CN103969411B - A kind of method directly measuring soluble organic nitrogen concentration in water body based on electrodialysis pretreatment mode - Google Patents
A kind of method directly measuring soluble organic nitrogen concentration in water body based on electrodialysis pretreatment mode Download PDFInfo
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Abstract
The invention provides a kind of method directly measuring soluble organic nitrogen in water body (DON) based on electrodialysis pretreatment mode, be characterized in that adopting electrodialysis isolation technics first to carry out DON is effectively separated with the quick of inorganic nitrogen (DIN), then directly obtains DON concentration by total dissolved nitrogen (TDN) test.Electrodialytic object removes DIN but retains DON, when after processing, DON accounts for TDN most in water sample (as DIN and TDN ratio is less than 0.1), and stopping electrodialysis process.Subsequently, the TDN content in water sample can be equal to DON content.The present invention substantially increases the accuracy and precision that in water sample, DON measures; overcome and measured the problem such as water sample indirect, consuming time, the low accuracy of DON method and low precision in the past; the detection of DON in various water body can be widely used in, also can be used for being dissolvable in water the measurement of the DON in the solid particle of water or atmospheric haze particle.
Description
Technical field
The invention belongs to environmental protection, water treatment field, be specially the method utilizing electrodialysis pretreatment mode to realize directly measuring soluble organic nitrogen (DON) concentration in water body.Can be applicable to the measurement of environmental protection and all kinds of DON utilizing water to be carrier, as water treatment, ocean, agricultural fertilizer and atmospheric haze etc.
Background technology
Extensively there is all kinds of dissolved organic matter in environment, nitrogenous type organic is wherein important ingredient.Total dissolubility nitrogen (TDN) comprises organic nitrogen (DON) and inorganic nitrogen (DIN).Under certain condition, DON can change into DIN and be utilized as nitrogenous source reserve by microorganism, is one of reason causing the environmental hazards such as body eutrophication.This is that recent research display, the DON in water body and sanitizer react, and can produce multiple " three causing property " DBPs (DBPs), such as: halo is cyanogen, halonitro toluene
[1]; And the cytotoxicity of nitrogenous DBPs 2-3 the order of magnitude more contour than three traditional methine halides, halogenated acetic acids.Therefore, DON, as the precursor substance of nitrogen class DBPs, more and more causes the concern of people, and to be expected in water processing control afterwards detection and control in addition.
Prior art mainly realizes the measurement of DON by " subtracting poor method ", and namely TDN deducts DIN(and comprises nitrate nitrogen, nitrite nitrogen, ammonia nitrogen).Because DON content in surface water is general all few than DIN, subtract propagation of error that poor process can cause DON to measure and amplify, the serious precision reducing DON measurement, even reaches one of percentage more than hundred sometimes.Suppose that in certain surface water, TDN concentration is 2.0mg-n/L, nitrate nitrogen is 1.8mg-n/L, and ammonia nitrogen is 0.05mg-n/L, and each index only has the analytical error of 5%, and so DON concentration ought to be 0.15mg-n/L(2-1.8-0.05); But TDN subtracts DIN errors but up to 0.19mg-n/L (2*5%+1.8*5%+0.05*5%), and error rate is up to 128%(0.19/0.15*100)
[2].
Therefore be necessary that DIN with DON is separated, and then improve accuracy and the intensive reading of DON measurement.Current Chinese scholars mainly adopts two kinds of methods to carry out being separated of DIN with DON, and one is: adopt dialysis membrane; Two are: NF membrane.First method adopts molecular weight to be that the dialysis membrane of 100-500Dalton carries out pre-service at present, DIN:TDN ratio can be made to be reduced to less than 0.6, thus improve DON accuracy of detection and accuracy.But the method needs more than 24 hours consuming time, consumes a large amount of high purity waters, and still needs after pre-service to obtain DON concentration by " subtracting poor method ", be therefore unsuitable for Routine Test Lab express-analysis
[3].For second method, the NF membrane that domestic scholars have employed 150 ~ 500Dalton carries out pre-service to water sample.The method can concentrate DON in water sample, also can realize the quick separating (4 hours) of DON and DIN.But the method can only remove 69 ~ 92%DIN at most, and DON loss is more than more than 20%, and sample water requirement comparatively large (300-500ml).Therefore also cannot realize the direct measurement of DON concentration after pre-service, and the accuracy of measuring DON may be reduced.
