Anal. Chem. 1994,66, 558R-594R
Chemical Microscopy Peter M. Cooke
McCrone Research Institute Inc., 2820 South Michigan Avenue, Chicago, Illinois 606 16 Review Contents Books of General Interest Articles of General Interest Optics Instruments Polarized Light Microscopy Microphotometry and Microspectrophotometry IR, UV, and Raman Microscopy Fluorescence Microscopy Laser and Holographic Microscopy Interference Microscopy Phase Contrast and Schlieren Microscopy Confocal Microscopy Ultramicroscopy X-ray Microscopy Acoustic Microscopy Cathodoluminescence Embedding and Mounting Ultramicrotomy Miscellaneous Specimen Preparation Photomicrography and Photomacrography Refractometry Hot Stage and Cold Stage Techniques Stereology Automated Image Analysis and Video Microscopy Particle Grain Size Measurement Miscellaneous Techniques for Specimen Examination Liquid Crystals Resins, Polymers, and Their Additives Textiles, Fibers and Films Wood and Paper Coal Emulsions Minerals Cement and Concrete Glasses, Ceramics, and Abrasives Metals Semiconductors and Electronics Forensic Science Food and Feed Biology and Medicine Pharmaceutical Microchemical Analysis Organic Analysis
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Peter M. Cooke is an Instructor and Research Microscopist at the McCrone Research Institute. He has extensive teaching experience in polarized light microscopyand associated microscopical applicationsand techniques, crystallography, and ultramicroanalysis. He also serves as a Technical Expert for the NVLAP/NIST lab accreditation program. Prior to working at the Institute, Mr. Cooke was VP of Universal Laboratories, Pittsburgh, PA. He received his BS from the University of Akron in 1980, majoring in b biology and chemistry, and completed his Masters course work in geology there in 1983. Other areas of interest in addition to teaching include pollination biology, mineralogy, and micropaleontology. He is a member of numerous national and international Microscopical Societies.
the last two years and articles of general interest to the amateur and professional microscopist are included. The alphanumeric referencing scheme is similar to the 1992 review. The current review is comprehensive but not exhaustive. The amount of new instruments, techniques, and consequent papers in the field of microscopy continues at an overwhelming pace. ACS guidelines also dictate that emphasis be placed on current progress in applications advancing microscopy, and in instumentation related to current or potential analytical methods, rather than publications of a more theoretical nature. Applications of advanced imaging techniques are selectively included. Several new journals made their debut in the last two years. Microscopy and Analysis, a United Kingdom publication that bridges the gap between formal microscopy journals and trade magazines, is now available in the United States. The U.S. version is similar in format, containing many, but not all, of the articles in the U.K. edition. Microscopy Today, a newsletter for current industry news and events as well as brief reviews in all areas of microscopy, claims a circulation of more than 14 500 in the United States, Canada, Mexico, and Europe. Since its inception two years ago, it continues to show improvementin both style and content. Acta Microschpica, a joint venture of the Venezuelan Society for Electron Microscopy and the National Committee for the Investigation in Science and Technolom. features applied and experimental microscopy in biology, medicine, and materials science. The first volume contained excellent micrograph reproduction. A new society-The Historical Microscopical Society-was founded in 1992. Its main objective is to exchange information about equipment and methods related to traditional light microscopy and its history. The Electron Microscopical Society of America (EMSA) celebrated their 50th anniversary,officially dropping the word “electron” from their name. This change emphasizes the broadening horizons of the society and is reflective of the v
This is a selective review of the chemical microscopy literature from approximately b x m b e r 1991 to ”ember 1993. As in previous reviews, references were obtained from major microscopical journals, periodicals containing contributions of interest to the microscopist, and Chemical Abstracts. A few publications related to electron optics are included, relecting the growing conjunction of light and electron microscopical techniques. Books published or reviewed in 558R
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growing applications and integration of instrumentation and techniques noted within this review. An ambitious educational program was recently launched by the Royal Microscopical Society in an effort to foster interest in microscopy at the primary and secondary levels. The purpose of “A Microscope in Every School” is to assist schools with the purchase of microscopes, to provide teachers and students with information in the form of brochures, worksheets, and booklets, and to set up a speakers’ bureau of professionals to visit schools and demonstrate the uses of microscopes. The Microscopical Society of America (formerly EMSA) is sponsoring a microscopical education program similar to that of the RMS, named “Micro”, in the United States. Both the Royal Microscopical Society and the Microscopical Society of America, recognizing that science education must begin early in life, are to be lauded for their formidable educational outreach efforts. The year 1993 marked the centennial of the landmark publication of a microscopical method of illumination described by a 26-year-old school teacher, August KBhler. Ein neues Beleuchtungsverfahren fur mikrophohographische Zmecke debuted in 1893 in Zeitschrift fur wissenschajiliche Mikroskopie. The Royal Microscopical Society marked the October event by publishing the full English translation of Kohler’s, “A new system of illumination for photomicrographic purposes”, in its Proceedings. The method, which remains synonymous with his name to this day, is important because it allows the maximum amount of even illumination to be obtained from inhomogeneous light sources. The fundamental principles of Kohler illumination are relevant not only to traditional light microscopy, but also to many modern imaging techniques which are found in this review. The last two years have seen significant applications in microscopy, due to improvements in optics, instrumentation, and contrast enhancement techniques. Confocal laser scanning microscopy, with its use of a diaphragm inserted into the intermediate plane of the scan unit, has become more routine, allowing a wide variety of three-dimensional imaging at a resolution approaching the diffraction limit. Scanning probe microscopy is increasingly being applied in materials science for surface studies, inspection of defects and fractures, monitoring crystal and thin film growth, etc., down to the atomic level. Scanning probe, with the integration of atomic force microscopy and its capabilities for use in fluids and nonconducting surfaces, is rapidly moving toward chemical and biological surface applications. Near-field optical microscopy, with its subwavelength resolution, is advancing from the development to application stage due to recent innovations in producing reliable and efficient probe tips. Acoustic imaging, because of its nondestructive nature, continues to be exploited in the materials sciences. There has been an increase in the use of more than one kind of microscope and/or technique for the analysis of materials at the molecular level, including X-ray, microFourier-transform infrared, laser, holography, polarized light, micro-Raman, and fluorescence, the various scanning probes, and the scanning electron microscope. There are now so many instruments called microscopes, and so many different microscopical techniques, that the very
idea of what a microscope is and can do has changed immensely. All the new microscopes have demonstrated their value in getting specific information and/or images never before obtainable. This gives today’s chemical microscopists, using the versatile polarized light microscope as their principal investigative tool, an unprecedented analytical capability.
BOOKS OF GENERAL INTEREST Richardson ( I ) succeeded in producing a book useful to both novice and professional in Handbook for the Light Microscope. A wide range of practical applications from biological to material sciences are found in discussions on a variety of topics including optics, various types of microscopes and imaging techniques, contrast enhancement, quantitative microscopy, accessories, photomicrography, and photomacrography. Up-to-date references are found throughout. An excellent text from a master in the field, Callaghan’s Principles of Nuclear Magnetic Resonance Microscopy ( 2 ) is written for advanced microscopists in the field of NMR imaging. ConfocalMicroscopy, edited by Wilson (3), is an enjoyable and readable text recommended for students as well as practitioners and researchers. A comprehensive book, it offers a broad view of applications in the expanding role and study of confocal microscopies. Both failure analysts unfamiliar with imaging techniques and instrumentation and microscopists unfamiliar with the mechanics of failure will benefit from The Role of Microscopy in Semiconductor Failure Analysis by Richards and Footner ( 4 ) ,the 25th addition to the RMS Handbook series. Included are classification of defects; procedural outlines; an introduction to imaging, instrumentation, applications, and techniques; specialized instruments including scanning microscopies, acoustic imaging, X-ray, microradiography, and electron imaging; reviews of thermal imaging and tunneling microscopies; and a helpful outline for choosing appropriate techniques. Acoustic Microscopy by Briggs ( 5 ) has been called a masterly volume that is complete, ambitious, and captivating in its coverage of acoustic imaging. Vivid practical applications abound, a discussion of lens design and selection for different operations is detailed, signal generation and detection circuitry are well described, and problems with image contrast are thoroughly explained. The Image Processing Handbook by Russ (6) covers a wide variety of techniques. It is highly practical, as opposed to theoretical, and contains many illustrations and figures with an emphasis on microscopy. The third revised edition of Kok and Bon’s (7) Microwave Cookbook for Microscopists contains additional general biological applications as well as much new information in an effort to gain more widespread acceptance in biological laboratories. Clear, practical advice is given in Humphries’ (8) The Preparation of Thin Sections of Rocks, Minerals, and Ceramics. Means for collection, preparation, mounting, grinding, covering, storage, staining, etching, making peels, thin and ultrathin section preparation, and polishing for reflected light are all well covered with up-to-date information on processes and instrumentation. Analytical Chemistty, Vol. 66.No. 12, June 15, 1994
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The fourth volume in the highly acclaimed series of photographic atlases of rocks in thin section is Atlas of Metamorphic Rocks and Their Textures by Yardley, MacKenzie, and Guilford (9). The photomicrographs, with mineral and all-important textural descriptions, are of high quality. Both student and professional will benefit. They succeed in their aim “to illustrate a range of the most common and most significant metamorphic rock types, and to demonstrate the way in which deductions can be made about metamorphic conditions and metamorphic history of a region, from observations in thin section”. The fourth edition of Faegri and Iverson’s (10) Textbook of Pollen Analysis has been highly recommended as “one of the two most useful books on the subject currently available”. A more modern approach represents a departure from previous editions and has been noted by reviewers as being more appealing. Complete with illustrated keys and concise definitions of up-to-date references, “no microscopist or laboratory responsible for pollen identification can afford to be without it”. Echlin’s (12 ) Low Temperature Microscopy and Analysis contains chapters covering the theoretical aspects and problems associated with water and freezing, various methods for preparation of biological samples, detailed procedures and equipment for low-temperature observation, and a thorough coverage of the actual freezing of the sample. The book is also useful for those who require sample preparation by freezing yet carry out studies at ambient temperatures. Of great practical use to those in the field is Free-living Freshwater Protozoa by Patterson and Hedley (13). Excellent line drawings, practical advice on finding and working with protozoa, keys, a useful glossary, index, and bibliography, color photomicrographs-many using flash/phase contrast technique-and a discussion of protozoa communities make the work valuable to amateur and professional alike. The Practical Entomologist by Imes (14 ) lays out the basics for collecting, recording, identifying, and photographing insects. It has many excellent color photographs, with basic keys full of simple, practical, accurate, and well-organized information for the beginner. With the burgeoning advances in instrumentation and equipment available for microscale experimentation, chemists will welcome the second edition of Mayo, Pike, and Butcher’s (15 ) Microscale Organic Laboratory. Coverage includes general rules and laboratory safety, equipment, technique and development of technique, determination of physical properties, preparative organic chemistry (with experiments), and organic compound identification. A companion text Microscale Techniquesfor the Organic Laboratory by Mayo, Pike, Butcher, and Trumper (Id) is written for both beginning and advanced students. Its primary role is “to provide flexibility to the instructor who wishes to introduce a more personalized set of microscale experiments than is possible with the current microscale laboratory texts”. The 13th edition of Materials Handbook: An Encyclopedia for Managers, Technical Professionals, Purchasing and Production Managers, Technicians,Supervisors, and Foremen by Brady and Clauser (17) comes as highly recommended as past editions. It is a must for any practicing microscopist. As always, it contains concise, authoritative information. More 560R
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than 1000 new or improved materials have been added since the last edition, providing very useful data on well over 15 000 materials and substances. Physical Methods of Chemistry;Second Edition; Volume IV: Microscopy by Rossiter and Hamilton (18) is highly endorsed particularly for the modern analytical microscopist as being “as major a contribution for the contemporary analyst as the first edition was for the chemists of the post-World War I1 era”. It contains contributions from leading microscopists. Given major coverage are principles and practice of electron microscopy, scanning systems, diffraction, image contrast, electron microscopy of defects in crystals, special electron techniques, scanning electron microscopy, highresolution imaging of crystalline and amorphous materials, methods of specimen preparation, many methods of practical applications of light microscopy, and methods for the determination of particle size. The volume is considered a companion to Volume V: Determination of Structural Features of Crystalline and Amorphous Solids. Biomedical Photography edited by Vetter (19) fills the need for a contemporary comprehensive text on the subject, containing contributions from 24 leaders in the field. It is encyclopedic in its coverage of the basic principles of optics, exposure and development control, common applications including photographic reproduction of diagnostic images, optical and computer graphic slide production, photomicrography and photomacrography, basic video and editing, specialized applications including UV, IR, and fluorescence imaging, endoscopic, opthalimic, gross specimen, veterinary, and dental photography, and photography of small laboratory objects. It is a must for biomedical photographers and very useful to industrial and general photographers. Standard Methods for the Examination of Water and Wastewater, 18th edition, edited by Greenberg et al. (20) continues the trend of earlier editions of being the foremost comprehensive reference for the water analyst. It is essential to all laboratories involved in water and wastewater analysis and is the standard reference work on the subject. Number 9 in the RMS Handbook series, Qualitative Polarized Light Microscopy edited by Robinson and Bradbury (21), fulfills its aim “to provide a text which tries to explain as simply as possible the principles of an important contrast technique in light microscopy”. The second edition of Uneno, Imamura, and Cheng’s ( 2 2 ) Handbook of Organic Analytical Reagents has been recommended to those who practice microchemistry both for the amount of information it provides and for its potential use to the microscopist. Of particular use to the chemical microscopist is the Reagents Index for Elements listing of the many organic reagents for detection of each element. Rawlin’s (23) Light Microscopy provides a comprehensive introduction for undergraduates in the biological sciences. It is the first volume in the Introduction to Biotechniques published in association with the Biochemical Society and is intended to be a practical guide covering the range of biological imaging methods and their setup and application. It covers the following topics: basic principles; guides for selecting a microscope for a particular specimen; imaging methods including bright-field, dark-field, phase contrast, fluorescence, DIC, and qualitative PLM; 3-D methods including confocal
microscopy; video microscopy and photomicrography; techniques for specimen preparation; specific setup for each instrument, equipment required and the limitations of interpretation of each imaging technique; and case studies demonstrating the information gleaned from using several imaging methods. A training package, Light Microscopy; An Electronic Textbook, by Rawlins (24) complements the print version. Features include the following: a mouse-driven guide to chapters, sections, and pages; ability to “bookmark selected pages”; an index of words that are searchable; visual keys indicating where more information is available and how to access it; and a schematic view of the entire package allowing a diagrammatical view indicating pages selected. It is for IBM or compatible PC with a minimum of Intel 286 processor, at least 640K of RAM (500K free), VGA or Super VGA graphics adapter and monitor. The revised Forensic Geology by Murray and Tedrow (25) provides a survey of the history, methods, and applications of forensic geology. As such, it is written for those professionals, forensic chemists, law enforcement officers, attorneys, geologists, or students unfamiliar with the field of forensic geology and its applications. Replete with detailed drawings, graphs, and qualitative explanations, Introduction to Scanning TunnelingMicroscopy by Chen (26) will appeal to both beginning graduate students and practitioners, even those uncomfortable with mathematical quantum mechanics. It is well referenced, well written, and complete in its coverage of imaging mechanisms and instrumentation. For the first time, a nearly complete representation of the microphotographs of the famous J. B. Dancer has been put together in a first-ratevolume: The Microscopic Photographs o f J . B. Dancer by Bracegirdle and McCormick (27). The atlas contains 265 of the 277 listed titles in the 1873 catalog. Each entry has a photograph of a production slide with an accompanying enlargement of the microphotograph on the slide complete with descriptions, explanations as needed, relevant dates, and biographical information. It has been highly recommended to “any microscopist or photographer interested in the history of their craft”. Volume 4 in Olympus America’s Basics and Beyond Series is Fluorescence Microscopy; The Essentials by Abramowitz (28),who also authored the previous volumes. It serves as a practical introductory text with a well-illustrated discussion on the subject. Heavy Minerals in Colour by Mange and Maurer (29) is a comprehensive manual with excellent photomicrographs that is intended to describe and illustrate the transparent heavy minerals most commonly authigenic in sediments. Complete optical properties, descriptions, and multiple illustrations for 6 1 transparent mineral species accompany a discussion of heavy mineral analysis, laboratory methods, and auxiliary techniques. It includes discussion of factors affecting mineral assemblages and will be a very useful reference for professionals and students. ARTICLESOF GENERAL INTEREST The successful bimonthly Microscopy and Analysis (30), which provides microscopists in the United Kingdom and
Europe with information on new techniques and products, is now available in the United States. The U.S. edition contains many, but not all, of the articles featured in the U.K. edition. Great color photographs, feature articles, and information about references to microscopy and analytical techniques in current literature are found along with new product descriptions. It successfully bridges thegap between formal scientific journals and trade magazines. Microscopy Today (31) is a free newsletter which debuted in 1992 and now has a circulation of over 14 500 in the United States, Canada, and Mexico. It contains a wide variety of articles featuring practical applications and review papers covering all microscopical imaging instrumentation, methods, and associated techniques, including the most basic and advanced. It also is a valuable resource for current industry news and events. A new journal, Acta Microscbpica (32) is a joint venture from The Venezuelan Society for Electron Microscopy and the National Committee for the Investigation in Science and Technology. It features both applied and experimental microscopy from research in materials science, biology, and medicine. Many, but not all, are contributions relevant to electron microscopical imaging and associated technique. The journal’s expressed purpose is “to publish, divulge, and stimulate research activities related with the application of microscopy” and in the “exchange in opinions and experiences between researchers and microscopists of American and other continents”. Volume 1 for 1992 contained 21 contributions in 220 pages-with excellent micrograph reproduction. Most of an issue of Royal Microscopical Society Proceedings (33) is devoted to contributions marking the 100-year anniversary of the publication of what we now call Kohler illumination. Collectively, they not only offer historical insight into Kohler’s era but demonstrate the lasting impact of his method. Evennett (34,35)provided an annotated translation and a simple interpretation of Kohler illumination in a discussion of the essential features of Kohler’s method. The separate effects of the aperture and field diaphragms were outlined and neatly illustrated. Microscopists will gain a greater appreciation of the importance and elegance of Kohlers innovation through Haselmann’s (36)review and explanations of the original work. Included was a discussion of the equipment and light sources available to Kohler in 1893, as well as a practical outline. Bracegirdle (37)surveyed original papers, popular microscopical textbooks, and equipment available in the early 1900sincluding illustrations, descriptions, and instructions, from Beale, Carpenter, Hogg, Spitta, and other classic references. Finally, the role of Kohler illumination in modern light microscopy was summarized by Gundlach (38). Bracegirdle (39) provided an historical insight into the Manchester firm of microscopists Flatters and Garnett, Ltd., once the largest producer of permanent slide preparations in the world. Brook (40) lauded amateur light microscopists and the importance of their useful contributions to science. A brief historical development of the professional microscopist was outlined, along with suggested research topics for the amateur. Bradbury (41) surveyed the impact that the use of microcomputers has had on light microscopy, both for control Analytcal Chemistty, Vol. 66, No. 12, June 15, 1994
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of the instrumentation and in the processing and analysis of the resultant images. The construction and use of F. J. Chesire’s and M. A. Ainslie’s apertometers were laid out by Martin ( 4 2 ) . Further discussion on original design features and continued use of apertometers was provided by Sanderson ( 4 3 ) . He (44) also presented details for the simple construction of a modern Abbe test plate for the evaluation of the degree of aberration present in an optical system. Of particular interest to light microscopists is Hartley’s ( 4 5 ) historical account of the evolution of the substage condenser and diaphragm. Turner (46)provided an historical account of the invention of the iris diaphragm. A fascinating new look at old slide mounts was offered by Bracegirdle ( 4 7 ) . Presented biological slide mounts, some well over 100 years old, were examined using modern techniques such as phase contrast, crossed polars, and Nomarski DIC, each which illustrated that much more detail was preserved by then in vogue preparation methods than had been visualized before. Evans (48)explored the cause of dewing of the inner surface of cover glasses of dry mounts. The cause and means to prevent the moisture build up were discussed. Watt (49) reviewed the unique features and uses of the portable McArthur microscope, a simple videoscope, a telemicroscope based on Maksutov Cassegrain Catadioptic optics, and the Infinivar zoom videoscope. Noble (50) provided an introduction to the basics of producing video images in light microscopy, reviewing cameras, monitors, printers, and new developments in video techniques. Fox and Hart (51) illustrated and discussed microscopy in the study of common plant pathogens. They stress thevaluable role of the unorthodox amateur as well as the professional in making important contributions to the understanding of plant diseases. Complete, detailed, and practical preparation techniques for single, double, and triple staining of plant chromosomes were laid out and illustrated by Brocklehurst ( 5 2 ) . Material scientists will enjoy Goodhew’s ( 5 3 ) account of the techniques and applicability of instrumentation available to the hyleographer today. In a discussion lauding classic microscopes from the 19th century, Cook (54) provided a captivating historical and working description of his favorite four: the Watson Service I and I1 models, Zeiss Universal I, Reichert Zetopan, and Reichert MeF. 1. LaRue (55) illustrated and described three Powell dissecting microscopes. Original trade catalogue references were included. Ford (56) reviewed Robert Brown’s 1927 publication and recreated his observations on Clarkia pollen with modern videomicrographs using Brown’s original microscope. He proved, once again, that what is now simply called Brownian motion (or movement) was “unmistakably discernable to Brown”. Martin (57)confirmed Ford’s assertion that Robert Brown most certainly observed the motion that bears his name yet produced evidence that three others-Jan Ingenhousz in 1784, James Drummond in 1815, and John Bywater in 18 19-may also have independently observed “Brownian motion”. 582R
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Marentette and Brown (58) describe their use of polymer spherulite PLM photomicrographs for classroom instruction of polymer theory and the concept of birefringence. Pins (59)put forth a suggested list of books for the amateur as well as the professional microscopist. Delly (60) provided a timely illustrated review of “microscopes for kids”, including an evaluation of toy microscopes and why images produced from them are so poor. Descriptions and recommendations for affordable microscopes more suitable for student use were given. As such, it would be invaluable for use in the recent microscopical education programs launched by the Royal Microscopical Society and the Microscopical Society of America. A simple convenient microwave technique for flattening insect mounts was given by Brocklehurst ( 6 1 ) . Schulman’s system of stereoscopic microscopy, through the introduction of Polaroid material suitably oriented in the lower focal plane of the substage condenser and ocular exit pupil, was reviewed by Martin ( 6 2 ) . He introduced a variation using effective circular polarizing filters suitably oriented in similar locations. Extinction at the exit pupil is adequate, with less regard for filter orientation. Root (63)suggested an infinite, transitory, K-universal H. T mobius strip for identifying Kohler illumination CKSs. The full proceedings of the 13th International Congress of X-ray Optics and Microanalysis was edited by Kenway et al. (64). Abstracts from the RMS Micro 92 can be found in the RMS Proceedings ( 6 5 ) . The 107 papers from leaders in the field cover a wide variety of microscopical imaging methods, sample preparation technique, image analysis, and practical applications. McCrone (66) reviewed and evaluated the CD-ROM version of the monumental reference work, The Particle Atlas, now available as The Particle Atlas Electronic Edition. It is having a profound effect on how microscopists retrieve data. The appearance of the photomicrographs is superior to the print version, and the ease and speed with which one can cross-reference text and data make this an invaluable resource. Cooke (67) provided a review (697 references) of noteworthy articles on microscopy that were published from December 1989 to December 1991. The review is subdivided into general categories: books and articles of general interest; optics and instrumentation; microscopical methods; techniques for specimen preparation; techniques for specimen examination; applications of microscopy. The proceedings of INTER/MICRO-92 and INTER/ MICRO-93 are found in The Microscope, refs 68 and 69, respectively. The proceedings (68, 69) feature 1 13 presentations from the conferences with annotations by McCrone. Featured were applications of polarized light microscopy, FTIR, SEM, TEM, SAED, forensic microscopy, authentication technique involving pigment, media, and other materials in art and archeology, and recent developments in asbestos analysis. The career of the late Vernon Ellis Cosslett, principal founder of ICXOM Congresses and a pioneer in electron optics, was traced by Mulvey ( 7 0 ) . The preparation of a modified Van Gieson Stain was described by Bird et al. ( 7 1 ) .
A description of the Society of Arts’ pattern microscopy stand was given by Martin ( 7 2 ) . Stoney ( 7 3 ) provided a copy of the original transcript testimony of John Quekett in “The Torbanehill Case” surrounding the microscopical classification of cannel coals, boghead coals, and torbanite. A new society ( 7 4 ) , The Microscope Historical Society, was founded for the exchange of information about equipment and methods related to traditional light microscopy and its history.
A. OPTICS The practical benefits of Kohler illumination in electron optics was outlined by Kermeen and Probst ( A I ) in an introduction of the Zeiss EM 910. A cuprous bromide vapor laser was used by Xiao et al. (A2, A 3 ) as a brightness amplifier in an active projection microscope and high-speed photomicrography system. Linear amplification of more than 500 and resolution near the objective’s diffraction limit was reported. Goldstein ( A 4 ) used computer simulation of light microscopical imaging to obtain resolution criterion for line and grating objects. Various image methods were tested. A simple method of achieving evanescent-wave illumination was described by Murray and Eshel (4.The technique uses standard optical microscope components and produces circularly symmetric illumination; specimen images were produced by both light scattering and fluorescence. Van Hulst and Seyerink (Ab) illustrated the advantages of a movement from development toward practical application of scanning near-field optical microscopy. Recent advances from evanescent field optical imaging demonstrated subwavelength resolution. Buczek ( A 7 ) reviewed (35 references) optical components including a discussion of polarizers, prisms, mirrors, gratings, lenses, and other various optical materials. Kobayashi (A8) reviewed (46 references) techniques to generate ultrashort light pulses with mode-locking lasers. Lehman and Wachtel ( A 9 ) described a simple method to measure the numerical aperture of light microscope objectives using the exit angle of the rear lens toward image space and the objective magnification. The method is independent of instrumentation-like apertometers. The nonlinear behavior of circularly polarized laser beams propagating through sodium vapor was explored by Roehricht et al. (A10). See also: References 1, 33-38,42-46, 56, 57,60,62, D4, D6, D9, E5, E8, E14, E15,E18, E19, E21, E26, F7, G1, G2, G4, G5, G7, G10, G13, 52, 56, 59, J15, 518, 523, 524, 531, K2,K4, K7,K10, K16,K17, K19, K25,K36,K37, K38-K43, K47, K49, L5, L6, L8, L29, L135, M8, R5, R17, R18, 116, and LL3. 6. INSTRUMENTS Laroye and Taylor ( B I ) described a simple acoustic device that attaches to the fine adjustment vernier of a light microscope and alerts the user of thevertical distances traveled by the microscope stage. The monitor may have applications as a practical stereological dissector or as an unbiased brick in confocal microscopy.
