Building an IC Clearinator

[queequeg152]

Also the 22L heating mantel is on the watched supplies list. It's is actually the only piece of equipment listed according to the AG.

thats hilarious, i didnt know that.

how fucking stupid.

what about oil and sand baths?

heating mantles are just fiberglass sheathed nicrome heating wire sewn together with nomex or fiberglass thread. you insulate the back side with rockwool or glass wool and a nomex jacket on the outside.

people make these things all the time for 1 off apparatus's and fancy column heaters... shit like that.

any idiot could build a heating mantle, even a large 22l mantle in a weekend. a good seamstress or upholstering person could do it in far less time.

 

[queequeg152]

lol elemental iodine is 'watched' to... yet nothing said about salts of iodine.

oxidation of iodide to elemental iodine is like a 5th grade home school chemistry experiment. wtf are they trying to accomplish?

 

[Sunfire]

nothing. they work fine. you might have trouble getting parts, but otherwise it will work fine.

if you can afford it, id suggest buying a used buchi machine and getting Chinese glass(if its missing pieces)... the resale value on a no name piece of equipment is always dog shit.

there is really no such thing as 'bad' lab glass... just too thin, or improperly binned pieces. Its all going to be boro glass... they might even be using the same suppliers that more reputable companies use.

glassware with bubbles is supposed to be discarded, and possibly recycled. you might find that a cheaper brand allows small imperfections like this. FWIW a bubble isnt a huge deal on something like a recieving flask thats not subjected to temperature stresses, but generally speaking your boiling flasks should be perfect and free of chips everwhere except the GG joint lips.

what do you even want a rotovap for btw?

As a lamp worker using boro for over a decade I would have to strongly disagree. Just like everything else we use such as viton and ovens, different components and process make different quality. Just because it's "boro" doesn't make it all on the same level of quality.

Chinese glass is shit and I'll never buy it, it's 1/3 the price of quality czech or American glass.

Even raw Chinese tubes and rods have mad jmperfections. Changes in thickness and not being properly annealed can cause issues. That's why bubbles are bad because there's a dramatic change in thickness.

This is all a matter of perspective though because as you pointed it, it's all about coefficiency of expansion related to heat changes. Slow and small heat changes would be fine. When annealing, 400F and 900F are the danger zones but I'm sure you guys arnt going anywhere near 400F.

Just be careful with the Chinese glass. It's cheap for a reason.

 

[queequeg152]

without getting into details, let me just say that ive first hand experiance with plenty of chinise made lab glassware and its comparable in every way to the likes of name brand pieces like kimax pyrex shott etc.

im assuming your experiences are typical of the cheapest possible glass. im sure if you were to seek out something other than cheap as possible you would find that quality is more or less comparable.

 

[Sunfire]

Lol bro, much love right, but I'm telling you, I've done it all. Simax, pyrex, both of the schott glass, Chinex, and more.

No I don't seek out the cheapest glass which is what i said earlier. I don't buy schott, not even their "artistic" glass and I don't buy Chinese either. I can get Chinese glass for 1.50$ per pound but I'll gladly play 6 or 7 per pound for Simax or pyrex. I forget the name of the cheap schott, not the artistic, I can get that for 1 dollar per pound.

I'm just trying to add perspective, you have personal experience using glass, I have personal experience making and working glass. There's a company near by in grass valley that makes scientific glass ware and a friend of mine who's been blowing glass since 1996 has made all sorts of everything, including scientific glass. Neither of them would ever use Chinese glass, mainly because it's harder to work and more delicate and it would suck to ruin a piece you've worked on all day or multiple days, right at the end, cause you had shitty glass.

I personally know, first hand, the quality of the actual raw material, not the finished product. Like I said, different perspectives. You have experience with the finished product, I have experience with the raw material, LOTS of experience. Please believe me Chinese glass is so inferior, as I said, I'll gladly pay 4 times the price, however I do get great deals on simax from one guy, like 3.50 a pound.

As I said though perspective, I totally believe you have mad experience using the equipment. I totally believe for the application of it making clear oil, the Chinese glass will be fine because your really not using that much heat. All i wanted to suggest was be careful, don't ramp up or down temps too fast. I'm sure since you have experience you know how to treat it, this is for mainly other people who don't have that experience.

Considering the viton/gasket thread going on, I just wanted to say it's the same thing with glass.

 

[queequeg152]

Lol bro, much love right, but I'm telling you, I've done it all. Simax, pyrex, both of the schott glass, Chinex, and more.

