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Terpenator Solvent: Iso-butane vs N-butane

Breakover

Member
We've been using n-butane from airgas in our terpenator since we started up. I got piddling around their website/catalog and saw they also have iso-butane in the same grades that they offer n-butane.

These two gases are very similar, and I believe iso-butane is what comes in most cans of lighter fuel. The major difference that I noticed was iso-butane boils at a much lower temp than n-butane, 11.2F for iso- vs 31.0F for n-. The vapor pressure of iso- is also significantly higher(31 vs 45 psia), leading me to believe that it would be easier to purge iso- than it would be to purge n-.

My question is, how MUCH easier? Is it a significant timesaver? Do you think it would produce a better/different/inferior extract? Has anyone used iso- in their terpenator or are you all using n-? I'd appreciate any info from anyone who has tried both and compared the two, terpenator or not.

Here's where I found the info: http://www.airgassgcatalog.com/catalog/

You have to select Appendix->Physical Properties if you want to check my numbers.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
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We mostly use instrument grade n-Butane, but I see no reason that Isobutane would not work as well as n-Butane, and could be better.

I have extracted with mixtures of n and Isobutane in a Terpenator with good results, but never with just Isobutane alone. If you are going to try it, I hope you share the results.

I am reviewing the requirements to run a Terpenator with n-Propane in it, which will require higher pressure, but will produce a lighter blond product, according to one of my SCFE resources.

I am currently requesting bids for instrument grade sources of n-Propane, without ethyl mercaptans added for leak detection, from Airgas, Matheson, and our cheapest GC gas supplier, Industrial Source.
 

Breakover

Member
Unfortunately, I just ordered another tank of n-, but a close friend and I are building another terpenator, so I'll try to talk him into trying iso- with his instead. If he goes for it, I will definitely share what we find with everyone here.

Propane sounds interesting. I saw that airgas has it from 99.0% to 99.99% purity. Not sure how pricing is, but instrument grade n-butane costs me about $300 total for an LP5 cylinder (std 20 lb cylinder) with freight. If propane is cheaper and does a better job, I'm sure you'll find a way to deal with running higher pressures. :)

You guys sure are blessed with a plethora of chemical and gas suppliers out there. Here in MI we're stuck with Airgas and ordering lab solvents on line. No local suppliers at all. Boo! :(
 

Gray Wolf

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Unfortunately, I just ordered another tank of n-, but a close friend and I are building another terpenator, so I'll try to talk him into trying iso- with his instead. If he goes for it, I will definitely share what we find with everyone here.

Propane sounds interesting. I saw that airgas has it from 99.0% to 99.99% purity. Not sure how pricing is, but instrument grade n-butane costs me about $300 total for an LP5 cylinder (std 20 lb cylinder) with freight. If propane is cheaper and does a better job, I'm sure you'll find a way to deal with running higher pressures. :)

You guys sure are blessed with a plethora of chemical and gas suppliers out there. Here in MI we're stuck with Airgas and ordering lab solvents on line. No local suppliers at all. Boo! :(

I'll give Isobutane a shot too, as soon as we run through our latest Lp-5. Perhaps I can get them to special order a smaller sample for R&D.

Yah, we are blessed that this has always been a high tech industrial area, with lots of aerospace, national defense, and cybertech presence. One of Portland's charms, but alas in the last four decades, tooooo many people have moved here...............

Airgas is no friend in these parts at $402 LP-5 Instrument Grade, and Matheson and Industrial Source are easier to deal with, but even higher.

We have a Texas source at $263 LP-5 Instrument Grade, but is unique to our relationship with the supplier and our volume is too low to negotiate a better price with the local suppliers.

As far as chemicals, we are fortunate to have national chain American Scientific and a Van Waters and Rogers here locally, and a registered research lab business.

We like American Scientific for our limited volume and scope; how far is the closest American Scientific or other school supply house, from you? Worth a days jaunt and adventure to pickup?

If you're in need of higher volumes and industrial prices, before retirement, the companies I worked for, bought tanker truck loads of chemicals from Van Waters and Rogers, as they typically had the best bulk prices for quality grades in volume.

I've never tried to do will call at VW&R, so I'm not sure what their policies are regarding will call delivery and site inspections.
 

Breakover

Member
Well, we've finally gotten two complete mk1 terps built. We're going to do a side by side comparison with Iso and N using the same material. Will post pics and weights after we're done.

We've discovered that a deep freeze makes for a great cooling bath replacement, especially with Iso, as it tends to run much higher pressures when we use a traditional ice bath. Obviously that is a function of the iso's lower boiling point.
 

JColtrane

Member
Looking forward to your results bro ... we just got access to n-tane within the past month, and I'll be using it in our system this weekend. We decided to work with Praxair instead of Airgas, and get great customer service ... what was the cost difference between these gases? I'd be wondering ... anyways, thanks :tiphat:
 

JColtrane

Member
Ever think about running iso w/ d/i in your closed loop? Might want to give it a shot ... it's almost like petroleum ether!
 

