Environmental Sampling and Analysis : Lab Manual

394 Pages·2017·27.47 MB·English

by  Csuros

M ARIA CSUROS
Environmental
Sam pling and
Analysis
Lab Manual
Boca Raton New York
Published in 1997 by
CRC Press
Taylor & Francis Group
6000 Broken Sound Parkway NW, Suite 300
Boca Raton, FL 33487-2742
© 1997 by Taylor & Francis Group, LLC
CRC Press is an imprint of Taylor & Francis Group
No claim to original U.S. Government works
Printed in the United States of America on acid-free paper
15 14 13 12 11 10 9 8
International Standard Book Number-10: 1-56670-178-3 (Softcover)
International Standard Book Number-13: 978-1-56670-178-5 (Softcover)
Library of Congress catalog number: 96-37154
This book contains information obtained from authentic and highly regarded sources. Reprinted material is quoted with
permission, and sources are indicated. A wide variety of references are listed. Reasonable efforts have been made to publish
reliable data and information, but the author and the publisher cannot assume responsibility for the validity of all materials
or for the consequences of their use.
No part of this book may be reprinted, reproduced, transmitted, or utilized in any form by any electronic, mechanical, or
other means, now known or hereafter invented, including photocopying, microfilming, and recording, or in any information
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Library of Congress Cataloging-in-Publication Data
Catalog record is available from the Library of Congress
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D
edication
To My Father
B
iography
Maria Csuros is an environmental chemist with many years of varied experience. She
received her Ph.D. in Environmental Chemistry from Janus Pannonius University in Pecs,
Hungary, and her Master of Science Degree in Chemistry from Jozsef Attila University in
Szeged, Hungary. Her postgraduate work involved research in environmental chemistry
under a grant from the Environmental and Public Health Insitution, Budapest, Hungary.
Most of her professional life has revolved around environmental testing laboratories
and teaching.
Her first encounter with environmental science occurred at the Environmental and
Public Health Laboratory, Pecs, Hungary, where she worked as a supervisor of the Water
Department. Her main area of interest at that time was the prevention and elimination of
methemoglobinemia caused by high nitrate content of private well waters. She spent six
years in Benghasi, Lybia, as part of an international team, studying the health effects of
brackish drinking water.
After moving to the United States, she continued to dedicate her knowledge and time
to environmental analytical work and education. She has designed and developed an
Environmental Science program for Pensacola Junior College focused on environmental
sampling and analysis. She presently is the coordinator of the this program and teaches
chemistry and environmental science courses.
She also conducts various continuing education programs for local, state, and federal
agencies as well as regional companies.
Her first book, "Environmental Sampling and Analysis," published by CRC/Lewis
Publishers in 1994, and has been on the "Best Sellers" list since.
She lives in Pensacola, Florida, with her husband, who is professor of Microbiology
and Anatomy and Physiology. She has two sons, and five grandchildren.
P
reface
Satisfying the requirements of the environmental laws and regulations is possible only
with défendable and accurate laboratory results, based on approved methodologies, up­
dated instrumentation and technologies, well-trained and qualified laboratory personnel,
and sufficient QC data.
Environmental analytical laboratories must offer a wide-scale analytical repertoire,
from the simple determination of physical properties to the most modern analytical per­
formances of trace organic pollutants. The concern of the microbiological quality of the
environment is also increasing and demands extended testing.
Chemists working in the environmental analytical field should be familiar not only
with the general laboratory techniques, and with the chemical background of different
analytical procedures and instrumentation, but they must also be knowledgeable about
approved methodologies, QC requirements, calculations, evaluations of analytical data,
and generation of correct, défendable analytical results, along with their regulatory levels.
The large diversity of the literature in this field and the diffuse sources of the necessary
information make this wide-scale training difficult. The goal of this text is to give com­
prehensive and easy-to-read information for any individual who is working in the envi­
ronmental analytical chemistry arena, and to provide essential information to consultants
and regulators about analytical and quality control procedures helpful in their evaluation
and decision-making procedures. The text also gives useful information for college and
university students taking chemistry and environmental courses, for graduate students,
and for chemists who need a ready source of information that meaningfully relates to
actual laboratory practice.
The book is designed as the first part of a comprehensive laboratory manual specially
designed for environmental professionals. It contains general laboratory considerations,
laboratory safety procedures, and laboratory techniques emphasized on the determination
of inorganic nonmetallic constituents in environmental samples along with their chemistry,
occurrence, source, fate, and their control by regulations and standards. Sample collection,
preparation for analysis, step-by-step easy to follow methodology with detailed quality
control procedures, as well as calculations for correct reporting units concerning different
matrices are discussed for each parameter.
All in all, this book will provide a valuable advantage to environmental education
and special training programs; as a practical handbook it will also assist environmental
chemists in their everyday chores; and it will give a helping hand to the reader to under­
stand analytical reports.
A
cknowledgments
I owe a great debt of gratitude to all the people who participated in making this book
possible.
