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Zan Divine
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Blogfast25...
Yes, I think this is the answer. Why strive to exclude all O2 from a big fat bag when it's much easier to do it for individual pieces of glassware
with rubber septa?
vmelkon....
I just put the lithium (as a few large pieces) into the reactor and dumped the CsCl on top of it. As the Li melts at ~170 C, the solid CsCl should
sink into it. Further mechanical mixing is apparently not an issue.
The mixing issue was another reason to opt for Li over Ca as reductant. I am inherently uncomfortable with solid phase reactions and the Ca doesn't
melt. I assume the vapors of the volatile CsCl react at the solid-gas interface that is the surface of the calcium but I favor the liquid reductant
being in direct contact with the CsCl.
The Li was in the form of a solid ingot as purchased. By the time it was cut and weighed (I haven't found an easy way to cut this gummy metal, it is
considerably harder to cut than Na. Saw teeth gum up & knives require a lot of force. A cold chistle is a workable but graceless option) it was
entirely coated with Li3N. I read or hallucinated that Li3N reverts to Li when heated, so this wasn't too troubling.
I have had weird experiences with Li manipulation ...contradictory observations. As received, the Li ingot turned black within less than a minute of
air exposure. However, if I add Li to a heated steel piston and extrude blobs of melted Li into a collection container, this silvery looking metal is
considerably more air-resistant and takes several minutes to begin to darken. Has anybody else made similar observations?
Fleaker....
I found your post both happy and depressing.
The offer of Rubidium is received with real heartfelt appreciation. The generosity of your offer is mind-blowing and I can't thank you enough. I need
to look around on this site to see how to contact you directly
Simultaneously, I thought this was a novel bit of basement chemistry but now I realize that others have preceeded me. C'est la vie.
What's left for the curious? Just F, I think. Unforgiving, hellishly reactive and very toxic. I guess I should check and see if it has been done here
before.
If I had a diffusion pump I'd love to redistill the Cs and get 99.9%, or better, metal but there are few inexpensive ones on e-bay. Making one from SS
(I don't have the ability to melt and form very large diameter pyrex) could be a project in itself.
As far as this run was concerned, the appratus was designed to allow both the application of vacuum as well as argon via a t-joint with appropriate
tubes and hose clamps. When the reaction was over and the bomb cool, the appratus was refilled with Ar before removing the flask with the Cs from it.
As soon as I hit the "pay" button for my new glass syringe, I realized that transfer needles were a better option. I had some ~1/16" OD SS tubing
laying around. After trimming and grinding beveled needle points on some, I found that I could easily force Hg through the line and into other rubber
septa-sealed glassware by gentle Ar pressure. I must have been away from the lab too long since that should have been the first thought. Better late
than never, I suppose...
[Edited on 24-12-2011 by Zan Divine]
[Edited on 24-12-2011 by Zan Divine]
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Fleaker
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Zan Devine,
If you look at plastics's post upthread, you'll see that he mentions that Len had made some Cs and had already published the experiment (by that I
mean he literally published it in his excellent book).
I think I had beaten Len to it at that point--I did the Cs experiment in 2009 I think, or perhaps 2010. I've yet to write it up, because I was going
to do it on the kilo scale and post that. I can recommend some improvements to the collection and re-distillation of the metal. I also have the synth
of Rb, black phosphorus (limited success), an excellent method for bromine, and a few other synthetic curiosities to post. Unfortunately, my day job
is also one I take home every night and every weekend and my laboratory is busy with projects that make me money, but aren't necessarily fun. I work
in the precious metals field.
[Edited on 25-12-2011 by Fleaker]
Neither flask nor beaker.
"Kid, you don't even know just what you don't know. "
--The Dark Lord Sauron
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Zan Divine
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Hi Fleaker,
Yes, I saw the reference to Len's work earlier.
I'd be interested in hearing any suggestions you may have on the distillation/collection phase of this work. One kilo, huh? That's a lot of money even
at the generally agreed upon value of Cs in bulk, namely $10/g.
I've always enjoyed the chemistry of the coinage and platinum group metals. Once you get them oxidized, anyway.
We made a few gold compounds for the NCI cancer program and lots of platinum ones starting from 60 ounces of the metal.
The bromine prep. I favor is the MnO4- oxidation of HBr generated in situ from H2SO4 + KBr. There are so many of them, but at least this one avoids
interhalogens.
Black P...interesting! It seems to require rather extreme conditions. Nice when your hobby overlaps with your profession so that you have advanced
facilities at your disposal. I'm guessing you didn't do this at home?
Concerning the RbCl you mentioned earlier, you can contact me at Bull8hit@hotmail.com. Or, if you prefer, I'll contact you if you post a method.
That's not my usual e-mail so if you do send anything, let me know here so I'll know to check it. Thanks!
