Anal. Chem.

1998, 70, 179R-208R

Chemical Sensors
Jir Janata* and Mira Josowicz

School of Chemistry and Biochemistry, Georgia Institute of Technology Atlanta, Georgia 30332-0400

Petr Vanysek

Department of Chemistry, Nothern Illinois University DeKalb, Illinois 60115

D. Michael DeVaney

Pacific Northwest National Laboratory,1 Richland, Washington 99352

Review Contents Table 1

Thermal Sensors 181R average
%
Mass Sensors 182R topic 1985-1989 1990-1991 1992-1993 1994-1997 % change
Electrochemical Sensors 182R reviews 78 145 347 453 22 +30
Potentiometric Sensors 183R thermal 6 15 12 64 3 +435
Amperometric Sensors 190R mass 21 40 126 182 9 +44
potentiometric 419 309 260 374 18 +44
Conductometric Sensors 192R amperometric 96 210 208 356 17 +71
Optical Sensors 195R conductometric 66 101 123 275 13 +123
Conclusions 197R optical 62 142 312 364 18 +16
References 198R totals/year 668 962 1391 2070 +49

In this review we are trying to cover the four-year gap in this
series (A1). In this period, over 8278 references (in English only)
have been retrieved from the Institute of Scientific Information
database by the same search routine that was used previously. It
represents 49% increase in the total. This relative increase alone
attests to the vitality of the chemical sensing field. However, the
absolute figures are somewhat distorted by the fact that many
papers using term sensors really describe a sensing system (i.e.,
a chemical assay). Moreover, the trend to publish the same data
several times, under a slightly modified title, has become a
common practice in all fields of science, and chemical sensors
are not an exception. As much as possible, we tried to use only
one article from such multiple clusters. With this amount of
information, it is only possible to scan the titles of the individual
papers and then to select only approximately 10% for the final
review. We hope that our colleagues whose paper is not cited
understand that the decision to include or not to include a paper
does not imply our judgment of the quality of that paper.
It is interesting to see where are most chemical sensor papers
published. From the papers included in this review, 17% appeared
in Sensors and Actuators, B, 11% in Analytical Chemistry, 6% in
Analytical Chimica Acta, 4% in Electroanalysis, and 3% in The
Analyst. The remaining 60% is scattered throughout the literature.
This surprisingly high figure indicates that the subject of chemical
sensors is not a hobby of a few specialists but draws from a broad
scientific and engineering base.
Our aim has been to provide a critical assessment of the new
trends, features, and distribution of effort in the entire chemical
sensor field. This information is summarized in Table 1, which
1 Pacific Northwest Laboratory is operated by the Battelle Memorial Institute
for the U.S. Department of Energy under Contract DE-AC06-76RLO 1830.
S0003-2700(98)00010-9 CCC: $15.00 1998 American Chemical Society
Published on Web 05/19/1998
shows the cumulative totals, percentage representation of the
individual types of sensors, and the change since the 1994 review.
The cutoff dates of this review period were 1 December 1993 until
30 November 1997.
The review is structured similarly to the previous reviews in
this series; i.e., it is divided by the transduction principles to
thermal, mass, potentiometric, amperometric, conductometric, and
optical sensors. The Introduction contains books and reviews.
Also included in the Introduction are the papers discussing
subjects of general interest that transcend the dividing boundaries
given by the individual transduction principles, such as data
reduction, fabrication, selectivity issues, etc. The selection rules
for this section are slightly different from the rest. Here we have
included reviews regardless of the language and only those
containing 50 or more references. The reviews dealing with a
specific transduction principle are included in the Introduction to
that particular section. The entire sensing database from which
review is written is available on the Web. The address is http:/
/www.chem.tamu.edu/walker/chemsensors.html.
Books and General Reviews. The maturity of the chemical
sensor field is reflected in a large number of books devoted to
sensors in general (A2-A4), biosensors (A5-A10), and gas
sensors (A11, A12). Whenever possible, we tried to exclude
bound proceedings of sensor conferences because they usually
contain material that had been published in regular journals or is
otherwise unpublishable.
Selectivity. The quest for better selectivity remains the
cornerstone of the chemical sensing research. It follows two
different routes: biologically derived selectivity, i.e., biosensors
and synthesized selective materials containing specific binding
sites, or selective matrixes, i.e., chemical sensors.
Analytical Chemistry, Vol. 70, No. 12, June 15, 1998 179R
 Biosensing in general has been the most reviewed topic both
in the article (A13-A15) and in the book form. Several general
discussions of enzyme sensors have been published (A16, A17).
Peroxidase-modified (A18, A19) and NAD dehydrogenase-modi-
fied (A20, A21) electrodes offer selectivity and a common
transduction principle for amperometric sensing of many oxidiz-
able substrates, such as neurotransmitters (A22). Conducting
polymers (A23-A25) and redox hydrogels (A26) provide a
convenient matrix for enzymes requiring electron transfer. On
the other hand, enzymes immobilized in inorganic supports have
been reviewed (A27). Synthesis of polymeric microcapsule array
containing enzymes has been described (A28). Metalloproteins
are closely related to enzymes in their application in chemical
sensors (A29). Hydrophobic enzymes working in nonaqueous
solvents (A30) have been suggested for optical sensors (A31).
Direct electron transfer in electrochemical enzyme sensors has
been discussed (A32). Epoxies containing graphite particles with
immobilized enzymes have been used as sensing layers in
amperometric biosensors (A33).
Immunochemically derived selectivity receives continuing
attention (A34) despite the obvious problems with the reversibility
and kinetic nature (A35-A37) of the antibody-antigen reaction.
The structure-binding relationship in antibody-antigen complex
formation and the role of orientation of immobilized immu-
noreagents (A38) have been examined (A39). A general strategy
for immobilization has been suggested (A40). Another class of
related recognition sites is catalytic antibodies, which combine
enzymatic and immunochemical functions in chemical sensors
(A41). Odorant-binding proteins have been suggested for con-
struction of odor-discriminating biosensors (A42, A43). The
general issue of protein-ligand recognition (A44) and molecular
modeling of host-guest inclusion (A45) has been discussed in
the context of chemical sensing.
Principles, manufacturing, and applications of immunochemical
internal reflectance biosensors have been reviewed (A46). The
potential for clinical application of immunosensors remains high,
but the only sensors that have found some commercial application
so far are optical immunosensors (A47). Nevertheless, electro-
chemical immunosensing has been reviewed (A48). A combined
immunochemical-enzyme approach to selectivity has been de-
scribed (A49).
Introduction of DNA to the direct chemical sensing area did
not have to wait too long, and biosensors utilizing DNA as the
recognition element (A50) have been given a new names
genosensors (A51). The irreversibility of this highly selective
binding places the DNA-based devices among detectors or assays,
rather than among conventional sensors (A52). A comparison
has been made between biosensors based on enzymatic, immu-
nochemical, and DNA recognition principles (A53).
A new type of glucose sensing based on an old principle has
been investigated. It involves formation of complexes between
boronic acid and various saccharides (A54). The use of glucose
oxidase in glucose sensors is an old subject, and the review of
this topic is included here only as an update (A55). Definitions
and official nomenclature for biosensors have been recommended
by the IUPAC (A56).
Synthetic as opposed to biologically derived selectivity in many
cases tries to mimic biochemical interactions. Molecular recogni-
180R Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
tion by supramolecular materials (A57, A58) has been proposed
for potentiometric (A59) and mass sensors (A60) for gases, vapors
(A61), and liquid media (A62). Molecular recognition of analytes
is a hot and controversial topic (A63). Thus, the reality of specific
recognition of vapors by cavitands has been shown to be wrongly
interpreted (A64). Phthalocyanines have been used as selective
materials in all types of chemical sensors (A65). On the other
hand, tunable selectivity of phenanthroline complexes has been
demonstrated for electrochemical sensors (A66). Calixarenes
have been used as specific binding sites in sensors based on
different transduction principles (A67-A69).
Molecular imprinting (A70-A72) is an idea that was intro-
duced in mid-1950s by Linus Pauling and that has now attracted
the attention of researchers developing selective layers for
chemical sensors. Its true value in chemical sensing remains to
be seen. Imprinted polyurethanes have been used for construction
of optical sensors (A73). A review containing over 700 references
covers the subject of fluorescence modulation by recognition
events. Composite materials used for optical (A74) and electro-
chemical (A75) sensing have been reviewed.
Self-assembly became a popular method of creating selective
layers for chemical sensors from, for example, phthalocyanines
(A76) or lanthanides (A77). The thiol-gold system dominates
this type of materials (A78). One of the oldest forms of
self-assembly is formation of free-standing and supported black
lipid membranes (A79, A80). Membrane proteins promote natural
self-assembly and can increase the mechanical stability of sensing
membranes (A81, A82). A 3-D self-assembly on the millimeter
scale has been demonstrated (A83). Self-assembled multilayers
(A84) and immunochemical layers (A85) have been described.
The Langmuir-Blodgett (LB) technique offers a better control
of creating thin films than the self-assembly although it is more
expensive and more difficult to use. Selective layers based on
LB films have been reviewed (A86) and the electron transfer and
mechanism of redox reaction in these systems have been
discussed (A87).
The selectivity can be also derived from the matrix not
containing any bona fide binding sites. In that respect, various
polymers remain the key building blocks of many chemical
sensors (A88). Organic polymeric membranes (A89) with cata-
lytic properties can be used in different types of chemical sensors.
Electroactive polymers are a class of materials that can be
conveniently used in many types of chemical sensors (A90-A92)
and biosensors (A93). Immobilization of metalloporphyrins in
these materials provides specific binding sites (A94).
Semiconducting metal oxide sensors (A95, A96), particularly
tin dioxide sensors (A97, A98), remain the most popular type for
automotive application. A bismuth oxide sensor (A99) is claimed
to offer some advantages over zirconium oxide sensors. Gas
sensors based on sulfate electrolytes (A100) and solid-state
electrolytes for chemical sensors (A101) have been reviewed.
Ceramic materials are the heart of many gas sensors (A102). The
assessment of the status of gas sensors and prediction of future
trends in this field have been presented (A103). There are several
reviews of proton-conducting materials for chemical sensing
(A104, A105). Matrixes created by the sol-gel process have
become a popular medium for immobilization of biological
molecules (A106-A108).
 Sensing Arrays and Higher-Order Sensors. Relatively new
and probably the most important trend in the chemical sensors
today are higher-order sensors and chemical sensing arrays.
Higher order means that more than one transduction principle
is applied to the same selective layer. For example, a selective
layer on a surface acoustic wave sensor can be simultaneously
interrogated as a chemiresistor or optically. On the other hand,
an array of different selective layers used in the same transduction
principle forms a sensor array of zero order. Both the order and
the number of sensing layers in the array increase the number of
data acquisition channels and thus the information content (A109).
It is essential that the different layers and higher-order sensors
are orthogonal in their response.
Rules for calibration of chemical sensing arrays have been
discussed (A110, A111). The use of neural nets for evaluation
of response from sensing arrays has been described (A112-
A114). A new name has been coined for the neural nets for
chemical sensorssChemNets (A115). The public domain software
PLSToolbox is a useful tool for chemometric evaluation of
response from sensing arrays (A116). A self-diagnostic feature
of a gas sensing array has been described (A117).
Progress in the sensor arrays has been summarized (A118).
It has been shown that the electrodes can be conveniently
arranged as interdigitated array of microelectrodes (A119). An
array of microhot plates has been described for detection of gases
(A120). A sensor array for tracking gradients of vapors and gases
(chemotaxic sensors) has been described (A121, A122).
Machine olfaction became a hot topic in the recent years
(A123-A125) and quickly became known as an electronic nose.
An electronic nose for detection of pollen has been described
(A126), but the electronic feature for suppression of hay fever
has not been mentioned. Mimicking of taste sensing using
chemiresistor arrays of phospholipid membranes has been dem-
onstrated (A127). Surprisingly, it has not yet been advertised as
the electronic tongue.
Another new trend has emergedsselectivity derived from the
dynamic behavior of the sensors. Thus, information contained
in the kinetic, as opposed to the steady state, part of the response
has been a focus of several reviews (A128) and articles (A129-
A132). Neural nets have been used for dynamic signal processing
(A133). Noise from the chemiresistor has been used as the
source of information in gas sensing (A134), and the chaotic
behavior of a biosensor has been analyzed (A135).
Description of a simple classroom experiment of monitoring
urea (A136) is an encouraging sign of the recognition of the
chemical sensors as an integral part of the academic curriculum.
Fabrication. An important aspect of fabrication of sensing
arrays is the ability to deposit multiple selective layers in defined
areas of the chemical sensor. This requirement presents both
materials and processing challenges, which increase with the
diminishing feature size of the sensor. In that context, the ultimate
limits of miniaturization of chemical sensors have been discussed
(A137). Dry (A138), ion beam (A139), electron beam (A140),
electrochemical (A141), and laser (A142) patterning of selective
layers has been described. A laser-assisted deposition has been
used for fabrication of biosensors, molecular electronic devices
(A143), and Nasicon and similar thin films (A144, A145). A
spatially controlled membrane deposition has been used in
fabrication of an integrated pO2, pCO2, and pH sensing array
(A146). Atomic force and fluorescence microscopies have been
used for characterization of patterned sensor surfaces (A147).
Photocurable polymers (A148) such as poly(vinyl alcohols)
(A149) are interesting for fabrication of sensing arrays. The
biocompatibility of polyurethanes used in construction of chemical
sensors has been critically evaluated (A150). Immobilization and
patterning of bacterial surface layers, so-called S-layers, on
biosensors (A151, A152) is a new addition to the library of
selective materials. The ability to immobilize biomolecules
photochemically opens a possibility for patterning sensing arrays
(A153-A155). An oriented immobilization of cell adhesion
protein onto the chemical sensor surface is an interesting design
tool (A156).
Applications. Specialized reviews describe the use of bio-
sensors in pharmaceutical (A157-A160), food (A161), clinical
(A162), and gas analysis (A163). Different principles can be
employed for sensing of oxygen in biomedical applications (A164).
Environmental sensing and monitoring is a subject of several
general reviews and covers both gas (A165) and liquid (A166)
applications.
The changing geopolitical situation impacts the sensor and
sensing systems applications as well. There is a growth of
literature describing sensors for security and defense applications
aimed mainly at the detection and prevention of terrorist activities
and detection of illicit substances in general (A167, A168). A
comprehensive review of detection of explosives (A169) and
organophosphorus compounds (A170) has been prepared. Many
of these sensors are based on inhibition of cholinesterase activity
(A171).
