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JOURNAL OF LIGHTWAVE TECHNOLOGY, VOL. 31, NO. 9, MAY 1, 2013

Tunable Diode Laser Based Concentration

Measurements of Water Vapour and
Methane on a Solid Oxide Fuel Cell
Michael Lengden, Robert Cunningham, and Walter Johnstone

AbstractThis paper presents concentration measurements

of water vapour and methane, taken in-situ on an operational
solid oxide fuel cell (SOFC) test rig using tunable diode laser
spectroscopy (TDLS). Methane concentration measurements are
presented for the TDLS system and are compared with concentration measurements taken using gas chromatography (GC).
Furthermore, purge times for the SOFC gas-analysis system have
been calculated using TDLS, which are measurements that cannot
be obtained directly using GC. Finally, water vapour concentration measurements in the SOFC cathode are shown for different
system operating conditions: a dry cathode cycle and during the
introduction of water vapour. As GC cannot be used to measure
water vapour in the SOFC cathode stream, a direct comparison
cannot be made with the TDLS measurements.
Index TermsFibre optic sensors, fuel cells, molecular spectroscopy, optical gas detectors.

I. INTRODUCTION

F the various fuel cell technologies available, the solid

oxide fuel cell (SOFC) is most suited to large-scale
stationary-power production [1]. The development of the
SOFC for stationary power generation has been underway for
a number of years [2][4]; however, the standard techniques
used for measuring gas compositions within a fuel cell test
rig, such as gas chromatography (GC), may be unsuitable for
a commercial system as they cannot provide real-time data
where operational conditions need to be continually monitored.
Additionally, gas chromatography cannot be used to measure
water vapour directly, which can constitute a significant fraction
of the gas in the SOFC fuel stream. Currently, water vapour
concentrations have to be calculated using a process of dry
gas analysis of products at various points around the system
and mass-balance calculations. The ability to employ real-time
measurement in an environment containing water vapour is
therefore essential for both SOFC fundamental research and
the development of an industrial unit. One technique that can
Manuscript received August 24, 2012; revised February 06, 2013; accepted
February 12, 2013. Date of publication February 14, 2013; date of current version March 13, 2013. This work was supported in part by the EPSRC, RollsRoyce Fuel Cell Systems Ltd., and Optosci Ltd.
M. Lengden and W. Johnstone are with the Centre for Microsystems and Photonics, Department of Electronic and Electrical Engineering, University of Strathclyde, Glasgow G1 1XW, U.K. (e-mail:
michael.lengden@eee.strath.ac.uk; walter.johnstone@eee.strath.ac.uk).
R. Cunningham is with Rolls-Royce Fuel Cell Systems Ltd., Derby DE24
8BJ, U.K. (e-mail: Robert.cunningham@rrfcs.com).
Color versions of one or more of the figures in this paper are available online
at http://ieeexplore.ieee.org.
Digital Object Identifier 10.1109/JLT.2013.2247378

provide real-time measurements in an environment containing

water vapour is tunable diode laser spectroscopy (TDLS)
[5][7] and recently we reported on a new gas analyser that has
been used to measure the methane concentration in an SOFC
system [8].
This previous work had been carried out in order to provide
a direct comparison of methane concentration measurements
taken using GC and the TDLS sensor simultaneously. However as the TDLS system had to be operated at the same temperature and pressure conditions as the GC, its full potential as
an in-situ, real-time gas sensor could not be realised. Here we
present a more extensive analysis of the previous methane measurements, including further details on how broadening parameters were estimated and the purge times of the SOFC and the
gas sampling system were calculated. Furthermore, we present
results for water concentration measurements, taken from the
cathode stream of the same SOFC system. This work has provided valuable data on the water vapour concentration on the
cathode which could be used to determine the fuel-cell performance as a function of water vapour concentration.
Prior to these results being presented a theoretical description
of TDLS gas spectroscopy is given in Section II, including a
methodology for concentration measurements, and the sensor
is described in detail in Section III.
II. TDLS SPECTROSCOPIC GAS MEASUREMENT THEORY
It is assumed that the transmitted intensity of light,
, at an
optical wavenumber, , passing through a gas cell of length, ,
is given by the Beer-Lambert law,
(1)
where
is the intensity of light incident on the gas cell,
is the gas cell pressure, is the molar fraction of the species of
interest, is the transition lineshape, whose area is normalised
to 1, and
is the transition linestrengh.
The transition lineshape, , is described using a number of
broadening mechanisms that affect the total energy distribution
of the transition. The two most dominant broadening contributions are due to the Doppler effect and gaseous collisions,
described using Gaussian and Lorentzian distributions respectively. The full-width half-maximum (FWHM) of the Doppler
broadened profile is given as

