Refractometer/Spectrophotometer Use in Cland. Labs

[killerbee888]

Swim's university has a a couple of old, working refractometers and spectrophotometers that they are selling for basically whatever they are offered.  if they don't sell them within a month they will donate them to local high schools.  Swim's question is this.  Can either of these instruments be used for anything in a clandestine lab?  For example, swim was thinking maybe to check the purity of safrole, ketone, or mda/mdma freebase without the use of chromatography, for those people who have 0 experience with any type of chromatography.  swim ain't lookin' for help in chromatography, he just wants to know if these pieces of equipment are of any use.  By the way, the spectrophotometer is the kind that you put a cuvette in, and it gives you a number, NOT the kind that is hooked up to a computer, etc.

[Osmium]

Refractometers are very useful to determine purity and identify compounds. Get one!
I'm not fat just horizontally disproportionate.

[killerbee888]

OK, say I get the thing.  How would swim use it to say, check the purity of swim's ketone?  Would he just get the nD and compare it to whatever 98%+ ketone's nD is?  Can one get a % purity for example from the nD of his ketone?

[Osmium]

> How would swim use it to say, check the purity of swim's
> ketone?  Would he just get the nD and compare it to
> whatever 98%+ ketone's nD is? 

Yes.

> Can one get a % purity for example from the nD of his
> ketone?

Probably not.
There are some rules about how to determine the compositions of binary mixtures from the nD, but I forgot how it works. I did it once, checking the purity of hexane with less than 1% ethylacetate contamination, but I can't remember any details.

As soon as you have more than 2 components this won't work anymore. But you can still check your ketone, compare the index of refraction to literature values or former measurements and decide if it's good enough or if it needs to be redistilled etc.
I'm not fat just horizontally disproportionate.

[hest]

But they are greath for identifying sasafras ect. (how much iso ect.)

[killerbee888]

So what would the nD of pure ketone be?  Couldn't find it in any of my ref books.

[TheBlindGenius]

Looks like nobody knows the nD of MDP2P.  Swim thought maybe killerbee wasn't looking hard enough but after looking everywhere he knows to look, he couldn't find the shit.  Maybe if a bee somewhere has some real 98% ketone (purchased, not home-made) they could get the numbers for everyone?  Hint....Sunlight?

[SPISSHAK]

Major tidbit would be the rf values of safrole, ketone, it's aldehyde, it's gloycol, and it's epoxide, Et. Al.
This would be very useful from a practical standpoint since thin layer chromatography is cheap, and doable for a lot of peop.e with a low budget.
If people were to verify thier observations with this simple (but crude) analytical method a lot could be learned that isn't subjective but in the proximate of real data.
Guess SWIM will have to look in Lange's, or CRC (older editions) for referenced standards.
This analytical procedure, although crude, and imperfect can give a very attainable method of presenting results.

[TheBlindGenius]

Not having anything better to do, and knowing that to his knowledge the nD and specific gravity of MDP2P are not posted on the Hive, swim had some of his Asian friends call some asian chemical companies and ask about their ketone.  He was gonna do a faq kind of like the safrole faq, but he doesn't have time.  The values given here are the range of the different numbers that the 4 different companies gave us.  By the way, the numbers here are for 97-98% ketone.  They said they could have purer ketone if we so requested but that it would be much more expensive.  So swim thinks some certain bees should stop saying their ketone is 99% pure if even the companies don't normally get it that pure.      Here you go

Refractive Index (nD) at 20 deg C: 1.532-1.540
note: apparently the higher nD is purer, according to two of the companies who do purer ketone at the buyer's specification.

Specific gravity at 25 deg C: 1.194-1.201
note: lower end of range corresponds to purer ketone

Distillation temps: at 2mmHg 132 deg C; at 4mmHg 141 deg C

So there you have it.  Swim also has a thin film IR of MDP2P, and also the NMR for anyone that wants them you could pm me and I will email to you.  I don't know how to post it online without losing anonymity.

[SPISSHAK]

Not  everyone has refracrtomenters, rf values are more useful.
Also do these asian companies export thier ketone in large qauntities?
Sounds like some people are sooo lucky!

[TheBlindGenius]

Oh come on now.  A brand-new 1.3300-1.5600 nD refractometer goes for like $1000.  I've seen less accurate ones for less than $300 new.  Swim likes this way because it doesn't require any skills whatsoever.  You just put a drop of the sample on the prism and that's it.  If you have an Abbe refractometer then you just turn some knobs and take the reading.  No chemicals required.  Not everyone knows how to do TLC you know.  I agree it would be good to have rf values for those who do know how to do it.  But I still think swim's post deserves some appreciation.     The only person swim thinks is qualified to give rf values out that would be close to that of lab-grade ketone would be Sunlight. Anyways, about the companies.  The problem is not that they won't export large quantities, it is that they will usually only ship enormous quantities.  They really deal in the metric ton quantities.  Swim is glad he is part of the asian car club though.  When he tried calling himself he got the cold shoulder.  But when these punks call and start talking in chinese it's all friendly talk and yes sir, yes, of course, of course we can give you more information.     Swim should go on a little vacation to China with some of these guys or something.  

[SPISSHAK]

[killerbee888]

Thanks for the figures!  This is really good.  I swear the refractive index was nowhere on the hive before this I searched everything.  I even look up the reference books in library.  Now basically swim can do rxn, use bisulfite, metabisulfite, steam distillation, and/or fractional distillation and then know that basically the closer to 1.540, the better.  Here are nD's of common contaminants of ketone as listed in Sigma-Aldrich catalog.

Isosafrole: 1.5760
Safrole: 1.5370

Isosafrole, for example, the main contaminant after a Wacker, is much higher nD than of ketone, so you could tell by if your nD of sample is to high, then must have too much isosafrole, right?

About importing, probably swim thinks it would be very risky, especially at those huge volumes you say.  Better to make it home-made and check and purify as much as can be dones.