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chemrox
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[*] posted on 18-2-2007 at 21:56
analytical machinery


As a student, like most students of the day, I had GC, IR and NMR available at almost all times. I have an old two column GC that can be resurrected. I want to read up on detectors and would appreciate help with the refs. As a next device, what do you think? GC with the right detector will tell me how pure. IR will tell me about functiuonal groups knowing mass would be really nice but for now I have to get there through colligative properties .... sometimes used machines are fairly cheap b ut not so cheap I can go and buy whatever I like at the same time. If you could get and IR and an NMR for about the same price and you could afford one, which? Why?
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Ozone
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[*] posted on 18-2-2007 at 22:07


The initial cost is not the question. The question is what does upkeep cost? In terms of overall use The best deal you will get is a good old scanning UV-VIS spectrophotometer (crappy characterization, but used for so many other things that you be glad to have it). Following this, a simple HPLC with a UV-VIS detector (which can be hacked off of auction sites for @$500US (GC is nice, but you need a constant supply of high quality gas a,dn expensive scrubbers). NMR is the best thing since cheese--but, it's expensive both to purchase and keep running (liquid N2 or you magnet quenches--and is probably very expensively dead). So, for the home lab I would recommend the IR (the only thing that ever usually dies is the globar), but, buy a decent FTIR instrument.

Cheers,

O3




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[*] posted on 18-2-2007 at 22:07


Quote:
Originally posted by chemrox
If you could get and IR and an NMR for about the same price and you could afford one, which? Why?


Assuming I already had a GC (which would be my first choice), I'd definitely go for the NMR. It gives you a lot more info to interpret to figure out your structure. IR spectra, if you don't have a library to compare to anyway, don't always give much useful information. Some, but not as much as NMR.

Personally, I think having an NMR in my Mad Scientist Lair would just be too cool. :cool:

EDIT: I just read Ozone's post, and I'm pretty sure he has a lot more practical advice than me. Do you really have to keep the magnets cold 100% of the time? That would really be a problem indeed.


[Edited on 19-2-2007 by pantone159]
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Ozone
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[*] posted on 18-2-2007 at 22:36


Well, services for dealing with magnet quenches are available for ~$18,000US a pop:

http://www.mrr.com/service/quench.shtml

They do look cool, don't they? Oh, and high field magnets are very large and heavy. The higher the MHz, the bigger the magnet. Our new one was delivered and moved in with a crane.

Cheers,

O3

[edit] the final cooling is with He (l), N2 (l) is used to pre-cool the magnets prior to bringing them up to field. The older, lower field instruments did use N2 (l), I think for primary cooling. He is much more expensive and may not be available in some countries without enormous shipping costs.

[Edited on 19-2-2007 by Ozone]




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[*] posted on 18-2-2007 at 22:59


Are there actually any NMR machines that get away with using high temperature superconductors and liquid nitrogen? I thought they all used niobium alloys at liquid helium temperatures -- and helium's a lot more expensive, and has much lower cooling capacity to boot. I seem to recall seeing plans for a (low frequency) DIY NMR machine that didn't use superconductors at all somewhere.



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[*] posted on 18-2-2007 at 23:22


Quote:
Originally posted by Polverone
Are there actually any NMR machines that get away with using high temperature superconductors and liquid nitrogen? I thought they all used niobium alloys at liquid helium temperatures -- and helium's a lot more expensive, and has much lower cooling capacity to boot. I seem to recall seeing plans for a (low frequency) DIY NMR machine that didn't use superconductors at all somewhere.


You wouldn't happen to know where to find these plans? It seems like an interesting, and challenging project for an amateur scientist. Plus who wouldn't want to proudly display there own home built NMR system. Now that's serious bragging rights!




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[*] posted on 19-2-2007 at 02:42


I have a Sequoia Turner 340 UV-VIS, a large pile of Waters HPLC analytical (mostly Mod 600) and preparative (Mod 4000) sets (controllers and FHUs) and detectors two 486 and four 490 and a couple older PDAs 990, 991, and 994. The 990/991 are good for nothing as I don't have the dedicated PCs and interfaces that ran them though I do have the software. Never mind, I paid little for them.

