The Clear .............Thread!

[mobin]

I have installed all stainless steel bellows and keep polymer hose to a few inches at the coupling points and the vscuum achieved went from the readins you mention including the leak down check as you cite, to meauring with a Pirani sensor near the point of distillaiton a vacuum of .00075 Torr (no typo). That also is stated as three quarters of one micron. A Pirani sensor typically cannot measure any lower.

In the video I demonstrate the problem with my HVAC gauge and not the piranni sensor from my vacuubrand.

where are you taking your pressure readings from? like where is the gauge in the system?

 

[SkyHighLer]

100 microns is much too high. I distill at three quarters of one micron and the temperatures measured at the glass on top of the flask are typically around 150C when distillate begins to form in the collection flask. You must not use polymer vacuum line except in very short pieces.

Attempting molecular distillation at pressures exceeding the very deep vacuum demonstrated in the video means the temperatures to achieve phase changes needed for distillation are geometrically higher. Although in this configuration the extract is not measured directly, the thermocouple is positioned on top of the flask at the neck and is a good rough estimate of extract distillation temp although the temp is likely somewhat higher. I just got a flask that will allow direct measurement in the flask, and along with a needle valve to micro adjust the vacuum I plan to produce a pressure and boiling point curve.

My initial computations using a single point conversion chart give a crude estimate of room pressure boiling point of somewhere approaching 500C, although it is a certainty that thermal breakdown would play a significant role. My full spherical mantle has an ultimate rating of 400C and must be set hotter than the boiling point. Using the single point chart to estimate temps, I estimate that at some point around 75 microns that the temp needed in my the boiling flask would exceed the safety limits of the mantle.

This video is only an attempt to demonstrate how I personally accomplish short path distillation. I have seen no other online example of anyme accomplishing deep vaccum molecular distillation like this and certainly not at the reduced temp and pressures easily obtainable with an appropriately sized and plumned up vacuum system.
https://www.youtube.com/watch?v=D-A-ZsU8ZxQ

I have one of those <$20 dual input K thermocouple thermometers,

http://www.ebay.com/itm/Dual-Channe...e=STRK:MEBIDX:IT&_trksid=p2060353.m2749.l2649


From watching the videos I perceive two areas you're not fully down with yet, the best sensor(s) location and means of heat conduction, and using a PID controller alone to control the action.

If you have the time and patience continue comparing temperature readings at multiple locations. And if you want to take the temperature of the glass you need to firmly attach the naked sensor bead directly to the glass, a drop of J-B Weld or there are products designed specifically for the purpose,

http://www.omega.com/temperature/pdf/OB_OMEGABOND_AIR_SET.pdf


The second area is turning up the set point on a PID controller past where you want and putting up with the results... as an experiment, get a 110V/20A Variac off of eBay for <$100, and limit the wattage instead of the temperature, if you like it you can combine it with your temperature controller.

Nice work!!

 

[jaybodankly]

I got trim and dont want to squish with a hair thing. I would like to learn and work on short path distillation. Found this glassware set on Amazon.
Laboy HMK3101 Glass Chemistry Lab Glassware Distillation Kit 24/40 Distilling Apparatus
https://www.amazon.com/gp/product/B018EFMBJU/ref=ox_sc_act_title_3?smid=ATVPDKIKX0DER&psc=1

I know I would need other parts. Is this junk or can I make it work small scale? This is not a commercial level production. Just a guy who wants to use up some trim and learn about chemistry. If you need to drop a lot of cash to play I understand. Thanks

 

[mobin]

I got trim and dont want to squish with a hair thing. I would like to learn and work on short path distillation. Found this glassware set on Amazon.
Laboy HMK3101 Glass Chemistry Lab Glassware Distillation Kit 24/40 Distilling Apparatus
https://www.amazon.com/gp/product/B018EFMBJU/ref=ox_sc_act_title_3?smid=ATVPDKIKX0DER&psc=1

I know I would need other parts. Is this junk or can I make it work small scale? This is not a commercial level production. Just a guy who wants to use up some trim and learn about chemistry. If you need to drop a lot of cash to play I understand. Thanks

i've made good distillate 90%+d9 with laboy glass.

i'd say for a around $1k you could have a functional setup that would be a great foundation to build on.

you can really stretch a dollar on craigslist and ebay finding deals on used equipment.

if you're gonna wait on china shipping, might as well wait for pieces that will work a lil bit better. get a jacketed head, helps things run a bit faster/smoother https://www.ebay.com/itm/24-40-14-2...606527?hash=item35e86b343f:g:XwAAAOSwZKBZLrOS

 

[jaybodankly]

Thanks. So, I should get the Amazon kit and swap out the head with the ebay one?

