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PREPARATION OF IODOFORM

Make a short abstract of these directions to use as a guide while doing


the work. Make a habit or preparing such abstract for all experiments.

Directions. In a 500cc Florence flask place 10g of iodine and pour onto
this 10g of aceton. Add in small portions, and with constant shaking, as much
as is needed of a solution made up of 200cc of 8N sodium hydroxide solution
and 80cc of water. If the flask become hot to the hand, cool it at once wit
running water. When sufficient sodium hydroxide solution has been added set
the flask aside. No free iodine should be present at this time, nor any
suggestion of brown color in the liquid. Look carefully on the bottom of the
flask for unattacked iodine.

After 5 minutes collect the yellow precipitate, using the small Buchner
funnel. Place filtrate at once in bottle labeled “ Iodoform filtrate.” Wash the
solid on the funnel whit a little water. The compound is then to be dissolved in
the smallest possible quantity of hot ethyl alcohol as follows. Put the iodoform
in the small flask arranged for refluxing ( see Expt.19 ). Pour a few cc or
alcohol down the condenser ( no flames within 6 ft ), and warm on electric hot-
plate or steam-bath, shaking the flask at times.

When the mix is warm add a little more alcohol, then wait till it
becomes hot to see whether enough has been added to dissolve all ( there will
always be a few shreds of filter paper, etc. which should not be mistaken for
iodoform ). Do not heat longer than necessary and avoid actual boiling if
possible.

When enough solvent ( about 40cc ) has been added to dissolve all the
iodoform at the boiling point of the solution, add about 2cc additional sovent,
then filter the hot solution through a fluted filter paper, using a funnel
previously warmed over the hot-plate or stean-bath.
Caution-do not inhale the vapor of solution.

Cover the filtered solution and set aside to cool slowly. In 15 minutes
add about 25cc of water, meanwhile stirring vigorously to completely
precipitate the iodoform, the filter with the Buchner funnel. Wash the crystals
on the funnel with a few drops of cold alcohol (cut off suction during the
washing ). Remove the crystals from the filter paper and spread the on a fresh,
dry piece of filter paper. The best way to remove paper, etc from Buchner
funnel is to hold it over a clean filter paper and blow gently through the stem.
The end of the funnel stem should first be washed so that no chemicals can get
on the lips. Any crystals remaining in the funnel are removed whit knife or
spatula. The crystals are to be placed in the desiccators. Place an identification
slip in the desiccators. Product in course of preparation should always be
labeled; do not rely on the memory.

The bottom of desiccators should contain granules of calcium chloride


to depth of about 15mm. the melting point and weight of the preparation will
be determinate after it is dry, at the next laboratory period. For directions for
melting point determinations Expt.4. submit the product in a sample bottle,
properly labeled ( see Expt. 18, p 46 ).