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无线电台会影响NMR

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发表于 2008-7-1 02:51:48 | 显示全部楼层 |阅读模式
 When it comes to polluting the environment, humanity has no equals. 5 Z3 K" m# K. P, a& T8 [This applies to all kinds of spaces, including the electromagnetic& }2 ?% d3 w, j( a( C ether. What follows is a contribution and a warning from Vanni Piccinotti,' ^6 z8 r9 _* J; u an engineer based in Florence, Italy, who has decades of experience" |, w( X# i0 k$ d- I with installing, testing, and servicing NMR and EPR spectrometers. The 8 C( B [5 q! D& p, ]0 eproblem of RF interference has never been trivial and it keeps slowly" K4 g- T: w" I but inexorably mounting. The spread of urban areas (combined with the$ y6 y9 o: _) j2 d tendency to install MR instruments in those same areas) and the x" M1 F; @) R. V mounting maze of wireless technologies penetrating our daily life spell 9 Y7 n+ m) h* m% [0 u( Nnothing good for the future quality of our NMR signals. With concurrent% n6 Z7 F! Q5 l; n. \: z* Z progress in basic sensitivity of the instruments, time might come when H* Z$ I$ V4 q8 ~% Venvironmental RF noise will be the single major obstacle to further( O3 C8 E6 b3 i w+ x progress. But let us hear what Vanni has to say:
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 楼主| 发表于 2008-7-1 02:53:56 | 显示全部楼层
 

, I; Z& g% S* l6 I( K" `Cross-talk between FM Broadcast Radio Transmitters (88-108 MHz) # _& j* B/ a6 a- D& i7 t2 t ^and NMR Spectroscopy: A recent experience# Q8 V) V! s, ^: s5 @

9 K) D. t) u9 j9 i4 cRecently I had to install a 400 MHz (9.4 T) NMR Spectrometer. The ; G h, s, ^- Tsystem worked fine and, using an Indirect Detection Probe , met quickly. s, L# ]3 N' t3 g1 m and effortlessly the specifications. But later on, when the customer ! ?5 p, c& {- R! finstalled a 13C direct detection Probe, the S/N ratio turned out to be+ f- f7 _6 {4 ?% \/ o, l quite low and, on top of it, the sensitivity was subject to erratic and 6 v. H; T6 [- F5 \very large variations from 50:1 to 130:1 (manufacturer's specs give% g c0 L$ N" R2 J" z+ L( X 155:1), without any apparent reason. 8 y( L# w; V' ^& b; H

Since the nominal 13C observe frequency at 9.4 T is 100,568& m4 b( }/ a- E. F; q MHz, right in the middle of the range of commercial FM broadcasts, I : D2 }1 w7 i7 t8 K' v6 g5 Ghave immediately suspected that the spectrometer was picking up one of6 g0 e9 D" U: r, N( \$ W those radio stations. In fact, using a cheap FM radio receiver, a( q% X; @4 i( I+ } strong station was quickly found at 100,60 MHz. At this point, I have0 i4 R% t; c5 r& ~ connected a simple audio amplifier ending with a loudspeaker to the 9 K* O+ L2 d1 a5 C" noutput BNC of the observe receiver which was there apparently just for9 A/ x$ n/ }- F$ b6 l5 \& B8 | this purpose, and all of us were listening to the radio using a 200.0008 Z& G. w* w9 j5 U; n; C7 c( V/ f1 q Euro NMR spectrometer, except that the audio quality was really poor,3 ^' L% d" U3 t( k/ [3 @ much worse than from the above-mentioned gadget radio (a shopping mall! I1 @7 i7 v8 W; w3 g gift)." K. F# l/ N# f4 A

The problem is well known from the old times, when the highest) i" Q! {+ a& G) L; S Z field was 2.45 T and the nominal H1 frequency was close to 100 MHz. One* t1 ?- v, F. b& W4 x of the first Italian NMR spectroscopists to experience it, back in % Q% ?' i2 ^. r& j* h% s1974, was Prof. L.Lunazzi at University of Bologna, on his brand new 6 P" X; Q: j) M( ~Varian XL100 spectrometer, and the radio station was Radio San Luchino, - E- ~( B. g; ?2 j6 t' rwell known to anybody living in Bologna, which broadcasts from the top5 d) g5 r& s% t0 K% D of the nearby Saint Luca hill. 6 U/ A; M0 p, ~% O8 B

The obvious solution is to change the magnetic field, and thus 4 p' e/ _1 v+ Fall resonance frequencies, in order to get out of the modulation % U' L1 W) p- a" }2 Eenvelope of the interfering transmitter. But this is not always easy,4 b0 C: C) Z+ g( w' S2 W since the range by which one can move the magnetic field changing just& o* f- b% m1 O G some software parameters is usually limited to a few tens of kHz in the, ?( x7 W5 V% [, t& ~! P frequency domain. If larger variations are required the poor engineer 3 e8 L0 r0 p! O7 z9 ^3 E' T6 chas to work on the superconducting coils of the magnet, which is a- c6 a7 P9 y0 F no-trivial job entailing the risk of a total or partial quench. , N* h/ \6 ?6 {. y, j

Bitter experience shows that persuading the involved radio 5 k$ p; Y k! [% ^9 `- [. jstation to change its operating frequency is a time consuming,7 v7 m. X) c7 y2 o2 s: m0 p* E/ t frustrating, and apparently quite impossible task. ! E/ l) _9 ~# y+ c

Being well aware of the problem, my preliminary spectrometer + C. i4 P& [ R4 |2 zchecks always include some blank acquisitions taken before running up+ m4 V$ a' P( z( v0 x the magnet so that there is no chance to observe an NMR signal. The 1 J2 p7 ~( M* r7 j- D R6 b7 ~resulting dataset should be pure white noise, without significant 4 i5 I3 \, n8 p. P/ |8 tspikes. This was done also in this particular installation but, as - }, R; X" _" h% p" S( j5 yusual, in the days following the energization the magnet drifted a bit, ; }" A& B6 w, z& @6 ?" \getting closer to the radio station carrier. Furthermore, the usual 13C 1 c# J& c8 j' y! dspectral widths are quite wide which makes things even worse. Murphy's! H- S$ C. _0 O0 ? Law has no exceptions!, E& Y! [! s# x, L e

But we are just at the beginning of my real troubles. Before 6 r+ S6 |; d4 A3 Y$ T5 xputting one's hands on the magnet, one should better know how much, in% z) r$ E3 P, }$ f* y: j9 L; _ which direction, should the field be moved. I have therefore used a - Y) g7 |$ H4 D( W8 zgood Spectrum Analyzer (Tektronix model 2710) to check the frequency( a' E% F% a! ~ spectrum around 100 MHz, ready for the worst. And the worst was what I+ Y0 V+ ^# m9 {6 @6 z2 H got! The band was filled with FM signals, evenly spaced by 250 kHz and " k0 ~# t/ Y* z2 Y7 F1 Cwith modulation envelopes as wide as 100 kHz, so that when I got far: E" T- m: S5 U" X1 k- T from one station I started receiving the next one; accounting for& m3 x/ g' y; F. i" w3 N4 j3 C folding and aliasing effects, there was no chance! The only somewhat ( X! z& g" n4 i( v. xfree region was at 100,120 MHz, but this implied proton frequency of - a, u! i {: {1 z. H' s8 U398.100 MHz. So now the spectrometer is no longer a "400"!% r+ g5 a7 g% ] m) X. N9 H* e6 ?

Before installing a spectrometer, you better get a Spectrum 6 T2 S$ l% Z2 ~2 u4 AAnalyzer and check for the presence of RF fields in the instrument 6 n# ]3 a/ C) f& ^$ q& |room, taking care to explore the areas close to the observe frequencies% w$ P- j: n6 t( }& L! y of all the most important nuclei. Don't forget the lock: at 14 T ) S( @% j0 |" ?$ B. C/ r. b(nominal 1H frequency of 600 MHz) 2H resonates at 92,095 MHz, once ( a, u5 z( R7 Y) Nagain in the FM broadcast band. The lock channel receiver has quite 3 }& B2 m" w- U$ _5 N vnarrow bandpass filters, so hitting a radio is a really bad luck, but 6 ] P( e5 @7 k) w# o$ ?it had already happened, resulting in fast lock level variations and , a+ `7 s$ r* o5 T/ d" }& rtotally malfunctioning Gradient Shimming which uses deuterium as; W8 I5 P( A8 O7 h4 g/ W- m observe nucleus!' Q' }" i# c. H/ R3 i- B0 ^

