CN117907315A - Phosphate radical detection reagent, detection kit and detection method - Google Patents
Phosphate radical detection reagent, detection kit and detection method Download PDFInfo
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- CN117907315A CN117907315A CN202311742161.3A CN202311742161A CN117907315A CN 117907315 A CN117907315 A CN 117907315A CN 202311742161 A CN202311742161 A CN 202311742161A CN 117907315 A CN117907315 A CN 117907315A
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- molybdate
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- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 107
- 238000001514 detection method Methods 0.000 title claims abstract description 57
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 36
- 239000010452 phosphate Substances 0.000 title claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 63
- 239000012445 acidic reagent Substances 0.000 claims abstract description 34
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 230000000873 masking effect Effects 0.000 claims abstract description 23
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 22
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 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 16
- 235000002639 sodium chloride Nutrition 0.000 claims description 16
- 239000012086 standard solution Substances 0.000 claims description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 13
- 239000011780 sodium chloride Substances 0.000 claims description 13
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims description 11
- KQROHCSYOGBQGJ-UHFFFAOYSA-N 5-Hydroxytryptophol Chemical compound C1=C(O)C=C2C(CCO)=CNC2=C1 KQROHCSYOGBQGJ-UHFFFAOYSA-N 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 235000015393 sodium molybdate Nutrition 0.000 claims description 9
- 239000011684 sodium molybdate Substances 0.000 claims description 9
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 9
- 229940026189 antimony potassium tartrate Drugs 0.000 claims description 8
- 235000010323 ascorbic acid Nutrition 0.000 claims description 8
- 239000011668 ascorbic acid Substances 0.000 claims description 8
- 229960005070 ascorbic acid Drugs 0.000 claims description 8
- 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 description 8
- 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 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 7
- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 0.000 claims description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 6
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 6
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 6
- -1 ammonium sulfate-fructose Chemical compound 0.000 claims description 6
- 235000015165 citric acid Nutrition 0.000 claims description 6
- 239000012493 hydrazine sulfate Substances 0.000 claims description 6
- 229910000377 hydrazine sulfate Inorganic materials 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 238000004806 packaging method and process Methods 0.000 claims description 6
- 229940074439 potassium sodium tartrate Drugs 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 5
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 5
- 239000011609 ammonium molybdate Substances 0.000 claims description 5
- 229940010552 ammonium molybdate Drugs 0.000 claims description 5
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 235000011150 stannous chloride Nutrition 0.000 claims description 4
- 239000001119 stannous chloride Substances 0.000 claims description 4
- ZVNPWFOVUDMGRP-UHFFFAOYSA-N 4-methylaminophenol sulfate Chemical compound OS(O)(=O)=O.CNC1=CC=C(O)C=C1.CNC1=CC=C(O)C=C1 ZVNPWFOVUDMGRP-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- 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 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- NFXPEBHDHBEHQC-YZJMRIMCSA-N [NH4+].[NH4+].[O-]S([O-])(=O)=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O Chemical compound [NH4+].[NH4+].[O-]S([O-])(=O)=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O NFXPEBHDHBEHQC-YZJMRIMCSA-N 0.000 claims description 3
- TXTQARDVRPFFHL-UHFFFAOYSA-N [Sb].[H][H] Chemical compound [Sb].[H][H] TXTQARDVRPFFHL-UHFFFAOYSA-N 0.000 claims description 3
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 claims description 3
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 235000007686 potassium Nutrition 0.000 claims description 3
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 3
- 235000011151 potassium sulphates Nutrition 0.000 claims description 3
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 3
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 3
- 239000004289 sodium hydrogen sulphite Substances 0.000 claims description 3
- 229940001584 sodium metabisulfite Drugs 0.000 claims description 3
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 235000010265 sodium sulphite Nutrition 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 3
- IUQQUDOPPAGCQI-UHFFFAOYSA-N 2-amino-3-(sulfanylmethyl)phenol Chemical compound C1=CC(=C(C(=C1)O)N)CS IUQQUDOPPAGCQI-UHFFFAOYSA-N 0.000 claims description 2
- JDXKTOBMLZLCSB-UHFFFAOYSA-N anilinothiourea Chemical compound NC(=S)NNC1=CC=CC=C1 JDXKTOBMLZLCSB-UHFFFAOYSA-N 0.000 claims description 2
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid group Chemical group S(N)(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000001476 sodium potassium tartrate Substances 0.000 claims 1