[Edited on 27-12-2011 by Zan Divine]
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Zan Divine
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As I needed to handle, purify and (for another outlet), package exhibitable samples of shiny lithium metal, I looked around and found a lot of
piecemeal info on the topic and it is assembled, for anyone interested, in this PDF.
Attachment: LITHIUM HANDLING.pdf (64kB)
This file has been downloaded 3934 times
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Zan Divine
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And here is the final commercial product....
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haroldramis
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I see you have them listed on eBay. You also have a purity listed for them(95% for one of them i think). How did you measure the purity of your
Cesium?
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Zan Divine
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I have no means of accurately measuring purity. The samples listed as 99% were prepared according to the previously listed US patent and it claimed a
99% purity for the conditions I used. The metal is entirely silver with a trace of golden color. No trace of any visible oxidation beyond that which
causes the trace color.
The 95% sample was estimated by visually comparing the relative volumes of the small amount of lightly oxidized material to that of the bulk.
Neither sample is currently listed as I see what I have to do to ship legally.
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Zan Divine
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Quote: Originally posted by Fleaker  | | Welcome to the cesium club! As congratulations, I can send you RbCl so that you can make that as well. I have a 50 or 100 g bottle to spare.
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Hi Fleaker,
I noticed you read my communications. It's been some time, but I haven't heard back from you. Do you still mean to do this? I have the time and
materials to do this, except for the RbCl. I also have people waiting for Rb samples and I keep telling them I don't know where this stands. So, when
you can, please let me know. Thanks.
[Edited on 21-1-2012 by Zan Divine]
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blogfast25
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Very nice, indeed. How much is there?
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Zan Divine
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Hi Blogfast25
I've only converted a small portion of the CsCl to metal. And only part of the last batch has been ampouled up simply because I lack an effective
outlet due to shipping regulations. I have made about 14 ampoules total. Each contains from 1.4 to 1.7 grams (from 27 mm long to 33 mm long samples in
6 mm ID tubing).
I can only sell locally (and not on e-Bay or Craig's list, it violates their User Agreement).
In the long term, the shipping regulations on the fun things from groups I and VII that I like to sell have changed my plans. I'll still make Rb if I
can obtain RbCl (after all, I still need a sample and the apparatus is already built). But production sized white P seems pointless and none of the
anticipated cashflow to try to build a F2 electrolysis/purification/packaging setup will materialize.
The F2 synthesis might just have become unnecessary, anyway. A fellow collector sent me a picture of himself holding two fluorine tanks. He has access
to pretty advanced facilities judging from other things he offers and says he makes. I am optimistic that he may make some quality samples.
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blogfast25
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To sell home produced Cs or Rb you might want to consider just doing the producing part and sell your product to various element collector outlets,
because setting up the marketing and advertising infrastructure (and for a ‘one product shop’ too) might be even more expensive than sacrificing
some of your margins by selling to known middlemen.
To try and beat the ‘known suspects’ (Sigma, Merck etc etc etc) at their own game with just one or two products is also planning to fail IMHO.
Just my two cents…
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Zan Divine
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Hi Blogfast25,
I could easily beat the usual suspects for the simple reason that they don't sell to individuals. If they did, Strem ($58/g, 99.5%) and the others
would drive sellers like GalliumSource.com ($140/g 99.5%) out of the Cs selling market overnight.
Actually, considering that I'm selling, on average, 1.5g for $50, est. 99% and that my cost for raw materials to make that was less than $1.50, if I
could just ship this it would be flying off the shelf and be very profitable. In the time it was e-bay (1 day) it drew lots of attention and an
immediate sale, which I refunded.
This was never intended to be a business. It's just how I've keep my net expenditures as I've collected elements to $0. As my remaining targets become
more costly, I use products like this to offset the increases.
Well, it's good that I've still got platinum for that purpose. You can't be a synthetic chemist all your life and not have accumulated that. At $80/g
I can undersell ....everyone. Except chemical houses and again, they don't count. My beads may not be electron beam melted, but platinum doesn't
especially need that since it doesn't react with oxygen at any temperature. Right now it's Pt black but an oxyacetylene flame on the oxidizing side
gives very shiny metal. I'll only be asking 100% over spot instead of their 300 - 400%. It may not be the sensation that cheap Cs was, but at least I
can go back to shipping from my front porch!
[Edited on 21-1-2012 by Zan Divine]
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Fleaker
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I thought this could go ORM-D if it's small quantities, much like sodium. If not, it'll have to be hazmat pack.
Meant to get back with you, but I've been busier than hell.
Anyway, I'll put the RbCl in the mail. I'll probably put a couple kg of CsCl in the mail too with check for Li.
Past couple weeks I've sold thousands of grams of Pt, but it certainly wasn't for $80/g!
