CN107515272A - A kind of ammonia nitrogen on-line computing model based on distillation titration - Google Patents
A kind of ammonia nitrogen on-line computing model based on distillation titration Download PDFInfo
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- CN107515272A CN107515272A CN201710759464.4A CN201710759464A CN107515272A CN 107515272 A CN107515272 A CN 107515272A CN 201710759464 A CN201710759464 A CN 201710759464A CN 107515272 A CN107515272 A CN 107515272A
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- 238000004448 titration Methods 0.000 title claims abstract description 108
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000004821 distillation Methods 0.000 title claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 240
- 239000007788 liquid Substances 0.000 claims abstract description 109
- 238000005070 sampling Methods 0.000 claims abstract description 61
- 238000001514 detection method Methods 0.000 claims abstract description 36
- 239000007853 buffer solution Substances 0.000 claims abstract description 26
- 238000010521 absorption reaction Methods 0.000 claims abstract description 20
- 238000012805 post-processing Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 90
- 239000004327 boric acid Substances 0.000 claims description 90
- 238000007599 discharging Methods 0.000 claims description 64
- 230000008676 import Effects 0.000 claims description 61
- 238000004140 cleaning Methods 0.000 claims description 60
- 239000000110 cooling liquid Substances 0.000 claims description 35
- 239000003513 alkali Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 24
- 241000628997 Flos Species 0.000 claims description 21
- 239000012530 fluid Substances 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 16
- 239000002699 waste material Substances 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 14
- 239000000498 cooling water Substances 0.000 claims description 12
- 238000005485 electric heating Methods 0.000 claims description 11
- 230000037452 priming Effects 0.000 claims description 10
- 239000002585 base Substances 0.000 claims description 6
- 230000003139 buffering effect Effects 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 1
- 229910052796 boron Inorganic materials 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 9
- 239000007787 solid Substances 0.000 abstract description 9
- 239000010865 sewage Substances 0.000 abstract description 4
- 238000011002 quantification Methods 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 239000002352 surface water Substances 0.000 abstract description 3
- 239000003002 pH adjusting agent Substances 0.000 abstract description 2
- 238000006467 substitution reaction Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 157
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 238000012545 processing Methods 0.000 description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 5
- 230000033228 biological regulation Effects 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 4
- 229960004889 salicylic acid Drugs 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000002479 acid--base titration Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 238000005375 photometry Methods 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 235000019628 coolness Nutrition 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000012928 buffer substance Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000002477 conductometry Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 229910000397 disodium phosphate Inorganic materials 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005206 flow analysis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
- G01N31/164—Determining the equivalent point by means of a discontinuity by electrical or electrochemical means
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
Abstract
A kind of ammonia nitrogen on-line computing model based on distillation titration, it is made up of sampling and pretreatment unit, dosing unit, distillation unit, absorption titration unit, post-processing unit, PLC.The present invention realizes the automatic addition of pH adjusting agent using liquid buffer solution substitution solid MgO；The present invention is improved distillation efficiency, is added the safety and reliability of instrument using the automatic distilling apparatus that electrical heating power is adjustable, distilling rate is controllable；The present invention realizes water sample and the accurate quantification of absorbing liquid using a kind of freely adjustable automatic liquid metering device of liquid measure；The present invention carries out the automatic judgement of titration end-point using pH potentiometric detections electrode, add sensitivity and the accuracy of instrument, and the measurement range of instrument is extended, enable the invention to adapt to the online automatic detection of the surface water such as trade effluent, sanitary sewage, river, lake simultaneously.
Description
Technical field
It is particularly a kind of to be based on distillation-neutralization titration and controlled by PLC the present invention relates to a kind of ammonia nitrogen on-line computing model
Ammonia nitrogen water quality online automatic monitor.
Background technology
The assay method of ammonia nitrogen is more in water, according to the difference of Cleaning Principle, mainly there is photometry, electrode method, distillation-drop
Determine method, gas-phase molecular absorption spectrometry method, the chromatography of ions, Blow-off-conductometry etc..
At present, the commonplace ammonia nitrogen on-line computing model of in the market is based primarily upon photometry, electrode method and distillation titration method
This three classes method.Nessler reagent and salicylic acid AAS are the classical ways for determining ammonia nitrogen in water, are had sensitive, stable etc.
Advantage, but easily disturbed by water body impurity, color, turbidity and suspended material, the more difficult preparation of reagent and stability requirement is strict, behaviour
Make comparisons complexity, the test data degree of accuracy is poor.Continuous flowing-salicylic acid AAS and flow injection-salicylic acid light splitting
Photometry is substantially salicylic acid AAS, and disturbed condition is identical, while Continuous Flow Analysis instrument and flowing note also be present
Penetrate the problems such as analyzer is complicated, measurement range is limited, measurement accuracy is not high enough.The electrode commonly used in electrode method is quick for ammonia
Electrode, this method are not usually required to pre-process water sample, and measurement range is wide, are not easily susceptible to disturb, and simple to operate, measurement
Speed is fast, the prefered method of Water quality ammonia nitrogen of can yet be regarded as detection, but the ammonia gas-sensing electrode used in the method is extremely tender and lovely, easily damage
The problems such as bad, service life is shorter, and stability and reliability are poor, measurement accuracy is not high need to further solve.
Distillation-neutralization titration is primarily adapted for use in the measure of sanitary sewage and ammonia nitrogen in industrial waste water, has measurement range
The features such as wide, reagent and waste liquid nontoxicity, and colourity, turbidity, suspended material are not influenceed and interference in by water body.But the method is deposited
Mixed indicator stabilization time is short, solid oxidation magnesium is difficult to automatic addition, titration end-point (indicator discoloration point) is difficult to
Automatic the problems such as judging and technological difficulties are realized exactly.
The content of the invention
In order to solve, mixed indicator stabilization time present in distillation-neutralization titration is short, solid oxidation magnesium is difficult to reality
Now automatic addition, titration end-point are difficult to accurate realization automatic the problems such as judging and technological difficulties, the present invention provide and be based on distillation-drop
Determine the ammonia nitrogen on-line computing model of method.Solve in the ammonia nitrogen online automatic detection of distillation-neutralization titration accurately sampling, solid
The problems such as MgO is substituted, efficiently distilled, titration end-point judges, online automatic detection, to improve every skill of ammonia nitrogen on-line computing model
Art performance indications, and improve accuracy, stability, reliability and the adaptability of systematic survey；And the titration detection electricity of the present invention
Pole uses pH potentiometric detection electrodes, adds sensitivity and the accuracy of instrument, extends the measurement range of instrument, make it not only
Adapt to the detection of trade effluent, sanitary sewage, at the same can also the surface water such as adjusted stream, lake detection.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of ammonia nitrogen on-line computing model based on distillation titration method, including sampling and pretreatment unit, dosing unit, steaming
Evaporate unit, absorb titration unit, post-processing unit and PLC；
Described sampling and pretreatment unit include water sample pretreatment tank V1, the tank body 2-1 of the water sample pretreatment tank V1
Outlet is sequentially provided with hollow cylindrical shape, and on water sample pretreatment tank V1 tank deck 2-6 with water sample pretreatment tank V1's
Sample tap 2-5, the acid-adding port 2-3 of intracavity inter-connection and plus alkali mouth 2-4；And the import of the acid-adding port 2-3 passes through acid adding pump P3
And connected with circuits with sour tank V3, described plus alkali mouth 2-4 import is by adding alkali pump P4 and being connected with circuits with alkali tank V4；
The first pH potentiometric detection electrodes J1, the first temperature sensor TE1 and the are provided with described water sample pretreatment tank V1
One agitator MS1；The top of the first pH potentiometric detection electrodes J1, the first temperature sensor TE1 top and the first stirring
