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All 5 posts Subject: Buffered performic distillation question Please login to post Down

FriendlyFinger
(Hive Bee)
12-01-03 10:55
No 474046
      Buffered performic distillation question

Hi there,
I'm in the middle of a buffered performic following Chemical Abstracts vol. 82, 72640z (1974) but using B-Methylstyrene, just finished 24Hr stiring, separated the layers and am about to distill the DCM from the glycol and esters. Checked the pH which is acidic.

So I'm wondering if there is any chance that some hydrolysis might occur if I distill at atmospheric pressure?

Thanks,
FF

cublium
(Hive Bee)
12-01-03 12:46
No 474060
      So I'm wondering if there is any chance that...

So I'm wondering if there is any chance
that some hydrolysis might occur if I distill at atmospheric pressure?
No,there will be very little if anything like hydrolysis.Formic acid is relativily weak acid unlike sulfuric which is used for hydrolysis and even then it takes 2-3 full hours at 80 C,a temp which you won't achieve when distilling out DCM from rx mix.Just heat till ya get distilling temp 70C or so and DCM is mostly out.

Rhodium
(Chief Bee)
12-01-03 12:56
No 474062
User Picture       Hydrolysis or decomposition?

Hydrolysis of some of the glycol formates to the glycol? Or are you talking about decomposition, rather than hydrolysis?

As long as you don't overheat (internal temperature in the distillation flask <100°C) I don't see any noticable decomposition occurring, as the rearrangement in the next step calls for heating with even stronger acid at ~65°C (bp of MeOH).

pacman_213
(Stranger)
12-02-03 04:38
No 474224
User Picture       just stick it on the water bath

DCM boils at such a low temperature that there's nothing to really worry about. How were you planning on distilling DCM under vacuum anyway?

If Pacman had influenced us, we'd run around dark rooms eating pills and listen to repetitive music

baalchemist
(Chef d'Equippe)
12-03-03 15:21
No 474494
      DCM distilling under a vac is usually bad...

DCM distilling under a vac is usually bad news, especially if using an oil pump(ends up in the oil reservoir). Unless of course there is a super-cooled condensing, trap & collection apparatus involved. Using a diaphragm pump is not any better, it turns it into mostly airborn vapors(unless using supercooled collection apparatus). Very similar to ether's properties, generally speaking.

GODISNOWHERE
Shoot Narcs, Not Drugs

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	All 5 posts		Subject: Buffered performic distillation question		Please login to post		Down


		FriendlyFinger (Hive Bee) 12-01-03 10:55 No 474046				Buffered performic distillation question
						Hi there, I'm in the middle of a buffered performic following Chemical Abstracts vol. 82, 72640z (1974) but using B-Methylstyrene, just finished 24Hr stiring, separated the layers and am about to distill the DCM from the glycol and esters. Checked the pH which is acidic. So I'm wondering if there is any chance that some hydrolysis might occur if I distill at atmospheric pressure? Thanks, FF



		cublium (Hive Bee) 12-01-03 12:46 No 474060				So I'm wondering if there is any chance that...
						So I'm wondering if there is any chance that some hydrolysis might occur if I distill at atmospheric pressure? No,there will be very little if anything like hydrolysis.Formic acid is relativily weak acid unlike sulfuric which is used for hydrolysis and even then it takes 2-3 full hours at 80 C,a temp which you won't achieve when distilling out DCM from rx mix.Just heat till ya get distilling temp 70C or so and DCM is mostly out.



		Rhodium (Chief Bee) 12-01-03 12:56 No 474062				Hydrolysis or decomposition?
						Hydrolysis of some of the glycol formates to the glycol? Or are you talking about decomposition, rather than hydrolysis? As long as you don't overheat (internal temperature in the distillation flask <100°C) I don't see any noticable decomposition occurring, as the rearrangement in the next step calls for heating with even stronger acid at ~65°C (bp of MeOH).



		pacman_213 (Stranger) 12-02-03 04:38 No 474224				just stick it on the water bath
						DCM boils at such a low temperature that there's nothing to really worry about. How were you planning on distilling DCM under vacuum anyway? If Pacman had influenced us, we'd run around dark rooms eating pills and listen to repetitive music



		baalchemist (Chef d'Equippe) 12-03-03 15:21 No 474494				DCM distilling under a vac is usually bad...
						DCM distilling under a vac is usually bad news, especially if using an oil pump(ends up in the oil reservoir). Unless of course there is a super-cooled condensing, trap & collection apparatus involved. Using a diaphragm pump is not any better, it turns it into mostly airborn vapors(unless using supercooled collection apparatus). Very similar to ether's properties, generally speaking. GODISNOWHERE Shoot Narcs, Not Drugs

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