Ill get to the point of this posting...

SWAN has a couple of questions...

What solvent should swan use in a/b?

Does anybody know where swan could find drawings or instructins on making a "quality" gasser? (Swan will not use his piece of shit gatorade bottle contraption again...so he says!)

Salt or foil?

Can you filter ani fume? How?

Last but NOT least...

Swan needs a stepbystep walk through on birch...that will give swan purer product with a better yield.. (swan was hoping maybe kirby could help) swan doesnt use h20 and cant vary his time in rxn. swan says this is s problem.

Any info on these subjects have been nagging swan for some time...He hasnt been as lazy as it sounds though...he just cant seem to find this info anywhere.

Happy stirring to all.....

There's a few diagrams on rhodium, if you'll just look around a little.

Candy prefers Xylene for her A/B extractions.

As far as a diagram for gassing goes, here is a very simplified version of a gassing flask.

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ill answer first to a good gassing device,,,this is what i thought up and used for many years,,,,two glass jars of about 250ml size,,,they must have air tight acid proof lids and ability to have two holes in each lid,(nescafe coffee jars with there plastic lid which you can poke a redhot small dia rod through for the piping holes),,,now the first jar holds 200ml of suplhuric acid,,has a 400mm long pipe coming out of the lid on one side,,,(all piping is 6mm dia od soft clear plastic tubing),,,on the other side of the lid is a pipe from the bottom of the sulph jar going to the top of the hydrochloric jar(500mm long and protrudes through the lid of the hyd lid by 10mm)),,,,,the other jar holds 80ml of hydrochloric acid, or 1 oz of salt,,or ali foil,,,,its lid has a hose coming from the sulphuric jar as previously explained,,and another hose(500long)on the other side of the lid, which is the hose the gas comes out,,,i would put a length of glass tubing (300mm) on this hose...,,, now place the suphuric jar on a brick on the ground and the hydrochloric jar on the ground,,the sulphuric jar should now be approx 100mm higher than the hydroch jar,,,,now blow on the blow pipe in the sulphuric lid,,this forces the sulphuric up the pipe and into the hydroch jar and starts a slow trickle feed,,,pick up the glass pipe and watch for smoke coming out,,when its nice and heavy(approx 40 secs),,then begin to gas the product,,i use hydrochloric acid in the gassing as i like the taste it produces in the product,,to stop trickle feed just reverse jar posistion eg;hydro jar goes on brick and sulph jar goes on ground,,,,before stopping trickle feed you must have gassing pipe out of product solvent or suck back occurs,,,can you filter anni fume,,,hmm, what for???i had a big thick walled bottle i did the ammonia/sodium metal reduction,with a one holed rubber stopper in it, hose going from stopper to roof line, at end of hose i had a S piece of hard clear plastic pipe,,this would catch anything being emitted by the ammonia,,i spose if you wished to put on the hose a tube with filter material very lightly packed in it,,and let the ammonia vent through that,,it couldnt damage the reduction,,,,,,,explain to me why you dont use dnh20 after the reduction ,,,and why you cant vary the reduction time,,,and a walk through is better when both people are online

i used about 350ml of hexane in the A/B,,and then just squirted the hexane and eph straight into the ammonia,,then just gas the hexane when the ammonia has evaporated,,most dont do it that way, but i find that hexane makes a better tasting product...

candy,,what do you do with the xylene after the A/B

Candy says, she makes sure it is free of any residual H2O by drying over anhydrous MgSO4.

Then proceeds to gassing, via HCl saturated with NaCl in a 500ml erlynmeyer adding ACS grade H2SO4 dropwise via addition funnel.

The gas travels a 18" length of tubing into a gassing flask similar to the one pictured.

The nipple on the filtration erlynmeyer has yet another 3 foot length of tubing, that is submerged in a bucket of soapy water. This is to alleviate any HCl escaping into work area.

( NOTE: if you intend to attempt a setup similar to this, be sure to loop the exhaust hose a couple times and affix an adjustable clamp to eliminate suckback)

why do you gas the xylene after the A/B???

In order to precipitate the amine.hcl for recrystallization.

(candy utilizes HI reduction)

mnm,,bare with me for a sec cause im a bit lost,,candy originaly said "candy uses zylene in the A/B",,,,then i asked "candy,what do you do with the zylene after the A/B,,,,you then answered by way of describing how you gas the solvent ,,,,i then asked "why do you gas the zylene after the A/B,,,,your answer was "to precipitate the amine etc,,then went on that you redphos/iodine,,,,,im not asking how you gas after reduction,,,im asking, the solvent that you use for the A/B,, What do you do with it?????