THERMAL SENSORS
Reviews of thermal sensors in general (B1), sensing arrays
based on tin dioxide (B2), pyroelectric sensors (B3,-B5) and flow-
through enzymatic reactors with thermistor detection, so-called
enzyme thermistors (B6), have been published.
It has been shown that ac modulation of thin-film pyroelectric
transducer (B7) or a Si-planar pellistor (B8) improves the response
to natural gas and methane. Similarly, a 20-Hz vibration of enzyme
thermistor improves the thermal noise rejection of this sensor
(B9).
Several new ideas and applications have emerged in the
thermosensing of gases. A solid-state catharometer with some
selectivity for different gases (B10), a pellistor array based on
Si-planar technology (B11), and a thick-film pellistor array (B11)
have been reported (B12). Detection of gases and organic vapors
by the photopyroelectric effect has been demonstrated (B13-
B15). A pyroelectric structure useful for sensing was prepared
using the LB method (B16). Change in the thermionic emission
due to the chemical modulation of work function appears to be a
new sensing principle (B17). The Seebeck effect has been used
as the transduction principle for sensing of combustible gases
(B18). A thermopile was used for measurement of heat absorp-
tion upon inclusion of organic vapors in various clathrates (B19)
and free-standing membranes (B20).
New materials for fabrication of pyroelectric sensors based on
perovskites (B21) and new copolymer materials (B22) have been
introduced. Correlation between porosity of the pellistor and its
response has been observed (B23).
Analytical Chemistry, Vol. 70, No. 12, June 15, 1998 181R
MASS SENSORS
A large number of papers and reviews in this category attest
to the popularity of sensors based on mass detection. Application
of acoustic wave sensors for liquid and gas sensing has been
reviewed (C1, C2). Mass sensors have been used for environ-
mental applications (C3). Figures of merit for different types of
mass sensors have been critically compared (C4), and mass
sensitivity of the Rayleigh and the Love waves have been
compared (C5, C6).
Impedance Analysis. Analysis of the complete admittance
curve has become a more refined approach for obtaining informa-
tion from both the quartz crystal microbalances (QCMs) (C7-
C9) and other mass transducers, such as surface acoustic wave
(SAW) devices (C10), and flexural plate (FP) devices (C11). This
analysis is necessary for the use of piezoelectric oscillators in
liquids (C12, C13) or with bioselective layers (C14-C16). A
theoretical model of energy transfer between the oscillating crystal
and the surrounding medium (C17) and the analysis of electrode-
separated piezoelectric sensors have been developed (C18). The
dynamic response of a QCM (C19) or SAW device (C20) is
another approach that can be used to enhance the chemical
selectivity for mass sensors.
There are several papers in which arrays of CMS for detection
of organic vapors and gases are described (C21, C22). Increasing
the number of selective elements in an array does not necessarily
lead to a more powerful information acquisition. The procedure
for determining the optimum type and number of selective layers
in an array has been discussed (C23).
Selective Layers. A rational as opposed to a random selection
of selective materials is the preferred approach for optimal design
of mass sensors and sensor arrays. A good correlation between
the vapor sorption and linear solvation energy for fullerenes has
been obtained (C24). Semiempirical molecular orbital theory was
used to predict gas/polymer interactions and the resulting
response of the QCM (C25, C26). Films containing modified
calixarenes (C27-C29) and cyclodextrins (C30) have been used
for selective sensing of organic compounds with SAWs. Paracy-
clophanes were found to act as specific layers for detection of
aromatic and chlorinated hydrocarbons (C31). Dendrimers (C32)
are a class of compounds that offer a range of designed selectivity
for use with mass sensors. Self-assembled monolayers (C33),
electrodeposited phospholipid films (C34), polythiophene LB films
(C35), and zeolites (C36) have been used as selective layers for
QCM. A complete admittance analysis was required to interpret
response of QCM coated with a clay selective layer (C37). The
degree of penetration of vapors of branched and linear hydrocar-
bons into fluorinated polyimide film has been studied in detail
using SAW (C38). Chirality is another aspect of chemical
selectivity that can be probed by mass sensors (C39, C40).
Selective intercalation of inorganic gases into metal phosphonates
offers a high degree of selectivity (C41).
Coupling selectivity of immunochemical and DNA interactions
with mass detection is a relatively old hope. The analysis of the
complete resonant curve or the use of different modes of vibration
has been examined as the possible means of avoiding the usual
pitfalls associated with the interfacial energy transfer in such
systems. Thus, performance of an immunosensor based on
horizontal polarized-SAW (C42) has been studied, and combined
182R Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
electrochemical/mass detection is claimed to be the basis of a
new immunosensor (C43). The effect of immobilization of DNA
on QCM has been examined (C44-C46).
Effects Related to Mass Change. Mass sensors are more
than just an analytical tool. Diverse effects have been studied
that rely on coupling of the chemical layer to the electromechani-
cal device through interfacial effects such as adhesion, wetting,
and microviscosity. The acoustoelectric effect on QCM operated
in liquids has been studied (C47). The feasibility of using SAWs
to determine adhesion of polyimide films to quartz has been
examined (C48). The effects of temperature and humidity on the
response of polymer-coated acoustic wave sensor arrays for gas
sensing has been evaluated (C49). Closely related are the
dewetting effects observed with polymer-coated SAW devices
(C50). The well-known temperature sensitivity of QCM has been
employed for calorimetric/mass measurements (C51). Simulta-
neous measurement of mass and viscosity (C52) and phase
transitions in lipid multilayers (C53) have been described. The
use of QCM for determination of potential of zero charge has been
described (C54), and chemical effects induced by the acoustic
waves have been described (C55).
Simultaneous measurement of multiple parameters (i.e., higher-
order sensors), such as mass and resistivity changes of polypyrrole
(C56) has been described. Grazing angle spectroelectrochemistry
was combined with QCM as a powerful tool for electrochemical
studies (C57). Assessment of the electrochemical quartz crystal
microbalance (EQCM) as a sensor and electrochemical tool has
been published (C58).
Design and Fabrication. New design features extend the
potential usability of mass sensors to some challenging applica-
tions. An acoustic wave sensor integrated with IC electronics has
been designed (C59). A probe consisting of two independently
oscillating and electrically isolated crystals has been used for liquid
and gas sensing (C60). It has been shown that by vibrating the
entire QCM the adverse effects of coupling of the shear-mode
energy to the surrounding liquid can be mitigated (C61). Piezo-
electric layers prepared by thick-film technology have been used
as substrates for mass sensors (C62). Resonating microcantile-
vers have been used as mass sensors for detection of vapors
(C63). It has been shown that 10-m-thick tensioned polymer
films can be used as oscillators for mass sensing (C64).
A partial casting on water (C65) and a multiple-droplet selective
layer casting (C66) were used to build a SAW array sensor.
ELECTROCHEMICAL SENSORS
A comprehensive review of electrochemical sensors is included
in a book on solid-state electrochemistry (D1). There is a large
number of reviews of biosensors based exclusively on electro-
chemical principles (D2-D4). Different types of chemical sensors
have been used for electrochemical sensing of gases of medical
interest (D5).
A review honoring the work of the late Professor W. Simon is
a fitting tribute to one of the leading scientists in the field of ion-
selective electrodes (ISE) (D6). Specialized reviews dealing with
perfluorinated ion-exchange membranes (D7), conductive epoxies
(D8), potentiometric sensors for pharmaceutical applications (D9),
intracellular ISEs (D10), and NMR techniques for investigation
of glass membranes (D11) have been published. The issue of
selectivity and detection limits of ISE has been revisited (D12-
D14). Ion-sensitive field effect transistors (ISFETs) and other
miniaturized ion sensors are the subject of another recent review
(D15). The performance of ISEs and ISFETs in flow systems has
been critically evaluated (D16). A review containing over 300
references of synthetic ionophores for the lithium ion (D17) and
detection of surfactants by electrochemical sensors (D18) has
been published. Preconcentration of analytes into the bulk of the
selective layer in amperometric sensors is one way to achieve
lower detection limits (D19). Nanostructuring of gold electrodes
has been used as the means of fabricating an electrochemical array
(D20). Modified carbon paste electrodes (D21-D24) receive
continuing attention as selective amperometric probes for organic
(A22) and inorganic species (D25, D26).
POTENTIOMETRIC SENSORS
(1) General Introduction. The IUPAC Commission on
Electroanalytical Chemistry critically elaborated procedures for
calibration of ISE and limitations of new approaches for determi-
nation of selectivity coefficients. Calibrations by metal ion buffers,
serial dilution, and flow procedures were discussed and compared.
Comments on activity standards, concentration standards, and
ionic strength were made (D27). The critical evaluation of
limitations of the Nicholsky-Eisenman (N-E) equation for the
detection of potentiometric selectivity coefficients, KA,Bpot, ions of
unequal charge, non-Nernstian behavior of interfering ions, and
activity dependence of KA,Bpot resulted in recommendation of
methods for reporting KA,Bpot values (D28).
IUPAC recommendations have been also made about terminol-
ogy and conventions for ISFET devices (D29). The terms gate
voltage, drain current, and gate bias potential were defined,
experimental techniques for measurements with ISFETs were
summarized, and the appropriate graphical representation of the
output signal was presented.
Thermodynamic interpretation of EMF of polyionic membrane
cells in terms of mixed activities was proposed for the detection
of transfer numbers of ions and solvent across membrane and
for the detection of selectivities of membranes to be used in ISEs
(D30). A measuring technique suitable for the prediction of the
electroanalytical equilibrium signal of a potentiometric sensor
based on the evaluation of asymptotes of the response of the cell
and the confidence interval from the signals measured in the so-
called information dominant section of the response was proposed
(D31).
Three new principles for discrimination of organic guests by
the membrane potential change, which are based on the host-
guest recognition of charged groups, hydrogen-bonding groups,
or steric shapes of nonpolar moieties, are described (D32).
A cation permselectivity at the phase boundary of ionophore-
incorporated solvent polymeric membranes has been studied by
optical second harmonic generation (SHG) using the space charge
separation model (D33, D34).
Impedance spectroscopy of plasticized PVC membranes con-
taining neutral ion carriers carried out under steady-state currents
showed that changes in ionic concentration profiles of neutral
carriers and ionic species were associated with an increase in bulk
membrane resistance and Warburg impedance (D35). Measure-
ments of diffusion coefficients of the neutral ionophores in
plasticized PVC membranes using small-amplitude ac/dc tech-
niques were shown to be possible (D36). The ac impedance
characteristics of an ISE|insulator|semiconductor (MIS) structure
designed for chemical sensing applications were modeled quan-
titatively for a frequency range from approximately 5 Hz to 40
kHz. The bulk resistance of the membrane contributed signifi-
cantly to the equivalent capacitance at <1 kHz. Experiment and
theory show that sensors based on ac or impedance measure-
ments of changes in the Si space charge will be subject to
significant errors if the membrane resistance is also a function of
the solution conditions (D37).
Telemetric ISEs were developed for in vivo applications, and
the sensor response was found to be nearly Nernstian and
reproducible from sensor to sensor (D38).
ISE characterization carried out with a mathematical and
computational program demonstrated its use for (1) the determi-
nation of detection limit, selectivity constants, and extrapolation
of selectivity coefficients of various interferent ions from one buffer
medium to another (D39); for (2) the calculation of multiple
equilibria between different ligands and metal ions (D40); and
for (3) evaluation and graphical representation of the potentio-
metric selectivity coefficients of ISE (D41). The use of SPICE
(D42), and BIOSPICE (D43) programs for simulating perfor-
mance of chemically sensitive field effect transistors was demon-
strated. Nonlinear curve fitting using Microsoft Excel Solver was
evaluated for solving nonlinear equations used for modeling data
obtained in ISE response characteristics (D44). The membrane/
solution interface of liquid membrane ISEs with neutral carrier
was modeled and evaluated in view of Nernstian response, cation
and anion interference, detection limit, and effect of lipophilic salt
additives (D45). Calculation of the thermodynamic characteristics
of the interface of two immiscible electrolyte solutions carried out
by a statistical thermodynamic approach using the lattice model
was found suitable to describe, at least qualitatively, some of the
most important characteristics of liquid membrane ISEs (D46).
Water distribution in poly(vinyl chloride) based on ISE
membranes (D47) and the behavior of lipophilic derivatives of
benzo- and naphtho-12-crown-4 in the membrane of ISEs were
studied (D48). Carbon-13 spin-lattice relaxation studies of the
effect of water on ISE membranes were reported for plasticization
levels ranging from 25 to 100% plasticizer (D49). A dual-sorption
model for uptake of water in poly(vinyl chloride)-based ISE
membranes at equilibrium and during the initial stages of water
uptake (D50) as well as a spatial image distribution of water in
the membrane and the effect of additives was elaborated (D47).
Immobilization of a novel photoresponsive ionophoric calix[4]-
arene in plasticized poly(vinyl chloride) membranes provided new
switch-functionalized ion-selective electrodes (SISEs) which allow
detection of two metal ions with one electrode (D51).
The light-addressable potentiometric (LAP) sensor was intro-
duced for rapid, sensitive, and specific detection of whole cells
and spores (D52), for monitoring enzyme activity (D53, D54), as
a gas sensor (for detection of hydrogen and oxygen) (D55-D57),
to visualize the spatial distribution and temporal evolution of redox
potential in chemical reaction systems (D58), and to study the
relationship between extracellular acidification and cell viability
Analytical Chemistry, Vol. 70, No. 12, June 15, 1998 183R
of mammalian cells (D59). A differential measurement method
based on a time-sharing technique, which makes it possible to
achieve a very sensitive and highly stabilized response due to the
noise compensation effect for a LAPS, has been developed and
applied to fabricate an integrated taste sensor with artificial lipid
membranes as the ion-sensitive material (D60). Comparison
between a LAPS and a FET-based sensor for various applications,
such as enzymatic and immunological activity detection and cell-
metabolism detection, was carried out (D61).
ISE array analysis using variable step-size, generalized, simu-
lated, annealing (VSGSA) can be used to detect model parameters
of ions in mixed solutions without any a priori information about
the analytical system under study, overcoming the disadvantage
of simplex method (D62).
A computer-controlled instrument for the simultaneous deter-
mination of pH and redox potential called the potentiometric
alternating biosensor, which drives an array of light sources,
allowing 2-D signal acquisition and processing, was presented
(D63).
A new potentiometric instrument was described which could
measure picomole quantities of sodium without the need for
special processing and permit the measurements to be made in
real time (D64).
