CN107340319A - A kind of method that non-contact gas membrane diffusion conductance directly detects ammonia nitrogen in waste water - Google Patents
A kind of method that non-contact gas membrane diffusion conductance directly detects ammonia nitrogen in waste water Download PDFInfo
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Abstract
The invention discloses a kind of method that non-contact gas membrane diffusion conductance directly detects ammonia nitrogen in waste water, including following operating procedure:Sample solution is drawn to inhale by peristaltic pump A is full of quantitative loop, after six-way valve switching, driven and drawn suction aqueous slkali to be sufficiently mixed with sample solution by peristaltic pump B, ammonia nitrogen is completely converted into ammonia in sample solution, into membrane diffusion unit sample solution cavity, the acceptable solution cavity that the non-contact hydrophobic membrane of certain proportion ammonia diffuses into opposite side becomes ammonium ion.By " arrheaing " or " flowing " dialysis pattern, the acceptable solution containing ammonium ion is entered membrane diffusion unit acceptable solution cavity, flow through conductance cell, electric conductivity detector directly determines ammonia-nitrogen content by electrical conductivity of solution change.The present invention have compared with prior art selectivity it is high, without distillation and colour developing, sample adaptability is good, the range of linearity is wide, diaphragm service life is long, without using toxic reagent, ammonia nitrogen directly in measure sewage or recycled water in 5min.
Description
Technical field
The present invention relates to a kind of detection method of ammonia-nitrogen content in waste water, more particularly to one kind to be expanded by non-contact air film
Dissipate, cause the method for the change directly detection ammonia nitrogen in waste water content of electrical conductivity.
Background technology
Ammonia nitrogen (NH3- N) it is with free ammonia (NH3) or ammonium salt (NH4+) form is present in water, it is China's water quality pollutant
One of overall control index.The assay method species of ammonia nitrogen is more, respectively there is feature, generally according to the discharge property and ammonia nitrogen of waste water
Concentration select corresponding method for monitoring and analyzing.
The method of measure ammonia nitrogen has Na's colorimetry, phenol-hypochlorite (or salicylic acid-hypochlorite) colorimetric at present
Method, electrode method, indophenol blue colorimetry, distillation titration method, and gas-phase molecular absorption spectrometry method.Na's colorimetry is ammonia nitrogen
Classical assay method, is most widely used, and suitable for mass disposal water sample, and water sample concentration range is wider, by many countries
It is classified as standard method of analysis;But the influence factor that nessler reagent is prepared is more, the metal ion such as calcium, magnesium and iron in water, sulfide,
The equal interference measurements such as aldehyde and ketone, color and muddiness, have a great influence to experimental result, need to distill absorption, and using
Need to handle the mercurous waste liquid after analysis in journey.Phenol-hypochlorite (or salicylic acid-hypochlorite) colorimetric method has
The advantages that sensitive, stable, but disturbed condition is identical with reagent colorimetric method, and also salicylic acid is unstable, and can only be to relatively cleaning
Water detected.Detection of the distillation-acidimetry suitable for ammonia-nitrogen content when higher, and distillation needs the regular hour,
The time of measure is long, is not also suitable for batch processing.Ammonia Gas Sensor Electrode Method be with alkali by the ammonia in water in the form of ammonia by
Go out, ammonia passes through the hydrophobic membrane of ammonia gas-sensing electrode, causes internal-filling liquid pH to change, and ammonia in sewage is determined by the change of electrode potential
Nitrogen, it is simple to operate, pre-processed without to sample, the operation such as distillation, flocculation sediment or filtering is eliminated, when having saved analysis
Between, it is suitable for high concentration and has more superiority with high-volume waste water, but electrode easily pollutes, and electrode fenestra is easily blocked, and stability is owed
It is good, it is necessary to timing change electrode (aging).Gas-phase molecular absorption spectrometry method can determine the sample of higher concentration, pre-treatment and other
