CN206362732U - A kind of nitrogen content detection device - Google Patents
A kind of nitrogen content detection device Download PDFInfo
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- CN206362732U CN206362732U CN201620500792.3U CN201620500792U CN206362732U CN 206362732 U CN206362732 U CN 206362732U CN 201620500792 U CN201620500792 U CN 201620500792U CN 206362732 U CN206362732 U CN 206362732U
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Abstract
The utility model discloses a kind of nitrogen content detection device, including:Sample introduction processing unit;Burner, for the burning of testing sample, and produces mixed gas;Reduction apparatus, the reduction apparatus is connected with the burner so that the mixed gas is reduced in the reduction apparatus;Purifier, the purifier is connected with the reduction apparatus, to be purified to the mixed gas after reduction;Detection means, the detection means is connected with the purifier, to be detected to the nitrogen content in purified gas.The utility model is solved in the prior art using corrosivity soda acid, the technological deficiency such as operating procedure is complicated, time-consuming and environmental pollution is serious.
Description
Technical field
The utility model belongs to detection technique field, more particularly to a kind of nitrogen content detection device.
Background technology
The measure of full nitrogen/protein content is widely used in dairy products, food, animal feed, cereal, fertilizer, tobacco, plant
The detection of the products such as thing, traditional detection means is Kjeldahl's method, and it for many years, but uses corrosion as industrial standard executed
Property soda acid, operating procedure is complicated, time-consuming and environmental pollution be seriously difficult to meet now detection development the need for.Specifically,
It is under conditions of having catalyst, organic nitrogen to be all transformed into inorganic ammonium salt with concentrated sulfuric acid sample digestion, then in alkaline bar
Ammonium salt is converted into ammonia under part, the acid solution absorption of excess is distillated and be with vapor, then with standard acidometric titration, so as to calculate sample
Nitrogen content in product, that is, predominantly detect process and titrated to clear up → distillation →.Clear up and be mainly manually with titration process,
Process is tired multiple and takes, and operating personnel are required with the possibility that higher and error is produced is larger.Importantly, in digestion process
Strong acid need to be used, to the safe there is also very big hidden danger of operating personnel, and time-consuming, workload big, makes detection efficiency relatively low,
The need for coherent detection unit far can not be met.
Utility model content
The utility model provides a kind of nitrogen content detection device, solves or part is solved in the prior art using corrosion
Property soda acid, the technological deficiency such as operating procedure is complicated, time-consuming and environmental pollution is serious.
According to one side of the present utility model there is provided a kind of nitrogen content detection device, including:Burner, is used for
The burning of testing sample, and produce mixed gas;De-watering apparatus, the de-watering apparatus is connected with the burner, for going
Except the moisture in the mixed gas produced after burner burning;Wherein, the de-watering apparatus includes:One-level is removed water
Mechanism, two grades of water removal bodies;Third class de-watering mechanism, the one-level water removal body, two grades of water removal bodies and the three-level are removed
Water dispenser structure is sequentially connected with, and the one-level water removal body is connected with the burner so that after the burner burning
Mixed gas sequentially passes through the one-level water removal body, two grades of water removal bodies and the third class de-watering mechanism and removed water;
Reduction apparatus, the reduction apparatus is connected with the third class de-watering mechanism so that from the third class de-watering mechanism come out after it is mixed
Gas is closed to be reduced in the reduction apparatus;Purifier, the purifier is connected with the reduction apparatus, with to reduction
Mixed gas afterwards is purified;Wherein, the purifier includes:First class purification mechanism;Secondary purification mechanism;The one-level
Purification mechanism and the secondary purification mechanism are in parallel, and one end after parallel connection is connected with the reduction apparatus, described to receive
The mixed gas produced after reduction apparatus burning;Three-level purification mechanism, the three-level purification mechanism with it is in parallel after the one-level
Purification mechanism and the other end of the secondary purification mechanism connection so that the three-level purification mechanism respectively with the first class purification
Mechanism, secondary purification mechanism are in series, and pass through the first class purification mechanism and described to be received by the three-level purification mechanism
Gas after secondary purification mechanism purified treatment;Detection means, the detection means is connected with the purifier, with to purification
The nitrogen content in gas afterwards is detected;Display device, the display device is connected with the detection means and carries out signal
Transmission, to receive the data message that the detection means is detected, and shows to the data message;Sample introduction processing dress
Put, the sample introduction for entering early stage of advancing to the testing sample is handled;And the burner is fitted vertically in the sample introduction
The top of processing unit so that the testing sample after sample introduction processing by early stage passes through the sample introduction processing unit, quilt
Send into the burner and burn.
Optionally, the burner is combustion furnace of the temperature control at 1100 DEG C;And the combustion furnace includes:Body of heater,
So that the testing sample burns in the furnace interior;Electron electric power device, is connected with the body of heater, for the body of heater
The temperature environment of 1100 DEG C of offer, so that the testing sample fully oxidized burning in the body of heater;Heating element heater, it is described to add
Thermal element is uniformly arranged on the inwall of the body of heater, the temperature of the inside of the body of heater is uniformly divided in the body of heater
Cloth.
Optionally, the heating element heater is the associated layer that Tercod is made, and is attached to the inwall of the body of heater
On.
Optionally, the sample introduction processing unit also includes:At least one sampler, takes described in each in vertical direction
Sample device is respectively positioned on the lower section of the burner;The crucible being adapted with the sampler quantity, each described crucible correspondence
Ground is fixed on a sampler, and is placed with the testing sample at least one described crucible;Mechanical arm, is set
There is correspondence on the lever arm being adapted with the sampler quantity, each lever arm to fix a sampler, to pass through
The up and down action of the lever arm drives the corresponding sampler to move up and down, then promote accordingly the crucible enter institute
State in burner.
Optionally, the reduction apparatus includes:Current divider, the current divider is connected with the third class de-watering mechanism, with right
The mixed gas transferred out by the third class de-watering mechanism is shunted;Reduction furnace, the reduction furnace respectively with the current divider
It is connected with the detection means, to be reduced to the gas after shunting, and the gas after reduction is sent into the detection means
It is middle to be detected.
Optionally, the first class purification mechanism includes:First absorber and the second absorber;The first absorber difference
It is connected with the reduction apparatus and second absorber;And, the secondary purification mechanism includes:3rd absorber and the 4th is inhaled
Adnexa;3rd absorber is connected with the reduction apparatus and the 4th absorber respectively;And, the three-level purification mechanism
Including:5th absorber and the 6th absorber;5th absorber is connected with second absorber respectively, the described 4th inhales
Adnexa and the 6th absorber connection, the 6th absorber are connected with the detection means.
Optionally, first absorber is sulfur dioxide/carbon dioxide halogen absorber;Second absorber is water
Absorber;And/or, the 3rd absorber is sulfur dioxide/carbon dioxide halogen absorber;4th absorber is that water is inhaled
Adnexa;And/or, the 5th absorber is sulfur dioxide/carbon dioxide halogen absorber;6th absorber is water absorption
Device.
Optionally, the detection means includes:TCD thermal conductivity detector (TCD)s;Mass flowmenter;Wherein, the TCD Thermal Conductivities
Device is connected with the purifier and the mass flowmenter respectively.
