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Author: Subject: Drunken Aga Challenge #1 - Finished
aga
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[*] posted on 11-11-2014 at 13:20
Drunken Aga Challenge #1 - Finished


Purification & Concentration of a Contaminated Dilute HCl Solution

First Prize: €50
Second Prize €20

Starting Material: 250ml of 3[M] HCl solution contaminated with 0.1[M] FeCl2

Product Required: 6[M] HCl solution with *almost* undetectable traces of Fe2+ ions. Volume irrelevant.

Time Limit for Process: 3 days

Glassware Available: Standard[1]

Machinery Available: Standard[1]

Reagents Available: IC only, available on Ebay for $1/g maximum

[1]Standard = Beakers, tubing, Erlenmeyers, Bungs, Non-Vacuum Distillation aparatus, heater/stirrer, clingfilm, bogroll, oven, kettle, microwave, fridge/freezer etc.

Rules :-

1. Concept/process must be accompanied by stoichiometric chemical formulae.

2. All reaction steps must be in 1 post only accompanied by a photo.

3. Dilutions and concentrations of reagents must be stated (e.g. 10g in 100ml).

4. Temperatures must be stated. If only Ambient temperature applies, state what that is in C.

5. Testing procedures must be explained with photos.

6. The Winner will be the first to post a repeatable Process with photos that You took of You doing it (faces not necessary)

7. Payment of Prize money will be by PayPal.

8. In the event of Dispute, aga's decision is final, unless it's not.

9. There MUST be a can (or bottle) of booze in at least 1 photo. Empty will do.

10. Exceeding the required purity of the Product(s) will be a +point in the decision of winner.


[Edited on 12-11-2014 by aga]

[Edited on 12-11-2014 by aga]

[Edited on 12-11-2014 by aga]




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Brain&Force
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[*] posted on 11-11-2014 at 13:27


Hey, Rador Labs is working on a challenge now! We were hoping to have it up soon.

But 50 euros sounds enticing...




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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[*] posted on 11-11-2014 at 13:33


This the Aga Challenge.

€50 = $62 = £39

Rador can buy it's own beer !




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bismuthate
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[*] posted on 11-11-2014 at 13:36


Curse my young age and lack of beer.
Is HCl an acceptable reagent to use?
Just kidding.




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unionised
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[*] posted on 11-11-2014 at 13:37


That's too easy to be worth $50.
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aga
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[*] posted on 11-11-2014 at 13:39


Quote: Originally posted by bismuthate  
Curse my young age and lack of beer.
Is HCl an acceptable reagent to use?
Just kidding.

Well, Yes !
All you'd have to do would be to add about $300 of Pure HCl and you'd get the conc up and the Fe2+ down.

Please post photos etc and i'll send you the prize.

Edit:

Hint: it's Chemistry.

[Edited on 11-11-2014 by aga]




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[*] posted on 11-11-2014 at 13:53


Am I missing something or does
"distil it through a half decent fractionating column"
not count for some reason?
The product you are after (6M HCl 21.9%) is pretty close to the azeotrope (about 20.2%).

If that's not close enough, a second distillation with added salt will get a higher concentration- you can measure that by determining the density or whatever and dilute it to exactly 6M if that concentration is critical.
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[*] posted on 11-11-2014 at 13:54


"Almost undetectable"? Would that translate as "an ICP masspec won't detect it"?

For reference:
http://en.wikipedia.org/wiki/Inductively_coupled_plasma_mass...
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[*] posted on 11-11-2014 at 14:03


@unionised: read the rules.
Do as you say, post photos, process, formulae and Win !

@DrMario: *almost* undetectable means there's *almost* no Fe2+, e.g. addition of potassium hexaferrocyanate solution will not go more than a teensy bit blue.

*almost* undetectable means *almost* undetectable by qualitative means.

An MS machine would not be available under the 'Machinery Available' part of the challenge.




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


Quote: Originally posted by unionised  
Am I missing something or does
"distil it through a half decent fractionating column"
not count for some reason?
The product you are after (6M HCl 21.9%) is pretty close to the azeotrope (about 20.2%).



Aga, the point he's making is that your task poses not much of a challenge, therefore isn't worthy of prizes or even of much praise when executed successfully.

A worthy competition needs a decent challenge, not something you just made up to get something going.

Let members put forward some ideas and commenters decide which of the proposals meets decent criteria.

