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Terpenation at Terpene Station

FatherEarth

Active member
Veteran
....In the shadow of the moon,
Terpene station,
And I know we'll be there soon...
Im starting this thread share tips and tricks picked up along the way as well as mistakes and extraction trials. I didn’t want to Hijack / clutter up the MKIII thread so I figured a Terp notebook and pic dump would be a better alternative.

Hopefully, Gray Wolf will be dropping in and answering questions and explaining a few things..
The MKIII operator tech support has been most helpful :)
GW has done a great job with this unit, he has been awesome at answering any questions I have had,
effectively keeping me on track the whole way.
So here are some pictures of MKIII preparations before the first run…. So here is a picture of the valves. I printed waterproof labels and sealed them on the handles so I could remember which to pull when reading the instructions. At first its kinda hard to remember whats where when you get started. This was great, now I can almost run the machine with my eyes closed. Also included is the operation procedure for the MKIII. Although I think there may be a typo in #15, I assume he meant turn of Vacuum pump instead of the recovery pump as it was turned off in #12...

The Terpenator series are operated as follows:
1.0 Open all valves, except for valve #4, the butane supply valve.


2.0 Turn on high vacuum pump and pump system down to -29.5″Hg.


3.0 Close valves #1 and #3.


4.0 Turn off high vacuum pump and turn on the recovery pump.


5.0 Place one hand on the vent line exiting the top of the column and turn on valve #4.


6.0 When you feel the sudden chill of liquid butane reaching the vent tube, close valve #2, and then valve #4. Record the number of seconds required to flood the column with the existing packing density.


7.0 Continue to pump with the recovery pump, until the internal pressure is reduced to -10″Hg.


8.0 Open valve # 2 and valve # 4 for the same number of seconds that it took to flood the column the first time.


9.0 Close valve #2 and then #4 and continue to pump, until the system pressure is again reduced to -10″Hg.


10.0 Repeat steps #8 and #9 for as many cycles as you choose to run. Typically three cycles for the Mk IA and II, and five cycles for the faster Mk III and IIIA.


11.0 At the end of the last cycle, when the gauge hits -10″Hg, open valve #2 and then valve #3 to dump column.


12.0 Continue to pump until the system reaches -22″Hg, at which point close valve #5 and turn off the recovery pump.


13.0 Open valve #1, and turn on the high vacuum pump.


14.0 Pump the system down to -29.5″Hg and close valve #1.


15.0 Shut off the recovery pump and allow the system to sit under hard vacuum for 5 minutes to purge.


16.0 Remove product from lower collection tank.
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Then after connecting a quick release compression fitting into valve 4. Connect to a compressor and begin pressurizing the system to 60 psi first check to see if its holding, then again at 100psi and submege in a barrel of water to check for leaks.
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After many attempts to get the MKIII airtight I gnarled the threads to one of the ss connection pieces and had to replace the part. Costs me around 3$ for a SS double ended thread connection. Before the replacement I had a slow ultra tiny leak. Was hard to notice unless you were at the right angle but I managed to snap a pic of the micro bubbles..Highlighted by the red arrow...
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FatherEarth

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Veteran
After getting it air tight it was time to see if if would hold a Vacuum.
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Holding 29.9 for 24 hours :)

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After getting the hang of the vacuum pump and overstanding the importance of the oil level in the vacuum pump.
Being that its key to the vacuum pump's ability to pull a hard vacuum.. time to move on to filling the tank via can tapper....
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
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Good thread bro and several good points!

One key point is that 300 series stainless to 300 series stainless fitting matches, gall badly if you don't keep the two metal surfaces from making contact. Once they gall badly enough, you can't even get them apart, much less stop them from leaking.

If you buy the heavy film Teflon tape, you don't have to wrap as many layers. We get the heavier Teflon tape at RSD refrigeration supply or the yellow hydrocarbon tape from Paramount Supply.

While even the cheap thin stuff will seal the joint and not gall with enough wraps, as a point of reference, the American Gas Association recognizes yellow Teflon tape as the color for hydrocarbon service.

The important thing in assembling the stainless to stainless joints, is to make sure that the PTFE Tefon film tape is thick enough to prevent metal to metal contact, even as the joint is tightened.

Pressure testing first is how we bring ours on line as well. If it will hold pressure, it so far has held vacuum. Easy to just look for bubbles but harder to find vacuum leaks.

Thanks for the heads up online 15; I fixed it to reflect shutting off the vacuum pump, vis a vis the recovery pump.
 

FatherEarth

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Thanks GW, I have a bunch of saved notes and pictures to share. Im just getting started putting it all together. Thanks for stopping in, hope you pull up a seat because we got a lot to cover.