So my shopping list, desultorily, is:

FTIR not too expensive to get into

NMR: Long range project. I am told you can get a second hand PNMR for about $25,000.

GC. Lots of 5890s around since Agilent dropped all support. They run $1000-$2600 without frills (autoinjector etc.) or up to double that with. Typically they will come with one or two FIDs, sometimes a TCD and a FID. Skip ones with radioactive detectors as you will have regulatory problems. Most desirable are the 5890 Series II+ which have advanced circuitry and better upgrade paths. You probably will want split/splitless injector(s).

Two things to hassle over with GCs: you will need a decent chromatography manager software package and unless you are lucky and get a machine with one installed, a HPIB (GPIB) card, that is an IEEE-488 interface card. Forget Agilent's software as they will rape you. But the most common third party GC software is a piece of shit. There are alternatives but you can expect to pay as much for the software as you do for the instrument.

Another is carrier gas. Americans use H2, Europeans prefer He, you can avoid having a big old tank of either around by investing in a H2 generator to feed your hungry lil ole GC that way. Again expect to spend as much as you did for the instrument.

At that point you are up to $7K-10K

And that is why I went with HPLC.

My ex partner does GC-MS and loves it but, I never got into mass spec. While I never say never I probably have enough on my plate for the balance of my lifetime, lord willing and the creek don't rise.
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[*] posted on 19-2-2007 at 08:01


@Sauron: That sounds pretty much like my rig. The ST 340's are robust and programmable (a good, relatively inexpensive choice).

I want a scanning spec, though (I have a Hach DR 2000 with data collection via chart-out to ADC with recording using Peaknet v5), A waters 510 pump, ABI absorbance detector (I have 2 differential refractive index detectors, a Waters and an Alltech) with a variety of column phases and sizes; my biggest HPLC (rather than using the pump on an LPC glass column) column is an original Dupont zorbax CN-Pr 250mm X 44mm (ID).

The 5890 series II are better GCs than the 6890, but they don't have automated flow control (which makes the 6890 win the bet). If you get one, make sure to also acquire a digital flow meter (if youve ever used a bubble flow meter, you know why!). Also keep in mind that GPIB (they called them HPIB boards) were ~$1000US *when they were supported*.

It's obscenely expensive, but Chemstation is, by far, my favorite (and most intuitive) chromatography interface. Peaksimple is crap. Peaknet (Dionex) 5 and 5.02 is good, intuitive, flexible, and can be had if you ask nicely--but--for you will need a Dionex ACI (the most flexible ADC w/ttl support I know of) or a Dionex UI-20 (straight ADC/ttl to TCP-IP or BNC) to interface it.

We use He most of the time for GC carrier gas, H2 occasionally or maybe P5 with an ECD. I was under the impression that in most places besides the US, He was prohibitively expensive (as you need 2 things for minable He, old U deposits and geology suitable for pocket capture)? I know, for example, that in South Africa they tend to adapt plumbing, mass flow, and method development around N2 carrier (once I found this out, it was obvious why my chromatograms looked so different:o).

FTIR is definitely doable, and to NMR, godspeed. I'm trying to find out this rt NMR that Polverone seems to remember. It would have to very low field (even 50MHz were cryo), but might be fun to construct nonetheless. Following this an ESR seems doable...

Cheers,

O3

For fun, a picture of Florida State's new 900 MHz, 110mm ultra wide bore, 21.1T SS NMR! Keep in mind how large the Dewar to the lower left actually is:D.


[Edited on 19-2-2007 by Ozone]

[Edited on 19-2-2007 by Ozone]

FSUs 900MHz 110mm 21.1T NMR.jpg - 20kB




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[*] posted on 19-2-2007 at 09:28


The 5890 Series II+ had AFC which is the "advanced circuitry" I referred to in earlier post, the Series II didn't but could be upgraded to it, the earlier versions could not be upgraded.

