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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.7 ?4 i9 O& v: x. G- Y This applies to all kinds of spaces, including the electromagnetic ! |" J) {3 n4 v7 h( }; Wether. What follows is a contribution and a warning from Vanni Piccinotti,, f& j) r/ G5 K% r3 D an engineer based in Florence, Italy, who has decades of experience 7 p) `6 s# F' b: l% H9 rwith installing, testing, and servicing NMR and EPR spectrometers. The: w6 c1 \% W9 f* ~) w* T1 w problem of RF interference has never been trivial and it keeps slowly . S8 Q0 B! k) W& A6 `+ r% Mbut inexorably mounting. The spread of urban areas (combined with the / L, p8 ?/ o; t4 `! z, Z* o( J1 H jtendency to install MR instruments in those same areas) and the ' D" g: Z( \) Q* g& o6 Xmounting maze of wireless technologies penetrating our daily life spell8 {# c- a8 f1 t! B" i nothing good for the future quality of our NMR signals. With concurrent0 s9 ?6 X0 R' q, d4 ?* N progress in basic sensitivity of the instruments, time might come when3 o: x' q' S5 L' d Q& T* B environmental RF noise will be the single major obstacle to further, L' U L) ^ {: G8 K3 B 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
 

3 f& p' t9 }% k5 O! tCross-talk between FM Broadcast Radio Transmitters (88-108 MHz) - A; a& ~# ^9 hand NMR Spectroscopy: A recent experience/ T( q& P9 _4 j" S s: A u

! G' l( s) E5 E3 n; c/ H/ PRecently I had to install a 400 MHz (9.4 T) NMR Spectrometer. The 0 R9 ?5 X4 g, J1 ^( f' Asystem worked fine and, using an Indirect Detection Probe , met quickly 3 f; T( ?! J7 q+ E, S4 G6 t9 z/ yand effortlessly the specifications. But later on, when the customer7 T& t3 [* R9 m installed a 13C direct detection Probe, the S/N ratio turned out to be 4 N0 W" m- \ b* u) E/ p5 q" dquite low and, on top of it, the sensitivity was subject to erratic and 1 a6 e3 M/ y8 L' Pvery large variations from 50:1 to 130:1 (manufacturer's specs give ) o- s" o# _/ _- R6 T155:1), without any apparent reason.2 Z; z1 Y1 U9 x2 h: R

Since the nominal 13C observe frequency at 9.4 T is 100,568 ) b* O. M7 z1 f l3 ^- JMHz, right in the middle of the range of commercial FM broadcasts, I ) `% K' [6 {/ N! {( _' khave immediately suspected that the spectrometer was picking up one of 8 j W* e+ E6 X+ G( S# `7 `3 Bthose radio stations. In fact, using a cheap FM radio receiver, a 8 g9 n) N; t* P2 G1 L% hstrong station was quickly found at 100,60 MHz. At this point, I have0 H" j/ D& M& h4 ~ connected a simple audio amplifier ending with a loudspeaker to the 3 i k/ ^$ @6 f3 q, a8 G& eoutput BNC of the observe receiver which was there apparently just for+ N$ I! V1 U5 W this purpose, and all of us were listening to the radio using a 200.000 4 k& z$ N& J5 i) r* u3 R: a( |. rEuro NMR spectrometer, except that the audio quality was really poor, . m8 ^ U8 [; N; S/ Kmuch worse than from the above-mentioned gadget radio (a shopping mall # X% p- U: N, V3 B! X" I: mgift).4 B; c0 P; i1 b& m' K3 j

The problem is well known from the old times, when the highest" M& O7 g* v4 K/ B field was 2.45 T and the nominal H1 frequency was close to 100 MHz. One \$ P7 j. ^/ P! ?8 I$ Pof the first Italian NMR spectroscopists to experience it, back in q9 T# \) O( A$ ]1 b: X- e* n 1974, was Prof. L.Lunazzi at University of Bologna, on his brand new 1 N" t7 i0 k3 ?( }9 W( T* a. qVarian XL100 spectrometer, and the radio station was Radio San Luchino, 1 v9 P! Q, f r$ u; a6 [well known to anybody living in Bologna, which broadcasts from the top% @" Z0 y" U5 R of the nearby Saint Luca hill. 7 p8 T) p" u4 J0 N5 g

