研究目的
To develop a fluorescent Eu(III) metal-organic framework for highly selective and sensitive sensing of picric acid, addressing the need for detection methods in homeland security and environmental protection.
研究成果
EuL is a highly selective and sensitive luminescent sensor for picric acid with a high Ksv value, good anti-interference ability, and repeatability. The quenching mechanism is attributed to synergistic effects of competitive absorption, fluorescence resonance energy transfer, and electrostatic interactions, making it a promising material for PA detection.
研究不足
The framework collapses in water after 24 hours, limiting its use in aqueous environments. The BET surface area of desolvated EuL is small, possibly due to partial framework collapse. The mechanism involves multiple factors, and further optimization may be needed for practical applications.
1:Experimental Design and Method Selection:
The study involved synthesizing a Eu(III) MOF using solvothermal methods, characterizing its structure, and evaluating its luminescence properties for sensing nitro explosives, particularly picric acid. Theoretical models included Stern-Volmer analysis for quenching constants.
2:Sample Selection and Data Sources:
The ligand 9H-carbazole-2,7-dicarboxylic acid was synthesized based on literature, and other chemicals were commercially obtained. Samples included EuL crystals and suspensions in DMF for testing.
3:List of Experimental Equipment and Materials:
Equipment included Perkin-Elmer 240C analyzer for elemental analysis, PerkinElmer FTIR spectrometer for IR spectra, NETZSCH STA2500 for TGA, Bruker D8 advanced diffractometer for PXRD, SHIMADZU UV-3600 spectrophotometer for UV-Vis, RF-5301PC spectrofluorophotometer for photoluminescence, Edinburgh FLS920P spectrophotometer for fluorescence lifetimes, and ASAP 2020M for gas sorption. Materials included Eu(NO3)3?6H2O, DMF, water, glacial acetic acid, and various nitro explosives.
4:Experimental Procedures and Operational Workflow:
Synthesis involved heating a mixture in a Teflon-lined autoclave at 120°C for 2 days. Characterization included elemental analysis, IR, TGA, PXRD, UV-Vis, NMR, photoluminescence, and lifetime measurements. Sensing experiments involved adding nitro explosives to EuL-DMF suspensions and measuring fluorescence quenching.
5:Data Analysis Methods:
Data were analyzed using Stern-Volmer equations for quenching constants, with linear regression for sensitivity. Detection limits were calculated based on titration data.
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Perkin-Elmer 240C analyzer
240C
Perkin-Elmer
Elemental analysis for C, H, and N
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Bruker D8 advanced diffractometer
D8 advanced
Bruker
Collecting powder X-ray diffraction patterns
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SHIMADZU UV-3600 spectrophotometer
UV-3600
SHIMADZU
Performing UV-Vis absorption spectra
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Edinburgh FLS920P spectrophotometer
FLS920P
Edinburgh
Measuring fluorescence lifetimes
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Bruker Smart Apex CCD area detector diffractometer
Smart Apex CCD
Bruker
Collecting X-ray diffraction data of single crystals
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PerkinElmer FTIR spectrometer
PerkinElmer
Collecting FTIR spectra using KBr pellets
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NETZSCH STA2500 simultaneous DTA-TG apparatus
STA2500
NETZSCH
Thermogravimetric analyses under N2 atmosphere
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RF-5301PC spectrofluorophotometer
RF-5301PC
Carrying out photoluminescence spectra at room temperature
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ASAP 2020M adsorption equipment
ASAP 2020M
Testing gas sorption isotherms
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