Academia and research institutions · TD-NMR

Molecular mobility in soft matter

Relaxation times show how freely molecules move in gels, hydrogels, polymer networks and biological samples. Follow gelation, swelling or ageing, and compare formulations on the same scale.

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What it tells you

From liquid to network

In a liquid, molecules move freely and the NMR signal lasts. As a network forms, movement is restricted and the signal fades faster. A relaxation time is therefore a measure of how mobile the molecules are, and it can be followed while the sample changes.

A liquid forming a gel, with the relaxation time falling as the polymer network forms
Following gelation by relaxation time. Schematic illustration, not measured data.
Typical samples

Where it is used

  • Gels and hydrogels, including those for biomedical use
  • Polymer networks and elastomers
  • Biopolymer powders and films that take up water
  • Biological samples and food-like soft materials

Typical tasks are following the gelling, swelling or ageing of one sample over time, comparing formulations, and relating mobility to mechanical or release properties.

How it works

Rigid and mobile parts, and several kinds of water

The signal right after the pulse separates a rigid part, which fades almost at once, from a mobile part, which lasts. The ratio of the two is a direct measure of how rigid the sample is. Water in the sample often shows several populations with different mobility, from water held tightly by the polymer to water that moves almost freely.

Stacked bars showing the share of tightly bound, loosely bound and free water as the water content of a biopolymer sample increases
States of water in a hydrating biopolymer sample. Schematic illustration, not measured data.
Distributions and maps

One dimension, then two

When the signal contains several components, an inverse Laplace transform turns the decay into a distribution of relaxation times, with one peak for each population of water or polymer. This is the one-dimensional version, and it already shows how many states are present and how much of the sample is in each.

Measuring T1 and T2 together and inverting in two dimensions gives a map. The position of a peak shows how fast the molecules move, and its distance from the diagonal, where T1 equals T2, shows how strongly their motion is held back. Water that is tightly bound to a polymer sits far from the diagonal, and free water close to it.

Map of T1 against T2 with peaks for tightly bound, loosely bound and free water in a hydrated polymer
A two-dimensional map of the water in a hydrated polymer. Schematic illustration, not measured data.
Why time-domain NMR

What it adds

  • Non-destructive, so the same sample can be followed from start to end
  • No labels, dyes or special sample preparation
  • Works on opaque, coloured and thick samples
  • Different formulations are compared on the same scale
Good to know

Points that matter in practice

  • Relaxation times depend on temperature, concentration and pH, so compare samples under the same conditions
  • Decays with several components need careful analysis. The number of water populations is partly a matter of the model used
  • The inverse Laplace transform needs good signal quality and uses smoothing, so peaks should be judged together with the settings that produced them. Maps in two dimensions need longer measurements and suitable software
  • Confirm the interpretation with a second technique, such as rheology or calorimetry, when the result will be published
How MSY Consulting helps

From your question to a routine method

Describe your materials and your question. MSY Consulting runs feasibility measurements, shows what the technique can and cannot tell you in your case, and helps you set up the analysis and the sample handling.

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