CN206198967U - A kind of de-watering apparatus for total nitrogen analytical equipment - Google Patents

Abstract

The utility model discloses a kind of de-watering apparatus for total nitrogen analytical equipment, including：One-level water removal body；Two grades of water removal bodies, the one-level water removal body and two grades of water removal bodies are in parallel, and one end after parallel connection is connected with burner, to receive the mixed gas produced after the burner burns；Third class de-watering mechanism, the third class de-watering mechanism is connected with the one-level water removal body and the other end of two grades of water removal bodies after parallel connection so that third class de-watering mechanism is in series with one-level water removal body, two grades of water removal bodies respectively；Reduction apparatus are connected with the third class de-watering mechanism so that from the third class de-watering mechanism out after mixed gas be reduced in the reduction apparatus.The moisture that the utility model is realized in produced mixed gas in detection process fully, is effectively removed, it is ensured that the accuracy of detection.

Description

A kind of de-watering apparatus for total nitrogen analytical equipment

Technical field

The utility model belongs to detection technique field, more particularly to a kind of de-watering apparatus for total nitrogen analytical equipment.

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, is distillated with vapor and for excessive acid solution absorbs, then with standard acidometric titration, so as to calculate sample Nitrogen content in product, that is, predominantly detect process to clear up → distilling → titrate.However, being set for total nitrogen analysis of the prior art It is standby, how the moisture in the mixed gas in detection process as produced by burner is carried out fully, effectively remove, to protect The accuracy of detection is demonstrate,proved, is always urgent need to solve the problem.

Utility model content

The utility model provides a kind of de-watering apparatus for total nitrogen analytical equipment, solves or part solves existing skill Above-mentioned technical problem in art.

According to one side of the present utility model, there is provided a kind of de-watering apparatus for total nitrogen analytical equipment, wherein, always Nitrogen analysis equipment includes burner and reduction apparatus, and the de-watering apparatus respectively with the burner and described also original-pack Connection is put, for removing by the moisture in the mixed gas produced after burner burning；The de-watering apparatus include： One-level water removal body；Two grades of water removal bodies, the one-level water removal body and two grades of water removal bodies are in parallel, and after parallel connection One end is connected with the burner, to receive the mixed gas produced after the burner burns；Third class de-watering mechanism, institute State third class de-watering mechanism to be connected with the one-level water removal body and the other end of two grades of water removal bodies after parallel connection so that institute State third class de-watering mechanism to be in series with the one-level water removal body, two grades of water removal bodies respectively, with by the third class de-watering machine Structure is received by the one-level water removal body and two grades of water removal bodies except the mixed gas after water process；The reduction apparatus Be connected with the third class de-watering mechanism so that from the third class de-watering mechanism out after mixed gas in the reduction apparatus It is reduced.

Optionally：The reduction apparatus include：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 are shunted；Reduction furnace, the reduction furnace respectively with the current divider It is connected with the detection means, is reduced with to the gas after shunting, and the gas after reduction is sent into the detection means In detected.

Optionally：The reduction apparatus also include：Sensor, the sensor is arranged on the reduction furnace and the detection Between device.

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.

Optionally：Two grades of water removal bodies include：Second glass physical condenser, the second electronic cooling dehydrater and Two adsorbents；The second glass physical condenser connects with the burner and the second electronic cooling dehydrater respectively Connect；Second adsorbent is connected with the second electronic cooling dehydrater.

Optionally：The third class de-watering mechanism includes：3rd glass physical condenser, the 3rd electronic cooling dehydrater and Three adsorbents；The 3rd glass physical condenser respectively with first adsorbent, second adsorbent and the described 3rd Electronic cooling dehydrater is connected；The 3rd electronic cooling dehydrater and the 3rd adsorbent are connected；3rd adsorbent It 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.

Optionally：The second glass physical condenser is third generation double-tee glass condenser, the second electronics system Cold dehydrater is semiconductor cooler, and second adsorbent is silica gel, activated alumina or activated carbon.

Optionally：The 3rd glass physical condenser is third generation double-tee glass condenser, the 3rd electronics system Cold dehydrater is semiconductor cooler, and the 3rd adsorbent is silica gel, activated alumina or activated carbon.

