A process for the preparation of acrolein by the vapor phase catalytic oxidation of propylene which comprises contacting propylene and oxygen with a catalyst composition comprising a catalyst system of the formula:Mo.sub.a Bi.sub.b Fe.sub.c Ni.sub.d Tl.sub.e P.sub.f X.sub.g Y.sub.h O.sub.iWherein X is one or more of Mg, Mn and Co, Y is one or more of Cu, Ca, Sr, Zn, Cd, Sn and Pb and a, b, c, d, e, f, g, h and i represent respectively the number of atoms and, when a is 12, b is 0.1 to 5, c is 0.1 to 12, d is 0.1 to 12, e is 1 or less but not 0, f is 0 to 5, g is 0 to 12, h is 0.1 to 12 and i is a number determined by the valence requirements of the other atoms present and from 36.5 to 95.8, provided that b plus c is from 0.2 to 12.5 and d plus g plus h is from 0.2 to 27. The process can provide acrolein in a high selectivity and an excellent single pass yield even at a large space velocity of the propylene feed.