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P~~S~G~ Chemistry of the Oxides of Lead. Part T71. the Anodic Behaviour of Lead and Lead Dioxide

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P~~S~G~ Chemistry of the Oxides of Lead. Part T71. the Anodic Behaviour of Lead and Lead Dioxide View Article Online / Journal Homepage / Table of Contents for this issue PHYSICAL CHEMISTRY OF THE OXIDES OF LEAD. PART VI. 2091 CCL.--P~~S~G~Chemistry of the Oxides of Lead. Part T71. The Anodic Behaviour of Lead and Lead Dioxide. By SAMUELGLASSTONE. IN a previous communication (this vol., p. 1469), the abnormal electromotive behaviour of electrolytic lead dioxide has been explained by assuming the presence in it of minute traces of 'a Published on 01 January 1922. Downloaded by Fudan University 25/12/2017 21:18:09. higher unstable oxide, possibly PbO,. In order to obtain further evidence of the existence of such an oxide, a series of experiments, on the polarisation and discharge of lead and lead dioxide anodes in alkali, was carried out. Since the electrode potentials of the known oxides of lead in A'-sodium hydroxide have already been determined, measurements of potential during polarisation and discharge should give information regarding the existence of any oxides in addition to those with which we are already familiar. Elbs and Forssell (2. Elektrochem., 1902, 8, 760) found that at low current densities a lead anode dissolves in N-sodium hydroxide as bivalent ions, but at higher densities the lead no longer dissolves, but lead dioxide is deposited, and oxygen is evolved. These authors attribute the evolution of gas to the decomposition of the dioxide into monoxide and oxygen, and state that this reaction occurs at a potential 0-23 volt more positive than that required for the deposition of lead dioxide from a solution of N-sodium hydroxide View Article Online 2092 GLASSTONE : saturated with lead monoxide. Observations and measurements to be described in the presenf paper, however, appear to show that oxygen evolution at a lead anode takes place through the inter- mediate formation of an unstable oxide, more highly oxygenated than the dioxide. Lorenz and Lauber (2. Elektrochem., 1900, 15, 167) polarised lead plates anodically in sulphuric acid and followed the back E.M.P. by discharging through a high resistance. Fourteen different halts in the discharge potential were reported, eight of which were said to correspond with the electrode potentials of the oxides of lead measured by Streintz and Neumann (?Vied. Annulen, 1890, 41, 97). Lorenz and Lauber make no mention of an oxide higher than the dioxide, although it may be pointed out that a potential of 2.05 volts is attributed to the electrode PblPbO, (which is actually PbO,lPbSO,, owing to the instability of the system lead-lead dioxide in sulphuric acid), and to the potential of the electrode PbJPbSO, is given the probably correct value of -0.29 volt. From these figures, the ordinary lead accumulator should have an E.M.F. of 2-34 volts, which is, of course, much higher than the actual value. The second halt in the discharge potential was found to be 1.62 volts; this probably represents the reaction Pb"" + Pb" (that is, PbO,lPbSO,), for then the lead accumulator should have an E.M.F. of 1-91 volts, which is in close agreement with the actual value if the sulphuric acid is about 2N. It therefore appears that the potential of 2.05 volts is to be attributed to an oxide higher than the dioxide. ExP E R I M E N TAL. Published on 01 January 1922. Downloaded by Fudan University 25/12/2017 21:18:09. A simple cell was made up consisting of a platinum foil kathode, 6 sq. cm. in area, and an anode of either pure lead (series I and 11) or lead dioxide (series I11 and IV). The anodic potential was measured during charge and discharge by comparison with a standard mercuric oxide half-element, the connecting tube of which was drawn out into a fine jet, which pressed close up against the anode. Xeries I. The anode was a small sheet of lead connected with a platinum wire; the whole was completely waxed over, and an area of about 2 aq. cm. of the lead scraped clean and bright. A small pit was made in the surface, and the jet of the standard electrode fitted into it. The electrolyte used in this series was N-sodium hydroxide, and all measurements were made at room temperature (about 17"). The direct anodic potential (with current flowing) wafi measured from time to time, with different current densities. With low View Article Online PHYSICAL CHEMISTRY OF THE OXIDES OF LEAD. PART VI. 2093 densities, up to 0.026 amp./cm.Z, the anodic potential remained almost constant at -0.53 volt; lead dissolved at the anode, but there was no evolutioh of oxygen. At the hathode, however, lead was deposited and alsa hydrogen evolved, consequently