Chemical Microscopy George G. Cocks Cornell University, Ithaca, N. Y. 14853
The previous review in this series (44) covered the 2-year period from January 1972 through December 1973. This review covers the period from January 1974 through December 1975. However, a number of references are included here which were omitted from the previous review. In this review, an attempt has been made to include articles and books of potential interest to those who use the microscope to solve chemical problems. However, no attempt has been made to report publications in the fields of biochemistry, petrography, metallography, or ceramography unless these appeared to be of direct interest to chemists or chemical engineers. The chemical applications of electron microscopy are also omitted. References to publications in the fields of optics and crystallography are included if they appear to be of direct interest to chemists or chemical engineers. The great diversity and number of publications of interest to chemical microscopists make it nearly impossible to find and review all of them. Therefore, we would appreciate comments or suggestions, particularly with regard to the omission of important published articles. I also appreciate the kindness of those who pointed out omissions from the 1973-1974 review, and those who sent reprints of papers for inclusion in this review. In preparing this review, many references to the literature were first found in bibliographic sections of several journals, notably Microscopica Acta and Mikroskopie. The Microscope has continued t o print a literature survey (221,222) although i t appears a t indefinite intervals.
BOOKS OF GENERAL INTEREST A “Short History of American Microscopes” has been written by Padgitt (250) and a brief version of this history has appeared (251 ). Several introductory books on microscopy have been published, “Beginning With the Microscope” by Moellring (229), “The Revealing Lens” by Ford (84),and “An Introduction to the Practical Study of Crystals, Minerals and Rocks” (49). A book entitled “Geological Thin Section Microscopy” has been written by Ahmed (1). Rinne and Berek (280) have published (in German) an introduction to general microscopy and to polarization microscopy of solids. An introduction to the theory and practice of chemical microscopy in research has been written (in German) by Emons et al. (76). Two more volumes of the “Handbuch der Mikroscopie in der Technik” have appeared, one (89,125) dealing with chemical microscopy and the other (90) concerned with food microscopy. Part two (378) of Zieler’s “The Optical Performance of the Light Microscope” dealing with the geometrical optical aspects of image formation has now been published. Part one (377) was reported in the previous review (44).Both of these books are part of an extensive series, “The Microscope Series“, being published by Microscope Publishing Ltd., Chicago, Ill. Other books in this series which are now available are “Accessories for the Light Microscope” (212) and “The Microscopy of Liquid Crystals” (148). An “Encyclopedia of Microscopy and Microtechniques” (mostly of interest to biologists) has been published by Gray (119).A small handbook of data on optics and microscopy (in four languages) is available from Heerbrugg (367).“The Focal Dictionary of Photographic Technologies” (319 ) includes information on light and electron microscopy and holography. Dainty and Shaw (55) have published a book entitled “Image Science; Principles, Analysis and Evaluation of Photographic Imaging Processes”. “Optical Information, Processing and Holography” by Cathey (39) contains information of interest to microscopists. A report of a symposium entitled “Quantitative Imagery in the Bio-Medical Sciences-11” (152) contains papers on densitometry, quantitative analysis of images, laser microbeams, x-ray and electro-optical imaging, and other
similar subjects. A series of books dealing with the general subject of microstructural analysis have been published (87, 93, 120, 204). These books are proceedings of meetings and symposia sponsored by the International Metallographic Society. The reports contained in these books are not confined to metallography. Chapters or sections on light microscopy have appeared in several books. McCrone (209) has contributed a chapter on light microscopy to a book entitled “Characterization of Solid Surfaces”. Richardson (273) has written a chapter on “Optical Microscopy” for “Systematic Materials Analysis, Vol. 3”. Stanley (32) has published a book on “Applied Physical Techniques” which includes sections on interference, polarizing, and ordinary microscopy as well as optics, optical instruments, and electron microscopy.
