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blogfast25
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aga:
It appears the addition of cupper sulphate has caused neodymium sulphate octahydrate to precipitate (middle photo). Nd2(SO4)3.8H2O is very poorly
soluble in water and does look a bit like that.
Try doing the same using larger sample of 'magnet chloride' soup but using H2SO4 as source of sulphate (NOT CuSO4).
Dissolving Nd magnets in 20 % HCl at RT is slow, especially if you didn't remove all the nickel protective coating. My magnets (coatings partially
removed) dissolve in simmering 37 % HCl in about 1 - 2 h...
[Edited on 6-5-2014 by blogfast25]
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aga
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DOH !
No Magnet Chloride left over.
All got added to the copper sulphate solution (got about a litre left of that mixture).
5ml in test tubes again of the Magnet Chloride + Copper Sulphate solution :
Ethanol precipitated *something*
Ammonia made a large portion of brown stuff immediately settle out, plus a well separated layer of something the same colour as the tetraammine
complex (this is the top layer).
What Test is applicable to Neodymium Sulphate ?
It looks exactly like the iron (III) sulphate photo to me, texture and all.
[Edited on 6-5-2014 by aga]
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blogfast25
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Huh?
How did you manage to 'lose' 500 ml magnet soup so quickly?
What do you mean by 'What Test is applicable to Neodymium Sulphate ?'
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aga
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I added about 500ml copper sulphate solution (mol unknown) to the roughly 500ml Magnet Soup = about 1 litre
The Test thing is basically How To Tell What The Pinky/Violet Stuff is.
There's more precipitated out, but i need to dry it.
I'll send you some to look at if you like.
It's a violet powder.
[Edited on 6-5-2014 by aga]
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blogfast25
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Try this.
Firstly wash it several times with small amounts of hot. dilute (10 % or so) H2SO4. Nd2(SO4)3.8H2O has the peculiar property of being less soluble in
hot than cold water. This procedure washes out any remaining iron, which later would be a nuisance factor.
Then treat it with strong ammonia: you'll see the texture change. Allow this some time by keeping it warm. The ammonia treatment converts the sulphate
to the hydroxide Nd(OH)3. This insoluble hydroxide can now be filtered and washed plentifully with hot water to remove the ammonia and any sulphates.
Look at the wet hydroxide under sunlight and under saver bulb light: it should look slightly different in colour, depending on light source.
Dry it and you've got basically fairly pure Nd(OH)3.
More detailed separation techniques for Nd are plenty, with several experimental examples in this long thread.
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aga
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many thanks blogfast25.
i will give it a go tomorrow.
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Töilet Plünger
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Does anyone have an IR camera? I'd like to confirm if neodymium salts fluoresce in the IR range. And, blogfast, I thought you told me in the terbium
thread that the potassium double sulfate is less soluble in water than neodymium sulfate alone. (Though, according to an old reference I found,
neodymium also forms an acid sulfate. I'll have to dig it up - it's on Google Books somewhere.)
Happy 5000th post blogfast25!
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aga
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Yay !
Happy 5000 to yooo. Happy 5000 to yoooo
[Edited on 6-5-2014 by aga]
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aga
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| Quote: | | Does anyone have an IR camera? |
You probably do.
Most cameras are IR sensitive anyway, so a Filter is inline with the lens to correct the colour response of even a $5 usb camera.
Hmm. that gives me an idea.
[Edited on 6-5-2014 by aga]
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Töilet Plünger
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Well, it has to be able to collect light at 1064 nanometers - that's one of the transitions visible. (A neodymium yttrium orthovanadate laser uses
second harmonic generation to get green light @ 532 nm.) If it can pick up the IR light from a neodymium laser with the KTP frequency doubler removed
or the green light selectively filtered, the camera works.
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aga
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Just try it.
Maybe a cheap camera will react to 1064nm with the IR filter removed.
Seems to me that far too much calculation is going on and not enough experimentation, on which ALL known science is based.
Once upon a time some madman distilled a large quantity of ants.
I seriously doubt that he had calculated the result before just doing it.
Time to put some madness back.
Does it Blend ?
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blogfast25
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Quote: Originally posted by Töilet Plünger  | And, blogfast, I thought you told me in the terbium thread that the potassium double sulfate is less soluble in water than neodymium sulfate alone.
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It is. But the Nd sulphate is insoluble enough for a crude separation. You'll lose more of it though. I was keeping things simple for aga. The K
double sulphate method is my preferred method.
A hydrogen sulphate? Possibly. We know for sure there are two variations of the sulphate, it's been discussed extensively in the various Nd threads.
One is pinkish and sandy and doesn't seem to crystallise easily, another is reddish and crystallises into beautiful crystals. Whether one of them is a
bisulphate I don't know.
