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Preparation of Bromine

Preparation of Bromine

by Magpie

12/10/09 Rev2

Introduction This procedure is for the preparation of ~25mL of Br2 using swimming pool grade NaBr, Rooto sulfuric acid, and 35% H2O2. The yield is very near theoretical.

The following oxidation-reduction reaction applies:

2NaBr + H2SO4 + H2O2 = Br2 + Na2SO4 + 2H2O

CAUTION Br2 is toxic, and some excess will be vented through the port on the vacuum adapter. Therefore this procedure must be conducted outside or in an efficient fume hood. (Note 1)

Do not spill any Br2 on your person. It will cause nasty and long-lasting burns.

Procedure

A. Reagent Preparation Weigh out 100g of NaBr in a beaker. Set aside.

In a 250mL beaker place 50mL of water. To the water carefully add, with stirring, 30mL of Rooto sulfuric acid (96wt%). The beaker should be cooled in a cold water (or ice water) bath during the addition of the acid. Set aside.

Have available 45mL of 35% H2O2 or an equivalent amount of aqueous H2O2 of a different strength.

B. Equipment Set-Up Using a 500mL round bottom flask (RBF) as pot and a 50mL RBF as receiver, set up for simple distillation. A pressure-equalizing addition funnel with sufficient capacity to hold the H2O2 solution is to be attached to the top port of the distillation adapter. All fittings are to be of ground-glass, coated with a thin film of silicone grease, and clamped.

Ice-water is to be supplied to the condenser. The receiver is to be placed in an ice-water bath. (The boiling point of Br2 is 59C.)

Heating is to be supplied with a 270w Glas-Col mantle (or equivalent) placed on top of a magnetic stirrer. Place a stir-bar in the 500mL RBF pot.

C. Distillation Temporarily remove the 500mL pot from the apparatus and add the acid prepared above. Using a powder funnel, add, with magnetic stirring, the

weighed out NaBr. Replace the pot in the apparatus. Keep the stir bar in operation to provide good mixing.

Connect the pressure-equalizing funnel to the top of the distillation adapter (valve closed!). Add the H2O2 solution prepared above to the pressure equalizing funnel and install its plug in the fill port.

Turn on the cooling water. Set the heating mantle at 60% and turn on. If using a hood, turn on the fan.

WARNING Be very careful when adding the hydrogen peroxide, as an uncontrollable reaction can result if too much hydrogen peroxide is in the mixture. HEAT AT 80 'C , ONE DROP OF H2O2/ 1-2 sec. nicely... everything is going

-MIGHT WANT TO USE A VIGREUX COLUMN TO MIN. THE LOSS OF Br2 When the pot has reached a temperature sufficient to support the reaction add the H2O2 solution a few drops at a time, keeping the reaction under control. A steady generation of Br2 will follow. The reaction is exothermic and the heating mantle power should be turned down as the pot heats up. By not overheating, the loss of Br2 via the vacuum adapter port will be minimized.

Continue the distillation after all the H2O2 solution has been added until the generation of Br2 has nearly stopped. There should be ~25mL of Br2 in the receiver.

Drying the Br2 The liquid Br2 will be wet with some water, much of it floating on the surface. This can be removed by shaking it with con sulfuric acid in a separatory funnel that has been pre-cooled in the freezer. The heavier bromine (sp. gr. = 3.12) is drained off the bottom of the separatory funnel.

Storage A narrow necked glass bottle with a PTFE lined cap is suitable for storage. Keeping it in a freezer will minimize any leakage.

Notes 1. SM forum member "not_important" has suggested that the fugitive Br2 escaping at the vacuum adapter port can be safely captured by bubbling it into a solution of NaOH, KOH, warm Na2CO3, or warm K2CO3. For example: 3 Br2 + 6 KOH => 5 KBr + KBrO3 + 3 H2O 2. The H2SO4 is in 14% excess. 3. The H2O2 is in 8% excess.

Reference This procedure is based on the recommendations of benzylchloride1 of the ScienceMadness forum.

Photos Photos will follow when available. In their stead is the following photo taken during the production of Br2 using a less efficient procedure.

[Edited on 7-12-2009 by Magpie]