CN102636446B - On-line detection device for detecting total nitrogen and total phosphorus through ozone ultraviolet collaborative oxidative digestion - Google Patents
On-line detection device for detecting total nitrogen and total phosphorus through ozone ultraviolet collaborative oxidative digestion Download PDFInfo
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- CN102636446B CN102636446B CN2012101415703A CN201210141570A CN102636446B CN 102636446 B CN102636446 B CN 102636446B CN 2012101415703 A CN2012101415703 A CN 2012101415703A CN 201210141570 A CN201210141570 A CN 201210141570A CN 102636446 B CN102636446 B CN 102636446B
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Abstract
The invention relates to an on-line detection device for detecting total nitrogen and total phosphorus through ozone ultraviolet collaborative oxidative digestion. The on-line detection device comprises a glass reaction pipe, wherein an ultraviolet lamp is suspended outside the glass reaction pipe. The on-line detection device is characterized in that the upper end of the glass reaction pipe is provided with a water sample inlet and a tail gas exhaust port; the water sample inlet is connected with a water sample storage tank; the bottom of the glass reaction pipe is provided with a discharge port; the discharge port is connected with two pipelines which are connected in parallel; the first pipeline is connected with an electrolysis process ozone generator; a gas output end of the electrolysis process ozone generator is provided with a needle type nozzle and a one-way valve; the second pipeline is connected with a first inlet end of a detection pond; a second inlet end of the detection pond is connected with a total phosphorous color developing agent supply tank; a first outlet end of the detection pond is connected with a spectrophotometer and a third injection pump; and a second outlet end of the detection pond is connected with a waste liquid barrel. According to the on-line detection device, both ozone and a water sample are irradiated by an ultraviolet lamp to perform oxidative digestion to produce hydroxyl free radicals, so that the situation of lose of a part of the hydroxyl free radicals is avoided.
Description
Technical field
The present invention relates to a kind of pick-up unit that detects online total nitrogen total phosphorus for water quality, especially a kind of ozone-ultraviolet synergistic oxidation is cleared up the on-line measuring device that detects total nitrogen total phosphorus.
Background technology
Lake, reservoir water body eutrophication are on the rise, and be closely related with the content of Water, phosphorus.The too high levels of Water, phosphorus, can cause the abnormal Growth and Reproduction of various hydrophyte, and extensive blue algae bloom event all once occurred on the ground such as Taihu Lake, Chaohu.
Present detection to content of material such as nitrogen phosphorus in water sample, the main method that adopts simulation laboratory's manual analysis: at first select certain oxidizing digestion method, organism is cleared up, and the elemental oxygen to be detected of various valence states in water sample is changed into to unified highest price state form, then utilize the difference of various element ions to the ultra-violet absorption spectrum characteristic, with UV spectrophotometer measuring, go out test substance content.Wherein, to the oxidizing digestion method of water sample, mainly contain at present following methods:
1, add the oxygenant method:
(1) add the potassium persulfate method: for the mensuration of total nitrogen in water sample, regulation in national standard (GB 11894-89) " the mensuration alkalescence alkaline potassium per-sulfate digestion ultraviolet spectrophotometry of water quality total nitrogen " (GB 11894-89), under the alkaline medium condition of 120 ~ 124 ℃, with potassium persulfate, make oxygenant, not only the ammonia nitrogen in water sample and nitrite nitrogen can be oxidized to nitrate, simultaneously most of organonitrogen compound in water sample be oxidized to nitrate.This method need to consume potassium persulfate reagent under the condition of alkali of heating, need often to change reagent, complicated operation, inefficiency.
(2) add By Ozone: ozone is a kind of strong oxidizer, and oxidation potential is 2.07V, and is fast with the organism reaction velocity.Ozone mixes with water sample by the method for aeration or jet, can react with the polluter that various forms in water exist, and the organism of complexity is transformed into to simple compounds, and progressively the lower valency ionic oxide formation is arrived to high valence state form.The solubleness of ozone in water is lower, and is selective to organic substance, is difficult to give full play to oxidation and clears up effect.