Device MS1 top is each attached on water sample pretreatment tank V1 tank deck, and the bottom of the first pH potentiometric detection electrodes J1, the
One temperature sensor TE1 bottom and the first agitator MS1 bottom are all extended in water sample pretreatment tank V1；
Water sample pretreatment tank V1 tank bottom 2-8 is provided with the first discharging tube 2-9, the first discharging tube 2-9 import and
Water sample pretreatment tank V1 intracavity inter-connection, the first discharging tube 2-9 outlet connects with floss hole PF, and the first discharging tube 2-9
It is provided with water sample pretreatment tank waist valve S4；
The both sides of the water sample pretreatment tank V1 are respectively equipped with water inlet pipe 2-2 and the first overflow pipe 2-7；Water inlet pipe 2-2's
Outlet and water sample pretreatment tank V1 intracavity inter-connection, water inlet pipe 2-2 import connect with water inlet pipeline a first outlet,
The import of the water inlet pipeline a is connected with sampling pump P1 outlet, and the import of the sampling pump P1 is connected with water source, and
The second outlet of the water inlet pipeline a is connected by delivery pipe with floss hole PF, and the delivery pipe is provided with self priming pump water outlet
Valve S2；The water inlet pipe 2-2 is provided with water sample pretreatment tank sampling valve S3；The import of the first overflow pipe 2-7 and water sample are pre-
Process tank V1 inner chamber connection, the first overflow pipe 2-7 outlet connects with floss hole PF, and the first overflow pipe 2-7 is provided with water
Sample pretreatment tank overflow valve S5；
Described dosing unit includes water sample constant volume tank V2 and boric acid constant volume tank V12, and water sample constant volume tank V2 tank body and
Boric acid constant volume tank V12 tank body is cylindrical tube 3-3, and the top opening of the cylinder 3-3 and base opening are respectively provided with detachably
Top cover 3-1 and bottom 3-6；The bottom 3-6 is provided with the second discharging tube 3-8 that import connects with cylinder 3-3 inner chambers；Cylinder
3-3 both sides are respectively equipped with the first feed tube 3-2 and drain pipe 3-5, the first feed tube 3-2 are located at drain pipe 3-5 top, and
The inner chamber of first feed tube 3-2 outlet and drain pipe 3-5 import with cylinder 3-3 connects；Being provided with cylinder 3-3 can be along cylinder
The second the overflow pipe 3-7, the second overflow pipe 3-7 moved up and down to body 3-3 axial seal top is located in cylinder 3-3 and the
Two overflow pipe 3-7 top opening is located on drain pipe 3-5, and bottom 3-6 is run through in the second overflow pipe 3-7 bottom；The cylinder 3-3
Outer surface on be provided with scale vertically；
The second discharging tube 3-8 of water sample constant volume tank V2 outlet is connected with floss hole PF, and water sample constant volume tank V2
The second discharging tube 3-8 be provided with water sample constant volume tank waist valve S6；The first feed tube 3-2 of water sample constant volume tank V2 import
Tank V1 sample tap 2-5 outlet is pre-processed by sampling pump P2 and with circuits and the water sample；The water sample constant volume
Tank V2 the second overflow pipe 3-7 bottom connects with floss hole PF；The drain pipe 3-5 of the water sample constant volume tank V2 is provided with water sample
Constant volume tank bleeder valve S8；
The second discharging tube 3-8 of boric acid constant volume tank V12 outlet is connected with boric acid tank V13, and boric acid constant volume tank
V12 the second discharging tube 3-8 is provided with boric acid constant volume tank waist valve S14；The first feed tube 3-2 of the boric acid constant volume tank V12
Import be connected by boric acid pump P8 and with circuits with boric acid tank V13；On the drain pipe 3-5 of the boric acid constant volume tank V12
Provided with boric acid bleeder valve S13；The second overflow pipe 3-7 of boric acid constant volume tank V12 bottom is connected with boric acid tank V13；
Described distillation unit includes evaporator V6, drainer V8 and jacket type straight tube cooler E1, the drainer V8
Positioned at the top of the evaporator V6, and the inner chamber of the evaporator V6 and the inner chamber of the drainer V8 pass through steam outlet pipe 4-4
It is connected, and tank bottom 4-10 of the steam outlet pipe 4-4 both ends respectively with evaporator V6 tank deck 4-18 and drainer V8 is connected；
The tank body 4-17 of the evaporator V6 is in hollow cylindrical shape, and evaporator V6 tank deck 4-18 is respectively equipped with clearly
Wash pipe 4-1, the second feed tube 4-2 and blow-down pipe 4-3；
The outlet of the cleaning pipe 4-1 connects with evaporator V6 inner chamber, and the import of the cleaning pipe 4-1 is respectively by slow
Fliud flushing pump P5 and be connected with circuits, cleaning liquid pump P6 and with circuits with buffering flow container V5, cleaning fluid tank V7, and it is described clearly
Wash pipe 4-1 and be provided with buffer solution valve S7；
The outlet of the second feed tube 4-2 connects with evaporator V6 inner chamber, the second feed tube 4-2 import and water sample
Constant volume tank V2 drain pipe 3-5 outlet is connected；
The import of the blow-down pipe 4-3 connects with evaporator V6 inner chamber, the outlet of the blow-down pipe 4-3 and ambient atmosphere
It is connected, and blow-down pipe 4-3 is provided with evaporator atmospheric valve S9；
Evaporator V6 tank bottom 4-16 is externally provided with electric heating plate H1, the electric heating plate H1 and is connected with adjustable heating power
Regulator；Evaporator V6 tank bottom 4-16 is additionally provided with the 3rd discharging tube 4-15, the 3rd discharging tube 4-15 top and evaporation
Tank V6 intracavity inter-connection, the 3rd discharging tube 4-15 bottom insulation are connected through electric heating plate H1 and with waste liquid tank V9, and
Evaporator waist valve S10 is additionally provided with 3rd discharging tube 4-15；
The tank body 4-5 of the drainer V8 is in hollow cylindrical shape, and is arranged with outside the tank body 4-5 of the drainer V8
Drainer chuck 4-8, the drainer chuck 4-8 side are respectively equipped with the coolings of the first cooling liquid outlet 4-7 and first up and down
Liquid import 4-9, and the first cooling liquid outlet 4-7 and the first cooling liquid inlet 4-9 are connected with cooling system respectively；
The jacket type straight tube cooler E1 includes condensate liquid drain pipe 4-14 and is set in outside condensate liquid drain pipe 4-14
Cooling tube chuck 4-12；Condensate liquid drain pipe 4-14 import is at the tank bottom 4-10 of the solidifying tank V8 and in drainer V8
Chamber is connected；The second cooling liquid outlet 4-11 and the second cooling liquid inlet 4- are respectively arranged with the cooling tube chuck 4-12
13, and the second cooling liquid outlet 4-11 and the second cooling liquid inlet 4-13 connect with cooling system respectively；
Described absorption titration unit includes absorbing titration tank V10, and described absorption titration tank V10 tank body 5-8 is in sky
The cylindrical shape of the heart, and the tank deck 5-2 for absorbing titration tank V10 is provided with condensate line 5-3, absorbs liquid pipe 5-4 and titration
Liquid pipe 5-5；
The inner chamber that the outlet of the condensate line 5-3 titrates tank V10 with absorbing connects, condensate line 5-3 import with it is cold
Lime set drain pipe 4-14 outlet is connected, and the condensate line 5-3 is provided with condensate liquid valve S12；
The outlet for absorbing liquid pipe 5-4 connects with absorbing titration tank V10 inner chamber, the import for absorbing liquid pipe 5-4
Outlet with boric acid constant volume tank V12 drain pipe 3-5 is connected；
Buret e is provided with the titration liquid pipe 5-5, the import of the buret e is by syringe pump P7 and with circuits
It is connected with titration flow container V11, the outlet of the buret e titrates tank V10 intracavity inter-connection with absorbing；
The tank deck 5-2 of the titration tank V10 is further fixed on the 2nd pH potentiometric detection electrodes extended in titration tank V10
J2, second temperature sensor TE2, level electrode LS, titration tank V10 tank bottom 5-6 are provided with the second agitator MS2；
The side of the titration tank V10 is respectively arranged with cleaning liquid pipe 5-1 and the 4th discharging tube 5-7；The cleaning liquid pipe
5-1 outlet and titration tank V10 intracavity inter-connection, the import of the cleaning liquid pipe 5-1 is by cleaning liquid pump P6 and with sleeve pipe
Road is connected with cleaning fluid tank V7, and the cleaning liquid pipe 5-1 is provided with cleaning fluid valve S11；
The import of the 4th discharging tube 5-7 connects with titrating tank V10 inner chamber, the outlet of the 4th discharging tube 5-7
Connected with waste liquid tank V9, and the 4th discharging tube 5-7 is provided with and absorbs titration tank waist valve S15；
The self priming pump outlet valve S2, water sample pretreatment tank sampling valve S3, water sample pretreatment tank waist valve S4, water sample are located in advance
Manage tank overflow valve S5, water sample constant volume tank waist valve S6, buffer solution valve S7, water sample constant volume tank bleeder valve S8, evaporator atmospheric valve S9,
Evaporator waist valve S10, cleaning fluid valve S11, condensate liquid valve S12, boric acid bleeder valve S13, boric acid constant volume tank waist valve S14 and suction
It is magnetic valve to receive titration tank waist valve S15, and the electromagnetism is respectively connected with PLC；
The sampling pump P1, sampling pump P2, acid adding pump P3 plus alkali pump P4, buffer solution pump P5, cleaning liquid pump P6, syringe pump
P7, boric acid pump P8, the first pH potentiometric detection electrodes J1, the first temperature sensor TE1, the first agitator MS1, the inspection of the 2nd pH current potentials
Electrode J2, second temperature sensor TE2, level electrode LS, the second agitator MS2 and the regulator is surveyed to control with PLC
Device is respectively connected with.
