CN101105440A - Method for measuring water body total nitrogen and total phosphorous by digestion spectrophotometry of ultraviolet cooperating with ozone - Google Patents
Method for measuring water body total nitrogen and total phosphorous by digestion spectrophotometry of ultraviolet cooperating with ozone Download PDFInfo
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Abstract
The invention provides an ultraviolet light and ozone coordinated luminosity counteraction method for measuring the total nitrogen and total phosphorus of water. The invention can solve the problem of the prior method that the real-time measuring can not be taken, the analyzing time is long, the analysis process is numerous and diverse, the measuring condition is harsh and the energy consumption is big, in particular that secondary pollution can be produced. Flow injection method and cavitations effect and ozone oxidation coordinated water sample counteraction method is adopted in the invention, the organic nitrogenous and inorganic nitrogen in the water sample are transformed into nitrate under the normal temperature and pressure, the phosphates of the water sample are transformed into normal phosphates; and lastly, the phosphates and the normal phosphates are measured by an ultraviolet visible light measuring system and the index of the total nitrogen and total phosphorus of water can be obtained.
Description
Technical field
The present invention relates to the environmental chemistry monitoring technical field, relate in particular to the method for ultraviolet cooperating with ozone measuring water body total nitrogen and total phosphorous by digestion spectrophotometry.
Background technology
Nitrogen, phosphorus are one of indispensable elements of biological growth, but total nitrogen and total phosphorus content are too high in the water body, and biology and microorganism are bred in a large number, cause water body, especially eutrophication of coastal waters, lake, reservoir, thereby total nitrogen and total phosphorus are one of important indicators of weighing water quality.The analytical approach of total nitrogen and total phosphorus substantially also is in the lab analysis stage in the water body at present, and the assay method commonly used of total nitrogen has potassium persulfate oxidation-ultraviolet method, reduction-azo colourimetry, and the chromatography of ions etc.The assay method commonly used of total phosphorus has the chromatography of ions and spectrophotometric method, and digestion procedure adopts Perchloric Acid Digestion method, sulfuric acid-nitric acid digestion method and oxygenant-high-pressure digestion method substantially.No matter use total nitrogen and total phosphorus in which kind of detection method analyzing water body, maximum shortcoming is still and rests on the manual analysis basis, in analytic process, hot digestion procedure or micro-wave digestion method are adopted in the decomposition of total phosphorus and total nitrogen, the method longer duration, analytic process is numerous and diverse, the condition harshness, reagent consumption is big, produce secondary pollution etc., therefore data discrete is big, and can not realize the online continuous analysis to measure that carries out, for water body environment complicated and changeable, its result's accuracy and reliability are under suspicion, and said method is difficult to satisfy on-the-spot, monitoring in real time needs.
In recent years, along with electronic technology, new material, new technology, the development of new optical device, especially computer technology makes rapid progress, adopt the corresponding appearance of automatic analysis of developing on the classic method basis, but because the technical difficulty of some realization aspect is too big, though these methods have been broken away from some shortcomings of lab analysis, but the pattern from on-the-spot real-time working also has a segment distance, big as reagent consumption, on-the-spot, the real time execution cycle is short, poor stability, sensitivity and resolution are low, the defective that ion interference etc. are difficult to overcome, the inreal pattern that realizes on-the-spot real-time continuous work.
Summary of the invention
The invention provides a kind of method of ultraviolet cooperating with ozone measuring water body total nitrogen and total phosphorous by digestion spectrophotometry, it can solve can not on-the-spotly detecting in real time of existing method existence, analyzes longer duration, and analytic process is numerous and diverse, condition harshness, energy consumption are big, especially produce secondary pollution problems.
In order to solve the deficiency of prior art, the present invention proposes and utilize the flow injection mode under a kind of normal temperature and pressure, adopt the ultraviolet cooperating with ozone oxidation to clear up means, by the method for total nitrogen and total phosphorus in the UV, visible light luminosity method measurement water body.
