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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. 0 T3 m, ^; M! e3 C% I. |, l$ h$ W$ qThis applies to all kinds of spaces, including the electromagnetic 2 N" D$ m$ y3 e- ?ether. What follows is a contribution and a warning from Vanni Piccinotti,% m9 a L) i, q* | an engineer based in Florence, Italy, who has decades of experience; J2 @/ ^9 v' m9 g" ^6 ? with installing, testing, and servicing NMR and EPR spectrometers. The# \( K) h3 u, O+ y problem of RF interference has never been trivial and it keeps slowly, e5 a' A% a: I# g* Z1 R; r" l4 a- ` but inexorably mounting. The spread of urban areas (combined with the ! g8 U. d0 N' T4 p7 |* gtendency to install MR instruments in those same areas) and the9 A/ I9 I3 K2 a5 P% l9 |( y A: J mounting maze of wireless technologies penetrating our daily life spell' G% c2 y% g8 y nothing good for the future quality of our NMR signals. With concurrent; w3 L6 }, I3 e2 n progress in basic sensitivity of the instruments, time might come when n" K" F- f4 R, l5 nenvironmental RF noise will be the single major obstacle to further1 z# s, Z% a: u" L* e0 ] 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
 

0 M; @5 S+ f6 S9 SCross-talk between FM Broadcast Radio Transmitters (88-108 MHz) 2 M/ V& J9 S' R2 S5 u" R6 xand NMR Spectroscopy: A recent experience3 i; i; x7 f: j' U" F

5 L$ } W1 g* G' QRecently I had to install a 400 MHz (9.4 T) NMR Spectrometer. The ' ^# P, X* C# d# I2 y9 P# wsystem worked fine and, using an Indirect Detection Probe , met quickly. U* \$ H, A9 U- n5 i and effortlessly the specifications. But later on, when the customer 8 E% w4 z9 S& P" g7 A+ ainstalled a 13C direct detection Probe, the S/N ratio turned out to be % I: z5 O7 _1 d" ?; ^quite low and, on top of it, the sensitivity was subject to erratic and7 e! Q6 @2 p# U4 R1 `$ ^ very large variations from 50:1 to 130:1 (manufacturer's specs give6 X4 j, o- A( Y- [) |9 j1 h: a 155:1), without any apparent reason.' _. U' G: I3 w& G( p3 l3 y# s7 y

Since the nominal 13C observe frequency at 9.4 T is 100,5684 P& }: a8 p1 p9 }5 m5 I0 A MHz, right in the middle of the range of commercial FM broadcasts, I 4 ~3 D; S. @6 j, shave immediately suspected that the spectrometer was picking up one of) N0 \' E! G, ~+ h$ j those radio stations. In fact, using a cheap FM radio receiver, a - T0 n9 L& v+ I$ _1 d2 t# @. vstrong station was quickly found at 100,60 MHz. At this point, I have . Z# V: F' T$ P# W2 U% n1 ~connected a simple audio amplifier ending with a loudspeaker to the ; S3 g9 }* H9 _6 b$ koutput BNC of the observe receiver which was there apparently just for W. z y" V9 Zthis purpose, and all of us were listening to the radio using a 200.000 / ]6 h j8 y4 P5 L, d& oEuro NMR spectrometer, except that the audio quality was really poor,& P+ r' m" \* R' ~, G) k) Z8 {6 D' B, [( N much worse than from the above-mentioned gadget radio (a shopping mall! Z" ^2 l4 r* l/ `0 | gift). # Y* |' a9 ^% Y6 |, c: J

The problem is well known from the old times, when the highest e* K" ~! \0 q; d- Lfield was 2.45 T and the nominal H1 frequency was close to 100 MHz. One2 G* c* w1 c! ] c4 w1 v of the first Italian NMR spectroscopists to experience it, back in& J! ]+ f2 J5 N! ^* C 1974, was Prof. L.Lunazzi at University of Bologna, on his brand new . t# r3 C2 C! Z8 x/ c# ?Varian XL100 spectrometer, and the radio station was Radio San Luchino,/ _4 i- |7 A0 ]: v1 [+ j+ S' c well known to anybody living in Bologna, which broadcasts from the top7 i4 N8 }& n; p6 z9 f2 R& I+ B/ } of the nearby Saint Luca hill.4 h% c% V5 t6 s! w8 r

