smaerd
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An Affordable Modular Rotary Evaporator
Here's my first write-up it's far from complete but I could use some input. The original work done was being done here:
http://www.sciencemadness.org/talk/viewthread.php?tid=7128
Any suggestions on things to add or test please let me know.
Attachment: write up.doc (30kB)
This file has been downloaded 1863 times
[Edited on 25-1-2013 by smaerd]
[Edited on 26-1-2013 by smaerd]
[Edited on 27-1-2013 by smaerd]
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smaerd
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Okay added some pictures here's the next one sorry for posting twice so fast.
[Edited on 23-1-2013 by smaerd]
Attachment: write up.doc (536kB)
This file has been downloaded 1620 times
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smaerd
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Alright tidied up some of the grammar and redundancy. Put in a circuit diagram heres the latest.
edit - prices updated due to this thread
http://www.sciencemadness.org/talk/viewthread.php?tid=23149
Is this an acceptable idea for a publication submission?
Edit(woelen): Removed uploaded file, it is replaced by newer version on request of smaerd.
[Edited on 25-5-14 by woelen]
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smaerd
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Alright, got new bearing today and ran some trials! Results are in and two more pictures were taken. I was actually surprised the rotary evaporator
beat out the vacuum distillation in all of the trials. Though it was close where there was more solvent per surface area.
This is it, The project is done. 
Edit(woelen): Removed uploaded file, it is replaced by newer version on request of smaerd, which can be found near the end of the thread.
[Edited on 25-5-14 by woelen]
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Magpie
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Very nice smaerd! This would be a nice project for those who like to build things.
The pictures didn't show for me.
[Edited on 26-1-2013 by Magpie]
The single most important condition for a successful synthesis is good mixing - Nicodem
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smaerd
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Thanks for letting me know I'll try and put them in another way
Does the PDF work?
Edit(woelen): Removed uploaded file, it is replaced by newer version on request of smaerd.
[Edited on 25-5-14 by woelen]
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Magpie
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Yes the pdf and pictures are good. However, the electrical circuit diagram is unreadable due to the black background.
The single most important condition for a successful synthesis is good mixing - Nicodem
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smaerd
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Thanks for the input. Changed the circuit diagram to a lighter scheme and provided the tool that was used to make it in the references.
Edit(woelen): Removed uploaded file, it is replaced by newer version on request of smaerd.
[Edited on 25-5-14 by woelen]
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smaerd
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Added standard taper symbols to the joint sizes to be more official or whatever. Also fixed up some of the wording. I'm really bad a proof-reading and
catching errors sorry... Anyways I think this is actually the last one, at least it's the one going on my web-site hehehe.
Edit(woelen): Removed uploaded file, it is replaced by newer version on request of smaerd.
[Edited on 25-5-14 by woelen]
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watson.fawkes
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I would really recommend putting in dimensioned drawings for, at the
very least, the two machined PTFE pieces. The lack of dimensioned drawings makes it harder for someone else to make use of this document as it is.
For example, in a photo you show a Keck clip. In order for that clip to work, the shaft has to be a particular diameter. Nowhere that I saw is there
mention that this dimension is important. If someone already had 1-1/4" ID pillow blocks in their parts bin but no 1" ones, it would be more
economical to use a 1-1/4" shaft. But the clip wouldn't work naively, you'd need to turn down the shaft for a bit to allow the clip to fit. So the
dimensions of the taper matter, and it's the kind of thing drawings are for.
Another thing I was looking for was a picture of how this was set up with the distillation head in place, just to see how everything is arranged on
the bench.
I would recommend taking a look at an issue of Home Shop Machinist or Machinist's Workshop (both by Village Press) for examples of
how other people write project articles.
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smaerd
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The shaft is actually just 1" outer diameter for the keck clip. The keck clip doesn't do too much holding to be honest but I put it there for good
measure I guess. I really appreciate the advice I will get to work on drawing up some more exact dimensions for the teflon attachments and reading
some more about the article format. I'll also take a picture of how I had it set up, the reason why I did not was because the way I had it set up was
very ... sloppy... The rotovap was simply placed onto a pile of wood and the glass attachment was clamped via a ring stand, stainless steel measuring
cup for a water bath, etc. I'll work on making it's implementation more practical as well. Thanks for being critical.
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smaerd
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Okay I added two schematics I drew in LibreCad and added the information using Gimp image editing program. That was not fun. I'm not an engineer, I
don't think I should have to adhere to a machinists type article base while sticking to a chemistry article. I thought about it, and my write-up
includes way more information then many of the ACS published roto-vap designs do if not the majority of them. Several of them are maybe five
paragraphs long with a picture, no tests done, no parts list for amateurs to look into let alone a redundant circuit diagram, or any explanation of
what goes where or how to improvise a pulley, etc.
I'll wait to get enough money to buy a decent metal bowl/pot and a cheap hot-plate I can dedicate to this as well as build a stand for it so it is
aesthetically appealing in use. For that final picture. Probably will be a month or so.