Technical scheme of the present invention is, a kind of method of ultraviolet cooperating with ozone measuring water body total nitrogen and total phosphorous by digestion spectrophotometry, described method adopts pick-up unit, pick-up unit comprises electrolysis type ozone generator, have ozone solution balance cylinder, the reactor of uviol lamp, have UV, visible light optical detection system, the delivery of ozone solution of twin-beam, the pump of water sample and other liquid, reactor is connected with the pipeline of delivery of ozone solution and water sample and with the absorption cell of UV, visible light optical detection system by pipeline, and described method is undertaken by following step by pick-up unit:
(1) utilize ozone generator to produce the ozone solution of steady concentration, make the ozone solution ozone solution balance cylinder that flows through by pump, the ozone solution mobile equilibrium pipe of optical glass system is housed in the ozone solution balance cylinder, be provided with uviol lamp in its side, when ozone solution was flowed through the mobile equilibrium pipe, ozone solution was through the irradiation of uviol lamp;
(2) after the ozone solution of ultra violet lamp is flowing through ozone solution mobile equilibrium pipe, mix with water sample in the detected water sample pipeline, enter reactor after the mixing, ozone solution and water sample are cleared up oxidation reaction under the non-mobile equilibrium condition that flows;
(3) after mixed reaction solution flows through reactor, be divided into two-way, the one tunnel directly enters the total nitrogen absorption cell in the UV, visible light optical detection system twin-beam absorption cell, mix with the phosphorus developer on another road, enter the chromogenic reaction device after the mixing, carry out chromogenic reaction, enter the total phosphorus absorption cell afterwards;
(4) the UV, visible light optical detection system is made of deuterium lamp tungsten lamp, convergent lens, plane grating beam splitting system, rotating mirror and reflective mirror, twin-beam absorption cell, photomultiplier,
The stepper motor in deuterium lamp and tungsten lamp and the plane grating beam splitting system and the modulator of rotating mirror are coordinated, enter the plane grating beam splitting system after making light that deuterium lamp and tungsten lamp send by convergent lens, grating resolves into spectrum as dispersion element with the complex light diffraction that receives in the plane grating beam splitting system, motion by stepper motor in the plane grating beam splitting system, obtain 220nm respectively, 275nm, the monochromatic light of 700nm wavelength, monochromatic light is along with the motion of rotating mirror modulator, 220nm, the light of 275nm wavelength enters the total nitrogen absorption cell successively, the light of 700nm wavelength enters the total phosphorus absorption cell, water sample after oxidized the clearing up absorbs the laggard photoelectricity multiplier tube of going into, and photomultiplier converts the light intensity signal that is received to corresponding electric signal, obtains 220nm, 275nm, the light intensity signal of 700nm place after detected water sample absorbs, the spectroscopic data that obtains according to blank water sample calculates 220nm again, 275nm, the light absorption value of 700nm wavelength;
(5) computer data processing unit quantizes the signal of total nitrogen absorption cell collection, according to the A of total nitrogen absorption cell
The school=A
220-2A
275Calculate A
The school, again according to A
The schoolWith the corresponding relation of standard total nitrogen, calculate the water sample total nitrogen content, and show, printout;
(6) computer data processing unit quantizes the signal of total phosphorus absorption cell collection, according to A
700With the corresponding relation of standard total phosphorus, calculate the water sample total phosphorus content, and show, printout.
In technical scheme of the present invention, also have following technical characterictic: described ozone solution flow is 10-15ml/min, and concentration is 8-15mg/L.
In technical scheme of the present invention, also have following technical characterictic: described detected water sample flow is 10-15ml/min.
In technical scheme of the present invention, also have following technical characterictic: described total phosphorus developer is ammonium molybdate-potassium antimony tartrate-ascorbic acid, and flow is 2-4ml/min.
In technical scheme of the present invention, also have following technical characterictic: described ozone generator is an electrolysis type ozone generator, and electrolysis type ozone generator adopts electrolysis distilled water,
In technical scheme of the present invention, also have following technical characterictic: described reactor adopts the coil reactor of crawling.