(3) add hydrogen peroxide method: hydrogen peroxide is a kind of colourless sticky liquid, and its aqueous solution is commonly called as hydrogen peroxide, is also strong oxidizer commonly used in water treatment, and oxidation potential is 1.77V, the inorganic and organic contaminant in the energy oxidize water.The hydrogen peroxide unstable chemcial property, generally deposit with 30% or 60% aqueous solution form, and the storage of hydrogen peroxide and use procedure all are not easy to control, and are difficult to be applicable to Site Detection.
2, electrolytic oxidation method:
The wastewater electrolytic facture is a kind of of waste water method of chemical treatment.The ultimate principle of application electrolysis, make objectionable impurities in water sample transform into innoxious substance to realize the method that purifies by electrolysis.Wastewater electrolytic is processed and to be comprised electrode surface electrochemical action, indirect oxidation and indirect reduction, and the process such as electricity flocculation, respectively with the pollutant in different effect removal waste water.Shortcoming is that the consumption of power consumption and electrode metal is larger when processing a large amount of waste water, and the sediment of separation is difficult for processing and utilizing.Also can in solution, produce simultaneously metal cation and disturb, be difficult to be applicable to water quality detection.
3, ozone, ultraviolet cooperating resolution method:
Ozone and ultraviolet cooperating are a kind of high-level oxidation technologies, can generate hydroxyl radical free radical, have oxidisability strong, the reaction conditions gentleness, and speed is fast, does not need the characteristics such as catalyzer.Patent 200710016757 proposes according to this principle: utilize ozone generator to produce the ozone of steady concentration and mix with distilled water to generate ozone solution, ozone solution is after ultra violet lamp, decomposed produces hydroxyl radical free radical, then clears up reaction with water sample generation oxidation under the non-dynamic equilibrium condition that flows.The shortcoming of this patent is: ozone is difficult for being dissolved in water, so the content of the ozone in ozone solution and the hydroxyl radical free radical that decomposition generates under UV-irradiation thereof may be not enough to the complete oxidation water sample; Secondly because hydroxyl radical free radical is the most active active substance, can not stable existence, in the ozone solution balance pipe after ultra violet lamp generating portion hydroxyl radical free radical, adopt again the flow injection mode, with water sample, in the sinuous coil reactor, mix, this process may lose the part of hydroxyl free radical.The mode of continuous flow can not guarantee that water sample has the sufficient time to carry out oxidation and clears up reaction in addition, causes oxidation efficiency not high.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of ozone-ultraviolet synergistic oxidation to clear up the on-line measuring device that detects total nitrogen total phosphorus, after adopting ozone and water sample jointly to mix, common irradiation uviol lamp carries out the structure that oxidation clears up to produce hydroxyl radical free radical, solved the central ozone of prior art and hydroxyl radical free radical thereof and adopted the flow injection mode to mix in reactor with water sample, the situation that causes the part of hydroxyl free radical to lose.
Another object of the present invention is to adopt aeration mode that ozone is sent in reaction tube, with ozone in the middle of solving prior art, is difficult for being dissolved in water, and hydroxyl radical free radical content is not enough to the problem of complete oxidation water sample.
According to technical scheme provided by the invention, described ozone-ultraviolet synergistic oxidation is cleared up the on-line measuring device that detects total nitrogen total phosphorus, comprises glass reaction tube, in the both sides external of glass reaction tube, hangs respectively the first uviol lamp and the second uviol lamp; Feature is: water sample import and tail gas escape hole are set in the upper end of described glass reaction tube, and described water sample import is connected with the water sample storage tank; Bottom at described glass reaction tube is provided with escape hole, and this escape hole connects respectively two pipelines that are arranged in parallel; Article one, pipeline is connected with ozone generator by electrolytic process, at the gas output end of ozone generator by electrolytic process, pin type nozzle and retaining valve is set; The second pipeline is connected with the first entrance point of detection cell, and detection cell the second entrance point is connected with total phosphorus developer charging-tank; The first endpiece of described detection cell is connected with the 3rd syringe pump with spectrophotometer, and the second endpiece of detection cell is connected with waste liquid barrel.
Described spectrophotometer is only exported the light absorption value of 220nm, 275nm and 700nm wavelength.
Between the second endpiece of described detection cell and waste liquid barrel, the second solenoid valve is set.
