Photoacoustics 28 (2022) 100401

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Photoacoustics
journal homepage: www.elsevier.com/locate/pacs

Multi-gas quartz-enhanced photoacoustic sensor for environmental

monitoring exploiting a Vernier effect-based quantum cascade laser
Andrea Zifarelli a, Raffaele De Palo a, Pietro Patimisco a, b, Marilena Giglio a, Angelo Sampaolo a, b,
Stéphane Blaser c, Jérémy Butet c, Olivier Landry c, Antoine Müller c, Vincenzo Spagnolo c, *
a
PolySense Lab - Dipartimento Interateneo di Fisica, University and Politecnico of Bari, Via Amendola 173, Bari, Italy
b
PolySense Innovations Srl, Via Amendola 173, Bari, Italy
c
Alpes Lasers SA, Avenue des Pâquiers 1, 2072 St-Blaise, Switzerland

A R T I C L E I N F O A B S T R A C T

Keywords: We report on a gas sensor based on quartz-enhanced photoacoustic spectroscopy (QEPAS) able to detect multiple
QEPAS gas species for environmental monitoring applications, by exploiting a Vernier effect-based quantum cascade
Widely tunable QCL laser as the excitation source. The device emission spectrum consists of ten separated emission clusters covering
Multi-gas sensing
the range from 2100 up to 2250 cm− 1. Four clusters were selected to detect the absorption features of carbon
Environmental monitoring
monoxide (CO), nitrous oxide (N2O), carbon dioxide (CO2), and water vapor (H2O), respectively. The sensor was
calibrated with certified concentrations of CO, N2O and CO2 in a wet nitrogen matrix. The H2O absorption
feature was used to monitor the water vapor within the gas line during the calibration. Minimum detection limits
of 6 ppb, 7 ppb, and 70 ppm were achieved for CO, N2O and CO2, respectively, at 100 ms of integration time. As
proof of concept, the QEPAS sensor was tested by continuously sampling indoor laboratory air and monitoring
the analytes concentrations.

1. Introduction gas sensors and electrochemical sensors [11]. Gas chromatography

represents a solid benchmark for the analysis of gas samples, but its
The pressing demand for gas sensing solutions in the field of envi­ application is still limited in the case of real-time, in situ monitoring
ronmental monitoring relies on the multiple benefits that the protection [12]. Conversely, gas sensors based on chemical reaction between the
of the environment reflects on human life and health [1,2]. The moni­ target analyte and the sensing element are suitable for in situ and
toring of the air contaminants concentration leads to a better under­ real-time analysis, but their response is affected by long recovery time as
standing of the emission processes and allows the mapping of the well as poor selectivity and cross sensitivity [13]. Gas sensors based on
emission sources, for both outdoor and indoor environments [3,4]. With optical detection techniques are a promising alternative for noninvasive
this perspective, the analysis of air pollutants can be considered as a tool measurements with high selectivity and sensitivity, being the perfect
to assist decision making, and to develop strategies aimed at reverse candidates for real-time, on-field operations [14]. Among the optical
negative environmental impacts [5]. Human activities lead to the spectroscopic techniques, quartz-enhanced photoacoustic spectroscopy
emission of greenhouse gases and their precursors, which are the main (QEPAS) has emerged as a reliable and robust technique for the detec­
responsible of global warming increase [6]. In this field, efficient tion of several gas species in trace concentrations [15,16]. QEPAS
monitoring activities require gas sensing technologies able to perform technique represents an evolution of traditional PAS, exploiting a quartz
multi-gas detection [7]. In fact, the evaluation of multiple analytes al­ tuning fork (QTF) to detect the weak sound waves produced by mole­
lows the quantification of the mixing ratio variations as well as the cules absorbing modulated light. The prongs deflection induced by the
analysis of the correlation among the gaseous emissions [8,9]. Quanti­ pressure waves hitting the QTF is converted into an electric current by
tative detection of gases has been traditionally performed with labora­ means of piezoelectric properties of quartz. Therefore, in QEPAS sensors
tory analytical equipment such as gas chromatographs and mass the QTF acts as both detector and transducer, reducing the overall size of
spectrometers [10], and with portable devices such as semiconductor the detection module. In addition, a pair of millimetric resonator

* Correspondence to: Dipartimento Interateneo di Fisica, University and Politecnico of Bari, Via Amendola 173, Bari, Italy.
E-mail address: [email protected] (V. Spagnolo).

https://doi.org/10.1016/j.pacs.2022.100401
Received 21 July 2022; Received in revised form 31 August 2022; Accepted 31 August 2022
Available online 5 September 2022
2213-5979/© 2022 The Authors. Published by Elsevier GmbH. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
A. Zifarelli et al. Photoacoustics 28 (2022) 100401

