Distillation vid

Well I finally made a video of my process..... Now I don't like talking in videos so it's very likely a bit boring.
It's also a series of about 30 videos stitched together in iMovie since I didn't have the battery life or any kind of stand to setup my phone on and record the entire process.

I also ran into the problem of having something in my condenser, I'm not really sure what it was since this glass was pristine when I setup the distiller.....at one point in the video you can see what I'm talking about as I hold the camera close to the condenser and you can also see it pouring out with the distillate into the cow.

I have no idea what this substance was.

*Puts on fire retardant suit*
I'm ready.... let's hear it.

https://www.youtube.com/watch?v=AAc8PUyrgjA

[youtubeif]AAc8PUyrgjA[/youtubeif]

Is that how you're all distilling? A few questions...

What's with the drip from the thermocouple tip? Looks like good stuff. I assume the actual sensor is in the very end of the thermocouple tip, raise the thermocouple a little, to where the tip is about level with the center of the head exit hole. Wrap a short piece of thin wire around the end of the thermocouple with the bottom end of the wire curving into the exit hole. The drip will follow the wire into the hole and pass into the condenser.

Look at all the action in the vigoreux, and little above it. Notice the reflux column has two unwanted energy sinks, the clamp contact points, and the head's glass support arm. The clamp on the head could be moved up past the exit, and/or further insulted with some padding. The solid glass support arm sucks, haven't a clue how to solve that one, except for a complete redesign, or maybe a little heat band clamp around the end of the support, heating just the last half inch or so of the support where it meets the column.

For <$25 you can plug your stirrer/mantle into a power meter, and even though changing the stirrer speed is going to alter readings, you can then observe what's gong on power wise when you vary the temperature control. P-3 Kill-A-Watt power meter.

still using that godamn pvc eh?

that head is shit. condenser is too small. you need to insulate your boiling flask, you've got a shiton of energy being wasted with all that glass exposed to cold air.

control the condensation coming off your condenser. that moisture is going right into your joints and being beckoned into the reaction by vacuum.

stop using brass. it's barely okay for gasses. it offgasses for a LONG time.

whats with quick connects AND hoseclamps? not so quick anymore. eliminate that source of leaks.

you've got a ton of oring connections. i bet a few of them are rolled. see what else i see when i sit down some more and look.

that wide margin between your vapor temp and the pot them lets you know your wasting something somewhere.

your temps are too high because your vacuum is too high.


looks like your vacuum grease made its way into the boiling flask.

those puffs of smoke are the tell tale that your temps/vac are off.

SkyHighLer said:

Is that how you're all distilling? A few questions...

What's with the drip from the thermocouple tip? Looks like good stuff. I assume the actual sensor is in the very end of the thermocouple tip, raise the thermocouple a little, to where the tip is about level with the center of the head exit hole. Wrap a short piece of thin wire around the end of the thermocouple with the bottom end of the wire curving into the exit hole. The drip will follow the wire into the hole and pass into the condenser.

Look at all the action in the vigoreux, and little above it. Notice the reflux column has two unwanted energy sinks, the clamp contact points, and the head's glass support arm. The clamp on the head could be moved up past the exit, and/or further insulted with some padding. The solid glass support arm sucks, haven't a clue how to solve that one, except for a complete redesign, or maybe a little heat band clamp around the end of the support, heating just the last half inch or so of the support where it meets the column.

For <$25 you can plug your stirrer/mantle into a power meter, and even though changing the stirrer speed is going to alter readings, you can then observe what's gong on power wise when you vary the temperature control. P-3 Kill-A-Watt power meter.

Click to expand...

I actually have a kil-a-watt around somewhere, I'll have to dig it up.

I have tried moving the thermocouple up to be closer to the condenser orifice but the vacuum just pulls it back in all the way and I haven't bothered to rig anything up to hold it in place yet.
I am however going to bother with it now. I wasn't really sure if the drop falling off of that was any good or not....guess I know differently now.

mobin said:

still using that godamn pvc eh?

that head is shit. condenser is too small. you need to insulate your boiling flask, you've got a shiton of energy being wasted with all that glass exposed to cold air.

control the condensation coming off your condenser. that moisture is going right into your joints and being beckoned into the reaction by vacuum.

stop using brass. it's barely okay for gasses. it offgasses for a LONG time.

whats with quick connects AND hoseclamps? not so quick anymore. eliminate that source of leaks.

you've got a ton of oring connections. i bet a few of them are rolled. see what else i see when i sit down some more and look.

Click to expand...

mobin said:

that wide margin between your vapor temp and the pot them lets you know your wasting something somewhere.

your temps are too high because your vacuum is too high.


looks like your vacuum grease made its way into the boiling flask.

those puffs of smoke are the tell tale that your temps/vac are off.

Click to expand...

