CN103969411A - Method for directly measuring concentration of DON (Dissolved Organic Nitrogen) in water body based on electrodialysis pretreatment manner - Google Patents
Method for directly measuring concentration of DON (Dissolved Organic Nitrogen) in water body based on electrodialysis pretreatment manner Download PDFInfo
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Abstract
The invention provides a method for directly measuring concentration of DON (Dissolved Organic Nitrogen) in water body based on an electrodialysis pretreatment manner. The method is characterized by comprising the following steps: firstly, quickly and effectively separating DON from DIN (Dissolved Inorganic Nitrogen) by adopting an electrodialysis separation technology, and then directly obtaining the DON concentration through the TDN (Total Dissolved Nitrogen) test. The purpose of the electrodialysis is to remove the DIN and retain the DON; when the content of DON accounts for a major part of the TDN (for example, the proportion of the DIN to the TDN is smaller than 0.1) in a treated water sample, the electrodialysis treatment is stopped, and after a while, the content of the TDN is equal to the content of the DON in the water sample. The method greatly improves the accuracy and precision of the DON measurement in the water sample, solves the problems that the conventional water sample DON measuring method is indirect, and low in accuracy and precision, and consumes time, can be widely applied to the DON detection in various water bodies, and also can be used for measuring the DON in solid particles or atmospheric haze particles capable of being dissolved in water.
Description
Technical field
The invention belongs to environmental protection, water treatment field, be specially and utilize electrodialysis pretreatment mode to realize the method for directly measuring soluble organic nitrogen (DON) concentration in water body.Can be applicable to environmental protection and all kinds of measurement that utilizes the DON that water is carrier, as water treatment, ocean, agricultural fertilizer and atmospheric haze etc.
Background technology
In environment, extensively exist all kinds of dissolved organic matters, 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, recent studies show that, the DON in water body reacts with sanitizer, can produce multiple " three causing property " DBPs (DBPs), such as: halo is cyanogen, halo nitrotoluene
[1]; And the cytotoxicity of nitrogenous DBPs is than the traditional contour 2-3 of three methine halides, halogenated acetic acids order of magnitude.Therefore, DON, as the precursor substance of nitrogen class DBPs, more and more causes people's concern, and be expected to after water processing control in detected and controlled.
Prior art is mainly by " subtracting poor method ", to realize the measurement of DON, and TDN deducts DIN(and comprises nitrate nitrogen, nitrite nitrogen, ammonia nitrogen).Because DON content in surface water is generally all few than DIN, subtract propagation of error amplification that poor process can cause DON to measure, seriously reduce the precision that DON measures, sometimes even reach one of percentage more than hundred.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 5% analytical error, and DON concentration ought to be 0.15mg-n/L(2-1.8-0.05 so); But TDN subtracts DIN errors but up to 0.19mg-n/L (2*5%+1.8*5%+0.05*5%), error rate is up to 128%(0.19/0.15*100)
[2].
Therefore be necessary that a DIN and DON carry out separated, and then improve accuracy and intensive reading that DON measures.Chinese scholars mainly adopts two kinds of methods to carry out the separated of DIN and DON at present, and the one: adopt dialysis membrane; The 2nd: NF membrane.It is that the dialysis membrane of 100-500Dalton carries out pre-service that first method adopts molecular weight at present, can make DIN:TDN ratio be reduced to below 0.6, thereby improves DON accuracy of detection and accuracy.But it is consuming time more than 24 hours that the method needs, and consumes a large amount of high purity waters, and after pre-service, still need to obtain DON concentration by " subtracting poor method ", be therefore unsuitable for Routine Test Lab express-analysis
[3].For second method, domestic scholars has adopted the NF membrane of 150～500Dalton to carry out pre-service to water sample.The method can concentrate DON in water sample, also can realize quick separated (4 hours) of DON and DIN.But the method can only be removed 69～92%DIN at most, and DON loss surpasses more than 20%, and sample water requirement large (300-500ml).Therefore also cannot realize the direct measurement of DON concentration after pre-service, and may reduce the accuracy of measuring DON.
In addition, have foreign scholar to adopt in the recent period electrodialysis pretreatment mode to carry out water sample pre-service [4], but still " subtracting poor method " mode of employing is obtained DON concentration, and DIN composition ammonium radical ion wherein is not removed in its research completely, therefore, can not directly measure water body DON concentration.
Summary of the invention
In order to overcome existing DON measuring method length consuming time, precision is low, and degree of error is high, indirectly and the deficiencies such as complicated operation, the invention provides a kind ofly can 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, make in water sample DIN and DON composition carry out effectively separated, thereby realize the Measurement accuracy of water body DON.
The described micro-filtration filter membrane that used aperture to be not less than 0.22 μ m before pre-service but be not more than 0.7 μ m is removed the impurity in water sample.
