Brain volume is altered by pathological processes such as swelling or atrophy yet until now this is a parameter which could only be determined at post mortem. This paper describes a non-invasive technique using MRI which permits the in vivo determination of brain volume (BV), intracranial cavity volume (ICV), ventricular, cortical sulcal and total intracranial CSF volumes. The technique was applied to 40 normal volunteers (20 males, 20 females) to investigate the variation of these parameters with age and sex after normalisation with respect to ICV. There was found to be a significant decrease in normalised brain volume between the ages of 20 and 60 years in males by 1.6% per decade. In females the decrease was less (0.5%) but was not statistically significant. This technique will make it possible, for the first time, to investigate prospectively the correlation between mental function and brain volume in illness and ageing.