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aga
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[*] posted on 11-4-2014 at 13:37
Home Made Analysis gear


What kind of stuff do the Pros use to analyse chemicals, and Why cannot that equipment be made by home-brewers ?

I have heard of Gas Spectrometry.
I assume that means zapping a specimen material and analysing the spectra of the resultant gas.

What analysis kit is actually useful, and why cannot it be home-made ?
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aga
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[*] posted on 11-4-2014 at 13:41


I saw a TV programme where Australian Border Control had a machine that picked up on any trace of a controlled substance really fast, using just a swab of the suspect container, not touching the actual chemical material itself.

How does that work ?

I would very much like to make one, but for all materials, not just drugs.

E.G. : Is this Benzene ? Put sample in machine ..... Beeep! No. It's water.
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[*] posted on 11-4-2014 at 13:58


Quote: Originally posted by aga  
I saw a TV programme
There is your answer. Most things used to analyze chemicals are way beyond the reach of an amateur, they require special machining to ensure they are precisely cut. Other equipment includes gas chomatographs, spectral analyzers, spectrophotometers, and NMR's(which are about .5 million per).
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aga
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[*] posted on 11-4-2014 at 14:14


Where there is a will, there is a way.

Machining : i was born in Sheffield. Machining to 0.001 mm is done routinely these days.
Etching to near-molecular tolerances is also a modern fact.

Gas chromatograph ? So measure the spectra of a gas. Do-able.

NMR i have no idea what that is.

OK.
That's some very good reasons why Not, so suggestions about 'How To' welcome.

[Edited on 11-4-2014 by aga]
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aga
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[*] posted on 11-4-2014 at 14:18


If the several brains in this forum could actually cause a home-brew Substance Identifier (hopefully quantifier as well) to be Possible, wouldn't every chemist want one ?

I would.
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[*] posted on 11-4-2014 at 14:22


Quote: Originally posted by aga  
If the several brains in this forum could actually cause a home-brew Substance Identifier (hopefully quantifier as well) to be Possible, wouldn't every chemist want one ?

I would.


I want one, I propose we call it a Tricorder. :D
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aga
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[*] posted on 11-4-2014 at 14:28


OK. TriCorder is the project name.

[Edited on 12-4-2014 by aga]
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hyfalcon
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[*] posted on 11-4-2014 at 14:54


These multiple posts are going to get you no where but detritus.
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gdflp
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[*] posted on 11-4-2014 at 15:08


NMR = Nuclear Magnetic Resonance. Have fun making one of those, they are very dangerous, magnetic fields and radiation and such.
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[*] posted on 11-4-2014 at 15:09


Sorry for the multiple posts.

Alcohol and the inherrent excitement about a project to make something good are to blame.

Mainly the alcohol.

[Edited on 12-4-2014 by aga]
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[*] posted on 11-4-2014 at 15:11


Thank you gdlfp for explaining, to some extent, NMR.
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HgDinis25
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[*] posted on 11-4-2014 at 15:24


C'mon aga here is bringing an important topic that hasn't been done yet. So stop saying you can't and let's start brainstorming to get somewhere.
hyfalcon, with all due respect, your post deserves much more to go to detritus. You didn't post neither to help nor to give new ideas, you simply post to warn about a little mistake (doublepost). Everyone here could see that, so if you are the "obvious pointer" guy, go point the obvious somewhere else. Otherwise, quit that attitude and say something interesting.

Now, on topic. I've made some CD spectometers just for fun. You can easily see some spectrum lines. I wonder if, by placing a sample in the spectometer, we could analyse it's spectrum? It seems doable to me. For those who don't know, here is one:
https://www.cs.cmu.edu/~zhuxj/astro/html/spectrometer.html
I prefer this aproach on making it:
http://www.youtube.com/watch?v=D_gT2dl3B5Q
I'm out of time to test it out, but as it is really simple to make someone here could test it?