A monolithic sensor array of 400 individually addressable Pt
microelectrodes, which can be used in potentiometric mode as
well as in amperometric mode for redundant measurements with
signal averaging, multianalyte measurements, and imaging of
analyte distributions, was fabricated (D65).
The approach of using electrically conducting polymers in the
development of an artificial neural network polymer pH sensor
showed much better reproducibility in detecting pH of different
acidic and basic media over the conventional polymeric pH
detectors (D66).
A comparison of sample handling and analytical methods for
determination of acid-volatile sulfides in sediment was carried out
(D67).
A new design of gas sensors with extremely fast response times
to CO2, O2, and NO gases with a direct gas contact to the triple
points at the intersection of the ambient electrode, the porous
electrode, and the electrolyte was reported (D68). Dependence
of the analytical characteristics of biospecific and gas sensors on
the type of potentiometric transducer was reviewed (D69).
Reference Electrodes. An improvement in the liquid junction
between an electrochemical sensor containing no liquid electrolyte
and a classical reference electrode of the second kind was
discussed (D70). The use of an internal redox reference electrode
in connection with a fluoride-selective electrode was demonstrated
to minimize the electrode drift immediately after assembly (D71).
Evaluation of a new solid-state reference electrode junction
material based on solid poly(vinyl acetate) that contains a very
large loading of KCl (1:1 w/w KCl/PVA) (D72) was conducted.
A nonequilibrium approach to development of reference electrodes
and oxygen sensors for high-temperature aqueous systems based
on a Pd electrode polarized continuously by cathodic current
below the H exchange current was shown to behave as a quasi-
reversible H electrode (QRHE) (D73).
Biomedical Applications. The International Federation of
Clinical Chemistry (IFCC), through its committee on pH, blood
184R Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
gases, and electrolytes, has developed specific recommendations
to minimize the undesirable effects of preanalytical variables
(D74). The committee has included pertinent guidelines and
suggestions on important aspects of specimen collection proce-
dures including patient status and special precautions during
specimen collection (D75) and recommended on mean molar
activity coefficients and single-ion activity coefficients of solutions
for calibration of ISE (D76).
Planar microsensors for in vivo myocardial pH measurements
based on tri-n-dodecylamine (TDDA) or ETH 5294 proton neutral
carriers, in aminated PVC matrix, were evaluated (D77). Direct
measurement of nitric oxide release from vascular endothelial cells
applying a NO-selective electrode was demonstrated (D78).
The electrochemical sensor for heparin measurement based
on a conventional ISE membrane doped with tridodecylmethyl-
ammonium chloride (TDMAC) as the heparin complexing agent
was able to measure heparin in small discrete samples of undiluted
whole blood (D79, D80). A tetrachloroferrate(III)-selective liquid
membrane electrode based on crystal violet was reliably applied
to detect Fe in human blood, hematite, and mineralized vitamin
syrup (D81).
It was demonstrated that the analysis of both lactate and
ammonium ion in sweat is an effective, noninvasive, and conve-
nient method for estimation of physical condition (D82).
Voltammetric lithium ISEs based on ion transfer at the oil/
water interface facilitated by neutral ionophores, when tested using
artificial serum, showed that the interference from a large amount
(140 mM) of Na+ in blood can be easily avoided by detecting
the Na+ concentration simultaneously with the same electrode
(D83).
A simplified dual-lumen catheter design for simultaneous
potentiometric monitoring of carbon dioxide and pH with relatively
high stability in flowing blood yields continuously measured values
in good agreement with those obtained on discrete samples with
a commercial blood gas analyzer (D84).
(2) Symmetrical Devices. These are classical ion-selective
electrodes in which the membrane is placed between two
solutions. The theory of the transient potential response of ISE
electrodes based on a polarizable liquid | liquid interface predicts
the effect of the ion concentrations, the ion-transfer kinetics and
the differential capacity of the interface on the response time of
ISE (D85), and the effect of the concentration of a neutral carrier,
which depends on the reaction mechanism of the carrier-assisted
ion transfer across the interface (D86).
A general expression for interference effects exhibited by ion-
selective membrane was derived (D87). The selectivity coefficient
of ISE based on charged carriers was described as a function of
the ionic site concentration which can be achieved by the
incorporation of a defined amount of the appropriate sites into
the membrane phase (D88). Radiotracer experiments were used
to study the selectivity of ion-exchange processes of plasticized
poly(vinyl chloride) (PVC)-based ISE membranes doped with
neutral carrier as the active material (D89).
A self-consistent model describing the potentiometric response
in mixed-ion solutions of different charges based on ion extraction
equilibrium at the sample/membrane interface was discussed
(D90). The measurement of ion activity coefficients in aqueous
solutions of mixed electrolyte with a common ion can be
considered as a corollary of the ion/ion and ion/solvent interac-
tions (D91). Tuning of the electrochemical recognition of
substrates as a function of the proton concentration in solution
using pH-responsive redox-active receptor molecules was dem-
onstrated (D92).
Voltammetric investigation of the response mechanism of the
ISEs based on polymer modified with poly(oxyethylene) deriva-
tives in acetonitrile was discussed (D93).
Ion pairing and acid dissociation constants, as well as limiting
conductances, have been estimated in ISE membranes based on
a 33 wt % PVC/66 wt % dioctyl adipate matrix using the Fuoss
equation of conductance for weakly dissociable species (D94).
Potentiometric responses of polypyrrole films doped with
potassium hexacyanoferrate(II), LiCl, and sodium dodecyl sulfate
were grouped into three major classes: ionic (sensitivity to
changes of ion concentration), pH-metric (sensitivity to the
changes of pH of the solution), and redox (sensitivity to the redox
potential of the solution) (D95).
The construction and performance characteristics of an ion-
selective PVC matrix based on the ion-pair complexes for selective
determination of various drugs in aqueous solutions have been
described (D96-D99). The criteria for the selection of a suitable
plasticizer for calix[n]arene-based ISEs were discussed in great
detail (D100).
When novel ISEs based on acidic ionophores are being
developed, both cationic and anionic additives as well as plasticiz-
ers of high and low dielectric constant should be tested since
completely different selectivity behavior could be obtained due
to the charged and neutral forms of the carrier in the organic
phase (D101).
The behavior of codeine reineckate and codeine tetraphenylbo-
rate PVC membrane electrodes shows a Nernstian response for
9.3 10-5-1.3 10-3 mol/L codeine sulfate solutions with a
satisfactory selectivity toward sugars, amines, amino acids, cations,
and some pharmaceutical compounds (D102). The dynamic
characteristics of ISEs based on ion-exchange materials (quater-
nary ammonium salts) were measured upon stepwise changes in
concentration of the potential-determining ion (D103). The
response of ion-selective PVC membrane electrodes with calix-
arene ionophores toward primary amines and amino acid esters
was elaborated to be in agreement with the concept of H-bonding
in the host-guest complex (D104, D105). Molecular designs of
calix[4]arene-based sodium-selective electrodes with a short-(CH2-
CH2O)2CH2CH2-crown loop on the lower rim with remarkably high
105.0-105.3 sodium/potassium selectivity were developed (D106)
and electrochemically characterized (D107). A formaldehyde-
selective electrode based on the host-guest interaction between
p-tert-butylcalix[4]arene tetraester and lipophilic hydrazone gener-
ated in situ from formaldehyde and a modified Girards reagent
has a long working lifetime and can be used for the microdetection
of formaldehyde (D108).
Multicomponent analyses of heavy metal cations and inorganic
anions in liquids by a nonselective chalcogenide glass sensor array
were discussed (D109). Neutral carrier-type ion sensing mem-
branes based on sol-gel-derived glass, when incorporated in the
ion sensors, showed high sensitivity, high selectivities, and fast
potential response (D110).
The dependence of the electrical properties of glasses on their
composition and ion mobilities in the surface layers was discussed
(D111).
Cations. A new procedure for detection of the selectivity
coefficient of neutral carrier-based cation-selective electrodes was
established that avoids exposure to the preferred ion prior to the
measurement of discriminated ions (D112).
The ion selectivity of Teflon film, Si rubber film, Teflon powder,
and poly(vinyl fluoride) powder electrodes toward H ion, alkali
metal, alkali earth metal, transition metal, and group III metal ions
was studied (D113).
The performance of an ISE for potassium, employing valino-
mycin as carrier in a poly(vinyl chloride) membrane and a poly-
(vinylferrocene) solid contact between the membrane and the
metallic substrate, was compared to electrodes in the coated-wire
configuration and the conventional electrode with an aqueous
internal reference electrolyte (D114). All-solid-state potassium-
selective electrodes, which were constructed on a Pt disk electrode
using a double-layer film of electropolymerized polypyrrole/poly-
(4-styrenesulfonate) (PPy/PSS) composite covered with a plasti-
cized PVC membrane containing valinomycin, showed no over-
shoot and lower drift of the standard potential than both a single
PVC-coated electrode and a double-layer electrode using polypyr-
role doped with ClO4- (D115). Cubane diester crown ethers
tested as K+ neutral carriers in PVC membranes showed the
highest selectivity for potassium relative to sodium, lithium,
calcium, and magnesium ions using potassium tetrakis(p-chlo-
rophenyl)borate as a resistance modifier and nitrophenyloctyl
ether (NPOE) as a plasticizer (D116).
The study of the behavior of cation-selective solvent polymeric
membrane electrodes based on acidic ionophores by determining
the selectivity coefficients as a function of cationic or anionic
additive concentration was pointed out as a possibility for
discrimination between neutral and charged carrier-related mech-
anisms (D101).
The influence of structure and lipophilicity of dicyclohexyl-
amide ionophores for the lithium selectivity in membrane elec-
trodes was discussed in terms of the form the ligand adopted in
the complex conformation (D117). Excellent Li+-selective iono-
phores were obtained by introducing a bulky block subunit into
the ethano-bridge section of the base crown ring, which effectively
prevents the formation of a 2:1 or 3:1 sandwich-type complex
consisting of the crown ether and cations larger than Li+ (D118).
Lithium ISE based on THF-based 16-crown-4 derivatives were
evaluated (D119).
Uranyl ISEs based on crown ethers in PVC matrix membrane
have been prepared (D120, D121). The performance of a silver-
selective membrane electrode using acyclic dithia benzene deriva-
tives as neutral carriers has been compared with related macro-
cyclic compounds (D122).
It was found that rubidium ISEs based on indanopyrazolo[1,5-
a]pyrimidines acting as a novel class of neutral carriers exhibits
good selectivity toward rubidium with respect to alkali, alkali earth,
and some other metal ions (D123).
Macrocyclic oxamides used as ionophores in solvent polymeric
membrane electrodes for lead-selective membrane electrodes
showed a pronounced preference for lead detection over other
divalent and some monovalent cations (D124). Lead-selective
Analytical Chemistry, Vol. 70, No. 12, June 15, 1998 185R
PVC membranes based on cation-exchanger diphenylmethyl-N-
phenylhydroxamic acid (PMPHA) provided selectivity to lead ions
in the presence of Cu2+, Hg2+, and Ag+ (D125).
The performance of the symmetrical, unsymmetrical, and
bridged calix[4]arene derivatives as neutral carrier ionophores
in PVC membrane for sodium (D126) and lead was evaluated
(D127). A lead-selective membrane electrode based on diben-
zopyrydino-18-crown-6, which exhibits a Nernstian response for
Pb2+ ions over a wide concentration range and comparatively good
selectivities with respect to alkali, alkali earth, and some transition
and heavy metal ions, was developed (D128). A PbOH+-selective
membrane electrode based on crown ethers was discussed
(D129).
PVC-based membrane with incorporated chelating ion-ex-
change resin (1-hydroxy-2-naphthaldoxime-formaldehyde poly-
mer) containing nitrogen and oxygen donor atoms behaves as a
Ni2+-selective electrode with the Nernstian response over a wide
concentration range (D130).
An ionophore based on N-hydroxylamide derivatives was used
for a mercury-selective electrode (D131). Also, a polystyrene-
based heterogeneous solid membrane of cerium(IV) selenite has
been shown to be suitable for Hg(II) ion detection (D132). A
PVC membrane sensor for mercury(II) ions based on hexathia-
18-crown-6-tetraone as membrane carrier was prepared (D133).
The examination of the conformational influence of different
amide substituents on ionophore applied for the preparation of
the magnesium-selective electrode showed that the addition of
bulky substituents increased the ionophore selectivity of Mg
(D134).
A universal approach for the realization of tailor-made ion-
selective membranes by overcoming a problem of high membrane
resistance has been demonstrated for calcium, potassium, and
nitrate polysiloxane-sensitive ISFETs (D135) or by a proper choice
of lipophilic salts (D136).
Electrochemical and thermal behavior in connection with ac
impedance and FT-IR analysis of calcium-selective membranes
based on a polyimide polymeric matrix plasticized with diethylene
glycol dibenzoate and containing calcium synthetic ionophores
was studied (D137).
The ion-selectivity features of the novel Ca2+ and Mg2+
ionophores prepared from the double-armed diazacrown ethers,
which have a base diazacrown ether ring with two diamide-type
side chains, supply important structural information about the
design of host molecules for alkali earth metal cations (D138).
Macrocyclic polyether dioxatetralactams were evaluated as neutral
carriers for Ca2+- and Mg2+-selective electrodes in PVC mem-
branes (D139).
Evaluation of a macrotetrolide nonactin-based ammonium
ionophore for use in PVC membrane ion-selective electrodes, in
the presence of plasticizing solvent mediators, was carried out
(D140). A substitution of monomeric by polymeric plasticizers
lowers the tendency of migration of the membrane components,
leading to long life (D141).
Potassium ion-selective PVC membrane electrodes based on
bis(crown ether) show selectivity coefficients that are better than
those of an electrode based on natural valinomycin (D142).
Potassium ion-selective electrodes based on alkyl thiophosphate
derivatives as electroactive substances show no significant inter-
186R Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
ference obtained for alkali, alkali earth, and other cations (D143).
Ion-selective polymeric membranes sensitive to cationic sur-
factants were fabricated using benzyldimethylhexadecylammo-
nium reineckate, dodecyltrimethylammonium reineckate, or hexa-
decylpyridinium phosphotungstate as exchangers, dispersed in
the PVC matrix (D144). An ISE membrane (plasticized PVC-
based) based on phosphoryl-containing pendands of the alkylpy-
ridinium series for the direct potentiometric detection of cationic
surfactants in water was developed and tested (D145).
The electrochemically polymerized o-methoxyaniline and o-
methylaniline on platinum electrodes showed an apparent Nerns-
tian response in the 1-12 pH range with a slope of 63.8 mV/
decade, while the linear range of the electrode prepared with
poly(o-methoxyaniline) exhibited a linear relation in the 2-11 pH
range with a slope of 62.0 mV/decade (D146). Polypyrrole and
poly(N-methylpyrrole) films on platinum or pyrolytic graphite
electrodes prepared by anodic polymerization from acetonitrile-
water mixtures containing naphthalenesulfonates and methylben-
zenesulfonate electrolyte salts show H+, alkali, and alkali earth
metal ion sensitivities which are a function of solvent composition
and dopant molecular structure (D147, D148).
Electroanalytical and biocompatibility studies on microfabri-
cated array sensors based on pH, potassium and calcium ion-
selective membranes immobilized in high molecular weight
carboxylated PVC (D149) or in aliphatic polyurethane (Tecoflex)
matrixes with normal and reduced amounts of plasticizers, were
carried out (D150).
Anions. A robust and sensitive chloride ISE with suppressed
sensitivity toward surfactants can be prepared by modifying the
surface of an iodide-selective electrode using a chemical reaction
with mercuric chloride in an oxidizing medium (D151).
The high selectivity of the cyclic polyamine, 3-decyl-1,5,8-
triazacyclodecane-2,4-dione (N3-cyclic amine), used as the iono-
phore for a dibasic phosphate-selective electrode was postulated
to be a function of the size and charge of the N3-cyclic amine
relative to the size and charge of HPO42- ions (D152).
Anion selectivities of membranes based on uranyl salophen
derivatives with substituents at the 4-position were applied to
design a nitrite-selective ISE which shows linear response in the
range 1-3 of pNO2- with a slope of 56.2 mV/decade (D153). The
nitrite anion electrodes based on polymer membrane formulated
with a palladium organophosphine complex (benzylbis(triphen-
ylphosphine)palladium(II) chloride) do not exhibit proton/
hydroxide response in the range of pH 3.5-12 and do exhibit a
non-Hofmeister selectivity pattern which represents a potential
advantage over previously reported nitrite electrodes prepared
with Co(III) corrins and porphyrin complexes (D154). A PVC
membrane electrode, using bis(tribenzyltin) oxide as the carrier,
displayed selective response to phosphate with anti-Hofmeister
behavior (D155).
Novel neutral anion ionophores based on fluorinated (poly)-
ether compounds have been synthesized and applied for an anion-
selective electrode (D156). Statistical and nonstatistical detection
limits of a fluoride-selective electrode were discussed (D157). A
novel potentiometric selective detection method for H2S (HS-)
by an electropolymerized membrane electrode based on a neutral
anion carrier, binaphthyl-20-crown-6, was developed (D158).
 A polymeric membrane based on lipophilic metalloporphyrin
derivatives containing electron-donating or -withdrawing groups
(D159, D160), or metallocenes or palladium organophosphine
complex (benzylbis(triphenylphosphinepalladium(II) chloride)
(D161) used as anion carriers, showed improved selectivity
characteristics.
Construction and evaluation of tetraphenylborate anion-selec-
tive electrodes and their application in determination of alkaloids
in pharmaceutical products were discussed (D162).
The dynamic properties of ISEs based on phosphoryl-contain-
ing podands were examined as a function of the structure and
concentration of the podands and the concentration and nature
of the potential-determining metal cation and its counterion
(D163).
The redox interferences of poly(pyrrole)-based perchlorate-
selective electrodes were studied in both perchlorate and redox
buffer media (D164).
The effect of film thickness, various pre- and postconditioning,
and lifetime were examined for the iodide ion sensor polymer
electrode based on the entrapment of iodide/I/triiodide into a
poly(3-methylthiophene) conducting polymer (D165). PVC mem-
brane iodide-selective electrodes based on the Ag complex of a
novel thiocarbamoylimine dithioether as an anion carrier were
developed (D166).
The characteristics of electrodes with pseudoliquid membranes
selective for phthalic acid isomers were presented (D167). An
anion sensor, in which a dinuclear macrocyclic metal complex,
which is shape-selective, was constructed as a cyanide-selective
electrode (D168).
(3) Asymmetrical Devices. In asymmetrical devices, one
side of the membrane is in contact with a solid phase while the
other is exposed to the measured solution. Screen printing can
be used to divide the fabrication into two distinct sequences:
semiconductor processing and sensor-specific steps, which makes
the batch fabrication of integrated chemical sensor arrays com-
parable to that of conventional liquid junction ion-selective
electrodes (D169). Microfabrication methods of silicon chips
make it possible to produce biosensor arrays coated with specific
ionophores or enzymes, in large volumes, with a high degree of
reliability, and at a low cost (D170, D171).
A new type of hybrid chemical sensor has been produced by
matching the technology of ISFET production with ISE using a
graphite-loaded Araldite layer to cover the gate opening of
encapsulated ISFETs (D172). A new class of modified sol-gel
C composite electrodes, based on the encapsulation of complexing
ligands, was described (D173).
Photocurable polymer matrixes for potassium-sensitive ISE
membranes based on urethane and bisphenol A (epoxy) diacry-
lates have been made (D174). Characterization of photopoly-
merized decyl methacrylate as a membrane matrix for ISEs that
has been cross-linked with hexanediol dimethacrylate was de-
scribed (D175).
Methods of the integration of ion-sensitive membrane based
on different disposition of the membrane (D176) or based on
acrylates deposited into pyramidal containments produced on
silicon by an anisotropic etching technique have been developed
and applied for nitrate- and ammonium-sensitive sensors (D177).
The effect of membrane structure, composed of a hydrophobic
inner layer and a hydrophilic outer layer, fabricated by a
photolithographic process on the performance of field effect
transistor potassium-sensitive sensor has been tested (D178). A
simple and fully IC-compatible microelectronic technology was
developed for the fabrication of backside-contacted (BSC) ISFETs
based on commercially available bond and etch-back Si on
insulator (BESOI) wafers (D179). Application of nickel electroless
plating to the fabrication of low-cost backside contact ISFETs was
presented (D180).
A highly automatic ISFET packaging at the wafer level is
possible by applying a lift-off method of common thermocurable
encapsulants as well as direct photopolymerization of UV-curable
encapsulant compounds containing either epoxy acrylate or
polyurethane acrylate oligomers together with monomers and
photoinitiators (D181). Characterization and testing of polymer-
oxide adhesion to improve the packaging reliability of ISFETs was
carried out by long-term C-V measurements and CO2 and NH3
response measurements (D182). Selective polymeric membranes
sensitive to inorganic analytes of biomedical interest (e.g., H+,
K+) were fabricated on a flexible polyimide (Kapton DuPont)
substrate, using a combination of thin-film, thick-film, and packag-
ing technologies, and encapsulated with a biocompatible polymeric
material such as poly(2-hydroxyethyl methacrylate) (poly-HEMA)
(D183).
Coated Wire and Hybrid Electrodes. A solid membrane
sensor which incorporates stannic oxide as an electroactive phase
and polystyrene as binder electrode possesses a high level of
selectivity for vanadate over many other ions in the pH range 4-10
(D184). Using the Ag/AgCl solid-state electrode as the substrate
and the chlorpheniramine tetraphenylborate ion-pair complex as
the active component, a new type of solid-state chlorpheniramine
ISE was constructed (D185).
An all-solid-state membrane electrode based on a conventional
mobile carrier sensitive to H ion and with no internal liquid contact
shows a sensitivity of 54-55 mV/decade within a linear range of
pH 3.5-10.5 (D186). The construction was described of ISEs,
with a mobile carrier sensor, for anionic species of saturated
monocarboxylates such as propionate, acetate, formate, monochlo-
roacetate, dichloroacetate, and trichloroacetate, in which the
sensor consists of a 2-nitrophenyl octyl ether solution of the
responsive tetradodecylammonium salts (D187).
Two new types of metal oxide pH sensors (samarium-
substituted ceria ceramic membrane and single crystals of several
molybdenum oxide bronzes) with a direct solid-state contact were
developed and tested (D188). Solid-state electrodes, containing
phase of vanadium oxide bronze Na2V12O30 as an ionophore,
exhibited selectivity for aluminum in sulfuric acid solutions
(D189).
A rubidium-selective electrode developed by coating a graphite
rod with a PVC membrane containing decylidene bis(4-benzo-
15-crown-5) ether, which was used as a neutral carrier, exhibited
a near-Nernstian response to rubidium in the broad concentration
range (D190).
The tungsten/tungsten oxide electrode was investigated as a
pH sensor over a wide range of pH at 200-300 C and was
compared with the yttria-stabilized zirconia membrane electrode
(D191).
Analytical Chemistry, Vol. 70, No. 12, June 15, 1998 187R
 Ion-Sensitive Field Effect Transistors (ISFET). Oxynitride
ISFET using a new encapsulation technique and a new geometry
was developed and its operation for pH detection in a differential
mode was demonstrated (D192). Two types of surface sites
(namely, silanol sites and amine sites) and their ratio on the
characteristics of an Si3N4 gate pH-ISFET were discussed (D193).
The behavior of solid-state ion sensors, in which the interface
between the ion-selective liquid membrane and the silver/silver
chloride electrode is modified with a hydrophilic intermediate
layer containing various concentrations and various kinds of
electrolyte salts, was described (D194).
Operation of a probe-type n-channel depletion-mode Si3N4
ISFET with the substrate in direct contact with solution was
discussed (D195). A Si3N4 ISFET with integrated signal-
conditioning electronics, expressly designed for on-line detection
of microorganisms in waters, is employed as an H+ sensor (D196).
On-line determination of the degradation of ISFET can be assessed
if structures sensitive to the variations of dielectrical and packaging
quality are fabricated together with the ISFET (D197).
Ca, Mg, and K ion-selective membranes were prepared by
immobilization of octadecyl monophosphonate, octadecyl diphos-
phonate, or dibenzo-18-crown-6 ionophores into cationic polymer
gels on ISFETs working in a differential mode (D198). An NH4+
ISFET sensor based on PVC membrane with improved long-term
stability was accomplished using a lipophilic type of plasticizer
and a graphite-epoxy layer as an internal reference between the
gate area and the PVC membrane (D199).
The development of polysiloxane-based chemically modified
field effect transistors (CHEMFETs) for heavy metal ions was
discussed (D200). Low-drift and high-sensitivity pH-ISFET with
Ta2O5 as a sensing membrane was obtained after heat treatment
carried out at various temperatures (D201). A ISFET combination
pH/pF for the fast determination of very low fluoride concentra-
tions in acid solutions was presented (D202). Correlation between
the electrical charge of polymeric membranes and the character-
istics of ion field effect transistors or penicillinase-based enzymatic
field effect transistors was studied (D203).
Biosensors. A biosensor based on direct detection of
membrane potential induced by immobilized hydrolytic enzymes
which do not require the specific introduction of an internal
reference system has been made (D204).
The use of enzyme chronopotentiometry as a new approach
to overcome inherent problems of steady-state potentiometric
processes was presented for the example of a glucose oxidase
(GOx) electrode (D205).
The performance of two simple biosensor designs, based on
potentiometric and conductometric transduction modes, has been
compared for the detection of organophosphorus pesticides
(D206).
FET-based sensors with robust photosensitive polymer mem-
branes for detection of ammonium ions and urea were fabricated
and tested (D207). Protein sensors based on the potentiometric
photoresponse of polymer membranes doped with photochromic
spiropyran were discussed in terms of response time, selectivity,
and reusability (D208). Enzyme biosensors for urea determina-
tion based on an ionophore-free pH membrane electrode show
high sensitivity, long lifetime (over 1 month), and short response
time (2-5 min for steady state) (D209). Urea-sensitive electrodes
188R Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
based on various styles of immobilizing enzyme in membranes
used in association with a nonactin-based PVC matrix membrane
on NH4+-cation-selective electrode were investigated (D210).
Carboxylated PVC membrane matrix with tridodecylamine as a
hydrogen ionophore allowed covalent enzyme binding to its
surface for urea detection within an extended lifetime (2 month)
(D211).
Modeling of the transduction mechanisms from biological
membranes to silicon sensors by computer simulations for steady
and transient conditions was considered (D212).
A potentiometric sensor for ATP anions with the selectivity
order ATP > UTP, GTP > was constructed based on a planar
bilayer lipid membrane (BLM) embedded with Na+,K+-ATPase
(Na+ pump) (D213, D214). A method to construct enzyme-based
biosensors, where the enzyme is entrapped in a lipid matrix, was
presented (D215).
Potentiometric responses of solvent polymeric membrane
electrodes for nucleotides based on neutral derivatives of cytosine
and thymine represent the first cases of ISEs with reported
Nernstian slopes in which potentiometric selectivities are due to
the formation of hydrogen bonds between a neutral ionophore
and a neutral moiety of the analyte. No explanation of the
mechanism is given (D216).
Bienzymic potentiometric electrodes for creatine and L-arginine
determination using an ammonium-selective electrodes as internal
sensor have been described (D217). PVC membrane containing
lipophilic alkylated cyclodextrins as hosts was used for detection
of subpicomolar levels of acetylcholine (D218) and for detection
of onium ions in clinical, pharmaceutical, and forensic analysis
(D219).
Functionalized, lipophilic (R-, -, and -cyclodextrins were
synthesized and their suitability as onium ion-selective, potentio-
metric sensors studied (D220, D221).
(4) Potentiometric Gas Sensors. Theoretical analysis of the
electromotive force of a high-temperature solid-state galvanic cell
incorporating a composition gradient solid electrolyte was carried
out (D222).
The potential-type sensor using the battery systems M1/MnOx/
M2 as the sensing elements, where M1/M2 are two electrodes of
different metals, and MnOx samples act as the solid electrolyte
was demonstrated for a systems consisting MnO2 electrolytes with
Pt/Cu electrodes, which is most favorable for obtaining high
electrical potentials in a high ambient humidity (D223). Direct
energy conversion by nonsymmetrical electrodes on an oxide
electrolyte electrochemical cell and its applications in multi-gas
sensing were demonstrated with several gas mixtures (D224).
The theoretical behavior of concentration cells based on ABO3
perovskite materials with protonic and oxygen ion conduction was
described (D225).
A ZrO2 solid-electrolyte sensor for the detection of oxidizable
gases which uses the generation of a non-Nernstian electrode
potential was developed (D226). A low-temperature zirconia
oxygen gauge, based on new Bi3Ru3O11-ZrO2 as electrode
material instead of other ruthenium oxides, hardly deteriorates
during the test period of 90 days (D227).
