HTFSE(high terpene full spectrum extract)

Gray Wolf said:

It was printed on the opening page, touting it as a "better way", because it avoided cross contamination between runs.

They don't give an address, but are marketing in CA.

The problem with lighter gas sources, is that they aren't held to the same standards as reagent grades, so their quality can and does vary more.

Mystery oil sensing becomes a little like tasting the tea bag in tea, once you recognize it, after a while it jumps out at you from then on.

At sensory thresholds, it ostensibly isn't toxic, but can detract from the quality of the extract, and since SPR is a medical research organization, we have concerns for folks with compromised immune systems and damaged livers, etc.

We start with 99.5% Instrument grade, which so far consistently analyzes 99.9%, but are still able to wipe a film of mystery oil from the distillation pot after re-distilling.

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It's my opinion the percentage of mystery oil per dab is so little it's odor is entirely masked by the scent of the terpenes.

But, though the amount of mystery oil per can of butane refill is of a fairly tight range with no outliers, the smell and tint does vary radically, from near zero odor to nasty hydrocarbon funk, and from clear to a yellowish tint. When I made my best to worst canned butane list I based it on amount of mystery oil not the smell or color. If you're concerned about smell and color I include that info with each post of my testing, just search the thread for the brand you're interested in, generally speaking, the Korean brands are the smelliest with the most yellow tint. I started my testing before finding the ICMAG Concentrate Forums so not all of my individual test results can be found here... here's the thread with everything concerning the mystery oil from the beginning,
http://www.tokecity.com/forums/showthread.php?51333-Lube-inside-canned-butane-Mystery-Oil

SkyHighLer said:

It's my opinion the percentage of mystery oil per dab is so little it's odor is entirely masked by the scent of the terpenes.

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Depending heavily ostensibly on the amount of which mystery oil, as well as which terpenes present.

Some of the butyl/fishy mystery oil is pretty gross and unless it is a regulated and tested grade, the quality can vary considerably over time.

IE: The bad batch of R600/290 Ecogreen refrigerant, where users on this forum reported having to toss their extractions.

Taste is where my aged and battered (gustatory) senses notice mystery oils presence.

Both of my younger Skunk Pharm Research Partners affirm that they also can taste its presence, soooo, even using reagent grades, we always pre-distill.

If this is so... it's night and day, the mystery oil is easily detected with unaided senses when taking a dab, and I have a question for you, and the entire community, why isn't testing for mystery oil done when certifying oil for the MMJ and recreational cannabis markets?

That's just a rhetorical question as far as I'm concerned, as I've already inquired pointedly and repeatedly of Steep Hill and SC Labs; their stance is firm, it's not going to happen unless a request is made with a list of specific chemicals to test for accompanied with funds up front to purchase the standards, develop procedure, and pay for the actual testing.

Show me where thy holy time and money is backing up thy holy words, brother! You were consulted on writing the regs GW, maybe you could share how this wasn't addressed when it seems to mean so much to you and yours now. Here's a chance to take the stand and create the change.

My own off the cuff guess is the levels of individual mystery oil components in open extracted BHO is going to be at or below the true level of accuracy of the testing procedures, so either the testing will be found to be impossible, or worse, produces flakey results few will ever agree to as a fair test.

I might as well address this too, "The problem with lighter gas sources, is that they aren't held to the same standards as reagent grades, so their quality can and does vary more."

"Reagent grades"??? Please show me a manufacturer Certificate of Analysis for bulk butane or propane that includes data from a 'residue after evaporation' test. Butane and propane weren't being used as solvents previously, so this test isn't done, it's what I've been doing because no one else seemed to care.