[Edited on 6-5-2014 by blogfast25]
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aga
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| Quote: | | I was keeping things simple for aga |
Very necessary.
I truly know next to nothing.
Thanks again blogfast25 for keeping it simple for a noob to understand.
You are a Guiding Light.
Finding things (out) is a lot easier when there is Light.
[Edited on 6-5-2014 by aga]
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Brain&Force
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I was going to propose the existence of a bisulfate as a possible explanation for the two different varieties in the thread, "two times neodymium
sulfate, different colors."
At the end of the day, simulating atoms doesn't beat working with the real things...
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aga
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All i did was put some hard drive magnets (no pre-processing) into 20% OTC HCl,
waited for the magnets to dissolve, filtered, added copper sulphate solution,
decanted, washed with water (repeat a few times).
When washing, the upper liquid layer has a blue tint, very much like the Copper Sulphate solution, rather than any hint of green.
Result from 125g magets is 10.12g of pale pink talc-like powder.
The nearest wiki photo suggests it's Iron (III) Sulphate,
but it looks identical to the photos in this thread,
which suggests that it's Nd2(SO4)3.8H2O
Am i missing something here ?
[Edited on 7-5-2014 by aga]
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blogfast25
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Nope. That's neodymium sulphate in one of its two forms. A bit silly to waste CuSO4 as a source of sulphate ions. Instead use sulphuric acid or Na2SO4
(Glauber salt) or K2SO4 or (NH4)2SO4. The latter two can be found in garden centres but need recrystallizing to use as reagents.
Ferric sulphate is so soluble it's hard to crystallise. The wiki photo is probably of the monohydrate.
Object lesson: appearances are deceptive.
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aga
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| Quote: | | silly to waste CuSO4 as a source of sulphate ions |
I can get copper sulphate for 4 euros a kilo, but have not found sulphuric acid yet.
Isn't the fact that on washing the precipitate you can see the blue copper sulphate a useful indicator ?
As in, keep washing until no blue colour seen = copper sulphate mostly gone.
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elementcollector1
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What about Epsom salts (magnesium sulfate)?
Elements Collected:52/87
Latest Acquired: Cl
Next in Line: Nd
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MrHomeScientist
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Blogfast is right, appearances are deceiving especially in the case of rare earth salts like neodymium sulfate. When describing what
it looks like, you have to specify under what lighting conditions because it can look very different depending on the light source. My neodymium
sulfate (pictured in this thread somewhere) was white to tan under small fluorescent tube lights, pink under incandescent bulbs, purple under long
tube fluorescent lights, and a very richly colored pink under sunlight. A fun past-time is to take a vial of your sulfate and walk from one room to
another and then go outside, watching the color change smoothly.
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blogfast25
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Yep, why not, indeed?
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elementcollector1
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In recent news, my neodymium oxide is proving immune to sulfuric acid (diluted with a little bit of water). I wonder if this requires prolonged
boiling in order to react?
Elements Collected:52/87
Latest Acquired: Cl
Next in Line: Nd
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IrC
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| Quote: Originally posted by MrHomeScientist | | Blogfast is right, appearances are deceiving especially in the case of rare earth salts like neodymium sulfate. When describing what
it looks like, you have to specify under what lighting conditions because it can look very different depending on the light source. My neodymium
sulfate (pictured in this thread somewhere) was white to tan under small fluorescent tube lights, pink under incandescent bulbs, purple under long
tube fluorescent lights, and a very richly colored pink under sunlight. A fun past-time is to take a vial of your sulfate and walk from one room to
another and then go outside, watching the color change smoothly. |
Is this not due to the amount and frequency of uV light in the source? The 'appearance' of the material ends up being a combination of both the
reflected light and the light being produced by uV induced fluorescence in the specimen?
"Science is the belief in the ignorance of the experts" Richard Feynman
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aga
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OK. Point gratefully received.
It's going dark here, so i'll trog down to the chem shed to see what it looks like under florescent light, LED light and a halogen light.
Under tri-colour LED light it appears pale violet
White Florescent light makes it grey/pink
Halogen light makes it appear violet/pink again.
[Edited on 7-5-2014 by aga]
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Brain&Force
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elementcollector1, why are you redissolving the oxide in sulfuric acid? Have you already separated the Nd?
At the end of the day, simulating atoms doesn't beat working with the real things...
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elementcollector1
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Yes. Now that it's separated, I need to convert it to a more volatile compound like chloride or fluoride to get the metal - this is most easily
accomplished, in my view, with sulfuric acid, followed by sodium hydroxide, followed by hydrochloric acid.
Seriously, though, I must have done a really good job calcining it. No reaction whatsoever, and it's been a whole day.
Elements Collected:52/87
Latest Acquired: Cl
Next in Line: Nd
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