Mystery Oil in Butane

A brother posted notice of finding a Mystery Oil in canned butane, so we decided to check and see what it was. To do so, we fractionally distilled 21.3 liters of Lucienne 4X under vacuum, and sent the .158 grams of mystery oil collected to a third party lab with a mass spectrometer attached to their gas chromatograph. Total oil collected was about 15 ppm.

We also cut the cans apart to see what remained in them and they were spotless inside.

I've attached a copy of the labs summary and am still working my way down the list, pulling up the MSDS sheets, starting with the items of concern.

The first thing to keep in perspective, is that the total oil was 12 ppm from 21.3 liters, so the PPM in the study should be divided by 1,000,000 and multiplied by .000,012, to get the concentration.

That concentration number X 1,000,000 will give you parts per millionth.

In summary, there were simple Alkanes present as long as C-16, which are not of concern at the levels present.

In addition there are aromatic Alkenes present, that are of serious concern, but not at levels remotely close to exposure limits.

The concern with those Alkenes is really not reaching toxic limits, but the fact that some are known carcinogens, mutagens, teratogens, etc.

IE: Cyclohexane, isocyanato, which most likely came from the gaskets and seals used in the cans and process, because it isn't found naturally in butane.

Nasty bad shit, with an no exposure limits established and an intravenous LD-50 mouse of 13 ppm and present at the level of .000000001728 concentration, or .001728 parts per millionth. That is about 7500 times lower than the LD-50.

Another bad nasty present was Benzenamine, 3,5, at the levels of .035778 parts per millionth, with a Permissible Exposure Limit of 2 ppm TWA for 8 hours. That is only 56 times lower than PEL, so of more concern.

Benzene 1,1 showed up at a concentration of .000000003678, or .000003678 PPM, with a Permissible Exposure Limit of 110 ppm TWA 8 hours. That's .00000334% of PEL.




I could go on, but it will take me awhile to pull MSDS sheets for the whole list, so I've attached the raw data. Sorry the quality isn't better, but the original is barely readable and this was copied at 1200 bit resolution

Even if nothing is present at levels of serious health concern, I would prefer to not have any of that stuff in there, so in addition to fractional distillation using vacuum, we will be experimenting with Bentonite filters.

Wow, scary and good to know. Sounds like you really know your crap too, distilling butane, gnarly.

Love readin ur post fadedawg, getting info to the masses! I dig!

Great, and I liked Lucienne
Butane is pissing me off, hexane for now on

Texas(THC) said:

Great, and I liked Lucienne
Butane is pissing me off, hexane for now on

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oh come on. he emptied like 20 cans and found something 7500x lower than the ld50.

with your typical 3 or 4 can run, youre looking at amounts that are 10,000x lower than the PEL/LD50. you do more damage to your body standing at a gas station for 2 minutes while you fill up, or crossing the intersection downtown and breathing in car fumes.

hell of a post fadedawg. "sounds like he knows his crap" is an understatement. this guy is serious stuff!!!!!!! I love it.

Ya I understand that I just am getting disgusted with info like this. Especially since that was my go to brand.
Either way I'm sure hexane is still a overall cleaner solvent and i would feel safer using it.

Thanks for the info fade dawg, keep it coming

would be very interesting to see the same test done with other brands of butane, as well as everclear, and 99% ISO, and hexane, etc....

I say we should start a fund and send the cash to fadedawg... those experiments cant be cheap. near 200$ I bet outta his own pocket for this one. thanks again FD.

vacpurge said:

would be very interesting to see the same test done with other brands of butane, as well as everclear, and 99% ISO, and hexane, etc....

I say we should start a fund and send the cash to fadedawg... those experiments cant be cheap. near 200$ I bet outta his own pocket for this one. thanks again FD.

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Thanks for the good thoughts, and once we get this test run to ground, we may test other brands and solvents.

What made the test less expensive for SPR, is that Skyhighler bellied up to the bar and subsequently sent the cost of the tests, so deserves part of the kudos and accolades.

It takes the better part of a day to vacuum distill 21 liters at low temperature and deliver the samples to Clackamas, Or, where the lab is. It cost $130 for the butane and $250 for lab analysis. The lab fee is a constant, but the cost of the butane itself can vary.

The good news of course, is that the butane is also subsequently available for extraction, so some of the costs are recovered. We will in fact have to use some up, to have an empty 50# recovery tank for further testing, as all four of ours are currently filled.

That brings us to re-distilling the butane a second time to check for contaminants and testing different filtration absorbents, which really should start with a brand new clean 50# tank, to eliminate any possibilities of cross contamination, so I've ordered a new one for that purpose.

We are also sharing the technical details with other labs who request it, so hopefully this new insight will start a flurry of testing by others, who will likewise share. The best of all worlds, because no one can fudge the results. Hee, hee, hee....................

The good news, is the ball is rolling and now has enough momentum that no one will ever get it back in the bag without the issue being resolved.

I nominate FD for president...

Lol..
I know I've said this many times, but seriously, thank you for your diligence in this regard.

Is this the same” mystery oil” that was found to be in Vector?

Also.. I've been reading up on SToK.. The dispensaries local to myself are now carrying this particular brand of butane..
It runs about 10-20$ a can depending on who you know.

The label reads... Can't recall the exact number but..it said
” 98.5% N-Butane”...that may be higher or lower...

What's that again about short term memory?...lol

I've only purchased one can, and ran about 14 grams of Chem-Dawg91..

Yielded just about 20%..

