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Reference Electrodes for Use in Nonaqueous Solutions

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Handbook of Reference Electrodes

Abstract

This chapter deals with the problem of the reference electrodes for use in conventional nonaqueous solvents, mainly from practical aspects. The reference electrodes used in nonaqueous solvents can be classified into two groups. One group uses, in constructing reference electrodes, the same solvent as that of the solution under study. The other group uses a solvent different from that of the solution under study; in most cases, aqueous reference electrodes are used but, in some cases, nonaqueous solvents other than that of the solution under study are used. Aqueous reference electrodes are usually an aqueous silver/silver chloride (Ag/AgCl) electrode or a calomel electrode (mostly saturated calomel electrode, SCE). Here, the reference electrodes of these two groups are discussed in detail in Sects. 6.1 and 6.2.

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Notes

  1. 1.

    In this book, there are other chapters related to nonaqueous systems. Chapter 1 by Inzelt is on the electrode potentials and includes a section on the problem to relate the electrode potentials between different media. Chapter 2 by Gritzner is on the reference redox systems in nonaqueous systems and their relation to water. Chapter 3 by Tsirlina is on the liquid junction potential and somewhat deals with the problem between different solvents. Chapter 7 by Bhatt and Snook is on the reference electrodes for room temperature ionic liquids. See these chapters as well.

  2. 2.

    (1) See footnote 11 for examples of the quasi-reference electrode of metal wire coated with a redox couple. (2) Supercritical fluids are not dealt with in this chapter, but, in the electrochemistry in them, pseudo- or quasi-reference electrodes are usually used.

  3. 3.

    These properties are not specific to the reference electrodes of this group. All reference electrodes, including ones for aqueous solutions, must have these properties in general.

  4. 4.

    Silver perchlorate (AgClO4, hygroscopic) may explode by friction or by heating and it must be handled with care. The use of other silver salts (AgNO3, AgBF4, AgSO3CF3, etc.) is recommended.

  5. 5.

    Solvent-independent potential scale is obtained by using, as the potential reference, a redox couple that is considered to have the same potentials in all solvents. Such redox couple, I +/I 0 or I 0/I −, should have the relation \( \Delta G_{{\mathrm{ t}{}({{\rm I}^{+}},\mathrm{ R}\to \mathrm{ S})}}^{{\rlap{-}{\mathrm{ o}}}}=\Delta G_{{\mathrm{ t}{}({{\rm I}^0},\mathrm{ R}\to \mathrm{ S})}}^{{\rlap{-}{\mathrm{ o}}}} \) or \( \Delta G_{{\mathrm{ t}({{\rm I}^0},\mathrm{ R}\to \mathrm{ S})}}^{{\rlap{-}{\mathrm{ o}}}}=\Delta G_{{\mathrm{ t}({{\rm I}^{-}},\mathrm{ R}\to \mathrm{ S})}}^{{\rlap{-}{\mathrm{ o}}}} \), where \( \Delta G_{{\mathrm{ t}{}(\mathrm{ i},\mathrm{ R}\to \mathrm{ S})}}^{{\rlap{-}{\mathrm{ o}}}} \) shows the variation in the solvation energy of species i between R (reference solvent) and S (the solvent under study). This relation is nearly satisfied by redox couples like BCr+/BCr and Fc+/Fc, especially when R and S are both aprotic (see page 41 of [177]).

  6. 6.

    The values of \( \log {\gamma_{{\mathrm{ t}{}(\mathrm{ A}{{\mathrm{ g}}^{+}},{{\mathrm{ H}}_2}\mathrm{ O}\to \mathrm{ S})}}} \) are 3.2 for (S=) PC, 1.6 for Ac, 1.2 for MeOH, −0.7 for TMS, −3.0 for DMF, −4.1 for AN, −4.6 for NMP, −5.1 for DMA, −6.1 for DMSO, −7.7 for HMPA, and −17.9 for DMTF (see Table 2.7 of [177]).

  7. 7.

    This reference electrode was used in the potentiometric study of acid–base equilibria in PC using a pH glass electrode, in which the potential of the reference electrode should be very stable [178].

