Infrared Physics and Technology 105 (2020) 103153

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Infrared Physics & Technology

journal homepage: www.elsevier.com/locate/infrared

A portable laser-based sensor for detecting H2S in domestic natural gas T

a a a a a a
Yuchen Guo , Xuanbing Qiu , Ning Li , Shiling Feng , Tong Cheng , Qiangqiang Liu ,
⁎
Qiusheng Hea, Ruifeng Kanb, Huinan Yangc, Chuanliang Lia,
a
School of Applied Science, Taiyuan University of Science and Technology, Taiyuan 030024, China
b
State Key Laboratory of Applied Optics, Changchun Institute of Optics, Fine Mechanics and Physics, Chinese Academy of Science, Changchun, Jilin 130033, China
c
School of Energy and Power Engineering, University of Shanghai for Science and Technology, Shanghai 200093, China

A R T I C LE I N FO A B S T R A C T

Keywords: Hydrogen sulfide (H2S) is a highly toxic gaseous component of natural gas that poses a significant hazard during
TDLAS the use of natural gas for domestic purposes; therefore, a high-sensitivity, on-line detection method is extremely
Hydrogen sulfide detection important to ensure its safety for domestic use. In this work, a portable sensor was developed based on near-
WMS-2f/DS-sine infrared tunable diode laser absorption spectroscopy (TDLAS). A special Herriott multipass cell (MPC) combined
with a home-made embedded electronics system allowed for the fabrication of a compact sensor with a size of
50 × 20 × 10 cm3. A rugged movable cell was used for detecting contaminated gas samples. An embedded
electronic system with a diameter of 8 cm was implemented to control the laser, acquire and process electronic
signal. To reduce external interference, the calibration-free TDLAS (wavelength modulation frequency-2f/direct
sine signal) was employed to suppress common field measurement noise. Based on the results of Allan deviation
analysis, the limit of system detection could reach 0.14 ppm using the H2S absorption line at 6336.61 cm−1. It is
suitable for on-line measurement because of its rapid response time. Its feasibility is validated for monitoring H2S
in a domestic natural gas of pipeline. This work demonstrates a system for real-time and field measurement of
H2S, which can be used to address the security risks associated with using natural gas.

1. Introduction [5,8]. Additionally, sulfur chemiluminescence, flame photometry, and

potentiometry are alternative methods used for measuring H2S con-
Natural gas, whose consumption has been growing steadily over the centration;however, these methods are generally time-consuming and
past two decades, is an important domestic fuel that is used for cooking suffer from aging effects, which make them unsuitable for applying in
and heating because it has high efficiency and is clean and safe [1]. the natural gas industry [9]. Therefore, optical methods which are
Hydrogen sulfide (H2S), a naturally occurring component of crude compact, robust, and highly sensitive are necessary for in situ and real-
natural gas, is colorless, flammable, explosive, and highly toxic. The US time H2S measurements, in particular for long-distance transmission of
Occupational Safe and Health Administration has set a concentration natural gas.
limit of 20 ppm for chronic exposure and a peak limit of 50 ppm for no In recent years, tunable diode laser absorption spectroscopy
longer than 10 min, while the International Standards Organization (TDLAS) has been successfully employed for monitoring industrial
regulates the maximum allowable H2S concentration of domestic nat- processes, and it is also a promising method for detecting H2S in natural
ural gas as 13 ppm. Therefore, it is essential to be able to monitor H2S in gas for domestic use [10–12]. Weldon et al. first utilized a near-infrared
natural gas in real time and in situ for both industrial and domestic distributed feedback (DFB) laser for detecting H2S gas based on the
applications [2–6]. υ1 + υ2 + υ3 absorption band [13]. Modugno et al. employed two-tone
A common method for detecting H2S is reflectometry, wherein the frequency modulation spectroscopy to realize a sensitivity of 4 ppm and
concentration of this gas is indicated by the reflected colors [7]; how- investigate the self and air-broadening of the υ1 + υ2 + υ3 band of H2S
ever, this method is only valid in the case of high concentrations. For [14]. A compact, rugged, and portable fiber-optic evanescent-field laser
low concentrations, a chemical sensor system is used in which H2S is sensor operating at 1.57 μm was developed for H2S detection in the gas
converted to SO2, and the concentration of H2S can be indirectly de- streams of volcanic fumaroles and had a detection limit of 100 ppm
termined by measuring the SO2 concentration via UV fluorescence [15]. Chen et al. realized DFB laser off-axis integrated cavity output

