Author Topic: How to tell what you have  (Read 135 times)

reDEEMed

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How to tell what you have
« on: July 06, 2011, 05:07:30 PM »
How would someone with my level of experience and equipment go about finding out or confirming which compounds they have synthesized? You guys can pretty much gauge my knowledge, not totally clueless, but not very confident yet either. As for equipment I have standard distillation apparatus up to 1000ml, a really bad ass 500mm graham condenser, erlenmeyers up to 1000ml down to 50ml, nice stirplate/hotplate, all kinds of stands and clamps and shit. So, not too much of either thing, but enough to get started. It's just that I listen to Shulgin talk and he talks about they were going after a particular compound and the methyl group was attached to the 4th position when they wanted it to be attached to the 5th and I'm like how in the hell do you know that?!

What are some ways that compounds are verified? Are they all destructive? I'm not afraid to read, but I can't really find something general. I have a hard time finding the docs I want to read because I think I don't search right. For instance, I've spent a lot of time searching for some documentation about the stability of aldoximes. I've read about their formation and everything else I can find, but no hint as to stability.

Those things go hand in had, IMO. Since I suspect that I will often have to figure out myself ways to check what I have and be able to deduce stability from looking at the chemical structure it's self.

Not asking for a spoon feeding, just some advice.
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
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JustDreaming

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Re: How to tell what you have
« Reply #1 on: July 06, 2011, 11:19:14 PM »
TLC/Column chromatography
Melting point tests
UV-VIS spectrophotometry

these are all possible for hobbiests, the more serious and accurate means of analysis require big toys.
This never really happens, but an eye still see's these things. It keeps happening. You just don't see it.

lugh

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Re: How to tell what you have
« Reply #2 on: July 07, 2011, 12:08:40 AM »
Chemists didn't always have modern methods of instrumental analysis, and those techniques that were used in the past are rather effective though comparatively tedious  :P You need to start reading some old textbooks such as:

http://www.erowid.org/archive/rhodium/chemistry/vogel3.html

and some others available from:

http://library.sciencemadness.org/library/index.html

since after some studying your questions will be a lot easier to answer  :-X  The end results from the effort applied  8)
Chemistry is our Covalent Bond

reDEEMed

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Re: How to tell what you have
« Reply #3 on: July 07, 2011, 02:26:22 AM »
That's good advice about the textbook, lugh. I've been pondering that one for some time along with chem as a second language since salat recommended it. I imagine my questions would be easier to answer. I can assure you I'm applying maximum effort, I'm just maxed out. Don't forget that I'm an old guy as it is and I've done horrendous shit to my head over the years. I'm not in need of figuring out what I have at the moment since I know it to be vicodin. It's just one of those things that a newbie thinks about a lot. I'm sure at some point I'll laugh that I asked, I look forward to that lol.

Pretend I know what you're saying for a minute. I wanna live vicariously through the burnt out, middle aged, self taught home chemist that lives in my head.

"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

java

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Re: How to tell what you have
« Reply #4 on: July 07, 2011, 10:39:24 AM »
......find out all its physical properties....i.e. density, boiling point. solubility. appearance, smell, melting poin, PHt....and then do tests for functiona groups, aldehydes or ketones (bisulfite test), amine groups, carboxylic groups, etc.   armed with information of the unknown one can make educated guess of the unknown as a start....java
¡Prefiero morir de pie que vivir siempre arrodillado!.Emiliano ZapataIt is better to die on your feet than to live on your knees!.......

reDEEMed

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Re: How to tell what you have
« Reply #5 on: July 07, 2011, 06:26:35 PM »
Thanks Java, testing for functional groups was a great tidbit from your post. I even found a pretty good pdf. Thanks!
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

Sedit

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Re: How to tell what you have
« Reply #6 on: July 08, 2011, 02:09:33 AM »
Java is correct on all front and this is the normal determinations I use when possible in accordance with what I believe I already have changing the game here or there to suit the reaction.

There is one issue doing it this way. You must get very good at microscale work because if not you will waste everything you have attempting to figure out what you have. Trust me on this and im sure others who know me well enough will tell you I am the master as the destruction of material just to be sure it is what it is.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

Enkidu

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Re: How to tell what you have
« Reply #7 on: July 08, 2011, 02:20:09 AM »
+1 for Microscale reactions

And don't forget the iodoform test for methyl ketones.
« Last Edit: July 08, 2011, 02:22:22 AM by Enkidu »

reDEEMed

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Re: How to tell what you have
« Reply #8 on: July 08, 2011, 02:31:30 AM »
Haha, well then, Sedit, you can expect a pm or two from me when the day comes that I can't find a way to destructively test my unknown compound.

Reading the microscale stuff in Zubrick's book already has me realizing the importance of microscale, especially for someone like me who is just starting out. Attention to detail is not an option in microscale, it's a necessity.

It's gonna take me a while to get to the point that new things instantly make sense. I'm still very much on the basics. I guess I could probably memorize more shit, but I want to understand it. It's the desire to understand that drives me to learn, otherwise I'd just follow one of the many shopping lists and recipes found online for damn near any compound one would want and be done with it.

I been eye ballin' a nice microscale kit for a while. I have a feeling I will have that bitch before it's all over with.
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna