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einstein(not)
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The distillate was crystal clear and smelled of ethanol with no layering.
I bet you're right about going too long. I thought the residue would be where I would find the benzaldehyde so I went slow to keep from pushing it
over. Think I might try it again with what I have left.
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Nicodem
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What is the declared concentration of benzaldehyde in that "imitation almond extract"? If it is a solution of benzaldehyde in 36% alcohol then it can
not contain more than a few percent, maybe 10% utmost, of benzaldehyde.
Also, you can not separate benzaldehyde from such a solution with fractionation, because once the cosolvent gets removed in the form of 96% ethanol
you end up with a biphasic system from which benzaldehyde starts distilling with steam. You must first extract the benzaldehyde and then distil it (if
there is anything more than a couple of % in there!).
Have you checked the pH of your "imitation almond extract"? If it is older than a couple of months and if it was not protected from air it is probably
mostly oxidized to benzoic acid.
Sedit: It would be nice if you could avoid using "BzO" as a shorthand for benzaldehyde. Using shorthand formula is useful but in needs to be done
properly. Bz- is stands for the benzoyl group (PhCO-) and if you want to use it for benzaldehyde you must write BzH. BzO stands for the benzoyloxy
radical (PhCOO*).
…there is a human touch of the cultist “believer” in every theorist that he must struggle against as being
unworthy of the scientist. Some of the greatest men of science have publicly repudiated a theory which earlier they hotly defended. In this lies their
scientific temper, not in the scientific defense of the theory. - Weston La Barre (Ghost Dance, 1972)
Read the The ScienceMadness Guidelines!
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Sedit
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I did not know that thank you Nicodem. So when people use BzCl for short hand for benzyl chloride they are really writing PhCOCl?
The extract I was talking about was water, 36% alcohol mixture. Mine contained almost no benzaldahyde.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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Nicodem
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Quote: Originally posted by Sedit  | | I did not know that thank you Nicodem. So when people use BzCl for short hand for benzyl chloride they are really writing PhCOCl?
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Yes, BzCl would stand for benzoyl chloride. Benzyl chloride would be BnCl. But "Bz" is nowadays avoided in scientific literature because historically
its use is not consistent (some authors used it for benzyl as well and this inconsistency can even be found in some of the old Chem. Abstr.
entries). Personally I'm also against its use since it brings nothing but confusion and since using PhCO instead is just as simple. With benzyl (Bn)
luckily there is no historical inconsistency.
…there is a human touch of the cultist “believer” in every theorist that he must struggle against as being
unworthy of the scientist. Some of the greatest men of science have publicly repudiated a theory which earlier they hotly defended. In this lies their
scientific temper, not in the scientific defense of the theory. - Weston La Barre (Ghost Dance, 1972)
Read the The ScienceMadness Guidelines!
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Sedit
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Ok I understand now. I use to write BnCl until someone corrected me and said that BzCl is the way it needs to be written and I blindly followed after
that. Sorry for any confusion.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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einstein(not)
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Doesn't show percentage and I haven't been able to find anything online. It is a well known brand that makes many different flavorings. M******k
Only reason I chose to try it was I noticed an 8 ounce bottle of it at our local foodservice retail outlet while my wife shopped for wedding food.
The procedure I tried was based on Polverones post on the first page of this thread.
| Quote: Originally posted by Polverone | I wanted a small amount of benzaldehyde to try making bisulfite adduct with. So I grabbed from the kitchen a bottle containing "water, 36% alcohol,
and benzaldehyde" (the usual artificial flavoring stuff) and saturated some of the liquid with table salt in a large test tube. Then I extracted by
shaking it several times with unrefined automotive starting fluid and pipetting off the top layer. This top layer gave a thick mass of white,
flocculent adduct when shaken with an alcoholic bisulfite solution made according to Vogel and left to stand for several minutes. Yield of adduct was
not determined by weighing because I did not want to dry it. Half the portion of adduct was filtered then while still wet shaken with sodium carbonate
solution in a smaller test tube to give a visibly distinct and heavenly-smelling layer of benzaldehyde on top of the aqueous solution. If you're not
interested in the behavior of bisulfite adducts, the starting fluid can simply be evaporated away to give fairly pure benzaldehyde, though if done in
open air you may well lose much of the aldehyde to oxidation.
