CN101419173A - Method for synchronistically detecting triaza concentration in water - Google Patents
Method for synchronistically detecting triaza concentration in water Download PDFInfo
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- CN101419173A CN101419173A CNA200810227699XA CN200810227699A CN101419173A CN 101419173 A CN101419173 A CN 101419173A CN A200810227699X A CNA200810227699X A CN A200810227699XA CN 200810227699 A CN200810227699 A CN 200810227699A CN 101419173 A CN101419173 A CN 101419173A
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- water sample
- nitrous
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 238000000034 method Methods 0.000 title claims abstract description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 106
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 53
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims abstract description 19
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005259 measurement Methods 0.000 claims abstract description 9
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims abstract 6
- MGSRCZKZVOBKFT-UHFFFAOYSA-N thymol Chemical compound CC(C)C1=CC=C(C)C=C1O MGSRCZKZVOBKFT-UHFFFAOYSA-N 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 15
- 239000003153 chemical reaction reagent Substances 0.000 claims description 12
- 239000005844 Thymol Substances 0.000 claims description 9
- 229960000790 thymol Drugs 0.000 claims description 9
- YUVLVONHNMXKBW-UHFFFAOYSA-L [Ag+2].OS(O)(=O)=O.[O-]S([O-])(=O)=O Chemical compound [Ag+2].OS(O)(=O)=O.[O-]S([O-])(=O)=O YUVLVONHNMXKBW-UHFFFAOYSA-L 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 claims description 5
- 229940074439 potassium sodium tartrate Drugs 0.000 claims description 5
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 4
- 230000001360 synchronised effect Effects 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- GEHMBYLTCISYNY-UHFFFAOYSA-N Ammonium sulfamate Chemical compound [NH4+].NS([O-])(=O)=O GEHMBYLTCISYNY-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims 2
- 238000004737 colorimetric analysis Methods 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 11
- 239000000126 substance Substances 0.000 abstract description 8
- 238000001514 detection method Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 238000005070 sampling Methods 0.000 abstract description 2
- 238000004448 titration Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 25
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 16
- 238000002835 absorbance Methods 0.000 description 11
- 238000005303 weighing Methods 0.000 description 9
- JVMRPSJZNHXORP-UHFFFAOYSA-N ON=O.ON=O.ON=O.N Chemical compound ON=O.ON=O.ON=O.N JVMRPSJZNHXORP-UHFFFAOYSA-N 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 7
- 238000012544 monitoring process Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 4
- 239000011550 stock solution Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- -1 polyethylene Polymers 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 238000000338 in vitro Methods 0.000 description 2
- 238000005375 photometry Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000001915 proofreading effect Effects 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical compound NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- NULAJYZBOLVQPQ-UHFFFAOYSA-N N-(1-naphthyl)ethylenediamine Chemical compound C1=CC=C2C(NCCN)=CC=CC2=C1 NULAJYZBOLVQPQ-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- RCTYPNKXASFOBE-UHFFFAOYSA-M chloromercury Chemical compound [Hg]Cl RCTYPNKXASFOBE-UHFFFAOYSA-M 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229960002523 mercuric chloride Drugs 0.000 description 1
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical compound Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- VZOPRCCTKLAGPN-ZFJVMAEJSA-L potassium;sodium;(2r,3r)-2,3-dihydroxybutanedioate;tetrahydrate Chemical compound O.O.O.O.[Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O VZOPRCCTKLAGPN-ZFJVMAEJSA-L 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- XSNQEMWVLMRPFR-UHFFFAOYSA-N silver nitride Chemical compound [N-3].[Ag+].[Ag+].[Ag+] XSNQEMWVLMRPFR-UHFFFAOYSA-N 0.000 description 1
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
- 229940074446 sodium potassium tartrate tetrahydrate Drugs 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
一种同步测定水中三氮浓度的方法属于水处理过程中的水质人工检测领域。具体涉及专用于测定水中三种氮素的含量。三氮检测方法的主要原理为化学滴定显色反应，其使用化学药品物耗比较大，而对于人工取样化验，虽然可以减少化学药品的消耗，但由于各方法的繁琐性，使得化验过程费时费力。本发明结合三氮检测各自的特点，以硝氮的测定为主线，在其测定过程中的放置时间内，进行了氨氮水样和亚氮水样的定容以及药剂投加。本发明在物耗成本较为经济的前提下，大大缩短了其测定时间。A method for synchronously measuring the concentration of trinitrogen in water belongs to the field of manual detection of water quality in the water treatment process. It is specifically related to the determination of three kinds of nitrogen content in water. The main principle of the trinitrogen detection method is the color reaction of chemical titration, which consumes a lot of chemicals. For manual sampling and testing, although the consumption of chemicals can be reduced, due to the cumbersomeness of each method, the testing process is time-consuming and laborious. The present invention combines the respective characteristics of trinitrogen detection, takes the determination of nitrate nitrogen as the main line, and carries out the constant volume of ammonia nitrogen water samples and nitrous nitrogen water samples and the addition of medicaments during the storage time during the measurement process. The invention greatly shortens the measurement time under the premise that the material consumption cost is comparatively economical.