My most sincere appreciation goes to James Tucci, manager of Law Engineering and
Environmental Services, Inc., for his valuable suggestions, comments, and technical infor­
mation. His professional input and respected expertise considerably contributed to the
correctness of the information contained in this publication. I can't imagine completing
this task without his help and support.
My very special thanks go to Bernie Fuson, project manager at Law Engineering and
Environmental Services, for his support, patience, and accuracy in proofreading and
correction of the text.
I also am pleased to express my thanks to my student and friend, Ken Connor, for
the preparation of the figures and tables.
I gratefully acknowledge the support of the outstanding editorial and production staff
of CRC/Lewis Publishers. My personal thanks to Ken McCombs, Acquiring Editor, and
Susan Alfieri, for their friendship, understanding and encouragement. I am grateful to the
project editor, Albert Starkweather, who guided the project with his careful work and
patience through the complexities of production. Thank you also for the superb design
work.
It is with particular pleasure that I thank my husband for his patience, support,
excellent ideas, and his cheerful spirit. Warm words of thanks also to my sons, Geza and
Zoltán, for their love, encouragement and technical assistance.
T C
able of ontents
Chapter 1 INTRODUCTION TO CHEMICAL ANALYSIS............................................1
1.1 The Nature of Analytical Chemistry...........................................................................1
1.2 General Direction of Chemical Analysis.....................................................................1
1.2.1 The Responsibility and Psychology of the Analyst....................................2
1.2.2 Cleanliness in the Laboratory..........................................................................3
1.2.3 Recording Analytical Data................................................................................3
1.2.4 Planning Laboratory Work..............................................................................4
1.2.5 Documents to be Saved.....................................................................................7
Chapter 2 SAFETY AND LABORATORY WORK............................................................9
2.1 Laboratory Hazards..........................................................................................................9
2.1.1 Chemical Hazards..............................................................................................9
2.1.2 Fire Hazards......................................................................................................13
2.1.3 Careless Habits..................................................................................................14
2.2 Safe Handling of Compressed Gases.........................................................................14
2.2.1 General Precautions When Working with Compressed Gases..............15
2.2.2 Hazardous Properties of Compressed Gases.............................................15
2.3 Stockroom Safety Rules.................................................................................................15
2.3.1 Checklist for Safety Storage Room...............................................................15
2.3.2. Storage of Chemicals.........................................................................................17
2.4 Laboratory Safety Rules................................................................................................18
Chapter 3 QUALITY ASSURANCE OF CHEMICAL MEASUREMENTS................21
3.1 Introduction.....................................................................................................................21
3.1.1 Quality Assurance (QA)....................................... 21
3.1.2 Quality Control (QC)......................................................................................21
3.1.3 Quality Assessment..........................................................................................22
3.2 Laboratory Quality Assurance Program ..................................................................23
3.2.1 Sampling.............................................................................................................23
3.2.2 Sample Custody............................................................. 27
3.2.3 Sample Preparation for Analysis..................................................................28
3.2.4 Analytical Methodology.................................................................................28
3.2.5 Analytical System Calibration......................................................................30
3.2.6 Detection Limits........................... 31
3.2.7 Statistics in Chemical Analysis.....................................................................33
3.2.8 Quality Control Charts.................................................................................35
3.2.9 Items for the Essential Control of Chemical Measurements.................36
Chapter 4 LABORATORY APPARATUS AND GLASSWARE.....................................39
4.1 Labware Materials...........................................................................................................39
4.1.1 Soft Laboratory Glassware vs. Heat-Resistant Glassware.....................39
4.1.2 Plastic Labware ..................................................................................... 39
4.1.3 Porcelain Labware ................................................................................. 40
4.1.4 Platinum Crucible ................................................................................. 40
4.1.5 Nickel Crucible ...................................................................................... 40
4.2 Volumetric Glassware ........................................................................................ 40
4.2.1 Volumetric Flask .................................................................................... 41
4.2.2 Pipets and Their Use ............................................................................. 44
4.2.3 Burets and Their Use ............................................................................. 46
4.2.4 Cleaning of Volumetric Glassware ...................................................... .48
4.3 The Analytical Balance ...................................................................................... 48
4.4 Desiccator ........................................................................................................... 50
Chapter 5 CHEMICALS, REAGENTS, AND STANDARDS ........................................ .51
5.1 Chemicals ........· . .................................................................................................. 51
5.1.1 Grades and Purity of Chemicals ........................................................... 51
5.1.2 Proper Storage of Chemicals and Standards ....................................... 52
5.2 Laboratory Pure Water ............................................................................... , ...... 52
5.2.1 Methods for Preparation of Laboratory Pure Water ........................... 53
5.3 Reagents and Solutions ............................................................... , ..................... 54
5.3.1 Expressing Concentration of a Solution ............................................... 56
5.3.2 Diluting Solutions ................................................................................. 60
5.3.3 Handling Reagents and Solutions ........................................................ 60
Chapter 6 STANDARD SOLUTIONS ................................................................................ 67
