Sciencemadness Discussion Board - Identification of following Apparatus

Identification of following Apparatus

CHRIS25 - 29-7-2012 at 01:54

Hallo, once again I need help please.

http://www.youtube.com/watch?v=gDojS7PWWPY

The above you tube video shows a distillation set up. Unfortunately he does not name his equipment except to call it a round bottom flask which I know is not the correct name. A search through a very extensive lab catalogue I have also does not have any pictures of this equipment. It is only the actual flask with its heads that I need to know the name of, and maybe the name of that heating unit, if there is one. I don't think three heads are necessary? But if there is a reason for the three heads I would love to know why. Again thanks once more for your help.

By the way, it will be used for the extraction of oils from plants.

Kind Regards
Chris

hames - 29-7-2012 at 02:19

Looks like an improvised soxhlet extractor to me using a pressure equalising addition funnel.I don't understand do want to know the brand name of the three necked round bottom flask or the name of the apparatus,there are heaps of uses for the three necks like having and addition funnel,mechanical stirrer and a still head on the one flask or gas inlet or additions while refluxing.

adamsium - 29-7-2012 at 06:00

Hi Chris... the flask is a three neck flask. It is indeed a round bottom flask, albeit of the three neck variant, commonly referred to simply as a 'three neck flask'. The heating unit is a heating mantle. These come in different varieties such as the 'solid' unit seen in the video, as well as 'soft' ones that basically wrap around the flask.

One advantage of having a multiple-necked flask I saw in the video was for the addition of the hot water, although you could do this by simply removing the flask from the rest of the apparatus. It may also be easier to remove the plant matter following the procedure with multiple necks, as this allows one to more easily reach more areas inside the flask, particularly the sides, for the method of removal demonstrated in the video - this could be important as I would imagine that tipping the flask on its side so that the plant matter falls to the side, inserting and twisting the brush to grab the plant matter, then withdrawing it, is likely the easiest way. If using only one neck, the brush will be right in the middle, not toward the side, so, after most of the plant matter has been removed, it may be somewhat more difficult to remove the remainder with only one centrally located neck as it will be harder to grab with the brush.

The apparatus attached to the top of the flask does indeed look like a pressure equalising addition funnel (he refers to it as a separatory funnel, but it is a pressure equalising addition funnel, not a separatory funnel) with an alihn condenser attached to the top, as hames said, being used, apparently, as an improvised soxhlet extractor.

http://en.wikipedia.org/wiki/Round-bottom_flask (see the "Gallery")
http://en.wikipedia.org/wiki/Heating_mantle
http://en.wikipedia.org/wiki/Dropping_funnel
http://en.wikipedia.org/wiki/Separatory_funnel
http://en.wikipedia.org/wiki/Soxhlet_extractor
http://en.wikipedia.org/wiki/Condenser_(laboratory)#Allihn_c...

[Edited on 29-7-2012 by adamsium]

CHRIS25 - 29-7-2012 at 06:17

Adamsium and Hames, thanks, now I can look it up. Adamsium as usual you have helped again, so many appreciations. Thankyou for all those wikpedia references. Now I have to work out the costs of everything, Mmm..

Funkerman23 - 29-7-2012 at 07:20

Quote: Originally posted by hames

Looks like an improvised soxhlet extractor to me using a pressure equalising addition funnel.I don't understand do want to know the brand name of the three necked round bottom flask or the name of the apparatus,there are heaps of uses for the three necks like having and addition funnel,mechanical stirrer and a still head on the one flask or gas inlet or additions while refluxing.

The name brand of the flask is samduk. this thread should tell you all the rest on the brand though http://www.sciencemadness.org/talk/viewthread.php?tid=12786 If I where you though I'd just buy the parts from Laboy or UGT if eBay can't help.

[Edited on 29-7-2012 by Funkerman23]

CHRIS25 - 29-7-2012 at 09:48

Thanks Funkerman, will definitely look into those two suggestions. and the thread. many appreciations.

Is there a difference between Perspex, plexi glass and ordinary sodium silicate glass when it comes to allowing UVA and/or UVB light through. In this instance I actually want the UV bandwidth.

Oh just looked at those two sites, both in the USA unfortunately.

[Edited on 29-7-2012 by CHRIS25]

Magpie - 29-7-2012 at 09:57

What is shown in the UTube video is not a proper steam distillation set-up, as any good organic chemistry lab manual would show. It's not very efficient or even economical, IMO.
Surely some searching in the forum library would show a better, cheaper set-up.

Edit- Here's a relevant thread:

http://www.sciencemadness.org/talk/viewthread.php?tid=14309

[Edited on 29-7-2012 by Magpie]

CHRIS25 - 29-7-2012 at 13:16

Quote: Originally posted by Magpie

What is shown in the UTube video is not a proper steam distillation set-up, as any good organic chemistry lab manual would show. It's not very efficient or even economical, IMO.
Surely some searching in the forum library would show a better, cheaper set-up.

Edit- Here's a relevant thread:

http://www.sciencemadness.org/talk/viewthread.php?tid=14309

[Edited on 29-7-2012 by Magpie]

Thanks Magpie, will read.

Funkerman23 - 29-7-2012 at 13:51

Given the material he was looking to extract ( video) would a soxhlet extraction give better yields?

adamsium - 29-7-2012 at 15:58

I was also going to add essentially what Magpie said. That was an unusual way to do it. I don't know that a regular soxhlet extractor would really be ideal, either, given the large volume of solid material. I'd agree that a more 'standard' steam distillation set up would be better.