No I don't seek out the cheapest glass which is what i said earlier. I don't buy schott, not even their "artistic" glass and I don't buy Chinese either. I can get Chinese glass for 1.50$ per pound but I'll gladly play 6 or 7 per pound for Simax or pyrex. I forget the name of the cheap schott, not the artistic, I can get that for 1 dollar per pound.

I'm just trying to add perspective, you have personal experience using glass, I have personal experience making and working glass. There's a company near by in grass valley that makes scientific glass ware and a friend of mine who's been blowing glass since 1996 has made all sorts of everything, including scientific glass. Neither of them would ever use Chinese glass, mainly because it's harder to work and more delicate and it would suck to ruin a piece you've worked on all day or multiple days, right at the end, cause you had shitty glass.

I personally know, first hand, the quality of the actual raw material, not the finished product. Like I said, different perspectives. You have experience with the finished product, I have experience with the raw material, LOTS of experience. Please believe me Chinese glass is so inferior, as I said, I'll gladly pay 4 times the price, however I do get great deals on simax from one guy, like 3.50 a pound.

As I said though perspective, I totally believe you have mad experience using the equipment. I totally believe for the application of it making clear oil, the Chinese glass will be fine because your really not using that much heat. All i wanted to suggest was be careful, don't ramp up or down temps too fast. I'm sure since you have experience you know how to treat it, this is for mainly other people who don't have that experience.

Considering the viton/gasket thread going on, I just wanted to say it's the same thing with glass.

well, im not going to try an argue with an actual glass blower, so ill take your word for what you are saying.
my understanding was that boro glass, like steel alloys can be ordered in what ever ASTM specifications you like.

people said the same things about chinise plywood for years... yea their cheap, sold in home depot ply was and still is dog shit... but that does not mean you cant get super high quality plywood from china, the 200 dollar per sheet plyboo products are supposed to be fantastic.

 

[Sunfire]

200 dollars per sheet wtf?!?!? Omg!

Whoa that's crazy I've never heard of astm specs for boro. Hmmm must be a scientific glass thing? I mean I guess a manufacturer could dial in different COE parameters, but idk myself really. Typical good boro is 32 coe. That stuff can take a lot of abuse. The cheaper stuff I'm sure gets closer to 40 coe or even higher, and is a bitch to work with bigger pieces.

I think the Chinese lab glass is fine for the temps and applications for clerinators. I just wanted to add some perspective as far as glass quality, cause that's about all I can add to this thread as I watch it daily but have no clue what you guys are talking about half the time.

 

[queequeg152]

200 dollars per sheet wtf?!?!? Omg!

yea, but think cabinet doors and fine quality furniture though. not subfloor material.

its beautiful stuff really, and very labor intensive to build, it a lumber core plywood too, so its pretty stable.

200 dollars is not out of line for very high quality plywood btw. euro ply ranges from like... 120 - 200 bucks for fine triple A quality veneer.

there are ASTM specs for all sorts of shit.

http://www.astm.org/Standards/E438.htm

 

[Sunfire]

Yeah when they say class A-low expansion borosilicate, that's the coe.

Low I never even heard of two of those tests before. That's just hilarious! As one of the tests indicate, annealing is important, cheap glass may not be annealed well because large kilns suck up a lot of power and a proper annealing process for larger pieces is long and requires a fuzzy logic pid. Good kilns with those programs are expensive in themselves too, like a grand per cubic foot. All factors that go into quality glass.

Oh well idk you were talking about finish grade sheet, shit I bet there's way more expensive and fancy rare woods.

I'm always de railing threads. Sorry guys. Back to the clear. I might give alpine a shot if I can get a good deal.

 

[hobb3s93]

anyone have any new insight into the process?
i just got my short path head and everything today...
i distilled out all of the clear liquid which im guessing was a mix of ethanol ,water and terps.
once it stopped dripping clear liquid into my receiving flask i swiveled over to next flask.

after that i coudnt pull anything into my fresh receiving flask, the starting flask had a lot of vapor floating around but seemed to just be recondensing and running down the sides of my starting flask.

any one have any insight as to what i should try differently tomorrow?
i started temps around 180 but got them up to 300 on the hopes of boiling off thc and recondensing it into a frsh receiving flask.

definetly think i extracted alot of terps who room stank aswell as my hands upon disassembly

 

[queequeg152]

proper instrumentation imo is vital in experimentation...
do you have a micron gauge hooked up to this thing?

how cold is your condenser?

you might try a very gentle heating at atmospheric pressures, then ramp up the vacuum, then ramp up the heat.

a sublimation trap prior to your vacuum pump is not a bad idea either.

might want to wrap the boiling flask and vapor tube in foil for a bit of extra heat retention. there should be no air currents on the apparatus.

do you have any pictures of this setup?

