无线电台会影响ＮＭＲ

syflu

 When it comes to polluting the environment, humanity has no equals. : D$ I! T8 c6 m ], nThis applies to all kinds of spaces, including the electromagnetic 4 m4 T2 R) R7 @& {, P; n$ P- ^ether. What follows is a contribution and a warning from Vanni Piccinotti, 4 B; t- ?2 E# V! f2 Zan engineer based in Florence, Italy, who has decades of experience . }/ m: \# M* ~with installing, testing, and servicing NMR and EPR spectrometers. The - a) a8 v( X; J) E) Bproblem of RF interference has never been trivial and it keeps slowly but inexorably mounting. The spread of urban areas (combined with the 1 V c" A# V4 f. b7 p) Ptendency to install MR instruments in those same areas) and the / ]+ d2 R% [! t2 L( _mounting maze of wireless technologies penetrating our daily life spell nothing good for the future quality of our NMR signals. With concurrent progress in basic sensitivity of the instruments, time might come when . \ Q3 }2 J; `. k" D4 cenvironmental RF noise will be the single major obstacle to further ( w2 r! M8 b/ O& q+ \progress. But let us hear what Vanni has to say:

syflu

 

" N* L z9 a! GCross-talk between FM Broadcast Radio Transmitters (88-108 MHz) and NMR Spectroscopy: A recent experience

/ ], e6 q, }4 N( ]Recently I had to install a 400 MHz (9.4 T) NMR Spectrometer. The ; }; W9 A u$ fsystem worked fine and, using an Indirect Detection Probe , met quickly 1 z4 V, P$ P- r2 Z6 S: Oand effortlessly the specifications. But later on, when the customer installed a 13C direct detection Probe, the S/N ratio turned out to be 3 q* u. i* j0 xquite low and, on top of it, the sensitivity was subject to erratic and very large variations from 50:1 to 130:1 (manufacturer's specs give 7 \8 U& L% F% k6 I1 O# U X155:1), without any apparent reason. 6 r3 s% ^1 C; C" u4 I' [

Since the nominal 13C observe frequency at 9.4 T is 100,568 # r, N- M# g# p. |MHz, right in the middle of the range of commercial FM broadcasts, I have immediately suspected that the spectrometer was picking up one of $ y1 F% P. k; u7 Y& E% L3 Zthose radio stations. In fact, using a cheap FM radio receiver, a % L$ \- S! J. E, u/ Fstrong station was quickly found at 100,60 MHz. At this point, I have ( D: a- ?7 z2 J2 ^4 F6 `connected a simple audio amplifier ending with a loudspeaker to the output BNC of the observe receiver which was there apparently just for this purpose, and all of us were listening to the radio using a 200.000 ' k% g! x" ~3 }" }$ C) _+ h5 ~9 AEuro NMR spectrometer, except that the audio quality was really poor, much worse than from the above-mentioned gadget radio (a shopping mall gift).

The problem is well known from the old times, when the highest 3 C$ f R6 b% w3 N. e- a ?% Bfield was 2.45 T and the nominal H1 frequency was close to 100 MHz. One 9 n, I7 B9 F2 S( P; G. ]7 Vof the first Italian NMR spectroscopists to experience it, back in 1974, was Prof. L.Lunazzi at University of Bologna, on his brand new Varian XL100 spectrometer, and the radio station was Radio San Luchino, well known to anybody living in Bologna, which broadcasts from the top ) a; ~( s1 |; a- B) `- A8 O0 zof the nearby Saint Luca hill. 9 Y* ~7 S5 l) B

The obvious solution is to change the magnetic field, and thus all resonance frequencies, in order to get out of the modulation ) \6 b0 R0 B+ ]envelope of the interfering transmitter. But this is not always easy, 6 s3 A, i& j6 Z0 I! N$ H$ R( C3 Gsince the range by which one can move the magnetic field changing just " l& U# t( u% _4 Hsome software parameters is usually limited to a few tens of kHz in the frequency domain. If larger variations are required the poor engineer 2 j0 R* g5 W ~$ w0 Dhas to work on the superconducting coils of the magnet, which is a no-trivial job entailing the risk of a total or partial quench. 9 } P! o8 p/ j! v8 P

Bitter experience shows that persuading the involved radio station to change its operating frequency is a time consuming, frustrating, and apparently quite impossible task.