metallic tubes are typically used to amplify the acoustic waves intensity obtained by varying the laser injection current in the active region,
[17], and, together with the QTF, compose the QEPAS spectrophone. labeled IL. Several approaches have been used to design the front and
The key aspect of QEPAS is that the QTF response is independent of the back gratings, including optimization algorithms [36]. The device used
light source wavelength employed to excite the gas target; thus the same in this work is composed of distributed Bragg reflectors (DBR), resulting
detection module can operate with laser sources emitting in a wide in constant cluster jumps [37]. Therefore, the emission wavelength of
range of wavelengths from UV to THz, making QEPAS an ideal technique the QCL can be selected using a specific combination of IF, IB and IL and
for multi-gas detection [18,19]. Therefore, the focus for multi-gas tuned to address specific absorption lines. As a first step, the spectral
detection is completely shifted to the laser source. Multi-gas detection emission of the laser device was characterized employing an optical
with standard DFB laser diodes is limited by the tunability range of the spectrum analyzer (Thorlabs OSA207C) with a spectral resolution of
source, typically few cm− 1 in the mid-IR for standard quantum cascade 0.25 cm− 1. The laser temperature was set to 0 ◦ C, employing a water
lasers (QCLs) and interband cascade lasers [20–23]. Moreover, the cooler (ThermoCube 200 W) as a thermal bath and driving the
selected absorption features can overlap, thus compromising the selec­ Peltier-effect cooler integrated in the laser packaging with the Arroyo
tivity of the developed sensor and often requiring complex statistical 5300 Series thermo-electrical cooler (TEC). This temperature was set
tools to retrieve analytes concentrations [24]. Semiconductor laser throughout all the measurements. The two heaters were alternatively
sources with broader spectral emission, as arrays of QCLs or external switched on, thus providing two different electrical configurations: (IL,
cavity QCLs [25–27]. can be used to extend the emission spectral range, IF, IB = 0) or (IL, IF = 0, IB). These configurations were explored by
but the spectral selectivity is still restricted by the laser source resolu­ varying both the heater current (IF or IB) and the laser injection current
tion. An alternative approach is to use an array configuration, namely (IL), mapping the emission range of the device and acquiring the cor­
multiple laser sources emitting at different spectral ranges, each one responding output power. The laser was controlled using three laser
targeting a single absorption feature, arranged in a single housing. current drivers, one for each section. The QCL section was driven using
Nevertheless, this approach complicates the sensor architecture an ILX Lightwave LDX-3232, while two Arroyo 4300 Series current
requiring for additional sensing modules and complex spectrophone drivers were used to inject current into the Front and Back sections. With
configuration [28,29]. IL varying in its dynamic range from 590 mA to 850 mA, IF was varied
In this work, an innovative Vernier effect-based QCL was employed from 450 mA to 1100 mA while IB = 0; conversely, IB was varied from
as the light source for a QEPAS sensor to detect multiple analytes with 450 mA to 1100 mA while IF = 0. The device was also operated as a
strong relevance for environmental monitoring, i.e., carbon monoxide traditional QCL with the configuration (IL, IF = 0, IB = 0). As represen­
(CO), nitrous oxide (N2O), carbon dioxide (CO2) and water vapor (H2O). tative, the laser emissions corresponding to six electrical configurations
The unique emission properties of this source allow the targeting of well- are shown in Fig. 1a–b. These spectra were acquired by setting IL = 840
separated absorption features in a broad spectral range, providing high mA, and IF (Fig. 1a) or IB (Fig. 1b) at three different values.
selectivity together with state-of-the-art sensitivity levels. The sensor The whole laser emission range is reported in Fig. 1c. For each
calibration was performed on CO, N2O and CO2 in a wet nitrogen matrix. collected spectrum, the center wavenumber was extracted and is plotted
The H2O concentration in the gas line was fixed to prevent alterations in together with the corresponding optical power value. All measurements
the QEPAS signal due to energy relaxation effects [30,31]. Finally, the
QEPAS sensor was tested by sampling indoor laboratory air and moni­
toring the analytes concentrations, as proof of concept.

2. Materials and methods

2.1. Laser source characterization

The laser device employed as the light source for the QEPAS sensor
was a custom Vernier effect-based QCL provided by Alpes Lasers. The
Vernier effect was firstly developed by Pierre Vernier and is mainly
known for its application in calipers. By employing two measurement
scales with different periods, it is possible to improve the accuracy of a
measurement by exploiting the overlap of the two scales. In a Vernier
effect-based QCL, the grating on the top of the active region is designed
following the same effect. Different configurations of integrated grating
reflectors have been used to extend the emission range of laser sources
by means of the Vernier effect [32–34]. However, the use of these de­
signs in spectroscopic applications can be limited by the required so­
phisticated electronic driving [35]. The laser source employed in this
work is characterized by a novel design employing two integrated heater
resistors buried close to the active region. The semiconductor resistors
are etched into the top cladding close to the QCL active region and act as
local heaters to shift two reflectivity combs, representing the Vernier
scales in the present case. By varying the current injected in the inte­
grated heaters, the optical properties of the laser cavity are tuned.
Indeed, the laser cavity is divided into two gratings, the so-called front
and back gratings, the effective refractive of which can be tuned by
Fig. 1. (a) Laser emission at IL = 840 mA and different values of IB: 450 mA
injecting a current in the corresponding resistor, labeled as IF for the
(red curve), 850 mA (blue curve), 1100 mA (black curve), while IF = 0; (b)
front resistor and IB for the back resistor, respectively. As a consequence, Laser emission at IL = 840 mA and different values of IF: 450 mA (red curve),
the emission wavelength can jump from one spectral region to another, 750 mA (blue curve), 1050 mA (black curve), while IB = 0; (c) Optical emission
over the spectral gain of the active region, as the alignment between the power as a function of the laser peak emission wavenumber for configurations
reflectivity combs evolves [36]. Once the amplitude of the current employing the Front Section (black dots), the Back Section (red dots) and the
flowing in one of the heaters is fixed, a predictable emission can be QCL section (green dots).

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A. Zifarelli et al. Photoacoustics 28 (2022) 100401

