Sciencemadness Discussion Board

Ideas/Request for a Reaction Chamber

Steam - 26-7-2019 at 17:15

Ok so I figured I would send this one out to the collective knowledge the community.

I am doing some reactions on pieces of laminated plastic with ionic liquids and I want to be able to take high resolution time lapse images of the delamination of the plastic. However, the ionic liquids I am using are worth a quite a bit more than their weight in gold so samples are small- approximately 5 mL.

The chamber must be built with glass or non reactive metal because these liquids will make short work of most polymers.

In addition, I need to vary the temperature of the liquids up to almost 300C (liquid dependent of course). Another reason why a plastic chamber will not work.

Furthermore, I need to hold a small polymer sample about 1 square centimeter stationary and completely submerged in the liquid However, the camp can only be on one side of the polymer as not to interfere with the delamination process.

Finally I can not put a hot plate underneath because the special camera which we are using is kind of like a microscope in that it has a stage and a hot plate will not fit.

If anyone has any ideas let me know. I am feeling like this is going to need a custom glass apparatus so if any of you all know any good scientific glassblowers recommendations would be very much appreciated.

[Edited on 27-7-2019 by Steam]

Funkerman23 - 29-7-2019 at 00:49 Prism Research glass might be an option... But at the moment I am not sure if they accept custom orders from individuals or not. If you are a school or business , then that does not apply. I will return after a bit of sleep , but if you decide a custom glass peice is what you need, then I hope prism can help.

Sulaiman - 29-7-2019 at 02:07

maybe a petri dish with a heating band and a thermocouple ?

andy1988 - 29-7-2019 at 11:41

From my bookmarks on custom glassware (eventually I intend to get quotes for custom glassware myself):

American Scientific Glassblowers Society. Highlight the tab to see regions. You can often find websites for the glassblowers by searching for their name/location with "scientific glassware" term or looking at their email domain, e.g. I have no recommendations but I'd expect everyone listed on there knows each other through the society (no drop shippers!). I was just going to get quotes and pick the cheapest or nearest.

Mentioned more than once on this forum is "Eagle Lab Glass".

I don't know if you need to get sophisticated with finding the highest transmittance glass for whatever spectra the special camera measures.

I know with plastic/plasticizer research their soup-can sized steel reaction vessels are high temperature (200-300C) and high pressure, and use cylindrical mantles. I think there were small glass/sapphire/whatever viewing windows, I couldn't find the paper again at a glance.

EDIT: The paper I'm thinking of was for foam prototypes, testing plastic/plasticizer/blowing agent combinations. I couldn't find it after looking more, it was nice in that it included CAD drawings designs for the reactor vessel & component suppliers. I did find this but no CAD design for insight unfortunately.

But it does sound like you haven't quite settled on the apparatus design, maybe Sulaiman is on the right track.

You are looking for at what temperature the laminated plastic delaminates?

[Edited on 30-7-2019 by andy1988]

RedDwarf - 29-7-2019 at 12:11

How about a flat bottomed borosilicate test tube such as: (available in different diameters)

cut the tube to an appropriate length and heat it by wrapping it in nichrome.

Off course this doesn't solve your problem if you need a lid.

markx - 30-7-2019 at 03:38

Perhaps something with a reasonably massive frame from suitable metal (stainless, aluminium alloy) that can accommodate a small heating element and a thermal sensor for PID control. Flat glass windows on opposite sides for observation, PTFE gaskets....
The chamber itself can be of small volume to cope with the expensive samples. One could machine grooves in to the chamber walls or make a metallic sample holder that can be submerged into the liquid, holding the polymer sheet from sides to not obstruct the delamination process.

This tends to become very involved and complicated though......perhaps a sample holder can be made to submerge the polymers into a suitable standard glass test tube/vial. The holder could be bent from stainless wire e.g. A heating apparatus of similar kind as I described above can be made rather easily from aluminium block: it would encase a small heating element and a thermal sensor, but instead of being part of the reactor itself it would have a seating to accommodate the bottom of the glass test tube for heating purposes. Or one could sink the glass test tube into the heating block completely and drill a observation channel through the block, exposing the reaction area for observation.

Steam - 30-7-2019 at 18:27

Hey everybody, Thank you for all of your suggestions. I have never heard of flat bottomed test tubes- ordered a box to try to cut up. Got some 35mm petri dishes to try as well.
To answer andy's question. I am looking to see what effect time, temperature, and reagents have on the process. We have a HIROX microscope that can take 3D images of the sample, so I was trying to model the process in 3D as a function of time. We also have an RAMAN probe which can monitor the concentration of chemical species in situ but raman goes through glass just fine.

I think I am going to try the petri dish first unless someone or myself comes up with a better idea. I'll post some images as the project evolves in case someone else has need of something like this.