ARTICLES OF GENERAL INTEREST A number of articles on the history of microscopy have appeared. Freund (88)discusses (in German) the development of polarizing microscopy, petrography, coal microscopy, metallography, and photomicrography during the past 150 years. Herzberger (153) has contributed an article on “The History of the Image of the Microscope”. Rienitz (276) writes (in German) on the early history of the theory of diffraction as it relates to the formation of the microscope image. Three authors (22, 278, 337) consider Abbe’s contributions to the theory and practice of microscopy. All three of these articles are written in German. A brief history of the American microscope has been written by Padgitt (251) (see also 250). The microscopes of G. S.Plossl are the subject of an article by Hoelzl et al. (160).The scientific work of W. J. Schmidts who was interested in using the polarizing microscope to study animal tissues is recounted by Frey-Wyssling (92). The same author (91) discusses ultrastructural research in biology before the introduction of the electron microscope. McCrone (210) discusses the future of chemical microscopy. Jebsen-Marwedel (168) discusses a trend in microscopy, namely the change from “Phenomenology to Metrology”. The use of the stereomicroscope as a time and labor saving device is the subject of an article by Gumpertz (129).He also includes a brief history of this valuable instrument. Watts (353) has written an article on technical writing and translating for microscopists in which he advocates the standardization of terms in microscopy. Turner (342) is concerned with the history of communication in microscopy, but his interest lies primarily with the means of illustrating the microscopical image. Bingley and Firth (24) discuss ways of testing microscopes. Swift (329) describes a moirk fringe technique for checking the magnification of a microscope. In an article (in German) on the accuracy of imaging in special microscopical techniques, Schaefer and Hanselmann (295) consider the relative merits of increasing contrast by instrumental means or by means of preparing the specimen. Frahm (85) describes the use of a finding chart for immersion lenses. The use of the aperture diaphragm to control depth of field in compound and stereo microscopes is the subject of an article by Schleuter (300).The use of PCB’s (polychlorinated benzenoids, which are carcinogens) in immersion oils is the subject of a letter written by Bennett and Albro (19). A study of the methodology of correlating light and scanning electron microscopy in the examination of minerals has been presented by Wilding and Geissinger (368). OPTICS See Books of General Interest (367) and Articles of General Interest (22. 153. 276. 278. 337). Phase retrieval in’ light and electron microscopy is the ANALYTICAL CHEMISTRY, VOL. 48, NO. 5, APRIL 1976
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subject of an article by Drenth et al. (67).Pulvermacher (268) discusses the imaging of partially coherently iluminated plane gratings in the transition region between Kohler and critical illumination. Albrecht-Buhler ( 2 )considers one-sided oblique illumination in light microscopy, particularly the effect of increasingly incoherent illumination. Diffraction images of truncated triangular wave objects formed by a polarizing microscope with crossed polarizers are the subject of a theoretical letter by Chopra et al. (42).The problem of resolution and its relationship to quantitative image analysis is discussed by Serra and Mueller (308).Gupta (131) writes concerning the influence of apodized condensers on microscopical images of slit and bar objects, and Gupta and Singh (132)have contributed an article on the frequency response of apodized systems. A book entitled “Atlas of Optical Transforms” has been published by Harburn, Taylor, and Welberry (141). The induction of birefringence in specimens through exposure to linearly polarized ultraviolet light is reported by Pliny and Vacek (260).Yamazaki and Satou (375)report on the measurement of optically induced refractive index changers. White (359) has written a comprehensive article on the correction of tubelength to compensate for coverglass thickness variations. Hinds (158) describes an OTF (optical transfer function) scheme for optical scanning microscopy. It consists of an electronic filter for the amplification section of the Vickers M85 scanning microscope. Hoffman and Gross (161) report on the theoretical and experimental aspects of a “modulation contrast microscope”. G6ke (112)describes (in German) the stereo-phase contrast method which concerns Pluta’s Stereo-phako microscope. Hielwarth and Christensen report on a “nonlinear optical microscope using second harmonic generation” (156),and on its use in examining the structure of polycrystalline ZnSe (155).Amato and Ewing ( 3 ) have written a letter concerning an instrument for simultaneous measurement of optical rotary dispersion, circular dichroism, and absorbance.
INSTRUMENTS A variety of accessories for the light microscope are described and discussed in a book by McLaughlin (212). Microscopes.See Optics (112,155,156,158,161).A variety of microscopes have been described in the literature. In addition to those cited under Optics they include: a monobjective stereo microscope described by Goke ( I l l ) , the Reichert UnivaR described by Schindl (298),a modular microscope described by Seidl(305), a scanning slit microscope described by Maurie (217),a “Sonomicroscope” described by Kessler (181),by Eggleton and Kessler (721,and by Eggleton, Kessler, Vinson and Boder ( 7 3 ) ,a superresolution microscope using electrical superposition of holograms described by Sato, Ueda, and Yamagishi (291),and a laser doppler microscope described by several authors in several articles (225, 226, 228, 332). The use of the laser doppler microscope to measure the velocity of blood flowing in capillaries has also been described in several articles (227, 281, 331). Lea (197) describes the modification of an incident light microscope for fluorescence studies. Several authors have described instruments which are either computer controlled or are automated image analyzing instruments. Among