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In this study, sulphated zirconia was directly synthesised and compared to the conventional wet method of preparation. The surface areas and pore sizes were 169
m
2/g, 0.61
μm (directly synthesized) and 65
m
2/g, 0.24
μm (conventional method), respectively. Directly synthesized sulphated zirconia was amorphous, whereas conventionally prepared sulphated zirconia is polycrystalline. Their IR spectra were broadly similar, although the area of the 1250 to 950
cm
−1 band was larger for directly synthesised sulphated zirconia. Not only were conversions greater for directly synthesised sulphated zirconia (63% vs. 42% after 4
h), but it exhibited significantly greater yield for fatty acid methyl esters. The percentage yield (after 1
h) of methyl esters was 43% for the directly synthesised catalyst and 15% for the conventionally synthesised.