Wednesday, February 24, 2016

Process Wednesday: cameras in process chemistry?

Thanks to Jyllian, I am reminded that Organic Process Research and Development has come out with its occasional (and wonderful) "Safety Notables" article [1]. Here's an interesting summary of an unusual set of experiments from a not-typical sector of research:
DSC Analysis of Liquid Sodium-Silica Reaction. 
Sodium-cooled fast reactors, used in the nuclear power industry, are typically built with steel-lined concrete. In the case of a structural failure, the liquid sodium coolant could potentially leak out and react with the concrete. This article (J. Therm. Anal. Calorim. 2015, 121, 45) looks at kinetic studies performed on the reaction of sodium with silica (SiO2) using differential scanning calorimetry. Samples of the reaction were run in open stainless-steel crucibles at different heating rates using a DSC within an argon glovebox. From the DSC data, five reaction stages were separated out using statistical deconvolution, and kinetic  parameters were calculated using the Kissinger and Ozawa methods. An interesting point about the experimental setup was the use of a videoscope with an optical fiber cable inserted into the sample crucible for viewing the sample as the reaction progresses. This allowed for a better understanding and characterization of the different reaction stages.
Certainly something I had not considered (that hot sodium and concrete could react), although it certainly seems reasonable.

It's also interesting to me that the article talks about using a "videoscope" to view the sample as the reaction progresses. I am intrigued by the possibility of sticking cameras in places we don't typically see them, i.e. inside a lab reactor or a plant reactor. I haven't heard about too many places where people are doing that, though - readers?

1. Brown, D.B.; Ironside, M.D.; Shaw, S.M. "Safety Notables: Information from the Literature." Org. Process. Res. Dev. DOI: 10.1021/acs.oprd.6b00013


  1. I remember that Ley had a recent paper where he uses his flow system connected to web cameras so that one can run everything remotely via internet.
    Great for lab work, just sit in the pub with a beer and watch your starting materials go in one end and product spitting out the other straight into the NMR or the Fujita sponge X-ray. Perhaps it will even write the publication for you?
    So all you need is a trained dummy to replenish the system.

  2. A turbidity probe is essentially a camera.

    A camera that points down into the reactor could be useful for the type of thing you might peer through the manhole to check (is it clear or soupy, did it change color?) but I would imagine they would get gunked up pretty well with solvent condensation or possibly chunks of solid if you're agitating a slurry.

  3. The obvious example for a process chemist is an inline microscope, such as Mettler's PVM.

  4. I use - err, used, before I got laid off - IP/network cameras to monitor reactions when out of the lab, at home, etc. I've trained them on temperature and pressure gauges, refluxing reactions, etc. They simply plug into an ethernet port and then you log into them remotely. I've even used them to collect kinetic data when I didn't have any other way to data log, just have it capture still photos at a designated timing.

  5. Have not really encountered cameras inside chemical reactors possibly due to harsh conditions but have seen security cameras in plants as remote monitors for dangerous operations (however wondered if in practice where something went wrong about all having watchers would do would guide recovery rather than rescue).

    On the other hand a good many of the Drug Product compounding vessels I have seen have built in video or ports to attach video lines, supposed to help confirm dissolutions but also effective in impressing clients (admittedly I found cool to watch my APIs go into solution).

  6. Off topic but the great Mean Gene Okerlund would always refer to the camera as a videoscope too

  7. @Anon 9:33 pm: I encountered just what you noted. The operators were trying to get pressure on a 10 cubic reactor in order to do a transfer. No pressure increase could be noted on the schematic on the screen, I looked at the camera and saw a fountain of reaction mixture venting out of a port. They were so intent on looking at the instruments the camera went entirely unnoticed. Well the clean up of the safety box took quite some time, not to mention disposal and doing the whole batch again (this time without yellow fountains).

  8. Some years ago I put together a setup with a glass 1L reactor, a fast camera with a telecentric lens, and a focused light source. I was following an idea published from Schering-Plough on observation of crystallization. The key was finding a glassblower who could fit an optical window in a jacketed 1L vessel.

    A few months later a group (from ETH?) published a setup with a borescope baffle to record the moment of the first crystal appearance.