CN108169277A - A kind of calibration equipment and its method of calibration of ammonia gas in nitridation furnace resolution ratio - Google Patents

A kind of calibration equipment and its method of calibration of ammonia gas in nitridation furnace resolution ratio Download PDF

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Publication number
CN108169277A
CN108169277A CN201711423745.9A CN201711423745A CN108169277A CN 108169277 A CN108169277 A CN 108169277A CN 201711423745 A CN201711423745 A CN 201711423745A CN 108169277 A CN108169277 A CN 108169277A
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China
Prior art keywords
valve
ammonia
resolution ratio
hydrogen analyzer
calibration
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CN201711423745.9A
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Chinese (zh)
Inventor
殷开山
陈红岩
古宏博
王军联
雷勇
王瑞
刘敏
赵闯
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AECC Aviation Power Co Ltd
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AECC Aviation Power Co Ltd
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Priority to CN201711423745.9A priority Critical patent/CN108169277A/en
Publication of CN108169277A publication Critical patent/CN108169277A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/18Investigating or analyzing materials by the use of thermal means by investigating thermal conductivity

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

Calibration equipment and its method of calibration the invention discloses a kind of ammonia gas in nitridation furnace resolution ratio are included on nitriding furnace discharge duct and are provided with gas collecting pipeline, connection verification ontology on gas collecting pipeline, and hydrogen analyzer is also associated on nitriding furnace exhaust pipe;Wherein verification ontology includes communicating pipe, and one end of communicating pipe is connected with gas collecting pipeline, and the other end of communicating pipe is communicated with graduated cylinder by third valve;The open top of graduated cylinder is communicated with water container by the first valve, and the second valve is provided at the bottom opening of graduated cylinder.Ammonia decomposition can be quickly detected, and is compared with the reading of hydrogen analyzer, whether the reading for monitoring hydrogen analyzer in real time is correct.

