Determination of cotton-bound glyoxal via an internal Cannizzaro reaction by means of high-performance liquid chromatography

Glyoxal, a non-formaldehyde cross-linking agent, was applied in combination with aluminum sulfate hexadecahydrate to impart durable-press properties t o cellulosic materials. The cotton fabric was impregnated with a pad bath f ormulation containing 6% (w/w) glyoxal and 4.5% (w/w) aluminum sulfate hexa decahydrate, The curing process was conducted at 140 degreesC for 3 min, th us affecting a cross-linkage between the cellulose chains. For the first ti me, a chromatographic method is presented that enables both qualitative and quantitative analysis of the portion of glyoxal that has reacted with the cellulosic material. For this purpose, the glyoxal-treated fabric was treat ed with an NaOH solution (c = 4 mol L-1) at 100 degreesC for 20 min. As a r esult, Glyoxal was extracted from the cellulosic sample and converted into glycolate via an internal Cannizzaro reaction, Subsequently, the glycolate was analyzed chromatographically using the strong cation-exchange column Am inex HPX-87H as the stationary phase and sulfuric acid as the mobile phase. The detection limit was 1.87 mg L-1 (UV detection). The recovery was 85%, Dry crease wrinkle recovery measurements gave evidence that the cross-linka ge was removed completely. The application of the analytical technique deve loped in the present study demonstrated that the amount of glyoxal that had ;reacted with the cellulose was 15.7 +/- 0.72 mg/g of fabric, In addition, glycolate thus formed was well separated from non-formaldehyde durable-pres s finishing agents based on polycarboxylic acids such as 1,2,3,4-butanetetr acarboxylic acid or citric acid.