www.elsevier.nl/locate/poly Polyhedron 19 (2000) 2493 – 2500 Activity coefficients of 3:3 electrolytes in aqueous solutions Francesco Malatesta *, Sara Trombella, Ambrogio Giacomelli, Massimo Onor Dipartimento di Chimica e Chimica Industriale, Uniersita ` di Pisa, Via Risorgimento 35, 56126 Pisa, Italy Dedicated to the memory of Professor Sergio Cabani. Abstract Activity coefficients of 3:3 electrolytes have not been liable to determination until 1994, when one of the authors devised a new type potentiometric cell able to trace La[Fe(CN) 6 ] down to about 5 ×10 -6 mol kg -1 . La[Co(CN) 6 ], [Co(en) 3 ][Co(CN) 6 ], and [Co(en) 3 ][Fe(CN) 6 ], are now studied by the same method. Like La[Fe(CN) 6 ], these electrolytes display in the dilute regions large negative deviations from the limiting slope instead of the moderate positive deviations predicted by the Debye – Hu ¨ ckel theory. Although the negative deviations can be easily interpreted in terms of only a partial dissociation, one should not conclude that the 3:3 salts are only sparingly dissociated. Theoretical calculations are presented, showing how long-range interactions, in a population of non associated +3 and -3 charged spheres, are able to produce effects that simulate the behaviour of a weak electrolyte. Preliminary information is provided of an unexplored method, here devised, to determine the mean activity coefficients in mixed electrolyte solutions. © 2000 Elsevier Science B.V. All rights reserved. Keywords: 3:3 Electrolytes; Activity coefficients; Electrolytic solutions; High-charge salts; High valency electrolytes; Mixed electrolytes 1. Introduction About 1 century since Lewis’ concept of the activity coefficient [1] and 76 years since the Debye–Hu ¨ ckel theory [2], experimental and theoretical information regarding 3:3 electrolytes is still lacking. Only in the last few years have potentiometric cells suitable for such salts and for the high dilution levels required become available [3 – 11], and only La[Fe(CN) 6 ] has been stud- ied appropriately [6]. Owing to the paucity of experi- mental data, essentially all restricted to La[Fe(CN) 6 ], theoretical treatments have not been able to reach ultimate conclusions either. For instance, the conduc- tivity data for La[Fe(CN) 6 ] have long been interpreted as evidence of a significant association of the elec- trolyte, comparable to formic acid [12]; conversely, the activity coefficients recently determined with the method of the liquid membrane cells [6] have proved identical to those expected for a theoretical model of charged spheres free from any association, the so-called ‘primitive’ model [6,7]. (The only partial dissociation of La[Fe(CN) 6 ] evidenced from the conductivity data re- lies on a theoretical framework that is incorrect for high-charge electrolytes). As no general value can be obtained from La[Fe(CN) 6 ] alone, three more salts of the same 3:3 type, lanthanum hexacyanocobaltate(III), tris(ethylene- diamine)cobalt(III) hexacyanocobaltate(III), and tris- (ethylenediamine)cobalt(III) hexacyanoferrate(III) are now examined. These salts are sparingly soluble, e.g. [Co(en) 3 ][Fe(CN) 6 ] does not reach 5 ×10 -4 mol kg -1 , but this does not represent a problem, as the liquid membrane cells in many electrolytes are able to provide stable and reproducible emf values down to 1 ×10 -5 mol kg -1 and less. Moreover, a later reported thermo- dynamic relationship (Eq. (3)), allows us to derive the values of the activity coefficients of a 3:3 electrolyte from the corresponding relative activity coefficients, regardless of the ability of directly performing extrapo- lation to zero for the 3:3 electrolyte. * Corresponding author. Fax: +39-050-918-260. E-mail address: franco@dcci.unipi.it (F. Malatesta). 0277-5387/00/$ - see front matter © 2000 Elsevier Science B.V. All rights reserved. PII:S0277-5387(00)00549-0