AAS, AES, and NMR spectroscopy

(Chapter 1) and ending with a list of recommended further ... incorporate a solid-state detector. (charge-coupled devices ... cal analysis. It provide...
6 downloads 0 Views 3MB Size
BOOKS

AAS, AES, and NMR spectroscopy Spectrochemical Analysis by Atomic Absorption and Emission. L.H.J. Lajunen. xii + 242 pp. Royal Society of Chemistry, Thomas Gra­ h a m H o u s e , Science P a r k , Milton Rd., C a m b r i d g e CB4 4WF, U.K. 1992. $45 Reviewed by M. W. Blades, Department of Chemistry, 2036 Main Mall, University of British Columbia, Vancouver, BC, Can­ ada V6T1Y6 T h i s book is q u i t e s h o r t — 2 4 1 p a g e s — a n d c o v e r s a b r o a d topic area. It is clearly intended for begin­ n e r s , a l t h o u g h t h i s information is not indicated in either the title or the preface. Unfortunately, because the topic a r e a is so broad, a book t h i s size cannot provide all the important details. However, it does give a quick and fairly digestible introduction to spectrochemical analysis and will be readily understood by anyone with a n u n d e r g r a d u a t e science d e g r e e . Ten chapters are organized in a pedagogically sensible m a n n e r , begin­ n i n g w i t h a brief overview of t h e field of s p e c t r o c h e m i c a l a n a l y s i s (Chapter 1) and ending with a list of recommended further reading (Chapter 10). C h a p t e r 2 t r e a t s t h e t h e o r y of atomic spectroscopy and contains all the usual fundamental atomic phys­ ics equations along with a brief ex­ p l a n a t i o n of t h e o r i g i n of a t o m i c spectra. However, it relies a little too heavily on equations and not enough on i n t u i t i v e description to get t h e m e s s a g e across. There is no doubt that the space allotted is too small to do justice to the topic of atomic phys­ ics. For example, a section entitled "Basic Concepts of t h e P l a s m a " is only a page and a half long and skips over m u c h t h a t is r e q u i r e d for a proper u n d e r s t a n d i n g of h i g h - t e m ­ perature plasmas. Also, fluorescence is i n c o r r e c t l y — a n d i r r i t a t i n g l y — associated with stimulated emission. Chapter 3, the longest in the book at 112 pages, covers atomic absorp­ tion spectroscopy and includes dis­ cussions of instrumentation, calibra­ tion, flame and electrothermal atomization, background correction,

and special methods (e.g., hydride generation and flow injection analy­ sis). T h i s c h a p t e r is s u r p r i s i n g l y comprehensive, considering the r e ­ stricted amount of space given to it. Chapter 4, on the other hand, covers flame atomic emission in only two pages; it clearly should have been in­ c o r p o r a t e d i n t o t h e d i s c u s s i o n of flame atomic absorption. Chapter 5 describes plasma emis­ sion spectroscopy and discusses plasma instrumentation, sample in­ troduction, spectrometers, interfer­ ence effects, background correction, and special methods such as hydride generation and the use of plasmas as c h r o m a t o g r a p h i c detectors. It also includes a brief description of induc­ tively coupled, direct c u r r e n t , a n d

.j J

Λ

f,

, 11 {J j NJ

άΐβ y J ci hi Β JiJ'Xϊ U il iJ [S ίΐ ΌΛΑ ' t U

u\) 'ό viz υ (jJi BJjiJ uni microwave p l a s m a s as well as t h e common spectrometers used for se­ quential and simultaneous analysis. However, there are a few omissions. Although the author describes a va­ r i e t y of m i c r o w a v e p l a s m a s ( a n d even includes a schematic diagram of a magnetron power tube), the most successful implementation—atmos­ pheric pressure Beenaker cavity mi­ crowave plasma—is not mentioned. Also notably absent from the section on spectrometer i n s t r u m e n t a t i o n is any mention of polychromators t h a t i n c o r p o r a t e a s o l i d - s t a t e detector (charge-coupled devices, photodiode a r r a y d e t e c t o r s , e t c . ) — a t y p e of p l a s m a spectrometer, commercial­ ized since 1985, t h a t is becoming in-

