Environmental Analysis: Ray E. Clement and Paul W. Yang

Environmental Analysis
Ray E. Clement* and Paul W. Yang

Laboratory Services Branch, Ontario Ministry of the Environment, 125 Resources Road,
Etobicoke, Ontario, Canada M9P 3V6
Carolyn J . Koester
Analytical Sciences Division, Lawrence Livermore National Laboratory, Livermore, California 94551
ReviewContents
General Trends 2761
Review Articles 2766
Solid-Phase Microextraction Applications 2766
Characterization of Organic Compounds 2767
Water Analyses 2767
Soil, Sediments, and Pore Waters 2767
Air Monitoring 2767
Inorganic/ Organometallic Compounds 2767
Air Monitoring and Analysis Applications 2767
General Comments 2767
Sampling 2768
Volatile Organic Compounds 2769
Semivolatile Organic Compounds 2769
Inorganic Compounds 2771
Chemometrics and Real-Time Monitoring 2772
Automated Analysis 2772
Deposition and Atmospheric Transport 2773
Incineration and Miscellaneous 2773
Water Analysis Applications 2774
Sample Collection 2774
Extraction and Sample Preparation 2774
Integrated Extraction and Detection 2775
Separation and Detection 2775
Analytes of Interest 2777
Solid Sample Types Analysis Applications 2777
Soils and Sediments: Metals 2777
Soils and Sediments: Organics 2779
Sewage Sludge: Metals 2780
Sewage Sludge: Organics 2780
Organometallic Analytes 2780
Biota Analysis Applications 2780
Radionuclides 2781
Quality Assurance, Reference Materials, and Related
Topics
2781
Biomonitoring and Biomarkers 2782
Literature Cited 2782
This review covers developments in applied environmental
analytical chemistry from November 1998 to the end of October
2000, as found in the Chemical Abstracts Service CA Selects for
gas chromatography, mass spectrometry, inorganic analytical
chemistry, pollution monitoring, and environmental pollution. We
have coordinated our efforts with Susan Richardson, who prepared
the review on Water Analysis for this issue, and therefore have
greatly reduced our coverage in areas she has reviewed in detail.
As in the previous review in this series (A1), we have not
attempted to cover industrial hygiene, greenhouse gases, guide-
lines and regulations, risk assessment, human levels, modeling,
commercial products, and food. We emphasize the determination
of trace organics, trace metals, and organometallics in real
environmental samples.
In an ongoing attempt to control the size of this review, we
changed our strategy somewhat this year, by focusing on overall
trends in environmental analysis, rather on the number of citations
in a given area. The citations we use are therefore representative
of the current state of the art and should be used by the reader
as a starting point for further investigation. However, for readers
who wish much more detail, an extensive annotated list of review
articles published by others over the past two years is presented
in Table 1.
In preparing this review, we have noticed that more citations
now appear in published conference proceedings than was the
case for the first reviewin this series. Also, some of the key studies
reported in proceedings may not appear in published journals at
all. We attribute this, at least in part, to our observation that a
proportion of environmental publications are generated from
industrial and government researcherssfor whom journal publica-
tion is often less important than for academic researchers. We
also note that although the Internet is not yet a significant source
of published papers in the environmental analysis field, it is likely
that more information will be disseminated in this manner in the
near future. Therefore, the authors believe that those who wish
to keep up to date in the environmental analysis field will have to
consider all of these sources of information, not just printed
journals. In the previous review in this series (A1), we included
a table of Internet URLs we believe are of significant value to
environmental analytical researchers. Some of these URLs refer
to science societies or conference sites where some of the
conference proceedings cited here may be obtained. The only
addition we wish to make this year is the web site of the
International Society for Optical Engineering (SPIE). Many
significant advances in chemometrics, sensor technology, and
remote and automated environmental monitoring are presented
at various SPIE meetings. Published proceedings for many
of these meetings can be found through their web site
(www.spie.org).
GENERAL TRENDS
The first review in this series was published in 1991 (A2).
Ultratrace methods were considered those that could achieve
Anal. Chem. 2001, 73, 2761-2790
10.1021/ac0103930 CCC: $20.00 2001 American Chemical Society Analytical Chemistry, Vol. 73, No. 12, June 15, 2001 2761
Published on Web 05/01/2001
Table 1. Environmental Analysis Review Artic les, 1998-2000
review topic/ analyte
no. papers cited
or pages published review title and comments ref
1. Conference Proceedings
general 240 pp EnviroAnalysis: Proceedings of the Third Biennial International
Conference on Monitoring and Measurement of the Environment
A3
general 249 pp Proceedings of the 2
nd
Euroconference on Environmental Analytical Chemistry A4
air monitoring 160 pp Air Monitoring and Detection of Chemical and Biological Agents A5
remediation 420 pp Environmental Monitoring and Remediation Technologies A6
2. Matrix-Specific
air many Analysis of organic compounds in air A7
air 16 Measurements of concentrations of air pollutants; covers methods,
deployment, site selection, networks
A8
air 45 Modern methods of the measurement of atmospheric trace gases A9
air 58 X-ray fluorescence analysis of ambient air samples A10
air 31 The physicochemical characterization of urban air particulate
matter; diesel exhaust particles and carbon black are emphasized
A11
air 106 Trace element determination of airborne particles by neutron activation analysis A12
air 57 Trace element analysis of airborne particles by atomic absorption
spectroscopy, and inductively coupled plasma mass spectrometry
A13
air 17 Composition of air pollution particles; includes definitions of airborne
particle types and sources of PM
10
A14
air 57 Sampling and analysis of individual particles by aerosol mass spectrometry A15
air many Organic atmospheric aerosols: review and state of the science; main objective
is to present a basis for defining what data are needed in this area
A16
air 22 Accelerator based ion beam techniques for trace element aerosol analysis A17
air 10 Health-related monitoring and assessment of airborne particulate matter:
an overview of recent IAEA (International At. Energy Agency) programs
A18
air 204 Mass spectrometry of aerosols; off-line MStechniques discussed A19
air 165 New concepts for sampling, measurement, and analysis of atmospheric
anthropogenic aerosols
A20
air 27 pp Real-time single particle mass spectrometry: a historical review of a
quarter century of the chemical analysis of aerosols
A21
air 26 Correlations of personal exposure to particles with outdoor air
measurements: a review of of recent studies
A22
air 58 Aerosol time-of-flight mass spectrometry A23
automobile 25 Gas detection for automotive pollution control; emphasis on chemical sensors A24
air 60 Reactive sorption concentration in air pollution A25
solid wastes and leachates 13 Multielemental analysis of solid wastes and leachates; NAA,
XRF, ICP-AESmethods are covered
A26
water 672 Water analysis; extensive review of developments in water analysis A27
groundwater 90 Field methods for site assessment and remediation of
contaminated ground waters
A28
wastewater 16 Trends in monitoring of waste water systems; focus on use of sensors A29
