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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 R% Y& I, ^, Z' A0 V o% }4 ] This applies to all kinds of spaces, including the electromagnetic6 G W* J8 `# i5 E% Z8 c ether. What follows is a contribution and a warning from Vanni Piccinotti, % p0 q2 L- [, t- P& ban engineer based in Florence, Italy, who has decades of experience 9 C' l5 X% N! Fwith installing, testing, and servicing NMR and EPR spectrometers. The ( Z q! `: ]% i8 I) yproblem of RF interference has never been trivial and it keeps slowly0 y: M7 i S0 | but inexorably mounting. The spread of urban areas (combined with the3 i; B/ T/ v! N' e) n- h9 o tendency to install MR instruments in those same areas) and the 6 `( J9 t: d8 ^! V7 P/ s% nmounting maze of wireless technologies penetrating our daily life spell / ~: ~" K, u0 o/ Anothing good for the future quality of our NMR signals. With concurrent) @8 L( U3 f2 [# P- ]: G& g progress in basic sensitivity of the instruments, time might come when. h1 y6 w W3 _( B, f% a# u environmental RF noise will be the single major obstacle to further # n! o: h3 u: Z8 I8 m. e" H6 tprogress. 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
 

+ p* U9 g: x, e" ]8 H Cross-talk between FM Broadcast Radio Transmitters (88-108 MHz)8 ^. ]: q8 _5 U# o and NMR Spectroscopy: A recent experience& |: M/ F+ u; w0 o! q9 r

9 [8 p, v5 k0 y2 ?! `7 t Recently I had to install a 400 MHz (9.4 T) NMR Spectrometer. The - {% ?6 e9 @0 |1 Q. X' Jsystem worked fine and, using an Indirect Detection Probe , met quickly 5 K! _/ O) T3 T- M; V$ w5 Oand effortlessly the specifications. But later on, when the customer ( H" g" L S7 ` ] Jinstalled a 13C direct detection Probe, the S/N ratio turned out to be! k# e8 W& h7 \8 B# M, l quite low and, on top of it, the sensitivity was subject to erratic and) @- }) T; \8 g8 W0 _. G very large variations from 50:1 to 130:1 (manufacturer's specs give2 }. n! F6 t: F- I9 e' G 155:1), without any apparent reason., C" g4 e6 r, G1 g' c, j7 k0 u

Since the nominal 13C observe frequency at 9.4 T is 100,568 9 ? F3 {0 u# A3 h& l( FMHz, right in the middle of the range of commercial FM broadcasts, I 7 M, Z" }/ `5 @' M$ lhave immediately suspected that the spectrometer was picking up one of 8 R5 Q$ q# `. r% z2 t0 Bthose radio stations. In fact, using a cheap FM radio receiver, a * Q. q7 m, n* y3 s D* ]0 m% tstrong station was quickly found at 100,60 MHz. At this point, I have8 m' r- l; z9 {, s# k4 e connected a simple audio amplifier ending with a loudspeaker to the5 d2 F" K$ }2 n& ^+ p; R output BNC of the observe receiver which was there apparently just for - B. B. U3 _# p. H, Qthis purpose, and all of us were listening to the radio using a 200.000 . S% X7 m' s9 ^" o' w4 L u# }5 f+ OEuro NMR spectrometer, except that the audio quality was really poor,& |" q/ g2 } J$ ?3 R t k7 E much worse than from the above-mentioned gadget radio (a shopping mall1 G# h% u& q" ^. q# S& ]6 f gift). $ t7 {6 Y1 Q0 P8 [$ Y

The problem is well known from the old times, when the highest ! [$ {- f- V6 ]field was 2.45 T and the nominal H1 frequency was close to 100 MHz. One. I: p8 g" |4 Y# J) \$ F of the first Italian NMR spectroscopists to experience it, back in 8 k6 ]! z" Z- D1974, was Prof. L.Lunazzi at University of Bologna, on his brand new% }4 m( M( i5 ]- v0 M Varian XL100 spectrometer, and the radio station was Radio San Luchino, @+ R+ \0 P X( l, K( J; K# o well known to anybody living in Bologna, which broadcasts from the top3 w ]. d4 ?. w/ s9 p of the nearby Saint Luca hill.3 @( N( G% N* O8 y# {. U

