CN116925379A - OPA-Tb-MOF material for detecting ammonia nitrogen in water body, and preparation method and application thereof - Google Patents
OPA-Tb-MOF material for detecting ammonia nitrogen in water body, and preparation method and application thereof Download PDFInfo
- Publication number
- CN116925379A CN116925379A CN202311005294.2A CN202311005294A CN116925379A CN 116925379 A CN116925379 A CN 116925379A CN 202311005294 A CN202311005294 A CN 202311005294A CN 116925379 A CN116925379 A CN 116925379A
- Authority
- CN
- China
- Prior art keywords
- opa
- mof
- ammonia nitrogen
- water
- mof material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 47
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 67
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims description 29
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 22
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 15
- 235000010265 sodium sulphite Nutrition 0.000 claims description 11
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 238000001917 fluorescence detection Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- GPNNOCMCNFXRAO-UHFFFAOYSA-N 2-aminoterephthalic acid Chemical compound NC1=CC(C(O)=O)=CC=C1C(O)=O GPNNOCMCNFXRAO-UHFFFAOYSA-N 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- 239000007853 buffer solution Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 19
- 239000003673 groundwater Substances 0.000 abstract description 11
- 230000035484 reaction time Effects 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 12
- 235000019270 ammonium chloride Nutrition 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 241000282414 Homo sapiens Species 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 238000000527 sonication Methods 0.000 description 3
- 238000002798 spectrophotometry method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000872 buffer Substances 0.000 description 2
- 230000000711 cancerogenic effect Effects 0.000 description 2
- 231100000315 carcinogenic Toxicity 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000012851 eutrophication Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- OJHBLBWMMQBLFD-UHFFFAOYSA-N 4-bromophthalaldehyde Chemical compound BrC1=CC=C(C=O)C(C=O)=C1 OJHBLBWMMQBLFD-UHFFFAOYSA-N 0.000 description 1
- 241000251468 Actinopterygii Species 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- ZNZYKNKBJPZETN-WELNAUFTSA-N Dialdehyde 11678 Chemical group N1C2=CC=CC=C2C2=C1[C@H](C[C@H](/C(=C/O)C(=O)OC)[C@@H](C=C)C=O)NCC2 ZNZYKNKBJPZETN-WELNAUFTSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004178 biological nitrogen fixation Methods 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000007665 chronic toxicity Effects 0.000 description 1
- 231100000160 chronic toxicity Toxicity 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 125000000904 isoindolyl group Chemical class C=1(NC=C2C=CC=CC12)* 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 231100000219 mutagenic Toxicity 0.000 description 1
- 230000003505 mutagenic effect Effects 0.000 description 1
- XKLJHFLUAHKGGU-UHFFFAOYSA-N nitrous amide Chemical compound ON=N XKLJHFLUAHKGGU-UHFFFAOYSA-N 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 231100000378 teratogenic Toxicity 0.000 description 1
- 230000003390 teratogenic effect Effects 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
-
- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Immunology (AREA)
- Physics & Mathematics (AREA)
- Polymers & Plastics (AREA)
- Molecular Biology (AREA)
- Organic Chemistry (AREA)
- Medicinal Chemistry (AREA)
- Optics & Photonics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides an OPA-Tb-MOF material for detecting ammonia nitrogen in a water body, and a preparation method and application thereof, and relates to the technical field of groundwater detection. The method comprises two steps of forming a metal organic framework and preparing the OPA-Tb-MOF material, and the finally obtained OPA-Tb-MOF material can be used as a high-efficiency fluorescence sensor for rapidly detecting the ammonia nitrogen content in underground water, has a wider detection range (0-110 ppm), has a detection limit as low as 0.00083ppm, and has a reaction time of only 5min. Meanwhile, the OPA-Tb-MOF material has good selectivity and high sensitivity, is easy to operate, and does not have any environmental pollution risk.
Description
Technical Field
The invention relates to the technical field of underground water detection, in particular to an OPA-Tb-MOF material for detecting ammonia nitrogen in a water body, and a preparation method and application thereof.
Background
The ammonia nitrogen content in the groundwater refers to free ammonia (NH) 3 ) And ammonium ion (NH) 4+ ) Nitrogen in the form of nitrogen. Sources of ammonia nitrogen in groundwater mainly include natural processes and human activities such as precipitation and dust fall, biological nitrogen fixation, chemical fertilizers, and wastewaterDischarge, etc.
Groundwater is one of important drinking water sources for human beings, and the excessive ammonia nitrogen content in groundwater can cause adverse effects on human health and water ecological environment, and mainly has the following points: the ammonia nitrogen can consume dissolved oxygen in the water body, so that the water body is anoxic, blackened and smelly, and the water quality is affected; ammonia nitrogen can promote eutrophication of water, increase growth of algae, cause filter blockage, water movement resistance, water color and taste change, blue algae toxin harm and the like; the ammonia nitrogen can react with chlorine in water to generate cancerogenic substances such as nitrosamine, or react with amines to generate three-induced substances (cancerogenic, mutagenic and teratogenic) such as nitrite, which causes chronic toxicity to human body; ammonia nitrogen damages the gill tissue of fish, reduces the oxygen carrying capacity of blood, and causes choking death. Therefore, the method can rapidly, accurately and efficiently measure the ammonia nitrogen content in the groundwater, is beneficial to evaluating the pollution condition and eutrophication degree of the water body, discovers and controls the pollution condition of the groundwater, and has important significance for guaranteeing the quality of the groundwater and the health and safety of human bodies.
Currently common methods for measuring the ammonia nitrogen content of the underground water comprise a Nahner reagent spectrophotometry, a salicylic acid spectrophotometry, an electrode method, a gas-phase molecular absorption spectrometry and the like. However, the method has the problems of long detection time, relatively complex operation steps, limited detection range, unfriendly environment and the like. Therefore, how to provide a method for detecting the ammonia nitrogen content of underground water, which is rapid, accurate, efficient, wide in detection range and small in environmental influence, is one of the technical problems to be solved at present.
Disclosure of Invention
In order to solve the problems, the invention provides the OPA-Tb-MOF material for detecting the ammonia nitrogen in the water body, which can accurately realize the accurate determination of the ammonia nitrogen content in the underground water in a short time, has a large detection range, is simple to operate and is environment-friendly.
The preparation method of the OPA-Tb-MOF material for detecting ammonia nitrogen in water body comprises the following steps:
s1, preparation of a metal organic framework (Tb-MOF):
tb (NO) 3 ) 3 ·6H 2 Adding O and 2-amino terephthalic acid (BDC) into a polytetrafluoroethylene lining container filled with N, N-Dimethylformamide (DMF), fully dissolving reactants under ultrasonic waves, sealing the container in a polytetrafluoroethylene autoclave, rapidly heating and preserving heat, naturally cooling the autoclave to room temperature after preserving heat, centrifuging the mixture solution, washing with ultrapure water and ethanol for three times, and freeze-drying to obtain Tb-MOF;
s2, preparation of OPA-Tb-MOF material:
dissolving Tb-MOF and 4-bromophthalic dicarboxaldehyde in water, adding potassium iodide and potassium carbonate, stirring at ambient temperature for 12h, and freeze-drying to obtain OPA-Tb-MOF material.
Further, the Tb (NO 3 ) 3 ·6H 2 The weight ratio of O to BDC is (1-4): (1-4).
Preferably, the Tb (NO 3 ) 3 ·6H 2 The weight ratio of O to BDC is 1:4.
further, the heating temperature is 100-140 ℃, and the heat preservation time is 24 hours.
Further, the centrifugal speed was 4000rpm/min and the centrifugal time was 10min.
Further, the weight ratio of the Tb-MOF to the 4-bromophthalic aldehyde to the potassium iodide to the potassium carbonate is 4:2:1:3.
further, the feed liquid ratio of Tb-MOF to water is 1mg/mL.
The invention also provides the OPA-Tb-MOF material for detecting ammonia nitrogen in the water body, which is prepared by the method.
The invention also aims to provide an application of the OPA-Tb-MOF material in detecting ammonia nitrogen content in water, and the specific method is as follows:
and (3) regulating the pH=7 of the water sample by using a Tris-HCl buffer solution, adding an OPA-Tb-MOF solution and a sodium sulfite solution, reacting for 5min, and performing fluorescence detection by using a fluorescence spectrophotometer to determine the ammonia nitrogen content in the water body.
Further, the volume ratio of the water sample, the OPA-Tb-MOF solution and the sodium sulfite solution is 1:8:1.
further, the concentration of the OPA-Tb-MOF solution is 2 mg.mL -1 。
Further, the concentration of the sodium sulfite solution is 5.160 ×10 -3 M。
Further, the fluorescence detection slit is 5nm, and the voltage is 450V.
