It is disclosed that aqueous systems containing the sodium salt of nitrilotriacetate monohydrate (NTA) can be converted into a dry particulate form of NTA of comparatively high bulk density and suitable hygroscopic properties when using a spray drying technique by delivering to the spray dryer an NTA-water mixture which contains a greater amount of NTA than that present in a saturated aqueous solution of NTA. Upon spray drying such a particulate mixture with hot gases in a counter-current or co-current flow under proper conditions, water is removed from the particulate mixture producing a particulate solid NTA product.