An investigation of a new method for measuring fibre material properties from ultrasonic attenuation in a dilute suspension of synthetic fibres of uniform geometry is presented. The method is based on inversely solving an ultrasound scattering and absorption model of suspended fibres in water for the material properties of the fibres. Experimental results were obtained from three suspensions of nylon 66 fibres each with different fibre diameters. A forward solution to the model with reference material values is compared to experimental data to verify the model's behaviour. Estimates of the shear and Young's modulus, the compressional wave velocity, Poisson's ratio and loss tangent from nylon 66 fibres are compared to data available from other sources. Experimental data confirms that the model successfully predicts that the resonance features in the frequency response of the attenuation are a function of diameter. Consistent estimated values for the compressional wave velocity and the Poisson's ratio were found to be difficult to obtain but in combination gave values of shear modulus within previously reported values and with low sensitivity to noise. Young's modulus was underestimated by 54% but was consistent and had low sensitivity to noise. The underestimation is believed to be caused by the assumption of isotropic material used in the model. Additional tests on isotropic fibre would confirm this. Further analysis of the model sensitivity and the reasons for the resonance features are required.