Distilled 10lbs 99.5 ISObutane lots of contaminents

I picked up about an LP5 cylinder of 99.5 ISObutane from Praxair the other day and finally got a chance to distill 10lbs last night. I'm using an MK3 system, in an 85 degree water bath, using a TRS21 pumping through a 25 ft coil and into a 50lb Mastercool tank.
I've distilled numerous times using canned tane and don't recall ever seeing quite as much "mystery oil" from this amount. Plus the Praxair gas had a "plastic petroleum" smell. The color was very dark orange almost verging on rust or something along those lines, leading me to believe the Praxair LP5 contains rust.
The pics may not exactly be the best representation, but you can definitely see the color of the oil in question that I wiped with a paper towel.
I haven't used this gas yet as I want to distill it again. Before I do however I figured I'd throw this post up to see if anyone has any insight into this. I had assumed this gas would have little to no residual oil after distillation. I have read that this Praxair gas is rumored to be very clean and should have next to no residual oils, however this is obviously not the case for me at least. Maybe I'm going to have to step up to 99.9%? I thought most people were using 99.5 when it came to research grade gas?

None of the bulk supplies have been tested for non-volatile residue (Mystery Oil) other than EcoGreen's initial lot of butane and propane I tested last year.

If anyone can counter that statement, bring it.


Looks too dark for non-volatile residue from the solvent itself.

"Internal inspections are done on all the cylinders we valve. Any loose particles inside the cylinder will be remediated before we re-valve the cylinder.
Most 1⁄2 ton cylinders received from Worthington will have to be dried. This drying process will be done before we re-valve the cylinders.

Typical new cylinders have oil residue along with water, both of which will affect cylinder life and product quality."

http://gasinnovations.com/literature/LOW-PRESSURE-CYLINDER-PACKAGING-2.pdf


Refined Hydrocarbon Solutions told me back channel he's going to test, test, test... his, EcoGreen's, and a few brands of canned. He's going to find a lab...yeah right, and maybe try my test. Until I see the results it's all shuck and jive, just like I got from Capital, Puretane, and EcoGreen back channel. Certificates of Analysis from the manufacturer don't show the non-volatile residue. Guys are open extracting with the straight bulk supplies, it's wrong, and I'm saying so, now, as strongly as I can.

Would you assume it is indeed rust? This cylinder appears to have some miles on it.
Curious if I should try to return this tank I got from Praxair or further distill in hopes to clean it up? If it were you, what would you do?
I appreciate any and all advice. Sorry I'm just in somewhat of a quandary as I had high expectations for this gas, I really assumed it would be a lot cleaner.

Keep distilling it, that looks like tank contamination, especially if ithe tank looked beat up. it looks like rust. Next time refuse any gas in a tank that looks beat up.

Sky I tried your test a couple weeks ago. Fresh tank squirted into a plastic cup, took the cup outside to gas off. Unfortunately the cup got contaminated but the light residue was minimal. I will find some tyvek and try again to get an accurate weight.

I have seen a large variation in non volatile residue from tank to tank, even from the same bulk supplier, Gas Innovations, who seems to be supply a lot of the gas theses days.

The latest batch of 99.5 was extremely clean, and came with a certificate of analysis testing at 99.8

My official rant, and how to do the test,

https://www.icmag.com/ic/showpost.php?p=6885056&postcount=606

I've said enough for one day, peace.

APK47 the tank of 95.5 n-butane 24 lb i got from JC in eugene oregon Praxair's tank look's to be a older tank with fresh paint and no dip tube inverted tank to distill no filter and got some rust flakes ? were black and a lite film of mo with a dark color in it almost black ? from 24 lb distill a lite petroleum" smell . a second distill from my 100 lb tank with a filter. no smell and a few rust flakes left over from the input line i be leve I will distill for a third time. look's like pay the price for 99.5 and a clean tank or pay the price in distill time.Praxair's butane so far is better than eco-green i have had .

Thanks for the info maxinum I really appreciate it. I will continue to distill at least 2 more times and I'll report back here after I do. Might not get to it till Tuesday, unfortunately running distilled newport until then. My praxair tank did have a diptube so I didn't invert.
I know they can fill my own supplied tank, which I may in fact do next. However they lost the last customer supplied tank in transit as they actually ship it from Detroit(where I am) to Toledo I believe. I've read far too many horror stories to trust ecogreen, so I bypassed that route and went to praxair. I'm going to inquire about 99.99 next go around, but if they supply it in a shit tank again, what's stopping from this happening with that too?