Optionally, the one-level water removal body includes:First glass physical condenser, the first electronic cooling dehydrater and
One adsorbent;The first glass physical condenser connects with the burner and the first electronic cooling dehydrater respectively
Connect;First adsorbent is connected with the first electronic cooling dehydrater;And, two grades of water removal bodies include:Second glass
Glass physics condenser, the second electronic cooling dehydrater and the second adsorbent;The second glass physical condenser respectively with it is described
First adsorbent and the second electronic cooling dehydrater connection;Second adsorbent and the second electronic cooling dehydrater
Connection;And, the third class de-watering mechanism includes:3rd glass physical condenser, the 3rd electronic cooling dehydrater and the 3rd absorption
Agent;The 3rd glass physical condenser is connected with second adsorbent and the 3rd electronic cooling dehydrater respectively;Institute
State the 3rd electronic cooling dehydrater and the 3rd adsorbent connection;3rd adsorbent is connected with the reduction apparatus.
Optionally, the first glass physical condenser is third generation double-tee glass condenser, the first electronics system
Cold dehydrater is semiconductor cooler, and first adsorbent is silica gel, activated alumina or activated carbon;And/or, described
Two glass physical condensers are third generation double-tee glass condensers, and the second electronic cooling dehydrater is semiconductor refrigerating
Device, second adsorbent is silica gel, activated alumina or activated carbon;And/or, the 3rd glass physical condenser is
The double tee glass condensers of three generations, the 3rd electronic cooling dehydrater is semiconductor cooler, and the 3rd adsorbent is silicon
Glue, activated alumina or activated carbon.
A kind of nitrogen content detection device that the utility model is provided, at least including sample introduction processing unit, burner, reduction
Device, purifier, detection means.Wherein, the sample introduction processing unit is connected with the burner, to enter to advance to sample
Sample processing, the burner is connected with the reduction apparatus so that testing sample fully burns in the burner, and
Produce mixed gas.Reduction apparatus is connected with purifier simultaneously so that produced mixed gas is passed through in purifier
A series of control techniques are purified.Realize and purity nitrogen molecule is comprised only in the gas after final purification, and the purifier and institute
State detection means connection so that the content of nitrogen in purified gas, detected by the detection means.The utility model is implemented
In example, the total nitrogen analysis system that there is multistage to remove water purifying function is constituted by least the above device, traditional skill is instead of
Used in art caused by Kjeldahl's method using corrosivity soda acid, operating procedure is complicated, time-consuming and environmental pollution is serious
Technological deficiency.
Brief description of the drawings
, below will be to embodiment in order to illustrate more clearly of the utility model embodiment or technical scheme of the prior art
In required for the accompanying drawing that uses be briefly described, it should be apparent that, drawings in the following description are only of the present utility model
Some embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to this
A little accompanying drawings obtain other accompanying drawings.
The structural schematic block diagram one for the nitrogen content detection device that Fig. 1 provides for the utility model embodiment;
The structural schematic block diagram two for the nitrogen content detection device that Fig. 2 provides for the utility model embodiment;
The structural schematic block diagram three for the nitrogen content detection device that Fig. 3 provides for the utility model embodiment;
Fig. 4 be Fig. 2 in burner structural schematic block diagram;
Fig. 5 be Fig. 2 in sampling processing unit structural schematic block diagram;
Fig. 6 be Fig. 2 in de-watering apparatus structural schematic block diagram;
Fig. 7 be Fig. 2 in reduction apparatus structural schematic block diagram;
Fig. 8 be Fig. 2 in purifier structural schematic block diagram;
Fig. 9 be Fig. 2 in detection means structural schematic block diagram;
The schematic flow sheet one of the method for the measure nitrogen content that Figure 10 provides for the another embodiment of utility model;
The schematic flow sheet two of the method for the measure nitrogen content that Figure 11 provides for the another embodiment of utility model;
Figure 12 is the schematic flow sheet of water removal phase in Figure 11;
Figure 13 is the schematic flow sheet of purifying step in Figure 11;
Figure 14 is the schematic flow sheet of reduction step in Figure 11;
The overall structure diagram for the nitrogen content detection device that Figure 15 provides for the utility model embodiment.
Embodiment
Below in conjunction with the accompanying drawing in the utility model embodiment, the technical scheme in the utility model embodiment is carried out
Clearly and completely describe, it is clear that described embodiment is only a part of embodiment of the utility model, rather than whole
Embodiment.Based on the embodiment in the utility model, the every other embodiment that those of ordinary skill in the art are obtained all belongs to
The scope protected in the utility model;Involved "and/or" keyword wherein in this implementation, represent and or two kinds of situations, change
Sentence is talked about, and A and/or B mentioned by the utility model embodiment illustrate A and B, two kinds of situations of A or B, describe A and B and deposited
Three kinds of states, such as A and/or B, represent:Only including A does not include B;Only including B does not include A;Including A and B.
Meanwhile, in the utility model embodiment, when component is referred to as " being fixed on " another component, it can be directly another
On one component or there can also be a component placed in the middle.When a component is considered as " connection " another component, it can be
It is directly connected to another component or may be simultaneously present component placed in the middle.When a component be considered as " being arranged at " another
Component, it can be set directly on another component or may be simultaneously present component placed in the middle.The utility model embodiment
Used in term " vertical ", " level ", "left", "right" and similar statement be merely for purposes of illustration, not
It is intended to limit the utility model.
Specifically referring to Fig. 1, the utility model embodiment provides a kind of nitrogen content detection device, at least including burning dress
Put 200, reduction apparatus 400, purifier 500 and detection means 600.Wherein, the burner 200 and the reduction apparatus
400 connections so that testing sample fully burns in the burner 200, and produces mixed gas.While reduction apparatus
400 are connected with purifier 500 so that produced mixed gas passes through a series of control techniques institutes in purifier 500
Purification.Realize and purity nitrogen molecule is comprised only in the gas after final purification, and the purifier 500 and the detection means 600
Connection so that the content of nitrogen in purified gas, is detected by the detection means.In the utility model embodiment, pass through
At least the above burner 200, reduction apparatus 400, purifier 500 and detection means 600 constitute the nitrogen content detection and set
It is standby, instead of in conventional art use Kjeldahl's method caused by using corrosivity soda acid, operating procedure is complicated, time-consuming and
The serious technological deficiency of environmental pollution.
In order to be elaborated to the nitrogen content detection device that the utility model embodiment is provided, with reference to Fig. 2-9 points
It is other that burner 200, reduction apparatus 400, purifier 500 and detection means 600 are elaborated, further to support this
Utility model technical problem to be solved.
For burner 200,
Temperature Distribution due to the temperature range of burning and in stove has vital effect to test result.
Therefore, the burner 200 described in the utility model embodiment is 1100 DEG C of combustion furnaces, and is uniform constant temperature.
Specifically, referring to Fig. 4,1100 DEG C of combustion furnaces at least include:Body of heater 201, for automatic constant temperature temperature control
Power electronic equipment 202 and heating element heater 203.Wherein, the power electronic equipment 202 is used to maintain inside body of heater 201
1100 DEG C of high temperature, to ensure testing sample fully oxidized burning in the body of heater 201, so as to eliminate due in body of heater 201
The temperature in portion is relatively low and can not make the oxidation of clearing up of the testing sample substantially uniformity, and causes unnecessary to test experiments do
Disturb, and then improve the degree of accuracy of test result.Meanwhile, heating element heater 203 is evenly provided on the surrounding of the inwall of body of heater 201, makes
The high temperature of furnace interior is uniformly distributed, so that testing sample thermally equivalent, it is ensured that sample uniform decomposition in combustion furnace, so that
Further obviate due to the even technological deficiency brought of the temperature distributing disproportionation inside body of heater 201.It should be noted that this implementation
Heating element heater 203 described in example can uniformly be arranged on the inwall of body of heater 201, naturally it is also possible to be arranged on the outer of body of heater 201
Wall, when being arranged on the outer wall of body of heater 201, can also set one layer of overcoat, with to place in the periphery of the heating element heater 203
Protected in the heating element heater 203 of the outer wall of body of heater 201.The overcoat can be made up of heat insulation layer and protective layer two parts.