An apparatus for locally marking specimen slides was patented by Feldman (B2). A moveable aiming device permits marking of slides precoated with material such as electrosensitive compounds containing solvents, binders, unstable acids, and pH indicators by providing a localized physical effect. Hirano et al. (B3) developed a new type microscope video system combined with a fiber-optic plate processed in the shape of a needle. The plate has thousands of optical fibers 3 pm in diameter, permitting viewing of single cells. Images are transmitted through an objective to a video system and digitized. Fluorescence images of cultured cells were analyzed. Brad1 et al. (B4) devised a tilting device and technique permitting transmitted light microscopical 3-D imaging of human lymphocyte cell nuclei. Optical sections wereobtained from a series using a computer-controlled stepping motor for z-axis movement and a device capable of turning the sample through any desired angle and x , y movement. Optical transfer reconstruction problems were minimized by acquiring different views of the same cell nuclei. A new 360’ single-axis tilt stage for high-voltage electron microscopy was described by Barnard et al. (B5). With the addition of a combined laser microbeam and optical trap, Greulich and Weber (B6) converted a light microscope into a preparative instrument, allowing micromanipulation of a variety of microscopic objects without any mechanical contact. Zuev et al. (B7)developed a vacuum-chamber device that connects to a laser microscope and mass spectrometer which was used for local determination of gas-forming impurities in solids. A small ring-shaped vacuumchamber was built by Putnam et al. (BB) and connected to the piezoelectric tube used for scanning in an atomic force microscope. A 50-L beer container serves as a buffer between the vacuum pump and chamber. Samples up to 50 mm in diameter can be attached to the piezoelectric tube. Washington (B9) described an improved light scattering device for particle size measurement ranging from 0.2 to 2.3 pm, which eliminates the background signal from out-of-focus particles. Lanni (BIO) combined piezoelectric elements and a capacitance gauge in a closed-loop system that maintains a constant plane of focus for light microscopical viewing of samples independent of thermal expansion and drift. Two novel, coherent and noncoherent, imaging, superresolving scanning microscopes were described by Walker et al. ( B I I ) . The coherent optics, similar to that in scanning confocal imaging, has a detector pinhole replaced by a special holographic mask, a Fourier lens, and a pinhole. Two intensitytransmittance masks, two integrating detectors, and an electronic subtractor are used in the incoherent system. The arrangements obviate the need for an array of detectors to produce singular-system processing, and direct phase measurement is no longer required when coherent imaging is used. Lee et al. (BIZ)presented data demonstrating the capabilities of a new Personal SEM designed for use by both novice and professional. The SEM requires no chilled water, compressed air, or special utilities, operating instead on 115-V ac, 15-Aservice. It displays macro, normal, and zoom images together with X-ray data, operating parameters, and sample Analytical Chemisrry, Vol. 66,No. 12, June 15, 1994
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notes. Acceleratingvoltageis 2,5,10,15, and20 kV. Polished concrete thin sections were characterized. Abramowitz (BJ3) described the new Olympus B-max modular series of microscopes. The December 1993 issue of Advanced Imaging ( B I 4 ) contains an extensive resource of imaging firms and their products and services. Listed under Image Acquisition are cameras, chip technology, fiber-optic, image intensifiers, lenses, lighting, scanners, 3-D digitizers, vidicons, and viewing devices. Listed under Image Processing Hardware are chip technology, complete systems, frame grabbers, image compression, memory expansion, and processors/boards. Listed under General Image Processing Software are for MacIntosh and for PC/ P52. Listed under Image Display are display control, flat panel, generators, monitors, test and measurement, and video conversion. Listed under Image Hard Copy are film recorders, hard copy control, hard copy media, and printers. Listed under Image Storage are magnetic storage and optical storage. Listed under Image Communication is communication systems. See also: References 1,39,49,54,55,60, D2, D4, D6, D9, E8,E15, E24,G7, K5,K16,K17, K19, K26, K28,L1, L31, R2, R6, R7, X7, AA20, FF3, FF4, FF15, LL10, and “4. C. POLARIZED LIGHT MICROSCOPY A scanning fiber-optic polarized light microscope was designed by Giniunas et al. (CI).Anisotropy of specimens was determined by directing reflected light into a birefringent optical fiber, adjusting the phase delay between the polarization modes, and measuring the interference signal. Monovoukas and Gast (C2)observed the morphology and orientation of colloidal crystals grown in thin capillary cells through polarized light microscopy. The Jones calculus was employed to predict color and intensity when viewed between crossed polars. A summary of the effect of crystal orientation on both diffraction wavelength and intensity was provided by construction of theoretical conoscopic images. An automated spindle stage for crystal orientation on a polarized light microscope was developed by Besancon (C3). Rapid and precise measurements of extinction positions were accomplished through the use of a stepper motor and the measurement of light intensity at each step. Ho and Lawrence (C4)used a polarized light microscopical technique for detection of small birefringences in ordered arrays of biological material. Embryonic development of Drosophilla and Daphnia were followed by observation between crossed polars with a suitably placed 560-nm compensator which produced high-contrast, high-resolution color images. Color and intensity were correlated to structure and phase ordering. Practicing optical crystallographers will appreciate Bryant’s (C5) investigation of factors affecting the precision of conoscopic measurements of optic axial angles. Bryant (C6) also demonstrated the practical use of polarized light microscopical technique in thorough optical characterization of crystalline organic compounds containing olefinic linkages and correlated those properties to conjugated unsaturation; p-terphenyl, 6-6 diphenylfulvene, 1,Cdiphenyl- 1,3-butadiene, a-truxene (ex nitrobenzene), 1,5-dipheny1-3-pentadienone, 1,3564R
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diphenyl- 1,3-propanedione, and trans-cinnamic acid were characterized. McCrone (C7)reviewed particle identification through the primary use of polarized light microscopy and associated techniques. The use of polarized light microscopy for identifying crystals at Westinghouse Hanford Site nuclear waste was described and detailed by Herting (C8). Delly (C9) penned a chapter entitled “Light Microscopy” in Encyclopedia of Materials Characterization, edited by Brundle, Evans, and Wilson. A new model of dispersion staining (focal masking) objective lens was developed by Uno (CIO).The lens is mounted on a polarized light microscope equipped with a headon type microphotometer and hot stage. Asbestos minerals were analyzed. Eser et al. (CII)characterized the solid deposits from the thermal stressing of jet fuels and related compounds using polarized light microscopy. Both liquid- and gas-phase reaction products were studied. Fractures in composite material were characterized by Choi and Takahashi (CI 2) using polarized light microscopical methods which revealed more about prefracture than surface analysis alone. See also: References 1,21,49,65,66,68,69, T2, Y 1, Y2, Y4,Y5,Y6,Y7,YlO,Y12,Y13,Y15, Z l , Z 4 , Z7,Z9, 217, Z19, AA7, AA14, AA20, AA22, EE1, EE3, EE4, EE6, EE7, EE13,EE17,EE19,FF3, FF4, FF6,FF8,FF10, FFll,FF13, FF15, GG7, HH2, 552, 554, JJ10, JJ11, 5521, KK1, KK3, LL17, LL18, MM1, ”1, PPI, PP5, PP8. D. MICROPHOTOMETRY AND MICROSPECTROPHOTOMETRY Katon and Sommer (DI)reviewed (24 references) present developments in and the future of IR microspectroscopy in light of its growing routine use within the analytical community. A scanning photoelectron spectrometer microscope based on focused coherent vacuum radiation was developed by Manakata and Kasuya ( D 2 ) . Spatial resolution was provided by focusing the V-UV light to its diffraction limit. A highefficiency time-of-flight energy analyzer generated the photoelectron energy. The microscope allows for detailed inspection of electronic structure, making it suitable for a spatially resolved study of adsorbed phases. Cooper et al. (D3) utilized IR microspectroscopical data to complement electron-probe microanalysis in investigations of natural corrosion on potash glasses. A microspectroscopical accessory using a symmetrical pair of identical parabolic mirrors was patented by Messerschmidt (04)for simultaneous measuring and observation. Identical symmetrical aberration canceling optics allowed multiplexing between and among different functions without any need for a significant loss of through-put efficiency. Jacobsen (D5)described a method for producing and correlating confocal scanning light images simultaneously with spectroscopical data. An IR microscope spectrometer was patented by Yamaguchi et al. (06)that has a collector for focusing the IR beams and a device for imaging the sample on the input surface of
the system. An operating mechanism moves the devices relative to each other and vertical to the center line, where attenuated total reflection analysis can be performed. Gardette (07) assessed the oxidative photochemical degradation of PVC under accelerated conditions in FT-IR microspectrophotometric analysis of polymer aging. Shala (08)focused on specific applications where FT-IR microspectroscopy was helpful in providing chemical fingerprints of materials and contaminants in a cleanroom FAB. A new acoustooptic light source, whose chromaticity coordinates can be changed arbitrarily based on a CIE 1991 chromaticity diagram, was developed by Cai et al. (09). Lin (D10)reports making accurate measurements of Si02 on polysilicon and thin Si02 on aluminum using a UV microspectrophotometer with a measuring spot size less than 10 pm. Blair and Ward (011 ) described an IR microprofiling technique using IR microspectroscopy with precise stage movements. A data reduction program allowed 3-D projections providing spatial information. A method of coding spectra from different pixel elements provided higher quality spectra without an increase in acquisition time. Reffner (012)traced the commercial development of FTIR microspectroscopy, noting historical improvements that have moved it from infancy into the viable analytical instrument it is today. FT-IR microspectroscopy was applied by Wu and Nakayama (013) to evaluate the microscopic orientation of extrusion-molded sheets of thermotropic liquid crystal polymers. Polarized IR spectra were measured down to a 40-pm area using a redundantly apertured I R microscope equipped with a wire-grid polarizer. Silicone fragments in human breast tissue were examined by Centeno and Johnson (014)using FT-IR microspectrometry. The vinyl ester resin around a silane-finished glass fiber was measured by Ikuta et al. (015)using a micro-FT-IR spectrometer. Cross et al. (016)described a technique for large-area X-ray microfluorescence imaging. Two-dimensional X-ray intensity maps over 5-50 mm were collected from a rock thin section and a synthetic multiphase alloy using an individual analytical area of 100 X 150 pm. See also: References E9, E20,Z1, BB7, BB8, CC2, CC7, EE2, 551, 552, 553, 555, 557, 558, 5517, 5520, 5523, KK4, KK5, KK7,KK10, KK12, KK13,KK14, LL13,LL19, MM2, QQL QQ3, and QQ4.
E. IR, UV, AND RAMAN MICROSCOPY Day and Young ( E l ) reviewed and discussed the progress made in the use of Raman microscopy for the examination of the structure and micromechanics of inorganic and polymer films. The potential of Raman microscopy for the examination of phase structure and composition of polymer blends was discussed by Garton et al. ( E 2 ) . Common heating problems with thin specimens were reduced by use of a low-power laser together with CCD camera and efficient collection optics. An intermediate slit permitted confocal operation when in the
spectoscopic mode. Means for examining thick specimens, highly scattering specimens, and large and small phases were explained. Grosse et al. (E3) reviewed applications of IR microscopy and the ability to take spectra from small sample spots when studying layer thickness variations in semiconductor systems and scattering characteristics of small particles. Pitt and Hayward ( E 4 )described a new, fast, and compact Raman microscope capable of showing molecular orientation, stress and strain, and defects and transformations in composite materials and polymers. Everall (E5) provided simple means for enhancing the sensitivity of a commercial Raman microprobe through the useof a holographic rejection filter. The filter allowed shorter data accumulation time or a reduction of the laser intensity at the sample. Two vastly different samples tested the efficiency of the filter: Ti02 powder gave a strong, diffusely scattered laser beam; silicon gave a strong specular reflection. Boogh et al. (E6)presented a Raman microscopical study of stress transfer in high-performance epoxy composites reinforced with polyethylene fibers. Ivanda and Furic (E7)introduced a cylindrical lens in a micro-Raman system to achieve line-focus microprobing. The lateral spatial resolution of Raman scattering was equivalent to point-focus spatial resolution. The line focusing enabled measurements with a laser power density 320 times lower than point focusing and had better signal-to-noise ratio with equal laser power. Morris et al. ( E 8 ) described the Hadamard multiplexed Raman imaging microscope and illustrated techniques for contrast enhancement, multispectral imaging, and optical sectioning by nearest-neighbor deblurring. A specially made FT-IR microscope-IR reflection absorption microspectroscope was used by Nakao et al. (E9) for the in situ detection of local and microscopic contaminants on magnetic disks and heads. The reflection absorption measurements enhanced the micro-FT-IR measurements in the detection of adsorbed species whose vibrational mode was perpendicular to the surface. Marcott et al. (EIO)developed a near-IR microscope technique for obtaining qualitative and quantitative aqueous surfactant phase diagram information from a single sample preparation. Gal and Toth (E1 1 ) demonstrated techniques to characterize multilayer films by FT-IR microscopy and IR microspectroscopy with computerized spectra manipulation techniques. Each layer produced discrete spectra. The state of dispersion of transparent noncompatible polymer blends was determined by Saito and Matuoka (E12) through irradiating polymer films with IR at a wave band having the greatest difference in absorbance between 1400 and 2400 cm-I and then photographing with an IR camera. Booker et al. (E13) reviewed (21 references) the development of the scanning IR microscope and its application to bulk silicon and gallium arsenide analyses. The design and development of a highly sensitive near-IR laser Raman system was offered by Mason et al. (E14). A conventional spectograph with CCD detector and optics optimized for the 700-1000-nm spectral range was used with Analytical Chemistry, Vol. 66, No. 12, June 15, 1994
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a tunable titanium sapphire laser source. A comparison of data with that from an FT-Raman system was given. Vess and Angel ( E l 5 ) described a portable, near-visible Raman instrument which is capable of measuring spectra simultaneously from 10 separate fiber-optic probes. Carlson and Bliss (E16)discussed an experimental approach to the determination of the absorption coefficient and the net-free carrier distribution in n-type/indium phosphate using near-IR microscopy. The two demonstrated the analysis of segregation in LEK grown crystals. Results from the polarized FT-IR microscopy of structural analysis of adsorbates in molecular sieves, by Schueth ( E l 7 ) , illustrate its potential. Silicate I single crystals fully loaded withp-xylene showed an ordered adsorbate for the first time. Determination of the orientation of the p-xylene molecules relative to the host structure was done through analysis of the polarized absorption bands. Dai et al. (E18)designed an all-silica fiber-optic probe. The fused fibers within a silica tube have been used for obtaining spectra at ambient temperatures and from various molten salt systems at temperatures up to 720 "C. The application of factor analysis to FT-IR microscopical data was put forth by Donahueet al. (E19). Thecombination of IR data collection and analysis by chemometrics methods increased the content of the data set, providing quantitative information and pure principal-component spectra while reducing the data set and improving the overall signal-tonoise ratio of compositional maps. Sommer and Katon (E20) improved an existing Fourier transform Raman microprobe by optimizing laser-input optics to the microscope and the optics coupling the microscope to the spectrometer as well as optimizing the spectrometer for near-IR use. The two demonstrated improvements in spatial resolution, Raleigh rejection, and increased sensitivity to weak Raman scattering materials with moderate excitation powers. Single crystal data and the results from holographic notch filter use are included. Esaki et al. (E21) developed and described a unique attenuated reflection prism, made from zinc selenide, for use with a conventional IR microscope. The ATR system is capable of point, line, and area analyses allowing local analysis of surfaces such as polymers and polymer composites. Windig and Market (E22) described a simple-to-use, interactive, self-modeling mixture analysis of FT-IR microscopy data for polymer laminates. Micro FT-IR reflection/absorption spectra of epoxy adhesive films on chemically treated aluminum was collected by Fondeur and Koenig (E23). Clark (E24) reviewed the applications and instrumental designs of FT-IR microscopy. Ottenroth ( E D ) provided a review on FT-IR microscopy and its applications. Reffner et al. (E26) extended grazing angle microscopy to microscopic sampling areas through the use of an FT-IR microscope with a special objective lens. A variety of applications were given. A combined IR and electron microscope study of interplanetary dust particles was done by Bradley et al. (E27). Chemical information from FT-IR microscopy was used by Murphy and Alvin (E28) with other imaging methods to 568R
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characterize fiber wall development in immature culms of the bamboo Phyllostachys virideglaucescens. See also: References D3, D6, D8, D10, D13, F7, G8, J10, 520, K24, K34, K35, L43, N7, R16, T1, Z10, 216, AA3, AAS, AA18, AA22, AA26, AA27, BB8, CC7, EE8, EE9, FF9,GG9, JJl,JJ2,JJ3, JJ5,JJ8,JJ20, KK5, KK7, KK14, LL10, MM2, PP8, QQl, QQ3, QQ4, QQS,and QQ6. F. FLUORESCENCE MICROSCOPY A fluorescence microscope was developed by Morgan et al. (FI)that allows contrast on the basis of fluorescence decay time. A radio frequency-modulated intensified CCD camera and a single-photon detector with external photon correlator were alternately used as detectors. Minuechi et al. (F2) devised a microscopical CCD video camera system with an image analyzer to examine the manner in which light penetrates and induces fluorescence associated with photosynthesis in an intact leaf in relation to its morphology. The distribution of laser-induced fluorescence (Ar 477 and 488 nm) was examined. A simple method for thecalibration of particle fluorescence measurements was tested by Recktenwald et al. (F3). Solid glass beads are immersed in a known concentration of dye solution. Both the drop in fluorescence intensity and dye volume displacement are measured and correlated. Once calibrated, the absolute fluorophore quantity can be determined from other fluorescence measurements. The method can also be used to measure a CCD camera's sensitivity. The first results obtained with a new combined atomic force microscope integrated with a standard Zeiss optical fluorescence microscope were presented by Putman et al. (F4). The combined microscopy allows direct comparison between both imaging methods. Fluorescence images of cracks in polymerized Langmuir-Blodgett films of 10,12-pentacosadiynoic acid were revealed to run parallel to one of the crystal lattice directions by AFM imaging. Stine and Knobler (F5)reviewed (73 references) fluorescence microscopy including basic instrumentation, resolution considerations, and confocal scanning techniques. A variety of applications are discussed on the growing use of fluorescence imaging beyond biology to include investigations of physical and chemical phenomena. Results from Langmuir monolayers studies are described. New and existing techniques for fluorescence lifetime imaging microscopy were explored by Wang et al. (F6).The instrumentation, theory, and concept were reviewed (104 references). Implementation with conventional and confocal systems was presented with numerous applications for making quantitative measurements in the biomedical, biological, physical, and environmental sciences. Modifications to a confocal laser scanning microscope by Bliton et al. (F7) allowed simultaneous fluorescence imaging of living specimens excited by UV- and visible-wavelength light. Modifications included the introduction of UV-pathspecific lenses which could be adjusted to correct for varying amounts of longitudinal chromatic aberration in commercial available objectives and specially designed UV transmitting ocular and tube lenses chromatically corrected for UV through visible wavelengths which minimized lateral chromatic errors.
Noonberg et al. (F8)minimized cellular autofluorescence in oligonucleotide uptake studies by adjusting laser scanning rates and aperture settings, modulating excitatory wavelengths, and controlling pH buffering environments. The utility of fluorescence microscopy for monitoring the developmental stages of fern sporangia was investigated by Singh and Devi (F9). Changes in the chemical composition of the cell walls were traced by following changes in autofluorescence. The dynamics of polymers in dilute solutions was studied by Matsumoto et al. (FZO)via direct observation of Brownian motions of DAPI-probed DNA. Leaback (FI 1 )outlined a few principles relevant to current practices in quantitative light microscopy’s increased dynamic range and sensitivity. Fluorescent and chemiluminescent measurements were considered. The use of two intracellular dyes for epifluorescent video imaging in observing cell surface iterations was evaluated by McClung and Feuerstein (FI2).The method permits exposure to light up to 30 min in the determination of cell adhesion, detachment, and movement at the surfaces of biomaterials. Rodgers and Glaser (F13)reviewed (50 references) the use of fluorescence digital-imaging microscopy of membrane domains. Spatial variations of fluorescence lifetimes in single cells served as a source of image contrast in a fluorescence microscopical method developed by Oida et al. (F14)to study endosome fusion in single cells. Several time-resolved fluorescence images of a sample are obtained at various delay times after pulsed laser excitation. The images are analyzed pixel by pixel, and the spatial variations of the calculated lifetimes are displayed in pseudocolor format. The extent of resonance energy transfer can be visualized in single living cells free from corrections necessary in fluorescence ratio imaging and steady-state microfluorometry. Hirayama (F15)provided a review (92 references) of timeresolved fluorescence microscopy including the principles of fluorescence decay, applications and methodology, and recent applications. Ryon and Warburton (FZ6)discussed the design of a scanning fluorescencemicroscope with X-ray optics in an effort to scan with resolution in the 1 to 10pm range using standard laboratory X-ray tubes. See also: References 28, G2, H6, 57, 518, 519, 524,527, 529, 531, 533, K17, Q l l , R17, R19, X5, Y14, 28, AA15, AA17, AA26, BB6, BB11, CC2, CC6, FF5, FF15, KK6, KK11, KK15, LL8, LL10, LL12, LL15, LL16, LL20, LL22, LL23, LL24, LL26, LL27, LL3 1, LL36, LL39, LL45, LL46, LL47, LL48, and LL49.
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G. LASER AND HOLOGRAPHIC MICROSCOPY A microscope illumination system was constructed by Yamamoto and Ueno ( G I ) that utilized fiber optics for light transmission and a newly developed, more efficient flash tube as the light source. A new design of a fiber-optic laser scanning microscope was developed by Ghiggino et al. (G2).The optical fiber served as the confocal pinhole and as the light path for both excitation and return beams. The instrument is adaptable to
many uses and offers the capability of imaging reflective as well as fluorescent objects. Full-color video images and stereo pairs from a confocal reflection microscope were produced by Cogswell et al. (G3). Three lasers (HeNe 633 nm; NdYAG 532 nm; HeCd 442 nm) and photomultiplier detectors were incorporated into the on-axis scanning system. Multistained fixed tissue was imaged as well as natural pigments in plant specimens. A holographic microscope for phase imaging was described by Brody et al. (G4). A temporary hologram recorded in real time is used, providing phase-conjugate illumination allowing phase contrast in phase objects, creation of contrast only in moving elements, and elimination of phase background due to embedding medium or absorbing objects. The application of circular and annular lens apertures for laser scanning microscopy was compared by Kempe et al. (GS).Spatial and temporal resolution limits in time-resolved imaging were investigated using Fourier optics. The dynamics of laser ablation transfer imaging were studied by Lee et al. (G6)using an optical microscope with picosecond time resolution. A laser microscope based on time- and space-resolved transient reflecting grating was desribed by Harata and Sawada (G7), and a laser-stimulated scattering method developed for the nondestructive investigation of materials surface modification. Biomedical and biological applications of UV lasers in confocal microscopy were presented by Cannon and Armas
(G8). Imaging microscopy with short-pulse X-ray lasers was described by Da Silva et al. (G9). The system offered highresolution 3-D images of biopolymers in an aqueous environment without blurring effects associated with natural motion and radiation-induced chemical decomposition. Applications and limitations of experimental instrumentation that make use of mode-locked lasers with scanning laser microscopes for ultrafast imaging were discussed by Bergner et al. (GZO). Illustrations for time-resolved studies in semiconductor physics and biology are included. Confocal scanning laser fluorescence microscopy was utilized by Van Blaaderen et al. (GI1 ) as a novel and versatile instrument in 3-D imaging of submicrometer colloidal particles in concentrated suspensions. MacGowan (GI2)reviewed (46 references) X-ray laser development as sources for X-ray microscopy in an effort to produce a more affordable, accessible, and compact laser Pump. See also: References A8, B6, B7, E5, E20, F2, F8, 511, 512,513, 519,526,527, 530,531, J33,K12, K24,K32,K35, K45, L4, L18, L20, L34, L40, M1, V2, X7, Y3, Z8, AA4, AA19, AA22, BB1, BB2, BB10, DD2, EE4, EE10, EE15, G G l , I I l , 116, LL1, LL6, LL29, LL30, LL32, LL33, LL34, LL35, and MM3. H. INTERFERENCE MICROSCOPY A new fringe-scanningmicroscopewas developed by Matsui and Kawata (HZ) that is based on coherence probe microscopy. An interference image is collected at various stage heights using a white-light, double-beam interferometer with either a Mirav or Michelson objective lens. Surface profiles are Analytical Chemistry, Vol. 66,No. 72, June 15, 1994
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reconstructed by tracing the darkest point of a white light interferogram for each pixel. The amplitude and phase reflectivity of spectrum are calculated pixel by pixel through Fourier transformation of a local interferogram, or crosscorrelation with referenced ones. The measurement of weak repulsive and frictional colloidal forces of microscopical spheres in liquid suspension were traced by Raedler and Sackmann ( H 2 ) with real-time image processing of reflection interference contrast images. Temporal fluctuations of sphere-to-substrate distance were determined from interference fringe pattern changes. Shape and distance of the interaction potential were obtained by analyzing the distribution of distances in terms of a Boltzmann distribution. The two (H3) also used the method to map the optical density of phospholipid vesicles and supported bilayers, to image the contact profile of the vesicles at surfaces, and to report ( H 4 ) on the DMPC vesicle substrate interaction with a supported DMPC bilayer. Tentori (H5)discussed the accuracy of a hologram interferometric method of measuring the refractive index of an optical glass in the form of a wedge. The technique can be applied to liquid or solid refractive index measurement. Foskett ( H 6 ) reviewed (39 references) simultaneous differential interference contrast and quantitative low-light fluorescence video imaging of cell function; the technique is applicable in correlating fluorescence intensity from any probe with specific cell structure. Direct viscoelastic strain relaxation measurements of polymer coatings on steel were obtained by Kyed and Matlock ( H 7 ) through a process involving interference microscopy, microhardness indentations, and annealing. See also: References J l l , K19, K32, X1, BB12, DD2, GG8, LL9, and LL21.
I.PHASE CONTRAST AND SCHLIEREN MICROSCOPY A technique for separating the phase distribution from the image of a semitransparent sample observed with phase contrast optics was proposed by Noda and Kawata (Zl); brightfield, and positive- and negative-phase contrast images from the same field, were each analyzed and the phase refractive index distribution was qualitatively reconstructed by solving a set of linear equations for each pixel of the sample image. See also: References G4, X5, BB5, and LL12. J. CONFOCAL MICROSCOPY A new technique was described by Lange et al. ( J l ) that exploits confocal imaging in the analysis of surface roughness. Optical sections are transformed into digital images and a topographic map. A straightforward algorithm is used to derive roughness parameters as well as the texture of the surface. Young et al. ( J 2 ) demonstrated superresolution in coherent confocal scanning images through the use of a special optical mask calculated using the theory of singular systems. The mask, Fourier lens, and detector pinhole carry out optical processing of the image. An introductory discussion on the fundamentals of optical sectioning using deconvolution techniques or confocal imaging was put forth by Entwistle ( J 3 ) . Applications were outlined 568R
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and direct means for improving image quality were given. Also included were suggested topics for inclusion in a formal introductory course in optical sectioning. A confocal-line technique, based on the introduction of line-shaped illumination and linear image detection, was desribed by Benedetti et al. (J4) as an alternative to the confocal point approach. A prototype confocal-line microscope was constructed and tested. The effects that pinhole size, detector type, imaging algorithms, and other system parameters have on the imaging performance of confocal microscopy were laid out by Sheppard et al. (J5). The interference axial response in a confocal scanning system consisting of either finite-sized pinhole detectors or optical fibers was measured by Gu and Sheppard (J6). The fringe visibility is degraded when using larger pinhole size and is unity when using optical fibers, even for finite values of the fiber spot size. Can and Sheppard ( J 7 ) introduced a new criteriondetectability for evaluating the performance of confocal microscopes in fluorescence imaging. The significance of 3-D transfer functions in confocal scanning imaging, and its role in deriving 2-D and 1-Dtransfer functions for in-focus and on-axis imaging, was detailed by Sheppard and Gu ( J 8 ) . Optimum recording conditions in scanning microscopes, such as scan velocity and response time, were considered by Damm and Wilhelm (J9) in an attempt to minimize distortion and noise influence. The confocal laser scanning microscope served Bossman et al. ( J I O ) as the fundamental building block of a failure analysis workstation; the microscope was easily equipped for emission, OBIC, and IR microscopy, providing several nondestructive analyses quickly with minimum preparation. Improvements for contrast enhancement and depth perception in 3-D representations of DIC and confocal scanning laser images were put forth by Schormann and Jovin ( J 1 2 ) . Images are enhanced prior to reconstruction, thereby increasing the number of usable optical sections. A gray-level probability density function and local statistics were incorporated for a new contrast enhancement transformation. A new scanning microscope, proposed and described by Sasaki et al, ( J I 2 ) for imaging a 3-D absorption structure, is based on a confocal system with excitation- and absorptionmonitoring lasers. A tutorial review (26 references) covering applications of confocal laser scanning microscopy for detailed study of noninvasive mapping on targeted systems was offered by Moss et al. (513). Specific problems demonstrating the wide-ranging potential of the technique included successful tracing of the effect of processing on dye penetration in fibers, mapping the interdependence and growth patterns in bacterial colonies, and noninvasive examination of epidermal tissue layers. Two computer-assisted procedures for realignment of light micrograph images from serial sections were developed by Rydmark et al. (J24). Several hundred consecutive sections of cat cerebral cortex were realigned using interactive and automatic methods. New data inversion formulas that allow for object reconstruction at a given point and make use of diffraction images
at other scanned positions were presented by De Mol and Defrise (J15). Van Blaaderen (J16) reviewed (1 3 references) theconfocal scanning light imaging of individual particles in concentrated colloidal dispersions and the advantages provided by specially prepared fluorescent silica particles. The performance of a confocal scanning system was compared with that of a conventional stylus profilometer in the examination of A1203 ceramic wear surfaces by Gee and McCormick (JI 7 ) . A new spectrally resolved confocal microscope with high photon efficiency for photoluminescence and fluorescence measurements was developed by Bowron et al. (J18). The diffraction-limited spot on the sample performs like the entrance slit through the use of a scanning grating in the detection arm. The detector pinhole acts as the exit slit of a standard monochromator and is functionally equivalent to the detector in a confocal microscope. The sizes of immunofluorescent-labeled gap junctions were analyzed from confocal scanning laser microscopic images and compared with measurements obtained by freeze/fracture electron microscopical techniques by Green et al. (J19); advantages and limitations of each technique were compared. Fricker and White (520) evaluated the use of a confocal microscope with lines at 325,442,488, 514, and 633 nm for optical sectioning investigations of botanical specimens over a wide range of wavelengths. Cox (J21) provided a review and illustrations depicting the present state and trends in confocal imaging from various instruments. The optical sectioning capability of tandem-scanning confocal microscopy permitted Chew et al. (J22) to demonstrate the 3-D array of fibroblast process and subsequent condensation on in vivo assessments of corneal stromal toxicity in rabbits. Oldmixon and Carlsson (J23) provided a technique that allows adjacent, high-resolution, and limited field-of-view images to be stacked, producing images 500 pm in diameter with 1-pm pixel resolution. Intensity variation within and between sectional views due to illumination/detection characteristics and depth-related absorption and detector sensitivities are corrected. Adjacent overlapping stack intensity levels are also adjusted. Fusion of a group of overlapping stacks produces a larger uniform stack. New fluorescence photobleaching recovery equations have been successfully developed by Blonk et al. (J24) for 3-D apertured scanning using a Gaussian approximation for the axial beam profile. Two-dimensional diffusion coefficient measurements from confocal scanning of 45-nm latex spheres, FITC molecules, and 2.45-nm protein-FTIC complex in water/glycerol mixtures were in close agreement to those calculated from the viscosity of the medium and the size of the diffusing species. The equations provided a basis for extrapolation of the lateral diffusion coefficient from confocal scanning light microscopical FPR experimental data. Fairbairn et al. (J25) utilized the improved depth discrimination and spatial resolution afforded by confocal laser scanning microscopy in the analysis of hydrogen peroxideinduced DNA damage in human cells.
