The paper describes an investigation of the preparation and properties of amylose phenylosazone and phenylhydrazone. Under the conditions used, amylose phenylosazone was not formed quantitatively and considerable degradation of the amylose occurred. The phenylhydrazone, however, can readily be prepared in quantitative yield and the polymer remains undergraded. Solutions of amylose phenylhydrazone in dimethylsulfoxide may be used to determine the number average molecular weight of amylose samples.