Anyway's here's the latest including the schematics of the teflon pieces.
Edit - I'm also not using a real roto-vap distillation head, I'm just using a 18/9 ball joint "blank"(http://www.safetyemporium.com/ILPI_Site/WebPagesUS/detail.ht...) with a bit of hose leading to a vacuum take-off(connected to a friedrich and a
flask)
Edit(woelen): Removed uploaded file, it is replaced by newer version on request of smaerd.
[Edited on 25-5-14 by woelen]
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smaerd
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Okay finished product. Got the pictures up of the whole thing working.
Attachment: An Affordable Modular Rotary Evaporator.pdf (908kB)
This file has been downloaded 2367 times
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smaerd
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The design is still holding up and working fine . Hasn't been used a tremendous
amount of times but has removed some liters of solvent now of several varieties. If I had to improve on this design here is what I would do and may
very well do in the future. Have to comment and say how refreshing it is to want solvent to be evaporated under mild conditions and 10 minutes later
be back at work.
I would use a servo motor to drive the rotor. I would have a thermostat going into the bath. I would use an arduino microcontroller to read out the
bath temperature and an LCD to display this information as well as the RPM's. I figure it would cost another 60 dollars or so but would provide very
similar functionality to a commercial rotary evaporator without too much more work.
[Edited on 18-5-2013 by smaerd]
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Nitrous2000
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A couple suggestions
Hi there,
Really, a very nice and ambitious project. On that theme, well done.
Now, a couple suggestions.
You've clearly identified the biggest challenge in this project, and that is the rotary vacuum joint. Unfortunately, it is the weakest part of your
write up. I've looked through countless (as in...."too many to bother counting"
) pdf's that you've uploaded, and not one of them actually shows the connection to the distillation column with the clear tube. You come close, but no
cigar!
So, I'd suggest the following. First, get a moderator to delete all but your final version. I suspect more than a few have download some, but not all
of your files. The second point would be to include a photo of the link between the condenser assembly and the teflon ball joint as it attaches to the
aluminum tube.
Finally, it would really add to your instructable if you actually diagrammed, in a linear fashion how all the parts fit together (including the vacuum
line and the ground glass flask that goes into the water bath). Ok, if you really want to polish it up, replace that out of focus picture of the
teflon/ground glass joint adapter! I think I see some o-rings....but I'm not sure 
Anyway, please don't take the above as anything but constructive criticism. I think you've accomplished a lot.
Oh, the following patent refers to the Yamato Scientific version of a Rotovap sealed joint. Very interesting. US005919339 dated July 6, 1999
My experiences with Rotovaps go back to my grad Chemistry days in the early 1980's. This may be a way more modern version.
Nitrous
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Steam
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I agree with Nitrous, The vacuum joint is not clearly defined at at, yet it is the most critical aspect of the design. It would be super nice if you
posted a close-up picture if it!
That being said am really liking what you are doing here, I have been thinking about building a rotovap for some time and your document is definitely
going to help!
Keep up the good work!
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No information contained in this post should be construed as legal advice from the individual author, nor is it intended to be a substitute for legal
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smaerd
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Hey Nitrous2000. Really sorry I will request a moderator to get on that. I will take a picture of the connections and diagram it more appropriately.
It still is running to this day. I have to admit the vacuum seal is not perfect and the set-up is kind of crude. There is definitely a better solution
but mine was to take the ground glass ball joint and 'mate' it with the teflon ball joint using some faucet grease to create a seal. A ring-stand
clamp holds the ground glass ball joint into place I'll work on that either today or tomorrow.
Edit - Okay asked Woelen if he would be so kind as to remove all of the attachements except for the final one. I have a bad habit of editing things a
hundred million times  .
Edit(woelen): I removed all uploaded versions, except the last one. For all other versions I placed a remark in the message, telling that there is a
newer version.
[Edited on 25-5-14 by woelen]
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smaerd
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As promised I added the picture of the connection. Please note I temporarily have wrapped the glass joint connection to the tubing in duct tape for
classiness. No, okay, well simply sticking tubing into the glass joint wasn't air tight after a few runs. Anyone experimenting with this who has
decent materials could concoct a much better connection. Viton + epoxy to a valve, etc... I am embarrassed that I haven't yet but I have been
incredibly busy and the duct tape is working fine.
It's kind of cute to revisit my writing style from 2013. I have drastically improved at technical writing, although I have no desire to improve the
text of the document anytime soon. Should be clear enough to understand what is happening without over-complicating things.
I would love to revisit this project knowing what I know now. Make a better glass to Teflon seal, do the electronics properly, create a better stand.
However, I am buried in other projects, school, and soon a temporary 'professional' research position. It still works, and doing the chemistry(when I
have the time which is rare now) means more to me than the device as of right now.