Caldwell et al. (J26) reviewed confocal laser microscopy and digital image analysis in microbial ecology. Entwistle and Nobel (527) employed confocal scanning laser imaging to quantify fluorescent emission from biological samples using analysis of polarization. Actin filament distribution was localized in lily pollen protoplasts by Xu (J28), using a TRITC-phalloidin probe, and characterized by employing confocal microscopy. The effect of refractive index mismatch on the image acquisition process in confocal fluorescence imaging was investigated by Hell et al. (J29). Carter (J30)outlined the development of a new transmission confocal laser scanning microscope. Leung and Jeun (J31) investigated measurement errors detected when using fluorescent bead calibration standards for similar use in confocal laser scanning. Varying illumination, detector aperture diameter, and signal applications produced varying measured diameters of the standards; XZ images showed distortion in proportion to the same changes. Micron and Microscopica Act (J32)contains papers from the Conference on Biomedical Image Processing and ThreeDimensional Microscopy held in 1992. Much of the material focuses on confocal light microscopy. The resolution and optical sectioning provided by confocal laser fluorescence was exploited by Van Blaaderen et al. (J33) for 3-D imaging of submicrometer model silica spheres within a concentrated suspension. Confocal imaging allowed easier study of the interparticle structure of the colloid particles. Seealso: References 1,3, B1, B4, D5, E2, F5, F6, F7, G8, G1 1, G12, X 4 , 2 2 , 2 8 , AA2, AA22, BB1, BB2, EE5, EElO, FF1, GG1, GG9, 116, KK2, LL1, LL6, LL15, LL29, LL30, LL32, LL33, LL34, LL35, LL38, and LL48.
K. ULTRAMICROSCOPY Pidduck (KI)reviewed (48 references) applications and techniques of atomic force imaging and outlined emerging scanning probe methods. Included were perspectives on contact-mode AFM, tip/surface interaction, and AFM imaging of inorganic solids and organic materials. The scan speed limit in atomic force imaging was calculated by Butt et al. ( K 2 ) . Thegroupdescribed techniques tomeasure the cantilever spring constant, its effective mass, and the damping constant of the cantilever in the surrounding medium. Practical scan limits for atomic resolution in vacuum was reported at 0.1 rcm/s, increasing in water to 2 pm/s. The surface topography of yttrium barium copper oxide thin films were studied by Thompson et al. ( K 3 ) using STM and AFM imaging. The group scanned with an STM tip, breaking off nanoparticles and depositing them at the edge of the scanned area, where they were later imaged with atomic force. Meyer (K4)provided a review (1 15 references) on the basic principles of atomic force microscopy comparing deflection sensor types and discussing the theoretical basis for the fundamental forces measured, A micrometer-driven coarse motion specimen stage was designed by Teuschler and Ley (K5)for use with a tube scanner-based STM, with lateral motions of f 4 mm with 8 X 8 mm samples. Analytical Chemlstw, MI. 66,No. 12,June 15, 1994
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Barrier height imaging technique was applied by Okumura et al. (K6)to a graphite surface covered with liquid crystals. Differences in STM images and barrier height images of both the liquid crystals and underlying graphite were obtained and compared. Majumdar et al. ( K 7 )presented a new and simple technique for thermal imaging with submicrometer spatial resolution using atomic force microscopy. The method permits simultaneous obtainment of thermal and topographical images of biased electronic devices and interconnects with different materials and variations on a scan surface. Boutonet al. (K8)reviewed (6 references) scanning thermal microscopy. Included in the discussion were experimental equipment, data acquisition, visualization and quantitative analysis of the data, control and optimization, and practical applications. The manufacture of a probe for use in STM imaging of macromolecules was discussed by Nakagawa ( K 9 ) . A scanning tunneling microscope developed by Suzuki et al. (KIO)was coaxially arranged with an optical microscope permitting simultaneous observation when scanning. The tube scanner with tip holder is arranged in the center hole of the objective lens and can be optically recognized as a shadow image of a submicrometer dot. Stranick and Weiss (KI 1)designed and built an STM that provided minimal microwave frequency loss and also operates over a wide frequency range without the use of a microwave resonance cavity. Ohtsu (K12) reviewed (14 references) the technique of controlling atomic motion by optical scanning tunneling with laser light. The strengths, limitations, and future applications of atomic force microscopy were reviewed (25 references) by Binnig
(K13). Sexton (Kl4)provided a review (61 references) of scanning tunneling imaging. Ehrlich (K15)reviewed (47 references) the ability of field ion microscopy to routinely observe individual metal atoms adsorbed on metal surfaces, making it feasible to directly examine atomic events in the growth of crystals from the vapor. Sharp et al. (Kl6)reviewed (15 references) the basic concepts, descriptions, and performance of a photon scanning tunneling microscope. The design and performance of an atomic force microscope integrated with microfluorescence optics was described by Radmacher et al. (K17).The unit covers a scannable field of view of 4 X 4 mm2 at a resolution of -3 pm in the fluorescence mode and a field of 15 X 15 pmz down to atomic resolution in atomic force imaging, producing roughly a 7 order of magnitude magnification range. Simultaneous microfluorescence measurements and AFM imaging of Langmuir-Blodgett films allowed the direction of the polymer backbone to be identified and a molecular model to be constructed. Anderson and Kern (K18)developed high-resolution EBL to make zone plates on Si3N4 membranes. Both gold and nickel zone plates as small as 30-40 nm were made for scanning instruments. 570R
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A low-temperature atomic force microscope with an allfiber interferometer was described by Albrecht et al. (K19). Zhong et al. (K20)demonstrated the utility of the tapping mode in atomic force imaging when studying fractured polymer/silica fiber surfaces. Fritzsche et al. ( K 2 1 ) were able to measure surface pore structure size of a 30K molecular weight cutoff acrylonitrilevinyl acetate copolymer ultrafiltration membrane in water using atomic force microscopy. Shrinkage during preparation precluded measurement using other techniques. The resolution of STM and SEM images of Nucleopore and polysulfone microfiltration and ultrafiltration membranes were compared by Chahboun et al. (K22). Nguyen (K23) obtained images of micrometer-sized corrosion products on steel surfaces under thick opaque and transparent organic coating by thermal wave microscopy. At appropriate modulation frequencies, electron-thermal-wave imaging provided better contrast on rough (ground) AIS1 1010 and 1015 cold-rolled steels. A combined arrangement of a UV laser and atomic force imaging allowed Wefers et al. (K24)to make highly sensitive irradiated surface characterization measurements between different laser pulses. The evolution in surface changes of poly(ethy1ene terephthalate) between UV laser light pulses of 248 nm was followed. Lewis and Ratner (K25) reported a technique for plasmadeposited polymer coating effective on scanning tunneling microscope tips. A compact STM compatible with a conventional SEM was constructed by Nakamoto and Uozumi (K26). The feasibility of characterizing water in bitumen emulsions by N M R microimaging was explored by Randall et al. (K27). A new, fully computerized and inexpensive scanning tunneling microscope was designed and built by Chwialkowski et al. (K28), whose key feature is application of the highsensitivity biomorph. Nakagiri (K29) reviewed the research work of the Yoshida Nano-Mechanism Project including development of scanning tunneling optics, the efficiency of zone plates, and tunneling applications to processed surfaces and biological materials. A description of the Oxford Position Sensitive Atom Probe was provided by Mackenzie (K30). Examples illustrating its high chemical specificity and spatial resolution include measurement of spinodel decomposition in duplex stained steels, interface characterization in multiquantum well materials, and study of precipitates and early stages of precipitation. Annealing effects on latex film surfaces was examined by Goh et al. (K31), utilizing STM. Sarid et al. (K32) described the use of a laser diode interferometer for an atomic force microscope. The performance and sensitivity were tested with resolution comparable to that of a laser beam deflection system. Plasma deposition of C3Fg on metals served as an insulating material for STM tips for Lewis and Ratner (K33),who noted the coated tips produced consistently stable images in buffered saline solutions. The feasibility of a surface electromagnetic wave microscope with excitation of SEW in the intermediate-IR range was discussed by Nikitin and Tishchenko (K34).
Voelcker (K35) demonstrated new modes of operation of a scanning tunneling microscope with IR laser radiation coupled into the tip of the tunneling junction. Ultramicroscopy (K36) contains papers on Resolution in the Microscope presented at the 1991 EMSA meeting. The complete issue of Ultramicroscopy (K37) contains 44 papers dedicated to the founding editor of the journal, Elmar Zeitler. Migus (K38-K43) outlined the basics of scanning probe microscopy in a series of reviews covering the following: its unique capabilities such as extremely high resolution coupled with 3-D imaging; the ability to operate in varied environments and generate chemical and physical measurements; the applications and principles of operation; the relationship between probe shape and image quality; the variety of AFM operating modes; considerations for choosing appropriate SPM techniques; and the continuing evolution of probe microscopy. Laser thermal effects on atomic force microscope cantilevers were studied by Allegrini et al. (K44, K45). Miyamura and Gohshi (K46) reviewed (24 references) the principles of STM imaging and its use in observations of liquid crystals, monomolecular membranes, DNA, proteins, polymers, and fullerenes. Dufour et al. (K47) discussed problems related to image interpretation in a review (17 references) of scanning tunneling, photon scanning, and reflection scanning tunneling microscopy. Wiesendanger et al. (K48) described a technique for the investigation of magnetic structure surfaces at high spatial resolution using an STM for observing vacuum tunneling of spin-polarized electrons. A photon scanning tunneling microscope using diode layers was fabricated by Jiang et al. (K49). Subwavelength optical data storage with a pit diameter less than 270 nm in a Langmuir-Blodgett thin film was achieved. Agrawal et al. (K50) developed a technique enabling the use of scanning tunneling imaging for studying the detailed fracture morphology of polycarbonate and other nonconducting materials. An atomic force microscope was used in the noncontact mode by Schaefer et al. (K.52)to produce images of individual nanometer-size metallic clusters preformed in the gas phase deposited on a variety of substrates. The technique allows imaging of clusters in their as-deposited position. Chernoff (K52) reviewed (4 references) basic atomic force imaging, providing practical applications in materials science and biology. Tsuno (K53) reviewed the reduction in resolution in conventional TEMs through the use of higher voltages and narrowing of bores and gaps with side-entry stages. The feasibility of 0.1-nm resolution at intermediate voltages was discussed. Geller (K54)provided a brief outline for accurate, SEM magnification calibration considerations. Dubson and Hwang (K55) developed a simple scanning tunneling microscope that can be operated at room temperatures down to 4 K. It was assembled without solder or glue. A complete list of components for practical self-assembly was provided along with preliminary results obtainable with the instrument. Mathai et al. (K56)designed and operated a magnetic flux microscope and demonstrated its use in imaging thin-film
strips of superconducting Pb in field strengths of 0-750 nT and in monitoring the position of a sample with a resolution of -0.5 nm HZ-'/~ at a frequency of 4 kHz. Black et al. (K.57) described the same magnetic flux microscope which uses a liquid nitrogen cooled thin-film YBazCu307 superconducting quantum interference device to produce 2-D images of magnetic fields with a spatial resolution of -80 pm within a field of view of 100 mm. The equivalent magnetic field noise ranged from 80 pT HZ-*/~ at 1 Hz to 20 pT H z 1 I Zat 1 kHz yielding a field resolution of -200 pT. Magnetic domains in ferromagnetic samples, small currents flowing in fine wires and trapped flux and diamagnetic susceptibility is superconducting thin films were examined. See also: References 2,4, 26, B5, B8, B l l , B12, F4, J19, 0 2 , 0 3 , 0 4 , 0 8 , P l , X 3 , X6, Y3,Y8, Y9,23,26,212,213, 214,217-Z19,AA9,AA11,AAl6,AA22, BB4, CC4,EE14, EE16, FF3, FF4, FF8, FF11, FF12, 112, KK9, LL2, LL14, and LL43.
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L. X-RAY MICROSCOPY Iketaki ( L I ) patented and described an X-ray microscope for biological use. The specimen is irradiated through an X-ray filter transmitting between 43.7 and 65 A. The microscope has a light source for emitting UV light, which allows for image formation from an X-ray detector in which the UV light is reflected from the X-ray filter to irradiate the specimen. Michette et al. (L2) reported the first successful attempts at utilization of a scanning transmission X-ray microscope with a laser-plasma source with an improved system; single shot per pixel resolution better than 50 nm will be routinely possible. A plasma focus device emitting line radiation of H-like N VI1 at X = 2.5 nm into the water window region was developed by Lebert et al. (153). The development of a new prototype Fourier transform microscope for an X-ray imaging system was described by Wood et al. (L4). The microscope is intended for use with X-ray emitting targets in laser fusion experiments. Results were presented by DiCicco et al. (L5) that demonstrated the capability of soft X-ray reflection imaging at 18.2 nm in the Schwarzschild configuration. Murakami et al. ( L 6 ) report construction of an X-ray microscope using Schwarzchild-type normal-incidence X-ray optics and 44.8-A carbon K a radiation. A 0.5-pm-wide pattern was resolved. The construction and performance of a sample chamber for X-ray microscopy was described by Goncz et al. ( L 7 ) . Designed for scanning transmission X-ray microscopy, the chamber permits high-resolution imaging of cellular and subcellular specimens suspended in aqueous solution while varying the environment. The design and fabrication of a Schwarzschild objective for soft X-ray imaging was put forth by Horikawa et al. (a). Hilkenbach (L9) experimented with the construction of sputtered sliced zone plates. Remmington et al. (L20) made in situ measurements of the spatial resolution function for two sectors of the 22-fold magnification Woelter X-ray microscope. Analytical Chemistry, Vol. 66, No. 12, June 15, 1994
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Burge ( L I I ) provided a review (25 references) of the historical introduction of X-ray microscopy and its achievements in the direct observation of molecular action in living cells; development parallels with electron microscopy are also discussed. Burge (1512) also reviewed (21 references) the principles of X-ray imaging, sources of soft X-rays, optical systems, and image contrast, providing a basis from which to assess its applications. X-ray optics for scanning fluorescence microscopy and other applications were discussed by Ryon and Warburton (L13). Soft X-ray multilayer mirrors suited for use in biological X-ray microscopy were developed by Nakamura (L14). A new time-resolved, X-ray, ring coded-aperture microscope for inertial confinement fusion applications was developed by Ress et al. (~515,156).The instrument produces 500ps duration sequences with a temporal resolution of 80 ps and a spatial resolution of 5-6 pm. Ress and other co-workers (72) discussed the X-ray detectors, apertures, and imageprocessing software that were used in its development. A nickel-phase zone plate for X-ray focusing and imaging was examined by Fujisaki et al. (L17). A tantalum X-ray laser (A = 4.483 nm) was utilized with an X-ray zone plate lens to image a test pattern by Da Silva et al. (198). Schmahl and Cheng (L19) provided a review of X-ray microscopy. T m i e et al. (L20) reviewed (60 references) the characteristics of X-ray microscopy, in addition to the development of zone plate, multilayered mirrors, and X-ray holography. Tomie (L21) also provided a review (15 references) of the applications of X-ray microscopy to biological studies. An X-ray microscope with a pulsed plasma source is being developed by Schmahl et al. (L22). The technique and advantages of soft X-ray contact imaging of living biological material for practical routine suboptical resolution was reviewed by Cotton (L23) and Cotton and Fletcher (L24). Ando and Kayoshima (L25) reviewed (5 references) the development of synchrotron radiation sources and the performance of their X-ray microscope. The properties and limitations of scanning X-ray imaging were discussed by Ebert (L26). Bauer (L27) reviewed (1 8 references) imaging systems, processes, and principles of X-ray imaging with applications and references to optical and electron microscopical methods. Margaritondo (L28) reviewed the progress in the instrumentation, photon sources, and general trends in the fields of X-ray microscopy and microspectroscopy. Suzuki (L29) reviewed (23 references) scanning X-ray microscopy and hard X-ray microprobing including X-ray condenser optics and elements, X-ray focusing optics utilizing ellipsoidal mirrors for probing, and applications to GaAs FET. Radiation damage of biological specimens and corresponding imaging properties was calculated by Goelz (L30),using a comparison of amplitude and phase-contrast X-ray microscopy. A prototype Fourier transform microscope for X-ray imaging is being developed by Wood et al. (L31); position resolution of 4 pm in the 3-7 keV is expected. 572R
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The instrumentation and optics of transmission and scanning X-ray microscopy were outlined and reviewed (24 references) by Michette (L32). Thieme et al. (L33) described, with applications and examples, X-ray microscopy for the examination of aqueous biological and chemical colloidal systems. MacGowan (L34) reviewed (46 references) X-ray lasers as potential sources for X-ray microscopy. The throughput of a multilayer (SOMo/Si) Schwarzschild objective for use at X = 23.2 nm was measured by Michette et al. (L35). High brightness and short pulse-width X-ray lasers offered Da Silva et al. (L36) the possibility of high-resolution 3-D imaging of specimens in an aqueous environment without the blurring effects associated with natural motions. Foerster et al. (L37)reported X-ray microscopical imaging in narrow spectral ranges comparable with the width of spectral lines through the use of Bragg reflections on two-dimensionally bent crystals. The Proceedings of the Third International Conference on X-ray Microscopy were edited by Michette et al. (L38). Schulz et al. (L39) studied the feasibility of using a laser plasma source in place of a synchrotron as a source for X-ray imaging. Carbon spectra in the water window were obtained using a transmission grating and were used to determine the absolute number of photons in individual carbon emission lines. Aoki et al. (L40) constructed a high-resolution soft X-ray microscope with a Nd-YAG pulse laser and grazing incidence mirrors. Single-shot resolution of about 40 nm was achieved with a beam energy of 1.4 J and a pulse width of 8 ns using a Wolter type 1 mirror as objective mirror and a toroidal mirror as a condenser. Aoki (L41) provided a review (17 references) on recent advances in X-ray microscopy. Circularly polarized soft X-rays were used with an imaging photoelectron microscope by Stohr et al. (L42)to record images of magnetic domains at partial resolution of 1 pm. Dhez (1543) provided a review (30 references) of X and XUV microscopes based on mirror optics and included a discussion on the likelihood of building efficient XUV microscopes. See also: References 4, 64, 70, F16, G9, and G13. M. ACOUSTIC MICROSCOPY Kent and Vary ( M I ) put forth a noncontacting scanning laser acoustic imaging technique for making in situ tensile strain measurements of small-diameter ceramic fibers. Individual Nicalon S i c (1 5 pm) carborundum S i c (40 Mm) and sephikon sapphire (140 pm) were measured. Gremaud et al. ( M 2 ) reviewed (6 references) applications of continuous-wave scanning acoustic imaging in materials science. Preliminary work by Grow et al. ( M 3 ) on single crystal and polycrystalline NiAl confirmed that acoustic contrast is very dependent on anisotropy and elastic discontinuities;other effects of crystal orientation, deformation, and fracture on contrast were discussed. Hashimoto et al. ( M 4 ) fabricated a novel acoustic lens through chemical isotropic etching of a single crystal silicon wafer. A variety of wafers, etchants, and etching conditions
were described to obtain a surface with good sphericity and smoothness. Moisture sensitivity of plastic surface mount devices was characterized using scanning acoustic imaging by Shook (M5). Hirose and Asami ( M 6 ) investigated the density distribution in a sintered aluminum compact using acoustic imaging. Three procedures were described to obtain density distributions. The acoustic image enabled detection of pore growth and substantial local elongation. Propagation of surface acoustic waves on thin films of various thicknesses deposited on the (001) plane of cubic crystals was monitored by Kim et al. ( M 7 ) . Phase velocities were measured as a function of the propagation, which demonstrated the advantage of directional measurement by the line focus acoustic microscope. Kundu ( M 8 ) set down an acoustic microscopical analysis to synthesize the V(z) curves of multilayered solids immersed in water. The attempt was made to avoid the three major simplifying assumptions of presently available techniques such as the paraxial approximation, assumption of perfect reflection, and the ambiguous pupil function or incident field strength in the illuminated region. Vickers hardness indentations were acoustically observed by Okada et al. ( M 9 ) . The microscope revealed vertical cracks and debonding on cement carbides coated with PVD and CVD processed titanium carbide films. A line-focus acoustic microscope and a depth-sensing nanoindenter aided Ashcroft et al. (MZO)in the direct measurement of the elastic moduli of 1 LiZn silicate and 3 Li allumino silicate glass-ceramic thick films on Cu and Cu/ Invar/Cu substrates. Briggs (MZZ) provided an extensive review of acoustic microscopy. Levin et al. (MZ2) discussed the principles of acoustically imaging highly anisotropic materials, applying the technique to the characterization of the internal structure and defects in pyrographite. Gurtoval and Eremenko (MI 3) achieved direct visualization of dauphine twins in quartz fillers using acoustic imaging. Ishikawa (MZ4) reviewed (21 references) the principles of acoustic microscopy with applications including in situ observation of anodic oxide layer formation and pitting on A1 surfaces, steel plate corrosion under paint coating, thickness of damaged layers on a polished Si wafer surface, residual thermal stress at interfaces between Si3N4/Ni/ W/Ni/Fe3OCr alloy, and structural anisotropy in plastically deformed Si steel plates. A line-focusacoustic microscope was utilized by Kielczynski and Bussiere ( M I S ) to measure the angular distribution of longitudinal surface skimming waves in Zr/Nb samples exhibiting orthorhombic macroscopic symmetry; texture coefficients were thus determined without prior knowledge of the single crystal elastic constants. Scanning acoustic imaging allowed Pangraz et a1 (MZ6) to monitor the effect of creep damage on the Rayleigh wave velocity in alloy 800H. Lawrence et al. (MZ7, MZ8) explored the microstructure of Nicalon-reinforced borosilicate glass as well as the magnesium and calcium aluminosilicate glass-ceramic matrix with acoustic microscopy.
Van Doorselaer et al. (MI 9 ) evaluated different methods for delamination detection by acoustic microscopy in plasticpackaged integrated circuits. Acoustic imaging was utilized by Carbone (M20) to facilitate identification of assembly-related defects across a range of IC package styles. The microscopy provided means for nondestructive detection of such defects. The depths of short cracks in PMMNA (Perspex) were measured using scanning acoustic microscopy combined with a time-of-flight diffraction technique by Zhai et al. (M2Z). Acoustic signature between 50 and 2000 MHz was achieved by Caplain et al. (M22) on low-alloy, C, stainless steel, and A1 microstructure; surface roughness and elastic properties were nondestructively determined. A silicon tip with a 500-Aradius of curvature was batchmicrofabricated with an integrated 1-GHz ultrasonic transducer for use in scanning near-field acoustic probing by Quate and Khuri-Yakub (M23). Briggs (M24)provided a novel review summarizing acoustic microscopy. Sections include “How to make a microscope”; “A little theory“; “Some pictures”; and “Where next?”. Heterogeneous matrix composites were scanned acoustically by Woo and Seferis (M25). Rubber domains within a thermosetting or thermoplastic continuous phase were easily resolved. Rayleigh wave distortion of imaging limited the resolution in the characterization of thermoplastic and thermosetting phases. Tokunaga et al. (M26) compared the photoacoustic response, both amplitude and phase, generated from an epoxy resin backing of either aluminum, white acrylic, or blackcoated white acrylic resin. Thevelocity of longitudinal wave (vs surface acoustic wave) propagation was derived in polymer material characterization by Nishimura et al. (M27). Ganz (M28) reviewed the principles, operation, and application of ultrasound imaging on solid surfaces. A C-scan-mode acoustic- and a through-transmission scanning laser acoustic microscope were both used by Wey et al. (M29) for the nondestructive evaluation of damage in graphite/epoxy composite laminates. The nondestructive imaging allowed correlation with compression-after-impact strength of the impacted samples. Wey et al. (M30) also demonstrated the usefulness of acoustic imaging in examining the relationship between residual strength and fatigue damage in several Nicalon fiber-reinforced glass matrix composites. Damage patterns evident from acoustic images showed that existing, undetected defects affected the resultant damage pattern after fatigue. Endo et al. (M31) developed an amplitude and phasemeasuring acoustic microscope; high-frequency (400 MHz) V(z) curves of fused silica and alumina were measured with high accuracy. Ceramics, monocrystals, and thin films were examined acoustically by Maev and Chernosatonskii (M.32). The interface between the growth of copper or nickel and tin or tin/Iead alloys was observed acoustically at high frequencies (1 GHz) by Drescher-Kasicka et al. (M3.3). A low-frequency ( 5 MHz) acoustic method was developed by Bashyam and Rose (M34) for evaluation of ceramic matrix composite materials. Analytical Chemistry, Vol. 66, No. 12, June 15, 1994
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See also: References 4, 5, A5, 214, AA4, AA22, GG4, GG5, GG6, GG9, HH1, 113, and 114. N. CATHODOLUMINESCENCE A scanning electron microscope and digital image processor were combined for high-sensitivity cathodoluminescence by Kitamura et al. (NZ). Growth zoning in acicular coated diamond, igneous quartz, and relict olivine in chondrite were studied. Hagni ( N 2 ) successfully applied reflected light- and cathodoluminescence microscopy to various industrial problems. Included, among others, were investigations of beneficiation products, leaching problems, phorphatic/iron ore and mill products, pyrometallurgical products, roasted refractory gold-bearing sulfides, ceramic buildups, and other industrial products. Cathodoluminescence microscopy was employed by Watson and Durose (N3) to investigate the optoelectronic activity of defects in CdTe crystals. The basic principles of cathodoluminescence microscopy and its practical application in the characterization of rocks and ceramics was put forth by Finch ( N 4 ) . Holt ( N 5 ) reviewed (63 references) the general principles and explored new directions for scanning cathodoluminescence microcharacterization. Petrov ( N 6 )provided a review (1 12 references) of cathodoluminescence microscopy. The action of a new etch for revealing defects in cadmium telluride was introduced by Watson et al. ( N 7 ) . Direct correlations with IR microscopy and cathodoluminescence showed the etch successfully revealed twin boundaries, ppts, and dislocations. Saparin and Obyden ( N 8 ) provided a brief discussion on new methods and applications of cathodoluminscence analysis of solids using color contrast with an SEM. See also: References EE2, EE11, 115, and LL5.