The obvious solution is to change the magnetic field, and thus 6 q e# q( e9 D2 x0 Y6 {6 oall resonance frequencies, in order to get out of the modulation 6 u! v/ f5 `6 A: w1 |% T4 z1 Lenvelope of the interfering transmitter. But this is not always easy, 2 G# _; m& c3 @since the range by which one can move the magnetic field changing just ) J' V9 A T: V1 `# F& S# d) Y9 vsome software parameters is usually limited to a few tens of kHz in the+ _2 V, i1 _; T/ B frequency domain. If larger variations are required the poor engineer " k9 r5 r& S$ `8 ?3 l/ g6 I. khas to work on the superconducting coils of the magnet, which is a" L6 O' \0 ^ o& |* p6 @0 J no-trivial job entailing the risk of a total or partial quench. 5 \. a c5 k; H3 c0 C7 w, n

Bitter experience shows that persuading the involved radio ?& E# u6 O# t; n" V. Zstation to change its operating frequency is a time consuming, ' c6 T+ K9 C) l7 m7 Nfrustrating, and apparently quite impossible task.3 b- t# e- n; x: [ T# M

Being well aware of the problem, my preliminary spectrometer/ P5 c B. b. r# p" d( G1 c checks always include some blank acquisitions taken before running up " h3 W0 q# U6 P; c2 O# l2 j( xthe magnet so that there is no chance to observe an NMR signal. The 7 M: d" h2 }7 h# O5 Y5 lresulting dataset should be pure white noise, without significant 9 l7 ~/ _6 ^" Y+ Gspikes. This was done also in this particular installation but, as# N- I. l: ^( _/ {, y usual, in the days following the energization the magnet drifted a bit,$ j2 _! T( _+ q0 `" k getting closer to the radio station carrier. Furthermore, the usual 13C n; o, O7 {; {spectral widths are quite wide which makes things even worse. Murphy's, f) f& f( O/ y/ ^7 ?8 @# \1 i O4 ] Law has no exceptions!! S# { q9 U& c+ [7 }2 A

But we are just at the beginning of my real troubles. Before* }8 d3 p/ x, ^, `- W putting one's hands on the magnet, one should better know how much, in 9 t" U7 i4 A5 C3 k- bwhich direction, should the field be moved. I have therefore used a ( b8 O' a }+ c% kgood Spectrum Analyzer (Tektronix model 2710) to check the frequency 4 z% m, a& z ]! q& q: @$ ^2 Kspectrum around 100 MHz, ready for the worst. And the worst was what I 0 ^! c* ^* J8 z d" @got! The band was filled with FM signals, evenly spaced by 250 kHz and- e3 k2 Q3 H | with modulation envelopes as wide as 100 kHz, so that when I got far3 k: Q/ g/ d0 E! J from one station I started receiving the next one; accounting for ' W' _* K) [! D4 o) qfolding and aliasing effects, there was no chance! The only somewhat2 |' [9 K2 ^! ~& y& a free region was at 100,120 MHz, but this implied proton frequency of 9 F* H+ h+ |4 J, i" ~1 W% ^6 J+ z398.100 MHz. So now the spectrometer is no longer a "400"! 6 S% ~( T$ ]) W

