Florasol (R134a) extractions.

[Doctor Vapor]

1st: Using 0 impurity commercial tane + glass or ss apparatus + vacuum purging/heat, makes an end product with a merc. level totally consumable and less harmful then 90% of the chemicals used to grow our "bomb commercial" weeds...
2nd: we in Europe can get pretty easily N-tane without drawing a target as we do not have that concentrate market blooming...
3rd: to the OP, how can your end product be free of wax/lipids and have a taffy consistency...I see this as impossible (as all the end products I have seen free of lipides= liquid concentrate or crystallized and powdery)?
4th: your pictured product looks exactly the same as 90% of the end results we picture in the Oil extravaganza & my stash threads... so no IMO that picture does not show at all the "superiority"of florasol extracts...
Don't get me wrong I'm really interested in your posts but I don't want mis-information to be spread!

FLskwat, Thank you for adding your perspective to this thread. Good to hear from the EU! I trust you are in one of the member states that is still financially stable for the time being.

Ahh, to be in Europe where it is actually possible to carry out this kind of research without fear of government agents knocking on your door! Even though some of us in the US are in 'medical states' there is always the threat of federal intervention.

Oh wait, wasn't it the UN that just tried to shut down Colorado and Washington for non-compliance with international 'drug treaties'?? Citizens here voted for legalization but the international law makers don't like that. International Pharma could perhaps have some powerful influence in the law. Maybe the situation is not as simple as it seems. What has happened to Amsterdam's cannabis tourism? I hear that you have to be a Dutch citizen now to visit the coffee shops. Correct me if I'm wrong.

Now if you are GW pharmaceutical and can afford to buy some politicians or have the backing of Big Pharma, that's different.

Not sure what you mean by a "merc level totally consumable". Yes it is 'consumable' but is it healthy? In the past I have consumed more than a few things that weren't so healthy in the bigger picture. In this little corner of the world, we tend to favor organic techniques that don't use ANY chemical nutrients. Some people are even growing "TLO" known as "True Living Organics" wherein you don't put anything artificial on the soil at all. Instituted by Skunk Magazine's Cultivation editor "The Rev", if you care to research it further. I'm not that much of a purist but it has been literally years since I grew using syntho nutes. Back in the day I even used the GH "bubble gum juice" that some people are still using. Thankfully GH now has an organic line as well. In recent times, I do my best to only grow medicinal grade. "Bomb Commercial" is the herb of commerce not the herb of medicine.

Please let me clarify the discussion regarding absolutes. I was responding to some questions Puffer asked regarding the idea of creating an 'absolute' with the florasol process by omitting the hydrocarbon co-solvents from the process. I was not purporting show an absolute in any of the previous pictures. Apologies for the lack of clarity but I did say that i prefer to use a co-solvent to include the waxes from certain strains. You are certainly correct in stating that an absolute would be more like shatter and less like taffy.

The product that comes from the florasol process is actually not so viscous. More like CO2 extract until you purge it under vacuum for a while and wash it.

You might care to have a look at "powdered toast" which I posted on another thread. We didn't know you cant crystalize THC until after we did it. Well, a bumblebee can't fly either.

I can't claim any of this to be my product. It is the product of the best chemist I know. The Cannabis plant.

There are some awesome concentrate pictures on this forum. Some of these pics are almost pornographic.

Maybe someday there will be a book published for concentrates that is along the lines of Subcool's "Dank" for flowers.

Again, thank you for your comments.

~Doctor Vapor

 

[FLskwat]

DV , yes commercial bomb was in between brackets to underline the absurdity of the 2 terms associated (I'm pretty much aware of the TLO movements & Cie, thx! ;-) and those chemicals in the weed are just an example... .. such as the saturated fats in the Oreos or/and 1 day of breathing in a megalopolis of 12 Mi inhabitants with diesel micro particles, etc...ALL OF THAT IS WAY ABOVE the level of intoxication I'm getting through a properly purged BHO, that was more or less my point!
About Amsterdam & tourists please feel corrected as my friends were there this WE and there is no problem going to any coffeeshops today in Dam for a French or Spanish citizen (FYI there is BTW a dedicated thread on FC to follow this issue almost live: it's an issue in Maastricht and other southern cities but not in Dam yet :-).
I have friends in the LA area that have the equipment for super critical CO2 extractions in their lab and have seen their end products so I see what you are talking about. Pure gold too.
Yes I have seen the powedered toast you have posted (very nice pix BTW), here and elsewhere too (this is yet using a 3rd process...).
This been said we need more people like you to push the community towards a better knowledge and understanding of the whole process, and at the same time a better product...welcome here my friend!

