Freeze vacuum

Heat, freezing, vacuum Addition of galenic excipients, supplements, stabilizers, and adjuvants... 

Freeze, vacuum, batch (conduction) drying temperature serum, -9 to -12 °C plasma, -20 to -25 °C penicillin -28 to -32 °C size vacuum pump to remove the water vapor avoid air leaks pressure 10 to 200 Pa or 1/4 to 1/2 the vapor pressure at the temperature 7-8 h drying cycle 2800 kj/kg water sublimated. Continuous ... 

All homo- and copolymers were synthesized by radical polymerization at 80 C for 4 hours using AIBN (2-4 mol% with respect to the total monomer amount) as radical initiator. The solvent used depended on the monomer sfMA-HlFl and sfMA-H2F4 were polymerized in chloroform, while sfMA-HlOFlO and sfMA-H2F8 copolymerizations with MMA required BFMB as solvent. The polymerizations were carried out under stirring in a two-necked Schlenk flask adapted to a Schlenk line after three freeze-vacuum thaw cycles in nitrogen atmosphere. After polymerization, the reaction mixture was diluted with BFMB/CHCI3 and precipitated into the 10-fold excess of methanol, filtered off, washed, and dried in a vacuum oven at 50°C. 

The crude o-phenylenediamine may be converted into the dihydrocliloride and the salt purified in the following manner. Dissolve it in 60 ml. of concentrated hydrochloric acid and 40 ml. of water containing 2 g. of stannous chloride, and treat the hot solution with 2-3 g. of decolourising carbon. Filter, add 100 ml. of concentrated hydrochloric acid to the hot colourless filtrate, and cool in a freezing mixture of ice and salt. Collect the colourless crystals of the dihydrochloride on a Buchner or sintered glass funnel, wash with a small volume of concentrated hydrochloric acid, and dry in a vacuum desiccator over sodium hydroxide. The yield is 61 g. 

It will be a little tricky but one can also try to purify by freezing I The sassafras oil is thrown into the freezer to chill. Safrole itself freezes at -14°C so anything that starts to freeze prior to that can be cold filtered in a prechilled vacuum filtration setup. The filtrate goes back in the freezer until -14°C is reached and the mother lode of safrole freezes up. This again is filtered cold but this time the frozen mass of safrole crystals are washed with some ice cold methanol or ethanol (preferably at -14°C) to wash away the unfrozen high-boiling constituents. 

Three generations of latices as characterized by the type of surfactant used in manufacture have been defined (53). The first generation includes latices made with conventional (/) anionic surfactants like fatty acid soaps, alkyl carboxylates, alkyl sulfates, and alkyl sulfonates (54) (2) nonionic surfactants like poly(ethylene oxide) or poly(vinyl alcohol) used to improve freeze—thaw and shear stabiUty and (J) cationic surfactants like amines, nitriles, and other nitrogen bases, rarely used because of incompatibiUty problems. Portiand cement latex modifiers are one example where cationic surfactants are used. Anionic surfactants yield smaller particles than nonionic surfactants (55). Often a combination of anionic surfactants or anionic and nonionic surfactants are used to provide improved stabiUty. The stabilizing abiUty of anionic fatty acid soaps diminishes at lower pH as the soaps revert to their acids. First-generation latices also suffer from the presence of soap on the polymer particles at the end of the polymerization. Steam and vacuum stripping methods are often used to remove the soap and unreacted monomer from the final product (56). 

Fig. 11. Flow diagram of the vacuum-freeze (direct) vapor-compression desalination process.

Extract is stored in insulated tanks prior to drying. Because high soluble soHds concentration is deskable to reduce aroma loss and evaporative load in the driers, most processors concentrate the 15—30% extract to 35—55% prior to drying (33). This may be accompHshed by vacuum evaporation or freeze concentration. Clarification of the extract, normally by centrifiigation, may be used to assure the absence of insoluble fine particles. 

Sublimation of ice crystals to water vapor under a very high vacuum, about 67 Pa (0.5 mm Hg) or lower, removes the majority of the moisture from the granulated frozen extract particles. Heat input is controlled to assure a maximum product end point temperature below 49°C. Freeze drying takes significantly longer than spray drying and requires a greater capital investment. 

Freeze drying has also been carried out at atmospheric pressure in fluid beds using circulating refrigerated gas. Vacuum-type vibrating conveyors, rotating multishelf dryers and vacuum pans can be used as can dielectric and microwave heating. 

Ultrafiltration (qv) (uf) is increasingly used to remove water, salts, and other low molecular-weight impurities (21) water may be added to wash out impurities, ie, diafiltration. Ultrafiltration is rarely used to fractionate the proteins because the capacity and yield are too low when significant protein separation is achieved. Various vacuum evaporators are used to remove water to 20—40% dry matter. Spray drying is used if a powdery intermediate product is desired. Tyophilization (freeze-drying) is only used for heat-sensitive and highly priced enzymes. 

Vacuum freeze. Usually used only See comments See comments See comments Expensive. UsuaUy See comments Applicable in spe- See comments... 

Use alternate drying method (ex. vacuum drying instead of atmospheric drying vacuum tray dryer, freeze drying, cryogenic CO2 drying, instead of vacuum rotary dryer) where material is subdivided in multiple locations... 

If the flow of cooling water is stopped while the apparatus is cold, the water may freeze and crack the immersion well. The vacuum jacket provides greater insurance against this problem than is available in the commercially available wells used with the usual 450 watt lamps. ... 

Conductivity grade benzonitrile (specific conductance 2 x 10" mho) was obtained by treatment with anhydrous AICI3, followed by rapid distn at 40-50° under vacuum. After washing with alkali and drying with CaCl2, the distillate was vac distd several times at 35° before being fractionally crystd several times by partial freezing. It was dried over finely divided activated alumina from which it was withdrawn as required [Van Dyke and Harrison J Am Chem Soc 73 402 7957]. 

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