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电化学质谱仪

Beyond bare potentiostatic data: get the broader picture of electrochemistry with the Spectro inlets ECMS system. A unique instrument for high-sensitivity time-resolved detection of volatile electrochemistry products directly from a liquid electrolyte. This instrument is optimized for half-cell investigations, i.e. it allows the user to decouple the evolution of volatile products and consumption of reactants at the working and counter electrodes during electrochemical reactions. Due to its extraordinary sensitivity, the system can measure all the individual volatile molecules desorbing from an electrode surface during a single electrochemical turnover. Product formation can be measured from total Faradaic currents of 1 mA all the way down to 1 nA, corresponding to approximately 10 ppm of a monolayer desorbing from the electrode surface in 1s. These features enable time-resolved, fully quantitative measurements of transient phenomena during electrochemistry, providing fundamental insight in the electrochemical reaction mechanisms.

The compact, tabletop instrument fits comfortably on standard laboratory tables. Upon installation, it operates straight out of the package with the embedded, fully functional 3-electrode EC cell and BioLogic SP-200 potentiostat.

In the following, the key features of the Spectro Inlets EC-MS system are explained, and some experimental results exploiting these features are shown. In the References section, the reader can find a selected list of scientific publications based on research conducted on a Spectro Inlets EC-MS system

 

FEATURES

 Membrane chip: Tailored analyte sampling and molecular flow for true quantitative analysis. • Standardized sample holder: Piranha-cleanable stagnant thin-layer EC cell for standard 5 mm cylindrical electrodes, common in RDE.

• Fast time-response: Sub-second time resolution.

• High sensitivity: Measure the desorption of 10 ppm of a monolayer in 1 sec.

• High dynamic range: Measure from 1 mA down to 1 nA of continuous product formation.

• Quantitative analysis: 100% volatile species collection efficiency and tailored molecule flux to the detector.

• Dosing of reactant gases: Fully defined mass transport to and from the electrode.

• Fast sample and chip exchange: Integrated vacuum system for effortless chip exchange without interrupting instrument operation or venting.

• Streamlined software solution: Complete system control and synchronized EC-MS data acquisition and plotting. Full documentation is available for customization by the user.

 

 

Figure 1. Working principle of the membrane chip. The chip is placed inside the interface block, on top of which the EC-cell is coupled. In the cartoon, the equilibration of volatile analytes between electrolyte and sampling volume is shown..3

 

 

 

Figure 2: Schematics of the stagnant thing layer flow cell. a) Electrode assembly, with a disk contact core assembly from Pine Instruments used to retain the working electrode in the EC cell b) mounting of cell onto membrane chip, c) cross sectional view of the assembled flow cell. d) The electrochemical cell mounted on the interface block and equipped with two glass compartments for reference and counter electrode, respectively.4

 

 

Figure 3. Photographs of the EC cell equipped with a B 3420+ Ag/AgCl electrode, a coiled Pt wire as counter electrode, and a gas-tight syringe to inject electrolyte in the cell.

 

Figure 4. H2 evolution and CO stripping experiments using a 5 mm polycrystalline Pt electrode in 1M HClO4. Potential sweeps are carried out at 20 mV/s. a) Different signals from the mass spectrometer corresponding to H2 (m/z=2), He (m/z=4), CO (m/z=28) and CO2 (m/z=44) along with the potential and current density as a function of time. b) MS signal as a function of applied voltage and CVs corresponding to the coloured sweeps in a).4

 

 

Figure 5. a) Mass spectrum of air being sampled through the membrane chip before a droplet of water is placed onto the membrane. b) Mass-time analysis of air with N2, O2, H2O, Ar and CO2 measured on m/z = 28; 32; 18; 40 and 44, respectively. At t = 60 s the user exhales on the chip, causing a spike in the CO2 and H2O signals. At t = 120 s, a droplet of water is placed on the chip, after which the sampling volume equilibrates with water, with the He carrier gas making up the pressure to 1 bar, measured on m/z = 4.

 

 

Figure 6. Schematic representation of a CO gas pulse sent via the gas exchange system.

 

 

Figure 8. Screenshots from the user interface and a photograph of the software in action during a Pt cyclic voltammogram in acid electrolyte.

 

 

 

Figure 9. The effect of oxygen demonstrated by two consecutive constant-potential CO electroreduction experiments performed at -0.9 V vs RHE. Gaseous Ar (a) and O2 (b) are injected as 90 s pulse injections into the carrier gas stream of the membrane chip, while holding the potential at 0.0 V vs RHE. This demonstrates that only gaseous O2 can activate the transient production of CH4. 3

 

 

Figure 10. a) EC-MS plot demonstrating the electrochemical desorption of gaseous H2 both at cathodic potential during HER and at potential anodic of the reversible hydrogen potential. The phenomenon shows during potential cycling from -0.3 to 0.45V vs RHE at a scan rate of 50 mV/s. b) EC-MS measurements plotted as a function of potential, where the anodic potential limit is set to 0.45, 0.60 and 0.85 V vs RHE, plotted in blue, green and red, respectively. Arrows indicate the direction of the potential scan during MS data acquisition. c) MS measurement of the anodic H2 desorption feature at different scan rates, indicating a strong potential dependence. d) Isolation of the anodic desorption feature by resting the electrode at an intermediate potential of -0.05 V vs RHE for 60 s and 120 s, respectively, in between HER and anodic desorption. HER is performed at -0.25 V vs RHE and anodic desorption is performed by sweeping the potential to 0.45 V vs RHE with 50 mV/s. 3

 

TECHNICAL DATA

MASS RANGE, AMU 0-200

SENSITIVITY  10 ppm of a monolayer in 1s, or 1 mA of continuous product formation 

RESPONSE TIME Down to 0.1 s (dependent on substance volatility)

SOFTWARE LabView (open source)

INTERFACE USB

DETECTOR Faraday cup/Continuous Secondary Electron Multiplier

DIMENSIONS 450 mm x 790 mm x 337 mm

POWER 110/220/240 V AC, 50/60 Hz, 1.2 kVA

 

 

REFERENCES

1.    Sebok, B. et al. Impact of nanoparticle size and lattice oxygen on water oxidation on NiFeOxHy . Nat. Catal. (2018).

2.    Trimarco, D. B., Pedersen, T., Hansen, O., Chorkendorff, I. & Vesborg, P. C. K. Fast and sensitive method for detecting volatile species in liquids. Rev. Sci. Instrum. 86, (2015).

3.    Trimarco, D. B. Real-time detection of sub-monolayer desorption phenomena during electrochemical reactions: Instrument development and applications. PhD Thesis (Department of Physics, Technical University of Denmark, 2017).

4.    Trimarco, D. B. et al. Enabling real-time detection of electrochemical desorption phenomena with sub-monolayer sensitivity. Electrochim. Acta 268, 520–530 (2018).

5.    Trimarco, D. B., Vesborg, P. C. K., Pedersen, T., Hansen, O. & Chorkendorff, I. A   device for extracting volatile species from a liquid. (2016). doi:10.1016/j.cities.2014.02.005.RIZZO

6.    Winiwarter, A. et al. Towards an atomistic understanding of electrocatalytic partial hydrocarbon oxidation: propene on palladium. Energy Environ. Sci. (2019).