Academia and research institutions · TD-NMR

Water in porous materials

The relaxation of water inside a porous solid reflects pore size and how the water is bound. Useful for cement, rock, wood, catalyst supports and other porous media.

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What it tells you

Pore size seen through water

Water molecules in a small pore are always close to the wall, and the wall makes the NMR signal fade quickly. In a large pore most of the water is far from the wall, and the signal lasts longer. A porous sample filled with water therefore shows a range of decay times, which reflect its range of pore sizes.

A porous solid with many small and a few large pores filled with water
Water in small and large pores. Schematic illustration.
Typical samples

Where it is used

  • Cement, concrete and plaster, including their hydration
  • Rocks and rock cores
  • Wood, paper and cellulose materials
  • Catalyst supports, ceramics and powders
  • Soils and other natural porous media

Typical tasks are comparing pore structures between samples, following how the structure changes during hardening or ageing, and studying how fluids sit in a rock.

How it works

From a decay to a distribution

The sample is saturated with water and the decay of the signal is recorded with a train of echoes. An inverse Laplace transform turns the decay into a distribution of relaxation times, where each peak is a group of pores of similar size and its height shows how much water sits in it.

A decay made of several exponentials turned by an inverse Laplace transform into a distribution of relaxation times with separate peaks
The one-dimensional inverse Laplace transform. Schematic illustration.
Distribution of relaxation times with two peaks, one for small pores and one for large pores
A distribution of relaxation times in a porous material. Schematic illustration, not measured data.
Two dimensions

Pore size and surface binding together

A distribution of T2 times alone cannot always tell water in a small pore from water bound to a surface, because both relax quickly. Measuring T1 and T2 together and inverting in two dimensions gives a map that pulls them apart. Along the diagonal, where T1 equals T2, the position shows how small or large the pores are. Above the diagonal, the distance shows how strongly the water is held at the surface.

Map of T1 against T2 with peaks for water in small pores, water in large pores and water bound to surfaces
A two-dimensional T1 and T2 map of a porous material. Schematic illustration, not measured data.

The same approach separates water from oil in a rock or a catalyst, and maps can also combine diffusion with relaxation.

Why time-domain NMR

What it adds

  • Non-destructive and quick, so many samples can be compared
  • Water is the probe, so no mercury, high pressure or special gases are needed
  • The measurement works on wet samples as they are
  • The same sample can be measured again as it changes
Good to know

Points that matter in practice

  • To turn a relaxation time into a pore size, the instrument has to be calibrated against a reference technique such as gas adsorption or mercury intrusion
  • Paramagnetic minerals, for example iron compounds in rocks, shorten the relaxation and can distort the result
  • Pores that are well connected exchange water, which can merge peaks
  • The inversion is a mathematically delicate step. It uses smoothing, so the distributions are smooth by construction and the exact width of a peak should not be over-interpreted
  • Good signal quality matters. Two-dimensional maps need longer measurements and software that includes the inversion, which should be checked for your instrument
  • The sample must be fully saturated and kept at a defined temperature
How MSY Consulting helps

From your question to a routine method

Describe your materials and your question. MSY Consulting runs feasibility measurements, helps you plan the calibration against your reference technique, and supports you with 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