Its heat insulation layer is made up of heat-insulating material filling, and protective layer is fixed on the outside of insulating barrier, so that insulating barrier is located at the outer wall of body of heater 201
Between protective layer.Protective layer outside insulating barrier can be the sheetmetal plate or insulation board of network structure, to prevent foreign objects
Body is collided or friction heat insulation layer.
Preferably, the combustion furnace can be a kind of circulating combustion furnace, also with unique combustion furnace sample introduction blowback system
System, it is ensured that all nitrogen component complete oxidations, to eliminate the interference of environmental factor, beneficial to low content sample detection, so as to realize
More accurate analysis, it is ensured that the reliability of result.
As a preferred embodiment, above-mentioned power electronic equipment 202 can be an applying electronic pipe higher-order of oscillation electricity
The automatic constant temperature controller on road, wherein, the energy storage coil of the electron tube high-frequency oscillating circuits is due to coupling the appropriate of electrical storage device
Coordinate, a certain frequency of oscillation can be secured to;Energy storage coil has constant temperature index, and has large-scale thermocouple thermometer, bright
Really indicate the temperature of high temperature furnace;Meanwhile, there is a metal penoncel on the pointer of energy storage coil, when furnace temperature is raised to required temperature, temperature
When the penoncel and energy storage coil for spending index are coupled, oscillating current stops at random, and electron tube plate current therefore changes, and makes it grasp
An extremely sensitive relay is indulged, then controls a strength relay to cut off the electric current of heating wire with this, temperature is no longer increased,
Upon a drop in temperature, the penoncel of pointer loses with energy storage coil couples, and electron tube recovers vibration, controlled strength relay again
Also recover to edge up again by the electric current of high temperature furnace, furnace temperature simultaneously.It is so interrupted because of electric current, automatic keep a constant temperature to reach
The purpose of degree.
Likewise, as a preferred embodiment, above-mentioned heating element heater 203 can be high-quality Tercod;
It should be noted that in the utility model embodiment, testing sample enters before burner 200, can be with
The physical treatment of early stage is carried out by sample introduction processing unit 100.Wherein, the early stage physical treatment of the testing sample can be divided into as
Lower two kinds of situations:(1) if testing sample is the solid sample of anisotropic, testing sample is pulverized and sieved into place before sample is claimed
Reason;(2) if testing sample is liquid and sauce class sample, directly it can claim in crucible.Wherein, implement in the utility model
Crucible is reusable described in example, to reach the technique effect without consumptive material.Meanwhile, required for the utility model embodiment
Crucible can be one kind in following crucible:Quartz, ceramics, steel, nickel, platinum etc., to reach the purpose for being applicable various testing samples.
When using other instruments analysis so as to overcome, the necessary pressing mold shaping of sample simultaneously just can sample introduction analysis, sample system with tinfoil parcel
Standby complicated, tin can is medical disposable material, and operating cost is high, combustion-supporting gas and the more technological deficiency of carrier gas consumption.Further, by
In the utility model embodiment without any extra sample chemical processing such as digestion and the chemical reagent of toxicity, so as to eliminate
Traditional Kjeldahl's method complex operation, digestion time length, the technological deficiency that environmental pollution is serious, safety coefficient is low.
In the utility model embodiment, the testing sample is directly weighed in the repeatedly used crucible, earthenware
Crucible be located at sampler on and can Reusability, the testing sample weigh can using PC ends automation record by the way of,
That is, sample introduction processing unit 100 can at least include an electronic weigher, can in real time be weighed and be located at by the electronic weigher
The quality of sample in crucible, and by the weight data information transfer gathered into PC ends, generate weight DBMS and preserve, from
And effectively eliminate the technological deficiency by recording error and/or calculation error caused by manual entry data.
Explanation is needed exist for, in order to be able to which data measured in the utility model embodiment are stored and shown
Show.Preferably, continuing with referring to Fig. 2, the utility model embodiment is additionally provided with a data storage 800 and a display device
700.Wherein, the data storage 800 carries out signal transmission with the electronic weigher and the detection means respectively, with right
The data of reception are stored.Meanwhile, display device is connected with the detection means and carries out signal transmission, to receive the inspection
The data message that device is detected is surveyed, and the data message is shown.Certainly, display device here can include one
The display end 702 of power supply source 701 and one.The display end 702 is connected with the power supply source 701, to pass through the power supply source 701
The display end 702 is powered in real time, and the display end 702 carries out signal transmission with the detection means.It is worth one
It is mentioned that, the display end is liquid crystal display.
Further, the sample introduction processing unit 100 at least includes:Sampler 101, mechanical arm 102, power source 103,
Plus/minus speed mechanism, transmission device and bracket institution etc.;Wherein, the sampler 101 is porous plate disc structure.It is intrinsic thereon
One crucible 104;Mechanical arm 102 is rotationally fixed on the sampler 101, and the power source 103 is mechanical arm 102
Operation provides power, to drive sampler 101 to be moved by the motion of mechanical arm 102, and then realizes that drive crucible 104 enters
Row motion.Here power source 103 can select stepper motor or servomotor as controlled motor.But preferably, this reality
With new embodiment from stepper motor as mechanical arm 102 power source 103, make it have control mode flexibly, occupation of land face
The advantages of product is small, cheap.Meanwhile, plus/minus speed mechanism, transmission device are connected with mechanical arm 102 respectively so that by adding/
Motion of the reducing gear to mechanical arm 102 is accelerated or slowed down, bracket institution to mechanical arm 102, acceleration and deceleration mechanism and/
Or transmission device is supported.And transmission device can be ball screw nut transmission, so that the rotation of mechanical arm is transported
It is dynamic to be converted to linear motion, to promote the crucible equipped with testing sample to be moved.Wherein, the fast mechanism of plus/minus and transmission device
Mechanical structure and motion principle think prior art, here is omitted.
In detail, in the utility model embodiment, 1100 DEG C of combustion furnaces are using unique upper furnace structure and under
And on vertical input mode.That is, body of heater 201 is located at the top of sampler 101.
Wherein, the transmission of the sampler 101 passes through the company of control using the vertical input mode of linear pattern from bottom to top
The mechanical arm 102 for being connected to the sampler 101 heads into the crucible 104 on sampler 101 in body of heater 201 so that sample
After being burnt completely in combustion furnace, it is transferred on sampler 101 by mechanical arm 102 from top to bottom.Sample after ashing is then protected
Stay in crucible 104, and instrument can be transferred to by controlling sampler 101 by the automatic interference-free of sample after ashing after analysis
Outside device, dust is cleaned without blow-on, without maintenance;Sample direct injected, without being wrapped up with tinfoil, without pressing mold, reaches solid
Body, fluid sample test all can obtain accurate result.The design is substantially shorter detection cycle, and can extend thermal cycle part
Service life (4-5 times).Determine to use the Dumars of the next furnace design to determine in blood urea/nitrogen analyzer so as to effectively overcome tradition
Nitrogen instrument sample must pressing mold be molded and after being wrapped up with tinfoil just can sample introduction analysis, and in cinder catcher sample ash reach it is a certain amount of
The technological deficiency that necessary manual blow-on removes the dust in cinder catcher afterwards.