- 238000011161 development Methods 0.000 abstract description 9
- 238000005259 measurement Methods 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 18
- 239000002994 raw material Substances 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 9
- 229910052698 phosphorus Inorganic materials 0.000 description 9
- 239000011574 phosphorus Substances 0.000 description 9
- 239000000377 silicon dioxide Substances 0.000 description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 7
- 229910052750 molybdenum Inorganic materials 0.000 description 7
- 239000011733 molybdenum Substances 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 238000002798 spectrophotometry method Methods 0.000 description 5
- 239000011550 stock solution Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 239000006193 liquid solution Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- HSNVNALJRSJDHT-UHFFFAOYSA-N P(=O)(=O)[Mo] Chemical compound P(=O)(=O)[Mo] HSNVNALJRSJDHT-UHFFFAOYSA-N 0.000 description 3
- 229910052785 arsenic Inorganic materials 0.000 description 3
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000012010 growth Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 239000008239 natural water Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 1
- FULZLIGZKMKICU-UHFFFAOYSA-N N-phenylthiourea Chemical compound NC(=S)NC1=CC=CC=C1 FULZLIGZKMKICU-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- BEWZPBWLGIPWFP-UHFFFAOYSA-N [V].P(=O)(=O)[Mo] Chemical compound [V].P(=O)(=O)[Mo] BEWZPBWLGIPWFP-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000005791 algae growth Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000011964 heteropoly acid Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003987 organophosphate pesticide Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 239000000271 synthetic detergent Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Abstract
The invention discloses a phosphate radical detection reagent, a detection kit and a detection method, wherein the detection reagent comprises a reagent A and a reagent B, the reagent A comprises a strong acid reagent, molybdate and a weighting agent, and the mass ratio of the strong acid reagent to the molybdate to the weighting agent is (2-98): (0.2-20.0): (0-50.0), the reagent B comprises a strong acid reagent, a masking agent, a reducing agent, a speed accelerator and a weighting agent, wherein the mass ratio of the strong acid reagent to the masking agent to the reducing agent to the speed accelerator to the weighting agent is (2-98): (1.0-30.0): (0.5-50.0): (0.1-50.0): (0-50.0). The detection reagent has no special environmental requirement, no special three-waste pollution, low cost, simple detection steps, no interference, more accurate measurement, short color development time and strong mobility.
Description
Technical Field
The invention belongs to the technical field of analytical chemistry, and particularly relates to a phosphate radical detection reagent, a phosphate radical detection kit and a phosphate radical detection method.
Background
Phosphorus is one of the elements necessary for biological growth, but too high a phosphorus content in the water body can interfere with the coagulation process in the water works. Phosphorus is a key element required by algae growth, and excessive phosphorus content can cause excessive growth of algae plants, can cause water quality eutrophication and influence ecological balance of water. The phosphate content in the natural water is not high, and the natural water is mainly from industrial wastewater in industries such as domestic sewage, chemical fertilizer, smelting, organophosphorus pesticide, synthetic detergent and the like. Phosphorus is one of the important indicators for evaluating water quality.
Currently, the determination of phosphate is commonly performed by gravimetric methods, titration methods, ion chromatography, spectrophotometry, atomic absorption spectrophotometry, raman spectroscopy and the like. The spectrophotometry is the most commonly used method, has more application in the water quality detection industry, has the advantages of simplicity, rapidness and accuracy, and has a complete standard analysis and determination method, but the method has the advantages of large reagent dosage, heavy environmental pollution, complexity and time consumption, high professional requirements and emergency difficulty, and limits the application of the spectrophotometry in the rapid detection. The weight method has the advantages of higher accuracy, is still recommended as a standard method at home and abroad so far, is suitable for standard laboratories and research institutions, but has the disadvantage of low analysis speed, so that the weight method cannot be used for on-site analysis of enterprises. The titration method has the advantages of very accurate measurement of the phosphorus content, and is different from an instrument analysis method in that the phosphorus content is higher than the measurement range, and the phosphorus content needs to be absorbed for multiple times to be detected to cause experimental errors. The rapid test method has the advantages of low cost, few hundred blocks for detection for tens of times, high speed, 5 minutes for result output, light weight and convenience, and the disadvantage of insufficient accuracy, and only one large range of values can be estimated.
