Bloch. Nuclear Induction Experiment 1946 PDF
Bloch. Nuclear Induction Experiment 1946 PDF
Bloch. Nuclear Induction Experiment 1946 PDF
(5) As in comparing the moments of neutron, There are unquestionably more problems which
proton, and deuteron, nuclear induction can well will become tangible in further deyelopment of
be developed as a simple and practical method to the new electromagnetic effects. The fact that
calibrate and measure high magnetic fields with they are simple to obtain and require only
great accuracy, and t o apply it, for example, very modest equipment should make it pos-
in the construction of cyclotrons and mass sible for many investigators to enter this field
spectrographs. of research.
The phenomenon of nuclear induction has been studied experimentally. The apparatus
used is described, both as to principle and detail. Experiments have been carried out in which
the signals from protons contained in a variety of substances were observed. The results show
the role played by the relaxation time, which was found to vary between about 10-6 second
and many seconds.
voltageasmuch as possible by using a multip1icit~- quite limited. For example, if one attains a Q of
of turns and by introducing a shunt condenser to 100, which is quite good for such small coils in the
induce resonance. In principle, such resonance presence of poor dielectric, the band width a t 7
does not alter the ratio of signal voltage to mc is 1.1 X lo5 c~cles/sec.,or much larger than
thermal noise voltage, but in practice it does alter the minimum set by the requirement that the
the ratio of signal to observed noise, because both response time be not inconveniently large. While
signal and thermal noise are raised relative to the somewhat larger Q values may be possible, it is
constant amplifier or tube noise. plain that no attainable value will make the band
The apparatus we used had 24 turns on a form as small as one might desire.
of diameter d = 1 . 7 4 cm and length h=0.84 cm, Some improvement might be obtained by
and had a Q, with the sample in place, of about making the modulation cyclic, and following the
81). The r.m.s. voltage available is then rectifying device which converts the 7-mc signal
to a unidirectional one with a filter, or amplifier,
sharply tuned to the modulation frequency. The
effectiveness of this scheme may be measured by
the effective band width, which is of the order
and, with a sample of volume 1 . 4 6 cc this comes ( A V ~ A Vwhere
~ ) ~ Avl and Ava are the band widths
out to be 3.7 X volt, so that large amounts of of the circuits before and after the rectifier. Thus
amplification are not needed. Also, this may be reducing Avz reduces the noise, but not as much
compared with the thermal noise voltage which, as one might hope, since the response time goes
for this coil, is about 0.7 X10-6 volt in a 3000- with l / A v z .
cqcle-per-sec, band. Thus, an enormous ratio of The proper way to reduce the band width is by
signal over noise is potentially available. This heterodyning the signal down to some lower
ratio is independenrof the number of turns on the frequency where a given percentage band width
coil, but could be increased for the same sample becomes a small absolute band width. This may
and coil size by increasing Q or decreasing the be clone with a detector, and following filter with
hand width. narrow pass band, if one introduces into the
' r ~ i ~further
o points nus st be noted, however. detector an additional signal of constant fre-
First, in order to know that the observed quency, usually called the local oscillator signal,
amplifier output is caused by the nuclear mo- and with magnitude large compared to either
ments and not by some unknown cause, it is signal or noise. Then the beats between local
essential that the voltage due to the nuclear oscillator and signal or noise components domi-
moments be varied, or modulated, in some known nate those between noise components, or between
and controllable manner in which case outputs are signal and noise components, and the output
real or spurious according as they do or do not noise then depends only on AvZ,being quite inde-
correspond to the known modulation. pendent of Avl. In this way the band width may
Second, the magnitude of any spurious signals be reduced by any desired amount, the only limit
or "noise" will depend on the frequency band being set by the response time 1,'Avz.
accepted by the resonant pick-up coil and the We come now to the question of the effects of
amplifier which follows. If the noise is of random the large field H I which, it will be remembered, is
type, its amplitude will vary with the square root a t least l o 6 larger than the field to be detected.
of the band width; if it is of impulse type, the This large background has two effects. First, if
amplitude will vary directly with band width. In even a moderate fraction appears in the receiver,
any case, it is desirable to reduce the band width any amplifiers that may be used will saturate long
as much as possible or convenient, for doing so before the signal is of suitable size. Second, and
reduces noise while leaving the signal unaltered. more fundamental, any fluctuation in the back-
The straightforward method of reducing the ground is indistinguishable from a signal and,
band width is, of course, t o increase the sharpness with such a large ratio of background to signal,
of resonance by reducing the losses as far as may such variations can be serious, though they could
be. Possibilities in this direction are, however, be, if necessary, controlled.