This would be a very expensive way to get benzaldehyde if you rely on the usual supermarket flavorings, but I've seen inexpensive containers of up to
300 ml artificial almond flavor at stores that target restaurant-scale customers. And of course the small Lorann Oils containers of pure benzaldehyde
("almond oil") are also available OTC at specialty cake/candy places. If you need more than 100 grams or so, though, I think the cassia oil method
looks much more attractive. |
[Edited on 15-5-2009 by einstein(not)]
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Arrhenius
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Why not have another shot at the vacuum distillation? I have a pretty good vacuum pump, which helps a lot. You'll really have to heat the boiling
flask quite hot to get the benzaldehyde to come over; probably >100ºC.
Nicodem's comment about water reiterates what I said about extracting the almond extract with ether/ethy acetate first. However, I think you might
find it considerably easier to just dry the extract with anhydrous magnesium sulfate (epsom salt... heat it in the oven for a bit to make it
anhydrous). Add the magnesium sulfate, let it sit for a while, then filter it off and carry the filtrate onto the distillation.
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Nicodem
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Or you could repeat the extraction like Polverone did with forming the bisulfite adduct in the usual fashion instead of those improvisations you
tried.
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Alastair
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Can purification be done with simple Na2SO3 (sodium sulfite)?
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Alastair
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Whoopsies, just realised this was an 2+ year old thread, ima post the question elsewhere.
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cal
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| Quote: Originally posted by Mendeleev | You know what, fuck the DEA, benzaldehyde is restricted, but they can't regulate an essential oil in my opinion. At least I don't think bitter almond
oil would actually be considered a LIST 1 chemical since it isn't pure benzaldehyde. So even if it is watched, they can't do anything about it
legally. If they get on you about it you can tell them to piss off since it isn't a chem supplier but an aromatherapy store.
[Edited on 30-12-2004 by Mendeleev] |
I have bought oil of bitter almond from a food flavoring supplier for years now. It is just a little more expensive.
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Doc B
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The flavouring round these parts has glycerine and propylene glycol along with water and natural almond flavouring. Any suggestion on extraction,
given the similarities of bp and solubilities of the ingredients?
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cal
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Bitter Almond Extract
| Quote: Originally posted by Organikum | Benzaldehyde is a list I chemical and watched. If you cannot get oil of bitter almonds locally OTC, I wouldnt recommend to order it from anywhere.
The purification depends on
- the oil, often alcohol and other stuff is added
- what you need it for, different reactions demand different grades of purity, or tolerate certain impurities or not. |
I have been purchasing Oil of Bitter Almond Extract from food supply companies for years now with no problem as it is not regulated as a food
additive. You can walk in to any restaurant supply and buy it cash no records all over the USA. 
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barley81
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I found a Polish supplier of benzaldehyde on eBay. $23 for 250mL, shipped to USA. It's a good deal, but customs would have a problem with this, right?
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DH2
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You can easily get bitter almond oil. There's a local store to me that sells it. Also, there's a brand out there that sells a diluted bitter almond
oil that's 48% vegetable oil, 52% bitter almond oil. Seeing the astronomical difference between boiling points, it's a a matter of simple
distillation to just separate the two.
Bottom line is that benzaldehyde is not exactly hard to come by. Even if you can't locate bitter almond oil (the nicest smelling essential oil of all
time, in my opinion) you should be able to easily make it from easily acquirable things like benzyl alcohol, DMSO, etc.
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Furboffle
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I quit working at a restaurant Cigar City Brewpub a couple months ago, it amazed me how much chemistry was involved in the cooking, they would buy
pure chemicals for a lot of the recipes mainly desserts and their staple, beer. But we had gallon jugs of oil of almond in the pantry, I check the
concentration and was shocked it was pure benzaldehyde. They got that specifically from the Sysco restaurant supply store. Luckily my relatives have a
sandwich shop so I have a ticket in. But if y'all have Sysco stores in your towns and know someone who runs or owns a restaurant just go buy a jug no
questions asked.
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