H. Nakashima et al., ANALYSIS OF TRIBUTYL-PHOSPHATE IN FLAME-R ETARDANT TEXTILES BY CAPILLARY GAS-CHROMATOGRAPHY, Eisei Kagaku, 40(5), 1994, pp. 461-466
Tributyl phosphate (TBP) in flame retardant textiles was analyzed by c
apillary gas chromatography using a flame photometric detector (FPD).
A successfully cleaned up preparation using the difference in liquid-l
iqiud partition behaviour and a florisil cartrige column has been deve
loped for the determination. The detection limit by this method was 10
pg. For the determination of TBP in textiles, TBP was extracted from
samples with methanol under reflux at 70 degrees C. For the removal of
polar materials, distilled water was added to the extract, and TBP wa
s reextracted into dichrolomethane from the methanolic phase. After ev
aporating the extract, the residue was dissolved in n-hexane, and appl
ied to the florisil cartrige column. After washing nonpolar materials
with n-hexane, TBP was eluted with 12-hexane containing 10% methanol.
After evaporating the elute, the residue was dissolved in n-hexane, an
d applied to the GC. The recoveries of TBP added to textiles at the am
ounts of 2, 20, 200, 2000 mu g were 93-96% on the average. TBP was det
ected in 3 out of 8 brands in textiles finished as flame retardant by
this proporsal method.