Method is identical, but gas phase molecular absorption spectrometer is expensive, is widely applied with certain difficulty.In recent years environmental protection
The voluntary standard of ammonia nitrogen determination has been promulgated again in portion《Measure flow injection-salicylic acid AAS of Water quality ammonia nitrogen》, it is base
In salicylic acid AAS, the online distillation equipment of part apparatus preparation, the tedious steps distilled by hand are eliminated, selectivity
It is good, high sensitivity, but cost is of a relatively high, and it is longer to handle sample time, instrument clean and preparation of reagents be required to it is higher,
Large-scale promotion stills need the regular hour.Based on the diversity of water sample species, the selection to Ammonia-nitrogen analysis method proposes
Higher requirement;Ammonia nitrogen is under alkalescence condition in Blow-off-conductometry measure water, and by ammonia, the stripping from water sample, ammonia draw air
The change of absorbing liquid conductance is played, determines ammonia-nitrogen content, but the time is longer, and volatilization amine can make result higher.Ion chromatography is analyzed
The method for detecting ammonia nitrogen, facilitates sensitive, quick and precisely, but high sodium ion, potassium ion etc. have interference to ammonium root detection;Improved steaming
Evaporate method combination ion chromatography analysis detection ammonia nitrogen method, the extraction effect of ammonium root is good, and eliminate high sodium ion, potassium from
The interference that the cations such as son detect to ammonium root, but sample processing time is grown, and still has room for improvement.
Ammonia nitrogen in current existing stripping-conductance or distillation-Means of Electrical Conductivity water, is easily disturbed by organic volatile amine.Connect
Ammonia nitrogen in touch film infiltration-conductance measurement water, being vulnerable to other ions may " seepage " interference.The infiltration or non-contact of contact film
Ammonia nitrogen in formula film infiltration-determination of color water, poisonous and harmful reagent need to be used.Ammonia nitrogen in Ammonia Gas Sensor Electrode Method measure water, glass
Electrode is easy to aging, and electrode fenestra easily blocks.Sulfate by ion chromatography high-salt sewage ammonia nitrogen, sample pretreatment time are longer.It is existing
More, Manual chemical, electrochemical analysis or spectrum analysis are disturbed in standard method.Generally will be according to the discharge property of waste water and ammonia nitrogen
Concentration selects corresponding method for monitoring and analyzing.The method that non-contact gas membrane diffusion-conductance of the present invention directly detects ammonia nitrogen in waste water, expand
Throwaway member constant temperature does not surpass 40 DEG C, and the outlet of sample solution inlet ratio is slightly higher in membrane diffusion unit, into acceptable solution cavity, non-contact gas
Membrane diffusion, after conductance cell, cause the change of solution conductivity directly to detect ammonia nitrogen in waste water, without distillation, be not necessary to colorimetric, have
There are high sensitivity, selectivity good, environment-friendly and the detection feature of sample wide adaptability.
With the closely related document of the present invention:
Wang Weide, Yu Baoxiang, beam show phoenix Blow-off-conductometries determine ammonia nitrogen and its automatic analyzer environmental monitoring pipes in water
Reason and technology .2003,15 (1):30-31, by ammonia in air stripping water sample, ammonia causes absorbing liquid conductance to change, and determines ammonia
Nitrogen content.
Ammonia Shanghai environmental science .2000,19 in Xu Huahua, Xie Biqin bloomings flow injection spec-trophotometry measure water
(12):577-578, contacted by film liquid, after ammonia osmotic absorption, develop the color photometric detection ammonia nitrogen.
The B. wastewater flows of CN 101598719, ammonia nitrogen concentration and ammonia nitrogen total content water quality on-line combined tester .2013-10-02.
In full, it is to detect ammonia nitrogen by after ammonia generator, gas-liquid separator, ammonia absorber, then with electric conductivity detector.
CN102721786A. a kind of method .2012-10-10. for determining ammonia-nitrogen content in water is by gas-liquid point in full
From membrane tube, the measurement of the absorbance of the acid-base indicator to absorbing ammonia, the ammonia-nitrogen content in water sample is obtained indirectly.
CN103245697A. a kind of ammonia nitrogen on-line computing model .2013-08-14. is wet method distillation-conductance method detection in full
Ammonia nitrogen.