A highly sensitive (10 ppb-1 ppm) O3 sensor using In2O3 as
sensing film was developed (D228). O2 sensors based on Y2O3-
stabilized ZrO2 (YSZ) can be protected by dense filters with high
electrochemical permeability to ensure longer lifetime (D229).
The response of the solid-state potentiometric CO2 sensors with
anion conductor (LaF3) and metal carbonate (Li2CO3) follows the
Nernst equation for the two-electron reduction of CO2 in the
concentration range 40-2000 ppm at 400 and 450 C (D230).
Development and testing of a miniature carbon dioxide solid-state
electrochemical gas sensor was described (D231). Nasicon
prepared by the sol-gel method has been used as a solid
electrolyte for carbon dioxide detection (D232).
A solid-state sensor based on two platinum electrodes that
differ in their true-to-geometrical surface area ratios and that are
in contact with Nafion 117 was tested as a hydrogen sensor
(D233). Operating characteristics and modeling of a solid-state
hydrogen sensor fabricated by covering one of the planar Pt
electrodes with an oxide catalyst mixture containing CuO/ZnO/
Al2O3 were described (D234). A high-temperature hydrogen
sensor based on stabilized zirconia and a metal oxide electrode
showed fairly good sensing characteristics and excellent selectivity
to H2 in the presence of NO, NO2, CH4, CO2, and H2O, as well as
good long-term stability (D235).
The possibility for a potentiometric humidity sensor of com-
posite membranes prepared from anion-exchange membranes and
polypyrrole was presented (D236).
NOx determination with galvanic zirconia solid electrolyte cells
used for O2 detection was discussed (D237).
A potentiometric gas sensor capable of monitoring gaseous
sulfur and/or hydrogen sulfide based on silver -alumina solid
electrolyte (Ag|Ag -alumina|Ag2S, MoSx, S2, N2, Au) was designed
and tested in oxygen-free atmospheres at temperatures between
908 and 1043 K (D238).
The carbon dioxide sensing characteristics of solid-state
electrochemical sensors based on sodium ionic conductors, Na3-
Zr2Si2PO12, operated from 370 to 520 C were presented (D239).
The effect of yttria addition to Na2CO3/BaCO3 composites for
potentiometric CO2 sensors was studied in respect to ionic
conductor, microstructure, and sensing properties (D240). The
EMF and the sensitivity of ceramic CO2 sensors with thin- and
thick-film electrodes with Na-R-Al2O3 and Nasicon were evaluated
(D241).
The analysis of the response of a zirconia sensor to multicom-
ponent gas mixtures providing insight and design guidance in
optimizing sensor operation for specific applications was per-
formed (D242).
Detection of hydrocarbons in air and purification of exhaust
gas under lean-burn conditions using solid electrolytes has been
demonstrated (D243). A high-temperature (973 K) ceramic
sensor for detection of gaseous hydrocarbons was constructed
using CaZr0.9In0.1O3 and yttria-stabilized zirconia as the proton and
O2 conductors, respectively, with a Pt/La0.6Ba0.4CoO3 and an Au
electrode (D244).
Improvement of the thermal shock resistance of R-Al2O3
ceramics for sensor applications has been achieved by incorpora-
tion fibers of Al2O3 and ZrO2 into R-Al2O3 (D245).
A perovskite-type oxide of LaGaO3 doped with Sr and Mg
exhibits a high oxide ion conduction over a wide range of oxygen
partial pressures (D246).
A hydrogen sensor based on ammonium tantalum tungsten
oxide as a proton-conductive solid electrolyte for a hydrogen
sensor based on EMF measurement exhibited the highest level
of conductivity and sensitivity to H2 at temperatures from 400 to
723 K and a response within 30-100 s (D247).
A hybrid metal-free phthalocyanine/silicon FET sensor for
reversible detection of NO2 has been demonstrated (D248).
Application of iodine-doped poly(cyclophosphazene) film for
potentiometric detection of tributyl phosphate vapor using a Kelvin
probe was described (D249).
Catalytic metal gate-SiO2-SiC (MOSiC) capacitors operating
at 800 C were used as high-temperature H or H-containing gas
sensor devices (D250).
A novel hybrid technique for manufacturing gas sensing field
effect structures (GasFETs) with an air gap is reported (D251).
Gas sensing results of charge flow transistors incorporating
polyaniline films to very low concentration of NOx and SO2 have
been obtained via an operation mode similar to that used for the
conventional MOSFET (D252). Fabrication advantages of a new
chemical sensor based on a MOS transistor with rear contacts
and two flat surfaces based on some initial results from the
development of this technology have been reported (D253). In
situ modification of the NOx sensitivity of thin discontinuous
platinum films as gates of chemical sensors was discussed (D254).
H2 gas sensing devices based on a porous platinum metal oxide-
semiconductor field effect transistor (MOSFET) were fabricated
(D255). The mechanism of hydrogen adsorption effects on
diamond-based MIS hydrogen sensors has been analyzed (D256).
The catalytic effect of the Pd metal gate structure of the MOS
can be modulated by applying a cyclic treatment (HCT) which
modifies the structure of the palladium film evaporated on the
silicon dioxide (D257). Langmuir analysis on hydrogen gas
response from 1 to 10 000 ppm of palladium gate FET was carried
out (D258). The optimization, characterization, and analytical
performance of a suspended gate field effect transistor (SGFET),
with a selective polyaniline/Hg layer, for monitoring low levels
of HCN in air were described (D259).
The use of semiconductor sensors for detection of H2 in nuclear
reactor installations was discussed (D260).
Two-dimensional numerical simulation for gas chemisorption
on metal oxide layers and their implementation in the work
function change on the sensitive layer of a suspended-gate field-
effect transistor and the current modulation in a ZnO layer were
described (D261).
A probe consisting of a water-cooled metal support, an Y2O3-
stabilized ZrO2 reference electrode, and an Al2O3 indicator
electrode was developed for measuring O activity in molten glass
(D262). Development of a long-term oxygen sensor in molten
copper using a MgO-PSZ electrolyte tube was discussed (D263).
Several types of solid reference electrodes for potentiometric gas
sensors based on solid sodium ion conductors (e.g., Na+/(-
alumina or Nasicon) were described and the observed experi-
mental results are discussed in view of theoretical predictions
(D264).
With Bi2Ru2O7 and Bi3Ru3O11 as electrode materials, the
zirconia sensor can be used at a temperature as low as 450 K
(D265).
The role of formation of charge-transfer complexes in work
function gas sensors has been discussed (D266).
Analytical Chemistry, Vol. 70, No. 12, June 15, 1998 189R
AMPEROMETRIC SENSORS
(1) General Introduction. Molecular recognition at mem-
brane surfaces was investigated by exploiting three different
principles of signal transduction, i.e., (1) active transport, (2) ion
channel function, and (3) membrane potential change (D267).
Ultrathin porous carbon films employed as transducers for
amperometric detection couple the advantages of high enzyme
loadings and large microscopic area with a small geometric area
which greatly enhances sensitivity (D268). The application of
dispersed palladium microparticle films in conducting polymer to
biosensors has been investigated (D269).
The influence that various experimental parameters have on
the electrochemical response of zeolite-modified electrodes was
studied using ion-exchange voltammetry (D270). Four potential
step in a single-pulse sequence mode, which tends to eliminate
the charging current, is recommended for amperometric sensors
(D271). The concept of combination of an Ag6I4WO4 pellet with
a UV decomposition unit as an amperometric sensor for detecting
hydrocarbons in the ppm range was presented (D272).
Fabrication. Nanometer-sized glass-sealed metal ultramicro-
electrodes (Umps) with effective electrode radii of 2-500 nm were
made (D273). Binder paste as a new composite material for
biosensors and electrochemical bioreactors was reported (D274).
It was found that electrochemically generated cresole film
mixtures protect glassy carbon surfaces from poisoning when used
for detection of different phenolic materials (D275). A new class
of composite electrodes made of sol-gel-derived C-SiO2 materials
can serve as an indicator electrode in amperometric sensing and
biosensing applications that offer higher stability than carbon paste
electrodes and are more amenable to chemical modification than
monolithic and composite carbon electrodes (D276).
A printed microelectrode array of some 1000-3000 electrodes
and an amperometric sensor, which consists of an amperometric
transducer in combination with an adjacent Ag ink reference
electrode, was fabricated for the detection of heavy metal traces
for environmental field analysis (D277). The performance of
microsensor arrays with 1024 individually addressable ampero-
metric cells which were realized in silicon planar technology (10
mm 10 mm and 30 mm 30 mm substrates) with separated
hydrogel membranes was presented for two-dimensional oxygen
concentration mapping (D278). Polyhydroxy cellulose enzyme
electrodes for the water-free organic phase have been fabricated
and tested (D279, D280).
To decrease the mass-transfer resistance of oxygen permeation
and to improve the response of the enzyme electrode, a series of
amphiphilic poly(vinyl cinnamate) membranes were prepared by
using photosensitive PVC (D281).
Enzyme-entrapping membranes for biosensors were obtained
by radiation-induced polymerization (D282), deposition of en-
zymes using electrochemical aided adsorption in the presence of
glutaraldehyde (D283, D284), electrochemical deposition of
enzyme in a conducting polymer (D285, D286), or using screen
printing of the enzyme from the carbon ink (D287). Spatially
controlled on-wafer and on-chip enzyme immobilization using
photochemical and electrochemical techniques (D288) as well as
polyacrylamide polysiloxane membrane depositions (A146) was
reported. Specific examples of microencapsulation of enzyme
layer in ex vivo biosensors have been presented (D289).
190R Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
Interdigitated array, thin-film noble metal microelectrodes
deposited with different geometries were fabricated by photoli-
thography and electron beam lithography on silicon substrates
(D290).
A radio frequency plasma-polymerized perfluoroallylphospho-
nic acid film was prepared for use in amperometric biomedical
sensors (D291). Application of excimer laser micromachining for
the fabrication of disk microelectrodes in a composite membrane
or thin laminate arrangement has been demonstrated (D292).
(2) Modified Electrodes. A nonlinear reaction/diffusion
equation with Michaelis-Menten kinetics in electroactive polymer
films was formulated, and approximate analytical solutions for the
substrate concentration profiles and corresponding current re-
sponses were developed (D293). A theoretical analysis describing
the transient current response of a conducting polymer-based
amperometric chemical sensor to a concentration step was found
to be in a good agreement with that obtained experimentally for
the detection of ascorbate at polypyrrole electrodes (D294). A
polyaniline-dispersed mercury electrode for the detection of
monochloramine and dichloramine was made (D295).
A novel photoelectrochemical sensor, the microoptical ring
electrode (MORE), based on a thin-ring microelectrode and a
fiber-optic light guide as the insulating material acting as an
interior to the ring, is capable of delivering light directly to the
region of electrochemical measurement. It can be used to conduct
microelectrochemical studies of systems with complex photo-
chemistry and to conduct detection of photogenerated species
(D296).
Chemically modified carbon paste electrodes containing Fe-
(III)Y zeolite (D297) or zeolite molecular sieves (D298) were
applied for detection of ascorbic acid or copper trace in aqueous
solution, respectively. Polycrystalline platinum electrodes modi-
fied with Nafion and cellulose acetate were investigated for the
detection of nitric oxide based on its oxidation (D299). A
ruthenium(II) complex/Nafion-modified electrode combined with
a carbon dioxide sensor was used for selective determination of
oxalate (D300).
A preliminary examination of a simple and rapid screening
method for quantifying the range of toxic organohalides directly
in aqueous solution with a metalloporphyrin catalyst was described
(D301).
A sensor with a poly(tetrafluoroethylene) (PTFE) membrane
(10% voids) and a porous carbon felt electrode was fabricated for
the detection of residual ozone in water (D302).
A gold electrode modified with a self-assembled monolayer of
thiols was examined as an electrochemical detector for ionic
surfactants (D303). Gold ultramicroelectrodes (UMEs) modified
with a thioctic acid monolayer show selectivity for electroinactive
electrolyte anions, which participate indirectly in the electrode
reaction (D304).
A mixed-valent ruthenium oxide-ruthenium cyanide film on
glassy carbon electrode exhibits excellent electrocatalytic activity
toward oxidation of simple aliphatic alcohols and polyhydric
compounds in acidic media (D305).
(3) Gas Sensors. The detection of volatile compounds with
chemical gas sensors is of increasing interest in the nondestructive
detection of food quality (D306). The development of a new
microelectrode gas sensor for the simultaneous measurement of
O2 and CO2 was described (D307, D308). Low detection limits
for AsH3, SiH4, and organic vapors were reported with a thin gold
film electrode ion-plated on a gas-permeable membrane (D309).
A study of the rapid detection of CO in air employing protonic
conductor/Pt interfaces shows that electrochemical oxidation of
CO is controlled by the formation of the precursor OHad radicals
which react rapidly with CO (D310). A planar type of limiting
current oxygen sensor with Pt electrodes on only one side of the
zirconia disk was fabricated and parameters affecting the sensor
characteristics were investigated (D311). Hydrogen sensing with
a solid-state H sensor fabricated with a 9% YSZ disk sandwiched
between two Pt films covered by a catalyst was examined under
limiting current conditions (D312). The possibility for CO2
detection in N2/CO2 gas mixtures by a zirconia (solid-electrolyte)
electrolysis cell operating in a limiting-current mode was demon-
strated (D313, D314). A novel amperometric ZrO2 gas sensor
for measurement of air/fuel ratio on either side of the air/fuel
stoichiometry was described (D315). A new technique was
proposed to study the kinetics and the surface reactions of high-
temperature zirconia electrode reactions (D316).
The measurement of D2O concentration in a mixture of H2O
and D2O was studied using CaZr0.9In0.1O3- as a high-temperature
protonic conductor (D317). An amperometric solid-state sensor
for NO and NO2, based on protonic conduction of (zirconium
phosphate with titanium hydride as reference and Au as counter
electrode, was able to operate at room temperature (D318).
Factors that influence the open-circuit potential of a Pt/solid
polymer electrolyte (SPE) electrode in air containing low concen-
trations of H2 were studied (D319). The electrochemical response
to H2, O2, CO2, and NH3 of a solid-state cell based on a cation- or
anion-exchange membrane serving as a solid polymer electrolyte,
with response time in the order of 1 min, was determined (D320).
