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Acid to Base vacuum tek

Migrated topic.
Quoting this for reference, from the above pdf:

MHRB Vacuum extraction tek

v1.1


This tek is an Acid to Base extraction and using vacuum to speed up the evaporation stage without oxidizing the end product which can happen if you use a fan.

Safety warning

  • Although the condenser catches most naphtha (highly flammable and toxic), some will still flow through the pump and end up in the air. Use outside only. The pump produces sparks and you do not want to blow up your room, nor do you want to inhale the fumes.
  • Naphtha vapors are heavier than air, so ventilate a room well. You do not want to blow up your house.
  • Only use a lab grade vacuum pump with a fluid trap.
  • This tek uses a very dangerous chemical (sodium hydroxide). Protective clothing, gloves, and safety glasses are absolutely required. Lye in your eyes can blind you. No kids or pets nearby!
  • Only use lab grade vacuum compatible Erlenmeyer's. Weak glass can implode when vacuum is
    applied.
  • Never add water to lye (sodium hydroxide) as this will cause the lye to explode.
  • When adding lye to water, the water temperature will increase significantly. Use a heat and chemical resistant container.
  • Keep eye washing equipment and acid/base neutralizers nearby.
  • At some point you need to warm up a naphtha mixture. Use an electric stove. Do NOT use fire heating! Naphtha will combust on a hot metal surface too, so use with care. Use outside only!
  • Shaking the Base solution needs to be done gently. A lot of heat can be generated which heats up
    the air in the container, causing the pressure to rise dangerously. You do not want the container to
    explode or the cap to fly off.
  • Keep a fire extinguisher nearby.

Equipment

  • 500 gram Mimosa Hostilis Root Bark (MHRB), either powdered or raw bark.
  • Blender (only required if MHRB is not powdered).
  • Hammer (only required if MHRB is not powdered).
  • Scissors (only required if MHRB is not powdered).
  • Lye: sodium hydroxide (NaOH). Preferably in powdered form as it dissolves faster. Amount: 1g MHRB = 1g Lye, so for 500 gr MHRB use 500 gr lye.
  • Acid: citric acid powder. Do not use sulfuric acid as this is dangerously corrosive and really not necessary.
  • Solvent: 1 litre naphtha (approximately, you might need more or less). But make sure it doesn't contain any additives by placing a small amount on a glass surface and checking that it leaves zero residue when evaporated. Purchasing a large amount of lab grade naphtha is monitored in some
    countries. Source from regular consumer stores (Zippo fluid for example). Do not purchase at the local chem shop.
  • 4 litre Lab grade distilled water (1x distilled is fine, no need for de-ionized water).
  • 4 litre chemically resistant plastic jerrycan (must be able to see liquid level).
  • Pipettes (chemically resistant).
  • pH strips (for low pH).
  • Two 500 ml heat resistant beakers.
  • Two metal spoons.
  • Two 1 liter vacuum Erlenmeyer flasks.
  • Two rubber stops for Erlenmeyer.
  • Device to create a hole in the rubber stop. A regular drill will not work. There exists a special hollow press for this purpose. Search for a "cork borer".
  • Small pipe which fits in the rubber stop hole and connects to the vacuum hose.
  • Two meter vacuum resistant hose.
  • Three meter copper pipe which fits in the vacuum hose. This will be used to condense the naphtha vapor.
  • Hose clamps.
  • Lab grade vacuum pump with moisture trap.
  • Mobile electric stove.
  • Optional: magnetic stirrer with a heated base, and a stirring magnet.
  • Aluminum pan.
  • Bucket to place water and ice in.
  • Chemically resistant gloves (absolute must).
  • Lab eye protection (absolute must).
  • Fire extinguisher.
  • Acid and Base solution to neutralize spills.

Extraction

If you have raw bark instead of powdered bark, you first need to break up the bark. Whack the pieces of bark with a hammer to break the fibers apart. You can do this inside a plastic bag with a flat stone in it to prevent the pieces of bark from flying around. After all pieces of bark are flattened with a hammer, cut it into small pieces with scissors. After that, place a small amount of bark into a blender and blend for a minute or so. You might have to shake it a bit while blending. If a ball of wool like structure appears, take it out, cut it apart with scissors, and blend again. When done, take out the blended bark and put aside. Then repeat the process until all bark is blended. Note that blending the bark will create very fine dust (looks like smoke), so wear a dust mask.

