posted 03-09-2000 08:49 PM         

Gee, you could rig this baby up and put it in your lounge room, next to the t.v. even!

hellman
I'm sure you can buy that glass tubing as plastic as well.

posted 03-09-2000 08:51 PM         

Glycerol should be in every household,
Man, can't wait to see the results!!.

posted 03-09-2000 08:54 PM         

Glycerol should be in every household,
Man, can't wait to see the results!!.

hellman
(time for the hellman to learn UBB!)

posted 03-10-2000 12:53 AM         

Semtex; That's right it was dissolved in a beaker. The pressure stays about the same for about the first 1.5 hours as the heat rises then starts going down. Sounds as though there is a serious leak in your system.. there's no way it could all be consumed and have so little product. The ketone I got definately is the real deal, it aminates, responds to the bisulphite, color is right, distil temp is right. I cleaned out the keg using Acetone and there didn't appear to be any signs of corrosion. How did you monitor temp if no bath was used??

As far as this pd recovery stuff I think an easy method would be to convert it back to PdCl2 with cupric after the O2 is removed, then centerfuge in a dryer, then vac filter. Possibly add water first to make it less soluble?I dunno.. will try.

posted 03-10-2000 09:47 AM         

Hellman:
As I am a very lazy bee I prefer the idea not to mix or shake like a crazy, just sit and watch the bubbles doing the job for me. Probably some kind of plastic will suffice, but the ketone is very agressive to plastics and could dissolve it. So I would be carefull at high pressures.

KrZ:
I am impatiently waiting for your results and praying for success. If you will not reuse glycerol residue, I can send you some proven ideas about Pd recovery. Look at your e-mail.
I know the vac. filters, but how do you want to mix them? Or are you thinking about some kink of shaking device? Not sure if shaking will be so easy with a 12 gallon one.

posted 03-11-2000 09:00 PM         

[i]my two cents[\i][\b]

The can of worms is opening again, will we push on through amist these variabls or will we stagnate [b][i] LIKE BEFORE[\i]!

1) reactions must stay around 50 , no higher than 55C
2) ALL Catalyst & co-catalyst to be pre mixed 24 hours before adition,.
3) Safrole to be introduced over 1 hour
4) ALSO ONE OF MY BELIEFS IS THAT NOT DOING A NAOH WASH AFTER REACTION AND NOT DISTILLING CAUSES SIGNIFICANT ANIMATION PROBLEMS

As this method has the potential for great reward, as I have had not success I believe it deserves professional investigation and attention,.
[i]Gee, if someone had good access to a [b]tlc, nmr[\b] we could really nut this bastard down,.'
Obviously we need control conditions, ratios and samples over time of a standard amount of ketone[\i]

Or just someone like equarius to freak us repeatable results??..

[b][i]3 Successes in a roy eh??!!![\i][\b]

Write the Whole baby up equarius, QUICK!! .

[b]Tips[\b]

1) to prevent the stirr bar causing damage on the reaction vessel, Just insert a ceramic disc or some other inert substance to be placed where the bar doth spin.

hellman
That's all for now

posted 03-12-2000 08:33 PM         

I wish you would put a reference on who you are pissing off, [b]Geez your an anoying arrogant shit sometimes![\b]

Come on

posted 03-12-2000 08:52 PM         

Sorry, about the short post before, had to change terminals

If your post was refering to mine,,-I do my best to contribute here, and expereiment when possible,
It may be true that I am not as insane as your character appears to be,.
I'm not a ketone once a day man. O.K.
I only try to catalze a lil' success, as if that isn't obvious.

I just want the problem licked,.
And to lick this problem we could fuck around for years which we have done, or do something reasonably scientific.

My question to you is?
You have been experimenting for some time in this o2 field,
You must have a reliable method that consistently works, right?

What is it?[\b]

[b]Equarius,
I would love for you to fully explain your proceedure, as it seems to be reliable.
\

hellman- Fuck that for a post

posted 03-12-2000 09:25 PM         

So it's a malee,
Such an arogant pimp as KRZ won't stay here or leave here on my account,.
If you keep making him feel this good, that will give him more reason to leave and hurt you and people like you,.
There's no excuse for the way he carries on, FUCK HIM, I've tended to ignore it,until now

We can carry on without him b1o55,
The instergator of conflict is he,

Anonymous am I

posted 03-13-2000 01:27 AM         

Osmium gave us this reaction eons ago. He used a champagne bottle, 100 psi O2, hard shaking, and elevated temp. None of us listened to the higher temp thing as THE O2 ref (joc 34) and others indicate the best selectivity at 30C. KrZ improved (drasticly) the procedure by proving that hard stirring and can be used to uptake the O2 instead of shaking and got us back on track with the higher temp. I believe a higher temp than 25C is needed to get the reaction to progress (Osmium agree?). The annoying thing about glass jugs and such, besides explosion risk, is an annoying curve which makes it very hard to attain vortex stirring.

This reaction even works with air as spiceboy proved with a measly 17% oxygen. Everyman did the O2 wacker in the SRV and had success long ago (see his posts).

This reaction is very high yeilding and consistent. I'm not claiming I had 90% yields or anything as my workup really sucked and I lost alot there and durring distillation but I am saying that of the oil recoverred it was ketone (*possibly* some aldehyde) and no evidence of Safrole. That's using the keg, which apparently everone thinks is reacting with the catalyt. As Cesium pointed out above, this reaction is a function of catalyst (pd) concentration and cl. In my case the catalyst concentration was very low at 2g PdCl2 per 500g olefin and it appeared that, yes, there is a coating on the wall with the appearance of pd which is resistant to removal (which should only help things).

If the reaction does't work for you guys then its time to cut variables and find out why, in your case, it doestn't work. Ie. O2 in the solvent can be verified by checking if it comes out uppon depressurization.

Normally I would be doing this reaction alot but I'm swimming in ketone and busy making precursers and doing the final reaction.. and building glass wheels.

Gotta go.. the crack pipe is beconning me.

posted 03-13-2000 03:01 AM         

Walked over to my selction of plastic. Selected a blue 4L HDPE ice cream pail. Regret, should have chosen the orange.
Folded it.
Put it into the keg.
Opened it up inside.
Perfect radius.

posted 03-14-2000 02:37 AM         

The pail can be made maleable by heating with boiling water so it doesn't create holey creases upon insertion.

Sliding the pail to the bottom makes it FB and raises the stirring surface to a degree at which vortex stirring unnatainalbe. The solution to this is to form the plastic to the rounded bottom using heat and imagination.

posted 03-15-2000 08:22 PM         

PASSIVATING - A very confusing term, since the common usage has taken on a different meaning than the technical definition. In past experience, users (including engineers) of commercial fasteners seldom mean the old technical terminology. Technically, passivating is not cleaning but is a process of dipping fasteners into a nitric acid solution to rapidly form a chromium oxide on the surface of the material, creating a passive film that protects stainless from further oxidation (see PASSIVE FILM). The purpose of passivating is to remove both grease left from manufacturing and traces of steel particles which may have rubbed off manufacturing tools onto the fastener. In common commercial parlance (meaning non-military and aerospace), passivating means cleaning to users, and the terms “passivating” and “cleaning” are used interchangeably. A wide range of cleaning methods using different mixtures containing nitric, phosphoric and other acids or simply exposing cleaned stainless fasteners to air for a period of time will result in a “passivated” condition. For fasteners that have been properly cleaned, it is impossible to determine the method of cleaning or passivation that was used.