 

[Doctor Vapor]

That's why I can't afford making concentrates. I don't joke with purity. Here there is only expensive or homegrown herb. With the available resources I got it seems more logical to use the herbs directly thru hi end vaporizer and glass. I wish I could make a batch of quality for the convenience and experience

Can't wait to see it all ! I love gear

There is nothing more natural than vaping the herb the way Goddess intended it......
The reason for concentrates has more to do with minimizing lung exposure for me.

I love gear too. Does that make me a 'gear head'?

I couldn't find another thread that mentions it but I wanted to post something about Mercaptan removal for those who use the commercial butane (not my thing but I know it is popular). So, in the interest of safety and at the risk of being a little off-topic here are some links.

Here is a reference to the DOT rules.
http://www.ogs.ny.gov/BU/BA/FS/lpgregulations.asp

Here are some methods to remove the odorant.
http://www.onepetro.org/mslib/servlet/onepetropreview?id=IPTC-13512-MS
http://www.faqs.org/patents/app/20080245703

 

[OO]

The product is less pure, but higher in terpene content, a sacrifice that is IMHO worth it. That is why it looks different, it is very much less pure, but at least the aroma and flavor are preserved.

I'm interested in why the pump fails over time, is it due to friction or cavitation?

Either way, I'm glad you are making this information available.

That being said, I know those who subscribe to the same rulebook as you with regards to horticulture, I do not, but I can respect it. That being said, I've witnessed far more frustration with the TLO that I believe is necessary, but to each their own.

As far as mercaptans are concerned, I do find them exceptionally repulsive, even in minute quantities, and have found brands of butane where I have been unable to detect it, doesn't mean it's not there, just that I can't detect it.

I'm done dragging this thread off topic, but I would like to thank you again for the contribution, it is quite valuable.

 

[Puffers]

I am not Doc but from my understanding the seals in the recovery pump start to dry out and the pump loses it effectiveness. The refrigeration recovery pump is meant to pump an oiled refrigerant which uses the oils for lubricating and keeping the seals hydrated [similar to a compressor used in residential/light commercial a/c systems but more vital in that scenario which is why airflow and refrigerant charge (they are a function of each other a concept doc applies with his heat jacket and collection vessel) have such an impact on a compressors life span]. Butane and the variation of 134a in use here contains no oils so the seals are compromised more quickly.

 

[FLskwat]

Here are some methods to remove the odorant.
http://www.onepetro.org/mslib/servlet/onepetropreview?id=IPTC-13512-MS
http://www.faqs.org/patents/app/20080245703

Mouahaha French inventors... This is pretty funny knwing what happened a few weeks ago in Rouen= big Merc. leak at 400 km from Paris:
AT 4am I wake up saying to my wife, don't you smell gas? So basically the leak was so important that I could smell it in my parisian flat, 400km from the leak original point!!!

http://www.mirror.co.uk/news/weird-news/uk-hit-by-french-gas-leak-1549236

 

[Doctor Vapor]

OO had some interesting observations and comments, including:

I know those who subscribe to the same rulebook as you with regards to horticulture, I do not, but I can respect it. That being said, I've witnessed far more frustration with the TLO that I believe is necessary, but to each their own.

As far as mercaptans are concerned, I do find them exceptionally repulsive, even in minute quantities, and have found brands of butane where I have been unable to detect it, doesn't mean it's not there, just that I can't detect it.

I'm done dragging this thread off topic, but I would like to thank you again for the contribution, it is quite valuable.

Thank you for your contribution. I'm honored that you find this information valuable and have taken the time to read it.

To set the record straight I have some friends who are way into TLO. I don't subscribe to any rulebook. Call me impatient but it takes years to build up the proper soil. I DO love to grow using organic nutrients in soil with teas to enhance flowering. The interplay of soil organisms and plant nutrients is fascinating. Much useful information can be learned by studying it.

My earliest experiences were with indoor hydro and chemical fertilizers. I always liked the idea of being able to grow plants lab style and have experimented with aeroponic and deep water culture as well as hydroponics. My observations over time have revealed that plants grown organically in soil (if grown well) have a better flavor, superb resin content and are more disease resistant.

Would you be kind enough to share the name(s) of the brands of butane that you have discovered to have undetectable mercaptans? I'm sure there are others who would appreciate the benefit of your experience.

