Harmala Extraction - Final Steps - Nexus Apprentice Help

[mutizen]

Salute,

Swim just tried his first Harmala extraction based on the wonderful information provided by endlessnesss "Harmalas Extraction and Separation Guide" and Phlux-s "Swims Peganum Harmala Extraction" thread.

Swim was hopeful to get his end product today, but somehow the results do not look quite like he imagined and he is not sure what to do next to not ruin all the days of effort already put into it.

Thus Swim hopes some of the powerful wizards dwelling here (e.g. endlessness, Phlux-, kemist, SyZyGyPSy, burnt, ...) might recognize his devotion to mastering the powerful arts of this magical spell and enlighten Swim about ways of completing it without dreadful backfire.



Swim did take 50g of Syrian Rue, boiled in vinegar H2O 6x (Step A from Separation Guide), reduced (Step B), saturated (Step C) and redissolved (Step D) 3x.

Swim did not dry the filtered precipitates from the salt saturated teas completely, he just let most of the water evaporate at 40 grade Celsius in an oven then redissolved them in hot vinegar H2O, saturated with salt and let it rest in a fridge overnight.

After 3 salt precipitations Swim decided the outcome is pure enough and he would like to finish with a freebasing precipitation. Thus Swim redissolved the precipitate without vinegar this time and slowly added Sodium Carbonate while stirring. With little acetic acid left there was only very little foaming.

Swim had difficulties determining how much Sodium Carbonate to add as adding more always, at least subtly, changed the color (Perhaps Swim is a bit oversensitive). But as he read in Phlux-s thread that it is better to add more than less and adding too much should not be a big issue later, he possibly added rather more than necessary.

Swim is neither sure about how much water would be best to use in every phase to not slow down the dissolving nor hinder/limit extraction but yet not waste way too much water, salt and soda. And he could not find some approximation anywhere of how much Sodium Carbonate to add per liter water either, so that he would not have to rely only on color changes but would have a way to crudely limit -- to prevent adding way more or less than 'reasonable' amounts of it.

After more than 12 hours in the fridge, the basified tea was full of crystals, but much more crystals than Swim expected. :shock:

Swims filtering yielded 3 pretty large piles of slightly different crystals - according to their taste and smell they contain pretty much Sodium Carbonate still and while they dry (and their temp rises from near zero Celsius to room temp) white powder emerges on top of them - probably excess Sodium Carbonate separating?

Swim will attach some photos of the piles taken with his iPhone (not the best quality, but should serve the purpose) ASAP (The plates holding the piles have all 18cm in diameter). The piles were not completely dry yet, thus H2O was slightly contributing to their weight:

• The 148g pile of large brown crystals did get caught in the coffee filter.
• The 62g pile of white crystals precipitated to the bottom of the destination pot in the fluid that passed the filter (filtering was done at near zero Celsius temperatures).
• The 374g pile of lighter brown crystals was left at the bottom of the originating pot after pouring the fluid into the filter.

Now Swim is not sure what to do next. There is way too much material than expected and it doesn't look very healthy to consume in any way in this state -- Swim is concerned about poisoning himself and does not quite understand why and how he got so much material. Sodium Carbonate in H2O on its own doesn't form crystals when put in the fridge. Is it possible that some other unwanted chemicals are involved?



As Swim had difficulties getting some of the Materials in ideal form, he had to make some compromises. Swim was hoping they would just slightly affect the quality and quantity of the yield, but not make it poisonous or impotent:

Swim was unable to get food grade distilled water and was not sure whether distilled water for chemical and automotive purposes would not contain potentially poisonous impurities unsuitable for this spell. Therefore Swim used normal tap water, letting it rest in a pot for at least an hour hoping that most of the Chloride would evaporate at least. Swim considered bottled water, but all locally available brands either contained no info about Chloride or had even more Chloride added than tap water in Swims cave (which should not have much, water near Swims Cave is considered to have way beyond average quality).

Swim also tried to get non iodated salt but there is some ridiculous law in his kingdom making iodation of food grade salts mandatory. Swim considered non-iodated salt imported from the Himalayas sold for 8 USD per 1 kg overkill for his purposes, so he used NaCl with 15-35 mg/kg KI (Potassium Iodide) and max 20mg/kg E535.

Sodium Carbonate was also problematic for Swim to get. Swim found 2 products from the same vendor labeled as "Pulverized Calcinated Soda" and "Crystalic Soda" (a bit cheaper). He got both, not sure which would be better suited for this spell.

Crystalized Soda Content: DECAHYDRATE of Sodium Carbonate (Na2CO3, EC 207-838-8 )
Pulverized Calcinated Soda Content: Sodium Carbonate (Na2CO3, EC 207-838-8 )

Intended usages of both products:

• Softening H2O
• Washing Clothes
• Efficiency increase of Washing Powder
• Suitable for Automatic Wash Machines
• Suitable for modifying PH in Swimming Pools
• Suitable for flushing Beer Tubes (only listed on the Crystalized Soda)

Swim was not sure which one to use, he used the Pulverized Soda in the end, hoping the quality is at least the same as that of the cheaper Crystallized soda claimed to be suitable for flushing Beer Tubes and therefore probably safe enough to use in this extraction?!


