The use of fiber from Harakeke (or New Zealand Flax plant) for the reinforcement of composites should be explored since Harakeke has similar properties to Sisal fiber. To maximize the cellulose content in the fiber, Harakeke fibers were prepared by thermal, combinative alkaline-thermal, and a novel combinative thermal-enzymatic-thermal treatments and characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and wide-angle X-ray spectroscopy. The characterization method provided an efficient and systematic method to evaluate the removal of amorphous components such as lignin and hemicelluloses. In particular, a sequential thermal-enzymatic-thermal fiber treatment produced fine discontinuous whiskers that could be useful for short fiber composites, whereas a combinative thermal-alkaline treatment resulted in thorough extraction of lignin and hemicelluloses. (C) 2009 Wiley Periodicals, Inc. J Appl Polym Sci 112: 2710-2715, 2009