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Author: Subject: Rador Labs Challenge 11-12/2014: High Stakes, High Mass
Metacelsus
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[*] posted on 24-11-2014 at 09:40


I understand what you're doing now. That's a really clever idea. However, sucrose has a molecular mass of 342.3 grams per mole, so according to the rules of the challenge, you can't use it as a pure starting material; you'd have to get it from an impure source (brown sugar, maybe?).



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[*] posted on 24-11-2014 at 10:31


K. I was going to submit an experiment, but a terrible thing happened to me and I won't be able to do it. My idea was a saccharide poliester (stearic or whatever), around 2500g/mol. Feel free to use it, easy isolations and reactions; isolation of final product is an odyssey. Still, the numbers are getting really huge here! Probably it won't be a winner.



Bromine, definitely bromine.
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[*] posted on 24-11-2014 at 10:43


Quote: Originally posted by Oscilllator  
I know at least one other member is trying to synthesise this compound and so in the interests of fair play I will disclose that I have successfully used hydrolysed sucrose and sodium metabisulphite to form the complex, forming visually identical products. I don't actually have any of the reagents that published procedures have used, so at this point I'm just mixing together reagents haphazardly to try and get some results.


Molybdenum Blue. I was thinking of using other reducers too, no reason to believe the prescribed dithionite or hypophosphite are the only potential reducing agents here. QED.

I was messing with some WO3 before (my original target was barium phosphotungstate hydrate, about 4000) and sodium sulphite induced a decidedly strong blue colour into some freshly prepared aqueous WO3 (adding peroxide made the blue disappear again). Like Mo(VI), W(VI) is prone to partial reduction to W(V) and the mixed valence W(V,VI) complexes show charge transfer absorption bands at 745 nm, resulting in intense blue colour. It's what led me onto the Moly Blues.

I won't be entering the race now, as I can't see how 23,000 can be beat. I hope you win, you were the first to have the idea. Isolating it will be a matter of time. Touch wood!



[Edited on 24-11-2014 by blogfast25]




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[*] posted on 24-11-2014 at 11:14


Quote: Originally posted by blogfast25  

Molybdenum Blue. I was thinking of using other reducers too, no reason to believe the prescribed dithionite or hypophosphite are the only potential reducing agents here. QED.


Hahahaha... btw the terrible thing was reading this page in the wiki.




Bromine, definitely bromine.
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[*] posted on 24-11-2014 at 12:32


Quote: Originally posted by blogfast25  
I can't see how 23,000 can be beat.

Add an atom or two of something else ?




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[*] posted on 24-11-2014 at 12:35


Make the potassium salt?




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[*] posted on 24-11-2014 at 14:04


Aga and Bismuth: enter the competition through the Big Wheel! But I'm out.

The wheel is an Mo154 structure. One paper claims an Mo358 'sphere' is theoretically possible but no amateur could ever characterise that convincingly, assuming it can be made even...

[Edited on 24-11-2014 by blogfast25]




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[*] posted on 24-11-2014 at 14:25


I have part of the workup to my pathetic entry drying in the shed.

If it survives the next 3 or 4 steps, i'll post it anyway, despite the fact it couldn't win.

Who needs transparent aluminium/titanium alloy anyway ?

[Edited on 24-11-2014 by aga]




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[*] posted on 24-11-2014 at 14:33


https://www.dropbox.com/sc/viz0y6wu75nzncn/AACv952dt-2bVk9fE...
https://www.dropbox.com/sc/2rcpwpsj1fvuuhy/AABmc5M3_RzP0mmDl...
I've had success in isolating molybdenum blue using sodium thiosulfate, sodium molybdate, and hydrochloric acid. Now read this all the way through. I don't plan on submitting this. I just want to say that I've seen that this compound seems to be ruining the competition. Everybody has seemed to have just given up. I can't stand for that, so not as a Rador Labs member, but as a contestant I say that Molybdenum blue should be disallowed. I don't want this as an official rule, but I would ask that nobody try to make this. I could win now, but it's just much fun this way and I think that should be the point of this competition. Could everybody stop the pursuit of this compound even though this isn't a submission?




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[*] posted on 24-11-2014 at 14:54


Bismuth:

Competitions like this will occasionally turn up these 'spoilers', but that's no reason to ban them.

Banning makes everything contrived and people like Oscillator have already spent considerable time and effort into looking for the highest MW entry possible. I think that should be honoured.

Changing the competition's rules every 5 minutes just because something pops up makes it into a farce, IMHO. Imagine if this had been published a bit more far and wide and 100s of people took part: you'd have a riot on your hands and rightly so IMHO.

[Edited on 24-11-2014 by blogfast25]




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[*] posted on 24-11-2014 at 14:58


While it's definitely true that molybdenum blue is a bit of an easy instant win for those who can get molybdenum fertilizers (assuming there isn't someone else lurking with something even more spectacularly heavy), it would be very unfair to change the rules at this point since some people have already put in a good amount of time and effort, and possibly money if they hadn't previously owned the needed molybdenum compounds. We may run a better version of this competition again sometime in several months, and that should run much more smoothly than this one.