Description
Technical field
The invention belongs to the water quality manual detection field in the water treatment procedure.Be specifically related to be exclusively used in the content of measuring three kinds of nitrogens in the water.
Background technology
The nitrogen index is the important indicator in the water quality detection.Three nitrogen are meant ammonia nitrogen (NH
4 +-N), nitrite nitrogen (NO
2 --N is called for short inferior nitrogen) and nitrate nitrogen (NO
3 --N is called for short nitre nitrogen), they can transform in water mutually, often need simultaneously its concentration to be detected.The method of three nitrogen is the standard of China's promulgation in 1987, i.e. NH always in the measurement water commonly used at present
4 +-N adopts nessler reagent photometry (GB747987), NO
2 --N adopts N-(1-naphthyl)-ethylenediamine photometry (GB749387), NO
3 --N adopts thymol spectrophotometric method (GB748087).
Because the cardinal principle of above-mentioned three nitrogen detection methods is the chemistry titration chromogenic reaction, it uses the chemicals material consumption bigger, especially for on-line monitoring, has improved the cost of water quality monitoring more.And for the hand sampling chemical examination, though can reduce the consumption of chemicals, because the loaded down with trivial details property of each method makes the chemical examination process waste time and energy.The problems referred to above make in the process that three nitrogen are monitored in to water, are difficult to the effect of the quick and cost economy of preparation method simultaneously.
Summary of the invention
The objective of the invention is to solve the problem that existing three nitrogen monitoring agility and economy are difficult to realize simultaneously, and a kind of method that detects three nitrogen concentrations in the water simultaneously and rapidly is provided.
The method of three nitrogen concentrations is characterized in that in a kind of synchronous mensuration water provided by the present invention, may further comprise the steps:
1) water sample to be measured is divided into 3 groups, is called nitre nitrogen water sample, ammonia nitrogen water sample and inferior nitrogen water sample, and every group is all done omnidistance blank determination with pure water;
Nitre nitrogen water sample, ammonia nitrogen water sample and inferior nitrogen water sample all are the same in original state in fact;
2) add sulfaminic acid ammonia in the nitre nitrogen water sample, shake up the back and placed 5-10 minute;
3) in step 2) in time of placing, ammonia nitrogen water sample and inferior nitrogen water sample are carried out constant volume with pure water;
4) add thymol in the nitre nitrogen water sample earlier, add the silver sulfate sulfuric acid solution after shaking up again, placed 5-10 minute behind the mixing;
In the time of 5) in step 4), placing, in inferior nitrogen water sample, add inferior nitrogen developer; Add potassium sodium tartrate solution in the ammonia nitrogen water sample earlier, after the mixing, add nessler reagent again, mixing;
6) in nitre nitrogen water sample, add ammoniacal liquor behind the adding pure water, carry out constant volume with pure water then;
7) carry out colorimetric according to the order of ammonia nitrogen, inferior nitrogen and nitre nitrogen;
8) carry out the concentration that data processing draws three nitrogen in the water sample to be measured.
In the concrete steps method, because the mensuration of nitre nitrogen is the most consuming time, so, in conjunction with three nitrogen detection characteristics separately, with the main line that is determined as of nitre nitrogen, in the standing time in its mensuration process, the constant volume and the medicament that have carried out ammonia nitrogen water sample and inferior nitrogen water sample add.More than various material additions be general knowledge in the prior art field, a kind of method that detects three nitrogen concentrations in the water simultaneously and rapidly provided by the present invention, be on the basis of original each national standard method, its combination and pool are optimized, under the comparatively economic prerequisite of material consumption cost, shortened its minute greatly.
