CN117740771B - Prefabricated reagent for simultaneously measuring total nitrogen and total phosphorus of aquaculture tail water - Google Patents
Prefabricated reagent for simultaneously measuring total nitrogen and total phosphorus of aquaculture tail water Download PDFInfo
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- CN117740771B CN117740771B CN202311713532.5A CN202311713532A CN117740771B CN 117740771 B CN117740771 B CN 117740771B CN 202311713532 A CN202311713532 A CN 202311713532A CN 117740771 B CN117740771 B CN 117740771B
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- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 105
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 94
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 46
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 44
- 239000011574 phosphorus Substances 0.000 title claims abstract description 44
- 238000009360 aquaculture Methods 0.000 title abstract description 8
- 244000144974 aquaculture Species 0.000 title abstract description 8
- 230000029087 digestion Effects 0.000 claims abstract description 57
- 238000001514 detection method Methods 0.000 claims abstract description 34
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 28
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000012916 chromogenic reagent Substances 0.000 claims abstract description 21
- 239000003755 preservative agent Substances 0.000 claims abstract description 21
- 230000002335 preservative effect Effects 0.000 claims abstract description 21
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 16
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 16
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- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 16
- 229940026189 antimony potassium tartrate Drugs 0.000 claims abstract description 11
- WBTCZEPSIIFINA-MSFWTACDSA-J dipotassium;antimony(3+);(2r,3r)-2,3-dioxidobutanedioate;trihydrate Chemical compound O.O.O.[K+].[K+].[Sb+3].[Sb+3].[O-]C(=O)[C@H]([O-])[C@@H]([O-])C([O-])=O.[O-]C(=O)[C@H]([O-])[C@@H]([O-])C([O-])=O WBTCZEPSIIFINA-MSFWTACDSA-J 0.000 claims abstract description 11
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
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- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- WPYMKLBDIGXBTP-UHFFFAOYSA-N Benzoic acid Natural products OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 10
- 235000010323 ascorbic acid Nutrition 0.000 claims description 9
- 229960005070 ascorbic acid Drugs 0.000 claims description 9
- 239000011668 ascorbic acid Substances 0.000 claims description 9
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
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- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 7
- 229940001584 sodium metabisulfite Drugs 0.000 claims description 7
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 7
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- WXBLLCUINBKULX-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1.OC(=O)C1=CC=CC=C1 WXBLLCUINBKULX-UHFFFAOYSA-N 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- CYEJMVLDXAUOPN-UHFFFAOYSA-N 2-dodecylphenol Chemical compound CCCCCCCCCCCCC1=CC=CC=C1O CYEJMVLDXAUOPN-UHFFFAOYSA-N 0.000 claims description 3
- 229920001661 Chitosan Polymers 0.000 claims description 3
- WEHWNAOGRSTTBQ-UHFFFAOYSA-N dipropylamine Chemical compound CCCNCCC WEHWNAOGRSTTBQ-UHFFFAOYSA-N 0.000 claims description 3
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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- IEORSVTYLWZQJQ-UHFFFAOYSA-N 2-(2-nonylphenoxy)ethanol Chemical compound CCCCCCCCCC1=CC=CC=C1OCCO IEORSVTYLWZQJQ-UHFFFAOYSA-N 0.000 description 1
- JYCQQPHGFMYQCF-UHFFFAOYSA-N 4-tert-Octylphenol monoethoxylate Chemical compound CC(C)(C)CC(C)(C)C1=CC=C(OCCO)C=C1 JYCQQPHGFMYQCF-UHFFFAOYSA-N 0.000 description 1
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- 240000003826 Eichhornia crassipes Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 241000192710 Microcystis aeruginosa Species 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000011481 absorbance measurement Methods 0.000 description 1
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- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention provides a prefabricated reagent for simultaneously measuring total nitrogen and total phosphorus in aquaculture tail water, and relates to the technical field of water quality detection. The preparation reagent provided by the invention comprises a digestion reagent, a first color reagent and a second color reagent; the digestion reagent comprises potassium persulfate with the concentration of 0.2-0.3g/mL, an alkaline regulator with the concentration of 0.3-0.5g/mL and a preservative with the concentration of 0.1-0.3 g/mL; the first chromogenic reagent comprises oxalic acid with the concentration of 0.03-0.05g/mL and a stabilizing agent with the concentration of 0.1-0.3 g/mL; the second color reagent comprises ammonium molybdate with the concentration of 0.03-0.05g/mL, antimony potassium tartrate with the concentration of 0.0003-0.0005g/mL and dispersing agent with the concentration of 0.05-0.1 g/mL. The invention can accurately measure total nitrogen and total phosphorus of the water sample to be measured, the total nitrogen concentration of which reaches 15mg/L and the total phosphorus concentration of which reaches 2.4mg/L, and simultaneously has the same detection effect as a newly prepared reagent after the prefabricated reagent is stored for one year.
