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Analytical Chemistry

The Latest Technology

Well, the latest for 1960, anyway. That’s the Bruker KIS-1 NMR machine there, folks, operating at 25 MHZ, and ready to dim the lights in the whole building when you switch on that electromagnet. Allow about 12 hours of acquisition time to get a decent spectrum.
For those of you outside the field, a 300 MHZ NMR machine is now considered a average workhorse instrument, and should give you a spectrum (with resolution that would have made someone back then faint with joy) in a minute or so of acquisition time. We can do things with modern machines that they wouldn’t have even dreamed of back in 1960, and people are still thinking up new tricks. All hail NMR!

27 comments on “The Latest Technology”

  1. SP says:

    Is that magnet even cooled? I’m a doctor, Jim, not a miracle worker!

  2. retread says:

    You betcha ! It may seem hilarious now, given the use of MRIs in medicine, but back then John Baldeschweiler had to keep water out of whatever he was running, so its protons wouldn’t swamp anything.
    The machines were huge, and my friend Tack Kuntz (probably Irwin to you) was never happier than when he was messing about with a machine big enough to allow him to climb inside.

  3. KJ says:

    No acquisition time Derek; this was surely a continuous wave NMR machine so it just worked its way across the spectrum in real time. Some later CW machines allowed you to do a number of runs of the same spectrum and ‘average’ them but FT did not come in until later (early 1970s?)

  4. katre says:

    Wow, that’s awesome. And I thought the old 60 MHz continuous wave machine we used as undergrads was bad. At least it was only the size of a desk, and only took about 10 minutes to get a decent spectrum (that’s five minutes for the first run, and then five minutes for the second after I realized the plotting pen had run out of ink.)

  5. startup says:

    I not even sure about 300’s, – we have retired our last one a few years ago.

  6. BFS says:

    @4 katre
    When I started at Pfizer in 1983, we had a bank of Varian T-60s. Overall, they served us pretty well, except during summer thunderstorms. Took hours to get them recalibrated. At that time the new 300 mHz was strictly off-limits.

  7. startup says:

    By the way, Derek, have you seen mini-NMR based on Halbach array that was in Angewandte earlier this year?

  8. S says:

    This reminds me of the time when my dad told me about the 60 MHz NMR in the lab. where he did his Ph.D. in India (mind you this was the first and only one of its kind in India in the mid-60’s….he said it like he felt privileged to have it at his beck and call :)). On his recent visit to the States, I did an NMR run for one of my compounds on the Varian 500 and the look on his face was just priceless…..

  9. HelicalZz says:

    Nothing wrong with a good scanning 60 (MHz). It would give you a decent look at the protons and tell you that ‘no, the solvent wasn’t all removed yet’ quick enough.

  10. Nick K says:

    God, that first Bruker looks like a monster! On the other hand, the early Varian 60MHz (introduced in the early 60’s) was quite small and compact. It produced superbly resolved spectra (better in Hz terms than any supercon) in less than 5 minutes. There’s one preserved in the Science Museum in London. I don’t know if it still works, though.

  11. gippgig says:

    This is off topic, but it is about drug development…
    Washington, D.C. is holding the first USA Science & Engineering Festival over the weekend. It includes this exhibit:
    “Can you make a new drug to cure cancer?
    In this exhibit, participants will get to step into the role of a biopharmaceutical researcher and take their great idea through the many challenges and successes of a virtual drug development process. Celgene Corporation”
    I might try this (altho I’m not involved in drug development). Would anyone be interested in a report (I won’t post anything further on this unless someone asks)?