The obvious solution is to change the magnetic field, and thus / v3 w' f4 | K7 hall resonance frequencies, in order to get out of the modulation : I7 a$ e2 I: y2 R# aenvelope of the interfering transmitter. But this is not always easy,( P, u8 S# G% m( B* ^0 `- d since the range by which one can move the magnetic field changing just' Y* u) s) u( b" C; L7 r. v3 \ some software parameters is usually limited to a few tens of kHz in the3 `$ s- J& t8 X& f- ?, R frequency domain. If larger variations are required the poor engineer6 x% a4 U/ o& D l0 I4 o1 f0 f has to work on the superconducting coils of the magnet, which is a @! L8 T* t2 c, I, k8 F& Q no-trivial job entailing the risk of a total or partial quench. 0 Z& O( I! D# p/ I, n. ]0 V

Bitter experience shows that persuading the involved radio 0 X( n" D6 E$ c. o% _5 h$ Ustation to change its operating frequency is a time consuming,4 k" \, @$ Y) ]7 m: Z" Z frustrating, and apparently quite impossible task. , I0 t% z ?% M+ N3 R% [# _

Being well aware of the problem, my preliminary spectrometer7 d9 h1 M2 D3 _3 b5 c checks always include some blank acquisitions taken before running up( c) K2 @4 J9 i% \( X' j the magnet so that there is no chance to observe an NMR signal. The ! C4 x9 b0 V/ }7 n1 c: D8 j; @resulting dataset should be pure white noise, without significant 2 \. g' Z! _/ c$ L1 `5 q' zspikes. This was done also in this particular installation but, as8 B4 O# u3 ?5 I, f) z$ k usual, in the days following the energization the magnet drifted a bit, - T' q e" {( i( |getting closer to the radio station carrier. Furthermore, the usual 13C ) j( Q% q" k$ b$ c7 _! rspectral widths are quite wide which makes things even worse. Murphy's , j& K- `2 r% {% x1 x. iLaw has no exceptions! 9 l8 l2 {: X9 M8 G, ~% g3 x

But we are just at the beginning of my real troubles. Before ) V( }) \ ~. C3 c$ a7 iputting one's hands on the magnet, one should better know how much, in6 h; P, f7 ^" H7 s) @+ U which direction, should the field be moved. I have therefore used a3 @! C7 q$ ^) v good Spectrum Analyzer (Tektronix model 2710) to check the frequency' ?( \+ K) k' K: k& l spectrum around 100 MHz, ready for the worst. And the worst was what I / Z* y' }& H+ ^$ C- C1 Q/ a0 bgot! The band was filled with FM signals, evenly spaced by 250 kHz and 0 X, k; O) a) wwith modulation envelopes as wide as 100 kHz, so that when I got far# x; g9 o) x0 `9 W from one station I started receiving the next one; accounting for6 A8 f$ g; l, {; I folding and aliasing effects, there was no chance! The only somewhat $ ? p* b9 @/ u! R5 Z L8 M* lfree region was at 100,120 MHz, but this implied proton frequency of p6 K; R, V. ~398.100 MHz. So now the spectrometer is no longer a "400"! ( r3 C$ d9 h) t2 j5 f9 j+ v* T6 g: M

Before installing a spectrometer, you better get a Spectrum9 c% z" E; B5 ^# p/ ]4 `4 Z Analyzer and check for the presence of RF fields in the instrument 7 b5 i0 ]1 r2 X6 l6 ^! aroom, taking care to explore the areas close to the observe frequencies( \5 W' j+ c2 ]6 T' v/ B4 s) K; A of all the most important nuclei. Don't forget the lock: at 14 T $ `- w) K7 L$ r. I5 q `/ H(nominal 1H frequency of 600 MHz) 2H resonates at 92,095 MHz, once 2 i# R5 m, _0 u% C) G# J& ~" |; Hagain in the FM broadcast band. The lock channel receiver has quite 3 I6 D5 B+ @% \- j2 Z# k7 knarrow bandpass filters, so hitting a radio is a really bad luck, but2 u. x8 |8 o2 x+ x) M- K# X' A it had already happened, resulting in fast lock level variations and4 m9 n; H {6 z* M totally malfunctioning Gradient Shimming which uses deuterium as * y" u- i( i( S robserve nucleus! ; x+ s) a3 d! D) Y n

