnace, a dust filter tube, a reformer and a sample gas purification tube; the detecting unit comprises a detection gas pressure adjusting valve, a detection and adjustment pressure gauge, an air throttle, a flow sensor, an infrared detector and a CO2 absorption tube. According to the oxygen and nitrogen analyzer, under an inert atmosphere, a sample is heated and decomposed by pulses, the infrared detector and a thermal conductivity detector respectively detect the contents of oxygen and nitrogen in various iron steels, nonferrous metals and novel materials, the operation is convenient and the detection and analysis accuracies are high.
Description
Technical field
The present invention relates to a kind of oxygen nitrogen analysis equipment.
Background technology
In recent years, along with development and the development of metal material, the research and production of mensuration to various iron and steel, non-ferrous metal and new materials such as Ti alloy with high performance of Oxygen in Metals nitrogen is essential.Argon in foreign applications inert gas fusion-thermal conductivity and gas chromatography determination metal, has commercial apparatus to sell.But this quasi-instrument can not get rid of the interference of nitrogen completely, confidence level and the accuracy of quantitative test are all affected.Domestic have this type of achievement, but analysis precision is lower, analyzes the requirement that lower limit does not reach new material.
Summary of the invention
Technical matters solved by the invention is to provide a kind of oxygen nitrogen analysis equipment, to solve the shortcoming in above-mentioned background technology.
Technical matters solved by the invention realizes by the following technical solutions:
The invention provides a kind of oxygen nitrogen analysis equipment, comprise and carry gas unit, detecting unit, described gas unit of carrying comprises nebulizer gas pressure table, purification furnace, carrier gas purification pipe, divide gassing reduction valve, analyze atmospheric pressure table, rinse variable valve, six-way valve, pulse heating furnace, filtering dust pipe, reburner, sample gas purification pipe, the cylinder outlet of carrier gas gas cylinder connects carrier gas reduction valve by stop valve, carrier gas reduction valve access purification furnace, purification furnace is connected with carrier gas purification pipe, carrier gas purification pipe leads up to point gassing reduction valve and analyze atmospheric pressure table access six-way valve, access the entrance point of pulse heating furnace again, separately lead up to and rinse variable valve access six-way valve, access the entrance point of pulse heating furnace again, the endpiece of pulse heating furnace connects filtering dust pipe, filtering dust pipe lead up to six-way valve access reburner, reburner is connected with sample gas purification pipe, six-way valve of separately leading up to connects flushing flow gauge, wherein, described purification furnace and reburner are copper oxide catalyzation stove, described detecting unit comprises detection air pressure regulator, detects adjustment tensimeter, air throttle, flow sensor, infrared detector, CO
2absorption tube, sample gas purification pipe regulates tensimeter connecting joint air valve, air throttle connection traffic sensor by detecting air pressure regulator and detecting, and separately leads up to solar term variable valve connection traffic sensor, flow sensor is connected with the inlet end of infrared detector, the outlet side access CO of infrared detector
2absorption tube, CO
2absorption tube linking parsing air-flow gauge, then access stop valve, the cylinder outlet of power gas bottle connects power gas reduction valve and power atmospheric pressure table, and power gas reduction valve one tunnel is connected with six-way valve and pulse heating furnace, power controlled atmosphere air throttle of separately leading up to access infrared detector.
Solar term variable valve or flow valve is provided with between air throttle of the present invention and flow sensor.Stop valve of the present invention is two three-way electromagnetic valves.Carrier gas purification pipe of the present invention is for purifying carrier gas, and alkali asbestos are filled on top, and under-filled water absorbing agent, two ends absorbent cotton is filled.Filtering dust pipe of the present invention is for filtering the carrier gas and tested gas of flowing out from pulse heating furnace, and silica wool is filled on top, under-filled absorbent cotton.Sample gas purification pipe of the present invention is used for the steam in sorption enhanced stove effluent air, and absorbent cotton is filled at two ends, central filler water absorbing agent.CO of the present invention
2absorption tube is for absorbing the CO flowed out from infrared detector
2and steam, alkali asbestos are filled on top, and under-filled water absorbing agent, two ends absorbent cotton is filled.Copper oxide catalyzation stove of the present invention comprises body of heater, and body of heater is provided with two groups of lead-in wires, and one group is the thermocouple output line of thermometric, another group is heater strip extended line, be provided with quartz ampoule in the middle of body of heater, quartz ampoule two ends glass wool seals, central filler rare-earth oxidation copper.
