Distillation results

Pertains to the weight per cent for the D 2887 simulated distillation results and the volume per cent for the D 86 simulated distillation. 

Conversion of the Low Pressure Distillation Results into Equivalent Results for Atmospheric Pressure... 

To convert low pressure distillation results into those of atmospheric pressure, the Maxwell and Bonnel (1955) equations are used. 

Isomerization of cyclohexane in the presence of aluminum trichloride catalyst with continuous removal of the lower boiling methylcyclopentane by distillation results in a 96% yield of the latter (54). The activity of AlCl -HCl catalyst has been determined at several temperatures. At 100°C, the molar ratio of methylcyclopentane to cyclohexane is 0.51 (55). 

The frequency and method of testing feed streams varies from one refiner to another. Some refiners analyze daily, others two or three times a week, and some once a week. The frequency depends on how the distillation results are applied, the variation in crude slates, and the availability of lab personnel. 

In some cases we may benefit from adopting a semi-continuous mode of operation, e.g. to a batch of one reactant we continuously feed the other reactant, while removing a volatile product continuously. An example where this is advantageous is the production of ethyl-4-pentenoate, CH2=(CH2)3(CO)OEt from allyl alcohol and triethyl orthoacetate, CHs-CfOEt). Continuous addition of allyl alcohol to a batch of triethyl orthoacetate and continuous removal of the produced ethylalcohol (and. some allyl alcohol) by distillation resulted in high yields of the dersired ester ethyl-4-pentenoate. By contrast, if allyl alcohol and triethyl orthoacetate were reacted in a batch-wise manner the product consisted of a 1 1 mixture of the desired ester and the undesired ester (Anderson, 2000, p 279 Bollyn and Wright, 1998). 

The combined ether solutions are then subjected to distillation at 20° or below under the vacuum obtainable from a water pump until all the ether is removed. Prolonged distillation results in decomposition of the diazo ester and in a decreased yield. The yellow residual oil is practically pure ethyl diazoacetate and is satisfactory for most synthetic purposes (Note 3). The yield is about 98 g. (85%) (Notes 4 and 5). 

Transient blue colors in the distillate result from autoxida-tion. They do not, however, affect the purity of the final product. 

The isomerization with f-BuOK gives also a small amount of the amine with the reversed order of the double and triple bond. Its boiling point is by 20 to 30 C higher than that of the main product, and careful fractional distillation results in a satisfactory separation of these isomers. 

To explore the potential for loss of moderately volatile compounds during vacuum distillation, solutions of biphenyl (4 /zg/mL), phenanthrene (4 /zg/mL), and pyrene (0.14 /zg/mL) were freeze-dried or vacuum-distilled for varying times, and the amount of compound remaining in the flask was determined. The results (Table II) show that vacuum distillation resulted in greater losses than lyophilization and that the ease of loss varied considerably. Biphenyl was so readily lost that the mere degassing of its solution resulted in a loss of about two-thirds of the original compound (see Figure 2). 

The simulated distillation results are given in Table III, column A, along with literature values for the distillations of five other P. R. Spring samples. The 0.4% material appearing in fraction 1-4 for this study... 

The submitters distilled the azeotrope immediately after heating the mixture to reflux. If it is allowed to stand and cool it sets solid with magnesium chloride and subsequent distillation results in appreciably lower yields. 

After cooling, the solution was diluted with 1.5 liters of water and subjected to three extractions with ether. The amine was extracted from the ethereal solution with 2 N HCI and liberated therefrom by the addition of solid NaOH (while cooling). The alkaline solution was extracted with ether and the ethereal solution was dried with solid NaOH. Distillation resulted in 10.6 grams (70% of the theory) of 1-aminoadamantane which, after sublimation, melted at 180°C to 192°C (seal capillary). It is converted to the hydrochloride. 

Because 10,000 lb of R must be produced daily to meet plant capacity requirements, the laboratory distillation results must be scaled up to this basis. Doing so produces the following values ... 

The inclusion of unripe fruits or leaf and stalk material of the plant together with the spice during distillation results in a change in the physico-chemical constants. The specific gravity, optical rotation and alcohol (calculated as linalool) values are reduced somewhat, while the carbonyl value is enhanced (Purseglove et al., 1981 Smallfield et al., 1994). 

Nitric acid is miscible with water and distillation results in an azeotrope with a concentration of 68.4 percent HN03 and a boiling temperature of 121.9°C at atmospheric pressure. Two solid hydrates are known the monohydrate (HNCh H20) and the trihydrate (HN03 3H20). 

All toxic materials were disposed of in accordance with "Prudent Practices in the Laboratory National Academic Press Washington, DC, 1996. The malodorous, methanol distillate resulting from the borane reduction was first treated with commercial bleach before disposal. 

For the extractive distillation results of Tables V and VI, the reboiler load for the above ethanol rate would be about 20.9 million Btu per hour. The ethanol product contains about 16 ppm of water and about 1.2 ppm of ethylene glycol. For an ethanol recovery of 99.99% ra, 46 total equilibrium trays are required with a reflux-feed ratio of 1.55+ and a solvent-ethanol ratio of 4.09" mole basis. The condenser load is about 13.1 million Btu/hour, and the tower diameter is about 5.3 feet, based on a Glitsch sizing technique. 

Azeotropic Distillation Results from Automatic Computer Calculations... 

The methods used here to give the phase equilibria are reviewed, and the Azeotropic Distillation Program ADP/ADPLLE is described. Application of the program to calculate an azeotropic distillation problem is shown and discussed, and a sample computer output is given and is briefly discussed. Finally, calculated azeotropic distillation results are compared for dehydrating aqueous ethanol for the three entrainers, n-pentane, benzene, and diethyl ether. 

Simulated Distillation Results. Important insight concerning the molecular-size distribution of asphaltenes vs. maltenes is gained by the simulated distillation data. The boiling point distribution curves are shown in Figure 3. These curves were drawn as follows. Quantitative simulated distillation data was obtained on the virgin bitumen and the maltenes. Direct information is obtained up to a nominal boiling point of 535°C shown by the vertical dashed line. The area under the curve for the nonvolatile portion is... 

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