these are: a computer-controlled scanning optical microscope described by Jarvis (167),a scanning-interference microscope-photometer described by Boguth (27), and a microspectrofluorometer, with epi-illumination, operated under computer control described by Ploem, et al. (262).Dew et al. (62)described an automatic microscope system for differential leucocyte counting. Serra (307)gives the theoretical basis for the Leitz texture analyses system. Objectives. A new dispersion staining objective has been reported by McCrone (207).Pabst (248)tells of a new method for cleaning the front lenses of objectives with poly(styrene) foam and also with laps and with leather. Condensers. See Optics (2, 131,268). Illuminators. See Optics (2,268).Mohr (231)has written concerning light generation with luminous discharge lamps and their applications in microscopy. He is mostly concerned with illuminators for stereomicroscopes. Sutter (328) has measured the spectral output of quartz halogen lamps (Osram 7577, Phillips 6258 and Osram 64150) between 420 and 700 334R
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nm. Kraft (191)and Kraft and Koch (192)discuss the technology of new fluorescence illumination systems, especially the Ploempak 2. van Maaren (345)describes a variable electronic flash tube illuminator (called Visliflash) that can be run continuously at low powers for visual observations or operated as a flash tube for photomicrography. Hoc (159)describes a simple easily built light pipe illuminator used for top lighting a specimen. Stages. A very useful article entitled “High and Low Temperature Microscopy” has been written by McCrone (206).In it he describes a variety of cold and hot stages and tells about their use in microscopy. Smith (316)describes a simple cold stage using a Peltier element. Hartshorne (149) reports on the construction and use of a hot-wire stage. Frohne and Suhr (94) use a cigaret lighter to heat microscopical preparations. Rinehart (279)reports a microscope chamber for use with a flowing gas atmosphere. Davidson (57) describes various pressure cells for use with the light microscope. Kachel (178) has built a special Coulter counter cell and arranged it so that flash photographs can be taken of particles passing through the orifice. A microcultural chamber with continuous perfusion and temperature regulation has been reported by Pouchelet and Moncel (264).A similar cell has been designed by Rieb (275) who also describes a mechanical timer for time lapse cinematography using the cell. Drewinko (68) has also designed a culture flask for cinematography using phase contrast objectives. Whitehead (362)describes a chamber with which he can record, cinemicrographically, the growth of pyrene perchlorate crystals by electrolysis. A micromixing stage has been devised by White and Cunningham (360)for following the course of mixing as a function of shear rate, particle concentration, particle shape and size, and the rheology and properties of the continuous phase. Schmid-Schonbein et al. (301)have also designed a “Rheoscope Chamber” for studying blood aggregation by microscopical observation and microphotometry. Green (123)reports on an instrumented straining stage for light microscopy. van Eek (344) has designed and built a mechanical stage for use with comparison microscopes. Miscellaneous. See Optics ( 3 ) .Lemkin et al. (198, 199) describe a “Real Time Picture Processor for Use in Biological Cell Identification”. Troyer describes two devices for microcinematography: a simple film speed regulator (339),and a device for measuring film speed for short runs (340).Graham (118) presents an automatically focusing cinemicrographic system for studying blood circulation. A versatile drill stand for photomacrography has been described by Arendt and Beeman ( 5 ) . Denne (60)describes a simple two-circle goniostat for use with a high-powered microscope. Atosi and Bielick also describe a miniature goniometer head. Three instruments for irradiating small areas of microscopic specimens have been reported. Two of these use lasers (20, 52) and the other an ultraviolet beam from a Hg arc lamp (321). A “Schlieren Eyepiece” is described by Dodd and McCrone (66).Whitefield (361) reports on a “Noncontact optical profilometer”, and Greer and Brockman (124) describe an electromechanical micromanipulator. Steinkamp et al. (323)report on “A new Multiparameter separator for microscopic particles and biological cells”.
MICROSCOPICAL METHODS Polarized Light Microscopy. See Books ( 1 , 49, 76, 280, 320);Articles of General Interest (88, 91,92);Optics (3,42 ; and Instruments, Miscellaneous (10, 60). The general subject of polarized light is treated by Swindell (330) in his recent book. A book entitled “Polarisationsmikroskopie in der Histophysik” has been published by Schenner and Hutschenreiter (297). Two books on the use of the polarizing microscope in the physical sciences are: “Einfuhrung in die Praktische Polarisations-Mikroskopie” by Czaja (54) and “Laboratory Manual of Petrographic Techniques” by Hutchinson (164). Hartley (146) has written a simple introduction to the use of the polarizing microscope. Rienitz and Stock (277)compare statistically three methods of measuring optical path differences in interference microscopy. Soltzberg (317 ) describes a high-path-difference
George G. Cocks has been associate professor of chemical microscopy in the School of Chemical Engineeringat Cornell University since 1964. He has been interested in light and electron microscopy and in optics. He graduated from Iowa State University in 1941, having received a B.S. degree in chemical technology. After working as an analytical chemist for the Allison Division of General Motors for a year he joined the U S . Naval Reserve and spent the war years as an Engineering Officer. In 1949 he received a W.D. in chemical microscopy from Cornell University. He was employed in the Physics of Solids Division at Battelle Memorial Institute from 1949 until 1964. He is a fellow of the AAAS and the Royal Microscopical Society and a member of the ACS, the Optical Society of America, and the New Ycfk Microscopical Society. He is a member of the Electron Microscopy Society of America.
