an interdisciplinary approach to microinstrumentation

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An Interdisciplinary Approach to Microinstrumentation Microinstrumentation Gilbert Haugen Lawrence Livermore National Laboratory Livermore, Calif. 94550 Gary Hieftje Department of Chemistry Indiana University Bloomington, Ind. 47401 One of the clear trends in modern sci- ence is toward miniaturization. In the microelectronics industry, miniatur- ization began with the invention of the transistor and progressed through modern large-scale integrated-circuit technology. In a similar fashion, minia- turization and integration are occur- ring in optics. Image capture, complex signal processing, storage, and readout can all be carried out now in monolithic integrated-optical arrays; this new ap- proach permits complex operations such as Fourier transformation to be carried out literally at the speed of light. Optical computers are envisioned as one of the important areas to be de- veloped in the next few decades (i). We are witnessing the same phenom- enon in the field of chemical analysis. The recent emphasis on sensors, on Microinstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microlnstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microlnstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microlnstrumentation MkroInsUumentatlon MlcrotnstnjmanUitiwi INSTRUMENTATION taking measurements at the sample lo- cation (in situ) rather than in the lab- oratory, and toward in vivo measure- ments urges that analytical instrumen- tation be made not only more sophisticated but also smaller, more re- liable, and more self-sufficient. These goals can best be met through an ap- proach that couples the concepts of mi- croengineering, biology, chemistry, and modern chemical instrumentation. The design of chemical microinstru- mentation will require a joint effort from scientists skilled in a range of dis- ciplines, from engineering to chemistry and from biology to microcircuit fabri- cation. Although this task will not be straightforward, its benefits will be substantial. With properly designed microinstrumentation, it will be possi- ble to employ disposable systems that are self-indicating and that constitute the modern equivalent oflitmus paper. Other sophisticated instruments might couple sensing and measurement with telemetry to permit long-term moni- toring of in situ or in vivo processes. Already, pharmaceutical chemists and physicians are seeking ways of continu- ously monitoring the blood glucose lev- el in a diabetic patient. Coupled with such a device might be an automatic dispenser of insulin, suggesting the ul- timate application of microinstrumen- tation—to the real-time control of bio- logical, environmental, or industrial processes (2). As far as chemistry is concerned, the field of microinstrumentation is still in its infancy. In this brief review we will describe several undertakings into this new field, including devices designed for the sampling and direct sensing of chemical constituents and those that might form part of a larger system or instrument. It is important to recog- nize that these examples are meant to be illustrative only and represent mainly the experiences of the authors and activities in progress in the micro- structure project of Lawrence Liver- more National Laboratory. A great deal of additional activity is currently under way in the field of chemical mi- croinstrumentation, particularly in the areas of field effect transistor sensors, metal oxide semiconductor sensors, py- roelectric sensors, and sensors utilizing immobilized microorganisms and elec- trochemical devices (3-7). Instrument manufacturers have not been idle, as is evident from some of the miniature devices that are available: gas chromatographs, hydrogen detec- tors, fiber-optics temperature probes, piezoelectric fans, and miniature re- frigerators (8). Microinstrumentation—scope, benefits, and objectives Many of the benefits of microlnstru- mentation are obvious—for example, reduced weight, power consumption, and volume. In addition, with reduced size comes increased ruggedness and response speed and reduced fabrica- tion costs. Indeed, many of the strengths of mi- croinstrumentation are derived from changes that occur as systems are scaled down in size. Phenomena that 0003-2700/88/0360-023A/$01.50/0 © 1987 American Chemical Society ANALYTICAL CHEMISTRY, VOL. 60, NO. 1, JANUARY 1, 1988 · 23 A

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Page 1: An Interdisciplinary Approach to Microinstrumentation

An Interdisciplinary Approach to Microinstrumentation Microinstrumentation

Gilbert Haugen Lawrence Livermore National Laboratory Livermore, Calif. 94550

Gary Hieftje Department of Chemistry Indiana University Bloomington, Ind. 47401

One of the clear trends in modern sci­ence is toward miniaturization. In the microelectronics industry, miniatur­ization began with the invention of the transistor and progressed through modern large-scale integrated-circuit technology. In a similar fashion, minia­turization and integration are occur­ring in optics. Image capture, complex signal processing, storage, and readout can all be carried out now in monolithic integrated-optical arrays; this new ap­proach permits complex operations such as Fourier transformation to be carried out literally at the speed of light. Optical computers are envisioned as one of the important areas to be de­veloped in the next few decades (i).