0. EMBEDDING AND MOUNTING An improved technique to physically stabilize microbial aggregates for light microscopy by embedding in solidified agar is recommended by Ganczarczyk et al. (01). Bulk, powder, granules, and fiber sample preparation techniques for AFM were discussed by Marchese-Ragona et al. ( 0 2 ) , including the use of sticky tape, Norland optical adhesive, and Tempfix. Robertson et al. (03) evaluated a technique for progressively lowering the temperature of embedding for electron microscope immunolabeling. A standardized protocol was developed which can be applied to a wide variety of samples. A quick-curing, visible light curing resin with good adhesion to engineering plastics and polymers was developed by Ohno et al. (04) for electron microscope use. Hopwood (05) reviewed the technique of exploiting microwaves in tissue preparation. Simple procedures are laid out that dramatically decrease preparation time in fixation, stabilization of tissues, and staining for both light and electron microscopy. Giammara (06) reviewed (13 references) the use of microwaves to polymerize embedding polymers for light and electron microscopy. 574R
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Strategies for improving cytochemical and immunocytochemical sensitivity of ultrastructurally well-preserved, resinembedded biological tissue for light and electron microscopy were offered by Hobot and Newman (07). Harris et al. (08) presented a simple and quick technique for TEM preparation of metal alloyed powders involving electrochemical polishing powder-epoxy resin mixtures. P. ULTRAMICROTOMY A unique method was implemented by Jacobs et al. (PI) for sectioning solder/Cu and composite solder/Cu samples for TEM analysis. Carbon-coated samples dipped in cyanoacrylate ester were epoxy embedded, and trimmed thin sections were directly ultramicrotomed with a diamond knife. Artifacts were minimized by controlling sectioning conditions. Single samples thus yielded images of each phase simultaneously. The effects that thickness variations and surface layers in ultramicrotomed sections have on elemental mapping were outlined by Malis and Steele ( P 2 ) . Michel et al. (P3)discussed optimizing cutting parameters in cryosectioning. In addition, an ionization electrode with a primary voltage of 7-8 kV, used to neutralize the surface charge on a diamond knife, aided in reducing cutting artifacts. Webster (P4)described a modification to the LKB 7800 series Knifemaker that produces knives using a balanced break. A simple microtome utilizing a razor blade for sectioning stub-mounted critical point dried tissues for SEM analysis was described by Keijzer (P5).
Q. MISCELLANEOUS SPECIMEN PREPARATION A method involving freeze-drying an ash dispersion on vitreous carbon was described by Katrinak and Zygarlicke (QZ).The low-contrast background enabled characterization of particles as small as 0.1 bm for automated SEM analysis. A new method of studying airborne particles based on sampling those entrapped in tree resins was discussed by Valdre and Korlevic ( Q 2 ) . The method can be applied in a variety of fields where historical, reliable information is needed. Cross-sectioning techniques using the reactive ion etcher were described by Colvin (Q3). Laser cutters were used to open &windows"in printed circuit board ink resists for crosssectioning. An issue of Scanning (Q4) contains seven entries from a symposium on ultramicrowave specimen processing for light and electron microscopy. Innovations have come from both commercial and research-grade microwaves. Giammara (Q5) explains that since microwave irradiation is in its infancy, much knowledge will be gained through trial and error. In addition, contributions demonstrate that the technique can be applied to all aspects of sample preparation for optical and electron microscopy, both to improve results and to preserve structure and antigenicity. Kok et al. (Q6)explored the problems associated with hot spots in microwave equipment. In a review (62 references), Leong (Q7)traced the history of improvements in microwave technique for diagnostic laboratories. A standard protocol using large-cavity, domestic microwaves for improved fixation of tissue and cells was put forth
by Login and Dvorak (Q8).The two evaluated and reviewed (30 references) specimen integrity following irradiation in differing solutions and postembedding ultrastructure immunogold labeling. Hanker and Giammara (Q9)evaluated and illustrated microwave-accelerated cytochemical stains for image analysis and examination of light microscopical slides with electron optics. Giammara (QIO)outlined and reviewed (1 3 references) microwave methods for the polymerization of epoxy resins, LR white, and other polymers. De Tajada (QII ) reviewed the manufacture and properties of polycarbonate filters and their use in clinical diagnosis, monitoring of liquids by filtration, and epifluorescence microscopy. Garg (QI2)described the use of Napthalene Black B staining for the in situ examination of fungi growing in agar medium. See also: Reference 7.
R. PHOTOMICROGRAPHY AND PHOTOMACROGRAPHY Bracegirdle (RI)provided a brief, effective tutorial to familiarize the beginning microscope user with simple, yet necessary, techniques and equipment for recording microscopic images. Illustrated and explained were making contact negatives of specimen slides using an enlarger as a light source, enlarger-produced images recorded with a camera, negative prints from direct projection, photomicrography by direct projection, and photomicrography with or without an attached camera. Loveland (R2)provided a detailed discussion of the apparatus and techniques used in producing dark-field motion photomicrographs exhibiting flagella in motile bacteria. The actual film is part of an advanced educational film on bacteria. A brief historical insight into the role of photomicrography and the recording of microscopic images was traced by Fox and Saunders ( R 3 ) . Early efforts of Robert Hook, Anton Leeuwenhoek, J. J. Woodward,and J. S . Billings wereincluded with a discussion of the historical improvements in light microscopy, optics, printing methods, staining techniques, and recent contributions from the 20th century. The third part of a tutorial series on digital imaging techniques for enhancement of conventional silver halide-based photographs was offered by Kilbourne and Dodd (R4). The well-illustrated primers offer instruction for scanning 35-mm slides, correcting for color balance, density and contrast, artifact illumination, compositing multiple images to a single image, labeling, and outputting for production of the final image. The appendices contain helpful trademark notices and a sampling of vendor sources and contact information. Clarke (R5)demonstrated the working range of scanning light photomacrography to be limited to magnifications under 150X; image field width limitations at high magnifications, the effect of magnification variation within depth of field and within the illuminating beam, and depth of field for high resolution using optimum aperture control were considered. Delly (R6)provided detailed directions for modifying a Polaroid film holder for use as a labeler. The modified Polaroid
Model 54515453. film holder can be used for simultaneous labeling when larger format (4 in. X 5 in.) images are being shot. Delly (R7) also outlined directions for converting discarded Polaroid film packs into ground-glass viewing/ focusing screens, useful as a photomicrographic accessory, Pan (R8, R9) provided a detailed description and outline of a novel technique employing TTL autometering to accurately determine the manual exposure for closeup photography. Wildi (RIO)added a chart for compensated film speed settings for TTL cameras, based on similar engineering tests made at Hasselblad. The performance characteristics of Polacolor 64 tungsten film were reviewed by Saunders (RII). A test report on Polaroid’s polacolor tungsten film was offered by Walker ( R I 2 ) . He also outlined (RI3) useful information on image manipulation when duplicating 35-mm color photomicrographic transparencies. Of historical interest is Clarke’s (RI4) account of the development of photographic chemistry. As part of a special anniversary supplement, Biological Photography included actual 1933 procedures by Goosman (RI 5 ) for making colored lantern slides of photomicrographs from a single negative. As the first entry in a series, Williams and Williams (RI6) provided a review (73 references) and introductory tutorial on ultraviolet photography and reflected ultraviolet techniques. Tomographic methods for effectively increasing the depth of field and generating stereo pairs of fluorescence micrographs from a conventional microscope were introduced by Holmes et al. (RI 7). Inverse filtering and maximum-likelihood estimation were considered. Khosla and Holmes (R18)introduced a Wiener-type inverse filtering method for generating stereo pairs of bright-field micrographs. Ando and Fujisawa (RI9) described a method for photographing and studying autofluorescence that is likely to disappear when affected by UV radiation. Autofluorescence of vitamin A in bovine, swine, poultry, and sheep livers was investigated by photomicrographs using epifluorescence illumination. Fox and Dreyfuss (R20)described photographic techniques for optimum expression on the results of in situ hybridization autoradiography and the location of immunogold-silver intensified protein antigens in tissues and cells. Zieler ( R 2 I ) provided a brief discussion on the cause of and means for minimizing external vibration when taking photomicrographs. Dunlop (R22) reviewed relatively simple techniques for making good quality photomacrographs. Morgan (R23)discussed the use of Leica camera equipment for recording photomicrographs and photomacrographs. Priestley (R24)describes a convenient means for viewing emulsion autoradiograms through epi polarized rather than dark-field illumination. The technique is applicable whenever metallic particles need to be visualized and is convenient in that most microscopes equipped for epifluorescence can be adapted for epipolarized illumination. Davidson (R25) illustrated the use of polarized light, differential interference contrast, and reflected light microAnalytical Chemistry, Vol. 66,No. 12, June 15, 1994
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scopical images in a discussion of the history of investigations on high-temperature superconductors. See also: References 1, 19,27,58, A2, B14, D9, and E12. S. REFRACTOMETRY Su ( S I ) put forth simple microscopical methods and equations for calibration of refractive index liquids’ n~~~value by using optical glass standards whose refractive index is accurately and precisely known for three or six wavelengths. A single-glass and double-glass method allows accuracy of fO.OO1 and is convenient when a refractometer is not available. An equation to determine the real part of the refractive index, when loss must beconsidered, was put forth by Larrabee ( S 2 ) for use in refractometry of bulk transmissive optical materials. A measurement system was established by Allison et al. ( S 3 ) that can precisely determine the absolute refractive indexes of anaesthetic agent vapors at a wavelength of 633 nm. Komissarov et al. (S4) devised a refractometric method for determining the completeness of the dissolution of some aromatic diamines in an amide-salt solvent. See also: References H5,11, and PP5.
T. HOT STAGE AND COLD STAGE TECHNIQUES Gan and Seferis ( T I ) made use of an IR reflectance microscope equipped with a hot stage to follow the cure of a polyimide-carbon fiber matrix composite. A thermal vacuum chamber was developed by Abdulvakhidov and Gorbunova (T2) for use with a polarized light microscope. Thechamber permits crystal studies in the-1 50’ to +250° range; a study of the ferroelectrical crystals BaTi03 and PbSco,~Nbo,~O3 demonstrated the working temperature range. See also: References 12, E 18, and Y 15. U. STEREOLOGY Marcussen (Ul ) introduced a double-dissector method for estimating the number of particles within other particles. The technique is suitable for paraffin-embedded tissue. Results are unaffected by tissue shrinkage. The adaptability of stereological techniques was illustrated by Karlsson and Cruz-Orive (U2)in estimating pore size and number in sand-cast aluminum alloy. Nielson (U3) outlined estimation techniques for the derivation of particle number or mean volume of particles by reviewing the use of the dissector and optical dissector. Liu (U4) reviewed both the applications and underuse of stereological principles in materials science studies. Papers in an issue of the Journal of Microscopy (15’5)are entirely devoted to different areas of stereology. See also: References B 1, B 14, J 1, and 58. V. AUTOMATED IMAGE ANALYSIS AND VIDEO MICROSCOPY Willis et al. ( V I ) presented several image reconstruction algorithims based on the maximum likelihood estimation theory that were used to generate 3-D rendering of brightfield micrographs. Reconstructions from real biological data demonstrated the potential in practical applications. 576R
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Kempe et al. (V2)introduced a novel method for improving the spatial resolution of a laser scanning microscope. The image processing method is based on deconvolution of the image with the approximative point spread function. Thermal motion of one-dimensional domain wells in monolayers of a polar polymer were investigated by Ludwig et al. (V3)using video scanning tunneling microscopy. Direct observation of the motion in the walls was made, for the first time, by scanning with video frame rate. Time-lapse microscopical recording allowed Thomas et al. (V4)to observe and characterize slowly developing symptoms on fungal structures caused by low levels of dimethomorph. Grier and Murray (V5) reviewed the time-resolved video microscopy of the dynamics and statics of two- and threedimensional submicrometer sphere suspensions. Hawkes (V6)provided an introduction to the fundamentals of image algebra and its role in image enhancement and restoration. A low-cost digital tracking system was designed and illustrated by Chelihi and Gaydecki (V) for tracking prominent features moving in the field of view of a video camera and determining their positional coordinates at a normal video framing frequency. Hovmoller (VS)described the newly developed user-friendly program CRISP for crystallographic image processing of electron optical data on a personal computer. It is especially useful on submicrometer crystals and minerals. Zou et al. ( V 9 )describe another program, ELD, that was developed for quantifying intensities of electron diffraction spots. A brief description of each program and crystallographic image processing was offered by Hovmoller (VIO). Useful statistical consideration for the analyses of spatial patterns, orientations, and shapes via software controls for tablet and PCs was offered by James ( V I I ) . Fermin et al. (VI 2 ) demonstrated the usefulness of color thresholding for objective quantification of products of histochemical reactions or subtle differences in cells and tissues. See also: References 4, 16,41, 50, A4, B3, C2, C4, D11, E2, E l l , E14, F1, F2, F3, F14,G3, G6, H1, 11, 53, 58, 514, 523, 532, K49, R2, X12, Y11, 28, Z l l , AA24, BB3, BB6, CC1, CC3, EE12, FF2, FF15, 111, LL1, LL3, LL7, LL8, LL9, LL10, LL25, LL31, LL39, LL45, LL46, and LL49.
W. PARTICLE GRAIN SIZE MEASUREMENT The reliability and precision of a modified SEM method for particle size determination of fine ceramic powders was evaluated by Klevtsov and Mironova (VI). Particle sizes of an object’s microscopical image were determined by Davidson et al. (W2) from the analysis of detailed intensity profiles. Video image analyzers were used. The fundamental frequency of the Fourier components were analyzed to describe a particle’s size, allowing for accuracy chiefly dependent upon the signal-to-noise ratio and independent of classical microscopical resolution, provided that the objective’s numerical aperture is sufficient to pass the fundamental. A fiber-optic probe for particle sizing in concentrated suspensions was constructed and evaluated by Dhadwal et al. (W3). Results from studies on suspensions of polystyrene latex particles over a wider range of sizes and concentrations
indicated potential use for process control in industrial and laboratory applications. Different particle size measurement techniques for general purpose PVC resins were compared by Davidson et al. (W4). Good agreement was found between optical microscopy and image analysis, sieves, HIAC, and Coulter counter. See also: References B9, U2, U3, 216, and EE13.
X. MISCELLANEOUS TECHNIQUES FOR SPEC1MEN EXAM1NATION A noninvasive method for imaging cell behavior in vivo was described by Amanze ( X I ) . Embryos are embedded in a balanced salt solution within a low melting point agarose and oriented for microscopical observation within a chamber. Video Nomarski DIC images are recorded, processed, and analyzed in a speed-up mode. Recent advances in surface analysis were reviewed (1 5 references) by Reviere (X2). Mackenzie (X3)outlined the practical application of various imaging techniques in the characterization of nanometer-scale structures and their relevance to understanding ultrascale physical processes. Butler et al. ( X 4 ) described an optical profilometer which allowed vertical resolution of f 1 nm while simultaneously acquiring a confocal image; no active feedback is required during scanning, and the profile is independent of the objective reflectivity. A miniature anaerobic, continuous-culture unit which fits onto a microscope stage was constructed and described by Jones et al. ( X 5 ) . The unit allowed long-term growth studies of living anerobic biofilm development. Precise fluorescence and phase-contrast images were captured, stored, and videoanalyzed, permitting time-lapse analysis. Somorjai (X6) reviewed (31 references) a number of techniques and instruments that are expanding surface analysis to new types of surfaces and interface systems. Various imaging techniques such as STM and AFM were included. Afzal and Treacy ( X 7 ) made a simple modification to a conventional light microscope that enabled injection of light from a diode laser which functioned as an optical tweezer. Procedures are included, with experimental results for fitting any microscope to trap and manipulate single cells. Taylor (X8)described design changes in the Taylor Microcompressor Mark I1 that add increased control to the operator. Ramamurthy et al. ( X 9 ) provided an extensive review (322 references) on organized media for photoreactions including liquid crystals, clay, zeolites, micelles, and Landmuir-Blodgett layers. Traditional macroscopic optical measuring techniques and scanning laser microscopy were described. Application of microscopical technique in paleobotany was reviewed (20 references) by Collinson (XIO). Walz and Prieve (XII)presented a method for predicting and measuring the axial and radial components of a radiation force acting on a dielectric sphere. Total internal reflection microscopy techniques were described that were used to measure the net weight of a single polystyrene latex sphere caught in a stable optical trap. A new experimental technique for particle tracking by digital image processing and Brownian dynamics computer
simulations was introduced by Schaertl and Sillescu (XI2) for studying the dynamics of colloidal hard spheres in thin aqueous suspension layers. See also: References 17, LL4, LL7, and LL16. Y. LIQUID CRYSTALS The value of polarized light microscopical methods in the characterization of liquid crystals was set down by Viney (YI). The ease of specimen preparation and ability to study fluid, self-assembling biological macromolecules that may be sensitive to ionizing radiation were illustrated in the studies of natural silk secretions. Donkai et al. (Y2) reported using a novel polarized light microscopical technique to eliminate contrast variation and extinction when observing liquid crystal structures. The lyotropic phase of imogolite was characterized. Grafstroem et al. (Y3)improved the resolution of scanning tunneling images of individual singular features, such as the identification of individual molecules, through the use of laser light. Dye molecules in ordered liquid crystal structures were studied. Polarized light observations of axial and radial nematic droplets for a duel-frequency addressable liquid crystal were presented by Kitzerow et al. (Y4). A method for the determination of the elastic constant ratio K33/K11 in nematic liquid crystals from measured birefringence patterns is described by Scharkowski et al. (Y.5). A detailed discussion is presented. The effect that two potential moisturizers had on phase transitions of the liquid crystal phase of model stratum corneum lipids was traced by Mattai et al. (Y6) using polarized light microscopy and DSC. Yang et al. (Y7)investigated the phase transition of crown ether base liquid crystals utilizing polarized light microscopy and thermoanalysis. Shigeno (Y8)reviewed (7 references) observations of liquid crystals via scanning tunneling imaging. Scanning tunneling imaging allowed Matsushige et al. (Y9) to observe the molecular arrangement of a new type of liquid crystal, 5- [(p-dodecyloxy)phenyl] pyrazine-z-carbonitrile. Using polarized light microscopy, lyotropic liquid crystal formation by octadecylpyridinium bromide in a range of polar solvents was examined by Pleasdale (YIO).Phase diagrams were constructed and solvent interactions investigated using quadropole NMR. Video microscopy was used by Reamey et al. (YII)to observe the behavior of nematic droplet polymer films as the droplets responded to an applied electrical field. Schmid (YI2) provided a review (33 references) on polarized light microscopical studies of the orthorhombic ferroelastic domains and domain structures of yttrium barium copper oxide. Phase diagrams of lyotropic mesophases in selected binary trialkylphosphine oxidelwater systems were constructed by Doerfler (YI3) from PLM texture observations. Enantiomeric and racemic monolayers of N-stearoyl serine methyl ester were compared by Stine et al. (YI4) using fluorescene imaging and surface pressure isotherm measurements. Analytical Chemlstty, Vol. 66, No. 12, June 15, 1994
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Carboni (Y25) developed a polarized light microscopical apparatus for texture studies and collection of reflection spectra of liquid crystals at pressures up to 400 MPa and temperatures through 200 OC. See also: References D13, K6, K46, X9, and AA6.
Z. RESINS, POLYMERS, AND THEIR ADDITIVES Techniques for characterizing multilayer polymer films were demonstrated by Gal and Toth ( Z 1 ) . Individual layers were analyzed by optical microscopy, IR microspectroscopy, and computerized spectra manipulation techniques. Verhoogt et al. (22) described the use of confocal laser scanning imaging as a new technique for the determination of morphology of polymer blends. Three-dimensional images are obtained with minimal sample preparation. Using atomic force imaging, molecular packing on the surfaces of fibers and films from segmented polyimides with different rigidity was observed by Patil et al. (23). McCrone ( 2 4 ) reviewed (44 references) the characterization and identification of polymers by the appropriate use of polarized light microscopy. Simultaneous monitoring by light microscopy and acoustic emission allowed Karger-Kocsis and Czigany ( Z 5 ) to follow the fracture behavior sequence of glass-fiber, mat-reinforced structural nylon RIM composites. Legett et al. (26) reviewed (33 references) the basic principles of atomic force and scanning tunneling microscopy and their applications in polymer science. PLM observations on CO[poly(ethylene terephthalatepoxybenzoate)] thermotropic copolyester were continued by Shim and Lin (27). Moreau et al. (28) examined watertrees within polyethylene intended for power cable insulation. The resolution of the fine structural defects (watertrees) was improved with rhodamine and epifluorescence imaging, video-enhanced imaging, and confocal laser scanning. Rappe (29)examined the optical and physical properties of LDPE, HDPE, irradiated polyethylene, polypropylene (I), biaxially oriented-I, polystyrene, and PET. Sayyadnejad ( Z 1 0 ) reviewed (15 references) the study of polymeric materials by FT-IR and IR microscope techniques. Giuld and Summerscales ( Z I I ) provided a review (83 references) on the preparation of polymer composite samples for optical microscopy and discussed the use of image analysis for microstructural analysis. The use, basic concepts, and instrumentation of atomic force imaging were presented by Maganov and Cantow ( 2 1 2 ) . Numerous examples in the studies of polymer morphology and surface morphology were given. Recent progress in atomic force and scanning tunneling imaging were reviewed (82 references) by Fuchs ( 2 1 3 ) . Included were studies of bipolymers, individual chemisorbed molecules, and synthetic polymeric materials under various conditions such as fluids, vacuum, and air. The effect of tip/ surface interaction that result in image alteration was discussed. Mitchell et al. ( 2 1 4 ) reviewed (17 references) the techniques for electron and optical microscopy of fracture surfaces and the use of etching and acoustic imaging to reveal structure in polymeric components. 578R
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The preparation of aramid fiber-epoxy resin, carbon fiberethylene-propylene copolymer, and glass fiber-polypropylene samples for light microscopical study was discussed by Schemme and Ehrenstein (215). Diamond and alumina powder polishing effects were examined in detail. Model polyurethane foams with large cells were prepared by Steger et al. ( 2 1 6 )and localized analyses across single cell membranes were completed by IR microscopy to measure membrane thickness as well as polyurethane and polyurea content. Studies contributed to the understanding of cell opening and stability. Janik and Foks ( 2 1 7 ) reviewed (65 references) various microscopical techniques and results from the examination of segmented polyurethanes. They also characterized the morphology of segmented polyurethanes and a polyester prepolymer ( 2 1 8 , Z 1 9 )usingvarious polarized light, reflected light, and electron microscopical techniques. Knoll et al. ( 2 2 0 ) reviewed the use of evanescent light for optical characterization of ultrathin polymer films. The dispersion of carbon black particles, a determining factor in the physical properties of polymer composites, was investigated microscopically by We et al. ( 2 2 1 ) . See also: References 16, C9, D7, D13, El, E2, E4, E7, E12, E21, E22, G9, H7, K17, K20, K21, K24, K46, K50, M26, M27, M29, M30, 0 6 , 0 8 , T1, V3, W4, and Y1. AA. TEXTILES, FIBERS, AND FILMS Annis et al. ( A M ) reviewed (27 references) useful instrumentation and sample preparation techniques for routine textile microscopical analysis. Confocal and differential phase imaging of thin organic films was discussed by Hudson and Wilson ( A M ) . Theoretical models of the images provided measurements of film thickness, permittivity, and quality. The optical characteristics of Teflon AF fluoroplastics were examined by Lowry et al. (AA3). The new materials are optically transparent in the visible and near-IR and are chemically inert. Yoshida ( A M ) reviewed (8 references) the use of laser holography and scanning laser acoustic microscopy for nondestructive testing of fiber-reinforced plastics composites and monitoring delamination, impact damage, and local irregular orientation of fibers within the composites. Visible and near-IR cathodoluminescence of bismuth strontium calcium copper oxide and yttrium barium copper oxide films were investigated by Dominguez-Adame et al. (AA5). Kuz'min et al. ( A A 6 ) provided a review (81 references) presenting the status on optical studies of the surface structural layers of liquid sytems. The thermal behavior of Langmuir-Blodgett films were studied by Leuthe and Riegler ( A A 7 ) through reflection polarized light microscopy and X-ray diffraction techniques. Coexisting polymorphism, thermal annealing, and epitaxial layer growth of behenic acid multilayers were characterized. Pitkethly ( A M ) reviewed the use of microscopy in the evaluation of fiber-matrix interfacial properties. Biaxial and uniaxial corona-treated polypropylene films were characterized by Overney et al. ( A A 9 )with atomic force imaging.
Stanley (AAIO) illustrated and outlined the variety of microscopical applications, and the reliance on microscopical analysis and instrumentation, in leather research and manufacturing. The morphology of slip deformation bands of uniaxially drawn, notched, high-density polyethylene films was characterized by Morita et al. ( A A I I ) using SEM imaging. Nile red served as a useful probe for Jurdana and Leaver (AA12) in monitoring the penetration of solvents into keratin fibers. An elastic recoil detection technique with high depth resolution for thin-film analysis was developed by Dollinger et al. (AA13). Kaufman et al. (AAI4)provided a discussion of microscopes and microscopical techniques for measuring the optical behavior of plastics in order to characterize their macroscopic properties and processing defects. Practical examples include nylon 6, polyester fibers, and biaxially stretched polymer films studies, illustrating the versatility of microscopy in evaluating mechanical strength. Direct observations of transitions between condensed Langmuir monolayer phases were made by Schwartz and Knobler ( A A I 5 ) using polarized fluorescence imaging which permitted distinction of domains of different tilt azimuth in condensed phases of fatty acids. Schwartz et al. (AA16) also quantitatively determined the character of the surface order of the outermost layer of thin Langmuir-Blodgett films of cadmium arachidate, in air and water, using atomic force imaging. Splay strip textures in the liquid phase of Langmuir monolayers, characterized by Ruiz-Garcia et al. (AAI 7) using polarized fluorescence and Brewster angle microscopy, were found to be associated with regular variations in the molecular tilt azimuth. The capability of FT-IR grazing angle microscopy for microspatial chemical mapping of polymer organic and inorganic films on reflective substrates was put forth by Eng and Shebib (AA18). A perfluoropolyether lubricant film study was included. Nikitenko and Savranskii ( A A I 9 ) obtained images of Langmuir monolayers on transparent substrates using Brewster’s angle microscopy with a p-polarized laser. A rotating compensator-type polarizer compensator sample analyzer ellipsometer was described by Henck (AA2O) for in situ real-time thickness measurements during the etching of poly-Si films. A relative transmission fringedepth method for determining the optical constants and thicknesses of thin semitransparent films was put forward by Zhang et al. (AA21). Twenty two of the 47 papers presented at the 1992 International Conference on Microscopy of Composite Materials were published in the Journal of Microscopy (AA22). They included works on electron optical technique, acoustic imaging applications, scanning probe technique, and Raman, optical, and confocal scanning laser microscopical instrumentation and methodologies, giving a range of magnifications and resolution, structural, compositional, and internal microstructural images and information. Materials investigated included inorganic composites, fiber-reinforced ceramic matrices, and light metal alloy matrix samples reinforced with
particulate matter or silicon carbide filaments. A few of the contributions are referenced in this review. Mackenzie and Grant (AA23) provided an overview of the papers presented and the range of information from the various imaging techniques. Craven (AA24) introduced a method for detection of cavitoma in cotton fibers utilizing SEM technique. Reported advantages over current microscopical technique included increased resolution, depth of field, speed of analysis, and analysis capabilities after thedyeing process. Craven (AA2.5) also described a preparation method for cross-sectional measurement of fibers using image analysis and SEM; fibers are embedded in an epoxy resin, cured, cross-sectioned, and treated with 3% aqueous acetic acid. Measurement of the replica offered improved fiber edge definition and depth of field. Schaefer and Hoecker (AA26) detailed the need for and acquisition of combined data from UV, fluorescence, and scanning photometer microscopy in studying the localization and distribution of UV-active and fluorescent textile finishing agents in wool. Zhu et al. (AA27) used scanning tunneling imaging and UV-visible spectroscopy to characterize lead sulfide ultrafine particles synthesized in Langmuir-Blodgett films. See also: References C9, C12, E l , E4, E7, E10, E l 1, E16, E22, E23, F4, F5, K3, K20, K31, K56, K57, M1, M3, M7, M9, M10, M25, M29, M30, M32, T1, X9, 23, GG1, GG2, GG9, 5512, 5513, and 5517.