A kind of de-watering apparatus for total nitrogen analytical equipment that the utility model embodiment is provided, by one-level water removing machine Structure, two grades of water removal bodies and third class de-watering mechanism, the mixed gas exported to burner remove water, realize and detected Moisture in journey in produced mixed gas fully, is effectively removed, it is ensured that the accuracy of detection.

Brief description of the drawings

In order to illustrate more clearly of the utility model embodiment or technical scheme of the prior art, below will be to embodiment Needed for the accompanying drawing to be used 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 total nitrogen analytical equipment that Fig. 1 is provided for the utility model embodiment；

The structural schematic block diagram two for total nitrogen analytical equipment that Fig. 2 is provided for the utility model embodiment；

The structural schematic block diagram three for total nitrogen analytical equipment that Fig. 3 is provided for the utility model embodiment；

Fig. 4 is the structural schematic block diagram of the burner in Fig. 2；

Fig. 5 is the structural schematic block diagram of the sampling processing unit in Fig. 2；

Fig. 6 is the structural schematic block diagram of the de-watering apparatus in Fig. 2；

Fig. 7 is the structural schematic block diagram of the reduction apparatus in Fig. 2；

Fig. 8 is the structural schematic block diagram of the purifier in Fig. 2；

Fig. 9 is the structural schematic block diagram of the detection means in Fig. 2；

The schematic flow sheet one of the method for the measure nitrogen content that Figure 10 is provided for the another embodiment of utility model；

The schematic flow sheet two of the method for the measure nitrogen content that Figure 11 is provided 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 of the de-watering apparatus for total nitrogen analytical equipment that Figure 15 is provided for the utility model embodiment is illustrated Figure.

Specific 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 In the scope of the utility model protection；"and/or" keyword wherein involved 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 are 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 can also there is 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 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.

A kind of de-watering apparatus for total nitrogen analytical equipment that the utility model embodiment is provided, by one-level water removing machine Structure, two grades of water removal bodies and third class de-watering mechanism, the mixed gas exported to burner remove water, realize and detected Moisture in journey in produced mixed gas fully, is effectively removed, it is ensured that the accuracy of detection.In order to new to this practicality The de-watering apparatus for total nitrogen analytical equipment that type is provided elaborate, to support that technology to be solved in the utility model is asked Topic, below, in the embodiment that the utility model is provided, total nitrogen analytical equipment is elaborated first, then in narration total nitrogen During analytical equipment, the de-watering apparatus that the utility model is provided further targetedly are drawn, it is complete, clear to reach Chu, clear purpose.

Fig. 1 is specifically referred to, the utility model embodiment provides a kind of total nitrogen analytical equipment, at least including burner 200th, 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 are in purifier 500 by a series of control techniques institutes Purification.Realize comprising only purity nitrogen molecule, and the purifier 500 and the detection means 600 in the gas after final purification 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 described for total nitrogen analysis The de-watering apparatus of equipment, instead of in conventional art using using corrosivity soda acid, operating procedure caused by Kjeldahl's method The complicated, technological deficiency that time-consuming and environmental pollution is serious.

In order to be elaborated to the total nitrogen analytical equipment that the utility model embodiment is provided, distinguish with reference to Fig. 2-9 Burner 200, reduction apparatus 400, purifier 500 and detection means 600 are elaborated, further to support this reality With new technical problem to be solved.

For firstly, for burner 200,

Because the temperature range burnt and the Temperature Distribution in stove have 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.