CN204855385U. a kind of ammonia nitrogen in-line analyzer .2015.12.09. full text, gas-liquid membrane separation device and colorimetric
Device connects luminosity colorimetric, obtains the content of the ammonia nitrogen in water sample indirectly.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of non-contact gas membrane diffusion-conductance is direct
The method for detecting ammonia nitrogen in waste water, must distillation procedure, inspection to solve ammonia nitrogen in waste water detection time length, complicated substrate in the prior art
The technical problem of secondary pollution is caused in survey condition harshness and detection process to environment.
The present invention is achieved by the following technical solutions:
The invention discloses a kind of method that non-contact gas membrane diffusion-conductance directly detects ammonia nitrogen in waste water, including following behaviour
Make step:
1) liquid and cleaning are filled out:Peristaltic pump A is opened, sample solution is sucked through sample pipe by peristaltic pump A to be connected with six-way valve
Quantitative loop in, fill excessive sample solution flow after quantitative loop and enter in sample waste liquid bottle;Meanwhile acceptable solution is driven by peristaltic pump A
Dynamic and drawing is inhaled, and flows through the acceptable solution cavity and electric conductivity detector device in purifier, membrane diffusion unit successively through acceptable solution pipeline,
From conductive detection device come out after acceptable solution flow into acceptable solution waste liquid bottle in;Continuous service for a period of time after, close peristaltic pump
A;
2) non-contact gas membrane diffusion:Six-way valve switches, and starts peristaltic pump B, aqueous slkali displacement six is logical all the way for peristaltic pump B drivings
Sample solution in valve quantitative loop, then cross the sample cavity flowed into after mixing in membrane diffusion unit with another way aqueous slkali
It is interior, and it is ammonia to be completed in membrane diffusion unit by mineralized nitrogen, ammonia is diffused into through hydrophobic membrane in acceptable solution cavity and quilt
Acceptable solution, which receives, changes into ammonium ion, and the mixed liquor in sample cavity after diffusion is discharged to mixed liquor by sample cavity again and given up
In liquid bottle, peristaltic pump B is closed;
3) detect:Six-way valve switches to dress sample state again, restarts peristaltic pump A, and ammonia has been dissolved in peristaltic pump A drivings
Acceptable solution flow through electric conductivity detector device, finally flow into acceptable solution waste liquid bottle in, electric conductivity detector device passes through solution conductivity
Rate change directly determines ammonia-nitrogen content, and will check that data are shown on a display screen;
Wherein, the entrance of the sample cavity in membrane diffusion unit mixes higher than outlet, hydrophobic membrane with the sample below hydrophobic membrane
Liquid is closed not contact.Sample solution in the basic conditions, when flowing through the sample cavity of membrane diffusion unit, does not contact diaphragm, ammonia expands
Acceptable solution is dissipated to, acceptable solution is now in " arrheaing " or " flowing " state by software control, and not only detection range is wide, and improves
The test limit of ammonia nitrogen;Diaphragm service life length simultaneously, it is often more important that other ions may when eliminating sample contact diaphragm
" seepage " causes the false positive interference that conductance increases.When so-called " arrheaing " dialysis is sample solution flowing, acceptable solution is static;
So-called " flowing " dialysis is that acceptable solution is flowing, particularly, sample solution in sample cavity alkali mixed liquor and acceptable solution cavity
Flow velocity should be greater than receiving flow velocity.
Further, in order to preferably realize that sample solution does not contact with hydrophobic membrane, prevent other ions from passing through hydrophobic membrane
It is diffused into acceptable solution, sample cavity entrance and the line of outlet have the downward inclination angle of 2-20 ° of level with plane where hydrophobic membrane.
Further, in order to reach preferably test effect and the degree of accuracy, acceptable solution is deionized water or concentration is
0.001-0.005mol/L hydrochloric acid solution, aqueous slkali are the sodium hydroxide solution that concentration is 0.5-1mol/L.