NUCLEAR INDUCTION EXPERIMENT 47 7
found that there would be no in-phase component amplitude a t a 60 c/sec. rate because of the
of leakage. Actually this is not found t o be true, variations in field Ho, are amplified along with
the reason being that the currents which flow in stronger constant amplitude leakage signals. The
the paddle are not a out of phase with the leakage and the varying voltages due to pre-
currents in the transmitter coil, because of losses cessing nuclei are mixed in the detector, the
in the paddle, and so have a component in phase output of which then contains pulsating unidi-
with the signal. rectional current, the steady component due to
I t remains only to describe the methods of leakage and the variations corresponding to the
modulation and presentation. desired signal. The d.c. is removed by the
T o cause the signal to vary in strength one blocking condensers in the following amplifier
might vary either the z magnetic field Ho or the which increases the signal voltages to a magni-
frequency. The former seemed the easier and was tude suitable for operation of the cathode-ray
adopted for the experiments here described, the tube.
field Ho being varied cyclically about a value Hde. APPARATUS
The modulation frequency of 60 cycles/sec. was
chosen as being low enough to avoid excessive We now describe in detail the equipment
band width and high enough for the persistence constituting the various blocks in the above
of vision needed for the cathode-ray tube presen- diagram.
tation used. Within limits set by these factors a The steady magnetic field Hdc is supplied by a
considerable range of frequencies is possible: of lecture-demonstration magnet which easily pro-
these 60 cyclesisec. has the additional advantage duces the necessary fields of a few thousand gauss.
that any spurious hum pick-up appears as a The poles are 3 inches in diameter and these are
recognizable distortion of the final pattern rather provided with laminated extensions of trans-
than as a blurring. former sheet which are 34 inchesX3+ inches and
Presentation was on a cathode-ray tube with 1 inch thick. The spacing between these lami-
horizontal plates giving a deflection proportional nated extensions is 1; inches and within the
to the variation in Ho and the vertical plates central volume of 2 cc, occupied by the sample,
giving a deflection proportional to the signal the field was found, by flip coil measurements, to
which in turn depends on the y component of the be uniform to within 2 gauss. Since variations in
nuclear magnetic moment. Thus one observes on field of order H1=5 gauss could be tolerated
the screen a plot of M , vs. Ho, the center of the without undue broadening of the resonance peak,
screen corresponding to the field Ha,. this uniformity is satisfactory.
We may summarize by giving, in Fig. 3, a The 60 c/sec. modulation of the field is pro-
block diagram of the complete apparatus. Here vided by current flowing through two coils of
the spherical sample is immersed in a field about Helmholtz proportions, placed between the
Hd,+H,, cos 377t produced by a magnet, not laminated pole faces and carrying 60 c/sec.
shown. The nuclear moments oriented by this current. The magnitude of this current can be
field are caused to precess by a driving field II, regulated by means of a variac to give values of
~xoduccdby current from the box labeled trans- Ha,between zero and 50 gauss. The same current
mitter. 'l'he precessing moments induce voltages which passes through the coils passes also
i t 1 the rcceiver roil. These voltages, which vary in through a resistor, and the resulting voltage drop
actuates the horizontal sweep of the oscilloscope.
As to the transmitter, the main requirement in
addition to ability to deliver enough power to
maintain the field H I , is a very high order of
output amplitude stability. This requirement
arises because variations in leakage are indis-
tinguishable from signal and because even the
smallest leakage is large compared to the signal.
FIG.3. Block diagram of apparatus. For example, if the nuclear moment per unit
NUCLEAR INDUCTION EXPERIMENT
- I INCH
FIG.4. Scale drawing of an xy section of the r-f head. The spherical sample S is
surrounded by a receiver coil R, which is in turn surrounded by a transmitter
coil T, the whole being encased in a shield. A rotably mounted paddle P is used
to steer the transmitter flux. Leads to the receiver coil are the coaxial leads LlLz
while the transmitter leads are L3 and L4. The outer shield is split to avoid 60-cycle
eddy currents.
volume is lo-' times HI, as it might be in a Transmission lines a few inches long lead to a
typical case, then even if the leakage is reduced brass box about 4 inches by 8 inches by 8+inches,
to, say, of H I , a variation in transmitter which is divided in two by a horizontal partition.
output by a part in lo4 will cause a fluctuation The lower portion contains tuning condensers to
equal to the signal. resonate the transmitter coil ; the upper contains
The power required to maintain the field HI is a similar condenser for the receiver and also the
of the order 1 watt and this, together with con- detector and first audio stage of the receiver,
siderable excess to allow for imperfect impedance together with suitable batteries for same.
matching, etc., is easily supplied by an 815. The The receiver differs from the block diagram in
stability is achieved by deriving both filament that the r-f amplifier there shown is omitted, the
and plate power from batteries. Magnetic regu- receiver coil working directly into a diode de-
lators in the primary of an ordinary supply were tector. This has the disadvantage of a very con-
tried and found worthless because of slow re- siderable loss in potential signal/noise ratio, but
sponse. A carefully engineered and tested vacuum- in view of the large signal available from protons
tube regulator might do, but batteries were it was decided to sacrifice this in the interests of
adopted as quicker and absolutely reliable. simplicity. This simplicity appears in two ways:
The transmitter and receiver coils are best First, one replaces an r-f amplifier by a simpler
described by the drawing of Fig. 4, which shows audio stage, and second, whereas a volt or less
the coils and surrounding shield which we may might saturate an r-f stage, the diode will not
call the r-f head. The transmitter coil consists of saturate. This point is very important in tuning
seven turns of mean diameter 5" and length i", up, for a t the start the leakage voltage is usually
wound inside a threaded polystyrene shell. Inside 100 volts, or more, and it is only after con-
the transmitter coil is placed the receiver coil of siderable adjustment that this can be reduced to
24 turns, A" in diameter and A'' long, wound on about 0.1 volt which is usually used in operation.
the outside of a thin threaded polystyrene form. The diode detector is conventional as is the first
Inside this, in turn, is the sample, contained in a audio stage which acts mainly as an inverter and
glass bulb in. in diameter. The design aims a t impedance changer, giving push-pull output a t
the greatest mechanical rigidity and damping low impedance level. This low impedance output
possible, in an effort to avoid vibrations which, is carried to the main amplifier by a few feet of
by varying the coupling between transmitter and cable.
receiver, vary the leakage and so introduce The requirements on this amplifier are that it
microphonics. Such microphonics constitute the have a gain of a few thousand and pass all
biggest experimental difficulty with the equip- significant signal components without appreci-
ment here described. able amplitude or phase distortion. The fre-
480 BLOCH, HANSEN, AND PACKARD
RESULTS
Using the method and apparatus described
I iI l i above, we have so far investigated nuclear induc-
1.
-A, --
1' t
. tion of protons only. The advantage of working
with protons is twofold. In the first place they
FIG.5. Schematic representation of the modulated corn- have of all known nuclei the highest gyromagnetic
ponent Ha of the magnetic field in its dependence upon ratio y so that moderate fields are sufficient to
time. As the magnet current decreases, the resonance field
H* is first reached a t the initial time t, and last at the bring theresonance frequency into the convenient
final time 1,. During the interval At a positive signal is frequency range of a few megacycles. In the
observed to travel across the oscillograph screen as indi-
cated by the arrows on the traces, sketched for three second place there is a great choice of conlpounds
different times a t the beginning, the middle, and the and solutions containing hydrogen which facili-
end of At. tates variation of the conditions of observation,
particularly with respect to the relaxation times.
