In the present paper, near infrared (NIR) spectroscopy and X-ray diffractometry were used to rapidly predict the microfibril angle (MFA). MFA is one of the most important factors affecting wood properties. Wood resource utilization and tree improvement programs require cost-effective methods for the rapid analysis of thousands of samples. In the experiment, the average MFA of each sample were rapidly measured by X-ray scanning diffractometry. Then, the PLS model was built between NIR data and MFA by the X-ray measured. As a result, a very strong linear relationship has been found between NIR spectra fitted and X-ray measured, and the coefficients (r2) of calibration and prediction models were 0.867 and 0.816 respectively.