C. R.

Chimie 22 (2019) 695e711

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Designing and building a low-cost portable FT-NMR

spectrometer in 2019: A modern challenge
Concevoir et construire un spectrom

bas coût en
etre FT-RMN portable a
2019 : un d
efi moderne
Alain Louis-Joseph a, c, *, Philippe Lesot b, c
a
D 
epartement de physique, Ecole polytechnique, Laboratoire de physique de la mati
ere condens 
ee (PMC), Ecole polytechnique, Centre
national de la recherche scientifique (CNRS), IP Paris, 91128 Palaiseau cedex, France
b 
Equipe de RMN en milieu orient e, Universit
e de Paris-Sud/Paris-Saclay, Institut de chimie mol
eculaire et des mat
eriaux d’Orsay
(ICMMO), UMR CNRS 8182, Ba ^t. 410, 91405 Orsay cedex, France
c
Centre national de la recherche scientifique (CNRS), 3, rue Michel-Ange, 75016, Paris, France

a r t i c l e i n f o a b s t r a c t

Article history: High-field Fourier-Transform Nuclear Magnetic Resonance (FT-NMR) spectroscopy is a

Received 8 April 2019 high performance spectroscopic technique that is essential in many analytical fields. The
Accepted 1 July 2019 non-destructive nature of NMR makes it a preferred means of analyzing chemical and
Available online 4 September 2019
biological environments. Compact benchtop NMR spectrometers are low-cost alternatives
to conventional high-field and high-resolution spectrometers. A research laboratory may
Keywords:
want to develop its own compact FT-NMR spectrometer ("home-built benchtop NMR")
FT-NMR
with a very low financial cost (~10 kV). But why? First of all, to use it punctually as an
Home-built
additional channel (nucleus X) to a high-resolution spectrometer, and also to be able to
Benchtop
couple it with complementary physics instruments such as an optical microscope to study
Low cost
spin diffusion in semiconductors, for instance. In addition, a "home-built" NMR spec-
Electronics
trometer can be used with a low-field permanent magnet for the quantification of species
that does not necessarily require high-resolution, avoiding the need for weekly and
expensive cryogenic services. Outside the research laboratory, this portable NMR can be
used for the in situ analysis of outdoor natural environments. Finally, this compact spec-
trometer is naturally dedicated to the teaching of NMR technique and is open to the study
of the basic electronic functions that constitute an NMR spectrometer. The main question
then arises: how to build a robust "Home-Built” NMR? In this article, we describe the
realization of an NMR instrument based on electronic components and boards (LNA, ADC,
FPGA, ARM, DDS…) easily commercially available, allowing one to obtain a benchtop NMR
instrument presenting both a high acquisition dynamics and a good signal-to-noise ratio.
© 2019 Académie des sciences. Published by Elsevier Masson SAS. This is an open access article
under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).


* Corresponding author. Departement de physique, Ecole
re condense
polytechnique, Laboratoire de physique de la matie 
e (PMC), Ecole polytechnique,
Centre national de la recherche scientifique (CNRS), IP Paris, 91128 Palaiseau cedex, France.
E-mail address: [email protected] (A. Louis-Joseph).

https://doi.org/10.1016/j.crci.2019.07.001
1631-0748/© 2019 Académie des sciences. Published by Elsevier Masson SAS. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
696 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711

r é s u m é

Mots cl
es: La RMN
a transforme e de Fourier (RMN FT) et a
hauts champs est une technique spec-
RMN
a TF troscopique tre
s performante et incontournable dans de nombreux domaines analytiques.
Benchtop Le caracte
re non destructif de la RMN en fait un moyen privile gie
 pour analyser les milieux
Bas coût en chimie et en biologie. Les spectrome
tres RMN a
TF compacts, dits aussi de paillasse, sont

Electronique des alternatives, a
bas coût, aux spectrome
tres classiques hauts champs et haute
solution. Un laboratoire de recherche peut vouloir de
re velopper son propre spectrome
tre
RMN compact (home-built benchtop NMR)
a un coût tre
s re
duit (~10 kV). Mais pourquoi ?
Tout d'abord, pour l'utiliser de façon ponctuelle comme canal supple mentaire (noyau X) a

un spectrome
tre haute re solution, mais aussi pour pouvoir le coupler a
d'autres
instruments de physique, comme par exemple a
un microscope optique, pour l’e tude de la
diffusion de spin dans les semi-conducteurs. Par ailleurs, une RMN home-built peut e ^tre
e avec un aimant permanent bas champ pour la quantification d'espe
utilise
ces qui ne
necessitent pas ne cessairement une haute re solution, e vitant le recours a
des services
cryoge niques hebdomadaires et coûteux. Hors laboratoires de recherche, cette RMN
portable peut e ^tre utilise
e pour l'analyse in situ de milieux naturels en exte rieur. Enfin, ce
spectrome
tre compact est naturellement de die
a
l'enseignement de la spectroscopie RMN,
en etant ouvert
tude des fonctions e
a l’e lectroniques de base constituant l'instrument. La
question principale qui se pose alors est : comment construire aujourd'hui un spec-
trome
tre « maison »? Nous de crivons dans cet article la re alisation d'un spectrome
tre RMN
base sur des composants et des cartes e lectroniques (LNA, ADC, FPGA, ARM, DDS…) ac-
cessibles commercialement et permettant d'obtenir une RMN de paillasse pre sentant a
la
fois une grande dynamique d'acquisition et de bons rapports signal/bruit.
© 2019 Académie des sciences. Published by Elsevier Masson SAS. This is an open access article
under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction to 10
4) and stability and the significant improvement in