⁎
Corresponding author.
E-mail address: [email protected] (C. Li).

https://doi.org/10.1016/j.infrared.2019.103153
Received 2 October 2019; Received in revised form 4 December 2019; Accepted 5 December 2019
Available online 15 December 2019
1350-4495/ © 2019 Elsevier B.V. All rights reserved.
Y. Guo, et al. Infrared Physics and Technology 105 (2020) 103153

spectroscopy with a sensitivity of 0.67 ppm [16]. Recently, Xia et al. conditions. Therefore, the H2S rotational line at 6336.61 cm−1 of the
implemented a near-infrared TDLAS combined with a multi-pass cell to υ1+ υ2 + υ3 vibrational band was selected for concentration mea-
measure H2S and achieved a sensitivity in the ppm range and Tian et al. surements. Based on the Beer-Lambert law, the transmission coefficient
achieved a sensitivity as low as 60 ppb based on a compact dense- τ is expressed as [26]:
pattern multipass cell [17,18]. A compact photoacoustic spectroscopy
I
setup with a high sensitivity using a quartz enhanced photoacoustic τ (ν ) = = exp ⎡−α (ν ) ⎤ ≈ 1 − α (ν ),
I0 ⎢ ⎥ (1)
sensor was applied for detecting H2S in the 1.5 and 2.6 μ m region by ⎣ ⎦
Varga and Viciani [5,9,19]; however, photoacoustic spectroscopy suf-
where I and I0 are the incident and transmitted laser intensities, re-
fers from gas adsorption and corrosion of the system with use. Ad-
spectively, and α is the absorption coefficient with respect to laser
ditionally, a high-power laser source was required to obtain strong
frequency. For wavelength modulation spectroscopy (WMS), the in-
acoustic signals, and the setup is sensitive to disturbances during the
jection current of DFB laser is modulated with an angular frequency ω
monitoring of H2S in natural gas, such as those caused by mechanical
[27].
vibrations in harsh industrial environments. There have been a few
reports outlining the successful development of H2S sensors based on ν (t ) = ν + acos(ωt ), (2)
TDLAS for field measurements. Chen and Song developed the open path
H2S detection system for environmental monitoring and industrial I0 (t ) = I0 [1 + i1cos(ωt + ψ1) + i2cos(2ωt + ψ2)], (3)
production [20,21]. You and Zhang used near-infrared TDLAS to con- where ν is the center laser frequency and a is the modulation depth. I0
tinuously monitor the H2S concentration of a desulfurizing device and is peak-peak value of modulation signal detected by the photodiode,
for natural gas purification [22–24]. However, most previously re- termed as DS-sine [28]. The parameters such as i1, i2, ψ1 and ψ2 describe
ported H2S sensors were bulky and did not consider suppression of the characteristics of the laser. The spectral absorption α is a periodic
external interference such as mechanical vibration, optical-electrical even function in ω t and can be expanded in a Fourier cosine series:
gain, and laser transmission variations [25].
In this work, a portable H2S sensor was developed based on infrared ⎛ ⎛ ⎞⎞ ⎛ ⎞ ⎛ ⎞
TDLAS. The WMS-2f/DS-sine method was employed to suppress noise
− α ⎜ν + acos ⎜ωt ⎟ ⎟ = ∑ Hk ⎜ν , a⎟ cos ⎜kωt ⎟,
⎝ ⎝ ⎠⎠ k=0 ⎝ ⎠ ⎝ ⎠ (4)
from the circuit, the optical path, and the harsh environments. A special
Herriott structure with two reflective mirrors separated from the sam- The Hk coefficient is the Fourier expanding coefficient:
pling cell was designed to avoid contamination of the mirrors and allow
for easy cleaning of the cell windows. For compactness, a self-made ⎛ ⎞ PxL π ⎛ ⎞
H0 ν ,
⎜
a =−
⎟ 2π
∫−π ∑ Sj φj ⎜ν + acosθ⎟ dθ,
embedded electronics system was developed and served as the DFB ⎝ ⎠ j ⎝ ⎠ (5)
laser controller, the lock-in amplifier, the data acquisition and signal
processing system, the display, and for serial communication. For fur- ⎛ ⎞ PxL π ⎛ ⎞ ⎛ ⎞
ther verification, this sensor was deployed for the in-field detection of Hk ν ,
⎜
a =−
⎟ 2π
∫−π ∑ Sj φj ⎜ν + acosθ⎟ cos ⎜kθ⎟ dθ,
H2S in natural gas. ⎝ ⎠ j ⎝ ⎠ ⎝ ⎠ (6)