Between the water sample import of described glass reaction tube and water sample storage tank, the first syringe pump is set.
The first entrance point at described detection cell arranges the first solenoid valve.
Between the second entrance point of described detection cell and total phosphorus developer charging-tank, the second syringe pump is set.
Described ozone-ultraviolet synergistic oxidation is cleared up the online test method that detects total nitrogen total phosphorus, adopts on-line measuring device to carry out in the steps below:
(1) 10ml water sample to be measured is sent in glass reaction tube by the water sample import;
(2) ozone generator by electrolytic process generation mass concentration is 18 ~ 20% ozone gas, and ozone gas is entered in glass reaction tube with aeration mode by retaining valve and pin type nozzle, and aeration rate is 630 ~ 770mg/h; At the arranged outside uviol lamp of glass reaction tube, ozone gas and water sample to be measured water sample to be measured after carrying out oxidation under the irradiation of uviol lamp and being cleared up, the time is 25 ~ 30 minutes;
(3) after oxidation has been cleared up, the water sample to be measured after clearing up enters in detection cell;
(4) test total nitrogen content: the water sample to be measured that is extracted after 5ml clears up by syringe pump enters spectrophotometer, and remaining water sample to be measured enters in waste liquid barrel; Water sample to be measured after the spectrophotometer test is cleared up, at the absorbance at 220nm and 275nm wavelength place, calculates total nitrogen content;
(5) total nitrogen detect complete after, syringe pump is returned the water sample in spectrophotometer in detection cell again, in detection cell, adds the 0.2ml ascorbic acid solution, after 30 seconds, adds the 0.4ml molybdate solution; In detection cell, develop the color after 10 ~ 20min, again will clear up water sample and send in spectrophotometer, the water sample after spectrophotometer detection colour developing, at the absorbance at 700nm wavelength place, calculates total phosphorus content.
Processing is cleared up in the water sample oxidation that the present invention is applicable in ambient water quality on-line continuous detection system, broken away from the shortcoming of laboratory traditional analysis, without consuming chemical oxidizing agent, easy to operate, equipment is simply small and exquisite, and technological process is simplified, cost is low, realized that on-line oxidation clears up, and in time detected, demonstrated the total nitrogen total phosphorus content in water sample, be specially adapted to total Phosphorus in Environmental Water total nitrogen on-line detecting system.After the present invention adopted ozone to mix in reactor with water sample, the common uviol lamp that irradiates carried out the structure that oxidation clears up to produce hydroxyl radical free radical, avoided ozone and hydroxyl radical free radical thereof to adopt the flow injection mode to mix in reactor with water sample, the situation that causes the part of hydroxyl free radical to lose.The present invention adopts aeration mode that ozone is injected to reaction tube, has solved ozone and has been difficult for being dissolved in water, and hydroxyl radical free radical content is not enough to the problem of complete oxidation water sample.
The accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Embodiment
The invention will be further described below in conjunction with concrete accompanying drawing.
As shown in Figure 1: the ozone-ultraviolet synergistic oxidation is cleared up the on-line measuring device that detects total nitrogen total phosphorus and is comprised water sample storage tank 1, the first syringe pump 2, glass reaction tube 3, tail gas escape hole 4, the first uviol lamp 5, the second uviol lamp 6, pin type nozzle 7, retaining valve 8, ozone generator by electrolytic process 9, the first solenoid valve 10, total phosphorus developer charging-tank 11, the second syringe pump 12, detection cell 13, the 3rd syringe pump 14, spectrophotometer 15, the second solenoid valve 16, waste liquid barrel 17 etc.
