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5MbAbstract14 Crown 4 derivatives bearing either one or two oxymethyl, benzyl oxymethyl, methoxycarbonylmethyl or carbamoylmethyl substituents have been prepared in an attempt to obtain selective ionophores for lithiumions. Complexation has been monitored by IR steroids, (^13)C NMR, Fast Atom Bombardment Mass Spectrometry steroids, and solvent polymeric membranes have been fabricated and evaluated using the fixed interference method. Improved lithium selectivities of the disubstituted 14 crown 4 ligands compared to the monosubstituted analogues in the potentiometric experiments, bears out the premise that there is a need to suppress competitive 2:1 complex formation with sodium.