Sedimentation has been a standard methodology for particle size analysis since the early 1900s. In recent years laser diffraction is beginning to replace sedimentation as the prefered technique in some industries, such as marine sediment analysis. However, for the particle size analysis of soils, which have a diverse range of both particle size and shape, laser diffraction still requires evaluation of its reliability. In this study, the sedimentation based sieve plummet balance method and the laser diffraction method were used to measure the particle size distribution of 22 soil samples representing four contrasting Australian Soil Orders. Initially, a precise wet riffling methodology was developed capable of obtaining representative samples within the recommended obscuration range for laser diffraction. It was found that repeatable results were obtained even if measurements were made at the extreme ends of the manufacturer's recommended obscuration range. Results from statistical analysis suggested that the use of sample pretreatment to remove soil organic carbon (and possible traces of calcium-carbonate content) made minor differences to the laser diffraction particle size distributions compared to no pretreatment. These differences were found to be marginally statistically significant in the Podosol topsoil and Vertosol subsoil. There are well known reasons why sedimentation methods may be considered to 'overestimate' plate-like clay particles, while laser diffraction will 'underestimate' the proportion of clay particles. In this study we used Lin's concordance correlation coefficient to determine the equivalence of laser diffraction and sieve plummet balance results. The results suggested that the laser diffraction equivalent thresholds corresponding to the sieve plummet balance cumulative particle sizes of < 2 μm, < 20 μm, and < 200 μm, were < 9 μm, < 26 μm, < 275 μm respectively. The many advantages of laser diffraction for soil particle size analysis, and the empirical results of this study, suggest that deployment of laser diffraction as a standard test procedure can provide reliable results, provided consistent sample preparation is used.