The present invention includes and carry out the glass reaction tube 3 that oxidation is cleared up, this glass reaction tube 3 adopts the straight pipe type quartz glass tube, and glass reaction tube 3 internal diameters are 8mm, and external diameter is 10mm, and long is 550mm; Both sides external at described glass reaction tube 3 hangs respectively the first uviol lamp 5 and the second uviol lamp 6, and described the first uviol lamp 5, the second uviol lamp 6 can adopt the single-ended straight type uviol lamp of 14W, and wavelength is 254nm; Water sample import and tail gas escape hole 4 are set in the upper end of described glass reaction tube 3, and described water sample import is connected with water sample storage tank 1 by silica gel hose, and the first syringe pump 2 is set between water sample import and water sample storage tank 1; Bottom at described glass reaction tube 3 is provided with escape hole, and this escape hole connects respectively two pipelines that are arranged in parallel; Article one, pipeline is connected with ozone generator by electrolytic process 9, at the gas output end of ozone generator by electrolytic process 9, is provided for pin type nozzle 7 and the retaining valve 8 of aeration; The second pipeline is connected with the first entrance point of detection cell 13, the first solenoid valve 10 is set on the first entrance point of detection cell 13, detection cell 13 second entrance points are connected with total phosphorus developer charging-tank 11, between the second entrance point of detection cell 13 and total phosphorus developer charging-tank 11, the second syringe pump 12 are set; The first endpiece of described detection cell 13 is connected with the 3rd syringe pump 14 with spectrophotometer 15, and the second endpiece of detection cell 13 is connected with waste liquid barrel 17;
Between the second endpiece of described detection cell 13 and waste liquid barrel 17, the second solenoid valve 16 is set;
Described spectrophotometer 15 adopts micro spectrometer, only exports the light absorption value of 220 nm, 275nm and 700nm wavelength.
Ozone-ultraviolet synergistic oxidation of the present invention is cleared up the online test method that detects total nitrogen total phosphorus, adopts on-line measuring device to carry out in the steps below:
(1) by 10ml water sample to be measured from water sample storage tank 1 via in the first syringe pump 2 implantation glass reaction tubes 3;
(2) ozone generator by electrolytic process 9 generation mass concentrations are 18 ~ 20% ozone gas, and ozone generator by electrolytic process 9 adopts the electrolysis deionized waters, and ozone output is 700 ± 10%mg/h; Ozone gas enters the bottom of glass reaction tube 3 by retaining valve 8 and pin type nozzle 7 with aeration mode, aeration rate is 630 ~ 770mg/h, minute bubbles are along the pipeline rising of glass reaction tube 3, after water sample to be measured in glass reaction tube 3 fully contacts, from the tail gas escape hole 4 at glass reaction tube 3 tops, discharge tail gas; At the arranged outside uviol lamp of glass reaction tube 3, ozone gas and water sample to be measured water sample to be measured after carrying out oxidation under the irradiation of uviol lamp and being cleared up, the time is 25 ~ 30 minutes;
(3) after oxidation has been cleared up, the water sample to be measured after clearing up enters in detection cell;
(4) test total nitrogen content: the water sample to be measured that is at first extracted after 5ml clears up by the 3rd syringe pump 14 enters in spectrophotometer 15, and remaining water sample to be measured enters in waste liquid barrel 17 by the second solenoid valve 16; Water sample to be measured after spectrophotometer 15 tests are cleared up, at the absorbance at 220nm and 275nm wavelength place, calculates total nitrogen content;
(5) total nitrogen detect complete after, the 3rd syringe pump 14 is returned the water sample in spectrophotometer 15 in detection cell 13 again, in detection cell 13, add the 0.2ml ascorbic acid solution, after 30 seconds, add again 0.4ml molybdate solution (ascorbic acid solution as used herein and molybdate solution all adopt mentioned ascorbic acid solution and molybdate solution in the mensuration of GB11893-89 water quality total phosphorus-ammonium molybdate spectrophotometric method); The best developing time of 10 ~ 20min(that develops the color in detection cell is 15min) after, again will clear up water sample and send in spectrophotometer 15, the water sample after spectrophotometer 15 detection colour developings, at the absorbance at 700nm wavelength place, calculates total phosphorus content.
After the present invention adopted ozone and water sample jointly in reactor, to mix, the common uviol lamp that irradiates carried out the structure that oxidation clears up to produce hydroxyl radical free radical, avoided ozone and hydroxyl radical free radical thereof to adopt the flow injection mode to mix in reactor with water sample, the situation that causes the part of hydroxyl free radical to lose.The present invention adopts aeration mode that ozone is injected to reaction tube, has solved ozone and has been difficult for being dissolved in water, and hydroxyl radical free radical content is not enough to the problem of complete oxidation water sample.