 

[mobin]

Thanks. So, I should get the Amazon kit and swap out the head with the ebay one?

if i were you ya i'd grab that head, a 3way distribution adapter, a few vacuum take off adapters for use as "monocows", and a ton of 50ml collection flasks. your mantle size will determine your load flask size and a 250 or 500ml stirring mantle is all you need. SEOH on amazon has mantles for cheap. They also have a ton of cheap glassware if not everything you need but the head.

ebay search with "us only" and within xxx miles helps with getting things within the week.

the glassware and the pump are cheap, it's all the little shit that you'll find you NEED that will nickle and dime you continuously. I've never stopped collecting new pieces and still always find more to need.



for "small" batches one thing i learned was to never go too small. there are inevitable losses here and there that will really take the blood outta your dick. run 20-50g clean crude at a minimum!

 

[jaybodankly]

How does this list look so far?

1-24/40,Three way Glass adapter,75 degree bent,distillation head

6-50ml single neck round bottom flask,heavy wall,with 24/40 joint

2-Single Neck,250ml,24/40,Round bottom Glass boiling bottle. *Should this be a double neck with thermometer insert?

2- 24/40,Glass Adapter,With Ground Cone & Scock,PTFE Stopcock,

1-24/40,14/20,Jacket Distillation Head Short Path Condenser,Plastic Hose Adapter

Like you said I also need some Keck clips, Vac lube, clamp, stand, bottle brushes etc.

 

[mobin]

How does this list look so far?

1-24/40,Three way Glass adapter,75 degree bent,distillation head

6-50ml single neck round bottom flask,heavy wall,with 24/40 joint

2-Single Neck,250ml,24/40,Round bottom Glass boiling bottle. *Should this be a double neck with thermometer insert?

2- 24/40,Glass Adapter,With Ground Cone & Scock,PTFE Stopcock,

1-24/40,14/20,Jacket Distillation Head Short Path Condenser,Plastic Hose Adapter

Like you said I also need some Keck clips, Vac lube, clamp, stand, bottle brushes etc.

that should get you somewhere for now!

 

[jaybodankly]

Thanks for pointing me in the right direction Mobin.<br>

 

[jaybodankly]

With that head you dont use a vacuum? I dont see the vac port on it. Sorry, if it is a basic question.

 

[mobin]

With that head you dont use a vacuum? I dont see the vac port on it. Sorry, if it is a basic question.

basic shit right lol. good thing someone's paying attention. yes you'll want a receiver/cow with vac port

 

[jaybodankly]

Cool, same head just add a 3 port cow with vac port.

 

[mobin]

Cool, same head just add a 3 port cow with vac port.

yep. and vacuum take off adapters for when you just need one receiver and dont want so much prep/cleanup.

 

[jaybodankly]

OK, Should have all the parts and pieces in a month.

 

[jaybodankly]

Last question I think for a bit. I have a 1/4 hp vacuum pump, 5Pa. Will that be enough or do I need to look at bigger pump?

 

[mobin]

Last question I think for a bit. I have a 1/4 hp vacuum pump, 5Pa. Will that be enough or do I need to look at bigger pump?

ya vacuum becomes pretty important. check out the thread a few down with waterfarmfan.

 

[thump easy]

Just don't expose the absorbents and cannabinoids together to temps above 100°C.
never throw it in the boiling flask. For best results reflux carbon/clay/cannabinoids dissolved in ethanol at 80°C for 30 or more mins.
Also a little tip:
dont use alcohol and silicas together. You should always use a non-polar solvent with silica. It will help pull the more polar compounds out like pesticides

Gold leaf labs so your saying non polar like hexane for silica in a one wash and charcole with ethenol? all in diffent times meaning 2 diffrent times once hex is cleaned out or vise versa??

 

[thump easy]

Holy macanole talk about seizing the fucken head.. And i mean that in a bad way it took me 10.5 hours of trying to unsieze the head only if my chick was that lucky never ever fucken not put grease on that shit man luuuuuube for realz i called and researched like crazzy im supprizef it finally came loose....Fuuuucccckkk!lube for life

 

[negative37dBA]

Like to ask some questions if I could. Working in a lab trying to learn as much as I can from the "master extractor" and finding he does not know it all.....or is not willing to show me he does. Trying to fix some stuff he did.
We received some water hash that was very wet, he just put it straight into ethanol for winterization with out drying. I thought that was not going to fly. He then filtered it, evaped the ethanol and tried to process to clear...failure big time. He said oh it must have too much water, we need to dry it...lol. So now I have this black plastic like substance in the boiling flask I am wondering what to do with and wanting to know if drying the water hash first is the way to go? I started a comparison with 200 grams of bubble that was dry, it is now winterizing so it will be a bit before I can find out. Can I even skip the winterization? Help/ideas would be appreciated.
Thanks so much, negative

 

[BlackestofOps]

Anyone having testing labs returning erroneous results with distillate that is very pure? I am distilling with a spinning band system. Based on my run data and the yield figures combined with the input material potency, my math says that my distillate is in the 90% cannabinoid range. Twice now, labs have returned results that show 40% range, on different batches. This makes no sense, since my input oil is 60-70% cannabinoid, my pot leftovers are dark green/black, and redistillation on the poorly tested material goes exactly as you'd expect for a second pass on very pure input: very fast and nothing left in the boiling flask.