892 A · ANALYTICAL CHEMISTRY, VOL. 65, NO. 20, OCTOBER 15, 1993

creasingly i m p o r t a n t in a n a l y t i c a l plasma spectroscopy. Chapter 6 is a brief discussion of i n d u c t i v e l y coupled p l a s m a m a s s spectrometry (ICPMS) t h a t provides cursory coverage of instrumentation, sample introduction, and spectral in­ terferences. Chapter 7 describes atomic fluorescence s p e c t r o m e t r y , and Chapter 8 discusses methods for sample preparation, including collec­ tion, digestion, and selective extrac­ tion and preconcentration. Chapter 9 is a short three-page comparison of the various spectroscopic techniques with respect to detection limits and r a n g e of applications; a more com­ prehensive comparison would have been useful. The e r r o r s and omissions in this book are relatively minor and do not detract from its overall usefulness. M a n y of t h e figures, however, a r e oversimplified and lack detail, and worse, the captions are too brief to be of use in interpreting the figures. It would also have been helpful to in­ clude the references for further read­ ing in each chapter and to key them to specific topics. Overall, the book p r o b a b l y would be useful to n e w ­ comers to the field of spectrochemi­ cal a n a l y s i s . It provides a concise o v e r v i e w of t h e v a r i o u s p o p u l a r methods used for elemental analysis and is fairly easy to read.

NMR and Chemistry: An Introduc­ tion to Modern NMR Spectroscopy, 3rd e d . J. W. A k i t t . xi + 272 p p . C h a p m a n & H a l l , 29 W. 3 5 t h St., New York, NY 10001. 1992. $50 Reviewed by Pushpalatha Murthy, De­ partment of Chemistry, College of Engi­ neering, Michigan Technological Univer­ sity, 1400 Townsend Dr., Houghton, MI 49931-1295 The revolution in NMR spectroscopy in the past two decades can be traced to the development of superconduct­ ing magnets coupled with advances in m u l t i p u l s e t e c h n i q u e s a n d ever more powerful computers. Ingenious exploitation of t h e s e advances h a s

led to t h e d e v e l o p m e n t of m u l t i ­ dimensional NMR, solid-state NMR, and NMR imaging. These techniques have provided the chemist with new tools of wide applicability, immense practical importance, and fascinat­ ing intellectual challenge. The continued progress in NMR spectroscopy easily justifies a n u p ­ d a t e of m a t e r i a l from t h e second edition of this book. As t h e a u t h o r s t a t e s , t h e book is i n t e n d e d as a "nonspecialist text" for t h e u n d e r ­ g r a d u a t e s t u d e n t and aims both to familiarize newcomers with the sub­ ject and to convey a sense of the po­ tential of NMR spectroscopy by de­ s c r i b i n g t h e c u r r e n t s t a t e of t h e field. T h e book does not provide a c o m p r e h e n s i v e t r e a t m e n t of NMR spectroscopy; its purpose, which it fulfills, is to pique students' interest in t h e s u b j e c t a n d to s t i m u l a t e , rather than satisfy, their curiosity. The book is set in a nonmathematical framework and is basic enough to provide most of the information t h a t beginners may need. It pro­ gresses logically t h r o u g h 10 c h a p ­ ters, starting with a theoretical treatment of NMR that is followed by a description of the spectrometer and concluding with a discussion of dif­ ferent techniques and applications. The t h e o r e t i c a l section ( C h a p t e r s 1-4) includes discussions of nuclear m a g n e t i z a t i o n , n u c l e a r shielding, chemical shift, s p i n - s p i n coupling, and nuclear magnetic relaxation. The coverage of techniques and a p ­ plications includes topics such as the n u c l e a r O v e r h a u s e r effect, t w o dimensional spectroscopy, magnetic resonance imaging, and high-resolu­ tion solid-state NMR, as well as a very useful discussion of dynamic processes such as exchanging and re­ acting systems. The c h a p t e r s are well organized and well written, and the a r r a n g e ­ ment of the chapters and the m a t e ­ rial in t h e m is logical. All of t h e m c o n t a i n a good b a l a n c e of t h e o r y , technique, and applications. Several questions for students are presented at the end of each chapter; answers are provided at the end of the book. The author gives a good explana­ t i o n of w h a t h a p p e n s in a m u l t i pulse experiment, an understanding of which is e s s e n t i a l for designing and interpreting NMR experiments. He also attempts to familiarize read­ ers with important parameters such as acquisition time, resolution, repe­ tition rate, and relaxation times. The chapter on two-dimensional NMR spectroscopy provides a good i n t r o d u c t i o n to t h i s exciting tech-

