Dry HCl gas from muriatic and sulfuric acids conc.

G.Patton

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CaCl2 is considerably safer to handle than concentrated H2SO4. It also is available at low cost, sometimes as a byproduct of the Solvay process. The standard assemblies for gas generation shown above are appropriate for the preparation of crude HCl(g).

It is able to fix enough water (over the 30% of its weight considering it hydrates only to CaCl2·2H2O, which is stable up to 150 °C) to deliver a significant amount of HCl gas. In a typical run, 100 g of 35% HCl were added over 100 g of granular CaCl2 at room temperature (the thermal effect is not significant), and 15 g of HCl(g) were obtained. This represents over 40% yield, which may be compared with the 80%, yield reported for the process represented in Eq. 2; however, it uses approximately a 1:3 weight ratio between H2SO4 and HCl(aq).

CaCl2 also is easier to dispose of than H2SO4, and less base is required to neutralize the final waste. An additional advantage of this procedure regarding those based on H2SO4 concerns educational aspects. By heating at 200 °C, the resulting waxy mixture (or crystalline mass to which it converts after a few hours), the anhydrous CaCl2, can be regenerated for re-use once a solution of HCl is obtained. In this case, some calcium oxychloride formed can be ignored.

Even though this may be without value from a practical viewpoint, it may be of educational significance because it attracts attention to topics of current interest such as optimizing of processes, recycling of chemicals, and reducing of wastes. To this end, the assembly shown in Fig. b is more appropriate than that in Fig. a because the resulting mixture is ready to be distilled.

UPD: An alternative way:​
 
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Riot

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Hi , ım thinking the use fig. a but you mentioned water will decrease your yield how much decrease will drop , did ı suppose to use trapped hcı gas gen in smaller synteshis will make problem

Thanks.
 

G.Patton

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I'm sorry, but I don't understand your question.
 

ASheSChem

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sorry @G.Patton :(
i'm trying to understand well the answers... English + noob = difficulty ;)

I'm just trying to find out what equipment I still have to buy for this operation and be sure to understand all step and reagent ^^
"Preparation of methamphetamine hydrochloride is carried out by bubbling of dry HCl gas via organic layer. "
 

G.Patton

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Your set-up from pic is okay. I fixed in previous message on picture.
 

ASheSChem

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okok sooo last confimation ...
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1) in "fig 2" i put water or MgSO4 or nothing.. ?
2) in "fig 3" same question... :x
3) when i want to stop the gaz i use "fig 1" ?


thank you so much..
 

G.Patton

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You have to get rid of water!!!
fig 2- H2SO4 or solid NaOH/KOH
fig 3- CaCl2 or MgSO4
yes
 

ASheSChem

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thank you so much :)
I think now I won't be afraid and dare to try this ;)
 

ASheSChem

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I died laughing... today my sister-in-law sends me a picture from these science classes because she knows I like it..

Sbjq26coa0


me : "ho cool , you doing HCl gaz ?"
she : "i don't know... i ask... hmm wtf yes it's HCl gaz"

haha
 

diogenes

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Hi, I have seen e.g. in a the Uncle Fester video that he put a lot of table salt in the HCl generator, I guess he used this to dehydrate the HCl? Any experience/opinion about this method? Would one drying agent be enough if using NaCl in the generator? E.g. NaCl in the generator + just a CaCl2 drying tube.

I thought the circled container (where the bubbling tube is placed when not used) is filled with e.g. NaOH solution to neutralise the HCl, otherwise it would continue to fill the room?
 

G.Patton

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I think yes, it would be enough.
 

diogenes

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Thank you Patton, will try it like this then.
 

robertlouis

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About Anhydrous hydrogen chloride gas.
Whats the diffrent this thread with 2 other method below:

A. NaCl with little hcl acid in flask n drip H2So4 (fester meth version)

B. NaCl (without HCL Acid) in flask n drip H2So4
 

Saul

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@robertlouis there are 4 methods choose the one fits the best for you.

for me the microwave method is the easiest using 2
https://ae01.alicdn.com/kf/H8b97106480324459996555df0a565d94g/Spuit-500-Ml-Grote-Capaciteit-Spuit-Herbruikbare-Pomp-Meten-Met-1M-Buis-Voeden-Inkt.jpg_Q90.jpg_.webp
 

kharpa177

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wanted an instruction on how to bubble hcl in the final solution
 

WinterDust

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Hi,

Here is a quite good graphic setup for HCl Gas setup, the open flame can be exchanged with a magnetic stirrer with heating aswell.

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workworkwork

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My total dry HCL gas generation failure using CaCl2 method:

My setup were 3 plastic buckets connect by plastic tubes. The plastic bucket number 2 was an empty bucket, a trap, if the freebase on bucket number 3 got sucked.

In the first bucket I put 800g of calcium chloride. I put the lid on the bucket and through one of the previously prepared holes I poured muriatic acid. There was no reaction! Not 1 gas bubble in my mdma freebase in acetone. I don't understand what I did wrong. The muriatic acid could have some protection to not release vapors? Was necessary wait more than 20 minutes?
 

malignoalfa

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When using HCL gas to acidify the free base, I don't need to worry about over-acidification? Just bubble the gas until there is no more precipitate? Or should I bubble the hcl gas little by little and measure the pH?

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Osmosis Vanderwaal

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Since then I've got a couple of hose adapters so I don't have to use the 110° turn down for a hose adapter and steel kek clips ( the plastic ones become brittle instantly if they get gassed). Overall a mountainous contraption that will gas you in the blink of an eye if you aren't careful 😘 good luck with explaining those brown fingers 😉
 
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