electronic performance make it possible to offer very
Conceived and explored in 1945 in physics laboratories compact, versatile benchtop FT-NMR spectrometers at a
[1e5], Nuclear Magnetic Resonance (NMR) spectroscopy is reduced cost, making again this new generation of instru-
arguably nowadays one of the most essential tools for ment very attractive for various applications in chemistry
analyzing the structure of mineral, organic, or biological [17].
molecular systems. This fantastic achievement was In this article, we propose to revisit the development
possible with the development of Fourier-Transform NMR and assembly of a very low-cost (~10 Keuros), portable
(FT-NMR) proposed by R.R. Ernst [6], that in turn opened (benchtop) FT-NMR spectrometer by integrating magnetic
the door to first NMR experiments based on sophisticated and electronic classical elements. For this, the essential
multipulse sequences [7,8]. Concomitantly, the application units required will be described, detailing their respective
of NMR principles/concepts has also offered fundamental role in the excitation/detection process of signal, for
opportunities for medical imaging for robust diagnostic instance. In a memorial approach, in particular, toward
purposes. Behind the vast practical aspects of analysis of chemists who have generally forgotten the NMR principles,
matter, NMR basics underlie varied and sophisticated we will start from some (important) basic physical princi-
theoretical concepts in physics (data sampling), mathe- ples of NMR to organize and choose the key block elements
matics (Fourier Transform (FT) principle), electronics necessary for the realization of this "artisanal" or home-
(resonating circuit), or quantum mechanics (Hamiltonian, made (as anglicists would say) spectrometer. Interest-
operator density…), as nicely described in many theoret- ingly, such a project is possible with laboratory instru-
ical/practical books that are references for any NMR spec- mentation (function generator, oscilloscope…) accessible
troscopists or experienced users [9e16]. at a lower cost. All requested, specific electronic compo-
As a brief reminder, Table 1 provides a chronological nents/devices with their current nomenclature are listed in
summary of the main technological/methodological ad- Appendix and are commercially available.
vances from the 1950s to the present days, in conjunction Proposing an inexpensive, home-made FT-NMR instru-
with the magnetic field strength for a continuous enhanced ment is above all an exciting task of engineering integrated
spectral resolution and sensitivity. into an educational project, for instance. It obviously cannot
Unfortunately, the increasing "race of Tesla" has a sig- be considered as a competition with the new generation of
nificant financial cost (purchase) and periodic maintenance benchtop FT-NMR spectrometers available in the market
(cryofluids), and hence the need for cryofluid-free, FT-NMR today from different manufacturers (Magritek, Oxford,
spectrometers is becoming acute again. In addition, Thermofisher, Nanalysis…), which integrates many
nowadays, the availability of rather small permanent optional modules (locking, sample spinning…) [17].
magnets (soft iron) with a good magnetic homogeneity (up Moreover, although the overall cost (material/electronic
 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711 697

Table 1
Historical overview of main instrumental/methodological achievements.

CW-NMR FT-NMR
NMR
methodology 1D 2D 2D heteronuclear 3D, 4D, TROSY FAST NMR
homonuclear gradients …

Supraconductor Ultra shielded magnet, cryogenic probe

magnet
Size of analyzable
molecules (kDa) < 10 25 35 50 100

B0 (T) 0.70 1.41 2.11 4.22 6.34 9.39 11.74 14.09 17.61 18.78 21.13 22.32 23.48

1
H Larmor (MHz) 30 60 90 180 270 400 500 600 750 800 900 950 1000

Microprocessors 4004 8080 80490 Pentium 4 Intel

Intel family name Core i7

Number of
transistors in 2.3 u 103 6 u 103 1.2 u 106 9.5 u 106 42 u 106 291 u 106 1.1 u 109
microprocessors
(Intel family)
1965 1975 1985 1995 2005
Years
1950 1960 1970 1980 1990 2000 2010

supplies) of the instrument seems attractive at first sight, it operating frequency of the hardware circuits has also
does not include the actual human costs (total cost), in increased considerably. Hardware can now operate at fre-
particular in view of its pedagogical dimensions in Aca- quencies of several gigahertz compared to a few hundred
demic Education. This home-built NMR spectrometer can kilohertz in the 1970s. These high working frequencies
be seen as an “alive” support instrument for teaching NMR. allow complex processes to be carried out with extremely
Finally, this type of mobile NMR apparatus is well suited for short times.
scientific research by coupling NMR and another instru- Another huge leap in the field of electronic equipment is
ment (such as a microscope). the memory capacity of components. It is now possible to
To have an idea, the time needed by a single engineer to store and manipulate memory spaces of more than 64
build a one-channel mobile NMR may be estimated as two gigabytes. Data storage is no longer a real limitation and it
months, including the tests (and assuming that all elec- is possible not only to acquire large amounts of data, but
tronic hardware components have been already also to store the ever more sophisticated programs to
purchased). control and process these data.
The frequency synthesis is now digitally based on DDS
2. Contribution of modern electronics (Direct Digital Synthesis) cards over a very wide range of
frequencies with very high accuracy. In Table A1 (nomen-
Electronics has developed considerably in recent de- clature of components) presented in Appendix, we list the
cades, making it possible to build high-performance sys- references of a synthesis unit capable of generating fre-
tems with high functional integration. To illustrate the quencies from a few kHz to more than 300 MHz. Analogi-
evolution of the power of electronic component, we have cally, the sizes and costs of low-noise preamplifier
included the number of transistors integrated on the same components, mixers, and other hardware have been
chip over the years in Table 1. For example in 1965, a reduced. For example, the low-noise preamplifiers in the
microprocessor integrated nearly 2000 transistors on the acquisition chain can be made with a few circuits for a
semiconductor chip. The density of the components has hundred euros.
increased by a factor of 106 in 45 years (1965e2010), Finally, an important point to keep in mind is the
thereby reducing the size of the electronic circuits. reduction of the energy consumption of modern compo-
Currently, a simple integrated circuit is capable of per- nents, allowing complete battery-powered systems to be
forming signal acquisition, processing, and control func- powered, making them autonomous and therefore
tions. The modern smartphone is a blatant illustration of portable. This aspect was unthinkable in the 1980s. In
the high-tech concentrate contained in such a small vol- summary, the performance of electronic components has
ume. As the density of the components increases, the increased while sizes and costs have been reduced, so the
698 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711

realization of complex units such as a small NMR spec- NMR is often defined as rather insensitive and high-field
trometer is possible in research laboratories. magnets are needed to achieve robust sensitivity and res-
olution to analyze complex molecules. In high-resolution
3. Some specificities of a benchtop FT-NMR NMR, chemical shifts must be measured with a resolution
spectrometer of about 0.01 ppm to solve the J couplings of a few Hertz.
Magnetic fields are of the order of several Tesla and are
Classical or benchtop/mobile FT-NMR spectrometer is a generated by superconducting magnets cooled by helium
complex instrument, but it can be easily divided into and liquid nitrogen. A system of compensation for in-
distinct and clearly identified functional blocks [18]. In homogeneity (shims) is essential to obtain the required
practice, this instrumentation involves many domains of resolution.
electronics such as radiofrequency (RF), audio chain, power Permanent magnets with low field (<0.94 T or 40 MHz
electronics, low-noise preamplification, and transmission for 1H) are called low resolutions due to their low sensi-
lines. In this first decade of the 21st century, FT-NMR tivity and homogeneity. In an inhomogeneous field, the
spectrometers are fully digital and multi-nucleus. Gradu- magnetic strength varies in relation of the spatial position
ally, they are connected by internet, and therefore they can in the magnet. Such effect leads to significant broadening
be remotely controlled and (unfortunately for experi- or/and overlapping of resonance peaks on spectra, thus
menters) fully automated. The two operating modes of FT- preventing exploitable spectral resolution. Nevertheless,
NMR spectrometers (excitation and detection steps) are the measurement of distribution of relaxation times or
performed by fast microprocessors and executed by suit- diffusion coefficients of molecules is accessible at low
able softwares. fields. Quantitative analysises are also possible. The char-
As a matter of principle, the channels (1H, 13C, X…) of acterization of materials (liquid, powder) can be carried out
spectrometers are similar but independent of each other, all at low resolution with a home-made spectrometer that is
of them are synchronized by a master clock; a dedicated much less cumbersome, less expensive in cryogenic
pulse sequencer controlling the complex multi-channel maintenance, and accessible because it is close to the
pulse sequences of the spectrometer. This sequencer synthetic bench of molecules. The latter reduces the cost
takes into account the different transmission delays and and workflow of any research activity. The mobile NMR
hardware dead times (such as the pre-scan delay) to pro- spectrometer we are describing is part of this approach: it
duce a reliable and precise pulse timing controlled by the is compact and can be used with a low-field magnet at
software. The duration of the (hard or soft) electromagnetic Larmor frequencies ranging from 1 to 15 MHz in the set
pulses (ms to ms) and the delays between events (ms to s) presented.
are those actually achieved by the electronics, without the Although intended for low-field, low-frequency appli-
need to add small compensation delays in the pulse pro- cations, as mentioned above, the design and electronic
grams. These specificities are made possible, thanks to the components of our mobile NMR spectrometer can operate
very high speed and stability of modern electronics. at frequencies up to 300 MHz (see the Table in the
The assembly of mobile NMR consists of three distinct Appendix). As a result, this mobile NMR spectrometer can
parts: the magnet, probe, and data acquisition and pro- also be used, without major modifications, at high field
cessing spectrometer. The magnet and probe depend on the using the magnet and the probe part of the industrial
chosen application: low field or high field. We discuss these spectrometer. In this type of application, the interest is
aspects later in this article. methodological: development of a specific auxiliary chan-
The electronics of our mobile NMR spectrometer is nel, magnetization manipulation to control radiation
designed to acquire very low value signals (less than mV) damping, and development of new strategies (multiple
over a high dynamic range (the noise factor of the detection acquisitions).
chain is less than 2 dB), and the sampling is adapted to the
required dynamics (8, 12, 16, or 24 bits). The same applies to 5. Back to the principles of NMR and practical
frequency synthesis and quadratic demodulation, which consequences
can be adapted to a very wide range of frequencies. Note
that all the electronic hardware components (RF power The nucleus of atoms (1H, 13C, 15N, 19F, 31P…) is charac-
amplifier, mixer, preamplifier…) have been chosen to work terized by a quantum quantity, the spin, which is specific to
in a wide frequency range (from 1 to 400 MHz). This allows each nucleus and determines its magnetic properties. The
the portable FT-NMR spectrometer to work at low field magnetic moment, m, of a nucleus is directly related to I by
(with a static permanent magnet) or at high frequency its gyromagnetic ratio, g, which is a constant depending on
(with a superconducting magnet). the nature of the nucleus. The magnetic moment being
quantified, the energy states are degenerated.
4. Sensitivity and resolution When this nucleus is immersed inside the static mag-
netic field, B0, the degeneration of energy level is lifted,
The homogeneity and strength of the magnetic field of a leading to several energy levels according to the spin value
permanent magnet define the sensitivity and spectral res- (Zeeman effect). If the nucleus is then subjected to a
olution of any NMR experiment. The temporal magnetic radiofrequency wave at a specific frequency (Larmor fre-
stability of a magnet obviously limits the duration of the quency), the atomic nucleus will absorb the energy of this
measurements. Homogeneity and magnetic stability must radiation and release it during relaxation mechanisms. This
allow a coherent accumulation of signals in phase. process at the origin of the NMR phenomenon depends on
 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711 699

Fig. 1. Pulse-acquisition 1D NMR experiment. The macroscopic magnetization is aligned along the B0 axis (Oz) at equilibrium state, ideally at the end of the
relaxation delay. After an RF excitation pulse, M0 is flipped in the Oxy plane. The precession of this magnetization gives the impulse response (or FID) which is
detected.

the magnetic field and the properties of the molecules. The is to excite the spin system with a (generally short) RF pulse
study and measurement of an isolated atom is not possible to remove it from its equilibrium state by tilting the M0
due to a lack of sensitivity of NMR; the result is that we are magnetization in the xy plane (see Fig. 1). The return of M0
still dealing with a very large set of nuclear spins, the to equilibrium (denoted Free Induction Decay (FID)) is then
macroscopic result of which we will measure: magnetiza- detected and processed by FT to obtain a frequency spec-
tion. In the presence of a magnetic field B0, the resultant of trum in Hertz or expressed in parts per million (ppm). The
macroscopic magnetization is collinear to B0 at equilibrium magnetization, M0, observable for a set of nuclei of spin I, is
and proportional to the spin populations (number of given by the following law:
nuclei).
Under the action of B0, the magnetic moment, m, of any
magnetically active nucleus (I s 0) is subjected to a force, Ng2 ZIðI þ 1Þ
M0 ¼ B0 (3)
3kT
! where T is the sample temperature, N is the number of
C ¼ !
m ^ B 0; (1) nuclei per unit volume, I is the spin of the nucleus, k is the
which causes a spontaneous precessional movement Boltzmann constant, and B0 is the static magnetic field.
around the z axis (// to the B0 axis) at the Larmor frequency In practice, the magnetization, and therefore the sensi-
(resonance condition) (see Fig. 1), tivity of a NMR experiment, is directly dependent on the
value of B0. The exact magnetic-field dependence of the
NMR sensitivity (considering the detection coil) can be
nLarmor ¼ n0 ¼
gB0 =2p (2) written as the energy (E in Joule) detected in a coil of vol-
ume, V, namely:
where g is the gyromagnetic ratio of the considered
nucleus.
At equilibrium, all nuclei of a sample are subjected to B0. E ¼ M0 ·B0 ·V (4)
The resulting macroscopic magnetization (M0) is oriented
along the Oz axis. The first step of any FT-NMR experiment
700 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711

varies between 0.15 and 1.5 T, makes the experimental

NMR detection much more critical.
From an electronic viewpoint, the voltage of detected
signal (before its amplification) is of low amplitude, with
an order of microvolt (mv). In practice, the experimental
conditions as well as the instrumentation electronics
must therefore be optimized to reach acceptable signal-
to-noise ratios (SNR). This challenge can be met, thanks
to the performance of modern electronic components. In
addition, the transmission power required to energize a
frequency band of about 10 kHz (for the 1H nucleus) for a
1 cm3 volume sample is about 11 W (@500 MHz or 11.7 T).
For a low-field spectrometer, an excitation power of about
5 W for a pulse duration of about 20 ms is sufficient to
generate an instantaneous tilting of 90 of M0, i.e. in the xy
plane.

6. NMR instrumentation

Fig. 2. Permanent horizontal magnet and its probe placed at the center of 6.1. The magnet
the magnet gap with a sample tube of 5 mm, inside.

