-- ============================================ Perry J. Pellechia Director of NMR Services University of South Carolina Department of Chemistry and Biochemistry <mailto:pellechia_at_sc.edu> <http://homer.chem.sc.edu/perry> I have one of the first triple resonance HCN Prodigy probes on our 600 MHz system. It was first installed in the summer of 2012. I's been in nearly constant operation since then. We had a few issues with C13 noise, but they seem to have been resolved by warming up the probe every 2-3 months and improving the vacuum in the warm state for 12-24 hours then recooling. the sensitivity is quite amazing on this probe. Rivaling that of our Agilent 800 Helium based cryoprobe (of the same age) on really protein samples. Brian Cherry Magnetic Resonance Research Center Arizona State University Ph: (480) 965-3613 Fax: (480) 727-8563 Dear Bill, I've copied this to Professor Guy Lloyd-Jones, whose group purchased a 19F-free Prodigy last year. Guy might be able to comment on the performance and background. There are some discussions in the UK at the moment about issues with 13C decoupling artifacts on a batch of Prodigy probes that you might want to ask Bruker about. I can put you in touch with someone who has been having problems with bthis if it's of interest. Craig Hi Bill, We have two prodigy probes, both installed 21 months ago. One on a 500 and one on a 400. For 19F acquisition we use the zgbs pulse sequence as standard in automation. Most users feel that this gives an acceptable baseline whereas the roll in the baseline when only a 90 pulse is used is not acceptable for the majority. In general I am very happy with the probes. They have a few issues - the transfer line from the prodigy dewar to the probe requires pumping down every 6 months or so due to it going soft, and ice builds up in the prodigy fill port over about the same period requiring thawing. There is also an issue regarding some systems (I have seen it once on one of mine) for 1H{X} decoupling - ie hsqc - showing side bands. This issue is currently being discussed at length in the UKMRM group. If you would like some example 19F spectra then let me know and I'll find some pdfs. Regards, Ralph _______________________________________________________________ Dr. Ralph W. Adams Research Fellow in NMR Spectroscopy School of Chemistry, University of Manchester, Oxford Road, Manchester, M13 9PL Tel: 0161 30 60389 Hi Bill, We have a broadband LN2 Prodigy probe (there are now a variety of probes that Bruker calls "Prodigy"). It was installed in Sept 2012 onto a new Avance III 500 MHz spectrometer. Our setup is likely a bit unique, in that we switch it in and out on a regular basis with a BBFO+ Smartprobe; now about once every 10 days. So we've had a lot of practice swapping the probe in and out of the magnet; haven't counted, but likely > 50 probe swaps by now. I think the probe is really great, especially in its build quality, which hopefully will translate into durability down the road. We've had no problems of any serious nature with the probe. The 1st LN2 transfer line we got did not hold vacuum well, so Bruker replaced it. The bottom plate on the probe that the ATM screws into tends to come unscrewed with used, so we've gotten used to checking it during each probe change. Otherwise a very high quality probe, doing just as Bruker promises: 2.5-3x S/N improvements across all X nuclei, and very good 1H line shape and water suppression compared to older BB probes (the new BBFO+ is similar in line shape and suppression). There is 19F background, similar to the BBFO+. I have no experience with 19F background free versions. We really like the probe a lot. I see no negatives. It is intermediate in s/n compared to LHe probes, but same with cost. We had our first once-per-2-years maintenance, and that went well. And I would not want to take a LHe probe in and out as we're doing with the Prodigy. Charlie Hi Bill, We have a 600 MHz Prodigy BBO that was installed in 2012 (Serial #001). Overall we have been extremely pleased with it. It iss versatile and the performance is very good (S/N was 15-20% above specs for the various nuclei). We are just now setting up a new 500 system which will also have the Prodigy BBO. Specific problems: When first delivered was DOA due to bad cryo temperature sensor. The delayed installation by a month while the probe made a trip back with Switzerland. Liq-N2 hold time wasn't up to spec... they replaced the flexible vacuum line. I would recommend getting the optional scales to provide a direct measure of the liq-N2 consumption/level. As with all cryoprobes (it seems) there is a gradual build up of crud (ice?) on the coil electronics that causes "micro-arcing" that results in bad fids & glitches particularly in 2D sequences with X-nucleus decoupling during acquisition (HSQC) or spin locks (TOCSY). The general remedy is to warm the probe and pump the vacuum for a day or two. Reportedly there are pulse sequences that can be used to "burn out" the crud... we haven't tried that. The last time the warm pump protocol didn't solve the glitch problem so Bruker had us send the probe back to Switzerland for warranty service. They didn't reveal exactly what they did to it. Possibly the coil was swapped out or they pumped it while baking in an oven (don't try this at home...). There is some discussion about contamination coming through the liquid N2 supply. To pressurize the liqN2 dewar we use N2 from a membrane separator provided by Bruker (this is supplied with dry air from a