Sugar instead of shatter


#1

First off, greetings! Finally making a post on my favorite site! Need the help of those more wise and experienced than I…

The help I’m seeking is for a serious problem with sugar forming instead of shatter, and though I have surely read the answer to my problem on here, for some reason I am unable to crack the case.

I am starting with a subzero scientific extractor, running trim, with a co2 material column chill. We started using ntane, but have now switched to 70/30 isotane/pro blend. (Thought it may be a leaner option for nucleation problems). We thought there may be water in the solvent, so we sent it on a dry run over fresh beads 3 times, in an attempt to dry it out, though it didn’t solve our problem.

Our process is to bring the extractor to temperature. First by adding liquid co2 to the material columns, starting our denatured alcohol/ dry ice coils to temp, as well as getting our hot water bath for the honeypot to temp.

Then we take the material and put it in the material columns to start bringing actual material to desired cold temperature. (we used to cryo freeze overnight the next days material, but after considering the possibility of moisture buildup in the cryo freezer, we stopped doing that)

After the material has been inside for about 20 minutes, we begin the soak for about 10-20 minutes. As the solvent leaves the fuel tank, it passes through two coils to chill the solvent before entering the material column.
We soak the material about 20 minutes then nitrogen assist into the collection chamber, where we have the temp set currently at 115f. We have ran that at verious temps from 78 up to 120*f. As one column empties, we switch to the next one, and when we estimate the running column to be about half empty, we refill the empty column, and back a forth until both material columns have had two flushes.

Towards the end of the process, we recollect down to a vacuum of 10lbs, then pour. To pour, we usually have to nitrogen assist it out with between 5-10 psi depending on material because of vacuum. We have a spout at the bottom of the honeypot that we pour out of, our honey pot is permanently mounted to the rack system that support the extractor. Our extractor is outside on a wood platform with a tent around it. Because we are outside in the cold and humidity, we pour 2-4 oz sheet as quickly as possible to avoid condensation as much as we can.

Once out of the extractor, we take it to the garage that has been walled in half. The tent is connected to the front of the garage, to a walled off car door opening that has man doors to enter the tent through. We walk through the front room of the garage that is closed off, into the back of the room that is closed off and usually 60*f with 30% humidity. This is where the vac ovens are. I know the vac ovens are key.

We have tried purges that range from 82-88* with full vac, to a preheat at 120 til it’s liquid, then full vac down to -29.5. Once the vac is achieved, lower temp for remainder of purge to 94, and to be frank, everything in between.

Just to name a few…

A
1-set slab in oven at 85f, no vacuum. leave for 1 hr.
2- pull to 10lbs, leave for 15 min
3- pull to 17lbs, leave for 15
4-pull to 20lbs, leave for 15
5-pull to 23lbs, leaave for 20
6-pull to 26lbs, leave for 20
7-leave at 26lbs, change temp to 86, then every hour to hour and a half, raise temp 1 degree, sugar at 89…

B
1-set slab in oven at 120 for 25 min, no vac
2-pull full vac until activity become minimal, til you get those turp bubbles.
3-once full vac is achieved (29.5 inches at 1100ft ?), lower temp to 94 degrees.

left this MAYBE 12 hrs, nucleation appeared

C
1-set slab in oven, immediately pull full vac, oven preheated to 90f.

overnight nucleation (14 hrs)

D
1- preheat oven to 91, leave slab in without vacuum for 1 hr.
2-pull vac to 13 lbs for 20 min
3-pull vac to 20 lbs for 20 min
4-pull vac to 25 lbs for 20 min
5-pull vac to 27.5 lbs for duration

then raise temp by 1 degree every 2 hours or so to pop bubbles… sugar.

These are but a few we have tried…

I have tried cleaning out material sock by loading them in my extractor and then doing a dry run full of bags.

I have switched filters in event of contamination

I have done dry runs with fresh beads to dry out my solvent

i have cryo frozen material and left it at room temp going in

i have tried every variation of purge times and temps i can think of.

last october i had no problem making shatter, and when we ran live resin, and got into fresh harvest, everything we have ran since has sugared. We have dismantled the extractor, cleaned it, and put it together. Dry runs to make sure we didn’t miss any…

PLEASE SOMEONE, ROCK MY WORLD WITH SOME KNOWLEDGE.

For the record, i prefer the sugar wax, but the people holding the cash don’t, and i somehow cant make the shatter. With the cold weather also came the sugar. Thats why we walled of our space and added the heater and dehumidifier, because naturally, that was my first thought, but the slabs are in uncontrolled circumstances for less that 5 minutes, straight into the back room.