It's going to take me years to get the HPLC stuff all plumbed and settled in. Another reason I went with Waters HPLC vs HP GC: All the Waters stuff is 110/220 V 50/60 Hz. All you need to do is change out the fuses (sometimes internally too) and away you go. A 5890 is 110 V, they made 220V models but I have never seen one on used market. So a major hassle to use one here, I can step down the local voltage but still have to deal with frequency difference. An inverter will do the trick but that's still more $$$.

An NMR is pretty much just a dream.

Yeah HPIB mean Hewlett Packard Interface Board, but what the hell - they invented them so why not? GP just means General Purpose.

The Waters software (now yesterday's falvor since they switched to Empower) is Millenium32, I use v3.2 w/PDA option under Win98. It works.

The lousy 3rd party GC/LC software is Peak Simple which will run you $1500+ but itn't worth it. I will double check on the superior alternative, it is out of Czech Republic. It runs just a little more than Peak Simple.
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[*] posted on 19-2-2007 at 12:42


Just for the record, the first NMR I used had a permanent magnet (30MHz IIRC). The only problem with NMR is the photons are too low energy so it's a bit of a pig trying to get decent sensitivity. On the other hand if what you are trying to do is characterise a pure product they are great.
By an odd coincidence I use the same HPLC software as Sauron, but I'm using it at work. We really need to upgrade our LC kit.
The toy I would personally like to have is an FTIR microscope. Is there anyone out there with much more money than sense?
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[*] posted on 19-2-2007 at 13:18


Not me! The nearest FTIR uscope I can get to is at CAMD. Obviously, the synchrotron facility is not worried overmuch about instrument costs.

But I agree, the FTIR 'scope is about as bad-ass as you get (have not played with a Raman yet, though).

Awesome photos too,

O3




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[*] posted on 19-2-2007 at 17:59


Quote:
I seem to recall seeing plans for a (low frequency) DIY NMR machine that didn't use superconductors at all somewhere.


This might be the page you saw:

http://www.geocities.com/CapeCanaveral/2404/

The kind people at Exstrom will provide plans upon request:

http://www.exstrom.com/magnum.html

An online source for other NMR equipment:

http://www.sdsnmr.com/larmor.htm

:D

From the SA article

In the apparatus designed at the Aero Medical Laboratory the magnetic bias­ing field is supplied by a Type 220A 150 surplus magnetron magnet. The pole faces of the magnet were replaced by soft iron disks 3 1/2 inches in diameter and 7/8 inch thick to provide a field over a large area. For maximum response all protons must precess at the same rate, which means that all must be acted upon uniformly by the modulated biasing field. The intensity of the field will vary with the distance between the pole faces. Hence these must be made par­allel and free from surface irregularities. Surplus magnets from magnetrons of the radial-cathode type usually bear a small white dot on the base which gives an approximate figure in gauss for the field strength that may be expected in the air gap. The magnet used in the instrument constructed at the Aero :Medical Labora­tory is rated at 1,450 gauss. It was modulated by a coil consisting of 20 turns of No. 30 cotton-covered magnet wire wound on a Bakelite tube 1 5/8 inches in outside diameter and 7/8 inch long. Ten turns of the coil are wound at one end of the tube and 10 turns are wound in the same direction at the other end. A hole 5/8 inch in diameter is cut in the center of the coil form to admit the test tube. A second hole 3/8 inch in diameter is made at right angles to the first to admit a length of coaxial cable for linking the oscillator coil to the source of high-frequency current. The modulating coil is energized by the transformer which supplies the tube heaters, and it sweeps the strength of the biasing field 50 gauss above and below its mean value.
The test tube is 12 millimeters in di­ameter and 75 millimeters long. A two ­layer coil of No. 22 enameled magnet wire, consisting of 16 turns per layer, is wound on the straight portion of the tube as close as possible to the closed end. The tube and coil are mounted vertically in the Bakelite form on which the modulating coil is wound.
The circuit construction is conven­tional. The oscillator is designed around a 6AK5 pentode tube. When used with an oscilloscope of high sensitivity, out­put from the oscillator may be taken at the junction between the 22,000-ohm resistor and the 200,000-ohm resistor in the plate circuit. With 'scopes of lower sensitivity, such as the Heathkit Model 0-10, a single-stage amplifier using a 6AU6 pentode is added as shown in the circuit diagram. A variable capacitor, such as the Hammarlund Type MG 140-MI, is used for adjusting the fre­quency of the oscillator. These compo­nents are assembled on an aluminum chassis three inches high, five inches wide and six inches long. Input and out­put connections are made through RC 58/U coaxial cable equipped with UC 290/U and UG 88/U terminals. Power may be taken from any supply capable of delivering 100 milliamperes of direct current at 150 volts to the tube heaters and 60-cycle alternating current at 6.3 volts to the modulating coil.

