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Book Review Inorganic Thermogravimetric Analysis. By C. Duval

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which swell up the book with redundant and erroneous information. This section has apparently not been revised since
the appearance of the first edition in 1944. - The subject
index I s unsatisfactory: it should be more extensive and
built up on a better system of classification.
Despite these shortcomings, the book may be recommended
as a cheap but authoritative introduction to spectroscopy.
W. F. Berg
[NB 332/190 IE]
Infrared Spectroscopy and Molecular Structure. An Outline of
the Principles. Edited by M. Davies. Elsevier Publishing
Co., Amsterdam-London-New York 1963. 1st Edit., XIII+
468pp., 171figs.,70tables,linenca.DM42.-(about$10.50).
This book is intended for all who use infrared spectroscopy
n3t merely as an empirical fingerprint method but as a theoretically founded process for the investigation ofthe structures
and properties of molecules. Here the theoretical and methodical principles as well as the scope and limitations of the
various applications of infrared spectroscopy are presented
by 13 authorities in clear and understandable terms. The
most important concepts and facts, from both the chemical
and physical points of view, are unraveled so lucidly even
when the material dealt with is complicated that also those
who are less experinced find a good introduction to this discipline. The fact that the authors have concentrated on important examples contributes significantly t o this effect.
The introductory section written by the editor is followed by
chapters on instrumentation and experimental techniques
( A . E. Martin), on long-wave infrared spectroscopy in the
region from 1 to 200cm-1 which has only recently become
utilizable (G. R. Wilkinson), on the infrared spectra of simple
molecules ( W . J . Jones), on the calculation of force constants (J. M. Mills),and on Raman spectra (J. C. Evcins).
The chapter by D . Hndzi on the origin of characteristic group
frequencies deserves special mention. Further sections deal
with the infrared spectra of crystals and high polymers (S.
Krimm) and of inorganic compounds (E. A . V. Ebswortlr).
The technique of infrared intensity measurements, which
becomes more and more important, and its application for
the determination of polarity are discussed by J. Overend. The
methods of dispersion measurements, including the practically important technique of attenuated total reflection, are
described by J. Fahrenfort. The book then closes with chapters on hydrogen bonding and solvent effects ( H . E. Hallnm)
and on infrared emission spectra ( W. C. Price). The text is
supplemented by some 800 references.
The editor has succeeded well in coordinating the contributions from the individual authors into a largely homogeneous
book with an up-to-date selection of themes. On account of
its admirable didactic qualities, it is recommended in general
as a textbook of spectroscopy for the advanced specialist and
for those striving to attain this status, for it teaches the reader
to think in spectroscopic terms. The outlay and print of the
book are exemplary in their clarity.
W. Liitrke
[NB 3261184 IE]
Infrared Spectra of Inorganic and Coordination Compounds.
By K. Nnkamoto. Sohn Wiley & Sons, Inc., New YorkLondon 1963. 1st Edit., XI1 324 pp.. numerous illustrs.
and tables, linen E2.12.0 (about $7.25).
There has long been a lack for a book reviewing the greatly
increased literature on vibrational spectra of inorganic compounds and giving a critical appraisal of publications in this
field with regard to both the practice of spectroscopy (e. g.
for structural analysis) and the theory of molecular physics
as related to force constants. The author attempts to satisfy
this need, to assign the published data to normal vibrations,
and to interprete their significance for the structures of molecules and ions. The first of the three sections of the book
(63 pp.) gives a brief but lucid discourse on the theory of spectra. In the second part (69 pp.), the spectra of simple organic
compounds are discussed, again very briefly. In the large
+
616
third section; which forms the maiiipart of the book, data for
inorganic complex compounds are desciibed. Five appendices
(45 pp.) include infer d i n tables of point groups, F and G
matrix elements of model cornpounds, and, by way of an
example, the complete normal coordinate analysis of an acetylacetonate. The text is supplemented by numerous tables,
illustrations, and literature references.
On account of the expansiveness and ready surveyability of
the material and its intelligible presentation, the book could
be warmly recommended to inorganic chemists interested in
spectroscopy and especially to complex chemists, if the author
had only discussed the material (particularly in Part 11) with
greater criticism. For example, in contrast to the data given
Oil p. 7 I, hydrogen halides (except for H F ) d o not associate in
the condensed phase; this follows from the fact that the vX-H
frequencies of liquid hydrogen halides are lower by 2-3X
than those of the gaseous compounds. It does not follow from
the appropriate spectra that there are “essentially covalent
bonds” in AgCN and AuCN (p. 73); the high CN frequencies
indicate only the presence of Ag..CN-..Ag.CN,.. bridges (or
Au). A free U O l 3 ion (p. 77) cannot be observed, according
to more recent publications; ligands are always coordinated
i n the plane vertical to the UOz axis, Results dating from 1938
are given for HzSe and DzSe (p. 831, although more recent
measurements (Palik, 1959) with some remarkably great
differences in frequencies are available. NT3, PT3, and AsT3
(p. 84) have never been measured, but were only calculated.
