Photoacoustic instruments calibration method

Tomasz Borowski a, Tomasz Starecki b

a
independent researcher, Warsaw, Poland
b
Institute of Electronic Systems, Warsaw University of Technology,
Nowowiejska 15/19 00-665 Warsaw, Poland

ABSTRACT

Some aspects of calibration of photoacoustic instruments are discussed in this paper. In most reports concerning
photoacoustic experiments, measurement results are given in arbitrary units. Traditional calibration methods of
photoacoustic cells are based on measurements of known concentration of a reference substance. However, from the
point of view of such calibration methods, instruments of identical sensitivity but with different internal volumes will
produce different responses if the same amount of investigated specimen is used in both cases. This may create problems
in measurements when the amount of investigated specimen is limited. The paper presents a method that can be used to
improve calibration of photoacoustic cells and associated electronics. The method uses acoustical pressure produced by a
piezoelectric disc mounted in the cell and driven from an external oscillator circuit, so that it is possible to compare the
amount of sound energy with the amplitude of the electric signal at the sound detector output. In such a way it is possible
to evaluate energetic efficiency of the cell and the associated electronic circuit, to determine overall sensitivity of the
setup, its signal to noise ratio, etc.

Keywords: photoacoustic calibration, acoustic calibration

1. INTRODUCTION

The instruments based on photoacoustic effect were primary used as monitors for qualitative identification of substances
by determination of their specific photoacoustic characteristic spectrum – similar to “fingerprints”. In such applications
photoacoustic instruments response can be expressed in arbitrary units. However, when quantitative measurements are
required the photoacoustic instruments should be calibrated in terms of sample standard or in terms of energy units.
Additional benefits of this kind of calibration is a potential possibility of comparing sensitivity of different photoacoustic
instruments. It should be always taken into account that photoacoustic cell signal response depends not only on optical
and thermal properties of fluid (gas or liquid) filling the chamber, but also on many other factors, e.g. cell design, body
material, etc.

For the purpose of calibration a stable signal simulating photoacoustic signal response is required. The calibrating signals
should have stability at last one order better than the acoustic detector used. There are some methods that can be used for
generation of calibrating signals. All of them are based on techniques used for microphone calibrations. For example:
when a condenser microphone is used as an acoustic detector, the electrostatic excitation by a third electrode mounted
close to the microphone diaphragm is utilized. Another well know technique of absolute calibration of microphones is
pistonphone, in which the sound pressure is created by a vibrating mechanical piston mounted in the wall of the
measuring cell. Another method which can be used for calibrating photoacoustic instruments in terms of absolute energy
units is based on electrical heat generation. The sound pressure is produced by releasing heat by a thin film heater
mounted in the photoacoustic cell.1 The most accurate technique of acoustical calibration of photoacoustic instrument is
reciprocity technique, which is normally used for absolute calibration of condenser microphones.

Generally, the photoacoustic instruments performance is based on the acoustic effect which is a result of convertion of
the light energy absorbed by the specimen into energy of sound waves. The energy of sound waves is then converted into
electrical signal. Due to this fact any photoacoustic instruments characteristics depends on acoustical properties of the
cell, which depends on the cell design. And the acoustic signal response of photoacoustic cell can be measured by some

Photonics Applications in Industry and Research IV, edited by Ryszard S. Romaniuk, Stefan Simrock, Vladimir M. Lutkovski,
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 acoustical calibration methods. In such a case, accuracy of the measurements depends on accuracy of sound pressure
measurements. This paper present results of acoustical calibration of a photoacoustic cell by means of photoacoustic
effect and electromechanical method. Equivalency of acoustical energy, excited in photoacoustic cell by photoacoustic
effect and by electromechanical method has been already experimentally proved.2

2. PHOTOACOUSTIC CALIBRATION METHOD

In conventional photoacoustic experiments with gasous samples energy used for excitation of acoustical oscillation of
the fluid inside the cell is taken from light energy. The light is modulated at a given frequency. The absorbed light energy
is released by means of non-radiative internal intermolecular sequence process. The released energy is transferred to the
working fluid and if the cell volume is constant results in pressure oscillations which are converted by a pressure sensor
into electrical signal. Usually condenser microphone is used as a pressure sensor.