O mighty Wizards of Inter-Spice, please help lil' Swim reduce his confusion and tame his first spell so that it wont tame him and his magic skills might grow! :?


Sincerest Regards,

from a Humble Nexus Apprentice

 

[Crystalito]

Hmmm let it dry and try a bit its taste to evaluate what you have there : if its salty, well its lots of NaCl also for example. It should be bitter. I find it highly inpropable poisoning yourself by trying a little bit.

How much vinegar did you use? Personally as a base i use ammonia (heh,people do not like ammonia around here), but this way i am sure i have no base in the product, its evaporates off. If i get hysterical over what impurities ammonia could have in, i wash my freebase with water and there you go!


If you started with 50 grams and you mention such numbers then i bet you have lots of salt in there. Also, weight for them to dry, or else knowing how much of this is water is pure guesswork. Could you elaborate a bit more on the "saturated (Step C) and redissolved (Step D) 3x." how did you do it exactly? How did you judge it was saturated (at what temperature really?). Did you utilise fridge?

Also ,what volumes or liquid were you working with more or less?

Good thing is ,that if what we are seeing is NaCl (which propably is) ,it can be removed from the product.

 

[endlessness]

wow thats really amazing that you start with 50g rue and end up with over 500g of something

you didnt mention how much salt you used, and neither how much sodium carbonate... Did you add half a kg of either of them? Its just sooo much impurities that you must somehow have an idea what it can be, no?

how does the quantity compare of the salt precipitated stuff and all of this that precipitated with sodium carbonate addition?


Also, for example , you say sodium carbonate doesnt form crystals in water in the fridge, so you suppose that is not the contamination.. but, if a solution is saturated, whatever more sodium carbonate you add will simply remain undissolved so will be as a contaminant.. so that is a possibility


I dont know theres much we can ask you.. so lets see what you say first..

but anyways what I would personally do, I guess, since I wouldnt consume that, is try to redissolve this in lightly acidic water, filter, and try to precipitate again with sodium carbonate.. I wonder how much water youre gonna need to redissolve this all, though..

 

[mutizen]

Swim salutes the mighty wizards of Nexus and thanks them very much for their much appreciated feedback. :d


Swim is doing this the first time and he could not find approximate quantities of Sodium Carbonate to use per liter nor any recommended amounts of H2O to use anywhere. He also has difficulties determining what would be the best temperatures and times for each of the reactions beyond what he could learn from endlessnesss guide and Phlux-s thread. Could the mighty wizards please enlighten Swim him on these matters?

Swim in his ignorance did use approximately 1 - 1,5 liter of H2O in every phase. What would be an near ideal amount to use for say 50g of rue?

To saturate Swim used quite a lot of NaCl to make sure he is not wasting any magic - he added circa 200g per liter (the upper limit recommended in endlessnesss "Harmalas Extraction and Separation Guide" ). He put the gunk into simmering water, added the salt, added vinegar (quite a lot as it does evaporate and Swims cave water is rather basic), let it simmer for 10 minutes, then let it cool down a bit, then put it into a fridge overnight. Thus the saturating temp was close to 100 grade celsius. (BTW: Would speeding up the cooling of the simmered fluid in a near zero degrees Celsius environment harm the product?)

After 3 salt washes though, as Swim already mentioned, he did not put anymore salt nor vinegar into the fluid he dissolved the gunk in (AFASK: Adding acids at this point would be contra-productive, right?). The gunk looked as expected, Swim did not dry completely nor weight it but the amount was reasonable, just a few grams he would guess. And it was quite potent as Swim learned while sacrificing 1/8 of the sacred gunk during his weekly HBWR spirit worshiping sabbath.

Swim then just slowly added Sodium Carbonate (The Pulverized Calcinated Soda mentioned) until he thought it should be rather enough. The quantity added was 300-400g into circa 1 liter of water. (Swim did read somewhere that circa 455g of Sodium Carbonate is needed to saturate 1 liter of water, he was not sure whether nearly saturating the fluid was a good idea and what difference the type of pulverized Soda makes in terms of weight).

Then he put it into the fridge and those large crystals formed overnight.

What Swim meant is - only the Soda alone dissolved in H2O and put into the fridge doesn't yield any crystals, therefore something else must be involved in their formation as well. Though Swim surely does realize that Soda is the main constituent of the crystals for sure.

The taste of the product does confirm this hypothesis:

• it doesn't taste salty (no salt was added and and little left in the gunk)
• doesn't taste sour (no vinegar was added)
• it does taste and smell much like the soda used though and white dust emerges on top of the material which Swim suspects to be Na2CO3
• it does taste bitter, especially the brownish crystals

Thus Swim will now make it dry and meanwhile he hopes for much appreciated feedback on what the recommended next steps would be.

