Nitration centrifugal

Assay preparation Transfer an accurately weighed portion of topical powder, equivalent to about 20 mg of miconazole nitrate, to a stoppered 50-mL centrifuge tube. Add 25 mL of methanol, and shake by mechanical means for 30 min to dissolve the miconazole nitrate. Centrifuge to obtain a clear supernatant liquid. Transfer 5 mL of this solution to a test tube, add 2 mL of Internal standard solution and evaporate at a temperature not higher than 40 °C with the aid of a current of nitrogen to dryness. Dissolve the residue in 2 mL of a mixture of chloroform and methanol (1 1). 

Fig. 137. Diagram of a nitration centrifuge of Selwig and Lange, according to Pascal [14].

Fig. 139. General view of nitration centrifuges. Discharge of nitrocellulose with aluminium forks (Bofors Nobelkrut, Sweden).

Ma.nufa.cture. The batch nitration processes for nitrocellulose have included the pot process, the centrifugal process, the Thompson displacement process, and the mechanical dipper process. Semicontinuous nitration processes are also widely used for military and industrial grades. 

Centrifugal separators are used in many modem processes to rapidly separate the hydrocarbon and used acid phases. Rapid separation greatly reduces the amounts of nitrated materials in the plant at any given time. After an explosion in a TNT plant (16), decanters (or gravity separators) were replaced with centrifugal separators. In addition, rapid separation allows the hydrocarbon phase to be quickly processed for removal of the dissolved nitric acid, NO, etc. These dissolved materials lead to undesired side reactions. The organic phase generally contains some unreacted hydrocarbons in addition to the nitrated product. 

The rate (kinetics) and the completeness (fraction dissolved) of oxide fuel dissolution is an inverse function of fuel bum-up (16—18). This phenomenon becomes a significant concern in the dissolution of high bum-up MO fuels (19). The insoluble soHds are removed from the dissolver solution by either filtration or centrifugation prior to solvent extraction. Both financial considerations and the need for safeguards make accounting for the fissile content of the insoluble soHds an important challenge for the commercial reprocessor. If hydrofluoric acid is required to assist in the dissolution, the excess fluoride ion must be complexed with aluminum nitrate to minimize corrosion to the stainless steel used throughout the facility. Also, uranium fluoride complexes are inextractable and formation of them needs to be prevented. 

By contrast, HLW from LWR fuel reprocessing is stored ia cooled, well-agitated, stainless steel tanks as an acidic nitrate solution having relatively few sohds. Modem PUREX flow sheets minimise the addition of extraneous salts, and as a result the HLW is essentially a fission-product nitrate solution. Dissolver soHds are centrifuged from the feed stream and are stored separately. Thus the HLW has a low risk of compromising tank integrity and has a favorable composition for solidification and disposal (11). 

The manufacture of silver nitrate for the preparation of photographic emulsions requires silver of very high purity. At the Eastman Kodak Company, the principal U.S. producer of silver nitrate, 99.95% pure silver bars are dissolved in 67% nitric acid in three tanks coimected in parallel. Excess nitric acid is removed from the resulting solution, which contains 60—65% silver nitrate, and the solution is filtered. This solution is evaporated until its silver nitrate concentration is 84%. It is then cooled to prepare the first crop of crystals. The mother Hquor is purified by the addition of silver oxide and returned to the initial stages of the process. The cmde silver nitrate is centrifuged and recrystallized from hot, demineralized water. Equipment used in this process is made of ANSI 310 stainless steel (16). 

Barium nitrate is prepared by reaction of BaCO and nitric acid, filtration and evaporative crystallization, or by dissolving sodium nitrate in a saturated solution of barium chloride, with subsequent precipitation of barium nitrate. The precipitate is centrifuged, washed, and dried. Barium nitrate is used in pyrotechnic green flares, tracer buUets, primers, and in detonators. These make use of its property of easy decomposition as well as its characteristic green flame. A small amount is used as a source of barium oxide in enamels. 

Sodium fluoroborate [13755-29-8] M 109.8, m 384 , d 2.47, pK -4.9 (for fluoroboric acid H30 BF4 ). Crystd from hot water (50mL/g) by cooling to 0 . Alternatively, purified from insoluble material by dissolving in a minimum amount of water, then fluoride ion was removed by adding cone lanthanum nitrate in excess. After removing lanthanum fluoride by centrifugation, the supernatant was passed... 

On the completion of nitration the batch is dropped from the reaction vessel into a centrifuge and the acid mixture spun off and recovered. The nitrated linters, which still contain appreciable quantities of acid, are then plunged into a drowning tank, where the nitric acid is diluted with a large volume of water. The resultant ester is then pumped, as a slurry, into storage vats which may hold the products of several nitrations. 

The stabilised nitrate may then be bleached with sodium hypochlorite, centrifuged to remove much of the water in which the polymer has been slurried and dehydrated by displacement with alcohol while under pressure in a press. It is interesting to note that in these processes approximately 35 000 gallons (160000 litres) of water are used for every ton of cellulose nitrate produced. Control of purity of the water is important in particular the iron content should be as low as 0.03 parts per million since iron can adversely affect both the colour and heat stability of the polymer. 

Fertilisers For nitrates, non-molybdenum austenitic steels are satisfactory, but in the manufacture of ammonium sulphate some free acid is often present, so that evaporators and centrifugal dryer baskets in this case are generally made from molybdenum-bearing steels. For super-phosphates this has limited application. 

Flow-sheet of Injector Nitration of Glycerin and Centrifugal Separation of... 

It is obvious that the nitrated product must be separated from the acid in equil with it (spent acid). If the product and the spent acid form two immiscible liq phases, eg, NG, EGDN, or molten TNT, separation is effected by gravity or centrifuging. If the product and spent acid form a solid and a liq phase, eg PA, NC or PETN, separation is effected by centrifuging (PA NC) or filtration (PETN). If the nitration is carried in the vapor phase (NM), separation is effected by distillation... 

The centrifugal separator used in conjunction with the tubular nitrator is described in two patents (Refs 53 64)... 

Preparation. It is prepd by dissolving pure Sr nitrate in an excess of perchloric ac, the excess ac neutralized with Sr carbonate, all solids centrifuged off, and the soln chilled until crysts appear (Ref 2). The anhyd salt can also be prepd by drying the hydrate at 250°, yield 50% (Ref 3) or the addn of anhyd perchloric ac to a soln of Sr ion in anhyd trifluoroacetic ac, the pptd solid filtered, and the excess acid removed in a vacuum (Ref 7)... 

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