Description
Technical Field
The invention relates to the technical field of water quality detection, in particular to a prefabricated reagent for simultaneously measuring total nitrogen and total phosphorus in aquaculture tail water.
Background
At present, the water environment is used as a system with the widest radiation range and the strongest influence in the global environment ecology, along with the development of society economy, domestic sewage, industrial wastewater, agricultural irrigation wastewater and the like are randomly discharged into rivers and lakes, especially the tail water discharge amount of aquaculture industry is greatly increased, so that the content of nitrogen, phosphorus and other plant nutrient substances in water is rapidly increased, and the water body is eutrophicated, so that a plurality of lakes and algae eruptions and water hyacinth overgrow, the stability and development of the global ecological system are seriously influenced, and the environment-friendly development concept proposed by the country is contrary.
Therefore, in order to objectively evaluate the quality state of the water body, and the surplus of the nitrogen and phosphorus nutrient salts is used as a key factor for triggering eutrophication of the water body and water bloom outbreaks, the content measurement is an important index for measuring the water quality condition. At present, the determination of total nitrogen and total phosphorus is usually carried out by adopting a national standard method (spectrophotometer), however, as nitrogen in a water body exists in various valence states such as organic nitrogen, inorganic nitrogen and the like in various forms, phosphorus also exists in the forms such as orthophosphate, polyphosphate, organic phosphate and the like, in order to accurately measure the total nitrogen and total phosphorus content in the water body in actual test, the water sample is required to be digested and pretreated in a certain way, and various forms of nitrogen and phosphorus in the water body are respectively oxidized into nitrate and orthophosphate by adopting different digestion reagents, and then color development test is carried out.
However, the current method for measuring total nitrogen and total phosphorus in water has various national standards and line standards, the time for measuring the total nitrogen and the total phosphorus is long, the maximum measuring range for measuring the total nitrogen is less than 3mg/L, the maximum measuring range for measuring the total phosphorus is less than 0.5mg/L, the method is difficult to be applied to the cultivation tail water with higher total nitrogen and total phosphorus concentration, and meanwhile, different digestion reagents are needed for measuring the total nitrogen and the total phosphorus, so that the detection process is complex. It is therefore desirable to provide a solution to the above-mentioned problems.
Disclosure of Invention
The invention aims to provide a prefabricated reagent for simultaneously measuring total nitrogen and total phosphorus, which can be used for simultaneously digesting total nitrogen and total phosphorus in culture tail water and accurately digesting and measuring total nitrogen and total phosphorus with higher concentration.
In a first aspect, the invention provides a prefabricated reagent for simultaneously measuring total nitrogen and total phosphorus in culture tail water, which comprises a digestion reagent, a first color reagent and a second color reagent; the digestion reagent comprises potassium persulfate with the concentration of 0.2-0.3g/mL, an alkaline regulator with the concentration of 0.3-0.5g/mL and a preservative with the concentration of 0.1-0.3 g/mL; the first chromogenic reagent comprises oxalic acid with the concentration of 0.03-0.05g/mL and a stabilizing agent with the concentration of 0.1-0.3 g/mL; the second color reagent comprises ammonium molybdate with the concentration of 0.03-0.05g/mL, antimony potassium tartrate with the concentration of 0.0003-0.0005g/mL and dispersing agent with the concentration of 0.05-0.1 g/mL.
