On April 9, 1860 the earliest known recording of a human voice was accomplished by Edouard-Leon Scott de Martinville, pre-dating Edison by 18 years. Known as a phonautograph and consisting of lines traced on smoke-blackened paper or glass, its intention was the study of acoustics.
Firstsounds.org is a very cool initiative that preserves phonautograms and makes them freely available to the world under a Creative Commons License. This is Scott de Martinville singing Au Clair de Lune in French.
http://www.firstsounds.org/sounds/scott.php
