decomposes at 313 °C
TNO stands for 2,4,2,4-tetranitro-oxanilide. This substance is fairly stable, being able to resist shock, friction, and heat. It is primarily used as a component in pyrotechnical devices or in gunpowder formulations. It was first prepared in 1892 when A.G. Perkins heated oxanilide powder in nitric acid. I believe this lab procedure hails from an anonymous work in 1971.
|acetone||500-mL Florence flask|
|ethyl alcohol||graduated cylinder|
|nitric acid||stirrer/stirring rod|
Measure out 100 mL of 98% nitric acid into a round bottomed 500-mL Florence flask. Place the flask into a salt-ice bath to provide cooling. While stirring rapidly, slowly add 50 g of oxanilide while the temperature is maintained below 40 °C. After the addition of the oxanilide is completed (addition should take 2.5-3 hours), the agitation is continued for 10-15 minutes. The flask is now transferred to a water bath where the temperature is then raised to 80 °C over a period of 1 hour and maintained at 80-85 °C for 3 hours. The acid slurry is then cooled to room temperature and drowned by pouring over cracked ice. The product is filtered on a Buchner funnel and washed with water until it is almost acid free. The filter cake is placed in a beaker and sufficient water added to form a slurry. Steam is run into the slurry under agitation for 10 minutes. The slurry is filtered and the residue washed. The latter treatment of the slurry is repeated until the wash water is found to be neutral to litmus paper. The TNO is washed with ethyl alcohol, then acetone, dried in the air, and finally dried at 100-110 °C. Yield is 90-97% of the theoretical. You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to monitor the temperature.
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