The prefabricated reagent provided by the invention has the beneficial effects that the preservative, the stabilizer and the dispersing agent are respectively placed in the potassium persulfate, the first chromogenic reagent and the second chromogenic reagent, so that the preservation durability of the three reagents can be improved, the dispersion uniformity of components in the three reagents in the reagents can be improved, the reagents are prevented from being denatured in the preservation process, and the prefabricated reagent is beneficial to large-scale industrialized peptide sites; meanwhile, the component content of the potassium persulfate and the component content of the preservative in the digestion reagent are adjusted, so that the digestion reagent can digest some culture tail water with higher total nitrogen and total phosphorus concentration, and the accuracy of total nitrogen and total phosphorus determination is improved.
Optionally, the preservative comprises at least two of ascorbic acid, chitosan, alkylphenol ethoxylates and dipropylamine, and the preservative at least comprises ascorbic acid.
Optionally, the preservative is ascorbic acid and alkylphenol polyoxyethylene ether in a concentration ratio of 1:1, a mixture of two or more of the above-mentioned materials; the alkylphenol ethoxylates are at least one of octylphenol ethoxylates, nonylphenol ethoxylates and dodecylphenol ethoxylates, and the polymers of the alkylphenol ethoxylates are 8-12.
Optionally, the preparation method of the digestion reagent comprises the following steps: dissolving potassium persulfate in deionized water, and adding an alkaline regulator to adjust the solution to be alkaline to prepare potassium persulfate mixed solution; heating and boiling the potassium persulfate mixed solution in a sealed environment at 120-130 ℃ for 2-3 hours, and cooling to room temperature to obtain a modified mixed solution; dissolving the preservative in an ethanol solution with the ethanol concentration of 15-20%, uniformly mixing the solution with the modified mixed solution, and then fixing the volume to prepare the digestion reagent.
By adopting the technical scheme, the method has the beneficial effects that after the potassium persulfate mixed solution is boiled, chemical bond changes can be generated between the potassium persulfate and the alkaline regulator dissolved in the mixed solution, so that the potassium persulfate is modified to a certain extent, the dispersion uniformity of the potassium persulfate in the digestion reagent can be improved, and the potassium persulfate can play a good digestion role on a water sample to be tested in an alkaline environment, so that the digestion accuracy is improved.
Optionally, the digestion reagent further comprises silver nitrate at a concentration of 0.05-0.1 g/mL. The method has the advantages that silver ions generated by ionization after the dissolution of the silver nitrate can improve the antibacterial performance of the digestion reagent, so that the preservation durability of the digestion reagent is improved, meanwhile, bacteria in a water sample to be detected can be inhibited, and adverse effects on total nitrogen and total phosphorus detection are avoided.
Optionally, the stabilizer comprises a concentration ratio of 1:1 sodium metabisulfite and benzoic acid. The sodium metabisulfite and the benzoic acid with the concentration ratio have the advantages that the sodium metabisulfite and the benzoic acid with the concentration ratio can improve the preservation stability effect on the first chromogenic reagent, the first chromogenic reagent is not easy to settle and deteriorate in the preservation process, and meanwhile, the sodium metabisulfite and the benzoic acid cannot interfere when absorbance measurement is carried out on total nitrogen and total phosphorus.
Optionally, the preparation method of the first chromogenic reagent comprises the following steps: and dissolving oxalic acid and a stabilizer in deionized water to prepare a mixed solution, and then fixing the volume to prepare the first color reagent.
Optionally, the dispersing agent is at least one of sorbitan, glucose and fructose.