In technical scheme of the present invention, also have following technical characterictic: described pump is a peristaltic pump, and described pipeline adopts polytetrafluoroethylmaterial material to make.
In technical scheme of the present invention, also has following technical characterictic: adopt the two light source twin-beam beam split of ultraviolet-visible to detect, the stepper motor of light that deuterium lamp and tungsten lamp send and plane grating beam splitting system and rotating mirror modulator carry out synchronously, and one-period obtains total nitrogen total phosphorus and blank extinction signal.
In technical scheme of the present invention, also have following technical characterictic: photomultiplier adopts Japanese shore pine Photosensor Modules H5784 Series.
In technical scheme of the present invention, also has following technical characterictic: utilize the computer control data handling system, by the control of software programming realization to system, signal Processing and calculating, again by the corresponding relation of absorbance and standard method total nitrogen total phosphorus, calculate the water sample total nitrogen total phosphorus and show, printout.Aspect data processing, adopt standard substance can cause that to optical system gain, sample turbidity the factor of systematic error carries out data correction and handle.
The present invention utilizes the flow injection mode, adopt the ultraviolet cooperating with ozone oxidation to clear up means as water sample, make under the normal temperature and pressure that organic nitrogen and inorganic nitrogen are converted into nitrate in the water sample, make that various phosphate transfections turn to orthophosphate in the water sample, measure the method that nitrate and orthophosphate in the water body get total nitrogen and total phosphorus in the water-outlet body by the UV, visible light optical detection system again.The employing of flow injection mode makes the consumption of the sample of total system and reagent considerably less, has the characteristics of economic environmental protection; Carry out oxidation by ultraviolet cooperating with ozone and clear up reaction, make the oxidation of system clear up ability height greatly, having solved the classic method oxidation, to clear up efficient not high, the inclined to one side end of numerical value, do not utilize the defective of scene, on-line measurement, ultraviolet cooperating with ozone carries out the employing that mode is cleared up in oxidation simultaneously, has changed the method for using the conventional oxidation agent, has solved the defective of secondary pollution; The employing of two light source twin-beam spectral detection systems.Make the detection of total nitrogen total phosphorus in the very short cycle, finish, saved the time, be beneficial to field quick detection.With the complicated operation that classic method has than technology itself, the character that the marketing difficulty is big is compared, and the advantage that this method had can make this method developed and popularization in fields such as environmental analyses.
Contrast as follows:
The water body total nitrogen:
| The contrast feature | Classic method | Ultraviolet and ozone cooperative photometry |
| Measurement range mg/L | 0.01-10 | 0-200 |
| Measuring Time/each | 1-2 hour | (less than 5 minutes) continuously |
| Whether need reaction reagent | Need | Do not need |
| Have or not noxious material to form | Have | No |
| Environment for use | Only for the laboratory | On-the-spot |
The water body total phosphorus:
| The contrast feature | Classic method | Ultraviolet and ozone cooperative photometry |
| Measurement range mg/L | 0-1.0 | 0-100 |
| Measuring Time/each | 1-2 hour | (less than 5 minutes) continuously |
| Whether need reaction reagent | Need | Do not need |
| Have or not noxious material to form | Have | No |
| Environment for use | Only for the laboratory | On-the-spot |
Description of drawings
Fig. 1 is the inventive method principle of work process flow diagram;
Fig. 2 is the pick-up unit structural representation that the inventive method adopts.
1. distilled water gatherer; 2. electrolysis type ozone generator; 3. distilled water feeder; 4. cool cycles hydrophone; 5. ozone solution balance cylinder; 6. uviol lamp; 7. ozone mobile equilibrium pipe; 8. ozone solution peristaltic pump; 9. water sample peristaltic pump; 10. water sample; The coil reactor 11. crawl; 12. photomultiplier; 13. total nitrogen absorption cell; 14. reflective mirror; 15. rotating mirror; 16. plane grating beam splitting system; 17. convergent lens; 18. tungsten light source; 19. deuterium lamp light source; 20. waste collection; 21. total phosphorus absorption cell; 22. total phosphorus developer; 23. developer peristaltic pump; 24. rotating mirror modulator; 25. computer data processing unit; 26. control device.