The test solution is prepared by dis­solving .4 gram of ferric nitrate in 100 cubic centimeters of distilled water. Two cubic centimeters of this solution are added to the test tube and placed in the biasing field. Power is applied. After the horizontal-sweep circuit of the oscillo­scope has been made synchronous with the 60-cycle modulating voltage, a pat­tern should appear on the screen. The pattern may resemble a horizontal figure eight, as shown at left in the illustration. This indicates that the frequency of the oscillator coil lies outside the lim­its within which the particles are pre­cessing and that resonance is not estab­lished. To search for resonance, set the oscillator capacitor for minimum fre­quency (the plates of the capacitor meshed fully) and adjust the intensity (feedback) control to the point where the oscillator is on the verge of going out of operation. Then increase the fre­quency slowly while observing the scope. It may be necessary to trim the feedback control occasionally to maintain the marginal oscillating condition. The procedure can be simplified with the aid of a short-wave radio receiver. If the receiver is equipped for continuous­ wave-reception, the oscillator signal will be heard as a shrill whistle. If not, it will make a rushing sound, perhaps accom­panied by a 60-cycle hum. The receiver is particularly useful in checking the point at which the oscillator goes out of operation when adjusting the feedback control. If the receiver is calibrated, it may be used to calibrate the oscillator. If not, the receiver can be calibrated easily by tuning in on the time signal of Station WWV.
When resonance is established, the display will resemble the center figure. Usually two peaks appear which are joined at the bottom by loops. This indicates a displacement (phase differ­ence) in the time at which signal arrives, at the vertical and horizontal plate of the 'scope. The Heathkit Model 'scope is equipped with a line sweep switch and a phase control for manipulating the display. When these are properly adjusted, the peaks coincide, shown in the figure at right.
What does the display mean? The height of the figure is proportional to the number of protons resonating with the oscillator; the width of the figure, to the range through which the particles precess. Accordingly if all of the particles were precessing at precisely the same rate and all flipped over precisely in resonance with the oscillator, the pattern would resemble an inverted T. The spectrometer could then be said to have perfect resolution. Evidently in the instrument all the particles do not precess at the same frequency. Part of the explanation lies in the interaction of magnetic forces within the test sample, The fields of neighboring protons merge in such a way that some particles are partially shielded from the influence of the outside field. But in this instrument the breadth of the peaks is large, explained by cross-sectional variations in the strength of the biasing field. Particles in regions of high-field intensity precess at higher rates than those in regions where the field is relatively weak. These differences are preserved when the field is modulated. Some particles are swept into resonance with the oscillator earlier or later than others, and the displayed peak is broadened accordingly. The width of the peak illustrated is 26 gauss, which means a difference of 85,000 revolutions per second in the of precession of the slowest and fastest particles.
With an instrument of high resolution many substances show fine multiple peaks. This is due to the complex magnetic interaction between systems of particles and the consequent shielding of ­the biasing field. Many substances are not sensitive to an external magnetic field because the magnetism of the spinning particles cancels out. But those substances that do respond can be identified by the characteristic pattern that shows up on the 'scope. The resolution of the apparatus described here is high enough for fine spectroscopic work As indicated earlier, it is intended to serve as a simple demonstration of the magnetic-resonance effect.
Modifications to adapt the apparatus for limited applications would include the provision of larger pole faces on the magnetron magnet to provide a more uniform biasing field. In contrast the 20-gauss peak-width displayed by the apparatus, the best instruments made. today resolve to a few ten thousands of a gauss; this means that irregularities in the biasing field must be kept below this figure. High resolution also requires precise and calibrated control of the intensity, frequency and amplitude of the biasing field. in this demonstration the. high sweep-rate of 60 cycles per second,: is made possible by limiting the experiment to a test solution of ferric nitrate. Few substances are so responsive.