BTW: What would be the best way speed up the drying process at this stage? Would putting the crystals into an electric oven or hot-air oven at some rather low temperature hurt the magic?


Can someone with insight please enlighten Swim what difference the materials he used can make? Are they safe to use? Do they lower the yield or decrease its quality considerably?

1. Tap water with some NaClO2 and Ca. Can letting it rest in a pot for some time help get rid of NaClO2 and Ca? Would boiling it first help? Would be distilled water intended for chemical reactions and automotive use safe enough to use and considerably better than Swims tap water to be worth the additional cost?
   
2. NaCl with 15-35 mg/kg KI (Potassium Iodide) and max 20mg/kg E535. Can the amounts of KI and E535 cause some problems?
   
3. Is the soda he used safe? Would the Crystallized soda work better than the Pulverized and Calcinated Decahydrate one? Does Decahydrate make some difference? If its suitable for swimming pools and washing of beer tubes, should it be safe to use for this spell? The cover says one should seek medical help when ingesting it -- is this related solely to the PH of concentrated Sodium Carbonate or might the Soda contain other potentially toxic impurities? Should Swim rather invest more time, money and electricity into food grade Sodium Bicarbonate and turn it into Carbonate in a Oven?

Is Swim right in the assumption that putting the crystals into H2O and slowly adding acetic acid (vinegar) wont hurt or decrease the magic? What would be the byproducts of the soda and vinegar reaction, would they be separable through another salt saturating and filtering step?

Swim is a bit confused and concerned about doing the freebasing step. Swim did read that in the soda freebase precipitation some amount of magic gets lost, thus he would like to minimize freebasing. Should he aim for the salt precipitate gunk or the freebasing precipitate crystals as the final product? Which would be better? Is there a relatively safe way to do the freebasing for unexperienced Swim without risking adding not enough soda and thus loosing magic, or adding too much and getting a huge pile of soda again? What temperature should the fluid have when adding the Soda, should Swim put it into the fridge then and for how long?


P.S.: Swim is not afraid of learning to use more powerful magic (Ammonia, Ethanol, etc.) if it could help yield a better product. Though Swim does not have any and does not know where to safely get it and cost might be an significant issue as well.

Sincerest Regards,

from a Humble Nexus Apprentice

 

[Crystalito]

I like wordy people, they tend to explain what goes on and being one of them i tend to sympathise Now things are clearer.

From what you say ,your troubles started from the basification precipitation stage.Before we go into that lets see a bit the previous steps. Personally i tend to work with liberal amounts of water when extracting ,given that i have the option to reduce them.The water of my choice is distilled water simply because i cannot know what salts are in my tap water, how "hard" and basic it is. With distilled water a) i get more reproducible results b) when it evaporates it evaporates clean. As far as acids go, you dont need to add lots of vinegar: by the way how much vinegar are we speaking about? I usually try to get the cleanest vinegar possible and add about two shots worth per liter of extraction.Recently i have turned to using dilute HCl aqueous solutions (muriatic acid) to have my salts in HCl form in the first place.As for salt addition,yes you can be liberal, personally i add about 35 grams of salt per 100 ml, which would make it akin to 350 per liter but here many might disagree. A rule of thumb is to heat up your concentrate in a glass jas using "waterbath procedures" and add salt with vigorous stirring.When you see it starts taking a bit to dissolve ,go easy on it by adding small quantities until some of it does not dissolve. Another method here which i have followed to success is to let your concentrate evaporate to a paste (or to a very very small volume) and have preprepared a saturated NaCl solution in water.I use the preprepared solution to reconstitute the resin and in the fridge it goes. A propable advantage of this is that for example i prepare my solution not caring much if i add an excess of salt, and then i subject it to 0 degrees celcius.Salt will precipitate but what does not will be saturate with salt ,so by using this i know that i will have no or minimal salt precipitation when i reconstitute the resin and put it to 0 degrees.

Should i also propose a buchner filtration set up with a tap aspirator? It can make life easier, along with decanting, because it can also DRY your precipitate if you leave it running for a bit:it can help ! Filtering becomes way easier, and it tends to draw solvent out of your precipitateso it will not be as contaminated with whatever was in solution compared to leaving the quite soggy precipitate to dry in air.

On the sodium carbonate part i am afraid i cannot help you alot ,be be sure that here there are many masters of this artform that have more than enough knowledge on such procedures and i believe will chime in.You can also make your own sodium carbonate (so as to be sure what it is) by baking sodium bicarbonate (cooking soda) in the oven.Personally what i do , is take my dried "Manske" extract and shake it in a small amount of pharmaceutical grade ammonia.Not much is needed i do it sometimes in a shotglass or an equivalent tube.Then i let it sit in the fridge overnight , filter, collect precipitate and dry thoroughly.I have not tried carbonate because i have the fear that i might run into the same problems you run in : i tend to prefer a base that will evaporate off.

