Sciencemadness Discussion Board

Steam Distillation semi-disasters

arkoma - 13-7-2014 at 05:39

Yesterday I decided to try and get cinnamon oil from ground cinnamon for a friend of mine in Cali--I knew not expect much--it's more the point of "do it cause I can" and my friend MB uses it for "spiritual" purposes so therefore it would mean more to her.

Anyway, using my guerilla balance I weighed out 20gms ground cinnamon


And then I charged my 250ml Erlenmeyer with the cinnamon, 150ml of distilled water and 2 drops of "Dawn" as a wetting agent. No stir capability at the moment. The flask capacity was my big FekUp.



Off to the (stupid) races!!! I used the flat bottom, cause I didna wanna be arsed to set up my oil bath (five WHOLE minutes) for an RBF.



Anyhow, I spent ages babysitting this critter:

0818 Started heating
0845 Boiling-stillhead at 78c
0948 Stillhead at 98c--distillate with oil visible in the receiving flask



I'm like YEAH, and turned up the heat. Bad Idea. Bumping commenced





there is a good end to this sad sad story--spending five minutes, I set up my oil bath and redistilled my oil.



I was surprised that it is heavier than water.


[Edited on 7-13-2014 by arkoma]

aga - 13-7-2014 at 06:00

I use bits of broken glass as boiling chips, and do help to reduce the bumping severity.

arkoma - 13-7-2014 at 06:14

I guess I didna mention it, but in the photo showing the funnel in the flask, there are bits of broken glass on the counter I used as chips. However, I damn sure violated the "rule" of overfilling my flask--150ml of water and 20gms of cinnamon in a 250ml flask. Soon as I feel like braving Phoenix heat gonna go get ice and do it again :)

Edit--I posted the "tale of my disaster" for the benefit of other n00bs in a hurry/looking to shortcut LOL

[Edited on 7-13-2014 by arkoma]

blogfast25 - 13-7-2014 at 06:15

It seems unlikely to me that cinnamon bark oil (there's also cinnamon leaf oil) is more dense than water. Typical components of (leaf) oil are eugenol, eugenol acetate, cinnamic aldehyde and benzyl benzoate, all of which contain carbon, hydrogen and oxygen only and as a result have densities slightly lower than 1. This is a general rule of thumb for organics: unless you introduce heavier exoatoms like Cl or other heavier than oxygen atoms into organic molecules, you end up with something less dense than water.

Use anti-bumping pebbles to reduce/eliminate bumping. Sharp edged glass can work but aren't ideal because the contain little porosity. Round bottoms also help.

I like your 'guerrilla scales' but mine (thirty years ago) was smaller and more accurate I think. I used an aluminium curtain rail (an I profile, about 50 cm long) and the Roman (asymmetric) design with water calibration:

http://en.wikipedia.org/wiki/Steelyard_balance

It worked very well, even for small weighings (< 5 g).

Photos are over sized: See FAQ on how to reduce size.

[Edited on 13-7-2014 by blogfast25]

arkoma - 13-7-2014 at 06:25

photos were links--no server load to speak of--however I changen to thumbs. And I beg to differ over the density as cinnamaldehyde is a major ingredient::
Quote:
Cinnamaldehyde is the organic compound that gives cinnamon its flavor and odor. This pale yellow, viscous liquid occurs naturally in the bark of cinnamon trees and other species of the genus Cinnamomum. Wikipedia
Formula: C9H8O
Density: 1.05 g/cm³
Melting point: 18.5°F (-7.5°C)
Molar mass: 132.16 g/mol
Boiling point: 478.4°F (248°C)


not much denser than water, but denser nonetheless

Edit--not much better pic of my product, but definitely a "yellow, viscous liquid" under the water--super strong cinnamon smell




[Edited on 7-13-2014 by arkoma]

blogfast25 - 13-7-2014 at 06:51

Relatively very expensive cinnamaldehyde though: so little from 20 g of ground cinnamon.

arkoma - 13-7-2014 at 06:58

Quote: Originally posted by blogfast25  
Relatively very expensive cinnamaldehyde though: so little from 20 g of ground cinnamon.


yes indeed--but heck, I ain't doing this stuff for anything but "fun" The $3.95 I spent on the can of cinnamon has already provided a priceless benefit to me.

edit--and there is about 90gm of it left w00t. My yield ought to be higher as I get this stuff dialed in. Why I am still posting in "beginnings" I'm a beginner.

[Edited on 7-13-2014 by arkoma]

Texium - 14-7-2014 at 09:47

Sounds like fun! I'll have to test that out as one of the first things I do with some of my new distillation equipment once I get it all cleaned up. For some reason we have two or three bottles of cinnamon, and rarely ever use it, so I'll sacrifice one to chemistry.