In addition, have foreign scholar to have employed electrodialysis pretreatment mode in the recent period and carry out water sample pre-service [4], but still " subtracting poor method " mode of employing obtains DON concentration, and it studies the DIN composition ammonium radical ion do not removed completely wherein, therefore, water body DON concentration can not directly be measured.
Summary of the invention
In order to overcome existing DON measuring method length consuming time, precision is low, and degree of error is high, deficiencies such as complicated operation indirectly, the invention provides a kind ofly can to realize directly, fast, the method for Measurement accuracy water body DON.
The technical solution adopted in the present invention is:
Measure a method for DON concentration in water body, adopt electrodialytic technique to carry out pre-service to water sample, DIN and DON composition in water sample is effectively separated, thus realizes the Measurement accuracy of water body DON.
The described aperture of use is before pre-processing not less than 0.22 μm but is not more than the impurity in the micro-filtration filter membrane removal water sample of 0.7 μm.
Described micro-filtration filter membrane comprises cellulose ester membrane etc.
Described electrodialytic technique refers to and adopts the electrodialysis mode of constant voltage or constant current to carry out pre-service to water sample, and the voltage preferably adopted is the DC voltage of <30v, and ensures that in electrodialytic process, water sample pH remains between 1 ~ 10.
Get appropriate volume after membrane filtration water sample, drop into electrodialysis reactor, adopt the electrodialysis process mode of constant voltage or steady current, middle part adds water sample, and both sides add nonnitrogenous salt solution and constantly update.
What added salt solution will ensure is to conduct electricity, but nonnitrogenous class material is to avoid interference.Preferred concentration is 0.5mol/l sodium chloride brine, or concentration is the metabisulfite solution of 0.01mol/l.
Amberplex in electric dialyzator used is chosen anion exchange membrane (AEM) and selectivity cation-exchange membrane (CEM).
Described water sample, after electrodialysis preprocessing process, makes DON in water sample account for the leading position of TDN, as DIN and TDN ratio is less than 0.1.
Preferred DON content detection scope 0.1mg/L-100mg/L of the present invention, but be not limited to detection that is higher or lower concentration.
After in water sample, DIN and TDN ratio is less than 0.1, the pretreated water sample of power taking dialysis carries out TDN analysis, measures the concentration that the TDN concentration obtained is DON in water sample.
Measuring method of the present invention may be used for the analysis of DON in various water sample, and described water sample comprises surface water, underground water, potable water, seawater, rainwater and water maybe can be utilized for other water samples of carrier.Wherein, other water samples that water can be utilized to be carrier comprise the solid particle or atmospheric haze particle that are dissolvable in water water.
Electrodialysis isolation technics of the present invention realizes the quick of DON with DIN in water body and is effectively separated, and the TDN recorded subsequently is DON.
Electrodialysis take electric field as charged particle driving force, and the selective penetrated property of coupled ion exchange membrane is the isolation technics of ultimate principle.Under the effect of electric field, amberplex can selectivity through Small molecular inorganic nitrogen ion, but retain large molecular polarity or without charge organic nitrogen molecule, therefore can realize being separated completely of inorganic nitrogen ion and organic nitrogen molecule.Utilize the quick and precisely measurement that this mechanism can realize DON in water body.
After electrodialysis pre-service completes, after getting pre-service, water sample carries out TDN analysis, measures the concentration that the TDN concentration obtained can be equal to DON in water sample.
