CN107219102A - A kind of method of soluble organic nitrogen concentration in superposition of electric field pretreatment mode direct measurement water body based on dialysis - Google Patents
A kind of method of soluble organic nitrogen concentration in superposition of electric field pretreatment mode direct measurement water body based on dialysis Download PDFInfo
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Abstract
The method that one kind determines soluble organic nitrogen (DON) concentration in water body, using the mode based on dialysis superposition of electric field, makes (DIN) ion of inorganic nitrogen in water sample be effectively separated with DON compositions, so as to realize water body DON accurate measurement.Using electric field as charged ion driving force, DIN is mainly the small charged ion of relative molecular weight, can pass through dialyser；Relative molecular weight is big, uncharged DON is retained by dialyser, so as to reach separation DON and DIN purpose.Take water sample of the appropriate volume after micro-filtration membrane filtration, put into inside dialyser, and unazotized salt solution is added in dialyser both sides superposition constant pressure or constant current electric field, and in both sides, continuous updating salt solution, make in film ion in the presence of the electric field fast transferring to outside film.Water sample is after preprocessing process, and DON accounts for TDN leading position in water sample.The pretreated water sample of dialysis superposition of electric field of learning from else's experience carries out total dissolubility nitrogen (TDN) analysis, and it is DON concentration in water sample to measure obtained TDN concentration.
Description
Technical field
The invention belongs to environmental protection, water treatment field, specially utilize and be based on dialysis superposition of electric field processing mode, directly
The method for measuring soluble organic nitrogen (DON) concentration in water body.It can apply with environmental protection and all kinds of utilization water as in carrier
DON measurement, such as water process, ocean, agricultural fertilizer and atmospheric haze.
Background technology
Nitrogen has very important effect in geochemical cycle.Total nitrogen (TDN) includes organic nitrogen (DON) and nothing
Machine nitrogen (DIN).Total nitrogen (TDN) concentration in natural water water sample is to weigh the important indicator of water quality, wherein soluble organic nitrogen
(DON) be total nitrogen important component.DON can support body eutrophication, cause the microorganisms such as algae, bacterium largely numerous
Grow, be contaminated water source.In water system, DON is capable of the growth of cooperating microorganisms, cause in unit for treating water filter tank or
The blocking of film, so as to reduce water factory's water outlet efficiency.In water factory's disinfecting process, DON can produce strong toxicity with disinfectant reaction and contain
Nitrogen DBPs (N-DBPs).Also cause the life of three causes (carcinogenic, teratogenesis, mutagenesis) DBPs (DBPs) simultaneously
Into[1]1428.Therefore, in order to prevent and control DON harm, it is necessary to quick and precisely measure organic nitrogen concentration.
Although the problem of having appreciated that organic nitrogen, the method for quick and precisely measuring organic nitrogen is there is no at present.It is existing
Organic nitrogen method of testing be all to be obtained indirectly by subtracting poor method without exception.Conventional method has total nitrogen to subtract inorganic nitrogen at present
Two kinds of ammonia nitrogen is subtracted with total Kjeldahl nitrogen.
Method one：
Organic nitrogen (DON)=total nitrogen (TDN)-inorganic nitrogen (DIN) (1-1)
DIN=ammonia nitrogens (NH4 +)+nitrate nitrogen (NO3 -)+nitrite nitrogen (NO2 -) (1-2)
Method two：
Organic nitrogen (DON)=total Kjeldahl nitrogen (TKN)-ammonia nitrogen (NH4 +) (1-3)
In order to improve the accuracy of organic nitrogen measurement, reduce error and reduce the fussy degree in measurement process, portion
Scholar is divided to propose various corrective measures.Some scholars obtain more by being pre-processed to water sample, directly or indirectly
Accurate organic nitrogen concentration.But the difficult point for the pretreatment of water sample is the reservation for the removal and DON for causing DIN while most
Bigization.The method of these pretreatments includes four major classes：Membrane separating method, adsorption method, catalysis process and pre-concentration method.