An example of 'residue after evaporation' data of a typical traditional solvent,

"Petroleum Ether (Ligroin), ACS, 35-60°C, 1L (32oz)

For Research & Development
Not for drug, clinical use in humans, for food or food additive use

Specifications:
Meets ACS Specifications
Boiling range 35° - 60°C Pass
Color (A.P.H.A.) <10
Acidity Pass
Copper corrosion Pass
Doctor Test - Negative - Pass
Residue after evaporation <10ppm
Sulfur <5ppm
Benzene (GC) <2ppm

CAS: 8032-32-4

FORMULA: N/A"
http://www.ebay.com/itm/Petroleum-E...108592?hash=item3aa4dde4b0:g:n7gAAOSwFEFXJi3p

SkyHighLer said:

If this is so... it's night and day, the mystery oil is easily detected with unaided senses when taking a dab, and I have a question for you, and the entire community, why isn't testing for mystery oil done when certifying oil for the MMJ and recreational cannabis markets?

The journey of a thousand miles starts with the first step, and some places are starting to check for mystery oil, which will show up as pentane, hexane, heptane, octane, etc. If you have any of those markers, you can infer the presence of the rest.

One step states are taking, is specifying the quality level of the LPG that can be used for extraction. Washington for instance.

Reagent grades come with test results and certs, so to use lighter grades you would have to have each batch tested for compliance first.

In Nevada, the lab results came back with a separate line for Mystery Oil, marked ND, but we pre-distilled our 99.5% Instrument grade before extracting with it. It costs us about twice what lighter butane cost in bulk.

The test isn't without associated costs, and the labs love to sell time, so it is ostensibly the market, not the labs that isn't yet willing to pay the additional costs.

That's just a rhetorical question as far as I'm concerned, as I've already inquired pointedly and repeatedly of Steep Hill and SC Labs; their stance is firm, it's not going to happen unless a request is made with a list of specific chemicals to test for accompanied with funds up front to purchase the standards, develop procedure, and pay for the actual testing.

Show me where thy holy time and money is backing up thy holy words, brother! You were consulted on writing the regs GW, maybe you could share how this wasn't addressed when it seems to mean so much to you and yours now. Here's a chance to take the stand and create the change.

Consulted and listened to are not the same. Here locally the rules makers listened and then wrote them to suit themselves. We got listened to only after we descended en-mass on our legislators in protest at being ignored and abused.

My own off the cuff guess is the levels of individual mystery oil components in open extracted BHO is going to be at or below the true level of accuracy of the testing procedures, so either the testing will be found to be impossible, or worse, produces flakey results few will ever agree to as a fair test.

I might as well address this too, "The problem with lighter gas sources, is that they aren't held to the same standards as reagent grades, so their quality can and does vary more."

"Reagent grades"??? Please show me a manufacturer Certificate of Analysis for bulk butane or propane that includes data from a 'residue after evaporation' test. Butane and propane weren't being used as solvents previously, so this test isn't done, it's what I've been doing because no one else seemed to care.

An example of 'residue after evaporation' data of a typical traditional solvent,

"Petroleum Ether (Ligroin), ACS, 35-60°C, 1L (32oz)

For Research & Development
Not for drug, clinical use in humans, for food or food additive use

Specifications:
Meets ACS Specifications
Boiling range 35° - 60°C Pass
Color (A.P.H.A.) <10
Acidity Pass
Copper corrosion Pass
Doctor Test - Negative - Pass
Residue after evaporation <10ppm
Sulfur <5ppm
Benzene (GC) <2ppm

CAS: 8032-32-4

FORMULA: N/A"
http://www.ebay.com/itm/Petroleum-E...108592?hash=item3aa4dde4b0:g:n7gAAOSwFEFXJi3p

Click to expand...

Sometimes cutting to the chase is the shortest distance between two points.

I never run your evaporation test in a plastic bag, because I have a better process for determining the presence, though not the actual gm/ml.

Instead of a a small amount in a plastic bag, each and every time we load new LPG, we pre-distill it as much as 48 pounds at a time and check to see how much residue was visibly left behind after evaporating that volume.

The difference between 99.5% Instrument grade and lighter butane, is that the instrument grade leaves a thin film in the collection vessel, and the lighter butane leaves drops.

The difference isn't subtle and no rocket science is required to see.

In addition, you would have to be anosmic to not detect the odor when the pot is opened, and the taste is even less subtle.

As long as unregulated quality gases are used, quality will always be hit or miss. Perfection this time is no reliable indicator of quality next time.

On a personal level, it really does get down to how much of what is present, and the individuals sensory thresholds.

