Hi there, I have some questions about color/smell refinement of some distillate we just ran through our short path for it’s first pass.
I’ve Included two images below of the dark oil I’d like to adjust. It has a burnt rubber sort of smell and seems much too dark. Before or after a second pass I am hoping to perform a clay bleach scrub of this material. I have some Summit research filtration aid stuff as well as bentonite clay and diatomaceous earth to choose from. I’d like some advice on what clay material (or combination of materials) to use other than Cbleach which we do not have.
Furthermore, I have been unable to find a relevant SOP for the bleaching/scrubbing process in terms of what ratios of oil to clay to use.
I observed my first fraction heads at around 95 degrees and the main body a couple hours later at 195 degrees. The main body coiled for quite some time and I finally began to see tails at 196 degrees five days after we began.
This is my first run ever so any advice would be welcomed. Mostly trying to determine the best way to achieve colorless odorless oil.
These guys have multiple tricks up their sleeves. Clay’s and saline/hexane washes seem to help with color and carbon seems to help with smell.
I don’t see a point for water clear myself, but a lot of these guys are putting Cbleach in the flask to get there. Not here, but I have seen people use packable heads to get there too. Not sure how common that is.
I did mean days yes- we ran low and slow as it was our first run. Not 5 full days by any means, I would say we have ran the short path for ~35 hours during business hours.
3% in the flask is what I hear most people doing. This could lead to water clear, pH imbalances causing oxidation and/or isomerization. Do it at your own risk.
You have stinky oil because you broke down the terps and seemed to collect them in the flask with the main body.
Although some pre-processing before your second pass is a good idea, it is not 100% necessary to lighten up your material.
I generally do a 1:1 mix of wyo clay and carbon and then put that in my boiling flask for the second pass. I use 10% of my first pass distillate mass as a guage for how much of this mix to add.
The other option is to dissolve in heptane 1:1 (distillate to heptane) and then add the 10% wyo/carbon mix and stir under heat using a heating mantle and stir bar. I recommend doing this step AFTER saline scrubbing.
It seems you are taking a verrryy long time to run. Even a long run should not exceed 12 hours.
Our mantle is fit for a 5L flask and I’ve achieved vac depth of 64 microns prior to adding material to the flask. On average the vac depth has been 400-600 during boiling.
It is important to verify; at what point are these measurments taken? Is the temp being sampled up near the condenser as is typical, is it being sampled in the boiling flask also typical, or is it the heating mantle temperature setting (likely not)?
Here is why I ask. You describe a burnt rubber smell that I myself call a burnt transmission oil smell. (I have been so very brutal on my cars so I know the smell… I do not drive anymore from injury off a motorcycle but my last drive in a car I saw 147 on my digital speedo just moments before I saw 35 on a yellow triangle with a black arrow showing me the way I had to go… It is SURPRISING how quickly the distance between car and curve closed )
ok… flashback over… but my point is that the stuff smells like burnt tranny fluid because something very hot interacted with the compound far and away hotter than those temperatures you listed. I believe your readings 100% because they jive with my own observations about first pass crude. However my temps are measured under the boiling flask.
When my crude is run over about 170C then the beginnings of burnt tranny smell appear UNLESS terpenes have been removed first. In that case it does not have that same smell as when we lit the neighbors car on fire as kids and that acrid smoke from the seats? Aweful. Just like terpenes sizzled. In my case this happens when above 170C and I have to run up to at least 185C on first run crude like rosin when not using chemicals and such. More gunk = higher temps under the boiling flask are needed in order to push that vapor cloud up high enough for collection.
If you are running say 220C under the flask in order to get the vapor to heat the uptake tube to the temps you list (which is really how distillation is best visualized) then it means that all compounds get in contact with sizzling hot surfaces (just like in a Tiptronic transmission at 147 mph…). So even the gunk is cooking away and much of the visible vapor then is actually smoke particulate and really nasty smell.
A suggestion is to examine your uptake path centimeter by centimeter and see where heat might be getting lost because you are trying to heat that uptake path up with the cloud of vapor you are pushing. Same with the boiling flask itself. Some flasks are like ten pounds of glass and insulating every last bit will help heat the uptake path through conservation.
Finally you should get a badge if you have gotten this far… but I purchased this as a tool
I suggest checking the temp under the boiling flask and at the neck of the boiling flask on top. Use foil tape to tape one probe to the top of the flask and one at the bottom. This is an important measurement.
If you want to troubleshoot your run these are the readings that I and many others on here can help you interpret and is important data for troubleshooting… These tell us the glass temp being contacted and the gradient tells us efficiency of the process which is also a measure indirectly of vacuum (in a subtle way). My prediction based on the data you presented is you will see a temperature difference (gradient) from bottom of flask to top of flask in excess of 40C. Maybe a whole lot in excess.
It is fixable with a bit more data methinks? I am gonna vape some more now and get back to some flashbacks…
)