A discussion of hydrocarbon gasses is not entirely off-topic in that n-butane can be one of the modifiers used to obtain more complete extracts of herbs using R-134a. A better choice would be deodorized propane which has physical characteristics that more closely match those of R124a but some people have successfully used butane.

Please understand that very small amounts (>10%) of modifier gas are used and this is done to get a better yield. This is obviously not the same as a conventional BHO extraction due to the relatively small amounts of butane in the gas mixture. You will notice in the following list that butane is recognized as a refrigerant gas and is called R-600 while propane is R-290.

http://en.wikipedia.org/wiki/List_of_refrigerants

This gives rise to the thought that a refrigeration system could be considered a model for many different kinds of herbal extractors. Therefore, the information being discussed in this thread may have widespread applications in various herbal extraction processes.

In response to your pump question: I value Puffers' input because of his experience in the refrigeration industry. I'm not a mechanical engineer and will have to do some research into the seal wear that he suggests is the mechanism involved. I believe he is correct in his reasoning.

Because even pumps that do not rely on the gas for lubrication also need periodic rebuilding, I think there are other factors at work as well. The fact that you could be pumping a liquid or a gas, depending on pressure and temperature, also contributes to pump wear. For example, the expensive SS extractor pump shown in the above pictures needed to be rebuilt after about 300 hours of use although it has a separate crankcase lubrication system and teflon seals.

The Appion G5 twin also has a separate crankcase which is the main reason I would recommend it.

http://www.appioninc.com/products/g5features.html


It seems that all these pumps need periodic rebuilding. I'm not sure how often in the case of refrigeration use but maybe Puffers can tell us.

Rebuild kits are not too expensive: http://www.centurytool.net/Appion_G5_Twin_s/16907.htm

"The scientist asks "why does it work?" The engineer asks "how does it work?" The liberal arts major asks "do you want fries with that?"

 

[Puffers]

It seems that all these pumps need periodic rebuilding. I'm not sure how often in the case of refrigeration use but maybe Puffers can tell us.

Thanks DV, its good to know my input may helpful at least, while you let me peek through the window of the lab and pick your brain. Yes a recovery pump does need a rebuild periodically anyway. Unfortunately in my applications the biggest factor in our rebuilds is how much the pump was abused during use, whether the pump was properly throttled so it wasn't over pumping or pumping excessive amounts of liquid causing compressor knock. It varies so much and one tech not paying attention or having the proper knowledge can enormously reduce time between rebuilds. If i was to hazard a guess a unit like the G5 (sweet pump btw) with its features, properly used could probably do in the range of 300 hrs, i may be off base though because most places i have been they probably last a 1/3 of that due to neglect or incompetence. Unfortunately Doc a lot of HVAC techs could benefit from your thread and some of the basics of refrigeration we have glossed over in discussion but you have so kindly put up videos for. If you ever need a job Doc you let me know , you have a much better grasp of thermodynamics then many techs i have attempted to train out school

"The scientist asks "why does it work?" The engineer asks "how does it work?" The liberal arts major asks "do you want fries with that?"

While i unfortunately don't have a degree in engineering as a mechanic i definitely ask myself how it works before i ask why, guess i picked the right field for me

 

[Doctor Vapor]

I've been looking around the forums her a bit and am very impressed with some of the people here. The level of knowledge on FC has certainly improved over the years. Thank you all for your interest in the material being presented in this thread. If you take the time to dig into the data I think it can help improve your ability to produce herbal concentrates. I'd really like to see some of you who have the facilities be willing to conduct some experiments and share the results with the group.

In the interest of stimulating more discussion, I want to show everyone a few pictures and graphics of the work a FOAF has done in the last two years.

First some CAD drawings:

Then a bit more refined concept:

Here is the look of the finished extractor:

This design incorporates a process control computer with a touch screen and has electronic sensors rather than the mechanical gauges of the prototype seen earlier.

Here is the actual build:

(Static testing of the larger extraction vessel shown in the lower left above)

Never criticize anyone until you have walked a mile in their shoes, because then you are a mile away and you have their shoes.

 

[Puffers]

Wow DV..... that is stunning.... ok so first question is are the filters in your picture are they water filters for the chiller? Which leads me to the chiller itself, what function does it serve? Is it just to speed extraction? Is there a scale where it becomes a necessity?

 

[Doctor Vapor]

Wow DV..... that is stunning.... ok so first question is are the filters in your picture are they water filters for the chiller? Which leads me to the chiller itself, what function does it serve? Is it just to speed extraction? Is there a scale where it becomes a necessity?

