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neutrino
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Another Update
I haven’t done too much with the Bi lately, but I am playing with an idea. Basically, Bi is melted under a liquid of some sort. The liquid keeps air
from the Bi and thus prevents sticking due to oxide formation. The problem is, what do I use? It has to be something inert at ~280*C (no phosphoric
acid), does not evaporate considerably at this temperature (glycerin, vegetable oil), and can be cleaned from the crystals (no silicone oil,
unfortunately). Any thoughts?
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BromicAcid
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Many brands of mineral oil (rock oil) have very high boiling points, anywhere in the range of 260 - 360 C depending on the manufacturer, I
consistently use it for oil baths near 200 C and I've tried to use it higher (for a blanket in NaOH electrolysis). Cheap and widely avalible and
you can use it as a laxitive 
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sparkgap
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"...you can use it as a laxative..."
Yeah, but lipid pneumonia isn't nice to have, so don't. 
A question for neutrino: do you have a picture of the biggest Bi crystal you ever grew? 
sparky (~_~)
"What's UTFSE? I keep hearing about it, but I can't be arsed to search for the answer..."
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neutrino
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Really, mineral oil? I would have thought it would smoke far below these temperatures (paraffin does). Well, it’s worth a try. I just wish my
hotplate hadn’t died again yesterday.
The biggest crystal I’ve grown so far is 1.5 x 2.5 x 1 cm. It grew as a result of uneven cooling (too much on the top). A picture will follow.
edit: I just remembered that someone borrowed my camera for a trip, so those pictures will be delayed a few days. I finally fixed my plate, time to
play with that.
edit2: I fixed the plate (again) and tried some mineral oil. It smoked excessively by the time the Bi was molten. I guess I need a new brand...
[Edited on 22-5-2005 by neutrino]
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neutrino
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Well, my search has not found anything feasible yet. A summary of all the materials tried:
Glass beaker: sticking, nucleation.
Coatings on glass:
Plaster: Best nonstick properties, nucleation over entire bismuth-plaster boundary.
Charred gelatin-based glue: weak, nucleation.
Charred oil: Not as weak as glue-based coating, nucleation.
Charred sugar: excessive foaming during charring leads to weak, unreliable coating.
Charred plaster + glue: Similar but inferior to pure plaster.
Teflon: Sticking, possible decomposition.
Salt (NaCl): Sticking, nucleation, impossible to get an even coating.
Liquids added to melt (to prevent Bi sticking to glass):
Mineral oil: Boils, chars.
Butter: Boils, chars.
Vegetable oils: Smoke somewhat, char slowly where contact with air is present, no unwanted nucleation, no sticking.
HDPE: Smokes excessively with decomposition.
Soap (synthetic): Smokes excessively, chars and decomposes.
Sodium Acetate: Chars, decomposes.
Other crucibles:
Nickel crucible (with heavy surface oxidation to prevent alloying): sticking, nucleation (probably over entire Bi-NiO boundary).
Aluminum crucible: same as nickel.
So far, the best material is vegetable oil, meaning that I’m right back where I started. I’m running low on ideas, having tried just about
everything within my reach. Does anyone have any other ideas that could possibly work? What I don’t understand is why nothing can even come close to
matching that simple copper crucible.
Before I forget, here's that picture:
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12AX7
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Ooo, nice
If you want a cover flux, you might try a low-melting chloride - bismuth should be low enough potential to support just about anything, let's
see, hey it's about the same voltage as copper in fact. Lead chloride comes to mind, *cough* if with poisonous fumes. An eutectic could be
mixed with other common chlorides to get melting point down to bismuth range.
Tim
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neutrino
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I’ve looked into salts and the most feasible thing I found was indeed bismuth chloride. Unfortunately, it would require burning Bi in a stream of
dry Cl<sub>2</sub> to make. Eutectics might work. Where could I find a chart of these?
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12AX7
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You can find a list of SGTE phase diagrams on Fact-web, the tree sort page is here:
http://www.crct.polymtl.ca/fact/xmltree/pdTree.php
And one I found on here in an old thread:
http://ras.material.tohoku.ac.jp/~molten/molten_eut_query1.p...