Further, in order that test environment is gentle, test scope is extensive, and the temperature in the membrane diffusion unit of this programme is
20-40℃。
It is direct based on non-contact membrane diffusion+conductivity variations present solution provides under a kind of constant temperature for not surpassing 40 DEG C
Test sample ammonia nitrogen in solution method.Testing conditions are gentle, without distillation, titration or colour developing, without making for poisonous and harmful reagent
With with discharge, using the teaching of the invention it is possible to provide preferably analyze security.Can be dense directly to determine height in more complicated matrix waste water in 5min
The ammonia nitrogen of degree, it is easy to use and reliable.Sample solution in the basic conditions, when diffusion unit sample solution cavity is flowed through under normal temperature,
Diaphragm is not contacted, ammonia diffuses to acceptable solution, and acceptable solution is now in " arrheaing " or " flowing " state by software control, not only examined
It is wide to survey scope, and improves the test limit of ammonia nitrogen;Diaphragm service life length simultaneously, it is often more important that eliminate sample contact membranes
Other ions possible " seepage " cause the false positive interference that conductance increases during piece.
Wherein, test platform of the present invention also includes:Experimental rig is designed, designed by analytical instrument factory of Taizhou City Jiangyan City (ginger
Analytical instrument factory of weir city) manufacture;Peristaltic pump BT100N, Baoding Shen Chenbeng industry Co., Ltd product.Ultra-pure water:Mill-Q ultra-pure waters
Machine, MILLIPORE companies of the U.S. (existing German Merck-Millipore companies).
The present invention has the advantages that compared with prior art:
1. selectivity of the invention is high, hydrophobic membrane is non-contact with sample, and not only diaphragm service life is grown, it is often more important that eliminates
Sample contact diaphragm other ions may " seepage " cause the false positive interference that conductance increases;
2. the present invention is environment-friendly, testing conditions are gentle, without distillation, titration or colour developing, without poisonous and harmful reagent
Using with discharge, using the teaching of the invention it is possible to provide preferably analyze security.
3. detection range of the present invention is wide, arrheaed by software exchange acceptable solution and flow combination, by receiving solution conductivity
The change of rate, can be directly to determine the ammonia nitrogen of high-concentration and low-concentration in more complicated matrix waste water in 5min.
Brief description of the drawings
Fig. 1 is that sample fills sample and stream purification process schematic diagram;
Fig. 2 is the ammonia nitrogen overhaul flow chart after six-way valve switching;
Fig. 3 is membrane diffusion cellular construction side view;
Fig. 4 is membrane diffusion unit front view.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
Present embodiment discloses a kind of method of non-contact gas membrane diffusion-Conductivity detection ammonia nitrogen in waste water, oozed using " arrheaing "
Analysis pattern, including following operating procedure:As shown in Figure 1,3, peristaltic pump A 1) is opened, the sample solution 2 containing ammonia nitrogen is through sample cell
Road flows into sample by the quantitative loop 4 that is connected with six-way valve 5 of peristaltic pump A suctions, filling excessive sample solution 2 after quantitative loop and given up
In liquid bottle 21;Meanwhile the hydrochloric acid solution 1 that concentration is 0.005mol/L drives and drawn suction by peristaltic pump A, through acceptable solution pipeline successively
The acceptable solution cavity 7.1 and electric conductivity detector device 6 in purifier 8, membrane diffusion unit 7 are flowed through, is come out from conductive detection device 6
Hydrochloric acid acceptable solution afterwards is flowed into acceptable solution waste liquid bottle 11;After continuous service 1 minute, peristaltic pump A is closed;
2) non-contact gas membrane diffusion:Six-way valve 5 switches, and as shown in Figure 2,3, starts peristaltic pump B, peristaltic pump B driving concentration
For 0.5mol/L sodium hydroxide solution 3, sodium hydroxide solution 3 divides for two-way, replaces the sample solution in quantitative loop 4 all the way,
Then cross and mix in mixing tube 9 with another way, then mixed liquor is flowed into the sample cavity 7.3 in membrane diffusion unit 7, and
It is ammonia to be completed in membrane diffusion unit 7 by mineralized nitrogen, and the constant temperature in membrane diffusion unit 7 is 20 DEG C, and ammonia is through thin
Moisture film 7.2, which is diffused into acceptable solution cavity 7.1 and received by acceptable solution, changes into ammonium ion, by diffusion in sample cavity 7.3
Mixed liquor afterwards is discharged in mixed liquor waste liquid bottle 31 by sample cavity 7.3 again, closes peristaltic pump B;
3) detect:Six-way valve 5 switches to dress sample state again, restarts peristaltic pump A, and ammonia has been dissolved in peristaltic pump A drivings
The acceptable solution 1 of gas flows through electric conductivity detector device 6, finally flows into acceptable solution waste liquid bottle 11, electric conductivity detector device 6 is by molten
Liquid conductivity variations directly determine ammonia-nitrogen content, and will check that data are shown on a display screen;
Wherein, the entrance of the sample cavity in membrane diffusion unit is higher than outlet, hydrophobic membrane 7.2 and the lower section of hydrophobic membrane 7.2
Sample mixed liquor does not contact, as shown in Figure 3;The entrance of sample cavity 7.3 and the line of outlet have 2 ° with the place plane of hydrophobic membrane 7.2
Horizontal downward inclination angle.
