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Author: Subject: Cesium from CsCl
mr.crow
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Zan Divine, you are a hero!

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elementcollector1
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I hate to ask this again, but it has been quite a while, so... How could I get my hands on a small amount of elemental cesium?

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Zan Divine
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Cesium is available on e-Bay currently.

[Edited on 8/14/2012 by Zan Divine]

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haroldramis
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They look nice.
I never heard of the 1g exemption though. Do you have a link or reference for it? I remember last time you tried to list it was de-listed as there were shipping issues.
Zan Divine
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 Quote: Originally posted by Zan Divine Cesium is available on e-Bay currently.

...and now it's gone.

He who makes a beast of himself gets rid of some of the pain of being a man. --HST

Sublimatus
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All bought, or forcibly removed?
Zan Divine
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Sold to forum member off e-Bay.

Actually, both (I only advertise 1 at a time on e-Bay).

More ampoules will likely take time. Ripped a calf muscle and I'll be in a cast after surgery. Getting my exhausted O2 cylinder out of the basement and refilled is a task even with both legs. So, unless and until I get someone to do this, no ampoules can be made.

[Edited on 8/17/2012 by Zan Divine]

He who makes a beast of himself gets rid of some of the pain of being a man. --HST

elementcollector1
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Ouch! We can wait for the cesium, then.

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BromicAcid
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 Quote: Originally posted by haroldramis They look nice. I never heard of the 1g exemption though. Do you have a link or reference for it? I remember last time you tried to list it was de-listed as there were shipping issues.

173.4b De minimis exceptions.

 Quote: (a) Packing Group II and III materials in Class 3, Division 4.1, Division 4.2, Division 4.3, Division 5.1, Division 6.1, Class 8, and Class 9 do not meet the definition of a hazardous material in §171.8 of this subchapter when packaged in accordance with this section and, therefore, are not subject to the requirements of this subchapter. (1) The maximum quantity of material per inner receptacle or article is limited to— (i) One (1) mL (0.03 ounce) for authorized liquids; and (ii) One (1) g (0.04 ounce) for authorized solid materials;

This is the regulation that a DOT rep quoted me when I asked if I could have a vial of bromine hanging from my rear view mirror back when I was attending hazardous waste conferences. Although with some of the other stipulations written in the remainder of the reg I have my doubts if a glass vial hanging from a mirror would really pass the test although let's face it, not many people would recognize it for what it was.

Edit: Looked up cesium in the shipping table, it's actually a packing group I so this wouldn't apply. Then again, so is bromine.

[Edited on 8/18/2012 by BromicAcid]

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elementcollector1
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Haha, I'd love to see that car.

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elementcollector1
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Topic bump! Anyway, I was wondering: What are the major difficulties of distilling cesium? Namely, if I welded together a good steel reactor for distilling with lithium from batteries, or pure sodium / magnesium / calcium (depends on which works best), and connected that to a glass receiving tube under vacuum (what strength vacuum to use? I'm assuming pretty high), and simply melted the end of the tube off so as to make an ampoule, would that work? Or are there things I've not considered here? First things first, to get some cesium compounds.

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blogfast25
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EC1:

Everything you need to know is really in this thread. I suggest you print it off and as the man says because this is no sinecure if you haven't done it before!

'Roger' to getting reasonably priced CsCl (all the others need messy conversions): that's the first serious hurdle!

MyNameIsUnnecessarilyLong
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 Quote: Originally posted by elementcollector1 connected that to a glass receiving tube under vacuum, and simply melted the end of the tube off so as to make an ampoule, would that work? Or are there things I've not considered here?

I created an o-ring adapter for connecting ampoules directly to my condenser. The neck on these ampoules should be long enough for me to pull it out (after the cesium drains from the condenser) to near the front o-ring then melt and squeeze it shut. I haven't got around to testing it yet, though. After I made it I got a feeling that the thin-walled ampoules I'm using might cave in at the molten areas under high vacuum. Thick-walled tubing probably wouldn't have this problem, and that's probably what you should go with if you do at all.

http://i47.tinypic.com/2cfqt6g.jpg

http://i45.tinypic.com/eb6fix.jpg
elementcollector1
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Is steel required for the receiving end? I seem to remember the cesium-pioneers on this forum using glass.

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MyNameIsUnnecessarilyLong
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 Quote: Originally posted by elementcollector1 Is steel required for the receiving end? I seem to remember the cesium-pioneers on this forum using glass.

Glass is fine. The hard part is connecting it to the reactor, which has to be steel/stainless/iron. Zed accomplished this by using a metal taper to glass joint. If you go with a metal taper, the neck needs to be long enough so that the taper itself won't heat up from the cesium or heat of the reactor.
elementcollector1
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What about the condenser; can this be glass as well? Again, according to Zan's original setup, it does work (although again, there is that metal taper to think about)...
Also, will a hand vacuum pump be any good for the vacuum required, or will a real pump be necessary?

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blogfast25
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EC1:

Pressure ranged from 0.005 to 0.07 mm Hg, although one specific run stands out at 700 mm Hg (and still yields about 50 %!)

