Powders, evacuation

In the flask were succesively placed 0.10 mol of the sulfinate (note 2), 25 ml of dry, pure HMPT (note 3), 4 g of powdered sodium iodide, 40 g of zinc dust and some boiling stones. After swirling for a few seconds the flask was connected with the other parts of the distillation apparatus, the system was evacuated immediately by means of the water pump (note 4) and the flask was then heated cautiously (free flame). A vigorous reaction started suddenly and the cumulene and part of the HMPT passed over. When the distillation had stopped completely... 

The fluid plasticizer (solvent) consists of an energetic compound, eg, nitroglycerin, an inert carrier, and a stabilizer. The system is evacuated to remove volatiles, moisture, and air, and the plasticizer is then pressurized and passed slowly upward through the powder bed while the powder is held stationary by a pressure plate on the powder column. Casting solvent may also be added from the top of the mold. 

Chromium (II) also forms sulfides and oxides. Chromium (II) oxide [12018-00-7], CrO, has two forms a black pyrophoric powder produced from the action of nitric acid on chromium amalgam, and a hexagonal brown-red crystal made from reduction of Cr202 by hydrogen ia molten sodium fluoride (32). Chromium (II) sulfide [12018-06-3], CrS, can be prepared upon heating equimolar quantities of pure Cr metal and pure S ia a small, evacuated, sealed quartz tube at 1000°C for at least 24 hours. The reaction is not quantitative (33). The sulfide has a coordination number of six and displays a distorted octahedral geometry (34). 

This technique is based on the Dewar flask, which is a donble-walled vessel with reflective surfaces on the evacuated side to reduce radiation losses. Figure 11-66 shows a typical laboratory-size Dewar. Figure 11-67 shows a semiportable type. Radiation losses can be further reduced by filling the cavity with powders such as perlite or silica prior to pulling the vacuum. 

Powder Insulation A method of reahzing some of the benefits of multiple floating shields without incurring the difficulties of awkward structural complexities is to use evacuated powder insulation. The penalty incurred in the use of this type of insulation, however, is a tenfold reduction in the overall thermal effectiveness of the insulation system over that obtained for multilayer insulation. In applications where this is not a serious factor, such as LNG storage facihties, and investment cost is of major concern, even unevacuated powder-insulation systems have found useful apphcations. The variation in apparent mean thermal conductivity of several powders as a function of interstitial gas pressure is shown in the familiar S-shaped curves of Fig. 11-121. ... 

Foam Insulation Since foams are not homogeneous materials, their apparent thermal conductivity is dependent upon the bulk density of tne insulation, the gas used to foam the insulation, and the mean temperature of the insulation. Heat conduction through a foam is determined by convection and radiation within the cells and by conduction in the solid structure. Evacuation of a foam is effective in reducing its thermal conductivity, indicating a partially open cellular structure, but the resulting values are stiU considerably higher than either multilayer or evacuated powder insulations. 

The 213 g. (0.8 mole) of finely powdered silver salt is placed in a 1-1. three-necked flask (Note 3) two necks of the flask are stoppered, and the third is connected to a water pump through a U-tube or flask containing Drierite. The flask is then placed in an oil bath and evacuated to a pressure of about IS mm. The temperature of the oil bath is maintained at 100-110 for 36 hours (Notes 4 and S). 

In preparing any of the above for use in columns, the dry powder is evacuated, then mixed under reduced pressure with water or the appropriate buffer solution. Alternatively it is stirred gently with the solution until all air bubbles are removed. Because some of the wet powders change volumes reversibly with alteration of pH or ionic strength (see above), it is imperative to make allowances when packing columns (see above) in order to avoid overflowing of packing when the pH or salt concentrations are altered. 

Citrazinic acid (2,6-dihydroxyisonicotinic acid) [99-11-6] M 155.1, m >300°, pK] 3.0, pK2 4.76. Yellow powder with a greenish shade, but is white when ultra pure and turns blue on long standing. It is insoluble in H2O but slightly soluble in hot HCl and soluble in alkali or carbonate solutions. Purified by precipitation from alkaline solutions with dilute HCl, and dry in a vacuum over P2O5. The ethyl ester has m 232° (evacuated tube) and a pKa of 4.81 in MeOCH2CH20H [IR Pitha Coll Czech Chem Comm 28 1408 1963]. 

Graphite [7782-42-5]. Treated with hot 1 1 HCl. Filtered, washed, dried, powdered and heated in an evacuated quartz tube at 1000° until a high vacuum was obtained. Cooled and stored in an atmosphere of helium [Craig, Van Voorhis and Bartell 7 Phys Chem 60 1225 1956]. 

Thermal insulation is available over a wide range of temperatures, from near absolute zero (-273 C) ( 59.4°F) to perhaps 3,(1()0°C (5,432°F). Applications include residential and commercial buildings, high- or low-temperature industrial processes, ground and air vehicles, and shipping containers. The materials and systems in use can be broadly characterized as air-filled fibrous or porous, cellular solids, closed-cell polymer foams containing a gas other than air, evacuated powder-filled panels, or reflective foil systems. 

More advanced insulations are also under development. These insulations, sometimes called superinsulations, have R that exceed 20 fthh-°F/Btu-m. This can be accomplished with encapsulated fine powders in an evacuated space. Superinsulations have been used commercially in the walls of refrigerators and freezers. The encapsulating film, which is usually plastic film, metallized film, or a combination, provides a barrier to the inward diffusion of air and water that would result in loss of the vacuum. The effective life of such insulations depends on the effectiveness of the encapsulating material. A number of powders, including silica, milled perlite, and calcium silicate powder, have been used as filler in evacuated superinsulations. In general, the smaller the particle size, the more effective and durable the insulation packet. Evacuated multilayer reflective insulations have been used in space applications in past years. 

A reaction vessel as shown in Fig. 1 is made from Pyrex tubing (Note 1). The vessel is evacuated and the stopcock closed. A 500-ml. round-bottomed two-necked flask equipped with a gas inlet and a cold finger condenser containing dry ice is charged with 1 g. of finely powdered 4,4 -bis(dimethylamino)benzophenone... 

A mixture of Nd(OAc)3 (0.21 g, 1 mmol) and 4-/er/-hutylphthalonitriIe (7 1.47 g, 8 mmol) was fused in an evacuated glass ampule with gradual raising of the temperature to 290 JC and this temperature was then maintained for 2 h. The cooled melt was ground and purified by column chromatography (alumina, benzene) to ohtain a blue powder yield 1.03 g (60%). 

For food and pharmaceutical applications, the microbial count must be reduced to less than 10,000 viable cells per g exopolysaccharide. Treatment with propylene oxide gas has been used for reducing the number of viable cells in xanthan powders. The patented process involves propylene oxide treatment for 3 h in a tumbling reactor. There is an initial evacuation step before propylene oxide exposure. After treatment, evacuation and tumbling are alternated and if necessary the reactor is flushed with sterile nitrogen gas to reduce the residual propylene oxide level below the Food and Drug Administration permitted maximum (300 mg kg 1). The treated polysaccharide is then packaged aseptically. 

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