The problems for the mass spectrometry of organic substances with M>1000 are discussed and several examples of mass spectra of high molecular weight are shown. Using a second order double focusing mass spectrometer (rm=50cm) and an FD ion source with silicon emitters, mass spectrum of polystyrene up to M=11000 was obtained. The FD mass spectrum of a polymer sample indicates the distribution of the degree of polymerization. These mass lines can be used as standards of mass calibration for heavy mass region. Quasi molecular ions (M+H)+ appear normally in the FD mass spectra of peptides. A new method for the determination of amino acid sequence of a peptide is described. A new type of mass spectrometer using E×B crossed field is useful for the mass analysis of very heavy molecule.