By Walter Huber
Titrations in Nonaqueous Solvents
summary: Titrations in Nonaqueous Solvents
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Extra info for Titrations in Nonaqueous Solvents
Example text
Water, alcohol) that may be present. The statistical error in the end-point determination can be minimized by a pendulum titration method (74). This method is based on the repeated determination of the end point to reduce chance error. To avoid any need to carry out numerous identical titrations (for which there may not be sufficient substance available), the following procedure is used: The sample is dissolved in a suitable solvent, and made up to a known concentration (not too low) in a graduated flask.
Thus the titration curve falls off to zero at the end point (Fig. 11). *Not ideally reversible in practice. III. Voltammetric and Amperometric Methods of End-Point Detection 33 In many cases, one of the two systems may be irreversible. One example of this is the determination of water by the K. Fischer method. In this method, only the system I2 4- 2 O ^ 2 I~ is reversible, so that a current flows only when excess iodine is present (iodide is always present). Thus if a standard solution of water in methanol is added to a Fischer solution, the current decreases with the free iodine content and finally reaches zero, where it remains on further titration.
The design of the measuring cell is such that its capacitive or inductive properties can be altered during the titration. The cell is inserted into an oscillating circuit, and changes in the ohmic resistance, the dielectric constant, and, in the case of coil cells, the permeability are measured. Since impedances and admittances are composed of reactive and active components, the measurements can be carried out by several methods. It should be noted that the sensitivities of the various methods differ with the conductivity of the solvent (Fig.