river water 21 Use of flow injection analysis for continuous monitoring of river water quality A30
marine water 27 Introduction - environmental analytical chemistry as a tool for
studying chemical processes in marine environments
A31
3. Metals and Organometallics Speciation
metals 30 The role of speciation in analytical chemistry; coverage includes
use of sequential extraction
A32
metals 47 Speciation in the environmental field. Trends in analytical chemistry;
special attention to need for speciation analysis in biota
A33
supercritical fluid extraction 25 Supercritical fluid extraction in speciation studies A34
liquid chromatography 141 Liquid chromatography: a tool for the analysis of metal species A35
stripping voltammetry 117 Stripping voltammetry for the determination of trace metal speciation and
in-situ measurements of trace metal distributions in marine waters
A36
HPLC-ICPMS 11 High-performance liquid chromatography-isotope dilution inductively
coupled plasma mass spectrometry for speciation studies: an overview
A37
atomic spectroscopy many Speciation studies by atomic spectroscopy A38
capillary electrophoresis 179 Element speciation analysis by capillary electrophoresis A39
ICPMS 118 New approaches for elemental speciation using plasma
mass spectrometry
A40
SPME 40 Metal speciation by SPME-CGC-ICPMS A41
metals 199 Chemical speciation of trace metals A42
microwave-induced
plasmas
131 Microwave-induced plasma-optical emission spectrometry-
fundamental aspects and applications in metal speciation analysis
A43
phosphorus 93 Phosphorus speciation in water and sediments A44
organometallics 17 Improving the reliability of speciation analysis of
organometallic compounds
A45
Hg 80 Analytical methods for mercury speciation in environmental and
biological samples - an overview
A46
Hg 322 The determination of mercury species in environmental and
biological samples
A47
Hg 80 The speciation of mercury and organomercury compounds by using
high-performance liquid chromatography
A48
Hg, As, Se 34 Speciation and analysis of mercury, arsenic, and selenium by atomic
fluorescence spectrometry
A49
2762 Analytical Chemistry, Vol. 73, No. 12, June 15, 2001
Table 1. (Continued)
no. papers cited
3. Metals and Organometallics Speciation
As, Se 152 Speciation of arsenic and selenium compounds by HPLC hyphenated to specific detectors:
a review of the main separation techniques; covers papers published since 1980
A50
Sn 129 Determination of tin species in environmental samples A51
Cr 224 Chromium occurrence in the environment and methods of its speciation A52
4. Organic Analytes
POPs many Persistent Organic Pollutants (POPs): state of the science A53
endocrine disruptors 14 Monitoring endocrine-disrupting chemicals A54
endocrine disruptors 21 Endocrine-disrupting chemicals in a source water; drinking water source reservoirs A55
endocrine disruptors 12 pp Identifying endocrine disruptors by high-resolution mass spectrometry A56
endocrine disruptors many Endocrine disruptine chemicals in the aquatic environment A57
estrogens 7 pp Mass spectrometry applied to the analysis of estrogens in the environment A58
toxaphene 257 Toxaphene. Analysis and environmental fate of congeners A59
PCBs 302 Methods for the determination and evaluation of chlorinated biphenyls in
environmental matrices
A60
pharmaceuticals 154 Pharmaceuticals and personal care products in the environment: agents of subtle change? A61
PAH many The analysis of polycyclic aromatic hydrocarbons in marine samples A62
PAH 11 Application of stable carbon isotopic analysis to source polycyclic aromatic hydrocarbons
in the environment
A63
nitro-PAH 9 pp Chromatographic methods for carcinogenic/ mutagenic nitropolycyclic aromatic
hydrocarbons
A64
VOCs 157 Anthropogenic volatile organic compounds in ambient air and natural waters: a review on
recent developments of analytical methodology, performance and interpretation of
field measurements
A65
drinking water 67 Analysis of organic micropollutants in drinking water A66
herbicides 50 Determination of herbicides in water using HPLC-MStechniques A67
phenols 108 Liquid chromatographic and biorecognition techniques for the determination of
phenols and their substituted derivatives in water samples
A68
aldehydes 16 pp A users guide to aldehyde analysis using PFBHA derivatization and GC/ ECD
detection: avoiding the pitfalls
A69
isocyanates 138 Determination of isocyanates in air A70
petroleum hydrocarbons 61 Environmental monitoring of petroleum products A71
petroleum hydrocarbons 82 Oil and greases and petroleum hydrocarbon analysis A72
algal analysis 89 Algal analysis-organisms and toxins A73
microorganisms 107 Bacteriological analysis A74
5. Inorganic Analytes
heavy metals in water 57 Heavy Metals; review covers the biosensor monitoring of heavy metals in water A75
metals many Metals and air pollution particles; includes discussion of lung injury from exposure A76
trace elements 90 Plasma source isotope dilution mass spectrometry: an optimum combination for
high-precision analysis of trace elements
A77
Hg 52 Sampling and determination of particulate mercury in ambient air: a review A78
Hg 85 Sample preparation procedures for total mercury determination in
materials of natural origin
A79
Sb 117 Methodologies for determination of antimony in terrestrial environmental samples A80
tributyltin 24 Collaborative evaluation of methods for tributyltin determinations
in sediment and mussel tissue
A81
organometallics 69 Separation of metal chelates and organometallic compounds by SFC and SFE/ GC A82
phosphate 29 Phosphate; review covers multi-enzyme-based biosensors for phosphate in water A83
lanthanides 484 Trace determination of;anthanides in metallurgical, environmental,
and geological samples; covers literature since 1980
A84
sulfide 125 Analytical strategies for the detection of sulfide: a review A85
As many Arsenic compounds in terrestrial biota A86
marine waters many Automated techniques for real-time shipboard determination
of dissolved trace metals in marine surface waters
A87
marine biological samples 99 Trace metal status in marine biological samples: a review A88
seawater 60 Flow injection with chemiluminescence detection for the shipboard
monitoring of trace metals
A89
marine waters 27 Electrochemical monitor for near real-time determination of dissolved
trace metals in marine waters
A90
6. Radionuclides
radiochemistry many Environmental radiochemistry and radioactivity. A current bibliography A91
radiochemistry many Radiochemistry and radiochemical separations. A current bibliography A92
NAA many Analysis by nuclear reactions and activation. A current bibliography A93
radionuclides 181 Determination of radionuclides in environmental samples A94
long-lived radioisotopes 27 Ultratrace determination of long-lived radioactive isotopes A95
radiochemistry many Radiochemistry: inconvenient but indispensable A96
radiochemistry 7 Chemical yield tracers for radiochemical analysis A97
proficiency testing 32 ISO recommended reference radiations for the calibration and proficiency testing of
dosimeters and dose rate meters used in radiation protection
A98
accelerator MS many Accelerator mass spectrometry analyses of environmental radionuclides: sensitivity,
precision and standardization
A99
Ra 132 Radon in the environment: a current bibliography A100
Analytical Chemistry, Vol. 73, No. 12, June 15, 2001 2763
no. papers cited
6. Radionuclides
U many Analytical methods for the determination of uranium in geological and
environmental materials
A101
Pu 8 Determination of Pu isotopes at trace levels in environmental samples: radioisotopes
and stable elements evolution during the radiochemical method. Comparison of
three radiochemical protocols.
A102
actinides 10 Separation of mono-, di-, tri-, tetravalent and actinide cations on a cation exchange
chromatography column with ICPMSdetection
A103
7. Atomic Spectroscopy
general review 84 Analytical atomic spectroscopy going into the next millennium: photons or ions,
atoms or molecules?
A104
general environmental 859 Environmental analysis; extensive review of field A105
general review 319 Atomic mass spectrometry A106
monitoring 54 Atomic spectroscopy in environmental monitoring and process control A107
ICPMS 101 Environmental applications of plasma spectrometry A108
flow injection 255 Applications in environmental analysis A109
general review 676 Advances in atomic emission, absorption and fluorescence spectrometry, and
related techniques
A110
XRF many X-ray fluorescence spectrometry A111
remote sensing 32 New spectroscopic methods for environmental measurement and monitoring A112
acid interferences 161 Acid interferences in atomic spectrometry: analyte signal effects and
subsequent reduction
A113
8. Mass Spectrometry and Chromatography
portable MS 22 Advances in field-portable GC/ MSinstrumentation A114
portable MS 22 Advances in field-portable GC/ MSinstrumentation A114
membrane MS 37 pp Membrane introduction mass spectrometry; review of MIMStechniques and
applications, including environmental
A115
environmental MS 532 Environmental Mass Spectrometry; comprehensive coverage of mass spectrometry
as applied to environmental analysis, covers 1998-1999
A116
LC/ MS 241 LC/ MSinterfacing systems in environmental analysis: application to polar pesticides A117
LC/ MS 159 Applications of liquid chromatography-mass spectrometry in environmental chemistry:
characterization and determination of surfactants and their metabolites in
water samples by modern mass spectrometric techniques
A118
LC/ ICPMS 21 Speciation of metal-containing compounds found in the environment by micellar liquid
chromatography interfaced to inductively coupled plasma mass spectrometry
A119
INAA and ICPMS 8 pp Comparative use of INAA and ICP-MSmethods for environmental studies; review
includes an element-by-element assessment
A120
GC-AED 59 Environmental applications of gas chromatography-atomic emission detection A121
IC 211 Advances in the determination of inorganic anions by ion chromatography A122
IC 131 Ion chromatography in elemental analysis of airborne particles A123
IC and CE 119 Developments in sample preparation and separation techniques for the determination
of inorganic ions by ion chromatography and capillary electrophoresis
A124
CE 43 Recent developments in the separation of inorganic and small organicions by
capillary electrophoresis
A125
9. Sensors and Electrochemical
biosensors 421 pp Biosensors for environmental monitoring A126
sensors 393 pp Proceedings of the seventh international meeting on chemical sensors A127
sensors 30 Chemical and biological sensors: meeting the challenges of environmental monitoring A128
sensors 76 Other types of sensors for organic pollutants; focus on immunosensors for
organics in water
A129
biosensors 32 Update on environmental biosensors A130
biosensors 76 Other organic pollutants: enzymatic biosensors A131
biosensors 5 pp Enzyme sensors for environmental analysis A132
sensors 71 Fiber optic sensors in environmental monitoring A133
electrodes many Electrodes; extensive review on signal transduction by electrochemical techniques A134
biosensors 122 Gas-phase enzyme electrodes A135
sensors 20 In situ electrochemical monitoring: from remote sensors to submersible
microlaboratories
A136
sensors 48 Affinity sensor systems A137
sensors 95 Microelectrode sensors for biomedical and environmental applications A138
microelectrode arrays 53 Microfabricated ultramicroelectrode arrays: developments, advances, and
applications in environmental analysis
A139
sensors 171 Advances in the microfabrication of electrochemical sensors and systems A140
biosensors 205 Molecular probes and biosensors in bioremediation and site assessment A141
gas sensors 15 Next-generation diode laser gas sensors for environmental and industrial monitoring A142
microbial sensors 36 Biochemical oxygen demand A143
sensor arrays 10 pp Electronic tongues for environmental monitoring based on sensor arrays and
pattern recognition: a review
A144
stripping voltammetry 230 Stripping voltammetry in environmental and food analysis A145
electrochemical detection 110 Metalloporphyrin, metallophthalocyanine and related macrocycle complex-based
film modified electrodes: review of selected significant designs and
applications to the electrochemical detection of pollutants
A146
SPME 44 New developments in SPME A147
no. papers cited
10. SPE, SPME, and Sample Extraction
SPME 40 Analysis of industrial pollutants in environmental samples A148
SPME 12 pp Solid-phase microextraction: a promising technique for sample preparation in
environmental analysis
A149
SPME 40 Metal speciation by SPME-CGC-ICPMS A150
SPME 16 Organometallic speciation by combining aqueous phase derivatization with
SPME-GC-FPD-MS
A151
SPME 41 The application of SPME-LC-MSto the determination of contaminants
in complex environmental matrices
A152
SPE 9 pp Advances in solid-phase extraction disks for environmental chemistry A153
SFE 29 On-line detection for supercritical-fluid extraction A154
11. Sample Handling and Extraction
sample preparation 36 pp Sample preparation for environmental analysis; state-of-the-art review A155
microwave extraction 73 Microwave assisted extraction of organic compounds A156
microwave extraction 33 Application of microwave techniques in analytical chemistry A157
microwave extraction 61 Microwave-assisted solvent extraction of environmental samples A158
pressurized liquid
extraction
40 Pressurized liquid extraction of persistent organic pollutants in
environmental analysis
A159
membrane extraction 24 Liquid membrane extraction in analytical sample preparation A160
membrane and SPE extraction 43 Ion separation in membrane and solid-phase extraction systems A161
cellulose sorbent
preconcentration
42 Functionalized cellulose sorbents for preconcentration of trace
metals in environmental analysis
A162
organic analytes in water 167 Chemical analysis: sample handling and analysis of organic pollutants
in water matrices
A163
water removal from samples 55 Water vapour removal from gaseous samples used for analytical purposes A164
