Brand in question: Sunnyside VM&P Naphtha

I want to isolate some pentane and hexane from the naphtha i got, and so far i only have basic equipment:
( 1L electromantle, distillation flask, 200mm liebig, 200mm graham, 90deg vacuum adapter, homemade water aspirator, and typical basic glassware and support rods/clamps )

Is it possible for me to do that without vigreux? can i use one of the other condensers i do have? do i even need fractionating column in this process? what if i would just heat my naphtha to 36.1^C and collect the condensed vapor would it be significantly polluted with other condensed volatile constitutients of naphtha? How would i go about setting up my labware to get this done?

Brand in question: Sunnyside VM&P Naphtha

I want to isolate some pentane and hexane from the naphtha i got, and so far i only have basic equipment:
( 1L electromantle, distillation flask, 200mm liebig, 200mm graham, 90deg vacuum adapter, homemade water aspirator, and typical basic glassware and support rods/clamps )

Is it possible for me to do that without vigreux? can i use one of the other condensers i do have? do i even need fractionating column in this process? what if i would just heat my naphtha to 36.1^C and collect the condensed vapor would it be significantly polluted with other condensed volatile constitutients of naphtha? How would i go about setting up my labware to get this done?

Look at the bp °C of both chemicals, if i recall general rule is if the difference is smaller then 30 no need for a fractionating column, but i am afraid you will have to ! :(

Look in vogel lab handbook!

Look also the solubility of your solvents, maybe you can separates like this (doubt it tho').

Packed fractionating column is what i think will do the job, but then again i have not checked the bp of the two hydrocarbons!

Totally doable.

Pentane will come over at 36.1deg C, Hexane will come over at 69deg C. You won't need a vigreux column because the BP difference between both of them are more than 20deg C. But you probably will want to carefully re-distill your product(s). Simple distillation *should* do it.

Another way would be to have a Two Way Fractional Distillation setup. This will require two condensers, two distillation adapters (or just a vigreux column), two 90deg vacuum adapters, and two collection flasks.

The bottom fraction will be your hexane(s),

The top fraction will be your pentane(s).

Redistill each after collecting.

Distilling gasoline is even cooler. You need a 4-Way fractional distillation setup to do it the coolest way:

The bottom fraction (1st fraction) will be your Octane, the 2nd fraction will be your Heptane, the 3rd fraction will be your hexane, and the 4th (top) fraction will be your pentane. Redistill each separately after you are done.

Remember that if you do distill gasoline, the Octane comes at about 152deg C, and Heptane comes at 98.4deg C.

Well then im going to go ahead and see how it goes. What is the general consensus on using the distillate for extractions that are to be ingested? (after clean evap test) Is it safe?

I will get some pics posted tomorrow.

Well then im going to go ahead and see how it goes. What is the general consensus on using the distillate for extractions that are to be ingested? (after clean evap test) Is it safe?

I will get some pics posted tomorrow.

If you're using them as a solvent, then the substance to be taken internally should pose no problem. Think about it - methylene chloride is a more than common solvent for extractions, and is used on substances to be taken internally.

Just be sure to wash whatever the resultant product is with a non-carcinogenic chemical that the product is NOT soluble in, that way you can wash off your carcinogenic junk (like hydrocarbons, I guess).

If you're just going to be using this to acquire a clean grade of naphtha based solvent, is there actually a necessity to separate them into chain length fractions? Instead, you could surely just distill at a certain temperature, say 100, and what's received will be a clean and relatively fast evaporating grade of (hopefully) alkanes.

I'd be careful though, often naphtha has the shorter chain, more volatile, more bloody useful, fractions removed, becuase they're worth more for various other uses than for filling your zippo or whatever. I once heated swan lighter fluid to at least 140 degrees and nothing boiled.

Thanks for the advice, my main concern is that this sunnyside naphtha evaps leaving some poo behind. Distillation @69C should help me out with that. The reason i dont want to go above that temp is because i've read that naphthas can contain other ?aromatics? (which are not naphthalenes? ) that are also volatile, but idk what if they can react with whateve is being extracted to form nonvolatile and toxic compounds that will reside in the end product? im probably overthinking this but i would hate to think that i poisoned myself in mids of an..you know.. experience...

Thanks for the advice, my main concern is that this sunnyside naphtha evaps leaving some poo behind. Distillation @69C should help me out with that. The reason i dont want to go above that temp is because i've read that naphthas can contain other ?aromatics? (which are not naphthalenes? ) that are also volatile, but idk what if they can react with whateve is being extracted to form nonvolatile and toxic compounds that will reside in the end product? im probably overthinking this but i would hate to think that i poisoned myself in mids of an..you know.. experience...

