Alright fellas I can confirm, I think @Cheebachiefextracts was correct, the last owners were carbon scrubbing in the flask. I’m thinking this has to be the culprit. As far as i know none of the biomass we touch ahs been sprayed with any type of fire retardent. Assuming our clients are being honest, the only thing being sprayed is sulfur, which I can’t find any info stating that it can cause delta 10 conversions.
I’m assuming it’s gotta be the chipped glass of the boililng flask holding onto the carbon. We went from 189c in the boiling flask to 180c and saw significantly higher delta 10 (6%) vs the 189c boiling flask runs which were between .5 and .7%. To me this suggests the residency time in the flask is a huge factor and also supports that something in the flask is the catalyst for this bullshizzzy d10 lol. We will be ordering another flask, but in the meantime does anyone have any tips that may work for properly cleaning glass that has been chipped and holding onto carbon?
If you absolutely positively want to make sure all carbon is gone then piranha acid seems to do the trick but it’s nasty. What I’ve been doing to clean up glassware that’s a real pain in the ass, is drop some automatic dishwasher pellets into the boiling flask fill it up with water inside the mantle (do not overfill or you’ll have a mess) and set the temp just below boiling (about 95°C) set the stirring as fast as you can and let it run for 24 hours. Usually my flasks came out mostly squeaky clean afterwards.
Appreciate all the feedback from everyone! Going to try scrubbing my glassware as best as possible, modify a few temps and will get back once labs are in. Should be able to nail down wether its the carbon, sulfur or temps within the next week or so.
We have our pump exhaust plumbed into the extraction booths hepa filter and then straight outdoors so we should be ok, thank you for the heads up though! Don’t have the chance to smell the exhaust (thankfully lol) Haven’t seen any delta 6a or 10a just yet and our CBN tends to hover between 1-3% pretty consistently. And as for the crude it generally smells wonderful lol even during decarb the stuff is generally pretty terpy, I would think I would be able to smell it at least a hint in decarb, or it could be such trace amounts I can’t smell it and it’s still boning the oil lol. More tests to come!
I would advise against using consumer/residential grade soaps and detergents. They have lots of weird chemicals and more importantly, fragrances, which are hard to remove. I’ve always had really good experience with Alconox/Detonox lab glass cleaner. If you’re patient, you can see it do real magic-I’ve seen it strip off layered thick black tar and carbon off glass like it was nothing.
Piranha Acid is a good suggestion, but be careful! Its fun to throw hot dogs in it for safety demonstration purposes to lab techs.
Edit: If anyone goes the Piranha Acid route, be sure to thoroughly clean your glass AFTER piranha acid. The use case is to break down carbon-bonds and dissolve any residue. It seems painfully obvious, but the acid can cause unintended reactions if not thoroughly cleaned out.
No problem. I found the folks over at Alconox to be super friendly and helpful too. If you have technical questions or are facing a particularly challenging cleaning job, they can give really good suggestions. I personally like Detonox liquid more than Alconox powder, even though they are extremely similar. They also sell low-foam products optimized for ultrasonic cleaning baths, which may help for your particular situation.
If and when putting anything glass in a sonicator make sure you put a layer down cloth/towel or some sort of cork/ptfe holder compatible to your cleaning solution/ solvent so you don’t have any abrasions or micro cracks ensue from the sonicator directly on glass.
@WolfeXtracts how old is your ethanol? I’ve heard that ethanol that has been stored improperly with exposure to heat and light for a long period can cause issues with isomerization. If your ethanol is coming out of the hotter part of the country, make sure to ask your supplier if it has been stored outside, and for how long. You might be able to look up the date that your ethanol was packaged by lot number or whatnot to give you an idea of how long it has been stored prior to reaching you.
Interesting.We’re in Colorado but our ethanol is distributed out of Nebraska. Will follow up on this as well and see how our drums are being stored as well as if they have a born on date. Thanks for the suggestion!
While a little wild and not designed for that application, it probably would work too. Don’t let anything touch the probe outside of the engineered stand clamped at the appropriate point. PTFE will melt and release pretty terrible toxic/cancerous gas. Fabrics and fibers can easily catch fire. The clamps are situated at nodal points where vibrations are minimized.
Long story short: If you use a probe, be careful and hang it so it does not touch the walls of the glass, and the tip is submerged. You’ll be better off with a large bath. Both baths and probes can be pretty pricey, and I would not buy used transducers. For a large bath big enough for 2x20L, expect to pay $4-$10k.
@WolfeXtracts, you could just keep it simple and put an overhead stirrer inside the bf with hot water+alconox. Thats the simple stupid method which will work well.
Xtractor Depot has a fairly decent sized ultrasonic cleaner that should do the job. The tank dimensions are 750mm x 550mm x 480mm. It has 3kw of ultrasonic power, and 8kw of heating power. It runs on 220v.
You’d be surprised at the amount of glass that’s been broken after not using a buffer. It will without a doubt cause microscopic cracks and while you heat your mantle in turn they expand and your flask typically cracks.