The obvious solution is to change the magnetic field, and thus : ~+ u2 j/ }$ T8 a5 Jall resonance frequencies, in order to get out of the modulation 6 R2 `+ U) N, ~% r7 d# w1 n0 z4 y) |envelope of the interfering transmitter. But this is not always easy, 2 T. B( v& t# Qsince the range by which one can move the magnetic field changing just : W _" @; X# R5 q$ @# g7 P1 \some software parameters is usually limited to a few tens of kHz in the 9 ]3 U& s- W* ]! Ufrequency domain. If larger variations are required the poor engineer9 V) V2 d3 [% J% \; D' Y% w has to work on the superconducting coils of the magnet, which is a& \- S4 } F/ M" L3 g no-trivial job entailing the risk of a total or partial quench. : l& ]: q: \5 @5 E

Bitter experience shows that persuading the involved radio3 g/ ?- U& G! W3 p0 r W station to change its operating frequency is a time consuming,2 g5 W2 Q; g) x, r3 A! x frustrating, and apparently quite impossible task.( A' G$ x9 d! N

Being well aware of the problem, my preliminary spectrometer 0 w9 F( I5 @4 `9 Kchecks always include some blank acquisitions taken before running up ; p# f B1 p; ~% Rthe magnet so that there is no chance to observe an NMR signal. The: p: j, d' D( a a6 J- W resulting dataset should be pure white noise, without significant* D$ D* X) O) X% o9 z; J spikes. This was done also in this particular installation but, as + Q" I' S6 l: a9 n" m$ N- Q7 }usual, in the days following the energization the magnet drifted a bit, % O( q$ Y( }) B0 Y8 ]getting closer to the radio station carrier. Furthermore, the usual 13C5 Y, e" K% z% @: J spectral widths are quite wide which makes things even worse. Murphy's 6 p) X7 ~0 t1 A! }( d, \5 P$ OLaw has no exceptions! + T$ u7 \6 X# i2 C! f' O S

But we are just at the beginning of my real troubles. Before1 n8 ]% D/ a6 m, @! H' B putting one's hands on the magnet, one should better know how much, in6 U+ F, E! c$ V; m which direction, should the field be moved. I have therefore used a 8 n2 Q1 M% q0 r) S% S, [' zgood Spectrum Analyzer (Tektronix model 2710) to check the frequency : V) |5 Q: ~, \% C. wspectrum around 100 MHz, ready for the worst. And the worst was what I 6 e! z1 p @2 R" m5 cgot! The band was filled with FM signals, evenly spaced by 250 kHz and - p. Z; Z5 d/ u4 mwith modulation envelopes as wide as 100 kHz, so that when I got far 7 C$ x0 V2 |$ C9 |* M* X" B! V5 D bfrom one station I started receiving the next one; accounting for6 _' k0 M9 j2 T! K folding and aliasing effects, there was no chance! The only somewhat ( c/ E! h' V# V3 {$ efree region was at 100,120 MHz, but this implied proton frequency of- O1 v- Q6 {5 B9 z9 i 398.100 MHz. So now the spectrometer is no longer a "400"!9 g& k9 h. \" O) p

Before installing a spectrometer, you better get a Spectrum# E+ L0 L D- n4 H8 N, K Analyzer and check for the presence of RF fields in the instrument # p" S) P% y! Z" Froom, taking care to explore the areas close to the observe frequencies3 i: G; N$ @! h) K* V$ Q of all the most important nuclei. Don't forget the lock: at 14 T 0 t$ f: S2 l7 ~4 [6 w% O& X(nominal 1H frequency of 600 MHz) 2H resonates at 92,095 MHz, once 4 |5 a. q3 E8 z8 D# H2 ?7 O; Jagain in the FM broadcast band. The lock channel receiver has quite 8 D6 b# S: w2 h- b( Q9 tnarrow bandpass filters, so hitting a radio is a really bad luck, but3 N. u3 \ ?; q7 R" i2 N) e0 f it had already happened, resulting in fast lock level variations and ; q% X# _ ]& ltotally malfunctioning Gradient Shimming which uses deuterium as3 b4 ?; a2 D* t% S1 Z- w, U2 g observe nucleus!+ r& c+ ~$ I! V* J7 W3 a( {, m/ G) f