Described TDN analyzes can adopt ultraviolet spectrophotometry, combustion method, clear up the method and apparatus such as rear survey nitrate ion analyzes.
Above-mentioned DON assay method can be applied in the water treatment procedures such as surface water, underground water and potable water.
Measuring method of the present invention specifically includes, but are not limited to following technical scheme:
Directly measure a method of DON in water body based on electrodialysis pretreatment mode fast, comprising:
Be the cellulose esters membrane filtration removal graininess impurity of 0.45 μm by detected water sample aperture, get 50 ~ 100ml water sample after filtering, in electric dialyzator, carry out electrodialysis pre-service; After pretreatment, in water sample, soluble organic nitrogen composition accounts for the principal ingredient of total dissolved nitrogen to detected water sample, and the measurement result of TDN is the concentration of DON subsequently.To the anion-exchange membrane used in electric dialyzator and cation-exchange membrane, and ensure that in electrodialytic process, water sample pH remains between 1 ~ 10.The voltage adopted is the DC voltage of <30v.In electrodialysis preprocessing process, when the ratio of DIN and TDN is less than 0.1, stop electrodialysis preprocessing process.After process, water sample TDN analyzes and adopts uv-spectrophotometric.The TDN concentration measuring water sample is DON concentration in former water sample.
Wherein, electric dialyzator operational factor is determined by following experimental program: the operational factor of electric dialyzator comprises voltage, flow velocity, dense room concentration, light room ionic strength, ionic membrane area, adopts the water of artificial preparation to test, analyze the DIN clearance under different operational factor condition and DON retention rate, draw the optimal operating parameter of electric dialyzator.
Owing to have employed such scheme, bring following beneficial effect relative to prior art, include but not limited to:
1, this method can effectively be separated DIN and DON in water sample, can be separated by the DIN of more than 99%, thus after realizing pre-service, DON directly measures in 3 hours from water sample;
2, this method is compared to the dialysis membrane method for pretreating proposed in the world, and under identical separating effect (99%), its processing time at least saves more than 40 times, thus can realize the measurement of quick DON;
3, this method is compared compared to the NF membrane method for pretreating of domestic scholars, and under identical separating effect (90%), the time saves more than 3 times, and operating conditions is simple, and without the need to controlling pressure, temperature, directly measures the concentration that TDN just can obtain DON after process.
4, the ratio that runs off of this method DON for most of tested material lower than 20%, therefore can realize the Measurement accuracy of DON.
5, this measuring method revision test standard deviation is in 10% scope, effectively improves accuracy and the accuracy of DON measurement.
Accompanying drawing explanation
Fig. 1, the principle schematic before electrodialysis preprocessing process of the present invention electrodialysis
Fig. 2, the principle schematic after electrodialysis preprocessing process of the present invention electrodialysis
Fig. 3, electrodialysis plant of the present invention and pretreatment mode operational flowchart
Fig. 4, the clearance design sketch of various nitrogen substance under embodiment of the present invention
Fig. 5, the lower pretreated recovery design sketch of electrodialysis of the different DIN/DON value of the inventive method
Fig. 6, uses this method of the present invention directly to the measurement result comparison diagram of 5 natural waters
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described:
Embodiment 1
Concrete total embodiment and step
The first step: before electrodialysis pre-service, filters with the water sample of the cellulose ester membrane of 0.45 μm by required test, elimination suspension, granule foreign (as can not measure in time, need by the Refrigerator store of water after membrane filtration stored in 4 degrees Celsius).
Second step: amberplex is processed by ionic membrane requirement of dispatching from the factory, and the good electrodialysis plant of Installation and Debugging, and ensure that in electrodialytic process, water sample pH remains between 1 ~ 10.
