Distillate process help please!

Hash and Stuff Distillation
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Hi yall, im having 2 problems and i gtreatly could use the help

1.) not getting much separation between fractions and I believe that’s in part to not having enough theoretical plates. Just yesterday I inserted a few rings but havent ran anything thru it yet. so i do believe i may have this figured out but my biggest complication is listed below…

however a big issue im running into is ill start with about 700-1000ml in the HM and by the time i’m done because the HM is now at 200c-205c and nothing else is distilling, well thats my issue. i’m barely getting any yield. from a 700-1k mL start, i probably end up distilling a total of 200- 300 ml, with roughly 60-80% of my original starting material still remaining in the HM flask. what am i doing wrong?

quick overview of what im doing:

2L short path setup…
heating mantle set to 80c, stirrer in HM on, cold trap cold, pumped warmed up, pump below 130 micron on whole system (when gauge hooked to pump directly and only pump, yes i get below 15micron and i do this test every time before i connect to short path to make sure pump is in good shape for run), beginning vapor temp reading 14-17c,. ill start to ramp the temp up on the HM from 80c by about 10c until i get to 120c and i let the HM catch up, from then i turn HM up 5degrees and let it boil and distill, i normally increase my HM 5c whenever the Vapor temp drops 0.5c. (my first two runs i increased the HM by 2c all the way from 120c to 200c. increasing 2c every time my HM would catch up by the 2c, id increase HM by another 2c. i was informed by someone else i was doing that wrong and they told me to do the increase by 5c on HM everytime my vapor temp dropped 0.5c. i made a pass one time like this as well but i did so with a heating pad on distillation head because i thought the room temperature was condensing my vapors in the head before they could reach the temp probe. however i do believe i shouldnt have put the heating pad on my distillation head, regardless my biggest problem of barely any yield and ample material left over in HM still presented itself after the run.,) meanwhile vacuum level is still under 130 micron, 40-80 micron on a good day. so i continue this process until i get to about 190-200c on the HM. thru this whole thing my Vapor temp never gets above 100c and its like I’m getting bits of terps, heads, and tails, but no mains, all mixed in hence bad separation, correct? and definitely not much of a yield or purity. all distillate recovered so far has seem to have had another oil or liquid in the distillate as well and thats where my first problem comes in, the separation but as stated above i do believe i may have fixed that but i havent tested it yet…

my real issue is the lack of distillate im yielding by the end of it. yes i want pure product but i know i cant be doing this right with hat much starting material left over in the hm.
well thats my issue. i’m barely getting any yield. from a 700-1k mL start, i probably end up distilling a total of 200- 300 ml, with roughly 60-80% of my original starting material still remaining in the HM flask. what am i doing wrong?

thank you for all and any help,
Take care every1

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Are you seeing distillate condense in the head before its reached your condenser?

Is your setup wrapped with some kind of insulation?

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It’s doubtful you’re getting tails mixed with your heads.

Probably just all heads.

Your mantle, and ambient conditions can all be playing a part in what your mantle temp actually reads.

Try just increasing heat slowly until your body comes through.

I’m anywhere from 195-225c on the mantle temperature, pending on the system I’m running.

Hell… I’ve ran some stubborn gross shit at 255+ before, you’ll get some degredation at those temps, but that might just be what you’ll need pending on the grade of your starting crude.

I’d say just slowly increase heat and see.

Is your head jacketed/vaccuum jacketed?

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This^^^

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i have heat wrap rope on most poft of the mantle every run… first two runs i had nothing on distillation head, this last run i also put a heating pad on distillation head but that left me with no view to see the head, so as of now no i havent seen distillate condense in the head, i also havent noticed much reflux either the first two times.

thank you for your time and advice sir

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you think probably just all heads really?

on the prior runs when my heating mantle is anywhere from 120c to 190c i get a orangish/yellow color and the color does go from say orangish, to a darker color orangish, to dark, than seems to lighten up and be a nice opaque kind of color and i get a few drops of that and than i slowly starting getting a greener color. in my last run i did get HM to 216-217c and it was also my first time keeping a heating pad on the head the whole run. with the heating pad wrapped on distillation head just last run, starting vapor temp was 69c and towards 200c-210-c on HM, i seen vapor temp go up to 140c-170c. but as i mentioned i dont think putting the heating pad on the distillation head is the correct answer for this problem, i couldnt see my reflux, if i had any at all cause heating pad blocked my view of the head…

just curious. what the normal ambient temp typically you have seen any results with if i may ask?