Needles to say, the extremely high sensitivity of an NMR7 s6 i* ~- `8 u0 A7 e3 M& ?# G Spectrometer shows up. The signal from the guilty radio, as observed on 8 z% D8 q2 g9 wthe spectrum analyzer inside the spectrometer room, had very low ' b9 f+ X% M7 P+ Dintensity level of about -70 dBm, some microvolt/meter, but that was : _& N) X C: K. v3 wenough to almost completely hide the quite strong 13C signal from the! ?7 s6 J$ p9 p u& G ASTM sample!% J6 e0 L; l3 L3 K' [! f7 F+ p$ W# H

The radio was clearly picked up by the Probe (closing the" \- v7 u- n* o+ n! E! Y) I) q Preamplifier input with a shielded 50 ohm RF load, all signals H% ]% j% ^ Adisappear) but, quite surprisingly, there is almost no shielding effect s' H" J9 e" q7 y6 e" K5 h7 N, q attributable to the metal body of the magnet, which is after all an - t% s5 r/ b0 q& nalmost completely closed cylinder all around the Probe. Most probably a7 r! Q1 Q/ `! T( f/ Q$ _! e good deal of the signal leaks in through the Shim Coils which are - M) j _' ~9 x/ e; y0 Lmounted very close to the Probe and, together with their connection. o! F$ d2 M' {: J cables to the Console, constitute a quite good antenna. 9 P. C( F7 H1 b/ c+ h( ?

Too bad the Shim Coils are essential, and effective shielding) S! ?; f3 J& W of the instrument with a Faraday's cage is always difficult and. y, b0 j% c: _# ]1 f( f5 ~ expensive (it may be almost impossible once the spectrometer is . F8 x' Q: u8 U& Pinstalled). 4 L2 G5 C# |9 V, u1 s

: U5 [6 S' L1 i+ x) q1 a$ PBefore concluding, let me venture some additional advice based on my experience:# D( x. b8 g1 [$ O7 M, J2 c m

" o; @" z/ g' O0 V* f7 B, b = Install the spectrometer in the best shielded room 9 D* Y& z1 h8 eyou can get; the best choice is once again in the basement, where you3 @- h1 O# X+ j0 ?" `$ T5 g( t$ u have the whole building above the ceiling and its [grounded]$ Z6 T! A T9 C) e L: I5 T! j foundations all around the rest, done in iron-reinforced concrete,3 u. H J# b. l7 |! W& M amounting to a good Faraday's cage at no extra cost. 4 U/ N# M; _! {6 i. g1 b

, g" B; C" S7 A+ R5 I$ g= If possible, avoid top floors. If you can't avoid1 U2 l$ T) G9 |2 N N+ e going upstairs, take a good look out of the window: if you see nearby6 o- m- H/ g* G5 _2 z4 F' d transmission antennas, get ready for troubles proportional to their( [! ?' Y. f# e! h$ ?' L dimensions and closeness (to my knowledge, however, mobile telephony # A. {; Y; `7 D$ n9 _/ j R+ Bantennas cause so far no harm). % P( c8 E! y, H/ Y, G

+ @1 X4 Z$ @5 j/ U = I'm sure that an exchange of experiences and/or/ G2 x% U$ c& v3 o! x8 K1 D suggestions regarding this matter would help a lot to solve many 3 Z1 y5 g$ j1 m. c Q' {7 B% iexisting 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. B; ]* p8 W2 s7 g' k! j! s+ a

- ~4 w! u* {6 A+ q! G& n 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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