reported in Fig. 1a–c are referred to spectra with single-mode emission. (Tektronix AFG3021C), providing also a low-frequency triangular ramp
With the configuration (IL, IF, IB = 0), five well-separated spectral ranges used to scan across the targeted absorption line. The piezoelectric cur­
can be clearly identified (black dots in Fig. 1c). These five regions have rent generated by the QTF was converted into a voltage signal using a
the central emission wavenumber at 2180 cm− 1, 2190 cm− 1, transimpedance preamplifier (gain factor = 30, Rfb = 10 MΩ) [38], and
2205 cm− 1, 2212 cm− 1 and 2239 cm− 1, respectively. With the config­ then was sent to a lock-in amplifier (EG&G 7265) to be demodulated at
uration (IL, IF = 0, IB), other six well-separated spectral ranges can be f = f0. The lock-in time constant was set to 100 ms for all measurements
covered by varying IB and IL (red dots in Fig. 1c). These ranges are reported in this work. The lock-in amplifier analog signal was digitalized
characterized by a central emission wavenumber at 2105 cm− 1, by a National Instruments DAQ card (USB 6008) connected to a personal
2113 cm− 1, 2125 cm− 1, 2135 cm− 1, 2212 cm− 1 and 2243 cm− 1, computer. The collected QEPAS signal was then recorded using a
respectively. Operating the device as a traditional QCL (IL, IF = 0, IB LabVIEW-based software. The gas line was composed of certified con­
= 0), a spectral emission range characterized by a central emission centrations gas cylinders, a gas mixer, a humidifier, a pressure
wavenumber at 2212 cm− 1 was observed (green dots in Fig. 1c). controller, a system of needle valves and a vacuum pump. The QEPAS
Therefore, all the three employed configurations are spectrally over­ sensor calibrations were performed using the following certified con­
lapped in this range, resulting in ten well-separated spectral regions centrations: 10 ppm CO in N2, 10 ppm N2O in N2 and 7000 ppm CO2 in
covered by the Vernier effect-based QCL. N2. One at a time, they were connected to the inlet of the gas mixer,
together with a cylinder containing pure nitrogen for successive di­
2.2. Experimental setup lutions. The pressure of the gas mixture flowing inside the ADM was
regulated using a pressure controller (MKS Type 649), while the flow
A schematic of the QEPAS sensor developed using the Vernier effect- rate was set by the gas mixer (MCQ Instruments, Gas Blender 103). A
based QCL is shown in Fig. 2. The collimated laser beam exiting the Nafion humidifier (PermSelect PDMSXA 1 cm2) was placed after the gas
device was focused through the acoustic detection module (ADM) by mixer to humidify the gas samples, fixing the water vapor concentration
means of a CaF2 plano-convex lens with focal length of 50 mm (Thorlabs for all measurements. The humidity level within the gas line was verified
LA5763-E). The size of the beam spots obtained when changing the using a capacitive hygrometer (not shown in Fig. 2). The sensor was
device electrical configuration was preserved, and no significant dif­ operated at room temperature Troom = 25 ◦ C, during all the measure­
ferences were observed in the lens focal plane. The employed ADM was a ment sessions.
stainless-steel vacuum-tight chamber equipped with two wedged ZnSe
windows with an anti-reflection coating in the 2–13 µm range (Thorlabs 3. Results and discussion
WG 80530-E). Inside the ADM, the QEPAS spectrophone consisted of a
T-shaped QTF acoustically coupled of a pair of resonator tubes. All 3.1. QEPAS sensor characterization
geometrical parameters and the assembly of the spectrophone are re­
ported in Ref. [17]. The spectrophone had a fundamental resonance Four gases relevant for environmental monitoring exhibit absorption
frequency at f0 = 12,458.1 Hz with a quality factor Q = 11,900 at at­ features within the laser full emission range: carbon monoxide (CO),
mospheric pressure (P = 760 Torr). The light exiting from the ADM was nitrous oxide (N2O), carbon dioxide (CO2) and water vapor (H2O). The
then collected by a power meter for alignment purposes. absorption cross sections of the analytes within the laser emission range
QEPAS measurements were performed in 2f-wavelength modulation were simulated using the HITRAN database [39] and are plotted in Fig. 3
spectroscopy (WMS), namely the laser emission was modulated by (solid lines) together with the corresponding laser optical power (green
applying a sinusoidal waveform to the injection current IL at a frequency squares). The spectra were simulated at atmospheric pressure for mix­
f = f0/2. This modulation was generated by a waveform generator tures in nitrogen containing the typical analytes concentrations in air,

Fig. 2. Schematic of the employed experimental setup. QTF, quartz tuning fork; mR, resonator tube; ADM, acoustic detection module.

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A. Zifarelli et al. Photoacoustics 28 (2022) 100401

Fig. 3. Absorption cross section of target analytes at atmospheric concentration simulated using the HITRAN database (solid curve) and laser optical power within
the simulation spectral ranges (green squares). a) 150 ppb of CO (black curve) and 1.19 % of H2O (red curve) in N2; b) 310 ppb of N2O (black curve) and 1.19 % of
H2O (red curve) in N2; c) 330 ppm of CO2 (black curve) and 1.19 % of H2O (red curve) in N2; and d) 1.19 % of H2O (red curve) in N2. All the spectra were simulated at
atmospheric pressure.

taking as reference the values of standard air sample reported on

HITRAN database (H2O: 1.19 %; CO2: 330 ppm; N2O: 310 ppb; CO:
150 ppb). The selected CO absorption feature peaked at 2123.69 cm− 1
with a close H2O absorption peak at 2123.6 cm− 1 is shown in Fig. 3a. In
this spectral region, the laser optical power varies from 69 to 80 mW,
corresponding to the device configuration: IF = 0, IB = 800 mA, IL
= 800–860 mA. The selected N2O absorption feature is peaked at
2212.35 cm− 1 with a close H2O absorption peak at 2212.57 cm− 1, as
shown in Fig. 3b. In this spectral region, the laser optical power varies
from 20 to 35 mW, corresponding to the device configuration: IF = 0, IB
= 0, IL = 730–790 mA. The selected CO2 absorption feature is peaked at
2243.59 cm− 1 isolated from any interferent present in atmosphere, as
shown in Fig. 3c. In this spectral region, the laser emission power ranged
from 0.1 to 3.5 mW, corresponding to the device configuration: IF = 0, IB
= 450, IL = 620–660 mA. The selected H2O absorption feature peaked at
2124.29 cm− 1 is shown in Fig. 3d. In this spectral region, the laser
emission power ranges from 70 mW to 75 mW, corresponding to the
device configuration: IF = 0, IB = 800, IL = 760–800 mA. A preliminary
investigation was performed to determine the best operating pressure
for the QEPAS sensor, which was found to be P = 450 Torr. This value
was selected as it provided the highest QEPAS signal for CO, which is the
gas species with the lowest atmospheric concentration among the Fig. 4. (a) 2f-QEPAS spectral scan of the H2O absorption feature at 2 % con­
centration in N2; (b) peak values from a 75-min-long acquisition of QEPAS
investigated gas species. The gas flow rate was fixed at 60 sccm to keep a
signal for 2 % H2O in N2.
constant 2 % water concentration within the gas line. The need for a
stable water concentration comes from the well-known dependence of
the photoacoustic signal on the presence of energy relaxation promoter, H2O concentration measured in our laboratories. The QEPAS spectrum
such as H2O. This effect was already observed for the target gases in the reported in Fig. 4a matches the expected sensor response, since it
selected spectral regions [40–42]. Therefore, a fixed water vapor con­ retraces the 2nd derivative of the Lorentzian absorption feature shown in
centration was required to perform an efficient calibration of the QEPAS Fig. 3d. The right-hand side negative lobe is only partially reconstructed
sensor. During the measurements, the water vapor concentration was due to narrow spectral range covered by the device configuration, as
monitored using the QEPAS signal measured at the absorption peak shown in Fig. 3d. However, the positive lobe is completely defined,
shown in Fig. 3d. allowing the extraction of the peak value which is, in turn, related to the
The 2f-QEPAS spectral scan corresponding to a concentration of 2 % actual water concentration within the ADM.
H2O in N2 acquired scanning across the water absorption peak (see No calibration of the H2O QEPAS signal has been performed since we
Fig. 3d) is shown in Fig. 4a. This humidity level was selected to remove decided to keep the water concentration at 2 % via the humidifier and
the effects of environmental water fluctuations as it was higher than the no significant variations of the values were expected. To verify the long-

