SpaceshipNelson
Active member
significant losses Jump. . . makes you think twice before using.. .
-
Happy Birthday ICMag! Been 20 years since Gypsy Nirvana created the forum! We are celebrating with a 4/20 Giveaway and by launching a new Patreon tier called "420club". You can read more here.
-
Important notice: ICMag's T.O.U. has been updated. Please review it here. For your convenience, it is also available in the main forum menu, under 'Quick Links"!
It's not clear that that much charcoal per weight of extract was needed. For general decolorization in the lab, the amount of carbon added is usually small. How do we know the 150 mg was THC instead of something else?
The patent's extract getting treated was 12.5x more concentrated, 100 mg/ml ethanol, and this extract was only passed through a column containing an nonspecific mass of carbon.
The patent's extract getting treated was 12.5x more concentrated, 100 mg/ml ethanol, and this extract was only passed through a column containing an nonspecific mass of carbon.
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.......................
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.......................
UNREGISTRD
Active member
Not sure im following you here...Im guessing your saying the only way you could use the gasone or Iwatani is in the closed loop either way cause of the smell?......Cause you still had them both tested??
Mercaptan makes the Iwatani and Gasone unusable, my apologies all around. I'm still going to try filtering it with a turkey baster packed with powdered activated carbon later this week. Can't make much bigger a fool of myself than I already have... ;-)
UNREGISTRD
Active member
Thats what i was thinking..But lost as to why he still had them tested? maybe im the retarded one?
I figure he went ahead and had it tested, figuring I couldn't possibly have missed the stench of mercaptan. Once again, sorry.
Au contraire, you now know what to look for and weren't afraid to experiment. Hard to make a mistake without ever investigating new stuff.
Charcoal won't take it out.
Check out FOAF's post on mercaps in Propane.
https://www.icmag.com/ic/showthread.php?threadid=186573
We are interested in more than one thing. One is what is in the butane, and the other thing is how much.
We are only checking these two to see how much, as we are also doing with lighter butane, as well as n-Butane from industrial suppliers.
Actually it sounds like he came close, he doesn't say how much propane he ran through the filter, maybe less propane/more filter...His testing was also done before everyone had vacuum purging equipment...I just ordered the zeolite/molecular sieve 13x.
I've read these gasses (butane/propane) are stored in bulk with mercaptan added and then the mercaptan is removed with a catalyst before use or blending for distribution, anyone know the details?
"In situations where thiols are used in commercial industry, such as liquid petroleum gas tankers and bulk handling systems, an oxidizing catalyst is used to destroy the odor. A copper-based oxidation catalyst neutralizes the volatile thiols and transforms them into inert products." http://en.wikipedia.org/wiki/Thiol
Works, added four heaping teaspoonfuls of powdered activated carbon/charcoal to one can of Iwatani butane fuel squirted into a Mason jar, covered the jar with 2.5 micron laboratory filter paper, swirled for a minute, and poured off into another Mason jar for boil off. Jar looks nearly clean. ~320ml of butane to start, ~220ml after filtering. The charcoal created a cloud of dense black 'smoke' when I dumped it in, I'm going to wrap it up in a coffee filter and slip it in next time, once the filter paper is in place it's no problem.Previous to the above I tried packing a turkey baster with the powdered activated carbon/charcoal with cotton balls top and bottom and the pressure was too much, liquid butane kept squirting out the top no matter what...but the 100ml or so I got before I gave up was clean as a whistle, no residue or mercaptan, imo. When I get bored I'll get this working also, I'll probably try jump117's suggestion to use crumpled up coffee filters top and bottom instead of the cotton balls and not pack quite so tight. If the government adds mercaptan to all butane there may be a simple work around!
This is what I used,
http://www.amazon.com/gp/product/B0026XWKKM/ref=oh_details_o01_s00_i00?ie=UTF8&psc=1
Here's a picture of the nearly clean jar (~95% improvement imo...)
Attachments
I see there are two main types of diatomaceous earth used for filtering,
http://en.wikipedia.org/wiki/Diatomaceous_earth
"Freshwater-derived food grade diatomaceous earth is the type used in United States agriculture for grain storage, as feed supplement, and as an insecticide. It is produced uncalcinated, has a very fine particle size, and is very low in crystal silica (<2%).
Salt-water-derived pool/ beer/ wine filter grade is not suitable for human consumption or effective as an insecticide. Usually calcinated before being sold to remove impurities and undesirable volatile contents, it is composed of larger particles than the freshwater version and has a high silica content (>60%)."
Food grade,
http://www.amazon.com/Diatomaceous-...sr=8-1&keywords=food+grade+diatomaceous+earth
Pool filter grade,
http://www.amazon.com/Diatomaceous-...r=8-1&keywords=pool+filter+diatomaceous+earth
The food grade is ubiquitous in our lives, can it be used to filter butane? Is 2.5 micron filter paper sufficient?
http://en.wikipedia.org/wiki/Diatomaceous_earth
"Freshwater-derived food grade diatomaceous earth is the type used in United States agriculture for grain storage, as feed supplement, and as an insecticide. It is produced uncalcinated, has a very fine particle size, and is very low in crystal silica (<2%).
