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a_bab
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[*] posted on 15-10-2009 at 23:13
Elements for trade


Having lots of elements collected over the years, I had finally managed to put some in order. I'm missing quite a few though.

I've got for trading:

-In metal, pure (wire)
-Au (gold leaf, looks great)
-Mn powder + turnings
-Fe (H reduced; OR from pentacarbonil)
-Sn foil/shots
-Li, Na, K ampouled 1 gram (I need to work on these)
-P (red, ampouled) - 1 gram
-I (crystals, ampuled) - 1 gram
-Se (amorfous, shots, ampouled) - 1 gram
-S (crystals)
-Mo powder

All of them ampouled.


I'm looking for:
-Ge
-Ga
-Nb
-Ta
-Hf
-Y

I've got some CsNO3 and RbI and I'm planning to isolate the metals from them with the azide method (thermal decomposition in vacuum). Actually I've got quite an amount of elements I'd isolate (Ba, Sr, Ca, Si, B, Be, and others. I need time!).


I do NOT sell any of these, especially P, I (so fuck off meth wreks), hence the low amounts (just for display purposes, more then enough to make the point).
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watson.fawkes
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[*] posted on 16-10-2009 at 05:51


Quote: Originally posted by a_bab  
I do NOT sell any of these, especially P, I (so fuck off meth wreks), hence the low amounts (just for display purposes, more then enough to make the point).
A small point to remember: the List I regulations prohibit selling without reporting, but they also prohibit bartering-away in the same breath. There's no de minimis exemption, nor is there an element-trading one. So to be perfectly legal, you don't want to be trading phosphorus or iodine.

For the record, I think the law in this case yields an injustice.
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Nick F
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[*] posted on 16-10-2009 at 08:06


Do you have photos of the ampouled alkali metals? I'd be interested in those if they're fairly clean.
Also, if you do manage to isolate Cs & Rb via the azides, I'd love to hear about it. I have a load of NaN3 and was thinking about trying it, but I'm a bit scared of trying to produce any useful amount of sodium metal using this method.
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JohnWW
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[*] posted on 16-10-2009 at 08:45


What country are you in, A_Bab? "List 1" etc. applies only in the U$A, and some other countries that the U$ Govt. has bullied into copying its recent fa$cist laws.
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a_bab
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[*] posted on 16-10-2009 at 09:12


To watson: You are righ. i do not need unwanted attention. Not that I have a whole bunch on I and P anyway.

To Nick (cought Mr Cool): I will certainly share the results. I'm planning on Ba/Sr from the same route; unfortunately these azides are similar to lead in behaviour. I happend to know about your azide too; I'd be scared about the amount too :)

Pics soon.
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[*] posted on 17-10-2009 at 12:10


a_bab:

What country are you in?

Regards homemade beryllium, good luck with that! Any ideas for a route? Starting from beryllia? Or from another starting point?
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a_bab
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[*] posted on 17-10-2009 at 22:14


I live in Europe.

I have some Be(NO3)2 and I'm planning on a simple reduction with Na.
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[*] posted on 18-10-2009 at 08:17


Quote: Originally posted by a_bab  
I live in Europe.

I have some Be(NO3)2 and I'm planning on a simple reduction with Na.


Be(NO3)2 + 12 Na ---> Be + N2 + 6 Na2O, I'm guessing.

If that's what you're aiming for you might actually obtain 'lump Beryllium' (a regulus) because the formation of 6 moles of sodium oxide (per mol of Be) might just generate enough heat to reach the MP of Be (in roughly adiabatic conditions).

For Niobium, you can use aluminothermia (thermite) with Nb2O5. The system Nb2O5 + 10/3 Al needs a small amount of a heat booster (KClO3 + Al or similar) to reach the MP of Niobium. I've done it on a small scale (20 g batch of mix) in an open crucible. Nice little lump of Nb...
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a_bab
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[*] posted on 18-10-2009 at 08:42


The reaction is going to be much more complicated, with many side reactions.

I will conduct the reaction is a closed pipe, very pressure resistant, and the pipe will be heated untill the reduction starts. The reaction itself will take only few seconds, during wich the pressure could go above 100 atm.
The Be(NO3)2 is very hygroscopical, much like Mg(NO3)2 (deliquescent), and I got it in liquid form (so a very concentrated solution). I'll have to dehydrate it very well before attempting the reaction in order to increase the amount/reduce the danger. The quantity is very limited too. I didn't study the matter, maybe berillium oxide/hydroxide will work better (and it should do). Basically it has to be pretty similar to Mg/Ca thermo isolation. We'll see...

There are a whole bunch of elements I want to isolate; when I'll do it I'll post the results. Unfortunately my time is very limited for this kind of experiments.
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halogenstruck
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[*] posted on 18-10-2009 at 11:28


you want a very good hint for Y2O3 AND Eu source.
7 years ago i had a customer who was interested to pay a lot for Y2O3,i extracted it from a every house item.around 700GR for 500$.
it`s an electric gadget.
RED PHOSPHOR OF high performance lamps is made of 99.5% Y2O3 and 0.5% Eu2o3!!!although i separated trace of Eu by reduction with Zn/Hg of the phosphor solution in HCl.phosphor does not dissolve in HCl first but if you heat it suddenly start dissolution when approach boiling point then gets vigourus and needs cold water addition.then precipitation with SO4 ion.
i took the phosphor from lamp company for free as he was my relative.i guess real price would be 80$ every KG.


PHILIPS_Economy_Energy_Saving_Lamps.jpg - 120kB

[Edited on 18-10-2009 by halogenstruck]
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[*] posted on 18-10-2009 at 11:32


for tantalium you can get from some electric capacitors[they are called tantalium c.,one electrode or both is from this metal,not sure].maybe from some resistors.Nb i can not remember well but i guess one of them again.
laser diode red maybe is from gallium arsenide
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blogfast25
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[*] posted on 18-10-2009 at 12:08


Quote: Originally posted by a_bab  
The reaction is going to be much more complicated, with many side reactions.



I meant the overall stoichiometry.

BeF2 + Mg ---> Be + MgF2 at 1,300 C maybe the best bet.

Alternatively BeF2 + 2 Na ---> Be + 2 NaF may do it. At least the slag is water soluble (-ish), in case the reaction doesn't reach the MP of Be.

I wonder if mixing anhydrous BeCl2 with another inert halide (NaCl or KCl) in a eutectic mix (for lowest temperature) and then reacted by gradually adding Mg powder would do it? Then heat the metal/slag mixture above the MP of Be under Argon, to separate the slag from the metal... A similar method has been used for Manganese.


[Edited on 18-10-2009 by blogfast25]
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blogfast25
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[*] posted on 18-10-2009 at 12:13


Quote: Originally posted by halogenstruck  
you want a very good hint for Y2O3 AND Eu source.
7 years ago i had a customer who was interested to pay a lot for Y2O3,i extracted it from a every house item.around 700GR for 500$.
it`s an electric gadget.
RED PHOSPHOR OF high performance lamps is made of 99.5% Y2O3 and 0.5% Eu2o3!!!although i separated trace of Eu by reduction with Zn/Hg of the phosphor solution in HCl.phosphor does not dissolve in HCl first but if you heat it suddenly start dissolution when approach boiling point then gets vigourus and needs cold water addition.then precipitation with SO4 ion.
i took the phosphor from lamp company for free as i was my relative.i guess real price would be 80$ every KG.


What do you mean by 'RED PHOSPHOR' in this context.

Do you mean the UV fluorescent inside white coating in so-called saver bulbs? That would be an interesting source of Yttrium indeed. But saver bulbs aren't cheap and will yield little of the substance... And you 'cheated'!

Oh, I see after looking it up: you mean the phosphor of red light emitting CFLs. Presumably white light CFLs contain some red phosphor too (but less and combined with other phosphors...


[Edited on 18-10-2009 by blogfast25]
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halogenstruck
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[*] posted on 18-10-2009 at 14:22


yes u r right,i took it in bulk from lamp producer company but he is just interested to have just 1 gr as sample and just one old burnt lamp which does not work is enough!!!
they are 3 kind green blue red,for white they use the mixture of them.
pure y2o3 is not fluorescent but Eu impurity make it glow red.Eu2O3 by itself is strongly red fluorescent.just like Hg2Cl2.i experimented all of them under uv light
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halogenstruck
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[*] posted on 18-10-2009 at 14:24


some of bulbs are pure red.that kind of lamps have relatively pure red phosphor.i assume.
.no in fact,i did not cheat at all.i took Y2O3 99.5%,0.5%Eu2O3,extracted Eu then precipitating Y as oxalate salt then strong heating.it was completely pure.Eu when is reduced to 2+ resemble to Ba2+ and makes sulfate insoluble salt.
for any practical information u can see brauer handbook.

[Edited on 18-10-2009 by halogenstruck]

[Edited on 19-10-2009 by halogenstruck]
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[*] posted on 18-10-2009 at 15:08


Quote:
have relatively pure red phosphorus


You mean red phosphor correct?





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halogenstruck
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[*] posted on 19-10-2009 at 03:25


sorry red flourescent phosphor [not red phosphorus]
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blogfast25
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[*] posted on 19-10-2009 at 06:48


By you 'cheated' I meant that you obtained the Y2O3 phosphor straight from the bulb (lamp) manufacturer, not from recycling spent bulbs.

Do you happen to know what is used for the green and blue phosphors?
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JohnWW
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[*] posted on 19-10-2009 at 09:31


Quote: Originally posted by blogfast25  
Do you happen to know what is used for the green and blue phosphors?

Phosphorescent or fluorescent compositions are mainly based on rare-earth metal oxides mixed with others, including especially Eu (its ability to be reduced to the (II) oxidation state being important), along with some d-transition metals including Zn, Cd, Cu, and Ag. Depleted U oxides are another possibility. In some cases sulfides or nitrides are used.

For CRTs, the usual compounds used are, according to http://en.wikipedia.org/wiki/Phosphor which has a table with more detailed info :

White (in black-and-white): The mix of zinc cadmium sulfide and zinc sulfide silver, the ZnS:Ag+(Zn,Cd)S:Ag is the white P4 phosphor used in black and white television CRTs.

Red: Yttrium oxide-sulfide activated with europium is used as the red phosphor in color CRTs. The development of color TVs took a long time due to the long search for a red phosphor. The first red emitting rare earth phosphor, YVO4,Eu3, was introduced by Levine and Palilla as a primary color in television in 1964.[16] In single crystal form, it was used as an excellent polarizer and laser material.[17]

Yellow: When mixed with cadmium sulfide, the resulting zinc cadmium sulfide (Zn,Cd)S:Ag, provides strong yellow light.

Green: Combination of zinc sulfide with copper, the P31 phosphor or ZnS:Cu, provides green light peaking at 531 nm, with long glow.

Blue: Combination of zinc sulfide with few ppm of silver, the ZnS:Ag, when excited by electrons, provides strong blue glow with maximum at 450 nm, with short afterglow with 200 nanosecond duration. It is known as the P22B phosphor. This material, zinc sulfide silver, is still one of the most efficient phosphors in cathode ray tubes. It is used as a blue phosphor in color CRTs.

If there are ever shortages of those metals used in phosphors, it may well become worthwhile extracting them from junked TVs and CRT screens.
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halogenstruck
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[*] posted on 19-10-2009 at 10:49


as i remember,one of the was just a mixture of mainly aluminium oxide the blue one,the green one contained Yb and another rare earth.no one was that pure like red.
i will check later my resources. one of them i think was ullmann or kirk othmer. then i will add it here.
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[*] posted on 19-10-2009 at 10:58


in the upper mentioned link in wikipedia i checked them and as i remember they were like this or very close:

(Ce,Tb)MgAl11O19 Green 546 nm 9 nm - Lamp Trichromatic fluorescent lamps[19]

BaMg2Al16O27:Eu(II) Blue 450 nm 52 nm - Lamp Trichromatic fluorescent lamps[19]
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[*] posted on 19-10-2009 at 11:35


Thanks, both of you.

Now I'm tempted to try an recover the phosphors from that kaput TV I've got in my backyard! It'd be quite an interesting exercise in chemical separation...

No rest for the wicked!
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halogenstruck
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[*] posted on 19-10-2009 at 20:27


u r welcome
extraction of Y2O3 from red phosphor in economy lamp [red light]is relatively easy but in TV all phosphors get mixed and separating rare earth metals from each other is really hard and needs ion exchange resin column elution.only Eu can be separated and Ce from the others easily because of their unique properties.
another point,as i remember,only red one could be dissolved easily and completely after boiling with Conc. HCl but not the other which can not be digested easily in acids.
care ur hands and eyes too!!!broken glass:D
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[*] posted on 20-10-2009 at 06:46


I was thinking fusing with Na bisulphate (for the mixed phosphor) actually. Precipitate the REs with oxalate.

After that, either ion exchange or some very old tricks (from 'Ye Olde Chemistry' book) ;) Yttrium stands just that little bit on its own...

Hard to do without some prior element analysis of the mixed phosphor, though...

Broken glass: tape it off with gaffer tape.

[Edited on 20-10-2009 by blogfast25]
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JohnWW
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[*] posted on 20-10-2009 at 14:29


That reminds me: in view of the fluorescence of many of its compounds, and ability for polyvalence like Eu, I wonder if anyone has thought of using depleted uranium compounds as phosphors on CRT tubes, particularly green or yellow? Especially as there are huge stockpiles of the stuff sitting around after extraction of the U-235 for enriched U bombs and nuclear fuel rods, with few industrial-scale uses other than in DU-tipped projectiles or bullets, keels of racing yachts (being much heavier than Pb), and pigments in some glazing enamels and paints.
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