I think you're overthinking it. The distillate(s) will all be solvents advantageous in their own way.

The naptha leaving gunk behind - the gunk would (obviously) be soluble in sunnyside naphtha; so wash your flask out with sunnyside naphtha to clean out the crap.

Also, would there be a reason to collect the vapor through bubbling it in water and collecting the top layer? im afraid that the liebig i got will not suffice to condense ALL of the vapor by itself, and im too lazy to carry all this shit outside.
What do you guys think about bubblin it?

Also, would there be a reason to collect the vapor through bubbling it in water and collecting the top layer? im afraid that the liebig i got will not suffice to condense ALL of the vapor by itself, and im too lazy to carry all this shit outside.
What do you guys think about bubblin it?

Why do you think your liebig isn't going to condense the vapor? It's not like you're going to get a pressurized jet of condensed liquid flowing out. . . I've never had a problem distilling anything. Distillations are generally so slow that there would be no reason why vapor would not condense. And if they don't condense, it would be because they aren't light enough to get to the condenser in the first place, thus falling back down into the distillation flask.

Why bubble it through water, really? I mean, you're just going to get a water-contaminated solvent in the end, thus having to go through more pain. Ultimately you would have to re-distill that in the end to rid it of all water.. That is, unless you chemically dried it, but that's not 100% in my opinion.

Just distill it. It will work.

Well its not miscible in water so it would float on top so why would i need to redistill?

Also, could i just drop the naphtha into 70C heated water inside my distil flask?

So i used just naphtha without any water in the distillation flask... ice cold water recirc in condenser, collection flask in ice bath, 1st hour at 70C second hour at 92C and still not a single drop of distillate, no visible condensation of naphtha on the inside of any glassware, WTF ?!?! anyone here actually tried it with success ?

Well its not miscible in water so it would float on top so why would i need to redistill?

Also, could i just drop the naphtha into 70C heated water inside my distil flask?

When I think 100% waterless, I mean on the very-very small level, as well. Distillation, IMHO, is the best way to get any sort of true waterless condition, followed by drying.

Of course it's not miscible, or even soluble in water. But there's still water there, IMHO.

The lower degree's of the naphtha will lower the degrees of your 70C water due to temperature variance + dilution of two temperatures, therefor you will have to heat, even still.

Thanks for the advice, i got more questions though.

So after 3 hrs of nearly 100c i got equiv to 3 drops of distillate...

turn up the temp or give it more time?

I put a drop on a piece of paper and it evaporated in room temp in <3minutes, while the drop of undistilled naphtha is still there after ~8mins so far. At least im getting somewhere..

Thanks for the advice, i got more questions though.

So after 3 hrs of nearly 100c i got equiv to 3 drops of distillate...

turn up the temp or give it more time?

I put a drop on a piece of paper and it evaporated in room temp in <3minutes, while the drop of undistilled naphtha is still there after ~8mins so far. At least im getting somewhere..

http://www.sunnysidecorp.com/pdf/msds800.pdf

The naphtha does contain hydrocarbons, but where does it say pentane & hexane? The MSDS says light aniphatic naphtha. I don't know if this would necessarily mean, though, that it contains pentane and hexane; though it would make sense I guess.

That stuff that came over at 100C, it might be miniscule amounts of water that was picked up from the humidity in the atmosphere.

The Naphtha that you have will distill at whatever range the MSDS says, probably.

Distill gasoline. It seems a lot more worth it.

http://www.sunnysidecorp.com/pdf/msds800.pdf

Thanks!!


The naphtha does contain hydrocarbons, but where does it say pentane & hexane? The MSDS says light aniphatic naphtha. I don't know if this would necessarily mean, though, that it contains pentane and hexane; though it would make sense I guess.

My thoughts exacly.For some reason i thought Naphta=pentane+hexane+heptane or something like that. Well i guess VB was right when he said:

I'd be careful though, often naphtha has the shorter chain, more volatile, more bloody useful, fractions removed, becuase they're worth more for various other uses than for filling your zippo or whatever. I once heated swan lighter fluid to at least 140 degrees and nothing boiled.
That makes sense. Now im sure there is no pent/hex in significant quantity in my naphtha if nothing is coming over at 70C :(

That stuff that came over at 100C, it might be miniscule amounts of water that was picked up from the humidity in the atmosphere.

Definitely not. it probably wasn't pentane or hexane but it might've been heptane because like i said:

I put a drop on a piece of paper and it evaporated in room temp in <3minutes, while the drop of undistilled naphtha is still there after ~8mins so far. At least im getting somewhere..
AND it had a distinct smell.


The Naphtha that you have will distill at whatever range the MSDS says, probably.