Density tests using a Pycnometer and a good analytical scale are also pretty acurate determining a sample density. One could then compare it to a density table and look for your compound. Determining the melting or boiling point of a sample also helps do determine the compound and purity.
ChemicalMyst speaks about this in a video of his (right in the end of it):
http://www.youtube.com/watch?v=k7ZDSFEsrGg

Any more ideas to add on the table?
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Chemosynthesis
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[*] posted on 11-4-2014 at 18:14


Most forensic drug testing uses mass spec heavily. I'm most familiar with MALDI TOF. You need different systems for liquid, solid, or gas phase analytes. Flame ionization would probably be simpler than laser for LCMS (maybe), definitely GCMS.
http://en.wikipedia.org/wiki/Mass_spectrometry
http://en.wikipedia.org/wiki/Matrix-assisted_laser_desorptio...

I can't imagine making most analytical instruments because here you need precise timers, magnetic focusing and acceleration, an inert gas flow/vacuum, sensitive ion sensors, possibly a quadrupole. I can't even begin to give it justice. The combination of everything makes it harder than just spraying sample through a purged nichrome wire and hitting a screen.

My favorite analytical technique, and one also used in the drug industry frequently is NMR. NMR uses extremely strong magnetic fields under liquid helium, with an insulating layer of liquid nitrogen. This is expensive, hard to maintain, can lead to very difficult to diagnose issues, and is dangerous if you get a "purge." It requires dedicated space away from all magnetic object, computers, credit cards, and the software to run them tends to be licensed and is designed to run on Solaris/sunOS UNIX on every system I've used (Varian). It is also extremely sensitive, so you need very pure sample, a standard (generally TMS), deuterated solvent, and very fine calibration to compare spin-anisotropies to get Knight and chemical shifts through perturbing the nuclear spin states. It's pretty complicated, I've forgotten a lot about it (except how to read some of the spectra), and I was never considered an expert in the technique. People get paid fulltime to do these kinds of things, including mass spec... and I never was. It's so sensitive (ppb/ppt), there were plenty of times I had to rotovap material repeatedly and high vac overnight to get a clean spectra without extra solvent peaks. Maybe not necessary for home science, or even all publications, but it can be annoying.

HPLC is also complicated. You have special columns, pumps, etc. I think you'd be best off faking this with flash chromatography after TLC, but I could theoretically see someone plumbing this together. Won't be a Waters or Agilent UPLC, but I could see it, maybe.

Now you move into things like IR spec, Raman, and UV-Vis. I could actually see you making these, though I have seen FT-IR for hundreds used, and Raman for a grand. At the very least, you can easily get these in your choice, used for a couple grand any day of the week, so I don't see why you would make one unless for fun.
http://www.sciencemadness.org/talk/viewthread.php?tid=23422
http://www.youtube.com/watch?v=-lVMYa25jtU
doi:10.1021/ed800081t

All in all, though machining is amazing, don't underestimate how electronic a lot of this will be, including calibration and maintenance. I do want to emphasize I am impressed by your machining background. Don't laugh, but I bought a CNC Taig micro mill (the larger one... can PM model numbers), thinking I would learn how to use it, and never found the time or anyone willing to teach me, so I am fascinated. I would love a Sheffield and some experience!

Edit- are you more interested in the fun and accomplishment of building your own, or just the end result? A lot can be done with melting point analysis, rf values in various solvents, and even a density estimation, as well as various chemical characterization techniques for functional group presence.

[Edited on 12-4-2014 by Chemosynthesis]
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[*] posted on 11-4-2014 at 18:48


Some instruments require very complex electronics, complex gases, cold temps, or expensive parts. But if you look through the other parts of this forum, you will see discussions on home made, portable, or smaller NMRs, home made GC and HPLCs, and polarimeters. There are smaller versions of many instruments which could be adapted for home or hobby use. The reality is that if you could build most of these items for cheap and they worked well, someone would be working on it already. But some instruments like CG and MS have been miniaturized recently and are much smaller and less expensive than they were just a few years ago, I would not be surprised if that trend does not continue.

That may be true of analytical tools, but preparative equipment, larger scale instruments used for purification of larger amounts of material, where the purified material is the product, not the analytical information, are still expensive in general, like prep HPLC, flash chromatography instruments (although they have dropped in prices due to being more common now.)

High quality NMR is still expensive, mostly due to the cost of the superconducting magnets used for most higher quality machines, but if anyone can make higher temp superconductors work for NMR magnets, then that could make a huge impact on NMR, as the magnets often cost $100,000's alone, and the electronics (like radio freq. probes and ppm signal amplifiers) are very complex and not trivial to build cheaply, but that also may change also.


