Nitric Acid Bath

This method is to be used when a primer or surface coating is applied.  

Immerse for 10 min in coating bath of 1.0 g purified stearic acid dissolved in 95—99 mL of acetone and 1—5 mL of nitric acid 

Store in distilled water in a polyethylene bottle at60°C 

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Salpetersaure. /. nitric acid, -anhydrid, n. nitric anhydride, (di)nitrogen pentoxide, nitrogen(V) oxide, -ather, m. nitric ether (ethyl nitrate), -bad, n. nitric acid bath, -dampf, m. nitric acid vapor or fume. 

A titanium-containing sludge from a nitric acid bath was separated, before completely dry it exploded, killing a workman. Investigation showed the dry sludge to be a powerful explosive sensitive to heat, friction and impact, composed of about 60 40 silver nitrate titanium. 

CERNOX [Ceramic NOx] A process for destroying NOx by reaction with ammonia, catalyzed by a zeolite. Developed by Steuler Industrie Werke in the 1950s for treating vapors from nitric acid baths used for pickling stainless steel. The zeolite was developed for this process by Mobil Corporation and is still proprietary. The process was introduced to the market in 1982, and by 1988 100 units had been installed in Europe alone. 

Glassware is cleaned by soaking it overnight in a coned nitric acid bath. 

Caution. TeCU is highly toxic as well as hygroscopic. Consequently, reactions should be carried out in an efficient fume hood. Reaction vessels that come in contact with tellurium compounds are rinsed with water first (fume hood), the washings are combined in a beaker, and concentrated nitric acid is added the next day. The water-rinsed reaction vessels are placed into a concentrated nitric acid bath for 24 h before final cleaning. 

Acid wash all glass, Teflon, and plastic vessels by soaking them in a nitric acid bath containing a 4 1 solution of watermi-tric acid. After acid soaking, rinse acid-washed items in deionized water, dry them, and store themin clean, covered cabinets. 

About 0.5 g of iodine is placed in a small flask fitted with a long reflux air condenser and 15 cm of fuming nitric acid (b.p. 380 K) are added. The mixture is then heated on a water bath at 385-390 K in a fume cupboard until the reaction seems to be complete. This takes about an hour. The solution is then transferred to an evaporating basin and evaporated to dryness on a steam bath. The iodic acid... 

Procedure for Bromine and Iodine Estimations. Again cover the beaker as before, but before adding the nitric acid add i g. of hydrazine sulphate and heat the solution on the water-bath until evolution of gas ceases. To ensure complete decomposition of an iodate, however, the heating should be continued for i hour. 

Place 18 g. (12 ml.) of fuming nitric acid, sp. gr. 1 5, and 30 g. (16-5 ml.) of concentrated sulphuric acid and a few fragments of broken glass in a 250 or 500 ml. round-bottomed flask. Add gradually, in small portions, 14 g. of p-nitrotoluene do not allow the temperature to rise above 50 and cool the flask, if necessary, by immersion in cold water. Place a small funnel in the mouth of the flask and heat on a water bath at 90-95° for 30 minutes. Allow to cool almost to the laboratory temperature and pour the reaction mixture slowly into about 500 ml. of ice water containing a few small pieces of ice. Filter the crude dinitrotoluene through a Buchner funnel at the pump, wash it thoroughly with cold water, and drain as completely as possible. RecrystalUse from the minimum volume of hot methyl alcohol (flask, reflux condenser, and water bath experimental details as in Section IV,12). The yield of pure 2 4-dinitrotoluene, m.p. 71°, is 12 -5 g. 

Equip a 500 ml. three necked flask with a reflux condenser, a mercury-sealed mechanical stirrer and separator funnel, and support it on a water bath. Attach an absorption device (Fig. II, 8, 1, c) to the top of the condenser (1). Place 134 g. (152 ml.) of A.R, benzene and 127 g. of iodine in the flask, and heat the water bath to about 50° add 92 ml. of fuming nitric acid, sp. gr. 1-50, slowly from the separatory funnel during 30 minutes. Oxides of nitrogen are evolved in quantity. The temperature rises slowly without the application of heat until the mixture boils gently. When all the nitric acid has been introduced, reflux the mixture gently for 15 minutes. If iodine is still present, add more nitric acid to the warm solution until the purple colour (due to iodine) changes to brownish-red. 

Add 1 g. of the compound to 4 ml. of concentrated sulphuric acid and cautiously introduce, drop by drop, 4 ml. of fuming nitric acid. Warm the mixture on a water bath for 10 minutes, then pour it on to 25 g. of crushed ice (or 25 ml. of ice water). Collect the precipitate by filtration at the pump, and recrystallise it from dilute alcohol. 

Method 1. Place 20 g. of crude benzoin (preceding Section) and 100 ml. of concentrated nitric acid in a 250 ml. round-bottomed flask. Heat on a boiling water bath (in the fume cupboard) with occasional shaking until the evolution of oxides of nitrogen has ceased (about 1 -5 hours). Pour the reaction mixture into 300-400 ml. of cold water contained in a beaker, stir well until the oil crystallises completely as a yellow solid. Filter the crude benzil at the pump, and wash it thoroughly with water to remove the nitric acid. RecrystaUise from alcohol or methylated spirit (about 2-5 ml. per gram). The yield of pure benzil, m.p. 94-96°, is 19 g. 

Methyl m-nitrobenzoate. In a 1 htre round-bottomed or bolt-head flask, fitted with a mechanical stirrer, place 102 g. (94 ml.) of pure methyl benzoate (Section IV,176) support a separatory funnel containing a mixture of 62 -5 ml, of concentrated sulphuric acid and 62 -5 ml. of concentrated nitric acid over the mouth of the flask. Cool the flask in an ice bath to 0-10°, and then run in the nitrating mixture, with stirring. 

Method 2. This preparation should be carried out in the fume cupboard since nitrous fumes are evolved. Place 62 g. of benzoic acid and 300 ml. of concentrated sulphuric acid in a 2-litre roimd-bottomed flask, warm on a water bath with shaldng until the benzoic acid dissolves, and cool to 20°. Add 100 ml. of fuming nitric acid (sp. gr. 1-54) in portions... 

Purification of charcoal. Heat Norit charcoal on a water bath for 6 hours with 10 per cent, nitric acid, filter, wash free from acid, and dry at 100°. If the acid-washed form of Norit charcoal is available, it may be used directly without further purification. 

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