If your main contaminant is the soda, you can try adding small amounts of water, shaking and putting it in the fridge.The soda will dissolve in water making it basic, and the harmalas will precipitate. Repeat till you start having a product more aking to harmala and less akin to soda.

 

[mutizen]

Swim thanks Crystalito for his kind words. Swim has to admit he has some slight professional deformations (bordering on Aspergers Syndrome actually) including an oversensitive eye for detail, enjoyment of pragmatic perfectionism and above average maximum speeds of linguistic artifact emission and absorption (he is used to read/write fast in many natural and artificial languages). Has to do with him spending most of his time working on distributed software systems at a Ph.D. level, writing university lessons for other Swims and taking science, art and health seriously.

Swim is happy and surprised to find a forum where constructive wordiness (i.e. not just some narcissistic self-serving reduction of the signal-to-noise ratio of relevant information) is appreciated rather than just scaring off potential readers. Swim could have included more detail in the first post already, but as he was studying and following endlessnesss guide and Phlux-s thread closely, he did not want to risk scaring potential readers off with sheer quantity of possibly redundant information and felt that the steps before the freebasing went reasonably well and according to recommendations.


Swim does acknowledge the benefits of distilled water, but as he does not own any purification system and currently does not know where he could get it in food grade form at a reasonable price and he does not feel like multiplying the cost of his product only for getting it a few percent purer and/or a few percent more of it, that would not be economical neither ecological he thinks. He is even having good results with preparing LSAmonade with the tap water from his cave, where NaClO2 and other minerals possibly destroying sacred alkaloids should be even of more concern -- therefore he thinks the water in his cave (having a pretty good reputation BTW) is not that bad. Does the hardness of tap water and the minerals contained therein somehow harm the extraction and reduce the yield of Harmalas or do they just make them less pure?

Swim spend some time considering the choice of acid and its quantity to use. He had little luck finding information in SI (Système international d'unités) on the units "little dash", "dash" and "bunch" referenced in the mentioned Guide and Thread, heck he could not even find the "shots" unit you mention. :lol: Therefore he decided to adapt Manske's recommendation of using 30g acetic acid in 1 liter. Swim was using vinegar supposedly containing 8% acetic acid, drinking water and E150c (Ammonia caramel) thus according to Manske and his own calculations Swim would be supposed to add 572,52 ml of 8% vinegar to each liter.

Swim felt this was pretty much and having good results with much less acid before when making simple traditional Harmala tea and trying to avoid hefty acetic acid fumes he decided to use less, perhaps 100-200 ml in each step, hard to tell exactly due to its evaporation and some acid residue in the gunks.

Swim hopes this to be a reasonably sufficient amount.

By "waterbath procedures" you are referring to not heating up the concentrate in a pot filled with water directly but to put it in a glass jar instead and place the jar on a towel in the pot filled with water or are there any other waterbathing teks? And the reason for doing this would be to prevent the percipitates at the bottom from being damaged or degraded by overheating from the pot? Swim was using a induction cooker with a stainless steel pot, would heat not dissipate from the pot into the fluid smoothly and evenly enough?

Swim likes the other method you mention, he was already planning to use a saturated NaCl solution in his next wash instead of putting the NaCl into the tea. He has some questions though:

• Is Swim right in the assumption that the solubility of NaCl in water is temperature dependent and by saturating it at room temperature then cooling to 0 degrees Celsius more excess salt will precipitate but the solution will be better saturated?
• Would Swim have to dry the gunk more thoroughly before putting the saturated NaCl solution on it compared to the first method to make sure there is little water left in it that would need to be saturated as well?
• Should the saturated solution be warmed up to accelerate the dissolving of the magic or is it better left at near 0 degree Celsius temp? Is Swims assumption correct than warming up the NaCl solution to dissolve acidified gunks is safe, but warming it up to speed up dissolving of crystals obtained via basing could harm the alkaloids and therefore they should rather be dissolved at 0 degrees Celsius?

Swim thanks Crystalito for his advice and finds buchner funnels and vacuum filtering interesting. Pardon Swims ignorance, but what exactly is a tap aspirator?

Swim hopes some other wizards may enlighten him on the suitability of the materials he used to cast his spell. Swim acknowledges that turning Sodium Bicarbonate into Sodium Carbonate is trivial, but he would like to avoid wasting electricity, environment, time and money on its production if the material he can acquire directly would be suitable.

The ammonia procedure sounds interesting. Is ammonia sold freely or is it a somehow scheduled substance?

Dissolving the excess soda with water sounds ingenuously simple - Swim feels embarrassed he did not envision such a simple and straightforward solution himself before.

Swim just wonders whether "small amounts of water" would be enough to dissolve circa 584g of soda? :shock:

Sincerest Regards,

from a Humble Nexus Apprentice

 

[Infundibulum]

Dissolving the excess soda with water sounds ingenuously simple - SWIM feels embarrassed he did not envision such a simple and straightforward solution himself before. Embarrased

SWIM just wonders whether "small amounts of water" would be enough to dissolve circa 584g of soda? Shocked

This is SWIY's best solution to the problem atm.