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[*] posted on 19-2-2007 at 19:19


Holy shitballs, Leu!

That actually looks doable. No doubt the bulk of the cost lies in the power supplies and DAQ board. I think I'll try to contact them for some schematics or equivalence RE. the amps.

And:

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

Economical 60/90MHz FTNMR Instruments
Anasazi Instruments, Inc. provides complete FT-NMR systems and CW-NMR console upgrades for educational and industrial applications. Using an existing 60 or 90MHz permanent magnet (Varian EM360 or EM390), Anasazi provides all the necessary components to perform most modern measurements.

Complete NMR systems use refurbished EM360 magnets. These systems are ideal for sites which cannot support a superconducting magnet because of budget or availability of cryogens.

The Eft spectrometer can be operated by personnel with little or no FT-NMR experience. All instrument functions are computer controlled including magnet shimming.

The Eft spectrometer is an inexpensive, easy to use and robust FT-NMR spectrometer that obtains H1 spectra in less than three minutes and C13 spectra in less than ten minutes. Currently the Eft is available in three configurations: H1, C13/H1, and Wideband/H1 which covers the ranges from H1 to F19 on the high frequency channel and P31 to Si29 on the low frequency channel.

The Eft spectrometer is covered by a five-year warranty and exceptional service.

For more information on Eft NMR spectrometers please contact:

Anasazi Instruments, Inc.
4101 Cashard Ave., #103
Indianapolis, IN 46203
Phone: 866 494-9369 toll free
Email: sales@aiinmr.com
Web: www.aiinmr.com

I emailed asking for a quote on their HETCOR capable model. I'll let you all know what happens, viz. how much a 50MHz NMR goes for these days (heck, if it's reasonable I'm thinking about trying to get one for work that the students can use).

Cool!

O3


[Edited on 20-2-2007 by Ozone]




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[*] posted on 19-2-2007 at 21:08


Hmm little more than a regenerative radio, huh? That is pretty easy.

"Power may be taken from any supply capable of delivering 100 milliamperes of direct current at 150 volts to the tube heaters and 60-cycle alternating current at 6.3 volts to the modulating coil."

Heh....heh....um....yeah, you'll need a few orders of magnitude more than 100mA to run the heaters at 150V! Fortunately, transistor regenerative recievers are also easy to build (though you only get that mystique when you use tubes ;) ).

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[*] posted on 20-2-2007 at 19:05


@O3, I for one will be most interested to hear how they quote for their baseline PNMR setup w/magnet.
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[*] posted on 20-2-2007 at 19:21


Righto!

They got back to me almost immediately! The cost for a HETCOR capable instrument with computer, software and everything (installation, training, etc.) was $74,000; this is about the cost of a GC/MS with an autosampler. I know it sounds crazy, but that's pretty cheap (and they have *free* support with a 5 year warranty).

The best part: Permanent magnets. 50-90MHz (which, face it, is good enough for normal everyday structure elucidation of "small" molecules) without He or N2 (l); granted, the 90MHz is *very heavy*, but I think that delivery is included.

I think that this is the ceapest, easiest to keep-up, and comparably functional instrument I have ever seen for the money (hey, Chemistry *is* and expensive hobby:D).

