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  Section: Practical Skills in Chemistry » Instrumental techniques
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Oxygen electrodes

Instrumental techniques
  Basic spectroscopy
    Introduction to spectroscopy
    UV Ivisible spectrophotometry
    Fluorescence spectrophotometry
    Phosphorescence and luminescence
    Atomic spectroscopy
  Atomic spectroscopy
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    Inductively coupled plasma
    Decomposition techniques for solid inorganic samples
  Infrared spectroscopy
  Nuclear magnetic resonance spectrometry
    1H-NMR spectra
    13C-NMR spectra
  Mass spectrometry
    Interfacing mass spectrometry
  Chromatography ~ introduction
    The chromatogram
  Gas and liquid chromatography
    Gas chromatography
    Liquid chromatography
    High-performance liquid chromatography
    Interpreting chromatograms
    Optimizing chromatographic separations
    Quantitative analysis
    The supporting medium
    Capillary electrophoresis
    Capillary zone electrophoresis (CZE)
    Micellar electrokinetic chromatography (MEKC)
  Electroanalytical techniques
    Potentiometry and ion-selective electrodes
    Voltammetric methods
    Oxygen electrodes
    Coulometric methods
    Cyclic voltammetry
  Radioactive isotopes and their uses
    Radioactive decay
    Measuring radioactivity
    Chemical applications for radioactive isotopes
    Working practices when using radioactive isotopes
  Thermal analysis

The Clark (Rank) oxygen electrode
These instruments measure oxygen in solution using the polarographic principle, i.e. by monitoring the current flowing between two electrodes when a voltage is applied. The most widespread electrode is the Clark type (Fig. 34.6), manufactured by Rank Bros, Cambridge, UK, which is suitable for measuring O2 concentrations in cell, organelle and enzyme suspensions. Pt and Au electrodes are in contact with a solution of electrolyte (normally saturated KCl). The electrodes are separated from the medium by a Teflon® membrane, permeable to O2. When a potential is applied across the electrodes, this generates a current proportional to the O2 concentration. The reactions can be summed up as:

  4Ag → 4Ag+ + 4e (at silver anode)
  O2 + 2e + 2H ↔ H2O2 (in electrolyte solution; O2 replenished by diffusion from test solution)
  H2O2 + 2e + 2H+ ↔ 2H2O (at platinum cathode)

Oxygen probes

Clark-type oxygen electrodes are also available in probe form for immersion in the test solution (Fig. 34.7) e.g, for field studies, allowing direct measurement of oxygen status in situ, in contrast to chemical assays. The main point to note is that
Transverse section through a Clark (Rank) oxygen electrode.
Fig. 34.6 Transverse section through a Clark (Rank) oxygen electrode.
the solution must be stirred during measurement, to replenish the oxygen consumed by the electrode ('boundary layer' effect).

The glucose electrode
The glucose electrode is a simple type of biosensor, whose basic design is shown in Fig. 34.8. It consists of a Pt electrode, overlaid by two membranes. Sandwiched between these membranes is a layer of the immobilized enzyme glucose oxidase. The outer membrane is glucose permeable and allows glucose in the sample to diffuse through to the glucose oxidase layer, where it is converted to gluconic acid and H2O2. The inner membrane is selectively permeable to H2O2, which is oxidized to O2 at the surface of the Pt electrode. The current arising from this release of electrons is proportional to the glucose concentration in the sample within the range 10−7 to 10−3 mol L−1.

Electrochemical detectors used in chromatography operate by voltammetric principles and currents are produced as the mobile phase flows over electrodes set at a fixed potential: to achieve maximum sensitivity, this potential must be set at a level that allows electrochemical reactions to occur in all analytes of interest.

A Clark-type oxygen probe.
Fig. 34.7 A Clark-type oxygen probe.
Underlying principles of a glucose electrode.
Fig. 34.8 Underlying principles of a glucose electrode.


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