optical compensator, and its use in observing solid-solid phase transformations. Miller and Duffy (223) discuss the orientation of crystals between crossed polarizers. Bryant has published two excellent articles: one entitled “Dispersion of the optical indicatrix as a key identifying characteristic for small particles” (35) and the other on “Accessory techniques for particle identification in polarized light” (36). Flinn (82) has described two flow charts for orthoscopic universal stage techniques. Nelson (242) discusses apparatus for the microscopical determination of ore minerals. Clancy (43) reports on the crystallographic and optical characterization of a and fl silicon nitride. Tanner and Fathers (333) discuss the contrast of crystal defects under polarized light. Patrick et al. (254) report on the development of optical anisotropy in vitrains during carbonization. They include a quantitative classification of anisotropy. Sieminski (313) has published a note on the measurement of birefringence in fibers. Whitehead (363) has quantitatively analyzed fish scales using polarized light. Gathercole et al. (97) have used polarized light microscopy to examine the periodic pattern in native tendon collagen. Nihei et al. (246) have used fluorescence polarization to observe changes in attitude of S-1 moieties in muscle fibers. Taylor et al. (334) have determined the polarization optical properties of the amyloid-congo red complex by phase modulation microspectrophotometry. Harosy and Malerba (144) discuss the role of plane polarized light in microspectrophotometry. Goldstein and Williams (115) have improved the quantitative assessment of autoradiographs using polarized light photometric microscopy. Microphotometry and Microspectrophotometry. See Optics ( 3 ) ;Instruments, Microscopes (27,262), Stages (301); and Methods of Microscopy, Polarized Light (115, 144,334). “Modern Technique in Reflectance Measurements” is the title of an article by Piller (259). Such measurements can be used to identify components of a mixture, for chemical analysis, and for determining refractive index and absorbance. Fischer (80) discusses the potential for miniature spectrophotometers. Goldstein (113) considers an important aspect of microdensitometry, the monochromator system. Jacob and Knickrehm (166) show how photometrically determined reflectivities of solids immersed in given immersion oils can be converted to reflectivities exhibited when the solid is immersed in other media. A number of authors have described microphotometers or microspectrophotometers. Loeb (203) describes a new modular microscope photometer. Nagy (.240) tells how the Leitz Orthomat 35 mm automatic camera can be converted to a cytophotometer without losing its regular functions. Casella et al. (37) describe a simplified recording microspectrophotometer. The Denver Universal Microspectroradiometer (DUM) is described by David and Galbraith (56). This instrument can also be used as a fluorometer and microrefractometer. The optical design of a special microspectrophotometer is given and its use to study the waveguide properties of frog rods is described by Enoch and Tobey (77). Mayer and Novacek (218) describe a direct recording corrected microspectrofluorometer. Bassleer et al. ( 1 6 ) describe recent progress in cytophotometry as exemplified by the Barr and Stroud GN2, and Leitz MPV instruments. Ruch and Trapp (285) discuss microscope photometry and cytofluorometry.
Two papers, one by Entingh (78) and one by Haas (133), are concerned with the use of microeflectometer and a scanning densitometer, respectively, for measuring autoradiogram densities. Applications of microphotometers and microspectrophotometers include a method for studying opaque minerals (261) and a study of the relation between microstructure and optical properties of polycrystalline alumina (256). Microphotometry combined with cinemicrography can be used to follow pigment migration in fish melanophores (312) and to determine light-induced chromatophore movements in brown algae (258).
Interference Microscopy. See Instruments, Microscopes (27);and Methods of Microscopy, Polarized Light Microscopy (277). Beyer (23) has written a book (in German) on the theory and practice of interference microscopy. Hannes (140) dis-
cusses (in German) the use of interference microscopy in the chemical industry, e.g., the measurement of the thickness of transparent foils and fibers. Gundlach and Huenert (130) discuss (also in German) the use of interference microscopy in biology. Wolter (372) compares and contrasts the methods of phase contrast, schlieren, and interference microscopy. Phase multiplication, a new and sensitive method of interference microscopy has been described by Khashan (182). Boguth (28) has designed a device for interchanging object and reference fields in a Leitz transmission interference microscope. Wolf (371) tells in great detail how the Nomarski interference contrast apparatus (DIK of C Zeiss) can be modified for use with planachromatic objectives and other supplementary parts. The accuracy and precision of the Vickers M86 scanning and integrating microinterferometer is the subject of an article by Goldstein and Hartmann-Goldstein (114). Israelachvili (165)tells how thin films can be studied using multiple beam interferometry. Gillis and Wibo (108) describe how the thickness of ultrathin sections can be measured accurately using interference microscopy. Seeber and Beyer (303) tell how interference microscopy can be used to determine the dry mass of the nucleus, the plasma, and the nucleolus. Ando ( 4 ) has used differential interference microscopy to observe T-wall domains in NiO. Florian and Heyer (83) describe the use of interference microscopy to study the growth of single crystals, e.g., hexamethylenetetramine, and Rhodes (272) has used holographic interference microscopy to study polymer crystallization. Fluorescence Microscopy. See Instruments, Microscopes (262), Illuminators (191, 192); Methods of Microscopy, Polarized Light Microscopy (246), Microphotometry and Microspectrophotometry (56,218,285). Thaer and Sernetz (336) have edited the proceedings of a conference on “Quantitative Fluorescence Techniques as Applied to Cell Biology”. Lane (196) explains how the amateur can practice fluorescence