In the utility model embodiment, before testing sample enters burner 200, can also be processed by sample introduction and filled Putting 100 carries out the physical treatment of early stage.Wherein, the early stage physical treatment of the testing sample can be divided into the following two kinds situation：(1) If testing sample is the solid sample of anisotropic, testing sample is pulverized and sieved into treatment before sample is claimed；(2) if to be measured Sample is liquid and sauce class sample, then directly can claim in crucible.Wherein, crucible can described in the utility model embodiment Reuse, to reach the technique effect without consumptive material.Meanwhile, the crucible required for the utility model embodiment can be following earthenware One kind in crucible：Quartz, ceramics, steel, nickel, platinum etc., the purpose of various testing samples is applicable to reach.Adopted so as to overcome When being analyzed with other instruments, sample must pressing mold shaping and with tinfoil wrap up just can sample introduction analyze, sample preparation is complicated, and tin can is Medical disposable material, operating cost is high, combustion-supporting gas and the more technological deficiency of carrier gas consumption.Further, due to the utility model Chemical reagent of the embodiment without any extra sample chemical treatment as digested with toxicity, so as to eliminate traditional kjeldahl determination The technological deficiency that method complex operation, digestion time are long, 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 by the electronic weigher and be located at In the quality of sample in crucible, and the weight data information transfer that will be gathered to 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 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.The display end 702 is connected with the power supply source 701, with by 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, drives sampler 101 to be moved with by the motion of mechanical arm 102, and then realizes driving crucible 104 to enter 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 plus/ Motion of the reducing gear to mechanical arm 102 is accelerated or is 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, plus/minus speed mechanism 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 the upper furnace structure of uniqueness 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 is connected using the vertical input mode of linear pattern from bottom to top by control It is connected to during the crucible 104 being located on sampler 101 heads into body of heater 201 by the mechanical arm 102 of the sampler 101 so that sample After being burnt completely in combustion furnace, be transferred on sampler 101 from top to bottom for it by mechanical arm 102.Sample after ashing is then protected Stay in crucible 104, and the automatic interference-free of sample after ashing can be transferred to instrument by controlling sampler 101 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 determine using the Dumars of the next furnace design in blood urea/nitrogen analyzer so as to effectively overcome tradition Nitrogen instrument sample must pressing mold shaping and with tinfoil wrap up after just can sample introduction analyze, and in cinder catcher sample ash reach it is a certain amount of The technological deficiency that necessary craft blow-on removes the dust in cinder catcher afterwards.

The utility model embodiment is solid by using unique upper furnace structure and vertical input mode, can not only realize The quick detection of body, fluid sample, moreover it is possible to reach the full automation from sample process to assay.Additionally, burning is produced Carrier gas stream can automatically take away sample dust, clean dust without blow-on, 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, thus from burner 200 gaseous state NOx out need by de-watering apparatus 300 Carry out except water process.The de-watering apparatus 300 are 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 explanation, in 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, and one is fixed with each lever arm Corresponding sampler, is fixed with a crucible on each sampler 101.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 are removed water including one-level 310, two grades of water removal bodies 320 of mechanism 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 using 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 burns；The other end with The third class de-watering mechanism 330 connects so that the third class de-watering mechanism 330 respectively with 310, two grades of the one-level water removal body Water removal body 320 constitutes the structural relation of series connection, to realize being received by the third class de-watering mechanism 330 being removed by the one-level Water dispenser structure 310 and two grades of water removal bodies 320 are except the mixed gas after water process.

It should be noted that in the utility model embodiment, why de-watering apparatus 300 are arranged into multistage water removing machine Structure, it is to carry out multistage water removal to mixed gas that one side purpose is, 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 are 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 cannot 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 for being exported mix in one-level water removal body 310 and two grades of output ends of water removal bodies 320, Ran Hou Removed water again in inflow third class de-watering mechanism 330, same principle, this is also caused 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 cannot 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 burns；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 310, two grades of water removal bodies of the one-level water removal body 320 structural relations for constituting series connection, this kind of connected mode can be defined as the connected mode 1 of water removal body.Certainly, the connection Mode 1 is only merely a kind of 310, two grades of connection sides between water removal body 320 and third class de-watering mechanism 330 of one-level water removal body Formula, the utility model embodiment is not limited to.