Optionally, the preparation method of the second chromogenic reagent comprises the following steps: dissolving ammonium molybdate and a dispersing agent in deionized water to prepare an ammonium molybdate solution; dissolving antimony potassium tartrate in a dilute sulfuric acid solution to prepare an antimony potassium tartrate sulfuric acid mixed solution; and adding the ammonium molybdate solution into the mixed solution of the antimony potassium tartrate and the sulfuric acid at the dropping rate of 3mL/min, uniformly mixing, and then fixing the volume to prepare the second chromogenic reagent.
In a second aspect, the invention provides a digestion assay employing any of the optional preformed reagents described above, comprising the steps of: adding 5mL of water sample to be detected into a digestion tube filled with 1mL of digestion reagent; digesting a water sample to be measured at 120 ℃ for 30min, cooling to room temperature, and filtering to obtain a digested water sample; the method comprises the steps of uniformly dividing a digested water sample into two detection test tubes with the same specification, namely a first detection tube and a second detection tube, adding a first color reagent into the first detection tube in a volume ratio of 2-3%, stirring and uniformly mixing to obtain a first color-developing water sample, adding a second color-developing reagent into the second detection tube in a volume ratio of 3-4%, stirring and uniformly mixing to obtain a second color-developing water sample; and respectively carrying out absorbance detection on the first chromogenic water sample and the second chromogenic water sample, and determining total nitrogen and total phosphorus in the water sample to be detected.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. Unless otherwise defined, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. As used herein, the word "comprising" and the like means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof without precluding other elements or items.
The embodiment of the invention provides a prefabricated reagent for simultaneously measuring total nitrogen and total phosphorus in culture tail water, which comprises a digestion reagent, a first color reagent and a second color reagent. When the total nitrogen and the total phosphorus of the water sample are measured, after the digestion reagent is mixed with the water sample to be measured in advance, nitrogen existing in the water sample to be measured in the forms of organic nitrogen, inorganic nitrogen and the like is fully oxidized into nitrate radical in a high-temperature state, phosphorus existing in the water sample to be measured in the forms of polyphosphate, organic phosphate and the like is fully oxidized into orthophosphoric acid radical, the water sample to be measured is developed by using a first developing reagent and a second developing reagent, absorbance detection is carried out by using a spectrophotometer, and the total nitrogen and total phosphorus content in the water sample to be measured is rapidly obtained by comparing the absorbance detection data with a standard curve calibrated in advance.
Specifically, the digestion reagent comprises potassium persulfate with the concentration of 0.2-0.3g/mL, an alkaline regulator with the concentration of 0.3-0.5g/mL and a preservative with the concentration of 0.1-0.3 g/mL. In practice, the preservative comprises at least two of ascorbic acid, chitosan, alkylphenol ethoxylates, dipropylamine, and the preservative comprises at least ascorbic acid. The preservative is added into the digestion reagent, so that the state stability of the digestion reagent in the storage process can be improved, and the digestion reagent is prevented from being denatured.
Specifically, the alkaline regulator used in the digestion reagent may be an alkaline regulator commonly used in the art, such as sodium hydroxide or ethylenediamine.
In some embodiments, the preservative is ascorbic acid to alkylphenol ethoxylates at a concentration ratio of 1:1, wherein the alkylphenol ethoxylate is at least one of octylphenol ethoxylate, nonylphenol ethoxylate and dodecylphenol ethoxylate, and the polymer of the alkylphenol ethoxylate is 8-12.
In some embodiments, the digestion reagent further comprises silver nitrate with the concentration of 0.05-0.1g/mL, silver ions generated by ionization after dissolution of the silver nitrate can improve the antibacterial performance of the digestion reagent, so that the preservation durability of the digestion reagent is improved, meanwhile, bacteria in a water sample to be tested can be inhibited, adverse effects on total nitrogen and total phosphorus detection are avoided, and the silver nitrate and the preservative can have good synergistic effect.
