An Introductory Course of Quantitative Chemical Analysis - With Explanatory Notes by Henry P. Talbot
page 63 of 272 (23%)
page 63 of 272 (23%)
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repeat the boiling (Note 1). If the color does not then reappear, add
alkali until it does, and a !drop or two! of acid in excess and boil again for one minute (Note 2). If no color reappears during this time, complete the titration in the hot solution. The end-point should be the faintest visible shade of color (or its disappearance), as the same difficulty would exist here as with methyl orange if an attempt were made to match shades of pink. From the corrected volume of alkali required to react with the oxalic acid, calculate the percentage of the crystallized acid (H_{2}C_{2}O_{4}.2H_{2}O) in the sample (Note 3). [Note 1: All commercial caustic soda such as that from which the standard solution was made contains some sodium carbonate. This reacts with the oxalic acid, setting free carbonic acid, which, in turn, forms sodium bicarbonate with the remaining carbonate: H_{2}CO_{3} + Na_{2}CO_{3} --> 2HNaCO_{3}. This compound does not hydrolyze sufficiently to furnish enough OH^{-} ions to cause phenolphthalein to remain pink; hence, the color of the indicator is discharged in cold solutions at the point at which bicarbonate is formed. If, however, the solution is heated to boiling, the bicarbonate loses carbon dioxide and water, and reverts to sodium carbonate, which causes the indicator to become again pink: 2HNaCO_{3} --> H_{2}O + CO_{2} + Na_{2}CO_{3}. By adding successive portions of hydrochloric acid and boiling, the carbonate is ultimately all brought into reaction. |
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