The solid monoxime of 2, 3-butanedione is a more convenient material than liquid dione for the homogenous generation of DMG. 2, 3-butanedione dioxime. Determinations of Ni in steels and in pure Ni(II) solutions have shown the optimum pH and order of adding reagents. Gravimetric and/or an EDTA titrimetric finish are possible for a method of reliability within ± 0.2 mg of Ni in 50–150 mg Ni. The solid has the same character and filterability as that from the 1960 dione method of Salesin and Gordon1.