无线电台会影响ＮＭＲ

syflu

 When it comes to polluting the environment, humanity has no equals. This applies to all kinds of spaces, including the electromagnetic ether. What follows is a contribution and a warning from Vanni Piccinotti, an engineer based in Florence, Italy, who has decades of experience with installing, testing, and servicing NMR and EPR spectrometers. The problem of RF interference has never been trivial and it keeps slowly but inexorably mounting. The spread of urban areas (combined with the tendency to install MR instruments in those same areas) and the mounting maze of wireless technologies penetrating our daily life spell nothing good for the future quality of our NMR signals. With concurrent . Q4 F! Q8 U# L* n. ?6 oprogress in basic sensitivity of the instruments, time might come when environmental RF noise will be the single major obstacle to further ' m: q h9 m8 k) V y/ H3 Cprogress. But let us hear what Vanni has to say:

syflu

 

Cross-talk between FM Broadcast Radio Transmitters (88-108 MHz) 2 O0 W$ G, J5 b9 x4 ^0 t+ jand NMR Spectroscopy: A recent experience

Recently I had to install a 400 MHz (9.4 T) NMR Spectrometer. The ) w# `7 F# v! S8 v7 t. J, m2 d. Qsystem worked fine and, using an Indirect Detection Probe , met quickly and effortlessly the specifications. But later on, when the customer : J1 I/ M4 \ R5 {' Kinstalled a 13C direct detection Probe, the S/N ratio turned out to be quite 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 155:1), without any apparent reason. , W4 ]1 P! V/ N3 ~$ l* e# Y# q

Since the nominal 13C observe frequency at 9.4 T is 100,568 & ]% z2 B. Y" b1 u/ gMHz, right in the middle of the range of commercial FM broadcasts, I 3 k9 |+ c. R' @7 `8 ~8 jhave immediately suspected that the spectrometer was picking up one of % u$ N$ j, f5 K; O7 X% a+ h$ P9 hthose radio stations. In fact, using a cheap FM radio receiver, a , P: E5 I7 D6 q) M1 ustrong station was quickly found at 100,60 MHz. At this point, I have 2 w1 }. h6 @" X! P* Iconnected a simple audio amplifier ending with a loudspeaker to the output BNC of the observe receiver which was there apparently just for 3 P" {6 B+ y D% b, T- hthis purpose, and all of us were listening to the radio using a 200.000 Euro 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 field was 2.45 T and the nominal H1 frequency was close to 100 MHz. One of the first Italian NMR spectroscopists to experience it, back in 1974, was Prof. L.Lunazzi at University of Bologna, on his brand new 2 \+ a7 q0 d/ a$ A* c! NVarian XL100 spectrometer, and the radio station was Radio San Luchino, well known to anybody living in Bologna, which broadcasts from the top 7 Y& [/ H$ {, {6 I; w1 e' t+ lof the nearby Saint Luca hill. - J( I! Q( S0 V% w6 Z/ m! m. q" ?

The obvious solution is to change the magnetic field, and thus all resonance frequencies, in order to get out of the modulation envelope of the interfering transmitter. But this is not always easy, / F& F# A' f! e/ A6 y$ \since the range by which one can move the magnetic field changing just 5 p: ^4 r8 w$ ^/ h# gsome software parameters is usually limited to a few tens of kHz in the ( K3 A9 e/ O* g8 H' Cfrequency domain. If larger variations are required the poor engineer - F0 p% w# G" R8 F3 D" Vhas to work on the superconducting coils of the magnet, which is a # a4 Y+ {9 Q+ {$ w/ S- x% ono-trivial job entailing the risk of a total or partial quench.

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 ( Y6 O( z* R2 g* K2 w, E- T) Fchecks always include some blank acquisitions taken before running up / i$ ^8 `3 j- P( E9 Bthe magnet so that there is no chance to observe an NMR signal. The resulting dataset should be pure white noise, without significant spikes. This was done also in this particular installation but, as 3 w) U/ x- y9 L# Eusual, in the days following the energization the magnet drifted a bit, ^$ K/ P' l, F0 f! W- D3 Dgetting closer to the radio station carrier. Furthermore, the usual 13C spectral widths are quite wide which makes things even worse. Murphy's * k+ h! T+ k" l) y& t- d; YLaw has no exceptions!

