Republication or reproduction of this report or its storage and/or dissemination by electronic means isAbstract: Available experimental data on stability constants of proton and metal complexes for 10 phosphonic acids [methylphosphonic acid, 1-hydroxyethane-

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Factors affecting the NMR titration procedures for the determination of pKa values in strongly basic and strongly acidic aqueous solutions (2 > pH > 0 and 14 > pH > 12) are analyzed. Guidelines for experimental procedure and publication protocols are formulated. These include: calculation of the equilibrium H+ concentration in a sample; avoidance of measurement with glass electrode in highly acidic (basic) solutions; exclusion of D2O as a solvent; use of an individual sample isolated from air for each pH value; use of external reference and lock compounds; use of a medium of constant ionic strength with clear indication of the supporting electrolyte and of the way the contribution of any ligand to the ionic strength of the medium is accounted for; use of the NMR technique in a way that eliminates sample heating to facilitate better sample temperature control (e.g., 1H-coupled NMR for nuclei other than protons, GD-mode, CPD-mode, etc.); use of Me4NCl/Me4NOH or KCl/KOH as a supporting electrolyte in basic solution rather than sodium salts in order to eliminate errors arising from NaOH association; verification of the independence of the NMR chemical shift from background electrolyte composition and concentration; use of extrapolation procedures.

Part I. Aromatic ortho-hydroxycarboxylic acids, Pure Appl. Chem. 69, 329-381 (1997

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