Hi everyone,
Thank you for your feedback regarding the Bruker Prodigy cryoprobe. I
received numerous positive responses with very few caveats. We were able
to get some preliminary data from Bruker and another laboratory and the
data look fantastic. We were able to get 13C and HMBC data with comparable
S/N in 1/4 the time at 400 MHz vs. our 500 MHz BBO probe. Users reported a
2.5 to 3x sensitivity improvement across all X nuclei resulting in one case
in an ~8 fold time savings for 13C and 10 fold for 29Si. Another user said
having a 3 min 13C experiment on a walk up instrument has made my organic
chemists very happy.
Usage seems to be split roughly even between 400 and 500 MHz systems and
there appear to be several in the marketplace at this time. Users reported
mostly positive feedback about ease of set up and switching probes,
maintenance, and N2 filling.
Below is the original post, along with the summarized responses and some
additional info I got from Bruker.
Thanks again,
Mark
Original post:
We are applying for a NSF grant to purchase a Bruker 400 MHz spectrometer
equipped with a Prodigy cryoprobe. Does anyone have one of these probes at
400 MHz who would be willing to acquire a couple of spectra for us to
include in our grant? Also, any feedback you have about this type of probe
(regardless of field strength) would be appreciated.
AMMRL comments:
1) We have a 500 Prodigy BBO probe. It is very good and we are happy
with it. Only suggestion is ask for temp up to 130C degree option. The
price is the same!
2) We have a Prodigy probe at 500 MHz. We have been happy with our
probe; great build quality from Bruker, and works almost exactly according
to their specifications: 2.5 to 3x sensitivity improvements across all X
nuclei compared to BBFO/SmartProbe (which we also have at 500MHz). It of
course has added costs of constant LN2 fills (we do them once per week),
and once per two years maintenance from Bruker. NSF will want to see
strong evidence that your facility will be able to afford these costs down
the line. You lose the ability to do 19F{1H} or 1H{19F} compared to BBFO,
and also have a more limited VT range. But otherwise I'm very enthusiastic
about the probe. We do a lot of 29Si, as well as 1H-15N experiments.
Prodigy significant out-performs our BBFO+ on these experiments. It is
very good for direct 13C as well. We get ~10x improvements for 29Si, and
~8x for 13C in lengths of experiments to get same data quality on the
Prodigy compared to BBFO+.
3) I think it is an absolutely fantastic probe, and an excellent value
when you
consider the cost of ownership compared with a helium temperature
cryoprobe.
4) We just recently acquired a 500Mhz Prodigy probe and are very
impressed by the results. Excellent sensitivity and fantastic lineshape.
It is a reasonably simple system to maintain and operate once you get it
down. So far no issues. I would mention that the installation was a bit of
a chore on our older system. In addition, the requirements for nitrogen
gas supply may not always be available out of the box. Do you have in
house Nitrogen of 100psi minimum? If not, they will try to sell you an air
compressor/dryer/N2 exchange system that will run upwards of $20K. We set
up a simple dual gas protocol system running off 240L high pressure liquid
dewars. This does require you to swap out tanks about once a week, but
it's very simple. This is a far more economical system that the setup they
suggest.
5) The system required filling a liquid N2 dewar weekly, but this is
little different that filling a magnet. There is also a biannual
maintenance requiring replacement of the compressors/filters in the Prodigy
system which I think runs about $7K.
6) We're running a 5 mm Prodigy TXI at 500 MHz that has the best line
shape of any of the cryoprobes we have in service at Merck. The LN2 hold
time is a little short of spec but filling the Dewar once a week is no big
deal. We're also running a 600 MHz broadband Prodigy that gives superb
carbon sensitivity when you need it.
7) We operate more or less the same system since June 2014 (Avance III
400 MHz / Prodigy BBO with ATMA / please note our special case: wide bore
magnet). Compared to our room temperature BBI probe (this is not really a
new model, we used it since 1997) we observe a sensitivity boost of > 3 on
X and > 2 on H channel. Since regularly we also measure solid state NMR we
have (as mentioned above) a wide bore magnet and, therefore, we have to
insert and connect a narrow bore shim system whenever we change back to the
Prodigy configuration. We operate the system together with a SampleXpress
(changer sits at the top of the shim system, 16 positions only, assemble
and disassemble within 10 min.). For cooling down and thawing up the
Prodigy system you have to expect with approximately two hours. Although
this operation takes so long, the high sensitivity of the prodigy system
justifies the long conversion time. Although the hold time of the N2 Dewar
used for cooling is specified to 10 days we refill earlier (consumption of
ca. 50 kg/7 days), then the interrupt time is shorter and you do not run
into problems when the N2 level is too low. As soon as the N2 level falls
below ca. 30 kg the probe might thaw up automatically.
Using a Shigemi tube it is e.g. possible to record an overnight 1D 13C NMR
experiment with a reasonable S/N of approx. 0.2 mg of a natural product (MW
of 340) with many quaternary carbons not in proximity of protons.
Prodigy system advantages: High sensitivity / stability of pulses / in the
first 18 months of use no big issues / “Bruker cryo service” period of 2
years (fees much cheaper than for He cryo probes)
Prodigy system disadvantages: cooling down and thawing up time of 2 hours
in the case of probe change / periodic refill of liquid N2 used for cooling
(50 kg/7 days) / freezing of “N2 suck in” capillary (remove, warm up, dry,
install again) / freezing of “N2 outlet” used for filling Dewar (perhaps
could be improved with the new hardware, if this happens you have to thaw
up completely the N2 dewar)
8) In general I would say they’re great. They are a bit thirsty –
taking an extra 60-100 L of N2 a week, they have filters in the probes for
the lock which means you can’t acquire some of the more exotic nuclei, and
the baseline for 19F is terrible. They are a hassle to change so you want
to make sure that all the samples are cleaned before they go in and that
you have a sampleXpress type autosampler that covers the magnet and stops
dirt getting in. There have been issues with 13C decoupling on some systems
(giving bad to terrible stripes in HSQC) so I’d go for a 2 year warranty if
you can afford one. Other than that, the signal – noise ratio is brilliant
and having a 3 min 13C experiment available on a walk up system has made my
organic chemists very happy.
Comments from Bruker:
1) 400 MHz is our most popular field strength. This year, in North
America alone, we sold 47. Ten were here in California, but only two to
universities.
2) It seems as if most customers perceive the 400 with a Prodigy to
provide the most bang for their buck, although the Prodigy is also pretty
popular at 500.
3) The Prodigy probes have been very well received by industry, at both
400 and 500 MHz.
Received on Thu Jan 07 2016 - 08:31:34 MST