bho, winterizing ... still no shatter :(

[Graywolf]

trying it out... my aluminum 20qt pot folded on me during testing and I don't even think it was full vac. still need a gauge so I have no idea if its pulling full vac. back with more pics

Might I suggest a ball valve between the pump and the chamber, so when you shut it off, it won't aspirate oil from the pump crankcase.

 

[montanamike1]

Greywolf is absolutely the person to talk to on this, the rest of us are just amateurs, but I'll repeat what's been said in a more comprehensive manner. My $.02 is that you are not heating up your solution uniformly to a high enough heat for a long enough period of time. Even though the water you add is 115, the temperature of your solution in the glass container will be far, far below this, especially if you are trying to evaporate a thick layer of solvent. Try adding much hotter water; I pour water that's just below boiling from my electric tea kettle into a pyrex dish and then float the pyrex dish with the solution on top of that. I keep changing the water until the reactions are mostly completed, at which point I take it to the vac-purge chamber for 10 mins, scrape it out of the pyrex and transfer to parchment paper, and re-purge for another 10 mins. Shatter *almost* every time.

Don't forget that you need a THIN layer of solution on the bottom of your pyrex dish to allow the most even, complete evaporation of your solvent. Often large growers blast too much solution into a single dish and cannot effectively purge it afterwards; for large runs use large containers or many small ones.

 

[connoisseurde420]

Might I suggest a ball valve between the pump and the chamber, so when you shut it off, it won't aspirate oil from the pump crankcase.

the ball valve is there I just put it right next to the pump. please excuse my shady craftmanship I was in a hurry to see how it works. Pretty sure its close to full vac there's a good amount of action when I vac purge. next step is a vac meter.

I read a lot of your posts and remember you saying something about oil coming back thru the system so I made sure to put a ball valve.

 

[connoisseurde420]

thanks for all the replies guys. when I really make shatter I'm going to shit my pants. I'll take a pic. :p. but seriously. I use a griddle that keeps the inside of Pyrex 115-120 with parchment on top of that (making absolute). my initial purge is done in the same fashion. I dont add water it stays hot continuously. I have a infared to be sure of temps.

so just to be sure here's all the things I have tried. old trim. newly dried trim (5-7 days). fresh frozen taken from my ice hash stash. always a thin film no more than a oz in 7x13 pan. vac and no vac. 10-15 different strains. 5 different butanes confirmed to be good. ALL BUTTER/WAX

things I may be doing wrong. filtering absolute while solution is cold. not adding enough ethanol. too hot, a couple time in the 130-150 range before I was using vac tho so no terp loss really. please don't give up on me lol. I'm going to a DIY with lots of pics but not till I come out with shatter. but I must say I love the butter that I have been coming out with! just wish it was clear..

Greywolf is absolutely the person to talk to on this, the rest of us are just amateurs, but I'll repeat what's been said in a more comprehensive manner. My $.02 is that you are not heating up your solution uniformly to a high enough heat for a long enough period of time. Even though the water you add is 115, the temperature of your solution in the glass container will be far, far below this, especially if you are trying to evaporate a thick layer of solvent. Try adding much hotter water; I pour water that's just below boiling from my electric tea kettle into a pyrex dish and then float the pyrex dish with the solution on top of that. I keep changing the water until the reactions are mostly completed, at which point I take it to the vac-purge chamber for 10 mins, scrape it out of the pyrex and transfer to parchment paper, and re-purge for another 10 mins. Shatter *almost* every time.

Don't forget that you need a THIN layer of solution on the bottom of your pyrex dish to allow the most even, complete evaporation of your solvent. Often large growers blast too much solution into a single dish and cannot effectively purge it afterwards; for large runs use large containers or many small ones.

 

[connoisseurde420]

well guys today I made progress. let me tell Ya exactly how it went down...


I have some blue dream trim/lower nug I need to use for edibles. thought I might blast them and use the oil instead. fir the practice for me and oil is really easy to cook with. awesome.

