I make terrible distillate....why?

help
distillation
distillate

#1

I’ve been (trying) to make distillate for years, but everything I make just comes out dark, and reddish, like dark rum coloured.

Basically I think I’m an idiot an unable to do this right.

I start with my BHO, and put it into ethanol (10:1) stick it in the freezer then filter the next day through Summits stage one filters.

Back into the freezer again, and then I’ll filter through stage 2 and 3.

Once that filtering is done I do a carbon scrub then rotovap and distill.

but even after the carbon the ethanol/BHO is super dark (dark rum coloured) and has a red tint to it.

When distilling it ends up taking about 6 hours and even the distillate comes out dark, red and smelling like rubber.

yesterday I tried using bentonite after the 3rd stage filtering and before the carbon…and still no god damn change…it still looks just as dark but maybe MAYBE just slightly more clear.

Can anybody help identify wtf I’ve been doing wrong for 3 years?!!?

I have videos on my youtube channel if anyone wants to take a look and maybe identify any of the things I’m doing wrong or ways to improve. That’s the whole reason I started the channel and posting vids, but that hasn’t helped thusly. It’s MedEx Cannabis Lab on YouTube.


How to get rid of rubber smell in distillate
What should I change, bad results!
#2

Your videos were the base for my first distillation. I can’t tell you how many times I’ve watched your videos before I attempted this. Thanks.

What I noticed about what you do. Is you vacuum levels are always pretty high when you start. I didn’t hear you mention about decarbing your oil either.

Welcome buddy. Thanks a ton for YouTube channel. I hope you figure this out.


#3

I am an extreme newb to disty here but I just checked out a vid of one of your runs. Your SPD head appears to be flooding or overcome with crude. Are you running your SPD with too little vacuum and too high of heat?


#4

Ahh, it’s BigJohnny from ICMAG Forums, I was just going to suggest you come over here for help.

It could be your filtering procedures, but burned rubber smell is most likely too high a boiling rate, which is usually brought on by not getting the vacuum down low enough.

Are you still using the BVV stirrer/mantle? If so, I suggest bypassing the PID controller and feeding the mantle with a power regulator, be it a simple $40 Variac (10 amp) or any of the other options I came up with in my thread titled “Distillation controllers with both temperature and power control.”

You simply open up the base of the stirrer/mantle, disconnect the leads to the mantle, and connect a couple of wires leading to the outside where you can plug them into the Variac. Plug the Variac into a Kill-A-Watt power meter so you can monitor exactly what wattage produces what boiling rate.

A quote from a quote in my controller thread,

"Now on to the kind of controller like I said this is not about the best controller. It’s about what that controller needs to be able to do for you. The controller needs to be able to adjust the amount of heat being put into the boiler. In a steady variable amount you want the heat to be as steady as possible. You do not want it cycling on and off wildly. If cycle times are more than say one time a second. It’s more than likely not a good choice because every time it cycles on more vapors are created. Then when it cycles off no vapors are created and you get surging. It would be like if you were trying to use a hose and your kid was around the corner pinching off the hose and laughing at you because the hose sprays then shuts off, then sprays and shuts off again. This variance in vapor amounts can and will wreak havoc on the still operation causing surging which in turn will cause smearing of the heads hearts and tails and it can give you false readings on a thermometer in a reflux column.

The other thing you do not want is a controller that works off of temps. A thermostat controller or PID controller (without manual mode) are examples. First off we can’t control a still by boiler temp. As it will be ever changing and these types of controllers cycle very widely. They reach the set temp while at full power then shut off all power till the temp drops below the lower setting which is usually a long time span. Since it’s trying to control temps and you are trying to control amounts of vapor produced the temp settings usually get set high so you get really long surges of full power heat. All this creates bad surging within the still and the same holds true as stated above about the surging."

Another quote from a quote,

gonzo
“I find a variac gives me the best temperature control and the most even heating, far above a PID which is above a dimmer. A guy from california is selling a good variac for 38$ shipped, I got his 46$ version (10amp).”

BTW, BigJohnny just posted this up at ICMAG Forums, maybe you guys could help him out over here,

"Bentonite clay, how to use it?
basic question, how do you use the clay to clarify distillate?

after winterizing and filtering out the waxes through 3 stages, do you just add clay into the ethanol/bho solution and mix under heat for a little while?

How much clay is added to the solution?"


#5

Already threw him a lifeline over there, and told him about this site in a PM yesterday. I’ll send him out celite 545 and aluminum oxide if he needs.


#6

Your video guided me through my first run. Thank you so much!


#7

My best advice is get a good vacuum pump that can go below 20micron during distillation. Don’t go over 210c. Follow the breakingdabs hot condenser tech.

I always give it a second pass with a hot condenser to get rid of all smell.


#8

I don’t think it has anything to do with your pre-processing. You need to focus your efforts on the distillation side. The dark color is due to it being a first pass which is normal, this is because the bandwidth of the crude is still very complex so it’s very easy for other compounds to co-distill with your Cannabinoid fraction even if you have tight tollerences on your fractions (which I think need some work as well). If your second pass is also coming out dark, it may be due to the type of crude you are using, but I’ll bet money that you will see a substantial improvement by studying up on distillation parameters.
Here are some tips:
We need to know what’s going on in the system during your runs in order to coach you properly - it’s important to have accurate data reading equipment: 1. Thermal probes: In-boiling flask to measure boiling temp and in the head to measure vapor temperature. This, along with visual ques and vac levels should tell you approximately which fraction your in. 2. You need to have accurate vacuum readouts - it doesn’t really matter where you place your in-system sensor (before the cold trap or after the cold trap), you just need to correlate the vac depth to the other parameters to understand where you are in the process. I always keep one sensor before the cold trap (La Society’s heads have a vac port right at the condenser discharge) and one directly at the pump. This allows me to understand if the pump is experiencing vapor load which means I need to wait to increase mantle temps or invest in more cold trapping power. Ideally you want your pump at it’s ultimate vac point as much as possible when you have your bleed valve completely shut (usually 4-20 microns).
It’s important to keep a log as you progress through your distillation IE Time. Mantle Set Temp. Mantle Actual Temp. Stir RPM, Vapor Temp. In-system Vac, Pump Vac. And Visual comments. Here’s a pic of one of my guys doing this prior to popping the main THC fraction:

