NEMO-Chemistry
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Slightly unusal crystals
I have been thinking of doing some crystal growing after I have done the chili extraction. I think crystal growing is a kind of 'right of passage' for
anyone taking up chemistry  , I was putting together a list of crystals I would
like to grow, when it occurred to me that my list was probably exactly the same as everyone starts with!
While there is nothing wrong with that as such, i figured it was unlikely 'ANOTHER' copper sulphate crystal growing thread would draw much interest.
So i had a rethink and decided I would try and do some plant extractions and get crystals from those!
first on my hit list is menthol from mint, i chose this because our mint is in top form at the moment and hopefully will have plenty of menthol in.
I like the shape of the needle like crystals as well. I have yet to read up and see what is the best way to extract and purify, but as i find more
information i will post it here (if thats ok) so everything is in one place for me .
After loosing the pepper papers and being a completely HDD disorganized person, having a thread with the papers in and experimental notes will be
useful for me .
Depending on what solvent's are used I should be doing this in the next couple of days unless I have to order some solvents, I will be making some
chloroform and acetone on Weds.
I also have more ethanol being made (yeast) and hope to try out my home made solar still, nothing special but might help with electric costs even if
it only gets me to azeotropic strength then it will save agro from the parents and the electric bill  .
If anyone has some plant based crystal suggestions for me I would be grateful. piperine springs to mind as well.
I will post my chosen ones here as I think of them and post the results as I do them over the next couple of weeks.
I will start with ones i have the reagents for already, I can order some solvents this week for some of the other ones.
[Edited on 30-5-2016 by NEMO-Chemistry]
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NEMO-Chemistry
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managed to find a patent for separating the menthol but I dont think its going to be much use. The abstract sounded straight forward with 'fractional
distillation' being used, but then the devil in the detail was it used a 50 plate column!
Now I dont know exactly what that means but I do know my little vigreaux condenser is probably a bit under that , ok maybe its a massive amount under lol.
Still reading through some papers at the moment, most seem attached to research gate and I cant get an account there. It seems google scholar favors
research gate, does anyone know the name of a free paper research site? I was told one a month or so back but i cant remember what it was called now.
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Fulmen
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Sci-hub will probably work. As for 50 plates, this will tell you the plate equivalent for a filled column: http://homedistiller.org/calcs/hetp_calc
We're not banging rocks together here. We know how to put a man back together.
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UC235
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Plenty of mint varieties contain no menthol at all, notably spearmint. The best varieties for menthol production are Mentha piperita (peppermint) and
especially Mentha arvensis (corn mint). Menthol can be isolated from the essential oil of the latter by simply cooling it and is the basis for
commercial production of natural menthol.
[Edited on 30-5-2016 by UC235]
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NEMO-Chemistry
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Thank you for the information. I thought 50 plates would be a little hard to do lol!
I have no idea which mint we have, I know we have water mint and 2 others but I have no idea which they are. Cant hurt to try can it
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NEMO-Chemistry
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Caffeine would be another, i know the yields are low from coffee but it feels slightly more in the spirit of things to use it rather than caffeine
pills.
Looking around at different spices there seems to be a few that have compounds with crystals, i just thought it would be slightly more cool than just
doing the normal copper sulphate type ones. I have done copper sulphate but left the solution in a 1 ltr too long (months) and the crystals eventually
seem to have cracked the beaker!!
While not from a plant I would also like to do sulphur as I like the crystal's.
Anyone got any thoughts on compounds that are crystalline and extract-able from plants?
Three months ago not long after I started Chemistry I put some cloves in chloroform in a small bottle. It now has 3 very distinct layers, the bottom
layer is a very deep red colour and slightly viscous, the middle layer is like a amber oil and more viscous than the bottom layer. The very top layer
seems watery but has a yellow tinge to it. If I shake the bottle up then the layers combine but separate again very quickly, the top layer I am sure
contains water as the whole thing goes milky white if you shake it all up.
I hope to have some TLC plates arriving soon so I can do some TLC experiments with the three layers, I will get some pictures at the same time. Any
ideas for a good solvent mix to do some TLC experiments on these layers? I also have a small amount of iodine coming so I can develop the plates.
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Fulmen
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Raphael Ikan's "Natural products, a laboratory guide" has a procedure for caffeine from black tea, it lists the content as 2 - 4,6%.
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NEMO-Chemistry
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Quote: Originally posted by Fulmen  | | Raphael Ikan's "Natural products, a laboratory guide" has a procedure for caffeine from black tea, it lists the content as 2 - 4,6%.
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Thanks for that, I will see if I can get a copy of that book.
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Fulmen
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Heres a rough transcript :
100g of tea is extracted for 3 hours with 400ml 95% EtOH (soxhlet or similar apparatus). The extract is mixed with 50g MgO and 300ml H2O and
evaporated to dryness with stirring. The residue is boiled with 500ml H2O, then 2x250ml and filtered hot.
50ml 10% H2SO4 is added to the filtrate and reduced in vacuo to 1/3 volume. It is again filtered hot and extracted with 5x30ml chloroform. The rxtract
is then decolorized by adding a few ml's of 1% NaOH and evaporated. The crude caffeine is then recrystallized from a very small volume of hot H2O.
Yield: 2-2.5g
Murexide test: A few crystals and 3drops of HNO3 is evaporated to dryness in a porcelain dish. 2 drops of NH3 imparts a purple color.
We're not banging rocks together here. We know how to put a man back together.