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A. Zifarelli et al. Photoacoustics 28 (2022) 100401

term stability of the humidifier, subsequent spectral scans were per­ amplitude modulation contribution. The contribution to the overall
formed over a 75-min-long acquisition; then, the QEPAS peak signals spectra given by the H2O absorption feature peaked at 2123.6 cm− 1 (see
were extracted and plotted as a function of time in Fig. 4b. The collected Fig. 4a) is clearly visible, causing a slight distortion on the left hand-side
data show relative fluctuations within an interval of ± 6 % of the mean negative lobe of the 2f-Lorentzian lineshape, without affecting the CO-
value of the H2O QEPAS signal over more than one hour. The observed QEPAS peak signal. In Fig. 5b the 2f-QEPAS spectra for N2O concen­
fluctuations are related to the operating principle of the employed hu­ trations ranging from 0 to 7 ppm in humidified N2 are shown. The
midifier, consisting in hollow fibers releasing water vapor molecules in spectra were acquired tuning the IL current in the 730–790 mA range,
the gas flow passing through. Slight variations in the thermo- and fluid- while fixing both the IB current and the current IF to 0 mA. Neither the
dynamics parameters in the gas line can lead to small fluctuations in the N2O absorption profile nor the N2O-QEPAS peak signal are affected by
H2O released in the gas flow. Moreover, the collected trend shows 30- the H2O absorption peak at 2212.59 cm− 1. The asymmetry of the
min-long acquisitions characterized by a relative standard deviation of negative lobes is due to the residual amplitude modulation contribution.
~ 1 % indicating a good humidification stability. Such low variations of In Fig. 5c the 2f-QEPAS spectra of CO2 for concentrations ranging from
water concentration do not significantly affect the QEPAS signal of the 0 to 7000 ppm in humidified N2 are shown. The spectra were acquired
target gas species [40,41]. Then, the QEPAS sensor was calibrated for tuning the IL current in the 620–660 mA range, while fixing the IB cur­
CO, N2O and CO2 detection. The gas blender was used to generate rent to 450 mA. The collected QEPAS spectra partially retrace the 2nd
several dilutions in humidified N2 of each gas target independently, derivative of a Lorentzian lineshape. In fact, the right-hand side negative
starting from the certified concentrations available in the gas cylinders. lobe could not be reconstructed since the lasing threshold current for the
The 2f-QEPAS spectral scans collected at different gas target concen­ employed device configuration was IL = 620 mA (corresponding to
trations are shown in Fig. 5a–c for the three analytes. 2243.7 cm− 1, as shown in Fig. 5c), thus low optical powers were pro­
The 2f-QEPAS spectra collected targeting CO at concentrations vided by the injection currents nearby. The peak values of each QEPAS
ranging from 0 to 7 ppm in humidified N2 are shown in Fig. 5a. The spectrum reported in Fig. 5 were extracted and reported in Fig. 6 as a
spectra were acquired tuning the IL current in the 800–860 mA range function of the corresponding gas target concentrations. For each
while fixing the IB current to 800 mA, as previously reported. The shape dataset, the dashed line represents the best linear fit of the experimental
of the collected scans retraces the 2nd derivative of the Lorentzian data.
lineshape with a small alteration on negative lobes due to the residual For each gas target a 1σ-fluctuation of 2 % of the peak value was
estimated for each target concentration. In Table 1, the results of the
linear fits, namely the slope (the sensitivity) and the intercept, with the
noise level, the estimated minimum detection limit (MDL) and the
normalized noise equivalent absorption (NNEA).
For each of the three analytes, the noise level was estimated as the
1σ-fluctuation of the QEPAS signal acquired while pure N2 was flowing
in the ADM and the sine-modulated injection current was fixed at ab­
sorption peak. The minimum detection limits are the concentrations at
which the signal-to-noise-ratio is equal to 1, for each gas species.

Fig. 6. (a) QEPAS peak signals as a function of the CO concentration (black

squares) and the corresponding best linear fit (black dashed line); (b) QEPAS
Fig. 5. (a) 2f-QEPAS spectral scans of the CO absorption feature at eight CO peak signals as a function of the N2O concentration (red triangles) and the
concentrations; (b) 2f-QEPAS spectral scans of the N2O absorption features at corresponding best linear fit (red dashed line); (c) QEPAS peak signals as a
eight N2O concentrations; (c) 2f-QEPAS spectral scans of the CO2 absorption function of the CO2 concentration (blue dots) and the corresponding best linear
peaks at eight CO2 concentrations. fit (blue dashed line).

