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Book Review The Analysis of Gases by Chromatography. By C. J. Cowper and A. J. DeRose

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To our knowledge, this is the first
of a crown
ether containing nitrogen atoms acting as both a first and
second sphere ligand towards a transition metal. Clearly,
an extensive range of such complexes should existf141.
This
report could herald the preparation of a wide range of
novel compounds, including polymers, in which transitionmetal complexes and aza-crown ethers are covalently
bonded.
Received: November 7, 1984 [ Z 1062 IE]
German version: Angew. Chem. 97 (1985) 124
H. M. Colquhoun, J . F. Stoddart, J. Chem. Soc. Chem. Commun. 1981.
612: H. M. Colquhoun, J. F. Stoddart, D. J. Williams, ibid. 1981, 847,
849, 851: J. Am. Chem. Sac. 104 (1982) 1426: H. M. Colquhoun, J. F.
Stoddart, D. J. Williams, J. B. Wolstenholme, R. Zdrzycki, Angew. Chem.
93 (1981) 1093: Angew. Chem. Int. Ed. Engl. 20 (1981) 1051; H. M. Colquhoun, D. F. Lewis, J. F. Stoddart, D. J . Williams, J. Chem. Soc. Dalton
Trans. 1983, 607; H. M. Colquhoun, S. M. Doughty, J. F. Stoddart, D. J.
Williams, Angew. Chem. 96 (1984) 232: Angew. Chem. Int. Ed. Engl. 23
(1984) 235; D. R. Alston, A. M. Z. Slawin, J. F. Stoddart, D. J. Williams,
ibid. 96 (1984) 804: 23 (1984) 821.
A. Werner, Neuere An.rchauungen auf dem Gebiete der anorganischen
Chemie, 3rd Edition, Vieweg, Braunschweig 1913; J. Bjerrum, Adz).
Chem. Ser. 62 (1967) 178.
For two recent examples, see J.-P. Lecomte, J:M. Lehn, D. Parker, J.
Guilheim, C. Pascard, J . Chem. Soc. Chem. Commun. 1983, 296; P. K.
Coughlin, S. J. Lippard, J. Am. Chem. Soc. 106 (1984) 2328.
B. Dietrich, J:M. Lehn, J.-P. Sauvage, Tetrahedron 29 (1973) 1647.
Experimental: 3: 27.3 mg (0.07 mmol) 2 was dissolved in CH2CIZcontaining 18.4 mg (0.07 mmol) 1 . Dull yellow prisms, suitable for X-ray investigation were obtained by vapor diffusion using EtzO (P. G. Jones,
Chem. Br. 17 (1981) 222). After 48 h, the crystals were filtered off and
dried. Yield 20 mg (42%): m.p.=216-219”C; 1R (Nujol): 3350, 3330,
3290, 3270, 3230, 3190 (all vNH), 1620, 1610 (both 6NH) c m - ’ :
‘H-NMR (CD3COCDI): 6= 1.87 (XH, m, CH,,H,,-cod), 2.46 (8H, bs,
CH,g,H,,-cod), 2.60-3.10 and 3.63-4.05 (32 H, broad multiplets, OCH:,
NCH2, NH, NH,), 4.20 (8H, bs, CH-cod).
161 2 , m.p. 209-215”C, was prepared from [Rh(cod)Cll2 (R. B. King, Organomet. Synth. l(1965) 132).
[7j The reaction between I and 2 is slow in CD2CIz. ‘H-NMR data indicates that a non-covalently bonded adduct is formed initially.
[8] Nicolet R3m diffractometer, w-scan, Cu,, radiation (graphite monochromator). Empirical absorption correction based on 360 azimuthal
measurements. Structure solution by heavy-atom method: anisotropic
refinement. The ammine hydrogen atoms were located in a AF map and
the NH3 group refined as a rigid body. Four complete analyses using
different crystals all resulted in R values of ca. 0.10. In all cases, the relatively high magnitude of these values was a result of disorder both in the
PF; ions and in the cyclooctadiene portion of the complex. Further details of the structural investigation can be obtained from the Director of
the Cambridge Crystallographic Data Centre, University Chemical Laboratory, Lensfield Road, Cambridge CB2 1 EW (England). Any request
should be accompanied by the full literature citation for this communication.
[9] The conformation of the macrocycle with alternating (+)- and (-)gauche helicities for the C-C bonds and inward directing N-H bonds
is similar to that observed in uncomplexed 1 (M. Herceg, R. Weiss, Bull.
Soc. C h i i . 1972, 549).
[lo] D. J. Cram, K. N. Trueblood, Top. Curr. Chem. 98 (1981) 43: K. N.
Trueblood, C . B. Knobler, D. S. Lawrence, R. V. Stevens, J. Am. Chem.