For individuals providing medications to others, it also gets down to what quality level your patients have a right to expect, and you have a moral obligation to provide.

My test is similar to the EN 15471 & ASTM D2158 tests, I just chose an extremely low mass evaporation dish, a common plastic bag, so it could be weighed accurately with an inexpensive milligram scale, and the tint could be easily observed by placing the bag against a white background.

"Analysis of Oily Residues in LPG

Fuel specifications for oily residue in LPG list ASTM Method D2158 or EN Method 15470-1. ASTM Method D2158 is commonly called the oil stain method. After evaporating 100 milliliters of the LPG stream, the remaining volume of residue is read from the glass evaporation tube.

This volume is one quantification used for fuel specifications. In addition, the residue is dissolved in a solvent and the resulting solution is slowly dripped on the adsorption paper. The size and persistence of the stain which remains on the paper after the solvent evaporates is the other, empirical, quantification of the oily residue in the LPG sample. Both quantifications are not very accurate.

EN 15470 determines the oily residue by performing a gas chromatographic analysis of the residue that remains after evaporation of an LPG sample. EN 15471 uses the weight that remains after evaporation of 100 ml of LPG sample as the quantification."

http://www.scientificss.co.uk/products?format=raw&task=download&fid=169

If someone sold you reagent/instrument grade, or whatever grade LPG, ask them how it was tested, the above was from 2010 - the proper equipment for accurate residue testing of LPG is still being developed.


Here's 'my' residue after evaporation test procedure for those unfamiliar with it or my stance,

https://www.icmag.com/ic/showpost.php?p=7229147&postcount=650

SkyHighLer said:

My test is similar to the EN 15471 & ASTM D2158 tests, I just chose an extremely low mass evaporation dish, a common plastic bag, so it could be weighed accurately with an inexpensive milligram scale, and the tint could be easily observed by placing the bag against a white background.

"Analysis of Oily Residues in LPG

Fuel specifications for oily residue in LPG list ASTM Method D2158 or EN Method 15470-1. ASTM Method D2158 is commonly called the oil stain method. After evaporating 100 milliliters of the LPG stream, the remaining volume of residue is read from the glass evaporation tube.

This volume is one quantification used for fuel specifications. In addition, the residue is dissolved in a solvent and the resulting solution is slowly dripped on the adsorption paper. The size and persistence of the stain which remains on the paper after the solvent evaporates is the other, empirical, quantification of the oily residue in the LPG sample. Both quantifications are not very accurate.

EN 15470 determines the oily residue by performing a gas chromatographic analysis of the residue that remains after evaporation of an LPG sample. EN 15471 uses the weight that remains after evaporation of 100 ml of LPG sample as the quantification."

http://www.scientificss.co.uk/products?format=raw&task=download&fid=169

If someone sold you "reagent/instrument grade, or whatever grade LPG, ask them how it was tested, the above was from 2010 - the proper equipment for accurate residue testing of LPG is still being developed.


Here's 'my' residue after evaporation test procedure for those unfamiliar with it or my stance,

https://www.icmag.com/ic/showpost.php?p=7229147&postcount=650

Click to expand...

Brother SH, we do indeed get certifications of purity from Praxair, but because we, without exception, pre-distill each and every batch, what is left behind is blatantly obvious.

Praxair provides certifications, but we sent samples to a third part lab for analysis, which showed the <99.5% Instrument grade to actually measure 99.9%, with regard to molecules heavier than C-4.

99.9% is of course available at a higher price, but do you really think they cut off quality at 99.5% or maintain two supplies and spigots?

The reagent gas parameters are different than lighter gas standards, which were developed to not clog small butane orifices with "oleaginous waxes" when burned, and are typically a blend of normal & Isobutane, plus n-Propane.

Because we were denied the availability of reagent grade gases, we used more available lighter butane, which was mercaptan free, but alas contained molecules heavier than C-4, which are deposited in the extraction when open blasting.

Once we'uns were aware of their presence, we implemented means to remove them prior to extraction, so that we weren't stuck with trying to remove them from our extract, and still hold on to monoterpenes.