The present invention also provides a kind of detection method of oxygen nitrogen analysis equipment, and it is characterized in that, it comprises the following steps:
(1) metal powder nickel foil to be measured is wrapped up, put into pulse heating furnace;
(2) stop valve is opened, make carrier gas from stop valve out after, purification furnace is entered into successively through carrier gas reduction valve and nebulizer gas pressure table, carrier gas enters again carrier gas purification pipe after carrying out filtering and purify in purification furnace and purifies further, more successively by a point gassing reduction valve, analyze atmospheric pressure table, six-way valve enters pulse heating furnace;
(3) energising makes pulse heating furnace heat, metal powder to be measured melting in nickel foil, under the drive of carrier gas stream, and CO, N of discharging in metal powders melt process to be measured
2enter into filtering dust pipe dust removal by filtration;
(4) to be entered in reburner by six-way valve above by the gas of filtering dust pipe dust removal by filtration and carry out catalysis, CO is converted into CO
2;
(5) from reburner CO out
2, N
2successively through detecting air pressure regulator, detect regulate tensimeter, air throttle, flow sensor enter infrared detector, infrared detector detects O, and the signal detected is flowed to computing machine carries out analyzing and processing;
(6) CO is entered from infrared detector gas out
2absorption tube, CO
2with steam by CO
2absorption tube absorbs;
(7) from CO
2absorption tube gas out by analysis air-flow gauge connects stop valve, is linked into thermal conductivity detector (TCD) measures N by stop valve.
The present invention is when needs paired pulses heating furnace rinses, unload filtering dust pipe, regulate six-way valve, to make from the carrier gas out of carrier gas purification pipe successively by rinsing variable valve, six-way valve enters pulse heating furnace, block the upper end of joint 2-3 second of filtering dust pipe, then decontrol, carrier gas is discharged by flushing flow gauge, repeatedly several times, until gas circuit is unobstructed.
Advantage and beneficial effect:
(1) the present invention is provided with purification furnace, purification furnace is copper oxide catalyzation stove, depth-type filtration and purification are carried out to the carrier gas entering pulse heating furnace, eliminates the interference of the gas that the reaction in carrier gas in foreign gas paired pulses heating furnace produces, also improve the precision of measurement;
(2) the present invention is provided with reburner, and reburner is also copper oxide catalyzation stove, and play catalytic action, the CO restored in analysis by metal powder to be measured is converted into CO
2, by alkali asbestos agent absorbent below, thus prevent CO or CO generated by oxygen in sample
2the interference to nitrogen brought, therefore, reburner transformation efficiency is high, directly affects the measurement result of nitrogen, makes the measurement of nitrogen more accurate;
(3) the present invention is provided with six-way valve, six-way valve is two six three-way electromagnetic valves, the open to shut to regulate that quick and precisely can carry out gas circuit is controlled by controller, thus respond different functional requirements, easy to operate, can rapid and accurate determination iron and steel, copper, titanium, rare earth material and various alloy, oxygen in pottery and other inorganicss and nitrogen content;
(4) the present invention is provided with stop valve, and when detecting, stop valve leads directly to, when cleaning, and stop valve short circuit, carrier gas reenters purification furnace by stop valve and cleans whole gas circuit, makes operational maintenance of the present invention and easy to maintenance;
(5) the present invention under an inert atmosphere, by PULSE HEATING decomposition samples, measured the content of oxygen, nitrogen in various iron and steel, coloured technology and new material by infrared detector and thermal conductivity detector (TCD) respectively, easy to operate, detects analysis precision high.
Accompanying drawing explanation
Fig. 1 is the gas circuit structure figure of a kind of embodiment of the present invention.
Fig. 2 is the structure schematic diagram of a kind of embodiment of the present invention.
Fig. 3 is the Facad structure schematic diagram of a kind of embodiment of the present invention.
Fig. 4 is the structural representation of copper oxide catalyzation stove.
Embodiment
The technological means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with concrete diagram, setting forth the present invention further.
