Where is my spice? First 0%yield

[CTZeus]

Hello fellow Nexians,
So I've run a few teks now and I'm still struggling with yield but averaging 1% however on my last run-through I had my first 0% and I'm hoping you guys can tell me where I've lost my spice. So basically I've been doing a hybrid of sorts using bits of earthwalker/max ion/phathfinder and its been working well up until the last run through.
~ 100g ACRB
~ 650ml water
~ Pre-heat 2 hour @ 55c
~ Freeze/Thaw x3
~ 250ml distilled water + 5ml Phosphoric Acid; PH 2
~ Acid Cook Low 55c-65c 8-9 Hours.
~ Salt (90g-800ml)
~ Base (50g-200ml); PH 13
~ Base Cook Low 55-65 - 3 Hours.
~ 8 * 50ml Pulls
~ Mini A/B - 500ml distilled water – 8ml Phosphoric Acid; PH 2
~ Wash & Pull
~ Base 200ml water - 50g lye; PH 12
~ 14 * 60ml pulls from mini A/B.

The only thing I have changed this time is the use of phosphoric acid ala the DMT handbook and I left my soup to cool over night before the first pull – Could that have been the issue?
Could I have accidentally got my pH too low and trapped my spice in the soup?

Could it be trapped in my mini A/B/clean?
(this didn't turn very milky when I based; a tell tail sign for me so far. Did check the pH of this after seeing the results and it was bang on pH 13)

Where would be the best place to start looking for my spice?

I have had a few issues with my bark but have never got 0% yield....

I am about to pull from the soups and no mini a/b to see if I can get it out, but if anybody had any ideas where I've gone wrong or key places I could have trapped my spice it would be great to know

anyway,
hope I hear from you guys soon
CTZ

 

[BongWizard]

What do you mean when you say wash and pull (after your second acid stage)? It looks to me like that's where the goodies are gonna be

 

[CTZeus]

What do you mean when you say wash and pull (after your second acid stage)? It looks to me like that's where the goodies are gonna be

So take the pulls from soup apply to acidic solution take the shellite out of the acidic solution - rebase then pull from there..

 

[Tryptallmine]

A pH of 2 for your acid phase is actually pretty ideal so no you haven't lost spice there.

What did your very first round of solvent pulls (8x) look like when you drew them from your soup? - This is the important bit - well before the cleanup (A/B)

Were they saturated? If they weren't you might as well have stopped right here.

Usually the very first pull will go very cloudy if you've got decent bark. To be honest, I don't ever bother with more than 4 x 50 ml pulls. Most of it is extracted in the first two pulls.

You need to get into the habit of checking your work at various steps of the way through to make sure you are not wasting your time going to the next step. If your mini A/B didn't turn milky then work back from there.

It's either still in your solvent that you've removed from the Mini A/B or it's in your original soup. Then there is the possibility that the starting material you used is of poor quality, which does happen from time to time - we've all been there.

--------------------

1. Do another mini A/B on your naphtha that you removed from the wash - if you still have it. Don't shake the hell out of it, just gently swirl it for a good 10 minutes. Warm the whole solution up in a heat bath - careful of sources of ignition and solvent please.

Re base and pull. If there is nothing there then you can work back again.

2. If you have your original soup? Check the pH make sure its above 12.
Warm it up until the temp reaches 55 Deg C. Agitate it lightly over the period it's warming.

Take it off the heat and do a single 50ml heated pull. If you don't get anything out of there then I would cut your losses.

My overall piece of advice for you is - Use 1 tek that has proven results from start to finish with no deviation rather than mix and matching teks. EarthWalkers tek - which is a spin off of Cyb's is very simple and effective. I can usually complete the whole thing in 6 hours and end up with 2% yields - with good material.

 

[tseuq]

Thank you Tryptallmine for your support with your well explicated posts! In my opinion they are written clearly and rich in detail, what makes them easy to understand and follow. Beside of that, you offer precise recommendations! :thumb_up:

Love tseuq

 

[JustCurious.]

Regarding what tryptallmine said, I don't believe there is a problem mixing teks, as long as you get the pH's etc. correct, there should be no problem in creating your own hybrid tek.

14 pulls ? Is that a typo, beacuse that is a ridiculous volume of solvent to use for just 100 g, especially in a mini A/B where you can usually use less naptha IME. And as trpytallmine said, 8 pulls initially is again way too much, 4 would probably be enough.

Have you evaporated down your 14 pulls ? Because there is a real possibility that there is just too large a volume of solvent for you spice to precipitate...

 

[The Traveler]

I changed the topic of this thread, please use language in a dignified manner.


Kind regards,

The Traveler