CN103245697A - Ammonia nitrogen on-line monitoring instrument - Google Patents
Ammonia nitrogen on-line monitoring instrument Download PDFInfo
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- CN103245697A CN103245697A CN2013101394947A CN201310139494A CN103245697A CN 103245697 A CN103245697 A CN 103245697A CN 2013101394947 A CN2013101394947 A CN 2013101394947A CN 201310139494 A CN201310139494 A CN 201310139494A CN 103245697 A CN103245697 A CN 103245697A
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Abstract
The invention discloses an ammonia nitrogen on-line monitoring instrument. The ammonia nitrogen on-line monitoring instrument consists of a sample feeding tube, a sample feeding peristaltic pump, a distillation heating bottle, an alkali liquid sample feeding peristaltic pump, a cleaning peristaltic pump, an air pump, a cooling tube, an absorption bottle, a boric acid absorption liquid sample feeding peristaltic pump and a communication pipeline. According to the ammonia nitrogen on-line monitoring instrument, a conduction measuring method for testing ammonia nitrogen, namely a wet process distillation-conductance method, is established. Comparing an analysis result of standard samples, various kinds of surface water and wastewater with a synchronously-adopted national standard analysis result, various technical requirements of monitoring technology standard are met, so that the instrument is easy to operate, time-saving, labor-saving, efficient and correct; the experiment cost is also reduced; and the instrument is suitable for popularization and application of ammonia nitrogen during on-line monitoring.
Description
Technical field
The present invention relates to a kind of ammonia nitrogen on-line monitoring instrument, belong to the on-line monitoring technique field of ammonia-nitrogen content in the water body, be specifically related to a kind of instrument that can be used for ammonia-nitrogen content on-line monitoring in surface water, sewage treatment plant, the industrial pollution source.
Background technology
Ammonia nitrogen concentration is important pollutant index in the water bodys such as surface water, sewage.The analytical approach that common ammonia nitrogen on-line monitoring instrument adopts on the home market mainly contains at present: 1, nessler reagent photometry; 2, salicylic acid hypochlorite photometry; 3, gas-sensing membrane electrode method etc.
Domestic manufacturer adopts photometry more, and the pre-treatment of measurement has only steps such as simple filtering, flocculation.But organic compounds such as the fatty amine in the waste water, aromatic amine, aldehydes, acetone, alcohols and organochlorine amine, and inorganic ions such as iron, manganese, magnesium and sulphur, because producing the heterochromatic or muddy interference that causes, so adopt the Spectrophotometry for Determination of simple pre-treatment regularly to be subject to the interference of suspension and coloring matter in the water.The instrument of these two kinds of methods has a common problem, be exactly in the process of using, because the mensuration curve in stability, the stability of measurement light source and the influence factors such as cleanliness of cuvette of developer, instrument all needs often to proofread and correct, otherwise easily causes measuring error.
Adopt the apparatus structure of gas-sensing membrane electrode method simple, convenient operating maintenance, be applicable to the mensuration of surface water and the Sewage Plant waste discharge of cleaning.Because air-sensitive film easily stain, if water sample, is directly used in the mensuration of ammonia nitrogen in the surface water of sewage or heavy contamination without pre-service, also have any problem.Owing to the signal drift of ammonia nitrogen electrode and the influence of cleaning method, the built-in measurement curve of instrument also needs often to revise simultaneously.In addition, because of the reason of technology and technology, the level of homemade electrode is not as good as external like product, and state's external electrode price is higher.
This several method measurement result and national standard method are compared, as when running into complicated wastewater sample, measurement result is inaccurate, often exceeds error range.
Summary of the invention
The invention provides a kind of simple to operate, and save time, laborsaving, the suit ammonia nitrogen on-line monitoring instrument in the on-line monitoring of ammonia nitrogen, promoted the use of efficiently, accurately.