Balston air drier). The same N2 is used for the probe VT. There is talk of adding an additional N2 separator in tandem with the first to improve the purity. If contamination of the supply dewar is the problem then we may also need to look at more a stringent protocol when we refill the dewar possibly purging the transfer line with dry N2 before connecting to the supply dewar. A couple of other labs have had noticeable ice/frost buildup in the Prodigy dewar, but we are not aware of that happening on our system. The Prodigy is very verstile... we've looked at nuclei all over the periodic table. In addition to 1H, 13C, and 31P that are mainstays in our labs, people regularly run 27Al, 29Si, 195Pt, 11B, 51V, 119Sn and many others. Indirect heteronuclear experiments work well, e.g. 15N or 13C HSQC. The sensitivity is great for DOSY of oddball nuclei, e.g. 119Sn in metal cluster systems which are popular here. The probe appears to be made from all sorts of exotic materials, which Bruker is very secretive about, but they obviously include 11B, 29Si, 27Al, and 19F. The background is generally manageable if one increases the DE time. For 19F narrowing the spectral width usually gives a satisfactory result. I wasn't aware that a 19F-free version was being offered. I'll have to ask about it. With 195Pt there is another quirky issue. There is a wild background, but apparently is caused by probe ringing, as I learned from talking to Clemens Kumerle (the Prodigy group leader in Switzerland) at the ENC in April. I haven't had time to play with that since the conference. Presumably the 500 MHz version of the probe will behave differently in that regard. The liquid N2 service is a pain, but is routine. We do it once a week on a fixed schedule. We use about 90-100 liters/week. If the N2 runs out accidently, it is no big deal... the probe just warms up. Cool-down is less than two hours. Forced warm-up is about 3 hours hours. It is completely quiet... none of the chirping etc from a helium cryoprobe or noise from heat exchangers. The PCU (control unit with turbo pump etc) is supposed to be serviced every two years. We are now at 2.5+ years, waiting for the service to be scheduled. There is no obvious change in performance that would make us be in a hurry to get it done sooner. All in all we have been extremely pleased with Prodigy... to the extent that we ordered a second one with our new 500. The sensitivity, versatility and cost are a great match for our user base. Let me know if you have further questions. --Mike ----------------------------- Michael Strain, PhD Director, CAMCOR NMR Facility University of Oregon Eugene, OR 97403-1253 mstrain_at_uoregon.edu<mailto:mstrain_at_uoregon.edu> 541-346-4605 office/lab 541-556-4077 mobile http://nmr.uoregon.edu Hi Bill, We have now had our BBO Prodigy for over 2 years on an AV III HD, we are going to have the 2 year PM done it tomorrow, and I am quite happy with this probe. We have had no down time with the probe and it has been very robust and performed quite well. We have not used this probe for 19F, so I cannot comment on 19F background signal. Let me know if you have any specific questions about the probe? Best Regards, Kurt The Lubrizol Corporation * Senior Fellow, Applied Science * phone 440 347 2026 * iphone 440 364 9006* kurt.wollenberg_at_lubrizol.com<mailto:kurt.wollenberg_at_lubrizol.com> Hi Bill, While we don't have a Prodigy cryoprobe (or any for that matter) I recently attended Bruker's service and maintenance course which covered the cryoprobe. - The most important warning they listed regarding the cryoprobe was sensitivity to power setting. If you're using a newer instrument with PICS as well as zg safety enabled you will never have a problem, but if you feed the probehead too much wattage and burn it out, you'll be in for a very expensive repair (read: overseas strip down and rebuild in a cleanroom). - Nitrogen fills are weekly, and VT, or at least nitrogen gas is mandatory, so budget accordingly for the correct VT board (depends on your console, ECL level, Bruker will be able to determine what you'll need exactly). - If you're inexperience in mounting the cryoprobe rigging and lifting/lowering the probe, you may want to get trained properly since it is much heavier than the average probe. Also this is a 2 person job. - Bruker states service intervals of 24 months, at 1/3rd the cost of a traditional cryoprobe. They'll switch the entire control unit (which contains the diaphragm roughing pump and turbopump) and refurb at the factory so you won't have any significant downtime. >From my perspective I could never make the cost/benefit equation work out, we don't do enough heteroatom work to justify the added labour and capital cost, so we opted to go for a more durable BBFO probe with ATM accessory. Hope this helps! Thanks & Regards, Norman Chu ________________________________ Norman Chu R & D Chemist Torcan Site Piramal Healthcare Limited<www.piramalpharmasolutions.com> 110 Industrial Parkway North Aurora, Ontario, Canada L4G 3H4 Direct +1 905 727 9417 x 327 norman.chu_at_piramal.com<mailto:norman.chu_at_piramal.com> [cid:image001.gif_at_01D0B4DA.6FC6BCB0] ________________________________ This message may contain confidential information. If you are not the designated recipient, please notify the sender immediately, and delete the original and any copies. Any use of the message by you is prohibited.
(image/gif attachment: image001.gif)
This archive was generated by hypermail 2.4.0 : Mon Jun 19 2023 - 16:29:32 MST