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Long-term RC storage

Damn, that's a great analogy about mixing water with milk (although I think they are closer in density than argon and air), but I hadn't thought of it that way. I think you are correct in that they will diffuse into each other rather than the argon completely displacing 100% of the air.

However, I'm with entho in that if I can displace a large percentage of the air, and seal it in air-tight vials, I will be happy. I don't know what else I can do, considering my lab is my kitchen, my skill comes from chemistry classes over 30 years ago, and my equipment is homemade.

I'll tell you what though - this discussion has improved my chances of success immeasurably. My hat is off to everyone that provided such valuable suggestions throughout this thread.

One other cautionary - since I will be doing a fairly large quantity of vials, it will probably take several hours. I plan to elinst the help of a trusted fellow. I think the buddy system is definitely in order if you''re going to be working around something that displaces oxygen. Especially since part of the design criteria is to work over a fairly large mouthed container with as little fresh air currents as possible.

At least we don't have to worry about explosions.......that's something. :)
 
i think you're trying too hard. CO2 is very easy to make in large, low pressure quantity (to avoid the puff of powder issue) and displaces air just as well. either use dry ice (added benefit: the cold gas falls even quicker to the bottom of your container) or use vinegar and baking soda like the 2nd grade science fair. if you mix up a big enough vat of it you can literally pour the heavy gas off the top of the reaction mixture. but don't take my word for it... try it yourself! (bill nye)

easiest would probably be to set up a large bucket (5 gallon jug), place several chunks of dry ice at the bottom, add a rack or screen for holding your vials, place all vials on top of the dry ice, wait for CO2 to push all the air up and out of the bucket (non-sealed lid would ensure no stray currents) and then seal all the vials. no need to top off with the wine thingamajig.
 
In Jwndy's large batch situation - its sounds as though you are on to something.

Good deal - I get to show my ignorance of chemistry. 8)
Would not the dense vapor of dry ice obcure one's vision and therefore preclude filling the vials while in the iced bucket? And if so, wouldn't filling the vials with powder prior to gas treating/capping leave some air trapped in the powder itself?
And now for the really stupid questions...
What is the greater enemy here - "air" or "oxygen"?
If the culprit is oxygen - is there not oxygen in CO2? (Isn't that what the "O" means?) Or is the oxygen only damaging to the compound in it's pure form?
And if it is only destructive in it's pure form - why is it destructive when in "air" -but not in CO2?

Oww...asking even the stupid questions makes my head hurt. :o

Like I said - I barely passed high school chemistry - true story. It was extremely embarassing because my oldest brother has a PhD in chemistry, was a high school chemistry teacher his entire working career - head of the department in a large high school, no less. That's part of the great irony of this entire situation. If these RCs had come along thirty years ago - when we were both much younger and I was still the well-known black sheep of the family - he might have clued me in on how to do this process. Now that I'm older, wiser, more "respectable" and finally "did something with my life" - he would be horrified that I would even ask him the questions in the first place. :\
 
Here's the blind leading the blind, but.........

I think it gets into the chemistry equations. C + O2 = C02 and the valence (or electron) shells are all full. It takes some energy to split CO2 back out into C and O2.

We know from reading about oxidation of our favorite chemicals, and seeing rust on all those metal things we forgot to paint, that O2 by itself likes to react with lots of stuff without needing a lot of energy.

So once you "marry" the O2 with something it really likes, it takes a lot to get a "divorce" so it can go after your JWH.

I'm sure all the professional chemists and even kitchen chemists reading this are laughing at my simple analogy, but hopefully they can provide a more educated explanation.

I think you are right on with the fog created by the dry ice being a problem obscuring your vision, not to mention that it will get damned cold if you are sticking your hand in it filling vials for any period of time, but I appreaciate the discussion of alternative methods.
 
I hardly think you're counted among the blind here. I'm confident they're laughing harder at my question than at your answer. But I actually think I might understand a bit of it. The oxygen is so firmly bonded to the carbon that in the joining it is therefore rendered inert - more or less?

I gotta take another aspirin...
 