6.1 Stock Standard Solutions .................................................................................. 67
6.2 Standardization of Solutions ............................................................................ 67
6.3 Preparation and Standardization of Common Standard Solutions ................ 68
6.3.1 Sulfuric Acid (H2S04) Solution 0.1 N ................................................... 68
6.3.2 Hydrochloric Acid (HCI) Solution 0.1 N .............................................. 69
6.3.3 Sodium Hydroxide (NaOH) Solution 0.1 N ......................................... 70
6.3.4 Iodine (12) Solution 0.1 N ...................................................................... 71
6.3.5 Sodium Thiosulfate (Na S 0 Solution 0.1 N ...................................... 72
2 2 3)
6.3.6 Potassium Permanganate (KMn04) Solution 0.1 N ............................. 73
Chapter 7 COMMON LABORATORY TECHNIQUES ................................................... 75
7.1 Filtration ............................................................................................................ 75
7.1.1 Filtration Methods ................................................................................. 75
7.1.2 Filter Media ........................................................................................... 75
7.1.3 Gravity Filtration .................................................................................. 79
7.1.4 Vacuum Filtration .................................................................................. 80
7.2 Centrifugation ................................................................................................... 81
7.2.1 Using a Common Laboratory Centrifuge ............................................ 83
7.2.2 Centrifuge Safety Rules ........................................................................ 84
7.3 Distillation ......................................................................................................... 84
7.3.1 Simple Distillation ................................................................................ 84
7.3.2 Fractional Distillation ........................................................................... 86
7.3.3 Vacuum Distillation .............................................................................. 87
7.4 Refluxing ............................................................................................................ 88
7.5 Ion Exchange ...................................................................................................... 89
7.6 Drying and Ashing Samples ............................................................................. 90
7.6.1 Drying Samples ..................................................................................... 90
7.6.2 Ashing .................................................................................................... 90
7.7 Dissolving the Sample ....................................................................................... 91
7.7.1 Decomposition under Pressure in a Closed System ............................ 91
7.7.2 Decomposition in an Open System ...................................................... 91
7.7.3 Digestion ................................................................................................ 91
7.7.4 Fusion .................................................................................................... 92
7.8 Extraction ........................................................................................................... 92
7 .8.1 Liquid-Liquid Extraction by Separatory Funnel.. ............................... 92
7.8.2 Continuous Liquid-Liquid Extraction ................................................. 94
7.8.3 Sohxlet Extraction ................................................................................. 95
Chapter 8 GRAVIMETRIC METHODS OF ANALYSIS ................................................. 97
8.1 General Principles ............................................................................................. 97
8.1.1 Types of Precipitate ............................................................................... 97
8.1.2 Aging and Digestion of the Precipitate ................................................ 98
8.1.3 Manipulations Associated with the Filtration Process ....................... 98
8.2 Gravimetric Calculation .................................................................................. 100
8.2.1 Utilization of the Gravimetric Factor ................................................. 101
8.3 Gravimetric Analysis and Modern Analytical Chemistry ............................. 102
Chapter 9 TITRIMETRIC ANALYSIS .............................................................................. 105
9.1 General Principles ........................................................................................... 105
9.1.1 Chief Requirements for a Titration .................................................... 105
9.1.2 Indicators ............................................................................................. 106
9.1.3 Volumetric Glassware ......................................................................... 106
9.1.4 Reactions Used for Titration ............................................................... 106
9.1.5 Performing a Titration ........................................................................ 107
9.2 Calculating the Result of a Titration .............................................................. 107
9.2.1 Results Given in the Same Concentration as the Titrant .................. 107
9.2.2 Results Given in Concentrations, Using Normality .......................... 108
9.3 Back-Titration .................................................................................................. 108
Chapter 10 ACID-BASE TITRATION ................................................................................ 111
10.1 Acids and Bases ............................................................................................... 111
10.1.1 Arrhenius Theory of Acids and Bases ................................................ 111
10.1.2 Bronsted-Lowry Concept of Acids and Bases ................................... 112
10.2 Basic Concept of Chemical Equilibrium ........................................................ 112
10.2.1 Acid-Base Equilibrium ....................................................................... 112
10.2.2 Self-Ionization of Water ...................................................................... 113
10.2.3 pH Calculations ................................................................................... 114
10.2.4 Measurement of pH ............................................................................ 117
10.2.5 Buffers .................................................................................................. 117
10.3 Acid-Base Titration ......................................................................................... 117
10.3.1 Acid-Base Titration Curves ................................................................ 117
10.3.2 Acid-Base Indicators ........................................................................... 120
Chapter 11 COMPLEXOMETRIC, OXIDATION-REDUCTION,
AND OTHER TITRATIONS ........................................................................... 123
11.1 Complexometric Titration ............................................................................... 123
11.1.1 Complex Formation ............................................................................ 123
11.1.2 Complexometric Titration ................................................................... 126