CN111982847A - Method for testing total nitrogen by using flow injection analyzer and application thereof - Google Patents
Method for testing total nitrogen by using flow injection analyzer and application thereof Download PDFInfo
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- CN111982847A CN111982847A CN202010931404.8A CN202010931404A CN111982847A CN 111982847 A CN111982847 A CN 111982847A CN 202010931404 A CN202010931404 A CN 202010931404A CN 111982847 A CN111982847 A CN 111982847A
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- total nitrogen
- flow injection
- injection analyzer
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 54
- 238000012360 testing method Methods 0.000 title claims abstract description 39
- 238000004401 flow injection analysis Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000000243 solution Substances 0.000 claims abstract description 57
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 55
- 230000029087 digestion Effects 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000007853 buffer solution Substances 0.000 claims abstract description 38
- 239000000126 substance Substances 0.000 claims abstract description 29
- 230000009467 reduction Effects 0.000 claims abstract description 27
- 239000002738 chelating agent Substances 0.000 claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 13
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000002835 absorbance Methods 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000010998 test method Methods 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 6
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 20
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 20
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 claims description 20
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 19
- 229940001584 sodium metabisulfite Drugs 0.000 claims description 19
- CDMADVZSLOHIFP-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane;decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 CDMADVZSLOHIFP-UHFFFAOYSA-N 0.000 claims description 18
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 18
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 16
- 229940124530 sulfonamide Drugs 0.000 claims description 16
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 10
- 229910021529 ammonia Inorganic materials 0.000 claims description 10
- FXKZPKBFTQUJBA-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;sodium;dihydrate Chemical compound O.O.[Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O FXKZPKBFTQUJBA-UHFFFAOYSA-N 0.000 claims description 7
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical group [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 claims description 7
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 7
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 claims description 6
- 239000010842 industrial wastewater Substances 0.000 claims description 5
- 239000010865 sewage Substances 0.000 claims description 4
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 claims description 3
- FZQSLXQPHPOTHG-UHFFFAOYSA-N [K+].[K+].O1B([O-])OB2OB([O-])OB1O2 Chemical compound [K+].[K+].O1B([O-])OB2OB([O-])OB1O2 FZQSLXQPHPOTHG-UHFFFAOYSA-N 0.000 claims description 3
- 229960003330 pentetic acid Drugs 0.000 claims description 3
- RWPGFSMJFRPDDP-UHFFFAOYSA-L potassium metabisulfite Chemical compound [K+].[K+].[O-]S(=O)S([O-])(=O)=O RWPGFSMJFRPDDP-UHFFFAOYSA-L 0.000 claims description 3
- 229940043349 potassium metabisulfite Drugs 0.000 claims description 3
- 235000010263 potassium metabisulphite Nutrition 0.000 claims description 3
- 239000013535 sea water Substances 0.000 claims description 3
- 239000002352 surface water Substances 0.000 claims description 3
- NFMWFGXCDDYTEG-UHFFFAOYSA-N trimagnesium;diborate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]B([O-])[O-].[O-]B([O-])[O-] NFMWFGXCDDYTEG-UHFFFAOYSA-N 0.000 claims description 3
- HCFPRFJJTHMING-UHFFFAOYSA-N ethane-1,2-diamine;hydron;chloride Chemical compound [Cl-].NCC[NH3+] HCFPRFJJTHMING-UHFFFAOYSA-N 0.000 claims 1
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract description 11
- 229910021645 metal ion Inorganic materials 0.000 abstract description 3
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 42
- 239000000047 product Substances 0.000 description 36
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 20
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 18
- 238000002360 preparation method Methods 0.000 description 18
- WZRRZVUZWWMSKH-UHFFFAOYSA-N n'-naphthalen-1-ylethane-1,2-diamine;hydrochloride Chemical compound Cl.C1=CC=C2C(NCCN)=CC=CC2=C1 WZRRZVUZWWMSKH-UHFFFAOYSA-N 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 239000002351 wastewater Substances 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 11
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 10
- 235000019270 ammonium chloride Nutrition 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 8
- 229910002651 NO3 Inorganic materials 0.000 description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 229960001484 edetic acid Drugs 0.000 description 5
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 4
- 238000004537 pulping Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 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 description 2
- 238000004458 analytical method Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 125000001477 organic nitrogen group Chemical group 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- JTNCEQNHURODLX-UHFFFAOYSA-N 2-phenylethanimidamide Chemical compound NC(=N)CC1=CC=CC=C1 JTNCEQNHURODLX-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000005337 ground glass Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- -1 nitrogen containing compound Chemical class 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 229910000343 potassium bisulfate Inorganic materials 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000004296 sodium metabisulphite Substances 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
A method of testing total nitrogen using a flow injection analyzer, the method relying on a flow injection analyzer for testing, comprising the steps of: (1) under the irradiation of ultraviolet light, adding a digestion solution into a water sample to be detected and heating to obtain a digestion product A; (2) adding a buffer solution into the digestion product A, and reducing to obtain a reduction product B; (3) adding a color developing agent into the reduction product B to obtain a substance C to be detected; (4) and (4) measuring the absorbance value of the object C to be measured, and calculating the corresponding total nitrogen concentration. The solute of the buffer solution comprises acid, ammonia water and a metal chelating agent, the ammonia nitrogen in the water sample to be tested can be reduced to escape in the form of ammonia gas, the interference of the metal ions and the acid-base degree in the water sample to be tested on the testing accuracy is reduced, and the testing accuracy and stability are improved. The digestion product is reduced by the cadmium column firstly and then reduced by the reducing agent twice, so that the digestion product is reduced thoroughly, and the precision and accuracy of the test are improved.