Thank you permaculture and skyhighler as well. As noted above I'm going to further distill this stuff and I'll let ya know how goes.
I'll also try Skyhighler's test both before and after distillations, and report back. I still have about 12lbs or so that I have yet to distill, so I can test it and compare to each successive distillation.

APK47 -Have you read horror stories about Ecogreen other than the one shipment of propane and propane blend? From reports here is seems only the one shipment of propane had issue. Sunfire used a ton of butane from that same shipment and says it was great.

If you need to double/triple distill use a catch tank you can clean out. Get the solvent clean before adding to you tank or your tank will not stay clean. Try slowing down the boil of distill a lot so the first pass gets it cleaner. 50-60 F water bath.

I can't verify if the people that were bitching about ecogreen in fact had gas from the same batch of gas. As some of this came from instagram and others from here. I have a decent connection at praxair and figured it would be relatively easy, which it was.
By a "catch tank I can clean" are you referring to a stainless design with removable lid or something along those lines? I'm looking into it as we speak but currently only have 1x50lb tank and 2x30lb tanks.
I'm currently distilling with the bath temp @85 but what you say makes a lot of sense. I did in fact control the rate of distillation with the initial 10lbs that I did, it took several hours, as evidenced by the clear line marking how high the liquid got in the collection spool, or how high it didn't in fact get. I will lower the temp and see how that goes as well as continue to distill slowly. Any recommendation as to how slow exactly to distill this stuff with a 6x6 or 6x12 spool?

You can build a temp "tank" from 6" or smaller spools. Just don't store solvent in them overnight. Temp and surface area of the liquid control the rate of "flow"/ boil rate. Take your time. Keep temps low so crap is not drawn along into the flow.

This step done slow and correctly will provide extremely clean solvent in your tank. In theory you don't need a middle tank. One pass should work if done slow enough. Using a middle clean out tank helps you be sure while getting the technique down.

SkyHighLer said:

None of the bulk supplies have been tested for non-volatile residue (Mystery Oil) other than EcoGreen's initial lot of butane and propane I tested last year.

If anyone can counter that statement, bring it.


Looks too dark for non-volatile residue from the solvent itself.

"Internal inspections are done on all the cylinders we valve. Any loose particles inside the cylinder will be remediated before we re-valve the cylinder.
Most 1⁄2 ton cylinders received from Worthington will have to be dried. This drying process will be done before we re-valve the cylinders.

Typical new cylinders have oil residue along with water, both of which will affect cylinder life and product quality."

http://gasinnovations.com/literature/LOW-PRESSURE-CYLINDER-PACKAGING-2.pdf


Refined Hydrocarbon Solutions told me back channel he's going to test, test, test... his, EcoGreen's, and a few brands of canned. He's going to find a lab...yeah right, and maybe try my test. Until I see the results it's all shuck and jive, just like I got from Capital, Puretane, and EcoGreen back channel. Certificates of Analysis from the manufacturer don't show the non-volatile residue. Guys are open extracting with the straight bulk supplies, it's wrong, and I'm saying so, now, as strongly as I can.

Click to expand...

I haven't tested any Praxaire Isobutane. Joe did the propane and I did the n-Butane.

Both were significantly cleaner than the typical R-600 or lighter gas, at distillation.

I took an LP-5 in for analysis, which showed the level of residuals larger than C-4 to be below the test cutoff of .2 ppm.

Next we will distill the balance of the n-Butane, and then filter it for retest.

While MO content is relative low, an Lp-5 has enough millions of parts, that even at a low PPM value, we should get a good sample.

Gray Wolf said:

I haven't tested any Praxaire Isobutane. Joe did the propane and I did the n-Butane.

Both were significantly cleaner than the typical R-600 or lighter gas, at distillation.

I took an LP-5 in for analysis, which showed the level of residuals larger than C-4 to be below the test cutoff of .2 ppm.

Next we will distill the balance of the n-Butane, and then filter it for retest.

While MO content is relative low, an Lp-5 has enough millions of parts, that even at a low PPM value, we should get a good sample.

Click to expand...

"I took an LP-5 in for analysis, which showed the level of residuals larger than C-4 to be below the test cutoff of .2 ppm."

.2 ppm my ass, and my assets, bet me if you really believe it. I'll come up there and and boil off a sample on camera, no slight of hand. Is this from Specialty Analytical again?