The utility model embodiment can not only be realized solid by using unique upper furnace structure and vertical input mode
The quick detection of body, fluid sample, moreover it is possible to reach the full automation from sample process to assay.In addition, burning is produced
Carrier gas stream can take away sample dust automatically, without blow-on clean dust, without maintenance, realize that multiple samples are detected simultaneously, and
And sample-adding can be circulated.This improvement can greatly promote automaticity, shorten sample processing time, improve system effectiveness, and
System service life can significantly be extended.
It should be strongly noted that in the utility model embodiment, due to the testing sample and in burner 200
Contain moisture in the product of interior burning, therefore the gaseous state NOx come out from burner 200 is needed by de-watering apparatus 300
Carry out removing water process.The de-watering apparatus 300 is connected between the burner 100 and the reduction apparatus 400, specifically may be used
As shown in Figures 2 and 3.
Certainly, it is necessary to which in explanation, sample introduction processing unit 100 here, the quantity of sampler 101 can also be many
Individual, mechanical arm 102 is provided with the multiple lever arms being adapted with the quantity of sampler 101, each lever arm and is fixed with one
A crucible is fixed with corresponding sampler, each sampler 101.It can thus cause by set by mechanical arm 102
Several lever arms put, while being flexibly controlled to several samplers 101, i.e. realize selectivity to sampler
Sample in 101 is burnt.
Further, refer to shown in Figure 15, de-watering apparatus 300 described in the utility model embodiment is removed water including one-level
Mechanism 310, two grades of water removal bodies 320 and third class de-watering mechanism 330.Wherein, the one-level water removal body 310 and described two grades are removed
Water dispenser structure 320 is in parallel, and regard the one-level water removal body 310 after parallel connection and two grades of water removal bodies 320 as an entirety
From the point of view of, its one end is connected with the burner, to receive the mixed gas produced after the burner burning;The other end with
The third class de-watering mechanism 330 is connected so that the third class de-watering mechanism 330 respectively with the one-level water removal body 310, two grades
Water removal body 320 constitutes the structural relation of series connection, is removed with realizing to receive by the third class de-watering mechanism 330 by the one-level
Water dispenser structure 310 and two grades of water removal bodies 320 remove the mixed gas after water process.
It should be noted that in the utility model embodiment, why de-watering apparatus 300 is arranged into multistage water removing machine
Structure, one side purpose is to be to carry out mixed gas multistage water removal, is sufficiently removed with the moisture ensured in mixed gas.Separately
On the one hand by the one-level water removal body 310 and two grades of water removal bodies 320 by the way of being connected in parallel, so that from
The mixed gas of burner output is carried out in the receiving terminal of the one-level water removal body 310 and two grades of water removal bodies 320
Mixing, buffering, are balanced, it is to avoid the mixed gas gas of output with the airflow rate to the mixed gas exported by burner
Flow excessive velocities and can not fully be removed water.Simultaneously by the one-level water removal body 310 after parallel connection and two grades of water removals
Mechanism 320, the mixed gas exported is in the output end mixing of one-level water removal body 310 and two grades of water removal bodies 320, Ran Hou
Flow into and removed water again in third class de-watering mechanism 330, same principle, this also causes by one-level water removal body 310 or two grades
The airflow rate of mixed gas of the output end output of water removal body 320 obtained effective buffering, balance, it is to avoid mixing for output
Close air velocity after gas input third class de-watering mechanism too fast and can not fully be removed water.
Certainly, in the utility model embodiment, the one-level water removal body 310 and two grades of water removal bodies 320 phase
Parallel connection, and using the one-level water removal body 310 after parallel connection and two grades of water removal bodies 320 as one on the whole, its one end
It is connected with the burner, to receive the mixed gas produced after the burner burning;The other end is removed with the three-level
Water dispenser structure 330 is connected so that the third class de-watering mechanism 330 respectively with the one-level water removal body 310, two grades of water removal bodies
320 constitute the structural relation of series connection, and this kind of connected mode can be defined as to the connected mode 1 of water removal body.Certainly, the connection
Mode 1 is only merely a kind of connection side between one-level water removal body 310, two grades of water removal bodies 320 and third class de-watering mechanism 330
Formula, the utility model embodiment is not limited to.
Words sentence is talked about, for other companies of one-level water removal body 310, two grades of water removal bodies 320 and third class de-watering mechanism 330
Mode is connect, as long as the technique effect effectively removed water can be reached, the utility model embodiment is may also apply to.Such as, for letter
Change structure design, the utility model embodiment can use the connected mode 2 of water removal body, directly mutually go here and there three water removal bodies
Connection, i.e., one-level water removal body 310, two grades of water removal bodies 320 and third class de-watering mechanism 330 are sequentially connected with, or in order to reduce into
This, using the connected mode 3 of water removal body, removes third class de-watering mechanism, by two grades of water removal bodies 320 and one-level water removal body
310 are in series.Again or in order to further reduce manufacturing cost, using the connected mode 4 of water removal body, only removed from one-level
Any one water removal body in water dispenser structure 310, two grades of water removal bodies 320 and third class de-watering mechanism 330, and respectively with burner
Connected with reduction apparatus, with the technical scheme for the technique effect for reaching water removal, also within protection domain of the present utility model.Need
It should be noted that one-level water removal body 310, two grades of water removal bodies 320 and third class de-watering mechanism in the utility model embodiment
" one-level ", " two grades ", " three-level " in 330 is only to carry out coding label to several water removal bodies, to describe convenient description,
Namely three water removal bodies are identical in the utility model embodiment.
That is, in the utility model embodiment, the one-level water removal body 310 can include:First glass physical
Condenser 301, the first electronic cooling dehydrater 302 and the first adsorbent 303.Two grades of water removal bodies 320 can include:The
Two glass physical condensers, the second electronic cooling dehydrater and the second adsorbent;The three-level purification mechanism 330 can include:
3rd glass physical condenser, the 3rd electronic cooling dehydrater and the 3rd adsorbent.
Due to one-level water removal body 310, two grades of water removal bodies 320 and third class de-watering mechanism in the utility model embodiment
330 completely similarly hereinafter, below only by taking the connected mode 4 of above-mentioned water removal body as an example, to be elaborated to the utility model, is placed in
The connected mode 1 of water removal body, 2,3 non-detailed portions, and two grades of water removal bodies 320, the self structures of third class de-watering mechanism 330
Non- detailed portion, also referring to the specific descriptions of one-level water removal body 310 in connected mode in water removal body 4.
Specifically, Fig. 3 is referred to, for the one-level water removal body 310 in the connected mode 4 of water removal body, its
Including the first glass physical condenser 301, the adsorbent 303 of the first electronic cooling (2 DEG C) dehydrater 302 and first.Wherein, in institute
State in de-watering apparatus 300, removed water first by the first glass physical condenser 301, then pass through the first electronic cooling dehydrater 2
DEG C water removal, finally by the first adsorbent 303 adsorb remove water.That is, first allow after being burnt by the first glass physical condenser 301
Product carry out physics cooling and removed water by the way that vapor is liquefied, then pass through the further cooling of the first electronic cooling dehydrater 302
Under test gas simultaneously removes vapor again by by vapor liquefaction, fully absorbs moisture finally by the first adsorbent 303
The purpose thoroughly removed water with reaching, to ensure that the combustion product vapor is removed completely, so that moisture is completely eliminated to nitrogen content
The influence of the degree of accuracy of measure.
