Synthesis and Technique in Inorganic Chemistry, 3rd Edition. By Gregory S. Girolami

Synthesis and Technique in Inorganic Chemistry, 3rd Edition. By Gregory S. Girolami, Thomas B. Rauchfuss, and Robert J. Angelici. University Science Books: Sausalito, CA. 1999. 242 pp. $42.00. ISBN 0-935702-48-2.

Reviewed by: Dave Berry, University of Victoria, berryde@uvvm.uvic.ca

This third edition of Angelici's original fine collection of inorganic experiments suitable for the undergraduate lab has been comprehensively updated by the present authors. The second edition appeared some time ago (1977—frighteningly long ago now I come to think of it! Most of the student readers were not born then!) and although it still has an important place on my bookshelf, the revised version will soon edge it out. A few of the earlier experiments have been retained, but there are many new ones to add a broader perspective of the inorganic discipline as it stands today.

The book's style is much the same as that of the successful earlier edition. I particularly like the extensive set of references at the end of each experiment, along with a brief description of the content. There is also a section of independent-study suggestions so that substantial projects can grow from a modest synthesis. An approximate total time is given for each experiment and it is refreshing to see that chemistry happens in blocks of time longer, or shorter, than three hours! In my opinion, this makes the book an invaluable compendium of recipes for instructors running a laboratory course.

The authors, however, have clearly written the textbook for the student to read, and indeed the subtitle defines it as "A Laboratory Manual." There are the usual sections on how to keep a notebook, and the dos and don'ts of laboratory work. It is all sound stuff, but is it there for the lawyers to read? Surely the students will already be familiar with most of this? Perhaps the following comments reflect that the system in which I teach is dissimilar from the U.S. system. I find the explanations for the various spectroscopic techniques are written at a level below those written for the associated experiment. Let me give an example: a well-written, but very basic explanation of mass spectrometry is given in the experiment describing a relatively advanced synthesis of dodecacarbonyltriiron. A similarly basic treatment of NMR is given with the synthesis of chlorotribenzyltin, whereas a thorough explanation of the effect of ¹¹⁷Sn and ¹¹⁹Sn satellites might suffice for a student already expected to be using NMR as a characterization tool on such a compound.

Another reason why this book is perhaps a better resource than a manual is the recipe style in which each experiment is presented. In the tin example mentioned above, the questions posed for the report ask why the methylene protons differ in shift from the phenyl protons. Perhaps we should be encouraging the student to compare the spectrum of the product with that of the starting material as might be the case in an exercise focusing away from the verification style of learning. The scale of each reaction is also strikingly large for today's standards of "green chemistry."

But these are small points, and the instructor can easily override this influence of the book as a laboratory manual. There is something for everyone here, and a wide range of abilities and techniques can be addressed by selecting a handful of experiments from the twenty three discussed. I particularly liked some of the choices: nickelocene as a refreshing change from ferrocene; molybdenum acetate rather than the chromium analogue; the YBC 1-2-3 experiment is very well-written. Interested in an experiment on magnetic susceptibility? Read the instructor's notes for the experiment on Mn(acac)₃. If you haven't bought a balance from John Matthey (sic) then do so. It makes life so much easier!

In addition to the instructors' notes, there are selected spectra in the appendix. The inclusion of mass spectra must be well-received by readers in institutions not endowed with such an instrument. I would encourage the authors to add the nonstandard (i.e., not proton and carbon) NMR spectra to the next edition and group them with the experiment rather than in an appendix. The rest of the appendices, containing all sorts of useful information, were a great addition to the first edition (1969).

As one might expect, 22 years have seen changes in many safety issues. Happily, the authors now choose toluene over benzene, and chloroform over carbon tetrachloride. I was a little disappointed to still find perchloric acid used in a teaching laboratory, but suitably dire warnings advise the reader of the hazards.

The book is very well-presented and I noted very few typos. More importantly, the chemistry is totally trustworthy as it is written by well-respected practitioners. At a reasonable price, this is good value for the money and well worth the trip out of the lab to the bookstore!

P.S. Can the University of Illinois really afford to teach students how to make a Nujol mull using iridium compounds?