Place the MHRB in the mixing jerrycan. A decent amount can be added. If manually chopped up root is used, the apparent wood volume will be reduced once the wood breaks down in the lye.

Fill the jerrycan with some distilled water. Leave some space for the lye solution. You can always add more water later.

Add some citric acid powder to the mixture. Gently shake and test the acidity with the pH test strip. It should have a pH of 4 or less.

Leave the acid mix at least for 12 hours, but longer (even a few days) is better.

Now weigh out the right amount of lye. Place the right amount of lye in a separate container. Take a heat resistant beaker, add distilled water, and gently add a little bit of lye. Gently! Never add water to lye as this will make the lye explode. Do not use a wet spoon to scoop up lye. Use one spoon to scoop up lye and another one to stir the solution. Stir gently until all lye is dissolved. The temperature of the water will increase significantly. Wait for it to cool down and add some more lye.
You can use a fan to speed up the cooling process. Add more lye, stir, cool, and repeat the process until all lye is dissolved. When done, wait for it to cool down. Warm is good, but not hot. Make sure there are no undissolved lye particles left. This is important as it can dangerously increase the temperature of the MHRB mixture once added. If there are undissolved particles left, decant half the solution into another beaker, leaving the particles at the bottom. Then add more water and stir.

Gently add a little bit of lye solution to the MHRB mixture. Make sure the lye is still warm because this raises the temperature of the mixture, resulting in more efficient DMT extraction. Adding the lye to the MHRB mixture should turn the mixture black. You might see temporary white precipitation as well. Add a bit more lye. Repeat the process until all lye is added to the MHRB mixture. Do not add the pure lye directly to the MHRB mixture as this can cause the container to melt or explode. The pH should be at least 13 but it is not possible to test this with a pH strip due to the strong color of the mixture. Instead, enough lye is added by observation. After everything is mixed, shake gently and wait 10 minutes or so. Add some naphtha and place the cap on. Shake gently, then place upside down, then upright again. There should be very little emulsion and the layers should separate with clear naphtha on top. The black mixture should easily roll down from the top part of the jerrycan. If it doesn't do this, wait a bit longer and try again. If you still get emulsions with the black fluid sticking to the side of the jerrycan at the top, mix more lye in a separate beaker, wait for it to cool, and add it to the MHRB mixture.

Add naphtha to the MHRB mixture until you have at least a 5 mm layer of naphtha sitting on top.
Some teks tell you to use as little naphtha as possible but that is not necessary. Add some more water if needed in order to make sure that the mixture can rise a bit higher if the container is squeezed, making the surface area of the top of the liquid smaller.

Gently squeeze the container a bit, then place the cap onto the jerrycan. Now, gently shake. The aim is to check for pressure increase which you can see by the jerrycan bulging. This does not always happen, but it can. It depends on the temperature of the mixture and if there are any undissolved lye particles in the solution, causing a temperature increase. Remove the cap to release any pressure build-up.

When sure there is no pressure increase with further shaking, secure the cap very tightly and shake a bit harder. Do not shake aggressively as this can cause insoluble emulsions to occur. The added air bubbles will also oxidize the end product. You want to make sure the naphtha mixes completely with the solution. It will rapidly rise to the top when shaking is stopped, but this is normal. Once most naphtha has risen to the top, shake again. Do this a couple of times. When finished shaking, leave it long enough so that all naphtha rises to the top and the top layer is free of contaminants. You can speed up the naphtha moving to the top by vibrating the jerrycan with a device or tapping it with your fingers.