I didn't measure shit. should probably try just to see but I usually measure efficiency by how much I get per can. I average 2g per on trim/nug mixes. this batch I froze in the open not a closed bag only for a few hours in a sub zero fridge. the trim was pretty dry but not older than a month. I didn't break it down to crumbles like I usually do just packed it lightly with my fingers enough to pack it down some. one unbleached coffe filter and one can of butane thru small glass extractor in to small round Pyrex in water at 115. Pyrex 109-100. scrape to parchmentbas soon as liquid butane was gone but still bubbling. in to vac chamber with same temps as before. start purge, watch muffin till I see no more action. take oil out and smash. repeat vac, muffin, smush till nothin happens under vac. got 1.8 g after I dabbed a dunk. tube could have been fuller?

the improvement? it has a nice glittery shine I haven't seen before. smells better than anything that I've produced before def more terp retention. to top it all off I got shatter consistency. looks goopy but it snaps off. this tells me if I winterize it maybe clear shatter? idk. going to run some more and do a gram or so just to see....

must say that I am convinced fresh or semi dry frozen trim is the way to go. I see a big difference. low temps with a vac makes the proces less than a hour for what I did. mmaking up to a half would take about the same time I think.

keep you posted on the winterizing ... here's a picture of my efforts. the first is afterbtwo or three short burst in the vac chamber. the second is when it was being smoked on already haha. thanks all for the guidance.


I

 

[Watashi420]

Hi Connoissuer, It looks like you have the same vacuum pump I do from harbor freight. Does yours smoke a lot out of the black crankcase vent (where you fill the oil)?

Also I use the same Pan/plexiglass setup, would me not having a ball valve be causing me to get contaminants into the BHO from the crankcase oil vapor? I still get a bit of sparky sizzle when I heat my purged oil.

 

[connoisseurde420]

hey man I'm no expert but I'm learning...pretty sure it shouldn't sizzle mine never does

yes it is possible to suck back oil from the compressor after you pull a vac either sitting or trying to take lid off.. my compressor was not smoking at first and worked fine till I added all that oil they give you and woila! there's oil clouds everywhere. It takes many hours but it will burn off. Don't think it needs much oil to run...

 

[stevyjaytoday]

I have a very strong feeling that the vacuum pump you are using may be the culprit. Those pumps are junk, they do not pull a tight enough vacuum.. You get what you pay for, a good pump will cost you $200++, i personally wouldnt use that pump, robinair makes a good one, jb eliminator pumps are great

 

[Graywolf]

Hi Connoissuer, It looks like you have the same vacuum pump I do from harbor freight. Does yours smoke a lot out of the black crankcase vent (where you fill the oil)?

Also I use the same Pan/plexiglass setup, would me not having a ball valve be causing me to get contaminants into the BHO from the crankcase oil vapor? I still get a bit of sparky sizzle when I heat my purged oil.

Sliding vane rotary vane vacuum pumps put oil vapors out their exchausts.

If you don't have a valve between the pump and the chamber, when you shut off the pump, it will suck the crankcase oil backwards into the chamber. Always close the valve before shutting off the pump, and always start the pump before opening the valve.

 

[connoisseurde420]

thanks greywolf always giving a detailed explanation.

I'm going to do some runs tomorrow, I will post some pics of the process I have come to use. Hopefully one of them will be a clear shatter.. still have only achieved blonde shatter up to this point.

 

[cctt]

Greywolf, I read on your site that two-stage pumps will pull too much vacuum and boil off cannabinoids. Does this mean they're not suitable for this job, or is there a way to limit the vacuum in the chamber to the desired pressure?

 

[Graywolf]

Greywolf, I read on your site that two-stage pumps will pull too much vacuum and boil off cannabinoids. Does this mean they're not suitable for this job, or is there a way to limit the vacuum in the chamber to the desired pressure?