Fig. 1-4 is the structural representation of a kind of embodiment of the present invention, and it comprises analyser main tank A, analyser odd-side B, is provided with and carries gas unit, be provided with detecting unit in analyser odd-side B, carry gas unit and be connected with circuit by gas circuit with detecting unit in analyser main tank A.
Carry gas unit and comprise nebulizer gas pressure table 4, purification furnace 5, carrier gas purification pipe 6, point gassing reduction valve 7, six-way valve 9, pulse heating furnace 10, filtering dust pipe 11, reburner 12, sample gas purification pipe 13; Analyser main tank A is provided with carrier gas inlet A1, power gas entrance A2 and point gassing outlet A3, the cylinder outlet of carrier gas gas cylinder 1 connects carrier gas reduction valve 3 by stop valve 2, the outlet of carrier gas reduction valve 3 is provided with carrier gas and connects valve, and carrier gas connects valve and connects the carrier gas inlet A1 of carrier gas to analyser main tank A; Carrier gas inlet A1 connects purification furnace 5 by nebulizer gas pressure table 4, and purification furnace 5 is connected with carrier gas purification pipe 6; Carrier gas purification pipe 6 leads up to point gassing reduction valve 7 and analyze the 3rd joint that atmospheric pressure table 8 accesses six-way valve 9, and separately lead up to and rinse the first joint that variable valve 23 accesses six-way valve 9, the second joint of six-way valve 9 connects the entrance point of pulse heating furnace 10; The endpiece of pulse heating furnace 10 connects filtering dust pipe 11, filtering dust pipe 11 accesses the 5th joint of six-way valve 9,4th joint of six-way valve 9 is connected with reburner 12, reburner 12 connects sample gas purification pipe 13, sample gas purification pipe 13 is connected to a point gassing outlet A3, and the 5th joint of six-way valve 9 connects flushing flow gauge 24.
Six-way valve 9 is two six-way valves, during normality, and the second fittings the 3rd joint of six-way valve 9,5th fittings the 4th joint, the first joint and the 6th joint obstructed, during commutation, second fittings first joint, the 5th fittings the 6th joint, the 3rd joint and the 4th joint obstructed.
Analyser odd-side B is provided with a point gassing entrance B1, a point gassing answers back B2, and detecting unit comprises detection air pressure regulator 14, detects adjustment tensimeter 15, air throttle 16, flow valve 17, solar term variable valve 18, infrared detector, CO
2absorption tube, divide gassing entrance B1 to export A3 with point gassing on analyser main tank A to be connected, divide gassing entrance B1 by detecting air pressure regulator 14 and detecting atmospheric pressure table 15 connecting joint air valve 16, air throttle 16 passes through flow valve 17 or solar term variable valve 18 connection traffic sensor 19; Flow sensor 19 connects infrared detector 20, and infrared detector 20 connects CO
2absorption tube 21, CO
2absorption tube 21 is connected to a point gassing and answers back B2.
Point gassing B2 that answers back is connected with the analysis air-flow gauge 22 on analyser main tank A, and analysis air-flow gauge 22 connects stop valve 2; Stop valve 2 is two three-way electromagnetic valves, is straight-through at ordinary times, gassing will be divided to pass into thermal conductivity detector (TCD) and carry out nitrogen measurement, and when gas circuit needs maintenance, stop valve 2 is short logical, by airflow connection to carrier gas reduction valve 3, whole gas circuit is circulated through.
The cylinder outlet of power gas bottle 25 connects power gas reduction valve 26 and power atmospheric pressure table 27, power gas entrance A2 on the connect into analysis instrument main tank A of power gas reduction valve 26 1 road, be connected with pulse electrothermal stove 10 and six-way valve 9, adjusting air valve 28 of separately leading up to connects infrared detector 20; Power gas bottle 25 provides power for pulsed electrode stove 10 ON/OFF stove, application of sample action, and power atmospheric pressure table 27 is display power atmospheric pressure in real time, and power atmospheric pressure must be greater than nebulizer gas pressure, leaks to avoid carrier gas in pulsed electrode stove 10.
Carrier gas purification pipe 6 is for purifying carrier gas, and alkali asbestos are filled on top, and under-filled water absorbing agent, two ends absorbent cotton is filled.Filtering dust pipe 11 is for filtering the carrier gas and tested gas of flowing out from pulse heating furnace 10, upper end body fills 1/3 silica wool, absorbent cotton is filled in lower end, absorbent cotton will be torn, fill closely, high dust can be made to enter into the follow-up gas circuits such as six-way valve 9 as filled too pine, even damaging infrared detector 20 and thermal conductivity detector (TCD).Sample gas purification pipe 13 is for steam in sorption enhanced stove effluent air, and absorbent cotton is filled at two ends, central filler water absorbing agent.CO
2absorption tube 21 is for absorbing the CO flowed out from infrared detector 20
2and steam, alkali asbestos are filled on top 2/3, under-filled water absorbing agent, and two ends absorbent cotton is filled.
Reburner 12 and purification furnace 6 are two copper oxide catalyzation stoves, catalyst furnace comprises body of heater 30, body of heater 30 draws two groups of lead-in wires, one group is the thermocouple output line 31 of thermometric, another group is heater strip extended line 32, be provided with quartz ampoule 29 in the middle of catalyst furnace, quartz ampoule 29 two ends glass wool 33 seals, central filler rare-earth oxidation copper 34.Purification furnace 5 is for filtering and purification carrier gas, and reburner 12 catalytic action, the CO restored in analysis by sample is converted into CO
2, by CO below
2alkali asbestos in absorption tube 21 absorb, thus prevent CO or CO generated by oxygen in sample
2the interference to nitrogen brought.
Using method of the present invention comprises the following steps:
(1) metal powder nickel foil to be measured is wrapped up, put into pulse heating furnace;
(2) stop valve 2 is opened, make carrier gas from stop valve 2 out after, purification furnace 5 is entered into successively through carrier gas reduction valve 3 and nebulizer gas pressure table 4, carrier gas enters again carrier gas purification pipe 6 after carrying out filtering and purify in purification furnace 5 and purifies further, more successively by a point gassing reduction valve 7, analyze atmospheric pressure table 8, six-way valve 9 enters pulse heating furnace 10;
(3) be energized, make PULSE HEATING, 10 heating, metal powder to be measured melting in nickel foil, in metal powder, oxygen is at high temperature reduced, and spins off from metal with CO form, and in metal, nitrogen is at high temperature with N
2form spins off from metal, under the drive of carrier gas stream, and CO, N
2enter into filtering dust pipe 11 dust removal by filtration;
(4) to be entered in reburner 12 by six-way valve 9 above by the gas of filtering dust pipe 11 dust removal by filtration and carry out catalysis, CO is converted into CO
2;
(5) from reburner 12 CO out
2, N
2successively through detecting air pressure regulator 14, detect regulate tensimeter 15, air throttle 16, flow sensor 19 enter infrared detector 20, infrared detector 20 couples of O detect, and the signal detected is flowed to computing machine carry out analyzing and processing;
(6) CO is entered from infrared detector 20 gas out
2absorption tube 21, CO
2with steam by CO
2absorption tube 21 absorbs;
(7) from CO
2absorption tube 21 gas out by analysis air-flow gauge 22 accesses stop valve 2, is linked into thermal conductivity detector (TCD) to N by stop valve 2
2in N measure.
When needs paired pulses heating furnace 10 rinses, unload filtering dust pipe 11, regulate six-way valve 9, to make from carrier gas purification pipe 6 carrier gas out successively by rinsing variable valve 23, six-way valve 9 enters pulse heating furnace 10, block the upper end of joint 2-3 second of filtering dust pipe 11, then decontrol, carrier gas is connected to flushing flow gauge 24, repeatedly several times, until gas circuit is unobstructed.
Principle of work of the present invention:
The present invention under an inert atmosphere, by PULSE HEATING decomposition samples, is measured the content of oxygen, nitrogen in various iron and steel, coloured technology and new material respectively by infrared detector and thermal conductivity detector (TCD).Analytic process adopts PULSE HEATING metal powder to be measured, metal powder to be measured under the effect of nickel foil flux, melting under high temperature, CO, N of discharging
2cO is generated Deng the rare-earth oxidation copper of mixed gas in reburner
2, N
2and H
2o, is loaded in infrared detector by high-purity carrier gas, after measuring the percentage composition of oxygen, and CO
2and H
2o is absorbed by alkali asbestos and magnesium perchlorate respectively, then leads people's thermal conductivity detector (TCD) and detected, and obtains the content of nitrogen.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and instructions just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (8)
1. an oxygen nitrogen analysis equipment, comprises and carries gas unit, detecting unit, it is characterized in that:
Described gas unit of carrying comprises nebulizer gas pressure table, purification furnace, carrier gas purification pipe, divide gassing reduction valve, analyze atmospheric pressure table, rinse variable valve, six-way valve, pulse heating furnace, filtering dust pipe, reburner, sample gas purification pipe, the cylinder outlet of carrier gas gas cylinder connects carrier gas reduction valve by stop valve, carrier gas reduction valve access purification furnace, purification furnace is connected with carrier gas purification pipe, carrier gas purification pipe leads up to point gassing reduction valve and analyze atmospheric pressure table access six-way valve, access the entrance point of pulse heating furnace again, separately lead up to and rinse variable valve access six-way valve, access the entrance point of pulse heating furnace again, the endpiece of pulse heating furnace connects filtering dust pipe, filtering dust pipe lead up to six-way valve access reburner, reburner is connected with sample gas purification pipe, six-way valve of separately leading up to connects flushing flow gauge, wherein, described purification furnace and reburner are copper oxide catalyzation stove,
Described detecting unit comprises detection air pressure regulator, detects adjustment tensimeter, air throttle, flow sensor, infrared detector, CO
2absorption tube, sample gas purification pipe regulates tensimeter connecting joint air valve, air throttle connection traffic sensor by detecting air pressure regulator and detecting, and separately leads up to solar term variable valve connection traffic sensor, flow sensor is connected with the inlet end of infrared detector, the outlet side access CO of infrared detector
2absorption tube, CO
2absorption tube linking parsing air-flow gauge, then access stop valve;
The cylinder outlet of power gas bottle connects power gas reduction valve and power atmospheric pressure table, and power gas reduction valve one tunnel is connected with six-way valve and pulse heating furnace, power controlled atmosphere air throttle of separately leading up to access infrared detector.
2. oxygen nitrogen analysis equipment according to claim 1, is characterized in that, be provided with solar term variable valve or flow valve between described air throttle and flow sensor.
3. oxygen nitrogen analysis equipment according to claim 1, is characterized in that, described stop valve is two three-way electromagnetic valves.
4. oxygen nitrogen analysis equipment according to claim 1, is characterized in that, described carrier gas purification pipe is for purifying carrier gas, and alkali asbestos are filled on top, and under-filled water absorbing agent, two ends absorbent cotton is filled.
5. oxygen nitrogen analysis equipment according to claim 1, is characterized in that, described filtering dust pipe is for filtering the carrier gas and tested gas of flowing out from pulse heating furnace, and silica wool is filled on top, under-filled absorbent cotton.
6. oxygen nitrogen analysis equipment according to claim 1, is characterized in that, described sample gas purification pipe is used for the steam in sorption enhanced stove effluent air, and absorbent cotton is filled at two ends, central filler water absorbing agent.
7. oxygen nitrogen analysis equipment according to claim 1, is characterized in that, described CO
2absorption tube is for absorbing the CO flowed out from infrared detector
2and steam, alkali asbestos are filled on top, and under-filled water absorbing agent, two ends absorbent cotton is filled.
8. oxygen nitrogen analysis equipment according to claim 1, it is characterized in that, described copper oxide catalyzation stove comprises body of heater, body of heater is provided with two groups of lead-in wires, one group is the thermocouple output line of thermometric, and another group is heater strip extended line, is provided with quartz ampoule in the middle of body of heater, quartz ampoule two ends glass wool seals, central filler rare-earth oxidation copper.
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CN201510598174.7A CN105136661A (en) | 2015-09-18 | 2015-09-18 | Oxygen and nitrogen analyzer |
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CN201510598174.7A CN105136661A (en) | 2015-09-18 | 2015-09-18 | Oxygen and nitrogen analyzer |
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Cited By (1)
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CN106324197A (en) * | 2016-08-22 | 2017-01-11 | 芜湖市神龙新能源科技有限公司 | Atmospheric pollution detection device convenient to clean |
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