What went wrong in my Harmala extraction from P. Harmala? First time excellent, second time poor.

[La Alquimista]

Two extractions of Harmaline / Harmala HCl from P. Harmala were performed. The first used the Tao of Rue Extraction on 100g seeds and yield is fine amber crystals of first picture. These crystals were recovered from filtration after 5th Manske and washed with room temperature saturated aq. NaCl.

Second extraction also used Tao of Rue Extraction but start with the 250g seeds from same bag, with additional filtration (much was learned of the importance of repeated filtration after completing the first extraction). During second Manske the vessel overheated and cracked resulting in all fluid containing the product dropped into sand bath. Sand was washed 10x with hot water and 1.5L aqueous solution was recovered then reduced to 200mL. Manske was then repeated 3x to recover final results in picture 2. Much larger amber crystals and large chunks of fine cubic milky white and fine cubic dark brown crystals are obtained. The large amber crystals suggest higher purity as a result of more filtration however the two additional components are of concern. Second picture shows this result.

It is suspected the milky white regions could be NaCl and perhaps due to recovery from the sand some NaCl ended up in the final product. It is unknown why the dark brown crystals are present.

Are there any thoughts on what has gone wrong? What could these other parts be and what could be done to recover a pure product?

 

[La Alquimista]

A look was taken at the procedure followed in each process. In the first, manske was performed with 10g NaCl per 100mL water. In second, 25g NaCl per 100mL following a video found online. Read the Tao of Rue again and determined the translucent white portions are probably salt contamination from this change. This does not explain the dark portions.

An attempt is being made to recover pure crystals. Contaminated crystals are dissolved in hot water in a tall glass. This is filtered through a coffee filter and minimal dark specks are observed on the filter paper. Fluid is replaced in tall glass and pH is adjusted to 9.8 to precipitate freebase alkaloids. They will be left overnight to settle. At completion the alkaloids will be collected on filter paper then manske performed with lower NaCl concentration. Results will be reported.

 

[La Alquimista]

The freebase alkaloids were dissolved in minimal acetic acid (5%) and heated a little. 10g salt per 100mL solution was added. Crystals started crashing out. Heat was increased until the vessel was hot and all crystals dissolved, then heat reduced slowly over several hours. No crystals were observed until the next day. The bottom of the vessel had a lot of solid dark contamination. As many clean crystals as possible were removed and the picture in the post shows the result.

The rest of the sludge and crystals were removed from the vessel and as much sludge removed as possible.

The result was a different color than the first extraction shown in the first post and it smelled faintly of vinegar so another manske is being performed, separately on the pure and slightly contaminated results. In both cases this time not everything dissolved in hot water so whatever did not dissolve was filtered out.

It looks like there are red spots of some type of fluid at the top of the vessels this time, some contaminant seems to remain, if this remains as a fluid it may be removed when filtering the product. The result will be reported.

In conclusion La Alquimista has determined their faults in this extraction compared to the first time they did this.

Too much salt was used in the second extraction compared to the first. 25g salt per 100mL fluid. The salt contamination in the product came from this. La Alquimista is using less salt now. The crystals grow much smaller but this does not matter and there is no more salt contamination.

The vessels were not heated enough. Instead of pyrex La Alquimista used mason jars in the second extraction and these did not withstand heat. The mason jar broke the first time and the fluid was recovered from the sand bath which may explain the other contaminants. La Alquimista is using pyrex again.

 

[La Alquimista]

The image was not attached to the post so they have attached it here.

 

[downwardsfromzero]

The image was not attached to the post so they have attached it here.

It's still not attached! Are you using the right file extension, e.g. *.jpg rather than *.jpeg - the latter of which is not recognized by the uploader (Trav...)?

 

[Jagube]

The image attached has the .jpg extension, but apparently it's not a correct jpg file, i.e. either it's corrupt or a different format altogether.

 

[La Alquimista]

They're trying again, they don't know what happened. This is fine, they have another picture to share now. To summarize the contaminated product in the first post was dissolved in water, filtered, then brought to pH 9.8 to precipitate freebase alkaloids. The freebase was dissolved in minimal acetic acid and filtered again, then manske performed. This is where the last update left off, contaminants remained which La Alquimista calls sludge. Most of the crystals were removed in one coffee filter which is the pure large product. The sludge and remaining crystals were removed in second coffee filter which is the less pure small product.

Then each product was re-mansked separately. They were dissolved in minimal hot water and filtered through a stack of three coffee filters, grainy looking contaminants were removed. The next manske was performed. These pictures show the products. The large product is a beige white color. There were still The small product looks tan. La Alquimista has done more reading and believes the white product is pure and the tan color is some harmless impurity.

 

[La Alquimista]

They don't know what is going on, these photos are from the same camera used to take the original photos. They have been converted to png images now, maybe this will work. This is weird, this works but the jpg did not. As long as it works. The first picture is the large pure product. The light makes it look darker than it is. The color is actually closer to wheat color.