Preferably, in the de-watering apparatus 300 that the utility model embodiment is provided, the first glass physical condenser
301 can be third generation double-tee glass condenser, and 2-3 degrees Celsius is rapidly decreased to from high temperature, will be contained in combustion product
Water vapor condensation Cheng Shui, moisture then extracted and separated.Complete first step water removal.It is noted that this practicality is new
It is necessary to carry out the first step to condense water removal by the first glass physical condenser 301 in type embodiment, by high-temperature combustion product
Efficiently significantly cool, it is reduced to 2-3 DEG C, then provide and remove for the follow-up electronic cooling of electronic cooling dehydrater 302 water removal
Water condition.
Further, the first electronic cooling dehydrater 302 can be semiconductor cooler, using extraordinary semiconductor material
The P-N junction that material is constituted, formation thermocouple pair, generation Peltier effect (when two kinds of different metals are connected and pass to electric current,
Have joint heat absorption, another joint heat release), i.e., a kind of New Refrigerating method freezed by direct current.Electronic cooling effect
It is exactly principle by thermoelectricity to produce, and is the cooling piece of a monolithic, it is made up of two panels potsherd, has N-type and p-type in the middle of it
Semi-conducting material (bismuth telluride), this semiconductor element be on circuit with cascade connect constitute.Semiconductor chilling plate
Operation principle be:When one piece of N-type semiconductor material and one piece of p-type semiconductor material are coupled to galvanic couple pair, with copper sheet two
Individual semiconductor is connected.Connect in this circuit after DC current, the transfer with regard to energy can be produced, electric current is by N-type element
The joint for flowing to p-type element absorbs heat, and as cold end, the joint for flowing to N-type element by p-type element discharges heat, as heat
End.The heat in hot junction is taken away by various radiating modes, cold end is with regard to that can keep lower temperature.The size of heat absorption and heat release is logical
The size of overcurrent and semi-conducting material N, P element logarithm are determined.Galvanic couple is unified into by up to a hundred inside cooling piece
Thermoelectric pile, to reach the effect of enhancing refrigeration, when heat load is zero, most strong refrigeration can reach 80 DEG C of temperature difference.Electronics
The temperature difference amplitude limitation of refrigeration, also further illustrates the necessity of the first step glass physical condensation water removal.
And then, due to having there is the water removal phase of first two steps, most moisture have been removed, so only needing to
The first a small amount of adsorbent 303 is that can reach the effect for eliminating moisture well, so that the usage amount of adsorbent is greatlyd save,
Traditional azotometer is overcome using the high defect of a large amount of adsorbent costs.Preferably, the absorption in the utility model embodiment
Agent can be silica gel, activated alumina or activated carbon.
Finally it should be noted that by above-mentioned one-level water removal body 310, effectively ensuring by burner 200
Combustion product vapor afterwards is removed completely, to be completely eliminated influence of the moisture to the degree of accuracy of nitrogen analysis, and can be with
Direct Analysis fluid sample, so as to substantially reduce the use of adsorbent, reduces operating cost.Certainly, as stated above, herein
The utility model is only entered exemplified by only including one-level water removal body 310 in de-watering apparatus 300 come the operation principle to water removal body
Row description, also can be by one-level water removal body 310, two grades of water removal bodies 320 and third class de-watering mechanism during actual job
330 constitute de-watering apparatus 300 to carry out efficient water-removing according to above-mentioned connected mode 1-3, and the utility model does not limit to, herein
Also repeat no more.
Secondly, for reduction apparatus 400,
The reduction apparatus 400 includes:Reduction furnace 402, part flow arrangement 401, non-dispersive IR line (NDIR) sensor
403.Wherein, the part flow arrangement 401 and the direct phase of the electronic cooling (2 DEG C) dehydrater 302 in higher level's de-watering apparatus 300
Even, then it is connected with the reduction furnace 402, is sensed between the reduction furnace 402 and the purifier 500 by the NDIR
Device 403 is connected.
Specifically, part flow arrangement 401 described in the utility model embodiment is a kind of accurate gas diverter, shunting
Ratio is 1/35 or 1/80, the Partial flow dilution gas before gas is reduced into reduction furnace 402, so as to reach saving copper reduction stove
The consumption of 402 reducing agent and the purpose for saving the cost measured every time, meanwhile, built-in membrane disappears deimpurity interference.Specifically
Ground, it is because N (nitrogen) burning conversions are into substantial amounts of gaseous NOx, too high for detector concentration, and reduced
During can consume substantial amounts of reducing agent, therefore, out and three will be passed through from the burner 200 by part flow arrangement 401
Detection is reduced after gaseous sample shunting after individual condensing unit condensation water removal, remaining gas passes through adsorbent adsorption treatment heel row
Remove.
The nitrogen oxides generated burn after the accurate gas diverter shunting, is spread using helium as carrier gas
Send, the nitrogen oxides is completely reduced in 600 DEG C of copper reduction stoves as dinitrogen, while excessive oxygen is combined into oxidation by copper
Copper.Using non-dispersive IR line (NDIR) sensor for controlling the amount of oxygen needed for best combustion, this can ensure oxygen
Consumption with copper is minimum, and highest can save 95% oxygen consumption.
(non-dispersive IR line) sensor 403 used in the utility model embodiment can be measured in mixed gas not
With the concentration of gas.Asymmetric double atom and polyatomic gas have selection absorbability to infrared energy.This property is
A kind of property that infrared active material has in itself, with uniqueness, such as the DNA of human body, everyone DNA is different,
And will not change because of the change of any environmental factor or condition, therefore material can be carried out according to this property qualitative and fixed
Amount analysis.Different gas has different absorption spectrums, and spectral line of the absorption spectrum in the range of certain frequency is constituted, had
The absorption intensity of each Frequency point is different in certain broadband, broadband.If infrared radiating light spectral limit includes tested
The absorption bands of gas is strong in the energy of corresponding frequencies infra-red radiation when infra-red radiation is by air chamber full of tested gas
Degree is actually taken up by gas and causes the decay of energy, and gas concentration is bigger, and energy attenuation is more severe, by analyzing attenuation
It is finally inversed by the concentration of under test gas.
The detection method of non-dispersive IR line (NDIR) the principle sensor 403 can use spectral absorption calculus of finite differences
Detection.Infrared light is sent by light source and passes through divided beams, after reference channel and tested passage air chamber absorb, optical signal is detected
Device, which is converted into after electric signal, carries out enhanced processing.Because the change of such environmental effects and infrared light is to the effect phase of two paths of signals
Together, difference detecting method eliminates the influence of these destabilizing factors, can truly reflect tested gas concentration information.