We are witnessing the same phenom­enon in the field of chemical analysis. The recent emphasis on sensors, on

Microinstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microlnstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microinstrumentation Microlnstrumentation Microinstrumentation Microinstrumentation Microinstrumentation M i c r o l n s t r u m e n t a t i o n MkroInsUumentat lon MlcrotnstnjmanUitiwi

INSTRUMENTATION taking measurements at the sample lo­cation (in situ) rather than in the lab­oratory, and toward in vivo measure­ments urges that analytical instrumen­tation be made not only more sophisticated but also smaller, more re­liable, and more self-sufficient. These goals can best be met through an ap­proach that couples the concepts of mi­croengineering, biology, chemistry, and modern chemical instrumentation.

The design of chemical microinstru­mentation will require a joint effort from scientists skilled in a range of dis­ciplines, from engineering to chemistry and from biology to microcircuit fabri­cation. Although this task will not be straightforward, its benefits will be substantial. With properly designed microinstrumentation, it will be possi­

ble to employ disposable systems that are self-indicating and that constitute the modern equivalent oflitmus paper. Other sophisticated instruments might couple sensing and measurement with telemetry to permit long-term moni­toring of in situ or in vivo processes. Already, pharmaceutical chemists and physicians are seeking ways of continu­ously monitoring the blood glucose lev­el in a diabetic patient. Coupled with such a device might be an automatic dispenser of insulin, suggesting the ul­timate application of microinstrumen­tation—to the real-time control of bio­logical, environmental, or industrial processes (2).

As far as chemistry is concerned, the field of microinstrumentation is still in its infancy. In this brief review we will

describe several undertakings into this new field, including devices designed for the sampling and direct sensing of chemical constituents and those that might form part of a larger system or instrument. It is important to recog­nize that these examples are meant to be illustrative only and represent mainly the experiences of the authors and activities in progress in the micro-structure project of Lawrence Liver­more National Laboratory. A great deal of additional activity is currently under way in the field of chemical mi­croinstrumentation, particularly in the areas of field effect transistor sensors, metal oxide semiconductor sensors, py-roelectric sensors, and sensors utilizing immobilized microorganisms and elec­trochemical devices (3-7).

Instrument manufacturers have not been idle, as is evident from some of the miniature devices that are available: gas chromatographs, hydrogen detec­tors, fiber-optics temperature probes, piezoelectric fans, and miniature re­frigerators (8).

Microinstrumentation—scope, benefits, and objectives

Many of the benefits of microlnstru­mentation are obvious—for example, reduced weight, power consumption, and volume. In addition, with reduced size comes increased ruggedness and response speed and reduced fabrica­tion costs.

Indeed, many of the strengths of mi­croinstrumentation are derived from changes that occur as systems are scaled down in size. Phenomena that

0003-2700/88/0360-023A/$01.50/0 © 1987 American Chemical Society

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Figure 1. Operational sequence during microsample dispensing: (1-3) forma­tion of liquid filament, (4) filament de­taches from glass needle, (5) filament collapse, (6) microsample droplet. (Reproduced with permission from Reference 9.)

are important in our conventional world—gravity, inertia, magnetism, flow, and thermal emission—become relatively unimportant in the microworld. Instead, small devices are affected more by electrostatic forces, surface tension, diffusion, van der Waals forces, and quantum effects. Thus the design, fabrication, and use of microinstrumentation must follow pathways different from those that are customary.

For example, a propeller in the mac­roscopic world creates lift as it rotates. However, shrinking its dimensions pro­portionally does not yield a useful pro­peller in the microworld. As is exempli­fied by bacteria, a micrometer-sized helix provides a far more useful ap­proach for propelling small systems.

As this example suggests, the biologi­cal world has already solved some im­pressive microinstrumentation prob­lems on its own. For instance, the gypsy moth can detect molecules with a sensi­tivity of one molecule per second and a selectivity approximately one part in 1020; trained dogs can uncover clandes­tine material with a selectivity of one part in 1017 or 1018. Other examples could be readily cited; scientists who are developing microinstrumentation should consider whether the biological world has already undertaken a similar task.