microscopy. He describes a simple apparatus. Lea (197) tells how to modify an incident light microscope for fluorescence work. Stohr and Goerttler (326) discuss new instrumental possibilities for optimizing ultrarapid microfluorometry. Wrefort and Schofield (374) describe a microspectrofluorometer with on-line real-time correction of spectra. Elliot et al. (75) present a technique for preparing high-quality photomicrographs of fluorescent objects. Cytofluorometry is an important branch of fluorescence microscopy. A number of papers on this subject have been published, among them are: a discussion of the methodological and instrumentational aspects of cytofluorometry (265), pulsed tunable lasers in cytofluorometry (287), a two-channel microfluorometric method of analyzing metabolic interactions and transport phenomena in the intact cell (188), a spectrophotofluorometer for measuring very weak fluorescence from biological molecules (349), a fluorescence microscope attachment for flow-through cytofluorometry (306), and slitscan-cytofluorometry (357). Some other applications of fluorescence microscopy are listed below: an analysis of ceramic tissue interactions using morphologic, fluorescence, and autoradio raphic techniques. The ceramic was a dense alumina (1267, fluorescence microscopy in organic geochemistry which used polarized light fluorescence to study the interactions of lanthanoid elements and organic materials (255), a histochemical fluorescence ANALYTICAL CHEMISTRY, VOL. 48, NO. 5, APRIL 1976
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method for the demonstration of catecholamines (96)and a new fluorescent reagent (isocien) for calcium (162). Phase Contrast Microscopy. See Optics (112);Instruments, Stages (68);and Methods of Microscopy, Interference Microscopy (372). Gerlach ( 100, 101, 102, 103, 104, 105) has written a series of articles covering various aspects of phase contrast microscopy. Basuray ( 17 ) discusses the “resolution of phase particles in phase microscopy”, and Gerlach (106)describes the conversion of a brightfield condenser into a phase contrast condenser. Infrared and Ultraviolet Microscopy. Lloyd (202)has written a book on “Thermal Imaging Systems”. Cohen (45) describes some applications of infrared microscopy to the study of solid state devices. Jungbluth and Black ( 176)write on the scanning laser infrared microscopy of doping inhomogeneities in arsenic single crystals. Wood and Goring (373)describe how a modification of the Leitz uv microscope, the use of a low gelatin content photographic film, and the use of a new epoxy embedding material have permitted extension of uv microscopy to wavelengths as low as 220 nm. Holographic Microscopy. See Books (39);Optics (67, 141);and Instruments, Microscopes (291). Cox (50, 51) has written an article entitled “Holographic Microscopy-A Reassessment” and Rover (284)describes an application of high-speed microholography to the metrology of fogs. Dispersion Staining. See Instruments, Objectives (207). McCrone (208) tells how refractive indices for various wavelengths can be measured without monochromators, special illuminators, or filters and without having to match an index liquid. The technique is dispersion staining. Ultramicroscopy. McFayden and Smith (211) describe an automatic flow ultramicroscope for submicron particle counting and sizing. Yoshida et al. (376) present a new ultramicroscopical technique for the particle size analysis of aerosols and fine powders. Schlieren Microscopy. See Instruments, Miscellaneous (66) and Methods of Microscopy, Interference Microscopy (372). Cox and McLachlan ( 4 8 )report on the use of a schlieren type microscope for a study of crystal growth. TECHNIQUES FOR SPECIMEN PREPARATION
Embedding and Mounting. See Instruments, Stages (94); and Methods of Microscopy, Infrared and Ultraviolet Microscopy (373). A number of articles on embedding and embedding materials have appeared in the literature. Among these are: artifacts in the embedment of water soluble compounds for light microscopy ( 8 1 ) , a method of minimizing formation of spherulites in Carbowax-impregnated clays ( l o g ) , the impregnation of fine-grained sediments with a polyester resin ( 9 ) , and an embedding technique for lamellar and fibrous silicates (335).Germain (107)discusses the advantages and disadvantages of epoxy resins as embedding materials for light microscopy. Molnar (232)reports on double embedding with nitrocellulose and paraffin. Brian ( 3 2 )describes a modified paraffin wax for embedding. Goke ( 110) reports on the use of Aroclor 4465 as a mounting medium for diatoms. Perrie and Peach (257)describe the use of a gelatin coated slide for preparing sediments for particle size analysis, and Moore (233)gives a method of distributing grains for microscopical examination. Sayers (292)describes the use of an aerosol spray-coat acrylic resin lacquer in place of coverslips on microscope preparations. Microtomy. See Methods of Microscopy, Interference Microscopy (108). Stoll and Fengel (327)report on the use of cryomicrotomy for preparing sections of water soaked wood. Markham (214) describes a technique for sectioning paper and plastic films. Two articles on the cutting of epoxy resins have appeared. One (282)tells how to handle and stain epoxy resin sections for light microscopy, the other (283) tells how to prevent electrical charge effects while sectioning epoxies. Boll et al. (29) describe a technique for ultracryotomy. They spray the tissue with a lacquer to hold the section together. Grinding, Polishing, and Etching. Two books on these subjects are: “Metallographie” by Schumann (302) and 336R *
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“Metallographic Specimen Preparation” by McCall and Mueller (205).Sanwald and Gould (290)have written an article on ion etching of metallographic samples. Hartnagel and Weiss (147) discuss the etch polishing of GaAs. Two other articles describe the etching of pyroxenes (224)and etch figures on (012)faces of hematite. Miscellaneous. Porter (263)discusses the use of millipore filters for preparing samples for particle studies. Geissinger (99)tells how to prepare specimens for correlative studies in light microscopy, transmission electron microscopy, and scanning electron microscopy.
