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Author: Subject: For those distilling at home, how do you feed water into your condenser?
MidLifeChemist
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[*] posted on 4-10-2020 at 13:25
For those distilling at home, how do you feed water into your condenser?


My simple distillation kit just arrived from Deschem (in only ten days from China to USA!).

I posted a photo of the kit in action down below.

It came with a Liebig condenser and a few feet of latex rubber tubing. However, I soon realized that reaching the tubing to a water source, attaching it with appropriate adapters and pumping it through was easier said than done.

For those of you doing chemistry & distillation at home on a budget, how exactly do you force the water through your condenser, do you attach it to your sink, or a faucet, or use a pump? what adapters did you need and where did you source them? If you bought a pump, which one did you buy?

Curious to see how everyone else deals with this! Also if you have any distillation tips please share.

[UPDATE] I got 10ft of vinyl 1/4 inch tubing at home depot, and I was able to connect my new setup to the filtered water faucet at our kitchen sink. I'm doing a test distilling water. It's going well, but it's taking way longer than expected to boil 250ml of water! That's with the hotplate at 280C and the flash wrapped in a little Al foil. Since I can't do distillations other than water in our kitchen, looks like I'm going to have to invest in a bucket and a $20-$30 pump.

dist-setup.JPG - 2.2MB



[Edited on 5-10-2020 by MidLifeChemist]
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ArbuzToWoda
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[*] posted on 4-10-2020 at 13:45


If you can carry out a distillation at home yoou can use a faucet, but that's wasteful. Just get a cheap, 2USD 12 volt pump. Attach the outlet of the pump to the inlet of the condenser via a tube, attach the inlet of the pump to the water reservoir of choice. Attach a third tube to the outlet of your condenser. This tube will lead water back to the reservoir. Now suck on the third, non-pump tube so as to suck some water up to the condenser (in other words, replace the air in the system by some water). Now, pinch the tube you just sucked on so as not to let the water flow back to the reservoir and plug in/turn on your pump. It should start recirculating water. You could also get a more powerful pump that can do all the sucking for you, but I was not bothered to do so. It's literally 15 seconds of work if you know what you're doing.
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[*] posted on 4-10-2020 at 14:29


I have been known to attach the hoses to a couple of funnels, clamped to a stand. I can fill the hoses and funnels with ice water, and replace the ice as needed. Moving the clamps up and down makes the water flow.



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Syn the Sizer
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[*] posted on 4-10-2020 at 15:19


I use a outdoor pond water pump. I got a small one for $20CDN. I use a large rubbermaid container with about 30L of water and cycle the water. You don't need that much water if you have a smaller container but you want to balance the heat produce and heat dissipated. If you have too little water it will warm up too quick the cooling rate will go down.
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Sulaiman
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[*] posted on 4-10-2020 at 15:23


Lately I have been using an ac powered water pump intended for ponds and water features,
HJ-1100, 20W, 900 l/h, 1.5m head height.
(at home I previously used a 12V submersible water pump and even a 5v water pump)

For some distillations I use an expanded polystyrene box with water plus ice,
it works well but uses quite a lot of ice.
Also, it stresses the condenser when condensing water as the temperature difference across the glass is about 95oC

Most recently I have been using the pump to recirculate swimming pool water (about 30oC here)
this is better as the stress on the glass is less and the temperature is stable.
(also a lot quieter)

A surprisingly low rate of water flow is adequate.
__________________________________________________________
for simple distillations water flow rate and temperature are not critical,
colder and/or quicker water flow allows faster distillation rates.

if you use a packed column then constant flowrate and temperature are important to maintain equilibrium in the column,
also, for a reflux condenser if the coolant is too cold it returns the refluxed condensate to the column at too low a temperature so some fractionating efficiency is lost.

