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Messed up all 3 extractions, giving up

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Impeccable

Rising Star
My friend was using the glassware that comes with the coffee machine (the glass pot that holds the coffee).

He is using 50g MHRB, 500mL water, 12 tablespoons of lye, and only 25mL naphta (Ronsonal Lighter Fluid).

Problem is, the layer of naphta is very thin since the glass pot is very wide. He has overcome this problem by pouring out the MHRB/NaOH solution into a glass cup, then extracting the seperating the naphta layer from the cup.

So far he has not recovered any thing, could the thin layer of naphta be a problem?

Some notes about his last failed attempt
- more than 20 but less than 50 ml were used for 3 pulls
- they were each mixed once, half hour part
- the pulls began an hour after the NaOH/MHRB solution was made
- the solution was pretty smooth so he thought he had enough lye (he had 9 tablespoons of lye)
- no Turkey Baster was available so the little plumbing thing they have in shampoo bottles was used lol
- fan was used for a complete evap, ended up with some grey dust that turned into goo when attempting to remove

- He basically ended up with nothing, I can see where he could've improved, basically he could have mixed more, used left naphta, plus some other small things but I don't see where the big mistake was. Some deviations would reduce the yield but he pretty much got nothing :cry:


For his next attempt which he is in the middle of
- 12 tablespoons lye, Turkey baster, 25 mL naphta / 3 pulls
- for each pull naphta mixed for 5 mins, (wait 10 min, mix 30 seconds)3x
- he is noticing that his naphta layer appears a bit more clear this time around but still it feels like he is basically doing the same thing again and will get the same result (nothing)
 
Vortex tech, doing a STB

too much lye isn't a problem is it? It heats up the solution at least lol

today my friend will be doing the evap till it starts to get cloudy, he'll then put in a glass cup, put a plastic wrap on top, and in the freezer it goes

this is his 3rd and possibily last attempt, hoping he'll just get SOMETHING out of it
 
I also had some water get mixed in w/ the extracted naphta some how, I don't think this will be a problem will it? I plan on doing s freeze precip anyway.

If it dosen't work this time, then I'll have to through in the towel, I don't see where I could've possibly gone wrong.

basicity check - smooth mixture
right amount of naphta check - above 20 but never got more than 40
stirring/waiting enough check - (5 min initial stir + (10 min wait, 30 second stir)x3)/pull

for now
evap - when cloudy
freeze precip - 12 hrs

I've checked and re-checked every possibile point
 
I also had some water get mixed in w/ the extracted naphta some how, I don't think this will be a problem will it? I plan on doing s freeze precip anyway.
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No, this won't be a problem because water is polar and naptha is non-polar, so technically, no water got mixed in with your extracted naptha, it got dropped into your extracted naptha, whereupon it immediately preceded to sink to the bottom of your container. You are correct, when you free precipitate, you will easily distinguish any ice crystals from spice crystals.

Also, I'm not sure why I'm thinking this, but it sounds like your not mixing your naptha thoroughly enough with your basified rootbark sludge. As long as your pH is high enough, you can completely agitate your naptha/basified solution and not have to worry about emulsions. SWIM agitates his wine jug to the point that there is an emulsion through the entire naptha layer, which then falls out over the next 20 minutes or less.

Finally, you can always use a little excess naptha and evap it down at the end to guarantee you're getting everything in the sludge, but that really doesnt sound like the problem you're having. I'm really getting the sense you need greater agitation, perhaps slightly higher temperatures, are you heating your naptha before doing pulls? I see no mention of that and that could definitely effect your yields. I wouldn't give up just yet, there are definitely some things you can do that would be worth trying at this point.

Feel free to pm me if you want someone to work back and forth with on this.
 
Impeccable said:
so I'm sure now I screwed up, very little naphta left and it's not cloudy at all, I don't get this
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Hi,

You sound a bit impatient. Do not worry!

Just make sure that:

1) you use more naphtha (or lighter fluid)

2) mix well the basified solution, not just stir.

Basically what you need is to add more solvent (e.g. 50ml) and mix well.

Also, getting the solvent out without carrying the basified solution as well is elementary skill. Just give more time for the separation and exercise more caution.

Hope everything turns good.
 
Infundibulum said:
Impeccable said:
Also, getting the solvent out without carrying the basified solution as well is elementary skill. Just give more time for the separation and exercise more caution.
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for the record, the water that got in with naphta was tap water, nothing from the solvent, this being my 3rd time, I've gotten pretty good at it, no visibile speck of lye made it through

so you guys really think heating the naphta + mixing so much as to create an emulsion (before I tried to mix gently so I wouldn't get an emulsion) will make all the difference?

I kept my naphta volume extra low so it would be more likely to get something and I mixed it gently but over a long period of time.

The result this time is worse than the 2nd, where I left around 50mL of naphta over night but I also remember mixing that one more vigorously so maybe there really is something to it.

If that's the case, it would seem like a gentle stir dosen't cut it, you have to mix like crazy to make this work.
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Shake the hell out of it you want the naptha to go through as much of the solution as possbible. Also what is the weight of 12 tablespoons of lye.What you need to do is 1.add 50grams of lye to 750ml of water mix thoroughly.
2.add 50grams bark(powdered) mix thoroughly
3.add 100ml of naptha
4.separate the naptha.
5.Evap halfway
6. put naptha in freezer and you should have something.

hope this helps
 
Impeccable said:
Infundibulum said:
Impeccable said:
Also, getting the solvent out without carrying the basified solution as well is elementary skill. Just give more time for the separation and exercise more caution.
Click to expand...

for the record, the water that got in with naphta was tap water, nothing from the solvent, this being my 3rd time, I've gotten pretty good at it, no visibile speck of lye made it through
Click to expand...
But naphtha is the solvent! Or you mean that you didn't get the solvent out of the basified solution:p ?
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