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A. Zifarelli et al. Photoacoustics 28 (2022) 100401

Table 1 19:00). The analytes were acquired in the following order: CO2, CO, N2O
Sensor calibration results for the target analytes. and H2O. From the acquired scans, the QEPAS peak values were
Sensitivity Intercept Noise MDL NNEA extracted and converted into gas concentration employing the calibra­
(mV / ppm) (mV) (mV) (W cm− 1 /
tion curved shown in Fig. 6a–c. The target gases concentrations collected
√Hz) during day #1 are reported as a function of the acquisition time in Fig. 8.
CO 21.96 ± 0.06 0.13 0.13 6 ppb 6.3 ⋅ 10− 9 The CO concentration trend (Fig. 8a) showed an increase during the
± 0.05 whole measurement session, with a minimum of 40 ppb around 17:15
9
N2O 13.45 ± 0.06 0.08 0.10 7 ppb 5.4 ⋅ 10− and a maximum of 98 ppb around 18:15. The N2O concentration trend
± 0.08
CO2 1.73 ⋅ 10− 3 0.30 0.12 70 ppm 5.0 ⋅ 10− 9 (Fig. 8b) pointed out a rapid increase between the first and the second
± 0.04 ⋅ 10− 3
± 0.11 round of measurements. Then, the concentration stabilized around
315 ppb with a slight decrease until the end of the measurement session.
The CO2 concentration trend (Fig. 8c) showed a variation of ~ 160 ppm
3.2. Indoor air quality monitoring during the whole measurement session, with a minimum of 800 ppm
around 15:05 and a maximum of 960 ppm around 18:00. The mea­
As proof of concept, the developed QEPAS sensor was tested by surements reported in Fig. 8 were repeated the next day under the same
sampling ambient air in a closed environment, i.e., the laboratory air. experimental conditions, and the average concentrations of CO, N2O and
For each gas, the operating parameters were the same as the ones CO2 are reported in Table 2 together with the corresponding 1σ standard
employed for calibration (P = 450 Torr, flow rate = 60 sccm), and the deviation.
air samples humidity level was kept fixed around 2 % by fluxing the gas The mean concentration values estimated in day #1 and day #2
samples through the Nafion humidifier. The 2f-QEPAS spectral scans show a good repeatability, as expected since the environmental condi­
acquired targeting the selected gas species in the laboratory air are tions were similar during the two days of measurements. The average
shown in Fig. 7. values of CO concentration estimated in laboratory air are comparable
The CO and N2O QEPAS spectral scans exhibit an adjacent water to those reported by the apulian regional agency for environmental
vapor absorption contribution, as expected from simulations reported in protection (ARPA) [43]. The typical atmospheric CO concentration is
Fig. 3a and b, respectively. Nevertheless, the CO and N2O contributions taken as a reference since no CO sources were present in the laboratory
are well resolved and separated, therefore the peak values used to during measurements [44]. In late spring days, the concentration may
retrieve the analytes concentration are still reliable. The CO2 QEPAS reach up to 200 ppb near to the monitoring station placed close to traffic
spectrum in Fig. 7c shows an analogous shape compared to those re­ hotspots. Considering the position of our laboratory, far from traffic jam
ported in Fig. 5c, with a negative lobe difficult to be identified. Long- and below the ground level, a lower concentration was expected. The
term measurements of the three target gases were performed in two
consecutive afternoons in late spring (26th and 27th of May 2021). Each
analyte was continuously targeted for ten minutes before switching to
the next one. This 40-min-long measurement was repeated four times,
both the afternoons, for a total operating time of ~ 4 h (from 15:00 to

Fig. 7. (a) 2f-QEPAS spectral scan of CO absorption feature at atmospheric

concentration in indoor environment; (b) 2f-QEPAS spectral scan of N2O ab­
sorption feature at atmospheric concentration in indoor environment; (c) 2f- Fig. 8. Target gases concentrations estimated during the long-term monitoring
QEPAS spectral scan of CO2 absorption feature at atmospheric concentration in of indoor laboratory air. (a) Estimated CO concentration (black squares); (b)
indoor environment. 2f-QEPAS spectral scan of H2O at a concentration of 2 % Estimated N2O concentration (red triangles); (c) Estimated CO2 concentration
can be observed in Figs. (a) and (b). (blue dots).

