Industry: petrochemical · TD-NMR

Waxes, greases and lubricants

Solid content versus temperature, wax crystallisation and the behaviour of additive packages in oils and greases.

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What it tells you

How much is solid, at which temperature

Waxes in oils crystallise when the temperature falls. The crystals make the oil cloudy, thicken it and can block filters and pipes. Time-domain NMR separates the solid wax from the liquid oil by how quickly their signals fade, so the solid content is read as a function of temperature, and the temperature at which wax appears can be located.

Solid wax against temperature for an oil rich in wax and an oil with little wax; the wax appears as the oil is cooled
Solid wax against temperature. Schematic illustration, not measured data.
Typical samples

Where it is used

  • Petroleum waxes, and the oil content of waxes
  • Paraffinic crude oils and fuels
  • Lubricating oils and base oils
  • Greases and additive packages

Typical tasks are measuring the oil in a wax or the wax in an oil, locating the temperature at which wax appears, comparing oils, and studying how additives change the crystallisation.

How it works

A temperature series, or time at a fixed temperature

The sample is held at a series of temperatures in a temperature-controlled block, and the solid content is read at each. For crystallisation, the sample is cooled quickly to a chosen temperature and the solid content is followed over time. A crystallisation modifier shows up as a change in how early and how far the wax crystallises.

Solid wax against time at a fixed temperature: wax crystallises early without an additive, and later and to a lower level with a crystallisation modifier
Wax crystallisation with and without an additive. Schematic illustration, not measured data.
Methods and standards

Wet references

The oil content of petroleum waxes is traditionally determined by a wet method such as ASTM D721. NMR gives a fast alternative after a calibration against it.

Why time-domain NMR

What it adds

  • Quick, non-destructive and free of solvents
  • Dark and opaque samples are no problem
  • Shows how the solid content changes with temperature and with time
  • Compares additives on the same scale
Good to know

Points that matter in practice

  • The sample history matters. Melt the sample, and cool it in a defined way, before comparing
  • The temperature at which wax first appears depends on how sensitive the measurement is, so compare samples measured in the same way
  • Additives change the crystal form and the structure. The solid content alone does not show everything, so combine it with other tests when the question is flow behaviour
  • Calibrate with samples whose wax or oil content you know
How MSY Consulting helps

From your samples to a routine method

Send or bring representative samples. MSY Consulting runs feasibility measurements, plans the temperature programme and the calibration with you, and trains your team 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