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1.
Small amounts of papaverine (about 3 mg in 15 ml solution) can be determined heterometrically in the presence of thiocyanate by titration with cobaltous solution. A strong electrolyte (Na2SO4) must be added to obtain a clear endpoint. The titration can be carried out in the presence of large amounts (97%) of quinine and ephedrine. The titration takes 2–3 min and the error rarely exceeds 1%.Papaverine, quinine, and ephedrine can be determined individually by spectrophotometry as their cobaltothiocyanates, which are extracted in 30% cyclohexanone in carbon tetrachloride, and the optical density measured at 625 nm. The method is reproducible at milligram levels with a standard deviation of ±0.3% for papaverine and quinine and = 0.5% for ephedrine. 相似文献
2.
Nitron and tetraphenylarsonium chloride react with a cobaltous salt in the presence of thiocyanate to form blue ion-association complexes, which can be extracted with organic solvents. This fact has been made the basis for the analysis of mixtures of nitrate and perchlorate by difference spectrophotometry. An aliquot of the sample solution is treated with a known excess of tetraphenylarsonium chloride to precipitate perchlorate only. After separating off the precipitate, the excess of reagent is determined in the supernatant liquid as tetraphenylarsonium cobaltothiocyanate and the perchlorate content can be found from a calibration curve. Another aliquot is treated with an excess of nitron to precipitate both anions; the excess of nitron is then determined as nitron
2. Analysis of Nitrate-Perchlorate Mixtures
Perchlorate | Nitrate | ||||||
Taken (μg) | Found (μg) | Error (%) | Taken (μg) | Found (μg) | Error (%) | ||
400 | 404 | + 1.00 | 248 | 250 | +0.81 | ||
400 | 400 | 0.00 | 496 | 492 | ?0.81 | ||
400 | 400 | 0.00 | 992 | 992 | 0.00 | ||
800 | 796 | ?0.50 | 248 | 248 | 0.00 | ||
600 | 602 | +0.33 | 248 | 245 | ?1.21 | ||
800 | 792 | ?1.25 | 496 | 498 | +0.40 |