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Table 2 References
Estimated average analytes concentrations in laboratory air samples.
[1] D.L. Almeida, A. Pavanello, L.P. Saavedra, T.S. Pereira, M.A.A. de Castro-Prado, P.
Avg. concentration day 1 Avg. concentration day 2
C. de Freitas Mathias, Environmental monitoring and the developmental origins of
CO 64 ± 14 ppb 65 ± 21 ppb health and disease, J. Dev. Orig. Health Dis. 10 (2019) 608–615.
N2O 296 ± 18 ppb 294 ± 22 ppb [2] W.B. Gray, J.P. Shimshack, The effectiveness of environmental monitoring and
CO2 891 ± 57 ppm 855 ± 68 ppm enforcement: a review of the empirical evidence, Rev. Environ. Econ. Policy 5
(2011) 3–24.
[3] P. Saxena, V. Naik (Eds.), Air Pollution: Sources, Impacts and Controls, CABI,
Wallingford, 2019.
average values of N2O concentration measured in laboratory are [4] H. Hayat, T. Griffiths, D. Brennan, R.P. Lewis, M. Barclay, C. Weirman, B. Philip, J.
consistent with the typical atmospheric concentration of ~ 330 ppb [6] R. Searle, The state-of-the-art of sensors and environmental monitoring
but slightly lower. The average values of CO2 concentration are almost technologies in buildings, Sensors 19 (2019) 3648.
[5] M. Bacco, F. Delmastro, E. Ferro, A. Gotta, Environmental monitoring for smart
double compared to the typical outdoor CO2 concentration ~ 400 ppm cities, IEEE Sens. J. 17 (2017) 7767–7774.
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[17] P. Patimisco, A. Sampaolo, M. Giglio, S. Dello Russo, V. Mackowiak, H. Rossmadl,
were performed, and a linear response of the sensor was observed for A. Cable, F.K. Tittel, V. Spagnolo, Tuning forks with optimized geometries for
each analyte. Minimum detection limits of 6 ppb, 7 ppb, and 70 ppm quartz-enhanced photoacoustic spectroscopy, Opt. Express 27 (2019) 1401.
were estimated for CO, N2O, and CO2, respectively, at 100 ms integra­ [18] A. Sampaolo, P. Patimisco, M. Giglio, A. Zifarelli, H. Wu, L. Dong, V. Spagnolo,
Quartz-enhanced photoacoustic spectroscopy for multi-gas detection: a review,
tion time. The achieved detection limits were all below the natural Anal. Chim. Acta (2021), 338894.
abundance of the gas species in atmosphere. Therefore, as proof of [19] A. Zifarelli, G. Menduni, M. Giglio, A. Elefante, A. Sukhinets, A. Sampaolo,
concept, the sensor was tested by sampling indoor laboratory air and P. Patimisco, S. Fangyuan, W. Chongwu, Q.J. Wang, V. Spagnolo, Compact and
versatile QEPAS-based sensor box for simultaneous detection of methane and
monitoring the analytes concentrations in real-time. The measurements
infrared absorber gas molecules in ambient air, Front. Environ. Chem. 3 (2022),
were repeated in two consecutive days, returning average estimated 926233.
concentrations compatible with the expected atmospheric concentra­ [20] Z. Wang, J. Geng, W. Ren, Quartz-enhanced photoacoustic spectroscopy (QEPAS)
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[21] M. Jahjah, W. Ren, P. Stefański, R. Lewicki, J. Zhang, W. Jiang, J. Tarka, F.
Declaration of Competing Interest K. Tittel, A compact QCL based methane and nitrous oxide sensor for
environmental and medical applications, Analyst 139 (2014) 2065–2069.
[22] A. Sampaolo, S. Csutak, P. Patimisco, M. Giglio, G. Menduni, V. Passaro, F.K. Tittel,
The authors declare that they have no known competing financial M. Deffenbaugh, V. Spagnolo, Methane, ethane and propane detection using a
interests or personal relationships that could have appeared to influence compact quartz enhanced photoacoustic sensor and a single interband cascade
the work reported in this paper. laser, Sens. Actuators B Chem. 282 (2019) 952–960.
[23] Y. Ma, R. Lewicki, M. Razeghi, F.K. Tittel, QEPAS based ppb-level detection of CO
and N2O using a high power CW DFB-QCL, Opt. Express 21 (2013) 1008–1019.
Data Availability [24] A. Zifarelli, M. Giglio, G. Menduni, A. Sampaolo, P. Patimisco, V. Passaro, H. Wu,
L. Dong, V. Spagnolo, Partial least-squares regression as a tool to retrieve gas
concentrations in mixtures detected using quartz-enhanced photoacoustic
Data will be made available on request. spectroscopy, Anal. Chem. 92 (2020) 11035–11043.
[25] M. Giglio, A. Zifarelli, A. Sampaolo, G. Menduni, A. Elefante, R. Blanchard,
Acknowledgements C. Pfluegl, M.F. Witinski, D. Vakhshoori, H. Wu, V.M.N. Passaro, P. Patimisco, F.
K. Tittel, L. Dong, V. Spagnolo, Broadband detection of methane and nitrous oxide
using a distributed-feedback quantum cascade laser array and quartz-enhanced
Dr. Marilena Giglio acknowledges POR PUGLIA FESR-FSE 2014/ photoacoustic sensing, Photoacoustics 17 (2020), 100159.
2020 – Asse X – Azione 10.4. Research for Innovation – REFIN. The [26] H. Yi, R. Maamary, X. Gao, M.W. Sigrist, E. Fertein, W. Chen, Short-lived species
authors from Dipartimento Interateneo di Fisica di Bari acknowledge detection of nitrous acid by external-cavity quantum cascade laser based quartz-
enhanced photoacoustic absorption spectroscopy, Appl. Phys. Lett. 106 (2015),
financial support from the European Union’s Horizon 2020 research and 101109.
innovation program via the project PASSEPARTOUT, Grant no. [27] S. Zhou, L. Xu, L. Zhang, T. He, N. Liu, Y. Liu, B. Yu, J. Li, External cavity quantum
101016956 and THORLABS GmbH within the PolySenSe Joint-research cascade laser-based QEPAS for chlorodifluoromethane spectroscopy and sensing,
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H. Wu, H. Rossmadl, V. Mackowiak, A. Cable, F.K. Tittel, L. Dong, V. Spagnolo,
Dual-gas quartz-enhanced photoacoustic sensor for simultaneous detection of
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N. Passaro, H. Wu, L. Dong, V. Spagnolo, Quartz-enhanced photoacoustic X. Zhou, J.R. Ziemke, M. Ziese, Global climate, Bull. Am. Meteorol. Soc. 101 (2020)
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tuning of quantum cascade lasers with digital concatenated gratings, Appl. Phys. levels assessment in academic buildings with different heating, ventilation and air-
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Sampled grating, distributed feedback quantum cascade lasers with broad Energy Build. 40 (2008) 556–560.
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[35] M. Shahmohammadi, F. Kapsalidis, M.J. Suëss, E. Gini, M. Beck, M. Hundt,
B. Tuzson, L. Emmenegger, J. Faist, Multi-wavelength distributed feedback Andrea Zifarelli received the M.S. degree (cum laude) in
quantum cascade lasers for broadband trace gas spectroscopy, Semicond. Sci. Physics in 2018 from the University of Bari and his Ph.D. in
Technol. 34 (2019). Physics from the University of Bari in 2022. His research ac­
tivities were mainly focused on the development of spectro­
[36] N. Villa, G. Strübi, T. Gresch, J. Butet, S. Blaser, A. Müller, Quantum cascade lasers
with discrete and non equidistant extended tuning tailored by simulated annealing, scopic techniques based on laser absorption for the analysis of
