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How long does it usually take to distill?

BigJohnny

BigJohnny

Member
A question I probably should've asked back when I started, but also a topic I can't recall ever seeing mentioned....

But how long on average would it take to distill filtered/winterized BHO?

Lastnight I put my first fully winterized batch (1200g) into my distiller and over the course of about an hour I slowly brought the temperature up to 236F where I was starting to get a good reaction in the head but it wasn't boiling over into the condenser.

I get to the point it's looking like it's done with the heads, and the distillate is looking nice and yellow with good clarity so I rotate the cow.

Fast forward 6 hours later from this point and I'm still collecting hearts, up to maybe 250-300g in my collection flask, and still have a load flask full of what must be around 900g....it's 3am at this point and I have no choice but to shut it down and let it cool before I crash and fall asleep.



Is this a normal amount of time, or am I waaaaaayyyyyyyy off base here?
 
HashoftheTitans

HashoftheTitans

Member
BigJohnny said:
A question I probably should've asked back when I started, but also a topic I can't recall ever seeing mentioned....

But how long on average would it take to distill filtered/winterized BHO?

Lastnight I put my first fully winterized batch (1200g) into my distiller and over the course of about an hour I slowly brought the temperature up to 236F where I was starting to get a good reaction in the head but it wasn't boiling over into the condenser.

I get to the point it's looking like it's done with the heads, and the distillate is looking nice and yellow with good clarity so I rotate the cow.

Fast forward 6 hours later from this point and I'm still collecting hearts, up to maybe 250-300g in my collection flask, and still have a load flask full of what must be around 900g....it's 3am at this point and I have no choice but to shut it down and let it cool before I crash and fall asleep.



Is this a normal amount of time, or am I waaaaaayyyyyyyy off base here?
Click to expand...
That temp is pretty high leading me to believe that you aren't pulling a deep enough vacuum. Terps or solvent in your pump oil is a possibility. Also, make sure you aren't losing vac to your hoses. Grease your joints with krytox gpl207. First pass should come out from 200-225C and second pass at 190-210C. Also make sure any cold trap being used is empty when doing your main body.
 
HashoftheTitans

HashoftheTitans

Member
Krytox GPL207 has a higher heat tolerance. Dow high vacuum grease is silicone based and is not rated for temperatures that you will see during cannabis distillation which can contaminate your product.
 
WaterFarmFan

WaterFarmFan

Active member
Veteran
HashoftheTitans said:
Krytox GPL207 has a higher heat tolerance. Dow high vacuum grease is silicone based and is not rated for temperatures that you will see during cannabis distillation which can contaminate your product.
Click to expand...

Thanks. Is this still the best if you are using a lower temperature range (ie not short path) to cold boil off ethanol? What about grease for very low temperature (<-60C) cold trap pieces?
 
BigJohnny

BigJohnny

Member
HashoftheTitans said:
That temp is pretty high leading me to believe that you aren't pulling a deep enough vacuum. Terps or solvent in your pump oil is a possibility. Also, make sure you aren't losing vac to your hoses. Grease your joints with krytox gpl207. First pass should come out from 200-225C and second pass at 190-210C. Also make sure any cold trap being used is empty when doing your main body.
Click to expand...


Are you talking about mantle temperature or head temperature?

I'll have to double check my vac lines, they should be sealed though but it seems ive been having problems in this regard.

I've completely flushed my pump with fresh oil, so I'll haveto double check some other things I think.
 
A

Alister.Frazzle

New member
Totally depends on equipment, although that does sound slow. I assume you have at least a 2L boiling flask for a 1200g load. I run a 5L LabSociety double-head unit and during my first pass usually distill at 200-250g/hour, once I hit the main body. Usually run a little cooler and slower on 2nd pass, ~100-150g/hr. You can always turn up the heat to speed things up, but at your temperature thc degradation is likely.
 
G.O. Joe

G.O. Joe

Well-known member
Veteran
Is it possible that the upper part of your evaporator is acting as a condenser? The Krytox may be high temperature but I could find no vapor pressure data for it because it isn't sold as a vacuum grease. The LVP is their high vacuum grease.
 
