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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.. E8 n6 D6 l* z% j6 a2 h This applies to all kinds of spaces, including the electromagnetic $ B/ T6 \# _& U# wether. What follows is a contribution and a warning from Vanni Piccinotti, : B" g+ |' B; N9 Man engineer based in Florence, Italy, who has decades of experience4 Y. z0 s! ~% n* _% x( g1 o) u with installing, testing, and servicing NMR and EPR spectrometers. The! i$ h( ]) s( a problem of RF interference has never been trivial and it keeps slowly , g: e. R" W7 C3 E1 @2 Nbut inexorably mounting. The spread of urban areas (combined with the2 F# ?) E/ _* E tendency to install MR instruments in those same areas) and the 2 t$ v( [. y) d7 \1 umounting maze of wireless technologies penetrating our daily life spell - M- C }- u; J1 T1 U' Dnothing good for the future quality of our NMR signals. With concurrent* v; G) ^0 P/ z. R; H; K$ i% R progress in basic sensitivity of the instruments, time might come when# e1 Y: f/ g0 H) ^3 Z3 D1 W, e environmental RF noise will be the single major obstacle to further i1 b4 k3 M2 ]) t 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
 

- _( S. H# X' ~- i Cross-talk between FM Broadcast Radio Transmitters (88-108 MHz)4 A9 h, a4 q# h, y. O$ U and NMR Spectroscopy: A recent experience. {6 |' Y' ]& J: w/ z' T

3 o: @: @+ M, j$ Y/ c% v, NRecently I had to install a 400 MHz (9.4 T) NMR Spectrometer. The- @1 w: V7 O- f' m3 P+ o system worked fine and, using an Indirect Detection Probe , met quickly! C. h7 y, O0 m, B; Z8 Y and effortlessly the specifications. But later on, when the customer 0 ^, ]2 C: `/ ^ W/ binstalled a 13C direct detection Probe, the S/N ratio turned out to be& F2 z- ]) z5 ]; R" E quite low and, on top of it, the sensitivity was subject to erratic and 3 R. ~7 R2 Q7 [6 F* B9 wvery large variations from 50:1 to 130:1 (manufacturer's specs give4 C1 S& Z: C* \; w$ l 155:1), without any apparent reason.2 a7 [5 G& x" o6 L

Since the nominal 13C observe frequency at 9.4 T is 100,568* F1 D4 U* d Y1 Y. G MHz, right in the middle of the range of commercial FM broadcasts, I s& ?" F3 W# I# v6 ^have immediately suspected that the spectrometer was picking up one of 0 s+ f2 E$ \8 A* `+ athose radio stations. In fact, using a cheap FM radio receiver, a , R1 ~" Y6 _" Z( Y6 I' Z/ l- M# nstrong station was quickly found at 100,60 MHz. At this point, I have , E* S! G/ d" m1 m6 ~8 vconnected a simple audio amplifier ending with a loudspeaker to the2 Y& _$ G5 H A) Y' v output BNC of the observe receiver which was there apparently just for ; n4 v8 Z6 o+ hthis purpose, and all of us were listening to the radio using a 200.000# `$ j: S0 G- S Euro NMR spectrometer, except that the audio quality was really poor,; D; X2 V7 |3 E% m) y) F. x( | much worse than from the above-mentioned gadget radio (a shopping mall : I( E5 W4 G, A! a' v8 mgift).# v/ W8 P0 z5 v1 i: n

The problem is well known from the old times, when the highest% B5 P, v7 p2 u- s1 t9 N: k8 ` field was 2.45 T and the nominal H1 frequency was close to 100 MHz. One 5 I! Q! \3 \' J8 O+ ?of the first Italian NMR spectroscopists to experience it, back in, Q# y0 L- H, M, N. c 1974, was Prof. L.Lunazzi at University of Bologna, on his brand new& [5 B2 I9 K" ~ Varian XL100 spectrometer, and the radio station was Radio San Luchino, / x; W. Z; N. P ~well known to anybody living in Bologna, which broadcasts from the top8 L: ?; h. U: Y! M* r- c% L of the nearby Saint Luca hill. 9 `9 v* V/ ^2 f. n

The obvious solution is to change the magnetic field, and thus 9 M( [) f! T8 Q; c5 @all resonance frequencies, in order to get out of the modulation 8 g4 j. J9 S b3 V9 nenvelope of the interfering transmitter. But this is not always easy, * F0 K$ u# j- |& i2 R+ n( x$ N1 _since the range by which one can move the magnetic field changing just / G3 q7 ?1 ^3 M! O/ E+ \some software parameters is usually limited to a few tens of kHz in the 5 D4 L7 O+ i f; pfrequency domain. If larger variations are required the poor engineer ; a5 s- E0 f3 N* L' g" c, @. hhas to work on the superconducting coils of the magnet, which is a * H1 J4 Y( b1 R, ?) n# U: ano-trivial job entailing the risk of a total or partial quench.' ]) z' l i4 f' d0 W& k, e

Bitter experience shows that persuading the involved radio $ {8 ?/ [, R/ M8 ]: xstation to change its operating frequency is a time consuming,9 F+ v, J i7 n( r* } frustrating, and apparently quite impossible task.: M# B" D- x9 x( w6 P, O

Being well aware of the problem, my preliminary spectrometer! Y+ y& ?1 e8 z: g3 f; [/ A checks always include some blank acquisitions taken before running up, f4 t) A2 U1 b: [ the magnet so that there is no chance to observe an NMR signal. The - z" m9 Z" O) a' w2 F1 N* Kresulting dataset should be pure white noise, without significant ' I& r. L5 \ D7 }spikes. This was done also in this particular installation but, as, s$ \7 p$ }: S5 U) i usual, in the days following the energization the magnet drifted a bit,$ [ Y) t! `$ x) b' j/ C! |; Y getting closer to the radio station carrier. Furthermore, the usual 13C- _0 k' k* [% \ spectral widths are quite wide which makes things even worse. Murphy's8 H, N; u( r O2 Y$ q Law has no exceptions! ( G- ?4 W: g& K6 H& E; o, E

But we are just at the beginning of my real troubles. Before8 ]' P* o P) b: s putting one's hands on the magnet, one should better know how much, in . \) u0 ^% W E9 v3 owhich direction, should the field be moved. I have therefore used a' s/ P, H# B7 y good Spectrum Analyzer (Tektronix model 2710) to check the frequency) c+ C! Z! X4 M spectrum around 100 MHz, ready for the worst. And the worst was what I 6 Y4 Q6 A8 v" o. D: ] h7 qgot! The band was filled with FM signals, evenly spaced by 250 kHz and! U* I+ J" J, ?# r& G with modulation envelopes as wide as 100 kHz, so that when I got far% a; F+ c, D8 p; A( x* ] from one station I started receiving the next one; accounting for 6 |' ~- g$ M& w; _2 D7 gfolding and aliasing effects, there was no chance! The only somewhat' u( j0 D! j/ Q1 r. L8 Z( X free region was at 100,120 MHz, but this implied proton frequency of8 V6 Q7 \) v' _6 y 398.100 MHz. So now the spectrometer is no longer a "400"!1 Y; v9 o7 u0 L( J3 U! P. _) j1 D/ d: C

Before installing a spectrometer, you better get a Spectrum : s& }3 Z" [, A: P7 u3 V% NAnalyzer and check for the presence of RF fields in the instrument 9 L$ J& H7 i( f5 A) Jroom, taking care to explore the areas close to the observe frequencies7 J- T( f. S& r# ], h of all the most important nuclei. Don't forget the lock: at 14 T9 q- d6 d* s4 j5 x$ l" i (nominal 1H frequency of 600 MHz) 2H resonates at 92,095 MHz, once3 B2 v6 Z. x- U; @" _ again in the FM broadcast band. The lock channel receiver has quite + j, A, K# a* enarrow bandpass filters, so hitting a radio is a really bad luck, but ) o* Y, Z8 |- {; j0 q4 Iit had already happened, resulting in fast lock level variations and: \* e6 J! d' f u- u totally malfunctioning Gradient Shimming which uses deuterium as4 C% U$ h8 C7 e0 N! O, B observe nucleus!" f3 G5 m# W' L4 F$ v" v

