The invention provides a process for the separation of MEG and 1,2-BDO from a first mixture comprising MEG and 1,2-BDO in a weight ratio of at least 10:1 (MEG:1,2-BDO), said process comprising the steps of; (i) providing the first mixture as a feed to a distillation column at a point in the range of from 20 to 80% of the column height; (ii) operating the distillation at a temperature in the range of from 120 to 190° C. and at a pressure in the range of from 5 kPa to atmospheric pressure; (iii) removing an MEG stream from the distillation column at a point below the point at which the first mixture is fed; (iv) removing an overheads stream comprising an azeotrope of MEG and 1,2-BDO.