Synthesis and technique in inorganic chemistry (Angelici, Robert J

Feb 1, 1970 - McAfee. 2000 77 (9), p 1122. Abstract: Spectroscopy reference. Abstract | PDF w/ Links | Hi-Res PDF · Synthesis and technique in inorgan...
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book reviews quenbly, the uses of symmetry in later discussions of molecular orbitals and ahsorption spectra. of transition metal complexes will not seem to the student to beer any relation t,o the concepts of symmetry introduced with the crystalline state chapter. A little time spent in class can easily bridge this gap. Students always have liked this book because the derivations involved in the discussion of wave mechanics, e.g., the particle in one and t,hree dimensional boxes and the hydrogen atom, are carried out, in detail. I n fact the last time the reviewer looked for the first edition on the reserve shelf of the library, he found that. i t had been stolen which is a good cont,emporary criterion for a text's popularit,y. This book should serve admirably for an undergraduate course or perhaps for a graduate survey for studenk not majoring in inorganic chemistry. I n many respects i t is better suited to an integrated curriculum than to a highly strucbured one. I n t,he latter case the material in the three chapten on qnantnm theory, wave mechanics, and chemical bonding probably will be taught from a physical chemistry text.. Much of the three chapters on electromotive force, acids and bases, and non-aqueous solvents will have been covered in the generd-analytical sequence. Even where this is true, the six remaining chapters provide a good basis for a course in coordin~tionchemistry. R. STUARTTOBIAS Purdue University Lafayette, Indiana

Synthesis and Technique in Inorganic Chemistry

Robert J. Angelici, Iowa State University of Science and Technology, Ames. W. B. Saunders Co., Phil* 203 pp. Figs. delphis, 1969. xi and tables. 16 X 24.5 cm. $8.

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I n the not too distant past, the instructor of an inorganic laboratory course was hard put to locate suitable preparations for his students and was forced to select experiments from "Inorganic Syntheses," the original literature, or the few manuals then available. With recent increased interest and research in the inorganic field, the situation has changed radically. Within the last decade no fewer than half a dozen inorganic lahoratory manuals have been puhlished by American presses. Professor Angeliei's book is a n inspired example of the new, slim, streamlined look in modern inorganic manuals. Designed as "a practical manual for an upper-level inorganic lahoratory course" (one quarter or one semester, with two 3-hour lahoratory periods per week), i t is intended "to prepere the junior, senior, or first year graduate student for graduate-level or industrid research." Inorganic manuels have generally fallen into one of three broad cstegoriescollections of a great number of procedures with only minimal space devoted

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to theory; hooks emphasizing theory and techniques with a few detailed, illustrative experiments appended; and manuals with an integrated approach consisting of a balanced blend of theory and teehnioue with a. reasonable number of detailed preparations. Angelici's manual, which contains 20 carefully selected experiments, belongs to the third category. The experiments illustrate the fundamentals of the inorganic laboratory techniques of synthesis, purification, and compound characteriestion. For example, synthetic techniques are employed in experiments requiring a vacuum line, a high temperature furnace, a dry box or hag, nanaqueous solvents (NHs and NsO,), and sn electmlytic cell. Methods of purification include ion exchange, vacuum sublimation, thin-layeyer and column chromatography, distillation, recrystallization, and extraction, while methods of characterization include infrared, nltraviolet-visible, and nuclear magnetic resonance spectroscopy, mass spectrometry, ionic conductivity, optical rotation, msgnetic susceptihility, chemical reactivity and ratesof reaction, and equilibrium constants for metal complex formation. For the convenience of schools which do not possess nuclear magnetic resonance or mass spectral facilities, these spectra of t,he reaction products are provided for student interpretation. The experiments were selected on the basis of four practical considerations: inherently dangerous procedures were avoided; with t,wo duly noted exceptions, only experiments which can he completed in the course of a 3-hour lahoratory period were included; preparations were limited to those requiring only relatively inexpensive reagents; and in order to generate greater student interest and to place the student in the shoes of an actual research chemist, the preparations emphasize compoundswhich are either not commercially available or are very expensive when produced eommercidy. Thus the syntheses in the manual "are largely of compounds which have only been recently prepared and which border an the frontiers of research." Msny types of ompounds are represented, but coordination compounds, orgauometdlics, and anhydrous suhstances are emphasized. Although exotic compounds such as [1,3,5-CsHa(CHs)dMo(CO)Z and [CsH6Fe(CO)dz (this preparation is the most challenging in the manual) are featured, perennial favorites such as KISnOa and [Co(NHa),COaINOa are not neglected. Each experiment contains a discussion of historical, theoretical, and experimental background, a detailed experimental procedure, including prominent safety precautions, a list of items to be included and questions t o he answered in the report, and s list of classified and annotated references, many as recent as 1968. The results ohtained by the student will often require interpretation, and he is encouraged to consult original papers and standard reference works. The ~ r e ~ a r a t i o nmay s be performed in any order except for a few eases in which the product of a. previous synthesis is required as a starting material for a later

experiment. An introductory chapter discusses safety precautions, hasic lilboratory procedures, methods of keeping a research notebook, and standard references. The hook is replete with clear figures, tahles, and equations. Hints on laboratory organization and commercial sources for special equipment and reagents are provided in a separate chapter entitled Notes to Instructor. An index of compounds as well as a general index concludes the volume. Errata are not numerous and are mostly of the typographical sort. The repeated use of "Inorgsnic Synthesis" for the journal Inorganic Syntheses is annoying but in no way confusing. A campmison of this new manual with others already published is best left to the instructor. Experience has shown that students rsrelyread discussions of theory unless they are included in the actual experiment as is done in Angelici's hook. A number of competing manuals separate theory from practice, and an instructor with strong feelings about this point might prefer this book to its competitors on this hasis alone. Before making a choice of s. manual for his course, an instructor, however, should certainly examine carefully the highly praised and recently puhlished English manual, Pass and S u b liffe's "Prettied Inorganic Chemistry" (more than 90 preparations) [THIS JOURNAL, 46, A44(1969)1, the slightly alder Adams and Raynor's "Advanced Practical Inorganic Chemistry" (almost one hundred highly abbreviated experiments) 43, 222 (1966)1, and the [THISJOURNAL, open-ended, heuristic Jolly's "Synt,hetic Inorganic Chemistry" [(THIS JOURNAL, 38, 157 (1961)l. He may also wish to consider Grindley's "An Advanced Course in Practical Inorganic Chemistry" (Bnttenvorths, 1964), Dodd and Robinson's "Experimental Inorganic Chemistry" (Elsevier, 1954), and Palmer's "Experimental Inorganic Chemistry" [THIS JOURNAL,32, 218 (1955)]. He should also not overlook for supplementary use works which me largely collections of procedures such as Schlessinger's "Inorganic Lsboratory Preparations" (Chemical Publ. Co., 1962), Brauer's 2-volume "Handbook of Preparative Inorganic Chemistry" now availahle in English tramlation (Aeademic, 1963), or that much used journal in book format Inorganic Syntheses. All lahoratory manuals are the product of a selective process on the part of the author. I n the ideal case, the author's choice jibes with the individual instructor's own needs and preferences, an extremely rare event. As long as fielectivity is involved, obviously no one manual will satisfy all instructors. Nevertheless, Professor Angeliei's book, whether used alone or in conjunction with any of the above cited manuals, will he found most useful to the instructor of almost any inorganic lahoratory course. At lhe very least, the publication of this well conceived and well executed hook has expanded the choice rwd.ihble to such instructors. GEORGE B. KAUFFMAN California State College Fmsno (Continued on page A128)