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, the DC voltage that the voltage preferably adopting is <30v, and guarantee 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, both sides add nonnitrogenous salt solution and constantly update.
What add that salt solution will guarantee is to conduct electricity, but nonnitrogenous class material is to avoid interference.Preferred concentration is 0.5mol/l sodium chloride salt solution, or the concentration metabisulfite solution that is 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 are less than 0.1.
Preferred DON content detection scope 0.1mg/L-100mg/L of the present invention, but be not limited to the detection of higher or lower concentration.
After DIN in water sample and TDN ratio are less than 0.1, the pretreated water sample of power taking dialysis carries out TDN analysis, and the TDN concentration measuring is the concentration of DON in water sample.
Measuring method of the present invention can be for the analysis of DON in various water samples, and described water sample comprises that surface water, underground water, potable water, seawater, rainwater maybe can utilize water for other water samples of carrier.Wherein, can utilize other water samples that water is carrier to comprise solid particle or the atmospheric haze particle that is dissolvable in water water.
Electrodialysis isolation technics of the present invention realizes the effectively separated fast of DON and DIN in water body, and the TDN recording is subsequently DON.
Electrodialysis is to take electric field as charged particle driving force, and the selection permeability of the coupled ion exchange membrane isolation technics that is ultimate principle.Under the effect of electric field, amberplex can selectivity sees through little molecule inorganic nitrogen ion, but holds back large molecular polarity or without the organic nitrogen molecule of electric charge, therefore can realize the complete separated of inorganic nitrogen ion and organic nitrogen molecule.Utilize this mechanism can realize the quick and precisely measurement to DON in water body.
After electrodialysis pre-service completes, get pre-service after water sample carry out TDN analysis, the TDN concentration measuring can be equal to the concentration of 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:
Based on electrodialysis pretreatment mode, directly measure fast a method of DON in water body, comprising:
Detected water sample is removed to graininess impurity with the cellulose esters membrane filtration that aperture is 0.45 μ m, get and filter rear 50～100ml water sample, 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 using in electric dialyzator and cation-exchange membrane, and guarantee that in electrodialytic process, water sample pH remains between 1～10.The DC voltage that the voltage adopting is <30v.In electrodialysis preprocessing process, when the ratio of DIN and TDN is less than 0.1, stop electrodialysis preprocessing process.After processing, water sample TDN analyzes and adopts uv-spectrophotometric.The TDN concentration of 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 chamber concentration, light chamber ionic strength, ionic membrane area, adopts the water of artificial preparation to test, analyze DIN clearance and DON retention rate under different operational factor conditions, draw the optimal operating parameter of electric dialyzator.
Owing to having adopted such scheme, with respect to prior art, brought following beneficial effect, include but not limited to:
1, this method can effective separated water sample in DIN and DON, can be in 3 hours, more than 99% DIN is separated from water sample, thus after realizing pre-service, DON directly measures;
2, this method is than the dialysis membrane method for pretreating proposing in the world, and under identical separating effect (99%), its processing time is at least saved more than 40 times, thereby can realize the measurement of quick DON;
3, this method is compared than the NF membrane method for pretreating of domestic scholars, and under identical separating effect (90%), the time is saved more than 3 times, and operating conditions is simple, and without controlling pressure, temperature, directly measures TDN and just can obtain the concentration of DON after processing.
4, the ratio that this method DON runs off lower than 20%, therefore can realize the Measurement accuracy of DON for most of tested materials.
5, this measuring method revision test standard deviation, in 10% scope, has effectively improved accuracy and accuracy that DON measures.
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 substances under embodiment of the present invention
Fig. 5, the lower pretreated recovery design sketch of electrodialysis of the different DIN/DON values of the inventive method
Fig. 6, uses the directly measurement result comparison diagram to 5 natural waters of this method of the present invention
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, with the cellulose ester membrane of 0.45 μ m, the water sample of required test is filtered, elimination suspension, granule foreign (as can not measure in time, water after membrane filtration need be deposited in to the Refrigerator store of 4 degrees Celsius).
Second step: by the ionic membrane requirement of dispatching from the factory, amberplex is processed, and the good electrodialysis plant of Installation and Debugging, and guarantee that in electrodialytic process, water sample pH remains between 1～10.
The 3rd step: the good water sample of getting appropriate filtration is put into the light chamber of electrodialysis plant, in dense chamber, pass into salt solution, and load the constant DC voltage that is less than 30V, carry out electrodialysis pre-service (electrodialysis principle is shown in attached Fig. 1 and 2), the clearance effect of various nitrogen substances (seeing accompanying drawing 4).
The 4th step: the content of conductivity, DON and the DIN of water sample in the light chamber 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 (seeing accompanying drawing 5) of different DIN/TDN values.