Further, the second described agitator MS2 is magnetic-type agitator.
Further, the entrance point of the sampling pump P1 is provided with screen pack L.
Further, the tank deck 2-6 of the water sample pretreatment tank V1 is plane, and the tank bottom of the water sample pretreatment tank V1 is cone
Shape end socket 2-8, and the first discharging tube 2-9 is arranged at described conical head 2-8 centers.
Further, the first agitator MS1 and water sample pretreatment tank V1 is coaxially disposed.
Further, the top of the second overflow pipe 3-7 is flat mouth.
Further, the top opening of the cylinder 3-3 and base opening are threadedly coupled with top cover 3-1 and bottom 3-6 respectively.
Further, the drainer tank deck 4-6 is butterfly end socket, and tank bottom 4-10 is conical head.
Further, the first cooling liquid outlet 4-7 and the second cooling liquid outlet 4-11 are connected with floss hole PF；First is cold
But liquid import 4-9 and the second cooling liquid inlet 4-13 passes sequentially through cooling water valve S1, water outlet pipeline a the 3rd outlet with adopting
The sample pump P1 port of export is connected, and the cooling water valve S1 is magnetic valve, and the cooling water valve S1 is connected with PLC.
Further, cylinder 3-3 and the second overflow pipe 3-7 fit structure are：The second overflow pipe 3-7 by bolt with
The cylinder 3-3 is connected, and bolt is located on the outer surface of the bottom 3-6, and the second overflow pipe 3-7 is through the bolt and and spiral shell
Bolt is meshed.
Automatic addition is difficult to solve buffer substance light magnesium oxide solid state powder, the magnesia of adhesion is difficult to clean
The instability problems such as mutability be present with solid oxidation magnesium, present invention employs the cushioning liquid of liquid to replace solid oxide
Magnesium, realize automatic gauge and addition.It is difficult to accurate the problems such as realizing automatic judgement and technological difficulties to solve titration end-point, this
The principle and method of invention Applied Electrochemistry, the judgement of titration end-point is realized using automatic potentiometric titration technology, to substitute simultaneously
Solving indicator in new national standard method judges terminal during automatic detection the shortcomings that and deficiency.
The beneficial effects of the invention are as follows：The ammonia nitrogen online automatic monitor of the present invention solves existing distillation-acid-base titration
Mixed indicator stabilization time present in method is short, solid oxidation magnesium is difficult to automatic addition, titration end-point is difficult to accurate reality
Now automatic the problems such as judging and technological difficulties.Solid MgO is substituted using liquid buffer solution, realizes that the automatic of pH adjusting agent adds
Add；Using the automatic distilling apparatus that a kind of electrical heating power is adjustable, distilling rate is controllable, distillation efficiency is improved, increases instrument
Safety and reliability；Using a kind of freely adjustable automatic liquid metering device of liquid measure, the essence of water sample and absorbing liquid is realized
It is determined that amount；The judgement of titration end-point is carried out using pH potentiometric detections electrode, adds sensitivity and the accuracy of instrument, and extend
The measurement range of instrument, enables the invention to adapt to the detection of the surface water such as trade effluent, sanitary sewage, river, lake simultaneously.
Brief description of the drawings
Fig. 1 is the overall structure diagram of the present invention；
The water sample that Fig. 2 is the present invention pre-processes jar structure schematic diagram；
Fig. 3 is the structural representation of the water sample constant volume tank of the present invention；
Fig. 4 is the distillation unit structural representation of the present invention；
The absorption that Fig. 5 is the present invention titrates jar structure schematic diagram.
P1. sampling pumps in Fig. 1, P2. sampling pumps, P3. acid adding pumps, P4. add alkali pump, P5. buffer solution pumps, and P6. cleans liquid pump,
P7. syringe pump, P8. boric acid pumps, V1. water samples pretreatment tank (are used to contain water sample to be measured), and V2. water sample constant volumes tank (is used to contain
Pretreated water sample to be measured), V3. acid tank (is used for the dilute sulfuric acid for containing pH in regulation water sample pretreatment tank), and V4. alkali tank (is used
In the sodium hydroxide for containing pH in regulation water sample pretreatment tank), V5. buffer solutions, which fill, (is used to contain the mixed of pH in regulation evaporator
Buffer solution is closed, and the cocktail buffer is by Na2HPO4With NaOH proportionally 25:2 mix), V6. evaporators (are used to contain
Fill the water sample of ammonia nitrogen to be distilled), V7. cleaning fluid tanks (are used for the distilled water for containing cleaning), and V8. drainers (it is cold to be used for steam
Solidifying drainer), V9. waste liquid tanks (waste tank after waste liquid and titration after distillation), V10. absorbs titration tank and (inhaled after distillation
Receive the tourie of ammonia), V11. titration flow containers (the hydrochloric acid solution storage tank of the normal concentration of titration), V12. boric acid constant volumes tank (is inhaled
Receive the measuring tank of liquid), V13. boric acid tank (absorbing liquid boric acid storage tank), E1. jacket type straight tube coolers, a. water outlet pipelines, b.
Water sample overflow pipe, c. glass absorption tubes, d. boric acid overflow pipes, e. burets, S1. cooling water valves, S2. self priming pump outlet valves, S3.
Water sample pre-processes tank sampling valve, S4. water samples pretreatment tank waist valve, S5. water samples pretreatment tank overflow valve, S6. water sample constant volume tanks
Waist valve, S7. buffer solution valves, S8. water sample constant volume tank bleeder valves, S9. evaporator atmospheric valves, S10. evaporator waist valves, S11.
Cleaning fluid valve, S12. condensate liquid valves, S13. boric acid bleeder valves, S14. boric acid constant volume tank waist valves, S15. absorb titration tank waste liquid
Valve, the agitators of MS1. first, the agitators of MS2. second, the temperature sensors of TE1. first, TE2. second temperature sensors, J1.
One pH potentiometric detection electrodes, the pH potentiometric detection electrodes of J2. the 2nd, L. screen packs, LS. level electrodes, each magnetic valve carries in Fig. 1
The part for being labeled as s be electric control system, be also the drive part of magnetic valve.
Embodiment
A kind of ammonia nitrogen on-line computing model based on distillation titration method, including sampling and pretreatment unit, dosing unit, steaming
Evaporate unit, absorb titration unit, post-processing unit and PLC；And have in the PLC at control module and data
Manage module.