Words sentence is talked about, for other companies of 310, two grades of water removal bodies 320 of one-level water removal body and third class de-watering mechanism 330 Mode is connect, as long as the technique effect of effective water removal can be reached, the utility model embodiment is may also apply to.Such as, for letter Change structure design, the utility model embodiment directly can mutually be gone here and there three water removal bodies using the connected mode 2 of water removal body Connection, i.e., 310, two grades of water removal bodies 320 of one-level water removal body 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, removal 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 310, two grades of water removal bodies 320 of water dispenser structure and third class de-watering mechanism 330, and respectively with burner Connected with reduction apparatus, to reach the technical scheme of the technique effect of water removal, also within protection domain of the present utility model.Need It should be noted that 310, two grades of water removal bodies 320 of one-level water removal body and third class de-watering mechanism in the utility model embodiment " one-level ", " two grades " in 330, " three-level " they are 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 310, two grades of water removal bodies 320 of one-level water removal body 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 by the first glass physical condenser 301 first, then by the first electronic cooling dehydrater 2 DEG C water removal, finally by the first adsorbent 303 adsorb remove water.That is, first allow after the first glass physical condenser 301 will burn Product carry out physics cooling and removed water by the way that vapor is liquefied, then by the further cooling of the first electronic cooling dehydrater 302 Under test gas simultaneously remove vapor again by by vapor liquefaction, fully absorb moisture finally by the first adsorbent 303 To reach the purpose of thorough water removal, 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 of the utility model embodiment offer, 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 for carry out the first step condensing water removal by the first glass physical condenser 301 in type embodiment, by high-temperature combustion product Efficiently significantly lower the temperature, it is reduced to 2-3 DEG C, then removed for the follow-up electronic cooling of electronic cooling dehydrater 302 water removal is provided 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 coupled together and pass to electric current, There is a joint to absorb heat, another joint heat release), i.e., a kind of New Refrigerating method freezed by direct current.Electronic cooling effect It, by the principle of thermoelectricity, is a cooling piece for monolithic that generation is exactly, and it is made up of two panels potsherd, there is 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 coupled together.After connecting DC current in this circuit, the transfer of energy can be just 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 can just keep lower temperature.The size of heat absorption and heat release is logical The size of overcurrent and the element logarithm of semi-conducting material N, P are determined.Galvanic couple is unified into by up to a hundred inside cooling piece Thermoelectric pile (such as right figure), to reach the effect of enhancing refrigeration, when heat load is zero, most strong refrigeration can reach 80 DEG C of temperature Difference.The temperature difference amplitude limitation of electronic cooling, also further illustrates the necessity of the first step glass physical condensation water removal.

And then, due to the water removal phase for having had first two steps, most moisture have been removed, so only needing to The first a small amount of adsorbent 303 can reach the effect for eliminating moisture well, so as to greatly save the usage amount of adsorbent, Overcome defect of traditional azotometer using a large amount of adsorbent high 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 as a example by only including one-level water removal body 310 in de-watering apparatus 300 come the operation principle to water removal body Row description, during actual job, also can be by 310, two grades of water removal bodies 320 of one-level water removal body and third class de-watering mechanism 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, this Place also repeats no more.

Secondly, for reduction apparatus 400,

The reduction apparatus 400 include：Reduction furnace 402, part flow arrangement 401, non-dispersive IR line (NDIR) sensor 403.Wherein, the direct phase of the electronic cooling (2 DEG C) dehydrater 302 in the part flow arrangement 401 and higher level's de-watering apparatus 300 Even, then it is connected with the reduction furnace 402, is sensed by the NDIR between the reduction furnace 402 and the purifier 500 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, and preceding Partial flow dilution gas is reduced into reduction furnace 402 in gas, and copper reduction stove is saved so as to reach The consumption of 402 reducing agent and the purpose of the cost of measurement every time is saved, meanwhile, built-in membrane disappears deimpurity interference.Specifically Ground, it is due to N (nitrogen) burning conversions into substantial amounts of gaseous NOx, too high for detector concentration, and reduced During can consume substantial amounts of reducing agent, therefore, will be from the burner 200 out and by three by part flow arrangement 401 Detection is reduced after gaseous sample shunting after individual condensing unit condensation water removal, remaining gas pass through adsorbent adsorption treatment heel row Remove.