SFE 14 pp Properties of supercritical fluids relevant to extraction and chromatography A165
POPs 174 Separation, clean-up and recoveries of persistent trace organic
contaminants from soils, sediment and biological matrices
A166
12. Sampling, QA and QC, Chemometrics
sample handling 1138 pp Sample handling and trace analysis of pollutants: techniques, applications
and quality assurance
A167
water sampling 20 pp Sampling methods in surface waters A168
sediment sampling many Sediment trap sampling in surface waters A169
soil water sampling 33 Collection of soil solution A170
vocs in air 190 Sorbent trapping of volatile organic compounds A171
passive dosimetry 14 pp Passive sampling for long-term monitoring of organic pollutants in water A172
monitoring programs 10 Designing monitoring programs to evaluate the performance
of natural attenuation
A173
diffusive sampling 147 Monitoring the ambient environment with diffusive samplers: theory
and practical considerations
A174
quality assurance many Quality assurance in environmental monitoring A175
long-term monitoring 69 Ensuring quality in long-term environmental monitoring for chemical speciation A176
airborne particles 10 Quality assurance, quality control, and data validation in environmental
analysis of airborne particles
A177
airborne particles 38 Quality assurance and quality control in the elemental analysis of
airborne particles
A178
QA and QC 34 Quality of residue data A179
reference materials 54 Certified reference materials for quality control of measurements in
environmental monitoring
A180
reference materials 56 Standard reference materials for the determination of trace organic
constituents in environmental samples
A181
reference materials 16 Proper use of reference materials for elemental speciation studies A182
uncertainty 75 Sources of uncertainty in gas chromatography and high-performance
liquid chromatography
A183
uncertainty 15 Evaluating uncertainty in routine analysis A184
statistics 95 Some applications of statistics in analytical chemistry A185
chemometrics 142 pp Pattern recognition, chemometrics, and imaging foroptical environmental
monitoring
A186
chemometrics 60 Spectral pattern recognition: the methodology A187
TMSderivatization 65 Artifacts in trimethylsilyl derivatization reactions and ways to avoid them A188
blank optimization 25 Blank optimization for elemental analysis of laboratory water down to ppt levels A189
analyte stability 86 Stability of chemical species in environmental matrices A190
13. Biomonitoring and Biomarkers
freshwater biomonitoring 43 Biomonitoring for the 21
st
century A191
fish as biomonitors 144 Biomonitoring and ecotoxicology: fish as indicators of pollution-induced
stress in aquatic systems
A192
vegetation as biomonitors 154 Biomonitoring using aquatic vegetation A193
marine biotests 84 Choice of biotests and bioindicators for evaluation of the quality of the marine
environment
A194
great lakes fish 64 Neoplastic and inflammatory liver diseases of white suckers as environmental
quality indicators
A195
mussel biomonitors many The mussel watch approach and its applicability to global chemical
contamination monitoring programs
A196
parts-per-trillion (ppt) detection limits, and methods achieving
these levels were mostly based on high-resolution mass spec-
trometers (HRMS). Capillary columns for trace organics deter-
mination were commonplace, but many packed column methods
were still used. Many citations to methods for the chlorinated
dibenzo-p-dioxins, dibenzofurans, and PCBs werefound. Speciation
methods for organometallics werebeginning to achieveimpressive
results, with detection based mostly on atomic absorption (AA)
techniques. Supercritical fluids for extractions and microwave
ovens looked like huge new developments, and the promise of
immunoassays for rapid screening appeared promising.
Ten years later, the environmental analysis field has changed
significantly. Few references to improved methods for dioxins/
furans/ PCBs were found, as HRMS methods for these analytes
have now matured. Impressive improvements in detection limits
for such analytes are such that ppt detection is routine for many
organic analytes, even by using benchtop quadrupole and ion trap
mass spectrometers. Parts-per-quadrillion (ppq) detection is now
becoming routine, and detection of a few hundred femtograms of
some analytes is now possible, although such detection levels
cannot yet be considered routine. Relatively new organic groups
such as the nonylphenol ethoxylates, pharmaceuticals and steroids
as environmental contaminants, and higher molecular weight polar
compounds arebeing studied. Many seemingly different chemicals
are now listed under the label of endocrinedisruptors, the study
of which will be an exceedingly difficult analytical challenge
because of the low detection limits required and widely varying
analytical properties of the many chemicals in this group. Such
investigations have greatly expanded over the past few years
because of the maturing field of liquid chromatography/ mass
spectrometry (LC/ MS). Benchtop LC/ MSmodels are now avail-
able for this work that make such studies available to a much
greater range of researchers, much as the benchtop GC/ MSdid
in the early 1980s. For metals and organometallics determination,
the field is rapidly becoming dominated by the inductively coupled
plasma mass spectrometry (ICPMS) technology. Although AA is
still widely used, most significant new developments in the
environmental analysis field are ICPMSbased. Other technologies
that have been significantly advanced in the past two years are
GC/ time-of-flight mass spectrometry (GC/ TOFMS), membrane
introduction MS, pressurized liquid extraction, and real-time
emissions monitoring. Microwave ovens for sample extraction are
still being developed, but have not yet achieved the widespread
use that seemed inevitable afew years ago, and supercritical fluid
extraction (SFE) now seems to be aterrific technique for selected
applicationssbut it now appears SFE will not reach the status of
an essential, widely applicable technology. One relatively recent
development that has exploded in the past two years is solid-phase
microextraction (SPME). So many references to environmental
analysis applications by using SPME were published, that we
decided to highlight this technique in a special section im-
mediately following the summary of review articles.