Described sampling and pretreatment unit include water sample pretreatment tank V1, the tank body 2-1 of the water sample pretreatment tank V1
Outlet is sequentially provided with hollow cylindrical shape, and on water sample pretreatment tank V1 tank deck 2-6 with water sample pretreatment tank V1's
Sample tap 2-5, the acid-adding port 2-3 of intracavity inter-connection and plus alkali mouth 2-4；And the import of the acid-adding port 2-3 passes through acid adding pump P3
And connected with circuits with sour tank V3, described plus alkali mouth 2-4 import is by adding alkali pump P4 and being connected with circuits with alkali tank V4；
The first pH potentiometric detection electrodes J1, the first temperature sensor TE1 and the are provided with described water sample pretreatment tank V1
One agitator MS1；The top of the first pH potentiometric detection electrodes J1, the first temperature sensor TE1 top and the first stirring
Device MS1 top is each attached on water sample pretreatment tank V1 tank deck, and the bottom of the first pH potentiometric detection electrodes J1, the
One temperature sensor TE1 bottom and the first agitator MS1 bottom are all extended in water sample pretreatment tank V1；
Water sample pretreatment tank V1 tank bottom 2-8 is provided with the first discharging tube 2-9, the first discharging tube 2-9 import and
Water sample pretreatment tank V1 intracavity inter-connection, the first discharging tube 2-9 outlet connects with floss hole PF, and the first discharging tube 2-9
It is provided with water sample pretreatment tank waist valve S4；
The both sides of the water sample pretreatment tank V1 are respectively equipped with water inlet pipe 2-2 and the first overflow pipe 2-7；Water inlet pipe 2-2's
Outlet and water sample pretreatment tank V1 intracavity inter-connection, water inlet pipe 2-2 import connect with water inlet pipeline a first outlet,
The import of the water inlet pipeline a is connected with sampling pump P1 outlet, and the import of the sampling pump P1 is connected with water source, and
The second outlet of the water inlet pipeline a is connected by delivery pipe with floss hole PF, and the delivery pipe is provided with self priming pump water outlet
Valve S2；The water inlet pipe 2-2 is provided with water sample pretreatment tank sampling valve S3；The import of the first overflow pipe 2-7 and water sample are pre-
Process tank V1 inner chamber connection, the first overflow pipe 2-7 outlet connects with floss hole PF, and the first overflow pipe 2-7 is provided with water
Sample pretreatment tank overflow valve S5；
Described dosing unit includes water sample constant volume tank V2 and boric acid constant volume tank V12, and water sample constant volume tank V2 tank body and
Boric acid constant volume tank V12 tank body is cylindrical tube 3-3, and the top opening of the cylinder 3-3 and base opening are respectively provided with detachably
Top cover 3-1 and bottom 3-6；The bottom 3-6 is provided with the second discharging tube 3-8 that import connects with cylinder 3-3 inner chambers；Cylinder
3-3 both sides are respectively equipped with the first feed tube 3-2 and drain pipe 3-5, the first feed tube 3-2 are located at drain pipe 3-5 top, and
The inner chamber of first feed tube 3-2 outlet and drain pipe 3-5 import with cylinder 3-3 connects；Being provided with cylinder 3-3 can be along cylinder
The second the overflow pipe 3-7, the second overflow pipe 3-7 moved up and down to body 3-3 axial seal top is located in cylinder 3-3 and the
Two overflow pipe 3-7 top opening is located on drain pipe 3-5, and bottom 3-6 is run through in the second overflow pipe 3-7 bottom；The cylinder 3-3
Outer surface on be provided with scale vertically；
The second discharging tube 3-8 of water sample constant volume tank V2 outlet is connected with floss hole PF, and water sample constant volume tank V2
The second discharging tube 3-8 be provided with water sample constant volume tank waist valve S6；The first feed tube 3-2 of water sample constant volume tank V2 import
Tank V1 sample tap 2-5 outlet is pre-processed by sampling pump P2 and with circuits and the water sample；The water sample constant volume
Tank V2 the second overflow pipe 3-7 bottom connects with floss hole PF；The drain pipe 3-5 of the water sample constant volume tank V2 is provided with water sample
Constant volume tank bleeder valve S8；
The second discharging tube 3-8 of boric acid constant volume tank V12 outlet is connected with boric acid tank V13, and boric acid constant volume tank
V12 the second discharging tube 3-8 is provided with boric acid constant volume tank waist valve S14；The first feed tube 3-2 of the boric acid constant volume tank V12
Import be connected by boric acid pump P8 and with circuits with boric acid tank V13；On the drain pipe 3-5 of the boric acid constant volume tank V12
Provided with boric acid bleeder valve S13；The second overflow pipe 3-7 of boric acid constant volume tank V12 bottom is connected with boric acid tank V13；
Described distillation unit includes evaporator V6, drainer V8 and jacket type straight tube cooler E1, the drainer V8
Positioned at the top of the evaporator V6, and the inner chamber of the evaporator V6 and the inner chamber of the drainer V8 pass through steam outlet pipe 4-4
It is connected, and tank bottom 4-10 of the steam outlet pipe 4-4 both ends respectively with evaporator V6 tank deck 4-18 and drainer V8 is connected；
The tank body 4-17 of the evaporator V6 is in hollow cylindrical shape, and evaporator V6 tank deck 4-18 is respectively equipped with clearly
Wash pipe 4-1, the second feed tube 4-2 and blow-down pipe 4-3；
The outlet of the cleaning pipe 4-1 connects with evaporator V6 inner chamber, and the import of the cleaning pipe 4-1 is respectively by slow
Fliud flushing pump P5 and be connected with circuits, cleaning liquid pump P6 and with circuits with buffering flow container V5, cleaning fluid tank V7, and it is described clearly
Wash pipe 4-1 and be provided with buffer solution valve S7；
The outlet of the second feed tube 4-2 connects with evaporator V6 inner chamber, the second feed tube 4-2 import and water sample
Constant volume tank V2 drain pipe 3-5 outlet is connected；
The import of the blow-down pipe 4-3 connects with evaporator V6 inner chamber, the outlet of the blow-down pipe 4-3 and ambient atmosphere
It is connected, and blow-down pipe 4-3 is provided with evaporator atmospheric valve S9；
Evaporator V6 tank bottom 4-16 is externally provided with electric heating plate H1, the electric heating plate H1 and is connected with adjustable heating power
Regulator；Evaporator V6 tank bottom 4-16 is additionally provided with the 3rd discharging tube 4-15, the 3rd discharging tube 4-15 top and evaporation
Tank V6 intracavity inter-connection, the 3rd discharging tube 4-15 bottom insulation are connected through electric heating plate H1 and with waste liquid tank V9, and
Evaporator waist valve S10 is additionally provided with 3rd discharging tube 4-15；
The tank body 4-5 of the drainer V8 is in hollow cylindrical shape, and is arranged with outside the tank body 4-5 of the drainer V8
Drainer chuck 4-8, the drainer chuck 4-8 side are respectively equipped with the coolings of the first cooling liquid outlet 4-7 and first up and down
Liquid import 4-9, and the first cooling liquid outlet 4-7 and the first cooling liquid inlet 4-9 are connected with cooling system respectively；
The jacket type straight tube cooler E1 includes condensate liquid drain pipe 4-14 and is set in outside condensate liquid drain pipe 4-14
Cooling tube chuck 4-12；Condensate liquid drain pipe 4-14 import is at the tank bottom 4-10 of the solidifying tank V8 and in drainer V8
Chamber is connected；The second cooling liquid outlet 4-11 and the second cooling liquid inlet 4- are respectively arranged with the cooling tube chuck 4-12
13, and the second cooling liquid outlet 4-11 and the second cooling liquid inlet 4-13 connect with cooling system respectively；
Described absorption titration unit includes absorbing titration tank V10, and described absorption titration tank V10 tank body 5-8 is in sky
The cylindrical shape of the heart, and the tank deck 5-2 for absorbing titration tank V10 is provided with condensate line 5-3, absorbs liquid pipe 5-4 and titration
Liquid pipe 5-5；
The inner chamber that the outlet of the condensate line 5-3 titrates tank V10 with absorbing connects, condensate line 5-3 import with it is cold
Lime set drain pipe 4-14 outlet is connected, and the condensate line 5-3 is provided with condensate liquid valve S12；
The outlet for absorbing liquid pipe 5-4 connects with absorbing titration tank V10 inner chamber, the import for absorbing liquid pipe 5-4
Outlet with boric acid constant volume tank V12 drain pipe 3-5 is connected；
Buret e is provided with the titration liquid pipe 5-5, the import of the buret e is by syringe pump P7 and with circuits
It is connected with titration flow container V11, the outlet of the buret e titrates tank V10 intracavity inter-connection with absorbing；
The tank deck 5-2 of the titration tank V10 is further fixed on the 2nd pH potentiometric detection electrodes extended in titration tank V10
J2, second temperature sensor TE2, level electrode LS, titration tank V10 tank bottom 5-6 are provided with the second agitator MS2；
The side of the titration tank V10 is respectively arranged with cleaning liquid pipe 5-1 and the 4th discharging tube 5-7；The cleaning liquid pipe
5-1 outlet and titration tank V10 intracavity inter-connection, the import of the cleaning liquid pipe 5-1 is by cleaning liquid pump P6 and with sleeve pipe
Road is connected with cleaning fluid tank V7, and the cleaning liquid pipe 5-1 is provided with cleaning fluid valve S11；
The import of the 4th discharging tube 5-7 connects with titrating tank V10 inner chamber, the outlet of the 4th discharging tube 5-7
Connected with waste liquid tank V9, and the 4th discharging tube 5-7 is provided with and absorbs titration tank waist valve S15；
The self priming pump outlet valve S2, water sample pretreatment tank sampling valve S3, water sample pretreatment tank waist valve S4, water sample are located in advance
Manage tank overflow valve S5, water sample constant volume tank waist valve S6, buffer solution valve S7, water sample constant volume tank bleeder valve S8, evaporator atmospheric valve S9,
Evaporator waist valve S10, cleaning fluid valve S11, condensate liquid valve S12, boric acid bleeder valve S13, boric acid constant volume tank waist valve S14 and suction
It is magnetic valve to receive titration tank waist valve S15, and the electromagnetism is respectively connected with PLC；
The sampling pump P1, sampling pump P2, acid adding pump P3 plus alkali pump P4, buffer solution pump P5, cleaning liquid pump P6, syringe pump
P7, boric acid pump P8, the first pH potentiometric detection electrodes J1, the first temperature sensor TE1, the first agitator MS1, the inspection of the 2nd pH current potentials
Electrode J2, second temperature sensor TE2, level electrode LS, the second agitator MS2 and the regulator is surveyed to control with PLC
Device is respectively connected with.