Open the container and gently squeeze the plastic container to make the fluid rise a bit higher. The mixture is dangerous, so do it gently! Once the fluid rises to the small neck and the top surface area is reduced, take a pipette and suck out the top naphtha layer. Place the naphtha into a regular beaker. The pipette only holds a small amount so you need to repeat this process several times. Be careful not to suck up any contaminants. If you do, you can gently squeeze the pipette and put some of its contents back in the mixture. You can also hold the pipette steady for a while to make the contaminants sink to the bottom and then gently squeeze it out. This is a great way to remove nearly all naphtha from the mixture and still have a clean result. The naphtha should have a slight straw yellow color once extracted.

Once all naphtha is removed, add some more naphtha to the mixture and repeat the shake and extract process. Do this at least 3 or 4 times. It depends how much naphtha you use and what the temperature of the mixture is. When the naphtha does not change color anymore, you can stop.

Wait for the naphtha to settle in the beaker. Some contaminants will sink to the bottom. Gently decant the fluid into another beaker and use a pipette to more accurately separate the last bit. After that, place the naphtha in a vacuum Erlenmeyer. If a plastic beaker is used, do not let the naphtha sit in it overnight because it will soften the beaker and deform it.

Now the naphtha has to be removed so only DMT remains. We are going to use vacuum for that.
Make a vacuum condensation rig like this:
[diagram - see attached pdf]

Instead of a regular electric stove, you can use a magnetic stirrer with a heated base. You will still need a pan with water in order to increase the heated surface area. This will greatly speed up the evaporation process. If you don't have a magnetic stirrer, you have to manually swirl it around. If a magnetic stirrer is used, an aluminum pan has to be used, otherwise the magnetic field will not be strong enough.

The left Erlenmeyer contains the extracted naphtha and is placed in a pan with tap water. The pan is placed on an electric stove. Place a rubber stop on the top opening and squeeze an extended paperclip or needle in between. This is to make it leaks a small amount and creates some airflow.
Without airflow, the setup does not work well. Make the leak as small as possible. A large vacuum will be created and even a very small opening will create significant airflow. Only a small amount of airflow is needed because air can oxidize the end product. It requires adjusting when in operation.
You can judge the airflow amount by the ripples it creates on the naphtha. Also observe the vacuum gauge on the pump. Create the largest vacuum possible.

The copper pipe is used to condensate the naphtha vapors. If you cannot find a suitable copper coiled pipe, you can make one yourself by bending regular copper pipe around an existing pipe. Place the copper pipe into a bath with ice water. Using cold water is important, otherwise the naphtha vapor will not condensate well and will flood the room, causing an explosion hazard.

The right Erlenmeyer has a rubber stop with a hole in it. A pipe in the hole connects to the vacuum hose. This setup catches the condensated naphtha because the exit hole is on top. Having this condensation trap is important because the pump condensation trap has a too small volume and it does not catch enough naphtha. Even with the Erlenmeyer condensation trap, there might still be some naphtha in the small pump condensation trap. The amount of naphtha vapor discharged into the air is minimal but present. Do not use this setup indoors. You might be tempted to re-use the condensated naphtha as it appears to be very pure, but it contains enough contaminants to cause problems with re-extractions.

First switch on the vacuum pump. The naphtha might boil without heat being applied. After it stops boiling, start heating. Make sure the naphtha does not fly into the vacuum pipe. Slightly heat the left Erlenmeyer with the electric stove (via the pan with water, not directly). Do not use fire! If you don't use a magnetic stirrer, gently swirl the flask to speed up the evaporation process. After some time, only yellow or amber colored goo will be present in the Erlenmeyer. If a magnetic stirrer is used, it will not work anymore if the fluid level gets too low. In that case, use manual swirling.

After the solution cannot be swirled anymore because it is too sticky, turn off the heat and let it sit with the vacuum pump on for an hour or so. This will pull the very last amount of naphtha out of it and as it cools down, crystals will start to appear.

Once all goo has crystallized, it can be removed from the Erlenmeyer with a long knife.

Cleanup

The black base solution can be discarded in the toilet because it is basically the same as a sink unblocking solution. Make sure to wear gloves and eye protection. Carefully squeeze out a bit of sludge, flush the toilet, and repeat the process.

Flush the plastic container with lots of water. You can add some vinegar to neutralize any leftover base. Then cut the container with a box cutter so no one can re-use it when found in the trash.
 
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