Whats slowly?
i mentioned that in the description above, i increased relatively slow on my first run, (i increased it by 2c from 120c every time the HM point value hit my set value, so HM is at 120c, i set it to 122c, HM hits 122c so ill bump HM to 124c, HM hits 124c, i bump HM to 126, and so on.) but when i did my vapor temp never got above 30c… i assumed my pump was pumping the vapor out faster than it could load in the head…? (just so all info is disclosed, my pump does about 15L a minute if i remember correctly off top of my head, but i dont see truly how that would be an issue either but i just dont know)

Thank you for your time and the help sir.

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Try swapping out vapor head temp probe. Always make sure your temp probes are proper.

What stir bar speeds are you running?

Try setting up everything and doing a dry run. Pull your deepest vac and seal it up (blank off valve) and let it sit for about 2 hours and see if the vac depths drop.

Try using a stainless scrubbie in the head (loosely packed…just need to simulate a more aggressive vigouroux style). A pic of your head would help. A pic of your overall set up would help.

Also… are you running winterized material? The heat loss from “burning” off lipids and waxes would definitely interfere with distillation.

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Agreed.

What’s your starting material like? A bunch of junk in there can certainly interfere.

Can you send some photos of your head? You might need to wrap it in a pad or tinfoil or something, but generally the vacuum jacket on there should be enough insulation.

Just keep upping your temperature a bit when stuff stops coming out and see if another fraction comes out. Maybe it’ll be at 220, or 225.

Is your thermometer inside your flask? Or outside?

(My tails don’t distill until the main body is done, just because of how physics/distillation works… So there’s likely a near 0% chance you’d be mixing heads an tails, rather than heads and main body or something).

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I think op is still too low in temp. A lot of times my main won’t come off until 215-220 on a first run distillation.

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Hell, if it’s in a cold lab, low grade crude, and I didn’t have a jacketed head it might be 230+

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I have a cold lab and unjacketed head. The low grade crude would certainly add to that.:joy:

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Had he shown us pics of the crude?

If there is any amount of particulate present it makes it damn near impossible to distill at reasonable Temps (below 220C)

While ramping up I started at 165 and would check every 15 minutes and ramp when the reactivity stopped. I’d ramp 2-5C every time until the heads fractions were passed. Then. Then I’d let 50 grams of the body pass to ensure a clean cut . So I could clearly assess the activity I would use a heat lamp positioned just a few inches from the top of the head until I got the reactivity I sought. Then I’d turn the lamp off and wrap the head.

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*ok ill double check my head probe.
*my stir speeds start at 300 and i go to about 400, havent really needed to go any faster seeing as my material tends to stop distilling lol
*i have done a dry run but i didnt let it sit for to long, ill double check it tho for 2hours or so before next run.
*i just inserted a few more rings after my last pass but havent ran it since. technically i have about 4-5 therotical plates in my distillation head now, i believe.
*ill get pictures up today
*yes, as far as i was informed the material has been throughly winterized. and from my experience and from my visual inspection of the material i do believe it has been winterized.

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*starting material EHO crude oil, winterized,
*yes i can post pictures of it today. the heads jacketed, first two runs i didnt cover the head andthe average ambient starting vapor temp of 14-17c. the third time i had a heat pad wrapped all the way around it with a starting ambient vapor temp of 69-70c. i currently have distillation head wrapped in thin layer of foil with lil windows cut out for me to see head.
*220-225c, really? lol ive got it to 217-219c once but i didnt want to go much higher. any idea what the standard safety temp rating is on a 2l double neck round bottom ?
*HM thermometer is inside 2l flask making contact with my starting material.
*any idea why im getting light gold/orangish colors on heating mantle from 120c-200c with opaque and clear color at certain points and than towards 195c-217c i get alot of green?

thank you!

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thank you btw

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really? that seems hella crazy. dam lol guess ima have to ramp it up and find out

thank you man

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yes the lab tends to be chilly, the crude seems to be fine but i cant say 100% truly cause i didnt make it. and the distillation head is jacketed but not vacuum jacket. (i do believe thats not so great when its chiily cause id imagine the colder room temperature on the outside of the head is taking some effect on the air inside that would normally be a lil wamer thru heating up the HM and a warmer work atmosphere. but just an observation and assumption of mine)

thank you bud

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That sounds like you are going from volatiles into heads. There is a reason they call heads fools gold. Very difficult to visually see the difference between trash and THC. Vapor temp of THC should 180C I think, been awhile since I have used a probe.

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*may i ask how cold your lab tends to be? what temps do you normally see on the HM when the mains start to distill?

Thank you sir

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*ill post pics of crude soon
*what are you referring to when you say “reactivity”? (reflux, distillation,…)
*just curious but when about in the process did you find yourself turning the heat lamp on?

Thank you!