The existing method for detecting the phosphate content in the water system commonly uses an ammonium molybdate spectrophotometry, and the method comprises a molybdenum yellow method or a molybdenum blue method, and the ammonium molybdate spectrophotometry is simple to operate and low in cost. Molybdenum Huang Fa is directly measured by the action of phosphoric acid and vanadate and molybdic acid to form phosphovanadium molybdenum yellow heteropolyacid. However, in the conventional molybdenum yellow method, a liquid solution of a strong acid such as sulfuric acid or nitric acid is generally used. The liquid solution of the strong acid has high requirement on transportation, complex operation, unsafe and certain danger. The molybdenum blue method is to react active phosphate with molybdate to generate phosphomolybdenum yellow, and the phosphomolybdenum Huang Haiyuan is phosphomolybdenum blue with a reducing agent, the color depth of which is in direct proportion to the concentration of effective phosphorus, accords with the lambert beer law in a certain range, and can be measured by a colorimetric method. The reducing agent is stannous chloride, ascorbic acid, diamine sulfate, sulfite, etc. However, the following disadvantages exist, such as high cost, complicated operation, high professional requirements, difficult emergency and the like, of specific equipment are required, and the application of the method in rapid detection is limited. In order to complement the short plates of the detection, a rapid, accurate, portable, simple and quick phosphate detection kit has been developed in recent years. However, in practical operation, the kits are found to have high false positive, and cannot eliminate interference of elements such as arsenic, silicon and the like.
The Chinese patent with publication number of CN106442511A discloses a rapid phosphate detection kit and a detection method, and by using the detection kit and the detection method of matched test paper, the whole detection process of phosphate can only need 2min, the process is greatly simplified, and the quality guarantee period can reach two years. However, the disadvantage is that the interference of elements such as arsenic and silicon cannot be eliminated. In addition, liquid solutions of strong acids such as sulfuric acid or nitric acid are used. The liquid solution of the strong acid has high requirement on transportation, complex operation, unsafe and certain danger.
Thus, improving the measurement sensitivity of the kit and eliminating interference from other elements is a critical problem that needs to be solved at present.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of the prior art and provide a phosphate radical detection reagent, a phosphate radical detection kit and a phosphate radical detection method.
The specific technical scheme of the invention is as follows:
In one aspect, the invention provides a phosphate radical detection reagent, which comprises a reagent A and a reagent B;
The reagent A comprises a strong acid reagent, molybdate and a weighting agent, wherein the mass ratio of the strong acid reagent to the molybdate to the weighting agent is (2-98): (0.2-20.0): (0-50.0);
The reagent B comprises a strong acid reagent, a masking agent, a reducing agent, a speed accelerator and a weighting agent, wherein the mass ratio of the strong acid reagent to the masking agent to the reducing agent to the speed accelerator to the weighting agent is (2-98): (1.0-30.0): (0.5-50.0): (0.1-50.0): (0-50.0).
Further, the mass ratio of the strong acid reagent to the molybdate to the weighting agent in the reagent A is (5-10): (0.5-2.0): (0-5.0);
the mass ratio of the strong acid reagent to the masking agent to the reducing agent to the accelerator to the weighting agent in the reagent B is (5-10): (1.0-5.0): (0.5-1.5): (0.1-0.5): (0-5.0).
Preferably, the mass ratio of the strong acid reagent, the molybdate and the weighting agent in the reagent A is 7:1:2;
The mass ratio of the strong acid reagent to the masking agent to the reducing agent to the accelerator to the weighting agent in the reagent B is 5:1:1:0.2:2.
Further, the strong acid reagent is selected from one or more of sulfamic acid, citric acid and glycolic acid;
The molybdate comprises one or more of sodium molybdate, ammonium molybdate and potassium molybdate;
The masking agent comprises one or more of potassium sodium tartrate, citric acid, oxalic acid, tartaric acid and EDTA;
The reducing agent comprises at least one of ascorbic acid, hydrazine sulfate, stannous chloride, hydrazine sulfate, 1-amino-2-catechol-4-sulfonic acid, sulfanylmethyl aminophenol, hydroquinone, phenylthiosemicarbazide, ferrous ammonium sulfate-fructose, ferrous ammonium sulfate-glucose, sodium metabisulfite, metol, sodium formaldehyde sulfoxylate, titanium trichloride, sulfite-ferric salt, ferrous ammonium sulfate, sodium sulfite, sodium bisulphite and antimony (III);
the accelerator is at least one of antimony potassium tartrate and bismuth nitrate;
The weighting agent comprises one or more of sodium chloride, sodium sulfate and potassium sulfate.
