Table Of ContentCRC
Handbook
of
Furnace Atomic
Absorption Spectroscopy
Author
Asha Varma, Ph.D., F.A.I.C., C.P.C.
Naval Air Development Center
Warminster, Pennsylvania
First published 1990 by CRC Press
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PREFACE
During the last 30 years the progress and development of atomic absorption spectroscopy has
generally been covered satisfactorily and enthusiastically in modem textbooks and other
scientific and technical publications. However, during the last 15 to 20 years, there has been
tremendous expansion of graphite furnace atomic absorption spectroscopy (FAAS) technique.
The revolutionary progress in instrumentation, automation, and computerization has played a
major role in acceptance of this technique as a highly sensitive method for the determination of
trace and ultra-trace elements.
This handbook is intended to supplement and compliment all the FAAS - technique related
publications. The material presented here is of practical importance not only for the professional
analysts, but also for the clinical, environmental, and pharmaceutical chemists, who often are
faced with the problem of identifying, detecting, and quantifying the chemical ingredients of the
starting materials, intermediates, final products, and contamination products in a very small
amount of sample.
The first section of this handbook is an introduction to the furnace atomic absorption
spectroscopy. A general principle of atomic absorption spectroscopy and instruments required
to perform the analysis is described. Instrumentation set-up for the technique is described in
detail including sample preparation, time and temperature programming, parameters, optimiza
tion, verification of analytical results, and interferences common to this method.
The next section contains references pertaining to the developments in instrumentation for
the atomic absorption spectroscopy, such as, spectrophotometers, accessories, sampling de
vices, light sources, etc.
In the following sections the elements which have been determined successfully by the FAAS
technique are arranged in the alphabetical order. Because of fewer references, some of the
metals have been grouped together: Alkali metals (lithium, sodium, potassium, rubidium, and
cesium), Platinum group metals (iridium, osmium, palladium, platinum, rhodium, and
ruthenium), and Rare Earth metals (dysprosium, erbium, europium, gadolinium, holmium,
lanthanum, neodymium, samarium, terbium, thulium, uranium, ytterbium, and yttrium).
Due to application importance of elements in certain types of sample environments, separate
sections have been provided for convenience and easy reference (i.e., Clinical Analysis, Heavy
Metals, Trace Metals, and Wear Metals). Some of the miscellaneous applications of the FAAS
technique, which could not be categorized under any of the sections, are placed in the section
entitled Miscellaneous Analysis.
In each section, the instrumental parameter set-up for a particular element is given which will
help an analyst in developing a method suitable for the sample. References are followed by
author and subject indices, which will enable the location of any item desired in that particular
section. There are some large sections on cadmium, copper, lead etc. as well as very short ones
on boron, sulfur etc., but each section is complete in itself for easy reference purposes.
No mention has been made of elements that are not possible to determine by the FAAS
technique. No attempt has been made to provide an alternate method of analysis for these
elements either.
For convenience, a large number of appendices are included in this handbook.These appen
dices are Glossary of Terms and Definitions, Abstracts and Reviews, a list of books on atomic
absorption spectroscopy, and a list of manufacturers for spectrophotometer and related acces
sories, chemical supplies, lamps, etc.
Like any other instrumental analysis technique, FAAS has limitations such as slow heating
rates giving lower sensitivity, non-isothermal conditions, ’’memory effects“ causing erroneous
results and dependence on background correction for accuracy. Despite all these limitations,
FAAS has been widely accepted as a highly sensitive analytical technique. It is highly successful
in the (1) contract Lab Program of United States Environmental Protection Agency through
Superfund resources, (2) methods for regulations of food and drugs, (3) atmospheric and
industrial pollution caused by metallic elements, (4) forensic sciences, (5) pharmaceuticals, and
(6) most importantly, clinical chemistry.
Although, the frontiers of FAAS have extended to other analytical techniques such as
Chromatography (gas and liquid), mass spectrometry, Fourier Transform Infrared Spectroscopy
etc. through interfacing, I have not extended the scope of this handbook to include these
techniques at this time. These are subject to wider use and considerations.
Because of its relatively wide scope, there is every reason to anticipate that this handbook on
Furnace Atomic Absorption Spectroscopy will likewise find a wider circle of usability in various
spheres of trace analysis applications.
I am pleased to express my appreciations to John Sotera, Steve Sourhoff, and Frank
Fernandez for making suggestions. I must thank my professional acquaintances, advisory board
members, and fellow chemists world wide who have encouraged and supported me for my first
attempt at writing The Handbook of Atomic Absorption Analysis (CRC Press Inc., FL, 1984).
I anxiously look forward for their continued support for this handbook on Furnace Atomic
Absorption Spectroscopy.
My thanks are also due to my son, Vinay Agarwala, who spent his summer vacation typing,
correcting, and making author indices for this manuscript. Special thanks are due to my
daughter, Veena Agarwala, who encouraged me to complete this monumental task and consoled
me during the loss of my precious and irreplaceable mother.
I would appreciate any comments and suggestions to improve upon my further adventures
in analytical chemistry.
Asha
October 2nd, 1988
AUTHOR
Asha Varma, Ph.D. is affiliated with the Technology Base Office at the Naval Air
Development Center, Warminster, Pennsylvania.
Dr. Varma received her B.S. (1958) and M.S. (1960) from Bareilly College, Bareilly and
obtained her Ph.D. (1963) from Banaras Hindu University, Varanasi, India. She was appointed
Senior Research Fellow (1963 to 1966) by the Council of Scientific and Industrial Research,
Government of India at Banaras Hindu Universtiy and National Chemical Laboratory, Poona.