Before installing a spectrometer, you better get a Spectrum # x, p" ?1 D. y% q) a8 E2 V) gAnalyzer and check for the presence of RF fields in the instrument 0 g- O0 U0 j% z; i3 a* Wroom, taking care to explore the areas close to the observe frequencies5 L* _8 s" ~" e$ m; d8 ^ of all the most important nuclei. Don't forget the lock: at 14 T * X3 ?* B6 l+ u& V(nominal 1H frequency of 600 MHz) 2H resonates at 92,095 MHz, once; R6 D1 f7 L) U+ W! Q3 _ again in the FM broadcast band. The lock channel receiver has quite 2 y4 Q0 }: d, t; d% Y" u# Qnarrow bandpass filters, so hitting a radio is a really bad luck, but . }8 j# V( x! d9 u; @it had already happened, resulting in fast lock level variations and8 S3 E" a# r7 a- I9 M5 [! l totally malfunctioning Gradient Shimming which uses deuterium as. d# S0 Y; h( Q2 k1 [/ M observe nucleus! 9 [; d9 {* O1 ^5 Q

Needles to say, the extremely high sensitivity of an NMR 9 r. t. A, i0 D0 ?9 R9 g2 aSpectrometer shows up. The signal from the guilty radio, as observed on" \' H2 M0 @3 n- H; R) q V the spectrum analyzer inside the spectrometer room, had very low ' ]+ f$ i( x) p) J8 U+ sintensity level of about -70 dBm, some microvolt/meter, but that was H6 J- V# Q. k2 x5 p enough to almost completely hide the quite strong 13C signal from the5 b+ `+ W s, L/ Y+ | ASTM sample! $ J) H9 h4 O! q' s

The radio was clearly picked up by the Probe (closing the! X" Y! o0 U- h5 m( J4 P# j, w Preamplifier input with a shielded 50 ohm RF load, all signals; `% t4 z: d$ H disappear) but, quite surprisingly, there is almost no shielding effect6 s- V4 d8 E: t$ V2 x attributable to the metal body of the magnet, which is after all an - c1 R0 h* s* D- U* d2 F" ?almost completely closed cylinder all around the Probe. Most probably a. g R7 i" _! K; P, W5 e; s% K good deal of the signal leaks in through the Shim Coils which are # _6 q$ Z4 X/ e+ Xmounted very close to the Probe and, together with their connection+ X# A7 p) d+ _2 u cables to the Console, constitute a quite good antenna.1 N4 U8 W6 K& Z; J

Too bad the Shim Coils are essential, and effective shielding9 h5 [/ I0 N. N1 C of the instrument with a Faraday's cage is always difficult and & N! k: z1 | @8 G mexpensive (it may be almost impossible once the spectrometer is 9 L$ T: E+ @6 B; \( tinstalled). ]- ^! f- T+ T* o

# L/ R/ v' s$ U4 M, L2 E Before concluding, let me venture some additional advice based on my experience: : _4 n1 I/ F. B' I& C. N7 \

7 C' e O) @! a! `; u3 } = Install the spectrometer in the best shielded room/ T0 r1 v5 \3 D: X you can get; the best choice is once again in the basement, where you ; o) F, _2 S2 D! X, qhave the whole building above the ceiling and its [grounded]) U, q5 t6 L" o. R) o* W foundations all around the rest, done in iron-reinforced concrete, ; `# a! `* o) B: ?! ?amounting to a good Faraday's cage at no extra cost.8 {# Z6 J0 Y" e. t. E1 f8 h

0 c) Y- i* w+ C4 H9 Q= If possible, avoid top floors. If you can't avoid x7 n9 e0 |6 v6 C# i' x( `going upstairs, take a good look out of the window: if you see nearby % T, x4 a) K$ i: Ztransmission antennas, get ready for troubles proportional to their0 o" ^& B; W& | dimensions and closeness (to my knowledge, however, mobile telephony$ D, P$ z; i+ ]# u; R! E4 A antennas cause so far no harm).5 n6 c0 K/ v& v0 Q, t% f4 ?

" ]3 Z% ?/ q) ~6 ~7 j! u: A Z& C = I'm sure that an exchange of experiences and/or+ O0 G! T# T+ z$ O$ v1 q suggestions regarding this matter would help a lot to solve many ! \' S( O% K. a. Lexisting 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 Q3 U; T; A% U# p! @7 g

8 X0 z" G7 C! Y) D/ _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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