Specifically, the preparation method of the digestion reagent comprises the following steps:
Dissolving potassium persulfate in deionized water, and adding an alkaline regulator to adjust the solution to be alkaline to prepare potassium persulfate mixed solution;
heating and boiling the potassium persulfate mixed solution in a sealed environment at 120-130 ℃ for 2-3 hours, and cooling to room temperature to obtain a modified mixed solution;
dissolving the preservative in an ethanol solution with the ethanol concentration of 15-20%, uniformly mixing the solution with the modified mixed solution, and then fixing the volume to prepare the digestion reagent.
In practice, after the potassium persulfate mixed solution is boiled, chemical bond changes between the potassium persulfate dissolved in the mixed solution and the alkaline regulator can be generated, so that the potassium persulfate mixed solution is modified to a certain extent, the dispersion uniformity of the potassium persulfate in the digestion reagent can be improved, and the potassium persulfate can play a good digestion role in an alkaline environment on a water sample to be tested, so that the digestion accuracy is improved.
The first color reagent comprises oxalic acid with concentration of 0.03-0.05g/mL and stabilizer with concentration of 0.1-0.3g/mL, and the stabilizer comprises the following components in concentration ratio of 1:1 sodium metabisulfite and benzoic acid. The preparation method of the first chromogenic reagent comprises the following steps: and dissolving oxalic acid and a stabilizer in deionized water to prepare a mixed solution, and then fixing the volume to prepare the first color reagent.
The second color reagent comprises ammonium molybdate with the concentration of 0.03-0.05g/mL, antimony potassium tartrate with the concentration of 0.0003-0.0005g/mL and a dispersing agent with the concentration of 0.05-0.1g/mL, and the dispersing agent is at least one of sorbitan, glucose and fructose.
Specifically, the preparation method of the second chromogenic reagent comprises the following steps:
dissolving ammonium molybdate and a dispersing agent in deionized water to prepare an ammonium molybdate solution;
Dissolving antimony potassium tartrate in a dilute sulfuric acid solution to prepare an antimony potassium tartrate sulfuric acid mixed solution;
and adding the ammonium molybdate solution into the mixed solution of the antimony potassium tartrate and the sulfuric acid at the dropping rate of 3mL/min, uniformly mixing, and then fixing the volume to prepare the second chromogenic reagent.
The embodiment of the invention also provides a method for digestion determination of the prefabricated reagent prepared in any one of the optional embodiments, which comprises the following steps:
Adding 5mL of water sample to be detected into a digestion tube filled with 1mL of digestion reagent;
digesting a water sample to be measured at 120 ℃ for 30min, cooling to room temperature, and filtering to obtain a digested water sample;
The method comprises the steps of uniformly dividing a digested water sample into two detection test tubes with the same specification, namely a first detection tube and a second detection tube, adding a first color reagent into the first detection tube in a volume ratio of 2-3%, stirring and uniformly mixing to obtain a first color-developing water sample, adding a second color-developing reagent into the second detection tube in a volume ratio of 3-4%, stirring and uniformly mixing to obtain a second color-developing water sample;
And respectively carrying out absorbance detection on the first chromogenic water sample and the second chromogenic water sample, and determining total nitrogen and total phosphorus in the water sample to be detected.
Examples 1 to 5
This example 1-5 provides a preformed reagent for simultaneous determination of total nitrogen and total phosphorus in a aquaculture tail water, wherein the specific components and concentrations of the digestion reagent, the first color reagent and the second indicator are shown in Table 1 below.
