Apparatus, assembling drying

D. 4a(S),8a(R)-2-Benzoyloctahydro-6(2H)-isoquinolinone (4). Palladium (Pd), 10% on carbon, 4.0 g, (Note 21) is placed in a 500-mL Parr bottle under N2 and carefully wetted with 50 mL of cold denatured ethanol (EtOH). A slurry of 34.7 g of enone 3 (0.14 mol) in denatured EtOH (250 mL) is added and the Parr shaker apparatus assembled. After the system is purged with nitrogen-hydrogen (N2/H2), the reaction is shaken at 50 psi H2 and 50°C until H2 uptake is complete (1 hr, Note 22). The catalyst is filtered over a Celite pad (Note 23) and rinsed with warm chloroform (CHCI3) (4 x 75 mL). The filtrate is concentrated under reduced pressure, dissolved in 90 mL of CH2CI2 and crystallized with 200 mL of hexanes. The crystalline solid is filtered, rinsed with hexanes and dried to afford 34.3 g (98%, Note 24) of the ketone 4, representing a 51% yield over four steps. 

The glass components of the apparatus were dried overnight in a 150°C-oven and allowed to cool in a desiccator over a drying agent before assembly. 

All glass apparatus is dried in an oven at 100°C and assembled while still hot under dry nitrogen flow. All ground glass joints are tightly sealed with a Teflon tape and then wrapped with parafilm. 

Research effort at Albany International Research Co. has developed unit processes necessary for pilot scale production of several species of reverse osmosis hollow fiber composite membranes. These processes include spin-dope preparation, a proprietary apparatus for dry-jet wet-spinning of microporous polysul-fone hollow fibers, coating of these fibers with a variety of permselective materials, bundle winding using multifilament yarns and module assembly. Modules of the membrane identified as Quantro II are in field trial against brackish and seawater feeds. Brackish water rejections of 94+% at a flux of 5-7 gfd at 400 psi have been measured. Seawater rejections of 99+% at 1-2 gfd at 1000 psi have been measured. Membrane use requires sealing of some portion of the fiber bundle for installation in a pressure shell. Much effort has been devoted to identification of potting materials which exhibit satisfactory adhesion to the fiber while... 

The apparatus is dried in an oven and assembled under dry nitrogen. Alternatively it can be flamed dry in a stream of dry nitrogen. A magnetic stirrer can be utilized for small scale experiments. 

The glass components of the apparatus are dried overnight in a 120°C oven and then assembled and maintained under an atmosphere of nitrogen during the course of the reaction. 

Preparation of Sodium Bisulphide. Assemble an apparatus as shown in Fig. 66. Fill drying columns 4 with. phosphorus(V) oxide placed on glass wool. Weigh 2-2.5 g of metallic sodium, wash it with benzene and diethyl ether, thoroughly remove the oxide film from its surface, cut the sodium up into small pieces, and put them into test tube 2. Pour 75 ml of absolute ethanol into 150-200-ml round-bottomed flask 1. Fill the apparatus with dry argon (nitrogen) via tube 3. 

Preparation of Phosphorus Trichloride and Pentachloride. This experiment is performed by two students in a fume cupboard Assemble an apparatus as shown in Fig. 96. Put 0.2 g of dry red phosphorus into each of Wurtz test tubes 1 and 2. See that the lower ends of gas-discharge tubes 3 feeding chlorine into reaction tubes 1 and 2 are 2-3 cm above the phosphorus layer. Displace air from the apparatus using dry carbon dioxide gas, and then fill it with dry chlorine... 

Assemble an apparatus as shown in Fig. 102. Lubricate the ground-glass joints with phosphoric acid. Fill the apparatus with dry carbon dioxide using offtake 2. Pour 10 ml of dry carbon disulphide from dropping funnel 3 into flask 1. 

A 1-1. three-necked flask is equipped with a mercury-sealed stirrer, an inlet tube, and a reflux condenser which is connected through a soda-lime tube to a gas-absorption trap.1 The apparatus is dried in an oven and assembled rapidly to exclude moisture it is advisable to set up the apparatus in a hood to vent ammonia which may escape by accident. The flask is cooled in a Dry Ice-trichloroethylene bath, and 200 ml. of anhydrous (refrigeration grade) ammonia is introduced through the inlet tube from an ammonia cylinder which is either inverted or equipped with a siphon tube. Just before the apparatus is assembled, 8.1 g. (0.35 gram atom) of sodium is cut, weighed, and kept under kerosene in a small beaker. The Dry Ice bath is removed, the inlet tube is replaced by a rubber stopper, and a crystal of hydrated ferric nitrate (about 0.2 g.) is added. A small (about 5-mm.) cube of the sodium is cut, blotted rapidly with filter paper, and added quickly to the liquid ammonia. The solution is stirred until the blue color disappears, after which the remainder of the sodium is added in narrow, thin strips about as rapidly as... 

The various pieces of apparatus are dried in an oven and assembled rapidly in order to exclude moisture. 

Assemble the apparatus as shown in Fig. 5.3. Do not forget the water cooling of the stirrer guide and of the addition funnels. Flush the apparatus with dry nitrogen for 10 min. 

Clean all the glassware and other apparatus, and dry in an 120°C oven for at least 4 h before use. Assemble glassware while still hot. 

---