SkyHighLer

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Alister.Frazzle said:
Totally depends on equipment, although that does sound slow. I assume you have at least a 2L boiling flask for a 1200g load. I run a 5L LabSociety double-head unit and during my first pass usually distill at 200-250g/hour, once I hit the main body. Usually run a little cooler and slower on 2nd pass, ~100-150g/hr. You can always turn up the heat to speed things up, but at your temperature thc degradation is likely.
Click to expand...

Looking at the picture of that system, I see two head thermocouples, where are they taking the flask temperature to send to the controller? The pictures of their other systems show a thermocouple extending down into the flask which is connected to the controller.

You guys should take note, Lab Society's mantles are up to double the wattage found in many other packages. That's the point I've been trying to get across, use an oversized heater, and dial it down with a power regulator who's output is then controlled to limit temperature.

Doing some further experiments, I found the outside bottom the vessel to track exactly at the boiling point of the contents, but when you really start pilling on the power to the heater the outside bottom of the vessel will track several degrees high, while the inside bottom of the vessel and the contents will remain exactly at the Bp. Get a fast reading thermocouple down into the solution, the insulation just slides off common K thermocouples, strip one, and insert it through a stopper.

https://labsociety.com/lab-equipment/g2-short-path-distillation-kit-12l/

https://labsociety.com/lab-equipment/g2-short-path-distillation-kit-5l/


Here's is one of Auberins power regulator/temperature limiters, way less expensive than the J-KEM or Glas-Col devices.

https://www.auberins.com/index.php?main_page=product_info&cPath=53&products_id=559


I use a Variac as the power regulator, and temperature limit it with a separate controller that has PID, on/off limit, and cutoff limit functions. The advantage of the Variac is it's ability to over-volt up to 130%, that means it will drive your heater/mantle at up to 130% of it normal wattage rating.
 
Last edited:
BigJohnny

BigJohnny

Member
I have a thermocouple in the head, and also have one that extends into the flask.

At this point I'm going to have to assume my vacuum level is what's causing me my problems.

before making some changes to mysetup I was able to pull a vacuum down below 100 microns near the middle/end of the distillation, but never saw any vac level this low before that point.


As of now I don't seem to be able to get any lower than 1200 microns


in both cases I've started the same way.

Load collection flask with bho, pull vac as low as it will go then start heating it up.

previously I would get down to around 640 microns before starting the mantle heating.
now it'll only go down to about 1600 microns.....


Somewhere I've fucked up, and even using gum rubber tubing and a proper cold trap from summit. I can't figure out where I'd be leaking...... looks like I'm going to be running some tests today.
 
F

flatslabs

Member
The thermometer adapter is a common source of leaks, put a glass stopper in your head and flask and see if you can pull lower.
 
G

Goldleaflabs

Member
G.O. Joe said:
Is it possible that the upper part of your evaporator is acting as a condenser? The Krytox may be high temperature but I could find no vapor pressure data for it because it isn't sold as a vacuum grease. The LVP is their high vacuum grease.
Click to expand...
Thank you for this! I try and tell everyone that GPL is for bearings and what not. LVP is their only "vacuum grease"
Summit sells everyone the GPL and it's literally impossible to correct him.
 
HashoftheTitans

HashoftheTitans

Member
Goldleaflabs said:
Thank you for this! I try and tell everyone that GPL is for bearings and what not. LVP is their only "vacuum grease"
Summit sells everyone the GPL and it's literally impossible to correct him.
Click to expand...

I saw that on IG. I was just going to look into this because summit isn't the only one pushing GPL. Thanks for the correction, fellas.
 
WaterFarmFan

WaterFarmFan

Active member
Veteran
BigJohnny said:
I have a thermocouple in the head, and also have one that extends into the flask.

At this point I'm going to have to assume my vacuum level is what's causing me my problems.

before making some changes to mysetup I was able to pull a vacuum down below 100 microns near the middle/end of the distillation, but never saw any vac level this low before that point.


As of now I don't seem to be able to get any lower than 1200 microns


in both cases I've started the same way.

Load collection flask with bho, pull vac as low as it will go then start heating it up.

previously I would get down to around 640 microns before starting the mantle heating.
now it'll only go down to about 1600 microns.....


Somewhere I've fucked up, and even using gum rubber tubing and a proper cold trap from summit. I can't figure out where I'd be leaking...... looks like I'm going to be running some tests today.
Click to expand...

Just curious. What kind of pump are you using?
 
