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Abstract
Analytical atomic absorption/emission spectrometric methods have been developed for determination of 22 metallics at low concentration levels in high purity graphite material required in nuclear fuel industry. Of these, 21 metallics viz., Al,B, Be, Ca, Cd, Cr, Co, Cu, Fe, Li, Mn, Mo, Mg, Ni, Pb, Sn, Si, Ti, V, W and Zn are determined at trace concentration levels by D.C. arc Atomic Emission Spectrometric method using carrier excitation technique with a 6% carrier mixture of AgCl and NaF in a 5:1 proportion. Using the standardized procedure B, Be and Cd can be determined at 0.1 ppm concentrations while most of the other elements could be determined at 5–50 ppm concentrations. The detection limit for W was however 100 ppm. The precision of the method has been better than 20% RSD.
The determination of silver is carried out by Electro-Thermal Atomization Atomic Absorption Spectrometric (ETA-AAS) technique by removal of graphite matrix by heating the sample in air at 850°C and dissolution of the residue containing Ag in concentrated HNO3 and analysing the same for Ag. The linear analytical range obtained for silver is 0.001–0.05 microgram per milliliter, while the precision of method is 5% RSD.
The D.C. arc carrier excitation method developed here is also suitable as a general survey method for any miscellaneous sample which can be mixed homogeneously with requisite amounts of graphite (serving as buffer) prior to preparing the analytical charge.