HELP!!!!!!!!

Soap · Fri May 20, 2005 7:13 am

Ughhhh!!! Well swim was reacting his safrole with koh again because he didnt get a complete conversion the first time. well things are going nicely nice reflux then suddenly the aspirator went wrong and the flask was filled up with water. yes dirty salty water. what should swim do? safroel steam distills right? how can i recover (it was only like 50 ml) AHHHHHHHH!

IndoleAmine · Dreamreader Deluxe

No big deal, just extract the thing with toluene 3x, wash combined extracts with H2O couple times, then with bicarb, then brine, then dry and remove solvent with vacuum.

Then try again..

Soap · Fri May 20, 2005 9:55 am

ok thank you very much. swim will go ahead and try that. while he was gone at the store picking up more ice something happend. the thermometer adapter (with thermometer) somehow shot off and landed into the bucket of water used for the condendser (didnt break!!!!!) meanwhile the whole lab smells heavily of safrole. blah swim must have the worst luck ever!

brixtonj · Fri May 20, 2005 3:42 pm

Hi !!!!
Well , It happened to me as well !!!!! . The point is that when a water aspirators stop working (for whichever reason) It does NOT let pressure out of the system .. therefore instead vacuum .. you got pressure in you setup .. with these kind of consecuences

-indeed you were lucky ..as my adaptor broke off - and Its probbably the most expensive glass-piece in my setup.

Id seriously advice for adquiring a propper vacuum source. Sooner or later you are gonna need it. A good hobbyist ? air-compressor goes for around 80 Euros /100 Us$ and can be modified to suck air instead of compress . With that setup , you can see water boiling at room temp , if you want. I got safrole distilling at around 90 C. DCM / MeOH distills itself without heating !!! .

Good Luck !!

2spun · The Resistor

swiy get's his safrole to distill at 90c to 110c
his DCM at 50c in oil bath as far as MeOH swiy thinks
it may have come over with his DCM. (Not sure) next run hell pay close attn:
swiy likes this setup for his distil'n needs

2spun · The Resistor

Soap,

[quote=while he was gone at the store picking up more ice ![/quote]

ice cubes ? is this what swiy is read'n?
swiy stop use'n ice cubes he use's them small blue ice things one can get at a few of them larger stores around for about 1 to2 dollars.
plus he saves his soda bottles fills them up with h2o and freazes them .
this way he don't have to empty his 5gal bucket so much and can keep it very cold
by rotating his bottle'd ice? one can go up to Gallon size as well.
Much Thanks

methyl_ethyl · Riedel De Haen

sg43 · Sat May 21, 2005 11:52 am

brixtonj, How would one go about converting a hobby air compressor into a vacuum, and would it pull a better vacuum then just using the compressed air with air venturi to be worth converting?

Guest · Sat May 21, 2005 12:32 pm

Turning a hobby compressor into a vacuum source is definately possible, and when done properly would provide an excellent source of vacuum,.

I would suggest focusing your enegy around extending the inlet manifold.

Usualy there is a screw on Filter attached to the Air inlet port,

What you must do is put a series of traps inline to deal with the chance of solvents destroying your motor,
But with a bit of care this can be done, well.

You want to have a water trap inline, possibly two, and some other traps depending on the solvents you are using,

I am quite sure that the Vacuum produced would be significant

Syn

2spun · The Resistor

methyl_ethyl,

when swiy distill his sassafrass he use's vacuum. and swiy belives his safrole was comming over at this point 90c -110c

after cleaning his crude oil mdp-2-p and getting back to the distill'n
swiys DCM came over at right around 50c mabe a touch under(45plus) but no vacuum was apply'd after change of flask when no more DCM or MeOH was comming over
swiy put the vacuum back on and his mdp-2-p start'd to pull over at around 120c to 125c he belives. swiy will be doing this again very soon and will take better notes.
to verify. as far as swiy reads what things are to look like etc. everything looks fine.
swiy has not push it to it's final end yet. and that bee'n the story that tells the tell.
swiy is all ears tho if sometime is wrong.
hook a brother up.

ok swiy set up is not 100% professional but this is what he's work'n with.
glassware is all good has the setup as the pic above is.
swiy vacuum source he's work'n with right now is a medical aspirator
not the best kind and swiy don't trust the gages. (he don't think they are read'n proper). swiy can turn up the pull to where his glassware bumps but the gauge
reads at around 18.inHg.(and swiy really don't know what that means)
so swiy cuts it down don't like that bumping action.