Further, the strongly acidic reagent is sulfamic acid, the molybdate is sodium molybdate, the masking agent is potassium sodium tartrate, the reducing agent is ascorbic acid, the accelerator is antimony potassium tartrate, and the weighting agent is sodium chloride.
In another aspect, the invention provides a phosphate radical detection kit, which comprises a reagent A, a reagent B and a standard colorimetric card.
In another aspect, the present invention provides a method for preparing the above-mentioned detection kit, comprising the steps of:
Preparation of reagent A: fully grinding the strong acid reagent, the molybdate and the weighting agent according to the mass ratio, enabling the ground mixed components to pass through an 80-target standard sieve, sub-packaging, and vacuumizing or sealing by introducing inert gas;
Preparation of reagent B: fully grinding the strong acid reagent, the masking agent, the reducing agent, the weighting agent and the accelerating agent according to the mass ratio, enabling the ground mixed components to pass through an 80-target standard sieve, sub-packaging, and vacuumizing or sealing by introducing inert gas;
Preparing a standard color chart: preparing phosphate standard solutions with the concentration of 0mg/L, 2.0mg/L, 5.0mg/L, 10.0mg/L, 20mg/L, 50mg/L, 100mg/L, 200mg/L, 500mg/L and 1000mg/L, taking 1-5mL of each phosphate standard solution, respectively adding the reagent A, shaking uniformly, then adding the reagent B, shaking uniformly, and developing for 1-5min to obtain the standard colorimetric card.
Further, the reagent A and the reagent B are respectively packaged into 0.1-0.5g of each tube.
The invention also provides a method for detecting phosphate radical, which adopts the detection kit to detect, and comprises the following steps: adding 1-5mL of water sample to be detected into the reagent A, shaking uniformly, adding the reagent B, shaking uniformly, comparing with a standard colorimetric card after 1-5min, and determining the concentration of phosphate radical in the water sample to be detected.
The detection kit of the invention should be stored in a cool and dry place, and the storage temperature is preferably lower than 26 ℃. If the temperature is higher than 25 ℃, the unused test paper bag is put into a fresh-keeping layer in a refrigerator for preservation, and is put into a package which is light-proof and moisture-proof for preservation. The effective service life of the detection kit is about one year.
The beneficial effects of the invention are as follows:
1. The phosphate radical detection method is based on a phosphomolybdic blue method, and is a rapid and flexible phosphate radical rapid detection method which does not need instruments and equipment and has low production and use costs. The kit has the advantages of no special environmental requirement, no special three-waste pollution, low cost, simple detection steps, no interference, more accurate measurement, short color development time and strong mobility. Compared with the traditional method or other measurement forms, the invention is more convenient to use and does not need special technicians to measure. The reagents used in the invention are all common chemical reagents, safe and reliable and low in cost. The method has wide application range, and can be used for measuring the phosphate radical content of water bodies such as chemical sewage, surface water, urban sewage recycling-landscape environmental water, urban miscellaneous water and the like, in particular to the monitoring of phosphate radical in the environment protection field.
2. According to the invention, more acid is added into the reagent A, so that the interference of elements such as arsenic, silicon and the like is eliminated. The phosphate in the water sample to be detected reacts with the molybdate in the reagent A to generate light yellow phosphomolybdic yellow, and then the masking agent in the added reagent B can chelate the molybdenum in the molybdate, so that the detection sensitivity is improved.
Drawings
FIG. 1 is a standard color chart of the test kit of example 1.
FIG. 2 shows the color development results of example 1;
FIG. 3 shows the color development results of example 2;
FIG. 4 shows the color development results of example 3;
FIG. 5 shows the color development results of example 4.
Detailed Description
For a clearer understanding of the present invention, the present invention will now be further described with reference to the following examples and drawings. The examples are for illustration only and are not intended to limit the invention in any way. In the examples, each of the starting reagent materials is commercially available, and the experimental methods without specifying the specific conditions are conventional methods and conventional conditions well known in the art, or according to the conditions recommended by the instrument manufacturer.