If you want to sell all of that Pt, and any of the rest, let me know.
Neither flask nor beaker.
"Kid, you don't even know just what you don't know. "
--The Dark Lord Sauron
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blogfast25
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| Quote: Originally posted by Zan Divine | I could easily beat the usual suspects for the simple reason that they don't sell to individuals.
[Edited on 21-1-2012 by Zan Divine] |
I meant by breaking into their traditional, almost captive market: 'institutional science'; they've pretty much got that fenced off.
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Zan Divine
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Hi Blogfast25,
Ahhh, now I see what you meant and I agree. I never expected to sell to researchers or institutions.
The only target audience I had in mind was collectors. They are the ones who get raped for what amounts to ...let's see...$140 +
shipping..(GalliumSource pays the Hazmat on orders over $100).. must be at least $160 for a gram of Cs. Absurd.
Another reason I was doing any of this was because of the bond I feel with other collectors. I really enjoy delivering a long sought after sample to a
fellow collector. It really works out well for all involved.
[Edited on 22-1-2012 by Zan Divine]
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Zan Divine
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Hi Fleaker,
Thanks for the speedy reply. I was wondering if you were still interested in the RbCl --> Rb thing after I had replied that I simply can't take on
the large scale Cs project.
It wouldn't be fair to you for me to accept this piece of work. This type of thing is just a hobby for me. Moreover, my regular job has me on a very
unpredictable schedule, while you have a production schedule to keep with your clients. Even if my reactor were larger, ( I'd need from 16 to 20 runs
to process 2 kg with my existing setup) the amount of time it would take just makes this unworkable.
And payment in Cs metal would really not do me much good.
I've already got enough Cs (and potential Cs as CsCl) that I'll probably be throwing some of it into water this summer.
As nearly as I can tell, Cs cannot go ORM-D in any amount. I guess the fire hazard is paramount. When I meet buyers, I transport the Cs ampoules in a
short length of 1/2" pipe with the ends capped. I consider this to be absolutely bulletproof. Anything that can rupture that $3 overpacking is already
so severe that a gram of Cs is a fart in a windstorm by comparison. If only the mail services could grasp this, but it is beyond their comprehension
or imaginations. They aren't real receptive to logical arguments. "Rules are rules" is their mantra.
I defy anybody to suggest a reasonable scenario (not something like...what if the pipe has a defect?. They don't.) under which this container could
fail. No fire could breach this. It would take a devastating impact to open it. By any reasonable acessesment, this is utterly safe. But, it still
can't ship by anything but Hazmat.
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blogfast25
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Logic doesn’t really come into it, no. In their defence I’d say that they want to keep the rules simple and that postmen aren’t scientists or
engineers.
So what company would you use to ship ‘bullet proof’ Cs samples with and how much would it cost?
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Zan Divine
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Therein lies the irony. Despite being impervious to damage & leaks, I still can't ship it USPS, UPS or FedEx.
The authoritie's panties apparently bunch up rather severly on this issue. The same day the Cs went up for sale, I got a friendly warning letter from
another collector. I'll reprint part of his two e-mails:
just a heads up i got arrested for shipping sodium through the USPS, i got fined a large amount am now on probation for two years.... I had the
FBI and the postal
inspector show up at my house. believe me it is NOT worth it between the fines and the lawyer fees and having it on your record for the rest of your
life..
it was bad, they seized my computer and my entire element collection. I got it all back since it wasn't illegal to own those items. i was out the next
morning on a 1000 bond, which only cost me $150. i took a plea for two years probation and a hefty fine which is partially due to the hazmat team
coming
to my house to make sure it wasn't dangerous and that i wasn't making any bombs. it turns out i sold the sodium to an FBI agent....it was very scary
to see how much info they had on me. my discovery file was about 100 pages long. it had emails photos of me at the post office, posts on various
forums.
...but overall I'm about 10k in the hole because of it.
Hazmat shipping is inherently incompatible with lower cost items. I've heard different costs for the service, starting at $25. People balk at spending
$50 for an item that then costs them another $40 - $50 for Hazmat compliant shipping which includes special packing, the fee & the actual shipping
cost.
But Hazmat, to UPS anyway, means "things that are slightly intimidating" instead of "hazardous materials". See the picture below for all the things
they don't accept in the "UPS small package division".
"Poisons" fellas, really?! Hmmm...Where is the emoticon with eyes rolling back into the head?
This suggests to me that I can't ship with them. I'll concede that I may be wrong about exemptions simply because I can't say I'm definitely right
after looking through 49 CFR. I'm probably going to end up calling them to ask, but I'm not optimistic. I wonder how GalliumSource does it? It's
possible somehow...
All in all, I'm more confused now than when I started writing!
