Semimicroscale Preparation of Anhydrous Nitric Acid

Anhydrous nitric acid (HNO3) is prepared by the following procedure. 

CAUnON The reagents and the product of this preparation are highly corrosive. The distillation must be conducted in a hood. Appropriate gloves are strongly suggested. Prevent contact with eyes, skin, and clothing. Any spill should be neutralized using solid sodium carbonate or bicarbonate. 

Use this anhydrous nitric acid immediately for the nitration experiments given below. The amount obtained at the scale used here is sufficient for the preparation of two of the nitro compounds described in this experiment. 

Reagents and Equipment. Using two clean, dry 1.0-mL graduated pipets, add 0.7 mL of concentrated nitric acid, followed by 1.0 mL of concentrated sulfuric acid, to a 10-mL round-bottom flask containing a boiling stone. Swirl the flask gently to mix the reagents. Attach the flask to a Hickman still fitted with an air condenser (- ). 

NOTE It is useful to invert a 10-mL beaker over the air condenser to help contain 

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