The second described agitator MS2 is magnetic-type agitator.
The entrance point of the sampling pump P1 is provided with screen pack L.
The tank deck 2-6 of the water sample pretreatment tank V1 is plane, and the tank bottom of the water sample pretreatment tank V1 is conical head
2-8, and the first discharging tube 2-9 is arranged at described conical head 2-8 centers.
The first agitator MS1 is coaxially disposed with water sample pretreatment tank V1.
The top of the second overflow pipe 3-7 is flat mouth.
The top opening and base opening of the cylinder 3-3 is threadedly coupled with top cover 3-1 and bottom 3-6 respectively.
The drainer tank deck 4-6 is butterfly end socket, and tank bottom 4-10 is conical head.
First cooling liquid outlet 4-7 and the second cooling liquid outlet 4-11 are connected with floss hole PF；First coolant is entered
Mouth 4-9 and the second cooling liquid inlet 4-13 passes sequentially through cooling water valve S1, water outlet pipeline a the 3rd outlet and sampling pump P1
The port of export be connected, and the cooling water valve S1 is magnetic valve, and the cooling water valve S1 is connected with PLC.
Cylinder 3-3 and the second overflow pipe 3-7 fit structure is：The second overflow pipe 3-7 passes through bolt and the cylinder
Body 3-3 is connected, and bolt is located on the outer surface of the bottom 3-6, and the second overflow pipe 3-7 mutually nibbles through the bolt and with bolt
Close.
Described syringe pump P7 is industrial formula syringe pump；The first described temperature sensor TE1 and second temperature sensor
TE2 is Pt100 armored thermal resistances；Described syringe pump P7 is industrial injection pump, and described sampling pump P1 is self priming pump, is taken
Sample pump P2, acid adding pump P3 plus alkali pump P4, buffer solution pump P5, cleaning liquid pump P6 and injection boric acid pump P8 are described in peristaltic pump
First pH potentiometric detection electrode J1 and the 2nd pH potentiometric detection electrodes J2 are compound pH potentiometric detections electrode；Liquid-level switch LS is
Electric pole type liquid-level switch.
Ammonia nitrogen online automatic monitor of the invention as Figure 1-5 include sampling and pretreatment unit, dosing unit,
Distillation unit, absorb titration unit, post-processing unit, PLC controls and data processing unit (i.e. PLC).
Sampling and pretreatment unit pre-process tank V1, sampling pump P1, acid adding pump P3 plus alkali pump P4 etc. by water sample and formed.Such as
Shown in Fig. 2, described water sample pretreatment tank V1 is hollow cylindrical tank 2-1, and the inner top surface 2-6 of tank is plane, and tank deck
2-6 is equipped with pH potentiometric detection electrodes J1, temperature sensor TE1 and agitator MS1；Tank deck 2-6 is separately provided with sample tap 2-5, added
Sour mouth 2-3 and plus alkali mouth 2-4；Tank side is provided with water inlet pipe 2-2 and overflow pipe 2-7；Tank bottom 2-8 is conical head, described
Conical head 2-8 is provided centrally with the first discharging tube 2-9.Further, described water inlet pipe 2-2, overflow pipe 2-7 and the first discharge opeing
Water sample pretreatment tank sampling valve S3, water sample pretreatment tank overflow valve S5, water sample pretreatment tank waist valve are respectively arranged with pipe 2-9
S4, the magnetic valve are connected with PLC；Screen pack L, a points of sampling pump P1 water outlet pipeline are housed before described sampling pump P1
Cooling water valve S1, self priming pump outlet valve S2 and water sample pretreatment tank sampling valve S3 are not met；Described acid adding pump P1 passes through silicone tube
It is connected respectively with water sample pretreatment tank acid-adding port 2-3 and sour tank V3；Described plus alkali pump P2 is pre- with water sample respectively by silicone tube
Process tank adds alkali mouth 2-4 to be connected with alkali tank V4.
Sampling and pretreatment unit start, and open self priming pump outlet valve S2, water sample pretreatment tank sampling valve S3 and pretreatment
Tank overflow valve S5, sampling pump P1 startup, water sample flow into water sample pretreatment by filter screen L suction sampling pump P1 through water outlet pipeline a
Tank V1, overflowed through overflow pipe 2-7 after hydroful, the water sample of spilling flow to floss hole PF, overflow for a period of time, close sampling pump P1,
Water sample pre-processes tank overflow valve S5 and water sample pretreatment tank sampling valve S3, completes water sampling.Meanwhile agitator MS1 is opened, lead to
The pH of pH electrodes J1 detection water samples is crossed, when the pH for measuring water sample is excessive, then opens the PH of acid adding pump P3 regulation water samples to after neutrality,
Close acid adding pump P3；When the PH for measuring water sample is too small, then opening alkali pump P4 regulations water sample pH is adjusted to neutrality, is closed and is added alkali pump
P4.Meanwhile real time temperature signal is reached PLC by temperature sensor TE1.
Dosing unit includes water sample constant volume tank V2, sampling pump P2, boric acid constant volume tank V12 and boric acid pump P8 etc..Such as Fig. 3 institutes
Show, described water sample constant volume tank V2 and boric acid constant volume tank V12 are hollow cylindrical tube 3-3, at the top and bottom of cylinder 3-3
The top cover 3-1 and bottom 3-6 of screw thread are provided with respectively, and cylinder 3-3 surfaces are provided with scale mark, the upper and lower part of side
The first feed tube 3-2 and drain pipe 3-5 is not provided with, and bottom is provided with the second discharging tube 3-8；Second is provided with cylinder 3-3
Overflow pipe 3-7, the second described overflow pipe 3-7 is axially vertical to pass through bottom 3-6, and one end extends to cylinder 3-3 inner chambers, and one end is stretched
Go out outside cylinder 3-3；The second described overflow pipe 3-7 upper-lower positions are adjustable, and the second overflow pipe 3-7 upper ends are arranged to concordant overflow
Mouthful, and the height of upper end is higher than drain pipe 3-5 top edge；Set respectively on described drain pipe 3-5 and the second discharging tube 3-8
There are water sample constant volume tank waist valve S6, water sample bleeder valve S8, boric acid constant volume tank waist valve S14, boric acid bleeder valve S13, it is described electronic
Valve is connected with PLC；Described sampling pump P2 by silicone tube respectively with the first feed tube 3-2 of water sample constant volume tank and
Water sample pretreatment tank sample tap 2-5 is connected；Described boric acid pump P8 by silicone tube respectively with boric acid constant volume the first feed tube of tank
3-2 is connected with boric acid tank V13.
