Titration Application Note T-136 Determination of epoxide equivalents in two-component adhesive according to DIN EN ISO 3001 The analysis of the epoxide equivalent is based on the reaction of hydrogen bromide with the epoxide groups of the sample. Hydrogen bromide is produced by the reaction of tetraethylammonium bromide (TEABr) with standardized perchloric acid. Method description Sample Parameters Two-component adhesive Titration Mode DET U Stirring rate 8 Sample preparation Pause 30 s The sample should only be taken from the epoxidecontaining component. Signal drift 30 mV/min Min. waiting time 5s Max. waiting time 32 s Meas. point density 4 EP criterion 10 EP recognition Greatest Configuration 907 Titrando 2.907.0010 800 Dosino 2.800.0010 804 Ti Stand with stand 2.804.0040 802 Stirrer 2.802.0020 20 mL Dosing unit 6.3032.220 Solvotrode easyClean 6.0229.010 Solutions Titrant c(HClO4) = 0.1 mol/L in anhydrous glacial acetic acid If possible, this solution should be bought from a supplier. TEABr solution β(TEABr) = 250 g/L 25 g tetraethylammonium bromide are weighed into a 100 mL volumetric flask, dissolved in glacial acetic acid and the flask is filled up to the mark with glacial acetic acid. This solution is not very stable and should be prepared daily. Chloroform p.a. Glacial acetic acid p.a. Analysis Titration Application Note T-136 Version 1 The sample, containing 0.6 to 0.9 mmol epoxy groups, is weighed into a titration beaker. The sample is then dissolved in 10 mL chloroform. Afterwards, 10 mL β(TEABr) = 250 g/L and 20 mL glacial acetic acid are added and the solution is titrated with c(HClO4) = 0.1 mol/L until after the equivalence point. Results Mean result for n = 3 Epoxide equivalent / (g/mol) 186.35 s(rel) / % 0.98
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