11-30-02 03:12
No 384725
I love this stuff. I've read tons about it in the search engine especialy from Rhodium. I wanted to give one piece of advice for preparing the filter.
Take the buchner, and place the filter paper on it. Wet it with a few mls of solvent (eg water). Then take a teaspoon to a tablespoon of celite (not much is needed, often less is more) and put it into a beaker with a ten to twenty mls of solvent. Turn on the vacuum, swirl the beaker around, then suck it through. You'll get a perfect uniform depth of celite each and every time.
This stuff is cheap, usually $2-5/kg. I highly recommend anyone who runs into something that takes years to filter. It will speed it up to only take minutes. I can't believe I ignored the value of it for so long.
(Chief Bee)
11-30-02 05:06
No 384761
(Rated as: good read)
Yes, Celite (diatomaceous earth) is one of the organic chemist's best friends. It not only speeds up otherwise impossible filtrations, it also helps you filter out things that would go right through a fritted glass funnel or normal filter paper - something that immediately comes to mind is activated carbon (both decolorizing carbon, as well as for example Pd/C). If you have tried to filter off activated carbon using standard methods, you know what I mean - it is impossible to get rid of the last traces of suspended carbon particles in your filtrate.
Another thing that makes Celite invaluable is its ability to break any kind of emulsion you have managed to get in your sepfunnel. Just filter both phases and the emulsion inbetween through ~1cm of Celite on a buchner at the pump (don't forget to wash the filter cake with a little suitable solvent afterwards), and when the liquid collects in the filter flask, it will always be in two layers again. You will also have removed many of the colloidal particles which helped the emulsion form in the first place, so during subsequent extractions you are much less likely to get an emulsion again.
(Hive Bee)
11-30-02 05:50
No 384787
Awesome, Celite DOES rock!!
Sink or SWIM
(Hive Bee)
11-30-02 05:56
No 384790
Where do you get it? I always thought it was those Celite scrub pads.
(Hive Elder)
11-30-02 06:19
No 384798
One of the simplest places is a chem supplier, not suspicious at all, but often times is expensive, right Rhod...? Diatomaceous earth can be found OTC at garden supply places, CHEAP, I mean 50lbs would be under $20 from what I remember(I have a 2.5kg pail of the stuff from a chem-hut and haven't used any of it yet so I've had no need for more)... It's an organic pesticide, used from crops to mixing it in with Animal feed to swimming pool filters...
Mean People Suck
(Hive Bee)
11-30-02 06:24
No 384802
Is it the white rocky substance used to top off a vermiculite cake in mush cult? I can't think of the name of that stuff.. If so, they sell it at wallys, next to the vermiculite. It's like made of volcanic matter.
Found a pic of a celite bag on google
(Synaptic Self-Mutilator)
11-30-02 08:50
No 384842
Instead of decanting off ethanol repeatedly with an Al/Hg (a la Osmium) or basifying it (a la Ritter / Methyl Man), has anyone tried filtering the entire post reaction mixture with celite? Then distilling the ethanol to reuse it? It seems so simple and efficient.
(Chief Bee)
11-30-02 10:39
No 384861
Oh yes, most certainly! I couldn't imagine working with the sludges after Al/Hg or LAH reductions without having access to Celite. The beauty of recovering the solvent from Al/Hg aminations through distillation after filtration is that it contains a whole lot of methylamine freebase, so that you don't need to add as much in your next run. Recycling listed chemicals is always a nice thing to do.
(Stoni's sexual toy)
11-30-02 13:53
No 384886
There are many types of celite available from chem suppliers. Which one to use?
Never seen it OTC.
I'm not fat just horizontally disproportionate.
(Chief Bee)
11-30-02 14:50
No 384898
Os: The cheapest. The more expensive brands are for analytical work.
(Stoni's sexual toy)
11-30-02 14:56
No 384900
They seem to differ in many more respects than just extractable inorganics! Like surface area, density etc. The instructions by the manufacturer I once saw gave examples for all kinds of different filtrations, e.g. yeasts in beer manufacture, different analytic filtrations etc, and recommended different kinds of Celite for different filtration problems.
I'm not fat just horizontally disproportionate.