[Edited on 11-11-2014 by blogfast25]




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[*] posted on 11-11-2014 at 14:21


My proposal:

Synthesis of a 'pure' solid salt of the Fe(NO)<sup>2+</sup> complex cation. This dark complex forms when cold nitric acid is added to a ferrous salt solution. I've never heard of any solid salts of it being isolated though.

[Edited on 11-11-2014 by blogfast25]




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[*] posted on 11-11-2014 at 14:23


So HCl purification is too difficult then ?



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


Step 1: https://www.dropbox.com/s/uaotferzs2guekn/Photo%20Nov%2011%2...
Take .1mL of the 250mL of impure HCl and add it to 1 liter of reagent grade 6M HCl. Dump the rest of the impure HCl into a container if you want to use it for something else.

Step 2: Drink the unsafe beer that you tried to use in a salting out experiment.
https://www.dropbox.com/s/eq42pcj0w9puyls/Photo%20Nov%2011%2...
I agree this was too easy.
Although the process was a pain with the super small measurement.

[Edited on 11-11-2014 by bismuthate]




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[*] posted on 11-11-2014 at 14:40


*IF* this task is soooo easy to all the Experts, why are there Zero photos, Zero formulae, zero Prize payouts.

Perhaps this trivially simple task is rather too tasking ?




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[*] posted on 11-11-2014 at 14:44


Read the Rules.

Follow said rules, collect cash.

Edit

Did you not read rule 11 ? :)

[Edited on 11-11-2014 by aga]




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[*] posted on 11-11-2014 at 14:49


Ok. The temp was ambient and the leftover HCl must me mixed with the beer to see if anything happens.



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[*] posted on 11-11-2014 at 14:53


Quote: Originally posted by blogfast25  
A worthy competition needs a decent challenge, not something you just made up to get something going.

Let members put forward some ideas and commenters decide which of the proposals meets decent criteria.

An Excellent suggestion.

Aga Challenge #2 will certainly be along those lines.

Aga Challenge #1 remains unsolved.




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[*] posted on 11-11-2014 at 14:56


@bismuthate : Rules 1 ,3 and 5 remain unstated. Photos were nice.

[Edited on 11-11-2014 by aga]




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


The impure HCl was 11% by weight. There where no chemical reactions for rule 1.
Unfortunately without access to my full lab rule 5 remains unfulfilled.
Oh well I couldn't have claimed the money anyway.




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[*] posted on 11-11-2014 at 15:16


Dissolution of an acid in water *is* a chemical reaction.

An equilibrium even.




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[*] posted on 11-11-2014 at 15:20


I will attempt this this weekend. The can of beer might prove problematic, but I think I can find one.



As below, so above.

My blog: https://denovo.substack.com
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[*] posted on 11-11-2014 at 15:23


Well, here we go.

1. Measure out exactly 250ml of your dirty HCl. Close-up here to show dirty color.



2. Set up for simple distillation.



3. Distill. HCl has a negative azeotrope, so water comes over first. Measure and throw away the distillate until you have thrown away 130ml (this gives some leeway). Beer is good at this point because there will be a lot of waiting. Proceed to dryness, collecting everything at 110C. You should collect theoretically 120mL of 6M HCl. (Note that the azeotrope is slightly LESS than 6M, but there was no significant digit specified, and it's well above 5.5M.) :cool:



A sample of the product:



Absolutely no dissolved ions, of course, and well within the concentration specification. You can titrate that if you don't believe me.

A pic of the test method for demonstrating the concentration:



And finally, the test for iron. A sample of the original solution and a sample of the distillate were basified with excess sodium hydroxide, causing heating and boiling. Iron content is shown in the original by flocs of iron hydroxides, which are not present in the distillate, indicating that the iron has been substantially removed.



[Edited on 11-11-2014 by Praxichys]

[Edited on 12-11-2014 by Praxichys]




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[*] posted on 11-11-2014 at 15:30


Close, but no banana.

Rules 4 and 5 apply.




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[*] posted on 11-11-2014 at 15:44


The time limit on the procedure: does that include setup time, or just the time required for the purification, once the setup is completed?
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[*] posted on 11-11-2014 at 15:50


The time limit is the Time it would take from getting the Starting Material to delivering the required product(s).

If you happen to be already set up for that process, you have an advantage.




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