-
Members of the previous forum can retrieve their temporary password here, (login and check your PM).
.
- Thread starter Cyan23
- Start date
downwardsfromzero
Boundary condition
Hello and welcome to the Nexus!
It does seem promising on the basis of the information given so far. The composition is basically that of naphtha, and while the term 'hydrocarbons' could be considered a bit vague it seems the qualifiers 'C6' and 'isoalkanes' make up for that.
You would need to check the SDS to be absolutely sure. There should be some kind of website details on the container or perhaps a product reference number along with the exact name and brand of the product which will help you to search for this information. Some cleaning agents may contain detergents and you don't want this. The usage instruction should help clarify on this matter - if it says to rinse with water it may contain some kind of detergent. If not, you can be fairly confident that it should evaporate cleanly as you wouldn't want a stain remover to leave a greasy residue.
If you can share the details of the product here I'm happy to check for you as well. It can be difficult to make sense of this stuff but fortunately I'm well-versed in these kinds of technical details.
The only thing is, stain removers tend to come in very small bottles - or is this one available in slightly larger amounts? 250mL should suffice.
It does seem promising on the basis of the information given so far. The composition is basically that of naphtha, and while the term 'hydrocarbons' could be considered a bit vague it seems the qualifiers 'C6' and 'isoalkanes' make up for that.
You would need to check the SDS to be absolutely sure. There should be some kind of website details on the container or perhaps a product reference number along with the exact name and brand of the product which will help you to search for this information. Some cleaning agents may contain detergents and you don't want this. The usage instruction should help clarify on this matter - if it says to rinse with water it may contain some kind of detergent. If not, you can be fairly confident that it should evaporate cleanly as you wouldn't want a stain remover to leave a greasy residue.
If you can share the details of the product here I'm happy to check for you as well. It can be difficult to make sense of this stuff but fortunately I'm well-versed in these kinds of technical details.
The only thing is, stain removers tend to come in very small bottles - or is this one available in slightly larger amounts? 250mL should suffice.
downwardsfromzero
Boundary condition
That's great. So if there's no mention of any other components such as surfactants, detergents or polyethoxylated whatnot, cationic, anionic, amphoteric or nonionic anywhens, then a clean evaporation test is all you need in order to be reasonably confident that your chosen solvent will work. Just be sure to wipe your evaporation test surface with a small amount of the solvent and a clean paper towel before use as surface contamination from detergent residue or airborne grease can give misleading results.Cyan23 said:
merkin
Rising Star
Hey DF0, I am having a bit of an issue with spice solvent pulls and would like some advice on choice:
100g Powdered MHRB, basic A/B with 3 "boils" (less than 80°C), filtered.
Getting yields of less than 200mg tinted yellow crystally per pull with NPS solvent (Newport Lighter fuel 30% and the other 70% a 50/50 nHexane CP / nHeptane CP mix). After 3 pulls making yield ~0.4%, then switching to Xylene (x2) and FASA pushed total yield (+ accounting for Fumarate weight) to ~1.8%.
So after doing 3x100g with same results I would like to change the initial solvent to try and increase freebase yield.
Choices (ex MSDS listings):
1: C5/C6 nParaffins
Pentane 10-20%, nHexane 40-80%, Heptane 20-30%
BoilPt from 40°C
2: C7/C8 nParaffins
No % given: nHexane, nHeptane, nOctane
BoilPt 68°-128°C
3. Newport Lighter Fluid
"VM&P C Naphtha"
BoilPt from 32°C
4. Zippo Prem Black Tin
Light Hydrotreated Distillate 70%, Hydrotreated Light Naphtha 30%
BoilPt from 32°C
Also avail lab grade "Petroleum Ether" 40-120 in 4 variations: 40-60,60-80,80-100,100-120)
Would any of these (or a combination) produce better yields of freebase?
Would anything with a higher BP ( "C9/C11" ) be desirable?
Thnx
100g Powdered MHRB, basic A/B with 3 "boils" (less than 80°C), filtered.
Getting yields of less than 200mg tinted yellow crystally per pull with NPS solvent (Newport Lighter fuel 30% and the other 70% a 50/50 nHexane CP / nHeptane CP mix). After 3 pulls making yield ~0.4%, then switching to Xylene (x2) and FASA pushed total yield (+ accounting for Fumarate weight) to ~1.8%.
So after doing 3x100g with same results I would like to change the initial solvent to try and increase freebase yield.
Choices (ex MSDS listings):
1: C5/C6 nParaffins
Pentane 10-20%, nHexane 40-80%, Heptane 20-30%
BoilPt from 40°C
2: C7/C8 nParaffins
No % given: nHexane, nHeptane, nOctane
BoilPt 68°-128°C
3. Newport Lighter Fluid
"VM&P C Naphtha"
BoilPt from 32°C
4. Zippo Prem Black Tin
Light Hydrotreated Distillate 70%, Hydrotreated Light Naphtha 30%
BoilPt from 32°C
Also avail lab grade "Petroleum Ether" 40-120 in 4 variations: 40-60,60-80,80-100,100-120)
Would any of these (or a combination) produce better yields of freebase?
Would anything with a higher BP ( "C9/C11" ) be desirable?