It sure will. MSDS says 235-286F and when i hit bit over 110C it started simmering.

Distill gasoline. It seems a lot more worth it.
well, gasoline contains at best 3% hexane and 10% pentane. I was hoping that naphtha would be bit better than gasoline, but i guess it depends on what kind you get... and I got shafted by sunnyside corp :(
Besides, gasoline seems so... carciogenic and flammable :D i know i know it just seems to me that gasoline has so much different volatile shit in it, that god knows wtf might distil over even in lower temps..
(damn bastards diluting my gas!)

Thanks!!


My thoughts exacly.For some reason i thought Naphta=pentane+hexane+heptane or something like that. Well i guess VB was right when he said:

That makes sense. Now im sure there is no pent/hex in significant quantity in my naphtha if nothing is coming over at 70C :(

Makes sense to me.


Definitely not. it probably wasn't pentane or hexane but it might've been heptane because like i said:

AND it had a distinct smell.

I missed that. It very well could have been heptane.

It sure will. MSDS says 235-286F and when i hit bit over 110C it started simmering.

There ya go.

well, gasoline contains at best 3% hexane and 10% pentane.

lol, well that's not so bad considering the sunnyside naphtha has an estimated 0% . . .?

I was hoping that naphtha would be bit better than gasoline, but i guess it depends on what kind you get... and I got shafted by sunnyside corp :(
Besides, gasoline seems so... carciogenic and flammable :D i know i know it just seems to me that gasoline has so much different volatile shit in it, that god knows wtf might distil over even in lower temps..
(damn bastards diluting my gas!)

Yeah, be careful with gasoline. But it would still be kindof nifty.

Glad it's all figured out :) Hope I helped.

Brand in question: Sunnyside VM&P Naphtha

Dunno it.

I want to isolate some pentane and hexane from the naphtha i got

Last "naptha" I grabbed was a pretty clean mix of isoheptane 'n the napthelene ring. You, otoh, might get pentane 'n hexane. Or, it might be some other crap.

The general idea of "isolating mid-bp np through distillation" is fairly doable.

Is it possible for me to do that without vigreux? can i use one of the other condensers i do have?

1. Attach lightbulb to ice-bathed test tube.

2. Instal thermometer.

3. ???

4. win.

Or, you could, like, use... equipment. If that is what would work for you.

What is the general consensus on using the distillate for extractions that are to be ingested?

If you do it right, you do not even need to distill. If you water-wash the crap out of it, nothing in it will dissolve in water, no matter how fucked-up it is. Tautology.

Distilled 'n water-washed is a lot better. You could even, like, use an ice-filled bong as a condenser.

Don't use your friend's favorite bong. They'll never really forgive you for that strange flavor.

where u getting the temp readings from? does not sound like your taking it correctly. Is this the 1st time u distilled ?

Makes sense to me.
lol, well that's not so bad considering the sunnyside naphtha has an estimated 0% . . .?

Yeah, be careful with gasoline. But it would still be kindof nifty.

Glad it's all figured out :) Hope I helped.

Indeed :) Thanks for that msds, without it i would still be sittin there @<90C wondering why it isnt boiling.

where u getting the temp readings from? does not sound like your taking it correctly. Is this the 1st time u distilled ?

Nah we already estabilished that my target temp was too low anyways and when i hit ~110C it boiled a bit, and 112C=235F which is what the msds said it would boil at.

I took the temp in the first 5mm from the surface and also by the sidearm, which was irrelevant anyways.

And its not my first time distilling, unless you meant for these type of hydrocarbons then yea, ive never attempted it before.


Last "naptha" I grabbed was a pretty clean mix of isoheptane 'n the napthelene ring. You, otoh, might get pentane 'n hexane. Or, it might be some other crap.

that pretty much summarizes the thread. Along with: sunnyside naphtha has no pentane and/or hexane. It does however contain toxic impurities that do not evaporate at any temp.


Distilled 'n water-washed is a lot better. You could even, like, use an ice-filled bong as a condenser.

Don't use your friend's favorite bong. They'll never really forgive you for that strange flavor.
Lulz, my case might be a bit different - lab glassware i get is almost free, while all my friends own $400+ Roor bongs and treat them like their firstborn.

I came across some of your other threads in LT, and i noticed that you can get pretty creative with makeshift labware, it would be nice to see a thread by you on DIY labware, (I did build a hotplate/coldplate magnetic stirrer, and a vac aspirator so i can contribute too :) )

You know that you can buy hexane with no problem right?

Also as gigster said is this your first time distilling? Did you correctly place the thermometer in the three way?
If not sure refer to Vogel Lab manual, has all you want in there! Not trying to make you look stupid but most of the time it is small thing like these which can mess things up!