The cleanest I've tested was about 6ppm.

.001g of non-volatile residue divided by a sample weight of 165g times one million equals 6.06 parts per million.

.001g is already hardly readable on my milligram scale, your .2ppm would be .00003g with a 165g sample (300ml can of butane is about 165g.) In other words you're saying the lab determined there was basically no non-volatile residue (Mystery Oil) and I so doubt this I'm calling you on it.

No offense personally, you know you've got my respect.

Well I've now filtered and distilled this batch 4 times. It's still gross, I'm going to return it.
This stuff smells rancid, beyond just petroleum odor. I've managed to get it seemingly clean from a visual perspective, but this odor is too much for me to handle. I've never quite smelled anything like it, just a horrible chemical smell for lack of better terms.
Anybody else have any similar experiences with Praxair gas? I was under the impression that they had some of the cleanest gases around.
Skyhighler I never managed to do the residual test on this stuff. Still can, but I'm waiting on a scale to be shipped that will allow me to. If I can't test this batch I will the next, wherever it happens to come from!

APK47 said:

Well I've now filtered and distilled this batch 4 times. It's still gross, I'm going to return it.
This stuff smells rancid, beyond just petroleum odor. I've managed to get it seemingly clean from a visual perspective, but this odor is too much for me to handle. I've never quite smelled anything like it, just a horrible chemical smell for lack of better terms.
Anybody else have any similar experiences with Praxair gas? I was under the impression that they had some of the cleanest gases around.
Skyhighler I never managed to do the residual test on this stuff. Still can, but I'm waiting on a scale to be shipped that will allow me to. If I can't test this batch I will the next, wherever it happens to come from!

Click to expand...

All the Praxair gas I have gotten has been very clean ... returning it would be a good option.

APK47 said:

Well I've now filtered and distilled this batch 4 times. It's still gross, I'm going to return it.
This stuff smells rancid, beyond just petroleum odor. I've managed to get it seemingly clean from a visual perspective, but this odor is too much for me to handle. I've never quite smelled anything like it, just a horrible chemical smell for lack of better terms.
Anybody else have any similar experiences with Praxair gas? I was under the impression that they had some of the cleanest gases around.
Skyhighler I never managed to do the residual test on this stuff. Still can, but I'm waiting on a scale to be shipped that will allow me to. If I can't test this batch I will the next, wherever it happens to come from!

Click to expand...

Two inexpensive scales and some gallon ziplock bags, and then you'll know... know, know, know...it's something you get from experience I've heard.....

Color and odor can be confusing without weight/percentage. I just tested Marley 7X, the residue was clear, no yellow tint at all with just a moderate amount of odor, but I then discovered the weight was so much more than could be determined with the eye and nose alone. Nice clear little splotch of non-volatile residue, but when weighed it's obviously a nice thick clear little splotch of non-volatile residue. ;-)

The two scales I use and recommend for the residue test (imo, everyone on this Forum should have scales in these ranges, along with their go to 0.01 gradient scale. They're just too handy not to have at hand, and at minimal cost.)

http://www.amazon.com/dp/B0012TDNAM/ref=sr_ph?ie=UTF8&qid=1430690396&sr=1&keywords=milligram+scale

http://www.amazon.com/gp/product/B0012N1NAA/ref=oh_aui_detailpage_o04_s00?ie=UTF8&psc=1


To call my simple test "cute" (Capital) or "crude" (RHS) doesn't cut it when no one can post up data like I do; easily/simply replicated data, the scientific standard for proof.

You guy's are gobbling up RHS's tanks, how clean are they really? 99.0/99.5/99.9/99.95/99.99/99.995/99.999/99.9995/99.9999/99.99995/99.99999......percent??

Just give me a number, so when I'm dabbing some brother's dab at Chalice this year, I need have little concern it was run open with crappy solvent, much worse than even the lowliest canned butane.

Notice how full range yet tight the results are using my test versus the purity you're just hoping for with your bulk tank's vendor's claims.

Ultra Pure had 0.001g of residue
Ultra Pure, England, 300ml can, reads on the bottom "DOM 27.09.13 06:58”

.001/165 = .0000060606

x100 = .00060606%

99.9994%


Spark 7x had 0.04g of residue
Spark 7x, Korea, 300ml can, reads on the bottom “120404”

.04/165 = .0002424

x100 = .02424%

99.976%