Amplitude of the photoacoustic signal depends on sample concentration and transducer’s efficiency. In case of low
sample concentration, the acoustical signal generated by photoacoustic effect is very weak. In order to increase signal to
noise ratio acoustic resonance amplification3, 4 of photoacoustic signal is often applied, but even after substantial
amplification, which can be done in many different ways,5, 6, 7 detection of photoacoustic signal is still very sensitive to
many factors. For example, the photoacoustic cell acoustical response depends on sample pressure and temperature
which influences speed of sound in the working fluid resulting in change of resonance frequency of the cell.
Fluctuations of the light source wavelength has also direct influence on the acoustical response. Traditional methods of
calibration of photoacoustic instruments are based on measuring a known concentration of investigated specimen or a
reference substance. In this method the light sources and light pathway must be also calibrated.

Process of calibration of an acoustical device requires use of calibrated energy source. In case of photoacoustic cell
calibration, the energy is taken from modulated light, which induces acoustical oscillations of the working fluid. The
energy used for the excitation of acoustical oscillations can be taken from another alternative source. A calibration
method which utilizes local gas heating by a thin film heater mounted in the window of photoacoustic cell has been
reported.1 When the heater is excited by a square wave voltage, it dissipates heat, which is transferred to the working
fluid and produces acoustical signal similar to the one that would be produced by an acoustical signal which would have
been produced by optical absorption in the window. Electrical energy dissipated by the heater is measured and is used to
calculate absolute sensitivity of the cell. The acoustical signal generated by optical absorption in the window is a parasite
signal. A drawback of the discussed method is that it reflects parasite acoustical effects generated by the light absorption
in the window instead of a sample volume absorption response.

Another calibration method and experimental background based on similar principle (electrical heating) is considered
elsewhere.7, 8 In this arrangement, on the surface of an optical absorber a platinum black had been electrochemically
deposited (like carbon black which is usually used by many researchers as a standard optical absorber). The principle of
calibrating photoacoustic cell in the method was based on assumption that the heat source can be approximated on
infinitisimally thin layer and the cell response under optical and electrical heating is identical and also the frequency
dependent effects are similar. By correlating optical and electrical heating of platinum black sample, the optical response
of the cell can be measured and expressed in terms of the electrical energy.

This above examples of photoacoustic instruments calibration by electrical heating demonstrate that alternative source of
energy used for excitation of acoustical oscillations is located not in the place where photoacoustic effect signal is being
induced, but on the window surface or optical absorber. Moreover, these properties of the method limitate use of the
method to the cells with closed cavities and were not discussed for windowless or Helmholtz photoacoustic cells.

Much convenient method for calibration of photoacoustic instruments is the acoustical calibration, because photoacoustic
cell is an acoustic device. The photoacoustic instrument characteristics depends directly on its acoustical properties.
Hence, acoustic calibration method of the photoacoustic instrument should be based on reciprocity theorem.8, 9

The reciprocity theorem assumes equivalent replacements of signal sources. It means that primary acoustical source can
be replaced by an equivalent acoustical source. According to reciprocity theorem, the transient function obtained from
direct course should be identical to the transient function of reciprocal process. The transient functions of the

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 photoacoustic cell determined during direct and reciprocal experiments should be similar and compliant. Then it can be
assumed that characteristics of the photoacoustic cell arrangement is linear. According to reciprocity theorem, the
volumetric acceleration of the sound source acting in place where the force is extorted by piezoelement, has the same
directional characteristic and acceleration as the photoacoustic signal which works like virtual “piston”.