TECHNIQUES FOR SPECIMEN EXAMINATION Photomicrography. See Books (55, 319); Articles of General Interest (242); Instruments, Illuminators (345), Stages (264,275,362),Miscellaneous, (5,68,118,198,199,339, 340);and Methods of Microscopy, Fluorescence (75),Infrared and Ultraviolet Microscopy (373). Several authors have written books or articles on the general topic of photomicrography. Bergner (21) has published the second edition of his book “Praktische Mikrofotografie”. Hurtgen (163) has written an article entitled “Practical Photomicrography” and Braginski (31) discusses special techniques in photomicrography. Quackenbush (269) in an article entitled “Critical 35 mm Photomicrography” describes an attachment giving wide field and high resolution. Klosevych (184, 185) discusses microscopy and photomicrography. A systematic approach to color photomicrography is the title of a pair of articles by Vetter (346,347).In a series of four articles Habermalz (134, 135, 136, 137) discusses the correction of color balance for color reversal type films, and in another article he considers the determination of neutral color matching of photomicrographs on reversal color film (138). Special applications of photomicrography include cinemicrographic studies of slip band development in neutron irradiated copper single crystals (245)and the growth of refractory compounds (332).Dullien and Dhawan (69)characterize the pore structure of a material using a combination of photomicrography and mercury porosimetry. Laing et al. (195) present a technique for in-vivo photomicrography of the corneal endothelium. Castenholz (38) describes a new technique, “stripe-photomicrography”, to prepare photomicrographs of moving objects. The enlargment of photographs using the automatic Log Etronics enlarger is discussed by von Prosch (350). Refractometry. See Optics (260, 375); and Methods of Microscopy, Microphotometry and Microspectrophotometry (56, 166), Interference Microscopy (140), and Dispersion Staining (208). Hewlett (154)describes a simple stage refractometer made from a small plano-concave lens. Saylor (293)has constructed a more complex but highly accurate stage refractometer. A simple method for determining the dispersion of refractive indices has been described by Kerl (180). Cold- and Hot-Stage Techniques. See Instruments, Stages 149206,316,341). Charsley and Tolhurst (41) have applied hot-stage techniques along with photomicrography and cinemicrography to the study of pyrotechnic systems (namely Mg(NO& and the W-KzCr207 system) up to 1000 “C. Morrow has written three articles on hot-stage experiments; one on catalytic activity of lead salicylate-modified nitrocellulose (234),one on the “condensed phase behavior of nitrocellulose having different degrees of nitration” (235),and one on a “new microscopically measurable parameter, spreading factor, for characterizing olymeric films during decomposition. Autoraliography. See under Methods of Microscopy, Microphotometry and Microspectrophotometry (78, 133) and Polarized Light Microscopy ( 115). Jenkins (170) describes a method of applying liquid emulsions to slides using a wire loop. Bisconte (25)reports a rapid method for autoradiography of serial sections based on centrifugation. Weinstock and Leblond (356) have studied collagen synthesis using light and electron autoradiography. Stereology. See Instruments, Microscopes ( 111 ). Stereology has become a popular subject and many articles and books have appeared recently. A book by Gaunt ( 9 8 )is entitled “Microreconstruction”. Another book, edited by Weibel et al. (355),reports the proceedings of the third in-
ternational congress for stereology. Methods of stereological analysis are described by Briartz (33),Matheiu and Messier (216),and Prothero, et al. (267). Weibel (354)discusses the selection of the best method in stereology, and Underwood (343)writes on stereology in automatic image analysis. Three articles (13,157,219)discuss criteria for evaluation of threedimensional structures from projections and from sections. Two articles deal with corrections, one (296) for line intersection counts and one (220) for special cases of concentricity and eccentricity. Whitehouse (364) presents a method for calculating internal surface areas in structures which have become anisotropic because of linear expansion or contraction. Four papers discuss instruments. Padawer (249) suggests an aid for viewing stereopairs. Deter (61) describes a film projection system for quantitative stereology, and Vialli (348) proposes a method of obtaining volumetric data using a special eyepiece. E t z et al. (271)describe an on line computer system for point-counting stereology. A number of applications are reported: obtaining particle size distributions from measurements on plane sections through particle beds (71),on grain size from thin sections (179),on quantitative definition of topological properties of sintered materials (95), for characterization of aligned eutectics by electrical analogue modeling (352),determination of average grain sphericity in granular porous media (289), and on measuring microvolumes without using statistical methods (215). Automatic Image Analysis. See Optics (308);Instruments, Microscopes (62,307);and Techniques for Specimen Examination, Stereology (271, 343). Automatic image analysis is another very popular subject and many articles have been published. General articles include one on pattern recognition by automatic