Previously I have also used just a siphon from the cistern of an upstairs toilet to get a constant water pressure/flowrate - it works well.
(any elevated water tank will work)

Some people use two large water vessels and pump cooling water from one to the other.
___________________________________________________________
P.S. if you use the utility water supply or a pump, high water pressure can push hoses off of connectors
- causing at least a very wet workplace
- possibly causing damage
so hose clamps or something similar such as tying with string is required.

[Edited on 4-10-2020 by Sulaiman]




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Herr Haber
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[*] posted on 4-10-2020 at 17:18


Cheap aquarium pumps are good and usually have the plastic adapters you need.
Bigger ones when you are more at ease attaching the tubing and after you've had to deal with a flood :)

Keep in mind the pump heats the water !




The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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pneumatician
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[*] posted on 4-10-2020 at 18:47


The water not need to run until the vapour start to rise, so fill the condenser and wait. I use a fish tank pump.

If you distillate 8 Liters of water you need 250 Liters of water to cold down the hot vapour, but this depend of what temp is in your zone and if summer, winter...
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[*] posted on 4-10-2020 at 21:12


My ebay-China distillation setup, distilling HCl from tile cleaner + 10% CaCl2.



20200928_160020.jpg - 185kB 20200928_160030.jpg - 131kB
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[*] posted on 5-10-2020 at 02:44


Quote: Originally posted by MidLifeChemist  

However, I soon realized that reaching the tubing to a water source, attaching it with appropriate adapters and pumping it through was easier said than done.
[Edited on 5-10-2020 by MidLifeChemist]


The most complex thing is keeping things in order in a laboratory. The rest is manageable more or less. This is my solution based on garden hoses and silicone tubing. I am happy to have a washbasin in the same room - actually this is my most used equipment. The splitter is for water pump (which is used for vacuum filtration and some other things) and a hose. The hose I use both for washing glassware, as an emergency washer and to feed my coolers. The universal adapter from the second picture does any kind of magic of connecting hoses of different diameter.
Having base system on garden hoses allows me to use the same equipment outside in backyard or garage.


water1.jpg - 258kB water2.jpg - 105kB

[Edited on 5-10-2020 by teodor]
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Heptylene
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[*] posted on 5-10-2020 at 03:02


At first I used water from the tap, but it's pretty wasteful. Then I moved to using a 10 liter bucket with an aquarium pump. Because water has a huge latent heat of vaporization, you will need a lot of coolant to keep sustained reflux or for long distillations. You have to remove about 2250 kJ of energy to condense 1 kg of water, and that is enough energy to heat a 10 liter bath by 53 °C! You can use ice or just change the water periodically. I like to stock up ice in advance of experiments, so I have enough ready if I need it.
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MidLifeChemist
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[*] posted on 5-10-2020 at 07:00


Everyone, thanks for your comments, they are so helpful!

Here's my setup that I tested yesterday in the kitchen. Please read my notes below the photo, and tips or constructive criticism is greatly appreciated!



dist-setup.JPG - 2.2MB

#1 - this was in my kitchen, condenser supplied from my sink faucet. Future distillations will be in my garage, using a bucket and aquarium pump (both need to be purchased)

#2 - one of my tubes is latex, one is vinyl. That seemed to work fine, not sure if it will cause issues in the future. Vinyl was 1/10th the price of latex at home depot.

#3 - the glassware was purchased as a kit from Deschem, first impression is that the quality is not bad at all. It did include a 500ml round bottom flask, which I chose not to use in this test to make balancing everything easier.

#4 - I did not grease the joints. Everything worked fine but in what cases will I need to grease them?

#5 - boiling water with the hotplate at 280C took a very very long time. After I took this photo, I wrapped the flask in one layer of Al foil, which didn't seem to do much. Does it take a long time for everyone?

#6 - The stand wanted to tip over in the direction of the sink (where I was standing when I took the photo). That's why I used the cast iron pot to hold down the stand better. It will probably help if I A) get a 2nd stand, and B) change the orientation of the base which I too lazy to do once I had it all set up.