SWIY's got plenty of sodium carbonate in his precipitates. Just try to dissolve all teh precipitates in water (1-2 litres). If the contamination is sodium carbonate then this will dissolve away and at the same time it will be more than enough to keep the pH high and the harmalas undissolved.

Hope that helps,

 

[mutizen]

Thus might Swim reasonably assume that adding a larger amount of (slightly basic) tap water would be better than adding less slightly acidified tap water like endlessness did suggest (before possibly having enough information)?

What PH should Swim aim at achieving in his next Sodium Carbonate basification? Would going to PH 10 be good enough?

Could Swim (currently lacking a PH meter) simply compute the amount of Sodium Carbonate required to basify a reference volume of H2O to at least this PH value and use it as a guideline in his next basification to prevent such a contamination to happen again?


Sincerest Regards,

from a Humble Nexus Apprentice

 

[Infundibulum]

Thus might Swim reasonably assume that adding a larger amount of (slightly basic) tap water would be better than adding less slightly acidified tap water like endlessness did suggest (before possibly having enough information)?

What PH should Swim aim at achieving in his next Sodium Carbonate basification? Would going to PH 10 be good enough?

Could Swim (currently lacking a PH meter) simply compute the amount of Sodium Carbonate required to basify a reference volume of H2O to at least this PH value and use it as a guideline in his next basification to prevent such a contamination to happen again?


Sincerest Regards,

from a Humble Nexus Apprentice

SWIY's thinking too much and he's is getting confused.

Tell him to just add water, just tap water to the impure precipitates, mix well and then wait for the freebased harmalas to sediment.

As for guessing pH, a pH meter is very important. Otherwise, use this rough guide for guestimates.

 

[endlessness]

yeah definitely do it with the tap water, not acidified.. Before, I was thinking a completely different thing, which was to redissolve it ALL in acidified water and reprecipitate, which was more of a general solution, whatever the contamination was... but given all you said, indeed it will most likely be excess sodium carbonate, and just redissolving that in pure water will get rid of sodium carbonate will be much easier

 

[mutizen]

SWIM would like to express his thanks and sincerest gratitude to the mighty wizards for their kind advice and handy PH calculation sheet. :d

Now he feels reassured he is going to do the right thing which is important to him as he likes to play on the careful, reasonably safe side and understand the consequences of his actions.

Some confusion is still left in Swims head as he can clearly perceives the narrow borders of his limited understanding and many of his questions aimed at expanding them are still left unanswered.

For now he just hopes the Sodium Carbonate he used was safe enough for this purpose and concludes he should ASAP read some good sophisticated tome on alkaloid extraction related Alchemy. Could the mighty wizards kindly recommend some suitable alchemical reading for an scientifically educated and trained mind but with little biochemical knowledge yet?


Sincerest Regards,

from a Humble Nexus Apprentice

 

[Crystalito]

Hmmm.

On the water used,i do not think many things will change if you use tap water.I just like using distiled water ,feeling i know what it contains and that it lacking a salt content (salts,that is, found naturally i water) could extract more .I think its mostly my "obsession" with purer solvents and reagents, so feel free to disregard it : as i say i dont think its going to make much of a difference, its not as if your proccess will fail or become poisonous or something!

Now, on other issues you mentioned, i will use the quoting method to keep track of the questions and address them appropriately ,i hope it does not get too distracting.

SWIM spend some time considering the choice of acid and its quantity to use. He had little luck finding information in SI (Système international d'unités) on the units "little dash", "dash" and "bunch" referenced in the mentioned Guide and Thread, heck he could not even find the "shots" unit you mention. Laughing Therefore he decided to adapt Manske's recommendation of using 30g acetic acid in 1 liter. SWIM was using vinegar supposedly containing 8% acetic acid, drinking water and E150c (Ammonia caramel) thus according to Manske and his own calculations SWIM would be supposed to add 572,52 ml of 8% vinegar to each liter.

Ah, it was not meant to be a unit so much,it was more of indicative of volume.Lets say about 25 ml,so if i use vinegar i use about 50 ml per liter.I Have used from 25 to 50 ml with no problems at all,seemed to work fine. I am under the impression though that using HCl can lead to quicker precipitation of more alkaloids, but given how abundant is peganum harmala if i am correct you are not missing much.

By "waterbath procedures" you are referring to not heating up the concentrate in a pot filled with water directly but to put it in a glass jar instead and place the jar on a towel in the pot filled with water or are there any other waterbathing teks? And the reason for doing this would be to prevent the percipitates at the bottom from being damaged or degraded by overheating from the pot? SWIM was using a induction cooker with a stainless steel pot, would heat not dissipate from the pot into the fluid smoothly and evenly enough?

