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The microfibril angle of fiber walls is an ultra-microscopic feature affecting the performance of wood products. It is therefore essential to get more definitive information to improve selection and utilization. X-ray diffraction is a rapid method for measuring micro fibril angles. In this paper, the variability of microfibril angle in plantation-grown Masson pine was investigated by peak-fitting method. This method was compared with the traditional hand-drawn method, 40% peak height method and half peak height method. X-ray diffraction measurements indicated that the microfibril angle changed as a function of the position in the tree.The mean micro fibril angle decreased more gradually as the distance increased from the pith and reached the same level in mature wood. The microfibril angle also seemed to decrease clearly from the base upward. Differences of angle-intensity curves between heartwood and sapwood were also examined.