"I me Ώϋΰΐί •pjuviihs ±\ βϋΰά slnïlhig

ρ οίιϊί

ÏDÏ mm"

nique. A comprehensive discussion of the large number of pulse sequences t h a t can be used is beyond the scope of m o s t t e x t s . H o w e v e r , u s i n g D-amygdalin as an example, this book clearly demonstrates the variety of information t h a t can be obt a i n e d by some common pulse seq u e n c e s such as COSY, z e r o - a n d d o u b l e - q u a n t u m COSY, N O E S Y , / - r e s o l v e d 2D, a n d h e t e r o n u c l e a r COSY. Pull and confident use of the various techniques will probably require r e a d e r s to consult more a d v a n c e d books. The bibliography at the end of the text suggests books and review a r t i c l e s for specific i n t e r e s t s a n d should prove very useful. Although the list does not aim to be compreh e n s i v e , t h e references a r e recent and the list is adequate. The type of experiments an investigator needs to perform depends on the nature of the information sought and the complexity of the molecule. These factors only become clear with e x p e r i e n c e . T h i s book p r o v i d e s a good starting point for such investigations, and it nicely fulfills the need for an introductory NMR spectroscopy text aimed a t advanced undergraduates.

Books Received Physical Methods of Chemistry. 2nd éd., Vols. 8 and 9A. B r y a n t W. Rossiter and Roger C. Baetzold, Eds. xi + 531 pp., xi + 516 pp. John Wiley & Sons, 605 Third Ave., New York, NY 10016. 1993. $150, $140 New topics in the second edition of Vol. 8, Determination of Electronic and Optical Properties, include photoacoustic, photoconductivity, a n d photoelectron t e c h n i q u e s for m e a s u r i n g the electronic, optical, and dielectric properties of m a t t e r . The text also contains chapters on UV and visible

spectrophotometry, molecular fluorescence and phosphorescence spectroscopy, absorption spectroscopy of t r a n s i e n t species, and dielectric properties of polymers. Vol. 9A, Investigations of Surfaces and Interfaces—Part A, contains chapters on surface t e n s i o n m e a s u r e m e n t , t e c h n i q u e s for m e a s u r i n g t h e a d sorption of a n a l y t e s from solution, STM, high-resolution EELS, SIMS, molecular beams, and laser-induced thermal desorption. Remote Sensing by Fourier Transform Spectrometry. Reinhard Beer, xvii + 153 pp. J o h n Wiley & Sons, 605 T h i r d Ave., N e w York, NY 10016. 1992. $75 This book, which is volume 120 in the Chemical Analysis series edited by J. D. Winefordner, describes FT spectrometry (FTS) for remote sensing of planetary atmospheres. Topics include a n i n t r o d u c t i o n to F T S , a c o m p a r i s o n b e t w e e n ideal FT a n d dispersive spectrometers, the physics and chemistry of remote sensing, real FT systems, interferogram sampling and optical configurations, and interferences. Five case studies include FT spectrometers built for the Voyager a n d Spacelab 3 m i s s i o n s . The book contains a n appendix on optimal filters and is illustrated with p h o t o g r a p h s , schematic d i a g r a m s , and representative spectra.

Secondary Ion Mass Spectrometry: SIMS VIII. A. Benninghoven, K.T.F. Janssen, J. Tumpner, H. W. Werner, Eds. xxv + 915 pp. J o h n Wiley & Sons, 605 Third Ave., New York, NY 10016. 1992. $260 This book contains more t h a n 200 of t h e 300 p a p e r s presented at t h e Eighth International Conference on S I M S , held Sept. 1 5 - 2 0 , 1 9 9 1 , in Amsterdam. Papers are arranged by t o p i c s e c t i o n s on f u n d a m e n t a l s , quantification, instrumentation, depth profiling, imaging, postionization, a n d h y p h e n a t e d a n d r e l a t e d techniques. Applications sections include biology; isotopic a n a l y s i s for geology; and SIMS of metals and oxi d e s , p o l y m e r s a n d o r g a n i c compounds, and semiconductors. The Morrison Symposium, "Ion Microscopy for Biomedical Studies," is presented at the end. The book contains a list of contributors and indexes of r e v i e w e r s and c h a i r p e r s o n s a t t h e symposium. The papers are illustrated with graphs, spectra, schematic diagrams, and SIMS images. Because the book was set as c a m e r a - r e a d y copy, t h e print quality is very uneven.

ANALYTICAL CHEMISTRY, VOL. 65, NO. 20, OCTOBER 15, 1993 · 893 A