image analysis (53),one on automatic image analysis in the biological sciences (74),and a review of automatic image analysis by Jesse (171). The last article, by ,Jesse, coordinates six review papers appearing in Microscope, 2 2 , l . (1974). It is my understanding that a similar series on automatic image analysis will appear in Microscope in 1976. Among the papers in the series mentioned are two by Jesse: information sources in automatic image analysis (172),and a bibliography on the same subject (173). Also in this series is a paper on applications of automatic image analysis in materials science (241). Articles dealing with instrumentation for automatic image analysis are: “Instrumentation in Automatic Image Analyses” (139),a comparison of various instruments for the analysis of metals (15), “Simple Video Method for the Quantification of Microscopic Objects” (70), “The Omnicon T M Pattern Analysis System” (237),the “Leitz Texture-Analyse-System (TAS)” (239), and one on the millipore T MC instrument (174). This last article also discusses using the .rr MC for counting asbestos. Wilkinson et al. (369)evaluate the Quantimet 720 as a tool for determining particle size distributions of monodisperse latices. Leschonski et al. (200) also discuss on line measuring techniques for particle size analysis. A very important application of automatic image analysis is i n recognition and measurement of biological cells and organelles. Articles dealing with this subject are: the application of artificial intelligence techniques to biologic cell identification (309);computer generated synthetic cell images ( 1 4 ) ; a machine to find metaphase cells (121);the design, operation, and evaluation of an automatic metaphase finder (122); computer-controlled multiparameter analysis and sorting of cells and particles ( 6 ) ;a computer system for the measurement of cell and nuclear sizes (47). Particle a n d G r a i n Size. See under Instruments, Stages ( I78) Miscellaneous (323);under Methods of Microscopy, Polarized Light Microscopy (35, 36) and Ultramicroscopy (21I , 376); under Techniques for Specimen Preparation, Embedding (233, 257) and Miscellaneous, (263);and under Techniques for Specimen Examination, Stereology (71, 179). Jelinek ( I69) has written a book on particle size analysis which includes sections on optical methods and pore size analysis. Articles on particle size analysis include: “Particle Size Analysis; Past, Present and Future” (127),“Influence of Sample Volume on the Mean Error of Particle Size Analysis” (3181, and “The Computation of Particle Size-Shape Distributions in Transmission Microscopy” (315). Two articles consider counting particles in thin microtome sections: one deals with determining size distribution (12) and the other
with the number of particles per unit volume (299).DeLange and Selier (59)consider electrostatic fractionation followed by characterization, and Koglin et al. (187)d‘iscuss measurements of surface area. Miscellaneous. Raith (270) delineates p-n junctions in silicon electronic devices by their effect on a coating of liquid crystals. Schabtach and Parkening (294)present a method for sequential high resolution light and electron microscopical examination of selected areas of a specimen. APPLICATIONS OF CHEMICAL MICROSCOPY Crystallography. See Books (1,49,87,148,280,320),Instruments, Stages (149,362),Miscellaneous (10,60);Methods of Microscopy, Polarized Light (43,54, 83, 146, 164,223, 242, 254, 31 7, 333), Microphotometry and Microspectrophotometry (256, 261), Interference Microscopy (4, 83, 272), Infrared and Ultraviolet Microscopy (176),Schlieren (48). Volumes 9 and 10 of the series “Growth of Crystals” have been published (310,311).In volume 10 there is a summary of advances in crystal formation research over the past 20 years. Lieber (201)has published a small book “Kristalle unter der Lupe” which is concerned with micromounts of minerals. It also covers instrumental and photographic aspects of examining these specimens. Juretschke (177)has written a book entitled “Crystal Physics-Macroscopic Physics of Anisotropic Solids”, which has sections on crystal optics and polarization. Crystallographic studies of various materials have also been reported. Among these are: “Optical Detection of Magnetic Domains in Birefringent Crystals” (288),“Microcrystals as Nucleus Centers on Rhombohedral Surfaces of Cultured Quartz” (247),“Crystallographic Properties of Chalcomycin I” (193), “Twinning of P-Cyclotetramethylenetetranitrate (HMX) (189),and “The Optical and Crystallographic Properties of rn-Nitrobenzoic Acid” (175). Resins a n d Polymers. See Methods of Microscopy, Polarized Light Microscopy (313);Techni ues of Specimen Preparation, Microtomy (214), Hot- a n 1 Cold-Stage Microscopy (234,235,236). Battista (18) has written a book entitled “Microcrystal Polymer Science”. Gruber (128) describes topochemical dying and staining reactions on solid polymer phases. Kose et al. (190)report on the examination of ordered latex suspensions. Aronson ( 7 ) discusses some aspects of film formation in emulsion paints. Fraser (86)reports on spherulite content and distribution in polypropylene filaments. Moskowitz and Turner (238)have used metallographic techniques to characterize rubber-modified poly(methy1) methacrylates). Pritikin (266) describes the microscopic structure of reconstituted collagen sausage casings. Chanzy et al. (40)report a light and electron microscopical examination of nascent