For WMS detection, a lock-in amplifier is used to get harmonic

signals based on a quadrature demodulation scheme. For convenience,
2. Experiments
we matched the condition when the in-phase component signal was
maximum.The 2f harmonic signal is approximately represented as:
2.1. Measurement principle
GI0 ⎡ i1 ⎧ i H
To avoid cross interference from other species in domestic natural X2f = H1 + H3⎫ + 2 ⎧ 4 + H0 ⎫ + H2⎤,
2 ⎢ 2
⎣ ⎩ ⎨ ⎬
⎭ 2⎨⎩ 2 ⎬
⎭
⎥
⎦ (7)
gas, it is necessary to choose a discrete spectral line with strong ab-
sorption intensity. Based on the HITRAN 2016 database, the special where G is the optical-electrical gain of the detection system.
lines of H2S, as well as the main perturbing absorption lines from CH4, At fixed pressure, temperature, optical path length, and laser
H2O, and CO2 are all presented in Fig.1. Other main components of parameters, the line shape is insensitive to the sample concentration at
natural gas, such as C2H6 and C3H8, have no absorption lines in the low absorption conditions (typically less than 5%). Thus, the con-
observed spectral region. It illustrates that the influence of the per- centration relationship with 2f harmonic peak can be derived as
turbing lines can be neglected under the assumed measurement C∝ X2f .To reduce laser instability and the interference of the optical
path, a simple normalized method is applied and given by:
X2f
C∝ .
I0 (8)

Thus, all non-absorption transmissions can be ignored during the

measurement.

2.2. Experimental details

A schematic diagram of the laser-based H2S sensor is depicted in

Fig.2(a). A fiber-coupled DFB laser emitting at 1.578 μ m was used as a
light source. The laser was connected to an optical fiber-coupled GRIN
lens for beam collimation; then, the collimated laser was coupled into a
home-made Herriott-type multipass cell. The effective optical path-
length was 15 m with a cell length of 0.3 m. To protect the reflective
mirrors, the sampling cell was separated from both mirrors by two
windows with a distance of 5 mm, and the windows of the sampling cell
Fig. 1. Calculated spectra for 100 ppm H2S, 1500 ppm CO2, 1% H2O and 85% were coated with a dielectric anti-reflective film. Wedged-shaped 2°
CH4 in the range of 6335–6340 cm−1. windows were adopted to suppress the optical interference fringes. The

2
Y. Guo, et al. Infrared Physics and Technology 105 (2020) 103153

(a)

Optical part

Multipass gas cell

DFB
laser
Temperature sensor
Detector

Laser Temperature
AMP Pressure
Driver controller
sensor
Serial Valve
port BPF Valve
DAC

DS AD630 Mass flow

Pump controller
DAC STM32F405 ADC 2f
Integral
LPF
circuit
Butterworth Gas out
filter 74HC4046 2nd Gas in
CPLD
VCO
Electrical part Gas part

Electrical

8 cm
Herriott cell

DFB laser

Detector

50 cm

(b)
Fig. 2. (a) Schematic of the laser-based H2S sensor system; (b) photograph of the real instrument.

