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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.. A! }6 ^* L: l8 K$ Q This applies to all kinds of spaces, including the electromagnetic! f2 @1 ?1 E2 l5 G& I4 K& F ether. What follows is a contribution and a warning from Vanni Piccinotti, : X/ b+ k* _5 O$ d! u0 Q- c: Nan engineer based in Florence, Italy, who has decades of experience / Z: {, U0 i$ U2 h% q' Ywith installing, testing, and servicing NMR and EPR spectrometers. The 6 F/ ?: {1 z8 Y6 A" I* ^& aproblem of RF interference has never been trivial and it keeps slowly7 s: f* N( C V but inexorably mounting. The spread of urban areas (combined with the ' s6 Q4 K3 f0 `2 m" W- g/ z9 G Z: qtendency to install MR instruments in those same areas) and the & j# \( Q1 Y# J+ x! J; p& Qmounting maze of wireless technologies penetrating our daily life spell5 T7 D. i+ l# p4 ~* K$ F nothing good for the future quality of our NMR signals. With concurrent & R! d i | i- o1 l" a# p" Cprogress in basic sensitivity of the instruments, time might come when+ [+ Y9 D: x9 l% i environmental RF noise will be the single major obstacle to further7 e3 H( Q; K* D) O2 r* N# Q6 Z, k 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
 

. k& W& [+ O- Y Cross-talk between FM Broadcast Radio Transmitters (88-108 MHz)" G1 y4 @$ D: d) N9 K! [) ` and NMR Spectroscopy: A recent experience, _, `* C H8 [# n3 I) x: u" P

! d7 `9 E# M) i. X {7 b, r Recently I had to install a 400 MHz (9.4 T) NMR Spectrometer. The+ n% F" _: u" }% O9 f9 ` system worked fine and, using an Indirect Detection Probe , met quickly , X" X$ o& }" H r# }and effortlessly the specifications. But later on, when the customer 9 Q$ n% r' H {installed a 13C direct detection Probe, the S/N ratio turned out to be * P$ C# O" E4 b5 H# x, P& rquite low and, on top of it, the sensitivity was subject to erratic and% S2 l) t$ c0 Q f9 k% h8 M very large variations from 50:1 to 130:1 (manufacturer's specs give ! u" c( Z% b" b155:1), without any apparent reason.0 I- S3 O" Y4 K' w, [! }# Q

Since the nominal 13C observe frequency at 9.4 T is 100,568 ) ^( G# g" {8 BMHz, right in the middle of the range of commercial FM broadcasts, I 9 l. w3 m/ m( c/ j7 X1 v$ }have immediately suspected that the spectrometer was picking up one of % z6 ^, C' i8 I2 Vthose radio stations. In fact, using a cheap FM radio receiver, a2 ^! R* o2 g6 e/ Z strong station was quickly found at 100,60 MHz. At this point, I have! C% Z/ m4 V7 R# L9 Z" T# C9 K connected a simple audio amplifier ending with a loudspeaker to the w2 M) S" A' M0 @1 N output BNC of the observe receiver which was there apparently just for4 g u$ Z7 R; t4 q1 M! w this purpose, and all of us were listening to the radio using a 200.000 - W/ Y9 f @ \3 eEuro NMR spectrometer, except that the audio quality was really poor,5 j) E! g/ I' ~: I4 p0 P9 f much worse than from the above-mentioned gadget radio (a shopping mall 3 V. G; D6 a1 u- o- T" B" ?3 o' }gift).# @1 _2 m8 k# ^, w

The problem is well known from the old times, when the highest $ k8 Z% u; V% i" Q/ S( b5 b% {1 rfield was 2.45 T and the nominal H1 frequency was close to 100 MHz. One 1 X5 p" @8 W" [0 Oof the first Italian NMR spectroscopists to experience it, back in & Y( u" A' _/ R! @1974, was Prof. L.Lunazzi at University of Bologna, on his brand new& E; `7 |: o# u6 K5 K Varian XL100 spectrometer, and the radio station was Radio San Luchino,! l! H" n" w- r! a' l well known to anybody living in Bologna, which broadcasts from the top % v( V: g6 K# n+ l+ Mof the nearby Saint Luca hill. - ^0 K, Z/ b, _3 N. Z" u

