DP
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Calamus Oil Distillation Problems
125ml of calamus essential oil was distilled by fractional vacuum distillation @ 10 torr. At ~105C a highly refractive clear fraction started coming
over really fast and stopped at ~135C. It smelled just like the calamus oil, but not quite as strong... ~115ml was collected. Then at ~150C another
fraction started coming over, but much slower. It was also clear and didn't seem to refract light as much. This second fraction smelled a little
different... almost like the calamus oil, but there was like an ammonia type smell or something. This stopped coming over ~168C. This fraction was
only ~10ml. There was a very small amount of liquid in the distillation flask that was starting to turn dark brown so I stopped distilling. The
receiving flasks where left in the freezer on the highest setting for three hours to see if anything would freeze and nothing did.
Well... based on the distillation it’s pretty obvious whatever these are it's definitely not B-asarone. I was kind of in a rush when I
distilled it and I think I turned the heat up too fast. I started at 100C... then like 30min later 200C and at about an hour 300C so this may be why
it seems like it has no B-asarone etc. Also, my thermometer didn't seem to be working right... the mercury was all the way at the top throughout
the whole distillation... I guess I should have soaked it in ice water first or something. I just went by the temp of the oil bath and all temps
stated here is the temp of the bath, which is normally 25-30 degrees hotter than the solution of course. Should I toss it out or redistill? I added
the brown liquid to the 10ml hopping they both contain B-asarone. What's the best way to test for the presence of B-asarone without some high
priced equipment? This calamus oil was suspect from the beginning though because it was almost clear when I first got it and everyone says their oil
is dark yellow or yellow. Maybe it's really some low boiling fraction instead or has its asarone(s) removed. The CoA the supplier has
doesn't say much other than it’s from India and that it's steam distilled from the roots and they don't know anything else. This is
wishful thinking, but maybe its asarone content is so high that makes it look clear. Anyway, I look forward to any help you chem Guru's can give
me.
[Edited on 26-7-2005 by DP]
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flyingbanana
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Here's some random tidbits of calamus essential oil info that might help you on your journey:
Acorus Calamus oil
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Jammu, India variety:
beta-asarone 75.80%
calamene 3.84%
gamma-asarone 3.20%
alpha-asarone 1.32% mp:62-63°C bp:296°C
camphene 0.92% mp:51-52°C bp:158°C
beta-pinene 0.56% bp:165°C
asaronaldehyde 0.20%
D(20°C) 0.96-0.97
V Sl Sol H2O, Miscible EtOH
Asarones:
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Alpha:
Alpha-asarone (trans-2,4,5-Trimethoxy-1-propenylbenzene),
needles from light petroleum
mp 62-63°C, bp 296°C, d(20°C)1.165
Insoluble in water, soluble in alcohol, ether,
HOAc, CCl4, CHCl3, petroleum ether.
Beta:
Beta-asarone (cis-2,4,5-Trimethoxy-1-propenylbenzene)
C12H16O3, mw:208.26 d1.073
Gamma:
gamma-asarone (euasarone, selishone, calamol)
(2,4,5-Trimethoxy-allylbenzene)
C12H16O3, mw:208.26 bp685 283°C d(20°C)1.078
Distillation of 200ml of indian calamus oil at approx. 25 torr (aspirator
vacuum) yields three fractions coming over at these approx. temperatures.
The fraction intervals are around 5, 2.5 and 2.5 degrees.
140-145°C ~20 gram fraction with sharp smell (calamene/pinene etc.)
145-147.5°C ~40 gram fraction with aromatic smell (alpha/beta/gamma-asarone)
147.5-150°C ~140 gram fraction with aromatic smell (beta-asarone)
Redistillation of the two lower fractions yields the following fractions:
115-144°C ~21 gram, (calamene, pinene etc.)
144-147°C ~28 gram, (alpha/gamma-asarone)
147-150°C ~11 gram, (beta-asarone)
Each fraction has its own unique smell, with the first fraction being most
distinct. It is also slightly more yellow than the other two. One can tell
between the two other fractions after this redistillation, but not before.
The Total yield of beta-asarone is 75.5%, and of alpha/gamma-asarone 14%.
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DP
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Wow! Thanks for all the info! I have found a much better source for Calamus oil and I will do another distillation (much slower this time  ) once it has arrived.
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