无线电台会影响ＮＭＲ

syflu

 When it comes to polluting the environment, humanity has no equals. This applies to all kinds of spaces, including the electromagnetic ether. What follows is a contribution and a warning from Vanni Piccinotti, an engineer based in Florence, Italy, who has decades of experience with installing, testing, and servicing NMR and EPR spectrometers. The ! Q: w; v3 V2 O0 X& I2 n- Zproblem of RF interference has never been trivial and it keeps slowly + v7 ]" V# v1 j9 x$ zbut inexorably mounting. The spread of urban areas (combined with the tendency to install MR instruments in those same areas) and the mounting maze of wireless technologies penetrating our daily life spell nothing good for the future quality of our NMR signals. With concurrent 5 {$ u) n' @$ _0 ^. G( kprogress in basic sensitivity of the instruments, time might come when . d k; c2 t- i1 `$ tenvironmental RF noise will be the single major obstacle to further 3 ^# k8 V- b+ V! k% H7 aprogress. But let us hear what Vanni has to say:

syflu

 

Cross-talk between FM Broadcast Radio Transmitters (88-108 MHz) and NMR Spectroscopy: A recent experience

7 v) }) n& M( \/ d+ bRecently I had to install a 400 MHz (9.4 T) NMR Spectrometer. The : {8 J+ a! Q* f1 d. usystem worked fine and, using an Indirect Detection Probe , met quickly and effortlessly the specifications. But later on, when the customer installed a 13C direct detection Probe, the S/N ratio turned out to be , v- Q0 \5 w7 j4 H, w% p/ oquite low and, on top of it, the sensitivity was subject to erratic and very large variations from 50:1 to 130:1 (manufacturer's specs give . ^) o4 ]6 K: Z( C155:1), without any apparent reason.

Since the nominal 13C observe frequency at 9.4 T is 100,568 ( S/ c, H/ H( m: Y. H9 Y2 {MHz, right in the middle of the range of commercial FM broadcasts, I 4 I9 Z9 o/ y0 Fhave immediately suspected that the spectrometer was picking up one of & A$ i% D4 l0 Kthose radio stations. In fact, using a cheap FM radio receiver, a strong station was quickly found at 100,60 MHz. At this point, I have 1 V! |2 H; L1 }connected a simple audio amplifier ending with a loudspeaker to the 8 ^/ D0 G+ B* U" V9 joutput BNC of the observe receiver which was there apparently just for this purpose, and all of us were listening to the radio using a 200.000 Euro NMR spectrometer, except that the audio quality was really poor, much worse than from the above-mentioned gadget radio (a shopping mall gift).

The problem is well known from the old times, when the highest : ], z% a7 W4 T: f# S5 `6 ~field was 2.45 T and the nominal H1 frequency was close to 100 MHz. One / z. O+ Z9 j. y% I( ?( ~of the first Italian NMR spectroscopists to experience it, back in ( h4 p6 w( Q' O- ^' K( b6 Y' s) F1 k1974, was Prof. L.Lunazzi at University of Bologna, on his brand new Varian XL100 spectrometer, and the radio station was Radio San Luchino, ( m) T0 p9 Q4 cwell known to anybody living in Bologna, which broadcasts from the top : L. r( H# \6 {0 J0 @& \of the nearby Saint Luca hill.

The obvious solution is to change the magnetic field, and thus all resonance frequencies, in order to get out of the modulation envelope of the interfering transmitter. But this is not always easy, since the range by which one can move the magnetic field changing just * O: F# ~6 s8 @, [$ rsome software parameters is usually limited to a few tens of kHz in the frequency domain. If larger variations are required the poor engineer has to work on the superconducting coils of the magnet, which is a : n* F5 y# b c1 K9 mno-trivial job entailing the risk of a total or partial quench.