Again, for purifier 500,
Continuing with referring to Figure 15, purifier 500 described in the utility model embodiment include first class purification mechanism 510,
Secondary purification mechanism 520 and three-level purification mechanism 530.Wherein, the first class purification mechanism 510 and the secondary purification mechanism
520 are in parallel, and using the first class purification mechanism 510 after parallel connection and the secondary purification mechanism 520 as one on the whole, its
One end is connected with the reduction apparatus 400, to receive the gas produced after the reduction apparatus reduction;The other end and the three-level
Purification mechanism 530 is connected so that the three-level purification mechanism 530 respectively with the first class purification mechanism 510, secondary purification mechanism
520 constitute the structural relation of series connection, pass through the first class purification mechanism to realize to receive by the three-level purification mechanism 530
510 and the purified treatment of secondary purification mechanism 520 after gas.
It should be noted that in the utility model embodiment, why purifier 500 is arranged into multistage purification machine
Structure, one side purpose is to be to carry out multistage purification to gas, to ensure that mixed gas is sufficiently purified.On the other hand will be described
First class purification mechanism 510 and the secondary purification mechanism 520 are by the way of being connected in parallel, so that from reduction apparatus 400
The mixed gas of output is mixed in the receiving terminal of the first class purification mechanism 510 and the secondary purification mechanism 520, delayed
Punching, is balanced, it is to avoid the mixed gas gas velocity of output with the airflow rate to the mixed gas exported by reduction apparatus 400
Spend fast and can not be fully purified.Simultaneously by the first class purification mechanism 510 and the secondary purification mechanism after parallel connection
520, the mixed gas exported is mixed in the output end of first class purification mechanism 510 and secondary purification mechanism 520, is then being flowed into
Purified again in three-level purification mechanism 530, same principle, this also causes by first class purification mechanism 510 or secondary purification
The airflow rate of mixed gas of the output end output of mechanism 520 obtained effective buffering, balance, it is to avoid the gaseous mixture exported
Air velocity is too fast and can not be fully purified after body input three-level purification mechanism 530.
Certainly, in the utility model embodiment, the first class purification mechanism 510 and the phase of secondary purification mechanism 520
Parallel connection, and using the first class purification mechanism 510 after parallel connection and the secondary purification mechanism 520 as one on the whole, its one end
It is connected with the reduction apparatus 400;The other end is connected with the three-level purification mechanism 530 so that the three-level purification mechanism 530
The structural relation connected is constituted with the first class purification mechanism 510, secondary purification mechanism 520 respectively, can be by this kind of connection side
Formula is defined as the connected mode 1 of purification mechanism.Certainly, the connected mode 1 is only merely first class purification mechanism 510, secondary purification
A kind of connected mode between mechanism 520 and three-level purification mechanism 530, the utility model embodiment is not limited to.
Words sentence is talked about, for other companies of first class purification mechanism 510, secondary purification mechanism 520 and three-level purification mechanism 530
Mode is connect, as long as the technique effect effectively purified can be reached, the utility model embodiment is may also apply to.Such as, for letter
Change structure design, the utility model embodiment can use the connected mode 2 of purification mechanism, directly mutually go here and there three purification mechanisms
Connection, i.e., first class purification mechanism 510, secondary purification mechanism 520 and three-level purification mechanism 530 are sequentially connected with, or in order to reduce into
This, using the connected mode 3 of purification mechanism, removes three-level purification mechanism, by secondary purification mechanism 520 and first class purification mechanism
510 are in series.It is only net from one-level using the connected mode 4 of purification mechanism again or in order to further reduce manufacturing cost
Change any one purification mechanism in mechanism 510, secondary purification mechanism 520 and three-level purification mechanism 530, and respectively with reduction apparatus
Connected with detection means, with the technical scheme for the technique effect for reaching purification, also within protection domain of the present utility model.Need
It should be noted that first class purification mechanism 510, secondary purification mechanism 520 and three-level purification mechanism in the utility model embodiment
" one-level ", " two grades ", " three-level " in 530 is only to carry out coding label to several purification mechanisms, to describe convenient description,
Namely three purification mechanisms are identical in the utility model embodiment.
That is, in the utility model embodiment, the first class purification mechanism 510 can include:First absorber 501
With the second absorber 502.The secondary purification mechanism 520 can include:3rd absorber and the 4th absorber.The three-level is net
Changing mechanism 530 can include:5th absorber and the 6th absorber.
Due to first class purification mechanism 510, secondary purification mechanism 520 and three-level purification mechanism in the utility model embodiment
530 completely similarly hereinafter, below only by taking the connected mode 4 in above-mentioned purification mechanism as an example, to be elaborated to the utility model, puts
Connected mode 1,2,3 non-detailed portions in purification mechanism, and secondary purification mechanism 520, three-level purification mechanism 530 itself knot
The non-detailed portion of structure, also referring to the specific descriptions of first class purification mechanism 510 in connected mode in purification mechanism 4.
Specifically, continuing with referring to Fig. 3, for the first class purification mechanism 510 in the connected mode 4 of water purification mechanism
Speech, it includes the first absorber 501 and the second absorber 502, wherein, first absorber 501 directly with the non-dispersive
Property infrared ray sensor 403 be connected, second absorber 502 is connected with institute detection means 600.Specifically, by reduction
After processing, except nitrogen molecular in air-flow, also contain other impurities, it is therefore desirable to remove in reducing gas by purifier
CO2/SO2, water and halogen, it is ensured that the degree of purity of nitrogen molecular, and then ensure the accurate reliability of test.Gas after reduction passes through
First absorber 501, can remove CO2/SO2 and halogen;Further, can be with then by second absorber 502
Remove moisture removal.By two step adsorption processes, the removal of impurity can be reached, the purpose of gas nitrogen to be detected is purified.Wherein, it is described
First absorber 501 possesses dehalogenation function, can eliminate halogen, effectively prevents halogen from entering the detection means described in subordinate and making
Into infringement, so as to reach the purpose for protecting the detection means.Preferably, first absorber 501 is sulfur dioxide/bis-
Carbonoxide halogen absorber;And/or, second absorber 502 is water absorber.Certainly, as stated above, this reality herein
Only retouched with new exemplified by only including first class purification mechanism 510 in purifier 500 come the operation principle to purification mechanism
State, during actual job, first class purification mechanism 510, secondary purification mechanism 520 and three-level purification mechanism 530 can also be pressed
Constitute purifier 500 to carry out high-efficient purification according to above-mentioned connected mode 1-3, the utility model does not limit to, herein also not
Repeat again.
For detection means 600,
The detection means 600 includes:TCD thermal conductivity detector (TCD)s 601, mass flowmenter 602.Wherein, the TCD thermal conductivities inspection
Survey device 601 directly with the second absorber 502 described in upper level purifier 500 to be connected, the mass flowmenter 602 directly connects
It is connected on after the TCD thermal conductivity detector (TCD)s 601, is last device link of sample detection.
