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Author: Subject: Piecing Together the Ultimate Distillation Set
Yttrium2
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biggrin.gif posted on 22-9-2019 at 17:06
Piecing Together the Ultimate Distillation Set


So, in the future I plan to get a new distillation set

I fancy the kits containing the distillation apparatus

A sep funnel
A claisen adapter
And vigreux


I think this kit looks to be the highest quality, based on the looks of the edges and vacuum takeoff adapter.

https://www.ebay.com/itm/500ml-24-40-Glass-Distillation-Appa...

What I'm wanting to know is what sized ground glass thermometer adapter would work for distillations and what size ground glass thermometer, for an all glass setup-


I like how the thermometer adapter is separate from the 3 way distillation adapter


Also, does the entire distillation apparatus need to be heavy walked for vacuum applications -- the liebig condonser and everything?

...

This seems like it would be the perfect kit, especially with a ground glass thermometer and if I could get deschem to put it in a molded box for me. (Worth a shot!)
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CouchHatter
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[*] posted on 22-9-2019 at 17:35


That looks pretty standard to me, and surprisingly cheap - you might end up paying for it in quality. Hard to know. I got my setup from Laboy and it was nearly all-inclusive for $160. Four years old and still intact. Mine came with several extra flasks, though. Every single joint on mine is the same, 24/40. Unless otherwise specified all the joints in the linked item will be the same as the title.

Thick-walled glass isn't necessary for vacuum. My distillation kit has been used many times under ~65mmHg without failure. I don't know if distilling to a thin-wall Erlenmeyer under vacuum is safe, though, never done that. I guess overall that might vary by brand.
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Yttrium2
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[*] posted on 22-9-2019 at 18:04


$160! Dang, that seems like the prices from a few years back.



Its way cheaper now
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[*] posted on 22-9-2019 at 19:26


My initial kit was Chinese glass from a reputable seller (whom I contacted directly rather than through ebay.) I worked out what pieces I wanted and got a quote. From memory it was around $250 AUD. It included a range of flasks from 50mL to 1000mL including a few erlenmeyers, all the standard adapters and thermometer adapters, a claisen, a 3-neck, a vigreux, liebig and graham condenser (don't bother) a 250mL PE funnel and a mantle.

I have since added to the kit: it is about double the size. This is mostly bargains I spotted on eBay from time to time. I have replaced a few broken flasks and one condenser.

If you are doing stuff your kit can grow. But worth beginning with a basic setup that enables you to do a lot of routine things, such as you have chosen. You might consider a 300mm condenser rather than a 200mm.

Debates continue on the relative merits of cheap glassware. The consensus seems to be that it is good enough for many people for most of what they do. Things to watch for are glass defects (I have never seen one in my gear) and poorly-ground joints (which means more grease or using teflon tape). For a beginner I think it is perfectly fine. Replace with the high-end stuff once you have more experience and when you are replacing things you have broken -- that is, if you feel the need to up the quality.



Edit: typos

[Edited on 23-9-2019 by j_sum1]




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Sulaiman
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[*] posted on 23-9-2019 at 02:25


Quote: Originally posted by Yttrium2  
...What I'm wanting to know is what sized ground glass thermometer adapter would work for distillations and what size ground glass thermometer, for an all glass setup...


Thermometers with ground glass joints are nice to have, but VERY expensive,
AND you cannot use a typical size adapter (e.g. NS14 to NS24) as the thermometer bulb will be at the wrong height/depth relative to gas flow.

The thermometer adapter in the kit will be adequate for most requirements,
but the thermometer that came with my Chinese distillation kit was c7mm diameter which is too small for the adapter,
you may want to buy a laboratory standard thermometer of 8mm diameter.
you could buy a thermometer pocket/well/adapter
e.g. https://www.ebay.co.uk/itm/Lab-Glass-24-29-Thermometer-Well-...
and use a thermometer or thermocouple in it.

Do not consider distillation using vacuum (actually reduced pressure, rarely 'vacuum') for now,
as almost all hobby distillations can be done at atmospheric pressure.

In my opinion, there are few occasions when you will actually NEED to use reduced pressure;
- a simple distillation of high b.p. liquids such as conc. sulphuric acid, mercury etc
- distilling or refluxing mixtures with temperature sensitive components
- short-path 'molecular' distillation.
Of the above only the first usage is likely for many years,
then you could consider a 'vacuum' distillation setup for which glassware will be of relatively low cost.

A separation funnel is (I guess) nice to have,
but a pressure equalised addition funnel is in my opinion more useful.
e.g. https://www.ebay.com/itm/25ml-500ml-Pressure-Glassware-Organ...
I wish that I had bought the type with two stopcocks
e.g. https://www.ebay.com/itm/250ml-24-40-Glass-Pressure-Equalizi...
as this allows re-filling the funnel during use.

P.S. the topics of 'best joint size' and 'cheap Chinese vs. expensive branded Western' are always arising, and there is no definitive answer,
you can find many opinions here at SM in the various forum topics.
and
'Ultimate' is a big word for a distillation setup
... I always want more and better.