(Hive Bee)
11-30-02 15:08
No 384902
For example Pd/C
Pd/C is expensive but reusable, for the most part, although it does lose some of its activity each time you use it right? Is there any way to recover it from Celite? Or does swim have to just use a regular Buchner if he wants to reuse his Pd/C? If so, what is the best filter paper for this? They make so many, even each brand has dozens of numbers and materials.
(Master Searcher)
11-30-02 16:42
No 384919
Post 217504 (PolytheneSam: "Re: promotors of Urushibara ??", Novel Discourse)
Post 211468 (PolytheneSam: "Re: promotors of Urushibara ??", Novel Discourse)
Post 182801 (PolytheneSam: "Re: Nickel vs Pd", Chemistry Discourse)
ebay?
http://www.geocities.com/dritte123/PSPF.
The hardest thing to explain is the obvious
(Old P2P Cook)
11-30-02 16:54
No 384923
Never seen it OTC.
In the U.S. it is available in large bags from most any hardware or swimming pool supply store. It is used in the pool filters which have a canvas bag that is then coated with celite by adding a scoop of it to the filter intake.
Baseline Does Not Exist.
(Synaptic Self-Mutilator)
11-30-02 17:47
No 384932
Well this is an easy way to save adding many grams of NaOH to the alcohol to basify... I'll try it next time. I'm surprised no one has pushed this method.
(Chief Bee)
11-30-02 18:18
No 384942
(Rated as: good read)
BlindGenius: If you use a very small fritted glass funnel like the one below (they are about 5 cm across), you will be able to remove your catalyst for re-use without any contamination. But - some of the small carbon particles will penetrate the glass frit and get lodged in there forever, making it look somewhat ugly. If you would cover the bottom of that funnel with 5 millimeters of celite, and pour your solution containing suspended Pd/C onto it very carefully, it will stay in place, and after you are done with the filtration, you will have two layers of solids in the funnel, the Pd/C on top of the celite. Now you just take a small spatula and carefully remove the catalyst layer (and put it in a vial half-full with water) and next to no celite will be carried over. And even if a few grains would carry over, that doesn't really matter, as celite is completely inert, and will have no effect on your next hydrogenation reaction.
(Hive Bee)
11-30-02 18:34
No 384948
If your catalyst is for example 30 mikrometer standard (or the particels of the activated carbon you used to make it) you apply an filter (or fritte) with about 20 mikrometer pores. Of course many particels of the catalyst have broken down and got smaller, very much smaller, so after filtering you will still see a lot of catalyst left in the solvent. Refilter it several times through the same filter used before, so by principle the catalyst filters itself.
Thus spoken by DEGUSSA in their specifications on noble metal catalysts. Prior they advise centrifugation if any possible.
ORGY
(Old P2P Cook)
11-30-02 19:42
No 384965
What I find to be far superior to glass frit or celite are the glass fiber filters made by Whatman. They have very rapid filtration even when filtering fine sludge and retain particles down into the 1-2 micron range. They are a bit pricey, about $35.00 for a package of 100 7.0 cm filters.
http://www.whatman.com/products/analytic
http://www.whatman.com/tech_support/tool
http://www.whatman.com/index2.html
Baseline Does Not Exist.
(Chief Bee)
11-30-02 20:50
No 384980
terbium: Have you been able to filter precipitated metal (hydr)oxides using them? I bought Whatman glass-fiber filters like the ones above after some salesperson at the local chem supply said that they would be perfect as a "no-holdup" alternative to celite for removing precipitated TiO2/Ti(OH)2 from aqueous solutions, and when trying to put them to use I soon noticed that they aren't that different from paper filters, besides being inert and having exceptional wet-strength (is that a word?)
(Old P2P Cook)
11-30-02 23:04
No 385010
I can't remember the worst sludge that I have filtered with glass fiber filters. Seems I would have to agree that for a really fine sludge a deep bed of celite might be better. For most other cases, with slightly less intractable precipitates, I would still say that the glass fibers are far superior to paper - faster filtering, much slower to clog and better retention of fine particles.
Baseline Does Not Exist.
(Bear With Me)
12-02-02 02:18
No 385277
(empty)
(Old P2P Cook)
12-02-02 03:22
No 385301
I thought you were suppose to wet the filter, then make a slurry out of the Celite plus whatever solvent you will be filtering to pour into the funnel, vacuum running.