The embodiment provides a phosphate radical detection kit, which comprises a reagent A, a reagent B and a standard colorimetric card, and is prepared by the following steps:
Preparation of reagent A: according to the mass ratio of the strong acid reagent, the molybdate and the weighting agent of (2-98): (0.2-20.0): (0-50.0), preparing a strong acid reagent, molybdate and a weighting agent, adding the components into a mortar, fully grinding until all raw materials can pass through an 80-target standard sieve, then sub-packaging into 0.1-0.5 g of each tube, and vacuumizing or sealing by introducing inert gas. In a preferred embodiment, the mass ratio of strongly acidic reagent, molybdate and weighting agent is (5 to 10): (0.5-2.0): (0-5.0).
Preparation of reagent B: according to the mass ratio of the strong acid reagent, the masking agent, the reducing agent, the accelerator and the weighting agent of (2-98): (1.0-30.0): (0.5-50.0): (0.1-50.0): (0-50.0), preparing a strong acid reagent, a masking agent, a reducing agent, a accelerating agent and a weighting agent, adding the components into a mortar, fully grinding until all raw materials can pass through an 80-target standard sieve, then sub-packaging into 0.1-0.5 g of each tube, and vacuumizing or sealing by inert gas. In a preferred embodiment, the mass ratio of the strongly acidic agent, masking agent, reducing agent, accelerator, and weighting agent is (5-10): (1.0-5.0): (0.5-1.5): (0.1-0.5): (0-5.0).
Standard colorimetric card preparation: phosphate stock solution (1000 mg/L) is adopted to prepare phosphate standard solutions with the concentration of 0mg/L, 2.0mg/L, 5.0mg/L, 10.0mg/L, 20mg/L, 50mg/L, 100mg/L, 200mg/L, 500mg/L and 1000mg/L, 1-5mL of each phosphate standard solution is taken, solid reagents A are respectively added, shaking is carried out, solid reagents B are then added, shaking is carried out, and the color is basically stable after color development is carried out for 1-5 minutes, thus obtaining the standard colorimetric card.
Wherein the strong acid reagent is selected from one or more of sulfamic acid, citric acid and glycolic acid;
the molybdate comprises one or more of sodium molybdate, ammonium molybdate and potassium molybdate;
the masking agent comprises one or more of potassium sodium tartrate, citric acid, oxalic acid, tartaric acid and EDTA, and is used for chelating molybdenum in molybdate;
The reducing agent comprises at least one of ascorbic acid, hydrazine sulfate, stannous chloride, hydrazine sulfate, 1-amino-2-catechol-4-sulfonic acid, sulfanylp-methylaminophenol, hydroquinone, phenylthiourea, ferrous ammonium sulfate-fructose, ferrous ammonium sulfate-glucose, sodium metabisulfite, metol, sodium formaldehyde sulfoxylate, titanium trichloride, sulfite-ferric salt, ferrous ammonium sulfate, sodium sulfite, sodium bisulphite and antimony (III);
the accelerator is at least one of antimony potassium tartrate and bismuth nitrate;
The weighting agent comprises one or more of sodium chloride, sodium sulfate and potassium sulfate, and the weighting agent facilitates the weighing of the reagent A and the reagent B.
The prepared detection kit should be stored in a shade and dry place, and the storage temperature is preferably lower than 26 ℃. If the temperature is higher than 25 ℃, the unused test paper bag is put into a fresh-keeping layer in a refrigerator for preservation, and is put into a package which is light-proof and moisture-proof for preservation.
The embodiment further provides a method for detecting phosphate radical, which adopts the prepared detection kit for detection and comprises the following steps: adding 1-5mL of water sample to be detected into the reagent A, shaking uniformly, adding the reagent B, shaking uniformly, displaying bluish green if phosphate radical exists in water after 1-5min, comparing the color depth with the concentration of the phosphate radical in water, and determining the concentration of the phosphate radical in the water sample to be detected.
Example 1
The embodiment provides a detection kit, and the raw materials of each component of a reagent A are as follows: sulfamic acid 7g, sodium molybdate 1g and sodium chloride 2g. The reagent B comprises the following raw materials in parts by weight: sulfamic acid 5g, potassium sodium tartrate 1g, ascorbic acid 1g, antimony potassium tartrate 0.2g and sodium chloride 2g. Reagent A and reagent B were prepared as described above, and each of reagent A and reagent B was packaged in 0.2g per tube.