Description
Technical Field
The application belongs to the technical field of analysis and detection, and particularly relates to a method for testing total nitrogen by using a flow injection analyzer and application thereof.
Background
The total nitrogen content in water is one of the important indexes for measuring water quality. Total nitrogen is defined as the total amount of various forms of inorganic and organic nitrogen in the water. Comprising NO3 -、NO2 -And NH4 +And the inorganic nitrogen and the organic nitrogen such as protein, amino acid and organic amine are calculated by the nitrogen-containing milligrams per liter of water. Is often used to indicate the degree of nutrient contamination of a body of water. The nitrogen source in water is mainly divided into natural source and artificial source, and the artificial source mainly comprises fertilizer application, industrial manufacturing, domestic sewage irrigation, sludge and the like. Too high a total nitrogen content in the water can seriously affect the health of the drinking organisms and even lead to death. With the further development of economy, industrial wastewater becomes a main source of wastewater, and the industrial wastewater has a variety of types including dye wastewater, paper-making wastewater, electroplating wastewater and the like, and because the components of the wastewater are complex, the total nitrogen of the wastewater is tested, and the subsequent wastewater treatment is complex. The total nitrogen test in the paper making wastewater is particularly difficult because the components in the paper making wastewater are complicated. Particularly, for wastewater generated in an alkaline pulping process, due to high alkalinity, reagents used in a total nitrogen test process can be influenced to a certain extent, so that a test result has large deviation and poor stability.
Disclosure of Invention
In order to solve the above technical problems, a first aspect of the present invention provides a method for testing total nitrogen by using a flow injection analyzer, the method for testing by using the flow injection analyzer as a support, the method at least comprising the following steps:
(1) under the irradiation of ultraviolet light, adding a digestion solution into a water sample to be detected and heating to obtain a digestion product A;
(2) adding a buffer solution into the digestion product A, and reducing to obtain a reduction product B;
(3) adding a color developing agent into the reduction product B to obtain a substance C to be detected;
(4) and (4) measuring the absorbance value of the object C to be measured, and calculating the corresponding total nitrogen concentration.
Preferably, the digestion solution in the step (1) contains potassium persulfate and borate. Preferably, the borate is selected from at least one of sodium tetraborate decahydrate, magnesium borate, and potassium tetraborate.
Preferably, the reduction in step (2) includes cadmium column reduction and reducing agent reduction.
Preferably, the reducing agent is a metabisulfite solution.
Preferably, the metabisulfite solution is selected from at least one of sodium metabisulfite solution and potassium metabisulfite solution.
Preferably, the solute of the buffer solution comprises acid, ammonia water and metal chelating agent, and the pH of the buffer solution is 8-9.
Preferably, the acid is at least one selected from sulfuric acid and hydrochloric acid.
Preferably, the metal chelating agent is at least one selected from the group consisting of ethylenediaminetetraacetic acid, nitrilotriacetic acid, diethylenetriaminepentaacetic acid, disodium ethylenediaminetetraacetic acid dihydrate, and hydroxyethylethylenediaminetriacetic acid.
Preferably, the solute of the color-developing agent at least comprises sulfanilamide and N- (1-naphthyl) ethylenediamine hydrochloride.