O

Old Gold

Active member
Your vacuum levels sound similar to mine, but my gauge is knowingly inaccurate. It shows about 200 microns when it should read only 5 microns. Regardless, I usually distill the first pass right around 1000 microns (as per my gauge), and sometimes as high as 1200 like you. The second or third pass will always be in the 650-800 micron range for me. I had a run in which the thermometer adapter o-ring deformed mid-run somehow, and I was seeing about 1700 microns. If you are used to seeing 640 microns with no volatiles off-gassing, then you probably have a leak whenever you can't get close to that pressure (mind you that the first pass always has the highest pressure).

Anytime I've had a leak during a run, even if I only have to ramp the temperature up by 5-10 degrees, the flow rate drops SIGNIFICANTLY. What usually takes me about 4-5 hours was taking easily 8 or 9.

How often do you change your pump oil? Can you see any distillate residue in the oil chamber?

I'm going to guess that the 0.9 cfm that the DuoSeal pumps is one reason your runs are slow. The other reason is probably the 24mm glass joints and distillation head being restrictive in surface area. My pump pulls 14.6 cfm and it still takes me 4-6 hrs to distill 1000g in a 2L flask. I can push the flow rate higher but at the sacrifice of quality.
 
BigJohnny

BigJohnny

Member
I got to fucking around with it lastnight, and went from vac pump -> brass bulkhead through table -> gum rubber hose to vac controller -> gum rubber hose from vac controller to cold trap -> cold trap to my Omega DVG4 and I capped off the other side of the gauge.


setup like this I was able to pull down to 340 microns according to my DVG, but my J-kem says it was at around 0.8 torr if i recall correctly. The two gauges definitly don't match up and if I switch the DVG units to torr I get two completely different readings between the gauge and the controller.

I hadn't been cleanign my oil very frequently, but earlier this week I flushed the shit out of the pump by pouring oil into the inlet and flushing it through the system to the bottom drain plug.
This oil was horrible and nasty, so I kept flushing it until the oil came out clear, ran it for a bit and flushed it again.... basically went through 4L of oil to flush it out.

I changed the oil again lastnight and it smelled like absolute shit, but wasn't filthy.


The only thing that's different now compared to about 2 months ago is that I replaced BVV's cold trap with summits custom cold trap, added the vac regulator and switch to gum rubber hose over the PVC(I think) hose with metal wire wound through it. I still only use a small piece of that to go from the pump to the bulkhead.

but a couple of months ago I was easily able to do a distillation of unfiltered/winterized BHO and pull the vac down to around 90 microns nearing the end of the distillation.


Now I'm using fully winterized BHO, made very few changes to the system and now I'm seeing shitty vac levels.


This basically has me pulling my hair out at this point.
 
HashoftheTitans

HashoftheTitans

Member
BigJohnny said:
I got to fucking around with it lastnight, and went from vac pump -> brass bulkhead through table -> gum rubber hose to vac controller -> gum rubber hose from vac controller to cold trap -> cold trap to my Omega DVG4 and I capped off the other side of the gauge.


setup like this I was able to pull down to 340 microns according to my DVG, but my J-kem says it was at around 0.8 torr if i recall correctly. The two gauges definitly don't match up and if I switch the DVG units to torr I get two completely different readings between the gauge and the controller.

I hadn't been cleanign my oil very frequently, but earlier this week I flushed the shit out of the pump by pouring oil into the inlet and flushing it through the system to the bottom drain plug.
This oil was horrible and nasty, so I kept flushing it until the oil came out clear, ran it for a bit and flushed it again.... basically went through 4L of oil to flush it out.

I changed the oil again lastnight and it smelled like absolute shit, but wasn't filthy.


The only thing that's different now compared to about 2 months ago is that I replaced BVV's cold trap with summits custom cold trap, added the vac regulator and switch to gum rubber hose over the PVC(I think) hose with metal wire wound through it. I still only use a small piece of that to go from the pump to the bulkhead.

but a couple of months ago I was easily able to do a distillation of unfiltered/winterized BHO and pull the vac down to around 90 microns nearing the end of the distillation.


Now I'm using fully winterized BHO, made very few changes to the system and now I'm seeing shitty vac levels.


This basically has me pulling my hair out at this point.
Click to expand...
Dirty hoses can do this. Gum rubber absorbs more terps than silione or PTFE and of course, stainless bellows. Try replacing your hoses.
 
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