Remaining nitrogen in carrier gas stream is detected using the TCD thermal conductivity detector (TCD)s 601.TCD thermal conductivity detector (TCD)s 601 are also known as heat
Lead pond or heated filament examines hot device, be a kind of the most frequently used detector of gas chromatography.The operation principle of the thermal conductivity detector (TCD) is base
There are different thermal conductivities in gas with various, the sensing element of the detector is heated filament, such as tungsten filament, platinum filament, rhenium silk, and by heat
Silk composition electric bridge, in the thermal conductivity detector (TCD) of the new azotometer, uses tungsten filament, tungsten filament is replaced also with other heated filaments
Can, heated filament has the characteristic that resistance is varied with temperature.When there is a constant dc by the thermal conductivity detector (TCD), heated filament is added
Heat.Because the conduction of heat of carrier gas makes a part of heat of heated filament be taken away by carrier gas, a part is transmitted to pond body.When heated filament is produced
Heat and dissipated heat when reaching balance, hot-wire temperature just stablizes in certain numerical value.Now, heated filament resistance is also stabilized in necessarily
Numerical value.What is be passed through due to reference cell and measuring cell is all pure carrier gas, and same carrier gas has identical thermal conductivity, therefore the electricity of two-arm
Resistance is identical, bridge balance, no signal output, and record system record is straight line.It is pure when there is sample to enter detector
Carrier gas flows through reference cell, and carrier gas carries component air-flow through measuring cell, due to carrier gas and component binary mixture to be measured
Thermal conductivity is different with the thermal conductivity of pure carrier gas, and heat dispersal situations thus change in measuring cell, make in reference cell and measuring cell hole
Difference is generated between heater resistance value, electric bridge disequilibrium, detector has voltage signal output, and recorder draws respective components
Chromatographic peak.The concentration of component to be measured is bigger in carrier gas, and heat conductivity of gas changes more notable, temperature and resistance value in measuring cell
Change also more notable, voltage signal is stronger.The voltage signal now exported is directly proportional to the concentration of sample, and this exactly thermal conductivity is examined
Survey the quantitative basis of device.
Therefore, when with the new azotometer measurement total nitrogen content, in the thermal conductivity detector (TCD), N2 volume contents
Trigger a kind of electronic measurement signal, corrected by it, then by the independent of material, the nitrogen content in sample is with regard to automatically meter
Calculate, print and store.Specifically, the standard correction material uses EDTA or urea, and only needs to regular calibration, nothing
It must every time start shooting and make blank and standard correction.Possess it is simple to operate, the characteristics of be widely used.
The TCD thermal conductivity detector (TCD)s 601 do not destroy monitored component in detection process, are conducive to the collection of sample, or
It is combined with other instruments.The TCD thermal conductivity detector (TCD)s 601 can meet the quantitative requirement of peak height in Industrial Analysis, be suitable for factory
Control analysis.Meanwhile, TCD thermal conductivity detector (TCD)s 601 have a broad working range, measurable covering as little as ppm ranks, up to
The analysis of total nitrogen/protein of percentage concentration content.
The mass flowmenter 602 uses thermal measuring method, i.e., how much is the molecular mass taken away by split molecule
So that to measure flow.Because being measured with thermal, survey will not be had influence on because of the change of gas temperature, pressure
The result of amount.Mass flowmenter 602 be one it is more accurate, quick, reliable, efficiently, stably, flexible flow measurement instrument.
Mass flowmenter 602 can not control flow, and it can only detect the mass flow of liquid or gas, pass through analog voltage, electricity
Stream or serial communication output flow value.
It should be added that, in the utility model embodiment, the concentration for the combustion gas oxygen being passed through is
99.995%, the concentration for the carrier gas stream helium being passed through is 99.99%, and the oxygen and the flow of helium that are passed through are by matter
Amount stream controller is automatically controlled.Wherein, the mass flowmenter 602, is that one kind be able to can be controlled again simultaneously in detection
Instrument.Mass flowmenter 602 itself is except measurement part, also with a solenoid valve or piezo electric valve, such quality
Flow control constitutes a closed-loop system in itself, the mass flow for controlling fluid.The setting value of mass flowmenter 602 can be with
There is provided by analog voltage, analog current, or computer, PLC.
Supplementary notes are needed further exist for, need to also be in the nitrogen content detection device in the utility model embodiment
In built-in 40 DEG C of ± 0.1 DEG C of Thermotank devices, to ensure the dresses such as system detector, current divider, gas collection system, gas circuit control
The temperature constant state put, it is to avoid because the change of environment temperature causes the change of gas flow path stability, improve analysis precision and standard
Exactness.
To sum up, physical treatment of the testing sample by early stage and it is automatic weigh after, in the vertical mechanical sample introduction
Enter in the presence of arm from the sampler in the homogeneous combustion furnace of 1100 DEG C of high temperature, fully burnt with oxygen, then pass through
Combustion product and impurity are carried out cooling de-watering by " condensation of the three steps " device, then are shunted by gas diverter precision
Under test gas sample after burning, then helium is passed through as the current-carrying gas for the gaseous sample being diverted, send into together described
600 DEG C of copper reduction stoves, nitrogen molecular Restore All is come out, meanwhile, the oxygen needed for best combustion is controlled using NDIR sensors
Amount, this can ensure that the consumption of oxygen and copper is minimum, then remove CO2/ by first absorber and the second absorber
Pure nitrogen, is then passed through in the TCD thermal conductivity detector (TCD)s by SO2, halogen and water, detects the concentration of nitrogen, finally by
The mass flowmenter, detects the mass flow of nitrogen, in conjunction with the nitrogen gas concn surveyed, is calculated automatically by software for calculation
Total nitrogen content in the testing sample.
The device embodiment provided based on above-described embodiment, refers to Figure 10-14, another embodiment of the present utility model is also
It is specific as follows there is provided a kind of embodiment of the method corresponding with device embodiment:
Another embodiment of the present utility model provides a kind of method for determining nitrogen content, specifically includes as follows:Step
1000, combustion step for being burnt by burner to testing sample, and produces mixed gas, the combustion step
In, the ignition temperature of the burner is 1100 DEG C, and is constant temperature;Step 2000, reduction step, for passing through reduction apparatus
The mixed gas is reduced, in the reduction step, the reduction temperature of the reduction apparatus is 600 DEG C, and be constant temperature;
Step 3000, purifying step, for being purified by purifier to the mixed gas after reduction, goes the removal of impurity, is remained
Residual air body;Wherein, the impurity at least include it is following in one kind:Water, carbon dioxide or halogen;Step 4000, detection step
Suddenly, for being detected by detection means to the nitrogen content in the remaining gas.
Further, another embodiment of the present utility model also includes;Step 5000, sampling procedure, for passing through sample introduction
Processing unit is sampled, and obtains the testing sample, and the testing sample is sent into the combustion in the way of vertical sample introduction
Burn in device and burnt.Step 6000, water removal phase, for being carried out by the mixed gas produced by the combustion step
Except water process, to remove the moisture in the mixed gas.
Wherein, the water removal phase 6000 also includes following sub-step:Step 6001, the first water removal sub-step, will be described
Mixed gas feeding glass physical condenser is once removed water;Step 6002, the second water removal sub-step, will be by once removing water
Secondary water removal is carried out in mixed gas feeding electronic cooling dehydrater afterwards;Step 6003 the 3rd removes water sub-step, will pass through two
Three water removals are carried out in mixed gas feeding adsorbent after secondary water removal.
Wherein, the purifying step also includes following sub-step:Step 3001, the first purification sub-step, after reduction
Mixed gas feeding sulfur dioxide/carbon dioxide halogen absorber carries out primary purification;Step 3002, the second purification sub-step,
Double purification will be carried out in mixed gas feeding adsorbent after primary purification.
Wherein, the reduction step also includes following sub-step:Step 2001, sub-step is shunted, for being filled by shunting
Put and shunted mixed gas, to be diluted to the mixed gas;Step 2002, atomic step is gone back, after shunting
Gas is reduced in reduction furnace;Step 2003 flow control sub-step, for the flow progress to the oxygen in the reduction furnace
Control.