The 4-bromo-phthalaldehyde can be better modified to the Tb-MOF due to the advantages of large porosity, large specific surface area, multiple metal sites and the like of the Tb-MOF. The modified OPA-Tb-MOF material has special topological structure characteristics, and the OPA-Tb-MOF material organic ligand has fluorescent property. When ammonia nitrogen is combined with the dialdehyde structure exposed on the OPA-Tb-MOF, the isoindole derivative with strong fluorescence is generated, and the fluorescence intensity at 430nm is changed, so that the ammonia nitrogen can be detected and identified, and the detection range is wider.
Compared with the prior art, the invention has the beneficial technical effects that:
the OPA-Tb-MOF material can be used as a high-efficiency fluorescence sensor, the ammonia nitrogen content in the underground water can be rapidly detected through fluorescence enhancement, the detection range is 0-110ppm, the detection limit is as low as 0.00083ppm, and the reaction time is only 5min. Furthermore, the OPA-Tb-MOF material has good selectivity, high sensitivity and simple operation, and does not have any environmental pollution risk.
Drawings
The invention is further described with reference to the following description of the drawings.
FIG. 1 is a graph of pH of a solution versus fluorescence intensity;
FIG. 2 is a graph showing the relationship between sodium sulfite concentration and fluorescence intensity;
FIG. 3 is a graph showing the relationship between the reaction time and the fluorescence intensity;
FIG. 4 shows the detection limit and detection range of ammonia nitrogen for OPA-Tb-MOF material;
FIG. 5 shows selectivity and interference resistance of OPA-Tb-MOF for detecting ammonia nitrogen.
Detailed Description
The technical scheme provided by the invention is further described below by combining with the embodiment.
Example 1 selection of pH
OPA-Tb-MOF was dispersed in ultrapure water to prepare 2mg/mL of OPA-Tb-MOF solution, the solution was dispersed by sonication, and 8mL of OPA-Tb-MOF supernatant, 1mL of ammonium chloride (9.346X 10) were added to a centrifuge tube -6 M) and 1mL of sodium sulfite solution (5.157X 10) -3 M), and the pH of the ammonium chloride was adjusted by Tris-HCl buffer (ph=6-10). After 5min of reaction, fluorescence detection (slit: 5nm, voltage: 450V) was performed. The detection results are shown in FIG. 1.
From the results, the fluorescence intensity of the solution increases rapidly when the pH value is 7, and decreases when the pH value is less than 6.5 or more than 10. Obviously, the optimum pH is around 7, so the pH of the solution of the present invention is controlled at 7. In addition, the pH of high ammonium groundwater is also typically around 7, so that when this material is applied to groundwater, it is easier to control in pH environments.
EXAMPLE 2 selection of sodium sulfite concentration
8mL of OPA-Tb-MOF supernatant, 1mL of ammonium chloride (9.346X 10) -6 M) was added to the centrifuge tube, wherein the pH of the ammonium chloride solution was adjusted to 7 by Tris-HCl buffer. Sodium sulfite solutions (1 mL) of different concentrations were then added to the centrifuge tube. After 5min of reaction, fluorescence detection (slit: 5nm, voltage: 450V) was performed. The results are shown in FIG. 2.
From the results, when Na is contained in the reaction solution 2 SO 3 Is about 5.157 ×10 in concentration -4 M, the fluorescence intensity of the solution was the most varied, indicating 5.157X 10 -4 Na of M 2 SO 3 In an amount sufficient to effect a fluorescent reaction.
Example 3 selection of reaction time
OPA-Tb-MOF was dispersed in ultrapure water to prepare a 2mg/mL OPA-Tb MOF solution. The solution was dispersed by sonication. To the centrifuge tube, 8mL of OPA-Tb-MOF supernatant, 1mL of ammonium chloride (9.346X 10) -6 M) and 1mL of sodium sulfite solution (5.157X 10) -3 M), wherein the ph=7 of the ammonium chloride is adjusted by Tris-HCl buffer solution. After a controlled time, fluorescence detection (slit: 5nm, voltage: 450V) was performed at intervals. The detection results are shown in FIG. 3.
From the results, when the reaction time reached 80min, the fluorescence intensity was not significantly enhanced and gradually flattened. The reaction was equilibrated gradually at 80 min. When the reaction was continued for 5min, the fluorescence intensity change was already significant enough to support our detection. Therefore, 5min was chosen as the detection time.