candy thermometor
swiy use'd that in oil bath when distil'n the crude oil

((regalur thermometor swiy use'd and got his read'n on the distil of the sassoil to safrole)) this maybe where his read'ns are off.
as swiy push's air in at the same time it seems to go faster the distil prosess.

swiy has some crude oil that needs to become a clean mdp-2-p he'll work that today and take notes.

as well swiy has some sassoil that needs to become a clean safrole.(this will have to come later tonight or tomarro)
what he'll do is use his candy thermometor in a oil bath with this so he can get a better reading.
stirrer hot plate and magnet stirrer are very good.
swiy hopes he put this in a understandable fashion if any holes are found
swiy ask please punch away because swiy don't mind
it's all a learning thing and swiy likes that.
much thanks

2spun · The Resistor

swiy hope's
others can see the color of this pic. swiy is a bit color blind.
but his other 1/2 thats not(ColorBlind) tells swiy it's a piss yellow.
this is what swiy is gett'n as his mdp-2-p.

swiy is wondering. is the a black light test for this or something close?
is there some way to test without have'n advanced equipment (Chromatography) or what have ya?
Much thanks

brixtonj · Sat May 21, 2005 11:09 pm

Hi !!!
Regarding the converted air-compressor : Yep , It can pull shit loads of vacuum . Indded is a 3000 Watts vacuum pump ! . I put the adaptor at the inlet (instead of the air filter) .

I dont think that these vapours can damage the air-pump internals. For a start ..most of it is stainless steel (the bore and the rings) . Secondly .. It is running really cold ('cos of the vacuum ) so It won't react that much with the metal (remember that air/vacuum/vapours etc.. ) only contacts the piston and the cylinder .. not the electric engine.

The only thing to remember is to flush the system (i.e. compressor , pipes , pump , and reservoir) with air after using it as a vacuum source .

I am gonna take & post a picc of my vacuum- compressor .. to show how it is done.

>>>>> Ketone picture

That picture seems to got the white-balance quite off (probbably taken with a cameraphone- It is quite dificult to tell the actual colour of that fluid .

but , from my *extremely* limited experience .. It does not look like ketone. It looks like the results of the hydrolisis .. but BEFORE ketone distillation. I had that same colour .. before the distillation . Anyway , when taking a picture to show /discuss a colour , It really helps to include in that picture something of a known colour (such as Marlboro pack , for example ) so the gamma-correction (white-balance in the camera) can be corrected. Otherwise It is impossible to know which is the real colour for that fluid.

cheers/

2spun · The Resistor

right swiy understands about the pic,
swiy as well has not that experience to say.
was taken with a movie camra. good idea to ( include in that picture something of a known colour)
swiy will remember that for sure thanks.

the pic was after the distil . swiy don't doubt something may have gone wrong.
it's been a busy day so far and swiy still has some cude oil to wash and and distil .
will take better notes. as well as pic's
ok Much Thanks

2spun · The Resistor

OK,

Thanks frist swiy has to say. after moving a bit slo'r.
After Flood'n the mixture W/acidic water . this is where swiy got lost. with last
post etc.. swiy end'd up work'n more with the dark bottom layer. think'n thats what he want'd.W/(the messup's etc thru the hole prosses). Thats what swiy went to distil. give'n what was posted. things are moving a bit slo here for swiy. BUt what was posted earlier. as far as a ketone. can be but a mistake. see'n now what he did'nt understand then.swiy will give out better details. as well come soon.
Soap my apologies for take'n all this off topic.(as to everyone else).
Swiy doe's wish to set all right with a better wrightup(on his part) with some pic's
for helpers. so others may have a better understand'n than swiy.
So again thanks for all the help everyone.
Much thanks

brixtonj · Sun May 22, 2005 12:39 pm

Hi again..

It occurred to me that ...-after the expoxide/glycol with the acidic-water ... I =mistakenly= put a much more accidic water .. that -at the end of the reaction- the ketone layer was at the TOP , and not at the bottom.

I mean - if the 15% HsSO4 is made up by volume -and not by weight- the water layer is way more (twice !) dense =and accidic = than it should be . hence the ketone is on the TOP ! layer ,-not the bottom as in the writeup- and then You -perhaps- just washed & extracted the wrong layer.

In my setup , Ketone was definitely at the top layer and other times at the bottom . It just deppends on the accidic-layer's density.

Anyway .. a good way to tell if it is ketone/epoxide/glycol or just collored water is , either distillation temp ,or the smell .

If it has smell somehow similar to safrole and ITs yellow .. then It could be Ketone.

BTW : This is a gamma corrected (propper white-balance) colour picture of a ketone drop . This is a much more yellow (somehow like those fluorescent markers !) .

Good Luck !