  12. RTW says:

    I use to maintain an HA 100 built by Varian. The electro magnet was about the size of the console in your picture. It was water cooled and used a closed loop heat exchanger (which sprung a leak – thats another story). It was also a CW instrument and I beleive Varians first comercial NMR instrument. Its console was about the size central console shown in this picture and was filled full of Vacuum tubes. It could do Proton and Carbon. This was in the mid to late 70’s I was keeping this thing running. And frequently went through and checked the soder joints and replaced all the vacuum tubes.
    The Electrical Engineering dept, built a feedback locking system and I trhink a transmitter to pump in a pulsed wave form. The receiver’s output was sent across campus via a phone line to the math departments analog computer to “acquire” a FID and do the transformation. The Analog computer would then send the transformed spectra back across the phone lines to plot on the CW ploter.
    The professor I use to do this work for claimed that I could get it tuned better than the spec that it was delivered with. The department also had a Varian T-60 and EM-360. In the early 80’s the department finally got a Varian super con 200 MHz instruent for research. It was a sad day when I started to dismantle that HA 100 though. I certainly have seen a lot technological change over in in NMR Spectroscopy in the last 30+ years.

  13. J says:

    Does “more megahertz” = “better than” ?

  14. Derek Lowe says:

    J, that’s pretty much true. The Mhz frequency is proportional to the strength of the magnet that the machine uses. And the stronger the magnet, the more sensitive the instrument (other things being equal) and the higher the resolution.
    When I was starting grad school in the early 1980s, 90 Mhz instruments were still to be seen, and 200 and 300 Mhz machines were the high end. Now you don’t see so many 200s outside of teaching labs, and 300s are considered run-of-the-mill.
    400 and 500 Mhz machines are all around these days, and you can buy 800 and even 1000 Mhz instruments if you want to spend the serious cash. (They get fiercely more expensive as you go up the scale, since it gets harder to make the magnets, and harder to engineer the electronics on back end).

  15. Jose says:

    900 MHz magnet, even titled “The future beckons!”

  16. barry says:

    When I started grad school in the early 80s, our department still had an XL-100 running. That cost $5000/annum in current and $10,000/annum in cooling water for the power supply (but I could shim it down to 0.18Hz which I’ve never been able to match on a super-con). We also had a 300MHz super-con. You could write your data to a 14″ Winchester drive for storage–but if you wanted to process a COESY dataset, you had to over-write the data as you did so–that’s all the room we had.

  17. HK says:

    My alma mater ran a 60MHz for the undergrad labs (for perspective, I’m only 24 so this wasn’t that long ago). As I was graduating, they were able to purchase a 300MHz through donations dedicated just for the undergrad labs, which was pretty cool. I heard later that they were contacted by a museum to purchase their old 60MHz.

  18. Resveratrol Receptor says:

    I wonder if you can fetch something metal and use the 25’s magnetic field to work out?

  19. Karl says:

    The Bruker came complete with built-in Eico 460 oscilloscope, if the picture can be believed. (I actually have one of those things, and it worked the last time I turned it on, maybe 3-4 years ago. The Eico, I mean, not a Bruker!)

  20. Algirdas says:

    “Enjoy your helium-cooled superconducting magnet NMR machines while you can”
    i) I heard a rumour that Bruker have a system where they somehow recycle He via cryoprobe, making He refills much less frequent. (Similar system for nitrogen is already functional
    ii) air has 5 ppm He. Too expensive to extract at a moment, but when underground He is gone, this will become a plentiful source of (much more expensive than currently) helium.

  21. Physicist says:

    Helium recondensers are practical for 20 mK dilution fridges — no reason why they wouldn’t be reasonable for a magnet that’s in persistent mode for months at a time. Upfront cost is high, but not high compared to a 900 MHz magnet, and running costs are basically 10 kW continuous plus cooling water. At the moment, liquid helium is cheaper than that in the US, but that could certainly change.

  22. Denzil says:

    Alan, you and your caegeoluls at Varian have been critical to many successes in MRI. Thank you all!

  23. Denzil says:

    Alan, you and your caegeoluls at Varian have been critical to many successes in MRI. Thank you all!

  24. Denzil says:

    Alan, you and your caegeoluls at Varian have been critical to many successes in MRI. Thank you all!

  25. Eric says:

    There is a small bench scale NMR (picoNMR I think) which operates at 45 MHz and is about the size of a computer.
    Who would have thought that was possible 20 years ago?

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