Needles to say, the extremely high sensitivity of an NMR 2 A( O: I3 ?1 U# Z0 o5 R% k' D3 HSpectrometer shows up. The signal from the guilty radio, as observed on2 R+ c5 P5 x: k: j the spectrum analyzer inside the spectrometer room, had very low; m4 H6 d6 e. h8 y$ H" T: M intensity level of about -70 dBm, some microvolt/meter, but that was 4 ?4 t& O4 _0 L" @( cenough to almost completely hide the quite strong 13C signal from the " G) M$ ^4 f6 VASTM sample! 1 v! ^4 \- l: R/ l

The radio was clearly picked up by the Probe (closing the% ~! d/ j7 n" C) t9 X Preamplifier input with a shielded 50 ohm RF load, all signals" E, t- q$ [# u disappear) but, quite surprisingly, there is almost no shielding effect / e s7 B- _* T4 {attributable to the metal body of the magnet, which is after all an ( u! d/ [% v: A' ~! [6 c9 }( W8 palmost completely closed cylinder all around the Probe. Most probably a 5 z3 W0 L; H, f# r8 w" rgood deal of the signal leaks in through the Shim Coils which are 9 \9 Z i3 ~% \1 fmounted very close to the Probe and, together with their connection ! a0 q+ L8 g2 S+ S; G% ^ [* ~# f/ ^cables to the Console, constitute a quite good antenna. 8 S2 o7 X% K5 z% _$ A# h( E& F

Too bad the Shim Coils are essential, and effective shielding 9 |9 z* i9 j% J' Dof the instrument with a Faraday's cage is always difficult and f; f$ B1 K7 s: ?* _1 S5 N expensive (it may be almost impossible once the spectrometer is & A( N1 A/ Y+ U: E* g' O: c" Hinstalled).! O8 U/ z; `9 z; [, ~

; `& A, {# ^$ J' v5 g' } Before concluding, let me venture some additional advice based on my experience: 1 F% g$ @: A' n j! D" y3 u

! T5 e- `6 O0 x% Y = Install the spectrometer in the best shielded room x; q' ~! `2 E3 I1 p* G0 |' c you can get; the best choice is once again in the basement, where you! \ G3 X9 \2 u1 ^3 M/ O have the whole building above the ceiling and its [grounded]( G: P- A# r( c5 J. B foundations all around the rest, done in iron-reinforced concrete, ) \& J) c) E, J( B1 W9 oamounting to a good Faraday's cage at no extra cost. " X# R/ J$ n% h+ [4 r

! s, V! F. }; z* I = If possible, avoid top floors. If you can't avoid8 q; P i, Q Q" A# P) k going upstairs, take a good look out of the window: if you see nearby * v( h5 h" I0 A5 ^+ x% L' P( ttransmission antennas, get ready for troubles proportional to their ' z1 e0 @/ T- }. s2 [" \* o/ s! g+ f# Ddimensions and closeness (to my knowledge, however, mobile telephony * R% G" y' ?) G+ B; i+ w" t$ }antennas cause so far no harm).; U% c5 ]9 K% h- v0 @# c+ x

) P1 E8 L$ e1 T R7 u# a = I'm sure that an exchange of experiences and/or [# ]2 n. `: }( x6 z2 A suggestions regarding this matter would help a lot to solve many# i& k, C' ~+ J1 d% A- a5 k 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.2 S' u! ?+ E: c) V9 w$ `0 ` | E

5 R$ K8 E3 \% b5 A `2 _, z Vanni 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
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