Preferably, the solute of the color developer further comprises phosphoric acid.
The method for testing the total nitrogen by using the flow injection analyzer can be applied to detecting the total nitrogen concentration in surface water, industrial wastewater, domestic sewage and seawater.
Has the advantages that:
(1) ammonium chloride is directly used to prepare into ammonium chloride solution in the traditional buffer solution for flow injection determination of total nitrogen in water quality, then a metal chelating agent is added, the ammonium chloride is easy to deliquesce when stored, and the concentration of the buffer solution has certain influence, thereby influencing the accuracy and stability of the test. The buffer solution in the scheme prepares the ammonium chloride solution through hydrochloric acid and ammonia water respectively, and then the metal chelating agent can improve the stability of the buffer solution, especially aiming at the waste water with higher alkalinity generated in the alkaline pulping process in the technical scheme, the buffer solution in the technical scheme can reduce the escape of ammonia nitrogen in a water sample to be tested in the form of ammonia gas, reduce the interference of metal ions and acid-base degree in the water sample to be tested on the testing accuracy, and improve the testing accuracy and stability.
(2) In the scheme, the degradation product is reduced by the cadmium column firstly and then reduced by the reducing agent twice, and the total nitrogen in the water quality to be tested can not be reduced completely only by the cadmium column in the traditional flow injection water quality determination method, so that the total nitrogen content in the test result is low. According to the technical scheme, the reducing agent is added for reduction after the reduction of the cadmium column, so that the total nitrogen in the water sample to be tested can be thoroughly reduced, and the test stability is improved.
(3) The digestion solution in the scheme contains potassium persulfate and borate, so that nitrogen brought into a water sample to be tested can be reduced, nitrogen in the water sample to be tested escapes in a nitrogen form, and the accuracy of an analysis and test process is improved.
Detailed Description
For purposes of the following detailed description, it is to be understood that the invention may assume various alternative variations and step sequences, except where expressly specified to the contrary. Moreover, other than in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the invention are approximations, the numerical values set forth in the specific examples are reported as precisely as possible. Any numerical value, however, inherently contains certain errors necessarily resulting from the standard deviation found in their respective testing measurements.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range-describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein. For example, a stated range from "1 to 10" should be considered to include any and all subranges between the minimum value of 1 and the maximum value of 10. Exemplary subranges of the range 1 to 10 include, but are not limited to, 1 to 6.1, 3.5 to 7.8, 5.5 to 10, and the like.
In order to solve the technical problems, the first aspect of the invention provides a method for testing total nitrogen by using a flow injection analyzer, which takes the flow injection analyzer as a support for testing and at least comprises the following steps:
(1) under the irradiation of ultraviolet light, adding a digestion solution into a water sample to be detected and heating to obtain a digestion product A;
(2) adding a buffer solution into the digestion product A, and reducing to obtain a reduction product B;
(3) adding a color developing agent into the reduction product B to obtain a substance C to be detected;
(4) and (4) measuring the absorbance value of the object C to be measured, and calculating the corresponding total nitrogen concentration.
As a preferable technical scheme, the digestion solution in the step (1) contains potassium persulfate and borate.
As a preferable embodiment, the borate is at least one selected from the group consisting of sodium tetraborate decahydrate, magnesium borate and potassium tetraborate.
As a preferred technical solution, the borate is sodium tetraborate decahydrate.
Under the effect of ultraviolet light, potassium persulfate is in alkaline solution to be awaited measuring nitrogen containing compound oxidation digestion for nitrate in the water sample, and the hydrolysis that uses sodium tetraborate decahydrate in this scheme produces the hydroxyl ion, builds the hydrogen ion reaction that produces in alkaline environment and the potassium persulfate oxidation reaction, promotes the reaction of potassium persulfate completely, promotes to clear up thoroughly, improves the accuracy and the stability of test. The solution of sodium tetraborate decahydrate is weak base, so that nitrogen in a water sample to be tested can be reduced to escape in a nitrogen form, and the accuracy of the test is further improved.
As a preferred technical scheme, the reduction in the step (2) comprises cadmium column reduction and reducing agent reduction.
As a preferable technical scheme, the reducing agent is a metabisulfite solution.
As a preferred technical solution, the metabisulfite solution is at least one selected from sodium metabisulfite solution and potassium metabisulfite solution.
