|
. }* P; V0 m9 j+ J( a8 @% E( m) UCross-talk between FM Broadcast Radio Transmitters (88-108 MHz)" L) Z t# b+ V; Q2 ^
and NMR Spectroscopy: A recent experience2 k/ d! [* W% R3 A. Y
m, y N8 T: m' B% e
Recently I had to install a 400 MHz (9.4 T) NMR Spectrometer. The
4 W6 W2 f5 W0 Wsystem worked fine and, using an Indirect Detection Probe , met quickly0 V( M6 a9 g( Z# R
and effortlessly the specifications. But later on, when the customer
, ^7 v' w+ y, V* _( }installed a 13C direct detection Probe, the S/N ratio turned out to be
8 v; g; y7 @# r% A3 S$ O, yquite low and, on top of it, the sensitivity was subject to erratic and
8 W' G# ~6 ^( D* R% bvery large variations from 50:1 to 130:1 (manufacturer's specs give
. y1 W) C* k* D155:1), without any apparent reason.* ~3 |* [4 G$ S) r
Since the nominal 13C observe frequency at 9.4 T is 100,568
# d3 N" G; Y8 \' a8 RMHz, right in the middle of the range of commercial FM broadcasts, I0 i/ m. v) O& X* _' G
have immediately suspected that the spectrometer was picking up one of) f6 S5 J& `& `8 {5 ^) `0 X
those radio stations. In fact, using a cheap FM radio receiver, a
% \, t+ L/ y. G; m I3 }' s) e/ vstrong station was quickly found at 100,60 MHz. At this point, I have" \* o/ o* e) g1 `
connected a simple audio amplifier ending with a loudspeaker to the4 T" _1 ?5 V6 f/ u" I" W
output BNC of the observe receiver which was there apparently just for7 G; L' a' x: l! V7 E. B0 h
this purpose, and all of us were listening to the radio using a 200.000
) J( _: z% }$ C ]* F. jEuro NMR spectrometer, except that the audio quality was really poor,/ Z3 a( ]$ s$ G- |2 W, M
much worse than from the above-mentioned gadget radio (a shopping mall
4 k/ ?/ n& k+ @+ R' `gift).7 a% [6 w& k1 ]" J% E* s0 B8 S
The problem is well known from the old times, when the highest
Q' r6 u& X$ s* z0 R bfield was 2.45 T and the nominal H1 frequency was close to 100 MHz. One
( i& M `* H8 L$ Tof the first Italian NMR spectroscopists to experience it, back in) @2 l2 ]6 K; r1 F6 D
1974, was Prof. L.Lunazzi at University of Bologna, on his brand new9 _( D& w! C- s# D1 G1 U% q8 a. L& D
Varian XL100 spectrometer, and the radio station was Radio San Luchino,6 s+ ]1 e" p- B2 X
well known to anybody living in Bologna, which broadcasts from the top
# [$ P! ?6 C$ I5 Jof the nearby Saint Luca hill.1 ~) p. v* s; l: W2 v
The obvious solution is to change the magnetic field, and thus$ |8 F3 M/ _4 @+ O
all resonance frequencies, in order to get out of the modulation
' _% ^0 j/ r/ l* K$ Cenvelope of the interfering transmitter. But this is not always easy,
6 {7 E) v" x) z7 wsince the range by which one can move the magnetic field changing just( F- K+ V% [9 X0 y. ^* l, m
some software parameters is usually limited to a few tens of kHz in the; P# q- W' N' I* z; k$ {
frequency domain. If larger variations are required the poor engineer
1 Z9 ~ \! ]6 s4 J6 `4 thas to work on the superconducting coils of the magnet, which is a
) `4 D4 j* \! n+ O9 Fno-trivial job entailing the risk of a total or partial quench.
6 p! E2 t3 L3 |* v" v! j Bitter experience shows that persuading the involved radio. g+ o' Q+ O/ G( p- r5 P r& x
station to change its operating frequency is a time consuming,) ^! m# o+ z! c' k5 [
frustrating, and apparently quite impossible task.! |" O8 H: a$ N; k' T
Being well aware of the problem, my preliminary spectrometer
5 L# F$ X8 d0 d4 J( ?. A' Qchecks always include some blank acquisitions taken before running up
# P U. s+ c' \the magnet so that there is no chance to observe an NMR signal. The
; u6 k* Y, V- A6 k; C$ x5 i% h! kresulting dataset should be pure white noise, without significant
1 g" O6 X. F& M. Mspikes. This was done also in this particular installation but, as
+ Q2 R/ U9 z0 c* G& busual, in the days following the energization the magnet drifted a bit,
0 B( V* X+ q" D$ i7 |* G. y6 _getting closer to the radio station carrier. Furthermore, the usual 13C2 D6 R/ f. s& B. j( `8 L' h+ Y* T- O
