BARC/PUB/2014/1385

 
 

Development of Oxidative Pyrolysis Method for the Rapid Determination of Boron in Graphite Powders by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES)

 
     
 
Author(s)

Krishna, M. V. B.; Chandrasekaran, K.; Thangavel, S.; Karunasagar, D.
(CCCM)

Source

Atomic Spectroscopy, 2014. Vol. 35 (3): pp. 109-117

ABSTRACT

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.

 
 
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