Embodiment 2
Present embodiment discloses a kind of method of non-contact gas membrane diffusion-Conductivity detection ammonia nitrogen in waste water, oozed using " flowing "
Analysis pattern, including following operating procedure:1) peristaltic pump A is opened, the sample solution 2 containing ammonia nitrogen is through sample pipe by peristaltic pump A
Suck in the quantitative loop 4 that is connected with six-way valve 5, fill excessive sample solution 2 after quantitative loop and flow into sample waste bottle 21;Together
When, concentration is that 0.001mol/L hydrochloric acid solution 1 drives and drawn suction by peristaltic pump A, and purifier is flowed through successively through acceptable solution pipeline
8th, the acceptable solution cavity 7.1 and electric conductivity detector device 6 in membrane diffusion unit 7, from conductive detection device 6 come out after hydrochloric acid connect
Entered by liquid stream in acceptable solution waste liquid bottle 11;After continuous service 1 minute, peristaltic pump A, which drives, inhales hydrochloric acid solution 1 to be slower than in peristaltic pump B
The speed of sample and aqueous slkali mixed liquor is run, and the flow velocity of wherein sample solution 2 is twice of hydrochloric acid solution 1;Sample solution 2
Flow velocity 2mL/min, the flow velocity of hydrochloric acid solution 1 is 1mL/min.
2) non-contact gas membrane diffusion:The sodium hydroxide solution 3 that peristaltic pump B driving concentration is 1mol/L, sodium hydroxide solution 3
It is divided into two-way, replaces the sample solution in quantitative loop 4 all the way, then cross and mix in mixing tube 9 with another way, then mix
Liquid stream enters in the sample cavity 7.3 in membrane diffusion unit 7, and it is ammonia to be completed in membrane diffusion unit 7 by mineralized nitrogen, and film expands
Constant temperature in throwaway member 7 is 40 DEG C, and ammonia is diffused into acceptable solution cavity 7.1 through hydrophobic membrane 7.2 and connect by acceptable solution 1
Receipts change into ammonium ion, and the interior mixed liquor after diffusion of sample cavity 7.3 is discharged to mixed liquor waste liquid by sample cavity 7.3 again
In bottle 31;
3) detect:Peristaltic pump A drives suction hydrochloric acid solution 1 and run with being slower than the speed of sample solution 2 in peristaltic pump B, and sample is molten
The flow velocity 2mL/min of liquid 2, the flow velocity of hydrochloric acid solution 1 is 1mL/min, and the acceptable solution 1 that ammonia has been dissolved in peristaltic pump A drivings flows through
Electric conductivity detector device 6, finally flow into acceptable solution waste liquid bottle 11, electric conductivity detector device 6 is changed straight by electrical conductivity of solution
Connect and determine ammonia-nitrogen content, and will check that data are shown on a display screen;
Wherein, the entrance of the sample cavity 7.3 in membrane diffusion unit 7, which is higher than, exports, under hydrophobic membrane 7.2 and hydrophobic membrane 7.2
The sample mixed liquor of side does not contact.Sample cavity entrance and line and the place plane of hydrophobic membrane 7.2 of outlet have 20 degree of levels to
Under inclination angle.