Embodiment
Below in conjunction with embodiment the present invention is further described, but protection scope of the present invention is not limited thereto.
Embodiment
Test has been carried out artificial long term monitoring to three nitrogen water quality in the tertiary treatment process of certain community life sewage, utilizes said method, not only economy but also quick, and cost can reduce more than 90% than on-line monitoring, and manually the time of chemically examining can reduce more than 50%.
1) method principle
NH
4 +Wavelength 420nm is adopted in the measurement of-N; NO
2 --N adopts wavelength 540nm; NO
3 --N adopts wavelength 415nm.
2) scope of application
If get the 1mL water sample, NH
4 +The measurement concentration of-N should be less than 100mg/L; NO
2 -The measurement concentration of-N should be less than 20mg/L; NO
3 -The measurement concentration of-N should be less than 20mg/L.When estimating that water sample three nitrogen concentration values to be measured are higher, need dilute.
3) key instrument
3 of test tube racks (can put 12 test tubes), 36 in 50mL test tube, 2 of liquid-transfering guns (range is respectively 20-200 μ L and 100-1000 μ L), 1 of rubber pipette bulb, 1 in 10mL transfer pipet, 2 of 100mL reagent bottles (band glue head dropper), 1 and 2 of 2cm of cuvette 1cm, 1 in spectrophotometer.Other glassware (beaker, volumetric flask, reagent bottle etc.) is some.
4) reagent
A. survey NH
4 +-N reagent
Potassium sodium tartrate solution: take by weighing 500g sodium potassium tartrate tetrahydrate (KNaC
4H
4O
64H
2O) be dissolved in the 1000mL water, heated and boiled to be to remove deammoniation, puts coldly, is settled to 1000mL.
Nessler reagent: take by weighing the 50g potassium iodide and be dissolved in about 250mL water, gradation while stirring adds mercuric chloride (HgCl on a small quantity
2) crystalline powder (about 25g), when vermilion precipitation occurring and be difficult for dissolving, change into and drip saturated liquor hydrargyri perchloridi, and fully stir, when micro-vermilion precipitation occurring and be difficult for dissolving, stop to drip liquor hydrargyri perchloridi.It is water-soluble that other takes by weighing 150g potassium hydroxide, and be diluted to 625mL, fully be cooled to room temperature after, with above-mentioned solution under agitation, inject potassium hydroxide solution slowly, be diluted with water to 1000mL, mixing.Standing over night.Supernatant is moved in the polyethylene bottle, and close plug is preserved.
Ammonium standard stock solution: take by weighing 3.819g through 100 ℃ of dry pure ammonium chloride (NH of top grade that cross
4Cl) soluble in water, move in the 1000mL volumetric flask, be diluted to graticule.This solution contains the 1.00mg ammonia nitrogen for every milliliter.
The ammonium standard is used solution: pipette 5.00mL ammonium standard stock solution in the 500mL volumetric flask, be diluted with water to graticule.This solution contains 0.010mg ammonia nitrogen (10mg/L) for every milliliter.
B. survey NO
2 --N reagent
Inferior nitrogen developer: in the 1000mL beaker, add 500mL water and 100mL phosphoric acid (ρ=1.70g/mL), add 40.0g right-aminobenzene sulfonamide, again with 2.00gN-(1-naphthyl)-ethylenediamine dihydrochloride (C
10H
7NHC
2H4NH
22HCl) be dissolved in the above-mentioned solution, be transferred in the 1000mL volumetric flask, be used to be diluted to graticule, mixing.This solution is stored in the brown bottle, is kept at 2～5 ℃, can stablize one month at least.
Nitrite nitrogen standard stock solution: take by weighing 1.232g sodium nitrite (NaNO
2) be dissolved in the 150mL water, be transferred in the 1000mL volumetric flask, be diluted with water to graticule.Every milliliter contains about 0.25mg nitrite nitrogen (ρ NO
2 --N=0.25mg/mL).This solution is stored in the brown bottle, adds the 1mL methenyl choloride, is kept at 2～5 ℃, can stablize one month at least.