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[*] posted on 11-4-2014 at 20:44


If we start to see some hard references and , this is going to stay. I really hope that happens, I've seen "amateurs" and "makers" pull off things pros are hard put to do, and on a shoe string.

If it continues as blue sky, but has educational links to information on instrument design & theory, it's beginnings... Already enough info here to take it past detritus.

Whoo hoo! 30 + years ago, I got to help build an NMR.


[Edited on 12-4-2014 by Bert]




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[*] posted on 12-4-2014 at 00:17


Wonderful !
I knew it was worth waiting for some Enthusiastic Thinkers to turn up.
Thanks for the references - i will follow up each of them.

I suppose to be practical, the machine needs to characterise as much of the substance is is feasible.

Complex electronics and computer software are not an issue for me, neither is a modest degree of cost.

It sounds like NMR will not be an option, due mostly to the Hazards and immense cost.

Currently i'm thinking along the lines of :-
Freezing point
Melting point
Boiling point
Spectral analysis, including visible, IR and UV.
Without knowing what frequencies might be required (will look it up), RF resonance may be useful.
Then there's Excited/Activated state responses, such as spectra after zapping with 30kV, spectra after exposure to the collapse of a large magnetic field etc etc.
Piezo electric effect ? - maybe some substances squeak (in some sense) when exposed to high pressures, or a vacuum.


These all spring to mind because they should be measurable with electronic sensors.
Things like solubility in solvent x, y and z would be much harder to do electronically.


[Edited on 12-4-2014 by aga]
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[*] posted on 12-4-2014 at 00:50


Quote: Originally posted by Chemosynthesis  
I bought a CNC Taig micro mill (the larger one... can PM model numbers), thinking I would learn how to use it, and never found the time or anyone willing to teach me, so I am fascinated. I would love a Sheffield and some experience!


I found this to be excellent, and should help you to get your Milling machine cutting metal :

http://littlemachineshop.com/Info/getting_started.php

A first task would be to mill a straight slot in a piece of aluminium or brass (they're soft, so tolerate mistakes better and are less likely to snap your tooling).
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[*] posted on 12-4-2014 at 01:58


My only problem was the rapidity of his posts. If he has another thought that quick then he could just edit the previous post instead of making post after post. Look at the time stamp on the first posts.

And I'm sorry, the OP lost me with "My ass".

[Edited on 12-4-2014 by hyfalcon]
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[*] posted on 12-4-2014 at 05:23


Quote: Originally posted by hyfalcon  
My only problem was the rapidity of his posts. If he has another thought that quick then he could just edit the previous post instead of making post after post. Look at the time stamp on the first posts.

And I'm sorry, the OP lost me with "My ass".

[Edited on 12-4-2014 by hyfalcon]


Agree. I got to this late last night from a SPAM report, caused by that repeated posting. Also, "My ass" might JUST be suitable for whimsy, if you smile while you say that, Pardner! Definitely suitable for Hot Electron Death otherwise.

aga:

Please go back and edit/remove your earlier posts, for civility and content? Make it something worth keeping around- you've got 24 hours.

The first time I saw one of these, I have to admit I DID think "TRICORDER! WHOOT!!!"





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2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.

Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).

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[*] posted on 12-4-2014 at 05:26


how about neutron activaction?
depanding on the cross section of your sample you can identify metals (mostly)
How about XRF ?
withe the same equipment used for neutron activation plus a xray tube your in business!!!

http://www.sciencemadness.org/talk/viewthread.php?tid=27963





Http://www.d-radlab.com/
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[*] posted on 12-4-2014 at 10:39


XRF, That's what I was trying to remember and couldn't.

http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?...

[Edited on 12-4-2014 by hyfalcon]
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[*] posted on 12-4-2014 at 10:54


I always did wonder why no one had thought to try make a homebrew IR spec. or UV-VIS setup.

AFAIK the main problems would be obtaining IR/UV sources and sensors which could emit all the different wavelengths and detect them with high degrees of precision and accuracy. After that, it would simply be a case of analysing the output data.