The nitrogen oxides for generating burn by after the accurate gas diverter shunting, being spread as carrier gas using helium Send, it is dinitrogen that the nitrogen oxides is completely reduced in 600 DEG C of copper reduction stoves, while the oxygen of excess is combined into oxidation by copper Copper.Amount of oxygen needed for being used for controlling best combustion using non-dispersive IR line (NDIR) sensor, 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 absorption spectrum is made up of the spectral line in the range of certain frequency, has Certain broadband, the absorption intensity of each Frequency point is different in 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 divided beams by light source, after reference channel and tested passage air chamber absorb, optical signal is detected Device carries out enhanced processing after being converted into electric signal.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 are reduced；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 structural relations for constituting series connection, to realize being received by the first class purification mechanism 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, it is to carry out multistage purification to gas that one side purpose is, to ensure that mixed gas are 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 are mixed in the receiving terminal of the first class purification mechanism 510 and the secondary purification mechanism 520, are 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 cannot be fully purified.Simultaneously by the first class purification mechanism 510 and the secondary purification mechanism after parallel connection 520, the mixed gas for being exported mix in the output end of first class purification mechanism 510 and secondary purification mechanism 520, are then flowing into Purified again in three-level purification mechanism 530, same principle, this is also caused 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 for exporting Air velocity is too fast and cannot 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 of effective purification can be reached, the utility model embodiment is may also apply to.Such as, for letter Change structure design, the utility model embodiment directly can mutually be gone here and there three purification mechanisms using the connected mode 2 of purification mechanism 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, to reach the technical scheme of the technique effect of 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 " in 530, " three-level " they are 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 Purification 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 treatment, except nitrogen molecular in air-flow, also contain other impurities, it is therefore desirable to by purifier removal reducing gas 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, then by second absorber 502, can be with Remove moisture removal.By two step adsorption processes, the removal of impurity can be reached, purify the purpose of gas nitrogen to be detected.Wherein, it is described First absorber 501 possesses dehalogenation function, can eliminate halogen, effectively prevents the detection means described in halogen into subordinate and makes Into infringement, the purpose of the detection means is protected so as to reach.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 come the operation principle to purification mechanism as a example by only including first class purification mechanism 510 in purifier 500 with new State, during actual job, first class purification mechanism 510, secondary purification mechanism 520 and three-level purification mechanism 530 can also be pressed Purifier 500 is constituted according to above-mentioned connected mode 1-3 to carry out high-efficient purification, the utility model does not limit to, herein also not Repeat again.

For finally, 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 to be directly connected with the second absorber 502 described in upper level purifier 500, 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 warm 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, and 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 to pass through 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 an identical thermal conductivity, thus two-arm electricity 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, in making reference cell and measuring cell hole Difference is generated between heater resistance value, electric bridge disequilibrium, detector has voltage signal to export, 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 for now exporting is directly proportional to the concentration of sample, this exactly thermal conductivity inspection 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, by it, then by the independence correction of material, the nitrogen content in sample is just automatically counted Calculate, print and store.Specifically, the standard correction material uses EDTA or urea, and only needs to regular calibration, nothing 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 the 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 as to measure flow.Because be with thermal measure, will not because of gas temperature, pressure change so as to have influence on survey The result of amount.Mass flowmenter 602 is a more accurate, quick, reliable, efficient, stable, flexible flow measurement instrument. Mass flowmenter 602 can not control flow, and it can only detect the mass flow of liquid or gas, by analog voltage, electricity Stream or serial communication output flow value.

It should be added that, in the utility model embodiment, the concentration of the combustion gas oxygen being passed through is 99.995%, the concentration of the carrier gas stream helium being passed through is 99.99%, and the oxygen that is passed through and the flow of helium 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 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, in the utility model embodiment, need to also be set for total nitrogen analysis described Built-in 40 DEG C ± 0.1 DEG C of Thermotank devices in standby de-watering apparatus, with ensure system detector, current divider, gas collection system, The temperature constant state of the devices such as gas circuit control, it is to avoid because the change of environment temperature causes the change of gas flow path stability, improves Analysis precision and the degree of accuracy.

To sum up, the testing sample by early stage physical treatment and it is automatic weigh after, in the vertical mechanical sample introduction Enter in the homogeneous combustion furnace of 1100 DEG C of high temperature from the sampler in the presence of arm, 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 the way that the gas diverter is accurate Under test gas sample after burning, then current-carrying gas of the helium as the gaseous sample being diverted are passed through, send into together described 600 DEG C of copper reduction stoves, by nitrogen molecular Restore All out, meanwhile, using the oxygen needed for NDIR sensors control best combustion Amount, this can ensure that the consumption of oxygen and copper is minimum, then remove CO2/ by first absorber and the second absorber , then be passed through pure nitrogen 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.