For achieving the above object, the technical solution used in the present invention is: a kind of ammonia nitrogen on-line monitoring instrument,
One sample introduction pipe, this sample introduction pipe has an injection port and an outlet;
One sample sample introduction peristaltic pump, the outlet of the import of this sample feeding peristaltic pump and described sample introduction pipe is tightly connected, and described sample feeding wriggling delivery side of pump is communicated with a sample quantity tube;
One distillation heating bottle, the outlet of described sample quantity tube is positioned at described distillation heating bottle; Wherein, sealing is provided with heating arrangement in the described distillation heating bottle;
One alkali lye sample introduction peristaltic pump, this alkali lye sample introduction peristaltic pump is communicated with an alkali lye bottle by pipeline with described distillation heating bottle;
One cleans peristaltic pump, and this cleans peristaltic pump and by pipeline one cleaning fluid storage bottle is communicated with described distillation heating bottle;
One air pump, the gas outlet of this air pump connects a tracheae, and the gas outlet of this tracheae is positioned at the bottom of described distillation heating bottle;
One cooling tube, the air intake opening of this cooling tube is communicated with the top seal of described distillation heating bottle;
One absorption bottle, the middle part of this absorption bottle or bottom are communicated with the liquid outlet sealing of described cooling tube; Wherein, be provided with a conductance electrode and a temperature measurement probe in the described absorption bottle;
One boric acid absorption liquid sample introduction peristaltic pump, the import of this boric acid absorption liquid peristaltic pump is communicated with a boric acid absorption liquid storage bottle, described boric acid absorption liquid wriggling delivery side of pump is communicated with a boric acid absorption liquid quantity tube, and the liquid outlet of this boric acid absorption liquid quantity tube is communicated with described absorption bottle.
Related content in the technique scheme is explained as follows:
1, in the such scheme, described cooling tube is the spiral pipe of a band cyclic water jacket.
2, in the such scheme, described distillation heating bottle, cooling tube and absorption bottle are formed in one.
3, in the such scheme, described cooling tube is ball condenser or spirality refrigeratory.
4, in the such scheme, described heating arrangement is one to place the heater element in the sealed tube.
Because technique scheme is used, the present invention compared with prior art has following advantage:
Because the present invention has set up a kind of method for measuring conductance of measuring ammonia nitrogen: wet method distillation---conductance method.By the analysis result of standard model, all kinds of surface water and waste water is compared with adopting the National Standard Method analysis result synchronously, the present invention meets every technical requirement of monitoring technology standard, not only simple to operate, and save time, laborsaving, efficient, accurate, also reduced experimental cost, suited in the on-line monitoring of ammonia nitrogen, to promote the use of.
Description of drawings
Accompanying drawing 1 is synoptic diagram of the present invention;
Accompanying drawing 2 distills heating bottle and miscellaneous part connection diagram for the present invention.
In the above accompanying drawing: 1, clean peristaltic pump; 2, sample introduction pipe; 3, sample feeding peristaltic pump; 4, distillation heating bottle; 5, heating arrangement; 6, tracheae; 7, air pump; 9, cooling tube; 10, alkali lye sample introduction peristaltic pump; 11, boric acid absorption liquid sample introduction peristaltic pump; 12, temperature measurement probe; 13, conductance electrode; 15, absorption bottle; 16, first solenoid valve; 17, alkali lye bottle; 18, boric acid absorption liquid storage bottle; 19, waste collection bottle; 20, cleaning fluid storage bottle; 21, second solenoid valve; 22, thin glass tube; 23, sample quantity tube; 25, sealed tube; 26, the fluid portion of cooling tube.