3. RECIPROCITY METHOD

The reciprocity theorem was formed for acoustical systems by Helmholtz, for mechanical systems by lord
Rayleigh and for electromechanical systems by Ballantine. This principle has been extended to electrodynamics and to
propagation of electromagnetic waves, light and to acoustic measurements applied to accurate, absolute calibration of
microphones and vibration sensors. The reciprocity method was established as the primary standard for acoustics.10 The
essence of the reciprocity method is based on the ability of acoustical transducers to be used as sound sources as well as
sound receivers. The additional assumption of reciprocity calibration method is that the calibrated system should be
linear, passive, reversible and should have limited degree of freedom. Fortunately, the photoacoustic Helmholtz cell
fulfills these requirements. The acoustic coupling impedances of photoacoustic avity and microphone cavity are constant,
so the output voltage of the microphone is the only variable. If the sources of the acoustic fields (generated by
photoacoustic effect and by piezo acoustic transducer) are coupled and they are acting in different ways, the results of
their activity can be measured by measuring transmitter’s drive current, the coupler impedance and microphone output
voltage. Then if the method is used in calibration process of sound sources, it utilizes inverting properties of transducers.
As a result, relative sensitivity of the microphone, piezoelement, etc. can be defined.

Rayleigh confirmed8, 9 that a prerequisite and sufficient condition of reciprocity is a feature of linear, passive and
dynamic systems which have limited numbers of freedom degree. The system must also contain reversal elements which
can oscillate around equilibrium level. The principle of equality of acoustical sound sources is related to these sources
which in effect of periodic excitation produce sound, and as a result distribute in the same time the same amount of
energy. According to the above statement, the principle is valid and can be used in acoustical devices which are
stimulated to oscillation by external energy. It does not matter from which source and by which way the energy is
applied to the oscillating system. Therefore, an acoustical arrangement used in photoacoustics, like Helmholtz
resonators, can be classified as an energetic method. The energy used for excitation of the sample to acoustical
oscillation is taken from the light. When the sample is not excited by the light then the whole photoacoustic cell is in
equilibrium state and there is no photoacoustic response. When the light is switched on, the photoacoustic signal
response appears. The photoacoustic signal is converted into electrical signal by a condenser microphone. The diaphragm
movements is the effect of an external force. It can be proved that the force is responsible for diaphragm movements and
transfer of the photoacoustic signal energy into microphone.

Analysing acoustical response of the photoacoustic instrument (e.g. in Helmholtz resonator) two stages can be pointed
out. In the first stage the sample placed in the cell is irradiated by light. Some of the energy of light is absorbed and then
it is converted into heat, which in constant volume of the cell causes increase of the gas pressure. The pressure influences
the microphone’s diaphragm (force P1) and results in its movement (way F11). The work performed by this force equals:

A1= ½ P1F11. (1)

Is the second stage, when the light is switched off, the delivery of light energy is stopped. As a result, the gas pressure
decreases. During calibration of photoacoustic cell (in the second stage), the voltage is applied to the piezoelectric
transducer and as a result the additional pressure P2, which similarly to the pressure P1 influences microphone’s
diaphragm causing its additional displacement F22. The additional AII2 work is performed:

AII2= ½ P2 f22. (2)

In this stage force P1 on the way F12 performs work AII1:

AII1= ½ P1F12. (3)

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 The total work performed in these two stages equals:

A = AI+AII+AII1 = ½ (P1F11+P2F22+P1F12). (4)

If we exchange the sound sources, in photoacoustic cell the total work equals:

A’ = ½ P2F22 + A1F11 + P2F21. (5)

And according to the independence acting theorem A = A’. As a result:

P1 F12=P2 F21. (6)

Sensitivity of calibrator is the ratio of electrical voltage and acoustic output. Microphone is an acousto-electrical
transducer which sensitivity is defined as the ratio of its electrical output to acoustical input:

S=V/a [V/Pa], (7)

where:
V - electrical output,
a - acoustical input.

The electrical impedance of transducer, located in the photoacoustic cell, depends on acoustical impedance of the cell,
which depends on mechanical dimensions, thermal and viscosity properties of the working fluid.14, 15, 19, 20, 21

If piezoelement transducer is denoted as A and microphone as B, the acoustical impedance of the cell ZPAC including
both transducers is given by:

ZPAC = γ PBARO / j ω (V + VAe + VBe ), (8)

where:
γ – is the ratio of specific heat of the working fluid,
ω = 2 πf , where f is the signal frequency,
V – equivalent volume of the cavity,
VAe – equivalent volume of the piezo-transducer,
VBe – equivalent volume of the microphone.