The obvious solution is to change the magnetic field, and thus 1 r+ ?' ^! G7 n3 [, nall resonance frequencies, in order to get out of the modulation 2 @, N' V* S! c) w7 ~envelope of the interfering transmitter. But this is not always easy,- D7 ^9 o" b1 L) t/ V since the range by which one can move the magnetic field changing just( r8 y9 Q6 G( [% T% `( r$ m6 v/ B5 b some software parameters is usually limited to a few tens of kHz in the* x4 X' S% W" x% t frequency domain. If larger variations are required the poor engineer, c" @" ~% ]) f/ ^& b5 q has to work on the superconducting coils of the magnet, which is a 6 y5 o( |7 F/ ]! @no-trivial job entailing the risk of a total or partial quench.. `8 w P x: A- ]4 \5 L; {

Bitter experience shows that persuading the involved radio- [5 o* R4 m( g6 G5 ?$ B8 R station to change its operating frequency is a time consuming,3 G/ o! ?9 j: q frustrating, and apparently quite impossible task.! K3 h5 {# b+ U

Being well aware of the problem, my preliminary spectrometer 3 I/ z. V) K6 Ychecks always include some blank acquisitions taken before running up3 k1 C2 S9 b/ {5 l the magnet so that there is no chance to observe an NMR signal. The F8 l/ a- x8 z& a" ^ resulting dataset should be pure white noise, without significant & `+ k1 e( c6 Y5 H$ P. K3 nspikes. This was done also in this particular installation but, as ( i- d5 P! h) h- Xusual, in the days following the energization the magnet drifted a bit, # J! X# J) l0 l9 S# q' m) q, ~% pgetting closer to the radio station carrier. Furthermore, the usual 13C 6 ]! x( ^% N8 ospectral widths are quite wide which makes things even worse. Murphy's ! S/ e7 b: b1 e8 YLaw has no exceptions!& l! E6 b# K W5 G% s! i

But we are just at the beginning of my real troubles. Before8 n* [: h1 j) M4 o putting one's hands on the magnet, one should better know how much, in ( E- _+ g( a0 A p1 Y5 rwhich direction, should the field be moved. I have therefore used a1 t9 O* @/ b9 s$ S4 G: d good Spectrum Analyzer (Tektronix model 2710) to check the frequency ) U0 i; @# M2 Q0 l/ [3 Y( F) dspectrum around 100 MHz, ready for the worst. And the worst was what I& v% ]4 J' w; H. \* b) d) A got! The band was filled with FM signals, evenly spaced by 250 kHz and ( z" |8 a( o. \2 T" `with modulation envelopes as wide as 100 kHz, so that when I got far: d+ V' i! U6 j6 i3 [ from one station I started receiving the next one; accounting for % M9 W6 S6 V/ X1 C# Afolding and aliasing effects, there was no chance! The only somewhat $ k, e% F8 z4 D g, ofree region was at 100,120 MHz, but this implied proton frequency of0 M" c0 A; n4 c F. U 398.100 MHz. So now the spectrometer is no longer a "400"! 8 Y( M# F1 i& G: j

Before installing a spectrometer, you better get a Spectrum! ^3 V$ c4 a3 v5 Z Analyzer and check for the presence of RF fields in the instrument* Y' Z" a: P3 T' M room, taking care to explore the areas close to the observe frequencies & d/ v, ]" n4 H( sof all the most important nuclei. Don't forget the lock: at 14 T" S5 \5 w7 @ q: ?1 r5 j% T (nominal 1H frequency of 600 MHz) 2H resonates at 92,095 MHz, once! n# m* W! L6 P6 u7 I again in the FM broadcast band. The lock channel receiver has quite) _, {: t. m1 J9 t7 G narrow bandpass filters, so hitting a radio is a really bad luck, but 3 t9 ], J8 E# D' G$ Hit had already happened, resulting in fast lock level variations and 1 Q+ D9 k. d' }totally malfunctioning Gradient Shimming which uses deuterium as# ]- _9 Q+ A# _5 g$ r! B: L observe nucleus! $ a' I7 d3 e5 W3 u