cell was made of stainless steel to inhibit adsorption and corrosion by current and the wavelength. The amplitude of the scanning wave signal
H2S. The internal surface of the cell was polished, and the inlet and was 300 mV, corresponding to a scanning wavelength range of
outlet pipes were made of polytetrafluoroethylene to suppress adsorp- 6336 cm−1–6337 cm−1; the repetition frequency was set to 5 Hz; the
tion. Gas pressure was measured by Testo552 which was installed at the modulated signal at 7.572 kHz (1f) was generated via a high-speed logic
outlet of gas pipe and temperature was obtained by a DS18B20 sensor phase-locked-loop with VCO (74HC4046A), and was then sent to the
embedded at the bottom of the cell, as presented in the gas part of CPLD (Altera, EPM7064AE) for frequency-doubling (2f) and phase-
Fig.2(a). Furthermore, the valves were used for auxiliary pressure shift. The 1f TTL signal of the CPLD output was filtered into a sine
control of system. signal using a 5th Order Butterworth low-pass filter. The final sine
The electrical portion of the system was divided into two parts, one signal was superimposed on the triangle laser-scanning signal using an
part for the DFB laser drive circuit and the other was the analog to lock- adder. The laser intensity after passing through the multipass cell was
in amplifier circuit. Both PCB boards were 8 cm in diameter (shown in converted into an electronic signal using a high-speed InGaAs detector
Fig.2(b)), and the main control chip was a Microcontroller Unit (MCU, (ET-3010). Then, it was amplified by a pre-amplifier and filtered using a
STM32F405). The current driver circuit based on a Hall-Libbrecht de- band-pass filter (BPF). The analog phase-locked amplifier circuit was
sign and the temperature controller was implemented with an implemented using a balanced modulator and demodulator (AD630).
ADN8834. The laser wavelength characteristics are 0.014 cm−1/mA in Both the 2f signal of the CPLD output as a reference signal and half the
the range of 20–70 mA and 0.378 cm−1/°C in the range of 22–28 °C, BPF output as a modulation signal were sent to the AD630 for syn-
respectively.The stabilities of the current and temperature controllers chronous demodulation (i.e., WMS-2f). The output of the AD630 was
were 4 μ A and 0.0067 °C, respectively. The controller is a home-made further filtered using a low-pass filter (LPF). Finally, the filtered and DS-
instrument. These two parameters were obtained by measuring the sine signals were simultaneously acquired by two 16-bit analog-to-di-
error signal with ESCORT-3136A multimeter and the details could be gital converters (AD7606) and stored in the FLASH of the MCU. The
found from our previous published literature [29]. Triangular wave digital signals were processed and calculated using the STM32F405
signals were generated by a 12-bit digital to analog converter (AD5683) MCU, and the DS-sine normalized signal was used to determine the
controlled by MCU, and its amplitude was determined by the spacing of concentration of the H2S gas. Finally, the obtained concentration results
the selected absorption line and the relationship between driving were displayed using an LCD and transmitted to the host computer

3
Y. Guo, et al. Infrared Physics and Technology 105 (2020) 103153

Fig. 3. Observed signals for 100 ppm H2S is mixed with CH4 at 80 Torr at a
concentration of 100 ppm at room temperature.(a) Direct absorption signal
Fig. 6. The WMS-2f/DS-sine signal amplitude of H2S and fitting curve as a
with modulation and DS-sine value (insert figure); (b) WMS-2f signal of H2S.
function of H2S concentration.

H2S concentration (ppm)

55

50

45

40
0 720 1440 2160 2880 3600
0.8

0.6
Allan deviation (ppm)

0.4

0.2
Fig. 4. Variations of WMS-2f and 2f/DS-sine signals with external interference.
0.14 ppm@178 s

12 20 Torr 101 102 103

40 Torr Averaging time (s)
60 Torr
80 Torr Fig. 7. Obtained signal for a 50 ppm H2S sample at 80 Torr and 25 ° C for a
100 Torr
WMS-2f / DS-sine (a.u.)

duration of more than an hour and its Allan deviation analysis..

8
20

4
H2S Concentration (ppm)

10
0

0.09 0.12 0.15 0.18 0.21

Modulation amplitude (V)
Fig. 5. Observed WMS-2f/DS-sine signal amplitude for 100 ppm H2S with
different modulation amplitudes at five different pressure values.
0
0 12 24 36 48
Time (h)

Fig. 8. Continuous measurement of hydrogen sulfide in civil gas for 48 h.