Fig. 3 is the plane grating beam splitting system structural representation that the inventive method adopts
16-1. entrance slit; 16-2. stepper motor; 16-3. plane grating; 16-4. collimator objective; 16-5. collecting objective; The 16-6 exit slit.
Embodiment
The inventive method is carried out according to the following steps by pick-up unit:
(1) utilize ozone generator 2 to produce the ozone solution of steady concentration, the concentration of ozone is 10mg/l, under the 10ml/min flow, make ozone solution circulation ozone solution balance cylinder 5 by peristaltic pump 8, the ozone solution mobile equilibrium pipe 7 of optical glass system is housed in the ozone solution balance cylinder 5, be provided with uviol lamp 6 in its side, when ozone solution circulation mobile equilibrium pipe 7, ozone solution is through the irradiation of uviol lamp 6, part is decomposed the generation hydroxyl radical free radical, and hydroxyl radical free radical and ozone can be together as oxygenant oxidation water samples.The cooling circulating water 4 of ozone solution balance cylinder 5 has guaranteed the stable of ozone concentration.
(2) ozone solution mixes with the water sample 10 that peristaltic pump 9 is carried after flowing through ozone solution mobile equilibrium pipe 7 immediately, enters the coil reactor 11 of crawling after the mixing immediately, and ozone solution and water sample are cleared up oxidation reaction under the non-mobile equilibrium condition that flows.The water sample flow is 10ml/min.
(3) after mixed reaction solution flows through the reactor 11 that crawls, one the tunnel directly enters the total nitrogen absorption cell 13 in the UV, visible light optical detection system twin-beam absorption cell, mix with total phosphorus developer 21 on another road, developer adopts ammonium molybdate-potassium antimony tartrate-ascorbic acid, enter the coil reactor 11 of crawling after the mixing and carry out chromogenic reaction, enter total phosphorus absorption cell 20 afterwards.Total phosphorus developer flow is 2ml/min.
(4) UV, visible light optical detection system deuterium lamp 19 and tungsten lamp 18 are harmonious with the stepper motor 16-2 and rotating mirror 15 modulators 24 of plane grating beam splitting system 16, enter plane grating beam splitting system 16 after making light that deuterium lamp 19 and tungsten lamp 18 send by convergent lens 17, grating 16-3 resolves into spectrum as dispersion element with the complex light diffraction that receives in the plane grating beam splitting system 16, motion by stepper motor 16-2 in the plane grating beam splitting system 16, can obtain 220nm respectively, 275nm, the monochromatic light of 700nm wavelength, monochromatic light is along with the motion of rotating mirror modulator 24,220nm, the light of 275nm wavelength enters total nitrogen absorption cell 13 successively, the light of 700nm wavelength enters total phosphorus absorption cell 21, water sample after oxidized the clearing up enters photomultiplier 12 after absorbing successively, photomultiplier 12 converts the light intensity signal that is received to corresponding electric signal, therefore can obtain 220nm, 275nm, the light intensity signal of 700nm place after detected water sample absorbs, the spectroscopic data that obtains according to blank water sample again, calculate 220nm, 275nm, the light absorption value of 700nm wavelength.
(5) signal of 25 pairs of total nitrogen absorption cells of computer control data processing equipment, 13 collections quantizes, according to the A of total nitrogen absorption cell
The school=A
220-2A
275Calculate A
The school, again according to A
The schoolWith the corresponding relation of standard total nitrogen, calculate the water sample total nitrogen content, and show, printout.
(6) signal of 25 pairs of total phosphorus absorption cells of computer control data processing equipment, 21 collections quantizes, according to A
700With the corresponding relation of standard total phosphorus, calculate the water sample total phosphorus content, and show, printout.
Ozone generator 2 is an electrolysis type ozone generator, adopts the electrode film treatment technology, belongs to the on-consumable type, have easy to operate, install simple and easy, the safety coefficient height, long service life, environmental suitability reaches characteristics such as ozone concentration height, purity height by force.
