Complexation of Be(II) ion with 1-(2,4-Dihydroxy-1-phenylazo)-8-hydroxy-3,6-naphthalenedisulfonate as the chemical basis of the selective detection of ultratrace be by reversed-phase high-performance liquid chromatography

Hitoshi Hoshino, Takeshi Nomura, Kouji Nakano, Takao Yotsuyanagi

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17 Citations (Scopus)

Abstract

The complexation reactions of beryllium(II) ion with 1-(2,4-dihydroxy-1-phenylazo)-8-hydroxy-3,6-naphthalenedisulfonate (H-resorcinol) are studied. The acid dissociation constants of H-resorcinol, H3L2-, at 293 K and I = 0.10 [K(OH, NO3)] are pKa1 = 5.67, pKa2 = 8.57, and pKa3 > 13. The formation constant at 293 K and I = 0.10 [(K,H)NO3] is estimated to be log[{[Be(HL)2--][H-]2}/ {[Be][H3L2-]}] = -4.58, and pKa′ = 6.39 for [Be(HL)]2-, which give the basis for the optimization of the precolumn chelation reactions and the masking system with EDTA. The kinetic data for ligand substitution reactions with sutfosalicylate ion are also reported to demonstrate the remarkable inertness of the Be chelate, which is suitable for HPLC separation. Reported is an accurate method for determining traces of Be(II) ion at nanomolar levels with photometric detection coupled with ion-pair reversed-phase HPLC. The chelate, [BeIIL]3-, is efficiently separated on an Asahipak ODP-50 column using tetrabutyl-ammonium bromide as an ion-pairing agent in a methanol (35 wt%)-water eluent. Only Al and Fe give peaks under the conditions used. The large molar absorptivity of the H-resorcinol chelate, 3.99 × 104 M-1 cm-1 at 500 nm, and the short retention time with excellent peak resolution ensure the ultralow detection limit (30 blank) down to 7.2 ppt (0.8 nM) with no preconcentration procedures. The excellent toughness toward the matrix influence was demonstrated using the model solution for an air-dust sample. The HPLC separation, coupled with the EDTA masking procedure, enables one to detect Be(II) ion at 20 nM in the presence of metals at the natural abundance levels in air samples, such as Al, Fe, Ca, Mg, Zn, and Pb at 240, 140, 300, 66, 16, and 6.2 μM, respectively, in the final solution.

Original languageEnglish
Pages (from-to)1960-1965
Number of pages6
JournalAnalytical Chemistry
Volume68
Issue number11
DOIs
Publication statusPublished - 1996 Jan 1

ASJC Scopus subject areas

  • Analytical Chemistry

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