Embodiment 3
Sewage disposal is reclaimed in spinning:Quantitative loop is 100 μ L, sample solution flow velocity 1.5mL/min;Acceptable solution ---
0.005mol/L hydrochloric acid, flow velocity 0.8mL/min, aqueous slkali --- 0.5mol/L sodium hydroxides, flow velocity 1.0mL/min, purifier
For cation exchange resin column.38 DEG C of constant temperature, air film diffusion unit (the snakelike diffusion cell of runner symmetrical above and below, hydrophobic membrane φ 35mm,
Diffusion path about 25mm), the outlet of sample solution inlet ratio is slightly higher, and gradient is 15 °.Start control program, analyzed automatically,
Automatic to calculate display, it is 13.82mg/L to measure spinning recovery sewage ammonia nitrogen.
Embodiment 4
Refine oil peace and quiet lower water:Quantitative loop is 200 μ L, sample solution flow velocity 1.5mL/min;Acceptable solution --- deionized water,
Flow velocity 0.8mL/min, aqueous slkali --- 0.5mol/L sodium hydroxides, flow velocity 1.0mL/min, purifier is cationic ion-exchange resin
Post.33 DEG C of constant temperature, air film diffusion unit (the snakelike diffusion cell of runner symmetrical above and below, hydrophobic membrane φ 35mm, diffusion path about 25mm).
The outlet of sample solution inlet ratio is slightly higher, and gradient is 5 °.Start control program, analyzed automatically, it is automatic to calculate display, measure
It is 0.02mg/L to refine oil peace and quiet lower water ammonia nitrogen.
Embodiment 5
Cover circulating water treatment:Quantitative loop is 100 μ L, sample solution flow velocity 1.5mL/min;Acceptable solution --- deionized water,
Flow velocity 0.8mL/min, aqueous slkali --- 0.7mol/L sodium hydroxides, flow velocity 1.0mL/min, purifier is anion suppressor.
36 DEG C of constant temperature, air film diffusion unit (the snakelike diffusion cell of runner symmetrical above and below, hydrophobic membrane φ 35mm, diffusion path about 25mm).Sample
Product solution inlet is more slightly higher than exporting, and gradient is 20 °.Start control program, analyzed automatically, it is automatic to calculate display, measure
It is 2.12mg/L to cover recirculated water ammonia nitrogen
Embodiment 6
Biochemistry pool is intake:Quantitative loop is 100 μ L, sample solution flow velocity 1.5mL/min;Acceptable solution --- 0.002mol/L salt
Acid, flow velocity 0.8mL/min, aqueous slkali --- 0.9mol/L sodium hydroxides, flow velocity 1.0mL/min, purifier suppress for anion
Device.25 DEG C of constant temperature, air film diffusion unit (the snakelike diffusion cell of runner symmetrical above and below, hydrophobic membrane φ 35mm, diffusion path about 25mm).
The outlet of sample solution inlet ratio is slightly higher, and gradient is 2 °.Start control program, analyzed automatically, it is automatic to calculate display, measure
Biochemistry pool influent ammonia nitrogen is 42.1mg/L.
Embodiment 7
Chemical fertilizer always arranges saliva processing:Quantitative loop is 100 μ L, sample solution flow velocity 1.5mL/min;Acceptable solution ---
0.001mol/L hydrochloric acid, flow velocity 0.8mL/min, aqueous slkali --- 0.6mol/L sodium hydroxides, flow velocity 1.0mL/min, purifier
For cation exchange resin column.35 DEG C of constant temperature, air film diffusion unit (the snakelike diffusion cell of runner symmetrical above and below, hydrophobic membrane φ 35mm,
Diffusion path about 25mm).The outlet of sample solution inlet ratio is slightly higher, and gradient is 12 °.Start control program, analyzed automatically,
Automatic to calculate display, it is 2.13mg/L to measure sewage disposal and always discharge saliva ammonia nitrogen.