After water sampling and pretreatment terminate, PLC controls and data processing unit control boric acid pump P8 work, close simultaneously
The boric acid closed in boric acid bleeder valve S13 and boric acid constant volume tank waist valve S14, boric acid tank V13 is transported to boric acid constant volume tank V12
Interior, liquid level rises in boric acid constant volume tank V12, until overflow, the boric acid that overflow goes out is through overflow passage d (with boric acid constant volume tank V12's
Second overflow pipe 3-7 connections) flow back to boric acid tank V13.Boric acid pump P8 is closed after overflow certain time, then is beaten after standing certain time
Boric acid bleeder valve S13 is opened, closing boric acid after the boric acid of boric acid constant volume tank V12 quantification fully flows into absorption titration tank V10 puts
Liquid valve S13.Absorption titration tank V10, which has been fed, to be closed, and PLC control sampling pump P2 work, simultaneously closes off water sample bleeder valve S8
With water sample constant volume tank waist valve S6, the water sample that water sample is pre-processed in tank V1 is transported to water sample constant volume tank V2, water sample constant volume tank V2
Middle liquid level rises, until overflow, the water sample that overflow goes out (connects through overflow passage b with water sample constant volume tank V2 the second overflow pipe 3-7
Connect) it is discharged into floss hole PF.Sampling pump P2 is closed after overflow certain time, then opens water sample constant volume tank after certain time after standing and puts
Liquid valve S8, water sample constant volume tank bleeder valve S8 is closed after the water sample of water sample constant volume tank V2 quantification fully flows into evaporator V6.
When water sample charging finishes, PLC controls and data processing unit control start buffer solution pump P5 and open buffer solution valve
S7, cushioning liquid, which is quantitatively added dropwise, makes water sample in evaporator V6 be in closing buffer solution valve S7 after alkalescent, simultaneously closes off buffer solution pump
P5。
Described distillation unit includes evaporator V6, drainer V8 and jacket type straight tube cooler E1.As shown in figure 4, institute
The evaporator V6 stated tank body 4-17 is cylinder, and tank deck 4-18 and tank bottom 4-16 are plane；The tank deck of the evaporator V6
4-18 is provided with cleaning pipe 4-1, the second feed tube 4-2, blow-down pipe 4-3 and steam outlet pipe 4-4, tank bottom 4-16 and is provided with the 3rd discharge opeing
Pipe 4-15.Buffer solution valve is respectively arranged with cleaning pipe 4-1, the second feed tube 4-2, blow-down pipe 4-3 and the 3rd discharging tube 4-15
S7, water sample constant volume tank bleeder valve S8, evaporator atmospheric valve S9 and evaporator waist valve S10, the magnetic valve is and PLC
It is connected；Evaporator V6 outer bottom is provided with electric heating plate H1, the electric heating plate H1 and is connected with the tune of adjustable heating power
Pressure device, regulator are connected with PLC.Described drainer V8 is the cylinder for being provided with drainer chuck (4-8)
Tank body 4-5, the side of the drainer chuck (4-8) are respectively arranged with cooling liquid outlet 4-7 and cooling liquid inlet 4-9 up and down,
It is connected with cooling system；The drainer tank deck 4-6 is butterfly end socket, and tank bottom 4-10 is conical head, and the condensate liquid goes out liquid
Pipe 4-14 is located at conical head center.Cooling liquid outlet 4-11 and cooling liquid inlet 4-13 are provided with chuck 4-12, with cooling
System connects.
After water sample and buffer solution are quantitatively adding evaporator V6 successively, PLC controls start with data processing unit control
Sampling pump P1, and cooling water valve S1 and magnetic force the second agitator MS2 are opened, while control regulator to add evaporator V6
Thermal distillation, the ammonia in water sample quickly escape with the rise of water temperature, with water vapour in drainer V8 after water sample boiling
Interior condensation, and enter after further being cooled down in jacket type straight tube cooler E1 through glass absorption tube c and absorb titration tank V10, quilt
The boric acid solution being quantitatively adding in advance is absorbed.After distillation certain time (level electrode LS conductings), PLC control regulators stop
Only heat, obtain a certain amount of distillate.
Described absorption titration unit mainly includes absorbing titration tank V10, the second agitator MS2 and syringe pump P7 etc..Institute
The absorption titration tank V10 stated tank body 5-8 is cylinder, and tank deck 5-2 and tank bottom 5-6 are plane；It is described to absorb titration tank
V10 tank decks 5-2 is provided with condensate line 5-3, absorbs liquid pipe 5-4 and titration liquid pipe 5-5, the condensate line 5-3 and absorbing liquid
Condensate liquid valve S12 and boric acid bleeder valve S13 are respectively arranged with pipe 5-4, the magnetic valve is connected with PLC；It is described
Tank deck 5-2 is equipped with the 2nd pH electrodes J2, second temperature sensor TE2 and level electrode LS, and is inserted in tank at center；It is described
PH electrodes J2 be combined type current potential detecting electrode, second temperature sensor TE2 is Pt100 armored thermal resistances, level electrode
LS is bipolar system level electrode；Tank side is provided with cleaning liquid pipe 5-1 and the 4th discharging tube 5-7, the cleaning liquid pipe 5-1 and the
Cleaning fluid valve S11 is respectively arranged with four discharging tube 5-7 and absorbs titration tank waist valve S15, the magnetic valve controls with PLC
Device is connected；The second described agitator MS2 is magnetic-type agitator, is placed in the bottom for absorbing titration tank V10；Described syringe pump
P7 is industrial formula syringe pump, by buret e respectively with absorbing titration tank V10 titration liquid pipe 5-5 and titrating flow container V11 phases
Even.
When level electrode LS is turned on, PLC controls close condensate liquid valve S12 with data processing unit, start syringe pump P7, drop
Determine liquid and absorb titration tank V10 progress acid-base titrations by titrating tank e injections, the 2nd pH potentiometric detection electrode J2 and second temperature pass
The pH electric potential signals and temperature signal that are detected in titration process are continually entered PLC controls and data processing by sensor TE2 respectively
Unit.Meanwhile PLC controls judge titration end-point with data processing unit according to the temperature signal and pH electric potential signals of titrating solution
And stop syringe pump P7, the actual content of ammonia nitrogen in water sample is finally calculated according to syringe pump P7 titer, and deposit simultaneously
Storage and display.
Described post-processing unit includes two parts of discharging of waste liquid and cleaning.After the completion of each titrimetry, water sample
The raffinate that pretreatment tank V1, water sample constant volume tank V2, boric acid constant volume tank V12, evaporator V6, absorption are titrated in tank V10 is both needed to discharge
Totally, and cleaned, to treat on-line sampling analysis next time.V2 waste liquid is straight in water sample pretreatment tank V1, water sample constant volume tank
Connect and be emitted into floss hole PF, the boric acid in boric acid constant volume tank V12 is emitted into boric acid tank V13, evaporator V6 and absorbed in titration tank
V10 discharging of waste liquid is to waste liquid tank V9.Water sample pre-processes tank V1 and water sample constant volume tank V2 and carries out prewashing with water to be measured, and evaporator
V6 and absorption titration tank V10 are cleaned with distilled water, distilled water cleaning liquid pump P6 conveyings.The water sample pretreatment tank V1, water
Sample constant volume tank V2, boric acid constant volume tank V12, evaporator V6, absorption, which titrate, is respectively arranged with water sample pretreatment on tank V10 discharging tube
Tank waist valve S4, water sample constant volume tank waist valve S6, boric acid constant volume tank waist valve S14, evaporator waist valve S10 and absorption titration tank
Waist valve S15, the magnetic valve are connected with PLC.
Water sample constant volume tank V2 post processing is as follows：Water sample constant volume tank waist valve S6 is opened, treats that water sample constant volume tank V2 bottoms are arranged
After liquid certain time, water sample constant volume tank waist valve S6 is closed；Start sampling pump P2, treat sample introduction certain time, ensure water sample constant volume
When water sample expires supreme overfall in tank, sampling pump P2 is closed, and open water sample constant volume tank waist valve S6；Treat water sample constant volume pot bottom
After discharge opeing certain time, water sample constant volume tank waist valve S6 is closed.Water sample pretreatment tank V1 post processing walks with water sample constant volume tank V2
It is rapid identical, it is not repeated herein.