Microdispensers

In many situations it is necessary to obtain a representative microsample of a material before it can be chemically analyzed. Although such microsam­pling devices have long been available, only recently have they become capa­ble of computer control. Ideally, a mi-

crosampler should produce tiny (r ano-liter or below) aliquots of a sample so­lution on a demand basis. The system should be under electronic control so that computer manipulation is straightforward. Finally, microaliquots should be able to be dispensed on an individual basis or in rapid sequence so that signal averaging is possible.

The unit displayed in Figure 1 (9) offers many of these attributes. The operation of the microdispenser is re­vealed in the sequence of frames. In frame one, a glass needle (lower left) is poised for insertion into the bulk liquid (upper right) from which the micro-sample is to be drawn. As the needle penetrates the liquid (frame 2) and subsequently withdraws (frame 3), it pulls with it a tiny filament of the sam­ple solution. That filament then de­taches from the glass needle (frame 4) and from the bulk liquid (frame 5) to collapse into a tiny microdroplet (frame 6).

The sequence of operations depicted in Figure 1 can be carried out once or in rapid succession (up to several thou­sand times per second) so that droplets can be dispensed one at a time or in multiples for improved precision. Be­cause each droplet is somewhat smaller than one nanoliter and can be generat­ed with a relative standard deviation of about 2% (in diameter), it thus be­comes possible to dispense microliter-sized (thousand-droplet) aliquots at precision levels below 0.3% (9).

This entire microdispenser is operat­ed under computer control and already has been applied as a sample introduc­tion device for atomic absorption spec­trometry (10) and in titrimetry (11). Other droplet generators, based on a different principle (12), have been ap­plied to similar fields. These generators are capable of even finer volume reso­lution and have also been used in a "pH-stat" instrument (13). We are likely to see further developments in the field of microdispensers in the near future.

Microsensors

Microsensors are often integrated sys­tems that incorporate both a chemical­ly selective element and a readout de­vice (3-6). In other cases, microsensors require external components for ampli­fying or recording their output signals. In this paper we will briefly describe several kinds of sensors applicable to both chemical substances and physical phenomena.

Multicomponent quartz piezobal-ance. An attractive approach to chem­ical sensing involves a quartz piezobal-ance coated with a chemically selective adsorbing or absorbing layer (14). Be­cause the resonant frequency of the crystal depends on the total mass of the crystal and its coating, the absorption

of substances by the selective coating can be detected as a change in the crys­tal frequency. Of course, the selectivity of a typical quartz piezobalance arises only from that of the absorbing layer. Because few adsorbing or absorbing processes are completely specific, such detectors have suffered from a lack of selectivity.

As a variation of this traditional ap­proach, we and others (15-17) have coated an array of quartz piezobalance elements with different absorbing lay­ers. Although no single layer will be entirely specific, the degree of selectiv­ity attainable by monitoring the en­semble of resonant frequencies enables one to decode the response pattern for a single target species (18). Examples of such response patterns can be found in Figure 2, where the amplitude of re­sponse is plotted on the vertical axis and the identity of the absorbing layer on the horizontal axis.

Obviously the selective layers should exhibit for the target substances affini­ties that are as different as possible. If eight degrees of freedom are used in the coating-selection process and 10 indi­vidual coatings are used, a measure­ment with 10% reproducibility in the response pattern would be sufficient to resolve some 800,000 different chemi­cal vapors (19). Sensitivities to differ­ent vapor species are in the parts-per-million or subnanogram range, and the device is selective to more than 105 in­dividual compounds.

The next stage of miniaturization of this piezobalance device would be a single crystal driven at a high harmonic frequency. The pattern of vibration on the surface would be a standing wave (20); the locations of maximum ampli­tude would then each be covered with a different chemically selective layer. The resulting gas sensor would be ap­proximately 1 cm2 in area and 2 mm thick. Qualitative measurement with such a device would be possible by matching an observed pattern of oscil­lation to premeasured patterns; quan­titative measurements would be possi­ble by examining the magnitude of the response (19,21, 22).