I've never used that PVC, it was determined to be shit before I ever did start to use it, I just haven't pulled it off the wall.....there's nothing connected to it, I do follow advice you know.

what quick disconnects are you referring to? the GL-14 fittings? If I don't use hose clamps then I get leaks. If you're talking about the brass fittings connected to the vacuum gauge those aren't quick disconnects. other than that the only brass thing I have is a bulkhead fitting going through that table.
I don't have the funds to change any of the brass to stainless right now, so until I do this setup is what I'm working with.

I've got 3 o-ring connections that I can think of off the top of my head, the two thermometer inlet adapters, and the cold trap rodaviss joint..... I grease the rodaviss joint, and I haven't seen any rolling in the thermometer adapters.

I hate this fucking vacuum grease, I have 3 tubes of Krytox arriving tomorrow. There doesn't seem to be any middle ground with this dow corning garbage, I try applying a very very thin amount and it still pulls grease into the joints, or just doesn't form a complete seal.

Any suggestions for a better head/condenser? I can't do anything about changing them out right now, but when I can I will.

BigJohnny said:

Well I finally made a video of my process..... Now I don't like talking in videos so it's very likely a bit boring.
It's also a series of about 30 videos stitched together in iMovie since I didn't have the battery life or any kind of stand to setup my phone on and record the entire process.

I also ran into the problem of having something in my condenser, I'm not really sure what it was since this glass was pristine when I setup the distiller.....at one point in the video you can see what I'm talking about as I hold the camera close to the condenser and you can also see it pouring out with the distillate into the cow.

I have no idea what this substance was.

*Puts on fire retardant suit*
I'm ready.... let's hear it.

https://www.youtube.com/watch?v=AAc8PUyrgjA

[youtubeif]AAc8PUyrgjA[/youtubeif]

Click to expand...

Is that the Summit Research 2L setup? I had horrid leaking issues with those glass on glass thermometer joints, the black cap leaked like crazy and I ended up replacing it with a PTFE one.

To me your temp or the vaccum is set too high when it splashes that high into the boiling flask.

I distilled N-Hexane a few months ago and you could hardly see any movement in the boiling flask.

Fast boiling with lots of splashing is not something I ever want. I prefer a slow drip rate vs a stream.

I didn't use grease either even though I have some.

I used reusable PTFE sleeves that I got on EBAY from this same vendor below.

https://www.avogadro-lab-supply.com/item/24_40_PTFE_Joint_Sleeves_3_pcs_/944

With that much action in the head and so little condensing you probably have a leak at your upper thermocouple. If the vac is pulling your thermocouple down, then it is more than likely leaking. Wrap some teflon tape around your o rings to hold them in place and help create a better seal. I also second what Mobin pointed out.

Thomas@LRL said:

Is that the Summit Research 2L setup? I had horrid leaking issues with those glass on glass thermometer joints, the black cap leaked like crazy and I ended up replacing it with a PTFE one.

Click to expand...

no it's from bvv, but probably still just as bad, the original adapters I got with the blue soft plastic caps I've replaced with the chemglass adapters which are better, just not sure how much better.

troutman said:

To me your temp or the vaccum is set too high when it splashes that high into the boiling flask.

I distilled N-Hexane a few months ago and you could hardly see any movement in the boiling flask.

Fast boiling with lots of splashing is not something I ever want. I prefer a slow drip rate vs a stream.

I didn't use grease either even though I have some.

I used reusable PTFE sleeves that I got on EBAY from this same vendor below.

https://www.avogadro-lab-supply.com/item/24_40_PTFE_Joint_Sleeves_3_pcs_/944

Click to expand...

I've bought an umber of items off that guy, I'll probably order some of those because that would save a lot of hassle.

The excessive boiling is due (in part) to the stir bar. If I stop the stirring it would calm down a lot and not boil like that.

HashoftheTitans said:

With that much action in the head and so little condensing you probably have a leak at your upper thermocouple. If the vac is pulling your thermocouple down, then it is more than likely leaking. Wrap some teflon tape around your o rings to hold them in place and help create a better seal. I also second what Mobin pointed out.

Click to expand...

I'm fairly certain the larger adapter isn't leaking, it holds on to the thermocouple really tightly and I haven't noticed the oring doing anything it shouldn't be..... but that smaller adapter I've always had a problem with, I just don't feel like it's making a proper seal even though I've used a smaller oring. It does grab the thermocouple but I think it could be better.

When you say wrap it with teflon tape I'm assuming you mean around the threads and oring so as to keep the oring in place without the cap being on.

Speaking of teflon tape, my quick check shows some of the common varieties are pure PTFE except for the coloring agent.