  8. 8.

    In DMSO, if the electrode is 1 mM in Ag+ (Ag|1 mM Ag+ + 0.1 M LiClO4 (DMSO)), black precipitate of Ag0 is formed and the potential shifts by 150 mV to the negative direction in 10 days [89]. With 10 mM Ag+, the stability of the potential is much improved.

  9. 9.

    This applies to aprotic solvents that are hard base in HSAB concept. In soft base aprotic solvents like DMTF, AgCl is considerably dissolved by being dissociated into Ag+ and Cl−, because Ag+ is solvated extremely strongly.

  10. 10.

    A reference electrode of large area was used because the polarograph was a two-electrode instrument. With this instrument, the reference electrode also played the role of the counter electrode and considerable current passed through it. With a three-electrode instrument, which is now in common use, the reference electrode can be much smaller in size.

  11. 11.

    Peerce and Bard [191] coated a Pt electrode with poly(vinylferrocene) (PVFc) and the electrode was kept at the half-wave potential of the PVFc–PVFc+ couple to make their ratio 1:1. The electrode potential was constant and reproducible in deaerated AN over 21 h, but it was unstable in other nonaqueous solvents, probably because of the gradual dissolution of PVFc+. Efforts to prevent the dissolution of PVFc+ did not much improve the stability of the potential [192]. Bard’s group also prepared metal/polypyrrole quasi-reference electrode (QRE) for voltammetry in nonaqueous solutions [193]. It was easily fabricated by cyclic voltammetry of the metal electrode in 10 mM pyrrole + 0.1 M Bu4NPF6 (AN or DMC). Its potential was more stable than the Ag- and Pt-wire QREs and even a very small size for use in nanocells was possible.

  12. 12.

    The LJP between two solutions in the same (aqueous or nonaqueous) solvent has been discussed in Chap. 3 by Tsirlina. However, the LJP between two solutions in different solvents is quite different from that.

  13. 13.

    The reliability of the reference electrolyte (Ph4AsBPh4) assumption has been considered to be the best among various extra-thermodynamic assumptions (see page 41 in [177]).

  14. 14.

    (1) The variations in the actual (experimental) values of components (a) and (b) were obtained by measuring the potential differences of Cell (I): Ag|5 mM AgClO4, 20 mM Et4NClO4 (S1)¦¦20 mM Et4NClO4 (S1)¦c 1 MX (S1)¦c 2 MX (S2)¦20 mM Et4NClO4 (S2)¦¦5 mM AgClO4, 20 mM Et4NClO4 (S2)| Ag. In the case of component (a), the values of c 1 and c 2 were varied and necessary corrections were made. In the case of component (b), the electrolyte MX was varied, keeping the values of c 1 and c 2 constant and making appropriate corrections. E corrected in Figs. 6.4, 6.6, and 6.7 shows the corrected potential differences. (2) For the actual (experimental) variations in component (c), Cell (II): Ag|5 mM AgClO4, 25 mM Et4NClO4 (S1=AN)¦¦c Et4NClO4 (S1=AN)¦c 3 MX (S3)¦c Et4NClO4 (S2)¦¦5 mM AgClO4, 25 mM Et4NClO4 (S2)|Ag, was used and its potential differences were measured by varying solvent S3 for fixed MX, S1, and S2 and making necessary corrections. The values detected in this case (E) were the sum of the variations in component (c) at junctions S1/S3 and S3/S2.

  15. 15.

    Equations (6.1) and (6.2) were obtained by integrating the first and second terms on the right hand of Eq. (A), assuming linear variations in a (i), t (i), and \( \mu_{(\mathrm{ i})}^{{\rlap{-}{\mathrm{ o}}}} \) from the values in S1 to the values in S2 (Fig. 6.5a).

    $$ {E_{\mathrm{ j}}}=-({RT \left/ {F) } \right.}\int_{{{{\mathrm{ S}}_1}}}^{{{{\mathrm{ S}}_2}}} {\sum {({{{{t_{(\mathrm{ i})}}}} \left/ {{{z_{(\mathrm{ i})}})}} \right.}\mathrm{ d}\ln {a_{(\mathrm{ i})}}} -({1 \left/ {F) } \right.}} \int_{{{{\mathrm{ S}}_1}}}^{{{{\mathrm{ S}}_2}}} {\sum {({{{{t_{(\mathrm{ i})}}}} \left/ {{{z_{(\mathrm{ i})}})}} \right.}\mathrm{ d}\mu_{{(\mathrm{ i})}}^{{\rlap{-}{\mathrm{ o}}}}} } +{E_{\mathrm{ j},\mathrm{ solv}}}. $$
    (A)
  16. 16.