Yes, isn't this exactly what was described?
Baseline Does Not Exist.
(Bear With Me)
12-02-02 03:24
No 385302
I misread that; thought it described pouring dry Celite onto filter, then pouring water over the top, which is not ideal...
My bad
~ PB
As a consolation, I will change my signature to more attractive blonde school-girl sounding format. Once again, I sincerely apologize for my lapse in judgement...
Like, if you listen,
they will never lie.
To achieve the answer,
you must hit a big orgasm.
(Synaptic Self-Mutilator)
12-02-02 19:31
No 385554
I tried filtering the post-reaction of an Al/Hg with a shallow depth of celite (diatomaceous earth from a pool supply store)... with manganese oxide sludge the filtrate usually pours thru the celite at the beginning. With the Al/Hg sludge it was painful! There was just a very slow drip at the beginning that started to slow down right away...
Unfortunately celite didn't work well for me at this task. Bummer, I was really hoping. Oh well, at least it's easy to distill off some of the alcohol from a post-al/hg. Perhaps Osmium's alcohol extraction is the best way (I don't like it because it uses so much alcohol) or perhaps Ritter's sodium hydroxide basification is the best way (I don't like it because it uses so much hydroxide).
Does anyone have other tips and tricks for filtering?
(Chief Bee)
12-02-02 19:53
No 385564
Usually these slow filtrations is due to a thin gel layer forming on top of the Celite. Just scrape that gel off from the top of the celite with a large spatula, and when fresh celite surface has been exposed again, the filtration wil again go faster.
(Hive Bee)
12-03-02 01:16
No 385662
Place a fine filter paper on the buchner funnel and then a 1/2" layer of celite or D.E. Then place another COARSE filter paper on top. Somehow this makes filtration a WHOLE lot faster on post al/hg sludge.
Sink or SWIM
(Hive Addict)
12-03-02 16:16
No 385819
i don't use buchner on post rx crap,too messy.I just flood with NaOH solution and let stuff settle,then pour off clear yellow liquid and then flood the sludge again with some denat alcohol.
For those about to synth,we salute you
(Stoni's sexual toy)
12-03-02 16:31
No 385820
> i don't use buchner on post rx crap,too messy.I just
> flood with NaOH solution and let stuff settle,
But others do that. Because the amount of NaOH needed for a big Al/Hg batch would be excessive, and because some people want to reuse their MeNH2.
I'm not fat just horizontally disproportionate.
(Hive Bee)
12-03-02 20:06
No 385861
by contacting the funnel with a sonotrode (60W@80khz) usually not filterable solutions/emulsions/sludges can be filtered. Not with ease but it works. Care has to been taken as some mixtures solidify with ultrasound, so test with a small amount not to get a sudden solid surprise.
ORGY
(Synaptic Self-Mutilator)
12-04-02 03:18
No 385984
I've found that it's possible to distill off a lot of alcohol without filtering the sludge. Although it's not ideal, it's possible to recover some of the methylamine laden alcohol... then you can add your aqueous base and extract with toluene as per usual.
HiddenCloud, are you filtering right after the Al/Hg is finished, or after you've basified the alcohol? I imagine the basified alcohol solution would filter quickly, but I couldn't get the regular solution to filter with any speed (is this because of my shitty aspirator, or because this post-rxn crap doesn't filter well?).
(Hive Bee)
12-04-02 03:32
No 385989
Yeah, I basifyed first, then I vacuum filtered. I would imagine if you didnt basify that it would be alot slower.
Sink or SWIM
(Hive Bee)
12-04-02 03:34
No 385990
Oh yeah, and wash the dark filter cake with methanol to get out the rest of the freebase from the filter cake.
Sink or SWIM
(Synaptic Self-Mutilator)
12-04-02 03:49
No 385998
Damn, I was hoping it would be possible to remove the sludge before we basified to reduce the amount of base needed. It turns out to be a lot of hydroxide when you're talking about taking the reaction to larger scales.
(Hive Bee)
12-04-02 05:12
No 386027
I dont know yet. I havnt actually tried to filter right after post-al/hg before basification. This weekend swim will try a al/hg and see if he can filter it w/o basification.