Embodiment
Below in conjunction with drawings and Examples the present invention is further described:
Embodiment one: a kind of ammonia nitrogen on-line monitoring instrument
Shown in accompanying drawing 1 and accompanying drawing 2, a kind of ammonia nitrogen on-line monitoring instrument,
One sample introduction pipe 2, this sample introduction pipe 2 has an injection port and an outlet;
One sample sample introduction peristaltic pump 3, the outlet of the import of this sample feeding peristaltic pump 3 and described sample introduction pipe 2 is tightly connected, and the outlet of described sample feeding peristaltic pump 3 is communicated with a sample quantity tube 23;
One distillation heating bottle 4, the outlet of described sample quantity tube 23 is positioned at described distillation heating bottle 4; Wherein, sealing is provided with heating arrangement 5 in the described distillation heating bottle 4;
One alkali lye sample introduction peristaltic pump 10, this alkali lye sample introduction peristaltic pump 10 is communicated with an alkali lye bottle 17 by pipeline with described distillation heating bottle 4;
One cleans peristaltic pump 1, and this cleans peristaltic pump 1 and by pipeline one cleaning fluid storage bottle 20 is communicated with described distillation heating bottle 4;
One air pump 7, the gas outlet of this air pump 7 connect a tracheae 6, and the gas outlet of this tracheae 6 is positioned at the bottom of described distillation heating bottle 4;
One cooling tube 9, the air intake opening of this cooling tube 9 is communicated with the top seal of described distillation heating bottle 4;
One absorption bottle 17, the bottom of this absorption bottle 17 is communicated with the liquid outlet sealing of described cooling tube 9; Wherein, be provided with a conductance electrode 13 and a temperature measurement probe 12 (temperature sensor) in the described absorption bottle 17;
One boric acid absorption liquid sample introduction peristaltic pump 11, the import of this boric acid absorption liquid peristaltic pump 11 is communicated with a boric acid absorption liquid storage bottle 18, the outlet of described boric acid absorption liquid peristaltic pump 11 is communicated with a boric acid absorption liquid quantity tube (not shown), and the liquid outlet of this boric acid absorption liquid quantity tube (not shown) is communicated with described absorption bottle 17.Described cooling tube 17 is the spiral pipe of a band cyclic water jacket.Described distillation heating bottle 4, cooling tube 9 and absorption bottle 15 are formed in one.Described cooling tube 9 can also be ball condenser or spirality refrigeratory.Described heating arrangement 4 is one to place the heating rod in the sealed tube 25.
A kind of its ingredient of ammonia nitrogen on-line monitoring instrument comprises the microcomputerized control part; The ammonia nitrogen that is made of distillation heating bottle 4, heating arrangement 5, cooling tube 9, blowning installation and absorption bottle 15 etc. distills and absorption portion; The conductance measurement part; Sample quantitative sample injection part; Distillation heating bottle 4 cleaning parts; NaOH quantitative sample injection part; Boric acid absorption liquid quantitative sample injection part etc.
Sample quantitative sample injection part is made up of the glass sample quantity tube 23 in sample feeding peristaltic pump 3, the flexible pipe that is connected to distillation heating bottle 4 and the distillation heating bottle 4, and the quantitative volume of sample is 100ml.Sample feeding peristaltic pump 3 is just changeing earlier certain hour during sample introduction, guarantees that sampling volume is greater than 100ml; Sample feeding peristaltic pump 3 counter-rotating certain hour to sample introduction Guan Zhongwu solution flow out then, and this moment, quantitatively volume was required sample size.This process drives sample feeding peristaltic pump 3 controllers by micro computer and finishes.
NaOH quantitative sample injection part is made of sample introduction alkali lye sample introduction peristaltic pump 10, the flexible pipe that is connected to distillation heating bottle 4, the alkali lye bottle 17 that fixed concentration is housed.Drive alkali lye sample introduction peristaltic pump 10 by micro computer and finish the quantitative liquid feeding process.The used peristaltic pump of this instrument is the constant rotational speed peristaltic pump.Actual when making sample, peristaltic pump rotates a set time, adds a certain amount of alkali lye, uses PH＞9 of water sample, and water sample is alkalescence.
Heating arrangement 5 places in the sealed tube 25 of one section sealing, sealed tube 25 and distillation heating bottle 4 sealed attachment.
The part of blowing is made up of the adjustable air pump 7 of a tolerance, the flexible pipe that is connected to distillation heating bottle 4, and the coupling part of the flexible pipe of the tracheae 6 of distillation heating bottle 4 has a thin glass tube 22 to be inserted to apart from distilling heating bottle place, 4 end 1/3.
Cooling segment cooling tube 9 is the spiral pipe of a band cyclic water jacket.The latter end of spiral pipe is connected to the fluid portion 26 of the cooling tube of absorption bottle 15.
Boric acid absorption liquid quantitative sample injection part by boric acid absorption liquid sample introduction peristaltic pump 11, be equipped with absorption liquid, boric acid absorption liquid storage bottle 18 is connected to the flexible pipe of absorption bottle 15 and the glass quantity tube in the absorption bottle is formed, the quantitative volume of sample is 20ml.Boric acid absorption liquid sample introduction peristaltic pump 11 first main story certain hours during liquid feeding guarantee that sampling volume is greater than 50ml; Boric acid absorption liquid sample introduction peristaltic pump 11 counter-rotating certain hour to sample introduction Guan Zhongwu solution flow out then, and quantitative volume was and namely needed sample size this moment.This process drives the peristaltic pump controller by micro computer and finishes.