Adopt ozone solution mobile equilibrium chamber 5, make ozone produce hydroxyl radical free radical in the effect lower part of uviol lamp 6, ozone and ultraviolet cooperating adopt this device to guarantee the stable of ozone concentration to the oxidation efficiency of the water sample oxidation efficiency much larger than single-oxidizer simultaneously, are beneficial to quantitative test.
The employing coil reactor 11 of crawling, this reactor 11 has oxidation and clears up the efficient height, and oxidation is cleared up fully, the characteristics that the water sample demand is little.
The total nitrogen total phosphorus detection system adopts the two light source twin-beam spectral detection systems of ultraviolet-visible.Light that deuterium lamp 19 and tungsten lamp 18 send and the stepper motor 16-2 in the plane grating beam splitting system 16 and rotating mirror modulator 24 carry out synchronously, and one-period obtains total nitrogen total phosphorus and blank extinction signal.
Utilize computer control data processing equipment 25, realize control system by software programming, signal Processing and calculating, again by the corresponding relation of absorbance and standard method total nitrogen total phosphorus, calculate the water sample total nitrogen total phosphorus and show, printout.
Experiment is for example: from the river mouth, several places samplings such as bathing beaches, harbour, culture zone, be divided into two parts.Portion detects in Shandong Province's ocean monitoring technologytechnologies key lab, and portion is measured with method of the present invention.
Experiment shows that both methods have good corresponding relation, and its result error is smaller or equal to 10%.
| The sample sequence number | Total nitrogen | ||
| Method of the present invention (mg/L) | Standard method (mg/L) | Deviation between the method (%) | |
| 1 | 1.49 | 1.42 | 4.9 |
| 2 | 2.82 | 2.79 | 1.0 |
| 3 | 2.95 | 2.89 | 2.0 |
| 4 | 2.12 | 2.07 | 2.4 |
| 5 | 3.45 | 3.31 | 4.2 |
| 6 | 4.98 | 4.82 | 3.3 |
| 7 | 4.56 | 4.42 | 3.2 |
| The sample sequence number | Total phosphorus | ||
| Method of the present invention (mg/L) | Standard method (mg/L) | Deviation between the method (%) | |
| 1 | 0.049 | 0.046 | 6.5 |
| 2 | 0.182 | 0.179 | 1.6 |
| 3 | 0.395 | 0.381 | 3.7 |
| 4 | 0.568 | 0.553 | 2.7 |
| 5 | 0.654 | 0.645 | 1.4 |
| 6 | 0.854 | 0.829 | 3.0 |
| 7 | 0.874 | 0.854 | 2.3 |
The above only is preferred embodiment of the present invention, is not to be the restriction of the present invention being made other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not break away to any simple modification, equivalent variations and remodeling that above embodiment did, still belongs to the protection domain of technical solution of the present invention according to technical spirit of the present invention.
