Flakes in Saturated Solution

[Trickster]

SWIM is trying to extract harmaloids from rue. Here is what she did so far:

1. Combined 50 g of finely ground seeds with 3% white vinegar.
2. Stirred the solution for 2 hours with magnetic stirrer/heater.
3. Filtered the solids with an old t-shirt.
4. Repeated steps 1-3.
5. Combined liquids from 2 acid extractions (~220 ml).
6. Added NaCl while stirring vigorously and watching for precipitation to begin. It never did. The liquid color was just changing from light brown to light yellow and it was getting thicker.

After adding what seemed as awful lot of salt (30-40 g per 100 ml) she decided that the process is going nowhere. SWIM added more water (~230 ml). The liquid immediately separated into a darker and lighter layer. That looked encouradging but then SWIM thought that maybe the solution was not fully saturated, so she started adding more salt. There was no precipitation until more than 40 g of salt per 100 ml of liquid was added to the solution. Only then SWIM noticed that salt no longer dissolves. She expected to see some brown crystals but there were none, just salt. She decided that there is no point in addining more salt and left the solution to sit in a fridge.

In an hour she examined the solution and noticed that there was some precipitate at the bottom. The color was light tan instead of brown as expected. Also the liquid looks very strange. There is a thin layer of transparent liquid at the top of the glass. The rest of the liquid is full of light yellow flakes floating around. These flakes dissolve into the surrounding liquid if even very lightly agitated. At the bottom there is a thin layer of crystals that look exactly like salt.

SWIM had said that she would appreciate any comments.

 

[Trickster]

Progress report from SWIM

After another hour in the fridge the glass content separated into 3 layers

1. Almost transparent liquid (1/2 of the glass)
2. Lighter color opaque layer of large flakes (1/2 of the glass)
3. Thin layer of light tan solids.

Is this normal?

 

[acolon_5]

My guess is that the flakes are harmala alkaloids AND some salt contamination..this is normal.

After adding salt you need to stick it in the fridge overnight, thus reducing the amount of harmala alklaoids the salt water can hold, crashing out more of the alkaloids.


You can filter out what you have and then stick it in the fridge for 20+hours. There should be a lot more flakes/particles when you pull it out of the fridge.

After you have collected your alkaloids via filtration, I highly suggest drying it out completely, adding a FEW DROPs of vinegar and a SMALL amount of warm (not hot) water (100mL-200mL), stir/shake until almost everything dissolves. Filter again and toss the filtered material, there should not be much at all leftover. Add dropwise ammonia or a strong solution of sodium carbonate. Your brown liquid will turn a mustard color, filter this with the finest filter paper you have and ta-da, salt free freebase alkaloids.

 

[Trickster]

Thanks acolon,

My guess is that the flakes are harmala alkaloids AND some salt contamination..this is normal.

After adding salt you need to stick it in the fridge overnight, thus reducing the amount of harmala alklaoids the salt water can hold, crashing out more of the alkaloids.


You can filter out what you have and then stick it in the fridge for 20+hours. There should be a lot more flakes/particles when you pull it out of the fridge.

SWIM's always wondered why bother filtering precipitates? Why not just decant them and dry with a fan or hair dryer?

After you have collected your alkaloids via filtration, I highly suggest drying it out completely, adding a FEW DROPs of vinegar and a SMALL amount of warm (not hot) water (100mL-200mL), stir/shake until almost everything dissolves. Filter again and toss the filtered material, there should not be much at all leftover. Add dropwise ammonia or a strong solution of sodium carbonate. Your brown liquid will turn a mustard color, filter this with the finest filter paper you have and ta-da, salt free freebase alkaloids.

Are you saying that freebase alkaloids will precipitate as solids?

 

[endlessness]

yes, freebase precipitates as solids and WAY cleaner than the harmala salts from a manske.. specially if you repeat the whole process a couple of times

 

[Trickster]

yes, freebase precipitates as solids and WAY cleaner than the harmala salts from a manske.. specially if you repeat the whole process a couple of times

What is the point repeating it 2 more times?

Even crude manske tek worked fine for SWIM. Will there be any noticeable difference? Some people eat the seeds raw with little ill effect.

The question that bothers SWIM is - to filter the solids or just decant after a day in a fridge. SWIM's got a filter flask and a buchner funnel but no vacuum pump.

As with anything, in the process of cleaning there is a law of diminishing return.

 

[Trickster]

After 12 hours in the fridge SWIM's got her liquids separated in 2 nearly equal layers. She decanted carefully the 1st transparent layer and discarded it. SWIM's ended up with ~200 ml of thick yellow liquid which she suspects would be hell to filter. She will if there is not an easier way. But could she possibly reduce it with heat and fan until it's completely solid? Later she may proceed to freebasing the harmaloids.

 

[endlessness]

dont filter

just redissolve it in fresh warm water, filter the water many times with progressively finer filter (starting with, say, cotton funnel, last being coffee filter or two depending on how fast its filtering..) I usually try to filter as much as possible when its redissolved because only impurities will be eliminated, so the more the better..

and THEN add sodium carbonate to precipitate the crude freebase harmalas

If you want you can clean that up, redissolve in warm acidified water again, filter again, base again (or salt again, redissolve again, filter again, base again)..

Im sure you got the idea, the more runs the cleaner it gets.. Avoid filtering if possible, until the very last step, which you will have to filter with coffee filter

 

[Trickster]

dont filter

just redissolve it in fresh warm water, filter the water many times with progressively finer filter (starting with, say, cotton funnel, last being coffee filter or two depending on how fast its filtering..) I usually try to filter as much as possible when its redissolved because only impurities will be eliminated, so the more the better..

SWIM redissolved the extract and did a lot of filtering.

and THEN add sodium carbonate to precipitate the crude freebase harmalas

SWIM baked sodium bicarb for 2,5 hours and added supposedly what should be sodium carb straight to the filtered solution. The expected color change occured and SWIM kept adding sodium carb until changes stopped. Around 5 teaspoons were added to ~500 ml of solution.

She stirred the solution for a while with magnetic stirrer. When she stopped the liquid became cloudy and large flakes appeared. SWIM put the jar in a fridge and in 30 min. she noticed that there is a lot of precipitate, but its color is not brown but VERY light yellow - almost white. Also there are no crystals just very fine dust particles.

SWIM is worried that something went wrong.

 

[endlessness]

sounds good.. harmalas freebase like this dont tend to form large crystals, they do get small crystals, but should be big enough to stay on top of the coffee filter

sounds like you are going right.. Just leave on the fridge for some hours at least and then filter.. or if it settles nicely on the bottom and not floating around anymore, then just decant and then filter only the last bit

 

[Trickster]

sounds good.. harmalas freebase like this dont tend to form large crystals, they do get small crystals, but should be big enough to stay on top of the coffee filter

sounds like you are going right.. Just leave on the fridge for some hours at least and then filter.. or if it settles nicely on the bottom and not floating around anymore, then just decant and then filter only the last bit

SWIM did as you said and voila - 2.4 g of nice light brown goodies (yield is 4.8%).

Actually she did not filter all the liquid left after decanting. Once the filter clogged SWIM just collected the wet goo in a wide glass dish. She suspected that a lot of precipitate was passing through the filter. This was confirmed by 2nd and 3rd filtering of the liquid that came through the filter. Wet goo was evapped with a hairdryer. Filter paper was dried and scraped.

Thanks a lot everybody.