Salt-water-derived pool/ beer/ wine filter grade is not suitable for human consumption or effective as an insecticide. Usually calcinated before being sold to remove impurities and undesirable volatile contents, it is composed of larger particles than the freshwater version and has a high silica content (>60%)."
Food grade,
http://www.amazon.com/Diatomaceous-...sr=8-1&keywords=food+grade+diatomaceous+earth
Pool filter grade,
http://www.amazon.com/Diatomaceous-...r=8-1&keywords=pool+filter+diatomaceous+earth
The food grade is ubiquitous in our lives, can it be used to filter butane? Is 2.5 micron filter paper sufficient?
I decarboxylated at ~250F the oil I extracted using the "$1.25/can" Iwatani butane fuel, seems to have purged the mercaptan down to threshold levels. I had tried vacuum purging it at 135F and -29.5" Hg for several hours, even took the vacuum all the way down at the end, and once in the jar it still stank...
http://skunkpharmresearch.com/decarboxylation/
Not suggesting the decarbed 'crude' for vaping, though I tried it, and it's not bad, but how about for oral consumption? Wouldn't this even with the little bit of Mystery Oil and whatever mercaptan's left be way cheaper and possibly safer than hexane (or ???) for many purposes other than vaping? Surely it's better than naptha...
For decarbing I placed the oil in a small flat bottomed jar (imagine very small beaker,) which went into a turkish coffee pot with just enough olive oil to float the jar. Nifty how the coffee pot sits right on the burner.
To the ~3 grams of cooled, yet warm, decarbed oil I mixed in a little olive oil, three drops of cinnamon bark oil, and two drops of myrrh oil. Took about fifteen minutes of stirring, but seems a stable solution even after being in the refrigerator. A very strong, up effect, made from something I'm not familiar with, described as Jaguar MJ13. I'm not saying this is safe, no real risk assessment has been done, I'm just some old fool trying to see for himself what it would be like if a third world'er blasted his herb with the household propane. ;-) Hey, maybe he needed it for someone dying, and there was no other option.
http://skunkpharmresearch.com/decarboxylation/
Not suggesting the decarbed 'crude' for vaping, though I tried it, and it's not bad, but how about for oral consumption? Wouldn't this even with the little bit of Mystery Oil and whatever mercaptan's left be way cheaper and possibly safer than hexane (or ???) for many purposes other than vaping? Surely it's better than naptha...
For decarbing I placed the oil in a small flat bottomed jar (imagine very small beaker,) which went into a turkish coffee pot with just enough olive oil to float the jar. Nifty how the coffee pot sits right on the burner.
To the ~3 grams of cooled, yet warm, decarbed oil I mixed in a little olive oil, three drops of cinnamon bark oil, and two drops of myrrh oil. Took about fifteen minutes of stirring, but seems a stable solution even after being in the refrigerator. A very strong, up effect, made from something I'm not familiar with, described as Jaguar MJ13. I'm not saying this is safe, no real risk assessment has been done, I'm just some old fool trying to see for himself what it would be like if a third world'er blasted his herb with the household propane. ;-) Hey, maybe he needed it for someone dying, and there was no other option.
Attachments
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 has 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.
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 has 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.
UNREGISTRD
Active member
25% of the manufacturs stated level is pretty good IMO...NIce work GW..
Just wanted to mention here that I have purchased "Gasone 5x" which comes in the standard 300ml can size and it passed the (admittedly very crude) smell + mirror residue test. It actually smelled like *nothing* to me which was a very pleasant surprise because a master case of 96x300ml was $120.
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.
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.
Attachments
Me too!
10-7-13
The moment some of ya'll have been waiting for has arrived, with the actual ppm residual contaminants in butane, by some of the common brands, as well as a couple not commonly used for butane extraction for comparison.
No hoopla or fanfaronade, just the actual ppm residuals by brand, as measured by a certified third party analytical lab.
Note that the ppm in the Gasone and Iwatani include Thiol mercaptans for leak detection. Thiols are alcohol analogs, where the oxygen atom is replaced by a sulfur atom and adds a garlic odor.
Note that the highest ppm found in any brand was 7% of their certified maximum of 50 ppm.
Also note that except for Lucienne, these were single can grab samples, and Lucienne is only two different lots, so the differences between brands, especially by the same refiner, may even out. IE: Lucienne and Newport.
They may not too, as the same refiner doesn't necessarily mean the same refinery, which could also account for the differences.
So now that we have two bits of empirical scientific data, derived by a certified third party lab, instead of the anecdotal information on Facebook and the web that we started with, lets do the math to put this in perspective.
The previous part per billionth analysis showed 1,4 Dichlorobenzene at a combined total level of 55 parts per billionth, or .000,000,055. We all agree that we want no part of 1,4 Dichlorozenzene, because it has been declared a carcinogen, and given a low TWA CEIL of 110ppm by NIOSH.
http://www.sciencelab.com/msds.php?msdsId=9923722
55 parts per billionth in the concentrated residual itself, is 2000 times smaller than 110 parts per millionth TWA Ceiling imposed by NIOSH.