Based on the device embodiment that above-described embodiment is provided, Figure 10-14 are referred to, 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 to testing sample by burner, 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 by reduction apparatus The mixed gas are reduced, in the reduction step, the reduction temperature of the reduction apparatus is 600 DEG C, and is constant temperature； Step 3000, purifying step, for being purified to the mixed gas after reduction by purifier, 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 to the nitrogen content in the remaining gas by detection means.

Further, another embodiment of the present utility model also includes；Step 5000, sampling procedure, for by 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 Burnt in burning device.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 be by 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, By by carrying out double purification in the mixed gas feeding adsorbent after primary purification.

Wherein, the reduction step also includes following sub-step：Step 2001, shunts sub-step, for by shunting dress Put and shunted mixed gas, be diluted with to the mixed gas；Step 2002, goes back atomic step, after shunting Gas is reduced in reduction furnace；Step 2003 flow control sub-step, is carried out for the flow 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 deviating from this practicality to the utility model New spirit and scope.So, if it is of the present utility model these modification and modification belong to the utility model claim and Within the scope of its equivalent technologies, then the utility model is also intended to comprising these changes and modification.

Claims (9)

1. a kind of de-watering apparatus for total nitrogen analytical equipment, wherein, total nitrogen analytical equipment includes burner and reduction apparatus, And the de-watering apparatus are connected with the burner and the reduction apparatus respectively, fired by the burner for removing Moisture in the mixed gas produced after burning；Characterized in that, the de-watering apparatus include：

One-level water removal body；

Two grades of water removal bodies, the one-level water removal body and two grades of water removal bodies are in parallel, and the one end after parallel connection and institute Burner connection is stated, to receive the mixed gas produced after the burner burns；Third class de-watering mechanism, the three-level is removed Water dispenser structure is connected with the one-level water removal body and the other end of two grades of water removal bodies after parallel connection so that the three-level is removed Water dispenser structure is in series with the one-level water removal body, two grades of water removal bodies respectively, is passed through with by the third class de-watering authorities The one-level water removal body and two grades of water removal bodies are crossed except the mixed gas after water process；

The reduction apparatus are connected with the third class de-watering mechanism so that from the third class de-watering mechanism out after mixed gas It is reduced in the reduction apparatus.

2. the de-watering apparatus of total nitrogen analytical equipment are used for as claimed in claim 1, it is characterised in that the reduction apparatus bag Include：

Current divider, the current divider is connected with the third class de-watering mechanism, with mixed to what is transferred out by the third class de-watering mechanism Gas is closed to be shunted；

Reduction furnace, the reduction furnace is connected with the detection means in the current divider and the total nitrogen analytical equipment respectively, with right Gas after shunting is reduced, and will be detected in the gas feeding detection means after reduction.

3. the de-watering apparatus of total nitrogen analytical equipment are used for as claimed in claim 2, it is characterised in that the reduction apparatus are also wrapped Include：

Sensor, the sensor is arranged between the reduction furnace and the detection means.

4. the de-watering apparatus of total nitrogen analytical equipment are used for 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 Adsorbent is connected with the first electronic cooling dehydrater.

5. the de-watering apparatus of total nitrogen analytical equipment are used for as claimed in claim 4, it is characterised in that；

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 the burner and the second electronic cooling dehydrater respectively；Described second inhales Attached dose is connected with the second electronic cooling dehydrater.

6. the de-watering apparatus of total nitrogen analytical equipment are used for as claimed in claim 5, it is characterised in that：

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 removed water with first adsorbent, second adsorbent and the 3rd electronic cooling respectively Device is connected；The 3rd electronic cooling dehydrater and the 3rd adsorbent are connected；3rd adsorbent is also original-pack with described Put connection.

7. the de-watering apparatus of total nitrogen analytical equipment are used for as claimed in claim 6, 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.

8. the de-watering apparatus of total nitrogen analytical equipment are used for as claimed in claim 7, it is characterised in that

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.

9. the de-watering apparatus of total nitrogen analytical equipment are used for 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 semiconductor cooler, the described 3rd Adsorbent is silica gel, activated alumina or activated carbon.