Elasticity sensor. An illustration of a microsensor for a physical phenome­non is one intended to measure elasti­city. A miniature piezoelectric vibrator in contact with an elastomer behaves as a forced harmonic oscillator with damping. At relatively high frequen­cies (e.g., 6 MHz), oscillations of such a combination are not completely damped, and the magnitude of oscilla­tion depends on the load experienced by the piezoelectric element. In turn, this load is affected by changes in the modulus of elasticity of the elastomer caused by variations in its temperature or aging.

An experiment with a specific elasto-

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mer demonstrated a linear relationship between the Q of the oscillator and ag­ing time. For every week of aging, the value of Q changed by 15%. The same elastomer, when exposed for 20 h to an atmosphere containing 8 ppm of ozone, exhibited an observable change in reso­nant frequency. The piezoelectric os­cillator can be quite small (0.1 mm3 in volume) and easily embedded into gas­ket material. The necessary measure­ment of Q requires only a solid-state frequency meter (23). A prototype elas­ticity sensor would require an encapsu­lated oscillator that compensates for ambient fluctuations in temperature and pressure.

Integrating temperature record­er. Microinstrumentation can be sub­ject to small temperature variations that greatly exceed those encountered by larger systems. Consequently it is important to develop small devices for indicating temperature or, better, for recording it on a continuous basis. To be practical, such a temperature sensor should be inexpensive, should permit unattended operation, and should pro­vide a complete temperature history when interrogated.

A device that satisfies these criteria is based on the change in surface resis­tance and capacitance that occurs in doped semiconductors as their envi­

ronmental temperature is altered (21). Such devices, typified by the lithium-drifted germanium or silicon detectors used in measuring high-energy pho­tons, degrade in performance slowly as a dopant element (lithium here) dif­fuses farther and farther into the sub­strate. Because the diffusion rate is temperature-related, the dopant pro­files of such a detector can be employed to deduce its temperature history.

The dopant-semiconductor combi­nation that is currently being tested (24) is germanium doped with lithium. The total extent of lithium diffusion that has occurred during a particular time interval will be defined by the in-

Figure 2. Response of a coated piezobalance to different vapor-phase substances. The identity of the adsorbing or absorbing layer (coating) is indicated on the horizontal axis; the magnitude of response (change in crystal resonant frequency) is shown on the vertical axis. The pattern produced by a particular vapor can be used to identify it; the magnitude of the pattern can be used to determine vapor concentration. (Adapted with permission from Reference 17.)

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tegral of the time multiplied by an ex­ponential function of the temperature. As shown in Figure 3, this degree of diffusion can be measured by the change in surface resistance or capaci­tance that it produces. A 1% change in temperature at a mean temperature of 373 Κ causes a 7% change in surface concentration. Exposure of this wafer to a temperature step of 80 °C (293-373 K) causes nearly a factor of two change in dopant concentration profile within two hours.

Because the diffusion rate depends on an activation energy, one can alter the sensitivity of the integrating tem­perature microsensor through choice of the semiconductor material or the dop­ant. If several combinations of semi­conductor and dopant are used that possess a range of activation energies, the combination of readouts corre­sponds to a set of integral equations that can be inverted mathematically (inverse LaPlace transform) to pro­duce the full curve of time vs. tempera­ture.

Of course, the number of time-reso­lution elements that can be obtained in this way is limited to the number of different activation energies of dop­ant-semiconductor combinations that are employed. A dopant layer of vari­able initial thickness can be used over limited temperature ranges instead of changes in dopant or semiconductor composition. This kind of device is por­trayed in Figure 4.

Chemiresistor. Very thin layers of semiconductor materials exhibit sub­stantial changes in electrical resistance when even fractional monolayers of materials having a permanent or an in­

duced dipole moment are deposited on them (4, 6). Not surprisingly, individ­ual thin-film materials show different levels of response, not only from changes in the amount of vapor ab­sorbed or adsorbed on them, but also because of variations in sensitivity to the effect. Such devices offer attractive alternatives as microsensors. Organic semiconductive layers are particularly suitable here; they can be made in ex­tremely thin layers, they have a high intrinsic response to adsorbed materi­al, and they have no tendency to form surface protective layers during expo­sure to air. They can also be deposited easily in films of controllable thickness.

