swim distilled sassy for the first time a few...

[edo]

swim distilled sassy for the first time a few weeks ago.He used boiling stones and water aspirator. safrole came @ 140(thermometer 1" below 3 way adapter). Swin noticed the he increased the water flow the temp would rise and when he lowered the temp would fall.

Swim tried to distill sassy again but this time he used magnetic stirring. Safrole came 190 water on full blast. No matter how he adjusted the water flow the temp doest change. Swim isnt sure why. Maybe a leak ?

Swim is batting 1-4   when making ketone
 

thx

p.s damn boiling stones turned the sassy in boiling flask brown/orange

[Rhodium]

Swim is batting 1-4   when making ketone

What does this mean? (I'm not a native english speaker)

[ApprenticeCook]

I speak english and i still dont know what it means....

[edo]

1 success out of 4 attempts

[karl]

Too high a flow rate through your aspirator can be counter productive, pumping more water through it does not guarantee a higher vacuum and remember its risky to alter the water pressure in mid distillation.

Did it distill very rapidly? maybe the vacuum hadn't attained its peak while you were heating it and it over heated. That would explain the high temperature of 190'C

If this isn't what happened then obviously you have a crap vacuum and maybe you just have a leak or need a better aspirator.

[ApprenticeCook]

1 in 4? crap..... now that’s some major waste of precursor.

As its said, set it up and dont change it once your in flight, that may be your problem, and 190 is way to high, how strong is your vacuum???

In your vacuum line wack in a T joint and secure just a normal vacuum gauge to test it, swim has one stuck in there permanently, make sure you secure the pipe fitting, use glue and tape and whatever, swim first tried this and couldn’t find the leak when it wasn’t working, guess where it was.... stupid fitting didn’t quite sit right.

[amine]

you should invest in a pump IMO. Asspirators at least according to SWIM's experience just don't cut it. A nice yellow jacket or robinair will get the job done. I'm pulling sassy over at close to 70C thanks to the vacuum. Don't try to take short cuts, save up until you've got all the equiptment you need. Ghetto labs produce ghetto products.

Also a tip: Never shake up a warm seperatory funnel that has  glycol and warm water. I had a lovely facial yesturday which cost me 150g of glycol.

[karl]

A good aspirator can perform all of your requirements no problem, there are good and not so good ones on the market. Back in the day I ran the thing using a second hand water pump circulating water between two connected plastic drums as tap pressure was pathetically weak.
You don't need to brute force your vacuum like that unless you distilling some more heavily substituted phenethylamines. Just check to see if your vacuum is strong enough try distilling water.

A bit of practice or familiarity with your equipment goes a long way

[methlab]

i payed about 30$ for it and i collect safrole between 135-140 C, ketone between 165-170C, this should be good enough for personal use...

[ApprenticeCook]

Swim uses a nice aspirator, cost a pretty penny new but with it and a nice setup with a pump doing its job ala doco on rhodium's site works fine, 130^oC, those of you who crap on aspirators must be budget chem, go top shelf when it comes to things that really matter, its worth it!

[biotechdude]

Swix agrees with ApprenticeCook; in that a well constructed aspirator setup can work just as well as a mechanical vacuum pump. 

The main areas for consideration are the

- quality of the aspirator itself.  You get what u pay for.  Make spare rubber diaphragms using thin rubbber sheets cos they warp and hinder flow as they get older.  Also ensure it is setup to maximise water flow etc and hence the strength of vacuum.
 
- the tubing and connections. This is paramount as there is nothing worse than waking in the middle of the night to a faint 'hissing' sound; only to find connections from the tap have come loose and have flooded the lab!  Use quality 'braided' hose that wont expand (and 'slide' off) under the water pressure.  Then double clamp using quality clamps that wont give.

- the water used.  Or rather, ensure it is cool from the tap and at a high enough pressure.  If not, a pump setup will need to be constructed (check rhodium.ws) that circulates the water and creates ample water pressure (ice can also be added).  Also, landlords will get suspicious if you have 2x as much water usage than the rest of the building...

Swix has also seen a clear benefit of using aspirators when reducing a solution in volume.  The aspirator allows the hot vapours be absorbed straight into the water flow - eliminating any odours and negating the need for condensers or distilling.  A mechanical vacuum pump cannot be used straightforwardly for this purpose. 

However, a decent mechanical vacuum pump is ALWAYS going to provide the easier and more predictable route under a variety of situations.  But hey, sometimes its just overkill.  A sports car wont get you to work any faster when everyone is subject to the same traffic delays, but it does make the ride there a little more comfortable...

[ApprenticeCook]

Yeah biotechdude, everything you said is right! areas of focus but swim does things a little less tech and it seems to work...

Swim uses a nice setup glasswise, all the proper stuff, well now anyway    Read:

Post 492925

(ApprenticeCook: "Govt lab auctions", Chemicals & Equipment)
So with all the nice glassware and everything swim uses its great, aspirator is good but yes as its been said you have to buy quality aspirator and pump.
However heres where swim drifts from whats been said, instead of using braided hose just use a simple pressure line (really really thick flexible poly hose) which slides onto the nipple joints on the aspirator swim has and use a brass hose connector screwed onto a pressure pipe (solid type) which goes straight into the pump. Solid pipe from pump to bucket for water out.
This works well and has not leaked *YET*.

biotechdude - Use quality 'braided' hose that wont expand (and 'slide' off) under the water pressure.  Then double clamp using quality clamps that wont give.

How do attach the ends onto the pump and aspirator?? using clamps???    swim uses that plumbers pipe glue crap (containing MEK) the blue stuff and using copious amounts glues on the poly to the aspirator and on the pump end, also works to water seal joins...    Could you elaborate on what size braided hoses and what types of attachments on aspirator and pump end of hose? swim wouldnt mind looking at that for a safer alternative to what he currently has, its constanly in my mind while overnight operation ill wake up in a water park with a stuffed experiment and burnt out water pump....

[biotechdude]

The main point Swix was making is that u should use the best hose u can get your hands on.  Dont settle for simple clear PVC tubing from the hardware as that shit LOOKS good; but ends up warping and collapsing at any useful temperature.  So goto your favourite tubing store and get the best u can afford; proper vacuum tubing would be ideal for the connection from the aspirator to the glassware, and high pressure fluid tubing is best for the water connections.

It is recommended that u get the best fitting tubing that u can just squeeze over the aspirator fittings.  Then secure with quality hose clamps.  U can seal with glues etc - but then it makes cleaning, maintenence, and replacement of parts difficult. 

IN SHORT - take the aspirator into a decent hose store, and say 'this bit has cold high pressure water flowing through, this bit will be under vacuum and subject to heat, and it needs to clamp up tight'.  The dude will go, this bit for here, this bit for that etc.  Hand him the cash and leave.  If he asks questions, its for your hippy aromatherapy hobby, or you're an inventor or some bs.  Swix finds they shut up when they ask shit and u say, 'its a water-aspirator to create a vacuum', and they say 'cool mate' - then they are out of ideas.

Simple Simon