Sink or SWIM
(Hive Bee)
12-07-02 21:02
No 387185
I just now finished up an al/hg run using nitromethane/methanol without any ketone of some sort. I didnt basify this time but i vacuum filtered hot using filter paper/celite/filter paper. It filtered fast. I filtered about 1.4L of the solution in about 3minutes using aspirator vacuum.
Sink or SWIM
(Stoni's sexual toy)
12-07-02 21:59
No 387201
Do not apply too much vacuum for too long, and do not filter hot! You will suck all the good stuff out of your solvent!
Just pour your room temp post reaction mixture into the Buchner funnel, apply some vacuum to the filtration flask, switch it off again after a few seconds and let the filtration take its course. If you use an aspirator, use a valve between the pump and the filtration flask. Coarse, fast filter paper (coffee filters?) will usually do, doesn't matter when some Al sludge gets sucked through if you intent to use the MeNH2 in MeOH for an Al/Hg amination.
Who cares if it takes long?! Still better than all the fine methylamine product ending down the drain!
I'm not fat just horizontally disproportionate.
(Hive Bee)
12-07-02 23:38
No 387243
>> and do not filter hot! You will suck all the good stuff out of your solvent!
Good point! The thought never crossed my mind that filtering when hot could result in loss of yield. Good advice!
(Hive Bee)
12-08-02 03:05
No 387327
The al/hg when filtered was about 35-40C. I dont think i lost that much methylamine...atleast i hope not
Sink or SWIM
(Hive Bee)
12-19-02 08:57
No 390734
The guy at depot didn't have a clue.. "Celite? Huh? Whats it look like?"
I just stood there for a minute as the store became silent.. I didn't have a clue what it looked like, "I think it looks like perlite".
Needless to say the guy didn't know what perlite was either..
Not knowing what celite is, I tried to picture it visually from the info in this thread. I kept picturing Perlite, the white pourus volcanic material. Having used that in mushroom cultivation, I familiarized with it's properties and off to walmart I went. No deal, they were fresh out.. but I know they stock it certain times of the year, for a long while back I bought some there.
Well, no perlite, and for all I know it could be a totally different thing, but Im thinking perlite could work.
Empty handed, I thought I would try foil instead. If you tightly ball the foil up into little bb's!! Wait.. thats it! Could BB's work? A filter, with 1 even layer of bb's, then another filter on top?
Is Celite anything like Perlite? Educate me please.
(Hive Bee)
12-19-02 14:03
No 390787
It sounds very similiar to perlite.
I'll try it, I found some in the garage minutes ago. I hate when that happens.. out at the store lookin for shit I already have.
Heres more info on it. It's not soluble in water at all.
http://www.perlite.net/
(Old P2P Cook)
12-19-02 16:07
No 390812
I'll try it, I found some in the garage minutes ago. I hate when that happens.. out at the store lookin for shit I already have.
Heres more info on it. It's not soluble in water at all.
http://www.perlite.net/
Try what, perlite or celite? Just because the names sound similar and they perhaps even look similar does not mean that they are similar! Perlite is not a substitute for celite!
You tell the clerk at the hardware store that you need "the white powder that you add to a swimming pool filter after the filter has been cleaned".
Baseline Does Not Exist.
(Chief Bee)
12-19-02 20:38
No 390843
We are using fossils to make drugs? I wonder if my own remains will one day be used in a clandestine lab...
(Hive Addict)
12-19-02 22:15
No 390872
Maybe you could put a clause in your will about having your body cremated, then the ashes could be used as a celite substitute. Then someone could cook a batch of MDMA, and use your ashes for filtering a post-Al/Hg, then they could distribute the finished product out to bees who wanted a little taste of Rhodium. But that would be kinda creepy.....
It is seductive, way too seductive. -Eleusis
(Hive Bee)
12-19-02 22:33
No 390878
Terb, I found a bag of perlite in the garage, not celite. I will go get some celite though, now that I know what it's used for. Thank you :p
(Hive Bee)
12-19-02 23:10
No 390897
Perlite is used for holding and releasing moister over time. Best hive related use are humidifying mushrooms or hydrophonics. Get celite do not even consider using perlite.