Available data shows that the method in dialyser is more favored in many researchs, but time-consuming for this method, water consumption
Greatly, it is not particularly suited for promoting the use of on a large scale[2,3,4].Although electrodialytic method and the method for counter-infiltration are not applied to organic
The detection of nitrogen, it is well known that, both approaches are shown very well in terms of the removal of inorganic ions and the retention of organic matter
Effect.There is relatively good achievement in a few cases using the method for ion exchange resin, chromatographic column or adsorbent, still
The loss of organic nitrogen is larger[5,6].Therefore, the application of this technology is also to be developed.
South Korea scholar Lee et al. is pre-processed using the method for dialyser to water sample, and high DIN/TDN water sample is held
It is deionized water outside film in permeable membrane, and deionized water updates within the regular hour, using concentration gradient, makes nothing in film
Machine nitrogen material is moved in deionized water in film, reaches removal inorganic nitrogen, retains the purpose of organic nitrogen[2]880.This research selection
Molecular cut off is 100Da dialyser, that is, passes through the effect of film so that small molecular weight material is divided from macromolecule material
From.This studies the separating effect for demonstrating organic nitrogen and inorganic nitrogen, and applied to the detection of organic nitrogen.In dialysis 24h,
70% inorganic nitrogen can be removed, while the rate of recovery of organic nitrogen can reach more than 80%, average recovery rate is 95% (except urea
Outside), it was demonstrated that dialyser can reduce DIN/TDN.By extending pretreatment time, higher DIN removal can be reached,
During the dialysis of 5 days, DIN clearance can reach 99%.
Also there are some scholars using electrodialysis methods to separate organic matter and inorganic matter in addition.Although electrodialysis methods are ground
Study carefully comparative maturity, and effect is preferable in terms of separation organic matter and inorganic matter.But it is mainly used in desalinization, water body at present
In terms of softening desalination, and application is had no in organic nitrogen context of detection.Although this technology has not been used to the measurement of organic nitrogen,
But show that electrodialysis removes the speed of nitrate nitrogen much larger than dialyser in the research that electrodialysis removes inorganic matter[7]。
Domestic also less to the organic nitrogen studies of quick, Accurate Determining, Shanghai Tongji University Xu Bin et al. uses NF membrane
Pretreatment 4 hours is carried out to the water sample of high DIN/TDN ratios, part inorganic nitrogen is removed, retains organic nitrogen, reach concentration organic nitrogen
Purpose, so as to improve the accuracy and precision of organic nitrogen measurement, and achieve preferable effect.Nanofiltration is used in experiment
The molecular cut off of film is about 200Da.The preprocess method of nanofiltration membrane pretreatment method and dialyser has similarity, only
It is that removal of inorganic nitrogen power is changed into barometric gradient, both have similar effect in terms of the measurement accuracy of organic nitrogen, but may be used
To save at least 20 hours and substantial amounts of deionized water.Also nanofiltration membrane pretreatment method is optimized by Xu Bin et al., respectively
Studied in the type of NF membrane, sample volume and film surface area ratio, the pH value of solution and in terms of film pressure, utilized excessively
The method is pre-processed to the water body of high DIN/TDN ratios, has reached the purpose for improving organic nitrogen measurement accuracy and precision.
But also its weak point is pre-processed to water sample using NF membrane, this method can not make inorganic nitrogen all removals,
Research shows that the clearance that the clearance of nitrate is 69%~92%, ammonia nitrogen is 72%~77%, while the reservation of organic matter
For 77~82%[4]5376.Old white poplar of Harbin Institute of Technology et al. is pre-processed using electrodialysis mode to water sample[8][9], lead to
Amberplex is crossed, in the presence of electric field, DIN is removed, retains DON, after pretreatment, it is DON's to measure obtained TDN values
Value.The method achieve DON quick and precisely measurement, but DON the rate of recovery 93%~110%, percentage ratio error is
2.3%, further improved method it can also continue to optimize.
