Author Topic: Brown camphor oil and safrole  (Read 211 times)

uchiacon

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Brown camphor oil and safrole
« on: January 30, 2012, 02:22:59 AM »
Hey guys,

I bought 800ml of brown camphor oil that I was told was at least 90% safrole. It has an overpowering camphor smell and a teak brown hue. I tried freezing it by leaving a small amount in the freezer for a few days in a small bottle. Nothing resulted, I tried this several times and no oils solidified out. I weighed it and found that it had a density of 0.87g/ml.

Then I tried a vacuum distillation. I received about 400mls of a quite thin liquor that came over around 200C. It has a stronger camphor smell than the original mix and is almost completely colourless. Then a second fraction that came over around 250-260C. Light brownish colour with less camphor smell, but evidently still there.

A dark brown/red liquid is still remaining in the distillation flask. It has a faint smell of camphor to it but I cannot detect a strong presence of the typical safrole smell that it should possess.

The seller was adamant that it was over 90% safrole and told me it had been quality tested for 94% safrole on an earlier order of several thousand litres that was sent to a fragrance manufacturer. They could not provide an accurate break down of the constituents of the oil however.

According to the density of roughly 0.9g/ml (safrole being 1.1g/ml), is it possible that this oil is even over 80% safrole? No doubt it has scores of other camphor related compounds present in it, but I have no accurate way of finding out what these could be. I am thinking about demanding a replacement 800mls as it does not seem like I have been sent anything near 90% safrole.

The only thing that tells me that the oil has some kind of safrole content is that when the flasks are rinsed and the camphor smell washes away, a beautiful sweet candy smelling aroma is left behind, and it's pretty difficult to remove. It doesn't help that the camphor over powers any kind of safrole smell either. What do you guys think?

lugh

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Re: Brown camphor oil and safrole
« Reply #1 on: January 30, 2012, 03:50:37 AM »
Quote
What do you guys think?

The seller is lying about the type of oil he's selling:

http://www.erowid.org/archive/rhodium/chemistry/safrolefaq.html

ask for a refund  ;)  Don't deal with him anymore  8)
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Wizard X

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Re: Brown camphor oil and safrole
« Reply #2 on: January 30, 2012, 04:48:10 AM »
From Plant drug analysis: a thin layer chromatography atlas By Hildebert Wagner, Sabine Bladt.

Albert Einstein - "Great ideas often receive violent opposition from mediocre minds."

nigluhS

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Re: Brown camphor oil and safrole
« Reply #3 on: January 30, 2012, 12:17:37 PM »
I had 98+% pure sass and freezing ain't the easiest from my novice experience. Read up on everything I could, tried it on a spoon, and a tiny bit in a beaker. Did the blow on it thing to create crystals, etc.
Never froze, even at -16 C.

Been told with good pure oil, a good wash the glacial acetic acid, and then a baking soda wash would handle the purification process. Or with pure oil like it, just work with the 1-2 impurities that are there.

we'll see how that goes.
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fresh1

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Re: Brown camphor oil and safrole
« Reply #4 on: January 30, 2012, 03:13:33 PM »
sadly rip off are rife, and make for disappointing experiences

 I know anything "real" is pretty hard to come by these days where I live not impossible, but few, and faaarrr between, so...

are you somewhere you can find a plant source

steam distillation isnt hard

hey nigluhS just curious as to how you decided your saffy was 98%

 how did you decide this?
"Curiosity is a gift"

nigluhS

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Re: Brown camphor oil and safrole
« Reply #5 on: January 30, 2012, 05:03:16 PM »
I am trusting a reliable source that referred me to vendor, so there is some room for error I suppose.

I highly doubt I am getting snowed on this one though.
when the wasps and the bumblebees have a party, nobody comes that can't buzz...

uchiacon

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Re: Brown camphor oil and safrole
« Reply #6 on: January 30, 2012, 09:16:06 PM »
Hm, thanks for the input guys. This seperation process is a lot harder than originally anticipated.

I'm not in a country that has a lot of people, or any common plants that produce significant amounts of safrole. I don't like the idea of growing my own hoja santa as this would force me to stay at one residence for several years to get any decent yields. More or less out of the question to grow it.

The final remaining liquid after I removed the two fractions has a safrole smell to it. Boils at 234C, but has a density of 0.916g/ml and a dark brown red colour to it. Which confuses me considering its about 20% lighter than pure safrole but still exhibits the same boiling point?

You can use 80% pure safrole for ketone through a wacker can't you? Or does it need to be higher?

DopeBee

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Re: Brown camphor oil and safrole
« Reply #7 on: January 30, 2012, 10:15:23 PM »
Pretty much every company from those B2B sites like alibaba.com are shady at best.

uchiacon

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Re: Brown camphor oil and safrole
« Reply #8 on: January 31, 2012, 09:12:17 PM »
Pretty much every company from those B2B sites like alibaba.com are shady at best.

Yes, they just seem to waste my time and end up giving a refund when they send the wrong shit to me...