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woelen
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Smart-elements sells Cs at EUR 79 per 100 gram at ultra high purity.
http://www.smart-elements.com/?arg=detail&element=Cs&...
I myself have been quite lucky, I found CsCl on eBay around a year ago for GBP 8 per 100 grams. My CsCl, however, is not as pure as the material
mentioned above. It has a purity of appr. 98% with the remainder being mostly KCl and a small amount of RbCl. For my experiments, however, it is good
enough.
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blogfast25
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Thanks, woelen.
Well, well: standing overnight in an ice bath did yield a crop of crystals, from yesterday's 33 % batch:
Again, the colour is false, it’s really purple.
Although this could be NH4Ti(SO4)2.12H2O, it could also be plain (NH4)2SO4 doped with a bit of Ti2(SO4)3. The quantity (volume, visual estimate) is
decidedly more than the volume of (NH4)2SO4 I added though (but it’s subjective). The crystals are small but well formed and I’ll try and take a
look under my (crappy) microscope.
The only firm decider here is to determine the Ti content.
[Edited on 28-10-2013 by blogfast25]
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deltaH
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Nice blogfast25! Good luck with your determination.
Are you still going to try the cesium version?
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blogfast25
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It's low on my list. Ti assay of the last product, even higher concentrations of Ti2(SO4)3 and the KTi alum (assuming the NH4Ti is a real alum) are
more interesting than confirming what we already know (that the CsTi alum exists).
I can certainly confirm that the suspected NH4Ti alum is completely soluble in water, to a clear solution. And the colour seems far too intense for
just Ti3+ doped (NH4)2SO4. Just a few more sleeps before I know the definitive answer... 
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blogfast25
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The results of the Ti assay of the suspected NH4Ti alum are in.
The material was first washed with ice cold 10 % H2SO4, then gently patted dry with filter paper and stored in a CaCl2 desiccator. The material came
out much lighter in colour, so that made me fear partial oxidation to Ti(IV) had taken place. 6.4 g of dried material was obtained.
But making the stock solution of about 0.1 M concentration in 1 M HCl showed all of it dissolved without insoluble residue. It did not dissolve very
fast though and some gentle heating was applied to speed things up. Here’s the stock solution:
This solution was the titrated against 0.1 M ferric ammonium alum:
Ti3+(aq) + Fe3+(aq) === > Ti4+(aq) + Fe2+(aq), using KSCN as an indicator for excess Fe3+.
I found the titanium content of the sample to be 13.2 w%. The theoretical value for NH4Ti(SO4)2.12H2O is 10.1 w%. So a tad too high for
comfort.
A couple more qualitative tests were carried out too. The dried material doesn’t appear to dissolve/react with acetone or surgical ethanol.
When mixed with some powdered NaOH and heated in a test tube, the smell of ammonia is unmistakable, pointing to ammonium ions being part of the
material. This could also be the basis of a quantitative test: dry distilling off the NH3 into a known amount of standardised HCl, followed by
titration of the remaining HCl, to determine ammonium content.
I’ve also prepared another batch of Ti2(SO4)3 solution, this time of even higher concentration, this time aiming at the potassium alum again.
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soniccd123
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There is no more progress on this? I'm planing to try some of what is described at this topic with Zirconium in next months (in summer vacations
actually, right now i'm at med school so i really don't have time).
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blogfast25
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Quote: Originally posted by soniccd123  | | There is no more progress on this? I'm planing to try some of what is described at this topic with Zirconium in next months (in summer vacations
actually, right now i'm at med school so i really don't have time). |
What do you have in mind?
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soniccd123
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| Quote: Originally posted by blogfast25 | | Quote: Originally posted by soniccd123 | | There is no more progress on this? I'm planing to try some of what is described at this topic with Zirconium in next months (in summer vacations
actually, right now i'm at med school so i really don't have time). |
What do you have in mind? |
Well, I know that Zirconium (III) ions exists and supose that they may have similar properties to the Titanium (III) ions. I have some objetives in
mind:
- Produce a Zirconium (III) solution and understand how to handle and maybe stabilize it;
- Crystalize the Zirconium (III) salt from it;
- Crystalize a Zirconium alum from it.
I know that may be very hard, even impossible with the equipment i have at home, but i'm really willing to try it. To do this, i suspect that some of
the techniques, procedures and informations provided by this thread are going to be really helpful.
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blogfast25
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| Quote: Originally posted by soniccd123 |
Well, I know that Zirconium (III) ions exists and supose that they may have similar properties to the Titanium (III) ions. I have some objetives in
mind:
- Produce a Zirconium (III) solution and understand how to handle and maybe stabilize it;
- Crystalize the Zirconium (III) salt from it;
- Crystalize a Zirconium alum from it.
I know that may be very hard, even impossible with the equipment i have at home, but i'm really willing to try it. To do this, i suspect that some of
the techniques, procedures and informations provided by this thread are going to be really helpful. |
Do you have any literature references for Zr(+3) compounds? They would be even more prone to easy oxidation than Ti(+3) compounds, assuming they even
exist.
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woelen
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As far as I know, Zr-compounds cannot exist in +3 oxidation state as soluble ions in water. There are lower oxidation state Zr-compounds, but these
are high melting solid compounds, often with indeterminate stoichiometry, or extremely air/moisture sensitive compounds.
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soniccd123
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Yeah, you guys are right. I found Zirconium (III) Chloride and other halides names at the CRC Handbook of Chemistry and Physics, then, just for sake
of curiosity, i've got to search some articles about it; I found some and had them saved in my computer but didn't read till now. It really exists,
but is extremely sensible to moisture as woelen said.
My bad people, I should had researched a bit more before posting.
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blogfast25
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| Quote: Originally posted by soniccd123 | Yeah, you guys are right. I found Zirconium (III) Chloride and other halides names at the CRC Handbook of Chemistry and Physics, then, just for sake
of curiosity, i've got to search some articles about it; I found some and had them saved in my computer but didn't read till now. It really exists,
but is extremely sensible to moisture as woelen said.
My bad people, I should had researched a bit more before posting. |
That's not to say that a bit of Zr chemistry wouldn't be interesting for this forum. I have a few threads on it.
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soniccd123
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| Quote: Originally posted by blogfast25 | | Quote: Originally posted by soniccd123 | Yeah, you guys are right. I found Zirconium (III) Chloride and other halides names at the CRC Handbook of Chemistry and Physics, then, just for sake
of curiosity, i've got to search some articles about it; I found some and had them saved in my computer but didn't read till now. It really exists,
but is extremely sensible to moisture as woelen said.
My bad people, I should had researched a bit more before posting. |
That's not to say that a bit of Zr chemistry wouldn't be interesting for this forum. I have a few threads on it. |
Indeed! I'll try other things with it anyway, I just realized that Zr3+ is really impractical. I'm interested in this 3+ state on the
Titanium group metals, it seems to be not much explored. Besides being highly sensitive to oxidation, Ti3+ looks to behave in a very...
"classic" way like other transition metals do, i mean, just like Cu2+ or Ni3+
Have you ever been able to crystalize out pure Ti2(SO4)3?
[Edited on 26-9-2015 by soniccd123]
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blogfast25
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No. I'm not sure it's possible. Ti<sup>3+</sup> requires very low pH to prevent hydrolysis or oxidation of water. I have made
Ti2(SO<sub>4</sub>3 solutions of about 30 w%
though... with high acid reserve. Maybe with vacuum evaporation these solution would have yielded crystals, who knows?
[Edited on 26-9-2015 by blogfast25]
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