BB. WOOD AND PAPER The confocal laser scanning microscope provided a nondestructive method of monitoring sectioning pulp and paper sample integrity for Moss et al. (BBI). Drying proceses and distribution of fines were examined. Fiber structures were characterized and the use of this noncontacting profilometer was described and compared with those obtained by conventional tests. Cross-sectional images of cellulosepulp fibers were obtained by confocal laser scanning by Jang et al. (BB2). The technique allowed simplified sample preparation over mechanical microtome sectioning. An image analysis procedure was developed for rapid and accurate measurement of fiber crosssectional area and wall thickness. Reif et al. (BB3) explored the use of FT-IR microscopy for surface evaluation of coated paper measuring the relative binder composition and describing the chemical composition of the surface topography. Kropholler and Moss (BB4)utilized low-temperatureSEM, which permitted the examination of wet pulp and paper, thus avoiding problems associated with drying. The effect of milling on cell wall delamination was explored. Robertson (BB5) described the use of phase-contrast microscopy as a diagnostic instrument for the examination and differentiation of the complex microbial population in the deposit matrix of a paper mill. PAPI binder distribution on wood particles and in particle boards was investigated by Roll (BB6). Fluorescence imaging, with proper filter selection, facilitated reliable distinction between the PAPI and wood, allowing routine detection and quantitative studies through digital image processing. Analytical Chemistry, Vol. 66, No. 12, June 15, 1994
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Kojima and Fukazawa (BB7) reviewed (6 references) the methodology and applications of microspectrophotometry for pulp and paper study. Fukazawa (BB8) provided a review (39 references) of the applications, experimental techniques, and limitations of UV microscopical methods for the study of lignin in the solid state. The use of scanning laser optics combined with traditional macroscopic optical measuring techniques to monitor the consistency of pulp and paper was described by Preikschat (BB9). A final report by Preikschat (BBZO)and others included a discussion on how traditional limitations in measuring optical consistency were overcome, such as the ability to measure consistency in the presenceof small amounts of filler additives, sensitivity to pulp grade changes and entrapped air bubbles, varying amounts of black liquor carryover, and changes in color, brightness, and freeness. Johnson and Kamke (BBl I) developed staining techniques that provided a sharp contrast between cured adhesives and wood substrate when using fluorescence microscopy. Gross adhesive penetration into wood was then quantified by utilizing image analysis of the contrast. Donaldson (BBZ2) reviewed (24 references) the use of interference microscopy for measuring the lignin distribution in sections of wood or cellulose pulp fibers. See also: Reference 17. CC. COAL Matzakos and Zygourakis ( C C I ) developed a novel thermogravimetric reactor with an in situ video microscope that allows direct viewing of video recording of coal pyrolysis and combustion. Bensley and Crelling (CC2) reviewed (21 references) the in situ UV-fluorescence microspectrophotometry of coal macerals for rank analysis and detection of weathering in coals. An automated analytical SEM and image analysis method was implemented by Galbreath et al. (CC3)for characterizing the inorganic phases in coal and coal combustion products. Hippo et al. (CC4)demonstrated the possibility of imaging coal and coal-derived material with scanning tunneling microscopy. Existing quantitative fluorescence microscopical techniques were applied by Rathbone et al. (CC5, CC6) to characterize nondistillable coal residues. The spectral distribution and fluorescence intensity provided new insight into the composition, structure, and reactivity of the coal liquids and might be of use in more effective monitoring of control processes. The evolution of chemical structure of resinite during oxidation was monitored with a combination of optical microsocpy, FT-IR photoacoustics, and NMR by McFarlane et al. (CC7). The changes observed optically had a direct correlation with molecular changes determined by FT-IR and N M R spectroscopy. DD. EMULSIONS
A review (1 14 references) of emulsion characterization techniques emphasizing optical methods was provided by Mikula (DDZ). The spreading dynamics of a drop edge were studied experimentally by Chen and Wada ( 0 0 2 ) using a laser light 580R
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interference microscopical method; edge profiles and dynamic contact angles were characterized. See also: References G11, H2, H3, H4, 516, 533, K27, L33, V5, X12, and MM3. EE. MINERALS Smith ( E E l ) reports that the MinIdent database now includes optical data including refractive indexes, color, 2V, orientation of optic axial plane, dispersion, and reflectance at 470, 546, 589, and 650 nm. Optic sign, birefringence, and symmetry can also be used for identification. MinIdent ranks possible matches in order of merit rather than simply matching input data with stored data. MinIdent includes data for more than 4600 mineral species. The database use, originally containing physical and chemical properties, is now expanded for use with reflected light and polarized light microscopical methods. Redmond et al. ( E E 2 ) provided an extensive review (149 references) on the experimentation and interpretation of cathoduminescence microscopy and spectroscopy applied to the microcharacterization of mineral materials. Applications and potential applications in mineralogy were summarized, the merits and limitations of available techniques illustrated, and the origins of intrinsic and extrinsic luminescence in crystals discussed. Bryant ( E E 3 ) once again put forth an economical adaptation to a polarized light microscope for Vickers hardness and reflectivity of minerals. A simple vertical illuminator coupled with a metallograph light source extends the microscope’s use for ore mineral identification. A method for locally determining 2V in optically inhomogeneous crystals was put forth by Fortsch et al. (EE4) using a novel application of spindle stage techniques. A special milling tool cut cylinder-shaped sanidine crystals perpendicular to the optic axial plane, which were then mounted with the cylinder axis parallel to the spindle axis. The 2V values were directly determined from extinction position measurements on rotation of the spindle viewed in the 45O position between crossed polars. Petford ( E E S ) reviewed (9 references) confocal scanning laser imaging for mineral examination. Sample material and preparation, equipment, and experimental conditions appropriate for fission track imaging, surface relief examination, and mapping of zoning patterns were presented. Roedder ( E E 6 ) reviewed the advantages and limitations of the use of polarized light microscopical techniques in the characterization of phases within fluid inclusions in minerals. A spindle stage mounted in a polarized light microscope with a Nakamura half-shade plate was used by Armbruster and Bermanec ( E E 7 ) for the determination of the optical indicatrix dispersion of low albite at wavelengths of 480,540, 589, and 630 nm. Results demonstrated the value of the highaccuracy measurements afforded by the technique in detecting dispersion within the visible wavelength. Liang (EE8) explored the use of scanning FT-IR microscopy for the identification of minerals in polished rock sections. Mineral identification is based on reflectance measurement in the mid-IR range with the content of identified minerals estimated by comparison with spectra of mineral standards.
Zoning and fluid inclusions in pyrite were characterized by Richards and Kerrich (EE9), using transmitted IR light microscopy. Confocal scanning laser techniques were used by Petford and Miller (EEIO) to record and measure the 3-D orientation of selected fission tracks in apatite grains. The system provided means of measurement of inclined fission tracks not possible in transmitted light. Color cathodoluminescence SEM studies by Zezin (EE1I) revealed new growth features of natural diamonds. Marschallinger et al. (EEI 2 ) reviewed a method for 3-D reconstruction of chemically zoned garnets using computercontrolled digital image processing with 3-D modeling software. EPMA/SEM- scanned serial sections were reconstructed, producing 3-D chemical and phase images. A statistical method was developed by Marabini et al. (EEI3) for obtaining particle size distribution of dimeric idiomorphic minerals using a polarized light microscope with camera attachment. The technique is based on processing diameter/height ratio of particles considered cylinders with constant diameters. Surface features of calcium bentonite and sodium bentonite that were pillared with alumina clusters have been characterized by Ocelli et al. (EE14) using atomic force microscopy. A laser microscope was presented by Meisner et al. (EEI 5 ) for determining luminescence and acentric mineral phases in ores, rocks, and their byproducts. The method is based on optical-geometrical, quantum-ptical, coherent microscopy and photoluminescence. The composition and linear and nonlinear optical parameters on scheelite and apatite were determined. Interactions of xanthan gum and mica were examined, utilizing atomic force microscopy, by Meyer et al. (EE16) in an effort to better define adsorption on mineral surfaces during enhanced petroleum recovery. An entire issue of The Microscope (EEI7) contains contributions from an International Symposium held in honor of F. Donald Bloss in 1990. Abbott (EEI8) advanced the use of point-dipole theory to include calculation of the orientation of the optical indicatrix in homogeneous monoclinic and triclinic crystals from structural data and electronic polarizabilities. Gunter and Ribbe (EEI9) explored the correlation of measured microscopical optical properties and crystal chemistry in natrolite group zeolites. Gunter (EEZO) penned an optical mineralogy chapter in The Encyclopedia of Earth System Science. See also: References 8,9, 17,25,29, C2, C3, C5, C7, C8, E27, M12, M13, N1, N4, V8-Vl0, X9, FF9, FF12, FF15, JJ10, PP1, PP6, and PP10.
FF. CEMENT AND CONCRETE Lange et al. (FFI)analyzed surface roughness by optically acquiring confocal images and then transforming those sectional series into digital images and a topographic map by using a straightforward algorithm to derive a roughness parameter which allowed characterization of surface texture and fracture surfaces of silica fume pastes, control paste, and various cementfsand mortars.
A fully automated image analysis system for the microscopical determination of air void characteristics in hardened concrete was developed and described by Laurencot (FFZ). The 68 papers from the 14th and 15th International Conference on Cement Microscopy (FF3, FF4) emphasize microscopical technique for the evaluation of clinker, concrete, and building materials focusing on the relationship between processing technique and the properties of the product; all papers are referenced. As in previous years, the papers offer a comprehensive reference and an array of authoritative techniques for the practicing cement microscopist. Many analytical methods integrate polarized light microscopy and reflected light microscopy with other instrumentation. A few papers from the proceedings appear in this review, including the introduction of a novel personal SEM. Mitchell and Davis (FF.5) described techniques for the uniform measurement of fluorescence intensity and spectra that were developed and applied to the characterization of raw asphalts. A simple preparation method for microscopical evaluation of the phase composition and internal structure of portland cement clinker during cement plant operation was devised by Chromy (FF6). Select granules are crushed, screened, embedded in epoxy resin, polished, and stained before microscopical examination. ONeill (FF7)described simple microscopical methods for detection and identification of various sulfate materials in hardened concrete. Jie et al. (FF8) discussed sample preparation techniques and instrumentation used in investigating and monitoring hydration and degradation reactions under varying field and laboratory conditions; temperature *relics” in steam-cured concrete were analyzed, integrating PLM and fluorescence images with SEM imaging and EDS. Price and Caveny (FF9) explored the use of FT-IR microscopy for cement crystal-phase identification and examination of organic additives to various cement microstructures. The extent of carbonation in concrete was clearly traced by Curtil et al. (FFIO) by applying polarized light microscopical technique. Wakeley et al. (FFII) investigated the potential use of petrographic techniques for monitoring cement-solidified hazardous wastes. The effectiveness of waste dispersion in the cementing medium and distribution of cracks was investigated with PLM, SEM, and high-resolution X-ray mapping. Caveny (FF12) demonstrated the potential of an environmental scanning electron microscope in investigating cement hydration. The instrument is capable of operating at higher pressures, allowing wet cement samples to be analyzed in a more natural environment. New gel phases and crystal growth mechanisms were observed. Jang and Love (FFI 3) recounted the daily routine use of polarized light microscopy in the evaluation of kiln operation and monitoring of clinker quality. Microscopic cracks in precast, prestressed concrete railway sleepers were characterized by Shayan and Quick (FFI 4 ) . Draper and Skalny (FF1.5)discussed the use of computercontrolled stages with appropriate software that permitted Analytical Chemistry, Vol. 66,No. 12, June 15, 1994
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relocation of identical observed sample areas in and between stereoscopes, petrographic microscopes, and scanning electron microscopes. Digital imaging and database techniques allowed storage and retrieval of images from any of the instruments. A polished concrete section demonstrated the potential for integrating and complementing each instrument’s capabililities. See also: References 17, B12, and C9. GG. GLASSES, CERAMICS, AND ABRASIVES Subsurface damage induced by Vickers hardness indentation tests and single-particle impacts in ceramic-matrix composites was characterized by Powell et al. ( G G I ) using conventional reflected light methods and standard metallographic techniques. A more rapid, nondestructive analysis was ultimately employed which used confocal scanning laser microscopical techniques. Various ceramic-fiber composites were acoustically evaluated by Briggsetal. (GG2). Contrastwasdominatedbystrong excitation of Raleigh waves in the surface which contrasted different phases, revealing cracks and interfaces by characteristic patterns. Tanaka (GG3)reviewed (1 8 references) the principles and methods for residual stress measurement in ceramic/metal composites by scanning laser microscopy. Acoustic micrographs of phase-transformed regions surrounding Vickers indentations yielded microstructural information of deformed, partially stabilized zirconia ceramics for Fagan et al. (GG4). Contrast was due to interaction of the Raleigh waves and microstructure. Ikeda et al. (GG5) reviewed (12 references) ultrasonic testing and ultrasonic-wave acoustic imaging in ceramics evaluation. Microcrack damage in alumina ceramics was investigated using scanning acoustic imaging by Pangraz et al. (GG6). Small-angle X-ray scattering aided in determining microcrack formation. Polarized light microscopy afforded Fischer et al. (GG7) a quick study of large sample areas allowing high local resolution, fast texture identification, and crack detection in injection-molded ceramics. Quantitative failure analysis was demonstrated in combination with the turntable method according to Fedorov. A recently developed interferometric method was presented by Castell et al. (GG8) for the study of sol-gel transition in ceramic systems. An issue of The Journal of Microscopy (GG9) contains many contributions on the microscopical characterizations of composites including acoustic imaging, Raman microscopy, scanning probe and confocal imaging, and electron optics studies of fibers and composites. See also: References 8, C9, D15, H5,J17, K18, K32, M9, M10, M14, M17, M18, M20, M21, M32, N4, P2, T1, W1, Z5, Z15, and GG9. HH. METALS Kodai et al. ( H H I )reviewed (7 references) the applications of scanning acoustic imaging in metallography. Buscher and Reimer (HH2) mapped magnetic domain surface structures through Kerr scanning optical microscopy 582R
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principally based on the rotation of reflected plane polarized light from a magnetic surface. See also: References 53, K15, K23, K30, K51, M1, M3, M4, M6, M16, M21, M33, N2, U2, and X2. 11. SEMICONDUCTORS AND ELECTRONICS Digital laser imaging in real time was explored by Worster and Politzer (ZZI) for analyzing and reviewing defects on patterned semiconductor wafers. Three-dimensional images with enhanced spatial resolution and depth discrimination were reported. The method facilitates the need for complex defect identification, archiving, and data communication without the need for vacuum sample preparation. Quate (ZZ2) reviewed (39 references) the role of scanning probes in the fabrication of nanometer size structures on the surface of semiconductor wafers. Early stages of cathodic disbonding in microelectronics were distinguished by Kending et al. (113) using scanning acoustic imaging; in situ degradation of the interface of a 2-hm polyimide coating on Al-metalized Si02 was followed. Watanabe et al. (114) put forth a medium for acoustic imaging of solder in electronic components. An improved 3-D model for simulating cathodoluminescence in a semiconductor under electron-beam irradiation was developed by Phang et al. (ZZ5). Joseph et al. (ZZ6) developed and illustrated thecapabilities of a confocal laser scanning microscope system which allowed high-resolution reflected light imaging through heavily doped silicon. A 500 M W 1064-nm Nd-YAG laser gave the best performance for both Si transmittance and the optics of the microscope system. Reflected light images were obtained through 400 Fm of PtSi. Yoshioka (117) reviewed (2 1 references) surface analysis techniques for analysis of electronic materials. A new method for investigating the vertical position of nanometric defects in semiconductor materials was described by Castagne et al. (118). Submicrometer measurements are made by numerical performance on both the 3-D observation of the Fourier transform and the z-position location of the point source from the Fourier phase shift. Seealso: ReferencesC9,E3,E9,E13,E16,K7,Ml,M19, M20, M21, Q3, and AA20.
JJ. FORENSIC SCIENCE The sensitivity and specificity of microcrystal tests were lauded by Wielbo and Tebbet ( J J I )for the initial examination of controlled drug powders. Preliminary and confirmatory tests were carried out by combining microcrystal microchemical technique and micro-FT-IR analyses. Examples were given. Kirchhoefer (JJ2) reports that the USFDA screened more than 1400 drug samples for potential generic fraud by a combination of techniques. Excipients were examined rather than active ingredients. Polarized light microscopy, chemical tests, and liquid and gas chromatography were the most useful tools to differentiate formulations not resolved by FT-IR, TGA, or physical comparisons. A library of 37 IR spectra for drugs and other powders for stretching drugs, such as saccharoses, was generated by Kohn and Jeger (JJ3).
By way of example and illustration, McCrone ( J J 4 ) demonstrated the forensic value underlining the practical use of microcrystal tests to defeat any Frye rule challenge. Harris and Kane (JJ.5)combined preparative TLC followed by wick evaporation for yielding small crystals of pure LSD in a form suited for micro-FT-IR analyses. Examples of establishing provenance and travel history of illicit drugs through light microscopical applications of palynology were cited by Stanley (JJ6). Hartshorne and Laing (JJ7) developed and tested a glass calibrant for use in standardizing absorbance measurements made with different microspectrophotometers. Its use in a collaborative study for measurement standardization and detection of instrument faults was discussed. Examples and discussion of the use of FT-IR analyses using a diamond anvil cell with a beam condenser and an IR microscope for the examination of controlled particulate drug mixtures were given by Suzuki (JJ8). FT-IR use minimized diamond absorptions. Nanogram particles can be analyzed. Wilson (JJ9) provided a review of drug analyses relevant to forensic investigations. McCrone (JJZO)provided a review for the microscopical examination of soils, with detailed discussion and examples of procedural steps using polarized light microscopy and associated techniques for the identification of mineral components. A quick and simple scheme for the microscopical examination of soils was described by Fraysier and Van Hoven (JJ1Z). Primary emphasis is placed on dispersion staining (focal masking) to monitor refractive index, but optical properties such as color, birefringence, and relief are used as well. Robertson (JJZ2) provided an overview on different protocols of forensic fiber examination. Carol (JJZ3) reviewed microscopical methodologies available for fiber identification and comparison. Examples illustrating the value of microscopical analysis of human hair for the diagnosis and understanding of hereditary and metabolic defects were given by Ferguson (JJZ4). Gorski and Brauner (JJ15) reported a morphologic abnormality, discovered with polarized light microscopy, in the hair roots of patients from a methadone clinic in Israel. Kisin and Golovin (JJ16) demonstrated the wide possibilities offered by SEM methodology in the comparison and characterization of hair. Experimental data on pigment granules within the medulla were presented. Dunlop (JJZ7) reviewed (18 references) the use of microspectrophotometry for the forensic color analysis of textile fibers. A review on the applicability of SEM in forensic examinations was provided by Keeley (JJZ8). Zeichner and Glattstein (JJZ9)found that the transmission spectra of small samples of inked paper fibers crushed on glass slides resemble spectra of smeared ink deposits. This technique produced more reproducible spectra than inked fibers in a mounting media and may be advantageous when ink tissues on tinted paper are examined. General spectroscopic processes associated with the use of FT-IR microscopy of the forensicexamination of paint samples
were described by Allen (JJZO). Full experimental procedures are given for 11 methods of sample preparation with respect tovarious sampleconditions such as substrate, size, and degree of fragmentation. McCrone et al. (JJ21) discussed the microscopical identification of organic high explosives and high-explosive mixtures. Complete optical crystallographic data and procedures for microscopical dientification were included for TNR, TNT, ammonium picrate, PETN, RDX, picric acid, HMX, DINA, and EDNA. Further discussion for aromatic nitro compounds included the following: 1,5-DNN; 1-DNN; 2,4-DNP; 2,4-DNR; 4,6-DNR; 2,4-DNT; 2,6-DNT; HND; 1-MNN;picric acid; TENA; TNA; TNB; 1,2,5-TNN; 1,3,5TNN; 1,3,8-TNN; TNR; TNT; ammonium picrate. Nitramines and nitrates included the following: PETN; RDX; Tetryl. Mixed high explosives included the following: Alumatol; Amatex; Amatol; Ammonal; Baratol; composition A; composition B; composition C; Ednatol; Ednatal; Minol No. 1; Minol No. 2; Minex; Pentolite; Pentonal; Plumbatol; Schneiderite; Tetratol; Torpex No. 1;Torpex No. 2; Trimonite. Miscellaneous high explosive mixtures included the following: PETN/wax, 8,13, or 18; PETN, 85, crown oil, 15; picric acid/DNP; picric acid/wax; RDX/PETN; RDX/TNA; RDX/wax; RDX, 22/NHdNOj, 73/wax, 5 ; RDX, 72/Tetryl, 12/TNT, 16; TNT/Al; TNT/dinitronaphthalene; TNT/ HND; TNT/TNA; TNT/wax; TNT/Tetryl/wood flour; Tetryl/Al. The abrasives of 16 commercially available toothpastes were analyzed by Bailey (JJ22);the optical properties useful for microscopical identification were compiled. Microspectrophotometry and SEM, in combination with EDS, were evaluated by Choudhry (JJ23) for use in the comparison of minute lipstick samples. The advantages and disadvantages of tape lifting, glue lifting, and concentration technique sampling for SEM-EDX analysis of gunshot residue were discussed and summarized by DeGaetano et al. (JJ24). An immunohistochemical method using the antibody for pulmonary surfactant for the diagnosis of asphyxia was put forth by Morita et al. (JJ25). See also: References 10,13,14,17,25,29,66,72, C3, C7, C9, AA10, AA11, AA24, EE1, MM2, "1, "4, and PP2.
KK. FOOD AND FEED Flint (KKZ)reviewed (3 references) various microchemical and histochemical tests available to the food microscopist. Tandem scanning confocal imaging allowed MacDonald et al. (KK2) to investigate the dynamics of bubble formation and the influence of small particles on effervescence in carbonated beverages prepared and packaged under partial pressure of COZ. A polarized light microscopical method was devised for the quantitative measurement of the changes in light intensity during the loss of birefringence of starch granules in aqueous urea. Kim et al. (KK3) discussed the use of the technique in the evaluation of native potato starch, hydroxypropyl potato starches of varying molar substition, and hydroxypropyl and cross-linked potato starch. A microspectrophotometer with high-pressure xenon lamp and grating monochromator aided Rooney and Fulcher ( K K 4 ) Analytical Chemistry, Vol. 66,No. 12, June 15, 1994
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in differentiating and characterizing 13 common insoluble fibers used in bakery and dietary products. a-Cellulose, soy, cottonseed, pea, oat, and oat hulls had distinct spectra measured at 230-350 nm. Mandanis (KK.5) described the use of an FT-IR microscope equipped for horizontal attenuated total reflectance for the rapid identification of food packaging materials and coatings. Instrumentation for fluorescence imaging as an analytical tool was reviewed (29 references) by Irving and Gallant (KK6). Roles in food research and quality control demonstrated its practical application. Wetzel and Reffner (KK7) used spatially resolved FT-IR microspectroscopy for direct in situ examination of the microstructure of wheat kernels. Despite optical obstacles, useful spectra linked with morphology were obtained from thin sections. Insoluble contaminants from sucrose manufacture were characterized by Van Geijn (KK8). The use of microscopical nuclear magnetic resonance imaging was attempted by Ruan et al. (KK9) for the simultaneous and nondestructive measurement of transient moisture profiles and structural changes in corn kernels during steeping. Reisterer et al. (KKZO)described a method used to evaluate cleaning and sanitizing procedures used in cleaning membranes after concentration whey. Protein foulants including polypeptides were stained with coomassie blue and viewed on polysulfone membranes with a microspectrophotometer set for reflectance at 580 nm. Procedures for purification and modification of muscle proteins and fluorescent probes useful for structural studies on isolated myofibrils and muscle in relation to its properties as a food were discussed by Swartz et al. (KKI 1). Thedistribution of aromatic compounds in coastal bermuda grass cell walls was investigated by Ames et al. (KKZ2)using UV absorption scanning microspectrophotometry. Varying the wavelength resulted in similar but not identical images, suggesting that variations in the chemical structure of the aromatic compounds within the cell wall could be detected by the techniques. Ultraviolet absorption microspectrophotometry was useful for Akin and Rigsby (KKZ3) in the location and characterization of phenolic compounds within cell types of warmseason and cool-season grasses exposed to selective biodegradation. Akin and Hartley ( K K I 4 ) used the technique to evaluate the walls of sclerenchyma, vascular bundle sheaths, and parenchyma at different maturities in relationship to wall digestibility. Hung et al. (KK15)described a direct epifluorescent filter technique for the rapid and accurate enumeration of bacteria in raw milk. Connell and Cottell (KK16) put forth an improved, and reliable sample procedure for cells grown in culture for electron imaging. Cells are cultured in a monolayer on a Millipore type A membrane filter and processed. Cut filter pieces are encapsulated in an 00 BEEM resin-filled capsule and polymerized. See also: References 10, E28, and "1. 584R
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LL. BIOLOGY AND MEDICINE The development of an improved 3-D method for the fast, precise mapping of osteoclastic resorption was discussed by Jones et al. (LLZ). Video-rate confocal laser scanning imaging and dedicated software allowed for fast and precise measurement of resorption pit depth, area, and volume in order to quantify cell function. Cullen et al. (LL2) reviewed (26 references) biological applications of scanning probe imaging techniques, noting their spatial resolution and ability to observe samples in aqueous rather than vacuum environments. The group illustrated and discussed manipulation and molecular resolution of proteins, dynamic observation of protein adsorption, the effect of atomic force microscopy, and the ability for cell surface studies. Petrol1 et al. (LL3) developed a new objective lens which was used in combination with real-time acquisition procedures to obtain in vivo sequential serial sections from a rabbit cornea. Three-dimensional reconstruction of the corneals cells was accomplished through digital registration and stacking of sections on a computer. The technique provides a useful method for observing 3-D structures and analyzing 4-D phenomena at the cellular level. The manufacture, construction, and performance of a special sample chamber for biological specimens suspended in aqueous solution was described by Goncz et al. (LL4). Cathodoluminescence-emitting lipid droplets in rat testes were examined by Ning et al. (LL5), using analytical color fluorescence electron microscopy. The studies demonstrated the system's value for in vivo observation of specific compounds not visualized by other methods. Confocal laser scanning images were exploited by Kawachi (LL6) to investigate the mechanism of calcium wave propagation between paired heart muscle cells. Teunis et al. (LL7) developed methods for real-time 3-D tracking of fast moving microscopic objects with only slight modifications to the microscope. Anaxial illumination was used in the high-speed recording of stereoscopic images in two different, described setups. An improved method for estimating background fluorescence intensity for intracellular free calcium ion distribution with video fluorescence microscopy was put forth by Miyakawa (LL8). Miyakawa (LL9) also introduced an improved system for superimposition of calcium distribution and cellular microscopical images with transmitted light or Nomarski differential contrast. A two-excitation fluorescent video microscope was patented by Fay and Dellaville (LLIO). The microscope includes the following: a UV radiation source capable of a plurality of UV excitation wavelengths; a filter device to select a first and second wavelength from the plurality of excitation wavelengths; a sample changer to hold a sample for illumination by the radiation; a photometer to measure the intensity of the excitation wavelength(s) to generate an intensity signal representative of the measured intensity; and a processor in communication with the photometer to record the intensity signal. A microscope system for use in measuring the pH or enzyme activity of a biosensor membrane containing a pH indicator
or redox indicator for defect screening was described by Saito and Shionya ( L L l l ) . Two techniques, employingboth reflectance measuring and direct observation with phase-contrast microscopy, were developed by Takoshima, Masuda, and Mukasa (LLI 2), allowing investigation of the aggregation structure of fatty acid monolayers at the air-water interface without using fluorescent probes. Bruckner et al. (LL13) reviewed (21 references) the microchemical methods used by the researchers during the last 10 years in the analysis of urinary calculi. The accuracy and efficiency of the results were compared to classical spectroscopic analytical technique. Morris et al. (LL14) compared scanning tunneling imaging of biological macromolecules with data obtained from other methods. Examples indicate that the technique is successful in obtaining high-resolution images of bipolymers deposited onto conducting surfaces. Slavik (LL15)reviewed (16 references) and provided an explanation of the major applications of fluorescent probes and labels used in cell biology research. Included were how fluorescence is measured, fluorescence parameters, probes of polarity, probes for ions, and limitations of probe applications. A flow injection system, in conjunction with a novel perfusion chamber, was applied by Scudder et al. (LL16) to fluorescence microscopical studies of cultured cells. The technique allows cells to be exposed to single or multiple reagent zones of almost any sequence, duration, or profile with computer-controlled precision. The formation of colloidal metal dispersions, used in the analysis of T-cell substrates by polarized light microscopy and flow cytometry, was accomplished by Siiman and Burshteyn (LLI 7) using aminodextrans as reductants and protective agents. An analytical correction factor was developed and introduced by Chen et al. (LL18)to counter the effect of refraction when making optical microscopical measurements of internal blood vessel diameter. Tamm and Kalb (LL19) reviewed (104 references) microspectrofluorometry on supported planar membranes. Tamm (LL20) provided a review (65 references) of the theory, instrumentation, and applications of total internal reflectance fluorescence microscopy. Nomarski DIC methods for the analysis of microtubules in vitro were laid out by Williams (LL2I). Cherry (LL22) reviewed (21 references) the tracking of cell surface receptors by means of fluorescence microscopy or colloidal gold particles. A fluorescent light microscope-based technique has been developed by Schwartz et al. (LL23) for rapidly constructing ordered physical maps of chromosomes. Initial optical mapping applications of Saccharomyces cerevisiae chromosomes was described. Current procedures for fluorescence microscopical analysis of cytoskeletal organization and dynamics were described by Wang (LL24). A new class of fluorescent dyes complexing DNA allowed Auzanneau et al. (LL25)to observe video images of individual single strands.
