Is this yield normal?

[Istubar]

Hi nexians!

At the time I'm working on my own extraction, but I think that the yield is a little bit poor. I'm using 1L water, 50g MHRB, 50g NaOH, 50ml heptane.

In the first pull I did not pre-evaporate, I put it into the fridge and that was all. After pouring the solvent and let it dry for a couple of days, the harvest gave me 40mg (0.8%)

In the second pull I did the same, except that instead of scratching to do the harvest, I've filtered it using a vacuum filter, but I wasted all the pull because it "fused" with the paper. After that there was nothing to scratch. At least the amount was nearly the same, not too much.

The third pull is coming. This time I pre-evaporate a little (the solvent changed from a clear color to a yellow one). The crystals are like on the first extraction, too tiny, and they are not too much. The only difference is that this time they are not white, they are more yellow. I will scratch it tomorrow and I will compare the weight.

Am I doing something wrong or do you think that this yield is normal? Maybe this amount is caused by the solvent or the MHRB?

Cheers! :thumb_up:

 

[Psyren]

Psyren, do you heat your naptha before adding it?

Can you elaborate how you manage the extraction of all 12 jars... Can this be done by one person?

-No, if you follow that time table the jar says warm, so i dont see the need to add any extra heat.

-ha ya its a little bit of work, but its always worked great for me in the end. Just put all the jars on the table add ingredients and mix. Then go along and add solvent to each, cap em, and shake and roll, i do two at a time, for a total of 3x and then go along and pull the solvent of each one. and freeze.

If you can dedicate a day to it, you can have most of the hard work done in a few hours. Then most of the time is in freeze precip and drying afterwards. This all can be done in a day if you put the time in.

 

[cyantific]

Psyren, have you had any issues with lye causing glass to break? I've heard hdpe is really the safest way to go.

 

[Psyren]

Ive never had any issues. I use your standard ball mason jars.
id be more worried about lye interacting with the lids then it breaking the glass.
but i never reuse the jars for extractions, i always get a new pack.

 

[cyantific]

Ever consider HDPE containers? You could reuse them many times, without the fear of breaking. Something like this....

http://www.ebay.com/itm/1-Liter-HDPE-Plastic-Bottle-with-CRC-Foam-Lined-Cap-/230579898395?pt=LH_DefaultDomain_0&hash=item35afa2081b

 

[Psyren]

lol well now that i think about it the bottles my NaOH comes in looks just like that and prolly is hdpe. I think i might start saving them.
Im just so used to using mason jars, I use them all the time for mycology.

 

[Istubar]

Here we go again!

I'm very frustrated, because my extractions doesn't go as good as I thought.

I tried with another recipe. This time I've used 750ml of water, and 50ml of heptane (for 50g of MHRB). In this recipe the phase don't want to manifest, so I have had to wait until in the next day to see it appearing. When came the time to use the decantor funnel, the phase disappeared again. Maybe it was too little amount of heptane. I tried adding 25ml more and nothing. What the hell is happening? I should use 100ml or 150ml? Also I'm having problems when I try to evaporate the heptane. I need to wait for a long time. Heating it doesn't work, only if I apply hot air above it with a hairdryer (and if I do that as I discovered, I will produce dmt-oxide...).

Some advice please? Maybe using heptane is a bad idea.

Also I've read in another recipes the following ingredients:

350ml of water
14g NaOH
50g MHRB
200ml hexane

The author says, that he reached 1,5% of yeald, and that he used common salt to break the emulsion.

I've found that very surprising because the proportions are really different than mine.

 

[Electric Kool-Aid]

Also I'm having problems when I try to evaporate the heptane. I need to wait for a long time. Heating it doesn't work, only if I apply hot air above it with a hairdryer (and if I do that as I discovered, I will produce dmt-oxide...).

Some advice please?

Ok. Advice.
Fact. Hair dryers use a hot element that can ignite heptane, naphtha or many other flammable solvents. Danger danger!!!!
Advice. Do not use a hair drier or any sort of heater. Use either a regular fan or a box fan (large type used in computers works good. You can pull with heptane and precip out or use heptane to re-x in a very small amount and let stand, it evaporates quickly.