Sirdabsalot462 said:

The label reads... Can't recall the exact number but..it said
” 98.5% N-Butane”...that may be higher or lower...

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haha cant remember is right!! it says 99.995% BIG difference than 98.5%

Whoops, just went and grabbed the can...
I was mistaken...
It claims 99.995% pure N-Butane.
See pic..


I still got this can 3/4 of the way full, going to run about 20 grams pretty soon, will report back.

Fadedawg said:

Thanks for the good thoughts, and once we get this test run to ground, we may test other brands and solvents.

What made the test less expensive for SPR, is that Skyhighler bellied up to the bar and subsequently sent the cost of the tests, so deserves part of the kudos and accolades.

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ive been thinking about it. and if and when you do perform another experiment like this where you test BHO stuff. I would be willing to chip in and pay for something like Skyhighler did. 100$ or so not a problem!

I'm back and will get back on the analysis. Here is a second summary sheet of things present in Parts Per Billionth. It isn't sequentially numbered and I originally thought they were included in the PPM list.

Ignore the redacted lines, as they are the carrier solvents used for the analysis.

I appreciate all the offers to assist financially and am temped to set up a donation fund to do more extensive testing by brand. Perhaps ask the suppliers to donate the butane for testing.....................

Let's see where we end up on the first analysis, before we decide how to proceed.

Two things that are obvious at his point, and that is that the mystery oil is easily removed with vacuum fractional distillation, as evidenced by this experiment, and the second is that the Lucienne 4X is actually 99.999985% pure at 15 ppm. They claim to be below 50 PPM, so that is 99.999950% purity level.

The major difference being that when they are rating Research grades of n-Butane, they also consider propane and isobutane contaminants, while most lighter butanes use a mix of them and consider the heavier waxes and oils the contaminants.

The third point of confirmation that I'm seeking, is that nothing is in the two page summary that is at toxic levels, and so far that continues to be the case.

OK, I dropped off a new sample of Lucienne in the can at Specialty Analytical, as well as two cans each of Skyhighler's Iwatani and Gasone brands for ppm testing. I expect the results by Friday, which will be third party and should cut through any concerns about my accuracy.

Cost per run was $75/ea, so I limited it to these three brands, with double tests on the Lucienne. We will test other brands of interest at a later date, after we see what we get with these tests.

I discharged a can of Gasone and Iwatani into a bain marie for a sniff test, and they both definitely have mercaptans added, so even if they are ultra low residual, our sensory threshold for ethyl mercaptan is 2.8 parts per billionth., and the final oil would taste and smell of it.

Damn nice flame though! I also ordered a Iwatani creme brulee torch head on sale, and it works better than my propane plumbers torch.

Hee, hee, hee thanks Skyhighler for setting me up with a slick new dabbing torch and more than a years supply of butane for it!

Although I wasn't able to get the same lot of Lucienne that I tested before, because I picked up the last 6 pack at the distributor, I was able to get two different lots of Lucienne from a store shelf, so we can test for control. If they are all significantly different, it will support an out of control process theory.

I also talked to Marty about how we could further refine the tests on the items of interest, specifically just the compounds that that are considered evil spirits, despite their low levels. He is reviewing the list and costs for individual standards and we will discuss further later this week.

More to be revealed.......................

This thread should be a sticky

Wow. Great info. Subbed.

Solly that local storms took out the power, so my third party analytical lab is running behind on the samples I dropped off, but they do have the ppm results from the first can of Lucienne.

300ml Lucienne left 1.38 mg of contaminant. Butane weighs about .579 g/ml, so 300 ml weighs about 173,700 mg.

1.38 mg/173,700mg, equals .0000079, or 7.9 ppm.

They still have a third different lot of Lucienne to run, to pick up a third point of reference, but thus far, the Skunk Pham Research lab results on the first lot and Specialized Analytical's results on the second, are within sample error, besides being below 25% of the manufacturers stated maximum contaminant level of 50 ppm.

The third reference sample has yet to be run, but unless it is out, there is no evidence supporting at least Lucienne running out of control.

The lab also have some stove butane to test, and I've picked up cans of Vector, Powers, and Newport for testing, which I will drop by when I pick up the rest of the results on the others.

I am trolling for Colibri and have located some Ronson, but haven't picked it up yet.

When I pick up the test results, we will also discuss which tests and standards are called for, to put the issue to bed once and for all.

any updates? i need a new case of tane asap and im not sure if i should buy lucienne or newport

408isthebay said:

any updates? i need a new case of tane asap and im not sure if i should buy lucienne or newport

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Not yet and I am checking with them daily, because my Mk V fabricator is in Oregon City, which takes me within a couple of miles of their lab on the way home. They are still slammed recovering from the power loss, due to a storm.

Last check was last night and last promise was this morning. I too wait with bait on mah breath!

10-4-13

Still awaiting lab results for the last three, but did get the results for two different lots of Lucienne, as well as Gasone and Iwatani.

The nice lady in the office and I miss-communicated earlier in the week, and I incorrectly reported the last Iwatani results as Lucienne. Even the ppm is incorrect, as the Iwatana cans are 394 ml instead of 300 ml.

That aside, and cutting to the chase, here are the correct Parts Per Millionth residual contamination, after evaporating away the butane, as reported by a certified third party analytical lab, for the first three brands,

The, balance of the information on other brands to follow, ostensibly Monday:

On the subject of refining our search, Marty ordered the standards required to further investigate the aromatics detected in the ppm range, as well as the cyanide compound in the ppb range.

More on that after the standards arrive and more experiments are conducted.