complex gas mixtures by employing quartz tuning forks as
Opt. Express 27 (2019) 26701.
[37] Y. Bidaux, A. Bismuto, C. Tardy, R. Terazzi, T. Gresch, S. Blaser, A. Muller, J. Faist, sensitive elements. This investigation was performed by using
Extended and quasi-continuous tuning of quantum cascade lasers using innovative laser sources as well as developing new algorithms
superstructure gratings and integrated heaters, Appl. Phys. Lett. 107 (2015), for multivariate analysis approaches. Currently, his research
221108. activities are carried out at the PolySenSe Lab, joint-research
laboratory between Technical University of Bari and THOR­
[38] G. Menduni, A. Sampaolo, P. Patimisco, M. Giglio, S. Dello Russo, A. Zifarelli,
A. Elefante, P.Z. Wieczorek, T. Starecki, V.M.N. Passaro, F.K. Tittel, V. Spagnolo, LABS GmbH.
Front-end amplifiers for tuning forks in quartz enhanced photoacoustic
spectroscopy, Appl. Sci. 10 (2020) 2947.
[39] I.E. Gordon, L.S. Rothman, R.J. Hargreaves, R. Hashemi, E.V. Karlovets, F.
M. Skinner, E.K. Conway, C. Hill, R.V. Kochanov, Y. Tan, P. Wcisło, A.A. Finenko, Raffaele De Palo obtained his M.S. degree (cum laude) in
K. Nelson, P.F. Bernath, M. Birk, V. Boudon, A. Campargue, K.V. Chance, Physics in 2021 from the University of Bari. From the same
A. Coustenis, B.J. Drouin, J.M. Flaud, R.R. Gamache, J.T. Hodges, D. Jacquemart, year, he is a Ph.D. student at the Physics Department of the
E.J. Mlawer, A.V. Nikitin, V.I. Perevalov, M. Rotger, J. Tennyson, G.C. Toon, University of Bari, developing his research work at the Laser
H. Tran, V.G. Tyuterev, E.M. Adkins, A. Baker, A. Barbe, E. Canè, A.G. Császár, Micromachining Lab of Prof. A. Ancona and at PolySense Lab,
A. Dudaryonok, O. Egorov, A.J. Fleisher, H. Fleurbaey, A. Foltynowicz, joint-research laboratory between Technical University of Bari
T. Furtenbacher, J.J. Harrison, J.M. Hartmann, V.M. Horneman, X. Huang, and THORLABS GmbH. Currently, his research activities are
T. Karman, J. Karns, S. Kassi, I. Kleiner, V. Kofman, F. Kwabia-Tchana, N. focused on the development of a gas sensor based on Light-
N. Lavrentieva, T.J. Lee, D.A. Long, A.A. Lukashevskaya, O.M. Lyulin, V. Induced-Thermoelastic-Effect employing femtosecond laser-
Y. Makhnev, W. Matt, S.T. Massie, M. Melosso, S.N. Mikhailenko, D. Mondelain, H. textured Quartz Tuning Forks.
S.P. Müller, O.V. Naumenko, A. Perrin, O.L. Polyansky, E. Raddaoui, P.L. Raston, Z.
D. Reed, M. Rey, C. Richard, R. Tóbiás, I. Sadiek, D.W. Schwenke, E. Starikova,
K. Sung, F. Tamassia, S.A. Tashkun, J. Vander Auwera, I.A. Vasilenko, A.A. Vigasin,
G.L. Villanueva, B. Vispoel, G. Wagner, A. Yachmenev, S.N. Yurchenko, The
HITRAN2020 molecular spectroscopic database, J. Quant. Spectrosc. Radiat.
Transf. 277 (2022).
[40] J. Hayden, B. Baumgartner, B. Lendl, Anomalous humidity dependence in Marilena Giglio received the M.S. degree (cum laude) in
photoacoustic spectroscopy of CO explained by kinetic cooling, Appl. Sci. 10 Applied Physics in 2014, and the Ph.D. Degree in Physics in
(2020) 843. 2018 from the University of Bari. In 2012 she’s been visiting
[41] Y. Cao, R. Wang, J. Peng, K. Liu, W. Chen, G. Wang, X. Gao, Humidity enhanced the Academic Medical Center of Amsterdam as a trainee. In
N2O photoacoustic sensor with a 4.53 μm quantum cascade laser and Kalman filter, 2015 she was a Research Assistant with the Department of
Photoacoustics 24 (2021), 100303. Physics, University of Bari. She was a visiting researcher in the
[42] N. Maurin, R. Rousseau, W. Trzpil, G. Aoust, M. Hayot, J. Mercier, M. Bahriz, Laser Science Group at Rice University from 2016 to 2017.
F. Gouzi, A. Vicet, First clinical evaluation of a quartz enhanced photo-acoustic CO Since 2018, she is a Post-Doc Research Assistant at the Physics
sensor for human breath analysis, Sens. Actuators B Chem. 319 (2020), 128247. Department of the Technical University of Bari. Her research
[43] Agenzia Regionale per la Prevenzione e la Protezione dell’Ambiente - Aria, n.d. activity is focused on the development of gas sensors based on
(https://www.arpa.puglia.it/pagina2795_aria.html). Quartz-Enhanced Photoacoustic Spectroscopy and on the op­
[44] World Health Organization Regional Office for Europe, Selected Pollutants, 2010. tical coupling of hollow-core waveguides with interband- and
(ISBN code 9789289002134). quantum-cascade lasers.
[45] M. Ades, R. Adler, R. Allan, R.P. Allan, J. Anderson, A. Argüez, C. Arosio, J.
A. Augustine, C. Azorin-Molina, J. Barichivich, J. Barnes, H.E. Beck, A. Becker,
N. Bellouin, A. Benedetti, D.I. Berry, S. Blenkinsop, O. Bock, M.G. Bosilovich,
O. Boucher, S.A. Buehler, L. Carrea, H.H. Christiansen, F. Chouza, J.R. Christy, E.- Pietro Patimisco obtained the Master degree in Physics (cum
S. Chung, M. Coldewey-Egbers, G.P. Compo, O.R. Cooper, C. Covey, A. Crotwell, S. laude) in 2009 and the Ph.D. Degree in Physics in 2013 from
M. Davis, E. de Eyto, R.A.M. de Jeu, B.V. VanderSat, C.L. DeGasperi, D. Degenstein, the University of Bari. Since 2018, he is Assistant professor at
L. Di Girolamo, M.T. Dokulil, M.G. Donat, W.A. Dorigo, I. Durre, G.S. Dutton, the Technical University of Bari. He was a visiting scientist in
G. Duveiller, J.W. Elkins, V.E. Fioletov, J. Flemming, M.J. Foster, R.A. Frey, S. the Laser Science Group at Rice University in 2013 and 2014.
M. Frith, L. Froidevaux, J. Garforth, S.K. Gupta, L. Haimberger, B.D. Hall, I. Harris, Dr. Patimisco’s scientific activity addressed both micro-probe
A.K. Heidinger, D.L. Hemming, S. (Ben) Ho, D. Hubert, D.F. Hurst, I. Hüser, optical characterization of semiconductor optoelectronic de­
A. Inness, K. Isaksen, V. John, P.D. Jones, J.W. Kaiser, S. Kelly, S. Khaykin, R. Kidd, vices and optoacoustic gas sensors. Recently, his research ac­
H. Kim, Z. Kipling, B.M. Kraemer, D.P. Kratz, R.S. La Fuente, X. Lan, K.O. Lantz, tivities included the study and applications of trace-gas
T. Leblanc, B. Li, N.G. Loeb, C.S. Long, D. Loyola, W. Marszelewski, B. Martens, sensors, such as quartz-enhanced photoacoustic spectroscopy
L. May, M. Mayer, M.F. McCabe, T.R. McVicar, C.A. Mears, W.P. Menzel, C. and cavity enhanced absorption spectroscopy in the mid
J. Merchant, B.R. Miller, D.G. Miralles, S.A. Montzka, C. Morice, J. Mu¨hle, infrared and terahertz spectral region, leading to several pub­
R. Myneni, J.P. Nicolas, J. Noetzli, T.J. Osborn, T. Park, A. Pasik, A.M. Paterson, M. lications, including a cover paper in Applied Physics Letter of the July 2013 issue.
S. Pelto, S. Perkins-Kirkpatrick, G. Pétron, C. Phillips, B. Pinty, S. Po-Chedley,
L. Polvani, W. Preimesberger, M. Pulkkanen, W.J. Randel, S. Rémy, L. Ricciardulli,
A.D. Richardson, L. Rieger, D.A. Robinson, M. Rodell, K.H. Rosenlof, C. Roth,
A. Rozanov, J.A. Rusak, O. Rusanovskaya, T. Rutishäuser, A. Sánchez-Lugo,
P. Sawaengphokhai, T. Scanlon, V. Schenzinger, S.G. Schladow, R.W. Schlegel,
E. Schmid, Martin, H.B. Selkirk, S. Sharma, L. Shi, S.V. Shimaraeva, E.A. Silow, A.