more lead went into solution than was depasited. The potential of -0.53 volt corresponds with that of the half-element PblPbO N-NaOH (-0.56 volt), the small difference being probably due to cohcentration polarisation. The action at the anode is there- fore the discharge of OH' ions, and the dissolution of lead as plumbite : 30H' + Pb + 2 @ = HPbO,' + H,O. A certain amount of lead also went into solution as bivalent plumbous ions : Pb + 20H' + 3 @ = Pb(OH), z+ Pb"+ 20H'. If the current density is increased further, for example, to 0.03 amp.lcm.2, after a few minutes the current, as registered on an ammeter in the circuit, will suddenly decrease to about one-half of its previous value, and at the same time a dark grey film will be seen to creep across the hitherto clean surface of the lead anode. Coincident with this, the anodic potentid suddenly rises to 0.70 volt, but there is still no evolution of oxygen. A much higher potential is now necessary to cause lead to dissolve, passivation being undoubtedly due to the visible coating of oxide. This is probably the dioxide, since neither lead sesquioxide nor red lead, both of which give plumbous ions in solution (see Part IV, this vol., p. 1456), would be likely to cause such a large increase of potential, Published on 01 January 1922. Downloaded by Fudan University 25/12/2017 21:18:09. namely, from -0.53 to 0.70 volt. The lead is apparently dissolving its plumbic and plumbate ions : Pb + 40H' + 4 @ = Pb(OH), -ePb""+ 40H'. Pb + 60H' + 4 @ = PbO,"+ 3H,O. The presence of plumbate in the electrolyte may be readily sham by the addition of dilute nitric acid, when a precipitate of lead dioxide is formed. After a few more minutes, a further, but smaller, decrease in the current occurs, and a black film now passes over the surface of the anode. At the same time, the anode potential rises to 1-18 volts, and when the dark Alm completely covers the anode, evolution of oxygen commences. This second film, which causes such a high anodic potential, is very probably a higher oxide; since evolution of oxygen takes place only after the formation of this am, it appears &a%gm €orhation is due to the continual form- View Article Online 2094 GLASSTONE : ation and decomposition of this higher oxide.* Foerster (2. physilcal. Chem., 1909, 69, 236) and Grube (2. Elektrochem., 1910, 16, 621) have similarly correlated the evolution of oxygen at a platinum anode with the formation of the oxide PtO,, and possibly PtO,. Similar conclusions have been drawn by Muller (ibid., 1907, 13, 133) and Foerster (Zoc. cit.) for the evolution of oxygen at copper, nickel, and iridium anodes. If the current density is kept constant at 0.03 amp./crn2, the anodic potential rises slowly to 1-26 volts, but no further changes occur. Newbery (T., 1916, 109, 1066) measured the overvoltage at it lead anode in N-sodium hydroxide, using the commutator method; only one overvoltage condition is mentioned, namely, 0.6 to 1.0 volt (that is, an anodic potential of 1.0 to 1-4 volts) depending on the current density. These figures correspond with the third anodic potential of the present series of measurements. Discharge Potential.-After three hours’ polarisation at 0.03 amp./cm.2, the current was stopped, and the potential of the anode during self-discharge measured against that of a standard electrode. The initial fall from 1-26 to 0.82 volt occupied thirty-two seconds, and therefore very little of the high potential at the anode could have been due to the “ transfer resistance ” of oxide or gas film. During subsequent discharge, lasting twenty-one minutes, there was an indication of a break at 0.59 volt, a perfectly definite halt at 0.29 to 0.25 volt, and then a rapid drop to -0.56 volt. On allowing the electrode to stand, the potential rose again to 0.29 volt, at which value it remained for some time. The possible halt at 0.59 volt does not correspond with any known potential of the Published on 01 January 1922. Downloaded by Fudan University 25/12/2017 21:18:09. lead oxides, but the break at 0.29 to 0.25 volt was evidently due to mixtures, or more probably, solid solutions of lead monoxide, sesquioxide, and red lead, electrornotively active with lcad dioxide. After the discharge, it light brown coating of oxide had formed on the anode, and analysis showed it to contain lead monoxide and dioxide in the ratio of 1 : 0.85. This composition would agree with that of the mixture or solid solution suggested to account for the measured potential. Recharging of a Discharged Anode.-The results obtained on recharging a discharged anode were substantially the same as * Since the completion of this work in April 1922, Grube (Z.Elektrochem., 1022, 28, 273) has reported the results of a set of experiments similar to thoso in series I.
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