KonradZuse

Active member
any results yet good sirs? :).


Also we might want to start a post for different extraction methods. Simpson uses naptha, some use iso/ethanol, some use butane, some like CO2 or Hexane(I heard Hexane/Octane are very good solvents for BHO).
 

Gray Wolf

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any results yet good sirs? :).


Also we might want to start a post for different extraction methods. Simpson uses naptha, some use iso/ethanol, some use butane, some like CO2 or Hexane(I heard Hexane/Octane are very good solvents for BHO).


Hexane works slick but is harder to purge than butane without vacuum. Easy in thin films with a vacuum.

I've soaked up to 12 hours without picking up and green color.

Pentane also works good, but is more expensive than Hexane.
 

Breakover

Member
Sorry y'all, no test runs yet. Thought we were going to get to it this weekend, but no dice. Hopefully get something done this week.
 

Breakover

Member
Dual Terp setup. We share the 5 cfm vac pump. Deep freezers hold the butane storage/recovery tanks. N-butane unit is on the left and Iso-butane unit is on the right. Each 1.5" x 24" column was loaded with 150g each Super Lemon Haze trim...



After the standard 4 flood and 3 minute soak cycles and a nice deep vac purge, here's how they looked:

Iso:



N:



Finished wax:




Each run yielded a little more than 18g each of "cooked" oleoresin.

I couldn't tell a difference between the two batches, but a few associates suggested the Iso extract seemed slightly smoother, but both had good super lemony hazey flavor.

I will say the Iso took longer to 'wax up' to the finished form, requiring more working/purging time.

Yields were nearly identical, so I think we can conclude that yields were not affected by the choice of butane.

The color of the Iso extract was slightly lighter than the N- as you can see by the pic. Not enough evidence to conclude that the choice of butane made the difference, however.

Chromatography is next. I will report back once we have some solid numbers on potency.

Sorry it took so long folks, just been a madhouse around here lately...
 

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Gray Wolf

A Posse ad Esse. From Possibility to realization.
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Dual Terp setup. We share the 5 cfm vac pump. Deep freezers hold the butane storage/recovery tanks. N-butane unit is on the left and Iso-butane unit is on the right. Each 1.5" x 24" column was loaded with 150g each Super Lemon Haze trim...

[URL=http://i215.photobucket.com/albums/cc32/leftupnorth/2013-05-02_14-49-30_139_zpsb3e76c9f.jpg]View Image[/URL]

After the standard 4 flood and 3 minute soak cycles and a nice deep vac purge, here's how they looked:

Iso:

[URL=http://i215.photobucket.com/albums/cc32/leftupnorth/2013-05-02_17-44-03_933_zps82caa8a9.jpg]View Image[/URL]

N:

[URL=http://i215.photobucket.com/albums/cc32/leftupnorth/2013-05-02_17-44-37_861_zps9c034c04.jpg]View Image[/URL]

Finished wax:

[URL=http://i215.photobucket.com/albums/cc32/leftupnorth/2013-05-03_01-19-42_534_zps6e53c86c.jpg]View Image[/URL]

[URL=http://i215.photobucket.com/albums/cc32/leftupnorth/44a68c60-a139-404c-bc18-afc8ccfa9747_zpsf870f427.jpg]View Image[/URL]
Each run yielded a little more than 18g each of "cooked" oleoresin.

I couldn't tell a difference between the two batches, but a few associates suggested the Iso extract seemed slightly smoother, but both had good super lemony hazey flavor.

I will say the Iso took longer to 'wax up' to the finished form, requiring more working/purging time.

Yields were nearly identical, so I think we can conclude that yields were not affected by the choice of butane.

The color of the Iso extract was slightly lighter than the N- as you can see by the pic. Not enough evidence to conclude that the choice of butane made the difference, however.

Chromatography is next. I will report back once we have some solid numbers on potency.

Sorry it took so long folks, just been a madhouse around here lately...

Good job on the dueling Terpenators and thanks for sharing bro! We've been focused on critical path projects and have yet to make the comparison.

Not everyone has been dilatory however, associates Sean and Chun have both done experiments with Instrument grade Propane in their Terpenators and report lighter extract, at about half the yield.

It also takes longer for recovery because of Propane's lower boiling point.

Did you note significant differences in recovery time with the Isobutane, due to its lower boiling point?
 

Breakover

Member
Yes, although we didn't time each run, it definitely took longer to recover the iso. It also ran at higher operating pressures. The last soak cycle will bring pressure on the column up to 75psi or so when running a Michigan pound. I'd estimate it added probably 15 minutes or so to the total process time.

I wonder if a cooling coil after the discharge of the appion would help recovery times. We've been thinking of cobbling together a cooling coil and immersing it in a glycol bath in the deep freeze to test it.
 

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