An Introductory Course of Quantitative Chemical Analysis - With Explanatory Notes by Henry P. Talbot
page 87 of 272 (31%)
page 87 of 272 (31%)
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prevent contamination of the solution by water from the pump. After
preparation for use, or when left standing, the tube A should be filled with water, to prevent clogging of the zinc. [Note 1: The use of fine zinc in the reductor is not necessary and tends to clog the tube. Particles which will pass a 10-mesh sieve, but are retained by one of 20 meshes to the inch, are most satisfactory. The zinc can be amalgamated by stirring or shaking it in a mixture of 25 cc. of normal mercuric chloride solution, 25 cc. of hydrochloric acid (sp. gr. 1.12) and 250 cc. of water for two minutes. The solution should then be poured off and the zinc thoroughly washed. It is then ready for bottling and preservation under water. A small quantity of glass wool is placed in the neck of the funnel to hold back foreign material when the reductor is in use.] STANDARDIZATION PROCEDURE.--Weigh out into Erlenmeyer flasks two portions of iron wire of about 0.25 gram each. Dissolve these in hot dilute sulphuric acid (5 cc. of concentrated acid and 100 cc. of water), using a covered flask to avoid loss by spattering. Boil the solution for two or three minutes after the iron has dissolved to remove any volatile hydrocarbons. Meanwhile prepare the reductor for use as follows: Connect the vacuum bottle with the suction pump and pour into the funnel at the top warm, dilute sulphuric acid, prepared by adding 5 cc. of concentrated sulphuric acid to 100 cc. of distilled water. See that the stopcock (C) is open far enough to allow the acid to run through slowly. Continue to pour in acid until 200 cc. have passed through, then close the stopcock !while a small quantity of liquid |
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