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Question regarding azeotropes and proper lab technique for acid dillution Options
 
Afrikaaner
#1 Posted : 3/16/2014 1:32:12 PM
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Hey everyone, still relatively new to the whole organic chem thing, but it's slowly turning into an obsession, and I'm trying to make up for my lack of formal training now.

I was wondering what best practices are/anything to be aware of while dilluting acids. Specifically, I'm probably going to be trying to dillute muriatic acid to its azeotrope concentration of around 22% (or something around there), so hopefully when heated under reflux into a soxhlet extractor or similar, the pH of the condensate remains relatively close to the pH in the boiling flask.

Along this line, user benzyme kindly directed my attention to this thread, in which post 11 references the article Amino and Fatty Acids of Wild Edible Mushrooms of the Genus Boletus, Dembitsky (2010) and their preferred mixture of HCl for refluxing.

Quote:
2.2. General extraction procedures of fatty acids
Fresh mushrooms were extracted (Soxhlet) with ethanol-water-HCl (90:10:1, v/v/v) over 24h. The ethanolic residue was further extracted with light petroleum, and then dichloromethane. All fractions were combined, evaporated to dryness at 5oC under reduced pressure, and then dissolved in 2 mL of a cold mixture ethanol-dichloromethane (1:1, v/v). This solution was used for separation by HP-TLC and GC-MS, and followed chemical analysis [1,11,36].


*Is this a known "recipe" for an azeotrope of ethanol, water, and HCl?
*Are there such "recipes" in existence/where can I find them?
*Is the HCl they're talking about the pure gas form? If so, how would I go about calculating the volume of HCl gas dissolved in a specified quantity of muriatic acid? Would it be as simple as 100mL of 30% muriatic acid has 30mL of HCl dissolved in it?

Thanks in advance, and feel free to throw any other suggestions/tips about anything my way!
 

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cave paintings
#2 Posted : 3/16/2014 6:24:44 PM

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"Listen to your father - add the acid to the water"
Slowly, while continuously stirring, add acid to the water - making sure it is not getting too hot or spattering. Wear goggles and gloves.
I am not sure regarding your other questions so much. Make sure to ask if you have any more safety questions though! And maybe look around the interwebs for a organic chem lab manual, which should have lots of safety tips!
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Afrikaaner
#3 Posted : 3/16/2014 9:21:01 PM
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Ok, good to know, I have a small stirplate I was planning to use. And I'm supposed to use a glass stir rod to pour over or something? It's been a long time since any of these things...
 
downwardsfromzero
#4 Posted : 3/18/2014 1:29:25 PM

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Afrikaaner wrote:
[...]

Quote:
2.2. General extraction procedures of fatty acids
Fresh mushrooms were extracted (Soxhlet) with ethanol-water-HCl (90:10:1, v/v/v) over 24h. The ethanolic residue was further extracted with light petroleum, and then dichloromethane. All fractions were combined, evaporated to dryness at 5oC under reduced pressure, and then dissolved in 2 mL of a cold mixture ethanol-dichloromethane (1:1, v/v). This solution was used for separation by HP-TLC and GC-MS, and followed chemical analysis [1,11,36].


*Is this a known "recipe" for an azeotrope of ethanol, water, and HCl?

It worked for them in the context of extracting fatty acids and amino acids.

Quote:
*Are there such "recipes" in existence/where can I find them?

http://en.wikipedia.org/wiki/Azeotrope_%28data%29

Quote:
*Is the HCl they're talking about the pure gas form? If so, how would I go about calculating the volume of HCl gas dissolved in a specified quantity of muriatic acid? Would it be as simple as 100mL of 30% muriatic acid has 30mL of HCl dissolved in it?

They are almost certainly referring to lab standard 37% HCl, which is a lot easier to measure by volume than a toxic, corrosive gas Smile The percentage here is 37 g (weight) HCl per 100 mL (volume) hydrochloric acid: 37% w/v HCl (aq). "30% muriatic acid" would contain 30 g HCl per 100 mL acid.




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
 
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