extraction problem

[mrfi]

hi folx, been working on an a/b extraction and when reducing the combined acid cooks i may over reduced. The liquid was deep red and thickish. The problem though was tryng to basify. ph starting point was 3.8 . Then after adding lye and getting to about ph.8 it seemed to lock up there and even started dropping with the more hydroxide i added. Ended up adding about 400 grams with the ph still hanging around 7. Its been doing my head in. So i added some water to see what would happen and the ph rose a bit. Started with about 500mls originally of reduced liquid and added 1500 mls of water to it to get the ph to about 9. By this stage the container was full so i poured about 500mls to a new bottle and had to add about 1500 mls of water to this for the ph to rise to about 12.5. Could any of you lab type folx out there please explain whats going on here and is this project fixable because going on these ratios im going to end having to do solvent pulls from many litres which is undesirable?

Thanx in advance.

ps. sorry if this the wrong spot for post but its the only place i can yet.

 

[mrfi]

hi again, thinking about itand after reading a few more teks, im thinking the problem maybe that with the over reduction there is not enough water to allow either the hydroxide to react fully(although it had all disolved) or that it may have been to thick for my digital ph meter to work properly? One of the ratios ive read was 100gms lye too a 1500ml reduction achieving the required ph of 13, whereas i added 4 times that to only 500mls. Obviously way too much base.

My question now is has this over basing killed the alks or is it possible to combine the mess ive made , re acidify to ph 4 with vinegar, boil back down to 1500mls . then base and pull?

The over based liquid has been sitting for about 20 hours, please help.

thanks again in advance

 

[jimmy4fingers]

I haven't encountered your predicament before but if I was in your shoes I would take that extra concentrated liquid, add a tiny bit of water so its not too syrupy, then do a test pull from a small portion of this batch and see if crystals drop out at room temp.

If the basified solution is black then thats a good indicator. Good luck.

 

[mrfi]

hey mate, cheers for the response. So you think that theres obviously enough base regardless of what the ph reading is . The soup is very black. The origonal portion was 500mls to which i added 1500 mls to only gain only a slight jump in ph.

 

[jimmy4fingers]

hey mate, cheers for the response. So you think that theres obviously enough base regardless of what the ph reading is . The soup is very black. The origonal portion was 500mls to which i added 1500 mls to only gain only a slight jump in ph.

How many grams of bark did you start out with? Perhaps you could reduce it a bit as pulling from 2000ml would be a pain. Or just do a test pull and see what happen.

 

[mrfi]

yeah, that's the whole issue. In order to pull the alps you need a ph of 13 right,? Well atm in order to get 13 it seems I have to copious amounts of water. I think that due to way to much base the hydroxide is not reacting till there is enough h2o. could anyone verify this? Started with about 7502 Gms of bark and phylode material , did 5x 3litre water/vinegar boils which accidentally got reduced to 500mls. Due to the very thick vicinity of the liquid I think has caused the ratifying problem(once again, can anyone varify???).
Thanks again for the help.

 

[mrfi]

750 gms. Stupid text complete lol.

 

[mrfi]

vicinity=viscosity
ratifiying=basifying

 

[jimmy4fingers]

I've read that anything over PH8 would work, but ideally higher the better. Your best bet is to do a mini test pull and don't bother adding anymore vineger/lye in there lol.

 

[mrfi]

Been posting from my baby screened NE71 , post window only allows me to see 1 word at a time, sorry. Think ill wait till girlfriend gets back with tablet before reposting heh. Ok will do a test pull today and keep you posted. Cheers again for the help, appreciate it.

 

[mrfi]

On that note though, I've read on this forum somewhere that it must be over ph12 anything less will just produce slime? I will reference this for you when I get the tablet back.

 

[mrfi]

Oh and just for reference the color changes went from golden/red from the boils to dark red on reduction to stinky black after adding all that base.

 

[mrfi]

Ok got the tablet back now. A thought on your suggestion about reducing the 2000mls for workability, i think spice vaporizes at a much lower temp than the boiling temp of water and assuming (not sure due to ph problem) the alks have moved into there freebase form i would be losing the goods to the atmosphere. Thats why i was thinking of the re-acidifying path. Any thoughts?