The chiller runs a 'coldfinger' that is inserted into the reservoir to speed the change back to a iquid. Later my friend used a large radiator to further cool the flow and speed the process.

Filters are the "molecular sieve" I mentioned earlier and used to remove water from the stream.

 

[Doctor Vapor]

This nozzle is used in the recovery vessel and is based on something called Rapid Recovery of Supercritical Solutions or RESS.

 

[Doctor Vapor]

My phone gets notices when people post so even though I am in Lost Angeles right now, I'll be back to respond as time permits.

 

[Puffers]

This nozzle is used in the recovery vessel and is based on something called Rapid Recovery of Supercritical Solutions or RESS.

Is this for the powdered toast? Is this a super-critical process like the name implies?

 

[Doctor Vapor]

Is this for the powdered toast? Is this a supercritical process like the name implies?

Here is one method to make powdered toast. (Sorry, I couldn't resist posting this)

The "straight" answer is: In theory, yes but in practice, no. Powdered toast is made by spray drying.

http://en.wikipedia.org/wiki/Spray_drying

So far my friend has not been able to keep R-134a at the supercritical point. It seems to be a good solvent in the liquid phase but not quite right as a carrier for the spray drying of our extract..

So Puffers, are you ready to do some experiments, yet? All you really need is a few stainless vessels and you already know where to get those. (SF Research lists the sources)

I mentioned molecular sieves
http://en.wikipedia.org/wiki/Molecular_sieve

The 3A is best for this application:
http://www.deltaadsorbents.com/molecular-sieve-desiccants/t101c17.aspx

I asked a friend and found the critical temperature and pressure for R-134a
http://encyclopedia.airliquide.com/Encyclopedia.asp?GasID=141

Doing this will require some reading but it could be worth it for the knowledge you will gain. Not for everyone but I'm sure a few FC people have the ability and resources.

Thanks to everyone who has responded to this thread. IF there are any other questions, I'll do my best to answer.



Here's information about the concept of "triple point"
http://en.wikipedia.org/wiki/Triple_point

 

[Doctor Vapor]

FINDING PARTS TO BUILD YOUR OWN:
Here are some additional resources for those of you who would like to build an extractor. If you have other sources to add, please post them.

STAINLESS TUBING:
http://stainlessandalloy.com/index.php/stainless-pipe-tube-plate/sanitary-tube-fittings/tubing.html
http://www.amazon.com/s/ref=nb_sb_noss?url=search-alias=industrial&field-keywords=sanitary+tubing
http://www.n-c.com/CatalogGroup.asp...ubing_Flexible_Hoses_&_Couplings.Tubing.304SS

FILTER HOUSINGS:
http://www.jalttechnologies.com/housings/cartridgehousingsmetal.html
http://www.zenpure.com/products/housings.html
http://www.eaton.com/Eaton/Products...ration/BagFilterHousings/FLOWLINEII/index.htm

SANITARY SPOOLS:
http://www.glaciertanks.com/TriClamp_Products-Couplers_1_-2_TriClamp.html
https://www.gvc.net/p/4203/316l-ss-sanitary-tri-clamp-spool-pieces
http://stores.ebay.com/TPT-Sanitary-stainless-steel/Sanitary-pipe-spool-/_i.html?_fsub=4333685011

Please read through the above thread for other sources and further information about building your own extractor. The same basic principles also apply to other kinds of extractors, not just to R-134a. I hope this list will save you some time but it is only a starting point.

Vape in Good Health!

~DV


"Some people see things that are and ask, Why? Some people dream of things that never were and ask, Why not? Some people have to go to work and don't have time for all that." George Carlin

 

[tepictoton]

just stumbled upon this...

thanx now I've got shitloads of reading to do

 

[chun]

The chiller runs a 'coldfinger' that is inserted into the reservoir to speed the change back to a iquid. Later my friend used a large radiator to further cool the flow and speed the process.

Filters are the "molecular sieve" I mentioned earlier and used to remove water from the stream.

Was wondering the results of the chiller?

i have been thinking about using 316 SS Heat-exchangers but have yet to find a good cooling compressor to keep Res low enough.

so what i understand is that you dont pull plant waxes with R134a?

 

[Doctor Vapor]

Thanks for your thoughtful questions, Chun.

My mechanical engineer friend actually cut a hole and welded a tube into the big tank. The coldfinger from our chiller was placed inside to provide maximum thermal contact. You can see the hose going in to the bottom of the tank in some of the pictures above.

