C. Schramm et B. Rinderer, Determination of cotton-bound glyoxal via an internal Cannizzaro reaction by means of high-performance liquid chromatography, ANALYT CHEM, 72(23), 2000, pp. 5829-5833
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.