Sciencemadness Discussion Board

Another distillation setup, questions

Yttrium2 - 23-5-2021 at 14:56

Still trying to think of a way to acquire a couple hundred mL’s of solvent with the least cost / headache

Saw this distillation kit for $26 USD!
https://www.ebay.com/itm/353428654117?_trkparms=aid%3D111000...


Now, my questions are, could this kit be used to distill Coleman’s camp fuel without the naphtha dissolving the rubber hose which connects the distillation flask to the condenser?

It is a fairly basic setup, and it includes a stand, for well below the price of the ground glass variation.

Yttrium2 - 23-5-2021 at 14:58

Also,

What would I need as far as a water pump is concerned, I’m thinking about running my distillation outside away from the municipal hookups, so, if I remember correctly,

Portable battery powered shower head was the way to go?

Is there anything less expensive way of pumping the water for my condenser ?

What if I filled my condenser full of water and froze it? Would this provide sufficient cooling to collect about 150-200mL?

[Edited on 5/23/2021 by Yttrium2]

Sulaiman - 23-5-2021 at 15:36

I would not freeze water in glassware for fear of breaking the glass due to the expansion when water freezes.
Better choices are:
. A water container (bucket, bag etc.) higher than the condenser outlet,
refill the bucket as required.
siphon water via the condenser.
. A usb water pump and a usb power pack recirculating water to/from a bucket, changing the water as required as it heats up.

Latex tubing will be attacked by many solvents, use pvc or silicone tubing.

I would soon get frustrated by the distillation kit that you linked to because I'm used to ground joint glassware,
I can see the cost saving with this kit, but.....

Yttrium2 - 23-5-2021 at 15:47

I just saw the usb water pumps, very neat, not as bulky as the shower head.

What kind of power bank would I need to run the pump for, 3 hours?

If I left an air gap, the ice wouldn’t crack the condenser, would it??

It’s akin to having some water in a glass bottle and freezing it with the lid open, won’t there be room for expanansion?

Thanks for the input,
Not sure about the bag/bucket idea,

I have thought about it before though, I could raise one bag, and then let it drain, then lower that bag and have it drain into another..

Would it matter where the water outlet / inlet would be for this idea? It might be easier to have the inlet at the top of the condenser, see what I’m saying?


Anyways, I like the idea of the usb pump

arkoma - 23-5-2021 at 16:58

How good an idea is distilling white gasoline with an open flame with a disty rig that uses a rubber hose to carry the solvent vapors to the condenser?

I'll wager a not very good idea..................

Yttrium2 - 23-5-2021 at 17:04

Does anyone have any more information on the water pumps, what kind of power bank would I need and would it produce enough head?


And what about for regular submersible pumps that hook up to municipalities

Dr.Bob - 23-5-2021 at 17:35

I would not use that kit for anything, it is cheap and not designed for organic work. There are find 24/40 kits both from the US and China that are a little more, but safe to use. I would not use a flame to heat gasoline, it just seems like a terrible idea, you can use a water bath with a hotplate or even just pour some boiuling water from a kettle into a water bath. And an aspirator will work fine, and won;t pollute the water enough to matter. Most water rpumps cannot get the flow to create a useful vacuum. If you do it outside, you could drain the water somewhere to evaporate if you are worried. That would be muich safer also.

A battery opperated pump will not likely work enough to matter, people have tried it before on here. Even simple fish water pumps will not get much of a vacuum, you need 4 g/min at 60 psi to get a decent vacuum.

arkoma - 23-5-2021 at 17:55

This post is a recurrent "theme" with yttrium.

karlos³ - 24-5-2021 at 06:44

I can't get it why he always wants to use the most unsuitable most ghettoish sort of distillation equipment which is absolutely wrong for his purpose?


Just go to deschem and buy a cheap ground glass distillation kit, its thirty bucks but it is suitable for your purpose.

Does yttrium2 even read what we say, ever?
Or is he high again?