Engelhardt and Knebel (LL26) reviewed ( 2 2 references) the development,advantages, and limitations of confocal optics in applications of living cells, simultaneous fluorescence detection, and 3-D image processing in cancer research. Espada et al. (LL27) report that hematoxylineosin-stained tissue sections can be routinely analyzed by fluorescence microscopy. The emission of eosin 4 allowed easy and precise recognition of eosinophillic structures in grasshopper and mammalian testes. Ho et al. (LL28) demonstrated the use of dark-field illumination of May-Griinwald-Giemsa stained blood smears for the distinct delineation of eosinophils from other hematopoietic cells. The surfaces and interiors of wet spores, potential skin substitutes, were studied by Hanthamrongwit et al. (LL29). Confocal laser scanning imaging using water immersion objectives decreased the introduction of artifacts. Fujita (LL30) reviewed (21 references) the development, mechanism, and merits of confocal laser imaging in molecular cytology. Video epifluorescence microscopy permitted Viovy et al. (LL31)to make real-space observations of confined individual DNA molecules. Caldwell et al. (LL32) reviewed the use of confocal laser microscopy and digital image analysis in microbial ecological studies. Confocal laser scanning microscopy provided high-resolution images of the subcellular distribution of anthracyclines in parent and multidrug resistant cell lines for Coley et al. (LL33). Relocation of nuclear proteins around chromosomes a t mitosis was studied by Gautier et al. (LL34)utilizing confocal laser scanning microscopy. Biological and biomedical applications of UV lasers in confocal microscopy were discussed by Cannon and Armas (LL35). Fluorescence lifetime imaging and instrumentation were reviewed (104 references) by Wang et al. (LL36). Numerous biomedical applications were discussed. The techniques allowed quantitation of 2-D fluorescenceintensity distributions and lifetimes. Kornhauser et al. (LL37) put forth a modified nuclear emulsion coating technique for light and electron microscopical autoradiographs. The application of formvar was reversed to adhere to and cover thin sections placed on grids. The technique allows optimal conditions for specific nuclear activity tracing, prevents fogging caused by certain stains, and permits routine prestaining before emulsion coating. Lipp and Niggli (LL38)introduced a method for ratiometric confocal calcium measurements in isolated cardiac myocetes through the use of indicators with excitation spectra in the visible wavelengths. Rodgers and Glaser (LL39) reviewed (50 references) previous studies of fluorescence digital imaging of membrane lateral topology of lipid vesicles and labeled biological membranes. An improved preparation technique for light microscopy using extraction techniques of Spur’s resin sections was put forward by Wada et al. (LL40). Analytcal Chemistty, Vol. 66, No. 12, June 15, 1994
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formulation parameters such as component identification and Correlative light and SEM observations of incremental polymorphism. lines and cement lamellae of human molar apical cementum were made by Matsuo and Yajima (LL41). An evaluation of microscopical and laser light scattering methods for determining the physical stability of fat emulsions Warley (LL42) outlined the basic structure and function was given by Mueller and Heinemann ( M M 3 ) . of mammalian cells with the expressed intent of introducing materials microscopists to the rudiments of cell biology. See also: Reference "1. Via scanning tunneling techniques, Leggett et al. (LL43) examined relative humidity within an STM chamber and NN. MICROCHEMICAL ANALYSIS discussed the crucial role of water in image contrast formation Chemists and microscopists alike will appreicate Delly's when studying covalently immobilized protein molecules on ("I) historical and practical account tracing the evolution gold surfaces. of the chemical reagents that comprise the dedicated chemical A method using selective UV radiation fractionation microscopist's workbench. Enumerated and illustrated are followed by polymerase chain reaction allowed Shibata et al. the classic reagent blocks of Behrens, Chamot and Mason, (LL44) to obtain the specific and sensitive genetic analysis of the original set of bulk reagents from Chamot's laboratory microscopic tissue. classroom at Cornel1 University, and the chemicals in the Gilbert and Chemcraft chemistry set for young students along Mineuchi et al. (LL45)investigated the penetration of light with currently available Cargille microscopy sets. Of didactic and induced fluorescence associated with photosynthesis in interest is the compilation of the necessary reagents to perform relationship to an intact leafs morphology. The distribution all the experiments in Chamot and Mason's Handbook of of laser-induced fluorescence (Ar 477 and 488 nm) was traced Chemical Microscopy. microscopically with a CCD camera system, image intensifier, and microcomputer. Coates ("2) explored practical limitations of detection when using microcrystal tests for the presence of lead. Bronk et al. (LL46) detailed an approach to quantitate dynamic measurements of intracellular aminopeptidase activOdom ("3) proposed a single treatment of microscope ity in hepatocytes using multiparameter digitized video slides with RAIN-X to control drop size when performing microchemical tests. fluorescent microscopy. McClung and Feurstein (LL47)evaluated two intracellular Benko ("4) outlined a procedure for making a low-cost dyes, mepacrine and acridine orange, for epifluorescent video practically dispensible, stirbar centrifuge used in microchemimicroscopical observation of cell-surface interactions. The cal tests. two designed tests for the effect of incident light on platelet adhesion and determining sufficient light levels for accurate 00. ORGANIC ANALYSIS observations, which allowed longer exposures to light from 1 See also: References 15, 16, 18,22, C6, K1, S4, and AA2. through 30 min. Doglia et al. (LL48) report confocal fluorescence imaging PP. ASBESTOS ANALYSIS of nuclear and cytoplasmic drug fluorescence in living cells The new Test Method for the Determination of Asbestos permitted new insights into the mode of dry action not in Bulk Building Materials was compiled by Perkins and obtainable by conventional light microscopy. Harvey ( P P I ) . It replaces the interim method, 40 CFR, Part One of a new class of fluorescent dyes (YOHO-1) 763, Appendix A to Subpart F. It contains major revisions complexing DNA was evaluated by Auzanneau et al. (LL49) including detailed macroscopic examination procedures, for video microscopy of individual single-stranded DNA qualitative and quantitative polarized light microscopy promolecules in solution. The dye persists in denaturing condicedures, gravimetric preparation techniques, qualitative and tions, is stable under electrophoresis, and enables the imaging quantitative analytical electron microscopy methods, quality of stretched molecules. control/assurance guidelines, qualitative and quantitative See also: References 1, 10, 13, 14, 19, 20, 23, 24, 47,48, X-ray powder diffraction methodologies, procedures for the 51, 52, 56, 57, 65, 71, B3, B4, C4, D14, E28, F2, F3, F6, F8, preparation and use of calibration standards for each analytical F9, F10, F11, F12, F13, F14, F15, G3, G4, G10, G12, H6, technique, and an outline integrating each analytical technique 514, 520, 522, 525, 526, 527, 528, 532, K29, K46, K52, L1, for appropriate use in sample analysis. L3, L7, L10, L11, L14, L21, L23, L24, L33, L36, 0 3 , 0 5 , An EPA bibliography on surface contamination was put 0 6 , 0 7 , P3, P4, P5, 4 2 , Q4, 47-410, Q12, R2, R19, R20, forth by Brackett et al. (PPZ). The 144 references include R24, U1, V1,V4, V7, Vl2,Xl,XS,X7,X8,XlO,Yl,KK12,the following classifications: asbestos, aerodynamics, chemical and KK16. method, electron microscopy, experimental, lead, nonasbestos, optical microscopy, passive collection, radioactive substances, redispersion, risk assessment, soil, surface sampling, and MM. PHARMACEUTICAL theoretical. Additionally, Brackett et al. (PP3) outlined a The reference Pharmaceutical Analysis usingthe Polarized TEM methodology that uses MCE filters for the analysis of Light Microscope was penned by Watanabe ( M M l ) . asbestos fiber in water. Hu and Johnson ( M M 2 ) discussed the application of FTNIST (PP4)released the new Standard Reference Material IR microscopy in the examination of commonly encountered (SRM) 1867 to assist laboratories in the identification of pharmaceutical packaging components such as disposable regulated asbestos minerals by polarized light microscopy. syringes, rubber stops, and multilayered laminate films. The Bulk properties for each SRM (anthophyllite, tremolite, two also presented its use in the study of pharmaceutical 586R
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actinolite) include optical and crystallographic data as well as morphology, texture, and homogeneity. Verkouteren et al. (PP5) assessed the accuracy and precision of refractive index measurements using the doublevariation technique. Thorough procedures for calibration of narrow- and broad-band pass graded interference filters, fixedwavelength interference filters, immersion liquids, calibration glasses, and the hot stage were implemented and summarized in an effort to evaluate bias. The ability to measure matching wavelengths (Gs) was characterized, along with its effect on the calculated refractive index. Laughlin (PPS) reviewed (16 references) the role of dispersion staining (focal masking) in the microscopical identification of regulated asbestos minerals. Moss and McCrone (PP7)suggested simple means for preparing permanent preparations of asbestos fibers within Cargille refractive index liquids sealed with epoxy. Fibers maintained typical Us after two years, showing no apparent change in associated dispersionstaining (focal masking) colors. Fodor (PP8)reviewed the use of polarized light microscopy and IR spectrometry for the determination of asbestos content in fire dusts. Platek et al. (PP9) developed a computer-assisted digitized tablet technique of sizing asbestos fibers through the use of enlarged micrographs originally produced on the SEM. Wylie and Bailey (PPIO)compared size distributions of regulated chrysotile fibers, serpentine rock and composite particles detected at magnifications of 400X and 19OOOX for the purpose of assessing the NIOSH 7400 method in monitoring airborne fibers collected on membrane filters; TEM analysis may be necessary to adequately assess exposure. Nessler (PPII) briefly reviewed (3 references) the basic carbon coating preparation techniques for analytical electron microscopy. Millette et al. (PPIZ)demonstrated the capabilities of a vintage transmission electron microscope to analyze submicrometer-sizedasbestos fibers by both morphology and electron diffraction; grids were analyzed on a Phillips EM-200 using methods available in the 1960s. SEM imaging by Millette and Brown (PPI3) illustrated that the surfacial integrity of asbestos gasket materials may be predisposed to fiber release during abrasion. Yu et al. (PP14) demonstrated a method for the removal of calcium compound matrix materials from bulk samples through ammonium EDTA extraction. An analytical TEM was equipped with a microfilm reader by Verma et al. (PPIs)to characterize asbestos mineral fibers more quickly. Fibers are searched, counted, and sized with a microfilm reader and then identified on the TEM. Berghmans and Adams (PPI6)utilized electron energy loss spectroscopy (EELS) and electron spectrosopic imaging (ESI) for thelocalization oftitanium withinchrysotileasbestos. Visible beam damage was reduced by fitting a Zeiss EM902 with a cryoholder and performing ESI with the three-window background extrapolation method. Absorption effects in the quantitative X-ray microanalysis of asbestos mineral fibers by AEM was studied by Takao et al. (PPI7).
Seealso: References 17,20, C10, K22, K53, K54, Q1, S1, V8-Vl0, JJ10, JJ11, and 5524.
QQ. ART CONSERVATION/AUTHENTICATION Various preparation procedures of paint samples for FTIR microscopy were laid out by Allen (QQI). Full experimental procedures with observations as to applicability of various sample conditions including size, degree of fragmentation, and substrate are given. Guidelines to assist analysts are discussed. Combined cathodoluminescence measurements and EDX were utilized by Koschek (QQ2) in differentiating between zinc oxide pigments whose EDX spectra were virtually identical. Suggested was the possibility of distinguishing pigments on CL spectra and monochromatic CL micrographs. Shulz and Kropp (QQ3)discussed the use of microspectroFT-IR in the examination of paint binders on ground chalk. Turner and Watkinson (QQ4) suggested the use of FT-IR microscopy for the archeological and detection and examination of enamels. The use of Raman microscopy for the nondestructive analysis of pigments from medieval manuscripts was discussed by Best et al. (QQ5). The group (QQS)also analyzed pigments from an illuminated 13th century Paris bible. The spectra, script, and microscopical methods were presented. See also: References 6, 15, 21, 22, and 59. ACKNOWLEDGMENT Thanks to Walter C. McCrone for the opportunity and support. Thanks also to Debra Gilliand for tireless, accurate, and efficient typing. I appreciate the help of Mark Bukantis. The careful assistance of Annette Mambuca is gratefully acknowledged. I am indebted to my friend and colleague, John G. Delly, for his generous, sage advice and encouragement. LITERATURE CITED BOOKS OF QENERAL INTEREST Richardson, J. H. Handbook for the L&ht Microscope Noyes Publlcations: Park Ridge, NJ, 1991. Callaghan,P. T. Mn~lesoofNuclaerMa~blcResonenceMlcnwcopy; Clarendon Press: Oxford, U.K., 1991. Wilson, T., Ed. Confocal Mlwascopy; Academic Press: London, 1990. Richards, 8. J.; Footner, P. K. RMSMlcr0soopyHand;bOokM.25: The Role of Microscopyln Semiconductor FallweAnal)rsls;Oxford University Press: New York, 1992. ~ Press: Oxford, U.K.. Briggs, A. B. Acoustic h f k ~ o s c o pClarendon 1992. Russ, J. C. The ImageFrmesslng&ndbook CRC Press: Boce Raton, FL, 1992. Kok, L. P.; Bon, M. E. Mbvwave cwkbookforMlcrosoopists,314 ed.; Coulomb Press: Leyden, The Netherlands, 1992. Humphrles, D. W. The Remratbn of Thin Sectkms of Rocks, Mbhwls, and Ceramics; Oxford Unlverslty Press: New York, 1992. Yardley, B. W. D.; MacKenzle,W. S.; Q u M ,C. Atles ofkkrtamorphic Rocks and Thek TexWes Longman: Essex. U.K., 1990. Faegrl, K.;Iverson, J. Texfbook of Pokn Ana/ysls, 4th ed.;John Wlley and Sons: Somerset, NJ, 1969. Deleted in Braof. Echlln. P. LTbw Temperature Microscopy and Anal)rsls; Plenum Press: New York, 1992. Patterson. D. J.: Hedley. S. F r e e - L l W- Freshwater Rotoz&x WOne: London, 1992. Imes, R. The RacnrCal Entomologist; Aurum Press: London, 1992. Mayo, D. W.; Pike. R. M.; Butcher,S. S. Mlcroscak OrgankLaLw"ry, 2nd ed.; John Wiley and Sons: New York. 1989. Mayo, D. W.; We. R. M.; Butcher, S. S.; Trumper, P. K. Micfoscak Techniques for the Organ& Laboratgs John WHey and Sons: New York, 1991. Brady, Q. S.; Clauser, H.R. Materiels Haendbook: An €ncyc@ed& for Manam, T h b I Rofessbnak Pw&shgand F" khneg
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ers. Technicians, Supervisors, and Foremen, 13th ed.; McGraw-Hili: New York, 1991. Rossiter, B. W., Hamilton, J. F., Eds. Physical Methods of Chemism; Second Edition; Volume IV: Microscopy, John Wiiey and Sons: New York, 1991. Vetter, J. P., Ed. Biomedical Photography, Focal Press/ButterworthHeinemann: Stoneham, MA, 1992. Greenberg, A. E., Clescerl. L. S., Eaton, A. D., Eds. Standard Methods for the Examlnation of Water and Wastewater, 18th ed.; American Water Works Assoc. and the Water EnvironmentFederation: Denver, CO, 1992. Robinson, P. C., Bradbury, S., Eds. QuallitafivePo/ar/zedLl@?tMlwoscopy, Oxford Universlty Press: New York, 1992. Uneno, K.; Imamura, T.; Cheng, K. L. Handbook of Organic Analytical Reagents, 2nd ed.; CRC Press: Boca Raton, FL, 1992. Rawllns, D. J. LlghtMicroscopy, Bios Scientific PublishersLtd.: Oxford, U.K., 1992. Rawiins, D. J. L@htMicroscopy; An Electronic Textbook Bios Scientific Publishers Ltd.: Oxford, U.K., 1992. Murray, R. C.; Tedrow, J. C. F. Forensic Geology, Prentice Hall: Englewood Cliffs, NJ, 1992. Chen, C. J. Introduction to Scannlng Tunneling Microscopy; Oxford University Press: New York, 1993. Bracegirdle, B.; McCormlck, J. B. The Microscopic Photographsof J.B. Dance6 Sclence Heritage Ltd.: Chicago, IL, 1993. Abramowltz, M. Fluorescence Microscopy; The Essenfials; Olympus America Inc.: Lake Success, NY, 1993. Mange, M. A.; Maurer, H. F. W. H e a v y Minerals in Colouc Chapman and Hall: London. 1992.
ARTICLES OF GENERAL INTEREST Microsc. Anal. 1993, (1). Microsc. Today 1992, (1). Acta Mlcrosc. 1992, 7 (1, 2). Proc. R. Microsc. SOC.1993, 28 (4). Evennett, P. Proc. R. Mlcrosc. SOC.1893, 28 (4), 180-188. Evennett, P. Proc. R. Mlcrosc. SOC. 1993, 28 (4), 189-192. Haselmann, H. Proc. R. Mlcrosc. SOC. 1993, 28 (4), 166-188. Bracegirdle, B. Roc. R. Microsc. SOC. 1993, 28 (4), 196-201. Gundlach, H. Proc. R. Microsc. SOC.1993, 28 (4). 194-196. Bracegirdle, B. Proc. R. Microsc. SOC.1993, 28 (2), 55-62. Brook, A. J. Quekett J. Microsc. 1983, 3 7 (l), 1-6. Bradbury, S. Mlcrosc. Anal. 1993, (39, 5-7. Martin, L. V. Proc. R. Microsc. SOC.1992, 27 (2), 104-105. Sanderson, J. B. Roc. R. Microsc. SOC.1992, 27 (4), 283-286. Sanderson, J. B. Proc. R. Microsc. SOC.1992, 27 (3), 193-194. Hartley, W. G. Proc. R. Microsc. SOC. 1992, 27(3), 196-200. Turner, G. L. Proc. R. Microsc. SOC.1983, 28(1), 5-6. Bracegirdle, B. Mlcrosc. Anal. 1992, (34), 33-35. Evans, E. D. Microsc. Bull. 1992, 20, 14-15. Wan, I.Microsc. Anal. 1893, (38), 27-29. Noble, D. P. Roc. R. Microsc. SOC.1993, 28(3), 140-143. 64-72. Fox, R . T. V.; Hart, C. A. Quekeff J. Microsc. 1993, 37 (l), Brocklehurst, K. Quekeft J. Microsc. 1993, 3 7 (l), 56-63. Goodhew, P. J. Microsc. Anal. 1992, (33), 11-14. Cook, C. J. Mlcrosc. Anal. 1993, (35), 25-27. LaRue, B. J. Mlcroscope 1992, 40 (4), 251-254. Ford, B. J. Microscope 1992, 40 (4), 235-241. Martin, L. V. Proc. R. Microsc. SOC. 1993, 28(3), 143-144. Marentette, J. M.; Brown, G. R. J. Chem. Educ. 1993, 70(6), 435-439. Pins, H. Microsc. Bull. 1992, 19, 7-10. Delly, J. G. Microscope 1992, 40 (4), 269-274. Brockiehurst, K. G. Microsc. Bull. 1992, 79, 11. Martin, L. V. Proc. R. Microsc. SOC.1993, 28 (2), 123-124. Root, N. Microscope 1993, 47 (I), 44. Kenway, P. B. I n t Phys. Conf. Ser. 1993, 130. Proc. R. Microsc. SOC.1992, 27 (3), 131-178. McCrone, W. C. Am. Lab. 1993, 25(7), 39-40, 42-44. Cooke, P. M. Anal. Chem. 1892, 64(12), 219-243. McCrone, W. C. Microscope 1992, 40 (3), 175-192. McCrone, W. C. Microscope 1993, 47 (2/3), 57-86. Mulvey, T. Proc. R. Mlcrosc. SOC.1993, 28 (2), 64-68. Bird, L. N.; Cassella, J. P.; Yousef All, S. Proc. R.Microsc. SOC.1992, 27 (3), 202. Martin, L. V. Mlcrosc. Bull. 1992, 20, 19-20. Stoney, D. A. Mlcroscope 1993, 47 (4), 119-145. The Microscope Historical Society (new soclety); contact: Manuel del Cerro, M.D., MCS 14 Tall Acres Dr., Plttsford, NY 14534; (716-3814658).
A. OPTICS (AI) (A2) (A3) (A4) (A5) (A6) (A7) (AB) (As)
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Kermeen, T.; Probst, W. Proc. R. Mlcros. SOC.1992, 27(3), 222-224. Xiao, 2.;Zhang, G.; Song, X.; Chen, G.; Lin, F. Zhongguo J@uang1992, 79 (9), 712-714. Xiao, Z.; Zhang, G.; Lin, F. Appl. Opt. 1992, 37 (le), 3395-3397. Goldstein, D. J. J. Microsc. 1992, 766 (2). 185-197. Murray, J. M.; Eshel, D. J. Microsc. 1992, 767(1), 49-62. Van Hulst, N. F.; Segerink, F. B. Mlcrosc. Anal. 1992, (26), 21-23. Buczek, H. Sensors 1992, (6),39-75. Kobayashi, T. Klnzoku 1992, 62 (3), 91-98. Lehman, W.; Wachtel, A. J. Microsc. 1993, 769 (l), 89-90,
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(A10) Roehricht, B.; Eschie, P.; Dangel, S.; Hoizner, R . 2. Naturforsch. A. Phys. Sci. 1993, 48 (5-6), 621-623. 6. INSTRUMENTS
Laroye, G. J.; Taylor, W. B. J. Microsc. 1992, 767(3), 279-286. Feldman, M. Brit. UK Pat. Appl. 2, 253, 711, 16 Sept 1992; OB Appl. 91/3540, 1991. Hirano, M.; Yamashlta, Y.; Miyakawa, A. Anal. Sci. 1993, 9 (3), 375380. Bradl, J.; Hausmann, M.; Ehemann, V.; Komltowski, D.; Cremer, C. J. Microsc. 1992, 768 (l), 47-57. Barnard, D. P.; Turner, J. N.; Frank, J.; McEwan, B. F. J. Microsc. 1992, 767 (l), 39-48. Greuiich. K. 0.; Weber, G. J. Microsc. 1992, 767(2), 127-151. Zuev, B. K.; Skryabin, I.L.; Kunin, L. L. Izobreteniya 1992, (20), 257. Putman, C. A. J.; Van der Werf, K. 0.; Van Oort, 0.; De Grwth, B. G.; Van Hulst, N. F.; Greve, J. Rev. Sci. Instrum. 1982, 63(8),4012-4013. Washington, C. Meas. Sci. Techno/. 1993, 4 (6),659-664. Lanni, F. Rev. Scl. Instrum. 1993, 64 (5),1474-1477. Walker, J. G.; Pike, E. R.; Davies, R. E.; Young, M. R.;Brakenhoff, G.J.; Bertero, M. J. Opt. SOC.Am. A: Opt. Image Sci. 1993, 70 (l), 59-64. Lee, R. J.; Warner, D. A.; Lentz, H. P. J. Proc. Int. Conf. Cem. Microsc. 1993, 75,36-50. Abramowitz, M. Am. Lab. 1992, 25(9), 31-32. Adv. Imaging 1993, 7 (12), 4-78. C. POLARIZED LIGHT MICROSCOPY (‘21) . .
Giniunas. L.: Juskaitus, R.: Dvra. E.: Shatalin. S. V. Oof.Commun. 1993. 700 (1-4), 31-34. Monovoukas, Y.; Gast, A. P. Langmulr 1991, 7 (3). 460-468. 13-19. Besancon, J. R. Microscope 1992, 40 (l), Ho, M. W.; Lawrence, M. Mlcrosc. Anal. 1993, (36), 26. Bryant, W. M. D. Microscope 1992, 40 (3), 171-173. Bryant, W. M. D. Microscope 1992, 40(3), 153-158. McCrone, W. C. Am. Lab. 1992, 2 4 ( 6 ) , 17-21. Herting, D. L. Energy Res. Abstr. 1992, 77 (E), Abstract 22486. Deliy, J. G. I n Encyclopedia of Materials Characterlzatiofl Brundle, C. R., Evans, C. A., Wilson, S., Eds.; Butterworth-Heinemann: Boston, MA, 1992; Chapter 2, pp 60-69. Uno, Y. Nendo Kayuku 1992, 32(1), 42-52. Eser, S.; Song, C.; Gergova, K.; Parzynski, M.; Peng, Y. Prepr.-Am. Chem. SOC.,Div. Pet. Chem. 1992, 37(2), 463-468. Choi, N. S.;Takahashi, K. J. Mater. Sci. Lett 1993, 72(21), 17181721.
D. MICROPHOTOMETRYAND MICROSPECTROPHOTOMETRY (Dl) (D2) (D3) (D4) (D5)
Katon, J. E.; Sommer, A. J. Anal. Chem. 1992, 64(19), 931A, 934A, 937A-940A. Manakata, T.; Kasuya, T. Surf. Sci. 1993, 283 (1-3), 452-456. Cooper, G. I.; Cox, G. A.; Perutz, R. N. J. Microsc. 1993, 770 (2), 111-118. Messerschmidt, R. G. US. US 5, 225, 678, 1993. Jacobsen, W. Ger. Offen. DE 4,111,903, 15 Oct 1992; Appi. 12 Apr 1991. Yamaguchi, T.; Ukon. J.; Ikemoto, K.Ger. Offen. DE4,200,869, 1992. Gardette, J. L. Analusls 1993, 27 (9,M17-M21. Shala, F. J. ISTFA ‘92, Proc. Int. Symp. Test. Failure Anal., 18th 1992, 175-1 79. Cai, H.; Chen, Z.; Zhong, Y. Zhongguo J i g ~ n g l 9 9 2 ,79(3), 180-184. Lin, W.; Coates, V. J.; Singh, B. Proc. SPIE-Int SOC.Opt. Eng. 1992, 1673, 453-462. Blair, D. S.; Ward, K. J. Part. Surf. 1991, 3. 123-130. Reffner, J. A. Microsc. Today 1993, (3), 6-7. Wu, M.; Nakayama, K. Polymer 1892, 33 (13), 2672-2678. Centeno, J. A.; Johnson, F. B. Appl. Spectrosc. 1993,47(3), 341-345. Ikuta, N.; Suzukl, Y.; Maekawa, 2.;Hamada, H. Polymerl993, 34(1l), 244.52446. - . . - - . .- . Cross, 8. J.; Lamb, R. D.; Ma, S.; Paque, J. M. Adv. X-ray Anal. 1892, 358, 1255-1264.