0733-8724/$31.00 2013 IEEE

(2)

LENGDEN et al.: TUNABLE DIODE LASER BASED CONCENTRATION MEASUREMENTS

The transition linestrength

equation

TABLE I
CONSTANTS FOR THE VOIGT FUNCTION APPROXIMATION [9]

where M is the molecular mass,

is the transition line centre
in wavenumbers, is Boltzmanns constant and is the speed
of light. The Doppler broadening values for methane and water
vapour at the operational conditions of the in-line gas cell are
0.0184 cm and 0.0224 cm respectively.
The FWHM for the collisional broadened profile is given as
(3)
where
is the FWHM collisional broadening coefficient at a
reference temperature, , for each species, , contained within
is the temperature exponent. The collithe gas cell and
sional broadening values for methane and water vapour at the
operational conditions of the in-line gas cell are 0.24 cm and
0.143 cm respectively.
The convolution of the Doppler and collisional broadening
terms are described by a Voigt line-shape as
(4)
The Voigt function can be approximated analytically using
four generalized Lorentzians in two variables [9]

(5)
where
Table I,
is

are constants of evaluation and are shown in

is calculated using the

(8)
is a the linestrength at a reference temperature of
where
296 K, obtained from the HITRAN 2008 database [10],
and
are the partition functions at the gas cell temperature
and the reference temperature respectively, is Planks constant
and
is the transitional lower state energy. The linestrength
has to be converted from the HITRAN value using the equation
(9)
where
is Avagadros constant and is the gas constant in
units of cm atmK mol .
A number of parameters are given in the HITRAN 2008 dataand . The database also
base [10], including
provides values for self- and air-broadening parameters and the
temperature dependence of the self-broadening parameter, however, no gas-broadening parameters are included for other gases.
For the methane experiments a bulk-broadening parameter has
been calculated using absorption signals of known gas concentration, described further in Section IV. As there was no comparative measurement process for the water measurements it was
not possible to calculate a bulk-broadening parameter, therefore
the air-broadening parameter from the HITRAN 2008 database
was used.
The theory described in this section provides all the necessary information for deriving theoretical absorption profiles.
A MATLAB program has been written that compares experimental signals to the derived absorption profiles and carries out
a least-squares fitting routine to obtain concentration and pressure measurements, described in detail in Section III.
III. TDLS GAS COMPOSITION MEASUREMENT SYSTEM

(6)
and

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is
(7)

is classified as the Voigt parameter and describes the

overall effect of the two broadening contributions. For
the line-shape is accurately described using the
Voigt profile, and for the methane and water spectra used in this
work the values of are 9.5 and 5.4 respectively.

A schematic of the experimental apparatus is shown in Fig. 1.

Two butterfly packaged, pigtailed, distributed feedback (DFB)
laser diodes are used to detect methane and water vapour at
wavelengths of 1650.9 nm and 1390.8 nm respectively.
Both lasers are controlled using Optosci Ltd. Integral Precision
Laser Driver and Thermo Electric Cooler Controllers, allowing
current and temperature tuning of their output wavelengths.
Initially, the wavelength of each laser is thermally tuned to
a suitable absorption feature. Then, a 5 Hz current ramp,
obtained using a four channel direct digital synthesis (DDS)
signal generator board, is applied to each laser, in order to
tune their individual wavelengths over the chosen methane and
water absorption profiles.

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Fig. 1. Experimental Schematic.

Fig. 2. In-line gas sensor, constructed from 316 Stainless Steel Swagelok
fittings.

If only one gas species is being analysed the single-mode pigtail from the appropriate laser is connected to a 50:50 optical
splitter. If both gas species are being measured then single-mode
pigtails from each laser are connected to an optical switch, providing selection between the laser outputs via two 5 V sinusoidal signals from the DDS board. The selected laser output
then passes through the 50:50 optical splitter. One arm of the
splitter transmits 50% of the light through an in-line gas cell,
and the second arm is used to send 50% of the light to a fibre
ring resonator for wavelength referencing [10].
The in-line gas cell, shown in Fig. 2, is constructed from 316
grade stainless steel to reduce corrosion caused by high water
vapour concentrations. Both the gas cell and the signal processing have been described in detail previously for methane gas
composition measurements in a dry atmosphere [5]. Therefore,
only modifications applied to the system for the measurement
of water vapour are detailed here.
For water vapour measurements an 1/8 gas sample line is
taken directly from the SOFC test rig. The concentration of
%; the line preswater vapour in the sample line was always
sure was 6.4 bar ; the corresponding dew point was 72 C. The
sample line was trace heated to approximately 100 C and kept

as short as possible in order to ensure no water vapour could

condense prior to entering the gas cell. The gas cell is located
in an aluminium box that has been packed with Insulfrax insulation. Heat tape is wrapped around the box and a further
layer of insulation covers the tape. This process allows the gas
cell to be heated uniformly. The heating control system consists of a feedback thermocouple, located inside the stainless
steel box, and a Barnstead/Electrothermal MC810 digital temperature controller. A second thermocouple is located inside the
gas cell, allowing the cell temperature to be logged using a Pico
Technology TC-08 temperature logger.
The cell was operated at a temperature of 70 C and pressure
of 1.1 bar , monitored using a pressure gauge. A needle valve
was used to maintain a constant flow of approximately 250 ml
min through the gas cell. The maximum dew point of the gas
sample was calculated to be 36 C, so the operating conditions
of the gas-sensor box ensured there would be no condensation.
The experimental setup allowed the selection of either the SOFC
sample stream or a source of dry air from the test-facility compressors. When water vapour concentration measurements were
not being taken dry air was passed through the cell in order to
ensure any water vapour was purged from the gas sensor and to
provide a background signal.
A Thorlabs PDA10CS photodetector is used to monitor the
laser radiation from the gas cell, and the output voltage from the
photodetctor is measured using a Pico Technology 4424 digital
oscilloscope.
Spectral signals are filtered using a low pass elliptical filter
function, wavelength referenced and fitted to theoretically
derived profiles using a least squares fitting procedure in
MATLAB. In this method, all the parameters within the theoretical model are fixed except for the concentration, and a
least squares comparison is made between the derived profile
and experimental signals until the optimum fit between the
two spectra is obtained. This procedure is repeated for various
incremental values of pressure to account for any pressure
variation in the sample line. The total analysis time is between
530 seconds.

LENGDEN et al.: TUNABLE DIODE LASER BASED CONCENTRATION MEASUREMENTS

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IV. DRY METHANE MEASUREMENTS

The results presented in this section are an extension of work
published previously [5]. Methane measurements were taken
from a number of different sample lines located at various
strategic points around the SOFC test rig. A multi-position
valve was used to remotely select one of the sample lines
and the gas flowing from the selected sample line was cooled
and the water vapour removed prior to the gas entering the
gas chromatograph. The gas cell was located immediately
before the gas chromatograph, providing a direct comparison
between the two measurement techniques. All TDLS signals
were normalised using a sample line containing 0% methane
concentration.
The pressure of each sample line had to be reduced from
the SOFC operational pressure of 6.4 bar to 2 bar , to allow
GC sampling. The GC inlet pressure was measured using an
analogue pressure gauge. Each sample line contained a mixture of gases with various quantities of CH , CO, CO , N and
H . Each gas within the mixture will influence the collisional
broadening parameter, as described in (3). In order to account
for the various broadening terms, a bulk-broadening parameter,
, has been calculated, which encompasses all gases from
the sample line. An expansion of (3) gives

Fig. 3. Comparison of the final theoretical fit for the bulk-broadening parameter, obtained using a least squares fitting procedure of an experimental absorption profile from the anode ejector with a known methane concentration
of 11.8%.

(10)
is the self-broadening parameter, taken from the
where
HITRAN2008 database,
are the molar fractions of
methane and the rest of the gas mixture respectively and m and
n are the methane and bulk temperature exponents respectively.
As this data has been taken near room temperature, the ratio
of T to T is 1, therefore the values of m and n provide a
negligible contribution to the overall broadening.
The bulk broadening parameter was calculated using a
sample from the anode ejector. The fitting procedure was
similar to that described in Section III, however, in this method
all variables were fixed except for
.
The bulk-broadening parameter was calculated on two occasions, separated by two months, and an example calculation is
shown in Fig. 3. On both occasions a sample from the SOFC
system was analysed, where the methane concentrations were
calculated using GC as 11.8% and 14.9%, giving bulk-broadening parameters of 0.1211 cm
and 0.1252 cm
respectively. The overall variation between the two results is approximately 3%, and this error is assumed to be caused by the error
in the pressure reading from the analogue pressure gauge.
If both bulk-broadening parameters are used independently
to calculate the methane concentration from a different location in the SOFC system we obtain final concentration values
of 0.586% and 0.603% respectively. The overall error between
these two measurements is 2% and the absolute concentration
error is 0.017%. The concentration of methane determined by
the GC at the same location was 0.58% with an absolute error
of
%. The concentration values obtained from both bulkbroadening parameters are within the bounds of the GC measurement accuracy. Finally, assuming a signal to noise ratio of
3, the calculated lowest measurable absorbance is

Fig. 4. Time evolution of the methane concentration as a new sample line is

selected using the multi-position valve.

for these spectral signals. This relates to a minimum measurable

methane concentration of 210 parts per million.
Fig. 4 shows the variation of the methane concentration as
the multi-position valve is switched from one sampling location
with high methane concentration to another with low methane
concentration. Measurements were taken at 10 second increments for a total of 600 seconds. For the first 100 seconds there
is little change in the methane concentration, then for 60 s the
methane concentration increases up to 33%. This increase is due
to the multi-position sampling valve cycling through the main
fuel line to the test rig which has a methane concentration of
approximately 85%. The total purge time of the gas sensor and
sample lines, once a new position has been selected with the
multi-position valve, is approximately 9 minutes.
Fig. 5 further highlights the advantages of real-time measurement using the TDLS analysis rig. In this figure, the evolution
of the methane concentration is shown as methane is initially
introduced to the SOFC test rig, allowing the user to measure in
real time the time constants of the fuel system. A measurement
was taken every 20 seconds for a total time of 600 seconds and
was the time when methane was first measured in the gas
cell.

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JOURNAL OF LIGHTWAVE TECHNOLOGY, VOL. 31, NO. 9, MAY 1, 2013

Fig. 5. Methane concentration purge time through the in-line gas analyser as
methane is introduced into the SOFC test rig.

Fig. 6. The temperature of the gas cell as a function of time, recorded using a
TC-08 temperature logger, during warm up and isothermal operation.

In order to calculate the total purge time through the gas cell
a step response was fitted to the data in Fig. 5, of the form
(11)
where is the measured concentration,
is the final concentration, is the time in seconds and is the time-constant, calculated to be 50 s.
In order to ensure a true gas composition measurement for an
individual sample line it is necessary to purge a gas cell for 250
s, assuming 1% measurement accuracy is at a time of .
Fig. 4 provides the total purge time of the sample line and the
gas cell (540 s), whereas Fig. 5 only provides the purge time
of the gas cell (250 s). Therefore, the sample line purge time
can be calculated to be the difference in those purge times, i.e.,
290 s. The purging of the gas cell takes a significant amount
of time due to the much larger volume per unit length of the
cell, as compared with the sample line. This information is used
to ensure that following each change in sampling position or
incremental change in system operating conditions, the corresponding sample line measurement can be made with an appropriate time delay to ensure an accurate gas composition is
obtained.
V. WATER MEASUREMENTS
In addition to monitoring methane concentration from various points around the SOFC system, it is also important to measure the water concentration. This cannot be carried out directly
using GC as it is unable to directly measure water vapour concentration. Using the TDLS system it is possible to measure
the water vapour concentration in-situ. In order to ensure no
water vapour condenses upstream of the TDLS measurement,
the sample line from the SOFC cathode is trace heated and the
TDLS sensor is located as close to the SOFC as possible as
described in Section III. The temperature inside the cell was
recorded as a function of time during warm up and stable operation, and the results are shown in Fig. 6.
During isothermal operation the temperature varied by approximately 3 C between 65.568.5 C, providing an average
temperature value of 67 C. To estimate the contribution of the
temperature variation on the water concentration measurements,
concentrations have been calculated for a single absorption profile using three different temperatures, the maximum, minimum

Fig. 7. Recorded water spectra at 67 C, taken when the fuel cell was operating
at half-load, and a comparison with a theoretical profile.

and average temperature. The dry air line was chosen for this test
and the three calculated concentration values were 0.3745%,
0.3764% and 0.3759% respectively. The temperature difference
between the maximum and minimum temperature values accounts for a concentration variation of only 0.0019%. Using a
number of datasets for the dry air line the average water vapour
concentration was measured to be 0.367% with a standard deviation of 0.0141%. Therefore, the contribution of the temperature
variation is not the most significant factor in the concentration
measurement error. Finally, assuming a signal to noise ratio of
3 the lowest measurable absorbance has been calculated to be
using these datasets. This relates to a minimum
measurable water vapour concentration of 31 parts per million.
Water vapour concentration measurements were also taken
when the SOFC was operating at full-electrical load and halfload. At half-load the average water vapour concentration was
measured as 0.6378%, shown in Fig. 7, and at full-load the concentration was 0.83%; these values are proportional to fuel flow
rate at these specific test conditions.
The SOFC system must be able to operate under a range of
conditions similar to those that may be experienced by a commercial product. One of these is the moisture content of the
cathode. Fig. 8 presents the measurement of water vapour concentration as water is introduced into the SOFC cathode stream.
Measurements were taken at a rate of one measurement every
1020 seconds and four separate measurement runs were car-