Gas PTFE tape

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FatherEarth

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On to filling your tank…

So I had trouble filling my tank with the listed resources from the skunk pharm website. They all wanted my HVAC handlers license before they would sell to me. If you look or smell like a hippie they are going to turn you away with no gas for sure. I looked into getting licensed and its surprisingly easy. The EPA’s website gives you a study guide to take the handlers test and you can even take the test with open book you just cant miss as many questions, lol. Its really basic stuff that some of us need to know anyhow. I believe taking the test is something like 35$ and cheaper if you fail and have to retest. Anyhow I opted to tap cans to fill my tank. Thinking that Id need a lot of cans I bought two master cases of lucienne, only to find that filling my recovery tank with albs only takes approximately 10 cans I put in 15 before I knew anything. From the skunk pharm website in the comments and questions area “n-Butane weighs 0.575 grams per ml. A 300 ml can weighs 173.7 grams, plus can tare. 173.7 grams is .3836 lbs of butane. 72 cans would be about 27.6 lbs.”You want the can mostly empty so when the warm butane returns from the Appion G5 Twin the chilled tank that sits in an ice bath will be able to cool the butane. The more surface area thats cold the better. 5 lbs gets you enough to do runs and still meet the needs of condensing the butane in a timely manner.
So I figured I would take some pics and talk about the process to help those nervous can tappers out there. I was bit nervous at first as puncturing butane cans seems kinda dangerous, at least until you get the hang of it.


GW
“The way we fill it with a can tapper, is disconnect the vacuum pump hose from the Terpenator and attach the hose from the can tapper. With the recovery pump running, the can is tapped and the vacuum pump valve on the Terpenator opened, which allows the butane to inject into the recovery pot, and be sucked up by the recovery pump, which puts into the storage tank. When the can is empty, close the valve and tap a new can, before again opening the valve and repeating.
After the tank is loaded in this fashion, cool it down in an ice bath for a couple of hours and then open the vapor port valve to atmosphere, to burp off compressed non condensible atmosphere. At 30F, butane has little to no gas pressure, but canned butane contains propane as a propellant, so first there will be a burst of air leaving and then the propane. I burp off just the air and close the valve once I smell propane with my nose held close.
As the propane in lighter butane contains no ethyl mercaps odorant, the smell is not rotten eggs, but subtle and lightly petroleum.

Question from a Terpenator Operator
_____________________________________
Hi Guys! I’m not sure if I am doing it right….
Once you tap a can…. and it empties into the system… there appears to be some pressure in the system… but how do you know when the butane has been fully transferred to the storage container?
I left the appion running (Which I’m not even 100% sure is working… I bought it used… it starts up but im not sure how I can test it?) for about 3 minutes after the can was depleted, then shut all the valves… I then removed the gauge hose to see if there was anything in the system and didnt hear anything….
Oh and what side of the storage tank does the hose coming from the appion into the storage tank go into? Red or Blue?

==========================================
GW
You can tell by the pressure gauge whether it is transfered or not. We exchange cans at zero pressure and pump the system down to -22Hg after the last can, using the Appion.
The blue hose from the Appion discharge, goes to the vapor port on the tank, which on both of ours, is blue. Look on the top of the valve and see if it says vapor or liquid.
I suggest checking by reading the logo, because in refrigeration, typically blue is liquid and red is vapor, but every refrigeration recovery tank that I’ve found, is marked exactly the opposite.
_________________________________________________________
So….Here are some pics for those who need visual reference to understand.

The Can tapper

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We found out quickly that you need to first vac down the tank before you can fill it. Our tank was brand new and I believe its shipped with some sort of inert gas for shipping, but not sure. Anyhow we opened the vapor valve and let out any gas that was inside then connected the tank to the system and vacuumed it down to 29 hg using the robinair, closing the valve before reconnecting it in the tapping order seen here.

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So before you actually begin you should ice down the tank. I would have heated the collection pot but I was nervous as this was my first 'live' run with the appion and mkIII using butane. Would have made it much easier, emphasis on much.

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we found tapping the can in the middle and on its side worked best. With the appion already running and valve #5 open
Tap the can slowly and lock the tapper closed, then open the #1 valve. A quick rise in PSI can be seen on your gauge then the appion starts vacuuming it out. Once the gauge reaches zero again, close the #1 valve and tap another one. Repeat this until you have reached the desired amount of butane. Without heating the collection vessel it will take a long time to recover the butane. The whole thing becomes iced over and slows to a halt as seen below. This may be circumvented by attempting it on a hot day if you dont want to heat with a water bath.

tap and hold

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Iced collection pot

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FatherEarth

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You will not be able to vacuum down to 22hg until the butane is warm enough. If there is butane in the system you wont get to 22. This is an indicator for you to note, since your gauge is your eyes inside the MKIII and lets you know whats going on.

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Gray Wolf

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Good point on vacuuming out the storage tank before filling! Ours have come dry nitrogen filled.

An 50# refrigerant recovery tank will hold about 50#'s of water full, but because of thermal expansion hydraulics when the liquid gas is heated, an 80% fill is the maximum recommended. Water weighs .0361 pounds/cubic inch and n-Butane liquid has a specific gravity of .601, so it weighs .0217 pounds/cubic inch.

