Hey folk, brand new to distillation here. I recently borrowed a cheap SPD from a friend and have been giving it a go with my limited knowledge. I already know multiple things I need to correct from spending hours reading on this site, just wondering if someone can fill me in on how to proceed with the current issue I’m facing.
So, I poured my last runs mains into the same jar as the run before and was gonna do a second pass with both runs combined but once everything settled there is a noticeable separation in the two runs. The first run(bottom) looks more normal and clear while the second run(top) appears cloudy. Neither run had a proper winterization and they were slightly different starting materials. Could this be caused by excess fats/lipids in the top layer?
I know there could multiple different issues with my process as I’m still figuring this all out just wondering what my next move should be? What would you assume caused this? Should I winterize this jar before proceeding to do a second pass? Or can this be corrected with a proper second pass?
You’re on the right track. It looks like fats that need to be winterized out. There’s a fine line where only a few percentages of fats can totally cloud your first pass
It’s possible that it’s heads contamination. If both batches were prepared the same way, and only one is cloudy that is further evidence that you didn’t pull all the heads in the one distillation that is cloudy. I had a similar issue where I ended up with cloudy distillate and was unsure if it was lipids or heads. I extract in cold ethanol (-80 to -60C) so I was skeptical that it was fats. I ended up doing a 2nd pass it it cleared right up, so I’m pretty confident my issue was heads contamination. Here is that thread, it has a lot of pictures, if you scroll down a bit:
Yours looks a bit different than mine did tho. Did you save your heads fraction? Was it cloudy? Can you take a picture of it?
These are from two consecutive runs so were poured into the jar at different times.
I’m sure there could be head in there. I’m still learning how to do this right and the small amount of info given to me by my friend was sub par at best. He told me to run my condenser with ice water for the first fraction then move to the mains once the dripping turned into a stream and then warm the condenser from that point on. So the “heads” I’ve been collecting have all been non-viscous terps and water. From there I’ve waited a bit once the dripping turned more into a stream To clear the condenser then switched to my mains flask and turned up the condenser temp.
Does that all seem right? The more I’ve been reading it seems most keep the condenser warmer from the start and most of the terp/water collects in the cold trap?
@tetramethylsilane, reading thru your thread a bit I noticed someone talking about vac grease. I suspect it’s possible that could have made it in there as well as I’m pretty sure I’ve been greasing my joints improperly. If that were the case is there any way to remedy that?
I think grease contamination can look differently depending on the grease and conditions. When I had grease contamination it globbed up as you can see in the picture. What I did was pull the glob out with a metal spatula and then re distilled the material. That cleared it up and it looks fine, but I am waiting to have it tested on a GCMS just to make sure there are not traces.
There are a good few threads on grease contamination and remediation, where people have proposed other solutions. Apparently an ultrasonic bath can cause grease to coagulate and float to top of distillate.
Yeah, you don’t need much grease. For some joints you don’t need any at all - look up using distillate as grease with or without PTFE sleeves. If you use grease, just spread it thin on the upper half or so of the joint. And when assembled twist a bit.
Your pic looks too cloudy to be due to grease alone imo.
The latter heads portion can be pretty thick. Not as much as cannabinoid distillate, but thicker than the first stuff out of the condenser. When you say stream, you mean a continuous line from the outlet of condenser to wherever it hits? Did it coil?
More or less what you describe sounds right. At what vapor temp and vac depth did you switch to mains?
What you describe at the end of that post is hot condenser method which is a whole different style.
It actually dripped from the condenser on this last run(cloudy run) while previous runs produced a stream from the condenser. This last one dripped from the condenser for the whole run and only made a stream and very tiny spiral as it fell into the collecting flask. I also ran a larger amount of crude on this last one as well and noticed some of the reflux making its way up and into my condenser. I understand that’s not a good thing. Could that have contributed to that impurity? Also didn’t decarb this last run as well so could that be causing the reflux to make it into the condenser? Not sure what my actual vac depth is as I only have an analog gauge on there for now until I can afford a digital gauge(previous owner wasn’t using a vac gauge at all, smh) I know this is bad practice and a analog gauge will not cut it but just working with what I was given and hopefully can get the proper gear soon.
Your main fraction dripped the entire time? Depending on how hot your condenser is, and how hot your mantle is, cannabinoid distillate can drip rather than string/coil as it falls.
Yeah, actually when I had this issue I had run a lot more crude than normal, so my boiling flask was more full than any time previously. I think this probably contributed. Other people have noticed this too if I recall from my searching - large amount in boiling flask, greater chance of heads contamination.
Ah, definitely decarb before doing SPD. I would expect that to look more like bumping than reflux tho.
I wouldn’t rule out the possibility that it’s just heads contamination which can be remedied by a 2nd pass taking it nice and slow thru heads. But as was recommended, I would try to winterize a small amount of your cloudy distillate first and see if you get any precipitate. I am not super well versed in winterization since I extract cold enough not to really have to worry about it. But I would dissolve some in ethanol (1g in 5g ethanol or more using the same ratio) and stick it in the freezer like what @AlexSiegel said . If you get precipitate you’ll need to winterize the batch. If you don’t get a precipitate you may want to get some dry ice and try winterizing at colder temp. Or if you have methanol, you’ll get more precipitate at warmer temps.
Well damn… bout had me convinced on the heads theory but I just checked my pour out of the tails from the same run and the same thing is happening there, separate cloudy layer on top.
Thinking the starting material used may have something to do with it now.
Curious what the BP of plant waxes/lipids/fats are and if they are contributing to the cloudiness because the material from previous runs seemed to be a cleaner extract.
And yes I prob mean bumping, not reflux? Haha, still learning all the terminology when it comes to SPD
Do the cloudy heads and hearts fractions have a similar odor?
What about the cloudy tails fraction?
1 way to tell the difference between insufficient winterization and poorly cut fractions is the nose on the heads hearts and tails. Another indicator is pigment.
Poorly cut fractions of hearts with heads still present will be cloudy AND a special sour scent of fucking awful. Heads can also create a deep blue, green or neon yellow haze.
Tails odor is quite different. It smells like extra spicy rubber tires burning. Tails also carries deep red translucent streaks. Not the opaque colors in the heads.