The content of the invention
In order to overcome existing DON measuring methods, time-consuming, and precision is low, degree of error height, the indirectly deficiency such as complex operation,
The invention provides a kind of method that can realize direct, quick, accurate measurement water body DON.
The technical solution adopted in the present invention is：
The method of DON concentration, based on the mode of dialysis superposition of electric field, is pre-processed to water sample in a kind of measure water body,
(DIN) ion of inorganic nitrogen in water sample is set to be effectively separated with DON compositions, so as to realize water body DON accurate measurement.
The dialysis superposition of electric field technology refers to that during dialysis superposition of electric field is pre-processed to water sample；With tradition
Electrodialytic technique is distinguished as：The film that dialysis superposition of electric field technology is used is dialyser, by selecting suitable dialysis membrane aperture,
Pass through inorganic ions, and (with below and repeat) organic substance that makes molecular weight larger is trapped, and outside dialyser
DC electric field is superimposed, makes ion accelerate to move to the outside of dialyser.
The dialysis superposition of electric field technology, using electric field as charged ion driving force, it is small that DIN is mainly relative molecular weight
Charged ion, can pass through dialyser；Relative molecular weight is big, uncharged DON is retained by dialyser, so as to reach separation
DON and DIN purpose.
In set-up procedure before pre-processing, 0.22 μm but no more than 0.7 μm of micro-filtration filter membrane is not less than using aperture
Impurities in water is removed, the micro-filtration filter membrane can select cellulose ester membrane, and preferably membrane aperture is 100~500Daltons.
Take inside the water sample after micro-filtration membrane filtration of appropriate volume, input dialyser, (with below and repeatedly)
Constant pressure or constant current electric field are superimposed in dialyser both sides, and unazotized salt solution is added in both sides, continuous updating salt solution makes in film
Ion in the presence of the electric field fast transferring to outside film (as shown in Figure 1).
Added salt solution purpose is to ensure solution (powered), and does not introduce nitrogen class material to avoid interference, and preferred concentration is
0.5mol/L sodium chloride brines, or the metabisulfite solution that concentration is 0.01mol/L.
The superposition of electric field refers to the DC voltage of constant pressure or constant current electric field, preferably voltage ＜ 30V, and ensures pre- place
Water sample pH is maintained between 1~10 during reason.
After preprocessing process, DON accounts for TDN leading position in water sample, the average removal rate of inorganic nitrogen in 90min
For 98%, wherein nitrate nitrogen and nitrite nitrogen can reach the flat of the typical organic nitrogen that is selected in almost 100% removal, experiment
Equal retention rate is 90% (in addition to glutamic acid).
The dialysis superposition of electric field pretreatment will not change the structure of organic nitrogen.After dialysis superposition of electric field of learning from else's experience pretreatment
Water sample carry out the analysis of total dissolubility nitrogen (TDN), it is DON concentration in water sample, wherein TDN analyses to measure obtained TDN concentration
Can using ultraviolet spectrophotometry, combustion method, clear up after survey the method such as nitrate ion and analyzed.
The DON detections of the dialysis superposition of electric field preprocess method are limited to 0.033mg-N/L, and its accuracy is 0.03.
The measuring method of the present invention can be used for the analysis of DON in various water samples, including surface water, underground water, drinking water,
Seawater, rainwater etc., can also be applied to, using other water samples that water is carrier, such as be dissolvable in water the solid particle or big aerosol of water
Haze particle etc..
The dialysis superposition of electric field pretreatment system operational factor determined by experimental program, operational factor include voltage,
Flow velocity, dense room concentration, light room ionic strength, dialysis membrane area etc., are tested by the water sample of human configuration, analyze different fortune
DIN clearances and DON retention rates under row Parameter Conditions, draw optimal operating parameter.