Edit: some say you can use a hot bath to evap solvents too.

 

[Nmk8743]

-Sorry for bringing up an old thread for my first post but......I felt like I should chime in, just in case the op is still working on this.

-First off put the hairdryer down. Yes it is dangerous and yes using a hairdryer to evaporate saturated solvent will cause oxidization. Once this happens you will need zinc to recover the freebase. You can minimize loss by pouring a small amount of warm solvent over the oxidized dmt and proceed to re-freeze precip. This will pick up any freebase left mixed in with the goo because dmt-oxide is not soluble in naphtha/heptane. You can smoke the gooey oxidized junk. Just spread onto a favorite herb or onto steel wool/screen if using a 'machine' type device.

-Ok now for your methods. If you prefer a straight to base extraction that will work just fine. Your processes are good but your ratios (mhrb:naoh:water:solvent) are definitely negatively affecting the yield. Finding a good ratio that works best for you is personal preference and will take some time; but I would highly recommend starting with a ratio of 1:1:15 (mhrb:naoh:h20) . So for example let's say you want to process 250g of root bark. You would mix 250g shredded/powdered mhrb, 250g lye and 3750mL distilled water. I guarantee this change alone will almost double your yield. i.e.1%-1.3% (lower end % with stb, and higher % with a/b methods) yields are common and expected. I will mention that if you are using pre-powdered bark you may want to experiment with more h20 in the mix. Generally around 20% more water for pre-powdered mimosa.

-Alright the next item that will not only help increase yields, but also save your hard earned $$ is changing your solvent for pulls. Heptane is great...for recrystallizing; it's not so great for picking up freebase dmt. VM&P naphtha is much cheaper than heptane, it's easy to find at your local hardware store and it is superior to heptane as the solvent of choice for 'pulls'. Trust me on this one; you will use less solvent and pull more spice with naphtha than with heptane.

-To eliminate the problem of evaporating your solution before freeze precipitating and creating oxidized dmt by mistake you just need to use less solvent. For a one pound extraction using a 1 gallon jug, you will need no more than 40-50ml of naphtha per pull. On smaller extractions such as the 250g example above, I would recommend using 10-15ml of room temperature solvent per pull (don't use heat until the last pull or two as this will cause discoloration in final product). And I believe it was already stated to gently roll the naphtha within your container instead of shaking or using force; doing so will produce light yellow to white dmt freebase after freeze precipitating almost every time.

-Whew...that was long haha. I hope all this doesn't come off as arrogant, I'll be the first to say I have lots to learn about the process yet but I hope I answered some questions you had and I'd be happy to help further and/or post a detailed straight to base step-by-step extraction method that I've had success with in the past (1% yield avg). Take your time and find a tek you like then study it a little before you try it. Once you start to understand the process/reasoning behind each step you will find yourself ending up with some really nice spice.

-P.S.
Since it's my first post and I have no credibility here yet, here's are a few pics of an older stb extraction using a slightly modified Noman's tek to help validate some of my claims.

-Materials were 100g pre-powdered mhrb, 100g naoh, 1000ml distilled h20, naphtha for pulls and heptane for recrystallizing. Yielded 1.3g total spice white to light yellow in color... 3/4g of that was produced within 4 hours of beginning the process.

-Crystals forming through freeze-precip w/naphtha.

2012-08-08_14-00-15_901 by nmk8743, on Flickr

-.75g white powder.

IMG_20120912_104257 by nmk8743, on Flickr

-.60g light yellow powder.

IMG_20120809_133714 by nmk8743, on Flickr

-First recrystallization of yellow powder.

IMG_20120827_165120 by nmk8743, on Flickr

-First recrystallization of white powder.

2012-09-12_10-41-36_905 by nmk8743, on Flickr

-Experimenting with submerged thread during recrystallization.

2012-09-11_10-40-09_525 by nmk8743, on Flickr