E. I R , UV, AND RAMAN MICROSCOPY Day, R. J.; Young,. R. J. J. Mlcrosc. 1993, 769 (2), 155-161. Garton, A.; Batchelder, D. N.; Cheng, C. Appi. Spectrosc. 1993.47(7). 922-927. (E3) Grosse, P.; Kuepper, L.; Theiss, W. Proc. SPIE-lnt SOC. Opt. Eng. 1992, 7575, 269-270. (E4) Pltt, G. D.; Hayward, I.P. Mater. WorM 1993, 7 (l), 8. (E5) Everall, N. Appl. Spectrosc. 1992. 46 (5), 746-748. (E6) Boogh, L. C. N.; Meier, R. J., Kausch, H. H.; Kip, B. J. J. Polym. Scl., Part B 1992, 30 (4), 325-333. (E7) Ivanda, M.; Furic, K. Appl. Opt. 1992, 37 (30), 6371-6375. (E8) Morrls, M. D.; Govil, A.; Liu, K. L.; Sheng, R. Proc. SPIE-Int. SOC.Opt. Eng. 1992, 7439, 95-101. (E9) Nakao, Y.: Nakajima, M.; Harako, F. Proc. SPIE-Int. SOC.Opt. Eng. 1992, 7575, 292-293. (E10) Marcott, C.; Munyon, R. L.; Laughlin, R. G. Proc. SPIE-Int. SOC.Opt. Eng. 1992, 1575, 290-291. ( E l l ) Gal, T.; Toth, P. Can. J. Appl. Spectrosc. 1992. 37(2), 55-57. (E12) Saito, T.; Matsuoka, M. Jpn. Kokai Tokkyo Koho JP 03, 257,351 257, 351). (El) (E2)
Booker, 0. R.; Laczlk. 2.;Kldd, P. Semhnd. Scl. Technol. 1992, 7(1A), A110-A121. Mason, S. M.; Conroy, N.; Dlxon, N. M.; WiUlams, K. P. J. Spectrochlm. Acta, Part A 1993, 49A (5-6), 633-643. Vess. T. M.; Angel, S. M. Roc. SPIE-Int. Soc. Opt. Eng. 1092, 1637, 118-125. Carlson, D. J.; Bliss, D. F. Int. Conf. Indium Phosphm Relet. Mater. 4th 1992, 515-517. Schueth, F. J. Phys. Chem. 1992, 96(19), 7493-7496. Del, S.; Young, J. P.; Begun, G. M.; Cotfield. J. E.; Mamantov, 0. M k O C k n . Acta 1902, 708 (3-6). 261-264. Donahue, S. M.; Reffner. J. A.; Wlhlborg, W. T.; Strawn, A. W. Roc. sprwnt. soc.Opt. Eng. 1992, 1575, 490-492. Sommer, A. J.; Katon, J. E. Spectrochlm. Acta, PartA 1993,49A (5-6). 61 1-620. Esakl, Y.; Nakal, K.; Araga, T. BunsekiKapku 1993, 42(3), 127-132. Windlg, W.; Markel, S. J. Mol. Struct. 1993, 292, 161-170. Fondeur, F.; Koenlg, J. L. Appl. S p e c m c . 1993, 47(1). 1-6. Clark, D. A. Anal. Roc. 1992, 29(3). 110-111. Ottenroth, H. CLB Chem. Labor Biotech. 1992, 43 (9). 493-496. Reffner, J. A.; Wlhlborg, W. T.: Sweeney, M. C. Roc. SPIE-Int. Soc. Opt. €w. 1992. 1575, 298-300. Bradley, J. P.; Humecki, H. J.; Germanl, M. S. Astrophys. J. 1992, 394 (2, Pad I), 643-651. Murphy, R. J.; Alvin, K. L. Mlcrosc. Anal. 1992, (31). 13.
(H7)
1. PHASE CONTRAST AND SCHLIEREN MICROSCOPY (11)
(F2) (F3) (F4) (F5) (F6) (F7) (F8) (F9) (F10) (F11) (F12) (F13) (F14) (F15) (F16)
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0. LASER AND HOLOGRAPHIC MICROSCOPY Yamamoto, Y.; Ueno, M. Roc. SPIE-Int. Soc. opt. Eng. 1992-1993, 1801, 286-297. Ghigglno, K. P.; Harrls, M. R.; Splzzirrl, P. G. Rev. Scl. Instrum. 1892, 63 (5), 2999-3002. Cogswell, C. J.; Hamilton, D. K.; Sheppard, J. R. J. Microsc. 1992, 165 (l), 103-117. Brody, P. S.; Gamin, C.; Glllman, A. W.; Llan, S. Roc. SPIE-Int. SOC. Opt ~ n g 1992. . 7553.89-101. Kempe, M.; Stamm, U.; Gutewort, R.; Wllhelml, 6.; Rudoph, W. Inst. Phys. Conf. Ser. 1992, 726. 159-162. L w , I . Y. S.; Tolbert. W. A.; Dlott, D. D.; Doxtader, M. M.; Foley, D.M.; Arnold, D. R.; Ellls, E. W. J. Imaging Scl. Technol. 1992, 36 (2). 180187. Harata, A.; Sawada, T. Jpn. J. Appl. Phys., Part 11993,32(5B), 21882191. Canon, J.; Armas. M. Laser Focus WorM1993, 29(1), 99-100, 102104. Da Silva, L. 8.; Treks, J. E.; Mrowka, S.; MacGowan, B. J.; Koch, J.A.; Matthews, D. L.; Barbee, T. W.; Balhorn, R.; Gay, J. Inst. Phys. Conf. Ser. 1892. 125, 387-392. Bergner, H.; Stamm. U.; Hempel, K.; Kempe, M.; Krause, A.; Wabnitz, H. Inst. Phys. Conf. Ser. 1902, 126, 143-146. Van Bladeren, A.; Imhof, A.; Hage, W.; Vrlj, A. Langmuir 1992, 8(6), 1514- 1517. MacGowan, B. J. Roc. SPIE-Int. SOC.opt. mg. 1993, 7747, 2-11, H. INTERFERENCE MICROSCOPY (HI) (H2) (H3) (H4) (H5) (He)
Matsuil K.; Kawata, S. Roc. SPIE-rnt. soc. opt. Eng. 1992, 7720, 124- 132. Raedier, J.; Sackmann, E. Langmulr 1992, 8 (3), 846-653. Raedler, J.; Sackmann. E. J. Phys. 2 1993, 3 (9,727-748. Raedier. J.; Sackmann, E. Springer Roc. Phys. 1992, 66, 158-161. Tentori. D. Opt. Eng. 1992. 37 (4), 805-808. Foskett, J. K. Opt. Mlcrosc. 1993, 237-261.
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J. CONFOCAL MICROSCOPY
F. FLUORESCENCEMICROSCOPY (Fl)
Kyed, P. J.; Matlock, D. K. Metall. Trans. A 1993, 24A (7), 1678-1681.
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(K12) (K13) (K14) (K15) (K16) (K17) (K18) (Kl9) (K20)
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Analytical Chemistry, Vol. 66, No. 12, June 15, 1994
(M10) Ashcroft, I.A.; Lawrence, C. W.; Weihs, T. P.; Derby, B. J. Am. Ceram. soc 1nn2. 75 (5). 12a4-i2ae. ~-,, Brlggs, A. Rep. Rog. fhys. 1992, 55(7), 851-909. Levin, V. M.; Maev, R. G.; Maslov, K. I.; Senyushkina, T. A.; Grlgor6va, L. G.; Baranchikova, I.Acoust. Imaging 1992, 79, 651-655. Gurtoval, V. L.; Eremenko, V. G. Acoust. Imaging 1992, 70, 761-765. Ishlkawa, 1. Zairo to Kankyo 1093, 42(3), 172-178. Klelczynski, P. J.; Busslere, J. F. Uffrason. Symp. Roc. 1902, 10091013. Pangraz, S.; Wertsman, N.; Willems, H.; Arnold, W. Vortragsveranst. Arbeffskreises Rastermikrosk. Materia/pruef. 1902, 133-139. Lawrence, C. W.; Brlggs, 0. A. D.; Scruby, C. 6.; Davies, J. R. R. J. Mater. Sci. 1993, 28 (13), 3635-3644. Lawrence, C. W.; Brlggs, G. A. D.; Scruby, C. B. J. Mater. Sci. 1093, 28 (13), 3645-3652. Van Doorselaer, K.; Moore, T. M.; Tizianl, R.; Baelde, W. ISTFA ‘92, Roc. Int. Symp. Test. Failure Anal., 78th 1902, 425-431. Carbone, R. A. ISTFA ‘92 Roc. Int. Symp. Test. Failure Anal. 1902, 301-306. Zhal, T.; Beanink, D. D.; Knauss, D.; Brlggs, G. A. D.; Martin, J. W. Mater. Char. 1093, 37 (2). 115-128. Caplaln, R.; Ferdj-Allah, L.; Saurel, J. M.; Attal, J. Mem. Etud. Sci. Rev. Mi%//. 1902, 89 (lo), 643-651. Quate, C. F.; Khuri-Yakub. B. T. Gov. Rep. Announce. Index 1092, 92 (18); Abstract 248984. Brlggs, G. A. D. Rep. frog. fhys. 1992, 55(7), 851-909. Woo, E. M.; Seferls. J. C. J. Mater. Sci. 1903, 28 (2), 329-336. Tokunaga, Y.; Mlnamide, A.; Tamura, K.; Nakada, N. Jpn. J. Appi. Phys. Part 7 1993, 32 (5B), 2573-2576. Nishimura, Y.; Konomura. Y.; Wakayama, K. Kenkyu-Hokoku-Sen’i Kobunshi Zalryo Kenkyusho 1992, 772, 111-1 18. Ganz, S. Chem. Ind. 1992, 7 75 (9), 89-72. Wey, A. C.; Kessler, L. W.; Ho, B. Uffrason. Symp. Roc. 1092, (Voi. 2). 707-71 1. icy, A. C.; Kessier, L. W.; Dos Reis, H. L. M. Acoust. Imaging 1992, 19, 709-716. Endo, T.; Sasaki, Y.; Yamaglshi, T.; Sakai, M. Appi. fhys., farl 7 1092, 37, 160-162.
(M32) Maev, R. G.; Chernosatonskil, L. A. H@t Tc Sqercond. Thln FUms, ROC. Symp. A7 Int. Conf. A&. Mater. 1992, 795-800. (M33) Rescher-Kaslcka, E.; Yolken, H. T.; Tlttmann, B. R.; Shaplro, A. J.; Lucey. G. Mater. Scl. Forum 1993, 1 1S721, 337-345. (M34) Bashyam, M.; Rose, J. Wbnson. Symp. Roc. 1992, (Vd. 2), 741-744. N. CATHODOLUMINESCENCE Kbmura, M.; Fudakl. M.; Shwin, K.; Shimobayashi, N. Mneral. J. 1992, 76 (2), 106-1 16. Hagni, R. D. €pD Congr. 7993, Roc. Symp. TMS Annu. Meet. 1993, 487-495. . - . ..-. Watson, C. C. R.; Durose, K. J. Cryst. c)owlh 1993, 126 (2-3), 325329. Finch, A. ROC. R. M~WOSC. SOC. 1992, 27 (3), 179-184. HoR. D. B. Scannlng Mlcrosc. 1992, 6 (I), 1-21. Petrov, V. 1. phys. Status SOlMi A 1992, 733 (2), 189-230. Watson, C. C. R.; Durose, K.; Banister, A. J.; O'Keefe, E.; Bakrs, S. K. Mater. Sci. Eng. E 1993, E76 (1-3). 113-117. Saparin, 0. V.; Obyden, S. K. Mfwosc. Anal. 1992, (34), 5-7.
(S3) (54)
Alleon, J. M.; Birch, K. P. Crowder, J. 0. Meas. Scl. Techno/. W 3 , 4 (5), 571-577. Komissarw, V. I.; Mankra, 0. I.; Bogoslevskaya, T. N.; Zakharova, Y.M. Khh. V&na 1992, (4), 56-58.
T. HOT STAQE AND COLD STAQE TECHNIQUES (TI) (T2)
Oan, S.; SeferiS, J. C. CbWOS. Mater. 1992, 2(2), 119-126. AWub'akhldov, K. 0.; Gcfbunwa. A. G. P&. T&h. €ksp. 1992, (5), 21 1-212.
U. STEREOLOGY (U1) (U2) (U3) (U4) (U5)
Marcussen, N. J. Mlwapc. 1992, 165 (3), 417-426.
Karlsson, L. M.; CNz-Orive, L. M. J. MkfoSC. 1992, 165(3), 391-415. Nielson, K. hiYcrosc. Anal. 1992. (34). 22. LIU, 0. J. Mlcnwc. 1993, 771 (I), 57-68. J. Mcrosc. 1993. 170 (I), 3-93.
V. AUTOMATED IMAQE ANALYSIS AND VIDEO MICROSCOPY
0. EMBEDDINQ AND MOUNTING (01) (02) . . (03)
Oanczarczyk, J. J.; Zahd, W. M.; Ll, D. H. Water Res. 1992, 26 (12), 1695-1698. Marchese-Ragona, S.; Jobe, R.; Jacobs, A. Roc. R. hUcrmc. Soc. 1992, 2 7 (4),-284. Robertson, D. R.; Monaghan, P.; Clarke. C.; Atherton. A. J. J. Mfwosc. 1nn2. 168 .___ , l i b . 85-100. Ohno, Y.; Wakabayashi. S.; Doba, T. Anal. Scl. 1991, 7, 1291-1292. HopWood, D. Roc. R. MlcrosC. SOC. 1992, 27 (2), 71-74. Giammara, B. L. Scannlng 1993, 15 (2). 82-87. Hobot, J. A.; Newman, 0. R. ScannlngMfwosc. Suppl. 1991,5.27-41. Harris, A. M.; Schaffer, G. B.; Page, N. W. J. Mater. Scl. Left 1993, 72 (3). 160-161. . _ _ I
(04) (05) (06) (07) (08)
.,.__
P. ULTRAMICROTOMY (Pl) (P2) (P3) (P4) (P5)
Jacobs, E. 0.; Foster, L. A.; Wu, Y.; Wilson, A. R.; Plniuotto, R. F. J. Mater. Res. 1993, 8 (1). 87-94. Malls, T.; Steele, D. Mater. Res. SOC.Symp. Roc. 1992,254,257-270. Mlchel, M.; Gnlgi, H.; Mirller, M. J. Mlcrosc. 1992, 766 (I), 43-56. Webster, P. J. hUcrosc. 1993, 769 (l), 85-88. Keljzer. C. J. J. Electron Mlcrosc. 1993, 42 (2), 124-125.
Q. MISCELLANEOUS SPECIMEN PREPARATION Katrinak, K. A.: Zygariicke, C. J. Repr. Pap.-Am. Chem. Soc.,Dlv. Fuel Chem. 1993, 38 (4), 1203-1209. (Q2) Valdre, G.; Korlevlc. K. Uhmkroscopy 1993, 49 (1-4), 382-386. (Q3) Cohrin, J. Roc. Int. Symp. Test. Failure Anal. 1991, 69-75. (04) Scanning 1993, 15 (2), 57-1 19. (QS) Glammara, B. L. Scannlng 1993, 15 (2), 57. ((26) Kok, L. P.; Boon, M. E.; Smid, H. M. Scanning 1993, 75(2), 100-109. ((27) Leong, A. S. Scannlng 1993. 75 (2), 88-98. (Q8) Login, 0. R.; Dvorak, A. M. Scannlng 1993, 15 (2), 58-68. (Q9) Hanker, J.; Giammara, B. L. Scannlng 1993, 15 (2), 67-80. (QlO) Oiammara, B. L. Scannlng 1993. 15 (2), 82-87. ( a l l ) Femandez de Tajada, I. Tec. Lab. 1992, 74 (No. 179, 814-817. (012) Garg, A. P. J. Indlen Bot. SOC. 1991, 70 (1-4), 411-412.
Willls, B.; Roysam, B.; Turner, J. N.; Holmes, T. J. J. W o s c . 1993, 769 (3), 347-361. (V2) Kempe, M.; Damm. T.; Stamm, U.; Wilheimi, E. Optlc 1992, 69 (4), 159-165. (V3) Ludwig, C.; Eberle, 0.;Oompf, B.; Peterson, J.; Elsenmenger, W. Ann. phys. 1993, 2 (4), 323-329. (V4) Thomas, A.; Albert, 0.; Schloesser, E. Md&. Fac. Landbwwwet., UnW. Gent 1992, 57 (2a). 189-197. (V5) Qlier. D. G.; Munay, C. A. NATOASISer., Ser. C1992,369, 145-174. (V6) Hawkes, P. W. Mkosc. Anal. 1993, (35), 13-15. (V7) Chelihl, N.; (3eydeCk1, P. A. Meas. Scl. Techno/. 1993, 4 (4), 447-450. (V8) HovN&ler, S. Wbn-y 1992, (I), 121. (V9) Zou, X. D.; Sukharev, Y.; Hovm6Uer,S. wbamlcroecopyl993.(9). 147. (V10) Hovt"I&k, S. Mcrosc. Anal 1993, (36), 37. (V11) James, N. Mkosc. Anal. 1993, (35). 33-35. (V12) Fermln, C. D.; oerber,M. A.; TorrsBueno, J. R. J. kllcrosc. 1992, 767 (l), 85-95. (VI)
W. PARTICLE GRAIN SIZE MEASUREMENT (Wl) (W2) (W3) (W4)
(at)
R. PHOTOMICROGRAPHY AND PHOTOMACROQMPHY (Rl) (R2) (R3) (R4) (R5) (R6) (R7) (R8) (R9) (R10) (R11) (R12) (R13) (R14) (R15) (R16) (R17) (R18) (R19) (R20) (R21) (R22) (R23) (R24) (R25)
Bracegirdle, E. W e n J. Mlcrmc. 1993, 37 (I), 22-29, Loveland, R. P. EM. Pbotogr. 1992, 60 (3), 99-102. FOX, C. H.; Saunders, W. (3. EM. photog. 1992. 60(3), 111-118. Kilbowne, S.; Dodd, R. Ebl. Pbotogr. 1992. 60(1), 1-10, Clarke, T. M. Microscope 1993, 47 (l), 21-30. Delly, J. 0. MicroScope 1993, 41 (4). 155-158. Delly, J. G. Mcrmcope 1993, 47 (4), 159-160. Pan, M. L. E&/. photogr. 1992, 60(4). 131-134. Pan, M. L. Blol. photog. 1993, 67 (2). 45-49. Wlidi, E. Eiol. Pbotogr. 1993, 67 (2), 38. Saunders, W. 0. Am. Lab. 1992, 24 (6), 43-44. Walker, M. I. Microsc. Anal. 1992, (32), 29. Walker, M. I. Mlcmsc. Anal. 1992, (30), 35. Clarke, C. D. EM. photogr. 1993, 60(4), 148-152. Goosman. C. EM. Pbotogr. 1993, SO(4). 147. Wllllams, A. R.; Williams, 0. F. EM. Pbotogr. 1983, 61 (4). 115-132. Holmes. T. J.; Llu, Y.; Khosla, D.; Agard, D. A. J. Mlcrosc. 1991, 164 (3), 215-235. Khosla, D.; Holmes, T. J. J. Microsc. 1992, 768(2), 115-129. Ando, Y.; Fujisawa. T. Ebl. photog. 1993, 67 (4), 75-78. Fox, C. H.; Dreyfuss, R. EM. Pbotogr. 1992. 60(1), 39-44. Zkler, H. W. 8bl. R~~togr. 1992, 60(1), 19. Duniop, J. R., Jr. Ebl. photogr. 1992, 60(2), 50-51. Morgan, W. D. E&/. photo@. 1992, 60(2), 52-53. Prlestiy, J. V. Mcrosc. Anal. 1992, (32), 15-17. DavMson, M. W. Mlcrosc. Anal. 1992, (32). 5-7.
S. REFRACTOMETRY (Sl) (52)
Su. S. Mcroscope 1992, 40 (I), 95-106. LaRabee, R. D. Roc. SPIE-Int. Soc. Opt. Ew. 1992, 7846,86-93.
Kievtsov. 0. V.; Mkonova, N. A. Zevod. Lab. 1992, 58(10). 32-33. Davidson,J. A.; Butler, R. S. Part. Syst. Charact. 1992,9(4), 213-222. Dwadwai, H. S.; Anearl, R. R.; Meyer, W. V. Rev. Sci. Insfrum. 1991, 62 (12), 2963-2968. Davideon, J. A.; Etter. A. A.; Thomas, M.; Butler, R. S. Part. Syst. Charact. 1992, 9 (2), 94-104.
X. MISCELLANEOUS TECHNIQUES FOR SPECIMEN EXAMINATION
Amanre, D. M/crosc. Anal. 1992, (28), 29. Reviere, J. C. AnaMt 1992, 117(3), 313-322. Mackenzle, R. Roc. R. Mlcrosc. Soc. 1992, 27(3), 191-192. Butler, D. J.; Horsfall, A.; Hymevych, M.; Kearney, P. D.; Nugent, K.A. Opt. 1993, 100 (1-4), 87-92. (X5) Jones, R.; Watson-CraR. I.; Senlor, E. MkfoSc. Anal. 1992, (30), 3133. (X6) Somorjal, 0. A. Swf Interface Anal. 1992. 79 (1-12), 493-507. o(7) Afzal, R. S.; Treacy, E. B. Rev. Scl. I n s f " . 1992, 63 (4, Part I), 2 157-2 163. (X8) Taylor, H. L. Akroscope 1993. 47 (l), 19-20. (X9) Ramamwthy,V.; Webs, R. G.; Hammond, G.S. A&. photodwwn. 1993, (la), 67-236. (X10) COllinSOfI. M. E. Mlc*osC.Anal. 1992, (34), 19-21. ( X l l ) Walr, J. Y.; Prleve, D. C. Langmulr 1992, 6 (12), 3073-3082. (X12) Schaertl. W.; Slllescu, H. J. Cdb&lIntehce Scl. 1993, 155(2), 313318. (Xl) (X2) O(3) (X4)
."
Y. LIQUID CRYSTALS (Yl)
Vlney, C. PO!W?~. Rwr. (Am. Chem. Soc,,Dlv. Polym. Chem.) 1992. 33 (1). 757-758. Dorkal, N.; Hoshlno, H.; KaJiwara, K.; Miyamoto, T. Makromo/. Chem 1993, 194 (2), 559-580. &aktrOem, S.; hobst, 0.; Dey, S.; Freund, J.; Kowaldti, J.; Neuman, R.; Woertge, M.; Zu Putlltz, G. Roc. SPIE-Int. SOC. @t. €ng. 1993, 1697. 56-65. Kltzerow, H. S.; Xu, F. L ~ JCryst. 1992, 12(6), 1019-1024. Scharkowski, A.; Crawford, G. P.; Zumer, S.; Doane, J. W. J. AppL PhyS. 1993, 73 (1I), 7280-7287. Mattai, J.; Froebe, C. L.; Rhein, L. D.; Simlon, F. A,; Ohlmeyw, H.; Su, D. T.; Frlberg, S. E. J. SOC. Comet. Chem. 1993, 44 (2), 89-100. Yaw, 2.;Hua, 0.;WI,J.; Xb, M. SlchuenaaxueXuebeo, Zhan Kexueben 1992, 29 (2), 306-310. S h W o , M. Kawku K w k u 1992, 56 (2), 101-104. Mateushlge, K.; Taki, S.; Okabe. H.; Takebayashl, Y.; Hayashl, K.; Yoshlda, Y.; Horluchi, T.; Hara, K.; Takehara, K. Jpn. J. A m . mys., Part 1 1993. 32 (4), 1716-1721. Bleasda1e.T. A.;Tiddy.G. J.T. SurfactantSci.Ser. 1992.44.125-141. Reamey, R. H.; Montoya. W.; Wong, A. Roc. SPIE-Int. Soc. Opt. Eng. . 1992. i s ~2-7. ~ , Schmid, H. plrase TranslHDns 1991, 34 (1-4), 205-214. Doertier, H. D. Tens&, Surfactants, Deterg. 1992, 29 (5). 352-358.
Analytcal Chemistry, Vol. $6,No. 12, June 15, 1994
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(Y14) Stlne, K. J.; Uang, J. Y. J.; Dlngman, S. D. Langmuirl993, 9(8), 211221 18. (Y15) Carboni, C. Meas. Sci. Tech 1993, 4 ( l l ) , 1238-1243. 2. RESINS, POLYMERS, AND THEIR ADDITIVES Gal, T.; Toth, P. Can. J. Appl. Spechosc. 1992, 37(2), 55-57. Verghoot, H.; Van Dam, J.; Posthuma de Boer, A.; Draaljer, A.; Houpt, P. M. Polymer 1993, 34 (6), 1325-1329. Patil, R.: Tsukruk, V.; Reneker. D. H. folym. Bull. 1992, 29 (5).557563. McCrone, W. C. I n Applied Polymer Analysis and Characterizatlon; Mitchell, J., Jr., Ed.; Oxford University Press: New York, 1992; Chapter 2, pp 103-129. Karger-Kocsls,J.; Czlgany, T. J. Mater. Sci. 1993, 28(9), 2438-2448. Leggett, G. J.; Davlas, M. C.; Jackson, D. E.; Roberts, C. J.; Tendler, S.J.B. Trends folym. Sci. 1993, 7 (4), 115-121. Shlnn, T. H.; Lin, C. C. J. Appl. folym. Sci. 1993, 49(6), 1093-1105. Moreau, E.; Boudet, A.; Mayoux, C.; Laurent, C.; Wright, M. J. Mater. Sci. 1993, 28 (1). 161-169. Rappe, R. G. Microscope 1992, 40 (2), 93-101. Sayyadnejad, M. A. Iran J. folym. Scl. Technol. 1992, 5(3), 186-195. Guild, F. J.; Summerscales, J. Composites 1993, 24 (5), 383-393. MaganoviS. N.; Cantow, H. J. J. Appl. folym. Sci.: Appl. fo/ym. Symp. 1992, 57, 3-19. FuChS, H. J. Mol. StrUCt. 1993, 292, 29-47. Mitchell, A. B.; Chan, P.; Hiltz, J. A. failure Anal. Tech Appi., Roc. Int. Conf. 1992, 269-278. Schemme, M.; Ehrenstein, G. W. Sonderb. frakt. Metallogr. 1992, 23, 143. .- 153. . - -. Steger, W. E.; Machlll, S.; Herzog, K.; Gerhards. R.; Jussofle, I.; Schator, H. fresenlus' J. Anal. Chem. 1992, 344 ( 4 4 , 203-205. Janik, H.; Foks, J. Adv. Urethane Scl. Technol. 1992. Janik, H.; Foks, J. frog. Rubber plast. Technol. 1992, 8 (3), 240-260. Janlk, H.; Foks, J. Cell folym. 1992, 7 7 (4), 298-318. Knoll, W.; Hickel, W.; Sawodny, M. Teubner-Texte fhys. 1993, 27, 89-112. We, C.; Asai, S.; Sumlta, M.; Miyasaka, K. Sen'i Gakkaishi 1992, 48 (8), 389-392.