Here's links to some thick blue, and yellow gas tapes,

Composition: 99.6% PTFE < 0.4%
Pigment Color: Blue

https://cleanfit.com/blue_monster_ptfe_thread_seal_tape_70885.shtml

and,

Composition: 99.0% PTFE <1.0% Pigment

Color: Yellow Thickness: 0.004” +/-10% (0.102mm +/-10% Density: 1.5g/cm3 +/-10%

https://cleanfit.com/yellow_gas_tape_70820.shtml


MSDS of a 99.5% gas tape,

https://www.northtowncompany.com/pdfs/SDS Sheets 07 20 17/Yellow PTFE SDS.pdf


Can be confusing though, they add stuff,

Types

There are two US standards for determining the quality of any PTFE tape. MIL-T-27730A (an obsolete military specification still commonly used in industry in the US) requires a minimum thickness of 3.5 mils and a minimum PTFE purity of 99%. The second standard, A-A-58092, is a commercial grade which maintains the thickness requirement of MIL-T-27730A and adds a minimum density of 1.2 g/cm3. Relevant standards may vary between industries; tape for gas fittings (to UK gas regulations) is required to be thicker than that for water. Although PTFE itself is suitable for use with high-pressure oxygen, the grade of tape must also be known to be free from grease.

Thread seal tape used in plumbing applications is most commonly white, but it is also available in various colors. It is often used to correspond to color coded pipelines (US, Canada, Australia and New Zealand: yellow for natural gas, green for oxygen, etc.). These color-codes for thread sealing tape were introduced by Bill Bentley of Unasco Pty Ltd in the 1970s. In the UK, tape is used from coloured reels, e.g. yellow reels for gas, green for potable water.

White – used on NPT threads up to 3/8 inch
Yellow – used on NPT threads 1/2 inch to 2 inch, often labeled "gas tape"
Pink – used on NPT threads 1/2 inch to 2 inch, safe for propane and other hydrocarbon fuels
Green – oil-free PTFE used on oxygen lines and some specific medical gasses
Gray – contains nickel, anti-seizing, anti-galling and anti-corrosion, used for stainless pipes
Copper – contains copper granules and is certified as a thread lubricant but not a sealer

In Europe the BSI standard BS-7786:2006 specifies various grades and quality standards of PTFE thread sealing tape.

https://en.wikipedia.org/wiki/Thread_seal_tape#Types


Here's a technical data sheet confirming you need to be careful,

"Poly-Temp SSG (XHD) Stainless Steel Grade with its nickel content is designed to perform as a sealant and as an antiseize for difficult service conditions associated with stainless steel and SS alloys."

http://www.northtowncompany.com/msdspds/teflon_tape/teflon_tape_yellow_gas_ptfe.pdf



So, why not just wrap all the joints with pure teflon tape?

^this.

pull your system down clean and dry, wrap joints in tape tight and evenly. over lap too much in one area and it'll break your flask if your lucky.

get thick ass tape and its a breeze stretching out your own joint condoms.

blank off your pump and take the reading. now get the same reading on your glassware.

in actuality you should be off the range of a therm/piezeo gauge within seconds. if it take a while to pull down but you still get to spec, congratulations....you're not there yet. you just are within the range of your pumps cfm/present leaks. remove components as necessary and cap/stopper off pieces until you get a good reading, then work back towards a complete system cleaning, taping, adjusting joints until you're good.

or keep isomerizing.

mobin said:

^this.

pull your system down clean and dry, wrap joints in tape tight and evenly. over lap too much in one area and it'll break your flask if your lucky.

get thick ass tape and its a breeze stretching out your own joint condoms.

blank off your pump and take the reading. now get the same reading on your glassware.

in actuality you should be off the range of a therm/piezeo gauge within seconds. if it take a while to pull down but you still get to spec, congratulations....you're not there yet. you just are within the range of your pumps cfm/present leaks. remove components as necessary and cap/stopper off pieces until you get a good reading, then work back towards a complete system cleaning, taping, adjusting joints until you're good.

or keep isomerizing.

Click to expand...

At some point I will do this, all of it, I'm just stuck in a vicious cycle currently. In order to get out of this cycle I can't have down time.....without the down time I can't make these improvements that I need to make which is causing the problem of excessive times and temps resulting in a product which is slow to go anywhere.

I can't pay my bills at the moment and am waayyyy behind..... I definitely can't afford to replace components, buy new parts, etc.

I'm stuck working with what I have for the time being....hopefully things will start improving this month.

BigJohnny said:

excessive times and temps resulting in a product which is slow to go anywhere.

Click to expand...

You may want to consider a hotter shorter path to the condenser. That's a pretty flooded column you've got there are you sure it's a good idea. Some adapters are no more than a bent tube, which would be short. Standard kits come with a 24/40 3-way or 10/30 thermometer top and ordinary RBF's and everything else in them because those work fine. If there was foil over the boiling flask up to the condenser and something over the foil maybe your boiler wouldn't be so much of a condenser?

are you dewaxing and filtering the bho first with ethanol and a buchner funnel?