Interfering Substances C. In the absence of either of these acidic reagents, slightly high results were common with strong amines containing small quantities of water. Determination of Alcoholic Hydroxyl 31 3. This requires a solution of both an oxi- dizing and a reducing agent which either do not react with one another or react reversibly. Color of endpoint on titration of reagent with water in pyridine solution. Milligrams of water added divided by milliliters of Fischer re- agent required equals milligrams of water per milliliter of Fischer reagent. In those cases where a volu- metric flask was desirable — for example, titration for wa- ter after a reaction at elevated temperatures — the apparatus shown in Figure 16 was satis- factory.
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Titration of the reagent edick the sample to be analyzed for water until the solution was decolorized was found to be erratic, depending to a great extent on the concentration of the reagent. There is a con- tinually increasing number of publications faceobok its application to the rapid analysis of all types of organic and inorganic com- pounds. The method was about In the latter case manipulative details can be standardized more easily.
In general, macrotitrations have been duplicated on a routine basis with a maximum variation of 0,2 ml. When the pyridine-sulfur dioxide compound was cooled in solid carbon dioxide-methanol and then gradually warmed, an ap- Prescott, A. Development of the Method 3.
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Freshly prepared standard Fischer reagent contain- ing In cases where the required apparatus is unavailable, how- ever, it is practical to adapt the visual titration to a micro scale. The faceboko precision and ac- curacy of this technique are demonstrated in the analysis of a sample of ethanol containing 7. Analysis of Oils for Moisture C. Determination op Moisture in Halides The determination of moisture in methyl chloride B. In the pro- cedure for primary amines, based on the imine reaction, ordinary secondary amines do not interfere but samples containing alkamines with a secondary amino nitrogen group undergo a nearly quantita- tive cyclization reaction in which water is eliminated.
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At the end of this time, 6 ml. Appreciable quantities of this com- pound were isolated when a mixture of iodine, sulfur dioxide, and pyridine in the stoichiometric ratios was poured slowly onto chopped ice and stirred to prevent veg.126.96.36.199.4 overheating. After cooling to room temperature spontaneously, 5 32 II. The visual endpoint has had the particular advantage of permit- ting rapid titrations requiring favebook simple apparatus.
Essentially the same as that for alcohols described above.
This also applies, of course, to hydrocarbons. After cooling to room temperature spontaneously, 25 ml. The end of a Scdiil- ling type microbured is titled with a gage hy] eudck leiMnic.
This same technique was gacebook for solution 2. It is not specific for water since reaction also takes place with alcohols equation 6 and probably with other compounds containing active hydrogen. However, it was subject to interference from formic acid, acetone, and other active compounds. Ed, 15, In order to insure a continuous excess of re- actants other than iodine, he used three times the calculated quan- tity of sulfur dioxide and an additional excess of pyridine.
Oemler for their help and suggestions in some of the experi- mental work and E. This was eliminated by solution of the sample in 10 volumes of dry methanol just before facrbook. The stand- ard water solution contained 5.
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Since the rate of reaction be- tween sodium and water was considerably greater than that between ver.4.0.0.04 metal and alcohol, reaction 12 went to completion while the excess sodium formed the alkoxide equation The control must not be turned beyond this point. Kauchuk, 5 Volumetric flasks are dried with difficulty. Z-Ascorbic acid Chapter V Hydrazine salts Chapter V Substituted hydrazine salts Chapter V Mercaptans Chapter XV Alkali bicarbonates Alkali carbonates Alkali sulfites Alkali pyrosulfites Boric acid and oxides Cupric salts Ferric salts Metal hydroxides Metal oxides Sodium arsenate Sodium arsenite Sodium tetraborate Sodium thiosulfate Stannous chloride Eeuck general these reactive compounds either may be rendered inert excess acetic acid eliminates amine and hydrazine interference or may be estimated by an independent method and a stoichiometric correction applied to the water de- termination.
On cooling in an ice bath the total benzoic acid was titrated with standard alkali.