03-26-03 10:38
No 421479
I found one of those vacuum adapters with long drip tip, but the drip tip broke off. I put a short hose over the broken part to act as a drip tip. My question is, is this adapter safe to use under vacuum? Will the broken drip tip mess with the strength of the glass? Implosions are not fun.
(Hive Addict)
03-26-03 10:51
No 421482
but the drip tip broke off
Wierd,drip tube/tip is pretty inside of the adapter,how did you manage that?Anyways i think you can still use
For those about to synth,we salute you
(Stranger)
03-26-03 12:44
No 421506
the drip tip IS inside the adapter, but this particular one was designed so that the drip tip extends even further past the ends of the adapter a few cm so when connected to a flask, a few cm of the tip is actually inside the flask. I hope that clarifies things.
(Hive Addict)
03-26-03 12:48
No 421507
Guess you have to just try,if stuff jumps into your vacuum hose,it is not ok,but otherwise,yes.
For those about to synth,we salute you
(Hive Bee)
03-27-03 20:53
No 421895
swim has a vac adaptor with no drip tip left at all, and a crack running vertically down to the chipped male-connector. ketone still drips from the middle though so it skips past the vacuum nozzle.
swim threw some ptfe paste on the vac-adaptor and pulled some mdp2p at 85-89C. it forms hard chunky oxime crystals from nh2oh so purity is okay. vac adaptor held up fine. swim is just making do until he can have some new glass sent, like a vigreux for 20bux, and much much more...
(Newbee)
03-27-03 22:32
No 421922
This has nothing to do with the original question.Madprosr, what damn vacuum source are you using? Pulling ketone at 85C! Most GOOD vacuums get it at about 100-140C, I thought. Do tell!
Dr. Bumpz is 'da hottest chick on 'da Hive!! Hehehehe!
(Greenhorn)
03-28-03 11:34
No 422062
85c is good, but not uinheard of.A common hvac pump will pull ketone over at this temp.
I went into the business for the money, and the art grew out of it.-Charlie Chaplin
(Hive Bee)
03-28-03 11:51
No 422069
SWIM distilled MDMA freebase at 79-80 C with a ritchie yellow jacket 2 CFM model. Is this too strong for good seperation?
(Hive Bee)
03-28-03 17:01
No 422128
Some bee's say it's too strong, but for the life of me, I don't see why.. if safrole comes over at 60c and ketone at 85, then how is the separation going to get any better at 100/125?!
But anyway, the only downside to having a strong pump like that is the fact that you will need another pump thats not nearly as strong to distill water/solvents. If you are getting your ketone at 85c, then I bet your pump will boil water @ atmospheric pressure.
100% _______
(Hive Addict)
03-28-03 23:19
No 422197
My 10 mm pump boils water @ 10 degrees.Pump that pulls ketone over @ 80C should pull about 0,05 torr or close to that.Good pump ya got there mon.
For those about to synth,we salute you
(Hive Addict)
03-28-03 23:22
No 422199
My 10 mm pump boils water @ 10 degrees
Have you actuallty verified this by experiment?
Accept No Imitations, There Can Only Bee One; www.the-hive.ws
(Hive Addict)
03-28-03 23:27
No 422200
Yes,a week ago.Filled volumetric flask half full with 10C water and attached to pump.Then at some point water started boiling violently.0 degree water and 5 degree water didn't start to boil even if i waited few minutes.Then grabbed monograph and looked for corresponding pressure.I reached the same conclusion when i pulled MDP-2-P over @ 150C.Nomograph gave me 10 mm which is not very good but enough for me at this point.
For those about to synth,we salute you
(Hive Bee)
03-29-03 11:47
No 422320
just a Mastercool 250micron rotary vane pump. my point was that swim pulled 100 microns on a cracked vac adaptor without it shattering.
the pump used to pull mdp2p around 100C. then swim feed it some residual dcm and switched to a braided-hose, which somehow boosted it to like 100 microns.
ketone purity is ok at 85-89C, if you remove the forerun repeatedly. swim got 14g mda.hcl from 21.25g ketone via the oxime, which is okay...
swim will never use MeOH in the AcOH/al/hg again btw. post-rxn he added brine/base 3x vol of the MeOH and still got persistent emulsions when extracting with toluene...
(Hive Addict)
03-29-03 11:58
No 422321
Is there heavy bumping when distilling ketone @ so low temperature?Raf distills his ketone without stirring,there is some bumping but i can live with that.
For those about to synth,we salute you
(Hive Bee)
03-31-03 00:54
No 422666
With the good quality pump you mentioned, raf, you could get away with using a capillary, in order to avoid bumping. Do you think your Ketone seperation is going to be good at such a low temp? Swim would say that 130 C. would be a good temp to start collecting ketone at.
If I am wrong, educate me
If I am right, educate yourself
(Hive Addict)
03-31-03 08:54
No 422782
150C and low temp?Raf pump is just little better than aspirator.I was referring to somebee who pulls his ketone over @ 80 C.Good pumps are expensive and cool,but raf thinks 150 C will do no harm to MDP-2-P so he doesn't plan buying new one.
For those about to synth,we salute you