Conductance electrode 13 is inserted to the bottom of absorption bottle 15 from the top of absorption bottle 15, will guarantee in the measuring process that absorption liquid is higher than the measuring section of conductance electrode 13.Conductance electrode 13 and electric waveguide measuring circuit constitute the conductance measurement part.For guaranteeing the accuracy of conductance measurement, also have a temperature measurement probe 14 in the absorption bottle 15 simultaneously, be used for measuring the temperature of absorption liquid.
As shown in Figure 1, this ammonia nitrogen on-line monitoring instrument is mainly become by sample feeding peristaltic pump 3, alkali lye sample introduction peristaltic pump 10, distillation heating bottle 4, heating arrangement 5, air pump 7, cleaning wriggling 1, cooling tube 9, absorption bottle 15, boric acid absorption liquid sample introduction peristaltic pump 11, conductance electrode 13 and measurement module, temperature measurement probe 12 and measurement module, peristaltic pump tube and other hose set.
When ammonia nitrogen on-line monitoring instrument was started working, first solenoid valve 16 of absorption bottle 15 belows was opened a period of time, and the boric acid absorption liquid in the absorption bottle 15 is drained.3 forward rotation a period of times of sample feeding peristaltic pump, draw sample by sample introduction pipe 2, backward rotation a period of time drains the sample in the sample introduction pipe 2 then.Boric acid absorption liquid sample introduction peristaltic pump 11 forward rotation certain hours are drawn the boric acid absorption liquid, and backward rotation a period of time drains absorption liquid in the sample introduction pipe then.Alkali lye sample introduction peristaltic pump 10 is opened and is drawn alkali lye after a period of time, opens heating arrangement 5 heating and air pump 7 air-blowing simultaneously, and air-flow flows out from the bottom of distillation heating bottle 4 in the air pump tracheae 6, stirs sample solution.The sample of distillation in the heating bottle 4 becomes warm to boiling by cold, and the sample gas that distill out this moment enters absorption bottle 15 after cooling tube 9 coolings; Conductance measurement is partly measured the changing value of conductivity, when the changing value that electricity is led reaches maximal value, stops heating, or is heated to the stipulated time and stops.Instrument is preserved the maximum changing value of conductivity, and this value is calculated with value as later measurement.After stopping to heat a period of time, open second solenoid valve, the 21 emptying vinasses of distillation heating bottle 4 belows earlier to waste collection bottle 19, and then first solenoid valve, the 16 emptying absorption liquids of opening absorption bottle 15 belows are to waste collection bottle 19.Rotate and clean 1 a period of time of peristaltic pump, draw cleaning fluid, open distillation heating bottle 4 belows second solenoid valve 21 after several minutes again, the emptying cleaning fluid is closed air pump 7 simultaneously to waste collection bottle 19.Boric acid absorption liquid sample introduction peristaltic pump 11 forward rotation certain hours are drawn the boric acid absorption liquid, and backward rotation a period of time drains absorption liquid in the sample introduction pipe then.So far whole measuring process finishes.
Before instrument dispatches from the factory, need with multiple standards standardization of solution apparatus measures curve.Measure every some its maximum conductance changing value that comprises sample concentration and measurement in the curve.The correlativity of measuring curve should be greater than 0.999.During the actual measurement sample, only need record its electricity leads the variation maximal value, just can try to achieve the concentration value of sample according to measuring curve.
The built-in measurement curve of instrument can arrange many according to the concentration range of measuring sample, the demarcation condition difference of every curve correspondence, and difference is in the concentration of absorption liquid different with volume.When measuring low concentration, the concentration of absorption liquid is low or volume is little; When measuring enriched sample, concentration height or the volume of absorption liquid are many.Under the overwhelming majority situation, the concentration that only needs to change absorption liquid gets final product.Absorption liquid is the BAS of low concentration, and is highly stable, places that its conductivity can not change after 6 months; Conductance electrode also is very stable a kind of electrode simultaneously.Thereby instrument does not need to demarcate or proofread and correct in the use several months substantially.Improve operability and the maintainability of instrument greatly.