quencies involved are the modulation frequency Our first experiments were carried out with
of 60 c.p.s. and various harmonics thereof. With water contained in small spherical glass bulbs
2H1 of, say, 10 gauss and A H of 100 gauss, the which could be sealed off. The very first signal
first ten harmonics will be of about equal was observed with a sample of only 100 milli-
strength and from there on up the strengths will grams, but in all later experiments the amount
decrease rapidly. About fifty harmonics should was increased to about 1 gram, the glass bulbs
then be ample and the amplifier must then pass being increased to a volume of about 1 cc. These
frequencies between 60 and 3000 cycles/sec. samples were placed into the receiver coil and,
Actually the amplitude response must be practi- after mounting the shields and the a.c. coils,
cally flat to a considerably lower frequency, say, providing the field modulation, were moved into
6 cycles/sec., if phase shiftsin the lower harmonics the center of the magnet gap. With proper tuning
are not to cause undesirable pedestal effects. and adjustment of the apparatus we could then
These requirements were met by a three-stage observe the proton signal on the oscillograph
amplifier, using push-pull twin triodes (7F7) screen as the current in the magnet was set to a
throughout. The use of push-pull amplification
eliminates cathode bypass condensers and, more
important, cancels the otherwise very annoying n All
disturbances due to power supply variation.
Likewise, screen by-passes are not needed and the
h4iller effect is not bothersome because of the
rather low value of high frequency cut-off. The
amplifier was tested on 60 c/sec. square waves,
which it passes without distortion.
Although frequency response, as specified
above, is needed to give a completely undistorted
pattern on the oscilloscope, it is found in practice
that the amount of pedestal effect introduced by
raising the low frequency cut-off to 60 or 120 FIG. 6. Time dependence of HOas the magnet current
increases. A negative signal travels across the screen a s
cycles is not objectionable, and the reduction in indicated by the arrows on the three sketched traces.
NUCLEAR INDUCTION EXPERIMENT 48 1
The following three traces represent snapshots explain relaxation times of the order of a few
taken during the next 15 seconds a t regular seconds. In order to verify this hypothesis we had
5-second intervals and clearly show on trace b the one of our water samples purified by distillation
decrease and on traces c and d the reversal of the in a vacuum* with a final partial pressure of
signal. The fact that on traces a, b, c , and (slightly) oxygen of probably no more than mm. While
also on trace d there appear two separated signals with the previous unpurified samples the reversal
on top of each other is caused by stray 60-cycle of the proton signal was essentially completed
pick-up which has the same frequency as the after 4 to 5 seconds, it took with the purified
modulation and, appearing on top of the actual sample about 15 seconds for completion of the
proton signal manifests itself in a separation of reversal. There is thus a noticeable effect of
the forth- and back-sweep, recorded during the shortened relaxation times by impurities but it is
exposure of the camera. by no means sufficient to explain their abnormal
I t was most surprising thus to establish the shortness. We can, of course, not discard the
proton relaxation time in water to be of the order possibility that even after distillation there re-
of a few seconds, although it must be admitted mained impurities in the water (originating, e.g.,
that it is difficult, as pointed out in I, to give a from material adhering to the glass walls) of
reliable theoretical estimate. Whereas such an sufficient amount and catalytic effectiveness to
estimate can be given for a gas and, t o some determine mainly the observed relaxation time.
extent, also, for a crystal, there is not enough However, it does not seem very probable to us
known about the molecular motion in liquids to that this is the case, since in one of our experi-
predict more than a crude order of magnitude. ments mineral oil was used instead of water. I t
Treating the liquid either as a highly compressed exhibited a relaxation time of the same order of
gas or as a crystal with thermal amplitudes of the magnitude, while the entirely different chemical
molecules, comparable to the lattice constants nature should be expected to result in a different
one would expect the relaxation time to be of the composition of impurities. Nevertheless there
order of a few hours rather than of a few seconds. may be an accidental coincidence and more ex-
We must point out here that the "relaxation periments will be necessary to clarify the role of
time," as observed in our experiments, does not impurities.
necessarily represent the usual (and in I, referred Another experiment of interest was carried out
to as the "longitudinal") paramagnetic relaxation with ice. The water was frozen in a small con-
time T Ibut that it representsrather an "effective" tainer and placed into the transmitter-receiver
relaxation time, which can be influenced by the assembly. No noticeable signal was observed
possibly different transversal relaxation time Tz, while the water was still frozen but the signal
introduced in I. I t will require a good deal more started to show up with the beginning of the
experimentation and observation under various melting process. We interpret this result as indi-
conditions to separate clearly the effects of TI cating a very long relaxation time in ice, since it
and Tz and, with the use of Eq. (46) of I, to was shown in I, Section 4, that the magnitude of
ascertain their values separately. This point, the signal decreases indefinitely for sufficiently
however, relates to the quantitative rather than increasing T I .