Evaporator V6 post-processing step：When temperature drops to less than 50 DEG C in tank V6 to be evaporated, open water sample constant volume tank and put
Liquid valve S8, evaporator atmospheric valve S9, evaporator waist valve S10, after discharge opeing certain time, close valve water sample constant volume tank bleeder valve
S8, evaporator waist valve S10.After raffinate drains, buffer solution liquid feed valve S7 is opened, starts cleaning liquid pump P6；Treat from cleaning fluid
After appropriate distilled water is extracted in tank V7, buffer solution valve S8, cleaning liquid pump P6 are closed；After standing cleaning certain time, open and steam
Send out tank waist valve S10；After discharge opeing certain time, evaporator waist valve S10 and evaporator atmospheric valve S9 is closed.
It is similar to absorb the step of row's raffinate for titrating tank V10 and cleaning step are with evaporator V6, is not repeated herein.Inhaling
After the completion of receiving the V10 cleanings of titration tank, a certain amount of distilled water is extracted from cleaning fluid tank V7, for soaking and protecting pH electrodes
J2。
The ammonia nitrogen on-line computing model of the present invention automatically controls the work of other each units by PLC controls with data processing unit
Make process, calculating, display, printing, storage detected value enter row information by data communication mouth and exchanged, and can also facilitate composition net
Network, this instrument is controlled using remote terminal, realize ammonia nitrogen on-line checking.
The workflow of the ammonia nitrogen online automatic monitor of the present invention is as follows：Startup → water sampling → water sample pretreatment →
Boric acid quantifies and adds absorption titration filling → water sample and quantifies and add evaporator → buffer solution and quantify and add evaporator → heating
Distillation, absorption → end distillation → acid-base titration → titration end-point judges → calculate measured value → display, printing, storage measured value
→ discharging of waste liquid → is cleaned → waited to be launched to be detected next time.
Content described in this specification embodiment is only enumerating to the way of realization of inventive concept, protection of the invention
Scope is not construed as being only limitted to the concrete form that embodiment is stated, protection scope of the present invention also includes art technology
Personnel according to present inventive concept it is conceivable that equivalent technologies mean.
Claims (10)
- A kind of 1. ammonia nitrogen on-line computing model based on distillation titration method, it is characterised in that：Including sampling and pretreatment unit, determine Measure unit, distillation unit, absorb titration unit, post-processing unit and PLC；Described sampling and pretreatment unit include water sample pretreatment tank (V1), the tank body (2- of the water sample pretreatment tank (V1) 1) it is in hollow cylindrical shape, and outlet is sequentially provided with the tank deck (2-6) of water sample pretreatment tank (V1) and is pre-processed with water sample Sample tap (2-5), acid-adding port (2-3) and plus the alkali mouth (2-4) of the intracavity inter-connection of tank (V1)；And the acid-adding port (2-3) Import connects by acid adding pump (P3) and with circuits with sour tank (V3), and described plus alkali mouth (2-4) import is by adding alkali pump (P4) and with circuits with alkali tank (V4) connect；Be provided with described water sample pretreatment tank (V1) the first pH potentiometric detections electrode (J1), the first temperature sensor (TE1) and First agitator (MS1)；The top of the first pH potentiometric detections electrode (J1), the top of the first temperature sensor (TE1) and The top of first agitator (MS1) is each attached on the tank deck of water sample pretreatment tank (V1), and the first pH potentiometric detections electricity The bottom of the bottom of pole (J1), the bottom of the first temperature sensor (TE1) and the first agitator (MS1) all extends to water sample and located in advance Manage in tank (V1)；The tank bottom (2-8) of the water sample pretreatment tank (V1) is provided with the first discharging tube (2-9), and the first discharging tube (2-9's) enters The intracavity inter-connection of mouth and water sample pretreatment tank (V1), the outlet of the first discharging tube (2-9) connect with floss hole (PF), and first Discharging tube (2-9) is provided with water sample pretreatment tank waist valve (S4)；The both sides of the water sample pretreatment tank (V1) are respectively equipped with water inlet pipe (2-2) and the first overflow pipe (2-7)；Water inlet pipe (2- 2) outlet and the intracavity inter-connection of water sample pretreatment tank (V1), the import of water inlet pipe (2-2) and the first of water inlet pipeline (a) Outlet, the import of the water inlet pipeline (a) are connected with the outlet of sampling pump (P1), the import of the sampling pump (P1) It is connected with water source, and the second outlet of the water inlet pipeline (a) is connected by delivery pipe with floss hole (PF), the discharge Pipe is provided with self priming pump outlet valve (S2)；The water inlet pipe (2-2) is provided with water sample pretreatment tank sampling valve (S3)；Described first The import of overflow pipe (2-7) connects with the inner chamber of water sample pretreatment tank (V1), the outlet of the first overflow pipe (2-7) and floss hole (PF) connect, and the first overflow pipe (2-7) is provided with water sample pretreatment tank overflow valve (S5)；Described dosing unit includes water sample constant volume tank (V2) and boric acid constant volume tank (V12), and the tank body of water sample constant volume tank (V2) Tank body with boric acid constant volume tank (V12) is cylindrical tube (3-3), and the top opening of the cylinder (3-3) and base opening are matched somebody with somebody respectively There are dismountable top cover (3-1) and bottom (3-6)；The bottom (3-6) is provided with that import connects with cylinder (3-3) inner chamber Two discharging tubes (3-8)；The both sides of cylinder (3-3) are respectively equipped with the first feed tube (3-2) and drain pipe (3-5), the first feed tube (3-2) is located at the top of drain pipe (3-5), and the first feed tube (3-2) outlet and drain pipe (3-5) import and cylinder The inner chamber connection of (3-3)；Being provided with cylinder (3-3) can be along the second overflow pipe for moving up and down of axial seal ground of cylinder (3-3) (3-7), the top of the second overflow pipe (3-7) is located in cylinder (3-3) and the top opening of the second overflow pipe (3-7) is located at drain pipe On (3-5), bottom (3-6) is run through in the bottom of the second overflow pipe (3-7)；Set vertically on the outer surface of the cylinder (3-3) There is scale；The outlet of the second discharging tube (3-8) of the water sample constant volume tank (V2) is connected with floss hole (PF), and water sample constant volume tank (V2) the second discharging tube (3-8) is provided with water sample constant volume tank waist valve (S6)；First feed liquor of the water sample constant volume tank (V2) The import of (3-2) is managed by sampling pump (P2) and sample tap (2-5) with circuits and water sample pretreatment tank (V1) goes out Mouth connection；The bottom of the second overflow pipe (3-7) of the water sample constant volume tank (V2) connects with floss hole (PF)；The water sample constant volume The drain pipe (3-5) of tank (V2) is provided with water sample constant volume tank bleeder valve (S8)；The outlet of the second discharging tube (3-8) of the boric acid constant volume tank (V12) is connected with boric acid tank (V13), and boric acid constant volume The second discharging tube (3-8) of tank (V12) is provided with boric acid constant volume tank waist valve (S14)；The first of the boric acid constant volume tank (V12) The import of feed tube (3-2) is connected by boric acid pump (P8) and with circuits with boric acid tank (V13)；The boric acid constant volume tank (V12) drain pipe (3-5) is provided with boric acid bleeder valve (S13)；The second overflow pipe (3-7) of the boric acid constant volume tank (V12) Bottom be connected with boric acid tank (V13)；Described distillation unit includes evaporator (V6), drainer (V8) and jacket type straight tube cooler (E1), the drainer (V8) it is located at the top of the evaporator (V6), and the inner chamber of the evaporator (V6) and the inner chamber of the drainer (V8) pass through Steam outlet pipe (4-4) is connected, and the both ends of steam outlet pipe (4-4) tank deck (4-18) and drainer (V8) with evaporator (V6) respectively Tank bottom (4-10) be connected；The tank body (4-17) of the evaporator (V6) is in hollow cylindrical shape, and the tank deck (4-18) of evaporator (V6) is set respectively