The response behavior of electrodes for solid electrolyte Nernstian
CO2 gas sensors was characterized using the pressure modulation
technique (D321). A hydrogen sensor with a ppm-range sensitiv-
ity was accomplished by using poly(vinyl alcohol)-phosphoric
acid as the solid electrolyte sandwiched between two palladium
films (D322).
Monitoring of hydrogen at high-temperature, high-pressure
aqueous solutions has been demonstrated (D323). A hydrogen
probe equipped with strontium cerium oxide, SrCeO3-based proton
conductor, and calcium/calcium hydride reference electrode
generated a stable cell potential within 5 min after immersion in
molten Al or Mo (D324).
A galvanic sensor without applied external voltage was de-
scribed for the trace detection of hydrogen sulfide in aqueous
media (D325). A semiconductor gas sensor based on In2O3 was
exploited for detecting ethyl acetate (D326). A method for
correcting short-term fatigue in an electrochemical fuel cell sensor
provides a reliable means of detecting the concentration of the
range of gases in a variety of gas mixtures (D327). Ambient
temperature oxygen sensors based on insulating material-
dispersed PbSnF4 layers in a cell, Ag|Ag6I4WO4|PbSnF4|, were
discussed (D328). The electrochemical properties of metallopor-
phyrin-clay complex-modified electrode systems were investi-
gated as oxygen sensors (D329). A high-temperature oxygen
sensor (YSZ) with a porous Pt layer on the cathode operates on
the principle of an electrochemical pump (D330). Fuel cell-type
ceramic-carbon oxygen sensors composed of a hydrophobically
modified silicate network and a dispersion of carbon powder and
inert or cobalt porphyrin catalyst modifier provide a fast dynamic
response (D331). Results have been presented for the simulta-
neous measurement of the concentrations of the inhalation
anesthetic halothane and oxygen in gas streams with compounds
in a clinically important range (D332).
(4) Biosensors. The effects of both electrode material and
polymer configuration on the performance of the electrochemical
sensor based on immobilized enzyme electrode have been studied
on surfaces of glassy carbon, platinum, and gold rotating-disk
electrodes (D333). A study of electrical double-layer effects in
the pretreatment of two-electrode cells for enzyme electrodes was
described for a two-electrode cell (D334). Studies of the elec-
trochemical characteristics of H2O2 microarray electrodes, and as
the building elements for biosensors, were conducted (D335).
Bilayer electrodes, where the H2O2-producing enzyme and the
redox-epoxy-horseradish peroxidase (HRP) network are not
electrically connected, extend the range of amperometric biosen-
sors based on directly redox-epoxy-wired enzymes to enzymes
that are difficult to connect electrically to redox polymer networks
and whose preferred or only cosubstrate is oxygen (D336). Local
detection of photoelectrochemically produced H2O2 with a wired
HRP microsensor was demonstrated (D337). A novel chronopo-
tentiometric detection method based on the correlation of the
potential change in the selected section of the relaxation curve
with the concentration of the species to be measured was
developed with NADH as a model compound (D338).
Permeation of solutes through an electropolymerized ultrathin
poly(o-phenylenediamine) film used as an enzyme-entrapping
membrane was studied by cyclic and rotating-disk electrode
voltammetry (D339). It was shown that the sensitivity of multi-
layer enzyme electrodes can be controlled by the number of
enzyme layers assembled onto the electrode (D340).
Artificial electron donors for nitrate and nitrite reductases
usable as mediators have been selected and characterized by
electrochemical methods (D341). The detection of cyanide,
chlorophenols, atrazine, dithiocarbamate, and carbamate pesti-
cides was described, utilizing an amperometric biosensor con-
structed by the electropolymerization of a pyrrole amphiphilic
monomer-tyrosinase coating (D342). Characterization results
of mediated and nonmediated oxidase enzyme-based glassy
carbon electrodes compared favorably with the classical platinum-
enzyme probe (D343).
Chemically modified electrodes incorporating biological com-
ponents, such as enzymes, in a polymer-modified matrix that
couples a bioreaction with electrochemical detection were exten-
sively discussed (D344). The suitability of catalytic materials
(catalytic carbon powders, platinized materials), membranes, and
fabrication technologies for the construction of amperometric
biosensors was elaborated (D345).
Signal stability of amperometric biosensors for long-term
measurements such as consumption of substrate in the bulk
solution and for the release of electrochemically active products
from the enzyme layer was studied (D346).
Immobilization of enzymes into Nafion membranes by sus-
pending the enzyme in a water-ethanol mixture with a high
(>90%) ethanol content, followed by mixing with the dissolved
Analytical Chemistry, Vol. 70, No. 12, June 15, 1998 191R
polyelectrolyte, was proposed (D347). Highly selective electro-
chemical detection of dopamine using interdigitated array elec-
trodes modified with Nafion/polyester ionomer layered film was
reported (D348).
Preliminary investigation of a bioelectrochemical sensor for
the detection of phenol vapors that is based on ionically conducting
films incorporating a biological redox catalyst was reported
(D349).
Amperometric glutathione electrodes based on hydrogen
peroxide or Clark-type oxygen electrodes, coupled with a novel
enzyme glutathione oxidase, have been assembled and analytically
evaluated (D350).
Bienzymic electrodes for maltose were evaluated (D351).
Needle-type biosensors for rapid measurement and detection of
sugars in fruits with low detection limits were fabricated and
combined with a conventional three-electrode system (D352).
An enzyme microsensor with osmium complex and porous
carbon was developed for measuring uric acid (D353).
The use of recombinantory DNA technology in the design of
a highly specific heroin sensor has been described (D354).The
use of bacterial luciferase enables specific detection of heroin,
which opens a possibility for the development of a biosensor for
illicit drugs (D355). A fully active monolayer enzyme electrode
derivatized by antigen-antibody attachment was described and
tested (D356). The concept and first results for a multivalent
amperometric immunosensor system that is based on silicon
technology and focuses on site-specific immobilization of strepta-
vidin on silica and reduction of nonspecific binding of proteins
were shown (D357).
Steady-state kinetics of the functioning of organometallic
amperometric membrane biosensors has been modeled (D358).
A model describing aspects of the transient and steady-state
behavior of toxicity monitoring biosensors, which incorporate
living microbial cells immobilized in a thin layer between an
amperometric electrode and a porous membrane, was presented
(D359). The electrochemical properties of carbon fiber micro-
electrodes were investigated in view of their application for the
construction of amperometric biosensors based on oxidase
enzymes (D360). Preparation and amperometric response of
carbon and platinum dual-cylinder microelectrodes were evaluated
(D361).
The detection of hydrogen peroxide produced by the enzymatic
reaction of ATP with glycerol and the subsequent oxidation of
glycerol 3-phosphate was carried out with a platinum-dispersed
carbon paste electrode (D362). A hydrogen peroxide sensing
electrode prepared by incorporating cobalt(II) octaethoxyphtha-
locyanine [CoPc(OEt)8] into a carbon paste oxidizes hydrogen
peroxide at lower potentials than a CP electrode with unsubstituted
cobalt phthalocyanine (D363). Peroxidase-incorporated conduct-
ing polymer electrodes were examined as hydrogen peroxide
sensors in acetonitrile (D364). The behavior of HRP in different
reversed micellar systems has been studied (D365).
The application of redox enzymes as biocatalysts for ampero-
metric sensing of antigen-antibody interactions at the electrode
surface makes the electrode insensitive to microscopic pinhole
defects in the monolayer assembly (D366).
192R Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
The rate of electron transfer from the substrate-reduced
enzyme to the redox polyelectrolyte depends on the tightness
of the complex (D367).
Direct electron transfer between enzymes and electrode
surface was demonstrated for monolayer-immobilized enzymes
catalyzing the reduction of H2O2 (D368, D369).
The electron pathway, which has a maximum electron coupling
between the active site and the surface of the enzyme, was verified
experimentally (D370).
A new, highly sensitive enzyme sensor was developed for the
detection of inorganic phosphate using maltose phosphorylase,
acid phosphatase, glucose oxidase, and mutarotase enzymes
coimmobilized on a regenerated cellulose (D371).
The detection of organophosphate and carbamate pesticides
using amperometric biosensors based on immobilized cholinest-
erases (ChE) was investigated (D372). Tungsten sensor that does
not amalgamate with Hg found an application for indirect detection
of organic thiols and proteins in buffered solutions (D373).
An amperometric internal enzyme gas sensing probe arrange-
ment provides an excellent selectivity for hydrogen peroxide over
ionic species in solution that cannot penetrate the gas-permeable
barrier (D374). Electrical communication between electrodes and
enzymes mediated by redox hydrogels has been discussed in
terms of different redox mediators covalently attached to the
polymer backbone (D375). A nonleaking amperometric biosensor
based on high molecular ferrocene derivatives has been claimed
(D376, D377). The application of ferrocene-containing dendrim-
ers as mediators in amperometric biosensors shows that these
sensors respond rapidly to the addition of glucose (D378).
Benzoic acid determination through competitive inhibition of
mediated bioelectrocatalysis of oxygen was described (D379). A
prototype amperometric fructose biosensor based on membrane-
bound fructose dehydrogenase and the coenzyme ubiquinone-6
immobilized in a membrane mimetic layer on a gold electrode
has been constructed and tested (D380).
Correlation between permselectivity and chemical structure
of overoxidized polypyrrole membranes used in electroproduced
enzyme biosensors was determined (D381).
Data acquisition, signal processing, and modeling using an
integrated artificial neural network applied to amperometric
detection of the polypyrrole formate biosensor were examined
(D382). An electrochemically stimulated release of ATP from a
poly(pyrrole ATP) film-modified Pt electrode was presented
(D383).
CONDUCTOMETRIC SENSORS
Sensors in this group rely on changes of electric conductivity
of a film or a bulk material, whose conductivity is affected by the
analyte presence. On a few occasions, the sensor measures the
analyte conductivity directly. The most predominant materials
used in these sensors will be examined first. The methods of
numerical processing of the analytical signal will be next, followed
by certain phenomena or properties which lend themselves for
the purpose of sensing. Specific analytes or purposes are not
treated systematically here. Only an eclectic choice of examples
is given, mentioning either the very prevalent or the quite unusual.
Selective Materials. Thin films are used mostly as gas
sensors due to their surface conductivity change following surface
chemisorption. They can be tailored for specific purposes (D384,
D385). The films are thin to achieve sufficient sensitivity and
response time. Due to oxygen chemisorption, CdS thin films can
be used as oxygen sensors (D386). Surface adsorption on SnO2
film deposited on alumina resulted in a highly sensitive and
selective H2S gas sensor (D387, D388). Pure Au thin metal film
can sense H2S because its resistivity changes dramatically upon
exposure (D389). Catalytically active Pt, Pd, and Ru are often
used to dope metal oxides to prepare sensors for H2 (D390).
Thick-film sensors rely on the bulk resistance of their active
material. For example a film (40 m) of porous MnWO4 works
as a humidity sensor (D391). Pd films (D392) or oriented MoS2
(D393) were used to sense hydrogen, BaTiO3 can sense CO2
(D394), tin oxide can detect CO at room temperature (D395),
and gallium oxide can sense reducing gases (D396). The effect
of thickness on H2 sensitivity of SnO2 nanoparticle-based thick
film was studied (D397).
Zeolites (D398) were used, for example, as a coating of planar
interdigital capacitive sensor for hydrocarbons (D399). Diamond
films are very attractive for their high-temperature stability. They
were used to prepare hydrogen (D256, D400) or NO2, HCl, and
O3 sensors (D401). A fullerene (C60) was used to construct a
sensor for monitoring hydrogen and humidity (D402) or NH3,
amines, and organic vapors (D403). Oxides doped with copper
or copper oxide are very sensitive to gas containing H2S (D404-
D406). For room-temperature operation, copper phthalocyanine
(Pc) was employed to detect sulfur compounds in diesel exhaust
gas (D407) or NO2 (D408-D410). A metalloporphyrin-clay
complex with cobalt produced an oxygen sensor (D329). A
hydrogen sensor based Cu-Pc with palladium admixture was
prepared (D411). Polymer composite films can change conductiv-
ity upon exposure to vapors, an effect that is typically used in
humidity sensors (D412).
Semiconducting Ga2O3 thin film can detect CH4 (D413).
p-Type semiconducting cuprates of Tm or Yb formulated as Ln2-
Cu2O5 (Ln ) Tm, Yb) respond to NO2, while the n-type cuprate
of Tb does not (D414). A p-type semiconductor sensor based on
Cr2-yTiyO3+x reacted to hydrogen sulfide (D415). A Pd/ZnO/p-
Si heterojunction was the essence of a hydrogen sensor (D416).
Similarly, a film of SnO2 doped with Pd was used (D417). A
Schottky barrier diode based on a planar polymer (poly(3-
octylthiophene)) was used to sense nitric oxide and ammonia
(D418). A double Schottky diode gas sensor with two films, Au
and Pd, in parallel was reported for phosphine and hydrogen
(D419). Illumination can enhance the sensitivity of some of the
sensor materials because many are semiconductive (D420). Films
illuminated with UV light may become sensitive to oxygen and
reducing gases such as CO (D421). Solid solutions based on the
rutile structure offer the possibility of independently varying the
cation composition and dopant density, e.g., for CO (D422). The
best known protonic solid electrolyte HUO2PO44H2O prepared
from uranyl nitrate and H3PO4 was used as a hydrogen sensor
(D423). Polymetallorotaxanes have been proposed as possible
sensor material for transition metal ions, e.g., Zn2+ (D424).
A new structure can be also created by patterning. Silica
overlayer over tin oxide has sieving properties. It was prepared
by CVD on a template of preadsorbed benzoate anion (D425).
Latex spheres (60-nm diameter) were used as a masking material
during evaporation of a gold film. Openings left after liftoff of
the spheres were suitable in size to immobilize antibodies or
enzymes which can act as specific recognition elements (D20).
Polymers, either conductive themselves or with a modifier, are
also often used. A WO3-impregnated thin poly(vinyl alcohol) film
across two closely spaced microelectrodes was employed as a CO2
sensor (D426). Some conducting polymers can be prepared with
high sensitivity, e.g., polypyrrole toluenesulfonate-doped film
(D427). Micrometer tower structures of polypyrrole can be
grown, perhaps providing sensor material with new properties
(D428). Polypyrrole can detect volatile amines (D429), or when
doped with ClO4- and tosylate, it can be made into a sensor for
NH3 (D430). A novel sensing format for the detection of toxic
vapors uses thin films of polypyrrole or polyaniline coated onto
poly(ethylene terephthalate) or nylon threads woven into a fabric
mesh. The resistivity of these materials responds to several toxic
gases including dimethyl methylphosphonate, NH3, and NO2
(D431).
