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  • Determination of cobalt ions at nano-level based on newly synthesized pendant armed macrocycle by polymeric membrane and coated graphite electrode.

Determination of cobalt ions at nano-level based on newly synthesized pendant armed macrocycle by polymeric membrane and coated graphite electrode.

Talanta (2009-10-20)
Ashok K Singh, Prerna Singh, G Bhattacharjee
ABSTRACT

Poly(vinylchloride) (PVC) based membranes of macrocycles 2,3,4:9,10,11-dipyridine-1,3,5,8,10,12-hexaazacyclotetradeca-2,9-diene (L(1)) and 2,3,4:9,10,11-dipyridine-1,5,8,12-tetramethylacrylate-1,3,5,8,10,12-hexaazacyclotetradeca-2,9-diene (L(2)) with NaTPB and KTpClPB as anion excluders and dibutylphthalate (DBP), benzyl acetate (BA), dioctylphthalate (DOP), o-nitrophenyloctyl ether (o-NPOE) and tri-n-butylphosphate (TBP) as plasticizing solvent mediators were prepared and investigated as Co(2+) selective electrodes. The best performance was observed with the membranes having the composition L(2):PVC:TBP:NaTPB in the ratio of 6:39:53:2 (w/w; mg). The performance of the membrane based on L(2) was compared with polymeric membrane electrode (PME) and coated graphite electrode (CGE). The PME exhibits detection limit of 4.7x10(-8)M with a Nernstian slope of 29.7 mV decade(-1) of activity between pH 2.5 and 8.5 whereas CGE exhibits the detection limit of 6.8x10(-9)M with a Nernstian slope of 29.5 mV decade(-1) of activity between pH 2.0 and 9.0. The response time for PME and CGE was found to be 11 and 8s, respectively. The CGE has been found to work satisfactorily in partially non-aqueous media up to 35% (v/v) content of methanol, ethanol and 25% (v/v) content of acetonitrile and could be used for a period of 4 months. The CGE was successfully applied for the determination of Co(2+) in real and pharmaceutical samples and as an indicator electrode in potentiometric titration of cobalt ion.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Tributyl phosphate, puriss., ≥99.0% (GC)
Supelco
Tributyl phosphate, for extraction analysis, ≥99.0% (GC)
Sigma-Aldrich
Tributyl phosphate, ≥99%
Sigma-Aldrich
Tributyl phosphate, 97%
Supelco
Tributyl phosphate, Pharmaceutical Secondary Standard; Certified Reference Material
Tri-n-butyl phosphate, European Pharmacopoeia (EP) Reference Standard