Sac. 104 (1982) 1355.
[ l I ] B. L. Allwood, H. M. Colquhoun, J. Crosby, D. A. Pears, J. F. Stoddart,
D. J. Williams, Angew. Chem. 96 (1984) 806: Angen?. Chem. I n f . Ed.
Engl. 23 (1984) 824.
[ 121 There are also bifurcated hydrogen bonds of 2.40 and 2.23 A, respectively, between H,%and F(I) and H,, and F(3) of the major occupancy PF;
ion.
[ 131 The closest analogue is the macrocyclic aquo complex of a carbonyl(bisphosphino-ether)rhodium complex ( N . W. Alcock, J. M. Brown, J. C.
Jeffery, J. Chem. Sor. Chem. Commun. 1974, 829: J . Chem. SOC.Dalton
Trans. 1976, 583). In [RhCO(H20)(Ph2P(CH2CH,0),(CH2)2PPh2]][PF6],
the metal is coordinated by the H 2 0 molecule which is hydrogen
bonded to two of the oxygen atoms in the polyether chain.
1141 Compare with the reactions between crown ethers and AIMe, ( J . L. Atwood, R. D. Priester, R. D. Rogers, L. G. Canada, J. Inclusion Phenom. I
(1983) 61).
BOOK R E V I E W S
The Analysis of Gases by Chromatography. By C . J . Cowper
and A . J. DeRose. Pergamon Press, Oxford 1983. xii, 147
pp., bound, DM 114.00.
P. G. Jeffery writes in the foreword that he hopes that
this book will be received with the same enthusiasm that
greeted his contribution “Gas Analysis by Gas Chromatography” more than ten years ago. This book by Cowper
and DeRose, which is published as Volume 7 of the “Pergamon Series in Analytical Chemistry” and which really
ought to be entitled “The Analysis of ( I . I > C > Iiy Gas Chromatography” is long overdue; since t l i t . publication of the
2nd edition of P. G. Jeffery and P. J . Kipping’s book in
1972, this field of application of gas chromatography has
undergone immense development, which is documented in
countless publications. However, a comprehensive review
of this particular area has been lacking for a long time,
apart from a company brochure entitled “Fundamentals of
Gas Analysis by Gas Chromatography” by B. Thompson.
The present volume has certainly succeeded in largely
closing this gap. A short introduction devoted to the problems and peculiarities of gaseous samples as compared
with those of liquids is followed by an account of the apparatus required for such analyses. Alongside the equipment for regulating and controlling the flows of carrier gas
and auxiliary gases and for sample introduction the main
136
emphasis is on the detectors used in gas analysis. The focal
point of this book lies in the three chapters that follow, in
which there is a 43 page-long detailed discussion of the
normal separating materials, the choice of carrier gas in
connection with the detector of choice for a particular
problem, the possibilities of multi-column operation and
specific operating methods. Arrangements for two and
three column operation with valve switching and “valveless” according to Deans, the techniques of fore and back
flushing, heart cutting, and other techniques are discussed
with the aid of a large number of operating strategies.
A chapter devoted to examples of applications follows,
in which suggestions for the separation of the components
of air, of noble gases, of natural gas, of refinery, synthesis
and fuel gases are illustrated with numerous chromatograms. Neither is stimulation lacking concerning the separation of gaseous sulfur, nitrogen and halogen-containing
compounds, nor the separation of isotopes and the seldom
analyzed gaseous compounds of boron, silicon, germanium, phosphorus and arsenic. In all this, account is taken
of the circumscribed size of the book and, in the main, the
reader is referred back to the literature.
Chapter 7 is devoted to the analysis of liquified gases
and to gases dissolved in liquids. Emphasis is laid on the
devices used for sampling, handling and dosing. HeadAnyew. Chem. Inl. Ed. Engl. 24 (1985) No. 2
space analysis is deliberately omitted and the reader is referred to the book by Hachenberg and Schmidt. The authors devote the last two chapters to the quantification and
evaluation of chromatograms and to the preparation of
standard gas mixtures. For the latter they limit themselves
to a brief review of the various methods and techniques for
the preparation of mixtures of gases and their critical assessment.
The book includes an extensive reference list in order of
authors’ names (172 references), which includes publications up to 1981. Additionally an appendix includes publications from the years 1981 and 1982 (19 references).
A point worthy of criticism is the plethora of units
quoted. With Anglo-American nonchalance and uninfluenced by IUPAC recommendations or even SI regulations, pascals, pounds per square inch, atmospheres and
metric and imperial units of length are quoted alongside
each other. This will, however, not present any difficulty to
the analyst who practises gas chromatography every day.
This book is written for the man at the bench. It is easy
to read, comprehensibly laid out, and easy to understand
even for the reader whose native language is not English.
