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Freebase to fumarate crystals..[ Easier to read now ;) ] Options
 
halcyon
#1 Posted : 2/21/2009 7:38:03 PM

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Hello,

SWIM is trying to help a foafoaf who is seeking assistance with a problem related to dmt fumarate with FASA. This info was beamed into SWIMs head from Boa Vista, Brazil.

1. [Empsom Salts to Anhydrous Mag. Sulfate] Food grade epsom salts were baked at 400f for around an hour. After baking, the product was a still perfectly white solid that tended to clump. It was not gray or discolored in any way.

2. [Mag. Sulfate added to Acetone] A "bunch" of the mag. sulfate was added to a HALF can of regular hardware store acetone (note not "fresh" - maybe 3 weeks old, half full). Time passed and the salt settled to the bottom. When using acetone the liquid was pulled from the top with a piete.

3. [Creation of solution A and B] Now our Brazilian foafoaf follows the DMT handbook to a T. Two solutions were made: A) 1g of quite clean freebase was dissolved in 20ml of acetone, and B) where 100ml was used - 400mg of fumaric acid was added to this solution.

4. [Mixing of solutions - crashing out] Acetone/FASA was added slowly to the spice acetone rather slowly. With each drip, a something precipitated out.

5. [Waiting for xtals] Once all of the FASA was added to the spice laden acetone, the mixture was extremely cloudy indeed. This foafoaf was extremely excited to watch long slender xtals fall out and audibly clank around! But he was disappointed to not see or hear any xtal like thing. Over the course of a few hours the cloudiness "dropped down" - so the top portion of the vessel contained fairly clear (but not perfectly clear) acetone. It was covered to stop evaporation.

6. [Evapping acetone] 12 hours later the solution was not exactly cloudy but it was not clear either. It looked fairly clear from a distance, but up close it was nothing like normal acetone - something was in it. On the bottom was a very hard layer of something (almost like a sheet of not-cold ice) about a mm thick with some yellowish pieces of gunk in it (very few, but the foafoaf thought it was worth mentioning). No way did this glasslike stuff or the well named "gunk" weigh 1g. Foafoaf decanted the liquid, leaving the gunk as a memento. The decanted liquid was poured off into a new vessel.

8. [Evap shows precip] As the acetone evap'd, particles began falling out. They were quite yellow considering the source material. The particles looked by eye to be extremely similar to freebase particles. They were not long thin crystals, they were blobs.

9. [Evap cont.] The acetone had not fully evap'd when this foafoaf transmitted the data into my cranium via telepathy.

QUESTIONS

1. What could have gone wrong and where? SWIM has no idea - nothing makes sense about it.

2. What would be the absolute best way of determining whether the final precipitation is a salt or not? Clearly weighing would be a good start but there is that thorny issue of the ice-like stuff and gunk mentioned in step 6. What is the gunk?

3. What seems to make sense to SWIMs mind is just to dissolve the precip in acetone again - if it dissolves, freebase - otherwise, salt. Any tricks? Any reason not to do this (i.e. a much simpler and better test)?

3. This foafoaf wants to to see the long thin crystals.. so this will not be the last time. He/She/It will try again after some of the wildly smart people here chime in a bit.

Post if anything seems missing or doesn't make sense.

{h}
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amor_fati
#2 Posted : 2/23/2009 10:41:53 AM

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Yikes, it's a little hard to follow, but it just looks like SWIY didn't use enough FASA. Once it settles, add more and let it settle again, then keep repeating until no more reaction can be observed. Also, heating and fanning will not lend itself to proper freebase crystallization, as it sounds to be freebase that you ended up with after evaporation. SWIM would just redissolve and try it again.
 