Example 4
The preparation method of the OPA-Tb-MOF material for detecting ammonia nitrogen in water comprises the following steps:
preparation of S1, tb-MOF:
starting reactant Tb (NO) 3 ) 3 ·6H 2 O (0.2 g) and BDC (0.8 g) were added to a polytetrafluoroethylene-lined vessel filled with 50mL DMF, the reactants were sufficiently dissolved by sonication, then the vessel was closed in a polytetrafluoroethylene autoclave, rapidly heated to 100℃by an oven and held at this temperature for 24 hours, the autoclave was left to cool naturally to room temperature, the mixture solution was centrifuged at 4000rpm/min for 10min, then washed three times with ultrapure water and ethanol, and dried in a freeze-dryer to obtain Tb-MOF as yellow powder;
s2, preparation of OPA-Tb-MOF material:
then 20mg of Tb-MOF and 10mg of 4-bromophthalic aldehyde were dissolved in 20mL of water, then 5mg of potassium iodide and 15mg of potassium carbonate were added to the above mixed solution, followed by stirring at ambient temperature for 12 hours, and the final solution was freeze-dried to obtain OPA-Tb-MOF as dark red powder.
Performing the OPA-Tb-MOF pair NH in Jiang Han plain groundwater 3 The test results of the detection effect of N are as follows:
from this, it can be seen that the NH of the fluorescence sensing method based on OPA-Tb-MOF material of the invention 3 Calculated value and passage of-NThe concentrations of the real water samples measured by the ultraviolet spectrophotometry are very matched, and the relative standard deviation is less than or equal to 3 percent. The fluorescence detection method can be used for NH in actual water sample 3 High-precision detection of N and is very environmentally friendly.
The principles and embodiments of the present invention have been described herein with reference to specific examples, the description of which is intended only to assist in understanding the methods of the present invention and the core ideas thereof; also, it is within the scope of the present invention to be modified by those of ordinary skill in the art in light of the present teachings. In view of the foregoing, this description should not be construed as limiting the invention.
Claims (10)
1. The preparation method of the OPA-Tb-MOF material for detecting ammonia nitrogen in the water body is characterized by comprising the following steps of:
s1, preparation of a metal organic framework (Tb-MOF):
tb (NO) 3 ) 3 ·6H 2 Adding O and 2-amino terephthalic acid (BDC) into a polytetrafluoroethylene lining container filled with N, N-Dimethylformamide (DMF), fully dissolving reactants under ultrasonic waves, sealing the container in a polytetrafluoroethylene autoclave, rapidly heating and preserving heat, naturally cooling the autoclave to room temperature after preserving heat, centrifuging the mixture solution, washing with ultrapure water and ethanol for three times, and freeze-drying to obtain Tb-MOF;
s2, preparation of OPA-Tb-MOF material:
dissolving Tb-MOF and 4-bromophthalic dicarboxaldehyde in water, adding potassium iodide and potassium carbonate, stirring at ambient temperature for 12h, and freeze-drying to obtain OPA-Tb-MOF material.
2. The method for preparing OPA-Tb-MOF material for detecting ammonia nitrogen in water according to claim 1, wherein said Tb (NO 3 ) 3 ·6H 2 The weight ratio of O to BDC is (1-4): (1-4).
3. The method for preparing the OPA-Tb-MOF material for detecting ammonia nitrogen in water according to claim 1, wherein the heating temperature is 100-140 ℃ and the heat preservation time is 24h.
4. The method for preparing the OPA-Tb-MOF material for detecting ammonia nitrogen in water according to claim 1, wherein the weight ratio of Tb-MOF to 4-bromophthalic dicarboxaldehyde to potassium iodide to potassium carbonate is 4:2:1:3.
5. the method for preparing an OPA-Tb-MOF material for detecting ammonia nitrogen in a water body according to claim 1, wherein the feed liquid ratio of Tb-MOF to water is 1mg/mL.
6. An OPA-Tb-MOF material for detecting ammonia nitrogen in a water body, characterized by being prepared by the method of any one of claims 1 to 5.
7. The application of the OPA-Tb-MOF material for detecting ammonia nitrogen in water as claimed in claim 6, wherein the method is as follows:
and (3) regulating the pH=7 of the water sample by using a Tris-HCl buffer solution, adding an OPA-Tb-MOF solution and a sodium sulfite solution, reacting for 5min, and performing fluorescence detection by using a fluorescence spectrophotometer to determine the ammonia nitrogen content in the water body.
8. The application of the OPA-Tb-MOF material for detecting ammonia nitrogen in water according to claim 7, wherein the volume ratio of the water sample, the OPA-Tb-MOF solution and the sodium sulfite solution is 1:8:1.