Sulaiman - 24-5-2021 at 07:28

I have to agree with the opinion that open flame, latex tubing and distilling petroleum products is a poor choice, to put it mildly.

However, I've used a pump like this
https://www.ebay.com/itm/293252357000?_ul=MY
USD 2.48, usb powered, maybe three hours from a 5000mAh power bank/pack.
It was adequate for 500ml ethanol etc. distillations. (24/29 glassware)
eg rated=3m (at flow=0) and 3 l/min (at 0m lift/head)
should be ok for 1 l/min at 1m lift
1 l/min = 16.7 g/sec
16.7 x (specific heat capacity of water) x (temperature rise) = 700W
(for condenser outlet 10C higher than inlet)

Belowzero - 24-5-2021 at 13:33

Quote: Originally posted by karlos³  


Does yttrium2 even read what we say, ever?
Or is he high again?


I am glad you mention this because this has been my thought over the last dozen or so topics he created.
Kinda feels like he is exploiting the willingness of others to help and post the same question again.
At this rate he will be at 2k posts soon only to contaminate the board.
Or perhaps, indeed too much of the green stuff.


[Edited on 24-5-2021 by Belowzero]

arkoma - 25-5-2021 at 02:16

this threads harmless overall, and this just might be the only social interaction he gets and everybody needs a bit so there is that, y'all remember when he was "shopping" for a retort?

For the newer members, hes been advised to buy a >$40 24/29 disty kit probably several hundred times by now.....

Yttrium, I'd gift you one, but then what the heck wouldja do to keep us on our toes?


[Edited on 5-25-2021 by arkoma]

Yttrium2 - 25-5-2021 at 10:11

Deschem is down
Nanshin doesn’t have there stock listed.and are probably down as well,

I like to save $

But if Dr.Bob is against it, I’ll listen.

Probably would of employed a water bath, but just toying with the idea.

Interlabglassware seems to make quality stuff, they are a bit more. I’d go with other sellers…

This is the type of kit I fancy
https://www.ebay.com/itm/131156736530?_trkparms=aid%3D111000...


Nanshin used to have one for about 60 bucks, I like how the 3 way distillation adapter accepts the thermometer coupling, and isn’t 1 piece

Only thing id do is add a 24/29 400mm Liebig condenser, interlabglassware doesn’t have any listed for sale..


Also, I like these
https://www.amazon.com/Deschem-Distillation-Apparatus-Distil...

But in 24/29

Yttrium2 - 25-5-2021 at 10:15

I’ll have to wait till I’m off probation to get a distillation apparatus,

But a one can dream right?

What I’d really like is some sort of a box that I can repurpose into a fume hood. — one that’s not too big, or too small

Please see the fume hood construction thread for my post

I like aromas build :D

[Edited on 5/25/2021 by Yttrium2]

karlos³ - 25-5-2021 at 10:16

Don't forget if you want to distill organic solvents, you likely require a stirrer, boiling stones are not nearly as good in comparison.
And you want to distill alkanes from naphtha, those tend to bump heavily if not stirred...
And I mean HEAVILY, like, bumping their connections off, even with clamps(sp? right word?).

Deschem isn't down, I received an order while they were still on vacation.
Just buy from them, you get even tubing and some pH-paper with it.

[Edited on 25-5-2021 by karlos³]

Yttrium2 - 25-5-2021 at 10:20

Oh yeah right, not sure how I’ll heat and stir a round bottomed flask.

If I have the rbf in a water bath/glass bowl, can I still stir?

karlos³ - 25-5-2021 at 11:38

You need a heat resistant stir plate, and I don't think you can build that yourself.
The heatplate/stirrer combo is one of the greatest and most important tools for the homelab, and I think you just have to bite into the sour apple and order one.

This is where you can attempt to save money, not on the distillation kit.
Try to get an used one under 100$, if you are quick maybe even less than 80$.