Infundibulum
#3 Posted : 2/23/2009 11:09:09 AM

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halcyon wrote:

1. What could have gone wrong and where? SWIM has no idea - nothing makes sense about it.
2. What would be the absolute best way of determining whether the final precipitation is a salt or not? Clearly weighing would be a good start but there is that thorny issue of the ice-like stuff and gunk mentioned in step 6. What seems to make sense to SWIMs mind is just to dissolve the precip in acetone again - if it dissolves, freebase - otherwise, salt. But, should any heat or stirring or spell-casting help here? Any other tricks? Any reason not to do this (i.e. a much simpler and better test)?
3. This foafoaf wants to impress the aforementioned lemur with the "kryptonite"-like xtals - so he/she/it will likely try again. What adice would your domesticated farm animal give to him/her/it??

1. Nothing really seems wrong. But may I ask, where did SWIY buy the fumaric acid from?Which are the specifications of the pruduct? Is there anything else apart from fumaric acid? For instance, if the fumaric acid SWIY used cam efrom the manufacturer with some water (which depending on the product could range from 5% to 0.5% or less, then this trace amount of water could prevent dmt fumarate to precipitate.

2. Use the universal chemical analysing tools of your body. Taste and smell. Basically taste in this case. Fumaric acid tastes sour. dmt-fumarate tastes disgustign and bitter. 400mg of fumaric acid can totally salt 1g dmt freebase with very little fumaric acid remaining unused.

So yeah, just get SWIY's evaporated product, dissolve it in fresh anhydrouus acetone to get rid of any unused fumaric acid. Whatever does not dissolve is the good shit.

3. crystal shape tells little to SWIM. I propose SWIY exposes his genitalia and grind his teeth if he wants to impress the lemur!



Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
halcyon
#4 Posted : 2/23/2009 7:08:50 PM

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Thanks for writing amor_fati and Infundibulum. Both of you highly respected members found the context and intentional disjointedness to be rather disjointed. So, SWIM took away the context, lemur and all. The more interesting thing is what happened - not how. You'll see that each step now is boiled down to a single bracketed issue (i.e. [adding FASA to acetone/spice]) just to give you additional context. It should be skimmable now. Again thank you for your comments.

As for the fumaric acid - the vendor is well known on this form. Sells online $3/10g. Something about "flowing".. SWIMs foafoaf can't remember, maybe someone else can? They sell herbals, a few chems, and some other strange stuff. Supposedly food-grade. Not reagent, no data about it.

Conveying taste/smell issues might be hard, but SWIM likes the idea of adding fumaric acid to another acetone/possible-dmt-fumarate solution. If the pH doesn't go up as Fumaric is added, it is already salted. Correct?

Please keep the ideas coming. They will be appreciated.

Thanks again
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Viracocha
#5 Posted : 2/23/2009 9:10:29 PM

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I can't be sure, but I'd suspect an excess of water is present.
The fumaric acid should be of extremely fine, bone dry consistency. Is it?
Can you provide a picture of the acetone used? Some acetone is well known to be basically useless for such experiments..
Is the area you're in particularly humid?

When that tek was written, the acetone was used as is - no drying was performed.
I'm not sure if this matters, but perhaps could anything have happened during the drying to compromise the quality of the acetone?

Your fumaric acid source sounds extremely expensive!
Depending on the country you're in, you should really check this out, but likely fumaric acid and acetone aren't restricted chemicals so you can feel free to order them from a fine chemical supplier in your area. I found a source for AU$52 for 1KG of Fumaric Acid


As for the process, it sounds correct. All measurements are correct
When you made solutions A and B, were they perfectly clear?
How pure was the DMT used? This can be a big cause. I've found that pretty much the only way to get good crystals is to use recrystallised (maybe twice) dmt, fresh from an extraction - ie, not three week or three months old dmt.

Nonetheless, it sounds more likely that there was an excess of water present in the solution which the formed dmt fumarate ultimately resided in

Pictures say a thousand words, do you have any?

I'd be most curious to see your source of acetone
 
halcyon
#6 Posted : 2/24/2009 12:29:04 AM

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Thanks everyone. SWIM wishes swim could get some pics up or give more detail, but no contact has been made, so know way of knowing if he/she/it learned anything. Here is what SWIM knows:

* Acetone was from hardware store. Was partially used but clean. It sat at about 50% capacity for a few weeks and could have reacted with free oxygen in the air (though the lid was closed). Likewise, the baked Epsom Salt could possibly be not baked enough. As SWIM mentioned, it was a hard white substance - unlike the normal epsom salt granulars - but NOT gray.