Bitter experience shows that persuading the involved radio station to change its operating frequency is a time consuming, ' M2 a" h; j3 l& \frustrating, and apparently quite impossible task. 6 G8 A) I' q+ N" y) m3 y+ m

Being well aware of the problem, my preliminary spectrometer checks always include some blank acquisitions taken before running up the magnet so that there is no chance to observe an NMR signal. The resulting dataset should be pure white noise, without significant spikes. This was done also in this particular installation but, as usual, in the days following the energization the magnet drifted a bit, ) ~; I$ U: `2 Y1 r) kgetting closer to the radio station carrier. Furthermore, the usual 13C spectral widths are quite wide which makes things even worse. Murphy's Law has no exceptions! 9 ]1 t8 j9 q; k8 y3 w, \+ R

But we are just at the beginning of my real troubles. Before 4 r7 P9 W; r* `putting one's hands on the magnet, one should better know how much, in which direction, should the field be moved. I have therefore used a good Spectrum Analyzer (Tektronix model 2710) to check the frequency $ f3 b$ z/ z4 l) l+ z% A' X. B" dspectrum around 100 MHz, ready for the worst. And the worst was what I got! The band was filled with FM signals, evenly spaced by 250 kHz and with modulation envelopes as wide as 100 kHz, so that when I got far from one station I started receiving the next one; accounting for 4 ^% l: z; z2 K1 L$ E' ~ ^folding and aliasing effects, there was no chance! The only somewhat 2 y" J" G. C$ W: g X2 n3 Q, Ofree region was at 100,120 MHz, but this implied proton frequency of . r0 s z: T. Q9 S+ Z" G398.100 MHz. So now the spectrometer is no longer a "400"! ( O! |- d8 L# z! V

Before installing a spectrometer, you better get a Spectrum I' i: d' `' U% w1 P5 |Analyzer and check for the presence of RF fields in the instrument room, taking care to explore the areas close to the observe frequencies of all the most important nuclei. Don't forget the lock: at 14 T (nominal 1H frequency of 600 MHz) 2H resonates at 92,095 MHz, once % T5 q- j1 y" g* }4 Jagain in the FM broadcast band. The lock channel receiver has quite narrow bandpass filters, so hitting a radio is a really bad luck, but it had already happened, resulting in fast lock level variations and * b2 ]; |: J+ l* ttotally malfunctioning Gradient Shimming which uses deuterium as 6 P! C. p/ c* M0 C- Fobserve nucleus!

Needles to say, the extremely high sensitivity of an NMR Spectrometer shows up. The signal from the guilty radio, as observed on ! Z) R+ u" l+ L7 |3 ^. l) o* Bthe spectrum analyzer inside the spectrometer room, had very low / T) h, ?. v3 j% F( x( u0 bintensity level of about -70 dBm, some microvolt/meter, but that was enough to almost completely hide the quite strong 13C signal from the 4 a9 ?$ J/ g. A' U6 zASTM sample!

The radio was clearly picked up by the Probe (closing the Preamplifier input with a shielded 50 ohm RF load, all signals 4 C) o# ^* N7 P" D% udisappear) but, quite surprisingly, there is almost no shielding effect ! S: x' K' t& t" t+ tattributable to the metal body of the magnet, which is after all an almost completely closed cylinder all around the Probe. Most probably a : N. G# W! d$ B3 O2 bgood deal of the signal leaks in through the Shim Coils which are 0 Z5 c- i: A8 X% Rmounted very close to the Probe and, together with their connection cables to the Console, constitute a quite good antenna.

Too bad the Shim Coils are essential, and effective shielding of the instrument with a Faraday's cage is always difficult and expensive (it may be almost impossible once the spectrometer is installed).

7 G& Y7 m/ P6 w+ r4 xBefore concluding, let me venture some additional advice based on my experience:

# [' N% y0 f B/ ~6 K7 |# [* C= Install the spectrometer in the best shielded room you can get; the best choice is once again in the basement, where you + g! m8 b: L. ?' yhave the whole building above the ceiling and its [grounded] foundations all around the rest, done in iron-reinforced concrete, amounting to a good Faraday's cage at no extra cost.

= If possible, avoid top floors. If you can't avoid ! c4 S& N- Y6 B$ d. B/ ?going upstairs, take a good look out of the window: if you see nearby transmission antennas, get ready for troubles proportional to their . s# U5 v, }' a: R" D1 R gdimensions and closeness (to my knowledge, however, mobile telephony 8 Y) D! @( P# G) ~: fantennas cause so far no harm).

* v4 g% E( r; D. M+ ^ b% I= I'm sure that an exchange of experiences and/or suggestions regarding this matter would help a lot to solve many 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. 3 g8 r r' a$ Q

Vanni Piccinotti, Firenze, 11 April 2008

摘自stan' NMR Blog.

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