But you really need to be quick, there is no time to ask us all if that one is suitable, you have to be fast on your own and keep track of it.
In general, if it can stir and heat, it will suffice for most things... you don't need a top piece of equipment, just one thats working.
And when you got that piece of equipment, everything else is just a piece of cake.
With a heated magstirrer in possession, the world of chemistry became immediately much wider to access by yourself ;)

Maybe arkie will still gift you a distillation kit if you already got a stirrer to proudly present us? :P
I think he would, if you just listen to our advide ;)

Oxy - 25-5-2021 at 11:58

Quote: Originally posted by Yttrium2  

If I have the rbf in a water bath/glass bowl, can I still stir?


Yes, you can.
I used an ordinal heat-resistant kitchen vessel as water bath. Many people are using crystallizing dishes as the container for heating medium (or a beaker if the flask is small). You can also make a hot air bath if you will cover your flask and plate under a layer of aluminium foil and making a kind of skirt. It may be not ideal solution when working with something that is not compatible with aluminium.
I found recently a nice and small kitchen pot made from aluminium without any steel layer (which makes stirring very hard or even impossible). One of the best buys this year.

Yttrium2 - 25-5-2021 at 12:00

I here you, but am still unsure if it’s be able to stir with a glass bowl atop of it and a rbf submerged into the bath, can anyone answer this question?

I’d prolly go with one of these, which has been recommended against, though I’m not sure why

https://www.ebay.com/itm/201854894893?epid=26018567306&_...




Or maybe even one of these

https://www.ebay.com/itm/263416977723?_trkparms=aid%3D555023...

Which is best between these two, and can someone answer my above question?







Oxy - 25-5-2021 at 12:09

Have you taken any physics lessons and get some basic knowledge about magnetic field?
If not, try with a magnet and glass taken from your kitchen or read my post once again.

Yttrium2 - 25-5-2021 at 12:34

Quote: Originally posted by Oxy  
Have you taken any physics lessons and get some basic knowledge about magnetic field?
If not, try with a magnet and glass taken from your kitchen or read my post once again.


I didn’t see your post before posting mine,

I see, I knew a magnet would permeate through glass, but wasn’t sure about how far..

[Edited on 5/25/2021 by Yttrium2]

karlos³ - 25-5-2021 at 12:57

Stainless stell also is permeable for magnets.
But if you use a FBF directly on the hotplate, you don't actually require a bath really.

There are some distillation kits out there who come with both a RBF and FBF, so that might be even better for you?

As for the stirrer, just get one that you can afford, you will see if its sufficient, and if not, it will still be able to heat and stir... maybe heats up slower though or such, but it will work still.
And if not, you still have some level of guarantee from ebay(pay with paypal and customer protection), so you really don't need to worry much.
Just look for what your budget allows for.

Sulaiman - 25-5-2021 at 19:37

Quote: Originally posted by Yttrium2  


This is the type of kit I fancy
https://www.ebay.com/itm/131156736530?_trkparms=aid%3D111000...

Also, I like these
https://www.amazon.com/Deschem-Distillation-Apparatus-Distil...
One reason that people dis-recommend those hotplate stirrers is their relatively low heating power,
180W and 200W respectively.

Although I now have a 500ml and a 5000ml heating mantle,
for years I managed very well with a cheap domestic hotplate like this
https://www.ebay.co.uk/itm/194035851829?hash=item2d2d702235:...
when it died I found a cheap used dual unit similar to this
https://www.ebay.co.uk/itm/294190678849?hash=item447f218341:...

I had a go at adding magnetic stirring to my diy 500ml heating mantle and gave up because overhead stirring was easier to diy,
but for years I 'survived' without stirring.
STIRRING IS ESSENTIAL FOR SERIOUS WORK
but most procedures at my level work ok without it.
__________________________________________________________
When I started, I completely underestimated the cost of a distillation setup :
Distillation glassware - RBFs, joints, condenser, thermometer etc.
is only a small part of the cost, also required are ;
Stands and clamps - consider diy stands
Heating & Stirring - many options
Workspace - fume cupboard or well ventilated workbench or weather shielded outdoor workspace
Firefighting equipment - fire extinguisher, fire blanket, hosepipe etc.
Cooling water - tap/faucet, recirculating pump etc.
PPE - goggles at least
ALL OF THE ABOVE ARE REQUIRED
You will probably need extras such as
Filtration - gravity if patient, vacuum otherwise
Addition - a pressure equalised addition funnel is almost essential
Separation - a separation funnel would be good (I've not got one yet)
Good lighting