Phosphate stock solution (1000 mg/L) is adopted to prepare a phosphate standard solution with the concentration of 0mg/L、0.1mg/L、0.2mg/L、0.5mg/L、1mg/L、2.0mg/L、5.0mg/L、10.0mg/L、20mg/L、30mg/L、50mg/L、100mg/L、200mg/L、500mg/L、1000mg/L, 1-5mL of each phosphate standard solution is taken, solid reagent A is respectively added, shaking is carried out uniformly, solid reagent B is then added, shaking is carried out uniformly, color development is basically stable after 1-5 minutes, the color development results of phosphate standard solutions with different concentrations are shown in figure 2, and a standard colorimetric card prepared based on the reagent A and the reagent B of the kit according to the embodiment is shown in figure 1.
Example 2
The embodiment provides a detection kit, and the raw materials of each component of a reagent A are as follows: sulfamic acid 1g, sodium molybdate 1g and sodium chloride 8g. The reagent B comprises the following raw materials in parts by weight: sulfamic acid 1g, potassium sodium tartrate 1g, ascorbic acid 1g, antimony potassium tartrate 0.2g and sodium chloride 7g. Reagent A and reagent B were prepared as described above, and each of reagent A and reagent B was packaged in 0.2g per tube.
Preparing silica standard solutions with the concentration of 0mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L, 1mg/L, 2.0mg/L, 5.0mg/L, 10.0mg/L, 20mg/L, 30mg/L, 50mg/L and 100mg/L by adopting silica stock solution (1000 mg/L), taking 1-5mL of each silica standard solution, respectively adding solid reagent A, shaking uniformly, then adding solid reagent B, shaking uniformly, and developing for 1-5 minutes, wherein the color is basically stable. The results are shown in FIG. 3. The concentration of acid is reduced, and the kit cannot exclude interference of elements such as silicon.
Example 3
The embodiment provides a detection kit, and the raw materials of each component of a reagent A are as follows: sulfamic acid 7g, sodium molybdate 1g and sodium chloride 2g. The reagent B comprises the following raw materials in parts by weight: sulfamic acid 5g, antimony potassium tartrate 0.2g and sodium chloride 4g. Reagent A and reagent B were prepared as described above, and each of reagent A and reagent B was packaged in 0.2g per tube.
Preparing silica standard solutions with the concentration of 0.25mg/L, 0.5mg/L, 1.0mg/L, 2.0mg/L, 4.0mg/L, 8.0mg/L, 15.0mg/L, 30mg/L, 60mg/L, 120mg/L, 250mg/L and 500mg/L by adopting silica stock solutions (1000 mg/L), taking 1-5mL of each silica standard solution, respectively adding solid reagent A, shaking uniformly, then adding solid reagent B, shaking uniformly, and developing for 1-5 minutes, wherein the color is basically stable. The results are shown in FIG. 4. The reagent kit can not eliminate the interference of elements such as silicon without adding a masking agent.
Example 4
The embodiment provides a detection kit, and the raw materials of each component of a reagent A are as follows: sulfamic acid 7g, sodium molybdate 1g and sodium chloride 2g. The reagent B comprises the following raw materials in parts by weight: sulfamic acid 5g, antimony potassium tartrate 0.2g and sodium chloride 4g. Reagent A and reagent B were prepared as described above, and each of reagent A and reagent B was packaged in 0.2g per tube.
Preparing silica standard solutions with the concentration of 0.02mg/L, 0.05mg/L, 0.1mg/L, 0.2mg/L, 0.4mg/L, 0.8mg/L, 1.5mg/L, 3.0mg/L, 6.0mg/L, 12.0mg/L, 25mg/L and 50mg/L by adopting a silica stock solution (1000 mg/L), taking 1-5mL of each silica standard solution, respectively adding a solid reagent B, shaking uniformly, then adding a solid reagent A, shaking uniformly, and developing the color for 1-5 minutes until the color is basically stable. The results are shown in FIG. 5. The reagent kit can not eliminate the interference of elements such as silicon without adding a masking agent. The results are shown in FIG. 5. The sample adding sequence of the reagent is changed, so that interference of elements such as silicon cannot be eliminated.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (9)
1. A phosphate detection reagent, wherein the detection reagent comprises a reagent A and a reagent B;
The reagent A comprises a strong acid reagent, molybdate and a weighting agent, wherein the mass ratio of the strong acid reagent to the molybdate to the weighting agent is (2-98): (0.2-20.0): (0-50.0);
The reagent B comprises a strong acid reagent, a masking agent, a reducing agent, a speed accelerator and a weighting agent, wherein the mass ratio of the strong acid reagent to the masking agent to the reducing agent to the speed accelerator to the weighting agent is (2-98): (1.0-30.0): (0.5-50.0): (0.1-50.0): (0-50.0).