Claims (2)
1. an ozone-ultraviolet synergistic oxidation is cleared up the on-line measuring device that detects total nitrogen total phosphorus, comprises glass reaction tube (3), in the both sides external of glass reaction tube (3), hangs respectively the first uviol lamp (5) and the second uviol lamp (6); It is characterized in that: water sample import and tail gas escape hole (4) are set in the upper end of described glass reaction tube (3), and described water sample import is connected with water sample storage tank (1); Bottom at described glass reaction tube (3) is provided with escape hole, and this escape hole connects respectively two pipelines that are arranged in parallel; Article one, pipeline is connected with ozone generator by electrolytic process (9), at the gas output end of ozone generator by electrolytic process (9), pin type nozzle (7) and retaining valve (8) is set; The second pipeline is connected with the first entrance point of detection cell (13), and detection cell (13) second entrance points are connected with total phosphorus developer charging-tank (11); The first endpiece of described detection cell (13) is connected with the 3rd syringe pump (14) with spectrophotometer (15), and the second endpiece of detection cell (13) is connected with waste liquid barrel (17);
Described spectrophotometer (15) is only exported the light absorption value of 220nm, 275nm and 700nm wavelength;
Between the second endpiece of described detection cell (13) and waste liquid barrel (17), the second solenoid valve (16) is set;
Between the water sample import of described glass reaction tube (3) and water sample storage tank (1), the first syringe pump (2) is set;
The first entrance point at described detection cell (13) arranges the first solenoid valve (10);
Between the second entrance point of described detection cell (13) and total phosphorus developer charging-tank (11), the second syringe pump (12) is set.
2. an ozone-ultraviolet synergistic oxidation is cleared up the online test method that detects total nitrogen total phosphorus, it is characterized in that, described method adopts on-line measuring device to carry out in the steps below:
(1) 10ml water sample to be measured is sent in glass reaction tube by the water sample import;
(2) ozone generator by electrolytic process generation mass concentration is 18 ~ 20% ozone gas, and ozone gas is entered in glass reaction tube with aeration mode by retaining valve and pin type nozzle, and aeration rate is 630 ~ 770mg/h; At the arranged outside uviol lamp of glass reaction tube, ozone gas and water sample to be measured water sample to be measured after carrying out oxidation under the irradiation of uviol lamp and being cleared up, the time is 25 ~ 30 minutes;
(3) after oxidation has been cleared up, the water sample to be measured after clearing up enters in detection cell;
(4) test total nitrogen content: the water sample to be measured that is extracted after 5ml clears up by syringe pump enters spectrophotometer, and remaining water sample to be measured enters in waste liquid barrel; Water sample to be measured after the spectrophotometer test is cleared up, at the absorbance at 220nm and 275nm wavelength place, calculates total nitrogen content;
(5) total nitrogen detect complete after, syringe pump is returned the water sample in spectrophotometer in detection cell again, in detection cell, adds the 0.2ml ascorbic acid solution, after 30 seconds, adds the 0.4ml molybdate solution; In detection cell, develop the color after 10 ~ 20min, again will clear up water sample and send in spectrophotometer, the water sample after spectrophotometer detection colour developing, at the absorbance at 700nm wavelength place, calculates total phosphorus content.
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| CN103575869B (en) * | 2013-10-31 | 2015-04-22 | 江南大学 | Method and device for detecting COD (chemical oxygen demand) of water body through synergy of ozone and ultraviolet |
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| CN110174398A (en) * | 2019-07-01 | 2019-08-27 | 浙江工业大学 | Water body total chrome content on-line measuring device and method based on high-level oxidation technology |
| CN113281328B (en) * | 2021-03-19 | 2022-09-20 | 深圳市朗诚科技股份有限公司 | Method for detecting total nitrogen in water body and application thereof |
| CN114354588A (en) * | 2021-12-07 | 2022-04-15 | 浙江工业大学 | Total nitrogen online detection method based on advanced oxidation technology and dual-environment digestion scheme |
| CN114354587A (en) * | 2021-12-07 | 2022-04-15 | 浙江工业大学 | Water total phosphorus on-line detection method based on weak acid environment and advanced oxidation technology |
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