Complete solubilisation of barley or malt 13-glucan was obtained by extraction with dilute acid. Investigation of the extraction procedure by high performance size exclusion chromatography indicates that originally water insoluble high molecular weight 13-glucan is solubilized by degradation to smaller fragments. The fluorescence emitted by the specific complex formed between Calcofluor and D-glucan in solution was used to measure the total [3-glucan content of barley and malt samples. Examination of the residues after the extraction with dilute acid by degradation with (1--,3)(1--,4)-~-I~-glucanase and by fluorescence microscopy of Calcofluor stained residues confirmed the complete extraction of the [~-glucan. Comparison between the Calcofluor-FIA method and the enzymatic method of MCCLEARY and GLENNIE-HOLMES (20) revealed a high correlation between the values obtained by the two methods. 39 barleys and 57 malts were analysed for ~-glucan content with the two methods and linear correlation coefficients of r = 0.977 and r = 0.986, respectively, were found. The system enables a large number of barley or malt 13-glucan determinations to be performed within a short period of time with a minimum of manpower. The method is suitable for standard routine analysis in quality control laboratories.