2. The detection reagent according to claim 1, wherein the mass ratio of the strongly acidic reagent, the molybdate and the weighting agent in the reagent a is (5 to 10): (0.5-2.0): (0-5.0);
the mass ratio of the strong acid reagent to the masking agent to the reducing agent to the accelerator to the weighting agent in the reagent B is (5-10): (1.0-5.0): (0.5-1.5): (0.1-0.5): (0-5.0).
3. The detection reagent according to claim 1, wherein the mass ratio of the strong acid reagent, the molybdate and the weighting agent in the reagent a is 7:1:2;
The mass ratio of the strong acid reagent to the masking agent to the reducing agent to the accelerator to the weighting agent in the reagent B is 5:1:1:0.2:2.
4. A detection reagent according to any one of claims 1 to 3, wherein the strongly acidic reagent is selected from one or more of sulfamic acid, citric acid, glycolic acid;
The molybdate comprises one or more of sodium molybdate, ammonium molybdate and potassium molybdate;
The masking agent comprises one or more of potassium sodium tartrate, citric acid, oxalic acid, tartaric acid and EDTA;
The reducing agent comprises at least one of ascorbic acid, hydrazine sulfate, stannous chloride, hydrazine sulfate, 1-amino-2-catechol-4-sulfonic acid, sulfanylmethyl aminophenol, hydroquinone, phenylthiosemicarbazide, ferrous ammonium sulfate-fructose, ferrous ammonium sulfate-glucose, sodium metabisulfite, metol, sodium formaldehyde sulfoxylate, titanium trichloride, sulfite-ferric salt, ferrous ammonium sulfate, sodium sulfite, sodium bisulphite and antimony (III);
the accelerator is at least one of antimony potassium tartrate and bismuth nitrate;
The weighting agent comprises one or more of sodium chloride, sodium sulfate and potassium sulfate.
5. A detection reagent according to any one of claims 1 to 3 wherein the strongly acidic reagent is sulfamic acid, the molybdate is sodium molybdate, the masking agent is sodium potassium tartrate, the reducing agent is ascorbic acid, the speed increasing agent is potassium antimonate, and the weighting agent is sodium chloride.
6. A phosphate detection kit, which is characterized by comprising the reagent A and the reagent B according to claim 1 and a standard colorimetric card.
7. The method for preparing the detection kit as claimed in claim 6, comprising the steps of:
Preparation of reagent A: fully grinding the strong acid reagent, the molybdate and the weighting agent according to the mass ratio of claim 1, enabling the ground mixed components to pass through an 80-target standard sieve, sub-packaging, and vacuumizing or sealing by inert gas;
Preparation of reagent B: fully grinding the strong acid reagent, the masking agent, the reducing agent, the accelerator and the weighting agent according to the mass ratio of claim 1, enabling the ground mixed components to pass through an 80-target standard sieve, sub-packaging, and vacuumizing or sealing by inert gas;
Preparing a standard color chart: preparing phosphate standard solutions with the concentration of 0mg/L, 2.0mg/L, 5.0mg/L, 10.0mg/L, 20mg/L, 50mg/L, 100mg/L, 200mg/L, 500mg/L and 1000mg/L, taking 1-5mL of each phosphate standard solution, respectively adding the reagent A, shaking uniformly, then adding the reagent B, shaking uniformly, and developing for 1-5min to obtain the standard colorimetric card.
8. The method of claim 7, wherein the reagents A and B are dispensed in a quantity of 0.1-0.5g per tube.
9. A method for detecting phosphate, characterized in that the detection is carried out by using the detection kit as claimed in claim 6, comprising the following steps: adding 1-5mL of water sample to be detected into the reagent A, shaking uniformly, adding the reagent B, shaking uniformly, comparing with a standard colorimetric card after 1-5min, and determining the concentration of phosphate radical in the water sample to be detected.
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