The kind of vacuum pump used by Zan is a couple of posts below that one. Higher vacuum makes distilling the Cs metal easier.

elementcollector1
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So, according to that, more vacuum = more %yield, instead of high vacuum = results.

If I get an aspirator (and presumably do something to prevent the water running through it from vaporizing and hitting the cesium, though I don't know what - more dry CsCl in a trap, so the Cs won't react?), I apparently get down to 23-24 torr just from water (which, while not being quite so good as the vacuum pressures listed, should work).

A hand pump apparently will only pull a measly 620 torr, not nearly good enough for my standards even if it does remove the dangers of water vapor.

Vacuum pumps? Far too expensive, and not even the school lab has one. The university has them, but I don't know what those pull (and even if I did, there's no way they'd let me borrow one).

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blogfast25
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Yes, but I'd go with the highest vacuum possible, if given a choice.

Dan Vizine
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I am, btw, Zan. Another batch of Cs will be whipped up soon and it will be the purest yet as the reductant is 99.8% Ca (same as my ThO2 redn.)

What's expensive, really? Look at what you gain. Your time is neither endless nor free. The vacuum pump is one of the most important items in any synthetic lab. I got mine on eBay for $80 shipped, an untested unit. The main shaft seal is leaky, so what? The vac. is 0.002 mm Hg. I can recycle the filtered oil. Someday I'll find the time to replace it. elementcollector1 International Hazard Posts: 2684 Registered: 28-12-2011 Location: The Known Universe Member Is Offline Mood: Molten$80? Lucky. I think I will try first with the aspirator pump and a drying agent - but that's after I get the setup finished!
I now have access to (but not ownership of) welding equipment, so I'll see if I can get something put together.

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Dan Vizine
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Remember you need a fail-safe back flow preventer in the vacuum line. City pressure varies and when you are already pulling the best vacuum that your aspirator can, and water pressure drops because of demand changes elsewhere, water quickly backs up into the device under vacuum.

Also, welding ends onto SS pipe is very difficult. The coefficient of thermal expansion is large and cracks and pinholes are common. I brought half of a lecture bottle to a professional welder. He tried to weld a 316 bottom on. He failed to achieve gas tightness just as I had a half dozen times earlier. The composition of this bottle, which held NOCl previously, was unknown.

If you are operating at 10 mm Hg you could save lots of work by using common plumbing fittings. If you prefer to weld stick to mild steel.

[Edited on 18-4-2014 by Dan Vizine]
Dan Vizine
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Here's an idea. To transit from pipe to glass, just use a rubber stopper. Make sure the metal tube sticks out 1/2 inch past the bottom of the stopper. The stopper holds vacuum just as well as your rubber vacuum hose. The more I play with it, the easier it gets to make an apparatus, that functions well, out of simple materials.

Incidentally, for $40 you can buy a pre-manufactured 300 mL SS reactor on eBay right now. http://www.ebay.com/itm/191081558900?ssPageName=STRK:MEWAX:I... Unless you value your time at less than a few dollars per hour, how can you beat that? Also, the price of CsCl 99.9% or better is about$40/100g because ppl. use it as a putative cancer treatment. Google it and you'll have no problems.
Dan Vizine
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Quote: Originally posted by MyNameIsUnnecessarilyLong
 Quote: Originally posted by elementcollector1 connected that to a glass receiving tube under vacuum, and simply melted the end of the tube off so as to make an ampoule, would that work? Or are there things I've not considered here?

I created an o-ring adapter for connecting ampoules directly to my condenser. The neck on these ampoules should be long enough for me to pull it out (after the cesium drains from the condenser) to near the front o-ring then melt and squeeze it shut. I haven't got around to testing it yet, though. After I made it I got a feeling that the thin-walled ampoules I'm using might cave in at the molten areas under high vacuum. Thick-walled tubing probably wouldn't have this problem, and that's probably what you should go with if you do at all.

http://i47.tinypic.com/2cfqt6g.jpg

http://i45.tinypic.com/eb6fix.jpg

You're right. They collapse very easily. A deft touch and a really small torch (like the butane-oxygen models by Archer @ Radio Shack. IF they still carry them) are best. This is not easy. Highly suggest glass tubing. Much more durable too.

Oh, and another thing...the Cs will wet glass. You'll have trouble sealing any glass over which the molten metal flows. That's why I collect in one thing and use syringes (plastic) to move the Cs around for sealing.

[Edited on 18-4-2014 by Dan Vizine]
elementcollector1
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Why not combine both ideas and include a sort of drip tube that centers the caesium distillate so it drops into the center of the ampoule?

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 Sciencemadness Discussion Board » Fundamentals » Chemistry in General » Cesium from CsCl Select A Forum Fundamentals   » Chemistry in General   » Organic Chemistry   » Reagents and Apparatus Acquisition   » Beginnings   » Responsible Practices   » Miscellaneous   » The Wiki Special topics   » Technochemistry   » Energetic Materials   » Biochemistry   » Radiochemistry   » Computational Models and Techniques   » Prepublication Non-chemistry   » Forum Matters   » Legal and Societal Issues