REVIEW ARTICLES
This section is the only one of this review where our intention
was to be inclusive rather than exclusive. By summarizing other
published review articles relating directly to environmental
analysis, the authors hope to provide readers with a source of
more detailed follow-up information. We have done this because
it is impractical for a single article to be comprehensive in
coverage for such an active and broad field as environmental
analysis. These citations are presented in Table 1.
SOLID-PHASE MICROEXTRACTION APPLICATIONS
The use of SPME, in which a small, polymer-coated fiber is
used to extract analytes from aqueous samples or air, has exploded
since our last review. The first SPME device was described in
1990 (B1) and represented an innovative approach to sample
no. papers cited
13. Biomonitoring and Biomarkers
EROD induction 60 EROD induction in fish: a tool to measure environmental exposure A197
dendroanalysis 22 Dendroanalysis: a tool for biomonitoring environmental pollution? A198
tree monitoring 172 A decade of forest tree monitoring in Canada: evidence of air pollution effects A199
bivalve markers many Appraisal of prospective bivalve immunomarkers A200
biomarkers many Biomarkers of exposure A201
bioremediation efficiency 28 Biomarkers for monitoring efficacy of bioremediation by microbial inoculants A202
14. Toxicity
Watertox bioassays 98 pp Watertox Bioassays; comprehensive discussion of A203
toxicity testing guideline many Assessment of the U. S. EPA methods for identification of hazards
to developing organisms: the developmental toxicity testing guideline
A204
marine toxicity many Characterizing and identifying toxicants in marine waters: a review of
marine toxicity identification evaluations
A205
endocrine disruptors many Assays for endocrine-disrupting chemicals: beyond environmental estrogens A206
aquatic plants many Aquatic plants for toxicity assessment A207
whole effluent testing many Field assessments in conjunction with whole effluent toxicity testing A208
whole effluent testing many Whole effluent toxicity testing: usefulness, level of protection,
and risk assessment
A209
15. Miscellaneous Review Topics
monitoring trends 260 Trends in environmental analytics and monitoring A210
asthma agents monitoring 73 Environmental monitoring of chemical agents A211
management 11 The proper place of analytical chemistry in environmental management A212
humics 80 Humic substances in water A213
dendrochemical
monitoring
many Monitoring historical changes in soil and atmospheric trace
metal levels by dendrochemical analysis
A214
preparation. Analyte collection and concentration, from an aqueous
sample, were accomplished simultaneously. Because thermal
desorption was used to transfer the analytes from the SPME fiber
to the GC/ ECD, no harmful organic solvents were required for
sample introduction into the detection system. Continued interest
in SPME has been fueled by its commercialization by Supelco
(Bellefonte, PA) in 1993 and by the choice of almost a dozen
different fiber coatings, which allow the analyst to optimize the
extraction of various compound classes. SPME can be considered
auniversal extraction method, as it can be used on gases, liquids,
and solids (the headspace above the solid is typically sampled).
SPME can be coupled easily with both GCand LC. Because SPME
coupled with GC requires no solvent, it is an excellent sample
preparation technique for field analyses and is particularly well
suited to rapid response applications. Despite the fact that there
have been many publications about this technique, some aspects
of SPME, including the fundamentals of how analytes interact with
the fiber coatings and the stabilities of analytes collected on a
fiber, remain to be addressed. In addition, obtaining accurate
quantitation with SPME can be challengingsfactors such as
matrix composition, temperature, pH, and extraction times must
be strictly controlled. The theory and application of SPME were
summarized recently in several books (B2-B4). Because a
comprehensive review of SPME is outside the scope of this paper,
we will highlight articles that illustrate trends and recent SPME
applications.
Characterization of Organic Compounds. The largest use
of SPME is for the characterization and quantitation of organic
compounds. SPME/ GC/ MS was used to characterize landfill
leachate; aliphatic and aromatic compounds with alcohol groups
were detected (B5). SPME was used to sample the headspace
above fish tissue extract; approximately 170 organic compounds
were detected by GC/ MS (B6). Automated SPME/ GC/ FID,
which operated in a stop-flow mode, allowed on-line pH adjust-
ment of samples, internal standard addition, and unattended field
operation for 1 week, was used to monitor part-per-billion
concentrations of organic compounds in industrial wastewater
(B7). SPME/ GC/ FID and pattern recognition algorithms were
used to characterize different types of jet fuels and to determine
contamination sources (B8).
Water Analyses. SPME/ GC/ MS was used for the determi-
nation of 55 volatile organic compounds; this technique had
linearity comparable to and detection limits (50 ng/ L for some
analytes) better than purge-and-trap GC/ MS (B9). Precise pH
adjustment is critical for the extraction of organic acids and bases;
small changes in pH change the concentrations of neutral species
in water and, thus, affect their partitioning between water and the
SPME fiber (B10). This can make quantitation challenging.
SPME/ GC/ MS has been applied to the analysis of small, polar
molecules, such as volatile amines (B11) and gasoline oxygenates
(B12, B13). SPME/ GC/ MSyielded excellent detection limits, 10
ng/ L, for the gasoline oxygenate methyl tert-butyl ether (B12,
B13) and 15 g/ L for ethanol (B13). SPME/ GC/ MS, with
derivatization, was used for analyses of haloacetic acids at
concentrations as low as 10-500 ng/ L (B14) and pharmaceuticals
at concentrations of 0.2 and 50 g/ L (B15) in water.
There continues to be interest in coupling SPME with LC/
MS. Linear alkylbenzenesulfonates, at detection limits of 0.5 g/
L, were determined with SPME coupled with electrospray MS
(B16). In-tube SPME, which uses a polymer-coated tube instead
of a conventional fiber, coupled with LC/ MS was used to
determine trimethyl- and triethyllead, at 10 g/ L (B17). A home-
built electrospray probe was developed, coupled to a SPME
graphite fiber, and used to detect 10
-9
M Triton-X (B18).
Soil, Sediments, and Pore Waters. SPME was used to
concentrate organic compounds in the headspace above sediments
and soils. Polycyclic aromatic hydrocarbons, at an estimated
detection limit of 1 g/ kg sample, were detected in sediments by
SPME/ GC/ MS(B19). SPME/ GC/ MSwas also used to determine
polychlorinated biphenyls, at submicrogram per kilogram con-
centrations, in soils (B20). In an unusual application (called
matrix SPME), poly(dimethylsiloxane)-coated glass fibers were
used as samplers of polychlorinated biphenyls (PCB) in sediment
pore water (B21). The results of this work might be considered
controversial, as absorption partition coefficients are used to
calculate PCB concentrations (B22). It has been asserted that
surfaceadsorptionis moreimportant than absorptionfor controlling
SPME collection of high molecular weight compounds, such as
PCB (B23, B24); thus, PCB concentrations calculated on the basis
of adsorption partition coefficients would not be accurate.
