PH too low on Kash AB mescaline extraction

[Madhattress]

Hi guys,

So i did my first ever AB extraction with HCl. Everything went perfectly until i did the last step with HCl to lower PH. When i added my 1 ml (i did .5 increments) it made my water layer containing the alkaloids far too low. Ph 2.5.


Now i am unsure what to do to rectify this. Do i evaporate the crystals and then readd them to my zylene and redo the acid extraction/H20 with a far lower amount of HCl?

Any suggestions would be helpfull.

 

[Loveall]

I can suggest two options.

1) Continue with the TEK as is. Too low of a pH is not a big issue. You may have pulled extra stuff into the acidic water as more things become soluble in the lower pH. Slightly dirtier product, shouldn't be an issue.

2) Base the 2.5pH water, re-pull with xylene 5x times, and titrate again. This is a bunch more work. Personally I would not do all this extra stuff for the sake of less contaminants. They should be in trace amounts.

Do i evaporate the crystals and then readd them to my zylene and redo the acid extraction/H20 with a far lower amount of HCl?

No, the xtals won't dissolve in xylene. You need to base the mescaline.

 

[doubledog]

I would evaporate it, wash crystals with cold acetone or ipa and then try to recrystalize it from dual solvent system.

 

[Loveall]

I would evaporate it, wash crystals with cold acetone or ipa and then try to recrystalize it from dual solvent system.

I though mainly sulfate was good for dual solvent system (water + acetone). Is there a good system for HCl?

 

[doubledog]

Not sure, someone here on the forum suggested ethanol/acetone iirc. Definitely some experiments should be done to found out which are the suitable solvents and ratios.

 

[Madhattress]

I can suggest two options.

1) Continue with the TEK as is. Too low of a pH is not a big issue. You may have pulled extra stuff into the acidic water as more things become soluble in the lower pH. Slightly dirtier product, shouldn't be an issue.

2) Base the 2.5pH water, re-pull with xylene 5x times, and titrate again. This is a bunch more work. Personally I would not do all this extra stuff for the sake of less contaminants. They should be in trace amounts.

Do i evaporate the crystals and then readd them to my zylene and redo the acid extraction/H20 with a far lower amount of HCl?

No, the xtals won't dissolve in xylene. You need to base the mescaline.

Thanks for the advise. I think ill just skip and do option 1. Is ot normal for the h20 pull to be clear?

Also going to start the cielo tek tomorrow and see how it goes.

 

[Dogwigs]

I did Kash's A/B test from 100g of San Pedro dried powder material. I have a concern, as I yielded 8.5g. According to the lit, San Pedro should only consist of .1 - 2.3% of mescalin with rare extreme cases being 4.7%. So I have about 2x the amount of the maximum rare case scenario. The product I came up with is a light grey sandy material that clumps up easily. It melts into an annoying oily material at just above room temp. If I hold on the the glas to long it melts and is difficult to work with. I washed it 2x with ice cold MEK,and the MEK stayed clear after decanting. (Although my product did look a little closer to white after the washings) I'm concerned that I pulled more than just mescaline from the procedure. Anyone have any idea on what I have here or next steps to produce a more pure result?

 

[doubledog]

It doesn't seem right, you have some impurity there and quite a lot of it. Could you describe in more detail your extraction?

 

[Dogwigs]

It doesn't seem right, you have some impurity there and quite a lot of it. Could you describe in more detail your extraction?

I followed the Kash AB extraction process, used toluene as my solvent. NaCl solution as my base, and HCl as my acid. My HCl was 32%. I wonder if the conditions were too acidic and pulled more than intended.

 

[Dogwigs]

I accidentally got some water in it, so now I have it in the dehydrater, after a few hours im going to do another cold MEK washing. Or maybe acetone.

 

[pete666]

NaCl? You mean NaOH?
When you separated the toluene, are you sure there was not any water with it? How did the toluene look after separation? Was it clear?
When you say you accidentaly got some water in it, where was it from?
What was your final PH after addition of HCl?