Ammonia nitrogen on-line monitoring instrument experimental technique:
1, low concentration is measured curve method for building up and standard specimen mensuration:
Measuring condition: tolerance: 50ml/min.
Sample volume: 100ml.
Alkali addition: 5ml (1mol/l NaOH).
Heat time heating time: 20 minutes.
Cool time: 5 minutes.
Absorption liquid volume, concentration: 20ml4g/l (boric acid)
1.1 the precision of blank solution signal value conductivity
The precision (table 1) of blank solution distillation back absorption liquid conductivity variations value
As shown in Table 1, the relative standard deviation of blank solution signal changing value is 0, and it is better to show that blank sample distillation back absorption liquid electricity is led the consistance of changing value.
1.2 the correlativity of different ammonia nitrogen concentrations and signal value conductivity
With ammonium chloride preparation variable concentrations ammonia nitrogen standard solution, investigate it and the linear relationship of signal value, and set up instrument low concentration measurement calibration curve.The results are shown in Table 2.
The relation (table 2) of ammonia nitrogen titer and conductivity signal changing value
Ammonia nitrogen concentration value (C) in the table 2 and respective signal changing value (p) are returned:
Linearity of regression equation 1 C1=16.518p1-6.736 r=0.9999 linear relationship is good.Show that under this experiment condition the sample concentration value of measurement is available to 10mg/L regression equation linearity from 0.5mg/L.
1.3 the measurement result of environmental standard sample: (precision and accuracy)
With this method the environmental standard sample is measured, all in the guarantee value scope, relative deviation＜5% meets the requirement of environmental monitoring and analysis method to its measured value.
Under identical experiment condition, adopt the linear equation 1 with table 5, measure the result of environmental standard sample:
Environmental standard sample determination precision and error (table 3)
1.4 adopt the actual water sample recovery of standard addition of this method, data see Table 4.
Actual water sample recovery of standard addition (table 4)
Table 4 as seen, the relative standard deviation that standard model is measured is that method precision is better between 3.15% to 0.0%.All in the scope of set-point, the method accuracy is better for the measured value of standard sample.
2, high concentration is measured curve method for building up and standard specimen mensuration:
Measuring condition: tolerance: 50ml/min
Sample volume: 100ml
Alkali addition: 5ml (1mol/lNaOH)
Heat time heating time: 20 minute cool time: 5 minutes
Absorption liquid volume, concentration: 20ml20g/l (boric acid)
2.1 the precision of blank solution signal value conductivity
The precision (table 5) of blank solution distillation back absorption liquid conductivity variations value
As shown in Table 5, the relative standard deviation of blank solution signal changing value is 0, and it is better to show that blank sample distillation back absorption liquid electricity is led the consistance of changing value.
2.2 the correlativity of different ammonia nitrogen concentrations and signal value conductivity
With ammonium chloride preparation variable concentrations ammonia nitrogen standard solution, investigate it and the linear relationship of signal value, and set up instrument low concentration measurement calibration curve.The results are shown in Table 6.
The relation (table 6) of ammonia nitrogen titer and conductivity signal changing value
Ammonia nitrogen concentration value (C) in the table 6 and respective signal changing value (p) are returned:
Linearity of regression equation 2C2=14.210p2-4.134r=0.9998 linear relationship is good.Show that with this understanding in the 100mg/L scope, the regression equation linearity is available from 2mg/L for the sample concentration value of measurement.
2.3 the measurement result of environmental standard sample: (precision and accuracy)
With this method the environmental standard sample is measured, its measured value all definitely is being worth in the scope, and relative deviation＜5% meets the requirement of environmental monitoring and analysis method.
Under identical experiment condition, adopt the linear equation 2 with table 6, measure the result of environmental standard sample:
Environmental standard sample determination precision and error (table 7)
Table 7 as seen, the relative standard deviation that standard model is measured is that method precision is better between 1.36% to 0.43%.All in the scope of set-point, the method accuracy is better for the measured value of standard sample
2.4 adopt the actual water sample recovery of standard addition of this method, data see Table 8.
