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Purification of formaldehyde

Started by Rhodium, October 31, 2002, 02:13:00 AM

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Rhodium

An old bottle of formaldehyde of unknown concentration, with 1 cm of precipitate at the bottom, can this be distilled or something to get 37% formaldehyde solution?

SPISSHAK

Or polymerization, heat it and see if it dissolves.
I'm not sure exactly under what conditions formaldehyde floculates but It's a guess.

Rhodium

It will probably redissolve with heating, but the concentration is unknown, I'd like to make sure I have a 37% solution.

The conditions under which my bottle flocculated was by prolonged storage at 5-10°C.

SPISSHAK

Other than specific gravity, or by seperating the two, I think a certain percentage of methanol is added to formalin solutions to keep it from doing this so it probably is spontaneous.
If you heat it to much you'd either A: distill off the methanol
B: the methanol would condense on the formaldehyde and produce Methylal.
During this process the paraformaldehyde would depolymerize by reaction with water.
Depending on what extent you heat it to.

lugh

Paraformaldehyde is formed when formaldehyde solution is evaporated, it's probably what's on the bottom  :)  When paraformaldehyde is heated with a large quantity of water, it's reconverted into formaldehyde  :)

Rhodium

How can I determine the concentration? Or perhaps I should rather heat a known weight of paraformaldehyde with water instead?

lugh

The specific gravity of formaldehyde is 1.075-1.1081  :)  You could calculate the percentage of a solution prepared from heating paraformaldehyde in a large quantity of water to that to determine your concentration  :)  The aqueous solution boils at 98°C, the boiling point of the gas is -21°C  :)

b159510

How can I determine the concentration

iodimetric titration, after 5 minutes add hydrochloric acid and back titrate with na-thiosulfate.

or like you said, mix up a new batch, which would probably be easier if you don't have a standardized triiodide solution already made.


You don't fool me, Oilman

b159510

Paraformaldehyde is formed when formaldehyde solution is evaporated...

I've dissolved paraformaldehyde in water, but never evaporated the solution. Isn't that how trioxymethylene is formed? (aka metaformaldehyde, 1,3,5-trioxane)
You don't fool me, Oilman

lugh

Yes, as posted in

Post 209590 (missing)

(lugh: "Re: Acquiring Acetaldehyde OTC", Chemicals & Equipment)
 :)  Triformol is the trimer, paraformaldehyde is the hexamer, which melts at 171°C  :)

b159510

The titration I mentioned should still work for an aqueous solution of formaldehyde, even though that isn't the species that actually exists.
(What is that called, methanediol?)
You don't fool me, Oilman