Couple pH questions

[Kash]

I have noticed with limonene if you over acidify it will produce green crystals sometimes, but since you used toluene then thats probably just plant material that somehow made its way into your end product. Should be able to rmove it with water and filtering/decanting.

After pulling your base soln with your np 4-6 times, you can combine into one volume, and then you only need to do 1 salting to pull 99% of the mesc. No reason for multiple saltings this just leads to over acidifying and garbage being pulled into your product.

 

[cyantific]

After pulling your base soln with your np 4-6 times, you can combine into one volume, and then you only need to do 1 salting to pull 99% of the mesc. No reason for multiple saltings this just leads to over acidifying and garbage being pulled into your product.

Never thought about it like that. Certainly would save some time. Been following foafs tek which calls for 12 saltings which is very time consuming. If only salting once, does it need to be a large volume of water? What would be the ratio of np to water?

 

[foaf]

the green color is odd

and the reason my early tek says do it 12 times is that I just kept salting and pulling till nothing else of consequence was left. 4 xylene pulls salted 3 times each.

its a bit more trouble in some ways, but less trouble in other ways, but bubbling HCL gas through the toluene/xylene gives better crystals in almost all cases and precludes multiple salting steps. there are plenty of simple ways to set up a HCl gassing unit. I do it this way now using a little garden store pump sprayer.

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[foaf]

then you only need to do 1 salting to pull 99% of the mesc.

as with any extraction, multiple smaller volumes used to extract have a mathematical advantage over the same volume done once. Its standard practice and can also be related to the practical size of your sep funnel and the desire to keep the total volume of acidic water /mesc-HCL low so that there is less to evaporate.

I only did 3 salts per pull, but did 4 pulls, so the 12 is not really 12 saltings. And you still get a product with the 3rd salt in my experience, so I dont think you get 99% with one salting pass, unless you used a very large relative volume.

 

[cyantific]

the reason my early tek says do it 12 times is that I just kept salting till nothing else of consequence was left. its a bit more trouble in some ways, but less trouble in other ways, but bubbling HCL gas through the toluene/xylene gives better crystals in almost all cases.

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You're tek has been great, thank you foaf!

That hand held gasser is cool! What are the safety precautions needed? Won't the HCL react with the plastic sprayer? What role does the CaCl play?

 

[foaf]

If you do it outside with great ventilation, and this is of course preferred, I personally just wear gloves and a safety face shield. You can smell the HCL gas and it is noxious before it is dangerous, but a filter mask designed for organic solvents (yes HCl gas isnt organic) gets the fumes out if you want to be careful. I dont but perhaps should, I just keep a fan running to prevent any significant concentration from developing.

and CaCl2 forms HCl gas with hydrochloric acid by I think, dehydrating the solution and creating a super saturated HCl water solution that cant hold the HCl anymore. It is described here HCl Gas from conc. HCl(aq) and CaCl2 - [www.rhodium.ws]

good luck, be careful