Being well aware of the problem, my preliminary spectrometer checks always include some blank acquisitions taken before running up the magnet so that there is no chance to observe an NMR signal. The ( |/ G4 m. R1 }' a% [resulting dataset should be pure white noise, without significant & F' B3 l$ O, ]) q I% ?spikes. This was done also in this particular installation but, as usual, in the days following the energization the magnet drifted a bit, getting closer to the radio station carrier. Furthermore, the usual 13C spectral widths are quite wide which makes things even worse. Murphy's Law has no exceptions! 6 }4 s; r% w1 M

But we are just at the beginning of my real troubles. Before . p% L% l8 m7 T4 ^3 Z7 \putting one's hands on the magnet, one should better know how much, in which direction, should the field be moved. I have therefore used a good Spectrum Analyzer (Tektronix model 2710) to check the frequency spectrum around 100 MHz, ready for the worst. And the worst was what I ) ^8 R) t/ b2 ygot! The band was filled with FM signals, evenly spaced by 250 kHz and % M4 \+ l5 Q, nwith modulation envelopes as wide as 100 kHz, so that when I got far / i5 }# z7 }. k# Lfrom one station I started receiving the next one; accounting for " k# d' S i0 s( s0 [folding and aliasing effects, there was no chance! The only somewhat free region was at 100,120 MHz, but this implied proton frequency of 0 @/ `/ j- F+ o398.100 MHz. So now the spectrometer is no longer a "400"!

Before installing a spectrometer, you better get a Spectrum Analyzer and check for the presence of RF fields in the instrument room, taking care to explore the areas close to the observe frequencies of all the most important nuclei. Don't forget the lock: at 14 T (nominal 1H frequency of 600 MHz) 2H resonates at 92,095 MHz, once " ?( S+ B* c6 g g- ~8 l+ Fagain in the FM broadcast band. The lock channel receiver has quite narrow bandpass filters, so hitting a radio is a really bad luck, but it had already happened, resulting in fast lock level variations and totally malfunctioning Gradient Shimming which uses deuterium as ) J5 m; H4 f6 n' h, Mobserve nucleus! % [5 `0 k9 v2 c8 }, e3 [# \1 T

Needles to say, the extremely high sensitivity of an NMR Spectrometer shows up. The signal from the guilty radio, as observed on the spectrum analyzer inside the spectrometer room, had very low intensity level of about -70 dBm, some microvolt/meter, but that was ) w G% T" }2 h" k) ~enough to almost completely hide the quite strong 13C signal from the ASTM sample! 6 l* ?, E: @6 _* Y* S

The radio was clearly picked up by the Probe (closing the Preamplifier input with a shielded 50 ohm RF load, all signals disappear) but, quite surprisingly, there is almost no shielding effect : B i, V' T0 z1 M3 h2 `attributable to the metal body of the magnet, which is after all an : G; V- d& C, Z! s5 s9 Falmost completely closed cylinder all around the Probe. Most probably a good deal of the signal leaks in through the Shim Coils which are mounted very close to the Probe and, together with their connection cables to the Console, constitute a quite good antenna.

Too bad the Shim Coils are essential, and effective shielding $ _5 A/ N. x* z4 Q& {/ D6 wof the instrument with a Faraday's cage is always difficult and expensive (it may be almost impossible once the spectrometer is installed). 4 F# W# D; m) M- h

: @4 {; _' S8 `) A1 ]Before concluding, let me venture some additional advice based on my experience:

= Install the spectrometer in the best shielded room 2 W' a7 S1 f4 e8 K0 Z4 lyou can get; the best choice is once again in the basement, where you 9 n/ d& q# ?) Phave the whole building above the ceiling and its [grounded] 8 v( i: [& k% f. |! T3 z! sfoundations all around the rest, done in iron-reinforced concrete, amounting to a good Faraday's cage at no extra cost. 5 e3 n7 N' i' q2 i; g* v3 }

) U7 @5 F: Z; o0 u= If possible, avoid top floors. If you can't avoid going upstairs, take a good look out of the window: if you see nearby transmission antennas, get ready for troubles proportional to their dimensions and closeness (to my knowledge, however, mobile telephony " u9 Z7 g4 P$ {! y2 R7 santennas cause so far no harm).

" _3 J7 ^" g9 y= I'm sure that an exchange of experiences and/or suggestions regarding this matter would help a lot to solve many existing installation problems and prevent ones yet to come. Stan's Blog is an ideal location and, needless to say, I will be absolutely glad to cooperate.

4 ^" E3 Z: i+ ]* X8 ?/ hVanni Piccinotti, Firenze, 11 April 2008

摘自stan' NMR Blog.

sunny

see see！