Industry: chemical · EPR

Catalysts and metal species

Oxidation state and coordination of Cu, Mn, V, Fe, Co and other metals in catalysts, complexes and electrochemical or photochemical cells.

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What it tells you

Which state the metal is in

The activity of a catalyst often depends on the oxidation state of its metal, and on what surrounds it. Many metal ions have unpaired electrons, so they give an EPR spectrum, and the spectrum depends on the ion, its oxidation state and its environment. States without unpaired electrons give no signal, so a change of oxidation state can often be seen as the appearance or the disappearance of a signal.

The copper(II) signal in a catalyst over time: it falls when the reactant is added and recovers after oxygen is added
Following copper during a reaction. Schematic illustration, not measured data.
Typical samples

Where it is used

  • Heterogeneous and homogeneous catalysts, before, during and after use
  • Metal complexes and coordination compounds
  • Electrochemical and photochemical cells, with the metal followed in the cell
  • Materials with trace metals that influence a reaction

Typical tasks are checking the oxidation state of a catalyst, following how it changes during a reaction, studying the environment around the ion, and detecting traces of metals.

How it works

Seeing only the states that have unpaired electrons

A spectrum is recorded and compared with a reference of known spin number for quantity, and with simulation or known patterns for the type of ion. Followed in time, the signal shows how the metal responds when a reactant, light or a potential is applied.

Copper(II) in a catalyst gives a strong EPR signal, and after reduction to copper(I) the signal disappears
Following a change of oxidation state by EPR. Schematic illustration.
Why EPR

What it adds

  • Selective for paramagnetic centres, even at low concentration in a complex sample
  • Information on the oxidation state and the local environment, not only the amount
  • Non-destructive, with little sample preparation
  • Can follow a catalyst while a reaction takes place, with a suitable cell or flow set-up
Good to know

Points that matter in practice

  • Absence of a signal does not mean absence of the metal. Some oxidation states, such as copper(I), give none
  • Overlapping signals of several species can be separated with spectral simulation and fitting
  • Spectra of powders and frozen solutions are broad and complex, and the analysis takes some experience
  • Some ions give very broad lines and are best measured at low temperature, which needs a suitable accessory
  • Following a reaction in the instrument needs a suitable cell, flow or irradiation set-up
How MSY Consulting helps

From your catalyst to a routine method

Describe your catalyst and your question. MSY Consulting runs feasibility measurements, shows what the technique can and cannot tell you in your case, and supports the analysis until the method is part of your routine.

Contact

Let's talk about your application

Send an email describing your instrument and your application, and you will get a reply.

contact@msyconsulting.eu

MSY CONSULTING SAS · Wissembourg, France · LinkedIn