 

[hobb3s93]

proper instrumentation imo is vital in experimentation...
do you have a micron gauge hooked up to this thing?

no micron gauge just a lowside blue gauge

how cold is your condenser?
it was between 45-55 (estimation from various laser readings)

you might try a very gentle heating at atmospheric pressures, then ramp up the vacuum, then ramp up the heat.

ok this was my first attempt so obvoisly have a long way to go. should i try to distill my ethanol away at atmospheric pressure then crank down the vac once ive swivled flasks?

a sublimation trap prior to your vacuum pump is not a bad idea either.

do u mean a cold trap? im using a crappy harbor freight pump il have cold trap will be built soon but for now im not to worried about the pump

might want to wrap the boiling flask and vapor tube in foil for a bit of extra heat retention. there should be no air currents on the apparatus.

that makes perfect sense but kinda feel like id end up opening it to see whats going on maybe ill wrap some tin foil tomorrow...

do you have any pictures of this setup?

ill put some up tomorrow.

do u have any pics of your solventless runs or what experiences have u had trying to accomplish it?

what type of distilliation process are u using?

 

[queequeg152]

ive no pictures of my particular apparatus, as ive never attempted such a thing.

im sorry if i gave you the impression that im some sort of hash guru. ive no experiance in this particular area.

that being said, with molecular distillation you do not want any gradients of heat, as you will condense the heavier components of what every you are trying to distill.

hence why the kugelrohrs use oven type heaters. the tin foil is but a cheap attempt at this, and a good place to start.

laser thermometers are terribly inaccurate...but not ill suited to this task. the main issue is that they need to be calibrated to read the particular material that is emitting the IR light.
it should still be able to read gradients of temperature provided you are reading the same material... glass.
that being said, if it were me, id try getting an accurate thermistor down into the vapor stream just to see whats going on.

a sublimation cold trap pulls gasses out of the vapor stream by freezing them, rather than condensing them into a liquid.

a vapor sublimation trap will catch( if sized properly) what ever is making it over into your pump. meaning you will be able to monitor and examine what parts of the distillation your primary apparatus is missing, and where to focus your attention in improving the apparatus.

IMO you want a very cold condenser here... whats cool about the kugelrohrs is... you can drip water or hold ice cubes right onto the recieving bulbs as they rotate. it makes a great condensor. IMO you should look into getting your condensor colder, approaching freezing temps, and possibly below with a chiller of some sort.

 

[hobb3s93]

ive no pictures of my particular apparatus, as ive never attempted such a thing.

im sorry if i gave you the impression that im some sort of hash guru. ive no experiance in this particular area.

that being said, with molecular distillation you do not want any gradients of heat, as you will condense the heavier components of what every you are trying to distill.

hence why the kugelrohrs use oven type heaters. the tin foil is but a cheap attempt at this, and a good place to start.

laser thermometers are terribly inaccurate...but not ill suited to this task. the main issue is that they need to be calibrated to read the particular material that is emitting the IR light.
it should still be able to read gradients of temperature provided you are reading the same material... glass.
that being said, if it were me, id try getting an accurate thermistor down into the vapor stream just to see whats going on.

a sublimation cold trap pulls gasses out of the vapor stream by freezing them, rather than condensing them into a liquid.

a vapor sublimation trap will catch( if sized properly) what ever is making it over into your pump. meaning you will be able to monitor and examine what parts of the distillation your primary apparatus is missing, and where to focus your attention in improving the apparatus.

IMO you want a very cold condenser here... whats cool about the kugelrohrs is... you can drip water or hold ice cubes right onto the recieving bulbs as they rotate. it makes a great condensor. IMO you should look into getting your condensor colder, approaching freezing temps, and possibly below with a chiller of some sort.

thanx for the help. i had some results on my second run ill post pics when i take time to upload off my phone.

u definetly have some good suggestions like boiling my ethanol away with no vac i think that helped alot of my second run. but even in the tiny sample i yeiled had quite a bit of ethanol in it. although this could have been a problem with not replaceing my flasks correctly.

i also used dryice in my condensers water source and an iso/dryice slurry on my catch flasks as per chonkski's advice.
tin foil around the starting flask helped a considerable amount i beleive so thanx for that tip aswell

do u think i need to add some steel wool near my condenser? so i can reflux the alcohol and water better?'