3rd step: get the light room that the water sample filtered in right amount puts into electrodialysis plant, salt solution is passed in dense room, and load the constant DC voltage being less than 30V, carry out electrodialysis pre-service (electrodialysis principle is shown in attached Fig. 1 and 2), the clearance effect (see accompanying drawing 4) of various nitrogen substance.
4th step: the conductivity of water sample, the content of DON and DIN in the light room of Real-Time Monitoring, when the ratio of DIN and TDN is less than 0.1 in water sample, stops electrodialysis preprocessing process.For the lower pretreated recovery effect of electrodialysis (see accompanying drawing 5) of different DIN/TDN value.
5th step: get pretreated water sample in light room and carry out TDN analysis, TDN analyzes according to standard method (alkaline chitinase clears up ultraviolet spectrophotometry HJ636-2012(Chinese Ministry of Environmental Protection)) carry out, adopt the instrument such as ultraviolet spectrophotometer or ion chromatograph to analyze, measure the TDN concentration that obtains i.e. DON concentration in former water sample.
Embodiment 2:
According to concrete overall plan and the step of embodiment 1, and the concrete enforcement parametric scheme shown in Fig. 3
Investigate the recovery and the degree of accuracy of organic nitrogen in natural water, by adding quantitative DIN and DON in natural water, then DIN and DON content in tracking measurement water sample.According to the implementation step described by this programme, the recovery of contrast different time points DON and precision, its effect is as accompanying drawing 5.
Result shows, and along with the carrying out of electrodialytic process, DIN concentration constantly reduces, the ratio of DIN/TDN also constantly reduces, and the recovery of DON is between 93% ~ 110%, and measuring accuracy is then along with the continuous reduction of DIN, improve constantly, its percentage ratio error is decremented to 2.3% by 33%.Prove, after electrodialysis pre-service, have significant benefit to the measurement of DON in water sample thus.
Embodiment 3:
According to concrete total embodiment and the step of embodiment 1, and specifically implement parametric scheme shown in Fig. 3
Investigated lake, Shenzhen lake water respectively, river, Shenzhen river, the water outlet of waterworks, Shenzhen, Shenzhen's Sewage Plant water inlet and water outlet in DON content.
According to the invention process step, contrast the DON measured value in water sample after not carrying out electrodialysis pre-service and having carried out electrodialysis pre-service respectively, effect accompanying drawing 6.
Table 1: used instrument in experimentation
As can be seen from Figure 6, the water sample of several water body, when not carrying out electrodialysis pre-service, cannot obtain the concentration of the DON in water, even measures and obtains negative value; Adopt the pretreated DON measured value of electrodialysis, have good measurement result, revision test standard deviation, in 10% scope, effectively improves accuracy and the accuracy of DON measurement.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Background technology list of references:
1.Plewa,M.J.,etal.,HalonitromethaneDrinkingWaterDisinfectionByproducts:ChemicalCharacterizationandMammalianCellCytotoxicityandGenotoxicity.EnvironmentalScience&Technology,2003.38(1):p.62-68.
2.Lee,W.andP.Westerhoff,DissolvedOrganicNitrogenMeasurementUsingDialysisPretreatment.EnvironmentalScience&Technology,2004.39(3):p.879-884.
3.Chon,K.,etal.,Quantificationandcharacterizationofdissolvedorganicnitrogeninwastewatereffluentsbyelectrodialysistreatmentfollowedbysize-exclusionchromatographywithnitrogendetection.WaterResearch,2013.47(14):p.5381-5391.