#7 - Water flowed into the bottom of the condenser, and out the top.

[Edited on 5-10-2020 by MidLifeChemist]
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[*] posted on 5-10-2020 at 07:56


I use a large bucket, fill it with water, lift it up and let gravity do the job. Lifting the receiving end up reduces flow and vice versa. Once the bottom bucket is full, I pour it in the top bucket again.
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teodor
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[*] posted on 5-10-2020 at 08:35


Nice setup, MidLifeChemist. I am a bit jealous to your nice receiver part - I still don't have such thing and using something else which is not so convenient.
I used organic grease for vacuum and for ether. I used H2SO4 as a grease for bromine but it wasn't able to keep it inside completely.
Before applying any grease for any purpose I would suggest to change your fixture. This way as in the picture the joint between Erlenmeyer and the head can go out of connection. I always fix the flask firmly and then I allow gravity to fix the joint, supporting the cooler only very slightly. But you can find another method. Make a good practice with high IDLH (less toxic) liquids before going to poisons, even in a garage. There is necessary experience and errors everybody should (and necessary will) make, and it is better to make them on harmless things first.

[Edited on 5-10-2020 by teodor]

Also, notice the thread on your nice plate (I am very greedy also). It is for stand and fixing the flask, I would prefer to use it because in this case you can be sure it is stable (no need for that nice pan).

When looking for better fixture keep in mind that very often it is necessary to lift the flask over the plate, as a way to stop heating which is always a serious drawback of hot plates - they continue to heat flask even if you have a trouble and need to stop heating immidiately.
As a solution before I've made a good fixture I used a spray bottle with water to quickly cool the flask and plate.

[Edited on 5-10-2020 by teodor]

But I never used any special hotplate, just kitchen ones, may be your model has no such thermal capacity like plates I used.

[Edited on 5-10-2020 by teodor]

Also, may be it is needles to say because I am sure you are not so stupid as I was, but never lift any part relaying on a joint clamp. Once I took a flask with fresh distilled bromine taking it by the adapter joined to it. The flask was strong and not full, but it was a good lesson.

[Edited on 5-10-2020 by teodor]

[Edited on 5-10-2020 by teodor]
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[*] posted on 5-10-2020 at 14:41


#2 I prefer latex so I can move things around though that happens less during the distillation of course. I guess the choice depends mostly on you and your setup. Vynil is too rigid for me.
#4 For other things than water :)
#5 Wrap the hotplate with the lower part of the foil you are using for the flask
#6 Get a brick. Someday you'll probably want a second stand. That's normal :)




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[*] posted on 5-10-2020 at 18:10


buy a heating mantle, the use of a hot-stirring for this is a wasteful. For water I put the mantle at full temp until I find the right time before an explosion of vapour happend and then reduce the temp to "cruiser" temp. 280 and take a lot of time? this is the hotplate, with a heating mantle at full temp (350ºC) i need 45' to heat 8L of water near boommmboiling :)

I use silicon tubing, is more secure anti losing water. If for removing your tubing you need a strong force you end many times with the glass connectors broken and another condenser, whasing bottle... to send to trash... so with silicone tube I cut it near the nose with scissors and the rest in the glass tube I open it with a cuter and is removed easily with no force at all.

and is best fill all the condenser with water.
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[*] posted on 6-10-2020 at 05:16


I use a cheap aquarium pump.



0C4DD9B2-BAA4-4E34-9A78-7E534DCA47FE.jpeg - 600kB

I keep this set up under my bench, but it cant be too far below the condenser. Its just not strong enough. But its nice to be kept out of the way. I fill my reservoir with ice that I make in the deep freeze. And water of course.

[Edited on 6-10-2020 by ELRIC]



[Edited on 6-10-2020 by ELRIC]

FD4664A3-AD1E-414D-ADD0-D5AE52E47F04.jpeg - 792kB
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Sulaiman
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[*] posted on 6-10-2020 at 06:16


@MidLifeChemist : its not mportant but it is normal to set up the condenser with the water outlet at the very top, as in the photo above.
This allows air and any gasses to escape, filling the jacket with coolant.