The preprocess method of the present invention, following beneficial effect is brought relative to prior art, is included but is not limited to：
This method can efficiently separate DIN and DON in water sample, and the average removal rate of inorganic nitrogen is 98% in 90min,
Wherein nitrate nitrogen and nitrite nitrogen can reach almost 100% removal, so as to realize DON direct measurements.
The average retention rate of the typical organic nitrogen selected in experiment is 90% (in addition to glutamic acid), and dialysis powers up pre- place
Reason will not change the structure of organic nitrogen.
This method is compared to the dialysis membrane pretreatment method proposed in the world, under identical separation effect (99%), at it
The reason time at least saves 60 times, it is possible to achieve DON quick measurement.
This method is compared compared to the nanofiltration membrane pretreatment method of domestic scholars, under identical separation effect (90%), the time
Save more than 4 times, it is possible to achieve DON quick measurement.
The ratio that this method DON is lost in is less than 20% for most tested material, it is possible to achieve DON's is accurate
Measurement.
This method repeats testing standard deviation in the range of 10%, effectively increases the accuracy and accuracy of DON measurements.
Brief description of the drawings
Fig. 1, dialysis superposition of electric field preprocess method principle schematic of the present invention
The clearance design sketch of nitrogen substance after Fig. 2, dialysis superposition of electric field preprocessing process of the present invention
The rate of recovery design sketch of the lower pretreatment of Fig. 3, the inventive method difference DIN/DON value
Fig. 4, with measurement result comparison diagram of the inventive method to natural water
Embodiment
With reference to implementing, the invention will be further described with accompanying drawing：
Embodiment 1：
Specific total embodiment and step
The first step：Before pre-processing, the water sample of required test is filtered with 0.45 μm of cellulose ester membrane, filtered off
Suspension, granule foreign.
Second step, is handled dialyser by use requirement on dialyser specification, the good electric field arrangement of installation and debugging, and
Ensure that water sample pH is maintained between 2~10 in dialysis superposition of electric field preprocessing process.
3rd step, takes the appropriate water sample filtered to be put into the light room of electrodialysis plant, salt solution is passed through in dense room, and load
Constant DC voltage less than 30V, is pre-processed (schematic diagram is shown in accompanying drawing 1), and the removal effect of various nitrogen substances is shown in accompanying drawing 2
4th step, monitor in real time water sample in light room-(TDN), DON, DIN content, when DIN in water sample and TDN ratios
During less than 0.1, stop preprocessing process, accompanying drawing 3 is seen for the recovering effect of the pretreatment under different DIN/TDN values.
5th step, takes pretreated water sample in light room to carry out TDN analyses, TDN is analyzed according to standard method (alkaline over cure
Sour potassium clears up ultraviolet spectrophotometry HJ636-2012 Chinese Ministry of Environmental Protection) carry out, using ultraviolet specrophotometer or ion chromatograph etc.
Instrument is analyzed, and it is DON concentration in raw water sample to measure obtained TDN concentration.
Embodiment 2：
According to the specific overall plan and step of embodiment 1, the rate of recovery and accuracy of DON in natural water have been investigated,
Quantitative DIN and DON by being added into natural water, then DIN and DON contents in tracking measurement water sample.
According to the implementation steps described by this programme, contrast different time points the DON rate of recovery and precision, its design sketch is such as
Accompanying drawing 4.
As a result show, with the progress of dialysis superposition of electric field preprocessing process, DIN concentration is constantly reduced, DIN/DON ratio
Value also constantly reduces, and the DON rate of recovery is 100% ± 5%, and measurement accuracy is improved constantly with DIN continuous reduction, therefore
The accuracy and precision of organic nitrogen measurement can be significantly improved by powering up the organic nitrogen concentration of preprocess method measurement using dialysis.
Table 1：Used instrument in experimentation
Background technology and bibliography
[1] Her N, Amy G, Park H R, et al.Characterizing Algogenic Organic Matter
(Aom) and Evaluating Associated Nf Membrane Fouling [J] .Water Research, 2004,38
(6)：1427-1438.