LabDIRECT - 26-5-2021 at 02:03

Quote: Originally posted by Yttrium2  
Still trying to think of a way to acquire a couple hundred mL’s of solvent with the least cost / headache

Saw this distillation kit for $26 USD!
https://www.ebay.com/itm/353428654117?_trkparms=aid%3D111000...


Now, my questions are, could this kit be used to distill Coleman’s camp fuel without the naphtha dissolving the rubber hose which connects the distillation flask to the condenser?

It is a fairly basic setup, and it includes a stand, for well below the price of the ground glass variation.


What are you looking for specifically? Hexane? Heptane? Pentane? Naptha? Or are you talking about the EtOH based fuel? Either way, we'd be happy to supply you with the solvent itself for the same or less than what it'll cost you for the setup and fuel. Not to mention it'll certainly be a better product than what you could distill using a kit like that, especially if you're trying to distill out a specific fraction of the "white gas" type Coleman fuel.

Oxy - 26-5-2021 at 02:18

Quote: Originally posted by Sulaiman  
One reason that people dis-recommend those hotplate stirrers is their relatively low heating power,180W and 200W respectively.


I own 500W and the heating power is too low.

@Yttrium, do not buy the cheapest setup available. Buy something which have reasonable quality and price. This setup can last you for years of work. It's better to buy just once than throwing the money away.

Hoffit - 26-5-2021 at 07:31

Shape matters. Flat bottom bottle (or RBF) on a plate does not transfer heat well. I distill typical solvents (like toluene, ethyl acetate) just fine with erlenmayer bottles on my 300W plate on a liter scale without running it even close to max power. (typical pretty quick fractionating speed like a few drops per second).

For stripping something quickly like 20% alcohol you really want something faster. Better shape like round bottle on a 300W mantle is fine for 1000ml scale stirred. Upping to a 2-3 liter scale without stirrer and some reflux I prefer a separate kitchen stove with more power.

I prefer stirrer when possible and it makes stripping liquids faster. With kitchen stove you probably need boiling stones (like broken pieces of clay pot). My sirrer does not work through my 230v stove.

If you have very large reflux ration and still want decent output, you may prefer more power. Trying out is easy and you'll see what suits your exact use case. I'd not say something like 300W is not enough power, for most of my use cases it is. For some other use cases it is not.

Oxy - 26-5-2021 at 10:02

That's obvious. I don't use it as a direct heat source for RBF. If I need to use it for RBF I always use water/oil bath or aluminium skirt aka "air bath".
Today when I was making copper(II) oxide I needed to heat ~1 liter of solution (with precipitate) to boiling point. I stopped when the temperature went to 80 deg C as the process was really, really slow. I used beaker for that so heat should be transferred quite efficiently.
The next I will buy will be ~1000W. I think it will be enough for home-scale usage. 500W is generally ok when working with small quantities but there are situations when I feel that I really should change the hotplate stirrer. Thankfully I have a few of heating mantles so I can heat really efficiently when I really need.

Heating mantle is definitely better for RBF. There is also an option to buy (or make) an adapter for RBF which can be mounted on the hotplate. Then the flask is heated efficiently (as the adapter has a round shape like a mantle) and strong stirring is possible. But if there is a need to buy more than one adapter then it becomes expensive.

Yttrium2 - 26-5-2021 at 11:50

I’m tempted to buy the 180watt hot plate
I think it will be enough

Hoffit - 27-5-2021 at 00:16

Quote: Originally posted by Oxy  

Heating mantle is definitely better for RBF. There is also an option to buy (or make) an adapter for RBF which can be mounted on the hotplate. Then the flask is heated efficiently (as the adapter has a round shape like a mantle) and strong stirring is possible. But if there is a need to buy more than one adapter then it becomes expensive.