In the applications of this study, we use a permanent

magnet that is sufficiently homogeneous and stable to
where B0 and M0 are the static magnetic field and the provide consistent NMR measurements. Considering the
magnetization per unit of volume, respectively. analytical purposes of low-field NMR and its trans-
A priori, it is therefore preferable to work with high portability, the weight of the permanent magnet to be used
magnetic fields, which are also at the origin of high- must be reasonable (< 80 kg), and generate at least a field of
resolution NMR in liquids. For instance, at room tempera- 0.15 T (1500 Gauss), leading to a resonant frequency for
ture (300 K) and for a B0 field of 11.7 T (500 MHz), the protons around 6.4 MHz. The axis of the magnet is hori-
detectable magnetization is about 3  10
6 (in SI unit), or zontal and perpendicular to the probe (coil), which consists
an energy of about 10
4 mJ for a sample volume V of of a vertical solenoid, and in which the sample is positioned
1 cm3 (E ¼ M0$B0$V). This corresponds to a reception power (5-mm tube) (see Fig. 2).
of about 1 mW for an acquisition time of 0.1 ms. As seen, the The NMR probe (the antenna) is carefully placed at the
strength of detected signal is therefore very low. De facto, magnetic center of the magnet to both excite (with a
using a so-called low-field NMR, where the B0 strength perpendicular field, B1) and detect the signal along one of
the four axes perpendicular to B0 (x,
x, y,
y). The probe
includes its frequency and impedance system (tuning and

Fig. 3. Simplified "block" diagram of an NMR spectrometer.

 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711 701

matching) that is connected to the electronic chain of the in two components of low frequency (separate operations).
equipment. Note that it is easy to add two external coils on These two steps can be controlled by a "programmable
either side of the magnet to produce a field gradient that sequencer" that generates the multiple RF pulses trains and
can potentially be used for possible monodimensional im- controls the delays during the experiment. For very simple
aging applications. As the static magnetic field is not ho- experiments (pulse-acquisition), a laboratory pulse gener-
mogeneous over all the surface of the magnet, it is ator is sufficient. Finally, data processing and visualization
therefore necessary to accurately measure the value of B0 can be performed using a simple oscilloscope, but in a more
for determining the Larmor frequency (n0). To this aim, a modern way using a computer (PC) with its software
field map can be made within the permanent magnet to interface. It should be noted that the probe is connected to
determine the exact value using a gaussmeter (Teslameter) the excitation and reception blocks via a unit called
that is slowly moved into the air gap of the magnet. In our duplexer. This element can be seen as a signal "switcher"
case, the value measured at the center of the air gap is 1492 that aims to protect the preamplifiers of the detection
Gauss, which corresponds to a resonance frequency, n0, of channel from high RF excitation power. The duplexer di-
6.28 MHz for 1H. rects all RF power to the probe during the excitation step
(by closing access to the receiving channel) first, and then
6.2. Excitation vs detection redirects the detected NMR signal to the preamplification/
demodulation chain.
To perform FT-NMR experiments, three steps are For a spectrometer operating at frequencies of the order
necessary: i) create a homogeneous magnetic field, B0; ii) of 15 MHz and with relatively low powers, a simple struc-
excite the spin system to tilt it from its equilibrium state by ture based on a p quarter-wave filter can be used to
means of an excitation coil generating a B1 field perpen- perform this function. It is a design strategy for a very low-
dicular to B0; and iii) detect the FID signal by means of a cost mobile NMR. First, the p filter requires only a few
receiver coil (which is also the same generating the B1 field electronic components at a very low cost (self and capac-
excitation), the whole satisfying the Larmor's resonance ities), capable of withstanding high powers (several Watts).
condition, nexc ¼ ndec z n0. In addition, it works automatically and there is no need to
The "block" diagram setting up the main parts of an control it during acquisition, simplifying any pulse pro-
NMR spectrometer is shown in Fig. 3, which shows the grams. The realization of the circuit is simple and fast. We
permanent magnet and the NMR probe inside the magnet, will describe how to make a quarter-wave duplexer in
an electronic "transmitter" block responsible for exciting Section 8.4 for a frequency around 6.4 MHz. Because the p
the spin system with RF powers of several dozen watts, and filter (or quarter-wave filter) is a circuit tuned to the Larmor
a second "receiver/detection" block that amplifies the FID frequency of the nucleus under consideration, its use is
signal of very low power (mW) and demodulates the signal limited to a small frequency band.

Fig. 4. Schematic description of the NMR spectrometer blocks along with the visualization of some of key signals obtained. Note the presence of the duplexer.
702 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711

For wide band applications (i.e. frequencies from MHz to present in the nomenclature makes it possible to work up
a few hundred MHz), a duplexer based on fast RF electronic to frequencies around 500 MHz. The assembly of the
switches with fast diodes is mandatory. This type of various blocks can be made entirely on a printed circuit
duplexer is much more complex to implement because a board or more simply by connexion components (BNC or
pulse program within a microprocessor must control it. The SMA outputs).
description of such a circuit is out of scope for the version of
the mobile NMR spectrometer we present in this article.
8. Key electronic elements of the spectrometer
We are targeting here a low-cost mobile NMR, with labo-
ratory instrumentation, a duplexer p filter, and a low-field
Let us now review the key elements of the equipment
magnet operating at 0.15 T (or 6.4 MHz for 1H).
(probe, switch, RF preamplifier…) in the order of the syn-
optic block diagram presented in Fig. 4.
6.3. The lock system