The way he added 'alcohol' at the end, I think, was also a mistake (and he essentially said as much). Extracting in to a suitable solvent (i.e. one which will dissolve your product but is immiscible with water), separating with a separatory funnel (an actual separatory funnel, not an addition funnel - that would just be awkward) and then driving off the solvent if desired would be better, I dare say. Often the amount of product obtained is very, very small. I recall the first steam distillation I performed at uni - I was rather dismayed by having to dispose of my drop (it was literally a drop - barely) of eugenol that had taken me so much careful work to separate!

If you already have a distillation set up, you likely already have what you need for the 'stew' style steam distillation.

Edit: I also meant to add... I think that the main benefit of soxhlet extraction is that it is essentially a reflux process, thereby concentrating the solute in the solvent on each cycle. Although I know in general terms what soxhlet extraction is and for what it is used, I don't yet have any practical experience, so I'll let others comment on its merits here if necessary.

Edit 2: Magpie beat me to it with my edit. But the essence of his post agrees with what I was thinking.

[Edited on 30-7-2012 by adamsium]

[Edited on 30-7-2012 by adamsium]

Magpie - 29-7-2012 at 16:00

Quote: Originally posted by Funkerman23

Given the material he was looking to extract ( video) would a soxhlet extraction give better yields?

Steam distillation, when applicable, is much simpler I think. With a Soxhlet extraction one usually uses an organic solvent like ether or ethanol. This solvent must then be removed from the extracted oil by evaporation or distillation. With steam distillation a simple separation with a separatory funnel, or even just decantation, is all that is required. Soxhlet batch size would also normally be much smaller than with steam distillation using a 1000 mL RBF.

The best technique likely depends on the oil, and I know nothing about geranium oil per se

I keep telling my wife I am going to make her some rose perfume using our backyard roses and my Soxhlet apparatus.

If you had to choose one technique over the other I would think that it very much depends on what you plan to do. I have equipment for both but haven't yet used my Soxhlet apparatus.

CHRIS25 - 30-7-2012 at 23:00

I'll have to read through your materials again and then watch the video with a better understanding. It puzzled me why a normal Cheaper water distillation could not have been used? The soxhlet setup is far too expensive, I was looking at both new and some second hand set ups, out of the question. But a normal water distillation set up I could manage. Yes it's my wife that watched the video and got excited not realising that I would have to do all the learning!

So to sum up, Adamsium:"Extracting in to a suitable solvent (i.e. one which will dissolve your product but is immiscible with water), separating with a separatory funnel (an actual separatory funnel, not an addition funnel - that would just be awkward) and then driving off the solvent if desired would be better, I dare say". This is the Better route. But both you and Magpie agree that a normal cheaper water distillation set up would achieve the same end result, or just a satisfactory result?

Thankyou guys, you are a great help.

zoombafu - 30-7-2012 at 23:05

I remember seeing a video on youtube a while back of someone explaining their homemade soxhlet extractor. They used a pressure equalizing addition funnel and round bottomed flask. I cant seem to find it now.

Rogeryermaw - 30-7-2012 at 23:31

Quote: Originally posted by zoombafu

I remember seeing a video on youtube a while back of someone explaining their homemade soxhlet extractor. They used a pressure equalizing addition funnel and round bottomed flask. I cant seem to find it now.

that plus a condenser on top is what i use. at least till i can afford a real one. it's a bit of a pain getting the packing and sample in and out of a 24/40 joint but it definitely works. bad part is you can't just let it run. you have to baby sit it since there's no siphon.

adamsium - 31-7-2012 at 00:31

Quote: Originally posted by zoombafu

That's what this video mentioned here used.

Chris, as for the result you'd achieve, that's really where I can't help a lot. As I mentioned, although I know what soxhlet extraction is and how it's used, I have no practical experience with it yet (though I have some with steam distillation). Basically, I'd expect you can get a greater concentration and quite possibly yield with soxhlet extraction as the extraction essentially repeats over and over with 'fresh' lots of solvent. It's not actually fresh solvent, of course, it's simply being refluxed... so, at the beginning of each cycle, the concentration of the solute in the solvent will be essentially nil, meaning that more solute can dissolve in to it, then the now solute-bearing liquor flows back in to the flask below, to be re-evaoprated (meaning it is 'fresh' - the solute is left behind in the flask) and condensed to flood the chamber holding the material in order to dissolve more of the product from it.

So, the difference is, with regular steam distillation, you're only going to get whatever is dissolved in to the water / steam the first (only) time (though you could perform subsequent distillations and combine the products - this would be somewhat more work, though, obviously. With soxhlet extraction, the solvent is evaporated, the solid mass soaks in to it, giving up some of the product, the liquor drains, is re-evaoprated, dissolves more product, liquor is drained..... etc. This basically means that you can draw much more of the product out with a given volume of solvent when using soxhlet extraction, since it is 'refreshed' on each cycle.

Also, just as a side note - in determining what type of equipment to purchase, I'd expect that a regular distillation set up would be far more useful in general for other projects. With a good set, you can perform a very wide range of experiments. Unless you plan to extract from plant matter and such regularly, a soxhlet extractor is probably of a poor cost/benefit ratio to you.