Nitrite nitrogen standard intermediate liquid: divide and get 50.00mL nitrite standard stock solution (make and contain the 12.5mg nitrite nitrogen), place the 250mL volumetric flask, be diluted with water to graticule.This solution contains 50.0 μ g nitrite nitrogen (ρ NO for every milliliter
2 --N=50.0 μ g/mL).Intermediate liquid is stored in the brown bottle, is stored in 2～5 ℃, can stablize a week at least.
The nitrite nitrogen standard is used liquid: get 10.00mL nitrite standard intermediate liquid, place the 500mL volumetric flask, be diluted with water to graticule.Every milliliter contains 1.00 μ g nitrite nitrogens.When this solution uses, preparation on the same day.
C. survey NO
3 --N reagent
Sulfaminic acid ammonium salt solution (20g/L): take by weighing 10.0g Amcide Ammate (NH
4SO
3NH
2), with acetic acid solution (1+4) dissolving, and dilution is 500ml.
Thymol ethanolic solution (5g/L): take by weighing 5.0g thymol [(CH
3) (C
3H
7) C
6H
3OH, Thymol has another name called thymol], be dissolved in the absolute ethyl alcohol, and be diluted to 1000ml.
Silver sulfate sulfuric acid solution (10g/L): take by weighing 25.0g silver sulfate (Ag
2SO
4), be dissolved in 2500ml sulfuric acid (ρ
20=1.84g/mL) in.
Ammoniacal liquor (ρ
20=0.88g/mL).
Nitrate nitrogen standard reserving solution [ρ (NO
3 --N)=and 1mg/mL]: take by weighing the potassium nitrate (KNO of 7.218g through 105～110 ℃ of dry 1h
3), be dissolved in the pure water, and be settled to 1000ml.Adding the 2ml chloroform is preservative agent.
The nitrate nitrogen standard is used solution [ρ (NO
3 --N)=10 μ g/ml]: draw 5.00ml nitrate nitrogen standard reserving solution and be settled to 500ml.
5) measuring process
A. the drafting of typical curve
The ammonia nitrogen graticule: absorption 0,0.50,1.00,3.00,5.00,7.00 and 10.00mL ammonium standard are used in liquid and the 50mL color comparison tube, add water to graticule, add the 1.0mL potassium sodium tartrate solution, mixing.Add the 1.5mL nessler reagent, mixing.After placing 10min,,, be reference, measure absorbance with water with light path 20mm cuvette at wavelength 420nm place.By the absorbance that records, deduct the absorbance of zero-dose blank after, obtain proofreading and correct absorbance, draw with ammonia-nitrogen content (mg) proofreading and correct the calibration curve of absorbance.
Inferior nitrogen graticule: in one group of 6 50mL color comparison tube, add respectively 0,1.00,3.00,5.00,7.00 and 10.00mL nitrite nitrogen standard use liquid, be diluted with water to graticule.Add the 1.0mL developer, close plug, mixing.After leaving standstill 20min, in 2h,,, be reference, measure absorbance with water with the cuvette of optical length 10nm in wavelength 540nm place.From the absorbance that records, deduct the absorbance log of the blank pipe of zero-dose after, obtain to proofread and correct absorbance, drawing with nitrogen content (μ g) serve as the calibration curve of correction absorbance.
Nitre nitrogen graticule: get the 1.00ml water sample in the 50ml of drying color comparison tube.Other gets 7 of 50ml color comparison tubes, adds the nitrate nitrogen standard respectively and uses solution 0,0.05,0.10,0.30,0.50,0.70, and 1.00ml is diluted to 1.00ml with pure water.In each pipe, add 0.1ml sulfaminic acid ammonium salt solution, shake up the back and place 5min.Respectively add 0.2ml thymol ethanolic solution.Place 5min after adding 2ml silver sulfate sulfuric acid solution mixing after shaking up.Add the 8ml pure water, dropping ammonia to solution yellow reaches the darkest behind the mixing.And till silver nitride precipitation is dissolved (adding 9ml approximately).Add pure water to 25ml scale, mixing.In the 415nm wavelength, the 2cm cuvette is a reference with the pure water, measures absorbance.The drawing standard curve is found the quality of nitrate nitrogen the sample from curve.