The nitrate generated in the scheme is reduced into nitrite through the cadmium column and the metabisulfite solution, so that the reduction degree of the nitrate into nitrite is improved, and the test accuracy is improved.
As a preferable technical scheme, the solute of the buffer solution at least comprises acid, ammonia water and a metal chelating agent, and the pH value of the buffer solution is 8-9.
As a preferred embodiment, the acid is hydrochloric acid.
In a preferred embodiment, the metal chelating agent is at least one selected from the group consisting of ethylenediaminetetraacetic acid, nitrilotriacetic acid, diethylenetriaminepentaacetic acid, disodium ethylenediaminetetraacetic acid dihydrate, and hydroxyethylethylenediaminetriacetic acid.
Through mixing hydrochloric acid, aqueous ammonia and metal chelating agent and preparing the buffer solution, can improve holistic pH stability, reduce the influence of metal ion and other miscellaneous pair test effects, compound into the ammonium chloride solution through hydrochloric acid and aqueous ammonia, can reduce volatilizing of ammonia, compare in directly using the ammonium chloride to prepare the ammonium chloride solution, can improve buffer solution's stability, the waste water that produces is less to the pH and the cushioning effect influence of this buffer solution in the alkaline pulping process, can improve test effects's accuracy.
As a preferable technical scheme, the solute of the color developing agent at least comprises sulfanilamide and N- (1-naphthyl) ethylenediamine hydrochloride.
As a preferable technical solution, the solute of the color-developing agent further includes phosphoric acid.
The method for testing the total nitrogen by using the flow injection analyzer can be applied to detecting the total nitrogen concentration in surface water, industrial wastewater, domestic sewage and seawater.
Under the conditions of heating and ultraviolet irradiation, potassium persulfate can be decomposed to generate potassium bisulfate and oxygen free radicals, the oxygen free radicals can convert nitrogen elements in nitrogen-containing compounds in a water sample into nitrate, the nitrate is reduced into nitrite through a cadmium column and a reducing agent, the nitrite is diazotized with sulfanilamide, and then generates coupling reaction with N- (1-naphthyl) ethylenediamine hydrochloride to generate rose-red azo dye, then the absorbance is measured through a spectrophotometer, and the total nitrogen content is calculated through a computer.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the starting materials used are all commercially available, unless otherwise specified.
Examples
Example 1
In the embodiment, standard solutions with the concentrations of 0mg/L, 0.10mg/L, 0.50mg/L, 1.0mg/L, 5.0mg/L and 10.0mg/L are prepared by 1000mg/L of nitrate nitrogen standard solution, the method for measuring the total nitrogen in the scheme is used, the absorbance values with different concentrations are measured in a flow injection analyzer Baode BDFIA-8000, and various parameters in the flow injection analyzer are set as follows: the needle washing time is 19s, the sample introduction time is 40s, the current carrying time is 30s, the valve reaching time is 180s, the rotating speed of a peristaltic pump is 35r/min, the injection time is 60s, the sample period time is 105s, the set temperature is 1-105 ℃, the light source of the detector is a halogen lamp, and the wavelength is 540 nm. And drawing a working curve by taking the total nitrogen concentration value as an abscissa and the corresponding absorbance value as an ordinate, and obtaining a linear equation of unitary regression by adopting a linear fitting method, wherein the correlation coefficient is R (0.9999). The nitrate nitrogen standard solution is purchased from the national center for standards.
The water sample in this example is wastewater produced in an alkaline pulping process filtered by filter paper. The ambient temperature for the test operation was 25 ℃ and the relative humidity was 50%.
A first aspect of the present embodiments provides a method of testing total nitrogen using a flow injection analyzer, the method relying on a flow injection analyzer for testing, comprising the steps of:
(1) under the irradiation of ultraviolet light, adding a digestion solution into a water sample to be detected and heating to obtain a digestion product A;
the solute in the digestion solution is potassium persulfate and borate, the solvent is ammonia-free water, and the borate is sodium tetraborate decahydrate. The preparation method of the digestion solution comprises the following specific steps: in a 1L volumetric flask, 900mL of anhydrous ammonia was added, 10.0g of potassium persulfate and 8.75g of sodium tetraborate decahydrate were added, and the mixture was stirred until the solution was completely dissolved, and the volume was adjusted to 1L with anhydrous ammonia. The potassium persulfate was purchased from alatin, cat #: p112193, said sodium tetraborate decahydrate, available from merck chemical technology (shanghai) ltd, cat #: and V900209.