Air Monitoring. Air monitoring is arelatively new application
of SPME. A rapid, SPME-based method, with 1-min sampling and
15-min analysis times, was used to determine BTEX compounds
(benzene, toluene, ethylbenzene, and xylenes) in air; when
coupled with GC/ PID, detection limits were 1 ppb and results
were comparable to those produced by a standard method of the
National Institute of Occupational Safety and Health (B25).
SPME/ GC/ AED was used to determineorganic sulfur compounds
at detection limits of 4-50 parts-per-trillion; however, low storage
stability of the analytes, artifact formation, and the adverse effect
of humidity on extraction efficiency limit SPMEs utility for
quantitative, on-site analyses (B26). Bartelt and Zilkowski refined
their model of the relationship between airflow rates and the
absorption of analytes on aSPME fiber (the importance of sample
temperature was also considered). Using their new model, they
could measure abroad range of analytes, collected under different
conditions, without prior calibration of the SPME fiber, and
regardless of whether equilibrium conditions were established
(B27). Temperature and humidity influence the partitioning of
analytes between the air and SPME fiber, thus affecting method
calibration and increasing the complexity of analyte quantitation
(B28). While the previous studies focused on the determination
of volatile organic compounds in the gas phase, the feasibility of
using SPME (and also a needle trap device inspired by SPME)
to sample aerosols and airborne particles was demonstrated for
polycyclic aromatic hydrocarbons in diesel exhaust, triamcinolone
in an asthma drug, and DEET in insect repellent (B29).
Inorganic/ OrganometallicCompounds. The application of
SPME to analyses of inorganic compounds is increasing. Several
recent applications are described in Table 2. In these applications,
headspace sampling of the resulting extract was most often used
to minimize interferences.
AIR MONITORING AND ANALYSIS APPLICATIONS
General Comments. This review emphasizes the develop-
ment of novel sampling and analytical methods and their applica-
tions in the characterization and analysis of toxic airborne
pollutants. In addition, developments in areas of photochemical
precursors are also included. Articles related to nonmetal gases,
acid gases, and criteria gaseous pollutants are not covered here.
The review is organized by analytes and applications with the
intent to highlight new technologies and/ or methodologies for
the sampling and analysis of different types of toxic airborne
pollutants. These include sampling (design, phase distribution,
sector sampling, and specific sampling devices), volatile organic
compounds (VOCs), semivolatile organic compounds (SVOCs),
inorganic compounds, and spectroscopy/ chemometrics (optical
spectroscopy, mass spectrometry, postdata processing, and data
interpretation algorithms). Papers on the subjects of automated
analysis, especially its application to the monitoring of photo-
chemical precursors and emissions from incineration, have been
included. Finally, publications on the subjects of bacterial load,
single aerosol particle analysis using particle-induced X-ray emis-
sion (PIXE), and applications of a quartz crystal microbalance
sensor are reviewed.
Several newtrends were observed in air analysis since the 1999
review. As discussed earlier, SPME methods have been applied
to the sampling and sample preparation of VOCs and SVOCs in
environmental sample types such as water, soil, and air. SPME is
a great screening tool but, due to a limited amount of adsorbent
that can be coated on the surface of the SPME fiber, using SPME
to achieve accurate quantitative analysis can be challenging. The
development of an improved SPME method, the stir bar sorptive
extraction (SBSE) approach where a glass stir bar coated with
poly(dimethylsiloxanes) (PDMS), up to 500 of loading capacity
of atypical SPME fiber, was successfully applied for the sampling
and quantitative analysis of airborne VOCs and SVOCs (C10, E20).
SBSE is a relatively new method, and we expect to see more
applications in the future. Airborne polycyclic aromatic hydrocar-
bon (PAH) analysis continues to be apopular subject. In fact, more
than 40%of the SVOC publications are the sampling, analytical
method development, and characterization of airborne PAHs.
Similar to PAHs are the endocrine disruptors that may be released
from many sources but have yet to be characterized in a
systematic manner. We expect to see more PAH and endocrine
disruptor-related publications in the future. In the areaof inorganic
applications, we noted an increasing number of publications
related to the use of chromatographic separation followed by
various detection techniques for the analysis and speciation of
metals and organometallics. The instrumentation typically consists
of GC/ MS, ion chromatography (IC), LC/ ICPMS, and LC-atomic
emission spectroscopy (LC-AES). We expect to see more publica-
tions related to separation-enhanced speciation of inorganic
compounds.
Sampling. The collection of representative air samples for
laboratory analysis remains the most challenging part in environ-
mental air monitoring and analysis. Proper sampling and sample
storage procedures are essential to ensure that laboratory data
are representative of the sampling site and comply with applicable
technologies and regulations. Romano described a method to
determine and optimize the number of monitoring stations
required in an air pollution network (C1). Using clean quartz and
tobacco smoke particles as amodel for mineral surface and aerosol
organic matter, Pankow studied two mechanisms by which gas/
particle partitioning of SVOCs such as PAHs, PCBs, and organo-
chlorines (OCs) can occur via adsorption to particle surface or
organic aerosols (C2). Gas/ particle phase distribution of PAHs,
PCBs, and OCs was also studied by Bidleman using ahigh-volume
air sampler which employs a filter and a sorbent trap to retain
particulate and gaseous compounds (C3). Using a similar experi-
mental setup, Sanusi studied the characteristics of gas/ particle
distribution of OCs and carbamate pesticides in urban, rural, and
remote sites (C4). A study on the effect of meteorological
parameters on the size distribution of particle-adsorbed PAHs was
carried out by Schnelle-Kreis. Depending on wind direction,
maximum PAH concentrations varied on particles depending on
their geometric mean diameters, which varied from 75 to 920 nm
(C5). The capability of a porous plastic foam and an air-to-liquid
membrane for particle size-selective sampling and/ or direct
airborne particle sampling, respectively, was also evaluated (C6,
C7).