Such a chemiresistor is extremely sensitive and can be used to detect less than a monolayer of adsorbed material. Current detection limits, even before complete optimization, are on the or­der of picograms. As with piezosensors, the selectivity of a chemiresistor de­pends on the characteristics of the thin-film material on which the target material deposits.

Unfortunately, semiconductors that exhibit the strongest chemiresistance effect have extremely high resistivities. This fact, coupled with the very thin layers that are employed, yields a film of extremely high resistance. Therefore fairly high operating voltages are re­quired to produce easily measured cur­rents. Such high voltages can cause electrical breakdown and, even at lower levels, electrochemical decomposition.

Obviously it would be desirable to reduce the length of the chemiresistive layer and employ electrodes that have a relatively large area so that currents can be as large as possible for a given

Figure 3. Response curve for integrating temperature-exposure microsensor (see text for discussion).

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Measurements that measure up

are important to everyone who needs quality. When you measure how do you know your results are right? Link up to National Standards. The National Bureau of Standards has over 900 differrent Standard Reference Materials that can help you calibrate instruments and check on measurement accuracy.

If Quality measurements are important to you and you want more information phone or write for a free catalog on Standard Reference Materials Telephone (301) 975-OSRIM (6776)

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Figure 4. A Li-drifted silicon detector such as those used in measuring high-energy radiation can be used as an inte­grating temperature recorder. A Li-drifted layer with varying thickness is em­ployed. At each location along this layer, the tem­perature history of the device can be expressed as an integral equation (on right). Interrogating the layer at a number (n) of locations then permits the temperature at η discrete time intervals to be cal­culated.

driving voltage. Unfortunately, calcu­lations show that the optimal length of the resulting chemiresistor is on the or­der of only a few hundred angstroms— well below that obtainable with current integrated-circuit technology.

A new procedure has recently been developed to overcome this limitation. In this technique, a very thin (less than 300 Â) strip of gold is deposited on quartz between thicker contact strips of the same material. After these films have been vacuum-deposited, the layer is heated to approximately 120 °C, the temperature at which the films recrys-tallize into arrays of gold microcrystal-lites separated by some tens of ang-

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NBS

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Figure 5. A "chemiresistor" can be fabricated by heating a thin film of gold to pro­duce closely spaced microcrystallites on a thin layer of phthalocyanine. Quantum tunneling between the microcrystals then produces a measurable current that is affected strongly by even submonolayer deposits of a target compound.

stroms. This arrangement is shown schematically in Figure 5. In such a dis­continuous thin layer, current can trav­el between the electrodes by quantum tunneling across the narrow gaps be­tween gold crystallites. Currents up to

1 μΑ have been demonstrated by using 1-2 V across the electrodes—a voltage low enough to avoid instability and short device lifetimes. When the thin film (a few monolayers at most) of semiconductor (phthalocyanine) is de­

posited on top of the gold "layer," a sensitive and stable detector is pro­duced.

In a manner similar to that employed in the development of a selective piezo-sensor array, the thin-film semicon­ductor sensor is made selective through the use of arrays of devices. Such an array can be constructed by microfab­rications simply on a single sheet of quartz substrate material (25). The ar­ray of electrodes on the quartz sub­strate is then separated by thin strips of recrystallized gold and coated with different semiconductor (phthalocya-nines) layers. Again, a pattern of re­sponses is produced that is indepen­dent of sample concentration but that indicates the identity of a particular sample constituent (see Figure 6). Working curves showing the simulta­neous detection of ammonia and water on an electron-tunneling gas sensor are shown in Figure 6 (19).

The future The foregoing sections have provided a glimpse of new developments in mi­croinstrumentation. However, the ap­plications of microengineering are far more abundant than those we have dis­cussed here (3, 4-6, 8). Our findings have been encouraging, however, and several projects have made the transi­tion from research activity to direct ap­plication. In addition, the development of microsensors and microdevices of various kinds is proceeding in an in­creasing number of laboratories throughout the world. The use of mi­croengineering as a tool for materials and systems design is just beginning: The potential of this exciting tech-

Figure 6. (a) Working curves for ammonia and water vapor, obtained on the quantum-tunneling chemiresistor coated with phtha-locyanine-Mg depicted in Figure 5. (b) An array of six quantum-tunneling chemiresistors, each having a different phthalocyanine, demonstrates selectivity. The test vapors are water, ammonia, and ethyl alcohol.