As FE noted, we don't run our tank 80% filled, only with 5 to 10 pounds of butane, so as to leave a lot of open area on the tank walls for the incoming butane to be cooled back down to a liquid. It takes longer when the tank has more liquid already in it.

The feds sent the gas suppliers a letter saying that n-Butane is used to produce illegal drugs and that if they don't do their part to prevent it, they will be taken to task. They would like to sell you the gas, they are for the most part covering their asses.

Getting the gas here isn't a problem for a licensed business with a store front, but the price damn well is. It is relatively cheap in Texas but changes from a clear almost odorless substance to pure gold by the time it reaches Oregon.

We actually buy ours in CA at about $263 per Lp-5 of Instrument grade n-Butane, but the local Airgas wants $402, Matheson $500+ and Industrial Source $609. A long case of (72) 300 ml cans of Lucienne costs around $120 from A&S Marketing, and weighs about 28 pounds.

Don't forget to burp off the atmosphere after loading with cans. Entrapped atmosphere is not only potentially explosive, it isn't condensable, so it raises the internal pressure of the tank, dramatically slowing down recovery.
 

Gray Wolf

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As far as heating the lower Mk IIIA tank, it isn't necessary to produce product, it just saves a bunch of time.

It also changes the nature of the product. Unheated, the Terpenators produce a shatter product that looks like blonde cotton candy, and at 212F, it produces a partially decarboxylated dark amber oil. Cold takes about three to four times as long to recover as hot.

Here are a couple pictures:
 

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FatherEarth

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Wow GW that oil is white! I have yet to get it that light color, but I havent gone without at least 85 degrees and it still takes a long time to do so. Around an hour a tube IME. Im yeilding a minimum of 14g per tube with 150g of material packed tight and flooding until the butane is almost clear, still got a bit of yellow to it but I figure its not worth the extra time. I did leave out the burping of atmosphere and the propellant propane. When I did it I couldnt smell anything so I let if burp til I smelled butane and then stopped. More to come just getting around to doing some computer work.. Thanks


Respectfully,

FE
 

FatherEarth

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After filling the tank with butane, I forgot to remove/ purge the recovery hose. I left liquid butane sitting in the appoint and recovery hose over night. The next day I removed the line spewed butane and was left with a nasty red gooey oil. I figured this oil would be in the collection pot or the tank. To my surprise it was only in the recovery hose. . .FYI I was using a Goodyear Galaxy SAEJ2064 class II specs here: http://www.jgbhose.com/static/906102.asp

I have since switched to an Appion Mega Flow Vacuum Certified refrigerant hose part # MH120006EAK. The 1/2" diameter hose with 3/8" on one end and 1/4" on the other greatly increased recovery time. Twice the price but the quality is equal to the $ increase, you get what you pay for.

Word of advice/caution:
When I first got the MKIII I thought I was being cautious by using tape on the flared fittings. This is not needed and actually is more unsafe than anything. I had my first, oh shit moment when the fliter drier flared fitting I wrapped busted loose and spewed butane while the appion was running. This could have been disastrous had I not been standing right next to it to instantly shut down the appion.


Red Oil from the recovery hose before ever running any material.

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Clean pot
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FatherEarth

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So on to actually doing something with this fine piece of machinery. So I was reading at Skunk Pharm I needed to do a leaf run to get any oil in the ball valves out before doing a real oil run. So I saved some whole leaf from some plants nothing special just regular unfrosted leaf. I packed the 1st tube with 150g of screened leaf. I covered all the Buna screens with ss 400 mesh and packed the column ends with two wadded up cone coffee filters before packing. Here is how it went.

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FatherEarth

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Running the water bath at 120 F and flooding 3 times I yeilded a dark amber mostly hard taffy. 5.7 grams from un frosted lower leaf, I was kinda surprised. I did not see any petroleum oil fluoresce when under the black light. Although I did not dab any of this run..lol

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FatherEarth

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A trick I picked up from skunk pharm.. heating your oils to precise temps with a previously useless volcano. Preparing to make a topical for a psoriasis patient.

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icdog

Member
I'm happy I just bought one of these. Anyway you could make a video of it working and setting it up?
 

FatherEarth

Active member
Veteran
have you changed the sight glass gasket to a bunn-a gasket?


I searched high and low for a buna sight glass gasket to no avail. Im actually using a teflon gasket currently that is supposed to be used with the tri clamp. Its doesnt fit perfect but well enough I dont have any leaks. I have cranked down the bolts a few extra turns to make sure as the PTFE gaskets are quite stiff and allow for a swivel action seal when used with the tri clamps. If you know where I could buy a buna sight glass seal I would gladly switch.

ICdog, Im not a movie kinda guy. Short film maybe but narrated movies arent my thing. Although I know someone who may be willing to star as the Terpgineer.. Ill see what I can do. Assembly is simple and the pictures are rather self explanatory. What do you need help with specifically? Ill try and help best I can. Mine came loosely assembled as I picked up mine in person. Certain parts I would not want to disassemble and re do. I could do a basic rundown of what to where with pics.. Ill keep you posted.
 

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