9. the use of an OPA-Tb-MOF material for detecting ammonia nitrogen in water according to claim 7, wherein the concentration of the OPA-Tb-MOF solution is 2mg/mL -1 。
10. A method according to claim 7 for a body of waterApplication of OPA-Tb-MOF material for detecting ammonia nitrogen in water, wherein the concentration of sodium sulfite solution is 5.160 multiplied by 10 -3 M。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311005294.2A CN116925379A (en) | 2023-08-10 | 2023-08-10 | OPA-Tb-MOF material for detecting ammonia nitrogen in water body, and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311005294.2A CN116925379A (en) | 2023-08-10 | 2023-08-10 | OPA-Tb-MOF material for detecting ammonia nitrogen in water body, and preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116925379A true CN116925379A (en) | 2023-10-24 |
Family
ID=88377223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311005294.2A Pending CN116925379A (en) | 2023-08-10 | 2023-08-10 | OPA-Tb-MOF material for detecting ammonia nitrogen in water body, and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116925379A (en) |
-
2023
- 2023-08-10 CN CN202311005294.2A patent/CN116925379A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Chi et al. | A simple, reliable and sensitive colorimetric visualization of melamine in milk by unmodified gold nanoparticles | |
| CN107290316B (en) | Novel tetracycline fluorescence detection method based on zirconium-based MOF | |
| CN107478698B (en) | A kind of preparation method and application of in-situ preparation silver sulfide competitive type aflatoxin optical electro-chemistry sensor | |
| CN111687408B (en) | Fluorescent copper nanocluster, preparation method and application thereof | |
| Si et al. | Zeolitic imidazolate framework-8 for ratiometric fluorescence sensing tetracyclines in environmental water based on AIE effects | |
| Sepahvand et al. | Plasmonic nanoparticles for colorimetric detection of nitrite and nitrate | |
| Hassan et al. | Selective potentiometric determination of nitrite ion using a novel (4-sulphophenylazo-) 1-naphthylamine membrane sensor | |
| CN111253930A (en) | Fluorescent gold nanocluster and preparation method and application thereof | |
| Ji et al. | A lanthanide-MOF based host–guest intelligent dual-stimulus response platform for naked-eye and ratiometric fluorescence monitoring of food freshness | |
| El-Feky et al. | Quantification of silver in several samples using a new ionophore polymer membrane as an optical sensor | |
| áM Tzouwara-Karayanni | Simultaneous spectrofluorimetric determination of selenium (IV) and (VI) by flow injection analysis | |
| CN113249115B (en) | Preparation of metal organic framework composite material and application of metal organic framework composite material as ratio type fluorescent probe in detection of hydrogen peroxide and Pi | |
| Chen et al. | A novel resonance Rayleigh scattering assay for trace formaldehyde detection based on Ce-MOF probe and acetylacetone reaction | |
| Zhang et al. | An enhanced-stability metal–organic framework of NH2-MIL-101 as an improved fluorescent and colorimetric sensor for nitrite detection based on diazotization reaction | |
| Bulgariu et al. | Direct determination of nitrate in small volumes of natural surface waters using a simple spectrophotometric method | |
| CN110628040A (en) | Cd (II) MOF materials based on 5- (4- [1,2,4] triazol-1-phenyl) -1H-tetrazoles | |
| Hawke et al. | Flow-injection analysis applied to the kinetic determination of reactive (toxic) aluminium: comparison of chromophores | |
| Lin et al. | Quantum dot assisted precise and sensitive fluorescence-based formaldehyde detection in food samples | |
| Jia et al. | Eu3+-Functionalized MOFs for the simple and rapid 5-Hydroxymethylfurfural determination in food | |
| CN116925379A (en) | OPA-Tb-MOF material for detecting ammonia nitrogen in water body, and preparation method and application thereof | |
| Jiang et al. | Spectrophotometric determination of trace nitrite based on catalytic oxidation of thionine by potassium bromate | |
| CN113861962B (en) | Ratiometric fluorescent probe, preparation method thereof and application thereof in detecting hydrogen peroxide | |
| Fernández-de Córdova et al. | Solid-phase spectrophotometric determination of trace amounts of vanadium at sub-ng/ml level with 4-(2-pyridylazo) resorcinol | |
| Yemiş et al. | Nitrite in nature: Determination with polymeric materials | |
| CN114088668B (en) | Preparation method and application of ratio type fluorescent paper-based sensor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |