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Author: Subject: Lanthanum from pool cleaner
Brain&Force
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[*] posted on 13-10-2014 at 14:21
Lanthanum from pool cleaner


...because diddi's account accidentally got deleted, and we need to continue research.

Carry on.




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[*] posted on 13-10-2014 at 14:35


didi needs to get a new account and PM Polverone- Then he can re-set password & get anything not permanently deleted back up.

See here:

http://www.sciencemadness.org/talk/viewthread.php?tid=37991&...

Quote: Originally posted by Polverone  
I am very sorry, but your profiles were temporarily deleted. I have reactivated your accounts, but you will need to send me a U2U through a temporary account or email me to get your new password. My email address is gfxlist@yahoo.com

I am sorry for the inconvenience.




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[*] posted on 13-10-2014 at 14:42


If I wanted Lanthanum, I would get it from soil, rocks, or flint from lighters! Flint (not mineral with the same name) in lighters is mixture of La, Ce, Pr, Nd. Soil contains La in miligram amounts.


[Edited on 13-10-2014 by AsocialSurvival]
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[*] posted on 13-10-2014 at 14:48


Quote: Originally posted by AsocialSurvival  
If I wanted Lanthanum, I would get it from soil, rocks, or flint from lighters! Flint (not mineral with the same name) in lighters is mixture of La, Ce, Pr, Nd. Soil contains La in miligram amounts.


[Edited on 13-10-2014 by AsocialSurvival]

Or, you know, you could just buy a perfectly OTC and relatively pure source of lanthanum. But by all means, attempt to extract significant quantities from soil in an amateur setting. Have fun!
The lighter flint is something I've attempted before, and separating the 50% Ce, 25% La, 1% other RE's and balance of Fe and Mg is no easy task.
I wondered why I couldn't find the relevant thread here for a while... Never did see if anyone responded to my question of getting a smaller (but presumably more concentrated) amount of phosphate remover or a larger (but specified as diluted) different brand.




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[*] posted on 13-10-2014 at 14:51


Quote: Originally posted by AsocialSurvival  
If I wanted Lanthanum, I would get it from soil, rocks, or flint from lighters! Flint (not mineral with the same name) in lighters is mixture of La, Ce, Pr, Nd. Soil contains La in miligram amounts.


[Edited on 13-10-2014 by AsocialSurvival]
Good luck purifying visible amounts of it from those sources. Lanthanides, in case you weren't aware, are extremely hard to separate chemically. Also, the tiny amounts found in most soil would be so miniscule and hard to isolate that you might as well try and find gold in your soil.



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[*] posted on 13-10-2014 at 15:05


OK, anybody interested in these procedures, feel free to subscribe to my yt channel: http://youtube.com/user/AsocialSurvival

Also, I will never buy anything for Chemistry, I will only sell something. Chemistry's purpose, in my case is to become rich, not poor.

[Edited on 14-10-2014 by AsocialSurvival]
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[*] posted on 13-10-2014 at 15:10


I'm eager to see these procedures, but unfortunately it appears that your YouTube channel doesn't exist.
Anyway though, how is it that you expect to isolate lanthanum from your soil?




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[*] posted on 13-10-2014 at 15:16


Quote: Originally posted by AsocialSurvival  
Chemistry's purpose, in my case is to become rich, not poor.


Hey, it worked for Alfred Nobel. But Nicolas Leblanc, not so much. Let us know how this pans out for you...

BTW, YouTube link is not working.




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[*] posted on 13-10-2014 at 15:31


First dissolve soil or rock in Nitric Acid (which I have in unlimited quantity). That would dissolve almost all elements present there, except Si, Ti and few more. The rock will immediately disintegrate into insoluble powder. Then, by boiling solution of soluble elements, I could perfectly seperate them all. It's long explanation why would only Nitric acid in small quantity would be needed, and boiling that all, but once again, video will come one day! Fixed: http://youtube.com/user/AsocialSurvival

[Edited on 14-10-2014 by AsocialSurvival]
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[*] posted on 13-10-2014 at 16:52


Oh, the YouTube channel is there. Just no content of any type.

"Unlimited (free?) nitric acid"... Perhaps means someone else is paying for nitric acid they are not getting? Did you surreptitiously tap into an explosives factory pipeline or what?




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[*] posted on 13-10-2014 at 17:01


Surely you could just sell your unlimited nitric acid and get rich that way?

But we're getting distracted. The only method people said was viable was precipitating the fluoride and then reducing it with lithium?

This can all be done OTC in Australia then, yielding a few grams of lanthanum metal for about $50. Not cheap but an interesting project
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[*] posted on 13-10-2014 at 17:25


@ AsocialSurvival
You have a lot more confidence in your ability to separate compounds than I do. One of the characteristics of the REs is their similarity in chemical and physical properties which is why, historically, they have been so hard to isolate. (Hence the challenge and interest that they present.)
I am envious of your supply of nitric acid. Wish I had the same kind of resource. I have to make mine.

One of the appeals of using OTC LaCl3 is it enables some experimentation without going through the difficult process of isolating. And indications are that reduction of LaCl3 to La is by no means a trivial process in itself. If posters' experience with Nd is anything to go by, this is a difficult task in a home lab situation.


Given that the original thread disappeared into the ether, let me summarise what I remember of the findings.



  1. Lanthanum Chloride is available OTC – sold as a swimming pool additive to precipitate phosphates that can then be filtered out. Interesting use of the chemical.
  2. A likely route for refining is to convert to LaF3 and reduce with lithium. Potassium has also been suggested.
  3. The thermodynamics for reduction directly from LaCl3 are questionable. Blogfast reported a paper that had some success with CeCl3. No hard data presented for La.
  4. LaCl3 exists as a heptahydrate and is difficult to crystallise. It is extremely hygroscopic. LaF3 is insoluble which is another reason for suggesting this route.
  5. Precipitating LaF3 could conceivably be done using a fluoride salt. NaF possible but NH4F2H is suggested. This is available OTC as glass etchant and tile roughener. In Aus, Home Hardware sells a litre at 48g/L for around $27. I found a chemical supplier who will sell for $71 plus freight for 500g. It is available in bulk bags of 25kg each. I don't think i need that much.
  6. Blogfast has begun work with 2.5L of LaCl3 solution that he bought. I will let him post the details. Looked very interesting though.
  7. Some side discussion on the logistics of storing rare earths was also had. Standard techniques of ampouling under argon or oil seemed to be the way to go.
  8. I am sure I have missed something. I am fascinated by the whole project and while my participation in practical experimentation will probably have to wait for a few months, I am interested in the ideas offered. It seems like the original thread was of significant interest to a number of people on this board.


Now. Let me not die again and take my posts with me. :) In the interests of keeping this topic alive does someone want to quote this post so that if another glitch happens the information will not disappear.
Blogfast, if you remember what you posted before, I would love to take a look at some of those links.

J.
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[*] posted on 13-10-2014 at 20:39


Supply of nitric acid is simple, air contains nitrogen, wood gives energy.
Why are you all complicating this? So simple! Rare earth metals are easy to seperate just like any other element. I am confident in that that I can separate them all using only Nitric acid!

What fluorides? What Lithium? That is too complicated. OK, let's see how would I separate all rare earth metals?

Just add enough acid for one to dissolve (if all others are carbonates at the beginning). For reduction use K or Na or Li or Rb or Cs or electricity or something else. There're many ways.

Just like scientists complicate nuclear transmutation and want to force us to believe it is hard or impossible or complicated or a big deal. Not really! Some people just want to put me down, to force me to believe in negativity, and to waste my life trying and not succeeding. It's not about complications, not really - it's easy to do many things much more than you all think. But everybody will tell you "impossible", "complicated", "expensive".

Here's my promise for everybody: I won't talk with you until I prove to you that many things are possible. Next time I come here, I will show you how to separate all elements from soil or rocks using nitric acid only, and to make gold with nuclear fusion to become rich.

Bye until than!
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[*] posted on 13-10-2014 at 21:13


Thanks for your thoughts AsocialSurvival.
I rather suspect you are missing a few critical things. It is not like we are making things complicated just for the hell of it. Things become complicated out of necessity because they are difficult. Chemists consider energy changes that are required for chemical reactions. And that is why energetic materials like potassium, lithium and fluorine are needed. If you can obtain nitric acid from atmospheric nitrogen and energy from a wood fire then you really need to patent that. Reaction mechanics suggest that there are quite a few obstacles in that path.

And your promise... That sounds like a reasonable challenge you have set yourself. Good luck.
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[*] posted on 13-10-2014 at 21:52



Quote:

Just like scientists complicate nuclear transmutation and want to force us to believe it is hard or impossible or complicated or a big deal. Not really! Some people just want to put me down, to force me to believe in negativity, and to waste my life trying and not succeeding. It's not about complications, not really - it's easy to do many things much more than you all think. But everybody will tell you "impossible", "complicated", "expensive".


There is chaos under Heaven, and the situation is excellent...

You go, son.




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[*] posted on 14-10-2014 at 05:02


Before I resume my actual contribution here, this little gem below merits a short answer:

Quote: Originally posted by AsocialSurvival  
What fluorides? What Lithium? That is too complicated. OK, let's see how would I separate all rare earth metals?

Just add enough acid for one to dissolve (if all others are carbonates at the beginning). For reduction use K or Na or Li or Rb or Cs or electricity or something else. There're many ways.

Just like scientists complicate nuclear transmutation and want to force us to believe it is hard or impossible or complicated or a big deal. Not really! Some people just want to put me down, to force me to believe in negativity, and to waste my life trying and not succeeding.


You are a nut and possibly need help. Possibly a troll.

But do by all means come back when you've actually got something... I won't be holding my breath though.


[Edited on 14-10-2014 by blogfast25]




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[*] posted on 14-10-2014 at 05:43


I’ll summarise my work on the lanthanum bearing (10.3 % La glycolate, acc. MSDS) pool phosphate remover called ‘Lo-Chlor Starver’ (from Lo-Chlor Chemicals, AU) as follows.

2.5 L of this solution was neutralised with 33 % NH3 and the snow-white precipitate, presumed lanthanum hydroxide, quantitatively Buchnered and washed. This yielded about 1 L of product.

It was dissolved gradually and quantitatively in 280 ml HCl 37 % with mild heating, followed by simmering. It dissolved completely to a clear solution that was… slightly green! On further boiling that colour changed to yellow. I have very strong reasons to believe this colour is due to MORE than a bit of ferric chloride, more about that later. Possibly there is Pr present.

The solution (about 1.25 L) was then gradually boiled down to about 290 g, by which time it was urine yellow. On refrigeration a mass of small, white crystals formed (photos later) although much of the presumed lanthanum chloride heptahydrate remained in solution, as expected. The rest of the LaCl3 will now be recovered using the double sulphate method (with K2SO4), to try and separate it from the yellow contamination. If it cannot be separated I’m inclined to believe the original phosphate remover contained also Praseodymium. If it can, that would point to ferric chloride.

As regards possible methods of preparing La (and other REE) metals, I proposed the reduction of LaF3 with Li, which appears to be a thermodynamically favourable reaction, possibly with enough reaction heat to ensure clean separation between metal and slag. LaF3 is water insoluble, so fairly easy to prepare.

I earlier dismissed the use of reduction of anh. RECl3 but Brauer’s ‘Handbook of Preparative Inorganic Chemistry’ proved me wrong on that. I suggest strongly that anyone interested in contributing to this discussion go to the Library of this site, download Brauer and print off pages 1135 to 1150 from Volume 2.

There is an absolute wealth of information there that seems to have been overlooked by the ‘RE nutters in residence’ so far, including myself.

Reduction with K, with Ca, alcoholic electrolysis of RECl3 solutions with Hg cathode to REE amalgam and details on electrolysis of anh. RECl3/KCl melts are but a few topics covered. Details on preparing anh. RECl3 is also covered. And for the very curious (Brain&Force?): preparation of some REE(II) salts too, like EuSO<sub>4</sub>.

[Edited on 14-10-2014 by blogfast25]




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[*] posted on 14-10-2014 at 06:15


Does anybody else think we have a new resident troll here on SM?



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[*] posted on 14-10-2014 at 06:46


This was the LaCl3 solution at the start of the boiling process, light green:



Here after concentrating and chilling, with crystals of presumed LaCl3.7H2O on the bottom. The solution is over 50 w% LaCl3:




[Edited on 14-10-2014 by blogfast25]




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[*] posted on 14-10-2014 at 07:09


Quote: Originally posted by No Tears Only Dreams Now  
Does anybody else think we have a new resident troll here on SM?


I am not that new FFS :D
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[*] posted on 14-10-2014 at 07:11


Quote: Originally posted by j_sum1  

I rather suspect you are missing a few critical things.


Would they be just above the neck?
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[*] posted on 14-10-2014 at 07:36


Maybe if he could manipulate matter with will alone he might get somewhere. Otherwise, he doesn't stand a chance.
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[*] posted on 14-10-2014 at 07:54


Please let us now restrict further remarks to the science and engineering aspects of the OP's topic.

If being trolled, DO NOT FEED THE TROLL. It will go away or die.

If site rules are violated, user that little blue "report" button or PM a moderator.

And I JUST LOVE the swimming pool chemical supply section at various stores! Right up there with the ceramic glaze supply, photographic supply and auto supply stores.





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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[*] posted on 14-10-2014 at 07:58


Quote: Originally posted by Bert  
Please let us now restrict further remarks to the science and engineering aspects of the OP's topic.

If being trolled, DO NOT FEED THE TROLL. It will go away or die.

If site rules are violated, user that little blue "report" button or PM a moderator.

And I JUST LOVE the swimming pool chemical supply section at various stores! Right up there with the ceramic glaze supply, photographic supply and auto supply stores.



I wish I had the 2nd and 3rd ones :(




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[*] posted on 14-10-2014 at 09:25


Quote: Originally posted by blogfast25  
I’ll summarise my work on the lanthanum bearing (10.3 % La glycolate, acc. MSDS) pool phosphate remover called ‘Lo-Chlor Starver’ (from Lo-Chlor Chemicals, AU) as follows.

2.5 L of this solution was neutralised with 33 % NH3 and the snow-white precipitate, presumed lanthanum hydroxide, quantitatively Buchnered and washed. This yielded about 1 L of product.

It was dissolved gradually and quantitatively in 280 ml HCl 37 % with mild heating, followed by simmering. It dissolved completely to a clear solution that was… slightly green! On further boiling that colour changed to yellow. I have very strong reasons to believe this colour is due to MORE than a bit of ferric chloride, more about that later. Possibly there is Pr present.

The solution (about 1.25 L) was then gradually boiled down to about 290 g, by which time it was urine yellow. On refrigeration a mass of small, white crystals formed (photos later) although much of the presumed lanthanum chloride heptahydrate remained in solution, as expected. The rest of the LaCl3 will now be recovered using the double sulphate method (with K2SO4), to try and separate it from the yellow contamination. If it cannot be separated I’m inclined to believe the original phosphate remover contained also Praseodymium. If it can, that would point to ferric chloride.

As regards possible methods of preparing La (and other REE) metals, I proposed the reduction of LaF3 with Li, which appears to be a thermodynamically favourable reaction, possibly with enough reaction heat to ensure clean separation between metal and slag. LaF3 is water insoluble, so fairly easy to prepare.

I earlier dismissed the use of reduction of anh. RECl3 but Brauer’s ‘Handbook of Preparative Inorganic Chemistry’ proved me wrong on that. I suggest strongly that anyone interested in contributing to this discussion go to the Library of this site, download Brauer and print off pages 1135 to 1150 from Volume 2.

There is an absolute wealth of information there that seems to have been overlooked by the ‘RE nutters in residence’ so far, including myself.

Reduction with K, with Ca, alcoholic electrolysis of RECl3 solutions with Hg cathode to REE amalgam and details on electrolysis of anh. RECl3/KCl melts are but a few topics covered. Details on preparing anh. RECl3 is also covered. And for the very curious (Brain&Force?): preparation of some REE(II) salts too, like EuSO<sub>4</sub>.

[Edited on 14-10-2014 by blogfast25]


I'm actually downloading some references from the library for the first time. Frankly, this is embarrassing. I don't have europium (yet) but I will be making some EuSO4 shortly after I have some.

blogfast25, potassium sulfate may not be the ideal reagent for precipitating out the ferric ions. The sulfates of very light REEs appear to be relatively soluble, per the data I linked earlier:

1.png - 32kB

The oxalate method may be preferable, as all lanthanide oxalates are ridiculously insoluble.




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