They are of course, lost as more heat and time at vacuum is applied in attempts to remove the higher boiling point hydrocarbons.

Reagent grade standards include both molecules below C-4, as well as above, so the numbers are apples and oranges as compared to the "50 ppm lighter fuel statement of quality", with regard to clogging a small butane lighter orifice.

Thus far we've seen no noticeable deviations processing 48#'s at a shot and the Prax Air 99.5% Instrument grade, has consistently tested to 99.9%, with regard to molecules longer than C-4.

As a practical measure, how could I miss that 99.5% Instrument grade has far less solids in it, that the best lighter butane I've tested, when processing 48#'s at a shot. About as subtle as a baseball bat across the forehead.

As another practical matter, the smell is enough to convince me that I don't have to run tests to tell I don't want any of it in my extraction.

Got it, I now see the Gray area...

"Both of my younger Skunk Pharm Research Partners affirm that they also can taste its presence, soooo, even using reagent grades, we always pre-distill."

So, BHO open extracted with lighter refills as the link in the lead post indicates will fail in the market place as the smell of the mystery oil when dabbed is so offensive to everyone.

Done, NP.............


Oh, and you guys make fun of my test...

"Testing Method of LPG Residual Matter"
http://www.j-lpgas.gr.jp/en/download/dl/JLPGA-S-03.pdf

That's the current level of accuracy of testing in use, if you know of a lab that has the new LPG liquid injection chromatography, please share.

I'd be very interested to see how consistent results are across more than a can or two, as you did in most of your butane and dimethyl ether residue tests. Understandably, that requires both purchasing all that solvent from each source, and preferably distilling and recovering the clean solvent for later use.

As GW stated, he distills 48 lbs to see and smell the residue left behind. I distill a minimum of 20 lbs to prep for runs, and think that larger batch sizes give much more precise data (to the same level of accuracy). I don't think that is "making fun" of your test.
I can also personally attest to non-volatile mystery oil in distillation batches. How is a yellow oil filled with scattered, black spots - that doesn't go away after days in a hot outdoor shed - volatile? It simply isn't. And it smells like fish and urine and petroleum from across a 20 ft room.. After those few days in storage, it smelled perhaps a little LESS, but I didn't have to have my face in it to know it's nearby.

Sadly, SkyHighLer, mystery-infused hash oil hasn't weaved it's own way out of the marketplace yet, and I'm starting to doubt if it ever will, aside from the communiry of hash makers themselves and the future possibility of gas source requirements. It all starts with edumacation.

Yeah but uh... about this brand.

There has to be an ICmag member who's near one of these dispensaries+is able to take one for the team and buy some of this stuff, right? (I guess they're distributed at these places)

https://www.instagram.com/p/BI0rkZEAO2c/?taken-by=extractioneering.westcoast


I've been watching this company a good bit myself the past few months.. very curious if it's anything special.

If I had to guess, propane based live resin, left out at room temp nothing more nothing less.

Here is a residual solvent scan done locally

Old Gold said:

I'd be very interested to see how consistent results are across more than a can or two, as you did in most of your butane and dimethyl ether residue tests. Understandably, that requires both purchasing all that solvent from each source, and preferably distilling and recovering the clean solvent for later use.

As GW stated, he distills 48 lbs to see and smell the residue left behind. I distill a minimum of 20 lbs to prep for runs, and think that larger batch sizes give much more precise data (to the same level of accuracy). I don't think that is "making fun" of your test.
I can also personally attest to non-volatile mystery oil in distillation batches. How is a yellow oil filled with scattered, black spots - that doesn't go away after days in a hot outdoor shed - volatile? It simply isn't. And it smells like fish and urine and petroleum from across a 20 ft room.. After those few days in storage, it smelled perhaps a little LESS, but I didn't have to have my face in it to know it's nearby.

Sadly, SkyHighLer, mystery-infused hash oil hasn't weaved it's own way out of the marketplace yet, and I'm starting to doubt if it ever will, aside from the communiry of hash makers themselves and the future possibility of gas source requirements. It all starts with edumacation.

