Hey aethereon, sorry to see you having problems there. Normally this process, while time consuming, is quite simple. The TAO works but Loveall is right - Sakkedelic's tek is quite considerably more fast and effective due to less of that frustrating filtering.
I am certainly no expert here but I have done this extraction more than a few times. The Manske is one of my favourite parts due to the sheer beauty of those crystals surrounded by that weird fluorescent glow.
Some tips that might be useful:
+Start over and use sakkedelic's tek on a new batch. Keep what you've got because it may make more sense to you later what to do with it. Rue is inexpensive anyway.
+100g is a good chunk. I do about 3-4 batches of 100g at a time, processing one by one, to get a lot more source liquid to work with because settling and filtering takes time.
+Use a strong base at first to put pH of extracted liquor to > 12. No need to be too accurate here, KOH or NaOH is good. Forget about sodium carb. Ammonia is the only other base you will use if you want to go further separate Harmine and Harmaline. Sodium Carbonate is not suitable in this process and hugely messy.
+Sakkedelic's tek mainly differs in the fact that he doesn't spend time filtering the base phase (first phase) - this is smart because when that mud is basic, filtering is a bitch. Even vacuum. You only really want to filter the acid phases. The base stuff you want to dilute liquid with water, settle and decant (I siphon the liquid). Settling I allow overnight at first, it gets quicker the cleaner it all gets.
+Clean your base liquid as much as possible first - you want the precipitate here obviously but I find using a really large bottle (5litre for my amounts) the best here to dilute the brown stuff. You want it as clear as practical without going too overboard. Two dilutions of up to 5l on my 3 x 100g batch acid liquors (from boiling seeds) is a sweet spot for me. The precipitate is nicely and clearly separated. The liquid you want as close to transparent as practical.
+Right now you can filter dry the precipitate and use as "full spectrum" if you want. 300mg of this will do you 6+hours of harmala-land! (prolly a sudden but short purge in the middle somewhere - that stuff is not a friend of stomachs!)
+Dilute & Decant base liquids, Filter acid liquids. Base keep solids, acid keep liquids.
+ If you have the time, filter the base precipitates now and dry and weigh so you know roughly what you got. Then you can work with salt very accurately for Manske and not rely on Phlux's method (see below for conjecture on concentrations)
+Adding acid - once you have precipitate with as little liquid as possible (time...time...) you can acidify with vinegar (or you dried it in step above). Under 5pH is usually low enough, harmalas won't crash out under 5 but other stuffs do! As pointed out above, there is quite a color change (darker) to the liquid when in acid phase. Again use as little acidic liquid as possible - i.e. the alk concentration remains relatively high per volume. Acidified liquids should be very dark red colour.
+Now you can filter this. BEST FILTER WHEN HOT! A couple of times. There seems to always be black stuff left in the filter. Do it until it filters relatively quickly through a coffee filter.
+Phlux's Manske formula is the best one to follow in the TAO imo. Makes sure your saturated solution is really saturated though, and you heat both solutions. I do it in the microwave in bits (else overspill) to get them around ~90°C before mixing the two and leaving to cool.I filter BOTH the salt and the acidified liquids again after heating before combining.
+ Now the result of the manske depends very much on concentrations of alk contents. High concentration - the container fills choc-a-block with crystals. Low concentration and the crystals congregate in finer form at the bottom. But they are definitely crystalline.
+Now you can filter this and continue because you have got to the manske stage and past it (well, the first one anyway) - from hereon in its a matter of how clean do you want things.
+Other: the thread on VDS is well worth a read, long, but interesting and comprehensive. There is a lot of speculation about the relative concentrations of harm alas for the Manske there. But follow Sakkedelic and you should be right in the ballpark. The TAO aswell, but that first part of it is the problem area for me.
+From VDS thread and others ('me' is quote not me!) I clipped and kept:
"* For manske your solution is better to be somewhat concentrated, if the volume is too large, the crystals grow more difficult. Did 1 liter for 100 gr of seeds.
* Amount of salt: I go for 20gr per 100 ml of solution, it is high but it still delivers very long needles, and I have no pesky salt contamination. Phosphoric acid was used at pH 3."
"One of the factors in play is not only salt concentration but alkaloid concentration as well. This last is usually overlooked. "
If you not using Phlux TAO method and want to add salt directly to acidifed (hot) this may help:
"For all harmala-freebases, I use about 6ml of acetic acid 7% per gram. Then some demineralised water to make it practical."
"blue.magic: Yes I did a little experimentation and 20% salt works on crude, but crashes too fine harmalas - but 15% might also do the trick. Since 26% is maximum possible concentration, 17-18% seems sensible tradeoff as suggested (thanks). I would keep the crude harmala concentration below 15 g/L as otherwise there is too much impurity."
"In my experience, using 15% salt or more crashes everything too quickly.
The 3rd and 4th Manske works perfectly with just 7-8% salt.
Jees: I stand by this. "
+From one of my own lab notes: -- 25g/litre HarmalaHCl (10g/400ml dH2O + salt sat sol 400ml)(1g/40ml) - worked nicely - golden floaty crystal clusters "banana-slice" style
+Subsequent Manske's on same material -- no vinegar, just dH2O and the salt solution, with proper (2x at least) filtering of the dissolved HCl though. Always seems to be some more dirt no matter how you filter!
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See some of my posts - there are pictures of various stages and you can clearly see colours. Pictures help me a lot!
Hope this helps