Oxidative
pyrolysis (OP) was applied for the detennination of boron in graphite
powders by inductively coupled plasma optical emission spectrometry
(lCPOES). Aknown amount of graphite powder (~0.2 g) was mixed with
carbon powder (1:0.75) along with 5 mg of Na2C03 (250 µL of 20 mg mL-1
solution) and an appropriate amount of polyvinyl alcohol (binder).
After drying under the Rlamp, the sample mixture was pressed into a
pellet which was placed into a boat and introduced into the in-house
pyrolysis chamber. The chamber was then heated using a Bunsen burner in
the presence of an oxygen stream. The pyrolysis process commenced when
the temperature reached ~400 ºC and was completed in 5 minutes when ~0.2
g of graphite powder was used. After allowing the chamber to cool down
to room temperature, a mixture of 0.2 mL of 1% mannitol, 0.5 mL ofHN03 and
0.1 mL HFwas added to the boat for treating the sample residue. Then
the mixture was made up to the required volume with Milli-Q® water for
subsequent analysis by ICP-OES. The detection limit of boron was 0.05
/µg/g and the repeatability, expressed as the relative standard
deviation (RSD), was about 4%. The recoveries for the spike tests were
obtained ranging from 98-102%. Arecently reported fusion method was
adopted for validation of the developed method. The developed method was
finally applied to the analysis of graphite powder samples for the
detennination of boron.