Members of the previous forum can retrieve their temporary password here, (login and check your PM).

Reply to thread

Message

There certainly wasn't any quantitative data from the start of the experiment, so really it would only be fair to call it an inference based on the observation of the solution going a paler yellow from a deeper orange colouration, kind of a reverse of the colour change seen when DMT oxidises/is thought to oxidise.

As stated in the method it was a curdy white precipitate.

Quite possibly yes, although some basic level of analysis would be required to state that it was exclusively sodium fumarate. The moist IPA will certainly have contained some sodium ions, probably as carbonate - although when I discussed this matter recently I was told that the sodium carbonate had been made from sodium bicarbonate and a bit of extra sodium hydroxide had been added to the solution as there were concerns about the completeness of the conversion. So there was in all likelihood a bit of hydroxide present the solution, too. The precipitate could in all likelihood contain a trace or more of DMT.

Come to think of it, could IPA possibly extract NaOH preferentially from a mixture with Na2CO3?

That's probably another reason why it was stored in the fridge, besides attempting to encourage crystallisation; the reduction occured (or appeared to occur) when the mixture was heated on the hot water bath.

The rationale behind the reduction phase of this experiment was knowing that ascorbic acid is more rapidly oxidised at alkaline pH (so I'm told). Therefore ascorbic acid must be a more effective reducing agent at higher pH.

And remember, dear people, besides the interesting lightening of the orange colour to a yellow shade by heating known-to-be-oxidised DMT in alkaline solution with ascorbic acid, the other interesting observation (IMHO) was how the orange/yellow colouration of used limonene could be removed by washing with basic - i.e. alkaline - aqueous (wet) IPA.

I would suggest a final step, after ensuring that all precipitates have precipitated, is rebasification of the precipitate and extraction into anhydrous acetone or IPA.

Let's see how long that takes :lol:

EDIT: Maybe a last blast FASA on the limo too?

<blockquote data-quote="downwardsfromzero" data-source="post: 3687778" data-attributes="member: 1025">There certainly wasn&#039;t any quantitative data from the start of the experiment, so really it would only be fair to call it an inference based on the observation of the solution going a paler yellow from a deeper orange colouration, kind of a reverse of the colour change seen when DMT oxidises/is thought to oxidise.As stated in the method it was a curdy white precipitate.Quite possibly yes, although some basic level of analysis would be required to state that it was exclusively sodium fumarate. The moist IPA will certainly have contained some sodium ions, probably as carbonate - although when I discussed this matter recently I was told that the sodium carbonate had been made from sodium bicarbonate and a bit of extra sodium hydroxide had been added to the solution as there were concerns about the completeness of the conversion. So there was in all likelihood a bit of hydroxide present the solution, too. The precipitate could in all likelihood contain a trace or more of DMT.Come to think of it, could IPA possibly extract NaOH preferentially from a mixture with Na2CO3?That&#039;s probably another reason why it was stored in the fridge, besides attempting to encourage crystallisation; the reduction occured (or appeared to occur) when the mixture was heated on the hot water bath.The rationale behind the reduction phase of this experiment was knowing that ascorbic acid is more rapidly oxidised at alkaline pH (so I&#039;m told). Therefore ascorbic acid must be a more effective reducing agent at higher pH.And remember, dear people, besides the interesting lightening of the orange colour to a yellow shade by heating known-to-be-oxidised DMT in alkaline solution with ascorbic acid, the other interesting observation (IMHO) was how the orange/yellow colouration of used limonene could be removed by washing with basic - i.e. alkaline - aqueous (wet) IPA.I would suggest a final step, after ensuring that all precipitates have precipitated, is rebasification of the precipitate and extraction into anhydrous acetone or IPA.Let&#039;s see how long that takes :lol:EDIT: Maybe a last blast FASA on the limo too?</blockquote>

[QUOTE="downwardsfromzero, post: 3687778, member: 1025"] There certainly wasn't any quantitative data from the start of the experiment, so really it would only be fair to call it an inference based on the observation of the solution going a paler yellow from a deeper orange colouration, kind of a reverse of the colour change seen when DMT oxidises/is thought to oxidise. As stated in the method it was a curdy white precipitate. Quite possibly yes, although some basic level of analysis would be required to state that it was [i]exclusively[/i] sodium fumarate. The moist IPA will certainly have contained some sodium ions, probably as carbonate - although when I discussed this matter recently I was told that the sodium carbonate had been made from sodium bicarbonate and a bit of extra sodium hydroxide had been added to the solution as there were concerns about the completeness of the conversion. So there was in all likelihood a bit of hydroxide present the solution, too. The precipitate could in all likelihood contain a trace or more of DMT. Come to think of it, could IPA possibly extract NaOH preferentially from a mixture with Na[size=3]2[/size]CO[size=3]3[/size]? That's probably another reason why it was stored in the fridge, besides attempting to encourage crystallisation; the reduction occured (or appeared to occur) when the mixture was heated on the hot water bath. The rationale behind the reduction phase of this experiment was knowing that ascorbic acid is more rapidly oxidised at alkaline pH (so I'm told). Therefore ascorbic acid must be a more effective reducing agent at higher pH. And remember, dear people, besides the interesting lightening of the orange colour to a yellow shade by heating known-to-be-oxidised DMT in alkaline solution with ascorbic acid, the other interesting observation (IMHO) was how the orange/yellow colouration of used limonene could be removed by washing with basic - i.e. alkaline - aqueous (wet) IPA. I would suggest a final step, after ensuring that all precipitates have precipitated, is rebasification of the precipitate and extraction into anhydrous acetone or IPA. Let's see how long [i]that[/i] takes :lol: EDIT: Maybe a last blast FASA on the limo too? [/QUOTE]