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Senin, 02 Agustus 2010

STANDARD EDTA SOLUTIONS


Disodium dihydrogenethylenediaminetetra-acetate of analytical reagent quality is available commercially but this may contain a trace of moisture. After drying the reagent at 80 OC its composition agrees with the formula Na2H2C1,H1 20,N2,2H20 (relative molar mass 372.24), but it should not be used as a primary standard. If necessary, the commercial material may be purified by preparing a saturated solution at room temperature: this requires about 20 g of the salt per 200 mL of water. Add ethanol slowly until a permanent precipitate appears; filter. Dilute the filtrate with an equal volume of ethanol, filter the resulting precipitate through a sintered glass funnel, wash with acetone and then with diethyl ether. Air-dry at room temperature overnight and then dry in an oven at 80 OC for at least 24 hours. Solutions of EDTA of the following concentrations are suitable for most experimental work: O.lM, 0.05M, and 0.01M. These contain respectively 37.224 g, 18.612 g, and 3.7224 g of the dihydrate per litre of solution. As already indicated, the dry analytical grade salt cannot be regarded as a primary standard and the solution must be standardised; this can be done by titration of nearly neutralised zinc chloride or zinc sulphate solution prepared from a known weight

of zinc pellets, or by titration with a solution made from specially dried lead nitrate. The water employed in making up solutions, particularly dilute solutions, of EDTA should contain no traces of multicharged ions. The distilled water normally used in the laboratory may require distillation in an all-Pyrex glass apparatus or, better, passage through a column of cation exchange resin in the sodium form - the latter procedure will remove al1 traces of heavy metals. De-ionised water is also satisfactory; it should be prepared from distilled water since tap water sometimes contains non-ionic imiuriiies not removed by an ion exchange column. The solution may be kept in Pyrex (or similar borosilicate glass) vessels, which have been thoroughly steamed out before use. For prolonged storage in borosilicate vessels, the latter should be boiled with a strongly alkaline, 2 per cent EDTA solution for several hours and then repeatedly rinsed with de-ionised water. Polythene bottles are the most satisfactory, and should always be employed for the storage of very dilute (e.g. 0.001 M) solutions of EDTA. Vessels of ordinary (soda) glass should not be used; in the course of time such soft glass containers will yield appreciable amounts of cations (including calcium and magnesium) and anions to solutions of EDTA. Water purified or prepared as described above should be used for the preparation of al1 solutions required for EDTA or similar titrations.

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