I’m not sure if i’m getting fuel from a shit company or if its my procedures that are the problem… I am open to ideas, can run some sop’s, but typically, we don’t make it out more than 12 hours before nucleation…

I’m looking for my obwan kanobi!


#2

What strains are you processing?

What brand ovens do you have?

How much solvent is left in the mix before you nitro it out? Is it thick oil or is it runny liquid?


#3

strains that have sugared…
lemon larry OG
pineapple OG
pink lemonade
lemon kush
lemon chemdog
lemon jager
gorilla glue
magnum opus

all of them…

Oven, we have 1.9 AI all the way around, with an edwards xds10I pump.

As far as how much solvent, not sure on actual numbers, but we have tried purging to syrup that barely comes out, but with the iso pro, more often than not, its foam. I know im trying to avoid agitation, but if it won’t come out… We have been trying to let it heat a little further in the honeypot, but that makes the foaming worse…


#4

i should also say that when we were getting our incredible shatter last fall, it looked like canned foam coming out…

my sop used to be BASICALLY what @HanSan was minus the flips, just left it in for 4 days, always made good…


#5

While your collection base is filled with saturated solvent and begins to creep towards being super saturated, try stirring/ agitating your warm collection pot. You need to force whats crashing out to remain in a homogeneous solution.

This is much easier to do when open blasting. You could drain your saturated solvent into a big steel pot and operate under strict hazardous material guidelines. I know some people are gonna think im crazy here telling you to open blast but i am probably the biggest open blast advocate on here. It helps you learn if youre smart. If you blow yourself up maybe youre not so smart…

That being said: wear appropriate clothing, keep everything vented by being OUTSIDE ONLY, dont use ANY electronics near you. Only use explosion proof fan if needed.


#6

so just to make sure i understand what your saying, you think there is a possibility that in my honeypot things are crashing out… though my honeypot is set at over 100f, that doesn’t mean my actual material is warm. Thats why i turned up the temp, and though the machine moves faster, i figured my material, at least until it reaches super saturation, should actually be close to the solvents boiling point… am i correct in assuming that? The reason i ask is because with ntane boiling at 32f, i would have assumed that isn’t quite cold enough to crash out, 0 degrees with iso/pro i could see that being a problem then… my extractor is fixed state, so there isn’t really a way to agitate…

So when it basically starts leaving oil on the side walls, dump it and just let it off gas?

ext


#7

Id keep it agitating as it off gases. Or if you have a honey pot (collection vessel) that you can pick up, you can give it a few swirls to encourage blending.

Your solution should be crystal clear and not cloudy


#8

Warm water bath helps with that instead of stirring manually about 90 f keeps the tane moving and speeds up recovery


#9

I like your input on this, i might need to start bouling down futher then adding tane to my jars afterwards like i use to do


#10

Right but that has diminishing effeciveness. As you heat more youre becoming more saturated. We are trying to redissolve completely. I am assuming the micro crystals are being formed in the extraction column. But hey i may just be making an ass out out u and me by assume-ing lol


#11

@sonicgardens
so 120 may be too high… i steadily declined bath temp trying to preserve terpenes (not knowing at the time they are a solvent, killing my shatter) and all the way from 120 to 78 i was still getting sugar…

@Apothecary36
I thought agitation was the enemy in making shatter… with enough solvent will that make the agitation less impactful?


#12

Lol. I have been pulling my pot out of the water earlier to have a higher saturation for dimond and have noticed less stable products.


#13

That sounds alot like how i have always done it


#14

also i pour onto parchment paper, so too liquid is a bad thing, but to fix the problem i will adapt


#15

What temps are you running your tane and materials at


#16

I do also


#17

material columns are chilled with liquid co2, and my solvents go through a denatured alc-dry ice slurry cold injection coil, one for each column… i don’t know, but pretty cold on the temp, should be at least -50f i would guess.
Material, i was cryo freezing in the column socks at -80c and -60c… saw some stuff suggestion you can go too cold, so now i just pack socks at room temp, throw in columns for 15-20 minutes before soak…


#18

Your temps are definitely playing a roll, along with moisture. Especially your oven temps


#19

I prepack columbs on dry ice the night before. My tane is alot colder. Is your tane bottle that cold also


#20

Glad you are chimming in. Im running out if questions to ask. Im thinking its the exteaction process