In 1966 she became the first woman to be selected by the Madhya Pradesh Government as an
Assistant Director of the Forensic Science Laboratory, Sagar. She held a postdoctoral
fellowship at the Chemistry Department and Institute of Materials Science, University of
Connecticut, Storrs. She has served as the Supervisor of Analytical Laboratories at the
Laboratory for Research on the Structure of Matter, University of Pennsylvania, Philadelphia.
She was appointed Leader of Analytical Research Group (1983) at the Naval Air Development
Center, Warminster, Pennsylvania.
Dr. Varma is a Certified Professional Chemist. She is a fellow of the American Institute of
Chemists; a member of the American Chemical Society, IUPAC, Coblentz Society, Electro
chemical Society, Society of Spectroscopy; and an associate member of the American Museum
of Natural History and the National and International Federation of Wildlife. In 1986 she was
elected the President of Federally Employed Women, Buxmont Chapter, and during 1987 to
1988 she served as chairperson of the Federal Women‘s Program Committee at the center. Dr.
Varma is listed in American Men and Women in Science, Who’s Who in Technology Today,
Who’s Who in Frontiers of Science and Technology, The International Book of Honor, The
Directory of Distinguished Americans, Two Thousand Notable Americans, etc.
Dr. Varma has published over 40 research and technical publications. In 1984, she published
a best seller the CRC Handbook of Atomic Absorption Analysis. At present, she is involved with
independent research and exploratory development projects at the Naval Air Development
Center.
ADVISORY BOARD
Vinod S. Agarwala, Ph.D. Warren Neiderhauser, Ph.D.
Research Scientist Consultant
Materials Protection Branch Meadowbrook, Pennsylvania
Naval Air Development Center
Warminster, Pennsylvania Ram Rakshpal, Ph.D.
Environmental Protection Agency
Mitsutaka Hino, Ph. D. Washington, D.C.
Department of Metallurgy
Faculty of Engineering Zhang Zhong, Ph.D.
Tokyo Univesity Department of Chemistry
Sundai, Japan Shanghai Normal University
Shanghai, China
George Morse
Group Engineer
Lockheed California Company
Burbank, California
ACKNOWLEDGMENTS
The author is greatly indebted to Analyte Corporation, Great Pass, Oregon, Perkin-Elmer
Corporation, Norwalk, Connecticut, Thermo Jarrell Ash, Franklin, Massachusetts, and CRC
Press Inc., Boca Raton, Florida for providing materials for inclusion in this book.
TABLE OF CONTENTS
Furnace Atomic Absorption Spectroscopy (FAAS)
Introduction...............................................................................................................................1
Principle of Atomic Absorption Spectroscopy......................................................................2
General Instrumentation..........................................................................................................4
Modem Graphite FumaceTechnology...................................................................................9
General FAAS Instrument Set-Up..........................................................................................9
References...............................................................................................................................30
Author Index...........................................................................................................................32
General Instrumentation
General References.................................................................................................................33
Author Index...........................................................................................................................62
Subject Index..........................................................................................................................69
Alkali Metals (Cesium, Lithium, Potassium, Rubidium, Sodium)
Cesium.....................................................................................................................................71
Lithium....................................................................................................................................72
Potassium.................................................................................................................................73
Rubidium.................................................................................................................................74
Sodium.....................................................................................................................................75
References...............................................................................................................................76
Author Index...........................................................................................................................78
Subject Index..........................................................................................................................79
Aluminum
Instrumental Parameters........................................................................................................81
References...............................................................................................................................82
Author Index...........................................................................................................................87
Subject Index..........................................................................................................................89
Antimony
Instrumental Parameters........................................................................................................91
References..............................................................................................................................92
Author Index...........................................................................................................................95
Subject Index..........................................................................................................................96
Arsenic
Instrumental Parameters........................................................................................................97
References...............................................................................................................................98
Author Index..........................................................................................................................105
Subject Index.........................................................................................................................107
Barium
Instrumental Parameters.......................................................................................................109
References.............................................................................................................................110
Author Index..........................................................................................................................Ill
Subject Index.........................................................................................................................Ill
Beryllium
Instrumental Parameters.......................................................................................................113
References.............................................................................................................................114
Author Index..........................................................................................................................115
Subject Index.........................................................................................................................115
Bismuth
Instrumental Parameters.......................................................................................................117
References..............................................................................................................................118
Author Index..........................................................................................................................120
Subject Index.........................................................................................................................121
Boron
Instrumental Parameters.......................................................................................................123
References.............................................................................................................................123
Author Index..........................................................................................................................123
Subject Index.........................................................................................................................124
Cadmium
Instrumental Parameters.......................................................................................................125
References.............................................................................................................................126
Author Index..........................................................................................................................137
Subject Index.........................................................................................................................141
Calcium
Instrumental Parameters.......................................................................................................143
References.............................................................................................................................144
Author Index..........................................................................................................................145
Subject Index.........................................................................................................................145
Chromium
Instrumental Parameters.......................................................................................................147
References..............................................................................................................................148
Author Index..........................................................................................................................154
Subject Index.........................................................................................................................156
Cobalt
Instrumental Parameters.......................................................................................................157
References..............................................................................................................................158
Author Index..........................................................................................................................161
Subject Index.........................................................................................................................162
Copper
Instrumental Parameters.......................................................................................................163
References..............................................................................................................................164
Author Index...........................................................................................................................170
Subject Index.........................................................................................................................173
Gallium
Instrumental Parameters.......................................................................................................175
References..............................................................................................................................176
