研究目的
To develop a simple and rapid method for in situ detection of sulfite (SO3^2-) under high pressure using surface enhanced Raman spectroscopy (SERS) with a silver nanoparticles film fabricated on a diamond anvil.
研究成果
The method successfully enables in situ detection of sulfite at high pressures with a low detection limit of 5 μmol/L and good linearity in concentration response. Pressure causes a decrease in SERS intensity and a blue-shift in Raman peaks. This approach is feasible for monitoring sulfite in high-pressure environments and can be extended to hydrothermal systems in future research.
研究不足
The Ag NPs film may not be uniform, potentially affecting quantitative accuracy. The method is currently limited to room temperature and pressures up to 330 MPa; it has not been tested under high-temperature hydrothermal conditions. The detection limit and sensitivity could be improved with more stable and homogeneous substrates.
1：Experimental Design and Method Selection:
The study uses a diamond anvil cell (DAC) for high-pressure experiments, with SERS active substrates fabricated by depositing silver nanoparticles (Ag NPs) on the diamond anvil surface. The method is designed for in situ detection of sulfite concentrations under high pressure.
2：Sample Selection and Data Sources:
Sodium sulfite (Na2SO3) solutions with concentrations ranging from 5 to 40 μmol/L were prepared freshly to prevent oxidation. Ultrapure water was used as the solvent.
3：List of Experimental Equipment and Materials:
Diamond anvil cell (DAC), T 301 stainless steel gasket, silver nitrate (AgNO3), hydroxylamine hydrochloride (NH2OH·HCl), sodium hydroxide (NaOH), anhydrous sodium sulfite (Na2SO3), quartz piece for pressure measurement, FEI SCIOS duel-beam system FIB SEM for SEM imaging, Renishaw Invia confocal micro-Raman spectroscopy system with 514.5 nm laser excitation.
4：5 nm laser excitation.
Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: Ag NPs were synthesized and used to fabricate a film on the diamond anvil by dropping the suspension into the DAC gasket hole, evaporating the solvent, and then loading Na2SO3 solution. Pressures were applied and measured using the quartz pressure gauge. SERS spectra were collected at various pressures with specified laser settings.
5：Data Analysis Methods:
SERS intensities and Raman shifts were analyzed for linearity with concentration and pressure effects. Pressure was calculated from the quartz Raman peak shift using a provided equation.
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