Description

A kind of calibration equipment and its method of calibration of ammonia gas in nitridation furnace resolution ratio
Technical field
The invention belongs to chemical heat treatment technology fields;A kind of calibration equipment more particularly to ammonia gas in nitridation furnace resolution ratio and Its method of calibration.
Background technology
Hydrogen analyzer is as the precision instrument for measuring ammonia decomposition in stove in chemical heat treatment apparatus in real time, measured value Directly determine the quality of product.By taking NITREX companies NX-815S types, controlled atmosphere numerical control nitriding furnace as an example, principle is logical It crosses to thermal cracking NH in stove3The NH formed3、N2And H2Atmosphere be acquired, the H in measuring unit volume2Content, so as to count Ammonia decomposition in stove is calculated, and by data feedback to PLC and industrial personal computer, mass flowmenter (MFC) is being adjusted by industrial personal computer, Achieve the purpose that ammonia decomposition in regulating stove.
But due to equipment can generate in the long-term use dust and tetrachloro-ethylene cracking after remaining crystalline solid, and And the tail gas acquisition pipeline of hydrogen analyzer is blocked, ammonia decomposition in the stove that hydrogen analyzer measures is caused to deviate actual value, seriously It influences the quality of product or even causes waste product.
Invention content
The present invention provides a kind of calibration equipments and its method of calibration of ammonia gas in nitridation furnace resolution ratio, can quickly detect ammonia Gas resolution ratio, and compared with the reading of hydrogen analyzer, whether the reading for monitoring hydrogen analyzer in real time is correct.
The technical scheme is that:A kind of calibration equipment of ammonia gas in nitridation furnace resolution ratio, is included in nitriding furnace exhaust pipe Gas collecting pipeline is provided on road, verification ontology is connected on gas collecting pipeline, hydrogen analysis is also associated on nitriding furnace exhaust pipe Instrument;Wherein verification ontology includes communicating pipe, and one end of communicating pipe connects with gas collecting pipeline, and the other end of communicating pipe passes through the Three valves are communicated with graduated cylinder;The open top of graduated cylinder is communicated with water container by the first valve, is set at the bottom opening of graduated cylinder There is the second valve.
Further, it is of the invention to be further characterized in that:
Wherein third valve and the second valve are opened, and the first valve is closed.
Wherein third valve and the second valve are closed, and the first valve is opened.
The present invention also provides a kind of hydrogen analyzer methods of calibration, include the following steps:
Step S1 will verify ontology and be connected with nitriding furnace discharge duct as described in claim 1;
Step S2 closes the first valve, opens the second valve and third valve, the gas loading for discharging nitriding furnace Cylinder;
Step S3 closes the second valve and third valve, then opens the first valve;
Step S4, the water in water container are flowed into graduated cylinder by the first valve, and until the water in water container no longer flows;
Step S5, the volume number for reading water in graduated cylinder is the volume of ammonia, and is calculated according to the volume accounting of ammonia Go out the resolution ratio of ammonia;
The ammonia decomposition that the ammonia decomposition obtained in step S5 is obtained with hydrogen analyzer is compared by step S6, Complete the verification to hydrogen analyzer.
Further, the features of the present invention also characterized in that:
The total volume of graduated cylinder is V in wherein step S5, and the volume that graduated cylinder is read is VWater, therefore the resolution ratio of ammonia is (1- VWater/ V) %.
In wherein step S6 step 5 obtain ammonia decomposition and hydrogen analyzer obtain ammonia decomposition be not much different in ± 2%, then the reading of hydrogen analyzer is correct.
Step 5 obtains ammonia decomposition in wherein step S6 and hydrogen analyzer obtains ammonia decomposition and differs by more than ± 2%, Then the reading of hydrogen analyzer is wrong.
Wherein step S6 further includes the maintenance to hydrogen analyzer, i.e., the pneumatic filter of hydrogen analyzer is cleared up.
Compared with prior art, the beneficial effects of the invention are as follows:The discharge duct of existing hydrogen analyzer and nitriding furnace connects Logical, after long-time use, pneumatic filter is blocked to hydrogen analyzer, therefore hydrogen analyzer data can be caused to be not allowed Really, therefore introducing verification ontology the ammonia dissociation rate of nitriding furnace is detected, is then carried out pair with the result of hydrogen analyzer Than completing to verify.
Further, the first valve is closed, and the second valve and third valve are opened then as graduated cylinder air inlet step;First valve Door is opened, and the second valve and third valve are closed then as ammonia absorption step.
Beneficial effects of the present invention also reside in:The present invention is dissolved in the characteristic of water using ammonia, and the product nitrogen of ammonia and Hydrogen characteristic not soluble in water, the gas of the nitriding furnace exhaust pipe by being passed through full volume in graduated cylinder, then passes through water container Water is flowed into graduated cylinder, i.e., the water in water container can be inhaled into graduated cylinder after absorbing ammonia, when ammonia is only absorbed by the water it completely Afterwards, then the water in water container may not flow into graduated cylinder, can either be fully retrieved the volume of ammonia in graduated cylinder at this time, while can also Enough get nitrogen and hydrogen volume and, the resolution ratio of ammonia, and the resolution ratio and hydrogen are then can obtain by calculating The ammonia decomposition that analyzer obtains is compared, and completes the verification to hydrogen analyzer.
Further, the invention discloses the formula that verification ontology calculates ammonia dissociation rate.
Further, result is differed according to what step 5 obtained that ammonia decomposition and hydrogen analyzer obtain ammonia decomposition Judge whether the reading of hydrogen analyzer is wrong, and hydrogen analyzer is examined in the case where judgement hydrogen analyzer reading is wrong It surveys, is cleared up mainly for pneumatic filter.
Description of the drawings
Fig. 1 is the structure diagram that ontology is verified in the present invention.
In figure:1 is water container;2 be the first valve;3 be graduated cylinder;4 be the second valve;5 be third valve;6 be communicating pipe.
Specific embodiment
Technical scheme of the present invention is further illustrated in the following with reference to the drawings and specific embodiments.
The present invention provides a kind of calibration equipment of ammonia gas in nitridation furnace resolution ratio, including what is connected with nitriding furnace discharge duct Ontology is verified, is wherein also communicated with hydrogen analyzer on nitriding furnace exhaust pipe;Specifically gas is opened up on nitriding furnace discharge duct Collection tube, gas collecting pipe are connect with verification ontology;As shown in Figure 1, verification ontology include communicating pipe 6, one end of connecting tube 6 with Gas collecting pipe connects, and the other end of connecting tube 6 connected by third valve 5 with graduated cylinder 3, and the open top of graduated cylinder 3 passes through the One valve 2 is connected with water container 1, and the second valve 4 is provided on the bottom opening of graduated cylinder 3.
The present invention application method be:5 and second valve 4 of third valve is first turned on to being filled with nitriding fire grate in graduated cylinder 3 The gas of tracheae is treated to be packed into after above-mentioned gas in graduated cylinder 3, closes the second valve 4 and third valve 5, then opens first Valve 2 makes the water in water container 1 absorb the ammonia in graduated cylinder 3 in gas, and the water for absorbing ammonia is flowed by the first valve 2 Enter in graduated cylinder 3, when ammonia is absorbed completely, the water in water container 1 will not then be entered by the first valve 2 in graduated cylinder 3.
The present invention also provides a kind of methods of calibration of ammonia gas in nitridation furnace resolution ratio, include the following steps:
Step S1 is connected using above-mentioned verification ontology by gas collecting pipeline with nitriding furnace discharge duct, specifically will Communicating pipe 6 connects with gas collecting pipeline.
Step S2 closes the first valve 2 verified in ontology, and the second valve 4 and third valve 5 are opened, by exhaust pipe Interior gas is filled up completely to graduated cylinder 3.
Step S3 closes the second valve 4 and third valve 5, then opens the first valve 2.
Step S4, the step are reaction step, and water wherein in water container 1 absorbs the ammonia in graduated cylinder 3, then by the One valve 2 is flowed into graduated cylinder 3, until the ammonia in graduated cylinder 3 is absorbed, and the water in water container 1 is no longer flow into graduated cylinder 3 completely It is interior.
Step S5, reads the volume number of water in graduated cylinder 3, which is the volume number of ammonia in graduated cylinder, and according to ammonia The volume accounting of gas calculates the resolution ratio of ammonia;Its calculating process is:The volume of graduated cylinder 3 is V, and the volume of water is in graduated cylinder 3 VWater, therefore the resolution ratio for obtaining ammonia is (1-VWater/ V) %.
The ammonia decomposition that the ammonia decomposition obtained in step 5 is obtained with hydrogen analyzer is compared by step S6, when Step 5 obtains ammonia decomposition and hydrogen analyzer and obtains ammonia decomposition being not much different in ± 2%, then the reading of hydrogen analyzer is being just Really;When step 5 obtains ammonia decomposition and hydrogen analyzer and obtains ammonia decomposition differing by more than ± 2%, then the reading of hydrogen analyzer Number is wrong, needs to be corrected hydrogen analyzer, specifically needs to clear up the pneumatic filter of hydrogen analyzer, go to clean Matter.
Specific embodiments of the present invention are:
Embodiment 1
The verification of ammonia dissociation rate is carried out in the case where nitriding furnace temperature is 600 DEG C.
The verification ontology of the present invention is connected with the gas collecting pipeline on nitriding furnace discharge pipe first;Then by this hair The ammonia dissociation rate that the verification ontology of bright method obtains is 80%, and the ammonia that the hydrogen analyzer of nitriding furnace discharge duct connection obtains divides Solution rate is 80%;Then illustrate that the data of hydrogen analyzer are correct.
Embodiment 2
The verification of ammonia dissociation rate is carried out in the case where nitriding furnace temperature is 550 DEG C.
The verification ontology of the present invention is connected with the gas collecting pipeline on nitriding furnace discharge pipe first;Then by this hair The ammonia dissociation rate that the verification ontology of bright method obtains is 79.5%, the ammonia that the hydrogen analyzer that nitriding furnace discharge duct connects obtains Resolution ratio is 80%;Then illustrate that the data of hydrogen analyzer are correct.
Embodiment 3
The verification of ammonia dissociation rate is carried out in the case where nitriding furnace temperature is 600 DEG C.
The verification ontology of the present invention is connected with the gas collecting pipeline on nitriding furnace discharge pipe first;Then by this hair The ammonia dissociation rate that the verification ontology of bright method obtains is 60%, and the ammonia that the hydrogen analyzer of nitriding furnace discharge duct connection obtains divides Solution rate is 63%;Then illustrate that the data of hydrogen analyzer are wrong, need to be corrected hydrogen analyzer and the gas to hydrogen analyzer Filter is cleared up into market, the impurity of pneumatic filter is understood, so as to improve the accuracy of measurement of hydrogen analyzer.
Using apparatus of the present invention and its method of calibration, the measurement result of hydrogen analyzer can be monitored in real time, it is ensured that Product quality is monitored, can effectively reduce rejection rate 2-5 stoves/time.

Claims (8)

1. a kind of calibration equipment of ammonia gas in nitridation furnace resolution ratio, which is characterized in that be included on nitriding furnace discharge duct and be provided with gas Body acquires pipeline, and verification ontology is connected on gas collecting pipeline, hydrogen analyzer is also associated on nitriding furnace exhaust pipe;Wherein verify Ontology includes communicating pipe (6), and one end of communicating pipe (6) connects with gas collecting pipeline, communicating pipe the other end of (6) pass through third Valve (5) is communicated with graduated cylinder (3);The open top of graduated cylinder (3) is communicated with water container (1), graduated cylinder (3) by the first valve (2) Bottom opening at be provided with the second valve (4).
2. the calibration equipment of ammonia gas in nitridation furnace resolution ratio according to claim 1, which is characterized in that the third valve (5) it is opened with the second valve (4), the first valve (2) is closed.
3. the calibration equipment of ammonia gas in nitridation furnace resolution ratio according to claim 1, which is characterized in that the third valve (5) it is closed with the second valve (4), the first valve (2) is opened.
4. a kind of method of calibration of ammonia gas in nitridation furnace resolution ratio, which is characterized in that include the following steps:
Step S1 will verify ontology and be connected with nitriding furnace discharge duct as described in claim 1;
Step S2 closes the first valve (2), opens the second valve (4) and third valve (5), fills out the gas that nitriding furnace is discharged Charge cylinder (3);
Step S3 closes the second valve (4) and third valve (5), then opens the first valve (2);
Step S4, the water in water container (1) are flowed into graduated cylinder (3) by the first valve (2), and until the water in water container (1) No longer flow;
Step S5, the volume number for reading graduated cylinder (3) interior water are the volume of ammonia, and calculate according to the volume accounting of ammonia The resolution ratio of ammonia;
The ammonia decomposition that the ammonia decomposition obtained in step S5 is obtained with hydrogen analyzer is compared by step S6, is completed Verification to hydrogen analyzer.
5. the method for calibration of ammonia gas in nitridation furnace resolution ratio according to claim 4, which is characterized in that measured in the step S5 The total volume of cylinder (3) is V, and the volume that graduated cylinder (3) is read is VWater, therefore the resolution ratio of ammonia is (1-VWater/ V) %.
6. the method for calibration of ammonia gas in nitridation furnace resolution ratio according to claim 4, which is characterized in that walked in the step S6 Rapid 5, which obtain ammonia decomposition and hydrogen analyzer, obtains ammonia decomposition and is not much different in ± 2%, then the reading of hydrogen analyzer is being just Really.
7. the method for calibration of ammonia gas in nitridation furnace resolution ratio according to claim 4, which is characterized in that walked in the step S6 Rapid 5, which obtain ammonia decomposition and hydrogen analyzer, obtains ammonia decomposition and differs by more than ± 2%, then the reading of hydrogen analyzer is wrong.
8. the method for calibration of ammonia gas in nitridation furnace resolution ratio according to claim 7, which is characterized in that the step S6 is also wrapped The maintenance to hydrogen analyzer is included, i.e., the pneumatic filter of hydrogen analyzer is cleared up.
CN201711423745.9A 2017-12-25 2017-12-25 A kind of calibration equipment and its method of calibration of ammonia gas in nitridation furnace resolution ratio Pending CN108169277A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113376055A (en) * 2021-06-08 2021-09-10 青岛丰东热处理有限公司 Nitrogen potential calculation method and system

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Application publication date: 20180615

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