* Spice was re-x'd in Heptane and fresh.

* Fumaric didn't come free ebay.. SWIM can't remember where - but it was a website that also sold some herbal extracts - maybe even one the sells THH or Harmine. Ring any bells?

Likely a fumaric acid issue - not a super saturated solution is the prevailing theory right now.

Again, all help is GREATLY appreciated. Keep it coming. Anyone else see something like this?

Finally.. any known good sources in the US for fumaric?

}h{
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Faust
#7 Posted : 2/24/2009 3:15:27 PM

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Truth be told I didn't read any of that but I liked your little {h} signing there

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69ron
#8 Posted : 2/25/2009 6:29:34 AM

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Infundibulum wrote:

1. Nothing really seems wrong. But may I ask, where did SWIY buy the fumaric acid from?Which are the specifications of the pruduct? Is there anything else apart from fumaric acid? For instance, if the fumaric acid SWIY used cam efrom the manufacturer with some water (which depending on the product could range from 5% to 0.5% or less, then this trace amount of water could prevent dmt fumarate to precipitate.


I've looked at many a fumaric acid MSDS and even technical grade doesn't contain water.

I don't think you can buy fumaric acid that contains water. It's anhydrous by nature.

If you think your fumaric acid is somehow wet, you must have spilled water on it.

SWIM has that exact same fumaric acid and he tested it. It doesn’t contain any water at all.

This is how you test it. Weigh out 10.000 grams using a very accurate scale. SWIM’s scale is accurate down to +-1 mg. That’s VERY accurate. Put the weighing container in the oven and dry it at 200 C for 2 hours. SWIM did exactly that and then he weighed it. It weighed 10.000 grams.

There’s no water in fumaric acid no matter what grade it is, unless it contains other acids as impurities, in which case they could be hydroscopic and absorb water. But normally the fumaric acid would dry out the impurities present because it hates water, unless the impurities are extremely hygroscopic, it's going to dry them out. That's one of its common uses in the food industry. It's used to keep foods from getting moist.


The water is most likely from the acetone. Unless it's dried fully and kept away from air, it will become wet again. Acetone absorbs water directly from the air.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

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halcyon
#9 Posted : 2/25/2009 9:40:55 AM

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69ron,

Always helpful. Okay, I think SWIM's foafoaf has trouble with his Acetone. Does the description of baked epsom salts are quite crusty but stil beautifully white chunks make sense? In a given quart of acetone (fresh, from hardware store - not reagent) - how many grams would you add of the mag. sulfate to the acentone of uknown water content? 10g or ??

Here is the plan for SWIMs foafoaf (when I can get the infor to him/her/it):

* Test fumaric given your (69ron) procedure
* If all good, get new acetone, dissolve what is likely to be the salted form that precipitated out
* If it dissolves, it is a freebase and will likely need to be re-x'd and then goes through the whole process again
* If it doesn't dissolve, wash with acetone to remove any residual fumaric. Clean and store.

Sound about right?
{h}
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Infundibulum
#10 Posted : 2/25/2009 11:05:41 AM

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Aye, 69ron, SWIY's right. The water content found in fumaric acid's is basically minuscule and not to worry about it.

Thanks for clearing that up!

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
halcyon
#11 Posted : 3/26/2009 4:03:54 AM

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Quick report back from The Telepathic Brazilian Lizard person... must have been that the acetone pulled down some oxygen or free h20 on his/her/it's first salting via Fumaric. He/She/It used the same brand of everything but used quite new (not brand new) Acetone that was dehydrated with Mag Sulfate. Crystals came up right away using this acetone. So, the message from the other side is get that acetone's water content down.

Sorry for reviving an old thread, but the theta waves came...

{h}
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