B. the mensuration of water sample
Add water sample with liquid-transfering gun, and, do omnidistance preface blank determination with no aqueous ammonia to replace water sample.When nitre nitrogen water sample respectively in vitro guarantees to 1mL, add sulfaminic acid ammonia 0.1mL, shake up back placement 5-10 minute.Ammonia nitrogen and inferior nitrogen test tube are settled to 50mL, and this step was controlled at about 5 minutes.Nitre nitrogen in vitro adds thymol 0.2mL earlier, shakes up the back and adds 2ml silver sulfate sulfuric acid solution, places 5-10 minute behind the mixing.Inferior nitrogen test tube adds developer; The ammonia nitrogen test tube adds the 1mL potassium sodium tartrate solution earlier, and mixing adds the 1.5mL nessler reagent again, mixing, and this step was controlled at about 5 minutes.Nitre nitrogen test tube is opened spectrophotometer after adding about 7-9mL pure water, carries out ammoniacal liquor at ventilating kitchen again and adds, and is settled to 25mL at last.Colorimetric is according to the order of ammonia nitrogen, inferior nitrogen and nitre nitrogen.
C. data processing
According to above-mentioned graticule,, draw the concentration of three nitrogen in the water quality of surveying at last with excel list processing (LISP) data.
ρ＝m/V
In the formula: ρ is the mass concentration of three nitrogen (in N) in the water sample, mg/L;
M is for checking in the quality of three nitrogen from typical curve;
V is a volume of water sample, mL.
Compare with three nitrogen monitoring methods in the existing water, the present invention has following beneficial effect:
The inventive method is on the basis of original each standard method, according to a large amount of actual measurement experiences, by not The disconnected summary carried out combination and planned as a whole optimizing to it, finally drawn three nitrogen in the cover Simultaneous Determination water Method. Economically, can according to actual conditions, carry out the real time sample chemical examination, same online test method Compare, can greatly reduce material consumption and water quality monitoring cost; On manpower, with traditional independent consideration Each method is compared, and can reduce the water quality test time more than 50%, really accomplishes not only to make things convenient for but also quick.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102012362A (en) * | 2010-10-15 | 2011-04-13 | 宁波市环境监测中心 | Method for rapidly measuring permanganate indexes in water by spectrophotometric method |
| CN102323226A (en) * | 2011-06-03 | 2012-01-18 | 河南师范大学 | A kind of method of measuring three nitrogen concentrations in the water |
| CN103116011A (en) * | 2013-01-07 | 2013-05-22 | 北京工业大学 | Method for qualitatively comparing contents of NOBs (Nitrite-Oxidizing Bacteria) in different kinds of nitrosation sludge |
| CN103217394A (en) * | 2013-04-10 | 2013-07-24 | 中国科学院合肥物质科学研究院 | Online detection device of water dissolved-out nitrogen nutrients of chemical fertilizer |
-
2008
- 2008-11-28 CN CNA200810227699XA patent/CN101419173A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102012362A (en) * | 2010-10-15 | 2011-04-13 | 宁波市环境监测中心 | Method for rapidly measuring permanganate indexes in water by spectrophotometric method |
| CN102323226A (en) * | 2011-06-03 | 2012-01-18 | 河南师范大学 | A kind of method of measuring three nitrogen concentrations in the water |
| CN103116011A (en) * | 2013-01-07 | 2013-05-22 | 北京工业大学 | Method for qualitatively comparing contents of NOBs (Nitrite-Oxidizing Bacteria) in different kinds of nitrosation sludge |
| CN103116011B (en) * | 2013-01-07 | 2015-05-20 | 北京工业大学 | Method for qualitatively comparing contents of NOBs (Nitrite-Oxidizing Bacteria) in different kinds of nitrosation sludge |
| CN103217394A (en) * | 2013-04-10 | 2013-07-24 | 中国科学院合肥物质科学研究院 | Online detection device of water dissolved-out nitrogen nutrients of chemical fertilizer |
| CN103217394B (en) * | 2013-04-10 | 2014-11-26 | 中国科学院合肥物质科学研究院 | Online detection device of water dissolved-out nitrogen nutrients of chemical fertilizer |
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