4.Xu,B.,etal.,Measurementsofdissolvedorganicnitrogen(DON)inwatersampleswithnanofiltrationpretreatment.WaterResearch,2010.44(18):p.5376-5384。
Claims (6)
1. one kind measures the method for soluble organic nitrogen concentration (DON) in water body, it is characterized in that: adopt electrodialytic technique to carry out pre-service to water sample, amberplex in electric dialyzator used is chosen anion exchange membrane (AEM) and selectivity cation-exchange membrane (CEM), electric dialyzator positive pole and chosen anion exchange membrane, and form dense room respectively between electric dialyzator negative electrode and selectivity cation-exchange membrane, light room is formed between chosen anion exchange membrane and selectivity cation-exchange membrane, water sample puts into the light room of electric dialyzator, salt solution is passed in dense room, carry out electrodialysis pre-service, described salt solution is concentration be 0.5mol/l sodium chloride brine or concentration is the metabisulfite solution of 0.01mol/l, inorganic nitrogen in water sample (DIN) ion is effectively separated with DON composition, thus realize the Measurement accuracy of water body DON, water sample is after electrodialysis preprocessing process, the content ratio of DIN and TDN in water sample is made to be less than 0.1, the pretreated water sample of power taking dialysis carries out total dissolubility nitrogen (TDN) and analyzes, measure the concentration that the TDN concentration obtained is DON in water sample.
2. method according to claim 1, is characterized in that: use aperture to be not less than 0.22 μm before pre-processing but be not more than the impurity in the micro-filtration filter membrane removal water sample of 0.7 μm.
3. method according to claim 1, is characterized in that: described electrodialytic technique refers to and adopts the electrodialysis mode of the DC voltage of <30v to carry out pre-service to water sample.
4. method according to claim 3, is characterized in that: ensure that in electrodialytic process, water sample pH remains between 1 ~ 10.
5. the method according to the arbitrary claim of Claims 1-4, is characterized in that: described water sample comprises surface water, underground water, potable water, seawater, rainwater maybe can utilize other materials that water is carrier.
6. method according to claim 5, is characterized in that: other materials that water can be utilized to be carrier comprise the solid particle or atmospheric haze particle that are dissolvable in water water.
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| CN108444933A (en) * | 2018-03-19 | 2018-08-24 | 哈尔滨工业大学深圳研究生院 | A method of soluble organic nitrogen concentration in water is measured based on dialysis superposition of electric field mode |
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| CN107219102A (en) * | 2016-03-21 | 2017-09-29 | 哈尔滨工业大学深圳研究生院 | A kind of method of soluble organic nitrogen concentration in superposition of electric field pretreatment mode direct measurement water body based on dialysis |
| CN106093215B (en) * | 2016-05-26 | 2019-09-06 | 深圳合核环境科技有限公司 | The method and system of dissolubility organic halogen content in a kind of measurement water |
| CN106769946B (en) * | 2017-01-20 | 2020-08-07 | 南京大学 | Method for detecting concentration of soluble organic nitrogen in sewage based on dialysis pretreatment |
| CN109030643A (en) * | 2018-07-12 | 2018-12-18 | 西安理工大学 | It is a kind of while detecting the organic phosphorus method of soluble organic nitrogen and dissolubility in sewage |
| CN108982742A (en) * | 2018-07-12 | 2018-12-11 | 西安理工大学 | Algae can utilize organic phosphorus method in a kind of measurement sewage effluents |
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| TW201207374A (en) * | 2010-08-12 | 2012-02-16 | Univ Nat Kaohsiung 1St Univ Sc | Process for measurements of concentration of dissolved organic nitrogen (DON) with low concentration in water |
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| Title |
|---|
| Optimization of dissolved organic nitrogen (DON) measurements in aqueous samples with high inorganic nitrogen concentrations;Jeroen Vandenbruwane等;《Science of the Total Environment》;20070720;第386卷;第103-113页 * |
| Quantification and characterization of dissolved organic nitrogen in wastewater effluents by electrodialysis treatment followed by size-exclusion chromatography with nitrogen detection;Kangmin Chon等;《Water research》;20130620;第47卷(第14期);第5381-5391页 * |
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| CN108444933A (en) * | 2018-03-19 | 2018-08-24 | 哈尔滨工业大学深圳研究生院 | A method of soluble organic nitrogen concentration in water is measured based on dialysis superposition of electric field mode |
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