Thnx
downwardsfromzero
Boundary condition
Check what your solvent contains here
As I currently understand it, following Loveall, IridiumAndLace, DirtyT, Jees, and whoever-else's efforts in the goo-less extraction experiments it's the lower boiling solvents that seem better for pulling just DMT without the oligomeric goo. This entails following a fairly specific set of extraction steps quite carefully. On the other hand, if you're not too bothered about pulling a bit of goo while maximising your yields, my experience shows me that the heavier solvents are less selective, thus pulling the heavier oligomers.
If you have a lighter solvent and a heavier solvent already, you could do a side by side comparison and contribute to the science going on at the Minimum Polymer thread.
As I currently understand it, following Loveall, IridiumAndLace, DirtyT, Jees, and whoever-else's efforts in the goo-less extraction experiments it's the lower boiling solvents that seem better for pulling just DMT without the oligomeric goo. This entails following a fairly specific set of extraction steps quite carefully. On the other hand, if you're not too bothered about pulling a bit of goo while maximising your yields, my experience shows me that the heavier solvents are less selective, thus pulling the heavier oligomers.
If you have a lighter solvent and a heavier solvent already, you could do a side by side comparison and contribute to the science going on at the Minimum Polymer thread.
merkin
Rising Star
Thanks, unfortunately no product available here appears on that solvent list. I am just relying on the MSDS.
I am not concerned with a bit of goo/yellow chunkies, just with increasing the yield of freebase in the extraction process. It seems that it is all there in the 'soup', but not much is coming through in the solvents. Xylene and FASA are merely a method to ensure all good stuff has been removed, but has now turned into the main feature with over three times the yield amount.
Would nonane, decane and undecane (listed as nParaffins) be considered aliphatic or aromatic? Is it as simple as the -ane or -ene suffix rather than boiling points? I would definitely be aiming for it all to be good for freeze precipitation.
I am not concerned with a bit of goo/yellow chunkies, just with increasing the yield of freebase in the extraction process. It seems that it is all there in the 'soup', but not much is coming through in the solvents. Xylene and FASA are merely a method to ensure all good stuff has been removed, but has now turned into the main feature with over three times the yield amount.
Would nonane, decane and undecane (listed as nParaffins) be considered aliphatic or aromatic? Is it as simple as the -ane or -ene suffix rather than boiling points? I would definitely be aiming for it all to be good for freeze precipitation.
downwardsfromzero
Boundary condition
Those three alkanes (paraffins) you mention are not aromatic in the chemical sense, they are aliphatic hydrocarbons. They should freeze precipitate effectively enough.
It's unfortunate that all these synonyms can make it more than a little confusing for folks who haven't dedicated years of their life to studying chemical etymology
paraffins = alkanes = aliphatic hydrocarbons. These will always have the -ane ending, indicating saturation.And then we have the aromatic hydrocarbons which, in the case of solvents at least, will in all normal circumstances contain a benzene ring but usually will go by their respective trivial names. Most commonly encountered are toluene and xylene (or, more properly, xylenes) but unfortunately the -ene merely indicates unsaturation and is not specific to the aromatic compounds. Use of the alternative German suffix -ol (as in 'benzol', 'toluol', 'xylol') is very much to be discouraged as it gets very misleading.
Systematic naming of the aromatic solvents as their substituted benzene derivatives would make things clearer: toluene = methylbenzene; xylenes = dimethylbenzenes; cumene = isopropylbenzene. Then the various trimethylbenzens have their own individual trivial names depending on where the methyl groups are positioned, as do the tetramethylbenzenes. 1,3,5-trimethylbenzene is known as mesitylene, and hexamethylbenzene is known as mellitene - but what substitution patterns would you think durene, isodurene, hemimellitene, pseudocumene or prehnitene might have?
Ethylbenzene is always simply known as that, but methyl isopropylbenzenes are often known as o-, m-, or p-cymenes. The trivial names are often derived from the plant source where the compounds were first identified, or sometimes the physical appearance of the compound in question. Just in case you were wondering :lol:
Hexamethylbenzene does something super-interesting if oxidised to a dication: one of the carbon atoms pops out of the ring along with its methyl group and sits atop it forming a pentagonal pyramidal molecular ion where this central carbon atom is, extremely unusually, bonded to six other carbon atoms:
Hexamethylbenzene - Wikipedia
This has very little to do with what you are attempting to achieve, but perhaps this extra background information will help you to understand aromatic solvents a bit better.
merkin
Rising Star
It's unfortunate that all these synonyms can make it more than a little confusing for folks who haven't dedicated years of their life to studying chemical etymology
Agreed. Thanks - appreciate the chemical etymology lesson. Is it safe to assume then that despite high boil points of undecane etc (C >7) they will still be ok for freeze precip? I am thinking the higher bp solvents will pull broader spectrum of alkaloids but hopefully not cross into the aromatics like xylene which need the FASA or other method to retrieve spice. I thought the boil point was the determining factor, too high and then you stuck with FASA but now I see that that’s probably not the case here.
:thumb_up:
downwardsfromzero
Boundary condition
All I can say is that medium-heavy aromatic free naphtha (which includes undecane) will freeze precipitate quite acceptably well, but be prepared to clean things up with a mini A/B or maybe recrystallise from a light naphtha in order to eliminate low-volatility hydrocarbon residues.