We report the implementation of two new methods of accurate comparison of lattice parameters against a silicon standard using a high resolution X-ray diffractometer. The double axis method uses a specimen rotation stage which set the limit of reproducibility (at 3 sigma) to 3 parts in 105. An application of the technique is illustrated in measurements of the zinc concentration in Cd1-xZnx Te to an accuracy of 0.1%. The triple axis technique uses beam conditioner and analyser crystals to define the incident and diffracted wave vectors. In measurement of the lattice parameters of InAs, we found a precision of 1 part in 105 and traceable accuracy of a several parts in 105.