The pressure inside the cell is given by:

p = u ZPAC = u γ PBARO / j ω VPA, (9)

where:
u – volume velocity,
VPA = V + VAe + VBe – volume of photoacoustic cell.

The ratio of the volume velocity u to the current I used as a source of sound generated by piezoelement is equal to the
ratio of the voltage eA on the piezoelement to the sound pressure p acting on the microphone diaphragm when used as a
acoustic receiver and is equal to the ratio of the voltage eB to pressure p when sound pressure p is acting on the
microphone diaphragm when photoacoustic signal is produced. On the base of the reciprocity theorem the sensitivity of
the transducers can be expressed as follows:

SA = u/I = eq / p, (10)
SB = eB / p, (11)
SPAS = ePAS / p. (12)

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 After multiplying SA (9) by SB (10) and substituting p from (9) we get:

SA * SB = (u / I) / (eB / p) = SA * SPAS. (13)

The ratio of the voltage applied to the electrical side of the transducer to acoustical velocity produced on the mechanical
side is equal to the ratio of mechanical force applied to the mechanical side and the current produced on the acoustic
pressure detecting side. The relations between direct and reversal effects on acoustic and electric sides are quantitatively
connected by reciprocal relations. Hence, the piezoelectric transducer and condenser microphone satisfy requirements of
the reciprocal theorem. The Helmholtz theorem is exemplified by sound fields produced by simple point sources acting
in closed chamber. This theorem is valid even if there is a partial barrier and the walls of the chamber partially absorb the
sound energy between the sound sources. Supposing many simple sound sources, which create a sound field, the
theorem can be extended to acoustic field, no matters what way produced. Generally the reciprocity theorem applies to
electromagnetic waves of all spectrum and all cases, with exception of Faraday effect. Then the reciprocity of sound
sources is preserved when the sound is produced by optical means – e.g. by photoacoustic effect in fluids.

In case of a photoacoustic cell, the barrier might consist of a wall with a hole or short duct. In such a case, when simple
point sources act in sample cavity A, the volume velocity ua is produced. When activity of a simple point sound source
“a” producing volume velocity ua results with pressure pb at point “b”, then in reversal process: ub’ at point “b”
produces pressure pa‘ at point “a”, so that ua pa‘ = ub’ pb . The reciprocity is preserved when a source of sound at
point “a” produces (by photoacoustic means) sound pressure pb at point “b”. In case of photoacoustic sound generation
the reciprocity is also preserved. When simple photoacoustic point source of volume velocity uaPAS at point “b”
produces sound pressure ub’ at point “a” , then in reversal process produces pressure pa‘. So that uaPAS pa‘ = ub’ pbPAS .
The primary acoustic energy of the sample response to excitation by the light pulse is distributed to all elements
participating in its transferring process and then dissipated. The distribution depends on acoustical impedances of all the
components of the acoustical system. When the sample is in the form of solid, energy of photoacoustic signal is partially
distributed to the sample substrate body and partially to the environment, e.g. into the surrounding gas. In case of liquid
sample the primary energy of photoacoustic signal is distributed to the liquid and/or gas and partially to the walls of the
sample holder. For gas samples the energy of photoacoustic signals is distributed to the other gas molecules and/or to the
other idler gas molecules of the sample. In all cases the acoustical signal depends on photoacoustic cell design and is
being distributed amoung acoustical modes of cell. So the acoustical and thermal properties of the working fluid depend
on composition of fluid (gas sample / idles gas) pressure, and temperature. The photoacoustic method of calibration can
use any light wavelengths. Only photo-dissociation of the sample can limit use of this method to some specific
wavelengths.

4. EXPERIMENTAL SETUP

The cell used in calibration experiments was a Helmholtz resonator showed at fig. 1.
BK7 silica
glass window

condenser
microphone microphone preamplifier

piezoelement
transducer
Fig. 1. A cross-section of the cell used in calibration experiments.