But we are just at the beginning of my real troubles. Before 0 f9 y2 `; N7 E# E z8 O' d( Nputting one's hands on the magnet, one should better know how much, in $ ~3 L; U3 P& }( F+ v; P1 C0 Owhich direction, should the field be moved. I have therefore used a ( ^) i; q5 G: Ngood Spectrum Analyzer (Tektronix model 2710) to check the frequency ) G" `2 s9 u( Z2 G# }0 T6 U) \spectrum around 100 MHz, ready for the worst. And the worst was what I # x4 _/ A. s; E. d2 n, O0 {7 Hgot! The band was filled with FM signals, evenly spaced by 250 kHz and " V: m, a9 n+ k) c) Qwith modulation envelopes as wide as 100 kHz, so that when I got far from one station I started receiving the next one; accounting for 3 Z. `0 O! v$ H8 F4 T, lfolding and aliasing effects, there was no chance! The only somewhat 2 B2 ~5 g1 C" q: X) M$ w- hfree region was at 100,120 MHz, but this implied proton frequency of 398.100 MHz. So now the spectrometer is no longer a "400"! 2 O% I( n* p+ D+ F4 B+ k! z' F+ c

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 : z2 n# [) u2 q$ O5 @(nominal 1H frequency of 600 MHz) 2H resonates at 92,095 MHz, once 1 ]! T' ^1 i1 o$ W+ x2 lagain 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 * |1 e0 x2 u4 rtotally malfunctioning Gradient Shimming which uses deuterium as : k( y7 P$ ^7 ]observe nucleus! 0 b1 W( u9 |+ m

Needles to say, the extremely high sensitivity of an NMR Spectrometer shows up. The signal from the guilty radio, as observed on 6 \. O) I- q- [; G+ c: \0 x; c+ R+ Z! Dthe spectrum analyzer inside the spectrometer room, had very low 0 d/ ^! k7 Y; [1 mintensity level of about -70 dBm, some microvolt/meter, but that was # _( P! I2 g- @) W7 D/ Menough to almost completely hide the quite strong 13C signal from the ASTM sample! 7 U5 q7 M* ]. ?9 n C

The radio was clearly picked up by the Probe (closing the 2 o( ~0 Z* u+ V3 ]# F3 CPreamplifier input with a shielded 50 ohm RF load, all signals disappear) but, quite surprisingly, there is almost no shielding effect $ \% K# R) G, ~" Aattributable to the metal body of the magnet, which is after all an % _* ^; L: u, P9 x9 valmost completely closed cylinder all around the Probe. Most probably a + l ]/ K2 y6 b% pgood deal of the signal leaks in through the Shim Coils which are * u( X3 C, O4 }' t+ x+ i6 C& jmounted very close to the Probe and, together with their connection ( U/ C. S; j4 q+ i1 ~( G/ U& U, Z2 }cables to the Console, constitute a quite good antenna.

Too bad the Shim Coils are essential, and effective shielding 9 @+ h# q) ~+ qof the instrument with a Faraday's cage is always difficult and expensive (it may be almost impossible once the spectrometer is ( B! V: c/ v5 [% X6 p4 @; Y2 Z/ ?+ pinstalled).

! n/ i: D. y7 |7 v( gBefore concluding, let me venture some additional advice based on my experience: ) ~& o' J7 M3 i' f. G

/ y* P! q' H1 F' S( _= Install the spectrometer in the best shielded room you can get; the best choice is once again in the basement, where you 5 s$ U8 K3 S) O* |5 Z$ Khave the whole building above the ceiling and its [grounded] foundations all around the rest, done in iron-reinforced concrete, 7 m4 i7 I$ o% z2 `) E+ s3 x4 vamounting to a good Faraday's cage at no extra cost. ! l2 e; {7 g9 G; M" ^

= If possible, avoid top floors. If you can't avoid 6 ?$ B8 m; ?& w. y; h$ A( fgoing upstairs, take a good look out of the window: if you see nearby * S5 T" o. l u; {+ J( y1 p9 ftransmission antennas, get ready for troubles proportional to their 9 {8 I8 ?' E% L0 Odimensions and closeness (to my knowledge, however, mobile telephony 3 ~' B3 s$ [" r% B) n9 ~antennas cause so far no harm). 2 n7 w! J& r+ V

) F- `- g- K0 P= I'm sure that an exchange of experiences and/or suggestions regarding this matter would help a lot to solve many 4 ]# x* m) M: }$ {% x) X, oexisting 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. ( K6 e3 K( U, m. Q3 b& j6 k

% E# j" T* Q$ w+ Z4 gVanni Piccinotti, Firenze, 11 April 2008

摘自stan' NMR Blog.

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