New sensing materials can be prepared through LB films. A
low-conducting LB film, based on tetracyanoquinodimethane
(TCNQ) and tetrathiofulvalene (TTF) derivatives exhibits sensitiv-
ity toward nitrogen dioxide (D432). Other such films were
developed to sense methanol and ethanol (D433), odors (D434),
Cl2 (D435), or toluene (D433). Electrochromic LB films of
lutetium bisphthalocyanine were sensitive to electron donor and
electron acceptor gases and to tobacco smoke (D437). Self-
assembled bilayer lipid membranes on a metal support with
hemoglobin allow rapid detection of carbon dioxide in aqueous
solutions (D438). A charge-transfer system can be used as an
active component of conductive sensors. Tetrathiafulvalene salts
and oxanol dye have been investigated for use as gas sensors for
SO2, H2S, NO2, Cl2, CH4, and O2 (D439). Versatile devices can
be constructed by micromachining, for example, by integrating
heating on a single lithographic chip (D440) for CO (D441).
Integration of a sensor and attendant electronics is desirable and
is in some cases possible (D442).
Measurement Methods. Resistance measured from dc
current is typical. Often the measurement is done with ac current
(impedance), which also allows one to obtain changes in capacitive
impedance (reactance) (D443). Zeolite layers change capacitance
in response to the presence of combustion gases (D398-D444).
A pH detector based on capacitive structure was designed (D445).
Changes in permittivity of oxide mixtures was used in a sensor
for various gases, such as NOx (D446, D447), H2S (D406), CO2
(D448), SO2 (D449), butane or ammonia (D444), other organic
combustible gases (D450), or aroma sensing in meats (D451).
Discrimination between conductivity and capacitance through
impedance can extend the use of sensing materials. Conducting
polymer poly(N-(2-pyridyl)pyrrole) (D452) or zeolites (D444)
demonstrated the possibility to discriminate between capacitance,
conductance, resistance, and dissipation factor as a function of
frequency. A frequency spectrum technique proved useful in
monitoring the cure level of polymers (D443). A capacitive
immunosensor, consisting of an antibody layer fixed onto the top
of an oxide was also described (D453). Capacitance and resis-
tance changes of interdigitated electrodes were used to character-
ize directly some liquids (D454).
Analytical Chemistry, Vol. 70, No. 12, June 15, 1998 193R
 Frequency spectrum analysis of impedance can be used to
measure capacitance (vide supra), but it is also used to follow
noncapacitive properties such as ionic, electronic, contact, or
diffusional (Warburg) impedance (D443, D455). Impedance
sensors were described for NO2 and tobacco smoke (D456), odor
detection (D434) or determination of water in an oil-in-water
emulsion (D457). A Li-doped ZnO film responds to humidity by
change of dielectric relaxation (D458). CuO/ZnO semiconductor
heterocontact gave a distinct ac response to CO and H2 when a
different dc bias was superimposed (D459). In other work, CO
and H2 were distinguished using CuO/ZnO/Zn with Na-added
pn heterocontact. Each gas shows minimum reactance at a
different frequency (D460), and the selectivity can be improved
by dc bias (D461). Epoxy cure can be monitored by a method
known as frequency-dependent electromagnetic sensing (FDEMS)
(D462). Hall coefficient measurements for doped sensors based
on tin dioxide were used to sense a reducing or an oxidizing
atmosphere (D463).
Intelligent materials are a frequent theme (D464). Gas sensing
using an integrated sensor pair based on semiconducting oxide
with narrow and wide gaps allows some differentiation (D465).
Heterocontacts of La2CuO4/ZnO are usable as humidity sensors.
Their response is dependent on the tuning bias potential. They
also have a self-cleaning mechanism (D466). Intelligent materials
for humidity are Au/ZnO Schottky barriers, sol-gel processed
TiO2/K, or ceramic La2CuO4/ZnO p-n heterocontacts. The
intelligent functions of these systems are based on the multiphase
interaction of materials having different properties, such as p-type/
n-type semiconducting oxides, metal/ceramic, and conductor/
insulator (D467). A selective sensor based on temperature
switching was designed. At 700 C, the sensitivity toward other
reducing gases and H2O diminishes, whereas conductance sen-
sitivity due to CH4 increases (D468). A similar idea using doped
SnO2 film distinguishes between CO and CH4 (D469). Sinusoidal
voltage was applied to the heater of a SnO2 semiconductor gas
sensor. Nonlinear response ensued which was evaluated by FFT
and analysis for smart sensing (D470). Numerical procedures
became practical with the advent of omnipresent computers. A
thin-film sensor in conjunction with a neural network pattern was
used for recognition of trimethylamine and dimethylamine gases
as an indicator of food quality (D471, D472) or as gas sensor for
CH3SH, (CH3)3N, C2H5OH, and CO (D473). Odor sensing of
sulfur compounds for stomatological purposes was reported
(D474). Tin oxide is good material for combustible gases and
an artificial neural network (ANN) can improve selectivity (D475).
Frequency analysis is used in the nonlinear response from the
sinusoidal temperature change of a SnO2 gas sensor. FFT allows
discrimination between hydrocarbon gases and aromatic vapors
(D474, D476)). Fuzzy logic can handle the temperature depen-
dence of gas sensors to counteract nonlinearities in responses
(D477).
Examples of Measured Analytes. Humidity is very often a
parameter for which mixed oxides conductivity sensors are used
(D478, D479) although it can also be an unwanted interference.
A gas sensor for ethanol and acetone vapors, insensitive to
humidity, can be based on sintered bismuth tungstate (D480). A
humidity sensor was constructed using a composite film derived
from poly(o-phenylenediamine) and poly(vinyl alcohol) (D481).
194R Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
Conductive polyethylene as a sensitive layer for gas detection
reversible (CO2, O2), nonreversible (NO2), or partially reversible
to humidity was reported (D482). Conductivity caused by wetness
was used to detect moisture in food starch (D483). A humidity
sensor was prepared using potassium hexagonal tungsten bronze
synthesized from peroxopolytungstic acid and its resistivity change
mechanism was investigated (D484).
Reports on development of a multichannel aroma sensor are
quite frequent. They can be based on LB films (D434), conduct-
ing polymers, or metal oxides. A simple semiconductor system
was used to evaluate the efficiency of deodorants by sensing
ammonia, acetaldehyde, hydrogen sulfide, and methylmercaptan
(D485). A significant issue is monitoring freshness of meat
(D486, D487). For example, ethyl acetate, which appears in the
first stages of bacterial putrefaction (D326), trimethylamine,
dimethylamine, and NH3 (D471, D472) are all being detected.
Similarly, a multigas sensor detection of boar taint, an unpleasant
cooking odor exhibited by heating pork and mainly due to
androstenone and skatol, was introduced (D488), as well as
devices monitoring quality and ripeness of fruit (D489-D491).
Consomme` soup alone received three references, sensing acetone
(D492), capronaldehyde (D492), and 2-methylpyrazine (D493).
Arrays of several (six and more) aroma detectors able to
characterize more complex smells are called electronic noses
(D494). Often the results are enhanced by such algorithmic
methods as narrow-band filtering (D495), the use of neural
network processing (D471, D472, D496), or evaluation of inten-
tionally induced nonlinear response by fast Fourier transformation
(D474).
A convenient way to monitor the curing of an epoxy or a
thermoset is very desirable in the plastics industry. Conductivity
sensing is one of the means (D497, D498); another is capacitance
(D443) or impedance (D462).
Thermodynamically justified measurement of pH is done
potentiometrically. Some detectors using conductivity respond
to acidity, although not directly to the proton activity. Hydrogels,
which swell and change conductivity, were used as pH sensors
(D499), as were liquid membranes and polymers (D500) or the
conducting polymer polypyrrole (D501). A capacitive pH detector
was also described (D445). Resistance of a proton-conducting
electrolyte such as HUO2PO44H2O and PVA-H3PO4 changes with
H+ (D502), and at fixed H+ it also senses H2 pressure (D423).
Some sensors require high temperature for operation and may
therefore be suitable for applications in metallurgy or glass
making. An example is an oxygen sensor based on Y2O3-stabilized
zirconia used in glass melts (D503) or a sensor based on sodium-
alumina used to monitor the sodium level in Al alloys (D504).
Direct detection of antibody-antigen binding on silicon dioxide
or silicon nitride substrate plated with thin layer of platinum was
reported (D505). A conductive polyaniline antigen immunosensor
was also described (D506). A process to structure gold electrodes
with nanometer-sized dimensions for biosensor applications has
been developed. Impedance measurements at various frequencies
allow one to detect antibody-antigen binding (D507, D508).
Immunosensing for methamphetamine in human urine was
reported (D509). A urease biosensor for heavy metal ions was
developed based on their toxicity toward urease. The enzyme
can be reactivated by EDTA (D510). Another system uses urease
immobilized in porous glass. It relies on conductivity resulting
from hydrolysis of urea to charged products (D511, D512).
Ethanol was detected using a whole yeast cell-based conducto-
metric sensor (D513).
A simple conductivity sensor can measure solution resistance
in a gap between two electrodes. In others, chemical principles
are involved. Zinc oxide or tin oxide, doped with platinum
microcrystals, was useful for determining traces of hydrogen in
liquid hydrocarbons, e.g., transformer oil (D514). Aqueous ozone
can be measured by an In2O3 thin-film semiconductor ozone gas
sensor (D515). Polymer benzo[15]crown-5 complexes as sensor
materials were used to detect benzene in air and ethanol and
dichloromethane in water (D516).
A possible thick-film sensor distinguishing chirality based on
Cd2Sb2O6.8 was reported. An unusual feature is its stereoselective
response to limonene (orange oil) and pinene (pine oil) (D517).
OPTICAL SENSORS
Reviews. General fiber-optic sensors (E1, E2), Raman fiber-
optic probes (E3), and integrated optical sensors (E4) have been
reviewed. An extensive review containing over 700 references
covers the subject of fluorescence modulation by recognition
events. Optical sensors have found many applications in the
biomedical (E5) and environmental (E6-E9) fields. Plasmon
resonance is often included among optical sensors although it is
predominantly a benchtop optical technique. For the reviews of
this subject see refs E10 and E11. Quantitative optical spectros-
copy of tissues lies on the fringe of this review of direct chemical
sensors (E12). Apparently, the term optical nose does not have
the same appeal as the electronic nose but the idea is the same
(E13-E15)sa chemometric evaluation of multiple signal from the
optical sensing array. Optodes for heavy metal ions, their
performance, and applications have been reviewed (E16). As with
every sensing device, the two most interesting factors are the
sensing principle or phenomenon and the cleverness to choose a
modifier, which renders a particular property to the sensor. A
separate issue is the type of analytes detectable. Unless they are
for some reason unusual, this chapter does not mention them.
Various Measurement Modes. Surface plasmon resonance
is a technique that has found its way into a number of applications
in sensors. The plasmon resonance concept is sometimes
confused with evanescent waves. Distinction is given in ref E17.
The bulk sensor, which relies on a metal-coated Kretschmann
prism, has the needed geometry to allow the surface plasmon to
interact with the analyte on the opposite side of the metal film.
For example, detection for NO2 (E18), hydrogen via a palladium
film (E19), morphine (E20), or biological systems in which an
immunological principle is involved (E21, E22) have been
reported. More convenient experimentally but less well tuned
for the surface plasmon generation are planar waveguides (E23-
E27). The surface plasmon resonance depends on three experi-
mental variables: the incident beam angle, the incident beam
wavelength, and the refractive index near the surface along which
plasmons propagate. The latter parameter is usually the analytical
signal. The Kretschmann prism arrangement and monochromatic
light give the best SPR results, but it typically mandates a bulky
mechanical arrangement to measure the resonance angle. Poly-
chromatic light at a fixed angle is an alternative arrangement, in
which spectroscopic analysis of the throughput gives information
about the surface refractive index (SPR). Texas Instruments
introduced a compact single-chip design with polychromatic light
source and angle deflection measured by a solid-state detector
array. The device available as TISPR-1 has the dimensions of a
true sensor.
A more or less constant incident angle can be achieved if a
segment of an optical guide coated with thin metal film is used.
The spectrum of the light exiting the fiber can provide the
analytical signal related to the refractive index of the fiber surface.
With recent miniaturization of spectrometers built on a board that
fits into a PC, the method enters the sensor arena. Therefore,
sensors based on optical fibers have appeared. Organic solvents
were detected (E28, E29), and a humidity sensor constructed with
a coating of Nafion fluoropolymer was reported (E30-E32). The
shape of the fibers (e.g., U-shaped (E33)) is crucial for proper
performance, and tapered (E34) or conical fibers are the key to
improved performance. The gradual change in the taper cross
section results in distributed phase matching between the fiber
mode and the surface plasmon wave, permitting the plasmon wave
to be excited over a wide spectral range (E35).
Holography. The concept of using a hologram as the
interactive element in a biosensor was presented. A reflection
hologram in gelatin has been applied to the detection of the
enzyme trypsin (E36). Swelling due to water in solvent was the
basis of a holographic gelatin grating sensor (E37). An ellipsom-
eter from an optical fiber was constructed for applications in thin-
film sensor systems (E38).
Interferometry. A two-wave interferometer sensor was real-
ized in integrated optics. Spatially distributed interference fringes
give complete images of light absorption and phase variation in
the interferometer (E39). Intensity modulation can be used in
the Mach-Zender interferometer in which coherent light passing
along two paths is compared. In sensor application, the propaga-
tion in one channel is influenced by analyte interacting with the
surface of the light guide (E40, E41). Several such devices were
used as sensors for atrazine and other pesticides (E42-E44).
Another use was in immunosensing (E45). A novel type of
interferometric fiber-optic sensor based on a curved section of a
buffered single mode optical fiber was described (E46). Interfer-
ence occurs between the core guided mode and the whispering
gallery mode guided within the fiber buffer. The fiber buffer
coating thus serves as the sensing element.
Capillary optical sensors are promising because in addition to
the properties of the optical fiber they can serve as a sample cavity
of well-defined volume and are suitable for direct sampling (E47).
Sensors are often conveniently integrated in one device, e.g., for
measuring pH, oxygen, and carbon dioxide. The pH and the CO2
sensor can be based on the color change of a pH-sensitive dye
and the oxygen sensor on fluorescence quenching (E48).