The preparation method of the ammonia-free water comprises the following steps: adding concentrated sulfuric acid accounting for one ten thousandth of the volume of the distilled water into the distilled water, redistilling the concentrated sulfuric acid in an all-glass distiller, discarding 10mL of primary distillate, collecting the distillate, and storing the distillate in a glass bottle with a ground glass plug in a sealing manner.
(2) Adding a buffer solution into the digestion product A, and reducing to obtain a reduction product B;
the solute of the buffer solution is hydrochloric acid, ammonia water and a metal chelating agent, the metal chelating agent is disodium ethylene diamine tetraacetic acid dihydrate, and the pH value of the buffer solution is 8.5. The buffer solution comprises the following specific preparation steps: adding 500mL of anhydrous ammonia into a 1L volumetric flask, then adding 100mL of concentrated hydrochloric acid, then adding 100mL of ammonia, cooling, then adding 1.0g of disodium ethylene diamine tetraacetic acid dihydrate, uniformly mixing, and adjusting the pH value of the solution to 8.5 by using concentrated hydrochloric acid, wherein the mass fraction of the concentrated hydrochloric acid is 36% and the mass fraction of the ammonia is 28%. The disodium edetate dihydrate is available from merck chemical technology (shanghai) ltd under CAS number: 6381-92-6.
Digesting the digestion product A by a cadmium column and a sodium metabisulfite solution on a flow injection analyzer, wherein the sodium metabisulfite solution comprises the following specific preparation steps: adding 900mL of anhydrous ammonia into a 1L volumetric flask, adding 2.5g of sodium metabisulfite, stirring with an electromagnetic stirrer to completely dissolve the substances, adding anhydrous ammonia to a constant volume of 1L, and mixing uniformly to obtain the product. The sodium metabisulfite was purchased from merck chemical technology (shanghai) ltd, cat #: s9000.
(3) Adding a color developing agent into the reduction product B to obtain a substance C to be detected;
(4) measuring the absorbance value of the object C to be measured, and calculating the corresponding total nitrogen concentration;
the solute of the color developing agent is sulfanilamide, N- (1-naphthyl) ethylenediamine hydrochloride and phosphoric acid, the solvent is ammonia-free water, and the specific preparation steps of the color developing agent are as follows: adding 600mL of anhydrous ammonia into a 1L volumetric flask, adding 100mL of phosphoric acid with the mass fraction of 85%, 40.0g of sulfanilamide and 1.0g of 1.0g N- (1-naphthyl) ethylenediamine hydrochloride, stirring until the materials are completely dissolved, and fixing the volume to 1L by using the anhydrous ammonia to obtain the product. The sulfanilamide is purchased from Shanghai Hongshun Biotech limited, CAS number: 63-74-1. The N- (1-naphthyl) ethylenediamine hydrochloride was purchased from China chemical network, CAS number: 1465-25-4.
And (3) measuring the absorbance value of the object C to be measured, and automatically calculating the corresponding total nitrogen concentration through a computer. After the test is finished, a sulfuric acid solution with the mass fraction of 10% is used for cleaning a pipeline of the test equipment, and then ammonia-free water is used for cleaning.
Example 2
This embodiment is different from embodiment 1 in that: a first aspect of the present embodiments provides a method of testing total nitrogen using a flow injection analyzer, the method relying on a flow injection analyzer for testing, comprising the steps of:
(1) under the irradiation of ultraviolet light, adding a digestion solution into a water sample to be detected and heating to obtain a digestion product A;
the solute of the digestion solution is potassium persulfate and borate, the solvent is ammonia-free water, and the borate is sodium tetraborate decahydrate. The preparation method of the digestion solution comprises the following specific steps: in a 1L volumetric flask, 900mL of anhydrous ammonia, 10.0g of potassium persulfate and 8.75g of sodium tetraborate decahydrate are added, stirred until the components are completely dissolved, and the volume is fixed to 1L by using the anhydrous ammonia. The potassium persulfate was purchased from alatin, cat #: p112193, said sodium tetraborate decahydrate, available from merck chemical technology (shanghai) ltd, cat #: and V900209.
(2) Adding a buffer solution into the digestion product A, and reducing to obtain a reduction product B;
the solute of the buffer solution is hydrochloric acid, ammonia water and a metal chelating agent, the metal chelating agent is ethylene diamine tetraacetic acid, and the pH value of the buffer solution is 8.5. The buffer solution comprises the following specific preparation steps: adding 500mL of anhydrous ammonia into a 1L volumetric flask, then adding 100mL of concentrated hydrochloric acid, then adding 100mL of ammonia, cooling, then adding 1.0g of ethylenediamine tetraacetic acid, uniformly mixing, and adjusting the pH value of the solution to 8.5 by using concentrated hydrochloric acid, wherein the mass fraction of the concentrated hydrochloric acid is 36% and the mass fraction of the ammonia is 28%. The ethylenediaminetetraacetic acid was purchased from alatin, cat #: E299236.
digesting the digestion product A by a cadmium column and a sodium metabisulfite solution on a flow injection analyzer, wherein the sodium metabisulfite solution comprises the following specific preparation steps: adding 900mL of anhydrous ammonia into a 1L volumetric flask, adding 2.5g of sodium metabisulfite, stirring with an electromagnetic stirrer to completely dissolve the substances, adding anhydrous ammonia to a constant volume of 1L, and mixing uniformly to obtain the product. The sodium metabisulfite was purchased from merck chemical technology (shanghai) ltd, cat #: s9000.
(3) Adding a color developing agent into the reduction product B to obtain a substance C to be detected;
(4) and (4) measuring the absorbance value of the object C to be measured, and calculating the corresponding total nitrogen concentration.
The solute of the color developing agent is sulfanilamide, N- (1-naphthyl) ethylenediamine hydrochloride and phosphoric acid, the solvent is ammonia-free water, and the specific preparation steps of the color developing agent are as follows: adding 600mL of anhydrous ammonia into a 1L volumetric flask, adding 100mL of phosphoric acid with the mass fraction of 85%, 40.0g of sulfanilamide and 1.0g of 1.0g N- (1-naphthyl) ethylenediamine hydrochloride, stirring until the materials are completely dissolved, and fixing the volume to 1L by using the anhydrous ammonia to obtain the product. The sulfanilamide is purchased from Shanghai Hongshun Biotech limited, CAS number: 63-74-1. The N- (1-naphthyl) ethylenediamine hydrochloride was purchased from China chemical network, CAS number: 1465-25-4.
Example 3
The difference between this example and example 1 is that: a first aspect of the present embodiments provides a method of testing total nitrogen using a flow injection analyzer, the method relying on a flow injection analyzer for testing, comprising the steps of:
(1) under the irradiation of ultraviolet light, adding a digestion solution into a water sample to be detected and heating to obtain a digestion product A;
the solute of the digestion solution is potassium sulfate and borate, the solvent is ammonia-free water, and the borate is sodium tetraborate decahydrate. The preparation method of the digestion solution comprises the following specific steps: in a 1L volumetric flask, 900mL of anhydrous ammonia, 10.0g of potassium persulfate and 8.75g of sodium tetraborate decahydrate are added, stirred until the components are completely dissolved, and the volume is fixed to 1L by using the anhydrous ammonia. The potassium persulfate was purchased from alatin, cat #: p112193, said sodium tetraborate decahydrate, available from merck chemical technology (shanghai) ltd, cat #: and V900209.
(2) Adding a buffer solution into the digestion product A, and reducing to obtain a reduction product B;
the solute of the buffer solution is hydrochloric acid, ammonia water and a metal chelating agent, the metal chelating agent is nitrilotriacetic acid, and the pH value of the buffer solution is 8.5.
The buffer solution comprises the following specific preparation steps: adding 500mL of anhydrous ammonia into a 1L volumetric flask, then adding 100mL of concentrated hydrochloric acid, then adding 100mL of ammonia, cooling, then adding 1.0g of aminotriacetic acid, uniformly mixing, and adjusting the pH value of the solution to 8.5 by using concentrated hydrochloric acid, wherein the mass fraction of the concentrated hydrochloric acid is 36% and the mass fraction of the ammonia is 28%. The nitrilotriacetic acid was purchased from gaeder chemical network, CAS No.: 139-13-9.
Digesting the digestion product A by a cadmium column and a sodium metabisulfite solution on a flow injection analyzer, wherein the sodium metabisulfite solution comprises the following specific preparation steps: adding 900mL of anhydrous ammonia into a 1L volumetric flask, adding 2.5g of sodium metabisulfite, stirring with an electromagnetic stirrer to completely dissolve the substances, adding anhydrous ammonia to a constant volume of 1L, and mixing uniformly to obtain the product. The sodium metabisulfite was purchased from merck chemical technology (shanghai) ltd, cat #: s9000.