(883) Relf, L.; Seeiemann, R.: Wallpot, G. Wochenbl.faplerfabr. 1991, 179 (17), 666-669. (884) Kropholler. H. W.; Moss, P. A. Wochenbl. faplerfabr. 1992, 720(16), 648. (885) Robertson, L. R. Tappl J. 1993, 76 (3), 83-87. 456. (886) Roll, H. Hol. Roh-Werkst. 1992, 50 (1l), (887) Kojima, Y.; Fukazawa, K. Oputoronikusu 1992, 722, 67-72. (BB8) Fukazawa, K. I n Methodsin Lignin Chemistry;Lin, S. Y., Dence, C. W., Eds.; Springer: New York, 1992; pp 110-121. (BB9) Prelkschat, E. Energy Res. Absh. 1992, 77 (9,Abstract 12578. (BBlO) Prelkschat,E.; Hokanson, J.; Stern, M.;Nelson, R.; Mustonen, M. Energy Res. Abstr. 1992, 77 (5), Abstract 12579. (BBll) Johnson, S. E.; Kamke, F. A. J. Adhesives 1992, 40 (l), 47-61. (BB12) Donaldson, L. A. I n Methods in Lignin Chemism Lln, S. Y., Dence, C. W., Eds.; Springer: New York, 1992; pp 122-132. CC. COAL (CC1) Matzakos, A. N.; Zygourakls, K. Rev. Sci. Instrum. 1993, 64(6),15411548. (CC2) Bensley, D. F.; Crelling, J. C. Adv. Coal Spectrosc. 1992, 119-139. (CC3) Galbreath, K. C.; Brekke, D. W.; Folkedahl, B. C. frepr. Pap.-Am. Chem. Soc., Div. Fuel Chem. 1992, 3 7 (3), 1170-1 176. (CC4) Hippo, E. J.; Murdie, N.; Byrne, J. F.; Sebok, E. B. frepr. Pap.-Am. Chem. Soc.. Div. fuel Chem. 1992, 37 (3), 1124-1 130. (CC5) Rathbone, R. F.; Hower, J.; Derbyshire, F. J. fuell993, 72(8), 11771185. (CC6) Rathbone, R. F.; Hower, J. C.; Derbyshire, F. J. Energy Res. Abstr. 1992, 77 (B), Abstract 15021. (CC7) McFarlane, R. A.: Gentzis, T.; Goodarzl, F.; Hanna, J. V.; Vassallo, A.M. J. Coal Geol. 1993, 22 (2), 119-147. OD. EMULSIONS
(DD1) Mikula, R. J. Adv. Chem. Ser. 1992, No. 237, 79-129. (DD2) Chen, J. D.; Wada, N. J. ColloMInterfaceSci. 1992, 748(1), 207-222. EE. MINERALS
AA. TEXTILES, FIBERS, AND FILMS
(AAl) Annis, P. A.; Qulgley, T. W.; Kyllo, K. E. Text. Chem. Color. 1992, 24 (8), 19-22. (AA2) Wilson, T.; Hudson, A. J. J. Microsc. 1992, 768 (I), 59-69. (AA3) Lowry, J. H.; Mendlowltz, J. S.; Subramanian, N. S. Opt. Eng. 1992, 37 (9), 1982-1985. (AA4) Yoshida, H. furasuchikkusu 1992, 43 (lo), 66-70. (AA5) Domlnguez-Adame, F.: Fernandez, P.; Plgueras, J.; Prieto, P. Barrero, C.; Gomez, M. E. J. Appl. fhys. 1992, 77 (6), 2778-2782. (AA6) Kuz'mln, V. L.; Romanov, V. P.; Mikhallov, A. V. Opt. Spektrosk. 1992, 73 (l), 3-47. (AA7) Leuthe, A.; Riegler, H. J. fhys. 0 : Appl. fhys. 1992, 25(12), 17861797. (AA8) Pltkethly, M. J. J. Microsc. 1993, 769 (2), 183-188. (AA9) Overney, R. M.; Luethi, R.; Haefke, H.; Frommer, J.; Meyer, E.; Guentherodt, H. J.; Hild, S.; Fuhrmann, J. Appl. Surf. Sci. 1993, 64(3), 197-203. (AA10) Stanley, A. Microsc. Anal. 1992, (28)' 25-27. (AA11) Morita, H.; Sakabe, H.; Itoh, T.; Konlshi, T. Sen'i Gakkalshi 1992, 48 (8), 368-371. (AA12) Jurdana, L. E.; Leaver, 1. H. Text. Res. J. 1992, 62 (8), 463-468. (AA13) Dollinger, G.; Boulouednlne, M.; Faestermann. T.; Maler-Komor, P. Instrum. Methods fhys. Res., Sect A 1993, 334 (l), 187-190. (AA14) Kaufman,S.; Bergner, J.; Trempier, J. Kunststoffe 1992,82(1 l), 11061109. (AA15) Schwartz, D. K.; Knobler, C. M. J. fhys. Chem. 1993, 97(35), 88498851. (AA16) Schwartz,D. K.; Garnaes, J.; Viswanethan, R.; Chlruvolu, S.; Zasadzlnskl, J. A. N. fhys. Rev. E.: Stat. fhys., Plasmas, FluMs. Retat. Inderdiscip. Top. 1993, 47 (i), 452-460. (AA17) Rulz-Garcia, J.; Qlu, X.; Tsao, M. W.; Marshall, G.; Knobler, C. M.; Overbeck, G. A.; Moeblus, D. J. fhys. Chem. 1993, 97 (27), 69556957. (AA18) Eng. F. P.; Shebib, C. D. Roc. SfIE-In?.SOC.Opt. Eng. 1992, 1575, 266-268. (AA19) Nikitenko, A. A.; Savanskii, V. V. Opt. Spekhosk. 1993, 74 (2). 327330
(AA20) Henck, S. A. J. Vac. Sci. Technol., A 1992, 70 (4, Part l), 934-938. (AA21) Zhang, Y.; Zhou, C.; Ge, X.; Llang, X. J. fhys. 0 : Appl. Phys. 1992, 25 (6), 1004-1009. (AA22) J. Microsc. 1993, 769 (2). 95-295. (AA23) Mackenzie, R.; Grant, P. Roc. R. Microsc. SOC.1993,28(3), 162-164. (AA24) Craven, B. J. Microscope 1992, 40 (4), 243-246. (AA25) Craven, B. J. Mlcroscope 1993, 47 (4), 115-117. (AA26) Schaefer. K.: Hoecker. H. Meiliand Textjber. 1991. 72 (3). 213-221. (AA27) Zhu, R.; Min, G.; Wel, Y.: Schmm. H. J. J. fhys. Chem. 1992, 8210-821 1. BB. WOOD AND PAPER (BB1) Moss, P. A.; Retulainen, E.; Paulapuro, H.: Aaltonen, P. Pap. fuu 1993, 75 (1-2), 74-79. (882) Jang, H. F.; Robertson, A. G.; Seth, R. S. J. Mater. Sci. 1992, 27(23), 6391-6400.
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(EE1) Smith, D. G. W. Microscope 1992, 40 (l), 39-58. (EE2) Redmond, G.; Cesbron, F.; Chapoulle, R.; Ohnenstetter, D.; RoguesCarmes, C.; Schvoerer, M. Scanning Microsc. 1992, 6 (I), 23-68. (EE3) Bryant, W. M. D. Microscope 1992, 40 (4), 255-257. (EE4) Fortsch, E.; Uhr, W.; Wondratschek, H. Microscope 1992, 40(1), 3137. (EE5) Petford, N. Microsc. Anal. 1993, (37), 19-21. (EE6) Roedder, E. Microscope 1992, 40 (l), 59-79. (EE7) Armbruster, T.; Bermanec. V. Microscope 1992, 40 (I), 21-30. (EE8) Llang, K. K. Microbeam Anal. 1991, 26, 81-84. (EE9) Richards, J. P.; Kerrich, R. Econ. Geol. 1993, 88 (3), 716-723. (EE10) Petford, N.: Miller, J. A. Am. Mineral. 1992, 77 (5-6), 529-533. (EE11) Zezin, R. B.; Smlrnova, E. P.; Saparin, G. V.; Obiden, S. D. Scannlng 1992, 74 (I), 3-10. (EE12) Marschalllnger,R.; Hock, V.; Topa, D. Mlcrosc. Anal. 1993, (38), 7-9. (EE13) Marabini,A.; Battagiia, S.: Ciriachl, M. Part. Sci. Technol.1991, 9(3-4), 161-165. (EE14) Occelll, M. L.; Drake, B.; Gould, S. A. C. J. Catal. 1993, 142(2), 337348. (EE15) Meisner, L. B.; Eflmklna, E. Y.; Frez, A. I.; Raguzin, R. M. Razved, Okhr. Nedr 1991, (5), 20-22. (EE16) Meyer, A.; Rouguet, G.; Lecourtier, J.; Toulhoat, H. Collect. Colloq. Semin. 1992, 50, 275-279. (EE17) Mlcroscope 1992, 40 (1). 1-122. (EE18) Abbott, R. N. Am. Mlner. 1993, 78, 952-956. (EE19) Gunter, M. E.;Ribbe, P. H. Zeolites 1993, 73. 435-440. (EE20) Gunter, M. E. Encyclopedia of Earth System Science; Nlerenberg, W. W., Ed.; Academic Press: San Diego, CA, 1992; Vol. 3, pp 467-479. FF. CEMENT AND CONCRETE Lange, D. A.; Jennlngs, H. M.; Shah, S. P. J. Mater. Sci. 1993, 28(14), 3879-3884. Laurencot, J. L.; Pleau, R.; Pigeon, M. Roc. Int. Conf. Cem. Microsc. 1992, 74, 259-273. Gouda, G. R.; Nisperos, A.; Bayles, J. froc. Int. Conf. Cem. Mlcrosc. 1992, 74. Gouda, G. R.; Nisperos, A.; Bayles, J. Roc. Int. Conf. Cem. Mlcrosc. 1993, 75. Mitchell, G. D.; Davis, A. frepr. Pap.-Am. Chem. SOC.,Div. fueichem. 1992, 37(3), 1360-1366. Chromy, S. ZKG Int., Ed. B 1992, 45 (lo), 538-540, 542-543. O'Nelli, R. C. froc. Int. Conf. Cem. Mlcrosc. 1992, 74, 198-208. Jie, Y.; Warner, D. A.; Clark, B. A.; Thaulaw, N.; Skalny, J. froc. In?. Conf. Cem. Microsc. 1993, 75, 250-263. Price, R.; Caveny. 8. Roc. Int. Conf. Cem. Mlcrosc. 1992, 14, 114133. (FF10) Curtll, L.; Glelly, J.; Murat, M. Cem. Concr. Res. 1993, 23(2), 329-334. (FF 11) Wakeley, L. D.: Wong, G. S.; Burkes,J. P. froc. In?.Conf. Cem. Microsc. 1992, 74, 274-289. (FF12) Caveny, 8. Roc. Int. Conf. Cem. Microsc. 1992, 74, 29-52. (FF13) Jang, L. A.; Love, H. Roc. Int. Conf. Cem. Mlcrosc. 1993, 75,352-360.
(FF14) Shayan, A.; Quick. G. W. ACI kfrrter. J. 1992, 89 (4), 348-361. (FF15) Draper, E. A.; Skakry, J. Mwosc. T&y 1992. (S), 4.
GQ. GLASSES, CERAMICS, AND ABRASIVES
((XI) Powell, K. L.; Yeomans, J. A.; Smith, P. A. J. Mwosc. 1993, 769(2), 189-195.
W&w.G. A. D.; Lawrence, C. W.;
Scruby, C. 8. J. hfh~osc.1993, 769 (2), 139-153. (003)Tanaka, S. sosel to Kako 1992, 33 (381), I 119-1 123. (W) Fagan, A. F.; Brbgs, F. A. D.; Czemuszka, J. T.; Scruby, C. 8. J. Mater. Sd. 1992, 27(5), 1202-1206. (GG5) Ikeda, Y.; T o m , H.; Shlbata, H. .?i?kyoKa~aku1992.29(4),195-203. (-1 hngre2. S.; BaMkn, E.; A r d d , W. Awust. Imeghg 1992, 79, 691696. ( W 7 ) Fisdrer, R.; Franz, E. D.; T e k , R. Sprsdweell992, 725(12), 797-804. (Goa) Castell, R.; DI Glampolo, A. R.; h a , J. &ah & u n d a r y c O n ~ p r o p . Flne Ce”.1992, 300-308. ( W 9 ) J. Mfcrosc. 1993, 769 (2). (GG2)
HH. METALS (HH1) Kodel, A,; Mori, T; Om, H. hktu Shed 1993, 93 (l), 44-49. (HH2) a c h e r , P.; Reimer, L. Sann& 1993, 75 (3), 123-129. 11. SEMICONDUCTORS AND ELECTRONICS (111)
WotStW, B. W.; POlltZer.8. A. SOWS&& TechM. 1993,36(5), 55-56, 59. Quate. C. F. Springer Ser. SdMStste Scl. 1992, 777, 85-96. Kendlng, M.; AbdeKiewad, M.; Addison, R. Cwros/on1992, 48 (5), 368-372. WataMbe, I.; Sakuyama, S.; NetOri. K.; -0, M. Jpn. Kokai Tokkyo Koho JP 04,110.655 (92,110,655) 13 Apr 1992; appl. 90/226,560, 30 Aug 1990. Phang, J. C.; Pey, K. L.; Chan, D. S. H. Trans. € k h n Devices 1992, 39 (4). 782-791. Joseph, T. W.; Berry, A. L.; Bossman, B. I S F A ’92, Roc. Int. Symp. Test. Falhue Anal., 18th 1992, 1-7. Yoshkka, Y. Bun&/ 1992, (7), 517-525. Castagne, M.; Flllard, J. P.; Lussert, J. M.; M’tlmet. H. Roc. SPE-Int. SOC. Opt. EW. 1992, 1767, 280-286.
JJ. FORENSIC SCIENCE Wlelbc, D.; Tebbet. I.R. J. forens(c Scl. 1992, 37 (4), 1134-1 138. Klrchhoefer, R. D. J. AOAC Int. 1992, 75(3), 577-580. Kohn, W. H.; Jeger, A. N. J. Forensk Sd. 1992, 37(1), 35-41. McCrone, W. C. Mlcrosc~pe1992, 40 (3), 193-198. Harris, H. A.; Kane, T. J. Fofensk Sd.1991. 36 (4), 1186-1191. Stanley, E. A. Mlcrosc~pe1992, 40 (3), 149-152. krtshorne, A. W.; Laing, D. K. fmnsk Scl. Int. 1991, 57 (2), 263272. SUukl, E. M. J. fonmslc SC/. 1992, 37 (2), 467-487. Wilson, B. Chem. Bf. 1993, 29(5), 415-417. McCrone, W. C. Mlcrosc~pe1992, 40(1), 109-121. Fraysler, H. D.; Van Hoven, H. 1992, 40 (2), 107-109. Robertson, J. In Forensic 5amhaMon of F/befs Robertson, J., Ed.; Homood: ChlCheStW, U.K., 1992; pp 67-98. Carol, G. R. In fwensk €xamhaMon of Fibem Robertson. J.. Ed.; Hotwood: Chlchester, U.K., 1992; pp 99-126. Ferguson, D. J. P. Mlcrosc. Anal. 1992, (30), 5-7. Gorskl, A.; Brauner, P. Mcrusoope 1992, 40 (2), 103-106. KlSln, M. V.; QoloVln, A. V. MwoscOpe 1992, 40 (4), 259-264. Dunbp, J. I n fwensk €xamk?eMon of Fbem Robertson, J., Ed.; Homood: ChiChStW, U.K., 1992; pP 127-141. K-)ey, R. H. Chem. Bf. 1993, 29(5), 412-414. Zelchner, A.; Glattstein. B. J. f m k &I. 1992, 37 (3), 738-749. Allen, T. J. Vlb. SpeciXwc. 1992, 3(3), 217-237. McCrone, W. C.; Andreen, J. H.; Tsang, S. Mlcmscope 1903, 4 1 (4). 161-1 82. 1999, ~pe 4 1 (1). 13-14. Bailey, J. G. M l ~ r ~ ~ c Choudhry, M. Y. J. Foren& Scl. 1991, 36(2), 366-375. De betano, D.; Siegei, J. A.; Klomparens, K. L. J. Forenslc Scl. 1992. 37(1), 281-300. Morlta, M.; Tabata, N.; Ikdea, T.; Azuml, J. Nbpon Holgaku Zasshl 1992, 46 (6), 403-404.
KK. FOOD AND FEED (KK1) Flint. 0. Anal. Roc. 1992, 29 (3), 106. (KK2) MacDonaM, H. S.; Crocker, D.; Derby, J. Mlcuoscope 1902. 40(2), 125- 129. (KK3) Kim, H. R.; Hermansson, A. M.; Erlkeson, E. Starch/Staerke 1992, 44 (4). 136-141. (KK4) Rwney, M. K.; Fulcher, R. G. J. Fwd Sd. 1992, 5 7 (9,1246-1247. (KK5) Mandenis, A. AnahrPls 1993, 27 (9,M22-M26. AM/. 1992, (34). 15-17. (KK6) Irving, D. W.; allant. D. J. m. (KK7) Wetrel, D. L.; Reffner, J. A. Cereal Foods Wc& 1993, 38 (l), 9-20. (KK8) Van Geljn. N. J. Zuckeilmlusbk 1992, 7 77 (5). 338-342. (KK9) R u n , R.; utchtleld, J. E.; Eckoff, S. R. Cereal Ct”.1992, 69 (a), 600-606. (KK10) Relsterer, K. M.; Zottoia, E. A.; Rulcher, R. (3. Food Techno/. 1993, 47 (5), 104-108.
(KK11) Swartz, D. R.; Greaser, M. L.; Marsh, B. B. Meat ScI. 1993, 33 (2), 139-155. (KK12) A~,N.P.;Ha~y,R.D.;Akin,D.E.FwdSbuct.1992, 77(1),25-32. (KK13) Akin, D. E.; Rigsby, L. L. Food StfUCt. 1992, 7 7 (3), 259-271. (KK14) Akin, D. E.; Hartley, R. D. J. Sci. FoodAg*tc. 1992, 59(4), 437-447. (KK15) Hung, L. T.; Lee, S. R.; Lee, C. H.; Hung, C. E.; Shih. C. H.; -1 XuebaO 1992, 33, 1065-1071. (KK16) Connell, C. 0.;Cottell. D. C. Roc.R. Mlcrosc. Soc, 1992,27(2), 106107.
LL. BIOLOGY AND W D I C I N E Jones, J. J.; Boyde, A.; Piper, K. Mlcrosc. Anal. 1992, (30), 18-20. Cullen, D. C.; McKerr. G.; Hughes, E. M. Mlcrosc. Anal. 1993, (37), 29-3 1. Peboll, W. M.; Cavanagh, H. D.; Jester, J. V. J. Mlcmsc. 1993, 770(3), 2 13-2 19. Goncz, K. K.; Batson, P.; Clario, D.; Loo. B. W.; Rothman, S. S. J. M/C’OSC. 1992, 768 (I), 101-110. Nlng, 0.; Fujlmoto, T.; Kdke, H.; Ogawa, K. cell 7ZssueRes. 1993,277 (2), 217-225. Kawachi, H. Kyoto-twftsu Ika h @ k u zasshl1993, 702 (l), 15-26. Teunis, P. F. M.; Bretschnelder, F.; Machemer,H. J. Mfcrosc. 1992, 768 (3), 275-288. Miyakawa, A. Bunsekl Kagaku 1992, 41 (g), T119-Tl24. Mlyakawa, A. Bunsekl Kaaaku 1992, 47 (9), Tl13-TIM. iLLlOl Fav. F.: Dellavllle. F. U.S.US 5.149.972. Seot 1992. {LLlli hito, A.; Shionya, K. Jpn. Kokai Tokkyo Koho JP 05, 196, 578 (93, 196. 578). 1993. . (LL12) Takoshilr;;r,T.;Masuda,A.;Mukasa,K. ThinSdMF//msl992,27&277 (1-2). 51-56. (U13) Bruckner,A.; Moreth. M.; Trendelenburg. C. Laboratcdumsmedkln 1991, 75 (5), 281-288. (LL14) Morris, A. S.; McMaster, T. J.; Gunning, A. P.; Mlnglns, J.; Thatham, AS.; Mitchell, E. P o w . Rep. (Am. 0”.Soc.,D/v. Po/ym. Ct”.) 1992, 33 (l), 737-738. (LL15) Slavlk, J. Microsc. Anal. 1992, (28), 13-15. (LLl6) Scudder, K. M.; Christian, G. D.; Ruzlcka, J. Exp. Cell Res. 1993, 205 (2), 197-204. (U17) Sliman, 0.;Burshteyn, A. PCT Int. Appi. WO 93, 15. 117; US Appl. 827, 347; 92. (LL18) Chen, E. Q.; Lam, C. F.; Perlasamy, A. J. Mlcrosc. 1991, 764 (3). 237-243. (LL19) Tamm, L. K.; Kalb, E. Chem. Anal. 1993, 77 (Part 3), 253-305. (LL20) Tamm, L. K. Opt. Mlcrosc. 1993, 295-337. (LL21) Williams. R. C. Cykwkekton, 1992, 151-166. (LL22) Cherty, R. J. Trends Cell Bbl. 1902, 2 (8). 242-244. (LL23) Schwartz, D.; Li, X.; Hernandez, L. I.;Ramnarain, S. P.; Huff, E. J.; Wang, Y. K. Science 1993, 262(No. 5130), 110-114. (LL24) Wang, Y. L Cytoskeleton, 1992. 1-22. (LL25) Auzanneau, I.; Barreau, C.; Salome, L. C.R. Acad. Scl., Ser. 3 1993, 376 (5), 459-462. U 2 6 l Enaelhardt. J.: Knebel, W. phvs. Unserer Zen 1993. 24 (2), 70-78. (LL27) E&&, J.; Vahrerde, P.; Stkkert, J. C. Hlstochemkby 1993. 99 (5), 385-390. (U28) Ho, H.; Uede, T.; Sugiyama, T.; Iwasakl, R.; Narlmatsu, E.; Yachi, A,; Klkuchl, K. BW. Fhotoq. 1993, 67 (4). 141-143. (UP91 Hanthamrongwtt, M.; Wlklnson, R.; Grant, M. H. Microsc. Anal. 1993, (36), 9. (LL30) Fujita. S. Kagaku 1993, 63 (I), 45-54. (LL31) Vlovy. J. L.; Selome, L.; Bards, P. Po@?. Rep. (Am. Chem. Soc.. Dhr. poiym. &em.) 1992, 33 (I), 851-652. (LL32) CaMwell, D. E.; Korber, D. R.; Lawrence, J. R. A&. Mbob. E d , 1992, 12, 1-67. (LL33) Coley, H. M.; Amos, W. 8.; Twentyman. P. R.; Workman, P. Bf. J. Cancer 1993, 67 (6), 1316-1323. (LL34) butler, T.; Robert-Nicoud,M.; Guiliy. M. N.; Hernandez-Verdun, D. J. Cen SCI. 1992. 102 (4), 729-737. (LL35) Cannon, J.; Armas, M. LaserFocus WoM1993,29(1), 99-100, 102104. (LL36) Wang. X. F.; Perlasamy, A.; Herman, B.;Coleman, D. M. CM.Rev. Anal. Chem. 1992, 23 (9,389-395. (LL37) Komhauser,G. U.; K m . J. M.; Rosenstein, J. M. J. H&tdmm. Cyrocrwwn. 1992, 40 (S), 879-862. (LL38) Lipp, P.; Nlggli. E. Cell Cablum 1993, 14 (9,359-372. (LL39) Rcdgers, W.; Glaser, M. Opt. Mlwosc. 1993, 263-283. (LL40) Wada, T.; Miyake. H.; Suzukl, H.; Suzukl, K.; Takeoka, Y. Nbpon Sakumotsu Gakkal Kgl 1993. 62 (I), 128-129. (LL41) Matsuo, A.; Yajima, T. Shika Klso Igakkal Zasshll992, 34 (2), 171180. (LL42) Warky, A. Miwosc. Anal. 1002, (28), 7-9. U 4 3 ) Leggett, 0. J.; Davies, M. C.; Jackson, D. E.; Roberts, C. J.; Tendler, S. J. B.; Wllllams, P. M. J. phys. Chem. 1993, 97(35), 8852-8854. (LL44) Shlbata, D.; Hawes, D.; U. 2. H.; H “ d e Z , A. M.; Spruck, C. H.; Nichols, P. W. Am. J. Patho/. 1992, 747 (3), 539-543. (LL45) Mlneuchl, K.; Takahashi, K.; Tamura, K.; Nakamura, T.; Kolzuml, M.; Kano, H. Klserazu Kogyo Koto S e n m Qakko Kiyo 1893,26,67-71. (LL46) Bronk, J. F.; Powers, S. P.; Qores, G. J. Anal. Blochem. 1993, 270(2), 219-225. (LL47) McClung, W. G.; Feurstein, I.A. Blometerlals 1992, 73(12), 871-877.
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(LL48) Doglla, S. M.; Blanchl, L.; Colombo, R.; Allam, N.; Morjani, H.; Manfalt, M.; Villa, A. M. Proc. SPIE-Int. Soc. Opt. fng. 1993, 7922, 128-134. (LL49) Auranneau, I.; Barreau, C.; Salome, L. C.R. Aced. Sci., Ser. 3 1993, 376 (5), 459-462. MM. PHARMACEUTICAL (MM1) Watanabe, A. Pharmaceutical Analysis Using the Polarized Light Microscope; Hlrokawa Publishing Co.: Tokyo, 1991. (MM2) Hu, J. J.; Johnson, J. B. Proc. SPIE-Int. Soc. Opt. Eng. 1992, 7687, 339-348. (MM3) Mueller, R. H.; Helnemann, S. Clin. Nutr. 1992, 7 7 (4), 223-236. NN. MICROCHEMICAL ANALYSIS ("1) ("2) ("3) ("4)
Delly, J. G. Microscope 1992, 40 (3), 207-218. Coates, A. Microscope 1993, 47 (2/3), 53-54. Mom, J. L. Microscope 1992 40 (3), 225. Benko, J. J. Microscope 1993, 47 (2/3), 55-56.
(PP6) (PP7) (PP8) (PP9)
Laughlln, G. J. Roc. R. Microsc. Soc. 1992, 27 (l), 9-15. Moss, R. D.; McCrone, W. C. Microscope 1992, 40 (2), 123-124. Fodor, M.; Gyorgy. I.; Migaly, B. Epitoanyag 1992, 44 (6). 214-216. Platek, S. F.; Riley, R. D.: Simon, S. D. Ann. Occup. Hyg. W92, 36(2), 155-171. (PP10) Wylle, A. G.; Bailey, K. F. Am. Ind. Hyg. Assoc. J. 1992, 53(7), 442447. (PPl1) Nessler, R. Microsc. Anal. 1993, (37), 37. (PP12) Millette, J. R.; Longo, W.E.; Hubbard, J. L. Microscope 1993, 47(1), 15-17. (PP13) Millette, J. R.; Brown, R. S. Microscope 1992, 40 (2), 131-135. (PP14) Yu, S. Y.; Harris, M. L.; Llacer, V. Microscope 1993, 47 (2/3), 45-49. (PP15) Verma, D. K.; Clark, N. E.; Jullan, J. A. Am. Ind. Hyg. Assoc. J. 1981, 52(3), 113-119. (PP16) Berghmans, P.A.; Adams, F. C. Surf. Interface Anal. 1892, 79(1-12). 439-444. (PP17) Takao, S.; Sakural, T.; Nakamura, M.NipponKagakuKaishi1992, (12), 1470- 1478.
PP. ASBESTOS ANALYSIS
00. ART CONSERVATION/AUTHENTICATlON
(PPl) Perklns, R. L.; Harvey, B. W. Methodfor theDeterminationofAsbestos In Bulk Building Materials; EPA1600IR-93/116; 1993. (PP2) Brackett, K. A.; Seltz, S. D.; Clark, P. J. Microscope 1992, 40 (3). 164-170. (PP3) Brackett, K. A.; Clark, P. J.; Millette, J. R. Microscope l W 2 , 40 (3), 159-163. (PP4) NIST Certificate of Analysis SRM 1867, 1993. (PP5) Verkouteren, J. R.; Steel, E. 6.; Wlndsor, E. S.; Phelps, J. M. J. Res. NIST 1992, 97 (6), 693-705.
(QQl) Allen, T. J. Vib. Spectrosc. 1892, 3 (3), 217-237. (QQ2) Koschek, G. J. Microsc. 1992, 768 (l), 79-84. (QQ3) Schulz, H.; Kropp, B. Fresenius'J. Anal. Chem. 1993,346(1-3), 114122. (QQ4) Turner, N. E.;Watklnson, D. Glass Techno/. 1993, 34 (2), 89-70. (QQ5) Best, S. P.; Clark, R. J. H.; Withnall, R. Endeavour 1992, 76(2), 66-73. (QQ6) Best, S.; Clark, R.; Daniels, M.; Wthnall, R. Chem. Br. 1993, 29 (2), 118-119.
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