Due to the method for the measure nitrogen content that another embodiment of the present utility model is provided, with above-mentioned device embodiment phase
Correspondence, thus it is no longer excessive to embodiment of the method herein repeat, non-detailed portion see device implementation in embodiment of the method
Example.
Although having been described for preferred embodiment of the present utility model, those skilled in the art once know substantially
Creative concept, then can make other change and modification to these embodiments.So, appended claims are intended to be construed to bag
Include preferred embodiment and fall into having altered and changing for the utility model scope.
Obviously, those skilled in the art can carry out various changes and modification without departing from this practicality to the utility model
New spirit and scope.So, if these modifications and variations of the present utility model belong to the utility model claim and
Within the scope of its equivalent technologies, then the utility model is also intended to comprising including these changes and modification.
Claims (10)
1. a kind of nitrogen content detection device, it is characterised in that including:
Burner, for the burning of testing sample, and produces mixed gas;
De-watering apparatus, the de-watering apparatus is connected with the burner, is produced for removing after burner burning
Moisture in raw mixed gas;Wherein, the de-watering apparatus includes:
One-level water removal body,
Two grades of water removal bodies;
Third class de-watering mechanism, the one-level water removal body, two grades of water removal bodies and the third class de-watering mechanism are sequentially connected with,
And the one-level water removal body is connected with the burner so that the mixed gas after the burner burning is sequentially passed through
The one-level water removal body, two grades of water removal bodies and the third class de-watering mechanism are removed water;
Reduction apparatus, the reduction apparatus is connected with the third class de-watering mechanism so that after the third class de-watering mechanism comes out
Mixed gas be reduced in the reduction apparatus;
Purifier, the purifier is connected with the reduction apparatus, to be purified to the mixed gas after reduction;Its
In, the purifier includes:
First class purification mechanism;
Secondary purification mechanism;The first class purification mechanism and the secondary purification mechanism are in parallel, and one end after parallel connection and institute
Reduction apparatus connection is stated, to receive the mixed gas produced after the reduction apparatus burning;
Three-level purification mechanism, the three-level purification mechanism with it is in parallel after the first class purification mechanism and the secondary purification mechanism
The other end connection so that the three-level purification mechanism is in series with the first class purification mechanism, secondary purification mechanism respectively, with
Gas after the first class purification mechanism and secondary purification mechanism purified treatment is received by the three-level purification mechanism
Body;
Detection means, the detection means is connected with the purifier, to be examined to the nitrogen content in purified gas
Survey;
Sample introduction processing unit, the sample introduction for entering early stage of advancing to the testing sample is handled;And the burner is vertically
Be fixed on the top of the sample introduction processing unit so that the testing sample after the processing of sample introduction by early stage by it is described enter
Sample processing unit, is admitted in the burner and burns.
2. nitrogen content detection device as claimed in claim 1, it is characterised in that:
The burner is combustion furnace of the temperature control at 1100 DEG C;
And the combustion furnace includes:
Body of heater so that the testing sample burns in the furnace interior;
Electron electric power device, is connected with the body of heater, the temperature environment for providing the body of heater 1100 DEG C, so that described treat
The fully oxidized burning in the body of heater of test sample product;
Heating element heater, the heating element heater is uniformly arranged on the inwall of the body of heater, makes the temperature of the inside of the body of heater
It is uniformly distributed in the body of heater.
3. nitrogen content detection device as claimed in claim 1, it is characterised in that the sample introduction processing unit also includes:
At least one sampler, in vertical direction each described sampler be respectively positioned on the lower section of the burner;
The crucible being adapted with the sampler quantity, each described crucible is accordingly fixed on a sampler,
And it is placed with the testing sample at least one described crucible;
Mechanical arm, is provided with correspondence on the lever arm being adapted with the sampler quantity, each lever arm and fixes an institute
Sampler is stated, to drive the corresponding sampler to move up and down by the up and down action of the lever arm, correspondence is then promoted
The ground crucible enters in the burner.
4. nitrogen content detection device as claimed in claim 1, it is characterised in that the reduction apparatus includes:
Current divider, the current divider is connected with the third class de-watering mechanism, with to mixing for being transferred out by the third class de-watering mechanism
Gas is closed to be shunted;
Reduction furnace, the reduction furnace is connected with the current divider and the detection means respectively, to be carried out to the gas after shunting
Reduction, and will be detected in the gas feeding detection means after reduction.
5. nitrogen content detection device as claimed in claim 1, it is characterised in that
The first class purification mechanism includes:First absorber and the second absorber;First absorber respectively with the reduction
Device and second absorber connection;
And,
The secondary purification mechanism includes:3rd absorber and the 4th absorber;3rd absorber respectively with the reduction
Device and the 4th absorber connection;
And,
The three-level purification mechanism includes:5th absorber and the 6th absorber;5th absorber is respectively with described second
Absorber connection, the 4th absorber and the 6th absorber connection, the 6th absorber connect with the detection means
Connect.
6. nitrogen content detection device as claimed in claim 5, it is characterised in that
First absorber is sulfur dioxide/carbon dioxide halogen absorber;Second absorber is water absorber;
And/or,
3rd absorber is sulfur dioxide/carbon dioxide halogen absorber;4th absorber is water absorber;
And/or,
5th absorber is sulfur dioxide/carbon dioxide halogen absorber;6th absorber is water absorber.
7. nitrogen content detection device as claimed in claim 1, it is characterised in that the detection means includes:
TCD thermal conductivity detector (TCD)s;
Mass flowmenter;
Wherein, the TCD thermal conductivity detector (TCD)s are connected with the purifier and the mass flowmenter respectively.
8. nitrogen content detection device as claimed in claim 1, it is characterised in that;
The one-level water removal body includes:First glass physical condenser, the first electronic cooling dehydrater and the first adsorbent;Institute
The first glass physical condenser is stated to be connected with the burner and the first electronic cooling dehydrater respectively;Described first inhales
Attached dose is connected with the first electronic cooling dehydrater;
And,
Two grades of water removal bodies include:Second glass physical condenser, the second electronic cooling dehydrater and the second adsorbent;Institute
The second glass physical condenser is stated to be connected with first adsorbent and the second electronic cooling dehydrater respectively;Described second
Adsorbent is connected with the second electronic cooling dehydrater;
And,
The third class de-watering mechanism includes:3rd glass physical condenser, the 3rd electronic cooling dehydrater and the 3rd adsorbent;Institute
The 3rd glass physical condenser is stated to be connected with second adsorbent and the 3rd electronic cooling dehydrater respectively;Described 3rd
Electronic cooling dehydrater and the 3rd adsorbent connection;3rd adsorbent is connected with the reduction apparatus.
9. nitrogen content detection device as claimed in claim 8, it is characterised in that
The first glass physical condenser is third generation double-tee glass condenser, and the first electronic cooling dehydrater is half
Conductor refrigerator, first adsorbent is silica gel, activated alumina or activated carbon;
And/or,
The second glass physical condenser is third generation double-tee glass condenser, and the second electronic cooling dehydrater is half
Conductor refrigerator, second adsorbent is silica gel, activated alumina or activated carbon.
10. nitrogen content detection device as claimed in claim 8, it is characterised in that
The 3rd glass physical condenser is third generation double-tee glass condenser, and the 3rd electronic cooling dehydrater is half
Conductor refrigerator, the 3rd adsorbent is silica gel, activated alumina or activated carbon.
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