There are cleaning pipe (4-1), the second feed tube (4-2) and blow-down pipe (4-3)；The outlet of the cleaning pipe (4-1) connects with the inner chamber of evaporator (V6), and the import of the cleaning pipe (4-1) passes through respectively Buffer solution pump (P5) and with circuits, cleaning liquid pump (P6) and with circuits with buffering flow container (V5), cleaning fluid tank (V7) is connected It is logical, and the cleaning pipe (4-1) is provided with buffer solution valve (S7)；The outlet of second feed tube (4-2) connects with the inner chamber of evaporator (V6), the import of the second feed tube (4-2) and water The outlet of the drain pipe (3-5) of sample constant volume tank (V2) is connected；The import of the blow-down pipe (4-3) connects with the inner chamber of evaporator (V6), and the outlet of the blow-down pipe (4-3) and the external world are big Gas phase connects, and blow-down pipe (4-3) is provided with evaporator atmospheric valve (S9)；The tank bottom (4-16) of evaporator (V6) is externally provided with electric heating plate (H1), and the electric heating plate (H1) is connected with adjustable heating The regulator of power；The tank bottom (4-16) of evaporator (V6) is additionally provided with the 3rd discharging tube (4-15), the 3rd discharging tube (4-15) Top and evaporator (V6) intracavity inter-connection, the bottom insulation of the 3rd discharging tube (4-15) through electric heating plate (H1) and with Waste liquid tank (V9) is connected, and is additionally provided with evaporator waist valve (S10) on the 3rd discharging tube (4-15)；The tank body (4-5) of the drainer (V8) is in hollow cylindrical shape, and tank body (4-5) overcoat of the drainer (V8) Provided with drainer chuck (4-8), the side of the drainer chuck (4-8) is respectively equipped with the first cooling liquid outlet (4-7) up and down With the first cooling liquid inlet (4-9), and the first cooling liquid outlet (4-7) and the first cooling liquid inlet (4-9) respectively with cooling system System connection；The jacket type straight tube cooler (E1) includes condensate liquid drain pipe (4-14) and is set in condensate liquid drain pipe (4-14) Outer cooling tube chuck (4-12)；The import of condensate liquid drain pipe (4-14) tank bottom (4-10) place of the solidifying tank (V8) with it is cold The intracavity inter-connection of solidifying tank (V8)；The second cooling liquid outlet (4-11) and are respectively arranged with the cooling tube chuck (4-12) Two cooling liquid inlets (4-13), and the second cooling liquid outlet (4-11) and the second cooling liquid inlet (4-13) respectively with cooling system Connection；Described absorption titration unit includes absorbing titration tank (V10), and the tank body (5-8) of described absorption titration tank (V10) is in Hollow cylindrical shape, and the tank deck (5-2) for absorbing titration tank (V10) is provided with condensate line (5-3), absorbs liquid pipe (5-4) and titration liquid pipe (5-5)；The outlet of the condensate line (5-3) with absorb titration tank (V10) inner chamber connect, the import of condensate line (5-3) and The outlet of condensate liquid drain pipe (4-14) is connected, and the condensate line (5-3) is provided with condensate liquid valve (S12)；The outlet for absorbing liquid pipe (5-4) connects with absorbing the inner chamber of titration tank (V10), described to absorb entering for liquid pipe (5-4) Mouth is connected with the outlet of the drain pipe (3-5) of boric acid constant volume tank (V12)；It is provided with buret (e) in titration liquid pipe (5-5), the import of the buret (e) passes through syringe pump (P7) and supporting Pipeline is connected with titration flow container (V11), the outlet of the buret e and the intracavity inter-connection for absorbing titration tank (V10)；The tank deck (5-2) of the titration tank (V10) is further fixed on the 2nd pH potentiometric detection electrodes extended in titration tank (V10) (J2), second temperature sensor (TE2), level electrode (LS), the tank bottom (5-6) of titration tank (V10) are provided with the second agitator (MS2)；The side of the titration tank (V10) is respectively arranged with cleaning liquid pipe (5-1) and the 4th discharging tube (5-7)；The cleaning fluid Outlet and the intracavity inter-connection of titration tank (V10) of (5-1) are managed, the import of the cleaning liquid pipe (5-1) is by cleaning liquid pump (P6) and with circuits with cleaning fluid tank (V7) it is connected, and the cleaning liquid pipe (5-1) is provided with cleaning fluid valve (S11)；The import of 4th discharging tube (5-7) connects with the inner chamber of titration tank (V10), and the 4th discharging tube (5-7's) goes out Mouth connects with waste liquid tank (V9), and the 4th discharging tube (5-7) is provided with and absorbs titration tank waist valve (S15)；The self priming pump outlet valve (S2), water sample pretreatment tank sampling valve (S3), water sample pretreatment tank waist valve (S4), water sample are pre- Process tank overflow valve (S5), water sample constant volume tank waist valve (S6), buffer solution valve (S7), water sample constant volume tank bleeder valve (S8), evaporation Tank atmospheric valve (S9), evaporator waist valve (S10), cleaning fluid valve (S11), condensate liquid valve (S12), boric acid bleeder valve (S13), boron Acid cut holds tank waist valve (S14) and absorbs that to titrate tank waist valve (S15) be magnetic valve, and the electromagnetism is and PLC It is respectively connected with；The sampling pump (P1), sampling pump (P2), acid adding pump (P3) plus alkali pump (P4), buffer solution pump (P5), cleaning liquid pump (P6), syringe pump (P7), boric acid pump (P8), the first pH potentiometric detections electrode (J1), the first temperature sensor (TE1), first stir Mix device (MS1), the 2nd pH potentiometric detections electrode (J2), second temperature sensor (TE2), level electrode (LS), the second agitator (MS2) it is respectively connected with the regulator with PLC.
- A kind of 2. ammonia nitrogen on-line computing model based on distillation titration method as claimed in claim 1, it is characterised in that：Described Second agitator (MS2) is magnetic-type agitator.
- A kind of 3. ammonia nitrogen on-line computing model based on distillation titration method as claimed in claim 2, it is characterised in that：It is described to adopt The entrance point of sample pump (P1) is provided with screen pack (L).
- A kind of 4. ammonia nitrogen on-line computing model based on distillation titration method as claimed in claim 3, it is characterised in that：The water The tank deck (2-6) of sample pretreatment tank (V1) is plane, and the tank bottom of the water sample pretreatment tank (V1) is conical head (2-8), and First discharging tube (2-9) is arranged at described conical head (2-8) center.
- A kind of 5. ammonia nitrogen on-line computing model based on distillation titration method as claimed in claim 4, it is characterised in that：Described One agitator (MS1) is coaxially disposed with water sample pretreatment tank (V1).
- A kind of 6. ammonia nitrogen on-line computing model based on distillation titration method as claimed in claim 5, it is characterised in that：Described The top of two overflow pipes (3-7) is flat mouth.
- A kind of 7. ammonia nitrogen on-line computing model based on distillation titration method as claimed in claim 6, it is characterised in that：The cylinder The top opening and base opening of body (3-3) are threadedly coupled with top cover (3-1) and bottom (3-6) respectively.
- A kind of 8. ammonia nitrogen on-line computing model based on distillation titration method as claimed in claim 7, it is characterised in that：It is described cold Solidifying tank tank deck (4-6) is butterfly end socket, and tank bottom (4-10) is conical head.
- A kind of 9. ammonia nitrogen on-line computing model based on distillation titration method as claimed in claim 8, it is characterised in that：First is cold But liquid outlet (4-7) and the second cooling liquid outlet (4-11) are connected with floss hole PF；First cooling liquid inlet (4-9) and Two cooling liquid inlets (4-13) pass sequentially through cooling water valve (S1), the 3rd outlet of water outlet pipeline (a) and sampling pump (P1) The port of export be connected, and the cooling water valve (S1) is magnetic valve, and the cooling water valve (S1) is connected with PLC.
- A kind of 10. ammonia nitrogen on-line computing model based on distillation titration method as claimed in claim 9, it is characterised in that：Cylinder (3-3) and the second overflow pipe (3-7) fit structure is：Second overflow pipe (3-7) passes through bolt and the cylinder (3-3) It is connected, bolt is located on the outer surface of the bottom (3-6), and the second overflow pipe (3-7) is mutually nibbled through the bolt and with bolt Close.
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