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nique appears to be enormous and could bring about a revolution in mi­crominiaturization of measurement systems. The recent announcement of high-temperature superconductors suggests that large arrays of microin­struments might be possible and that computer capability will increase dra­matically in systems that formerly were impossibly small in size.

To realize success in the develop­ment of microinstrumentation, an in­terdisciplinary approach is extremely important. Basic research and scaling laws must be coupled with careful use of the literature in a broad range of areas (microelectronics, entomology, integrated optics, etc.) to generate new ideas. We hope that this "team" ap­proach to microinstrumentation will be used in many other laboratories and that it might form the focus of an effec­tive Science and Technology Research Center of the kind to be sponsored by the National Science Foundation.

Although a substantial number of al­ternative devices could be discussed here, we close by listing a few systems whose concepts have been confirmed by feasibility studies and that offer new capabilities in microinstrumentation or microdevices.

• A high-thermal-conductivity plas­tic has been designed around small-di­ameter glass capillaries that serve as an array of heat pipes. The resulting rela­tively inert unit possesses an equiva­lent thermal conductivity 3 orders of magnitude greater than that of an alu­minum rod of similar dimensions (26).

• New coatings have been developed that are resistant to both abrasion and impact. The coatings are designed from long filaments of materials such as carbon or aluminum oxide. The result is similar to the protective effect of mammalian hair (26).

• A miniature dryer has been con­structed that operates in a fashion sim­ilar to that of a human sweat gland. Operating with selective membranes made from Nafion and a fluorosilicone, the microdryer operates at 2 V and can dispose of nearly 2 g of water per year for each milliampere of current that it consumes (21,26)

• A microcamera has been designed that is piezoelectrically scanned and can transmit entire images over a single optical fiber (26).

• A microsensor is being explored that is capable of sensing organic va­pors by changes in the numerical aper­ture of an optical fiber that the vapors induce (26,27).

• A pocket-sized, low-voltage ioniza­tion detector that can detect organic vapors is being constructed (26).

• An optically driven piezobalance is being explored (26,28).

We hope that these concepts will en­courage many readers to explore the

exciting new world of microinstrumen­tation.

This paper is dedicated to the late Tomas Hirsch­feld, who headed the microstructure project at Lawrence Livermore National Laboratory and who initiated many of the concepts and devices described here. Work was performed under the auspices of the U.S. Department of Energy by the Lawrence Livermore National Laboratory under contract no. W-7405-ENG-48. Research was sup­ported in part by the Office of Naval Research and by the Upjohn Co.

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38 (28) Venkatesh, S.; Culshaw, B. Proc. SPIE

Annu. Tech. Symp. 1985,566,110.

Gilbert Haugen is a senior scientist with the Chemistry and Materials Sci­ence Department at Lawrence Liver­more National Laboratory. He re­ceived his Ph.D. in chemistry from the University of Southern California in 1962. His research interests include chemical kinetics and mechanistic thermochemistry, photochemical and photophysical processes, optical in­strumental and experimental design, and the application of information theory to chemical measurements. He is also interested in the application of lasers in chemical measurements and in time-resolved, correlation, Raman, luminescence, and remote sensing with fiber optics spectroscopy.

Gary Hieftje is distinguished profes­sor of chemistry at Indiana University in Bloomington. He received an A.B. degree from Hope College (Holland, Mich.) in 1964 and a Ph.D. from the University of Illinois in 1969. From 1964 to 1965 he was a research asso­ciate in physical chemistry at the Illi­nois State Geological Survey (Ur-bana). In 1969 he was appointed assis­tant professor of chemistry at Indiana University and was subsequently pro­moted to associate professor and then to full professor in 1977. He received a special appointment to a distin­guished professorship in 1985. His re­search interests include the investiga­tion of basic mechanisms in atomic emission, absorption, and fluorescence spectrometric analysis and the devel­opment of atomic methods of analysis.

ANALYTICAL CHEMISTRY, VOL. 60, NO. 1, JANUARY 1, 1988 · 31 A