[Edited on 23-9-2019 by Sulaiman]




CAUTION : Hobby Chemist, not Professional or even Amateur
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[*] posted on 23-9-2019 at 05:19
Deschem


I have ordered from deschem 5 times and not a single complaint. Glassware seems okay quality (I have glassware only from deschem, so no pieces to compare), nothing has broke for other reasons than my clumsiness. And from what I have heard - deschem will reship if something gets broken on the way.

You can find any standart piece you need on desschems ebay store, prices are one of the lowest on ebay. Make sure you choose everything in one fitting size and I think you are good to go!




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[*] posted on 23-9-2019 at 06:34


I got myself such a kit from this supplier, and have to say only the plastic clamps suck, otherwise they are working really well.
Even started switching my equipment from 29/32 to 24/40 because of these pretty neat prices.
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[*] posted on 23-9-2019 at 06:41


Quote: Originally posted by Sulaiman  

A separation funnel is (I guess) nice to have,
but a pressure equalised addition funnel is in my opinion more useful.
e.g. https://www.ebay.com/itm/25ml-500ml-Pressure-Glassware-Organ...
I wish that I had bought the type with two stopcocks
e.g. https://www.ebay.com/itm/250ml-24-40-Glass-Pressure-Equalizi...
as this allows re-filling the funnel during use.
[Edited on 23-9-2019 by Sulaiman]


Can a pressure equalizing funnel be used as a separation funnel?
The one with the 2 stopcocks perhaps?
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[*] posted on 23-9-2019 at 06:57


Quote: Originally posted by CouchHatter  
I don't know if distilling to a thin-wall Erlenmeyer under vacuum is safe, though, never done that. I guess overall that might vary by brand.


No, that is not safe. The shape of erlenmeyers is not suitable for vacuum. Erlenmeyers for vacuum filtratation are thick walled for a reason.




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[*] posted on 23-9-2019 at 07:05


Quote: Originally posted by artemov  
Can a pressure equalizing funnel be used as a separation funnel?
The one with the 2 stopcocks perhaps?

I have considered it but thought that the side tube may cause problems so not tried by me.

Generally I just use a transfer pipette to get the layer that I want
using either a beaker or measuring cylinder or test tube,
depending upon volume.
_____________________________________________________
I use a thick-walled sidearm Erlenmeyer flask for vacuum filtering as it is designed for that use,
I would not use vacuum and heat simultaneously with it,
and I would not try to use a thin-walled Erlenmeyer for vacuum - with or without heating.




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[*] posted on 23-9-2019 at 09:12


If you want to do an all glass distillation, I have 3 way distillation adapters with 10/30 glass jointed therm inlets at the top opening. I also have a few therms left with 10/30 joints, although the numbers are going down now. As well, I have lots of various extras in 24/40 joints, like claisens, gas inlets and outlets, condensers, etc. I also just found more sep funnels, so I have lots of them in almost every size from 30 ml to 4 L. I will be tied up the next week or so with some recent large orders, but should have some time to handle now orders after that. I also have some various 24/40 erlenmeyers of various types and sizes, but I also prefer round flasks for real vacuum work.

Note also, the US is now in "negotiations" to lower the US subsidy that allows Chinese vendors to mail small items to the US for almost no postage (under a dollar to anywhere in the US for many packages, which is way less than I can ship anything within the US). So if that happens, which is not clear, the price of shippnig from China may go up a lot, so if you want to buy cheap stuff from China, I would order it soon. And I have even bought a few things from Deschem, so nothing against him, just I do find it hard to compete against nearly free shipping (which is paid for mostly by the US due to an old postage traety from many years back). Just wanted to give people a heads up, as it may end soon.

[Edited on 23-9-2019 by Dr.Bob]
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Yttrium2
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[*] posted on 23-9-2019 at 13:11


Those jointed thermometers aren't cheap!

What is this for?

https://www.ebay.com/itm/14-23-19-26-24-29-Joint-Lab-Glass-T...

[Edited on 9/23/2019 by Yttrium2]
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[*] posted on 23-9-2019 at 16:38


Those are thermowells, you can use electronic sensors in them (Thermal couples) or even normal thermometers
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[*] posted on 23-9-2019 at 18:34


Have a look at simple glass to fancy glass, something I wish I'd found before I bought a PE addition funnel.

The last few sections of content at rhodium is great knowledge for amateur chemists in general.
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[*] posted on 23-9-2019 at 19:16


Sounds to me like what you want is an organic glassware kit, not a distillation set.

Those kits have a sep funnel, Claisen adaptor, and Distillation column included.

Nanshinglass has a wide variety of these at good prices on Ebay.

With luck you can pick up a used kit from a major glassware maker like Pyrex or Kimax for a bit more than a new kit of Chinese glass. They show up on ebay if you wait a bit.

Some of these kits have a Hempel column instead of a Vigreux.
You'll need packing material for those, but you can get much better performance. Vigreux columns are convenient, but not very powerful.




Ebay says they need to get their hands on my bank account if I want to keep selling there.
This sounds like the best idea since putting ortho tricresyl phosphate in Ginger Jake.
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[*] posted on 24-9-2019 at 14:17


I got a distillation set from Deschem. 1000mL boiling flask, 500mL receiver. All arrived safely, quality quite good.



Phlogiston manufacturer/supplier.

For all your phlogiston needs.
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