There are almost no printing errors. Within its compass of
140 pages the book contains a wealth of information,
which will be of great use to the reader who is acquainted
with the basic principles and practice of gas chromatography in helping him in his choice of apparatus and in the
analysis of complex mixtures of gases.
Erhard Grallath [NB 642 IE]
Max-Planck-Institut fur Metallforschung
Institut fur Werkstoffwissenschaften, Dortmund (FRG)
Atomabsorptionsspektrometrie. By B. Welz. 3rd completely
revised edition. Verlag Chemie, Weinheim 1983. xiii, 527
pp., bound, DM 128.00.
Almost every new edition of a scientific or technical
book is offered to the reader as being “completely revised”. During the period of eight years between the publication of the second edition“] and the present third edition
atomic absorption spectroscopy has undergone a great
deal of development. The basic principles of AAS remain
unaltered, but general knowledge has been greatly augmented through the large increase in the application of this
analytical technique. A really “new” book must combine
the old basic knowledge with the new developments, additional fields of application, and also a critical description
of the method. Welz has attempted this in the new edition
and seems to have succeeded well. The wealth of material
has almost doubled the size of the book; the number of figures has been enlarged from 73 to 140, the number of tables has only been slightly increased from 46 to 51. The
real extent of the enlargement of knowledge, however, is
best seen in the additional 1103 references; the total is now
2491. The increase demonstrable in these numbers is sufficient alone to justify the publisher’s claim of “complete revision” of this book.
The additional figures are particularly welcome, both in
the sections covering the basic principles and in those
dealing with interferences. The clarity is significantly improved in both cases. The beginner receives an easier entry
into the basics of the subject. Those who are already famil[“I
Cf. Angew Chem. lnl. Ed. Engl. I S (1976) 447.
A n g e w . Climni Inr. Ed. Engl. 24 iIY8Sl No. 2
iar with the problems of AAS can estimate the real extent
of interferences much better with the aid of the diagrams.
The methodic layout of the volume is very similar to that
of the previous edition. The chapters are naturally somewhat longer, but neatly tailored to accommodate the newer
methods. A short introduction is followed by a brief, but
adequate, description of the radiation sources in use
nowadays (eg. HCL, EDL). The chapter on atomization
techniques includes the flame technique, the graphite furnace technique, the hydride and cold vapor techniques.
The author deals both with the basic theory and with the
current design of apparatus for each method. The historical outline of the techniques and further reference to specific techniques convey not only topical hints but a general
picture to the reader with a greater interest in AAS. Concisely constructed chapters on optics and detection and
output give an insight into spectrometer structure. Since
most users of AAS d o not wish to rebuild their instruments
a short treatment here is appropriate. A great deal of space
is devoted to interferences in AAS. They are described in a
separate chapter, but also in the detailed section “Techniques of atomic absorption spectroscopy”. This indication of the many possibilities of interference can be of
great help to the practitioner in avoiding systematic errors
in his determinations. A great deal of space in this context
is devoted to the hydride and cold vapor techniques, where
even today the interferences often constitute unresolved
problems. The third edition too contains the indispensable
descriptions of the individual elements. For each element
the description of the standard conditions is followed by
allusion to the various sources of interference. Although
only a minority of possible interferences can be covered in
such a section, it will certainly be of help in avoiding a
multiplicity of the more usual errors.
N o matter what its length the chapter devoted to specific
applications is, considering its aims, of necessity too short.
This deficit is made up for here by the large number of references to specific applications in the original literature.
“Welz” is the only German-language book dealing with
atomic absorption spectroscopy. The 3rd edition can be
understood both as a textbook and as a laboratory handbook. It can provide both the interested laboratory technician and the experienced practitioner of AAS with a profusion of practical advice and a deeper understanding of the
method.
Harald Berndt [NB 636 IE]
Institut fur Spektrochemie, Dortmund (FRG)
Transition Metal Carbene Complexes. With contributions
by K . H. DOt2, H. Fischer, P. Hofmann, F. R . Kreissl, U.
Schubert, and K . Weiss. Verlag Chemie, Weinheim 1983.
xiii, 264 pp., bound, D M 120.00.
This book is dedicated to Professor E . 0. Fischer and is
written by some of his more recent senior co-workers in
honor of his 65th birthday (November 10, 1983). The
theme of the book relates to a n area discovered by the dedicatee in 1964, and has been a principal preoccupation of
his group in the intervening years. Hence, the appropriateness of the topic and the selection of the contributors is to
be commended.
The book is attractively produced. Details of its chapter
headings are as follows. 1. The Synthesis of Carbene Complexes (H. Fischer), 66 pages, 476 refs.; 2. Spectroscopic
Properties of Transition Metal Carbene Complexes (H.
Fischer and F. R . Kreissl), 1 pages, 12 refs.: 3. Solid State
137
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