Cheers,

O3

I'd expect the straight 1H rig to be *significantly* cheaper.

[Edited on 21-2-2007 by Ozone]

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[*] posted on 20-2-2007 at 21:27


Still, that's out of reach of most home users :)

My Mad Scientist vision is an NMR, that politely sits dormant when needed, but when the magnets are immersed in vats of LN2, just picked up from a welding supplier or something, condensation fog billowing, it all cools down to high-temp superconducting, and the low-budget home-brew NMR is ready to go.

Maybe someday.
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[*] posted on 20-2-2007 at 21:33


That is one heavy magnet on the 90 MHz version. Is that the major cost of a permanent-magnet NMR? I imagine that there's quite a markup on instruments like these because they're produced on a limited scale, but even if you were making a million a year of them, I doubt you can really make a "cheap" 2200 pound magnet.

I could imagine maybe dropping $35,000 on a machine like this -- I'd rather have it than a new car -- but $74,000 is a bit much. That's almost half the cost of a house around here.




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[*] posted on 20-2-2007 at 21:39


That's what I meant by heavy!

I'm pretty sure that the 1H machine will be quite a bit cheaper, maybe in the 35K range. Remember, I requested the HETCOR (COSY, 1H, 13C). I'll see what the 1H costs.

He aint heavy,

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[*] posted on 20-2-2007 at 23:38


That is actually, for what it is, very cheap.

Please do get a quote on the basic version.

I was told to expect a used instrument to run $25K so c.$35K for a new one is not intimidating. It would take me 18-24 months of scrimping and savings to put that together (or longer) but I have done it before.

@Polverone, if I read the original remarks about Anasazi cirrectly, they are using refurbished magnets which would certainly reduce the cost as long as the supply holds out. Also whenever possible they utilize a customer's existing magnet.

@O3 was spot on, these things are priced even at the top end, like a GC/MS or a HPLC/MS.

I am going to point a couple of my Thai analytical-instrument dealer friends at this company just in case they do not have a Thai agent yet. If they already have a dealer that may be bad news for me, as the local dealer likely will mark the thing way up. In a kickback-driven economy it is easy to see why.

[Edited on 21-2-2007 by Sauron]

[Edited on 21-2-2007 by Sauron]
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[*] posted on 21-2-2007 at 06:10


@leu, I believe the article you quoted from was not in SA (Scientific American) but rather in the April 1959 issue of The Amateur Scientist, which is (or maybe was) published by the Society for Amateur Science. Anyway the website with the Amateur Scientist Collection (1920s to 1990s) is indeed sponsored by SA and The Tinker's Toolkit, so that's probably what you meant, and I didn't get it.

However I already spotted at least one VERY interesting article in the January 59 issue which will be subject of its own thread as it definitely deserves the descriptor Mad Science, nothing this mad since Ghostbusters.

Anyway the primitive NMR described is not intended for analytical use at all but merely technology demonstration and was estimated to cost in 1959 $ - $100.

It is however interesting.

Here's the attachment for the PDF of the NMR article.

[Edited on 21-2-2007 by Sauron]

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[*] posted on 21-2-2007 at 08:55


Stong definitely was the father of amatuer science!



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[*] posted on 21-2-2007 at 17:12


@Sauron,

Done. I should get a reply in a day or two.

Cheers,

O3




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[*] posted on 23-2-2007 at 22:09


I've been watching labx and surpluslab for years without seeing a non-FT (grating) IR come up for sale that I can recall.

If one did, I'd be happy to buy one if price was right. Pass the KBr. Nujol anyone?

I have seen a few FT-IR machines for sale.
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leu
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[*] posted on 24-2-2007 at 16:46


If you want a device that's not sold on LabX then perhaps you should look elsewhere since there are many other sources of used equipment :D The fact is that the Amateur Scientist was a column conducted by C L Stong in Scientific American for many years and was very well known to any American, Canadian or other English speaking scientist who read that popular publication :P

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Chemistry is our Covalent Bond
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