TABLE 1 composition and concentration of preformed reagents in examples 1-5
The preparation method of the prefabricated reagent for simultaneously measuring total nitrogen and total phosphorus in the culture tail water in the embodiments 1-5 comprises the following steps:
s1, preparing a digestion reagent:
s11, dissolving potassium persulfate in deionized water, and adding an alkaline regulator to regulate the solution to be alkaline to prepare potassium persulfate mixed solution;
S12, heating and boiling the potassium persulfate mixed solution in a sealed environment at 120 ℃ for 2.5 hours, and cooling to room temperature to obtain a modified mixed solution;
S13, dissolving the preservative in an ethanol solution with the ethanol concentration of 15%, uniformly mixing the solution with the modified mixed solution, and then fixing the volume to prepare a digestion reagent;
S2, preparing a first color reagent: dissolving oxalic acid, sodium metabisulfite and benzoic acid in deionized water to prepare a mixed solution, and then fixing the volume to prepare a first color reagent;
S3, preparing a second color reagent:
S31, dissolving ammonium molybdate and glucose in deionized water to prepare an ammonium molybdate solution;
S32, dissolving the antimony potassium tartrate in a dilute sulfuric acid solution to prepare an antimony potassium tartrate sulfuric acid mixed solution;
s33, adding the ammonium molybdate solution into the antimony potassium tartrate sulfuric acid mixed solution at a dropping rate of 3mL/min, uniformly mixing, and then fixing the volume to prepare a second chromogenic reagent;
S4, respectively storing the digestion reagent, the first chromogenic reagent and the second chromogenic reagent into a brown bottle for shading storage.
Example 6
This example 6 provides a preformed reagent for simultaneous determination of total nitrogen and total phosphorus in aquaculture tail water, differing from example 3 in that the digestion reagent in example 6 further comprises silver nitrate at a concentration of 0.08g/mL, and that silver nitrate is added to the digestion reagent in step S13.
Comparative example 1
This comparative example 1 provides a preformed reagent for simultaneous determination of total nitrogen and total phosphorus in the aquaculture tail water, differing from example 3 in that the digestion reagent in comparative example 1 does not include a preservative.
Performance detection
Ten groups of standard water samples to be tested, of which the total nitrogen and total phosphorus concentrations are shown in table 2, are prepared in advance, and each group of water samples is digested and measured by respectively applying the prefabricated reagent in the embodiment 3, and the method comprises the following steps: adding 5mL of water sample to be detected into a digestion tube filled with 1mL of digestion reagent, placing the digestion tube at 120 ℃ for digestion reaction for 30min to obtain a digested water sample, equally dividing the digested water sample into two detection tubes with the same specification, namely a first detection tube and a second detection tube, adding a first color reagent into the first detection tube in a volume ratio of 2%, stirring and mixing uniformly to obtain a first color-developing water sample, and adding a second color-developing reagent into the second detection tube in a volume ratio of 3%, stirring and mixing uniformly to obtain a second color-developing water sample; respectively carrying out absorbance detection on the first chromogenic water sample and the second chromogenic water sample to determine total nitrogen and total phosphorus in the water sample to be detected, wherein the determination results are shown in table 3;
after the preformed reagents of examples 1 to 6 and comparative example 1 were stored in a light-shielding environment at 25℃for 1 year, the total nitrogen and total phosphorus were measured on the water sample 10 to be measured shown in Table 2 by the digestion measurement method described above, and the measurement results are shown in Table 4.
Table 2 total nitrogen total phosphorus concentration in ten water samples to be tested
TABLE 3 example 3 determination of the prefabricated reagents on the Water sample to be tested
TABLE 4 determination of the pre-formed reagents after storage on the sample 10 to be tested
As can be seen from tables 1 and 4, and examples 1-6 and comparative example 1, the prepared reagent provided by the invention can accurately measure total nitrogen and total phosphorus of a water sample to be measured, wherein the total nitrogen concentration of the water sample reaches 15mg/L, and the total phosphorus concentration of the water sample reaches 2.4mg/L, and meanwhile, the prepared reagent has the same detection effect as a newly prepared reagent after being stored for one year.
While embodiments of the present invention have been described in detail hereinabove, it will be apparent to those skilled in the art that various modifications and variations can be made to these embodiments. It is to be understood that such modifications and variations are within the scope and spirit of the present invention as set forth in the following claims. Moreover, the invention described herein is capable of other embodiments and of being practiced or of being carried out in various ways.