The 5th step: get pretreated water sample in light chamber and carry out TDN analysis, TDN analyzes according to standard method (alkaline alkaline potassium per-sulfate digestion ultraviolet spectrophotometry HJ636-2012(Chinese Ministry of Environmental Protection)) carry out, adopt the instruments such as ultraviolet spectrophotometer or ion chromatograph to analyze, the TDN concentration measuring 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 parameter scheme shown in Fig. 3
Investigated the recovery and the degree of accuracy of organic nitrogen in natural water, by add quantitative DIN and DON in natural water, then DIN and DON content in tracking measurement water sample.According to the described implementation step of this programme, the recovery and the precision of contrast different time points DON, its effect is as accompanying drawing 5.
Result demonstration, 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 constantly reducing along with DIN, improve constantly, its relative percentage error is decremented to 2.3% by 33%.Proof, after electrodialysis pre-service, has 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 the concrete parameter scheme of implementing shown in Fig. 3
Investigated respectively lake, Shenzhen lake water, river, Shenzhen river, the water outlet of waterworks, Shenzhen, the DON content in the water inlet of Shenzhen's Sewage Plant and water outlet.
According to the invention process step, contrast respectively the DON measured value in water sample after not carrying out electrodialysis pre-service and having carried out electrodialysis pre-service, effect accompanying drawing 6.
Table 1: used instrument in experimentation
As can be seen from Figure 6, the water sample of several water bodys, when not carrying out electrodialysis pre-service, cannot obtain the concentration of the DON in water, even measures negative value; Adopt the pretreated DON measured value of electrodialysis, have good measurement result, revision test standard deviation, in 10% scope, has effectively improved accuracy and accuracy that DON measures.
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, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
Background technology list of references:
1.Plewa,M.J.,et al.,Halonitromethane Drinking Water Disinfection Byproducts:Chemical Characterization and Mammalian Cell Cytotoxicity and Genotoxicity.Environmental Science&Technology,2003.38(1):p.62-68.
2.Lee,W.and P.Westerhoff,Dissolved Organic Nitrogen Measurement Using Dialysis Pretreatment.Environmental Science&Technology,2004.39(3):p.879-884.
3.Chon,K.,et al.,Quantification and characterization of dissolved organic nitrogen in wastewater effluents by electrodialysis treatment followed by size-exclusion chromatography with nitrogen detection.Water Research,2013.47(14):p.5381-5391.
4.Xu,B.,et al.,Measurements of dissolved organic nitrogen(DON)in water samples with nanofiltration pretreatment.Water Research,2010.44(18):p.5376-5384。
Claims (8)
1. a method of measuring soluble organic nitrogen concentration (DON) in water body, it is characterized in that: adopt electrodialytic technique to carry out pre-service to water sample, inorganic nitrogen in water sample (DIN) ion and DON composition are carried out effectively separated, thereby realize the Measurement accuracy of water body DON.
2. method according to claim 1, is characterized in that: before pre-service, use aperture to be not less than 0.22 μ m but the micro-filtration filter membrane that is not more than 0.7 μ m is removed the impurity in water sample.
3. method according to claim 1, is characterized in that: described electrodialytic technique refers to that the electrodialysis mode of the DC voltage that adopts <30v carries out pre-service to water sample.
4. method according to claim 3, it is characterized in that: the amberplex in electric dialyzator used is chosen anion exchange membrane (AEM) and selectivity cation-exchange membrane (CEM), and guarantees that in electrodialytic process, water sample pH remains between 1～10.
5. method according to claim 1, is characterized in that: water sample, after electrodialysis preprocessing process, makes the content ratio of DIN and TDN in water sample be less than 0.1.
6. according to the method described in the arbitrary claim of claim 1 to 6, it is characterized in that: the pretreated water sample of power taking dialysis carries out total dissolubility nitrogen (TDN) analysis, and the TDN concentration measuring is the concentration of DON in water sample.
7. according to the method described in the arbitrary claim of claim 1 to 6, it is characterized in that: described water sample comprises that surface water, underground water, potable water, seawater, rainwater maybe can utilize other materials that water is carrier.
8. method according to claim 7, is characterized in that: can utilize other materials that water is carrier to comprise solid particle or the atmospheric haze particle that is dissolvable in water water.
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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 |
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| 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 |
| CN106769946A (en) * | 2017-01-20 | 2017-05-31 | 南京大学 | Soluble organic nitrogen concentration detection method in a kind of sewage based on dialysis pretreatment |
| WO2018133378A1 (en) * | 2017-01-20 | 2018-07-26 | 南京大学 | Dialysis pretreatment-based method for measuring concentration of dissolved organic nitrogen in municipal sewage |
| 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 |
| 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 |
| 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 |
| 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 |
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