(3) Adding a color developing agent into the reduction product B to obtain a substance C to be detected;
(4) and (4) measuring the absorbance value of the object C to be measured, and calculating the corresponding total nitrogen concentration.
The solute of the color developing agent is sulfanilamide, N- (1-naphthyl) ethylenediamine hydrochloride and phosphoric acid, the solvent is ammonia-free water, and the specific preparation steps of the color developing agent are as follows: adding 600mL of anhydrous ammonia into a 1L volumetric flask, adding 100mL of phosphoric acid with the mass fraction of 85%, 40.0g of sulfanilamide and 1.0g of 1.0g N- (1-naphthyl) ethylenediamine hydrochloride, stirring until the materials are completely dissolved, and fixing the volume to 1L by using the anhydrous ammonia to obtain the product. The sulfanilamide is purchased from Shanghai Hongshun Biotech limited, CAS number: 63-74-1. The N- (1-naphthyl) ethylenediamine hydrochloride was purchased from China chemical network, CAS number: 1465-25-4.
Example 4
The difference between this example and example 1 is that: a first aspect of the present embodiments provides a method of testing total nitrogen using a flow injection analyzer, the method relying on a flow injection analyzer for testing, comprising the steps of:
(1) under the irradiation of ultraviolet light, adding a digestion solution into a water sample to be detected and heating to obtain a digestion product A; the digestion solution contains potassium persulfate and borate, and the borate is sodium tetraborate decahydrate. The preparation method of the digestion solution comprises the following specific steps: in a 1L volumetric flask, 900mL of anhydrous ammonia, 10.0g of potassium persulfate and 8.75g of sodium tetraborate decahydrate are added, stirred until the components are completely dissolved, and the volume is fixed to 1L by using the anhydrous ammonia. The potassium persulfate was purchased from alatin, cat #: p112193, said sodium tetraborate decahydrate, available from merck chemical technology (shanghai) ltd, cat #: and V900209.
(2) Adding a buffer solution into the digestion product A, and reducing to obtain a reduction product B;
the solute of the buffer solution is hydrochloric acid, ammonia water and a metal chelating agent, the solvent is non-ammonia water, the metal chelating agent is hydroxyethyl ethylenediamine triacetic acid, and the pH value of the buffer solution is 8.5.
The buffer solution comprises the following specific preparation steps: adding 500mL of anhydrous ammonia into a 1L volumetric flask, then adding 100mL of concentrated hydrochloric acid, then adding 100mL of ammonia, cooling, then adding 1.0g of hydroxyethyl ethylenediamine triacetic acid, uniformly mixing, and adjusting the pH value of the solution to 8.5 by using concentrated hydrochloric acid, wherein the mass fraction of the concentrated hydrochloric acid is 36% and the mass fraction of the ammonia is 28%. The hydroxyethylethylenediaminetriacetic acid was purchased from Condites chemical (Hubei) Inc., cat #: kds 414541651.
Digesting the digestion product A by a cadmium column and a sodium metabisulfite solution on a flow injection analyzer, wherein the sodium metabisulfite solution comprises the following specific preparation steps: adding 900mL of anhydrous ammonia into a 1L volumetric flask, adding 2.5g of sodium metabisulfite, stirring with an electromagnetic stirrer to completely dissolve the substances, adding anhydrous ammonia to a constant volume of 1L, and mixing uniformly to obtain the product. The sodium metabisulfite was purchased from merck chemical technology (shanghai) ltd, cat #: s9000.
(3) Adding a color developing agent into the reduction product B to obtain a substance C to be detected;
(4) and (4) measuring the absorbance value of the object C to be measured, and calculating the corresponding total nitrogen concentration.
The solute of the color developing agent is sulfanilamide, N- (1-naphthyl) ethylenediamine hydrochloride and phosphoric acid, the solvent is ammonia-free water, and the specific preparation steps of the color developing agent are as follows: adding 600mL of anhydrous ammonia into a 1L volumetric flask, adding 100mL of phosphoric acid with the mass fraction of 85%, 40.0g of sulfanilamide and 1.0g of 1.0g N- (1-naphthyl) ethylenediamine hydrochloride, stirring until the materials are completely dissolved, and fixing the volume to 1L by using the anhydrous ammonia to obtain the product. The sulfanilamide is purchased from Shanghai Hongshun Biotech limited, CAS number: 63-74-1. The N- (1-naphthyl) ethylenediamine hydrochloride was purchased from China chemical network, CAS number: 1465-25-4.