I actually know how most of these machines work inside (and if anyone wants proof of me being a capable analytical chemist, I can now provide it!), the main issue for the homebrewer is obtaining the detectors and emittors of various wavelengths/signals IMO. That and the tight tolerances, etc.

How a UV-VIS works, for example, is a very basic principle. Shine a certain wavelength through a sample, see if any of the light is absorbed. Record how much is passed through compared to how much was emitted on one side. Try this with a bunch of wavelengths of UV light. Different materials absorb at different wavelengths.

A = E.C.L where A is absorptivity, E is the molar absorptivity coefficient, C is the concentration of the material (moles per decimeter cubed) and L is path length of the cell, normally 1 centimeter. That is the basis of that.

An NMR machine would require extremely precise sensors, radio-wave sources, and strong electromagnets, among other kit. I doubt someone will be making one of those anytime soon.

If you want your samples analysed, your best bet IMO is to make friends with a chemistry student at a nearby Uni with a good lab. Most of us have no problem running a few samples out every now and then, and our lecturers often tend to be somewhat supportive of us getting more practice with the techniques.

Perhaps some genius will find a cheap source of IR and UV sensors/emittors capable of the frequency ranges needed with decent accuracy/precision, knock up a bit of software (probably Arduino based) and put up a kickstarter someday...

Edit: as for multiple-stuff-machines, I did once sketch out an "extension" for a HPLC machine that would take the fractions coming out (using a UV detector), do both IR/UV-VIS analysis on them to determine what wavelengths they absorb at (IR is useful for obtaining functional groups and suchlike, UV I have only ever used for concentration data, but it may come in handy), then pass it along to a little collection device that would neatly collect each fraction. A complete pipe-dream device, one I lack the expertise to build, but was fun to come up with. You could then run NMR and MS on the samples to gain more information.

[Edited on 12-4-2014 by packetforger]
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Etaoin Shrdlu
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[*] posted on 12-4-2014 at 11:38


I've never been much for mechanical work, but I have a lot of experience working with spectral data and quite a fair bit of programming knowledge. I recently cobbled together an excel spreadsheet with programming tagged on* to analyze the output of our visible-light spectrophotometer, express how a material appears under different light sources and through different receptors, etcetera, with a high degree of customizability for non-real-world scenarios, and I'm currently building an add-on to see if I can get it to pick up on specific patterns and output likely pigments/dyes contained in a sample, based on their spectral data. I can simplify readings to a "pure" color curve based on the spectrum of the light source, and (theoretically) known absorbance from the container (edit: or based on a reference sample if that's available). I think a lot of this could be adapted to UV/VIS/IR spectrometry, and all of it can be transferred to something standalone if necessary, though I'd have to learn how to get a program to talk to the machine, or have some way of retrieving data through an intermediary. So if anyone does try their hand at this, I'd be interested in offering assistance on the software side of things, however fumbling it may be.

*(Oh I know this would be better served by a separate database and program, but Excel allows me to have both together without fussing with compiling code or compatibility issues. Shhhhh.)

[Edited on 4-12-2014 by Etaoin Shrdlu]
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[*] posted on 12-4-2014 at 12:20


Quote: Originally posted by packetforger  
I actually know how most of these machines work inside (and if anyone wants proof of me being a capable analytical chemist, I can now provide it!),


Invaluable knowledge !
Do you also have access to 'proper' tst gear so that any results could be checked ?

(assuming a TriCorder gets built)

The incredible work done by radagast last year looks like a very promising place to start :-

Quote: Originally posted by radagast  
Amateur chemists need a way to identify and characterize compounds



[Edited on 12-4-2014 by aga]
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[*] posted on 12-4-2014 at 12:24


My apologies hyfalcon.

I did not intend to offend anyone.

Now i have a yardstick as how easily that can happen, i will make an effort to moderate my posting behaviour.

--------------

To avoid annoying anyone further, i am editing this post rather than posting a new one.

I do not feel that i will be able to avoid annoying people, as i do drink, think and post.

As new ideas crop up (in my mind) i find that sending them out as-is for discussion works well, as people react, flame, argue, and contribute.

So, best if i do not post anything further.

Thank you all for your very informative and detailed answers to questions i have asked, and please continue supporting beginners in the future.

Kind regards,

Adrian.

[Edited on 12-4-2014 by aga]
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