You are on page 1of 5

LABORATORY REPORT OF MATERIALS PHYSICS 2022 1

Nuclear Magnetic Resonance (NMR)


Measurement of Proton and Fluorine
Ferdiansyah Iqbal Rafandi (A877V0)
Master Program in Materials Science, Eötvös Loránd University

Abstract — This report explains the conducted nuclear magnetic where v is the speed of the particle. According to
resonance for water and Teflon sample which represent proton electromagnetic theory, this circular motion of the charged
and fluorine respectively. Firstly, proton sample was measured to particle creates a loop current, which carries a magnetic
see its g-factor, from the measurement it was obtained that the g- moment .
factor of proton is 3.00144 and for the fluorine is 2.83155.
Another observation was also performed to investigate the
frequency shift due inhomogeneous magnetic field which was
produced due to replacement of sample from the middle of (2)
distance between two magnetic cores. It was obtained that as the
distance was farther from the center, the frequency shift become
larger. Here, is the vector, with its magnitude equal to the area of
the loop, and its direction described by the right-hand rule
Kaywords — magnetic resonance, g-factor, proton, fluorine, following the direction of the loop current, which is
frequency. represented by unit vector . Meanwhile, such a gyration
motion (rotation motion) also can be quantified by an angular
I. INTRODUCTION momentum :

A toms are the basic composition units in chemical and


biological area. Each atom consists of a nucleus with
one or more surrounding electrons. Molecules are
(3)

constructed by bonding valence electrons of different atoms. The ratio between and is the gyromagnetic ratio γ:
The arrangements of valence electrons in these bonds show
the chemical properties of the molecule. For example, the
same carbon atom in a CO2 molecule behaves differently to
that in a CO molecule. The variations of the bonding between (4)
valence electrons also affect NMR signals, manifested as
shifts in NMR signals, called chemical shifts. This correlation So, this classical picture shows that the gyromagnetic ratio is
is used to derive the protein secondary structure, or electronic related to the charge and mass of the particle.
and magnetic properties in various insulators, conductors, and However, classical mechanics is not the most accurate
superconductors. theoretical framework to describe microscopic particles such
The diameter of an atom, for example, a helium atom, is as nuclei or electrons. So, quantum mechanics is required and
roughly 1 Å (10-10 m). The nucleus occupies only a tiny spot at for an isolated (noninteracting) charged particle, the
the center, with a diameter of around 1 fm (10-15 m). Outside Hamiltonian H is:
the nucleus, the electrons are moving about at high speed. The
ratio of the electrons’ speed to the speed of light is
proportional to the charge of the nucleus and the fine-structure (5)
constant (1/137). However, the location of the electrons
cannot be precisely determined at any specific time if the where is the momentum operator
velocity is measured precisely. Instead, quantum mechanics
uses the wave function φ(r) to represent the probabilistic
, is the vector
distribution of their locations, which is often described as the
electron cloud. Their most probable locations around the potential associated with the magnetic field,
nucleus resemble the orbits of the planets in the solar system, , and ϕ is the scalar field associated with the
so they are called atomic orbitals.
The nucleus as a charged particle q in the classical picture.
When a charged particle q adopts a uniform circular motion electric field, .
with a radius of r and period T, it produces a current. The particle is assumed that exists in a vacuum, where the
magnetization associated with the medium vacuum is 0, so
magnetic induction or magnetic field density comes entirely
(1) from the magnetic field strength .
LABORATORY REPORT OF MATERIALS PHYSICS 2022 2

Using the vector potential, and assuming all fields have no


time dependence,
(13)

(6)
where ge for electrons is about 2, as can be measured by the
This expression is equivalent to saying that we have an one-electron cyclotron.
Pauli introduced two concepts in 1924 to explain hyperfine
external magnetic field along in direction . structure found in some optical spectra: a nuclear angular
The corresponding x, y, and z components of the vector momentum, and a nuclear magnetic moment. Precise
potential are , and . Hence, experimental demonstration of the validity of these concepts
the Hamiltonian H can be rewritten as: was not possible with the then existing optical techniques. It
was not until molecular-beam techniques were devised by
Stern and Gerlach (Germany 1933), and refined by Rabi,
Millman, Zacharias, and Kusch (Columbia University 1939),
(7) that a precise determination of a nuclear magnetic moment
was possible. Utilization of experimental techniques
where the subscript i represents the x, y, and z components. developed during World War II permitted two experiments to
Rearranging the equation, we get be reported independently in 1946, by Purcell, Torrey, and
Pound (Nuclear Magnetic Absorption) at Harvard University,
and Bloch, Hansen, and Packard (Nuclear Induction) at
(8) Stanford University. The Purcell group's method was to
measure the energy absorbed by a bulk sample at resonance,
Recall the definition of angular momentum in Eq. (3). while Bloch's examined the signal transferred between
. orthogonal coils by a bulk sample at resonance. The simpler
(9) absorption technique (as defined by Bloembergen, Purcell, and
Pound) is the one used for this experiment, with the
experimental arrangement illustrated in Fig. 1.
So, it can be seen that . Hence, we can
rewrite this as:

(10)

with H = Ha + Hb + Hc, in which ,


, and . The Hb term
describes the interaction of angular momentum with external
magnetic field, which is called the Zeeman effect or Zeeman
interaction: Figure 1. Schematic diagram of major components in nuclear magnetic
resonance absorption apparatus

(11)
II. EXPERIMENTAL DETAILS
Here, ω0 is the Larmor frequency. By comparing to Hb, the A. Materials and Equipment
gyromagnetic ratio γ is
In this experiment, we used water which is mixed with
paramagnetic salt for measurement of the resonance of the
(12) proton. Besides, teflon sampe was also used to measure its
fluorine resonance. A plastic bars with different thicknesses (2
Note that Eq. 12 has an extra factor of c in the denominator, cm, 3 cm, 4 cm and 5 cm) were also utilized to create the
compared to Eq. 4. This is because we used the formula in cgs distance between sample and two coils in order to measure the
units in the quantum mechanical derivation above, while SI inhomogeneity of magnetic field.
and cgs units assume the same format as for the classical For the measurement of nuclear magnetic resonance,
mechanical derivation. To convert to SI units, all charges have homogeneous magnetic was produced by big iron core
to be multiplied by a factor of c. Then the quantum electromagnetic coil with thousand of turns with some 0.5 – 2
mechanical derivation of gyromagnetic ratio is the same as the DC flows. This DC flow is modulated to create better
previous classical derivation. With more rigorous derivation, resonance. This coil can also detect the absorption due to
beyond the scope of this book, the gyromagnetic ratio is.
LABORATORY REPORT OF MATERIALS PHYSICS 2022 3

resonance, which is also connected to oscillator circuit. The peaks in the same time, however these 2 peaks were not in the
schematic diagram of measurement apparatus is showed in same position. After that, it was just adjusted so that these two
Figure 2. peaks overlapped each other. The next step was that we must
look for floating interference between antenna and the
frequency that we have set from the signal generator box by
increasing or decreasing the frquency value more or less close
to 5,5 MHz. The floating interference was indicated by the
movement of amplitude up and frequency goes down. Once,
we reached this position, the magnetic field in the middle of
gap near to sample was measured with magnetometer and the
exact value of frequency in the antenna generator was noted.
The same measurement was conducted for 4, 4.5, 5, 6, 6.5, 7,
7.5 and 8 MHz. After that the result was plotted and curve
fitting was performed by using linear function. The g factor of
proton can be determined as the interception value of the
result from linear fitting.
Afterwards, the resonance of fluorine measurement was
Figure 2. Schematic diagram of measurement apparatus performed. By assuming that the ratio between g-factor of
proton and g-factor of fluorine is around 1,06, we can find
easily the g-factor of florine once we know the value of g-
factor from proton. However, in this experiment, we proved
that the ratio of g-factor between proton and fluorine is 1,06.
So, first the resonance like proton was investigated using
water sample. In my case, the freuqency was set to 5,5 MHz in
signal generator box. Once we found the resonance, then value
of magnetic field was measured and immediately the sample
was changed into teflon. Because we changed the material,
then we must adjust in oscillator that we should see 2 peaks
which overlapped each other. Then, the floating interference
was explored by approximating some value more or less near
to 5,5 MHz, once the signal was transformed by the upper
movement of amplitude and lower movement of frequency.
The value of exact frequeny was noted. Subsequently, we
changed again the sample again to water and we looked for the
floatinf interference due to sample changing, the exact value
of frequency was note down. Once we collected, the frequency
of proton and fluorine, we can prove that the ratio between it
Figure 3. The photograph of nuclear magnetic resonance absorption should be 1,06. So we can find the value of g-factor of
apparatus in the laboratory fluorine from the calculated g-factor of proton in the curve
fitting process.
B. Experimental Method The last measurement was inhomogenities of magnetic field.
In the beginning, we need to set up the apparatus. The We put some barriers using plastic bar to create some distance
multimeter was switched on and the unit was set into ampere of the sample from the middle of the gap. The resonance
to measure the current. Besides, we must make sure that the measurements were performed as other measurement for each
resistance must show a zero value so the current can flow different thickness of plastic bar. The frequencies shown in
constantly. The current will go to many loops of iron core and antenna generator were written down and the curve due to
in the gap between two iron core loop, the sample was placed effect of distance was then plotted.
with the holder.
Then, water sample was placed in the middle of the gap III. RESULTS AND DISCUSSION
between two loop. The frequency was set to 20 Hz. The
current generator was turned on and the intensity of current A. G-factor determination of Proton
was increased by rotating the arbitary unit rotator, while the The result of resonance measurement which showed by
increment of current was examined in multimeter and showing frequency and the magnetic field produced were plotted in
1,35 A. Constant magnetic field and small modulation must be Figure 4. It can be seen from the figure that; the value of
set up using modulator. After that, the resonance was observed magnetic field increase as the frequency is also improved. It
by put the value of signal generator at 5,5 MHz. While, in the proves that frequency is linear with magnetic field.
screen of oscillator, we found the resonance when there were 2
LABORATORY REPORT OF MATERIALS PHYSICS 2022 4