The use of a multisorbent-based cartridge for VOC sampling
followed by thermal desorption-GC/ MS(TD-GC/ MS) analysis has
been popular since the introduction of the USEPA method TO-17
in 1996. A study was carried out to evaluate the performance of
Tenax GRand Carbosieve SIII as VOC sampling media followed
by ashort-path thermal desorption analysis of 77 VOCs (C8). The
performance of a Carbograph 2 and Carbograph 5 multisorbent
cartridgewas also evaluated at various sampleloadings and sample
volumes ranging from 0.1 to 1000 mg/ m
3
(C9). Contrary to the
Table 2. SPME Applic ations to Environmental Analysis
a
analyte method matrix D.L (ng/ L) ref
Hg, methyl- water extraction, NaBEt4 derivatization, SPME/ GC/ MS spiked soil B30
Hg, methyl- SPME/ thermal desorption/ ICP/ MS water, reference tissue 200 B31
Pb, tetraethyl- NaBEt4 derivatization, SPME/ GC/ MS water 400 B32
Pb, alkyl- NaBEt4 derivatization, SPME/ GC/ MS water 100 B33
Se derivatization with 4,5-dichlor-1,2-phenyldiamine, SPME/ GC/ MS tap and river water 6 B34
Sn, Hg, Pb NaBEt4 derivatization, SPME/ GC/ ICP/ MS surface water and sediment 0.1-4 B35
Sn, butyl- and
phenyl-
NaBEt4 derivatization, SPME/ GC/ FPD water, sediment, sewage sludge 0.006-0.6 B36
Sn, butyl- NaBEt4 derivatization, SPME/ GC/ FID water, reference sediments 30 B37
Sn, triphenyl- TMAH or KOH-EtOH extraction, NaBEt4 derivatization,
SPME/ GC/ ICP/ MS
water, potatoes, mussels 0.1 B38
a
Abbreviations: AAS, atomic absorption spectroscopy; DL, detection limit; EtOH, ethanol; FID, flame ionization detector; FPD, flame photometric
detector; GC, gas chromatography; ICP, inductively coupled plasma; NaBEt4, sodium tetraethylborate; MS, mass spectrometry; SPME, solid-phase
microextraction; TMAH, tetramethylammonium hydroxide.
multisorbent-based VOC sampling is the SBSE-based approach,
where equilibrium sorptive enrichment on PDMS instead of an
adsorption process was used to concentrate VOCs in the air
sample prior to analysis. This allows the use of a high-inertness
sorption material such as PDMSand provides an analytical blank
free from interference (C10). The use of newsampling mediasuch
as mesoporous carbons for airborne polar VOC sampling (C11)
and a reversed-phase packing material (C
18
-Silica) for airborne
VOCsampling (C12) followed by off-line extraction or elution and
GC-flame ionization detector (GC-FID) or GC/ MS analysis was
evaluated against criteria such as compatibility with Tenax,
reusability, and background interference in the GC analysis. The
use of fullerene-extracted soot (a byproduct of fullerene produc-
tion) in place of the Tenax GR(C13) was also evaluated using 17
VOCs.
The applicability of two different types of Nafion membrane
dryers and apoly(phenylene sulfide) wool-based O
3
scrubber was
evaluated for the adsorptive sampling of selected volatile organo-
sulfur compounds and was demonstrated to provide an artifact-
free analytical results (C14). Due to the potential health effect
induced by the long-term exposure to ambient VOCs, continuous
sampling periods of 4 weeks, 7 days, and 24 h were evaluated at
0.5, 2.0, and 14 mL/ min sampling rates via a multisorbent
sampling tube followed by GC/ MS analysis (C15). It was found
that, except for vinyl group-bearing compounds, concentrations
of other TO-14 target compounds estimated by 4-week and 7-day
sampling methods were approximately equal to the 24-h mean
concentration.
The feasibility of using Carbopack B 60/ 80 for diffusive
sampling of VOCs was evaluated and found to have a superior
uptake rate to Tenax TA 60/ 80 for the majority of VOCs analyzed
(C16). The Carbopack 60/ 80 showed a stability of up to 28 days.
Similarly, the performance of the 3M 3520 organic vapor monitor
as a passive VOC sampler was evaluated for 24-h periods under
various humidity and temperature conditions. It was found that,
except for 1,3-butadiene, styrene, and methylene chloride, the 3520
device can be effectively used over the range of concentrations
and conditions tested with a 24-h sampling period with an error
of ( 25%(C17). In the bioaerosol sampling area, glycerol was
tested as a collection substrate for passive sampling from three
fungal species with results compared with a closed-face polycar-
bonate filter sampling method (C18). The glycerol was demon-
strated to have good correlation with the closed-face sampler and
to have a sample storage time of up to 7 days.
Indoor air sampling methods for the assessment of environ-
mental contamination were also investigated. A field comparison
of the standard dust wipes method and the Lioy-Wainman-
Weisel (LLW) sampler was carried out to evaluate comparability
of these two methods of indoor dust lead analysis. Correlation
results within paired samples indicated that the LLW sampler has
a significantly higher internal reproducibility for Pb loading than
the dust wipe method (C19). Tedlar air sampling bags were used
extensively for both indoor, ambient and abatement, sampling
purposes. A study examining the adsorption and desorption
behavior of six different organic compounds was carried out to
evaluate the reusability of Tedlar air bags for air sample collection
(C20). It was demonstrated that one should consider carefully
before the start of any sampling program using Tedlar air bags.
On the other hand, it was also demonstrated that Tedlar air bags
can be an effective and a convenient sampling tool collecting
volatile metalloid compounds in ambient air (C21). The ability of
Tenax or XAD or activated carbon-embedded solid-phase extrac-
tion (SPE) disks for SVOC sampling in diesel exhaust was
validated and compared with a conventional polyurethane foam
(PUF) sampling method (C22). The capability of a personal air
sampler for 24-h collection of fine particles and SVOCs, especially
PAHs, was critically evaluated (C23) for use in human exposure
and biomarker studies. The suitability of using diffusive samplers
for indoor air benzene, toluene, xylenes, and ethylbenzene
sampling was evaluated using headspace SPME and GC-FID
analysis (C24). Finally, a new personal aldehyde and ketone
sampler was developed and validated using dansylhydrazine
derivatization on solid sorbent with part-per-billion sensitivity
(C25).