Edit: blogfast replied while I was typing this, we said essentially the same thing.

[Edited on 11-24-2014 by zts16]




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[*] posted on 24-11-2014 at 15:06


I'm not banning this. I'm just saying that I can submit it but am choosing not to so that other compounds stand a chance and the competition is more fun. Anybody could still submit it if they want, I just ask that they don't to make the competition more fun. I'm not a member of Rador Labs saying this, just a participant. No rules were changed



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[*] posted on 24-11-2014 at 15:21


If you've Made it in relation to this competition, you *have* to submit it, or us noobs will not see how it's made !

Everybody stop panicing !

If Molly Blue is HUGE, groovy.

The POINT is not the $22 (it went up)

The POINT is having some fun, and learning something, so refusing to post MB now would be a severe disappointment to me at least, as it'd be great to see how it's made.

Edit:
a flash of genius: molly blue with a hint of pink ...

[Edited on 24-11-2014 by aga]




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[*] posted on 24-11-2014 at 15:28


I just mixed 1g sodium thiosulfate, 2g Sodium molybdate, and 10mL of 39% HCl is water. Then I filtered. Pretty simple actually.



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[*] posted on 24-11-2014 at 15:28


Molybdenum blue synthesis shots from a while back :)


image.jpg - 1.4MB image.jpg - 846kB image.jpg - 1.5MB




[Edited on 24-11-2014 by Mailinmypocket]
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[*] posted on 24-11-2014 at 15:30


When and how did you make it?



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[*] posted on 24-11-2014 at 15:34


About a year ago, something around that. I used the instructions from here http://lambdasyn.org/synfiles/molybdaenblau.htm which are from Brauer.

Instead of sodium molybdate I used molbdenum oxide, zinc and HCl


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[*] posted on 24-11-2014 at 15:38


Blue products are forbidden under the local Porn by-laws.

(is mine gonna be blue ? doh !)




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[*] posted on 24-11-2014 at 15:38


Ahh you made a very different molybdenum blue from the one I made.



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[*] posted on 24-11-2014 at 16:37


This is not an official submission, but it is my current personal best for heavy compounds. It is disodium copper(II) dichloroisocyanurate. It (I think) has the formula Na2[Cu(C3N3O3Cl2)4] which gives it a mass of 897.3552 g/mol
I made this some time ago, and it isn't the entry that I'm currently working on. I just thought it would be nice to look at something other than molybdenum blue for a bit.
IMGP0380.JPG - 726kB
It actually looks even more purple in person. My camera can't handle the purple.




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[*] posted on 24-11-2014 at 16:42


Beautiful !

What's the Procedure to make it ?




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[*] posted on 24-11-2014 at 17:15


Wow! That's really pretty!
I'll have to get my game on.
Good luck everyone.




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[*] posted on 25-11-2014 at 12:09


The moment you've all been waiting for ...

It's from page 326 of Brauer : Barium Periodate
Ba3H4(IO6)2
MM 861.9
Sample: 0.92g

To start with, i had some Barium Nitrate, KOH, Bleach, NaOH, KCl (no-sodium salt) and 2g of elemental I2

Starting with 1g of the I2, it was calculated that there would be 3.6g of end product. All stoichimetry was worked out from 1g of I2.

Brauer's called for KClO3, which was not available, so 1 litre of bleach was boiled down until crystals started to form, then allowed to cool, and 100ml of the supernatant liquid collected. The Crystals are apparently NaCl.

As this was OTC bleach, there were some oils and crud floating on top, so a separatory funnel was used to remove them before filtering.

Then some dissolved, filtered KCl was added, and a precipitate was seen.

After 2 recrystallisations, plate-like crystals of KClO3 were obtained (they're in the petri dish).

After that, Brauer's was followed.
Especially wonderful was the reaction of KIO3 + KOH + Cl2

The liquid is clear to start with, and as Cl2 is pumped through it, Nothing happens until a certain point, after which a worrying Iodine cloud forms, then sparkly blueish crystals of KIO4 snow out of solution.

Finally those crystals were separated, washed, dissolved in KOH solution and Ba(NO3)2 solution was added, at which point white Barium Periodate crystals dropped out of solution.

I only got 0.92g of the theoretical 3.6g (25.6%)
(see dribble on microscope slide)

Who cares ?
I never did most of those procedures before, and it was a blast !



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[*] posted on 25-11-2014 at 12:38


Nice. Now I would accept it if it were up to me, but the product must be a dry power. I'm sure it won't take too long to dry. Good job. Try making the copper complex. It's really cool.



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[*] posted on 25-11-2014 at 12:41


What's 'THE' copper complex ?

Copper complex with Barium Periodate ?




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