Needles to say, the extremely high sensitivity of an NMR - j0 k3 j) Y8 T1 V8 @. c1 |Spectrometer shows up. The signal from the guilty radio, as observed on % C4 A4 a5 d2 g# J. Dthe spectrum analyzer inside the spectrometer room, had very low 1 F d$ @ n) d5 n. Z* @4 T) m3 c: ?intensity level of about -70 dBm, some microvolt/meter, but that was9 R$ N5 g) W6 f) ^; m- N, _# N enough to almost completely hide the quite strong 13C signal from the! z8 N; t) I' p ASTM sample!# ?8 B9 ?+ ^' @4 j7 ^$ \

The radio was clearly picked up by the Probe (closing the 7 C7 @! H" w/ D3 f& sPreamplifier input with a shielded 50 ohm RF load, all signals) H+ v; E" P' e disappear) but, quite surprisingly, there is almost no shielding effect$ k' w5 r W; P. q- v) | attributable to the metal body of the magnet, which is after all an d7 A6 W( { R* N: E2 Malmost completely closed cylinder all around the Probe. Most probably a8 b, h. l, }/ _" E, h \ good deal of the signal leaks in through the Shim Coils which are0 |9 M! j& l/ `; W7 F7 Z/ o! x mounted very close to the Probe and, together with their connection! x% H. n# ~/ t cables to the Console, constitute a quite good antenna. % W+ Q- J+ H9 H

Too bad the Shim Coils are essential, and effective shielding; b' S" C5 q n7 U of the instrument with a Faraday's cage is always difficult and; z2 i- V6 s: O9 h expensive (it may be almost impossible once the spectrometer is$ \9 F! @: h& d0 S+ t8 M- m/ y installed). ) m, I- I7 U1 r6 \* z

: K* g* A5 h' Y7 BBefore concluding, let me venture some additional advice based on my experience: - U! k* i* j5 ?& A

2 [* I# K( Z- I( N) m& }5 z= Install the spectrometer in the best shielded room . F; S9 Q- f1 m$ P" z+ A3 }" ^you can get; the best choice is once again in the basement, where you $ e% K6 t/ Q. U5 k, Jhave the whole building above the ceiling and its [grounded] 9 R- D; L# E" L! xfoundations all around the rest, done in iron-reinforced concrete, " `) R+ y. [ @: a1 c$ B7 ramounting to a good Faraday's cage at no extra cost.. c& ^1 c, h- d7 o5 @; R

7 d9 p# m7 B# \5 y( m5 }; E = If possible, avoid top floors. If you can't avoid # c! B& _% `+ kgoing upstairs, take a good look out of the window: if you see nearby 1 t' B# K' B- o6 z; o6 d+ Qtransmission antennas, get ready for troubles proportional to their 4 v) _& K2 `/ |2 J7 L* }) idimensions and closeness (to my knowledge, however, mobile telephony . k9 C% U7 ^3 Q1 tantennas cause so far no harm).# V3 V6 {& [0 k3 K1 [. p5 }& B

# {3 n6 @% Q8 N& x= I'm sure that an exchange of experiences and/or# l4 q& U8 I' K* g5 {2 A H, v suggestions regarding this matter would help a lot to solve many 2 Z* B5 u& n+ ^4 S( N$ T, B3 eexisting 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. . ] D3 m# D6 y# h3 I6 a

. l9 H. ?# Q6 `' Q( q: {1 f3 S( \ 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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