SPD Distillation Worksheet.pdf (102.3 KB)

Edit: Attaching the PDF version of the worksheet - do a few runs with it and post your results with pictures at every stage of the process :slight_smile:


#9

I don’t have much time to reply here, but I doubt I’ll be doing any more runs after this most recent one. If I do it won’t likely be for a very long while.


#10

That sucks cause I learned a lot from what you shared and think the people here can really get you on the right path.


#11

God now I feel so damn lucky to have produced beautiful light colored 93% distillate my first run. I had half a day training and some simple direction and got lucky i suppose. I just remember slow and steady was my teachers moto. Shit my vac debth wasn’t even that low at 2200 because I only had a simple Welch pump. I still can’t get my vac debth under 300 but I’m about to have my pumps rebuilt. It’s funny the more I’ve learned from this site seems like the harder it’s become lol. Doing all these other steps and using more filterents I never did my first run. Beginners luck I suppose.

Ps I wish there were more videos out there showing more step by step. There really isn’t any that walk you all the way through it and learning has been a bitch. I am thankful for Everyone willing to help here.


#12

The rubber smell is from gums degrading at high temp this is commonly known in the veg oil refining there is a tone of info on this in the video and on the web. https://youtu.be/F71jVjBK6FU
These practices should be done before distilling
Also you need a better head that one clogs and increases run times decreaces yeild dracticly. Further pesticides can cause smell and can be concentrated in distillate by a azatropic bond . there is alot of info here about that thxs to @Future. Dont use vac grease ever again use ptfe plumbers tape start at bottom and go up to top one layer . god speed


#13

You want to focus in the alkaline chemical refining in the video thats your ticket. As the professor stats it removes more phopinoids the compounds you are tageting not so much the ffas that physical is best at.


#14

I think butane is part of the problem as well. Most are starting with xold ethonal less unwanted xompunds i dont trust butane its dangerous and dirty.


#16

Take your first pass smelly crap dissolve in heptane 3:1. Mix up a shit tone of water and wash in with diffrent ph water from 4-10 some say make the water saltly idk you tell me what works better. Occasonally put metal work prob into top of sep funnel to get probe wet with heptane solution wait to dry smell if residue is gone. After last wash drain solution and run threw magsil pr or is on a budget maybe just silica? Then distill. Again smell gone. If you dont have enough first pass around downsize boiling flask one size could work?


#17

so what is the hot condenser tech. I can’t seem to find any info on it.


#18

Run your condenser hot so volities will be rejected to the cold trap.


#19

Set your condenser temperature 30°C colder than your head temps durring main body. The idea is that the cannabinoid fraction is the only thing distilling up and out as a liquid - alot of the nasty trash that co-distills with the cannabinoid fraction will stay in vapor form (because the condenser is too hot for it to turn liquid and fall into the receiving flask with the distillate). This will allow for water solubles, gums, and sometimes lipids to bypass the receiving flask and condense later in the system (like in your cold trap).
I definitely won’t recommend anyone preform this method unless you have the proper full-bore system - systems with vac hoses will get clogged to shit. Also because we are talking about condenser temps in excess of 135°C - you will need to get a suitable oil reciruclator w/silicone oil which has a high smoke point as well as high temp GL-connections and PTFE lines.
Take a look at the third video in this post and turn on volume:

Cheers!


#20

Jesus, I can’t get my chiller that high and there’s no way I can spend money (I’m quite literally broke) to buy a new one, or new hoses, or silicone oil or anything of that nature.

That being said, What should my maximum mantle temperature be? I find that when I get to about 200C I won’t have any reaction and the head temp just goes up a bit, and then down and tends to stay around something like 60C or less.

Should I be waiting when this happens? because I’ve waited upwards of an hour before and still seen no reaction, and the head temps staying the same or lower than 60C.

I’ll be distilling some stuff tomorrow I think maybe and I’ll record the process so everyone can watch me fuck it all up.


#21

Why dont you do a thread live or post it in here and lets see if we can help. i kept my mantle at 217-220c during all my thc…it just kept dumping gold till about 170c head temp…then the red came in. I cut the run at 175C

Also, i seen where your head plugs like mine does. As @Roguelab instructed me…have a heat gun close to unclog the plug and your head temp wont fluctuate. Come on bro…lets get you dialed in. Start posting up your info.

Im sure your still using the holstrum…im sure your oil is fully dewaxed cause ive seen your process. How are you decarbing your material?

Here is what i followed…this is from the Good life gang sop. All props to Future and the GLG. This is not my procedure but it what i followed as these people are smarter than me.

|b.|Place decarboxylation vessel in convection oven or on stirring heat plate|
|c.|Bring solution to 120c for 45-60 minutes (until large bubbles cease)(Stir if possible)|
|d.|Devolatilization (Optional): Increase temperature to 140c for 10-15 minutes until small bubbles cease|
|e.|Allow temperature to decrease to less than 70c|
|f.|Pour resin into SPD boiling flask or Wiped Film feed container|