Sublimation apparatus

Checkers report that since the crude material is a light, fluffy powder, the sublimation procedure was improved by putting a wad of glass wool over the crude material and below the cold section of the sublimation apparatus. Sublimation of 5 g requires about 1.5 hr. 

The basin A is then gently heated by a small Bunsen flame, which should be carefully protected from side draughts by screens, so that the material in A receives a steady uniform supply of heat. The material vaporises, and the vapour passes up through the holes into the cold funnel C. Here it cools and condenses as fine crystals on the upper surface of the paper B and on the walls of C. When almost the whole of the material in A has vaporised, the heating is stopped and the pure sublimed material collected. In using such an apparatus, it is clearly necessary to adjust the supply of heat so that the crude material in A is being steadily vaporised, while the funnel C does not become more than luke warm. 

Dissolve 1 g. of anthracene in 10 ml. of glacial acetic acid and place in 50 ml. bolt head flask fitted with a reflux water-condenser. Dissolve 2 g. of chromium trioxide in 2 ml. of water and add 5 ml. of glacial acetic acid. Pour this solution down the condenser, shake the contents of the flask and boil gently for 10 minutes. Cool and pour the contents of the flask into about 20 ml. of cold water. Filter off the crude anthraquinone at the pump, wash with water, drain well and dry. Yield, 1 g. Purify by re crystallisation from glacial acetic acid or by sublimation using the semi-micro sublimation apparatus (Fig. 35, p. 62, or Fig. 50, p. 70). 

The only disadvantage is that the procedure does not give accurate results if the compound sublimes the capillary tube method should be used in such cases, and it may be necessary to employ a sealed capillary tube. This apparatus should find a place in every laboratory. It is... 

The simplest form of apparatus consists of a small porcelain evaporating dish covered with a filter paper which has been perforated with a number of small holes a watch glass of the same size, convex side uppermost, is placed on the filter paper. The substance is placed inside the dish, and the latter heated with a minute flame on a wire gauze or sand bath. The sublimate collects in the Fig. II, 45, 1. watch glass, and the filter paper below prevents the sublimate from falling into the residue. The watch glass may be kept cool by covering it with several pieces of damp filter... 

A simple apparatus for sublimation in a stream of air or inert gas is shown in Fig. II, 45, 2.. 4 is a wide-necked conical flask provided with... 

A simple apparatus for sublimation in a stream of air or of inert gas is shown in Fig. II, 45, 3.. d is a two-necked flask equipped with a narrow inlet tube B with stopcock and a wide tube C 12-15 inm. in diameter. The latter is fitted to a sintered glass crucible and the usual adapter and suction flask E. A well-fitting filter paper is placed on the sintered glass filter plate to collect any sublimate carried by the gas stream. 

Sublimation under reduced pressure. The so-called vacuum sublimation may be carried out in the apparatus of Fig. II, 45, 4. The cold finger is fitted into the larger tube by means of a rubber stopper... 

Sublimation.—This is a valuable means for the purification of many organic substances and is admirably adapted for small scale work since losses are generally small. Sublimation may be carried out either at atmospheric pressure or under reduced pressure. The apparatus shown in Fig. XII, 2, 20 is simple and effective the sublimate is collected on the cold finger condenser. 

Thermal Printing. Thermal printing is a generic name for methods that mark paper or other media with text and pictures by imagewise heating of special-purpose consumable media. Common technologies are direct thermal thermal, ie, wax, transfer and dye-sublimation, ie, diffusion, transfer. Properties and preferred appHcations are diverse, but apparatus and processes are similar (87—89). 

The sublimation apparatus should have at least a 1-cm separation between the upper surface of the crude solid to be sublimed and the bottom of the cooling surface in order to avoid splattering of the oily residue onto the purified product near the end of the sublimation procedure. 

If the pump is a filter pump off a high-pressure water supply, its performance will be limited by the temperature of the water because the vapour pressure of water at 10°, 15°, 20° and 25° is 9.2, 12.8, 17.5 and 23.8 mm Hg respectively. The pressure can be measured with an ordinary manometer. For vacuums in the range lO" mm Hg to 10 mm Hg, rotary mechanical pumps (oil pumps) are used and the pressure can be measured with a Vacustat McLeod type gauge. If still higher vacuums are required, for example for high vacuum sublimations, a mercury diffusion pump is suitable. Such a pump can provide a vacuum up to 10" mm Hg. For better efficiencies, the pump can be backed up by a mechanical pump. In all cases, the mercury pump is connected to the distillation apparatus through several traps to remove mercury vapours. These traps may operate by chemical action, for example the use of sodium hydroxide pellets to react with acids, or by condensation, in which case empty tubes cooled in solid carbon dioxide-ethanol or liquid nitrogen (contained in wide-mouthed Dewar flasks) are used. 