I just ordered a case of vials, but I think I screwed up. I got the 5/8 dram, clear, with Polyseal cone caps (the only place I have seen this trifecta), but I just noticed the neck opening size was 7.6 mm. I am hoping this is a typo because in 3 days of searching, I have not seen a single 5/8 dram vial that didn't use a 13/425 cap. I think the 13 stands for the OD of the neck. I also haven't seen clear 5/8 dram vials with cone caps. I've seen every other combination under the sun (lots (and lots) of amber vials with cone caps, but no clear). Don't these people know that if you are going to freeze something for years, you aren't worried about light, and you would like to be able casually observe if your powder is changing color??

I guess I should have gone ahead and ordered them seperately, but I only found cone caps at certain places and I only found clear 5/8 dram vials at other places. I kept looking because I just knew that somewhere there was someone that had put this combination together.

I know this is just a little off topic, but sometime you just have to rant.

To BanE: I tried responding to you but bluelight won't let a green lighter like myself send (or respond) to private messages, and I don't know how to achieve bluelighter status. I have found at least 4 reputable sources. If you go over to the Synthetic Cannabinoid Discussion thread at synchronium, they have recently been discussing one of the 4 I am talking about. If you search their old thread (JWH toxicity), you will find another one (starts with Res and ends with Chems).
 
Whew.......I just bought a 5/8 dram vial with the size opening I had been seeing on the amber vials at probably the only store in a 50 mile radius that sells that sort of thing around here (for $3!! each - man, 144 of them only costs about $50).

I just measured the ID, and it came out to 7.6 mm (and the OD was 12.5 mm).

All is right with the world again.
 
Here's an interesting site of a guy filling up a fish bowl with argon. The video is the third one (on the far right), entitled explanation.

http://amasci.com/tesla/heli1.html

He uses a tesla coil to test the argon boundry (I still think a match would work - especially if you don't have a tesla coil laying around), and he uses an aquarium stone to keep the argon from coming directly out of the hose and stiring up the air.
 
It looks interesting - I'm looking forward to having AT&T complete setting up the 3g wireless service here so I can actually view the video.

I'm quite glad to hear your vial/cap dilemma worked out. I feel quite fortunate that my small cache of vials only cost me 50 cents apiece.

And it's my understanding that bluelight status requires 50 posts. Gradually - we're getting there.
Which brings me to another stage in the planning of this process. As you and I seem to be the ones with the most immediate interest in this undertaking it would perhaps be best for us to communicate via PMs - but we're not there yet. Soo...I'll just briefly outline what I have in mind and do a little out-loud thinking.

Once filled with argon and product and then capped, I plan to place each filled vial in its own separate small ziplock bag. The individually bagged vials would then be placed in a foam-lined hard plastic case (not airtight), but the case would then be placed in (at least one) gallon ziplock freezer bag. By packaging each sealed vial separately I would be able to open the case and remove a vial at a time when needed - leaving the others undisturbed - and also unaffected by the brief - but necessary - light condensation that will form on the outside of each of the other individual vial bags when the case is opened. But the vials themselves would not be exposed to the condensation.

When product is to be accessed for preparing doses the vial is removed from its bag and allowed to reach room temp before opening (a critical step I understand). When the required product has been removed - prior to capping - I "may" be able to ever-so-carefully puff argon over the top of the vial before recapping and returning it to the bag/case for re-freezing. Ethanol solution will be made up in large enough batches to allow relatively infrequent access to the sealed vials and the solution will then be stored in the freezer as well.

I know the packaging process will seem to be overkill to some - but I live in a very humid environment and every instant the compounds are exposed to any level of moisture it may accelerate degradation. I tend to fear the moisture as much as I do the oxygen, heat and sunlight.

The somewhat elaborate packaging process would not be as practical for larger projects - but for my small-scale undertaking it, again, appears to be the best I will be able to do.

Now if I can just secure the funds for a medical freezer I should be set to proceed - but that will be a while yet.
 
Jwndy said:
He uses a tesla coil to test the argon boundry (I still think a match would work - especially if you don't have a tesla coil laying around)
Click to expand...

Cheap indicators exist which change colour reversibly in the presence/absence of oxygen, I'm not sure how suitable they would be though.