Claims (4)
1. A prefabricated reagent for simultaneously measuring total nitrogen and total phosphorus in culture tail water is characterized in that,
Comprises a digestion reagent, a first chromogenic reagent and a second chromogenic reagent; the digestion reagent comprises potassium persulfate with the concentration of 0.2-0.3g/mL, an alkaline regulator with the concentration of 0.3-0.5g/mL and a preservative with the concentration of 0.1-0.3 g/mL; the first chromogenic reagent comprises oxalic acid with the concentration of 0.03-0.05g/mL and a stabilizing agent with the concentration of 0.1-0.3 g/mL; the second color reagent comprises ammonium molybdate with the concentration of 0.03-0.05g/mL, antimony potassium tartrate with the concentration of 0.0003-0.0005g/mL and dispersing agent with the concentration of 0.05-0.1 g/mL;
The preservative comprises at least two of ascorbic acid, chitosan, alkylphenol ethoxylates and dipropylamine, and at least comprises ascorbic acid;
The preparation method of the digestion reagent comprises the following steps: dissolving potassium persulfate in deionized water, and adding an alkaline regulator to adjust the solution to be alkaline to prepare potassium persulfate mixed solution; heating and boiling the potassium persulfate mixed solution in a sealed environment at 120-130 ℃ for 2-3 hours, and cooling to room temperature to obtain a modified mixed solution; dissolving a preservative in an ethanol solution with the ethanol concentration of 15-20%, uniformly mixing the solution with the modified mixed solution, and fixing the volume to prepare a digestion reagent;
The stabilizer comprises the components with the concentration ratio of 1:1 sodium metabisulfite and benzoic acid;
The preparation method of the first chromogenic reagent comprises the following steps: dissolving oxalic acid and a stabilizer in deionized water to prepare a mixed solution, and then preparing a first color reagent by constant volume;
the dispersing agent is glucose;
The preparation method of the second chromogenic reagent comprises the following steps: dissolving ammonium molybdate and a dispersing agent in deionized water to prepare an ammonium molybdate solution; dissolving antimony potassium tartrate in a dilute sulfuric acid solution to prepare an antimony potassium tartrate sulfuric acid mixed solution; and adding the ammonium molybdate solution into the mixed solution of the antimony potassium tartrate and the sulfuric acid at the dropping rate of 3mL/min, uniformly mixing, and then fixing the volume to prepare the second chromogenic reagent.
2. The preformed reagent of claim 1,
The preservative is prepared from ascorbic acid and alkylphenol polyoxyethylene ether in a concentration ratio of 1:1, a mixture of two or more of the above-mentioned materials; the alkylphenol ethoxylates are at least one of octylphenol ethoxylates, nonylphenol ethoxylates and dodecylphenol ethoxylates, and the polymers of the alkylphenol ethoxylates are 8-12.
3. The preformed reagent of claim 1,
The digestion reagent also comprises silver nitrate with the concentration of 0.05-0.1 g/mL.
4. A digestion assay employing the preformed reagent of any one of claims 1 to 3,
The method comprises the following steps:
Adding 5mL of water sample to be detected into a digestion tube filled with 1mL of digestion reagent; digesting a water sample to be measured at 120 ℃ for 30min, cooling to room temperature, and filtering to obtain a digested water sample; the method comprises the steps of uniformly dividing a digested water sample into two detection test tubes with the same specification, namely a first detection tube and a second detection tube, adding a first color reagent into the first detection tube in a volume ratio of 2-3%, stirring and uniformly mixing to obtain a first color-developing water sample, adding a second color-developing reagent into the second detection tube in a volume ratio of 3-4%, stirring and uniformly mixing to obtain a second color-developing water sample; and respectively carrying out absorbance detection on the first chromogenic water sample and the second chromogenic water sample, and determining total nitrogen and total phosphorus in the water sample to be detected.
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