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Wiley-VCH:
New York, 1998. xxiv + 333 pp. ISBN 0-471-19458-1. $79.95.
I would have subtitled this book "All You Ever
Wanted To Know about ...Sample Preparation". Although its
principal thrust is geared towards the analytical chemist in an
X-ray diffraction (XRD) or X-ray fluorescence (XRF) service
laboratory, this text will be of use primarily as a reference
source in all milieus dealing with undergraduate research
projects and advanced laboratory courses in physical and
analytical chemistry. It contains dozens of suggestions for preparing
randomly oriented small samples of nearly anything. For
example, rocks and minerals, soft organics and hard ceramics,
radioactive and liquid materials, metals and oils are all treated.
As the availability of XRD and XRF equipment has
increased, so has the use of these techniques in the
teaching schedule. Many undergraduate laboratory and
research projects utilizing these methods have been described in
the literature and are found in laboratory textbooks. Very
often, especially with the increasingly common use of
automated computer-controlled instrumentation, sample preparation
has become the key experimental technique required for
successful data collection. However, it is not always easy to prepare
the statistically random distribution of small particles
(crystallites) that is required by these methods.
A multitude of techniques have been developed over
the past 70 years, but many of them have been handed down
by word of mouth or are scattered throughout the literature.
This book represents an attempt to systematically describe
the theory and practice of sample preparation.
This excellent guide to the intricacies of sample
preparation begins with a description of statistical sampling
methods and the principles of grinding techniques. After a discussion
of XRF specimen preparation, which includes pressing
pellets, fusion methods, crucible selection and handling very
small samples, detailed descriptions for handling rocks,
minerals, cements, metals, oils, and vegetation [sic] are given.
The preparation of XRD samples is described for
various diffraction equipment geometries (utilizing both counter
and film detectors), including specific information regarding
the use of flat specimens and slurries, the use of internal
standards, and the effects of crystallite size on the diffraction
pattern. Methods for handling ceramics, clays, zeolites,
air-sensitive samples, thin films, and plastics are described, along with
the special handling requirements for materials to be studied by
high-pressure, high-temperature, or low-temperature techniques.
One whole chapter is devoted to the equipment used
in specimen preparation, including grinders, pulverizers,
presses, specimen holders, repair of platinumware, and sources of
all types of special equipment. Did you ever want to know
where to get a Plattner steel mortar or a micronizing mill or
soft-glass capillary tubes with 0.01-mm wall thickness? It's all
here in this monograph.
The book ends with a good glossary of terms, a
general bibliography in addition to the extensive list of references
following each of its 9 chapters, and an index. It will be
of help in many areas of spectroscopy and analytical
chemistry, as well as in XRD and XRF analyses.
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