You nailed it right there with the towel method, its a very good home waterbath method, no need to go more fancy on it. Its purpose is to avoid contact of glass jar with the metal of the pan, because it might break and...there goes your solution all over the place. I use it every time i redissolve the precipitate in NaCl saturated water to try and solubilise it in the solution so more impurities will get dissolved into solution and not remain trapped inpossible crystal structures forming while initial precipitation.

# Is SWIM right in the assumption that the solubility of NaCl in water is temperature dependent and by saturating it at room temperature then cooling to 0 degrees Celsius more excess salt will precipitate but the solution will be better saturated?
# Would SWIM have to dry the gunk more thoroughly before putting the saturated NaCl solution on it compared to the first method to make sure there is little water left in it that would need to be saturated as well?
# Should the saturated solution be warmed up to accelerate the dissolving of the magic or is it better left at near 0 degree Celsius temp? Is Swims assumption correct than warming up the NaCl solution to dissolve acidified gunks is safe, but warming it up to speed up dissolving of crystals obtained via basing could harm the alkaloids and therefore they should rather be dissolved at 0 degrees Celsius?

1)Well as a general rules ,solubility of solids in liquids increases with increased temperature although NaCl (and also some other salts) do not stick so much to the rule.Believe it or not Nacl Solubility does not vary THAT dramatically with temperature.
Have a look at this wikipedia diagram:

Increased temperature might aid the conversion of beta-carboline acetate salts to their hydrochloride forms,propably aiding quicker precipitation.

2)Practically such small amount of water (soggy resing, sliiiiiiightly runny) will not make a difference ,so dont worry about it.

3) I answer part of the question in 1 plus a bit on the waterbath comments. I have had no problem heating up freebase beta carbolines in solution. They are not that sensitive in my experience.

Pardon Swims ignorance, but what exactly is a tap aspirator?

Check wikipedia for "Aspirator".Its a "three end device":You screw one end on the water tap, water goes through it and out of the opposite end ,and it creates a vacuum at the end that is perpendicular to the Water In/Water Out axis.Attach a tube there and rig it up to your vacuum flask and happy filtrations! No need to go for a high budget one, i use a flimsy plastic one and it works nicely.

The ammonia procedure sounds interesting. Is ammonia sold freely or is it a somehow scheduled substance?

Look for it in pharmacies, i dont think its scheduled.

Could the mighty wizards kindly recommend some suitable alchemical reading for an scientifically educated and trained mind but with little biochemical knowledge yet?

I hope others will chime in since i know of no webpages detailing them on the top of my head. Try typing though in google "Alkaloid extraction" or "Alkaloidal extraction" and i think you will find some webpages with basic guidelines on them.I think also Manske (the author) has a series of books called "The Alkaloids" which can be helpful if one is looking for chemical properties of certain alkaloids.

The philosophy behind extractions is to take advantage of differential solubilities of a compound ,in different solvents and in different forms of it so as to isolate it.For this to be successful one should know the solvents used (which is polar ,which is non-polar) and also he should know WHAT he is after.I would say that the first stop would be to review solubility data on the compound one wishes to isolate ,which can be found in Merck index and also scattered all over the web.If the principle is unknown (when working with novel plant material) some "general solvents" (i would try first alcohol) can be used ,or also one can try fractions of extract extracted by different solvents. For example if i had an "alien plant species" that one told me it contanins principles active in human/mice/apes, i would split the the plant mater in three portions and extract one with water, one with ethanol and one with lets say chlorophorm and see which part is active.

For extractions usually only basic chemistry knowledge can suffice,focusing more on simple reactions ( such as neutralisation -acid+base-) and physical/chemical properties of solvents and solutes.

 

[mutizen]

Swim did add 459g of the dried crystals into a pot with 1,5l of tap water at room temperature exactly as the archmages Infundibulum and endlessness suggested (Swim left the water rest in the pot for 2 days first in the hope of getting rid of some contaminants).

Swim did stir vigorously until the crystals dissolved completely, then put the pot into the fridge.

After 3 hours Swim thinks nothing precipitated. The cold brown fluid is murky and unfortunately he did not have any glass container of an appropriate size to pour it in, thus he regularly tries to catch something at the bottom of the pot with a tablespoon but without any success yet.

Should Swim wait longer or add more Soda? How long should it take for the magic crystals to start precipitating? Could it be that the Soda he used does not work as expected due to its Pulverization or Calcination?

Swim wonders what devious unknown forces could prevent his Harmala Spirits from being freed and how he could best aid them to release them from their torments?