Even a single stage will pull below 100 microns, but with either, you can crack your back fill valve, and control the pressure by bleeding in air. The air will also act like a gas ballast and help keep the solvent fumes cleared from the vacuum pump crankcase.

 

[SkyHighLer]

Greywolf, I read on your site that two-stage pumps will pull too much vacuum and boil off cannabinoids. Does this mean they're not suitable for this job, or is there a way to limit the vacuum in the chamber to the desired pressure?

Both one and two stage rotary vane vacuum pumps have the ability to boil off the the good oil components, an accurate dial gauge will suffice to stop at the desired vacuum level. Graywolf's lately been suggesting 115F @ -29.5" Hg and my research backs this up 100%. To clarify, this is 115F down to (and no further down than) -29.5" Hg. Dial vacuum gauges read about 1" Hg high for every thousand feet of elevation. For example, at a thousand feet instead of -29.9" Hg the needle will indicate -28.9" Hg.

How to test and recalibrate dial vacuum gauges by comparing the observed boiling point of water under vacuum to the standard boiling point of water under vacuum.

Place a half a glass of water in the chamber, note it's temperature. Take the pressure down slowly, just until the water starts to rapidly boil, valve off, tap the gauge down (they tend to stick,) and note the dial's reading. Compare the dial's vacuum reading and the water temperature noted earlier to the standard, here's a reference: http://www.jbind.com/pdf/Cross-Reference-of-Boiling-Temps.pdf

To recalibrate the scale of your dial gauge, repeat the above at various water temperatures and either place a piece of tape on the dial to record the correct pressure readings or make a table showing "if the dial reads this, it's actually this.."
52F H2O boils at -29.5" Hg

Here's the boiling points under vacuum data for what you're trying to remove, butane and water, and what you're trying to preserve, the phytocannabinoids, terpenoid essential oils, flavonoids, and phytosterol components. The first to boil off of the good components is ß-caryophyllene, Boiling point: 119*C / 246.2 degree Fahrenheit, Properties: Antiinflammatory, Cytoprotective (gastric mucosa), Antimalarial.

Boiling point under vacuum calculator http://www.trimen.pl/witek/calculators/wrzenie.html
(The enthalpy of vaporization value for delta-9 THC is 66.49 kJ/mol)

 

[Nuggatron3k]

I'm curious as to what you come up with. I'm sort of in the same boat as you and have been following closely. I get my gauge right at -28.9 but I'm almost 1000Ft of elevation so i think this must be ok. Temp is always proper but I should probably winterize. I've been following skunkpharm closely too (truly a big help).

I was wondering though...does it matter whether you winterize before or after hitting the vac chamber? I have been running on pirex transferring to vac. running the vac til it gets all tane out and terp bubbles are left. then i winterize then i hit the vac chamber again to remove the solvent. It appears to be ok, although it looks to be a little on the greener side with these last few runs. I'll snap some pics for yall to see

 

[Graywolf]

No need to vacuum before adding the alcohol. It will leave with the alcohol.

 

[connoisseurde420]

I think the green is clorophyl that can be broken down with some time in the sun before you put it in the freezer

 

[connoisseurde420]

going to try another run...

 

[connoisseurde420]

omg so many different textures I got this time. ran all different strains. only one came out clear but I think the material was decarb a bit because its A bit runny still even after 30-40 min vac time. going to winterize most of these so here's some before shots..

 

[connoisseurde420]

my next batch of trim I'm going to freeze the same day it come down so I know for sure! it was not decarb. also to keep the leaf from breaking down so much depositing more waxes than necessary.

 

[connoisseurde420]

could anyone chime in about straining the winterized oil? it takes forever pouring just a small amount at a time, letting it filter thru and coming back to freezer to do it all over again.

skunkpharm suggests using a buchner funnel, one that uses vacuum to help speed filtering oils and whatever else. any suggestions or things I should keep in mind while buying? don't necessarily need a website but it would be nice :o





thanks