spectral widths are quite wide which makes things even worse. Murphy's
5 O. [6 Z0 I, B$ x1 ~Law has no exceptions!
& o% e$ B, O* x But we are just at the beginning of my real troubles. Before
& ?$ `% x4 K, V+ j' Sputting one's hands on the magnet, one should better know how much, in/ I2 k4 V# b6 `3 o+ ~
which direction, should the field be moved. I have therefore used a
( O5 E2 V% {, R4 q) ugood Spectrum Analyzer (Tektronix model 2710) to check the frequency
" h7 M0 R7 }! e% Y1 r( s+ l" S6 bspectrum around 100 MHz, ready for the worst. And the worst was what I
5 P+ ?# N! P8 Xgot! The band was filled with FM signals, evenly spaced by 250 kHz and
5 K& A/ D5 y1 H1 y8 M, y' d/ `with modulation envelopes as wide as 100 kHz, so that when I got far
7 V d* W0 ~1 M2 V5 g$ w3 L! Efrom one station I started receiving the next one; accounting for
, D M+ I r9 {5 a% j( Nfolding and aliasing effects, there was no chance! The only somewhat
`& b) C. {5 l o; D7 c6 J, zfree region was at 100,120 MHz, but this implied proton frequency of: R. x& G5 w: u+ d1 k. p
398.100 MHz. So now the spectrometer is no longer a "400"!
/ ^0 V7 H8 {8 ^/ y0 P8 \5 e Before installing a spectrometer, you better get a Spectrum0 E8 J1 g w& E! C5 y" M
Analyzer and check for the presence of RF fields in the instrument
" m- i# s2 X3 d) h' nroom, taking care to explore the areas close to the observe frequencies
- J/ t6 S9 x8 dof all the most important nuclei. Don't forget the lock: at 14 T' I, _' H: ]! `8 i9 k6 j9 \2 T
(nominal 1H frequency of 600 MHz) 2H resonates at 92,095 MHz, once
0 L6 D H9 @8 s& ?6 z8 _4 t+ gagain in the FM broadcast band. The lock channel receiver has quite
- t E2 D0 ?. U, h5 p0 xnarrow bandpass filters, so hitting a radio is a really bad luck, but! y# B: ^) b) j7 ]& C* E) Z5 M
it had already happened, resulting in fast lock level variations and
% m1 s; u7 q# g9 O3 Y7 M- r- @totally malfunctioning Gradient Shimming which uses deuterium as! E$ U( K; d6 r$ [+ N& s$ N
observe nucleus!
- N. ?. V* K6 y" }" b1 ^& ` Needles to say, the extremely high sensitivity of an NMR3 E3 _" C9 w, O7 O! o
Spectrometer shows up. The signal from the guilty radio, as observed on
( [# g& j2 s% @- O$ rthe spectrum analyzer inside the spectrometer room, had very low
. Q/ p, Z1 i3 o! h' dintensity level of about -70 dBm, some microvolt/meter, but that was
4 G! |2 F' z' t& penough to almost completely hide the quite strong 13C signal from the
9 N$ p& H# q! D+ IASTM sample!
8 x# [8 V2 {& {' N( G The radio was clearly picked up by the Probe (closing the
* M9 A& V" `8 I" \3 R, B$ dPreamplifier input with a shielded 50 ohm RF load, all signals0 M2 }. Y- H: q9 m" U1 i/ N7 [0 B7 b9 E
disappear) but, quite surprisingly, there is almost no shielding effect
! P* S4 V5 { S X7 [attributable to the metal body of the magnet, which is after all an1 |/ U% F9 { T5 @3 \' e% M* r
almost completely closed cylinder all around the Probe. Most probably a o3 t6 Y: s# R4 m1 N1 g
good deal of the signal leaks in through the Shim Coils which are
$ b& b* c1 u0 d% d E* l2 Y& l" _mounted very close to the Probe and, together with their connection! e# A: y3 V% w- u* G Y: o B
cables to the Console, constitute a quite good antenna.
4 _9 n6 B9 K% w1 ^) b, i* j Too bad the Shim Coils are essential, and effective shielding
/ B8 \$ Q$ ?" [- r" `/ Pof the instrument with a Faraday's cage is always difficult and
; U# D: Q9 P0 N0 M; [! Oexpensive (it may be almost impossible once the spectrometer is& ]7 ^- m' Q. A
installed).- ?; c9 r, Z( Y) ]
) x5 y" Y/ U- H; z; {( ~1 O/ d
Before concluding, let me venture some additional advice based on my experience:
5 o: Y, `$ F/ B0 F4 i ) r3 ~- X' p) r3 a
= Install the spectrometer in the best shielded room
+ y6 N4 C7 o' a8 }$ vyou can get; the best choice is once again in the basement, where you0 w" W; c2 z, i1 _6 v
have the whole building above the ceiling and its [grounded]
0 x: w) }8 M. ?foundations all around the rest, done in iron-reinforced concrete,
; d% H4 R9 D7 ^) \amounting to a good Faraday's cage at no extra cost.
% b' g1 E/ O$ a9 b* {% G/ E 2 M, j7 m! Z1 \7 W: e
= If possible, avoid top floors. If you can't avoid
& \8 F. N, H$ ]# Ygoing upstairs, take a good look out of the window: if you see nearby
+ l5 H" P# b V P% N, e) U: g$ J3 ltransmission antennas, get ready for troubles proportional to their2 Y6 l& G" O. O5 W+ P2 M2 R1 G$ J! ?
dimensions and closeness (to my knowledge, however, mobile telephony7 b, b2 p. ^( u+ G% R) E
antennas cause so far no harm).
2 X& ?# ^4 ]) ~0 ^ ( m7 N7 ^: `- a% l2 o, _* Q
= I'm sure that an exchange of experiences and/or
6 a, c# m/ l& [& e. w# Dsuggestions regarding this matter would help a lot to solve many7 J3 U+ D$ l1 ~- ]8 A8 G
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.
9 F5 B1 d8 G8 ~( H* ?1 l L1 R
& g* A2 r, H: ]: N$ ZVanni Piccinotti, Firenze, 11 April 2008
摘自stan' NMR Blog.
|