Not a chemist I just follow directions on the box mix
(Synaptic Self-Mutilator)
12-19-02 23:11
No 390898
Perlite is exploded volcanic rock, where as celite is made by little microrganisms, there should be a huge difference in their properties... my question of the day is, how is vermiculite different from perlite?
(Hive Bee)
12-19-02 23:17
No 390901
Is simular to perlite. It does not humidify things like perlite does. The grain size is way too big and both tend to float. It does provide a looser structure and drainage. Main uses for bees would be hydrophonics and or growing mushrooms using rice cake methods.
Use a dust mask and goggles if handling dry vermiculite or perlite. The dust is awful on your lungs. I would compare it to fiberglass dust.
Not a chemist I just follow directions on the box mix
(Newbee)
03-21-03 12:52
No 419779
Can glass fiber filter also break emulsions as celite?
Paralysis by analysis
(Chief Bee)
03-21-03 22:55
No 419920
Yes, but there is a greater risk of the filter paper clogging up if you have particulates dispersed in your emulsion.
(Hive Bee)
05-01-03 02:45
No 430496
Sorry to drag up this old post but I seem to bee having trouble finding this stuff. I will assume that "Celite" is a brand name. In the pool suppliers I have been to they only stock a product known as "******* Filter Sand 16/30 size grain". The stores I have been to have never heard of "Diamotaceous Earth" either. Would this product suffice for our purposes??? Thanks
when we forget to pray for the angels, the angels forget to pray for us!
(Hive Addict)
05-01-03 03:09
No 430499
Hmm have a 50lb bag of this from the pool store.. is it necessary to run H2SO4 or HNO3 through it (or NaOH for that matter) to clean it up? Or can it be used straight from the bag?
Infinite Radiant Light - THKRA
(Hive Bee)
05-03-03 02:01
No 430977
Set out for a planned voyage to find this stuff recently, thinking it would be a bitch to find. Went to 3 pool/spa stores and 2 carried the same brand Dia-sumthing. $8 for 10 lbs. Now if I could figure out how to use it correctly. The guy corrected my pronounciation when "diatamaceous earth" was requested. So, some do know what it is. Its really fine grain, floats in the air.
(Synaptic Self-Mutilator)
05-03-03 15:58
No 431112
It's pretty easy. Wet the filter paper, suck celite mixed with solvent thru the filter paper, then pour whatever it is you want to filter (e.g. yeast in water, MnO2, etc)
(Hive Bee)
06-18-03 21:30
No 440864
Sparkolloid - found at better Beer & Winemaking stores in the "Finings" section.
---
Sparkolloid
Other names: Celite. Calcined diatomaceous earth. Kieselguhr. Siliceous rock.
Crystalline Silica, quartz aluminasilicate, cristobalite.
(Hive Addict)
07-18-03 06:21
No 448169
I am wondering about the merits of adding Celite directly to an Al/Hg and then filtering the whole shebang.
Celite when put in the buchner first tends to get disturbed, and sometimes clogs, thereby lowering filtering efficiency.
Has anyone had experience with adding Celite directly to an Al/Hg.
If so what are the best Celite/Al sludge ratios? 1:1, 2:1
Any tips appreciated.
SOMETHING WITTY!
(Hive Addict)
07-18-03 14:04
No 448254
(Rated as: good idea!)
Celite when put in the buchner first tends to get disturbed, and sometimes clogs, thereby lowering filtering efficiency.
I usually do the following:
Prepare the Buechner setup and put a sheet of filter paper in place. Take the amount of celite you need and suspend it in the solvent of your reaction mixture. Add a magnetic stirbar and mix the suspension for about 20 seconds. Immediately pour all of the suspension on the buechner filter, while you keep the filter paper in place with a (glass) rod. Turn on the vacuum pump and at the same time, retract the rod. You will get a nice equal distribution of your celite. I have never ever had problems when preparing my Buechner setup this way and always obtained nice results with it
.
Dirty old man
(Hive Adickt)
07-18-03 14:23
No 448258
Doo as GCMS!. Iff you wet the filterpaper, turn the vacum on and then add the celitsuspention, you don't need the glasrodtrick