Calculation steam distillation

The Hausbrand vapor-pressure diagram [127, 128] in Figure 8-40 is a useful approach for the steam distillation calculation. This particular diagram was prepared for six organic compounds and the corresponding water vapor pressure as (it - ps) for three system pressures of 760, 300, and 70 mm Hg versus temperature,... 

Figure 11.47. Vapour pressure curves for steam distillation calculations...

Di-n-amyl ether. Use 50 g. (61 5 ml.) of n-amyl alcohol (b.p. 136-137°) and 7 g. (4 ml.) of concentrated sulphuric acid. The calculated volume of water (5 ml.) is collected when the temperature inside the flask rises to 157° (after 90 minutes). Steam distil the reaction mixture, separate the upper layer of the distillate and dry it with anhydrous potassium carbonate. Distil from a 50 ml. Claisen flask and collect the fractions of boiling point (i) 145-175° (13 g.), (ii) 175-185° (8 g.) and (iii) 185-190° (largely 185-185-5°) (13 g.). Combine fractions (i) and (u), reflux for 1 hour in a small flask with 3 g. of sodium, and distil from the sodium amyloxide and excess of sodium this yields 9 5 g. of fairly pure n-amyl ether (iv). The total yield is therefore 22 - 5 g. A perfectly pure product, b.p. 184 185°, is obtained by further distillation from a Little sodium. 

The normal boiling point of /V-ethylaniline is 204°C. Therefore, steam distillation makes possible the distillation of /V-ethylaniline at atmospheric pressure at a temperature of 99.15°C instead of its normal boiling point of 204°C. Commercial appHcations of steam distillation include the fractionation of cmde tall oil (qv) (84), the distilling of turpentine (see Terpenoids), and certain essential oils (see Oils, essential). A detailed calculation of steam distiUation of turpentine has been reported (85). 

Cyclohexylcarbinol (6, 22), In the preparation of cyclohexylcarbinol as described in Vol. 6, 22, a high-boiling by-product, the cyclohexylcarbinol acetal of formaldehyde, is sometimes obtained. The by-product becomes the main product if the steam distillation of the reaction mixture is omitted. The by-product can usually be avoided if twice the calculated amount to decompose the Grignard reagent of io per cent sulfuric acid is added to the reaction mixture before steam distillation is earned out. The acetal which may be present is thus hydrolyzed. 

This is the basis for a common method for the determination of ammonia in soil.1 Soil is suspended in water and placed in a Kjeldahl flask. The suspension is made basic by the addition of a strong (5-50%) sodium hydroxide solution, and the flask is immediately attached to a steam distillation setup. Steam distillation of the suspension carries the released ammonia to an Erlenmeyer flask, catching the distillate in a standardized acid solution that is subsequently back titrated via acid-base titration. The amount of ammonia in soil can be calculated from the end point of the titration. This procedure is similar to a standard Kjeldahl determination and can be carried out using the same equipment, although no digestion is needed. 

The trees cultivated for oil production must be at least 30 years old to make oil production profitable. The oil yield, calculated on the amount of wood used for steam distillation, is 4-6.5%. The production in India and Indonesia amounts to ca. lOOt/yr. 

Martin B. Neuworth The Kuhn-Roth method has a number of limitations. These were discussed by Brandenberger et al. (Anal. Chem. 33, 453 (1961)). The normal method for estimating C-methyl groups is based on a determination of total acidity calculated as acetic acid. Brandenberger has shown that other acids can be produced during the oxidation—e.g., benzoic acid, and these acids steam distil with the acetic acid. Therefore, when the classical Kuhn-Roth procedure is applied to a substance like coal, it would lead to methyl group values of questionable significance. 

The filter disc is transferred to a stopperred flask containing ethanol and propan-2-ol, and shaken to extract the water present which is then determined by gas-liquid chromatography the quantitity of water present is calculated from the ratio of the areas of the peaks for water (unknown) and ethanol (internal standard). The alkaloids are extracted from the filter disc using sulphuric acid and determined by a specially developed autoanalyser procedure based on the Koenig reaction this is shown schematically in Fig. 21. Since the procedure was developed specially for this application, results obtained from it were compared closely with those produced by the traditional manual method, a steam distillation technique, before it was adopted as a standard method. 

They nitrated radioactive toluene-l-14C with a mixture of nitric and sulphuric acid at 0°, 30°, 45° and 60°C. After nitration the whole was diluted, with water and steam distilled. Thus mononitro-products were separated from unnitrated toluene and dinitro products. The weighted sample of isomeric mononitro-toluene was diluted with a known quantity of non-radioactive m- nitrotoluene and the mixture was distilled through an efficient micro-fractionating column in order to recover a pure sample of m- nitrotoluene. The m- nitrotoluene was oxidized by dichromate-sulphuric acid mixture to m- nitrobenzoic acid and this material was radio-assayed. The proportion of m- nitrotoluene in the mixed nitrotoluenes was calculated from the formula... 

The volatiles of fresh pineapple (Ananas comosus [L] Merr.) crown, pulp and intact fmit were studied by capillary gas chromatography and capillary gas chromatography-mass spectrometry. The fnjit was sampled using dynamic headspace sampling and vacuum steam distillation-extraction. Analyses showed that the crown contains Cg aldehydes and alcohols while the pulp and intact fruit are characterized by a diverse assortment of esters, h rocarbons, alcohols and carbonyl compounds. Odor unit values, calculated from odor threshold and concentration data, indicate that the following compounds are important contributors to fresh pineapple aroma 2,5-dimethyl-4-hydroxy-3(2H)-furanone, methyl 2-methybutanoate, ethyl 2-methylbutanoate, ethyl acetate, ethyl hexanoate, ethyl butanoate, ethyl 2-methylpropanoate, methyl hexanoate and methyl butanoate. 

The calculated quantities of benzene and aluminium chloride are placed in an enamelled vessel and maintained at 25° C. The chloroacetyl chloride is then added in small quantities while the mixture is agitated. At the end of this addition, the mass is warmed to 60° to 70° C. for 2 hours and then poured into cold water. The layer containing the chloroacetophenone is freed from benzene by distillation and the chloroacetophenone finally purified by steam distillation. 

At this point aniline can be isolated. You could reduce the solubility of aniline by dissolving in the steam distillate 0.2 g of sodium chloride per milliliter, extract the aniline with 2-3 portions of dichloromethane, dry the extract, distill the dichloromethane (bp 4rC), and then distill the aniline (bp 184°C). Or the aniline can be converted directly to acetanilide. The procedure calls for pure aniline, but note that the first step is to dissolve the aniline in water and hydrochloric acid. Your steam distillate is a mixture of aniline and water, both of which have been distilled. Are they not both water-white and presumably pure Hence, an attractive procedure would be to assume that the steam distillate contains the theoretical amount of aniline and to add to it, in turn, appropriate amounts of hydrochloric acid, acetic anhydride, and sodium acetate, calculated from the quantities given in Experiment 2. 

Rigoroas stage calculations can be mode for steam distillation columns, using methods described in Section 5.3. It is also possible to make approximate calculations on a sieam-frea basis, as if the tom] pressure in die columa were equal to the total vapor pressure of the material being distilled. 

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