[Edited on 23-1-2012 by Zan Divine]
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blogfast25
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Ouch: 10 k in the hole for practicing a legal hobby. Land of the Free?
GalliumSource must have similar problems: $140 for 1 g of Cs ('Free shipping' my *rse) can only be explained by high shipping cost. Perhaps you should
by a gram and see who and how it is delivered to your doorstep?
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Zan Divine
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Actually, Blogfast25, I'm going to just do what I should have all along...just call some postal officials and ask them.
I was quite confused after trying to interpret parts of 49 CFR. You get used, with the internet, to finding your own answers. I have no doubt that I
found them. But that's not worth much if you don't understand them.
For what it's worth dept:
Metallium, Inc. lists the hazmat fees for the following;
Group I metals $70
Bromine $35
Hg & Ga $25
It's a little hard for me to see the logic. Br is clearly a greater shipping hazard than Li. And an Hg accident, given the cost of clean up, could
argueably be as bad as most of group I. I thought that Ga couldn't ship by air because planes are largely aluminum. So, why is this Hazmat at all if
it ships by ground? It sure isn't a real toxicity concern.
One site that ships Cs gives this info:
Shipping Information:
Cesium, 4.3, dangerous when wet, UN1407, PG I
I would have thought that Cs would be "spontaneously flammable". NaOH is dangerous when wet. Hmmm, if they can classify it as merely "dangerous when
wet" and it flies, maybe there's hope. This class has some wiggle room if I'm reading my last posted picture correctly.
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watson.fawkes
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| Quote: Originally posted by blogfast25 | Ouch: 10 k in the hole for practicing a legal hobby. Land of the Free?
GalliumSource must have similar problems: $140 for 1 g of Cs ('Free shipping' my *rse) can only be explained by high shipping cost. Perhaps you should
by a gram and see who and how it is delivered to your doorstep? |
Shipping regulations are written
conservatively because there are lots of both foolish and venal people that will externalize risks onto the carrier and the public. The hobby is
legal, but like it or not, the shipping regulations are strict.
I am pretty sure that GalliumSource is simply rolling the cost of hazmat shipping into the base price of the product. It's essentially a marketing gag
to avoid having to educate a consumer about how expensive hazmat shipping really is. That feeling of offense that shipping isn't free, while emotional
and not rational, will still cause lost sales.
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blogfast25
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Watson:
Regulations, like laws (or any other texts), require interpretation. It becomes quite absurd when someone is willing to go to quite extreme lengths to
minimise the risk posed by the shipped product and STILL can't find (at least up to now) anyone who wants to do the running and get paid for it quite
handsomely! The packaging he proposes is probably safer than a can of Draino conc. H2SO4, as well as shipped in much smaller quantities. This isn't
just about safety, there are commecial interests at play here...
Regulations that regulate handling and shipping of small amounts of chemicals for hobby use often resemble a pneumatic drill to crack a peanut with...
[Edited on 23-1-2012 by blogfast25]
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watson.fawkes
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| Quote: Originally posted by blogfast25 | | It becomes quite absurd when someone is willing to go to quite extreme lengths to minimise the risk posed by the shipped product and STILL can't find
(at least up to now) anyone who wants to do the running and get paid for it quite handsomely! |
It helps to
actually read the regulation. The UPS image posted shows a restriction for "dangerous when wet" materials unless they satisfy 49CFR173.13. That's an
easy regulation to go read, and specifies what that regulation considers adequate packaging.
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UnintentionalChaos
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Group 1 metals can't ship by USPS, period, end of story, no matter how well packaged they are. Galliumsource ships group 1 elements by FedEx for a
reason. http://pe.usps.com/text/pub52/pub52apxa.htm
Department of Redundancy Department - Now with paperwork!
'In organic synthesis, we call decomposition products "crap", however this is not a IUPAC approved nomenclature.' -Nicodem
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Zan Divine
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A point worth making is the lack of gradation in the fees. Ship 5 g of Na or 5kg...same Hazmat fee. That is a perfect example of an absolutely
ludicrous one-size-fits-all rule that probably indicates a certain degree of laziness and short-sightedness among the people who devised the cost
structure.
Most other aspects of shipping are graduated, here it's all or nothing. You are never going to convince me that shipping collector-sized samples is in
any way equivalent to shipping in bulk. Except for the Hazmat fee.
Of course, if you one of those people who are inclined to see a 2 or 3 gram sealed ampoule of bromine as the same risk level as 1 kg, why would I want
to argue? Logic likely doesn't play a big hand in your opinions.
And on that note, I apologize for getting this off on the wrong track. My shipping abilities/impossabilities are not only not of scientic interest,
they are boring, as well. I'm not going to waste any body else's time on this subject.
[Edited on 23-1-2012 by Zan Divine]
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