I've never seen or heard of an adapter. What are they made of typically? I'd assume heating up for example solid adapter would have a long heat up time like sand or oil bath (that are basically kind of adapters).

Oxy - 27-5-2021 at 05:06

Here is an example and this one is made of aluminium, so it should be much faster than sand

https://www.sigmaaldrich.com/catalog/product/aldrich/z675075

[Edited on 27-5-2021 by Oxy]

Hoffit - 28-5-2021 at 02:41

Those could be interesting for some use cases. (even if I'm mostly into heating mantles)

My kid just had a home work assignment to measure efficiency of heat transfer to water. About 270g water in a 500ml erlenmayer on a 150x150mm hot plate had efficiency of 19% (water heated from room temperature to near boiling, full 500W all the time).

Some heat goes to warming up the plate and bottle and quite a lot escapes when the bottle covers only part of the plate. I was a bit surprised the efficiency is that low. With something like flat bottom bottle with even less surface contact I'd assume even lower efficiency.

Texium - 28-5-2021 at 05:30

Those aluminum blocks are nice. Had them in the teaching lab where I taught o-chem this year, and they worked really well for the most part. They heat up fast and avoid the mess of an oil bath. They have a small well for a thermocouple too so that if your hotplate is equipped with one, you can easily measure the temperature of the block. The one and only issue I had with them was that a couple times a flask would get stuck in its well somehow, to the point where the flask actually sheared in half when attempting to remove it from the block! :o Bear in mind though, over the course of two semesters, I had about 60 students who each used these several times, and this problem occurred exactly twice, so the failure rate is still very low. I’m sure if it does occur, it would also be possible to fix it by quickly heating up the block to loosen its grip on the flask. Honestly at only about $50, they’re less expensive than I expected, especially coming from Sigma. I think I’ll order one for my own hood.

Yttrium2 - 31-5-2021 at 20:14

To get this thread back on track, what or where is a submersible pump I can hook up to a battery?


And lastly, how could I provide stirring if I was out an the Appalachian trial without any electricity?


Will bumping stones suffice!? For Coleman lighter fluid distillation?

Yttrium2 - 31-5-2021 at 20:17

What’s a usb fountain pump that will provide enough head, and what kind of battery pack is compatible plz

Hoffit - 1-6-2021 at 13:58

For small flow volumes almost any small pump like fountain pumps will do. USB and 12V pumps are easily available. I often find I need a very slow water volume and the equipment is rarely high enough to need some pressure from the pump. (Matters change if you go for high power, large vessels with lots of vapor to flow or very volatile liquids).

I think someone told to use just vessels. Have one vessel above equipment to feed the input and dump the output on some other container. No pump needed.

Boiling stones are enough for most jobs. In case you have none, small rocks, pieces of broken ceramic items or pieces of broken glass are often useful. I use pretty often pieces of broken flower pot. They work very well due to porosity.

Mateo_swe - 2-6-2021 at 05:35

Just use a small waterpump of the types used for very small fountains or aquariums, they will work fine for circulating cold water from a ice bucket to your condenser and back in the bucket.
If distilling small volumes the cheap china hotplate stirrers will work but most regret they didnt buy a more powerful hotplate stirrer as they start distilling larger volumes.
It takes looong time to heat a larger volume to boiling using a weak hotplate.

If you are good with electric stuff and know you aint going to accidently kill yourself, you can buy a heating mantle replacement sleeve and power it with a dimmer or variac (the heating element wire is included in the sleeve).
Its a cheap option and you can place the sleeve on that cheap china hotplate stirrer and just use the stirring function on the hotplate, and you have a heating mantle with stirring for RB flasks.
I would go for the cheap china hotplate stirrer, a aquarium waterpump and a Deschem distill kit.
It will get you going and you are going to upgrade your gear later anyway.