to the qualitative interpretation of our results I t seems reasonable, from theoretical con-
and is by no means sufficient to explain the siderations, that the relaxation time in a solid
extraordinary difference in magnitude between should be considerably longer than in a liquid and
the observed effective and the theoretically ex- in this respect there is nothing remarkable in the
pected paramagnetic relaxation time. behavior of ice. I t was the more surprising to find
We suspected the origin of this discrepancy t o another solid, namely paraffin, to behave in an
be caused by slight impurities and particularly to entirely different manner. With the same method
oxygen dissolved in water. Because of the mag- of observation as indicated in Fig. 5 and 6 for
netic moment of the oxygen molecules, acting as
catalysts, it would actually take only one mole- * W e wish to thank Dr. R. A. Ogg for kindly preparing
the sample for us and for valuable discussions relating to
cule of 0 2 in about a thousand molecules of Hz0 to the chemical aspect of our experiments.
484 BLOCH, HANSEN,
order to obtain a case in which, because of the We have verified that the value of the reso-
atomic moments of the Fe ions, the relaxation nance field determined in this manner agrees with
time is short compared t o the time required to the gyromagnetic ratio for protons determined by
pass through resonance conditions. We obtain Kellogg, Rabi, Ramsey, and Zacharias.* After
thus the case of "slow passage," discussed in I, determining the resonance frequency and without
Section 5. The shape of the signal is here in com- altering the magnet current, the modulating a.c.
plete agreement with the theoretical formula, field was turned off, the transmitter-receiver
I (53), having a zero a t resonance and an up- and assembly removed and a carefully measured flip
down-swing for positive and negative values of 6, coil brought to the original position of the sample
respectively. Except for their position, there is between the pole pieces in order to determine the
no difference in the signals received on the three value of the resonant field H*. With a frequency
traces a, b, c which pertain to the corresponding v = 7.765 X lo6 set.-I it was found that the reso-
values of Ha,, represented in Fig. 6 . A "zero" nance field had the value H*= 1826 gauss which
trace d is again added, showing the slight leads to a value of the gyromagnetic ratio
separation of forth- and back-sweep.
With the time, required to sweep through the
signal of about 1/600 second we estimate the
relaxation time to be here of the order of to
sec. Other data, showing the dependence of
the relaxation time upon the concentration of the The agreement within one-quarter of a percent
paramagnetic salt will be published shortly. with the value y = 2.665 X lo4, obtained with
The shape of the signal obtained with Fe(N03)3 molecular beams, must be considered accidental
solutions makes it particularly easy to locate the since our field measurement can only claim an
resonance value of Hdc by setting the magnet accuracy of about 1 percent. We have also veri-
current to such a value that the zero point of the fied, although with somewhat less accuracy, that
signal is located a t the exact center of the the ratio v/H* for the resonance signal, obtained
oscillogram. With the whole resonance width from water, remains the same for v = 7.8X l o 6 ,
amounting to only about 1 percent of the total v = 8.8 X lo6, and v = 10.7 X lo6.
field, this setting can be easily adjusted to within
* J. M. B. Kellogg, I. I. Rabi, N. F. Kamsey, Jr., and
the order of one per permille. J. R. Zacharias, Phys. Rev. 56,!728 (1939).
FIG.10. Photopraphic record oi the proton sipnal in
water. The four traces from top to bottok correspond to
the times t l , 1 9 , tr, t . of Fig. 9. In the text they are referred
to a s a, b, c, d, respectively.
FIG.11. Photographic record of the proton signal in
paraffin. The four traces from top to bottom are in the
text referred to as o, b, 6, and d.
FIG. 12. Photographic record of the proton signal in a
concentrated solution of Fe(NOl), in water. The four
traces from top to bottom are i s the text referred to as
a, 1, c, d .
FIG.8. Photographic record of the proton signal from
water. The three traces from top to bottom correspond to
the situation a, b, c of Fig. 7.