The Czv structure given for N2FZon p. 102 has been shown
to be incorrect; the compound is subject to geometric isomerism. The numerical values given for CH4 and CD4 (p. 104)
are not up-to-date. The data for NH4CI (p. 104) are not characteristic of the NH4@ion, because v4 (1400cm-1) here is
strongly split by Fermi resonance. Insufficiencies of this kind
are easy to eradicate in a new edition, and it would also be desirable for the author to go deeper into the relations between
spectra and molecular structures (a. g . how t o derive information about the bond order from the force constants). Sufficient space can be made quite easily by omission or reduction
of some figures [e. g. on pp. 74, 94, 147, 170, 174, and 200).
All in all, the book is usefull for thecritical, well-informed
reader; the outward appearance and the print are good.
W. Liittke
[NB 327/185 IE]
Inarganic Thermogravimetric Analysis. By C. Duvof. Translated from the French by R . E. Oesper. Elsevier Publishing
Co., Amsterdam-London-New York 1963. 2nd Edit., XV +
722 pp., 77 figs., linen ca. D M 67.- (about S 17.00).
The principle of thermogravimetry is the continuous registration of alterations in weight of a solid sample during a heating program. Thanks to the development of modern automatically recording thermobalances, this process is easy and
rapid to execute and is a versatile aid in the investigation of
i9organic compounds: determination of moisture contents
and water of crystallization, controlled drying to constant
weight, testing of analytical precipitates for their suitability
for gravimetric estimations, detection of the limits of stable
phases, quantitative analysis based o n the loss of weight
during decomposition reactions (even of two components of
a mixture), investigations of reactions between solids and
gases, etc
Duvcil has compiled the first extensive monograph on this
field, in the development of which he has himself taken a
significant part. I n the first section of the second edition
(164 pp.), following a historical introduction, the apparatus
and experimental methods of thermogravimetry are dealt
with. This part has been extended by aboul 100 pp. in comparison with the 1953 edition, owing mainly to the description
of the automaticalIy recording thermobalances which have
been developed in the meantime and which are now commercially available. The main section of the book (519 pp.) contains the results of thermogravimetric investigations of analytical precipitates from 78 elements, arranged according to
increasing atomic weight. In all, the behavior of about 1200
Angew. Chem. internnt. Edit./ Vol. 4 (1965) NU. 7
precipitates during thermolysis is described ; here the author
has relied mainly upon the results of his own school. In contrast to the first edition, the reproduction of thermolysis
curves for individual compounds has been omitted, because
the detailed appearance of the curves depends too much upon
the experimental conditions. The author restricts his description t o the principal parts of the curves, the horizontal sections and the stability regions, and to the suitability of individual compounds for purposes of gravimetric analysis.
Duval’s book is thus a comprehensive reference work o n
thermogravimetry.
Despite the widespread application of thermogravimetry, it
appears to the reviewer that the relationships of this method
to the thermodynamics of heterogeneous equilibria have not
yet been sufficiently pointed out, even though a profitable
field is offered here. The processes that occur during thermogravimetry are in fact often highly complex and depend upon
the experimental conditions, since the ideal conditions of isobaric decomposition under equilibrium conditions are normally far from being attained. For this reason, the form of
the thermolysis curves depends upon the particle size and pretreatment of the sample, upon the rate of flow and composition ofthe gaseous phase, and upon the rate of heating. Therefore, the decomposition points found in this way need not be
identical with the temperatures at which the equilibrium pressure of a gaseous decomposition product, such as water vapor,
reaches the value of 1 atmosphere.
These comments are not intended t o depreciate the value of
Dirvnf’s book, but rather to serve as an incentive for its readers
to occupy themselves with the still unused potentialities of
t hermogravimetry.
The lay-out and appearance of the book are excellent, in
keeping with the high standards of the Elsevier publishing
house. This volume should not be missing in any chemical
library or inorganic chemistry laboratory.
Friedrich Becker
[NB 325/183 IE]
Analytical Chemistry of Uranium gzU238.03. Published by the
Academy of Sciences of the U.S.S.R. and edited by D . I.
Ryubclrikov and M. M . Senyurin. Translated from the
Russian by N. Kuner. Series: Analytical Chemistry of Elements. Israel Program for Scientific Translations, Jerusalem 1963. 1st Edit., VII + 374 pp., 70 figs., 51 tables, linen
S 14.00.