    At immiscible junctions H2O/NB and H2O/DCE, the slopes of the near-linear relations between experimental (actual) variations in component (b) and the values calculated by Eq. (6.2) are 1.0. Generally, the slopes approach 1.0 with the decrease in miscibility of the solvents on two sides [223]. Actually, at immiscible junctions, ions are distributed at the abrupt interface (thickness ~1 nm), as in Fig. 6.5b, and the distribution potential, Δϕ i , is generated. Moreover, on both sides of the interface, the LJPs between the same solvent, Δϕ 1 and Δϕ 2, are generated [223]. The potential difference at the immiscible junction is, therefore, the sum of Δϕ i , Δϕ 1, and Δϕ 2. Here, for immiscible c MX(H2O)¦c MX(NB), this potential difference was confirmed to agree fairly well with the results calculated by Eq. (6.2). It is interesting that Eq. (6.2) is nearly applicable even to immiscible junctions.

  17. 17.

    At miscible junctions, solvents on both sides mutually diffuse and the thickness of the diffusion layer expands with time (0.05–5 mm). Ions also diffuse between the two solvents; here, the ionic diffusion due to the gradients in ionic \( \mu_{{(\mathrm{ i})}}^{{\rlap{-}{\mathrm{ o}}}} \) value will cause a kind of ionic distribution at or near the layers of solvent diffusion. However, the fact that the experimental variations in component (b) are much less than the values calculated by Eq. (6.2) seems to show that the actual ionic distribution is much less in extent than the ionic distribution expected from the theoretically variation in \( \mu_{{(\mathrm{ i})}}^{{\rlap{-}{\mathrm{ o}}}} \) value. The cause for it must be elucidated, but ionic random walks which result in ionic diffusion seem to play some role [223]. Because the time and the distance of an average step of the random walk are very short, the solvation/desolvation processes cannot catch up with the theoretical \( \mu_{{(\mathrm{ i})}}^{{\rlap{-}{\mathrm{ o}}}} \) value, making component (b) smaller.

  18. 18.

    The values of component (c) at H2O/S can be estimated by assuming that the values of component (c) at H2O/NB and at AN/other aprotic solvent(s) are negligible. At the electrolyte concentration of 1 mM, the values estimated by this method are 122 mV for H2O/DMF and H2O/DMSO, 44 mV for H2O/AN, and 30 mV for H2O/PC, though the values somewhat decrease with the increase in electrolyte concentrations [235].

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Authors and Affiliations

  1. Faculty of Science, Shinshu University, Matsumoto, 390-8621, Japan

    Kosuke Izutsu

  2. 4-31-6-208 Kichijoji-honcho, Musashino, Tokyo, 180-0004, Japan

    Kosuke Izutsu

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Editors and Affiliations

  1. Dept. Physical Chemistry, Eötvös Loránd University, Pázmány Péter sétány 1/a, Budapest, 1117, Hungary

    György Inzelt

  2. Center for Process Analytical Chemistry, Åbo Akademi University, Biskopsgatan 8, Abo, 20500, Finland

    Andrzej Lewenstam

  3. Inst. Biochemie, Universität Greifswald, Felix-Hausdorff-Str. 4, Greifswald, 17487, Germany

    Fritz Scholz

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Izutsu, K. (2013). Reference Electrodes for Use in Nonaqueous Solutions. In: Inzelt, G., Lewenstam, A., Scholz, F. (eds) Handbook of Reference Electrodes. Springer, Berlin, Heidelberg. https://doi.org/10.1007/978-3-642-36188-3_6

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