Making copper chloride doesn't seem too hard, you should be able to do the same with bismuth by piling chunks on top of pool chlorine in a narrow
glass column and dripping HCl over it. Lead chloride of course can be made by refluxing lead with HCl.
Hm, BiCl3 decomposes to oxychloride, though apparently that is soluble in HCl. Probably a good idea to use more stable chlorides then. Maybe
something using FeCl2?
Tim
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neutrino
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Thanks for the links. I looked through everything and didn’t find anything suitable that I could make.
There’s one big problem with BiCl<sub>3</sub>. Bi doesn’t dissolve in HCl, so it has to be made by some other way.
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12AX7
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You sure? How about KCl-ZnCl2? (While you're making the ZnCl2, save some for tinning as well. )
Tim
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neutrino
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I'd forgotten that Zn was readily available. Time to start dissolving pennies.
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IrC
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I think you are making things hard on yourself. I bought 50 pounds of very pure bismuth, do not know the number but it appears from reading this
thread it must be 99.9 % or close. Anyway, I took a neat little aluminum pan that had a handle on it and cooked it hard in my kiln, keeping it well
below actually melting metal of course. This just to be sure it was positively coated with oxide, but still a shiny aluminum pan in appearance. I have
a little metal melting pot I bought on ebay which the pan fits into. Filling it up with 10 gram Bi pellots, and melting them, there is zero sticking.
Every time. I think you should be raiding your kitchen for bismuth melting implements!
I built a pyramid using the golden rectangle math thing and cast a couple pounds into it. The only problem I had was a crystal an inch long grew out
of the bottom of the pyramid (it is cast upside down so that pyramid bottom is liquid surface) as it very slowly cooled, which I had to cut off so as
to make the bottom smooth.
In a conversation with Patrick Flanagan (the famous neurophone inventor) years ago about pyramid power, I remarked that I believed the term most
people miss in pyramid power is the MASS, not just the shape. He made the comment that he would take discharged nicads and put them in homebuilt
pyramids and see no change in measured voltage. But on a trip to Khufu he went inside and did the same tests, measuring over a one volt rise and so he
agreed that the mass was a factor here. Anyway, this is not the subject of the thread but I thought I would throw that in.
In light of the facts I mentioned here, I have been casting really large quantities into correctly shaped pyramids in the hope of calling ET or in
general doing something or other mad science related. The point being if the aluminum dish has been heated in the past, I have zero tendency for
bismuth to stick, or alloy, with aluminum. Try that instead of glass, oils, or whatever else you have been playing with. It also casts nicely into
wood, kiln fired clay, and plaster. I would like to know though in anyone has any cool ideas how to stop these really big crystals from coming up.
What I am describing here is say I fill 5 pounds of molten bismuth into a form shape, which is upside down, so that you are looking at the bottom as a
layer of molten liquid, perfectly flat due to gravity. If I cool it very slowly without any trace of vibration to the form, suddenly I will notice
large shapes start to grow up out of the surface as it cools, sometimes several inches tall. When I cut these off to smooth the surface (the bottom of
the pyramid), I notice very large crystalline structures, very shiny and no trace of color (inside the cut crystal, the outside of the cast pyramid
looks beautiful!). Probably something you are trying for but to me a big pain.
The more I play with this stuff the more I am starting to believe Bismuth has just got to be one of the strangest elements on the chart. Certainly an
element no true mad scientist should overlook playing around with!
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12AX7
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| Quote: | Originally posted by IrC
If I cool it very slowly without any trace of vibration to the form, suddenly I will notice large shapes start to grow up out of the surface as it
cools, sometimes several inches tall. When I cut these off to smooth the surface (the bottom of the pyramid), I notice very large crystalline
structures, very shiny and no trace of color (inside the cut crystal, the outside of the cast pyramid looks beautiful!).
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Neato Wish I could get growth like that with any metal I have on hand... my
99.9% lead and aluminum only make at most 1/4" difference in height from peaks to valleys in the cubic crystals formed.
| Quote: |
Probably something you are trying for but to me a big pain.
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Try alloying with up to 20% or so of lead, tin, zinc (Zn doesn't mix well with Bi or Pb, no more than 1.5%), uh indium, cadmium, whatever white
metals you have on hand.
| Quote: |
The more I play with this stuff the more I am starting to believe Bismuth has just got to be one of the strangest elements on the chart. Certainly an
element no true mad scientist should overlook playing around with! |
Being a nitrogen column <I>metal</I> it certainly combines a number of properties.
Tim
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IrC
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I have several ounces of Gallium, thought about putting some of that in the mix. I was reading MSDS's and realize how useless those things really
are. A dozen different ones say a dozen different things! One tells not to put Bi with aluminum, reactivity problem and so on, but I haven't
blown anything up yet. I imagine heating my Al container beforehand is the reason, I doubt bismuth has much use for sapphire. I notice the MSDS will
give all the poison warnings, a 1 for health and mentions liver and kidneys, but the ones for lead are worse a 2 with no mention of target organs. I
have been soldering for 30 years and the only thing I notice is bouts of kidney problems from time to time. One thing I did wonder about was the
mention for Bi of kidney and liver toxicity, and the explosiveness of the fine powder. Of course not being K3VVL I did not light a pile of filings.
I notice to get the tall crystals coming up out of the metal I need two things. One is a lot melted, and the second is to have it in an insulating
form which holds the heat in for a limited time, to allow for very slow cooling.
What about the aluminum reactivity? Should I not be using my pan? I have not noticed anything going on, and like I said in the last post the liquid
does not stick, and letting a panfull cool just for the sake of checking it out, the whole mass falls out without any trace of bonding to the sides or
bottom of the aluminum. I am wondering about the safety from a toxicity standpoint as to melting/casting/filing and so on. Anyone know? I sure cannot
find anything from the MSDS's those things would say don't let water touch your skin, and five different ones would disagree with each
other. Is there a better online source to look up metals and chemicals as to safety concerns, actually written by people with some experience in the
field?
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12AX7
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Dunno about references but just don't forget a reality check... NOTHING on EARTH gets a rating lower than 1, because EVERYTHING is hazardous,
poisonous or reactive (no shit it'll explode when you put chromyl chloride on it! WTF!). Even table salt earns a 1 because you have to eat
"only" a half pound to kill yourself.
I personally have been soldering since age 9 (mind you I don't have the best ventilation or hygene, especially when it comes to handling solder!)
and I'm perfectly healthy. I hate everyone who BS's about lead. Hell, I wonder how many kids who got brain damage from eating paint chips
weren't already going south from the get-go... I mean... mmm, paint? 
(Yeah yeah toddlers, different story..)
Aluminum and bismuth form no intermetallics so I see no possibility of (whatever the term is) them combining exothermically. In fact they are largely
insoluble, indeed immiscible in each other below orange heat. Bismuth isn't nearly reactive enough to reduce Al2O3, although exposed aluminum
metal (say a scratch) can technically reduce Bi2O3. Would it ignite, let alone strong enough given the amount of available Bi2O3? Hell no!
So yeah... I really hate MSDS's... in fact I recently saw an online article taddling on "them" for essentially crying wolf about
everything...
Tim
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neutrino
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To be fair, water is not listed as hazardous. As far as I know, though, that’s the only thing that isn’t.
| Quote: | Originally posted by IrC
One thing I did wonder about was the mention for Bi of kidney and liver toxicity |
I really doubt that is a problem. After all, bismuth subnitrate is an FDA-approved stomach remedy (Pepto-Bismol…)
Bismuth has one peculiarity that is probably causing those peaks: it expands on cooling. In my experience, the following string of events usually
happens when casting bismuth: Liquid bismuth is poured into a mold. It instantly solidifies where it touches the cold mold, possibly remelting later.
The top, which is exposed to the air, eventually (and permanently) solidifies. At this point, you have a crust of bismuth with a good deal of liquid
inside. When this liquid solidifies, it expands. The extra liquid gets out however it can.
If you cool from the bottom and/or insulate the top, you don’t get this problem. Instead, you get a surface that tends to have visible bumps caused
by crystal formations. Remember that Bi expands as it cools, so the loose crystals that tend to form float to the top and effectively destroy any flat
surface.
I’ve tried using an aluminum crucible, but it kept sticking. Moreover, this started happening where Bi and Al met:
(sorry about the color here)
I didn’t think that heating would make the oxide film that much thicker, so I didn’t do it. If I ever come across another aluminum crucible of
these dimensions, I will try it.
Anyway, back to those crystals. I’ve decided against using zinc. Although it shouldn’t react with the Bi to a very large extent, it should still
be enough to contaminate the melt. I get the feeling that boric oxide might form eutectics of some sort (the pure material melts at ~450C), but I
can’t find any information on this at all.
P.S. IrC, where did you get your bismuth?
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IrC
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I have bought a little over 15 pounds on ebay from Emovendo over the last year. He is a good source and a very good ebay seller. Right now he has very
pure Bi at $60 US for 5 pounds, plus $10 S/H. I cannot give the information of an overseas supplier as it took way too long to find and all I would
accomplish is either causing the supply to dry up in the worst case, and without a doubt I would be throwing away my money for nothing as the price
would start going up the minute the world started buying there. It is just an economic thing, greater demand means I pay more for what I was getting
cheaper before I gave up the source.
The picture needs more light so I can see what you are trying to show. I do not use a crucible, it is just a neat aluminum pan with a handle which
fits the melting pot. Possibly you are applying way too much heat, I keep it as low as possible and wait for it all to liquify, no chemical reactivity
at all that I can see other than oxide which I skim off. Can you show a picture with more light of your Al crucible?
Also, I never thought about it but could the crystals be lighter than the liquid? That seems correct, as logically atoms would space out in a
structure as opposed to a liquid with no structure. The expansion statement also makes sense, except that what I see coming up is localized and of a
clear structure underneath the smooth metal which covers it. This is why it seemed like large crystals were just growing up. Possibly the expansion is
driving a crystal structure slowly up in a similar way to growing crystals by slowly pulling a seed up from a molten mixture as in the making of laser
rods?
"I really doubt that is a problem. After all, bismuth subnitrate is an FDA-approved stomach remedy (Pepto-Bismol…)"
Now I am scared. Everytime the FDA approves of something a year or so later there are 50 ads a day on TV by lawyers going after money to sue someone
or other over the latest rash of deaths caused by FDA approved medicines. I do not want 12 arms growing out of the side of my head. Or do I? I take PB
all the time to deal with ulcer problems over 20 years, which believe it or not I have directly related to the amount of handling of lead solder when
I am doing big runs of one thing or another. Don't know if that is backed up by the AMA but they are all a bunch of quacks anyway. No doubt they
also write MSDS's.
I looked at your cool water crystals, and that sure looks like the big glob of Samarium metal I have. Does Bi alloy with the lanthanides? I have a lot
of them all. I did try experimenting with Indium/Gallium/Bismuth/Tin and some other metals in alloys. One batch melts below the Gallium alone, you
cannot even hold it in your hand without it running out. Some of them form very interesting crystals. I did buy a quarter pound bar of pure Cadmium
with the thought in mind of alloying that. But so many studies of toxicity I have read for Cd convinced me to leave it sealed up. Maybe someday I can
find someone who wants to trade it for something I will use. Just do not want to take the risk of it burning. This I found out with Germanium. I had a
cheap helium source for ballons which I thought was an easy way to have an inert gas to melt things in. So when I tried melting several pure elements
with pure Ge, the Ge caught on fire forming the not so bad and the very poisonous oxides, all over the place, quite a big cloud in the room. After
that I started being much safer, reading all I could find about the dangers. Good thing this was before I ever decided to melt that bar of Cadmium. Oh
yeah, what I found was never use ballon helium, it contains a large amount of oxygen, in case some kid might inhale it, to keep them from suffocating.
The Ge started burning in it and of course got much worse when I opened the vessel in an attempt to stop the reaction.
Possibly if I ever found something to contribute to the book project it would be a chapter on the things to look out for, as like I have mentioned
here chemistry books never seem to quite cover these aspects of chemistry no matter which book I locate and read. This is exactly what led me to SCM
in the first place. I am not into drugs but I noticed that at least the sites related to the subject talked much more about what could go wrong and
what to watch out for than what I saw in any "mainstream" chemistry sites. Looking for a site which was more into real science and chemistry
overall, I came upon Science Madness. Here I have learned more about the pitfalls, dangers, what to do and what not to do, of so many experiments
covering such a vast realm of just plain chemistry than anywhere else I have found.
In just a few months I have learned more real world chemical experience right here on this site than I did in the last decade at any other site, book,
university, or you name it source on the science of chemistry.
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12AX7
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| Quote: | Originally posted by IrC
Also, I never thought about it but could the crystals be lighter than the liquid?
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Since bismuth expands on cooling, like ice, that would seem to be true.
| Quote: |
That seems correct, as logically atoms would space out in a structure as opposed to a liquid with no structure. |
Well, not really, a solid is ordered crystalline whereas a liquid is chaotic motion.
A solid block of legos takes up a lot less space than the bucket they came in.
With the exception of course for Bi, H2O and whatever other materials have that quirk.
| Quote: | | Possibly the expansion is driving a crystal structure slowly up in a similar way to growing crystals by slowly pulling a seed up from a molten mixture
as in the making of laser rods? |
It sounds to me like the liquid is solidifying, causing an internal pressure which ruptures the solid surface (remember that bismuth is horribly low
in conductivity), forcing out any crystals in the path.
| Quote: | "I really doubt that is a problem. After all, bismuth subnitrate is an FDA-approved stomach remedy (Pepto-Bismol…)"
Now I am scared. |
Now <B>I</B> am scared. First he mentions pyramids...which is bad enough, I mean geez...pyramids? But scared of the FDA? I can
understand anyone disliking a government agency, but seriously, their standards are too high...
(Heck- ever notice how medications always get approved in other countries before the USA?)
| Quote: | | Everytime the FDA approves of something a year or so later there are 50 ads a day <B>on TV</B> |
Ayop...my added emphasis explains this quite nicely.
| Quote: | | Don't know if that is backed up by the AMA but they are all a bunch of quacks anyway. |
Now you're either drunk posting, or you are a new-age quack yourself...tell me, has homeopathy healed anything for you particular well? Those
pyramids sharpen a razor blade for 'ya?
| Quote: |
I looked at your cool water crystals, and that sure looks like the big glob of Samarium metal I have. Does Bi alloy with the lanthanides?
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Probably, but forming intermetallics, all with high melting points, which generally describes those metals' behavior.
| Quote: | | I did buy a quarter pound bar of pure Cadmium with the thought in mind of alloying that. |
Good...
| Quote: | | But so many studies of toxicity I have read for Cd convinced me to leave it sealed up. |
...Bad.
Tim
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IrC
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"Good, Bad, snip"
Tells nothing and says nothing useful, just a waste of space. As to my correct statements about how dangerous Cadmium is I refer you to this link:
http://www.inchem.org/documents/pims/chemical/cadmium.htm
"Well, not really, a solid is ordered crystalline whereas a liquid is chaotic motion."
No kidding, to state the obvious.
"A solid block of legos takes up a lot less space than the bucket they came in."
Also obvious, the point I was making. Therefore less atoms per cubic centimeter therefore lighter. What did you think I meant.
"Those pyramids sharpen a razor blade for 'ya?"
No, but I never tried either, seeing as how I do not believe in the stupid. However, the very wise among us pick out the grains of truth in a subject
and study those. Much knowledge has been lost to history. What do you think the scrolls from the library of Alexandria had written on them, that is
until people like you burned them heating bath water for the elite.
"Now I am scared. First he mentions pyramids...which is bad enough, I mean geez...pyramids?"
What have you done? I don't recall seeing your name in lights, no magic inventions, no wonder drugs. People who are famous, such as Patrick
Flanagan and Thomas Bearden, who have strings of degrees, patents, and such, have spent time studying them and talking about it. So why try to deride
me here. People way better than you would not do so. I also do not see how you suddenly jump to homeopathy concerning me from anything I said on this
board. If you think the medical profession is filled with gods it's not my fault you do not know any better. A clue, they only care about your
money. I could say many things and back it up with many proofs but this is the incorrect place to discuss the subject.
As to pyramids, some of what I said was in jest but I see you are not able to discern such depths. I brought them up as that was what I was actually
doing with the bismuth so I felt it was in context. I find them easy and fun to make and people like buying them so why not. It makes me honest and
legal money so why are you complaining about it. Never mind I don't want to know.
"Now you're either drunk posting, or you are a new-age quack yourself"
How did this thread degenerate into personal attack and libelous slander against me? By the way I do not drink or do drugs. As to being a quack I
doubt you are qualified to judge, especially on the basis of no information. In fact only a fool makes such judgement.
"tell me, has homeopathy healed anything for you particular well?"
To answer your question shifts the thread into something else which I do not want to do, but I will answer here since you asked it here.
Yes. I have not had the flu or a cold in 7 years, since I started making colloidal silver. I use the term colloidal but I rather believe oxides are
also involved in it's properties. After August 20th 1988 when Bio Labs burned down in a suburb of Phoenix, I had constant cronic bouts of lung
infections. 1.5 million pounds of 111 cyanuric acid trichloride went up after the fire department ignored the placards plastered all over the place
and poured 3/4 million gallons of water all over it. Also a 75,000 gallon tank of muriatic acid exploded, the entire thing being an orange fireball a
quarter mile high into the sky, 4 blocks from my house.
There was HCN, greenish yellow chlorine gas rolling along the ground, and only God knows what else. I will not waste too much space here telling about
it, it was global news, go look it up. The sludge in the streets was loaded into boxcars that kept exploding weeks after, the California govenor
stopped the waste from being shipped into his state.
For years after that every cold or flu that came by nearly killed me every time, and I always caught them from everyone. Then one day there was a flu
in NM so bad it was killing many older people, and a friend of mine who was always in better health than me was out from work for 14 days with it,
quite ill. He said it took 6 weeks for all the symptoms to be gone, just a neverending low grade infection in his lungs. I was studying about CS at
the time and had ordered the wire, built a power supply and so forth, and the last step was building the cell itself.
With that in mind I was at Kmart in line to pay for my bottle, when I noticed I was soaking in sweat and feeling quite ill. I went home, finished my
generator, drank a glassfull, went to bed. The next morning I woke up and noticed that not only was my temperature gone, but I felt not the slightest
trace of pains, aftereffects, or any symptoms of being ill whatsoever. Around 7 years later, every time I notice people sick around me, and notice
slight symptoms coming on, I make a batch and drink it. The same thing, zero symptoms of illness the following day, every single time in nearly a
decade now.
Not one cold or flu since in all these years. The royals made it through the black death in the 12th century by eating and drinking from silver
goblets and plates. The only reason they became known as "blue bloods" is because they also stupidly ingested compounds of Ag. I do not want
to turn this thread away from the Bi origin but I thought your direct question deserved a direct answer. I could give you much more proof but you
wouldn't believe it anyway and I don't care whether or not you do. Homeopathy served mankind for millenia, and most modern drugs were based
upon the study of the healing power of natural substances. I would have thought you already knew that.
I have said it before, a man with experience is never at the mercy of a man with an argument.
I never voted in your poll, and was not going to so don't make me go vote no. I can see why so many did so if that helps in any way. I do hope
you are done with your assault on my intelligence so the thread can get back to the original subject, bismuth.
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neutrino
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Agreed. If you two must duke it out, please do so in the appropriate thread.
I will try to get a decent picture of the crucible again tomorrow. Today has been far too long already.
IrC, that Bi is ~$15/lb. Another seller usually sells chunks of the same purity for half that.
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IrC
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I not going to get into duking anything, I have said to 12AX7 all I am going to about the subject. I do not go out dragging others into stupid flame
wars and I try not to let others suck me into them either. I do feel it is right to respond to personal attacks to a point. I know about the other
guy, I have bought Bi there also, Emo is the first one that came to mind when I was thinking about an answer to the question as to where I find
Bismuth.
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Fleaker
International Hazard
Posts: 1252
Registered: 19-6-2005
Member Is Offline
Mood: nucleophilic
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Emovendo is a good seller. I ordered 5 pounds of 4N bismuth for general experimentation (yes, crystal growing mainly, but also fusible alloys) and
overpaid. He promptly sent the money back when he could've just kept it. He's honest.
But in regards to bismuth melting, if you have access to a muffle furnace and argon (or nitrogen) melt it in a thick crucible (I make mine out of
jewelry investment built up around a Coors crucible) and bring it up to 900C and slowly let it cool. Emphasis on slowly. Please note that any more
than 900C and you can decompose the investment, which makes for a stinky SO2 experience.
From my experience, the longer it cools (hours), the better the crystalline product will be. When it drops to near its melting point (271.3C) open
the furnace to let the atmospheric oxygen in and kill the blanket gas-and you get your vivid colors. Some crystals can get rather large (egg size
and beyond) using this method.
Alternatively, you can get one of those party balloon helium tanks for cover gas and get it very hot on a gas stove (a porcelain crucible can be
used).
Oh another great thing about those bismuth pellets, they make superb ball mill media. Virtually no static, they're hard, and they last pretty
long (I've ground iron oxide with them and they're still fine).
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neutrino
International Hazard
Posts: 1583
Registered: 20-8-2004
Location: USA
Member Is Offline
Mood: oscillating
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The thing about ebay is that all sellers are very honest and reputable. The only thing to choose by is price.
900*C? Crucibles are usually rated for temperatures much higher than that.
Do you get any nucleation around the crucible-bismuth boundary with that method? I'm working with small batches of bismuth (~40 cc) and
can't really afford any of those because they approximately halve the maximum crystal size.
How well does part balloon helium work?
You must have impure grinding media; my Bi can be dented with a fingernail.
I guess I should give another update about my tinkerings. My hotplate broke a while ago, I spent weeks trying to fix the damn thing, gave up, and got
a new one a few days ago. I discovered that boric oxide doesn't work (despite its semi-fluidity at these temperatures). That's about it for
now.
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Fleaker
International Hazard
Posts: 1252
Registered: 19-6-2005
Member Is Offline
Mood: nucleophilic
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In regards to the crucible, the gypsum/cristobalite coating is for insulation more than anything else. I want to keep the bismuth in a molten state
and without agitation as long as possible. Basically I dip a large 100mL porcelain crucible into jeweler's investment (for casting gold/silver
etc). Why not more than 900C? Sure the crucible can take 1200C easily, but that is pushing it for the calcium sulfate which at that temperature
decomposition can occur. Trust me, when it decomposes, it release a ridiculous amount of sulfur dioxide (and at those temperatures probably trioxide
as well).
So you're having problems with nucleation at the point of contact with the 'crucible' walls and bismuth eh? I don't know what
could cause that as I've not had that problem. Maybe a 4M sulfuric acid wash would clean up the glass. I'm guessing that some residue or
maybe microscopic oxide on the walls is providing the impetus for nucleation at that area.
Party balloon helium, from what I've heard is decent to use, but it is really ineffective as a cover because it is so light and doesn't
properly blanket the melt. I seem to recall that it's not just helium but a mixture of a few other gases.
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12AX7
Post Harlot
Posts: 4803
Registered: 8-3-2005
Location: oscillating
Member Is Offline
Mood: informative
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Balloon helium is diluted because people inhale it. Go to a welder's supply, theirs also lifts better!
The bismuth I have is listed as 4n5 (IIRC) and makes brittle crystals. (To be fair it's from Lou here so probably the same stuff he buys.)
Obviously it isn't impure because it makes crystals, and apparently the same goes for yours? Maybe you have lead?
Tim
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