Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
Author: Subject: Ni(IV) - periodatonickelates
Fery
National Hazard
****




Posts: 485
Registered: 27-8-2019
Location: Czechoslovakia
Member Is Offline


[*] posted on 10-2-2020 at 08:42
Ni(IV) - periodatonickelates


KNiIO6 . 1/2 H2O
Dissolve 3,0 g KIO4 in 500 ml boiling water in 1 l Erlenmayer flask, then add 2,0 g NiSO4 . 6 H2O, dissolve (solution is not completely clear, there is a turbidity). To the boiling solution add 4,0 g of K2S2O8 in 0,4 g portions during 30 minutes. The solution must be stirred. When adding K2S2O8 into the boiling solution it seems to immediately decompose into O2. So I suggest to add it few seconds after removing the flask from the heat when the boil ceases while swirling the flask by hand, then no such vigorous production of O2 bubbles. Then let it to boil for 10 minutes. Allow black very fine crystals to settle. Small additional amount of the product obtained when the same procedure repeated with the supernatant (adding 4,0 g K2SO4 to it). Decant the product 3 times with 100 ml of 1% hot K2S2O8 and 3 times with 100 ml of hot water acidified with HNO3 (0,5 ml HNO3 into 300 ml of water), transfer to sintered funnel and dry with suction. Sintered glas No 2. is not dense enough and the crystals pass through it, you must use denser sinter (No 4.). Do not use filter paper as it reduces the product. Dry out over CaCl2. Yield 0,53 g.
Use 10% oxalic acid to clean the glass (few minutes required, but it dissolves completely at the end).
some info here:
https://www.sciencemadness.org/whisper/viewthread.php?tid=72...
https://en.wikipedia.org/wiki/Periodatonickelates

photos will follow

201.png - 132kB 202.png - 152kB 203.png - 143kB 204.png - 142kB

Attachment: currie1994.pdf (604kB)
This file has been downloaded 78 times

Attachment: v69-630.pdf (162kB)
This file has been downloaded 74 times

[Edited on 10-2-2020 by Fery]




If there is a heaven, it seems not to be materially based. Does chemistry exist there and if yes, how does it look like? Are there good souls well supplied with laboratory equipment, glass, chemicals and information?
View user's profile Visit user's homepage View All Posts By User
Fery
National Hazard
****




Posts: 485
Registered: 27-8-2019
Location: Czechoslovakia
Member Is Offline


[*] posted on 10-2-2020 at 08:57
photos


reactants - KIO4, NiSO4 . 6 H2O, K2S2O8

IMG_20200203_103944_2_sm.jpg - 33kB



3,0 g KIO4 + 500 ml H2O + 2,0 g NiSO4 . 6 H2O

IMG_20200203_110039_3_sm.jpg - 17kB



after addition of first 0,4 g K2S2O8

IMG_20200203_111122_0_sm.jpg - 29kB



after addition of all 4,0 g K2S2O8

IMG_20200203_112034_4_sm.jpg - 30kB



a mirror formed on the flask

IMG_20200203_113647_3_sm.jpg - 19kB



boil for 10 minutes

IMG_20200203_113737_7_sm.jpg - 37kB



the mirror is reddish from inside of the flask

IMG_20200203_114048_9_sm.jpg - 20kB IMG_20200203_114109_2_sm.jpg - 20kB IMG_20200203_123348_8_sm.jpg - 29kB



but it reflects the light from outside of the flask

IMG_20200203_123522_8_sm.jpg - 31kB IMG_20200203_123611_9_sm.jpg - 33kB



small additional amount of product obtained when the procedure repeated with supernatant (adding K2S2O8 into it)

IMG_20200203_130918_6_sm.jpg - 25kB



the product KNiIO6 . 1/2 H2O

IMG_20200210_133157_8_sm.jpg - 21kB

[Edited on 10-2-2020 by Fery]




If there is a heaven, it seems not to be materially based. Does chemistry exist there and if yes, how does it look like? Are there good souls well supplied with laboratory equipment, glass, chemicals and information?
View user's profile Visit user's homepage View All Posts By User
woelen
Super Administrator
*********




Posts: 7448
Registered: 20-8-2005
Location: Netherlands
Member Is Offline

Mood: interested

[*] posted on 10-2-2020 at 11:48


Interesting material. I once made this material accidentally, in an attempt to make something else. I obtained a very dark red solution and interesting crystals. According to the wiki page about this material, it can be used to make perbromates. I think that in practice, however, this will be very challenging. Isolating the perbromate from all that nickel, periodate and bromate in the solution will be a difficult task, requiring many steps.



The art of wondering makes life worth living...
Want to wonder? Look at https://woelen.homescience.net
View user's profile Visit user's homepage View All Posts By User
Tdep
National Hazard
****




Posts: 496
Registered: 31-1-2013
Location: Fixed Lasers
Member Is Offline

Mood: *laser noises*

[*] posted on 10-2-2020 at 16:03


I really want to believe that you can use KNiIO6 to make perbromate. But looking at the journal article doesn't give me much hope even before opening it.

Its published in some no-name journal with an impact factor of 0.17 and had only 4 issues... fine sure, then the paper has 11 citations, which is nice, but 10 out of 11 of them are from the same author 'Sharanappa T Nandibewoor', so that's not a great sign. Not citations from the other perbromate literature?
This perbromate paper from 2011 did not mention Nandibewoor's work at all for example.

Ok sure, maybe they missed it. But I don't like the paper I gotta say. I think the main thing that you need to do when making some sort of exotic species is prove that you actually made the thing. How do they try and convince you they made it?UV-Vis. Yeah. And it gets worse. Because do they actually show that data? No. They just link to papers from the 1960s (!) and 70s and say 'it matched this'!!

If I want to procrastinate more work later today, I'll look up the 1960s references and find the UV-Vis data, but given its a colourless anion, I find it hard to believe it would be easily distinguished from periodate or bromate in this way

perbromate1.PNG - 224kB perbromate2.PNG - 70kB
View user's profile View All Posts By User
Fery
National Hazard
****




Posts: 485
Registered: 27-8-2019
Location: Czechoslovakia
Member Is Offline


[*] posted on 11-2-2020 at 03:52


woelen and Tdep, if you are interested in NaBrO4 then it is easier to separate it when reacting NaBrO3 + NaOBr at 40 C for few days - weeks
oxidation by F2 is not easy to done in home lab
also oxidation using Ni(IV) diperiodonickelate attached, but only kinetics, not the isolation of the product

Attachment: pisarenko2011.pdf (1.4MB)
This file has been downloaded 112 times

Attachment: bilehal2002.pdf (98kB)
This file has been downloaded 92 times

Attachment: appelman1969.pdf (619kB)
This file has been downloaded 89 times




If there is a heaven, it seems not to be materially based. Does chemistry exist there and if yes, how does it look like? Are there good souls well supplied with laboratory equipment, glass, chemicals and information?
View user's profile Visit user's homepage View All Posts By User
Justin Blaise
Hazard to Self
**




Posts: 80
Registered: 5-10-2011
Location: Parts Unknown
Member Is Offline

Mood: No Mood

[*] posted on 11-2-2020 at 19:06


Very cool compound. I wonder if it's an energetic oxidant with things like sugar or Al powder.
View user's profile View All Posts By User

  Go To Top