- Purification of Acetylacetone
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Small amounts of acetic acid were removed by shaking with small portions of 2M NaOH until the aqueous phase remained faintly alkaline. The sample, after washing with water, was dried with anhydrous Na2SO4, and did through a modified Vigreux column . An additional purification step is fractional crystn from the liquid. Alternatively, there is less loss of acetylacetone if it is dissolved in four volumes of benzene and the soln is shaken three times with an equal volume of distd water (to extract acetic acid): the benzene is then removed by distn. at 43-53 °C and 20-30mm through a helices-packed column. It is then refluxed over P2O5 (10g/L) and fractionally distd under reduced pressure. The distillate (sp conductivity 4 ×10-8 ohm-1crn-1) was suitable for polarography. To recover used Acetylacetone (CAS NO.), metal ions were stripped (1:10) from the soln at pH 1 (using 100mL 0.1M H2SO4/L of acetylacetone). The acetylacetone was washed with (1:10) ammonia soln (100mL/L) and with distd water (100mL/L, twice), then treated as above. It complexes with Al, Be, Ca, Cd, Ce, Cu, Fe2+, Fe3+, Mn, Mg, Ni, Pb and Zn.
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