An electronic locking system may be easily added to

make the mobile NMR device capable to continously con-
trol the stability of the magnet, to avoid a slow shift of the 8.1. RF pulse generator
magnetic field over time [see for instance, pp. 44 to 50 of
ref. 19]. The lack of lock control can be particularly trou- The first important function of an NMR spectrometer is
blesome when working at high magnetic fields, and/or the generation of the basic frequencies (BF) necessary for
when recording long-term acquisition NMR experiments. excitation/reception of signal. The RF excitation pulse is
Considering the aims (pedagogical aspects), application realized by means of a switch connected to a frequency
domains (1D NMR, detection of abundant nuclei), and the synthesizer and a pulse generator. However, to perform a
cost of this home-made instrument, no locking system has synchronous detection (resonance), part of this frequency
been integrated into the instrument. must be directed to the detection circuit.
The generation of RF pulses can be performed in
7. NMR device synoptic different ways. The first one consists of using a stan-
dard frequency and pulse generator present in any
For clarity, the general electronic diagram of a NMR physicist laboratory. To ensure sufficient stability and
spectrometer is schematically proposed in Fig. 4. As seen, accuracy for NMR, the resolution of the function
the attenuators and tuning/matching circuits are present at generator must be at least 10
6. Typically, an arbitrary
the input and output of the power amplifier to avoid excess function generator of type HP33120A or Agilent 33220A
power that can be harmful to the detection chain. The operating up to 15 and 20 MHz, respectively, with a
excitation step generates one or more RF pulses at the power of 10 dBm is perfectly suited for a low-field NMR
Larmor frequency. These pulses are directed via the spectrometer. For pulses, the pulse generator can also
duplexer to the NMR probe to tilt M0 perpendicularly to the be used to produce square-shaped pulses. For pulses of
z axis. The high-frequency resonance free induction decay the order of 10 ms, a pulse generator with a resolution
signal (HFFID) is then routed via the duplexer to the of less than 100 ns is sufficient (e.g., Keysight 33220A).
detection circuit. The detection circuit includes at least two The time and frequency parameters are adjusted from
very low-noise RF preamplifiers to amplify this HFFID the control panels of these laboratory instruments. In
signal. The signal is then demodulated with an intermedi- this case, only very simple single-pulse sequences are
ate frequency, in quadrature (quadratic detection leading to possible: 90 pulse - acquisition; 180 inversion pulse -
a 90 phase shift of the signal), to generate a real (R) and an acquisition, etc. The primary advantage of laboratory
imaginary (I) component accordingly to Eq. 5, equipment is their availability at a lower cost, their
speed, and simplicity of implementation (no software
development for pulse programs). The second way to
SðtÞ ¼ A  fcosð2pni t þ fÞ þ i sinð2pni t þ fÞg (5) generate pulse sequences is to use a board based on an
where A is the amplitude and f is the phase of the detected Advanced Reduced instruction set computing Machines
(ARM) microcontroller, a Field Programmable Gate Area
signal. This signal is then filtered to eliminate unwanted
(FPGA) unit, and a Direct Digital Synthesis AD9959
frequency components. At the output of the active "low-
(DDS), which allow digital frequencies up to 300 MHz
pass" filter, the signal is lowered to the 10-kHz range (often
to be synthesized. The advantage in this case is to have
wrongly called « audio filter »). The R and I components of a very compact and powerful unit to generate the basic
the signal can then be observed and checked on an oscil- pulses and frequencies. It can be developed, for
loscope or digitized via an analog-to-digital converter example, from an NXPLPC1768 ARM, an Altera Cyclone
(ADC) for further processing. II FPGA [20, 21], and a DDS. This board is capable of
Although the spectrometer is optimized to work around sequencing four fully independent channels. The FPGA
the 6.4 MHz frequency, it can easily operate efficiently over allows the most complex pulse sequences to be per-
a wider band. All the electronic components required for formed, and the ARM component then manages both
the construction of a low-cost NMR spectrometer are listed the system and data processing. This option allows
in Table A1, with the adequate associated nomenclature. stand-alone battery operation for outdoor (off-labora-
The choice of the bandwidths of the various elements tory) use.
 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711 703

Fig. 5. (On Left) Structure of an RF switch based on fast diodes. (On Right) Example of input and output signals from an RF switch. Here, the RF pulse has a length
of 80 ms.

Fig. 6. Electrical diagram of the duplexer, including two diode arrays and the p filter. The p filter has a minimum RF signal at the receiver (port C) when there is a
maximum on the probe (port B). The "noise gate 100 isolates any signal feedback from the probe to the power amplifier to minimize losses during detection. The
"noise gate 200 protects the detection chain from residual voltages eliminated by the p filter.

8.2. The switch 8.3. The RF power amplifier

The role of this circuit is to switch the RF signal for a As our mobile NMR is aimed to work from low to high
controlled pulse duration. This element can be realized by field, it is necessary to have a broadband RF excitation
means of four fast diodes (type 1N4148) mounted in head pulse. The excitation provided to the spin system must be
to tail or with a PS1211 mini-circuit component (switch), sufficiently high, with relatively short RF pulses (10e100
which offers fast switching times (< 500 ns) and very low ms) to excite a bandwidth covering the spectral width of an
channel imbalance (see Fig. 5). observed nucleus. The selected power amplifier must be
able to operate in pulse mode but also in continuous wave
(CW), if nuclear decoupling or any other type of low power
excitation needs to be achieved. It is imperative that the

Fig. 7. (a) Example of a probe made of glass with its integrated capacitive devices Cm and Ct. (b) NMR probe wiring diagram: Cm and Ct are adjustable capacitances
from 5 pF to 500 pF, inductance coil, L ¼ 2e3 mH.
704 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711

amplifier has a good linearity to adjust the RF pulse accu- a choke and two capacitors. The filter input is connected to
rately. A power amplifier generates a high noise level at the the probe (port B) and the output (port C) to the low-noise
output even at rest. It is therefore necessarily not activated. preamplifier chain. For a specific frequency, a quarter-wave
We used for our prototype a ZHL-5W-1 unit operating in a filter has a minimum amplitude at its output (C) when its
frequency range from 1 to 500 MHz. input (B) is maximum. To reinforce the protection of the
preamplifiers, a second network of head-to-tail diodes can
8.4. The duplexer be incorporated to protect the detection circuit by short-
circuiting (at the threshold of the diodes) any residual
As already mentioned above, the duplexer has a very voltages. The filter setting must combine input and output
important role, in particular, to protect, during reception, impedance matching, as well as phase shift and attenuation
the low-noise preamplifier chain from the high RF power at the resonance frequency. The characteristics of the
emitted during excitation. It is a three-port system A, B, and quarter-wave filter were adjusted to the network analyzer
C (see Fig. 6), where the first port (A) is connected to the with the Smith diagrams of the input (S11) and output
power amplifier, the port (B) is connected to the probe, and (S22) impedances as a function of frequency. The input
the output (C) is directed to the low-noise detection pre- (S11) and output (S22) impedances have been adjusted to
amplifier chain. For broadband systems, it is preferable to have an actual value as close as possible to 50 U (in practice
use a switch network electronically controlled by the pulse 44.5 U at the resonance frequency of 6.28 MHz), while
sequencer. In low-frequency (low-field) NMR applications, maintaining a 90 phase shift between the input and
a structure based on diode arrays and a quarter-wave filter output.
can be used; the diagram is shown in Fig. 6. A first network
of four head-to-tail diodes (noise gate 1) acts as an auto- 8.5. The NMR probe
matic switch: these diodes are blocked (open circuit) for
small amplitudes, thus preventing any return of the signal Different probe body shapes (solenoid, saddle coil) can
from the probe to the power amplifier. The quarter-wave be produced and used depending on the adaptability to the
system, referred to as the p filter, has an input (B)/output magnet. The most simple detection antenna consists of a
(C) phase shift of 90 . It is called a quarter wave because it solenoid coil. A probe body made entirely of glass (boro-
has a phase shift optimized at 90 around a given fre- silicate) can be used (see Fig. 7a). For a 10-mm probe, the
quency, in our case, around 6.28 MHz. This filter consists of solenoid is wound on the glass tube with an inner diameter