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A. Zifarelli et al. Photoacoustics 28 (2022) 100401

Angelo Sampaolo obtained his Master degree in Physics in Olivier Landry obtained his M.Sc. degree in physics (2005)
2013 and the Ph.D. Degree in Physics in 2017 from University from McGill University and Ph.D. in physics (2009) from the
of Bari. He was a visiting researcher in the Laser Science Group University of Geneva. His Ph.D. thesis focused on quantum
at Rice University from 2014 to 2016. Since March 2021, he is repeaters for the development of quantum networks. Since
assistant professor at the Polytechnic of Bari. His research ac­ 2010, Dr. Landry has managed technical strategic marketing,
tivity has included the study of the thermal properties of het­ customer relations and branding for Alpes Lasers.
erostructured devices via Raman spectroscopy. Most recently,
his research interest has focused on the development of inno­
vative techniques in trace gas sensing, based on Quartz-
Enhanced Photoacoustic Spectroscopy, Tunable Laser Diode
Absorption Spectroscopy, Light-Induced Thermoelastic Spec­
troscopy and covering the full spectral range from near-IR to
THz. He is author of more than 100 Scopus publications and of more than 50 conference
contributions. He is CEO and cofounder of PolySense Innovations.

Stéphane Blaser was born in Switzerland in 1973. He received the M.S. degree in physics Vincenzo Spagnolo received the Ph.D., both in physics, from
from University of Neuchâtel, Neuchâtel, Switzerland, in 1997, and the Ph.D. degree in University of Bari in 1994. He works as Full Professor of
Sciences from University of Neuchâtel in the group of Prof. Faist, Neuchâtel, Switzerland, Applied Physics at the Technical University of Bari. In 2019, he
in 2001. His studies focused on quantum cascade structures based on photon-assisted become Vice-president of the Technical University of Bari,
tunneling transitions in strong magnetic fields. He joined Alpes Lasers SA, St-Blaise, deputy to Technology Transfer. The main scientific activity of
Switzerland, in 2002, as production manager. He is currently Head of Back-End. Vincenzo Spagnolo has been related the development of opto-
acoustic gas sensors based on quartz-enhanced photoacoustic
Jeremy Butet received a PhD degree in physics at the University of Lyon, France, in 2012. spectroscopy. He has been visiting researcher at Rice Univer­
He joined the Nanophotonics and Metrology Laboratory (NAM), headed by Prof. Olivier J. sity (Texas) in 2009 and 2010 and visiting professor in 2017.
F. Martin at the Swiss Federal Institute of Technology, Lausanne (EPFL) in 2012 as a He is “hundred talents” visiting professor at Shanxi University
postdoctoral researcher. He develops new experiments and models for nonlinear nano­ in Taiyuan (China). Since 2017, he is the director of the joint-
photonics. He is currently a Product engineer and Data scientist at Alpes Lasers SA. research lab PolySense, created by THORLABS GmbH and
Technical University of Bari. His research activity is documented by more than 230 Scopus
publications and three filed patents (more than 4500 citations, h-index 41). He has given
more than 60 invited presentations at international conferences and workshops. Prof.
Spagnolo is Fellow member of the SPIE and senior member of the Optica.