It will in addition be further diluted in an extract, considering that at the worse case total residual contaminant found was 3.5 ppm, besides being dilute in the extracted oil itself. Lets look at that math.
.000,000, 055 X .000, 0035 = .000,000,000,000,192 or 200 parts per quadrillion in the butane used for extraction.
Assuming a 40 gram trim extraction, using 300 ml of butane, and yielding only 10%, 300 ml butane would deposit .000,000,000,058 ml of 1,4 Dichlorbenzene in 4 grams of concentrate.
.000, 000, 000, 058 ml X 1.2475 gms per ml = .000,000,000,072 grams of 1,4 Dichlorobenzene in 4 grams of concentrate.
.000,000.000,072 grams divided by 4 grams =.000,000,000,018 or 18 parts per trillion.
110 ppm TWA Ceiling (.000, 110) divided by residual 1,4 Dichlorobenzene level of 18 parts per trillion (.000,000,000,018) = 6,111,111 or about one six millionth (1/6,000,000th) of maximum allowable exposure level.
4 grams of oil will produce about 20 200 mg hits, so each hit would be about 1/20th of 1/6,000, 000, so exposure per hit would be about 1/1,200,000,000 of the 110 ppm maximum.
Soooo, now that we have put things in perspective, where do we go from here?
We are planning some more testing of different brands and sources and further refined testing of all the evil spirits, but we have come far enough to know that while we would prefer to not have the unwanted contaminants in our butane, its presence is thousands, or even billions of times below published levels of concerns by health professionals.
We've also learned that it is easy to remove, using a cold trap and a refrigerant recovery pump, so those of you with the required equipment can take it out, making the point moot.
That is what we now do, because we can, but continue to use the oil we produced before we started fractionally distilling the butane.
The moment some of ya'll have been waiting for has arrived, with the actual ppm residual contaminants in butane, by some of the common brands, as well as a couple not commonly used for butane extraction for comparison.
No hoopla or fanfaronade, just the actual ppm residuals by brand, as measured by a certified third party analytical lab.
Note that the ppm in the Gasone and Iwatani include Thiol mercaptans for leak detection. Thiols are alcohol analogs, where the oxygen atom is replaced by a sulfur atom and adds a garlic odor.
Note that the highest ppm found in any brand was 7% of their certified maximum of 50 ppm.
Also note that except for Lucienne, these were single can grab samples, and Lucienne is only two different lots, so the differences between brands, especially by the same refiner, may even out. IE: Lucienne and Newport.
They may not too, as the same refiner doesn't necessarily mean the same refinery, which could also account for the differences.
So now that we have two bits of empirical scientific data, derived by a certified third party lab, instead of the anecdotal information on Facebook and the web that we started with, lets do the math to put this in perspective.
The previous part per billionth analysis showed 1,4 Dichlorobenzene at a combined total level of 55 parts per billionth, or .000,000,055. We all agree that we want no part of 1,4 Dichlorozenzene, because it has been declared a carcinogen, and given a low TWA CEIL of 110ppm by NIOSH.
http://www.sciencelab.com/msds.php?msdsId=9923722
55 parts per billionth in the concentrated residual itself, is 2000 times smaller than 110 parts per millionth TWA Ceiling imposed by NIOSH.
It will in addition be further diluted in an extract, considering that at the worse case total residual contaminant found was 3.5 ppm, besides being dilute in the extracted oil itself. Lets look at that math.
.000,000, 055 X .000, 0035 = .000,000,000,000,192 or 200 parts per quadrillion in the butane used for extraction.
Assuming a 40 gram trim extraction, using 300 ml of butane, and yielding only 10%, 300 ml butane would deposit .000,000,000,058 ml of 1,4 Dichlorbenzene in 4 grams of concentrate.
.000, 000, 000, 058 ml X 1.2475 gms per ml = .000,000,000,072 grams of 1,4 Dichlorobenzene in 4 grams of concentrate.
.000,000.000,072 grams divided by 4 grams =.000,000,000,018 or 18 parts per trillion.
110 ppm TWA Ceiling (.000, 110) divided by residual 1,4 Dichlorobenzene level of 18 parts per trillion (.000,000,000,018) = 6,111,111 or about one six millionth (1/6,000,000th) of maximum allowable exposure level.
4 grams of oil will produce about 20 200 mg hits, so each hit would be about 1/20th of 1/6,000, 000, so exposure per hit would be about 1/1,200,000,000 of the 110 ppm maximum.
Soooo, now that we have put things in perspective, where do we go from here?
We are planning some more testing of different brands and sources and further refined testing of all the evil spirits, but we have come far enough to know that while we would prefer to not have the unwanted contaminants in our butane, its presence is thousands, or even billions of times below published levels of concerns by health professionals.
We've also learned that it is easy to remove, using a cold trap and a refrigerant recovery pump, so those of you with the required equipment can take it out, making the point moot.
That is what we now do, because we can, but continue to use the oil we produced before we started fractionally distilling the butane.
Attachments