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Not all the brands of canned butane have non-volatile residue that stinks, lol, I found several with very little to no odor even before vacuuming down the bag, and a couple I thought even seemed to have a refreshing odor! I've kept the test bags/data cards, and the bags of those that were real stinkers continue to stink to this day.

Multiple lots (date codes) of many brands of butane were tested, I found a brand's quality remains fairly consistent until they let their filter stacks go, two of the most disappointing were Puretane and Newport. They apparently don't have a simple way to test what they're canning. The industries' standard test is a way over complicated boil off test, I know this sounds extremely self aggrandizing, but if any of the LPG producers would use my test as a daily quick check there wouldn't be non-volatile residue issues.

This sounds absolutely moronic, but I'm completely serious, cover all my expenses, and I'll work with your plant manager to ensure your facility is putting out a consistently residue free product. I'd love to visit Asia.....

I've been closely following this extraction firm for months and reading their posts closely they aren't being as secretive as this thread is making it sound. I definitely wouldn't claim to have "figured it out" yet but I have refined my processing to much more terpene heavy samples (at least what I believe via observation, not tested examples) through reading more about their process. I have to say I am a huge fan and would imagine a lot of processing in the future starts leaning to very soft and "sugary" consistencies like they often picture. It doesn't cloud up, it doesn't lose terpene content, it doesn't change noticeably other than terpene content seeping out of the sugars for months on end. I have moved to smoking this consistency almost exclusively over shatter or wax because of how easily and tasty it dabs!


If you are interested in this firm, definitely check out the0therone on IG and posts about his product, he seems to have achieved very large clean THCa crystals through this process that look absolutely gorgeous. In my experiments the crystals are very small, I would love to hear more thought about how larger crystals can be achieved.

Dabstract labs also claims they have achieved a high terpene extract from a single pass, and a second pass is needed in their process to extract cannabinoid content. Their posts also seem to show this stuff or something similar in serious volume.

Somethings to note about claims of this technique from extractioneering:

-Extractioneering claims to use a mixed blend hydrocarbon 48% N-Butane, 26% ISOButane, 26% Propane in an "open and closed" apparatus, however the0therone claims to make his with 99.5% butane and in a state certified closed loop.

-They claim to achieve this consistency from a variety of material, all dry run, yet claim to always pull a small percentage of moisture content.

-Always claims to be "single pass virgin extract." I have seen them deny multiple passes unlike dabstract labs.

-Always claim an "ultra" dewax, whatever that exactly entails I do not know.


Here are some pics of my efforts to reach higher terpene preservation (I manage a compliant operation located in Colorado:

It seems like you nailed it or came pretty close bro, good job!would you care to share the processing steps you took in order to achieve the picture above?

check out the threads on thca isolation and crystallization. If you want larger singles you need slower more consistent evaporation, depth and surface area of the vessel play a role. Starting purity and terp volatility play a role as well, single pass at cold temp will achieve this readily. Looks like your purging in a deep vessel?

I have and that's definitely helped me get to the point I am at! That has definitely been what I have noticed, I usually fold up a parchment or teflon "boat" to purge on, so I definitely am purging in a deeper vessel than normal, but have noticed too many butane muffin issues going into smaller vessels like a mason jar . My solvent usually sits between -45 and -20 due to the chiller the company I work for utilizes.

I would love to talk shop in further detail but am worried my local contemporaries would be less then satisfied about such discussion.

I believe this can be achieved through dewaxing with limonene... they are adding terpenes in the dewax that allow the thca molecules to come together and crystallize.. as they purge the dewaxed oil thats in limonene they slowly form.. once the limonene is to the right amount 5-10% of final product they package it.. nearly all the solvent has to be out at this point leaving high terpene content sugared thca crystal dabs..

sugar wax obviously can happen without added terpenes if the terpene levels are high enough.. also heard it happening when adding alcohol and slowly evaporating.. so the dewax could be with alcohol but then I don't know where the high terpene levels are coming from..

Anyone I know doing this technique is not adding limonene or any secondary solvent. Also plenty of folks are making this from a variety of quality starting material, it's more about thinking of refining a process then altering it.