 

[2 Legal Co]

All of that is proprietary information and is for the client's eyes only. Pre/post weights and photos all depend on what the client's specifications are. They can not be generalized. Information from 3 months ago is outdated and no longer relevant today. If you are a client we are happy to work with you on your formulation. Recognize that every client has different needs and desires and our process is custom tailored to that.

To give an example of how useless this information is...it's the same as asking about yield %ages from a terpenator or to post "before and after" photos for extraction. There are too many variables to make this information useful.

Frankly, if this is an issue for you, we are ok with the lost business. You are welcome to take your business elsewhere .



Fe fi fo fum...I smell a troll. You are all welcome to perform your own experimentation. I encourage it. Unfortunately, due to conflict of interest, I can't participate except to point out safety concerns. I had the choice of becoming a mini celebrity a la the much respected GW and I chose not to do that. It's hard to yell at people "you're doing it wrong" and have trolls picking fights with you trying to paint you as a villain. Unfortunately, it gets personal. I prefer to spend my time quietly with my family.

Calling our processes a 'secret' implies that I have some sort of golden goose that I'm trying to hide from the world. That once this 'secret' is revealed I will be exposed as a one-trick pony. Many of our our processes are known to our clients and they continue working with us because of our professionalism, timeliness, and value we create for our clients and their patients. As time evolves we too must evolve to stay relevant. I'm sure its frustrating that you want to know how its done. Rest assured you'll figure it out with enough investment of time, money, research, and maybe collaboration. I've known that since day one. But as with all things, the devil is in the details. Just because Samsung can reverse engineer an iPhone or hire Apple developers doesn't mean they can make a similarly successful product. We skate to where the puck is going, not to where it's been.

You guys are welcome to do as your hearts desire and share or not share as much as you want of your own work. The world is your oyster. But if you're spreading misinformation or speculation about my work then I have to draw the line.

Enjoy your day!

RHH
Either you are yelling about nothing. (if you're improving so fast)

OR you're not changing anything at all and that's why you're wanting to keep it 'proprietary'.

Hard to tell from your multi-directional postings. You might want to reread your posts and figure out what/where your interests lie.

 

[Chonkski]

thanx for the help. i had some results on my second run ill post pics when i take time to upload off my phone.

u definetly have some good suggestions like boiling my ethanol away with no vac i think that helped alot of my second run. but even in the tiny sample i yeiled had quite a bit of ethanol in it. although this could have been a problem with not replaceing my flasks correctly.

i also used dryice in my condensers water source and an iso/dryice slurry on my catch flasks as per chonkski's advice.
tin foil around the starting flask helped a considerable amount i beleive so thanx for that tip aswell

do u think i need to add some steel wool near my condenser? so i can reflux the alcohol and water better?'

Im proud of the progress brother!

 

[SquattingBull]

hobbs are you using stationary short path glassware? As in do you have a flask with your starting material that is just sitting being heated? Pretty much every piece of equipment that is used for molecular distillation has a component that creates a "thin film" of sorts. Whether that be by wiping, turning, a spinning disc, a stir rod, whatever. Could be a piece of the puzzle missing brother. If you are already doing some component to achieve this carry on but It is a thought that crossed my mind when reading the updates today.

 

[flatslabs]

I have always tossed in an egg stir bar when distilling or refluxing from a roundbottom

 

[hobb3s93]

hobbs are you using stationary short path glassware? As in do you have a flask with your starting material that is just sitting being heated? Pretty much every piece of equipment that is used for molecular distillation has a component that creates a "thin film" of sorts. Whether that be by wiping, turning, a spinning disc, a stir rod, whatever. Could be a piece of the puzzle missing brother. If you are already doing some component to achieve this carry on but It is a thought that crossed my mind when reading the updates today.

awesome i knew i bought the stirring feature for a reason, guess we'll see how long this cheapo heating /stirring mantle can endure my tests.

hadnt thought about the "thin film" part of the equation but ill give that a try today. i know that what the pope unit uses just due to name but hadnt looked into much kus i knew it was far out off my price range.

do i just want a slow gentle speed or should i change speed depending on liquid level and other factors?

thanx for the help guys

 

[hobb3s93]

Im proud of the progress brother!

thanx man, i owe everything i know and am learning to icmag and ig.
speaking of ig lets do some brainstorming on the dm when u have a chance.