There was also an experiment with a tube-in-tube heat exchanger running water flow from a chiller.

After the extractor has been running a while it is very useful to have cooling capacity. The process slows down a lot due to stored heat energy in the gas phase. Chillers and heat exchangers speed up the extractions by making the transition back to liquid phase faster.

Here's a view of the 'radiator' style heat exchanger in the SS Extractor pump. This pump was both unbearably slow and terribly expensive ($10,000) . The bearings and seals failed and proved impossible to replace. Last I saw it it was in pieces in a friend's garage.

It was replaced by the Appion which was almost twice as fast once we installed an external heat exchangers. It has two small internal radiators but we added an external one with muffin fans similar to the one in the picture above.

============

Yes, that's correct. You don't pull plant waxes with pure R143a. Now, I love a few good plant waxes myself. That's the reason we experimented with hydrocarbon co-solvent mixtures.

It's surprising how compatable R134a is with certain hydrocarbon gasses.
http://www.ewp.rpi.edu/hartford/users/papers/engr/ernesto/huntek2/proj/Resources (previous deliverables-Resources)/Articles-Publications Cole Library/134a replacments.pdf

“I'm not crazy about reality, but it's still the only place to get a decent meal.”― Groucho Marx

 

[mendohoney]

Very curious as to the temperature/pressure conditions in your extraction vessel.

 

[Doctor Vapor]

http://www.engineeringtoolbox.com/refrigerant-temperature-pressure-chart-d_1683.html

 

[mendohoney]

From another forum:

I have some reservations about this use of r134a. I have worked with tetrafluoroethanes in my lab and we take additional precautions not to inhale any gases from a fluxing reaction where tetrafluoroethanes are used because they tend to produce gaseous HF above about 250 Celcius (483 F). Seeing as how the average torched ready to dab nail is in the range of 400-800F, this applies to dabs as well.
MSDS: http://www.refrigerants.com/msds/r134a.pdf

 

[Skeena]

I would like to see more pictures of the end result.

 

[Doctor Vapor]

From another forum:



I have some reservations about this use of r134a. I have worked with tetrafluoroethanes in my lab and we take additional precautions not to inhale any gases from a fluxing reaction where tetrafluoroethanes are used because they tend to produce gaseous HF above about 250 Celcius (483 F). Seeing as how the average torched ready to dab nail is in the range of 400-800F, this applies to dabs as well.
MSDS: http://www.refrigerants.com/msds/r134a.pdf

Interesting but how does this matter if all the florasol is purged from the extract?

I still recommend complete purging of the "solvent". Due to it's vapor pressure at room temperature, it's easy with R134a. Very quick purge if you use a good vacuum.

I believe it is safe. Florasol has been used in food flavorings in the EU since 1996.

On December 14, 1996 the Scientific Committee for Food of the European Commission approved an amendment to "The Solvents Directive", to include "Florasol" (R134a), the solvent upon which the process is based, as an acceptable solvent for the extraction of flavors for use in food. " Florasol" (R134a) is intrinsically safe and has also been approved by the FDA as a propellant for inhalers used by asthma sufferers. An application for the use of "Florasol" (R134a) as a flavor extractant in the USA is presently being considered by the FDA.

Source:http://www.essentialoil.com/pages/dr-wilde-florasols

 

[Botanical.Extracts]

This should help.

1. Compressor Pump (in this case a really expensive explosion proof one)
2. Reservoir (this has both gas and liquid ports and a dip tube)
3. Extraction vessel (put the herb in here, liquid flows through it. note the sight glass)
4. Molecular sieve (removes water)
5. Expansion valve (allows liquid to flow at a steady rate to change to gaseous phase)
6. Collection vessel (in this case with a water jacket to improve performance)
7. Water heater (for the water jacket on the collection vessel)
8. Water pump (circulates the hot water through the water jacket)
9. Vacuum pump (to evacuate the system before and after use)

Hello Doctor Vapor,
Any updates on Forasol R134A Extractors?

Do you have any details about the:
4. Molecular sieve (removes water)?
and the:
5. Expansion valve (allows liquid to flow at a steady rate to change to gaseous phase),
Where do folks buy one of these valves?

Thank you.

Doctor Vapor,
Please, more photographs, good work!
Is that the water trap on the floor with the red hose cut off in the photo?
What kind of pressure gauges did they use?
Thank you.

Mod note: Three posts merged