While you are set up you may as well make a small supply of distilled water,
unless you can buy distilled (or de-ionised) water cheaply.




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MidLifeChemist
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[*] posted on 6-10-2020 at 06:50


@Junk_Enginerd - thanks for the tip
@arbuzToWoda - thanks for the tips. "attach the inlet of the pump to the water reservoir of choice" - sounds like that is a large bucket of cold water
@DraconicAcid - thanks for the tips
@Syn the Sizer - thanks, I appreciate the useful tips
@Sulaiman - thanks for the detailed tips, including the one on the water outlet. yes, I can get cheap distilled water.
@Herr Haber - thanks for the tips, I think an aquarium pump is my next purchase :) and I've very glad to hear using a weight or brick is normal!
@teodor - thank you, I think you are right, I am going to use 2 stands and support my flasks instead of the condenser
@pneumatician - thanks for the tips. I'm going to stick with a hotplate for now and see how it goes
@ELRIC - thanks for sharing the photo! looks perfect. Nice to see you use a combo of latex + vinyl like I do :) question - what material is that under your wood, and how does it handle liquid & powder spills?
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ELRIC
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[*] posted on 6-10-2020 at 21:33


Im not really sure what the material is made of. I took some cabinetry and used them as my bench. I can find out possibly in a few hours when the original owner awakens. I can assure you its not that clean anymore lol. I need to get out there and wipe it down honestly. Plus do some dishes (lab glass) :(

As far as durability, it has handled NaOh and H₂SO₄ so far and has remained intact.
[Edited on 7-10-2020 by ELRIC]

[Edited on 7-10-2020 by ELRIC]
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draculic acid69
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[*] posted on 7-10-2020 at 00:00


Just buy the pump.its irreplaceable. Don't bother with dodgying it up and using funnels and stuff.for the price of the pump being so cheap U really can't pass it up.
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draculic acid69
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[*] posted on 7-10-2020 at 00:08


Here's a question; how many of us have thought ahead and bought the pump at the same time as buying the glassware rather than having the glassware arrive and then
going "shit now I need a pump"
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[*] posted on 7-10-2020 at 00:30


Definitely bought the glassware before the pump and I don't even have a water supply in my lab.....
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[*] posted on 16-10-2020 at 07:37


A bucket and a cheap submersible pump, really. It’s crude but I haven’t any problems with it aside from the pump just getting worn out after time. When doing distillations outdoors, make sure rocks and grass or leaves and twigs doesnt get in the water. It will clog up the pump and it sucks to clean it out.

I bought my pump for $15 at lowes, probably the most useful purchase I’ve made at a hardware store lol

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[*] posted on 16-10-2020 at 07:46


Quote: Originally posted by draculic acid69  
Here's a question; how many of us have thought ahead and bought the pump at the same time as buying the glassware rather than having the glassware arrive and then
going "shit now I need a pump"


When I started, I just wildly collected random stuff and never thought it through. When I needed to do something, I just figured some patent that worked 15% of the time, and usually ended up in some sort of catastrophe.

Nowadays I'm routine for checklists. It's not that ordering something at the same time, but the shipping that takes forever. Oh, I need a bigger funnel? Wait 4 weeks.
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[*] posted on 16-10-2020 at 14:24


At the beginning I thought I'd do way more electrolysis than I actually did, so I bought a cheap 12V 20A power supply. Then once that was available I bought two cheap 12V water pumps. I made a small pump "panel" attached under my lab table with one 12V water pump used for running water through the condenser during distillations, and the other permanently attached to a venturi pump for vacuum.

This setup allows to:
- run distillations
- perform vacuum filtrations
- run (not so low pressure) vacuum distillations
by just filling the tank with water, attaching the hose and flipping a switch.

pumps.jpg - 204kB
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