4
Y. Guo, et al. Infrared Physics and Technology 105 (2020) 103153

through the serial communication port. results demonstrated that values derived by continuous and real-time
measurement satisfied the standards set by document No.9 of the na-
3. Results tional standards management committee of the People’s Republic of
China in 2012. Therefore, the developed laser-based H2S sensor with a
The measured DS and WMS-2f signals for a 100 ppm H2S gas mix- high sensitivity and rapid response can be used to improve safety
ture that was pure H2S mixed with the pure N2 with the uncertainty of during the transportation and domestic use of natural gas.
±1 ppm sample are shown in Fig. 3(a) and (b), respectively. The results
show that the WMS-2f is more sensitive than direct absorption spec- 4. Conclusions
troscopy due to the significant reduction of 1/f noise and zero baseline
stability [30] In this experiment, the WMS-2f/DS-sine approach was In this paper, a laser-based H2S gas sensor was constructed based on
applied to reduce fluctuations in the optical intensity because of gas near-infrared TDLAS. A compact sensor of 50 × 20 × 10 cm3 could be
flow and mechanical vibrations. The airflow means varying the sample realized using a home-made embedded electronics system and a
velocity of flow and gas flow was changed from 0.5 L/min to 0.025 L/ Herriott cell. The WMS2f/DS-sine free calibration method was em-
min using the mass flow controller. Mechanical vibration was generated ployed for reducing external interference. Allan deviation analysis de-
by knocking the optical breadboard with a hammer, and the partial monstrated that the sensitivity could reach 0.14 ppm with an integra-
shading was accomplished by inserting a piece of lens paper. Three tion time of 178 s. Finally, the sensor was used for continuous
sections of interference occurred at the mid-duration lasting 2 min. The measurement of domestic natural gas for 48 h. The results demon-
corresponding standard deviations of WMS-2f signal for gas flow, par- strated that the sensor had a high sensitivity and fast response.
tial shading and mechanical vibration are 0.018, 0.016 and 0.020, but Therefore, it is suitable for application to the continuous on-line de-
they are reduced to 0.017, 0.015 and 0.019 for WMS-2f/DS-sine ap- tection of H2S in domestic natural gas.
proach. The results, as shown in Fig.4, validate the stability and ro-
bustness of the sensor with this strategy. While the amplitude of the Declaration of Competing Interest
WMS-2f signal varies significantly, especially for beam blocking, the
WMS-2f/DS-sine method is not affected by variation of the light in- None.
tensity. Therefore, the technique shows promise for in situ measurement
applications. Acknowledgement
The amplitude of the wavelength modulation signal is relevant for
both the modulation index and the pressure, so it is necessary to select This work was supported by the National Natural Science
optimal conditions [31]. Fig.5 shows a series of WMS-2f/DS-sine signals Foundation of China (Grant Nos. U1810129, U1610117 and
for H2S at different pressures and modulation amplitude values. The 11904252), State Key Laboratory of Applied Optics (SKLAO-201902),
measured sample H2S blending with pure N2. By recording the H2S Transformation of Scientific and Technological Achievements Fund of
spectra at 100 ppm of different pressures, the maximum signal for H2S Shanxi Province (201904D131025), Excellent Youth Academic Leader
was realized at 80 Torr and 0.152 V. The amplitude of wavelength in Higher Education of Shanxi Province (2018), Key Research and
modulated harmonic signal depends on the modulation depth relevant Development Program of Shanxi Province of China (Grant Nos.
with modulation amplitude and spectral width. The width of spectral 201803D31077 & 201803D121090), the Fund for Shanxi “1331
line, herein, is dominated by Doppler broadening and pressure broad- Project” Key Innovative Research Team (1331KIRT), Natural Science
ening, so the signal amplitude drops at 100 Torr and higher pressure. A Foundation of Shanxi Province of China (No. 201801D221017) and the
similar phenomenon could be found in our previous publication [26]. Fund for Shanxi Key Subjects Construction.
The H2S gas sensor was calibrated using a similar method to the
reported in Ref. [32]. In calibration process, the CO2 concentration was Appendix A. Supplementary material
15 times more than H2S, mixture was used for verifying whether H2S
adsorbs on the inner cell and gas tube or not. This is because CO2 ab- Supplementary data associated with this article can be found, in the
sorption line close to that of H2S and it is without adsorption char- online version, at https://doi.org/10.1016/j.infrared.2019.103153.
acteristic. It demonstrated that the adsorption of H2S could be neglected
in measuring the flow H2S sample according to the observed CO2 sig- References
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