Fig. 8. Picture showing the measurement of the frequency tuning and impedance matching curve (top) and on the Smith chart (bottom) on a network analyzer.
 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711 705

Fig. 9. Observation of the probe's dead time: about 250 ms. At the top and in the middle are displayed the two quadrature detection channels (yellow and blue). At
the bottom is displayed the rectangular (purple) RF excitation pulse (50 ms of length).

of 10 mm, thus allowing the detection of a large amount of In the model presented in this article, the dead time is
analyte, but small diameter (5 mm) could be used. The about 250 ms before the two quadrature detection channels
capacitive network is integrated into the probe. The sole- return to zero (see Fig. 9). The detection of the useful signal
noid is made of rigid copper wire with a diameter of needs to be delayed by this delay and the detection circuit
1e1.5 mm and includes about 20 turns with a diameter of is reinforced, by a network of diodes, to support the peak
10 mm over a length of 20 mm; the better the quality of the amplitudes of several volts for a few hundred
winding, the smaller the artefacts will be. The elementary microseconds.
structure of the frequency tuning and impedance matching
system is described in Fig. 7b. A network of capacitors 8.6. The receiving chain: radio frequency preamplifier
adjustable from 5 to 500 pF allows frequency tuning (Ct)
and impedance matching (Cm) for a coil of the order of The signal from the probe is too weak and cannot be
2.2 mH. The tuning allows the probe to be adjusted to the used directly, and so it must be amplified. The amplifi-
resonance frequency (n0 z n1 ¼ 1/2p√LC). Impedance cation chain consists of two stages with radiofrequency
matching is performed at this frequency to adjust the probe preamplifiers in series. The noise factor of a preamplifier
circuit to 50 U and minimize the energy losses. cascade is almost equal to that of the first stage. A
Frequency tuning and impedance matching are per- "BA01500" preamplifier with the lowest factor is placed
formed using a network analyzer to accurately position the first, followed by a RF2046 home-made broadband
probe's attenuation peak at the desired resonance frequency preamp unit. The low-noise amplifier LN BA01500-35
while observing the impedance evolution on the Smith chart has a frequency range varying from 0.1 to 500 MHz
(see Fig. 8). Impedance matching consists of refining and with a gain of 35 dB. The intermodulation product
lowering the resonance peak as low as possible to absorb all power at the output is þ12 dBm (output IP3), and the
the energy in the coil. In our case, the resonance is adjusted undistorted input power is
35 dBm (1 dB compression
with the network analyzer at 6.284 MHz, the attenuation point). Thus, the maximum permissible input power is
obtained is
50.816 dB with a very good impedance therefore
35 dBm.
matching (49.72 U), and consequently a good detection
sensitivity is obtained for a low-field spectrometer. The half-
height width obtained at this frequency is 35 kHz, giving a
quality coefficient Q of 179, a very acceptable value.
Once the frequency tuning has been achieved, the sec-
ond important parameter to be estimated is the dead time
(or response time) of the probe (see Fig. 9). The dead time is
the time required for the probe to dissipate the energy
stored during excitation. Some of the excitation energy is
sent to the probe via the duplexer, but once the RF pulse has
disappeared, significant energy remains in the probe. The
higher the quality factor Q of the probe, the higher the dead
time is. This is a disadvantage for detection, because it will
be necessary to delay the measurement of this time: i) not
to destroy the low-noise preamplifiers and ii) not to su-
perimpose the low detection signal on the high amplitude
due to the probe signal. Fig. 10. Structure of a Quadrature Intermediate Frequency Mixer demodu-
lator (QIFM). Mixers: X2L-06e414 from Pulsar Microwave.
706 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711

Fig. 11. 1H signal (one component) of a water sample (5 mm) obtained (one SCAN: NS ¼ 1) after the demodulation stage and low pass filtering, observed on a
digital oscilloscope with FFT. Top: FID component. Bottom: spectrum: presence of the peak at 4.92 KHz. Note the linewidth of 423 Hz. The Larmor frequency was
n0 ¼ 6.4 MHz. The RF excitation pulse length is 50 ms. See Appendix for the details of the experimental setup.

Our home-made preamplifier is made with three At the input of the 90 hybrid divider, we have the
RF2046 components in series: the overall gain of the base frequency of the Local Oscillator (LO) input spec-
channel measured at the network analyzer (without trometer; this is actually the Larmor frequency of the
distortion) is 35 dB at 6 MHz and 31 dB at 1 MHz and the spectrometer. At the input of the 0 divider, we have the
operating frequency range is from DC continuous to FID: this is the high-frequency response RF. At the
1 GHz. The output intermodulation product (IP3) is þ23 output of the quadratic demodulator on channels I
dBm and the noise factor (NF) is equal to 3.8 dB. This (imaginary) and Q (quadratic), the signals are of the
configuration of the elements as well as their perfor- form: i) cos [2p(nrf þ n0)t)] þ cos [2p(nrf
n0)t)]; ii) sin
mances allows us to ensure the detection of signals on a [2p(nrf þ n0)t)]
sin [2p(nrf
n0)t). We therefore obtain
large dynamic range without distortion: typically from two quadrature components with all the "sum" and
some 100 mV to 14 mV. "difference" frequencies of the demodulated signals:
2p(nrf þ n0) and 2p(nrf
n0), plus harmonics. Only low-
frequency signals in the 10-kHz range are interesting,
8.7. Quadrature demodulation and the signal must be filtered to retain only the lowest
frequencies using a low-pass filter.
Quadratic demodulation is based on the principle of
synchronous detection to obtain real and imaginary com- 8.8. Double active audio low-pass filter
ponents of the NMR signal. Its structure is based on a
Quadrature Intermediate Frequency Mixer (QIFM) An active double low-pass filter is required to keep only
demodulator whose schema is given (see Fig. 10). It consists the low frequencies of the demodulated signals (see
of a 90 hybrid splitter, two mixers, and a 0 combiner Fig. 11). Each filter is designed to charge the demodulators
(summing). Each of these elements is listed in the table of on 50 U and consists of two stages allowing an overall gain
components (see Table A1). of about 30 dB in voltage. As around the resonance, the
 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711 707

Fig. 12. (a) No NMR tube: real (high, channel 1) and imaginary (low, channel 2) components at the output of the audio frequency amplifier after an RF excitation
pulse length of 50 ms. (b) Example of one-scan quadrature detection of a low-magnitude 1H signal (5-mm water tube). See Appendix for the experimental setup.

measured frequency differences are about ten kilohertz, the response of both channels as a function of
the filter bandwidths are adjustable over a range from frequency.
100 Hz to 500 KHz.
The two filter channels must be adjusted to have the
same frequency and phase responses throughout the
useful bandwidth. This is to avoid unbalancing between
the real and imaginary components of the signal, which 9. Setting of spectrometer
would degrade the spectrum in frequency (quadrature
artifact, zero frequency…). Precise gain and phase ad- 9.1. Probe control
justments in the bandwidth are made with a network
analyzer, the only true and effective way to visualize The tuning of the probe to the resonance frequency has
been described above.
708 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711