structures observed during polymerization of ethylene. Textiles a n d Fibers. See Methods of Microscopy, Polarized Light Microscopy (313 ) . Three books dealing with fibers have been published: one an atlas of cotton structure (58),another an atlas of cell materials and paper fibers (1421, and one entitled “Haarmikroskopie” (64).Nettlenstroth (243)discusses microscopical methods for detecting and analyzing textile fibers. Goynes et al. ( I 17) have published a “Microscopical Survey of FlameResistant Cotton Fabrics, Part 1, Treatment Based on THPOH-”3”. This survey includes both light and electron microscopical work. Some structural and physical properties of yarn made on the integrated composite spinning system are reported by Mohamed, Rochow, and Heeralal (230).This is also a light and electron microscopical study. Wood and Paper. See Methods of Microscopy, Interference Microscopy (11);Techniques of Specimen Preparation, Microtomy (327);and in the section above, Textiles and Fibers (142). Bosshard ( 3 0 )has had published a book entitled “Holzkunde, Bd. 1 Mikroskopie and Makroskopie des Holzes”. Dinwoodie (65) reviews the structure-mechanical property relationships in timber. Kibblewhite and Thompson (183) report a light and electron microscopical study of the ultrastructure of the middle lamella region in resin canal tissue isolated from slash pine holocellulose. Cousins (46)describes a method of preparing charcoal for microscopical examination using microtomy. Minerals a n d Ceramics. See Articles of General Interest (368)and, under Techniques of Specimen Preparation, EmANALYTICAL CHEMISTRY, VOL. 48, NO. 5, APRIL 1976
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bedding and Mounting (9,109,335), Techniques of Specimen Preparation, Grinding, Polishing, and Etching (147,224,351 ). Rutherford (286) has edited a book on soil microscopy. Two articles discuss the microscopy of glass ceramics, one examining morphology and crystallization processes (253) and the other the structure of porcelain (244). Microscopical studies of the following materials have been reported: coal (213), coke (116), and electrolytic amorphous germanium (252). Other applications include a study of the catalytic hydrogenation of graphite (338), the solidification of Fe-FeSi eutectic ( 8 ) , the hardness and reflectance of metamict ABZOG-type rare earth (Ti, Nb, Ta) oxides (79), methods for staining the organic matter in marine sediments (365),and the identification of pulverized fuel ash (370). Metals. See Books (87, 93, 120, 204); Instruments, Miscellaneous (361 ); Techniques for Specimen Examination, Photomicrography (245), Stereology (352). Hasson (150) reports on an improved orientation-dependent anodizing color reagent for molybdenun. Air and Water. White (358) explores the role of microscopy in the study of air pollution and the effects of air pollution on soil, plants, and animals. Rover (284) uses high-speed microholography in the metrology of fogs. Biology a n d Medicine. See Books (119);Articles of General Interest (91, 92); Instruments, Microscopes (227, 281, 331), Hot and Cold Stages (68,264,275,301), Miscellaneous (118,198,199); Methods of Microscopy, Polarized Light Microscopy (97, 246, 297, 363), Microphotometry and Microspectrophotometry (16, 77,258,312), Interference Microscopy (130, 303), Fluorescence Microscopy (96, 126, 188,265,287, 306, 336, 349, 357); Techniques of Specimen Preparation, Embedding and Mounting (110); Methods of Specimen Examination, Autoradiography (356),Automatic Image Analysis (6, 14, 47, 121, 122, 309). Diamond (63) discusses the role of microscopy in controlling
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contamination in the pharmaceutical industry. Whittaker (366) reports a study of ice crystal formation during cryosurgery, and Brown and Reuter (34) have studied the freezing of nonwoody plant tissues using videotape micrography. Harris and Hunt (145) have examined the fine structure of iridophores in the skin of the Atlantic salmon. Hardman and Sofowora (143) use antimony trichloride as a reagent for identifying steroids, especially diasgenin and yamogenin in plant tissues. Segelman (304) uses a combination of thin-layer chromatography and microscopy for the detection and determination of Cannabis sativa L. Miscellaneous. See Techniques for Specimen Examination, Cold- and Hot-Stage Microscopy (41). Bluhm (26) uses light microscopy to determine contact angles. Rickard et al. (274) have made a search for the best polymer film for detecting CY particles by the track etch method. They have found that cellulose nitrate deposited on Kodak film LR115 is the best quantitative particle detector. Skalla and Mather (314) use a replica to record and observe the wear characteristics of phonograph records. ANALYTICAL MICROSCOPY See Methods of Microscopy, Fluorescence Microscopy ( I 62, 255);and Applications of Chemical Microscopy, Biology and Medicine (63, 143,304). Kuhnert-Brandstatter and Burger (194) report on the thermal analysis of the optical antipodes N-benzoyl-%methoxy-4-hydroxyphenylalanineand Metolazon. Techniques other than microscopy were also used. Kofler and KolGek (186) have carried on experimental work in identification of organic materials using the methods devised by Kofler. Stevens (324, 325) reports on the use of squaric acid (1,2-dihydroxycyclobutenedione) as a reagent for Fe3+, Ag+; Cu2+,and U022+ ions.
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