Nickel (II) phthalocyanine [14055-02-8] M 571,3, m >300 , Wash well with H2O and boiling EtOH and sublime at high vacuum in a slight stream of C02. A special apparatus is used (see reference) with the phthallocyanine being heated to red heat. The sublimate is made of needles with an extremely bright red lustre. The powder is dull greenish blue in colour. [J Chem Soc 1719 7936.]... 

Rhoeadine crystallises from a mixture of chloroform and ether, sublimes at 215-25" /0-02 mm., and then melts at 256-57-5° (vac.), and has [a] / ° -f 232° (CHClj). According to Awe it has m.p. 272-4° (Kofler s micro-apparatus), and [a]] ° -f 243° (CHClj). A crystalline liydriodide, B. HI. 2H2O, was prepared by the addition of potassium iodide to a solution of the alkaloid in acetic acid. Rhoeadine contains one methoxyl group and a dioxymethylene group, but no reactive hydrogen (Zerewitinoff). 

When a solid compound possesses a relatively high vapor pressure below its melting point, it may be possible to purify it by sublimation. Selenium dioxide, for example, is easily purified prior to use by sublimation at atmospheric pressure (Chapter 1, Section XI). More commonly, the method of choice is sublimation at reduced pressure, which allows more ready evaporation of solids with limited volatility. A convenient vacuum sublimation apparatus is shown in Fig. A3.19. The impure sample is placed in the... 

A solution of dimethyl 3-acetyl-3-azatetracyclo[3.2.0.02-7.04 6]heptane-l,5-dicarboxylate (2, R1 = Ac R = H), formed by the photolysis (14 h 125-W Hg lamp under N2) of dimethyl 7-acetyl-7-azabicyclo-[2.2.1]hepta-2,5-diene-2,3-dicarboxylate (1 R1 = Ac, R2 = H 1 g, 4mmol) in Et20 (400 mL) at — 40 C, was evaporated to dryness under reduced pressure. The residue (0.7 g, 2.8 mmol) was dissolved in CHC1, and the solution heated under reflux for 1 h. Evaporation of the solvent yielded the crude product which was purified by column chromatography (silica gel, C,H2C12). The yellow fractions were collected and, after removal of the solvent, the residual oil was distilled in a sublimation apparatus to give 3 (R1 = Ac R2 = H) as a yellow oil yield 0.8 g (80%) bp 50 60 C/5 x 10 4 Torr. 

Vapor pressures of phases in these systems were measured by the Knudsen effusion technique. Use of mass spectrometer-target collection apparatus to perform thermodynamic studies is discussed. The prominent sublimation reactions for these phases below 2000 K was shown to involve formation of elemental plutonium vapor. Thermodynamic properties determined in this study were correlated with corresponding values obtained from theoretical predictions and from previous measurements on analogous intermetallics. 

Equilibrium vapor pressures were measured in this study by means of a mass spectrometer/target collection apparatus. Analysis of the temperature dependence of the pressure of each intermetallic yielded heats and entropies of sublimation. Combination of these measured values with corresponding parameters for sublimation of elemental Pu enabled calculation of thermodynamic properties of formation of each condensed phase. Previ ly reported results on the subornation of the PuRu phase and the Pu-Pt and Pu-Ru systems are correlated with current research on the PuOs and Pulr compounds. Thermodynamic properties determined for these Pu-intermetallics are compared to analogous parameters of other actinide compounds in order to establish bonding trends and to test theoretical predictions. 

Figure 1. Apparatus for the preparation of radical anions (11). On connection of the entire vessel to the vacuum system, traces of water and oxygen on the wall are removed by heating and discharging with a tesla coil. When the apparatus is filled with purified nitrogen through A, the weighed sample of the hydrocarbon is put into B through C, a piece of sodium is put into D, and dimethoxyethane is distilled into E, where a small amount of an Na-K alloy is added. After the system is again evacuated the solvent is distilled from E into B, the bulb E is,sealed off at F, and the sodium is sublimed to form a mirror on the wall of the bulb G. After tubes at C and H are sealed off, the apparatus is pumped to high vacuum for 1 hr and then sealed off at J. Then the solution of the hydrocarbon is poured from B into G. After a time varying from several minutes to several hours, a color is observed, and the sample is ready for optical and esr measurements.

If the material whose single crystal we want is volatile or sublimable, then we may choose a vapor-method of crystal growth. These methods have been used for a variety of crystals including ZnS and CdS. In this method, a carrier- gas is most often used for material transport and for the sulfides, H2S is the gas of choice. The following shows a simple apparatus ... 

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