9.2. Cancellation of the DC offsets For this reason, the duration of the pulse is varied until a
magnetization is obtained whose intensity in the xy plane
Any DC voltage offset in the detection circuit generates a is maximum (see Fig. 13). The amplitude variation of the
zero frequency component that will affect the quality of the magnetization vector is observed as a function of the
spectra. To reduce this unwanted effect, it is important to excitation pulse duration. In our case, the pulse duration is
carefully cancel the offset voltages of the active double low- between 13 and 14 ms. Another approach is to determine
pass audio filter to have a signal close to zero when the the pulse duration corresponding to an angle of 180 , for
input signal is nul. which the macroscopic magnetization is then null (tilted
to the
Oz axis).
9.3. Signals at the output of the audio amplifier without
sample 9.6. Increase in the S/N ratio

At first, we work without putting a sample in the The signal-to-noise ratio of an NMR experiment in-
magnet to minimize the imperfections of the assembly: volves numerous factors such as: i) the magnetization M0,
adjustment of the LO level (10 dBm) and cancellation of ii) the filling factor and the quality factor of the probe, iii)
continuous offsets. In the absence of a sample, the voltage the noise factor of the preamplifier, and so on [22]. After
offsets are less than 1 mV. In addition, note that the optimization of all the electronic hardware and parameters,
deadtime of the probe after the RF pulse is 400 ms (see we can also increase the SNR during the acquisition. The
Fig. 12a). SNR can be improved by averaging the FID signals over a
large number of acquisitions (NS scans). Indeed, on an
9.4. Signals at the output of an audio amplifier with sample average of NS acquisitions, the noise will be averaged to-
ward zero due to its random origin, whereas the useful
The imperfections of the assembly having been mini- signal will increase on average. Thus, the SNR is improved
mized, we introduce our sample (a 5-mm tube of water), at the root of NS as displayed in Fig. 14.
and we visualize the precession signals in quadrature
mode (see Fig. 12b). Note the very low magnitude of the 10. Possible applications
signals.
Benchtop FT-NMR allows many applications in chem-
9.5. Optimization of the 90 flip angle istry, such as the analysis or characterization of small
molecules, or the monitoring of chemical reactions. The
The NMR signal obtained at this step, although teaching of NMR methodologies (effects of excitation/
observable, is relatively small in amplitude. To maximize inversion pulses, pulse calibration, optimization of
the amplitude of the FID, it is now necessary to adjust the acquisition parameters, as well as the description of some
strength excitation pulse for a tilting of M0 equal to 90 . experiments as the measurement of relaxation

Fig. 13. Adjustment of the RF excitation pulse duration to obtain a maximized signal corresponding to a 90 pulse.
 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711 709

Fig. 14. Effect of averaging on the SNR. Comparison of the FIDs obtained by adding successively: (a) 2, (b) 32, and (c) 64 scans (5-mm water tube). On (c), note the
vertical line setting at 3.45 kHz. See Appendix for the experimental set up.

parameters, spin echoes…) is also another aspect of their A (home-built) mobile NMR spectrometer can also be
use. The portable low-field NMR is particularly suitable for used to develop projects that aim to couple NMR and op-
nuclei with high natural sensitivity, such as 1H, 19F, 31P, tical microscopy in a semiconductor [23] to locally polarize
and 29Si. However, other « exotic » nuclei with high gy- nuclear spins (dynamic polarization) and measure the
romagnetic ratios such as 7Li, 11B, and 23Na can also be spatial profile of nuclear magnetization using an optically
detected [27,28]. detected NMR, with good spatial resolution. This
710 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711

fundamental study of nuclear spin diffusion does not terminology frequently encountered in the fields of NMR,
require a high magnetic field (less than 0.15 T). For this kind the B1 coil is a resonant LCR circuit tuned to the Larmor
of experiment, NMR functionalities are reduced to signal frequency. This coil is used for the detection and the exci-
excitation and detection for parameter optimization, tation of the nuclei in FT-NMR experiments. L is inductance,
without the need for frequency resolution. C is capacitance, and R is resistance.
CW: Continuous Wave
11. Conclusion dB: Decibel
dBm: Power in decibel: 0 dBm ¼ 1 mW/50 U
The low-field FT-NMR spectrometer presented in this DDS: Direct Digital Synthesis
article is fully operational. This revisited instrument can be FFT: Fast Fourier Transformation
exploited to carry out simple NMR measurements such as FID: Free Induction Decay
the determination of chemical shifts (d), spin echoes, mea- FT: Fourier Transformation
surement of T2(1H) or T1(1H) relaxation times, etc. On the FPGA: Field Programmable Gate Area
other hand, it provides a pedagogical approach to the HFFID: High-Frequency Free Induction Decay
teaching of NMR to students at all levels, from the physical LO: Local Oscillator
concept to the electronic realization through the many M0: Magnetization at equilibrium
possible analysis applications [24, 25, 26]. It is also an NF: Noise Factor
excellent demonstration element at scientific events for a NMR: Nuclear Magnetic Resonance
more general public. Finally, it can be inserted in real ex- Q: Quality factor
periments of physics requiring NMR to be coupled with QIFM: Quadrature Intermediate Frequency Mixer
another measurement technique such as optics, for example. RF: RadioFrequency
Noteworthy technical developments of the instrument SMA: SubMiniature version A (connector)
are possible. Thus if the permanent magnet is equipped SNR: Signal-to-Noise Ratio
with an additional pair of coils with currents in the range of TROSY: Transverse Relaxation Optimal SpectroscopY
1e3 A, it can then be injected to create additional field TTL: Transistors Transistors Logics
gradients to B0. The spectrometer is then able to perform T2: Spinespin relaxation time
some simple 1D imaging experiments or to experimentally T1: Spinelattice relaxation time
measure molecular diffusion coefficients. n0: Larmor frequency (MHz)
Although sensitivity is reduced at low-field strength,
quantification and measurement of relaxation and diffusion
parameters of neat samples or solutions are possible [27, 28].
This kind of portable NMR spectrometer could then appear
Table A1
the ideal tool for outdoor NMR analysis of ecosystems. Characteristics and nomenclature of electronic components.