Because of the widespread use of uranium in nuclear technology, there are numerous methods for determining and detecting uranium in ores, uranium compounds, and alloys scattered in the literature, but so far no comprehensive monograph
on the analytical chemistry of uranium has appeared (with
the exception, perhaps, of a few difficultly accessible compilations 11-41). The present volume is a critical review of
material from over a thousand publications. Following a
general introduction to the chemistry of uranium (Chapter 1),
in which the most important properties of the element, its
isotopes, and some of the most common uranium minerals are
described, a short review is given in Chapter 2 o n the special
[ I ] M . A . DeSesa: Raw Materials Development Laboratory
Handbook of Analytical Methods. National Lead Co., Raw Materials Div., Winchester, Mass. (U.S.A.), TID-7002 (March 30th,
1956); TID-7002 (Rev. 1) (July 30th, 1957).
[2] C. E. Rodden: Current Procedures for the Analysis of UO3,
UF4, and UFs. New Brunswick Lab., U.S. Atomic Energy Comm.,
TID 7003 (Del.) (Feb. 1956).
131 H . P. Raaen: Manual of Analytical Procedures for the U235
Recovery Process. Oak Ridge National Lab. Report ORNL-983
(August 20th, 1951).
[ 4] L. C. Bassett, D. J. Pjuurn, R. J . Rutman, C. J. Rodden, and
N . H . Furman, Manual of Analytical Methods. Vol. I: Analysis
of Ores; Vol. 2: Analysis of Refined Materials and By-products;
Vol. 3 : Analysis of Purified Materials. Manhattan Project Report
A-2912. VOIS. 1-3.
Angew. Chem. internal. Edit.
Vol. 4 (1965)
1 No. 7
inorganic chemistry of uranium, with particular stress upon
analytical aspects. Valuable tables of solubilities and complexing constants i n various solvents are given.
In Chapter 3, o n the qualitative detection of uranium, it is
mainly color and fluorescence tests that are dealt with.
Besides the well known fluorescence reaction in the NaF bead,
reactions with inorganic and organiccolorreagents are descrihed in detail and compiled in a long table. Although the
interferences caused by other elements are described, n o
reference is made to the behavior of neptunium and plutonium. There is also no mention here of the classical precipitation reaction as sodium uranylacetate crystals, which also
works with Np02*@, Pu022@, and Am022q. This is found
somewhat out of place on p. 236.
Chapter 4 contains 174 pages devoted to methods for estimating uranium and thus makes up over a third of the book.
It is subdivided into three sections: A) chemical methods of
analysis, B) physico-chemical methods of analysis, and C)
physical methods of analysis. The subsection on colorimetric
and spectrophotometric methods of analysis without and with
the use of organic color reagents is worth mentioning. Here,
too, the reader finds welcome extensive tabulations with data
on extinction coefficients (pp. 89 and 114).
Methods for separating uranium from other ekements are
given in Chapter 5 , and methods for determining uranium in
minerals and industrial wastes in Chapter 6. Although, for
example, the analysis of uranium/zirconium alloys is described briefly (p. 301), no attention i s called to the danger
of explosions on dissolution of such alloys in nitric acid. The
book closes with Chapter 7 on the testing of the purity and
estimation ofimpurities in uranium, and with a comprehensive
bibliography (1093 references). Here the translator has made
some errors in his retranscription of names from Kyrillic into
Latin script, for it should be CLitte and not Gotro in reference
554, and Ladenbnuer and not Ladenbnyer in reference 98 1. Tke
numerous practical procedures given would have profited
from tests of their experimental usefulness. The print is clean
and tidy, but the lay-out could have been better arranged.
Despite these minor shortcomings, the book is recommended
to all higher institutions of chemical learning, to uranium processing industries, and to analytical laboratories, for it covers
practically the whole of the more important literature on the
analytical chemistry of uranium i n a single volume and helps
one to find rapid recourse to original publications via its bibliography.
F. Wcigf [ N B 324/182 IE]
Nobel Lectures. Physiology or Medicine 1942 - 1962. Published
by the Nobel Foundation. Presentation Speeches and
Laureates’ Biographies. Elsevier Publishing Co., Amsterdam-London-New York 1964. 1st edit., XIV + 839 pp.,
numerous illustrs., a few tables, price for complete 3-volume
work i n half-linen HI?. 240.-.
The Nobel Prize in Physiology or Medicine was awarded
twenty times between 1942 and 1962, including thirteen
awards for work in biochemical research. For this reason,
the present volumes can be recommended to the chemist.
Many, especially biochemists, will find material in the contents which touches directly their own work. However, this
does not represent the prime purpose of the book; its aims
go much further. All the Nobel lectures held between 1942
and 1962 in the fields of physiology or medicine are reproduced here in English in chronological order, together
with the laudations and biographies of the prize-winners.
The result is an extremely vivid and fascinating picture of the
development of medicine, physiology, and physiological
chemistry over these two decades. When one reads at the
end of the Nobel lecture by Sir Alexander Fleming (1945)
“the time may come when penicillin can be bought by anyone
in the shops. . .” and then considers how soon afterwards not
only penicillin but also a great number of its derivatives became available in sufficient amounts, then one appreciates
eve2 as a n outside observer just how much has been achiev-
617
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