Currently running my first spd. Questions as I go


#61

Yea at this point I’m in no rush at all. I’m going to very very slowly ramp up my temps and let it sit there until I seem vacuum stabilization/drop. If I see my vac jump way up, and then start to come down I assume I’m on the right path. Mantle is back on, and we’re back in the game


#62

What vacuum pump are you running? Was your material decarbed fully prior to loading the SPD? Is there residual solvent from evaporation remaining, and do you know roughly how much?


#63

keep going, the vaccum will improve when once you remove the lower volitiles.


#64

I’m running a welch duoseal 1400… after winterizing, it was ran through a rotovap… I put the compound in a vac oven to remove any leftover solvent and started decarbing altho I can’t guarentee it was fully decarbed. Decarbing is still a science I’m not 1000% sure on. But I did my best to “clean” the compound before the spd. Although as of now I’m seeing better results. Slowly ramping temps, vacuum stopped climbing. Head temp slowly rising. I guess I just got spooked the first time around lol


#65

Maybe not by your side but we are there :+1:


#66

I swear I’m paypaling all of you crackas breakfast when I succeed lmao


#67

:joy::joy::joy::joy::joy:


#68

The good news is I brought enough peanut butter and jelly supplies to the lab for 3 days, and I got the hound here supervising…


#69

Mantle reading is 123. Head temp reads 44.6. Vac at 2660 micron. And I started to get some VERY light dripping, reddish color but I think that might be from my last run, as I saw a little red on the tip going into the cow. I’m keeping a record every 4 minutes lol


#70

Microns started to drop, but so has head temp.
Mantle-136
Head-34.5
Micron-1960

Should the head temp be dropping?
Time to jack up mantle?


#71

hey man, this is a great way to learn! keep goin!


#72

So, microns are dropping rapidly, and the head temp shot from 33 to 98 real quick, and I have a very steady dripping coming out now. Check out the numbers!
S=set point on mantle
P= Current mantle temp
H=head temp
M=microns

Look at that crazy change at the bottom of my notes



#73

#74

My plan is to follow what I believe soxhlet said way earlier. Bring my head to 140-150. Wait for it to stop dripping. Bring it up to 160ish and prepare to rotate. My only real worry at this moment is recognizing the change from head to main


#75

I will say I’m absolutely noticing the relevance to everything. I’m observing what numbErs are going up or down, and what the correlate to. Aka, I feel like I’m seeing and making sense of things changing!


#76

I decarb on a hot plate at 145C, it doesn’t take long and there’s minimal if any conversion to CBN and no detectable isomerization. A big factor in the fluctuation in vacuum depth that you’re seeing now is because your solution has to decarb first which is generating a lot of vapor as the Carbon and Oxygen (carboxyl group) make their way out of the system as vapor. I would suspect additional low boiling points like residual solvent and water, which is expected, but can be partially alleviated by decarbing first.


#77

Decarbing is my next big thing to learn/nail down for sure!
Little update, I figured by showing my numbers minute by minute it’s easy to follow what I’m doing


#78

I’m actually getting excited because things are starting to make sense. Head temp starts to fall, I jack up mantle a few degrees, head goes up and a little higher than before. Vacuum is down to 480 from 2100 starting. It’s just cool to see things directly reacting predictably. Head temp is nearing 140 so I guess I’m gearing up for shit to get real lol

I’m going to attempt to get the drip to stop by holding head temp at 140-150. I believe around 160 my thc should start rolling out. Any more suggestions of visual indicators that it’s time to rotate flasks? I’m getting slow dripping of light yellow watery liquid at 129 head temp currently


#79

You’re probably going to be closer to 200-210 based on what you’ve mentioned of your vacuum previously in the thread, but it’ll be fun to watch things change as you pass the 160C barrier.


#80

My head temp started to hit 160 and I got shook and lowered my mantle a bit. I was trying to hold it between 140-150 to Kill off that first reaction. Currently I’m juggling it between 135-150. Just nervous about changing flasks at the right time. Its hard to know what to look for if I’ve never seen it.