Characteristics Designation Number Frequency

Conflicts of interest of devices range (MHz)

1500 G permanent magnet, TE2M C4-1367 1 6.2e6.8

The authors declare no conflicts of interest. 40-mm air gap, NMR 1500 G
homogeneity on a useful
diameter of 20 mm,
Acknowledgements
divergent polar pieces on
a diameter of 200 mm,

A.L-J. thanks the physics department of the "Ecole pol- height 400 mm
ytechnique" and its Polytechnician students, as well as the Directional coupler 30 dB, C5-08-411 2 5e1000
LPMC (UMR CNRS 7643) for their contributions to the 3W, SMA (Pulsar)
SMA connector (pulsar) 20 0.1e1000
development of mobile NMR. P.L. thanks CNRS for its sup-
Mixer level 7 dBm SMA X2L-06-414 2 (LO/RF) 1e
port to fundamental research and the divulgation of (Pulsar) 1000: (IF)
fundamental sciences. DC-1000
Power divider/combiner, 2 P2-09-411 3 5e1000
way (0 ), phase balance:
Appendix
2 , amplitude balance:
0.3 dB
Insertion loss 0.8 dB, SMA
Definitions of acronyms and notations used (Pulsar)
90 hybrid power divider QE-01-412 1 2e10
Phase balance 2 , amplitude
ARM: Advanced Reduced instruction set computing balance 0.4 dB, insertion
Machines loss 0.5 dB, SMA (pulsar)
ADC: Analog-to-Digital Converter Low-noise RF preamplifier BA01500-35 1 0.1e500
BNC: Bayonet NeilleConcelman (connector) NF ¼ 2, gain: 35 dB,
RF output power: 5 dBm
B0: Static magnetic field
Absolute maximum rating
BF: Basic Frequency input
B1: RF coil.The term B1 is used to characterize the field, RF power:
35 dBm
in the plane, orthogonal to the static B0 field. In the (Elhyte)
 A. Louis-Joseph, P. Lesot / C. R. Chimie 22 (2019) 695e711 711

Table A1 (continued ) [4] J. Keeler, Understanding NMR Spectroscopy, John Wiley & Sons,
2005, 978-0-470-01786-9.
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of devices range (MHz) [6] R.R. Ernst, W.A. Anderson, Rev. Sci. Instrum. 37 (1966) 93e102.
[7] E.L. Hahn, Phys. Rev. 80 (1950) 580e594.
Low-noise RF preamplifier ZFL1000LNþ 1 0.1e1000
[8] J. Jeener, Lecture notes from the Ampe
re Summer School in Basko
NF ¼ 2.9, gain: 25 dB,
Polje, Yugoslavia, September 1971, later reprinted, in: M. Goldman,
output RF power: 5 dBm M. Porneuf (Eds.), NMR and more, in honor of Anatole Abragam,
(mini circuit) 
Editions de Physique, Les Ulis, France, 1994.
Low-noise RF preamplifier RF2046 3 DC -1000 [9] A. Abragham, Principle of Nuclear Magnetism, Oxford University
RF; NF ¼ 3.8, gain: 23 dB, Press, 1961.
RF output power: 5 dBm [10] I. Solomon, Phys. Rev. 99 (1953) 559e565.
(home made) [11] D. Canet, La RMN: concepts et me 
thodes, InterEditions, Paris, 1991.
Power amplifier ZHL 5W
1 1 [12] A. Abragam, M. Goldman, Nuclear Magnetism Order and Disorder,
Operational amplifier OP27 1 DC - 8 International Series of Monographs in Physics, Oxford University
Operational amplifier OP37 1 DC - 60 Press, New York, 1982.
Resistor 1 kU, 10 kU 10 [13] R.R. Ernst, G. Bodenhausen, A. Wokaun, Principles of Nuclear Mag-
Variable capacitor 5 pFe500 pF 4 netic Resonance in One and Two Dimensions, Clarendon Press,
Oxford, UK, 1987.
Probe (home made) 1 6.1e6.8
[14] M. Goldman, Introduction aux me thodes quantiques de calcul en
Sequencer board with ARM NXPLPC1767þ 1 0.01e301 solution. Centre d'e tudes nucle aires de Saclay,
RMN de haute re
þ DDS (home made) DDS 9959 1 Institut de recherche fondamentale, De partement de physique
Or frequency generator and ge ne
rale, Service de physique du solide et de re sonance magne -
laboratory pulse 
tique. CEA, Palaiseau: GERM, Ecole thematique RMN, Figeac, France,
generator (see text). 1996.
Analog or digital 1 [15] J.-Y. Lallemand, Spectroscopie, re sonance magne tique nucle aire:
oscilloscope with FFT Cours de majeure de chimie, Palaiseau (France), De partement de
AC/DC adapter 24 V/6.4 A AHM150PS24 1 
chimie, Ecole polytechnique, 2003.
Total estimated cost ~10 kV [16] D. Neuhaus, M.P. Williamson, The Nuclear Overhauser Effect in
Structural and Conformational Analysis, VCH Publishers Inc., New
York, 1989.
[17] E. Auguste, E. Lucas, L. Poigniez, D. Ramamurthy, H. Vaneeckhoute,
Experimental setup (except otherwise in the text) P. Lesot, Spectra Anal. 315 (2017) 32e43.
[18] A. Louis-Joseph, RMN: The orie pratique, cours, Enseignement
d'approfondissement, De partement de physique, Ecole  poly-
All NMR and test experiments have been made with the
technique, Palaiseau, France, 2015, pp. 1e197.
electronic setup outlined in Fig. 4. A permanent magnet [19] A.E. Derome, Modern NMR Technique for Chemistry Research,
with a field of 1500 G (6.4 MHz) is used for the static Organic Chemistry Series, vol. 6, Pergamon Press, New York, 1987,
magnetic B0 field (see Fig. 2). A home-made solenoid-type pp. 38e50.
[20] J. Gallegos Pablo Ignacio, A. Louis-Joseph, Pilotage programmable de
probe device and a 5-mm water sample tube were used for spectrome
tre RMN. Conception expe rimentale micro et
the tests. The frequency and the RF pulse duration have naoe lectronique, PHY573A, Rapport d'enseignement d'appro-
fondissement, De partement de physique, Ecole  polytechnique,
been set with the frequency generator and the pulse
Palaiseau, France, 2013.
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[21] A. Louis-Joseph, B. Thie
and processed using some digital oscilloscopes with sen- 
familles 68K/MCF5407. Electronique, composants et syste
mes :
sitivities of 1 or 2 mV/div. enseignement expe rimental, support de cours, De partement de

physique, Ecole polytechnique, Palaiseau, France, 2015, pp. 1e126.
[22] D.I. Hoult, R.E. Richards, J. Magn. Reson. 24 (1976) 71e85.
Characteristics and nomenclature of the electronic [23] D. Paget, Phys. Rev. B 24 (1981) 3776e3793.
[24] A. Bienfait, L. Bonin, R. Antonelli, A. Louis-Joseph, Instrumentation
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Table A1 provides the characteristics and nomenclature technique, Palaiseau, France, 2011.
[25] F. Lan, M. Weiss, Re sonance magne tique nucle aire : construction
of the electronic components used.
tre et application a
un gaussme
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tement de physique, Ecole polytechnique, Palaiseau, France, 2013.
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