µN is nuclear magneton and from reference the value of


nuclear magneton is 5,05 x 10-27 J/T. By substituting the
Planck constant then we obtained the value of g-factor for
proton is 3.00144.

B. G-Factor Determination of Fluorine


The measurement was conducted with finding resonance like
proton at 5,5 MHz. The measured magnetic field was 139,4
mT and the obtained frequency value for fluor is 5,705 and for
proton is 6,068. If we compare this value then we can get a
ratio of frequency between proton and fluorine which has the
value around 1,06 and with this relationship, we can determine
the value of g-factor for Fluorine.

Figure 4. Scattered plot of resonance measurement result (15)

Subsequently, linear curve fitting was performed from these Since we have g-factor for proton from the previous
scattered plot result. The curve fitting was conducted using measurement, then we can obtain the g-factor of fluorine is
OriginLab 2019 software. The result of curve fitting is 2.83155.
depicted in Figure 5. From this linear curve fitting, we will
obtain the intercept and slope of linear line, which are 0.9551 C. Inhomogeneity of Magnetic Field Measurement
and 22.87519. With this value then we can construct the linear
The resonance was observed using frequency 7,5 MHz. The
relation equation which connects the frequency and magnetic
sample was placed from 1 cm, 3 cm, 4 cm and 5 cm from the
field, which can be written as:
center. As the distance was introduced, the peak in
oscilloscope showing a shifting, and this curve shifting were
recorded for every distance which is depicted in Figure 6.
(13)

Figure 6. Peak shifting from the center of distance between two magnetic
cores
Figure 5. Linear curve fitting result

Besides, the frequency measured was also shifted in the


The obtain slope value from linear curve fitting can be utilized oscilloscope, the value of frequency shift can be seen in Figure
to determine the g-factor from the proton. In this case, we can 7. The position of the sample plays a key role due to frequency
use relation which is express by equation 14. And the division shift because the excitation coil that envelops the sample
of frequency and magnetic field represents the slope itself. should always be positioned properly, because the capacitive
coupling between the magnetic core metal and the coil for the
(14) sample can induce a frequency shift. Therefore, we can see
LABORATORY REPORT OF MATERIALS PHYSICS 2022 5

that once we give the distance from the middle distance


between two magnetic core metal, the frequency shift just
occurred. As the distance increase, the frequency shift become
larger as well.

Figure 7. Frequency shift from the the center of distance between two
magnetic cores

IV. CONCLUSION
Thus, the result of experiments showed that the g-factor of
proton and fluorine and can be observed from the magnetic
resonance using two magnetic cores which was made from
vast number of loops of coil and were transmitted by such
value of current. For proton from water sample, the g-factor
was obtained with value of 3.00144. While for Fluorine, the g-
factor was obtained using the ration between resonance
frequency of proton and fluorine which is 2.83155. The effect
of inhomogeneous magnetic field was also observed by
placing the sample for some centimeters from the middle of
distance between two magnetic cores. It was observed that,
due to inhomogeneous magnetic field, the resonance
frequency was shifted and it can observed from the
oscilloscope that there were some peak shift.

REFERENCES
[1] G. E. Maciel. Nuclear Magnetic Resonance in Modern Technology.
Springer Science+Business Media Dordrecht. (1994).
[2] H. Günther. NMR Spectroscopy: Basic Principles, Concepts, and
Applications in Chemistry. Wiley-VCH Verlag GmbH & Co, Weinheim
– Germany. (2013).
[3] S.E. Ashbrook, J. M. Griffin, K.E. Johnston. ‘Recent Advances in Solid-
State Nuclear Magnetic Resonance Spectroscopy’. Annu. Rev. Anal.
Chem. 11:1.1–1.24. (2018).
[4] B. Chen. Fundamentals of Recoupling and Decoupling Techniques in
Solid State NMR. AIP Publishing (online), Melville, New York. (2020).
[5] A. J. Olaide, E. Olugbenga, D. Abimbola. ‘A Review of the Application
of Nuclear Magnetic Resonance in Petroleum Industry’. International
Journal of Geosciences 11, 145-169. (2020).
[6] S. G. Karshenboim, V.G. Ivanov. ‘The g Factor of the Proton’. Physics
Letters B 566 27–34. (2005).

You might also like