Needles to say, the extremely high sensitivity of an NMR % M1 i' J' l8 e2 ^0 KSpectrometer shows up. The signal from the guilty radio, as observed on 3 N+ V; U& P. j7 f" ythe spectrum analyzer inside the spectrometer room, had very low - G! Q; Z7 U. f) {1 T# \intensity level of about -70 dBm, some microvolt/meter, but that was : ^1 M4 S( }) i# `8 ?enough to almost completely hide the quite strong 13C signal from the : m: n8 B1 `1 D. [& C( LASTM sample!* j( ~4 A. H. r

The radio was clearly picked up by the Probe (closing the v1 T: U+ Z+ S6 @. q- }( ` Preamplifier input with a shielded 50 ohm RF load, all signals+ ?7 U1 m2 j* O( H disappear) but, quite surprisingly, there is almost no shielding effect ) Z. s) K5 [( oattributable to the metal body of the magnet, which is after all an ) i& Y/ v8 D0 m1 a) c3 R9 }# zalmost completely closed cylinder all around the Probe. Most probably a3 k6 _) V6 s3 q+ P/ U- r good deal of the signal leaks in through the Shim Coils which are6 L3 g" J: x9 J3 Q mounted very close to the Probe and, together with their connection % {. n- T+ Y2 F1 I' u# F9 zcables to the Console, constitute a quite good antenna. 7 [0 M2 L% K4 ~6 ]5 h% ~

Too bad the Shim Coils are essential, and effective shielding! y- J+ A3 k0 v of the instrument with a Faraday's cage is always difficult and0 @, H. B7 @1 T) k2 Z" k8 H expensive (it may be almost impossible once the spectrometer is ) Q' o' Q5 R7 A& _' |" G$ F2 ~installed).8 c( O. ~* ]! B$ c+ |" Q) W9 u

- k" X: c2 o: }4 ?- A Before concluding, let me venture some additional advice based on my experience:: r$ y# O) E% A6 }- A8 Y, y

' _" p9 S3 l" a& ?/ U = Install the spectrometer in the best shielded room $ T2 y6 U$ O4 n0 M: X1 D; E6 `5 lyou can get; the best choice is once again in the basement, where you% D3 V5 }( @, q; C have the whole building above the ceiling and its [grounded]4 W' Y/ z6 s) t$ x7 K) N7 e/ j$ ?: u foundations all around the rest, done in iron-reinforced concrete, * h+ Q1 Q. K; |+ l1 L! {/ t9 tamounting to a good Faraday's cage at no extra cost.0 p& p5 M! Z( I- C: p( U6 m

/ }" N+ [% X: G; u3 @5 O6 n% y = If possible, avoid top floors. If you can't avoid " Q# |" F: c4 D \' Qgoing upstairs, take a good look out of the window: if you see nearby2 g+ M# s+ l) B! p7 \. i! W+ Y5 \ transmission antennas, get ready for troubles proportional to their6 S$ v5 X/ Z5 | M dimensions and closeness (to my knowledge, however, mobile telephony 1 _% ~. r2 E! [& c5 G H7 {7 wantennas cause so far no harm).& r7 ^& w' g, v. ?( z( x

$ M0 c- V+ ?" Z5 r6 _' | = I'm sure that an exchange of experiences and/or$ N: |" ~1 P" a9 D+ C: y/ E6 @ suggestions regarding this matter would help a lot to solve many, w; X) T, T q 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. & D" A% {9 [+ a6 L/ C2 v

c: M: X( o% QVanni Piccinotti, Firenze, 11 April 2008


摘自stan' NMR Blog.

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发表于 2008-7-2 09:22:51 | 显示全部楼层
see see!
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