Dan Vizine
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1/2 Pound Ampoules of Oxide-Free Potassium - The Oil Issue
When making large ampoules of oxide-free potassium, one of the most difficult things to remove is not the oxide, but the residual oil that the
potassium was packed in.
Even if you wash the crude lumps of potassium 3 times in fresh toluene and vacuum dry them, when you remelt them you will still see a film of oil on a
pool of freshly melted metal. See the picture with the 1.
I found that a cannula transfer under UHP argon into another flask through 1/8" 304 SS tubing gave oil free metal. Note the now-shiny surface in the
other rb picture.
The problem was now how to feed this stock into my purification device/ampoule for packaging. You can see in the picture of the glassblowing jig that
a larger oxy-natural gas torch was needed to work the 1 1/2 tubing. A picture of the top of the ampoule is also included to show details. The addition
of a male 24/40 joint to the side of the purification device/ampoule allows ingress of K which is melted by a heating tape. The side arm is reinforced
with steel-filled epoxy as a precaution.
The assembled device with the pad of SS steel wool already inserted up to the glass fingers meant to retain it is also pictured. Vacuum is applied for
an hour before heating begins. During this time the ampoule area (at right) is dried by a bushy oxy - gas flame. The device is inclined and electrical
heating is started. Soon, molten K flows through the SS filter plug (see the picture of the flow just beginning in the ampoule). Once the K has all
filtered, the ampoule is sealed in vacuo.
This ampoule is about a half pound of K.
      
[Edited on 6-4-2014 by Dan Vizine]
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thesmug
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Did you ever get rid of all the oil?
[edit] Also, where do you get these huge ampules?
[Edited on 4/6/14 by thesmug]
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Zephyr
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Wow, that is some beautiful potassium.
Where did you originally purchase your potassium from?
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Dan Vizine
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The K was from GalliumSource (for whom I made the ampoule). It was the standard "packed in mineral oil" stuff. The oil was completely gone after the
cannula transfer since the new K flask was filled with material from beneath the surface of the molten K in the initial flask. If the oil was not
completely gone you would see a cloudy film on the final ampoule, which you don't.
I made the ampoules from tubing. You don't live life as a vacuum-line chemist (a long time ago) without learning to glassblow, it's essential.
[Edited on 6-4-2014 by Dan Vizine]
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Zyklon-A
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Nice! I might make an ampule of K as soon as I can make some. I'm pretty good at glassblowing, I've never broken an ampule before, or had it shatter
when cooling.
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Bert
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Damn. A long, long time ago, at the University of W-------- Grad school's physical science labs, there was a glass shop, complete with lathe, many
different burner heads & arrangements, plus pumps and compressed air/propane still hooked up. With a good bit of leftover glass and no one
(important) useing it anymore, they had gone all metal for the beam lines and vacuum systems related to the 2 particle accelerators the electronics
shop I worked in as a lowly student LTE in served.
My supervisor thought it was cool for me to play with it on my lunch hours... I just wish the techs who had worked in the glass shop had not all
retired before I got access.
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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blogfast25
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Phwoar! Pure potassium porn! (Drooling....)
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Dan Vizine
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...there was a glass shop, complete with lathe, many different burner heads & arrangements, plus pumps and compressed air/propane still hooked up.
With a good bit of leftover glass....
Sweet, Bert. The things I miss most about access to a professional glassblowing shop are the annealing oven and the glass saw. Flame annealing and hot
wire cutting are my fall back options.
Nice to hear someone say that ZyklonB, I meet fewer and fewer people who are confident they can. I also have to remember that not everybody has oxygen
cylinders strapped to their basement walls.
You guys know about the hot wire technique? You can cut almost any size glass cylinder or tube neatly. If anybody wants a description I'll post one as
I can. You need thin Nichrome wire and a Variac and some misc. stuff.
[Edited on 7-4-2014 by Dan Vizine]
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Dan Vizine
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Quote: Originally posted by Zyklonb  | | Nice! I might make an ampule of K as soon as I can make some. I'm pretty good at glassblowing, I've never broken an ampule before, or had it shatter
when cooling. |
Incidentally, a technique for small tubes was published by a user who calls himself "Zan Divine".
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blogfast25
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Are we to believe that he, aka 'The King of Caesium', is not you?  If so, I'm
the Scarlet Pimpernel...
[Edited on 8-4-2014 by blogfast25]
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Bert
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Oh Cesium-
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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Dan Vizine
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| Quote: Originally posted by Dan Vizine | | Quote: Originally posted by Zyklonb | | Nice! I might make an ampule of K as soon as I can make some. I'm pretty good at glassblowing, I've never broken an ampule before, or had it shatter
when cooling. |
Incidentally, a technique for small tubes was published by a user who calls himself "Zan Divine". |
Someone has listened to the Doors too much and yet failed to come up with an anagram even 1% as cool as Mr. Mojo Risin'.
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