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NEMO-Chemistry
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| Quote: Originally posted by Fulmen | Heres a rough transcript :
100g of tea is extracted for 3 hours with 400ml 95% EtOH (soxhlet or similar apparatus). The extract is mixed with 50g MgO and 300ml H2O and
evaporated to dryness with stirring. The residue is boiled with 500ml H2O, then 2x250ml and filtered hot.
50ml 10% H2SO4 is added to the filtrate and reduced in vacuo to 1/3 volume. It is again filtered hot and extracted with 5x30ml chloroform. The rxtract
is then decolorized by adding a few ml's of 1% NaOH and evaporated. The crude caffeine is then recrystallized from a very small volume of hot H2O.
Yield: 2-2.5g
Murexide test: A few crystals and 3drops of HNO3 is evaporated to dryness in a porcelain dish. 2 drops of NH3 imparts a purple color.
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Thanks for that, sounds like a good book I will try and get hold of it.
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NEMO-Chemistry
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I am going to try a couple of mint extractions using different methods from several papers. I have picked the first two lots of mint leaves and have
them drying in the desiccator box over sodium hydroxide prills. I have picked 500g of leaves. The leaves are in a sealed plastic box (sealed with
model clay) and placed the leaves in a ovenware dish on top of the prills.
There wasnt enough leaves to pick for doing a green steam distillation, so by the time the desiccator has done its job the mint should have grown back
enough to pick some more .
We only have cheapo tea bags so will get some leaf tea when my mum goes shopping later in the week.
Reading up it looks like the yellow oil in the cloves bottle with chloroform is probably eugenol.
I need to do some more reading to see what the other two layers are and some TLC plates when I get the iodine.
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NEMO-Chemistry
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| Quote: Originally posted by NEMO-Chemistry | Caffeine would be another, i know the yields are low from coffee but it feels slightly more in the spirit of things to use it rather than caffeine
pills.
Looking around at different spices there seems to be a few that have compounds with crystals, i just thought it would be slightly more cool than just
doing the normal copper sulphate type ones. I have done copper sulphate but left the solution in a 1 ltr too long (months) and the crystals eventually
seem to have cracked the beaker!!
While not from a plant I would also like to do sulphur as I like the crystal's.
Anyone got any thoughts on compounds that are crystalline and extract-able from plants?
Three months ago not long after I started Chemistry I put some cloves in chloroform in a small bottle. It now has 3 very distinct layers, the bottom
layer is a very deep red colour and slightly viscous, the middle layer is like a amber oil and more viscous than the bottom layer. The very top layer
seems watery but has a yellow tinge to it. If I shake the bottle up then the layers combine but separate again very quickly, the top layer I am sure
contains water as the whole thing goes milky white if you shake it all up.
I hope to have some TLC plates arriving soon so I can do some TLC experiments with the three layers, I will get some pictures at the same time. Any
ideas for a good solvent mix to do some TLC experiments on these layers? I also have a small amount of iodine coming so I can develop the plates.
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Had mixed luck today.
I got a new/very old stock long burete arrive from ebay today, the glass stopcock is/was frozen, i decided i would try and unfreeze it with some hot
water. as i got to the sink i caught the tip of the end on the tap!
So i have snapped the end off! i will post some pics tomorrow (too angry with myself now), if i can get the stopcock unfrozen then the way its snapped
i might be able to use some silicon tubing and turn it into a kind of chromatography column, not ideal but makes the best out of the situation.
I was given some tiny size ten parts as well, i have a tiny sep funnel and test tube and flask. Also some very small distillation parts including a
vacuum flask.
I dont have a condenser that would fit yet but it will come in handy, especially the tiny sep funnel for the eugenol and clove stuff i have.
I am doing other things tomorrow but should get a chance to do some pictures friday.
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NEMO-Chemistry
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Well didnt go swimming! So got some pics, the first shows the three layers. I am not sure which is contains what yet! But the bottom layer looks like
the tannins, you cant tell from the pic but there seems to be two tannin layers.
The top most dark layer has a very defined interface from the middle layer. I am starting to think the middle layer is chloroform mainly and the top
layer the oils.
 
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NEMO-Chemistry
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My TLC went badly, as a noob i retain my right not to detail what happened! but looks like my carefully researched solvent didnt work on the plate and
all the bands shot to the top in one lump!!
So ordered more plates and will try again, why are the plates so much money?
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Deathunter88
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| Quote: Originally posted by NEMO-Chemistry | My TLC went badly, as a noob i retain my right not to detail what happened! but looks like my carefully researched solvent didnt work on the plate and
all the bands shot to the top in one lump!!
So ordered more plates and will try again, why are the plates so much money? |
Make your own plates; cheap, effective, and easy.
[Edited on 9-6-2016 by Deathunter88]
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NEMO-Chemistry
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| Quote: Originally posted by Deathunter88 | | Quote: Originally posted by NEMO-Chemistry | My TLC went badly, as a noob i retain my right not to detail what happened! but looks like my carefully researched solvent didnt work on the plate and
all the bands shot to the top in one lump!!
So ordered more plates and will try again, why are the plates so much money? |
Make your own plates; cheap, effective, and easy.
[Edited on 9-6-2016 by Deathunter88] |
I will look into that, i purchased plates because i was hoping for good results. My confidence in making plates that would work well is not high! I
used chloroform for the extraction, anyone have an idea what each layers is? In particular which is likely to be the oil layer?
It was hard to tell when separating, the top seemed more watery but i assumed oil would float on a more watery layer?
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