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 All parts of the experimental cell were made of brass. The sample cavity was 10 mm in diameter and 20 mm long. The
interconnecting duct was 1 mm in diameter and 20 mm long. The window was made from BK7 quartz lens and silicone
sealed. For acoustic signal detection a ½” condenser microphone, with sensitivity of 50 mV/Pa was used. The
piezoelectric transducer disk like diaphragm, made of PZT (lead-zirconate-titanate) was attached to the backside of the
sample cavity of the cell and clamped by a plate with electrical contacts. One electrode of the PZT was grounded through
the brass resonator chassis, the second was connected to the control voltage. Displacement of the piezoelectric transducer
disk was proportional to applied voltage. If the voltage was modulated, the transducer generated acoustical pressure in
the cavity. The measurements and control were performed by means of a dedicated microprocessor system.12, 13
Piezoelectric transducers have been already used in many photoacoustic experiments - e.g. for determination of the
resonance frequency and quality factor of the full-wavelength resonator tube.11

A system used for experiments on reciprocity acoustical calibration of the photoacoustic instrument is shown in Fig. 2.
Transducer A (the piezoelectric disc plate) was mounted in the sample cavity. Transducer B (a ½” condenser
microphone) was placed in the microphone cavity. Both cavities were coupled by a cylindrical channel. The light energy
source used in the experiments was a high power infrared LED. Transducer A generated calibrating signals and was
driven by the same signal that was used to control the light source.

Light source

Sample + 200V
cell Condenser
Microphone

Preamplifier

Cp

Piezoelement

C1 Cs

Input A Input B
R Computer
Oscillator
measurement and
Reference control system
Signal

Fig. 2. A block diagram of the system used for experiments with acoustical calibration of photoacoustic instruments.

5. RESULTS

The experimental setup was used for determination of frequency responses of the photoacoustic cell (with carbon black
and air) by means of photoacoustic and acoustic (sound induced by a PZT piezoelement) methods. The light source used
in the experiments was emitting infrared 940 nm light, modulated with a 50% duty-cycle square wave. Both measured
frequency characteristics are shown on fig. 3 and 4 respectively.

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 Amplitude [V] Amplitude [V]
1,2 a) 4
b)
3,5

1
3

0,8 2,5

2
0,6

1,5

0,4

0,2
0,5

0 0

0 500 1000 1500 2000 2500 3000 3500 4000

0 500 1000 1500 2000 2500 3000 3500 4000

Frequency [Hz] Frequency [Hz]

Fig. 3. Amplitude of the acoustic signal excited in the cell by photoacoustic method (a) and acoustic method (b).

Amplitude [V]
4

3,5

3
acoustics signal

2,5

PA signal
2

1,5

0,5

0 500 1000 1500 2000 2500 3000 3500 4000

Frequency [Hz]

Fig. 5. Normalized amplitude of acoustic signal excited by photoacoustic effect and acoustic method.

6. CONCLUSIONS

In this paper behaviour of photoacoustic and acoustical calibration method of photoacoustic instruments was
experimentally studied. The acoustic method can be used for improved calibration of photoacoustic instruments and
associated electronics. The method uses acoustical pressure produced in the cell not by converting the energy of
irradiating light into energy of sound waves, but by a piezoelectric disc mounted in the cell and driven from an external
oscillator circuit. It is possible to compare the amount of the sound energy to the amplitude of the electric signal at the
sound detector output, and in this way to evaluate energetic efficiency of the cell and efficiency of the associated
electronic circuit, determine overall signal to noise ratio, setup sensitivity, etc. The additional benefit of the method is
possibility to compare acoustic properties of different photoacoustic instruments and conversion efficiency of the cell.

Traditional calibration methods of photoacoustic instruments are based on measurements of a known concentration of
investigated specimen or reference substance. These methods require calibration of the light sources and light pathway.
Limited amount of the measured sample (e.g. toxic substance) results in problems with calibration of photoacoustic
instruments. This drawback can be eliminated is the discussed method of calibration is used. The experimental results
showed good agreement between electrical response of microphone to optical and acoustical excitation of photoacoustic
cell. The high linearity of both responses allow for use of the acoustical calibration as a calibration method.

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 Acoustical field reciprocity can be used for excitation and detection of acoustic waves in photoacoustic resonators and
can be used for calibration of photoacoustic instruments. The experimental results proved that acoustical calibration of
the photoacoustic cell, based on reciprocal technique, is in compliance with calibration procedures based on standard
calibration techniques.

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