Needles to say, the extremely high sensitivity of an NMR ; E9 p% j) H+ Y. Y& Y6 P( iSpectrometer shows up. The signal from the guilty radio, as observed on " E$ w9 s) U/ kthe spectrum analyzer inside the spectrometer room, had very low9 I6 k# `4 x: x+ O3 A! z w3 C intensity level of about -70 dBm, some microvolt/meter, but that was / x2 u& ?. `- s0 oenough to almost completely hide the quite strong 13C signal from the! |" K* t: r- N5 z/ z ASTM sample!" o) k: E0 C- F8 w, j9 _6 [

The radio was clearly picked up by the Probe (closing the6 c0 a3 Y% j4 X; {- \ Preamplifier input with a shielded 50 ohm RF load, all signals - w u4 \- J: i; h; y' sdisappear) but, quite surprisingly, there is almost no shielding effect " [5 c" y e- H; Q# B6 {; X5 T/ `attributable to the metal body of the magnet, which is after all an . y f8 q; }& f$ Z- O8 U+ m0 i: jalmost completely closed cylinder all around the Probe. Most probably a7 B; @3 A9 D7 G& E v1 v( Y' N good deal of the signal leaks in through the Shim Coils which are- D& e: n9 C7 E) S& }& n4 m mounted very close to the Probe and, together with their connection5 I |- k5 Y9 A+ q, c( } cables to the Console, constitute a quite good antenna. * c7 ~2 J' ~! `7 x R; F

Too bad the Shim Coils are essential, and effective shielding s5 R' ? b6 b1 ^! R of the instrument with a Faraday's cage is always difficult and 8 X0 Y% X- A% R2 D4 q" qexpensive (it may be almost impossible once the spectrometer is6 |9 I* m& G1 K installed).. e& L5 j0 r5 ?+ m

9 Y+ y; ?' H' B* rBefore concluding, let me venture some additional advice based on my experience: ( @4 Q. y7 ]- ~, q. o

- l4 Y8 s0 _, _' q) z, G m= Install the spectrometer in the best shielded room% ]' S8 T0 k) Y3 i* B: F* H* k( c you can get; the best choice is once again in the basement, where you 7 p+ v5 ]# w+ h/ h6 Lhave the whole building above the ceiling and its [grounded]) E2 L# }8 G2 W. K& v' R. r z foundations all around the rest, done in iron-reinforced concrete,( P2 ]. z. R# M/ j6 G: |* H3 G amounting to a good Faraday's cage at no extra cost. 9 e5 @5 [* I Z8 C6 X; j8 O

( U% M6 q" G9 z' q) I- y = If possible, avoid top floors. If you can't avoid# X5 t: [2 [% N( V4 D! r4 k, J9 Y" h going upstairs, take a good look out of the window: if you see nearby $ S+ Y1 y# V; ^3 Itransmission antennas, get ready for troubles proportional to their 6 h! n4 X V/ w- ~3 s5 L. r7 Ddimensions and closeness (to my knowledge, however, mobile telephony3 {- N# W+ n& }% o; d V& l antennas cause so far no harm).& m7 G: m' J2 W+ ?2 \' V

J: \2 e6 i& c; Y% k# Z2 F= I'm sure that an exchange of experiences and/or/ R( ~* o3 S+ M @8 G4 y suggestions regarding this matter would help a lot to solve many & R- n8 \# c# M: N8 \8 ?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. ; c# i& V/ z5 f1 S; [

" m, J% t; ?6 Q ]7 L! T1 i 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
see see!
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