LENGDEN et al.: TUNABLE DIODE LASER BASED CONCENTRATION MEASUREMENTS

Fig. 8. Measurement of water vapour concentration during water injection

to the SOFC cathode. Repeat measurements demonstrate repeatability of the
TDLS analysis method.

ried out. In the first run the cathode water-vapour concentration

was monitored for approximately 3 minutes prior to the injection of water into the SOFC test rig using a liquid mass flow
controller (MFC). A water flow of 8 ml/min was then injected
into the SOFC cathode, and was increased to a flow of 13 ml/min
after a further 8 minutes. The flow controller was then switched
off completely. This switch off can be seen more easily in the
second and fourth runs. In the third run, the water vapour concentration drops back to the nominally dry cathode value as the
MFC failed. It took approximately 4 minutes for the injected
water to be cleared from the SOFC and purged from the TDLS
sensor. Finally, as can be seen from runs 2, 3 and 4, the TDLS
system provides repeatable results for separate measurements
when the same flow of water has been injected into the SOFC.
VI. CONCLUSION
We have presented an optical system for measuring multiple
gases on an operational SOFC system. We have shown how this
TDLS system can provide comparable data to GC, but with a
reduced analysis time, potential for cost reduction and with the
added ability of direct water vapour measurements.
This system has provided new information on the purge times
of the SOFC and the gas sample lines from various locations,
providing all the necessary information for the implementation
of an automated gas sampling system. The time evolution of
both methane and water vapour concentration has been shown
for a number of different scenarios, providing further valuable
information to the fuel cell test-rig operator.
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Michael Lengden received the M.Phys. degree in physics and the Ph.D. degree from the University of Manchester, Manchester, U.K., in 2001 and 2006,
respectively, where he was engaged in stepwise excitation of atomic and molecular metastable states.
He was an Applications Engineer at the Laboratory Impex Systems, Ltd.,
prior to becoming a Research Fellow in the Centre for Microsystems and Photonics at the University of Strathclyde between 2007 and 2010. He is currently
a Lecturer in the EEE Department, University of Strathclyde, Glasgow, U.K.,
where he is engaged in high-temperature spectroscopy measurements using tunable diode laser spectroscopy. His current research interests include new techniques in tunable diode laser spectroscopy for concentration and pressure measurements in harsh environments, such as solid oxide fuel cells and aeroengines.

Robert Cunningham received the B.Sc. (hons.) degree in chemistry from the
Universiy of Glasgow, Glasgow, U.K., in 1989, and the Ph.D. degree in catalysis
from Brunel University, U.K., in 1992.
From 1992 to 1995 he worked at Eindhoven University of Technology, The
Netherlands, developing a new chemical process for the production of positronemitter labelled alkanes at the universitys cyclotron facility. From 1995 to 2000
he was employed as a post doctoral research fellow at the University of Keele,
where he investigated alkane steam reforming in solid-oxide fuel cells. Since
2000 he has been employed by Rolls-Royce Fuel Cell Systems Ltd. where he
has responsibility for SOFC performance analysis.

Walter Johnstone received the B.Sc. (Hons.) degree in chemical and material
sciences and the Ph.D. degree in laser physics from the University of Strathclyde, Glasgow, U.K., in 1977 and 1982, respectively.
From 1980 to 1986, he held Project Engineering and Senior Technical Management posts at Pilkington Optronics, Ltd. (now Thales) and Logitech, Ltd. In
1986, he joined the University of Strathclyde where he is currently Vice Dean of
the Faculty of Engineering and a Professor of Photonic Systems in the Department of Electronic and Electrical Engineering. Since 1994, he has been a Director of OptoSci, Ltd., Glasgow, where he has been instrumental in bringing a
number of photonics products to market. His work has led to more than 200 technical publications and several patent applications. His current research interests
include optical waveguide components, fiber lasers, distributed fiber sensing
systems, and optical gas sensing.