The idea of a visual indicator which actively absorbs oxygen appeals to me, but a match wouldn't re-ignite itself spontaneously with oxygen levels in normal air, everything I could think of involved heat or other byproducts that would interfere with the inert environment...

I found this paper quite interesting:

Oxygen indicators and intelligent inks for packaging food
Andrew Mills, Chem. Soc. Rev., 2005, (12),1003-1011
DOI: 10.1039/b503997p

The detection of oxygen using optical sensors is of increasing interest, especially in modified atmosphere food packaging (MAP), in which the package, usually containing food, is flushed with a gas, such as carbon dioxide or nitrogen. This tutorial review examines the ideal properties of an oxygen optical sensor for MAP and compares them with those developed to date, including the most recent advances. The basic technologies underpinning the different indicator types are described, examples given and their potential for application in MAP assessed. This tutorial review should be of interest to the MAP industry and researchers in optical sensors and oxygen sensing.
 
to be honest, i'm not convinced that there is anything in the JWH series structure that indicates a susceptibility to oxidation.

the reference to 'indole is easy to oxidize' was by a strong chemical oxidizer that can oxidize anything by free-radical addition. and the addition was at the 3-position of indole, which is already occupied by the napthoyl group in a JWH compound.

recall that freebase DMT is apparently very stable for months under standard handling conditions, and does not appear to change color or lose potency when heated to its vaporization temperature.

JWH compounds are probably not susceptible to increased degradation in moisture (H2O) because they are completely insoluble in H2O to begin with due to their highly lipophilic (oil-liking) nature.

i'm willing to bet $20 that one gram of JWH-018 stored in a clear glass vial under plain air (21% oxygen) for twenty years at room temperature will show no noticeable degradation or loss of potency.
 
greenmeanies said:
to be honest, i'm not convinced that there is anything in the JWH series structure that indicates a susceptibility to oxidation.

the reference to 'indole is easy to oxidize' was by a strong chemical oxidizer that can oxidize anything by free-radical addition. and the addition was at the 3-position of indole, which is already occupied by the napthoyl group in a JWH compound.

recall that freebase DMT is apparently very stable for months under standard handling conditions, and does not appear to change color or lose potency when heated to its vaporization temperature.

JWH compounds are probably not susceptible to increased degradation in moisture (H2O) because they are completely insoluble in H2O to begin with due to their highly lipophilic (oil-liking) nature.

i'm willing to bet $20 that one gram of JWH-018 stored in a clear glass vial under plain air (21% oxygen) for twenty years at room temperature will show no noticeable degradation or loss of potency.
Click to expand...
I've used jwh-018/073 blends merely stored at room temp in plastic sealed bags (or the reseable original container) that have retained full potency after two years. Seems subjectively reasonably stable.
 
I also live in an extremely humid part of the country. I just mixed up two batches of 018/073 (.5g ea in 375ml Everclear) this weekend - just to try the stuff out. My full post is over at synchronium, but the essence of the experience, at least for this discussion was my observation of the powders. First I chilled the house down to about 70 to get some of the moisture out, then I opened up the packages and weighed them out. I tied 4 separate powders from 2 suppliers. In all cases, the powders looked extremely stable (i.e. didn't look like they had a tendency to clump - unlike many other powders that we might have run across in our lifetime) in the presence of humidity. I have a feeling that as long as we can still get the pure stuff from a lab (i.e. without 3rd part cut on it), then the brief exposure to humidity we will experience when accessing the product from the freezer is probably not all that big a concern.

I too am using the multi-vial approach, and I will seal each with argon (my wine preservative kit came today). I found some really good ceramic jars at Bed, Bath, & Beyond that had wire clamps to hold the lid and its silicone seal against the jar. They had a 6-pack of these jars (all different sizes and all brown) for $19.99. I plan on just filling them up with vials, clamping the lid down, and putting it in the freezer. When I open one of the ceramic jars later on, I plan to do it inside the environment of the freezer (just a regular stand-up type, although I have a chest type too), but I am not going to take great precautions to prevent no moisture from getting inside. Hopefully, if I open the jar fast enough while still in the freezer, not much moisture will get into it anyway. My 5/8 dram vials only hold about .5g each (tried to stuff a g in one, and there was no way it would fit - it was full at .8g of JWH018). From what I have been reading, I think it would keep for a year or so at room temperature in the vial.
 
