How much HCL saturated Acetone to salt directly out of xylene?

[dumbstruck]

I hate to ask for these fairly simple little questions that I ought to be able to figure out, but alas, I am stuck with a wide potential range of values.

I have 2400 ml of dried Xylene -- a total of four pulls done on 250 grams of strong San Pedro powder. I plan to add about 150 ml of dried, HCL saturated acetone to the lot of it to crash out Mesc HCl; how much 33% HCL acid solution should I use? The best number I came up with was 8.33 ml of 33% muriatic acid to be sufficient, but this seems like way way way too much. I unfortunately have no pH papers presently. Can anyone help clear this up for me?

edit: Further number crunching has me thinking the other end of my wide range of values is correct. I am going to use 1 ml of 33% muriatic acid hopefully in total. I will prepare 300 ml of acetone with 2 ml of 33% HCL, dry it, and plan to only use 150 ml. I'll separate the solvent from the crystals and add some more HCL laden acetone to see if anything else precipitates. If anyone knows more clearly how much I should use I would still like your input.

 

[dumbstruck]

edit: Erp. Ignore below. Precipitate took a while to form, I suppose. Narmz mentioned the fumarate takes a little while to drop out of d-limonene, so perhaps the same is true for HCL out of xylene. There is some beautifully sparkling white, very fine crystals covering the bottom of the jar. I'm sure they will come out stained and a wee bit smelly, but I'm sure they will clean up just fine! Perhaps I'll report back with yields.

Added 50 ml of HCL saturated acetone into the weakest of three 800 ml xylene pulls. There was the equivalent of 1/3rd of a mL of 33% HCL acid solution in the 50 mL of saturated acetone. No precipitate resulted.

Did I use too little HCL? I figured maybe the epsom salts pulled it out of solution or something but I can still see it swirling around in there like heat in the distance. Surely that was enough for something to precipitate. I suppose there is a possibility the acetone didn't dry properly. In which case there would be something like 2.5 mL of water in the acetone (holds about 5% at stable, I think, so 5% of 50 mL). That would only explain the loss of some of the precipitate, though I have no idea how much mesc hcl is soluble in water.

What does that mean? I'm going to try some vinegar pulls on them or something I guess. I don't see how nothing could precipitate. D'oh. The jar was 3/4ths the fourth pull and a wee bit poured in from the third pull, so there definitely shouldn't have been much mescaline in there, but there should have been something! :?:

Anybody have any insights?

 

[narmz]

Did you keep the xylene warm while doing this? The only time this whole deal worked out for SWIM was when he kept the NP in a boiling water bath to keep the temps up and drive off excess water. Also, have to make sure everything is completely dry, so give it some time and quite a few shakings under anhydrous magnesium sulfate.

 

[dumbstruck]

Intiguing! I did not keep the xylene warm, in fact it was quite chilly (50-60F?) when I added HCL saturated acetone. I did however overdry my HCL acetone and xylene to be safe, so I don't imagine there is any water in either of them. Sealed them away from air immediately after mixing, so shouldn't be particularly wet. There are significantly more crystals in all three jars this morning as opposed to last night, so I suppose I will let them crash out for a couple days before removing and washing.

How does a boiling water bath drive off excess water? Does that just make the epsom salts more ravenous or something? Surely warm or cool xylene /acetone doesn't effect how long it takes to suck up moisture from the air again in a significant manner? If anything I would think warm xylene would collect water faster than cooler xylene. Would placing my salting xylene jars in a hot water bath now help anything?