P.S. As Swim was trying grok the pH calculation sheet archmage Infundibulum kindly provided, his professional deformations forced him to immediately verify the border conditions via functional testing (which is a proven technique to catch common bugs in software). Swim thinks it is essential to know the limits of any algorithm in order to be able to reliably use it (same goes for measurement instruments and many other simplified simulation models in life). Swim got very weird results thus he wonders at what input ranges the calculators work reliably:

The sheet does not allow to add 0g of acid/base to yield a pH of 7. Thus he tried to add 1 microgram units into 1 liter of water:

1 mcg CH3COOH + 1l H20 should have pH: 6.27
1 mcg C4H4O4 + 1l H20 should have pH: 4.89
1 mcg C6H8O7 + 1l H20 should have pH: 5.12
1 mcg H3PO4 + 1l H20 should have pH: 5.02
1 mcg HCl + 1l H20 should have pH: 7.56
1 mcg H2SO4 + 1l H20 should have pH: 7.99

1 mcg CHNaO3 + 1l H20 should have pH: 4.89
1 mcg Na2CO3 + 1l H20 should have pH: 8.15
1 mcg NH3 + 1l H20 should have pH: 8.01
1 mcg NaOH + 1l H20 should have pH: 6.4
1 mcg NaOH + 1l H20 should have pH: 6.25

Bases decreasing pH below 7 and strong acids increasing it above 7? Pretty weird Swim thinks. NaOH pH is calculated twice in the sheet, Swim is not sure which one is the correct one.

According to the calculator adding just 1g of Soda Carbonate to 1l of water would push the pH to 11.15 which AFASCT would be more than enough for extracting Harmalas. Thus adding merely 10g would even push the pH of 10 litres to 11.15. Why should then Swim add more and watch the color change? Swim is confused. :?


Sincerest Regards,

from a Humble Nexus Apprentice

 

[Phlux-]

Damn sorry i missed this thread - Seems sorted now.

 

[mutizen]

Swim would like to sincerely thank Crystalito for enlightening him on the methods and techniques of achieving his powerful magic and he would like as well to express his appreciation of interleaving replies with relevant quotes.

Swim has to admit, he did not really try to look up the quoted words in SI as with his scientific background he is well aware they are not identifiers for any standardized physical quantities and thus extremely hard to uniquely quantify in terms of SI units, which was sort of the point of the admittedly rather perverse joke he was trying to make and even underline by attaching a emoticon.

On a side-note: Based on his modest knowledge and success in the field of Philosophy of Science though, Swim would like to assure Crystalito that virtually nothing would hinder 25ml from being made into e.g. a standardized "shot" unit and added to SI if it would not be inherently redundant, decadic number system unfriendly and damn pretty unnecessary.

As for the waterbathing method, Swim now understands its importance when the desire or need to use a jar is present. He still wonders though whether the stainless steel pots he is using have somehow lacking properties compared to glass jars and whether pouring the fluid over from jars to pots and vice versa would also be less desirable than using jars and waterbathing as Crystalito suggests?

Swim was preparing his saline solution yesterday, so he looked up the solubility of NaCl at zero and 100 degrees Celsius already. Nevertheless he finds the diagram very enlightening and is thankful for its addition.

Did Swim apprehend Crystalito on temperature matters correctly that heat will not damage the magic even if it is put into a basified solution, thus he could e.g. without worries boil his fluids even with Sodium Carbonate added to make the magic dissociate faster? And would it not degrade much of Harmine into Harmaline?


Sincerest Regards,

from a Humble Nexus Apprentice

 

[Infundibulum]

The sheet does not allow to add 0g of acid/base to yield a pH of 7. Thus he tried to add 1 microgram units into 1 liter of water:

1 mcg CH3COOH + 1l H20 should have pH: 6.27
1 mcg C4H4O4 + 1l H20 should have pH: 4.89
1 mcg C6H8O7 + 1l H20 should have pH: 5.12
1 mcg H3PO4 + 1l H20 should have pH: 5.02
1 mcg HCl + 1l H20 should have pH: 7.56
1 mcg H2SO4 + 1l H20 should have pH: 7.99

1 mcg CHNaO3 + 1l H20 should have pH: 4.89
1 mcg Na2CO3 + 1l H20 should have pH: 8.15
1 mcg NH3 + 1l H20 should have pH: 8.01
1 mcg NaOH + 1l H20 should have pH: 6.4
1 mcg NaOH + 1l H20 should have pH: 6.25

You're right;

The calculator is not 100% complete. The algorithm is also not perfect that's why one gets such bizarre values if one goes to such the extremes. SWIM assumed that none would try to dissolve microgram or even miligram quantities per litre when wrote the equations.

For obvious reasons he did not allow for a 0 value since this was assumed to be ~7. The equations follow mostly a linear regression. In practise they should be exponential (with limit to "7" as "grams" goes to infinity). Equally weird results are obtained if, say one tries to compute the pH of dissolving 10 tonnes of sodium carbonate in water!

He's not great computing equations in Excel though. But thanks for pointing that out!

 

[mutizen]

Damn sorry i missed this thread - Seems sorted now.

Swim would like bring the sad fact to archmages (and fellow software architects : ) Phlux- attention, that there are still powerful devious forces inside of Swims magic cauldron reluctantly refusing to release the sacred spirits of Haoma as he mentions in post number #13. Swim is still very much concerned about their health and hopes for their revival soon.

Beside that, many unanswered questions from this thread are still lurking in Swims mind unsuccessfully trying to push the narrow borders of Swims alchemistic consciousness.