Actual water sample recovery of standard addition (table 8)
3 adopt the different industries actual water sample comparison of this method, and data see Table 9.
Actual water sample comparison result (table 9)
The result shows no significant difference between this method and the GB Na Shi method.
Above-described embodiment only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalences that spirit essence is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (5)
1. ammonia nitrogen on-line monitoring instrument is characterized in that comprising:
One sample introduction pipe (2), this sample introduction pipe (2) has an injection port and an outlet;
One sample sample introduction peristaltic pump (3), the outlet of the import of this sample feeding peristaltic pump (3) and described sample introduction pipe (2) is tightly connected, and the outlet of described sample feeding peristaltic pump (3) is communicated with a sample quantity tube (23);
One distillation heating bottle (4), the outlet of described sample quantity tube (23) is positioned at described distillation heating bottle (4); Wherein, sealing is provided with heating arrangement (5) in the described distillation heating bottle (4);
One alkali lye sample introduction peristaltic pump (10), this alkali lye sample introduction peristaltic pump (10) is communicated with an alkali lye bottle (17) by pipeline with described distillation heating bottle (4);
One cleans peristaltic pump (1), and this cleans peristaltic pump (1) and by pipeline one cleaning fluid storage bottle (20) is communicated with described distillation heating bottle (4);
One air pump (7), the gas outlet of this air pump (7) connects a tracheae (6), and the gas outlet of this tracheae (6) is positioned at the bottom of described distillation heating bottle (4);
One cooling tube (9), the air intake opening of this cooling tube (9) is communicated with the top seal of described distillation heating bottle (4);
One absorption bottle (15), the middle part of this absorption bottle (15) or bottom are communicated with the liquid outlet sealing of described cooling tube (9); Wherein, be provided with a conductance electrode (13) and a temperature measurement probe (12) in the described absorption bottle (15);
One boric acid absorption liquid sample introduction peristaltic pump (11), the import of this boric acid absorption liquid peristaltic pump (11) is communicated with a boric acid absorption liquid storage bottle (18), the outlet of described boric acid absorption liquid peristaltic pump (11) is communicated with a boric acid absorption liquid quantity tube, and the liquid outlet of this boric acid absorption liquid quantity tube is communicated with described absorption bottle (15).
2. ammonia nitrogen on-line monitoring instrument according to claim 1 is characterized in that: described cooling tube (9) is the spiral pipe of a band cyclic water jacket.
3. ammonia nitrogen on-line monitoring instrument according to claim 1, it is characterized in that: described distillation heating bottle (4), cooling tube (9) and absorption bottle (15) are formed in one.
4. ammonia nitrogen on-line monitoring instrument according to claim 1, it is characterized in that: described cooling tube (9) is ball condenser or spirality refrigeratory.
5. ammonia nitrogen on-line monitoring instrument according to claim 1 is characterized in that: described heating arrangement (5) is one to place the heating rod in the sealed tube.
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| CN105004761A (en) * | 2015-06-26 | 2015-10-28 | 华电电力科学研究院 | Denitration system escaping ammonia on-line continuous monitoring device and method |
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| CN108982597A (en) * | 2018-10-10 | 2018-12-11 | 浙江工业大学 | It is a kind of based on distillation-conductance method ammonia nitrogen water quality online automatic monitor and method |
| CN109382194A (en) * | 2018-11-30 | 2019-02-26 | 天津威特生物医药有限责任公司 | Thallus sample broke mechanism |
| CN110441469A (en) * | 2019-09-19 | 2019-11-12 | 威海长青海洋科技股份有限公司 | A kind of water body ammonia nitrogen detection kit and detection method |
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| CN108982597A (en) * | 2018-10-10 | 2018-12-11 | 浙江工业大学 | It is a kind of based on distillation-conductance method ammonia nitrogen water quality online automatic monitor and method |
| CN109382194A (en) * | 2018-11-30 | 2019-02-26 | 天津威特生物医药有限责任公司 | Thallus sample broke mechanism |
| CN110441469A (en) * | 2019-09-19 | 2019-11-12 | 威海长青海洋科技股份有限公司 | A kind of water body ammonia nitrogen detection kit and detection method |
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Application publication date: 20130814 |