Artificial Neural Network. The response range of an optical
fiber such as a pH sensor can be sometimes enhanced algorith-
mically, by the use of ANN (E49). ANN was used to handle the
output from a multilayer pH sensor at several wavelengths (E50),
and water pollutants were characterized by fluorescent sensors
with the help of neural network and pattern recognition schemes
(E51). An algorithmic approach to signal processing was used
to extend the linear operational range of an optical-fiber humidity
Analytical Chemistry, Vol. 70, No. 12, June 15, 1998 195R
sensor (E52). A multichannel optically based chemosensor using
ANN was constructed for odor sensing (E13).
Birefringence as an optical phenomenon was also used in
sensor construction (E53). The pockel cell is a device in which
an applied electric field causes birefringence. Bismuth germanate
(Bi4Ge3O12) is one such electrooptical material (E54). The
possibility to use ZnS:Mn and ZnS:Cu luminophores was also
presented (E55). The glucose sensor, a polarimeter of a kind,
was developed with this device, based on its optical rotation (E56).
Reflectance. An optical-fiber reflectance sensor for pH was
described (E57). A reflectance sensor based on a micromirror
with a palladium layer was constructed for hydrogen. The
mechanism consists of reversible microblistering of the film and
its changes in optical constants upon hydriding (E58). A
reflectance probe for uranyl was constructed by immobilizing
Arsenazo III on a cotton substrate (E59).
The resonant mirror biosensor uses the evanescent wave
associated with a dielectric resonant structure to detect reactions
occurring in a sensing layer, deposited within a few hundred
nanometers of the device surface (E60). A resonant photoacoustic
spectrophone was used for elemental carbon mass monitoring
(E61), and photoacoustic detection of trace gases with an optical
microphone was reported (E62). A sensor based on second-
harmonic generation at the surface of an ionophore-incorporating
poly(vinyl chloride) liquid membrane has been described (E63).
Fluorescent photoinduced electron-transfer (PET) sensors
were described in a few instances (E64): a saccharide sensor
based on the interaction of boronic acid and amine (E65), a pH
on-off sensor with pyridine (E66) or anthracene (E67) recep-
tors, or a calcium sensor (E68). Direct fluorescence and lumi-
nescence for sensing are quite common. A Ru(bpy)32+ lumines-
cent probe incorporated into Nafion film was described as an
oxygen sensor (E69), and a calcium probe using hydrophobically
associated calcein was reported (E70). The total internal reflection
fluorescence (TIRF) immunosensor was also described (E71).
Immunosensors are often based on fluorescence (E72). Chemi-
cally generated luminescence using tris(2,2-bipyridine)ruthe-
nium(III) was also used for sensing hydrazine (E73). Cyclodiene
insecticides (chlordane, heptachlor, aldrin, etc.) can be sensed
fluorometrically through fluorescein derivative-bovine serum
albumin conjugates (E74). Some fluorescent or luminescent
sensors use the decay time measurements as the sensing
technique. The concept is to take a single fluorophore with a
suitably long fluorescence decay time as the basic building block
for various sensors. Recognition can be performed by different
functional groups that are necessary for selective interaction with
the analyte (E75, E76). For example, NH3 (E77), Zn(II) (E78),
Cu(II) (E79), other 3d metal ions (E80) as well as organics
(methanol) (E81) can be detected. Concentration of an analyte
can be also deduced from its ability to quench fluorescence of a
fluorophore. Herbicide was detected by quenching a chlorophyll
fluorescence biosensor (E82), and plant tissue was used as a
pyruvate sensor (E83). Oxygen sensors based on luminescence
quenching using interactions of pyrene with polymer support were
described (E84). The widely used polar plasticizer NPOE is found
to act itself as a dynamic quencher of the luminescence of certain
indicators, and thus, 2-cyanophenyl alkyl ethers are more suitable
to use with fluorescent indicators in sensor manufacture (E85).
196R Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
Swelling was a basis for some optical sensors (E86). Swelling
of a polymer over a mirror system was used as a new principle
for measuring ionic strength (E87). A fiber optical sensor for
water in organic solvents used a bead of an anion-exchange resin,
which swelled continuously with the activity of water. The bead
size changes were coupled to movement of a reflecting diaphragm
(E88, E89). Reflectance changes due to aminated polymer
swelling were used to measure pH changes (E90).
Raman. An etched silver foil was used as an effective sensor
for surface-enhanced Raman scattering analysis of acridine,
9-aminoacridine, and quinacrine (E91). Another use was to follow
the progress of polymer resin curing (E92).
Selective Materials. Calixarene derivatives are an example
of a new material useful in optical sensing. They are used to build
supramolecular structures (E93-E95). Such structures can be
tailored to be ion or molecule selective and carry a chromophore.
A primary amine-selective optode membrane based on a lipophilic
hexaester of calix[6]arene was constructed (E96). A sodium-
selective optode was made based on calix[4]arene (E97, E98). A
uranyl ion-sensitive chromoionophore based in calix[6]arene was
made (E99) as well as a pH luminescent sensor (E100). Lipophilic
calixarene ionophores were used in the design of sodium-selective
optode membranes (E101). Calix[4]arenes with anthracene
moieties are sensitive to Li+, Na+, and K+ (E102, E103). In
general, any type of supramolecular structure may be useful for
sensor development (E104). For example, molecular imprinting
with exactly adapted cavities in polyurethane film was used for
solvent vapor sensing (E105) or sarin and soman were detected
by luminescence of Eu3+ embedded in a functionality-imprinted
copolymer (E106).
Sol-gels are excellent matrixes for entrapment of optical
probes. Not only are the dyes kept in place but often they better
resist photobleaching (E107-E111). For example, proteins, such
as copper-zinc superoxide dismutase, cytochrome c, myoglobin,
Hb, and bacteriorhodopsin, were encapsulated (E112). Another
useful class of compounds are the property sensitive dyes. They
usually change fluorescence as a function of potential (potential
sensitive dyes, PSD), lipophilicity, etc. A membrane responsive
to nitrite was developed with the PSD rhodamine B octadecyl ester
perchlorate. On exposure to nitrite its fluorescence intensity
increases (E113). A smilar idea was used in building a membrane
containing valinomycin, sensitive to K+ (E114). PSD are valuable
in both anion- and cation-sensitive polymer membranes. In
particular, nitrate-, nitrite-, K-, and Hg-sensitive membranes were
developed (E115).
Optical methods allow chiral discrimination. Results were
reported for odor perception distinguishing between enantiomers
of, limonene (E116). Chiral discrimination of D- and L-monosac-
charides using a designed receptor molecule that acts as a sensor
by virtue of its fluorescent response to binding of the guest species
was described (E117). A film of (N,N-bis(3,5-di-tert-butylsali-
cylidene)-1,2-cyclohexanediamine)manganese(III) chloride ad-
sorbed onto an n-type CdSe single-crystal substrate is stereose-
lective, coupling the complexation chemistry of the film to the
band gap photoluminescence intensity of the underlying semi-
conductor (E118).
Examples of Optical Sensing. Humidity. A fiber-optic
humidity sensor was based on the reversible pink/blue color
change of CoCl2 during hydration and dehydration (E119).
Another type was a luminescence lifetime-based sensor that
utilizes the Langmuir-Blodgett technique of depositing Pt- and
Pd-porphyrins (E120).
Aroma. Odor sensing is in the forefront of analytical interest,
and several optical sensors were also described. A chemilumi-
nescence gas sensor made of Al2O3 emits luminescence during
catalytic oxidation of a combustible odor vapor (E121). Novel
types are based upon the immobilization of a chemiluminescent
reagent between a miniature photomultiplier tube and a Teflon
diffusion membrane (E122). Taste and flavor monitoring was
done with a fluorescent optical probe detecting certain sulfur-
containing compounds in the vapors from the hams (E123).
Polymer Cure. Precise monitoring of the state of cure of
polymers is in significant industrial demand. A fiber-optic sensor
based on the principle of Fresnel reflection was built for intelligent
control of composite manufacturing (E124). In situ core monitor-
ing of diamine cured epoxy by fiber-optic fluorometry using
extrinsic reactive fluorophore was reported (E125, E126). Often
refractive index changes are used for such a task (E127, E128),
but even Raman spectroscopy was used (E92).
Acidity. Optical acidity sensors convey the pH changes of
their environment, although the true H+ activity measurement
must be done potentiometrically. Immobilized dyes are excellent
colorimetric sensors (E129, E130), often embedded in sol-gel
(E131, E132). The silica sol-gel system can handle high (1-11
mol/L) acidity (E133) and so can Nafion film, which coated with
cresol red served as a HNO3 sensor in the 0.1-10 mol/L range
(E134). Other possibility is to use fluorescence (E135, E136) or
even reflectance caused by swelling of aminated polymers (E90).
Acidity sensing can be also used indirectly, for example, for CO2
(E137). Ion-radical sensors are rare. One for hydroxyl radical
using nitrophenol as the sensitive-reagent phase was described
(E138).
Biosensor. A biosensor built upon Escherichia coli, genetically
engineered with a mercury(II)-sensitive promoter was used for
the detection of mercury (E139, E140). A fluorescent oxacyanine
dye (DiOC16(3)) as an optical transducer was used for the same
purpose (E141). Mercury(II) and cadmium(II) were detected
through a complexing porphyrin derivative (E142), and Cd(II)
was detected with a sensor constructed via the incorporation of
8-hydroxyquinoline-5-sulfonic acid into silica films prepared by the
sol-gel method (E143). A fiber-optic biosensor array is described
for the simultaneous analysis of multiple DNA sequences (E144).
CONCLUSIONS
The vitality of the chemical sensing field can be seen from
the growing number of published papers. Even if we allow for
mislabeling of sensing systems (assays) for true chemical sensors
and for duplicated reporting of results, the growth is overwhelm-
ing. So much so that the future reviews in this series should focus
entirely on the reviews of reviews and thus become a mother
of all reviews. The fact that data can be retrieved from the
commercially available sensor databases quite readily makes a
detail review of such a broad field almost redundant.
It is relevant to ask the question, why this apparently unbridled
growth? The partial answer lies in the fact that many authors
operate in the write-only mode, which results in unnecessary
replication of effort. It is also clear that the number of papers
describing sensing of individual species far exceeds the number
of the species themselves. This is true not only for glucose,
hydrogen, pH, and other all-time favorites but even for more exotic
analytes. The reason lies in the variety of applications that impose
specific and unique requirements on the figures of merit (or
performance characteristics) of the individual sensors. From this
point of view, it is imperative to publish the performance limita-
tions as well as the salient features of every new sensor.
The relative distribution of different types of chemical sensors
(by transduction principles) is about the same as it was when we
wrote the 1994 review. The electrochemical sensors again
represent the largest group (49%) by far (Table 1) followed by
optical and mass sensors. Although still the smallest group (3%
of total), the large relative increase of papers dealing with thermal
sensors (+435%) is interesting. It is due to the renewed interest
in pellistors and in new pyroelectric materials.
This table, however, does not reflect some very important new
trends that have emerged. More and more authors extract other
physical and chemical parameters from these devices than just a
calibration curve or a response. Thus, frequently, chemical
sensors become an integral tool of diverse scientific studies. This
may account for the large fraction of sensor papers being
published in the journals not dedicated to sensors or even
analytical chemistry. Another major development is the increasing
emphasis on multivariate analysis, i.e., extraction of data from
sensor arrays and higher order chemical sensors. The higher-
order (multiparameter) sensing somewhat complicates the sta-
tistics because a paper dealing with, for example, combined
sensing using optical and mass transduction is counted in both
optical and mass categories.
Some new selective materials figure prominently in this review,
e.g., calixarenes, DNA, cyclodextrins, dendrimers, and other
supramolecular materials. There are even hints of using the
combinatorial chemistry approach in design and optimization of
selective materials for sensing arrays. Materials problems related
to packaging of chemical sensors are also being rationally
addressed but not as much as would be needed. In our opinion,
these two materials issues will experience the above average
growth. Many new exciting sensors have appeared on the market.
Jir Janata received his Ph.D. in analytical chemistry from the Charles
University, Prague, in 1965. After postdoctoral studies at the University
of Michigan he joined the Corporate Laboratory of ICI in England and
in 1976 moved to the University of Utah where he was in the Department
of Bioengineering and in the Department of Materials Science and
Engineering, respectively. In 1991 he joined the Pacific Northwest
National Laboratory as Associate Director of Environmental Molecular
Sciences Laboratory. He left in 1997 for Georgia Institute of Technology
where he now holds Eminent Scholar Chair in the School of Chemistry
and Biochemistry. His main interests include chemical sensors, elec-
troanalytical and interfacial chemistry, and environmental chemistry.
Mira Josowicz received her Ph.D. in electrochemistry from the
Technical University, Munich, in 1978. She was a Research Fellow at
University of Bundeswehr, Munich, until 1983 and then an Alexander
von Humboldt Feodor Lynnen Fellow at the University of Utah until 1986.
She returned to University of Bundeswehr, Munich, where she remained
until 1992, when she became staff scientist in the Materials Sciences
Department of the Pacific Northwest National Laboratory. Since 1997
she has held a position of Senior Research Specialist in the School of
Chemistry and Biochemistry at the Georgia Institute of Technology.
Analytical Chemistry, Vol. 70, No. 12, June 15, 1998 197R
Petr Vany sek received his undergraduate degree from the Department
of Natural Sciences at the Charles University in Prague (Czechoslovakia)
in 1976 and a doctorate in natural sciences in 1977. He received the
Ph.D. degree in physical chemistry from the Heyrovsky Institute of Physical
Chemistry and Electrochemisty of the Czechoslovak Academy of Sciences
in Prague in 1982. In 1982-84 he worked as a research associate for
an electrochemistry group at the University of North Carolina at Chapel
Hill and during academic year 1984-1985 he was a faculty-in-residence
at the University of New Hampshire. In 1985 he joined the faculty of the
Chemistry Department of Northern Illinois University. He is currently
the Chairman of the Sensor Division of the Electrochemical Society.
Mike DeVaney received his B.S. in mathematics from the University
of Washington, where his Russian language skills helped pay for his
education. Before coming to the Pacific Northwest Laboratory in 1987,
Mike worked as a life insurance actuary, and as a mathematician and
computer scientist for the Naval Undersea Warfare Engineering Station.
At PNNL, Mike is currently a computer scientist in the Nuclear Safeguards
Program, a nuclear nonproliferation effort under the Comprehensive
Threat Reduction agreement. He assists Russia and other states of the
Former Soviet Union to develop automated systems for Nuclear Material
Protection, Control, and Accounting.
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