Comparative example 1
This comparative example differs from example 1 in that the solutes of the buffer solution are ammonium chloride and a metal chelating agent, the solvent is anhydrous ammonia, the metal chelating agent is disodium ethylenediaminetetraacetic acid dihydrate, and the pH of the buffer solution is 8.5. The buffer solution comprises the following specific preparation steps: in a 1L volumetric flask, 500mL of anhydrous ammonia water is firstly added, 40g of ammonium chloride is then added, 1.0g of disodium ethylene diamine tetraacetic acid dihydrate is added after cooling, the mixture is uniformly mixed, and the pH value of the solution is adjusted to 8.5 by sodium hydroxide. The disodium edetate dihydrate is available from merck chemical technology (shanghai) ltd under CAS number: 6381-92-6.
Comparative example 2
The difference between this comparative example and example 1 is that this comparative example does not contain a sodium metabisulphite solution.
Comparative example 3
The comparative example differs from example 1 in that the metal chelating agent in the comparative example is sodium tripolyphosphate, available from merck chemical technology (shanghai) ltd, under the trade designation: 238503.
and (3) testing: the test water samples of examples 1 to 4 and comparative examples 1 to 3 were collected at the same time, 10 water samples were measured for each example and each comparative example test method, the total nitrogen measurement values of examples 1 to 4 and comparative examples 1 to 3 were averaged, and the relative standard deviation was calculated from the average value to evaluate the stability of the test method.
Relative standard deviation (%) | |
Example 1 | 0.40 |
Example 2 | 0.39 |
Example 3 | 0.41 |
Example 4 | 0.42 |
Comparative example 1 | 0.73 |
Comparative example 2 | 1.20 |
Comparative example 3 | 0.71 |
From the above data, it can be seen that the test methods in examples 1-4 are more stable. The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art may modify or change the technical content of the above disclosure into equivalent embodiments with equivalent changes, but all those simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the present invention.
Claims (10)
1. A method for testing total nitrogen by using a flow injection analyzer, wherein the method is based on the flow injection analyzer and comprises at least the following steps:
(1) under the irradiation of ultraviolet light, adding a digestion solution into a water sample to be detected and heating to obtain a digestion product A;
(2) adding a buffer solution into the digestion product A, and reducing to obtain a reduction product B;
(3) adding a color developing agent into the reduction product B to obtain a substance C to be detected;
(4) and (4) measuring the absorbance value of the object C to be measured, and calculating the corresponding total nitrogen concentration.
2. The method for measuring total nitrogen using a flow injection analyzer according to claim 1, wherein the digestion solution in the step (1) contains potassium persulfate and borate.
3. The method of testing total nitrogen using a flow injection analyzer of claim 2, wherein the borate is selected from at least one of sodium tetraborate decahydrate, magnesium borate, and potassium tetraborate.
4. The method for testing total nitrogen using a flow injection analyzer of any one of claims 1-3, wherein the reducing in step (2) comprises cadmium column reduction and reducing agent reduction.
5. The method for measuring total nitrogen using a flow injection analyzer of claim 4, wherein the reducing agent is a metabisulfite solution.
6. The method for measuring total nitrogen using a flow injection analyzer according to claim 5, wherein the metabisulfite solution is selected from at least one of sodium metabisulfite solution and potassium metabisulfite solution.
7. The method for measuring total nitrogen using a flow injection analyzer according to claim 1, wherein the solutes of the buffer solution include an acid, ammonia and a metal chelator, and the pH of the buffer solution is 8 to 9.
8. The method for measuring total nitrogen using a flow injection analyzer as set forth in claim 7, wherein the metal chelating agent is at least one selected from the group consisting of ethylenediaminetetraacetic acid, nitrilotriacetic acid, diethylenetriaminepentaacetic acid, disodium ethylenediaminetetraacetic acid dihydrate, and hydroxyethylethylenediaminetriacetic acid.
9. The method for measuring total nitrogen using a flow injection analyzer as set forth in claim 1, wherein the solute of the developer includes at least sulfanilamide and ethylenediamine hydrochloride.
10. A method of measuring total nitrogen using a flow injection analyzer according to any one of claims 1 to 9, which can be applied to detect the total nitrogen concentration in surface water, industrial wastewater, domestic sewage, seawater.
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