Embodiment 8
Saliferous clarifies pool water treatment:Quantitative loop is 100 μ L, sample solution flow velocity 1.5mL/min;Acceptable solution ---
0.001mol/L hydrochloric acid, flow velocity 0.8mL/min, aqueous slkali --- 0.9mol/L sodium hydroxides, flow velocity 1.0mL/min, purifier
For anion suppressor.30 DEG C of constant temperature, air film diffusion unit (the snakelike diffusion cell of runner symmetrical above and below, hydrophobic membrane φ 35mm, diffusion
Path about 25mm).The outlet of sample solution inlet ratio is slightly higher, and gradient is 17 °.Start control program, analyzed automatically, automatically
Display is calculated, it is 42.1mg/L to measure sewage disposal and always discharge saliva ammonia nitrogen.
Claims (5)
1. a kind of method that non-contact gas membrane diffusion-conductance directly detects ammonia nitrogen in waste water, it is characterised in that including following operation step
Suddenly:
1) topping up and cleaning:Peristaltic pump A is opened, sample solution is determined through sample pipe by what peristaltic pump A suctions were connected with six-way valve
Measure in ring, fill excessive sample solution flow after quantitative loop and enter in sample waste liquid bottle;Meanwhile acceptable solution by peristaltic pump A driving and
Draw and inhale, the acceptable solution cavity and electric conductivity detector device in purifier, membrane diffusion unit are flowed through successively through acceptable solution pipeline, from electricity
The acceptable solution after detection means comes out is led to flow into acceptable solution waste liquid bottle;Continuous service for a period of time after, close peristaltic pump A;
2) non-contact gas membrane diffusion:Six-way valve switches, and starts peristaltic pump B, aqueous slkali displacement six-way valve is determined all the way for peristaltic pump B drivings
The sample solution in ring is measured, then crosses with another way aqueous slkali and is flowed into after mixing in the sample cavity in membrane diffusion unit, sample
Product solution and diaphragm are non-contact, and it is ammonia to be completed in membrane diffusion unit by mineralized nitrogen, and ammonia is diffused into through hydrophobic membrane
Received in acceptable solution cavity and by acceptable solution and change into ammonium ion, the mixed liquor in sample cavity after diffusion is again by sample cavity
Road is discharged in mixed liquor waste liquid bottle, closes peristaltic pump B;
3) detect:Six-way valve switches to dress sample state again, restarts peristaltic pump A, and connecing for ammonia has been dissolved in peristaltic pump A drivings
By liquid stream through electric conductivity detector device, finally flow into acceptable solution waste liquid bottle, electric conductivity detector device is become by electrical conductivity of solution
Change directly determines ammonia-nitrogen content, and will check that data are shown on a display screen;
Wherein, the entrance of the sample cavity in the membrane diffusion unit mixes higher than outlet, hydrophobic membrane with the sample below hydrophobic membrane
Liquid is closed not contact.
2. the method that non-contact gas membrane diffusion-conductance as claimed in claim 1 directly detects ammonia nitrogen in waste water, it is characterised in that
Step 1), 2) and 3) in membrane diffusion unit be in " flowing " or " arrheaing " two kinds of dialysis patterns, when membrane diffusion unit is in " flowing
It is dynamic " dialysis pattern when, the flow velocity of the sample solution is more than the flow velocity of acceptable solution.
3. the method that non-contact gas membrane diffusion-conductance as claimed in claim 1 directly detects ammonia nitrogen in waste water, it is characterised in that
The entrance of sample cavity and the line of outlet have the downward inclination angle of 2-20 ° of level with plane where hydrophobic membrane.
4. the method that non-contact gas membrane diffusion-conductance as claimed in claim 1 directly detects ammonia nitrogen in waste water, it is characterised in that
The hydrochloric acid solution that the acceptable solution is deionized water or concentration is 0.001-0.005mol/L, the aqueous slkali are that concentration is 0.5-
1mol/L sodium hydroxide solution.
5. the method that non-contact gas membrane diffusion-conductance as claimed in claim 1 directly detects ammonia nitrogen in waste water, it is characterised in that
Temperature in the membrane diffusion unit is 20-40 DEG C.
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Application publication date: 20171110 |