Thanks Kemist and Infinite I, yes my friend feels like an idiot,  but I guess we all screw up.  The previous efforts, done corretly, were very effective.  My friend is a little nervous about the acetone wash, since there is probably SOME basification going on with the additon of the water after thefact, but one supposes there is a trade off either way, as Kemist pointed out, the limonene having coating the powders.  Perhaps my friend will acetone wash 1/2, and just press and dry the other half, and see how they both go.