If you can see the green blinking eyes in my previous post, I have no idea how it got there, and I could not delete it and still leave the chemical name in. For some reason it turned the eight into one of the green symbols. I appologize.
 
morninggloryseed said:
It's worked fine for me. I know CO2 can form salts with some compounds, but so far I've not seen any evidence of that happening. The most delicate compound I have (besides LSD) is that old batch of 4-Ho-DET from 2001 (the infamous 'black gooey stuff' that turns to goo when exposed to oxygen) and and the 'hygroscopic' 4-AcO-MiPT that is also known to goo up when exposed to air...but both of those have remained crystalline compounds...They both have darkened somewhat but has not turned to goo.
Click to expand...

I can confirm that, mine have darkended over time and are still as good as i remember.

Being that they are stored somewhat in the same manner as morninggloryseed
Cheers
 
Instead of blowing argon into some kind of an open box, risking to powder your desk and living room with precious material, I'd recommend the following:

1. Put the vials in a dessicator or other vacuum resistant vessel, lids almost but not totally closed (for pressure equalisation).
2. Evacuate the vessel. Low-tech method of choice would be an aspirator.
3. Vent carefully with the aid of an argon-filled ballon.
4. Repeat the evacuation/venting-cycle about 4-5 times. The more often the better.
5. After opening the desiccator, close all lids immediately.

This should ensure minimum oxygen content. Store all vials in the freezer and you are safe with most drugs for centuries.

Final note: I recommend to seal several vials with a smaller amount of the same compound in contrary to one single vial with a larger amount. By this you don't need to thaw the whole charge at once but just as much as you need at a single instance.


PEACE! Murphy
 
Excellent references to the dessicator and aspirator. Thanks for including the hyperlinks. A picture is worth a thousand (more) words.

The only limitation with the dessicator approach is that you will have to fill the vials in the normal atmosphere because the dessicator looks too small to put both hands in to fill the vials. If I fill the vials first, then put them in the dessicator, then I worry about not being able to displace the oxygen trapped inside the vial. However, it would probalby be easy to adapt the concept to a large, deep plastic storage box. You could then remove the lid and put the scales, vials, etc in the bottom of the box and weigh the powder and fill the vials working completely within the box.

One interesting thing I found - there is a problem trying to pour .5g amounts of powder into the necks of small vials. To solve this I found that they sell very small funnels at many home decor type stores. Again, I found mine at Bed, Bath, and Beyond for a couple of bucks. I cut some of the bottom out of the funnel to give it as wide an opening as possible, but so it is still long enough to fit into a 5/8 dram vial without going down past the bottom of the neck. Even after cutting the bottom out of the funnel, I still had problems getting the JWH-018 to evacuate the funnel. Thumping on the side didn't help much. To solve this, I found a long sewing safety needle and used it to stir the 018 until it fell through the funnel. I didn't have this problem with the 073 - it fell through the funnel without needing to stir.
 
The vials get filled first, then placed in the desiccator. It is unproblematic that the samples have contact with air at that stage.

Lids have to remain slightly open (2-3 mm is enough) to ensure that absolute everything gets evacuated. If you completely close the lids at that point, your vials will pop up (and probably tilt over) upon evacuating the system due to internal overpressure.

Upon repeating the evacuation-venting-cycle several times all oxygen gets removed for sure.

This method is safe, reliable, reproducible and after all: Comparably cheap (provided that one can afford a desiccator and argon; aspirators should not cost much).


PEACE! - Murphy
 
There are some otehr posts in this thread that talk about how to manufacture your own CO2. Other people think it will be just as good as argon. I like argon because everything I've read indicated it is super stable, and it is really cheap at welding supply houses. It is a basic element on the period table and a "noble" gas that doesn't really react with anything.

I'm sure CO2 would work too. It doesn't react with much of anything either.
 
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