Claims (10)
1. the method for a ultraviolet cooperating with ozone measuring water body total nitrogen and total phosphorous by digestion spectrophotometry, described method adopts pick-up unit, pick-up unit comprises electrolysis type ozone generator, have ozone solution balance cylinder, the reactor of uviol lamp, have UV, visible light optical detection system, the delivery of ozone solution of twin-beam, the pump of water sample and other liquid, reactor is connected with the pipeline of delivery of ozone solution and water sample and with the absorption cell of UV, visible light optical detection system by pipeline, and described method is undertaken by following step by pick-up unit:
(1) utilize ozone generator to produce the ozone solution of steady concentration, make the ozone solution ozone solution balance cylinder that flows through by pump, the ozone solution mobile equilibrium pipe of optical glass system is housed in the ozone solution balance cylinder, be provided with uviol lamp in its side, when ozone solution was flowed through the mobile equilibrium pipe, ozone solution was through the irradiation of uviol lamp;
(2) after the ozone solution of ultra violet lamp is flowing through ozone solution mobile equilibrium pipe, mix with water sample in the detected water sample pipeline, enter reactor after the mixing, ozone solution and water sample are cleared up oxidation reaction under the non-mobile equilibrium condition that flows;
(3) after mixed reaction solution flows through reactor, be divided into two-way, the one tunnel directly enters the total nitrogen absorption cell in the UV, visible light optical detection system twin-beam absorption cell, mix with the phosphorus developer on another road, enter the chromogenic reaction device after the mixing, carry out chromogenic reaction, enter the total phosphorus absorption cell afterwards;
(4) the UV, visible light optical detection system is made of deuterium lamp tungsten lamp, convergent lens, plane grating beam splitting system, rotating mirror and reflective mirror, twin-beam absorption cell, photomultiplier,
The stepper motor in deuterium lamp and tungsten lamp and the plane grating beam splitting system and the modulator of rotating mirror are coordinated, enter the plane grating beam splitting system after making light that deuterium lamp and tungsten lamp send by convergent lens, grating resolves into spectrum as dispersion element with the complex light diffraction that receives in the plane grating beam splitting system, motion by stepper motor in the plane grating beam splitting system, obtain 220nm respectively, 275nm, the monochromatic light of 700nm wavelength, monochromatic light is along with the motion of rotating mirror modulator, 220nm, the light of 275nm wavelength enters the total nitrogen absorption cell successively, the light of 700nm wavelength enters the total phosphorus absorption cell, water sample after oxidized the clearing up absorbs the laggard photoelectricity multiplier tube of going into, and photomultiplier converts the light intensity signal that is received to corresponding electric signal, obtains 220nm, 275nm, the light intensity signal of 700nm place after detected water sample absorbs, the spectroscopic data that obtains according to blank water sample calculates 220nm again, 275nm, the light absorption value of 700nm wavelength;
(5). computer data processing unit quantizes the signal of total nitrogen absorption cell collection, according to the A of total nitrogen absorption cell
The school=A
220-2A
275Calculate A
The school, again according to A
The schoolWith the corresponding relation of standard total nitrogen, calculate the water sample total nitrogen content, and show, printout;
(6). computer data processing unit quantizes the signal of total phosphorus absorption cell collection, according to A
700With the corresponding relation of standard total phosphorus, calculate the water sample total phosphorus content, and show, printout.
2. method according to claim 1 is characterized in that described ozone solution flow is 10-15ml/min, and concentration is 8-15mg/L.
3. method according to claim 2 is characterized in that described detected water sample flow is 10-15ml/min.
4. method according to claim 3 is characterized in that described total phosphorus developer is ammonium molybdate-potassium antimony tartrate-ascorbic acid, and flow is 2-4ml/min.
5. method according to claim 1 is characterized in that described ozone generator is an electrolysis type ozone generator, and electrolysis type ozone generator adopts electrolysis distilled water
6. method according to claim 1 is characterized in that described reactor adopts the coil reactor of crawling.
7. method according to claim 1 is characterized in that described pump is a peristaltic pump, and described pipeline adopts polytetrafluoroethylmaterial material to make.
8. method according to claim 1, it is characterized in that adopting the two light source twin-beam beam split of ultraviolet-visible to detect, the stepper motor of light that deuterium lamp and tungsten lamp send and plane grating beam splitting system and rotating mirror modulator carry out synchronously, and one-period obtains total nitrogen total phosphorus and blank extinction signal.
9. method according to claim 1 is characterized in that photomultiplier adopts Japanese shore pine Photosensor Modules H5784 Series.
10. method according to claim 1, it is characterized in that utilizing the computer control data handling system, by the control of software programming realization to system, signal Processing and calculating, again by the corresponding relation of absorbance and standard method total nitrogen total phosphorus, calculate the water sample total nitrogen total phosphorus and show, printout.Aspect data processing, adopt standard substance can cause that to optical system gain, sample turbidity the factor of systematic error carries out data correction and handle.
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| CN111595789A (en) * | 2020-05-20 | 2020-08-28 | 中国科学院西安光学精密机械研究所 | Device and method for in-situ online monitoring of total nitrogen and total phosphorus in ocean water |
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