[2] Lee W T, Westerhoff P.Dissolved Organic Nitrogen Measurement Using
Dialysis Pretreatment [J] .Environmental Science＆Technology, 2005,39 (3)：879-884.
[3] Vandenbruwane J, Neve S D, Qualls R G, et al.Optimization of
Dissolved Organic Nitrogen(Don)Measurements in Aqueous Samples with High
Inorganic Nitrogen Concentrations [J] .Science of the Total Environment, 2007,
386(1-3)：103-113.
[4] Xu B, Li D-P, Li W, et al.Measurements of Dissolved Organic Nitrogen
(Don) in Water Samples with Nanofiltration Pretreatment [J] .Water Research,
2010,44 (18)：5376-5384.
[5] Huber S A, Balz A, Abert M, et al.Characterisation of Aquatic Humic
and Non-Humic Matter with Size-Exclusion Chromatography--Organic Carbon
Detection--Organic Nitrogen Detection (Lc-Ocd-Ond) [J] .Water Research, 2011,45
(2)：879-885.
[6]Sattayatewa.Measurement of Organic Nitrogen and Phosphorus
Fractions at Very Low Concentrations in Wastewater Effluents[J].Water
Environment Research, 2011,83 (8)：675-683.
[7] Abou-Shady A, Peng C, Almeria O J, et al.Effect of Ph on Separation
of Pb(Ii)and No3-from Aqueous Solutions Using Electrodialysis[J]
.Desalination, 2012,285：46-53.
[8] Anbang Zhu, Baiyang Chen, Liang Zhang et al.Improved Analysis of
Dissolved Organic Nitrogen in Water via Electrodialysis Pretreatment[J]
.Anal.Chem.2015,87：2353-2359
[9] Chen Baiyang, Zhu Anbang, beautiful one kind is based on soluble organic nitrogen in electrodialysis pretreatment mode measurement water body
Method China .201410140134.3 [P] 2014.08.06. of concentration
Claims (7)
1. the method that one kind determines soluble organic nitrogen (DON) concentration in water body, it is characterised in that：Using dialysis superposition of electric field skill
Art makes inorganic nitrogen (DIN) ion be effectively separated to realize DON accurate measurement with DON compositions.
2. according to the method described in claim 1, it is characterised in that：The dialysis superposition of electric field technology refers in dialysis process
In, superposition of electric field is pre-processed to water sample.
3. according to the method described in claim 1, it is characterised in that：The exchange membrane that the dialysis superposition of electric field technology is selected is to ooze
Film is analysed, membrane aperture is 100~500Daltons.
4. according to the method described in claim 1, it is characterised in that：Water sample is contained on the inside of dialyser, on the outside of dialyser
Electric field is added, and in order that ion can be migrated, electrolyte is added outside film.
5. according to the method described in claim 1, it is characterised in that：The dialysis superposition of electric field technology and conventional electrodialysis technology
Difference be that the film that the technology is used is dialyser, by selecting suitable dialysis membrane aperture, pass through inorganic ions, and
The organic substance for making molecular weight larger is trapped.
6. the method according to any claim of claim 1, it is characterised in that：Dialysis superposition of electric field of learning from else's experience is pre-processed
Water sample afterwards carries out total dissolubility nitrogen (TDN) analysis, and it is DON concentration in water sample to measure obtained TDN concentration.
7. the method according to any claims of claim 1-5, can be applied to the analysis of DON in various water samples, including
Surface water, underground water, drinking water, seawater, rainwater etc., can also be applied to, using other water samples that water is carrier, such as can dissolve
In solid particle or atmospheric haze particle of water etc..
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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 |
| 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 |
| CN113624831A (en) * | 2021-08-05 | 2021-11-09 | 广东农工商职业技术学院 | Method for separating enriched sediment organic nitrogen and determining isotope and content |
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Application publication date: 20170929 |