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Hive BB  Methods
Discourse  Question
for Bright Star, about Step 1
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| Author | Topic: Question for Bright Star, about Step 1 |
| takkimitsu Hive Bee |
posted 01-13-2000 10:13 AM
When first reading STEP 1, I thought it described simple distilation of sassafras (or yellow camphor), where just the safrole came over into the reciving flask. For this to be the case, safrole would have to be the component of the oil with the lowest boiling point (even under vacuum). But according to eleusis' document, sassafras oil is 10% phellandrene. Phellandrene has a boiling point of 171C, lower of that than safrole(232C). Do you mean that the safrole will remain in the boiling flask? For this to be true, safrole must be the component with the highest boiling point (which it might be, I dont know). But regardless of whichever flask you find the safrole, it seems these two components (safrole & phellandrene) wouldnt seperate very effectively using vacuum simple distillation. I know I'm missing somthing, could you please help? ------------------ |
| Bright
Star Hive Bee |
posted 01-13-2000 02:40 PM
There are many different sources for safrole. Yellow Camphor is one of them. There are many different sources of Yellow Camphor, and different sources/species, will have different amounts of safrole, and other components. Now, you can do a atmospheric (at ambient pressure, no vac) distillation of it and see. Only collect the stuff that comes over at 232C. If you want to do a vac distillation like the instruction says ... Put on the end of the distillation condenser another distillation adapter. This will allow you to have two recieving flasks. So when you get a little for-run, you can continue with the distillation, until it stops, rotate the distillation adapter, and then collect the saf. Either way, just collect the stuff that comes over at 232C. IE you can switch the flasks ... Was that what you wanted? |
| APOPLEX Hive Bee |
posted 01-13-2000 05:21 PM
Wash your Oil with 5% NaO, then three time with dH2O. Freeze this Sassafras Oil in the fridge. It freezes very hard. More Sassafras Oil want to take an eternity to freeze, even at -18°C. If it is solid, remove it from the fridge and let it come to between 8-11°C. Crusch the solid, wich contains mostly Safrole. At the above temp. some liquid should be formed. Crush the Sassafras and put the whole mass into a funnel to filter off the impurities. This is clean Safrole. Use it as it is, or distill it under reduced Pressurefor form ultra purity. ----------------- |
| scwam Hive Bee |
posted 01-13-2000 06:18 PM
Swinm has virtually mastered this freezing technique and can get raw oil to freeze anywhere between 0c to 6c w/o problems. The trick is to put the oil in a large container that will allow much surface area to be exposed to air, leave it open in a can overnight to collect dust and cyrstallization is almost immediate as soon as a small seed crystal is added (simply by spreading a few drops on the sides of the can and they turn to ice and become the seed). You can either buchner the stuff, the ideal temp for getting a clear oil is right at 8-10c. Throw the frozen oil in a blender and make it into a smoothee (works best with large amouts, over 200ml). immediately buchner that while its at that warm temp, first run changes it to pale yellow, second run even lighter. He recently discovered by accident that the resulting "dirty" orange oil when subject to 0c and not disturbed will start growing even more pure shards of safrole over 2 to 3 days. He even got shards the thickness and length of standard pencils once. Carefully Drain off the orange oil by turning the can upside-down over a strainer and after 3 days the crystals in the can are ready for use. These crystals need no filtration and when melted will result in a absolutely clear oil that has almost no smell at all (it recrystallizes at 11c with no effort) |
| scwam Hive Bee |
posted 01-13-2000 06:19 PM
Oh, and dont use a blender that is made from plastic or it will melt, use only glass. |
| Niels
Bohr Hive Bee |
posted 01-13-2000 09:55 PM
It sounds as if you might have perfected the purification via freezing/crystallization, but when I thought I had pure honey using the freezing technique, I checked the melting point of the picrate salt made with this method and it was lower than fractionally distilled sassafras oil fraction, indicating that it was still impure. The oil always has that typical anise smell, you just think you cannot
smell your purified oil because it is so strong that it desensitizes your
sense of smell after two or three whifs. |
| takkimitsu Hive Bee |
posted 01-14-2000 12:07 PM
Thanx Bright Star. So what youre saying is.. if i follow step one just as it says, my safrole will be impure? because it will contain components with lower boiling points? At any rate.. I supose i could just take each portion (by itself) as it
comes over at its respective temperature. ------------------ |
| Osmium PimpBee |
posted 01-14-2000 12:11 PM
>i could just take each portion (by itself) as >it comes over at its respective temperature. Absolutely. That's what we call distillation. |
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