Thus any kind of feedback from archmage Phlux- would surely be highly appreciated.

Sincerest Regards,

from a Humble Nexus Apprentice

 

[mutizen]

You're right;

The calculator is not 100% complete. The algorithm is also not perfect that's why one gets such bizarre values if one goes to such the extremes. SWIM assumed that none would try to dissolve microgram or even miligram quantities per litre when wrote the equations.

Experience suggests that many, sometimes even knowledgeable people will push even unreasonable inputs into an algorithm and will assume/expect the outputs to be correct.

The ideal solution would often be to let the algorithm check its preconditions (that the inputs are reasonable enough for it to be able to yield expected outputs) and show a error message to the user describing the expected inputs otherwise.

Another less sophisticated solution would be to at least document the preconditions. Swim would suggest to add them to your spreadsheet so that even confused users like Swim and even SWIY might know what to expect, because believe it or not, most programmers tend to forget many details of the code they have written over time and its always faster/easier to look at the usually concise specs than study the algorithm and reason about it. Otherwise its hard to tell whether the output is total nonsense as in the extreme cases provided or something one can rely on without having to verify it by doing calculations by hand what kind of destroys the whole purpose of automating it with an algorithm.

For obvious reasons he did not allow for a 0 value since this was assumed to be ~7. The equations follow mostly a linear regression. In practise they should be exponential (with limit to "7" as "grams" goes to infinity). Equally weird results are obtained if, say one tries to compute the pH of dissolving 10 tonnes of sodium carbonate in water!

SWIY could simply add some preconditions (predicates that must hold for the input values) as simple text to the sheet, e.g.:

The algorithm is correct iff:

• WA <= WW * C1
• WA >= WW * C2

Where:

• WA - weight of acid or base
• WW - weight of water
• C1 - some scalar coefficient, e.g. say 1 for limiting maximal acid/base to water ratios to 1:1
• C2 - some scalar coefficient, e.g. say 0.001 for limiting minimal acid/base to water ratios to 1:1000

Adding some info about the precision (maximal relative error of the approximation) might be even better though a lot more demanding.

He's not great computing equations in Excel though. But thanks for pointing that out!

SWIY is welcome and Swim is glad if he could be of any help.


Sincerest Regards,

from a Humble Nexus Apprentice

 

[mutizen]

Swim waited for many hours for the Haoma spirits to precipitate, finally he filtered his magic cauldron and obtained a small amount (a disc of 5cm diameter and 1mm height before drying) of brown gunk -- looks similar as the gunk obtained from the NaCl washing before, just less of it.

Thus he put it into a electric oven with hot air at 40 grade Celsius to speed up water evaporation.

Swim hopes this way he will obtain the sacred spirits in pulverized form and may then allow them to speak to him.


After what Swim read before he was kind of expecting some visible Haoma crystals to emerge after adding the Sodium Carbonate. Was Swim wrong in his assumption? Did he do something wrong, was his technique suboptimal or is it normal to obtain the product in gunk form?

Would it now be best for Swim, after thoroughly drying it, to apply it sublingualy or would he better dissolve it in water and drink it as a sacred tea?

Would it be reasonable to further purify and recrystallize with a 40% alcoholic distillate if Swim currently does not possess high proof alcohol? What other cave chemistry could Swim employ for recrystallization?


Sincerest Regards,

from a Humble Nexus Apprentice

 

[endlessness]

I dont know anymore what this brown gunk is.. could be harmalas... I guess you can only find out trying it

something else that calls a bit is using heat and air to dry. I dont know how easily harmalas oxidize with these conditions, if it's like dmt which does, for example. I usually preffer vacuum drying the bulk and then in the end just let on open air in the filter or on a plate to finish.

Its hard to say, my overal impression is that you over-complicated things, no offense of course.. Also the measures were exagerated.. Its hard to track what happened. Dont know either about where you got your seeds from, their quality...

As for cleaning harmalas up, alcohol+harmaline=harmala red, which is possibly inactive product (until someone tries it, we dont know... if you want to try it and bioassay after, tell us, but usually people try to avoid harmala red). So the way it is done is redissolving the harmalas in acidified water, filtering this water with very fine filters (like stacked up filters or something), and then precipitating with sodium carbonate again.

I wouldnt use so much quantities as you always use.. Lets say as an example I would use 1l warm water with a couple of splashes of vinegar (no idea in volume, maybe 25-50ml?).. Then this should redissolve the harmalas, and a little bit impurities maybe wont dissolve.. Then after filtering I would add a teaspoon of sodium carbonate, which should be plenty and after a while of stiring, should all dissolve and precipitate the harmalas again. If it wasnt enough sodium carbonate, I would add another teaspoon, and so on.. But definitely nothing around 300g of sodium carbonate! Repeating this process a few times cleans up to very clean, white for harmaline, light tan for harmine or the mix of both, as you can see in the pictures of the guide I put together.

good luck !