Attachment: An Affordable Modular Rotary Evaporator.pdf (979kB)
This file has been downloaded 2158 times
[Edited on 26-5-2014 by smaerd]
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smaerd
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I finally have a camera that can do short lengths of video.
Would anyone be interested in an operational video for this device?
How about a better write-up?
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Zombie
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You sir have inspired me.
A roto-evap. is one of the tools I would love to have, and your method here is, for lack of better words... Cool as hell!
I will not even begin to critique any aspect of what you have accomplished in this project BUT I do have a technical question.
Once your product has been separated, how do efficiently you recover it from the RBF? Noob question, yes. Obvious answer, no.
Great project. I'm very happy to have seen it.
They tried to have me "put to sleep" so I came back to return the favor.
Zom.
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smaerd
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That's actually a great question that stumped me until I toyed with it.
In an academic setting usually rotovaping is performed to remove ~98% of solvent. Then the flask is taken to a highvacuum line and sucked down for an
hour or so to get rid of 1.99% of solvent/volatiles. After that, a lot of people will store intermediates in the respective rbf. If the compound is
realllly dilute in solvent it will be spun down to like ~80% on the rotovap in a big flask, then transferred to a little flask and spun down 98% so
there isn't a tiny amount of compound in a ginormous flask.
At home, my rotovap yields are my yields I don't really have a means to get things any drier. In that write-up I was spinning down a sample of an
attempted indolinene imine hydrolysis I believe (was a while back), so it was pretty oily. Oils I tend to dissolve in the smallest amount of volatile
organic solvent such as DCM or acetone and transfer to a semi-closed vial to evaporate on their own. Or I'll recrystallize them in a dish -> filter
paper -> vial (some people prefer flask recrystallizations). Solids I break them up and transfer the powder/clumps via spatula, sometimes I get the
traces with DCM and do the semi-closed vial thing but usually the solid mass is good enough (the traces are great for TLC standards). Edit - I should
mention sometimes it's a ridiculous pain in the ass to scrape flasks via spatula depending on the compound, so just hitting it with solvent can save
20 minutes of scraping, but adds a few hours of evaporating.
So there are a few options when working under normal atmosphere. Vial storage, or RBF storage. RBF storage is real easy, rubber septa make it
convenient but you know as an amateur scientist I only have maybe 10 rbfs? Edit - and it always turns out that the flask I need for something else is
a baby chemical's home. A weird form of Murphy's Law. So I prefer little screw top vials even if it means using a little solvent, I have yet to run a
reaction that was effected by trace DCM.
[Edited on 10-2-2015 by smaerd]
Also thanks for the congratulations. It's been I think a year since I posted this up and still haven't seen anyone build one themselves yet. I really
hope that happens soon. I know Aga was working on something not sure if he's still in the process or not. Inspiring other's to either innovate and/or
reproduce the result was the goal.
[Edited on 10-2-2015 by smaerd]
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Zombie
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Thanks for explaining that. I was looking up tons of Evap. set ups, and very few went as far as recovering the product.
I like the idea of transferring to a smaller flask as the process is nearing completion. I think a couple cases of 10 - 50 ml RBF's are in my near
future.
See? Another project... Making a rack to store RBF's containing products... Inside the storage cabinet I still have to make... Under the bench I am
making... under the fume hood I am going to make... In the lab I have made.
And this is just the beginning???
I hope I live long enough to do you all proud. Thanks for helping. (no sarcasm, really) Thanks!
They tried to have me "put to sleep" so I came back to return the favor.
Zom.
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smaerd
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Hahaha, That's amateur science for you. A list of never ending projects. The trick is to start them while another project is nearing completion.
Things do get done and before you know it you'll be so consumed in things you are still working on that you won't even recognize how much you've
built/accomplished. At one point I didn't have a lab bench, or cabinets, or glass-ware aside from 10 test-tubes and some mason jars. It takes a
life-time to build a lab from the ground up, and the Work is never finished.
Any dope can buy equipment, but it takes a hobbyist to turn that equipment into laboratory. I've spent the last what, 5 years cultivating my
work-space and life-style into something formidable and there's miles to go. When people post pictures of their laboratories it's hard not to
appreciate all the sweat and effort they put into it.
So many unspoken and under-noted achievements have been made by this community .
It's the projects people don't talk about that are the most interesting. That's kind of what makes it fun though right? Excited to see what 2015 has
in store for us all.
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akok
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Smaerd that's a good project and effort on this rotovap!!! But it can be unproved a lot if we can find someone with 3D designing software skills. Many
parts can be made cheaply by 3D printer if there is a 3D design. Let's try to find someone that it can an upload an .stl file of the project on
thingiverse.com
I believe the following pdf manual would be a good guide for a designer to replicate the basic mechanism. http://www.lasallescientific.com/products/heidolph/BAL_LARO4...
FYI his is a example of magnetic stirrer.
http://www.thingiverse.com/thing:632714
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