VolatileOrganicCompounds. VOCanalysis requires the use
and preparation of low-concentration standard gas mixtures with
good consistency and high accuracy. This is usually prepared by
using either a static dilution system or a dynamic dilution system
with primary standards that can be traced back to a certified
reference material (CRM). Combining a diffusion device with a
dynamic dilution system, anew VOCstandard preparation system
was developed and validated at the part-per-trillion, v/ v (pptv) to
part-per-billion, v/ v (ppbv) levels for various VOCs over 21months.
The system was demonstrated to be suitable for compounds with
a wide range of boiling points from 305 (32 C) to 418 K (145 C)
and a linear dynamic range of 10
4
(D1).
A procedure using an active charcoal packed porous poly-
(tetrafluoroethylene) (PTFE)-based tube passive sampler followed
by toluene extraction and GC-electron capture detection (GC-
ECD) analysis of 18 indoor and ambient airborne organohalogen
VOCs was developed and validated using real world samples (D2).
Two direct sampling ion trap MS(ITMS) systems were evaluated
for monitoring trace levels of halogenated VOCs in air. It was
found that both direct sampling ITMSsystems offer comparable
analytical results with a detection limit at 50 ppbv in selection
ion monitoring (SIM) and MS/ MS operation modes (D3). The
capability of multisorbent-based sampling followed by GC/ MS
analysis of a wide range of VOCs was investigated and demon-
strated that by changing the sample volume and the amount of
Carbotrap B and Carboxen 1000 in the sampling cartridge, one
could analyze VOCs from dichlorofluoromethane (CFC12) to 1,2,3-
trichlorobenzene at method detection limits from 0.02 to 0.4 ppbv
(D4).
Analysis of odorous and/ or polar VOCs remains a major
challenge for analytical chemists. The capabilities of various
sampling methods, sample preparation procedures, in situ or off-
line derivatization schemes, and analytical systems were evaluated
with the goal to optimize the system performance to enhance data
quality. Table 3 summarizes these activities according to the
analytes, sampling methods, derivatizing schemes, and analytical
systems used in the method (D5-D14).
SemivolatileOrganicCompounds. New procedures for the
sample preparation and analysis of SVOCs including OCs, PAHs,
and pesticides have been reported. These measurements have
stringent quality control and quality assurance (QC and QA,
respectively) protocols to support the usability of analytical data.
In addition, the use of CRMs and standard reference materials
(SRMs) improve precision and accuracy. For the determination
of PAHs, the National Institute of Science and Technology (NIST)
has recertified PAH urban dust SRM 1649 as SRM1649a using
normal-phase liquid chromatography (NPLC) followed by reversed-
phase liquid chromatogrphy-fluorescence detection (RPLC-FL),
i.e., NPLC/ RPLC-FL for isomeric PAH analysis and GC/ MS
analysis using three different stationary phases (E1). Twelve new
procedures were developed for PAH sample preparation and/ or
analysis using optical or MS-based detection methods (E2-E14).
These applications are summarized in Table 4.
In addition to PAH analysis, the long-term performance of a
GC/ negative ion chemical ionization MS(GC/ NICI-MS) system
for the continuous measurement of peroxyl acetyl nitrate (PAN)
and its homologues was studied. Sensitivity and linearity of the
GC/ NICI-M system were demonstrated at the pptv level with
significant sensitivity drift that can be corrected using an internal
standard (E15). A method using GC/ ITMSand GC/ NICI-MSfor
atmospheric s-triazines and their metabolites, at detection limits
from 0.8 to 15 pg/ m
3
, was developed (E16). Identification of
unknowns in multicomponent organic aerosols was demonstrated
by a temperature-programmed thermal desorption particle beam
Table 3. Polar/Odorous VOC Analytic al Methods
analytes method/ description/ comments refs
chlorine- and sulfur-containing biogases from
sewage and landfill
Summa canister followed by GC/ MSor GC-atomic emission
spectroscopy (GC-AES) analysis
D5
ambient sulfur-containing odorous VOCs automated Tenax GRtrap preconcentration, liquid N2 focusing,
followed by GC and flameless sulfur chemiluminescence detection
D6
ambient polar VOCs such as carboxylic acids,
alcohols, and phthalates
impinger sampling followed by solid-phase extraction (SPE) and
GC/ MSanalysis
D7
airborne formaldehyde sampling with in situ derivatization of formaldehyde on
3,5-bis(trifluoromethyl)phenylhydrazine-coated silica followed by
GC-ECD and GC/ MSanalysis; results were validated with
NIOSH method 3500 and 2,4-dinitrophenylhydrazine derivatization
D8
atmospheric alcohols sampling with 200-mL glass bottle followed by the reaction with
200 ppmv nitrogen dioxide on the glass surface to form alkyl
nitrites and then by GC-ECD analysis.
D9
particulate matter-associated aromatic amines direct MSidentification of vapor-phase and particulate samples
collected in heavy traffic area; five chemical classes of aromatic
were found to exist in the samples.
D10
ambient carbonyls and hydroxy carbonyls impinger sampling and in situ derivatization of carbonyl
compounds with o-(2,3,4,5,6-pentafluorobenzyl)hydroxyamine
hydrochloride; further reaction of hydroxy carbonyls with
bis(trimethylsilyl)trifluoroacetaamine followed by GC/ ITMSanalysis
D11
ambient aldehydes and ketones multisorbent cartridge sampling followed by TD-GC using a new
PLOT column capable of separating ketones and aldehydes
from hydrocarbons
D12
ambient formaldehyde and acetaldehyde in situ 2,4-dinitrophenylhydrazine sampling and derivatization
followed by HPLC-APCI-MSanalysis using stable isotope-
labeled standards
D13
ambient formaldehyde and acetaldehyde in situ 2,4-dinitrophenylhydrazine sampling and derivatization
followed by micro-HPLC analysis and fiber-optic-based UV detector
D14
Table 4. Ambient PAH Analytic al Methods
analytes method description/ comments refs
PAH sample preparation method for airborne particulate-associated PAHs using focused
microwave extraction for GC/ MSanalysis with 3-h sample preparation time and
superior recovery and precision
E2
azaarenes airborne particulate-associated azaarenes analysis using normal-phase semipreparative
LC fractionation followed by RP/ LC-FL analysis of nine azaarenes
E3
PAH critical evaluation of LC-UV, GC-FID, and GC/ ITMSfor the analysis of 19
airborne particulate-associated PAHs
E4
PAH, DDT, BHC laser desorption-ITMSscreening method of target compounds on a single airborne particle E5
B[ a] P diones column chromatographic cleanup of soot aerosols followed by LC/ atmospheric pressure
chemical ionization/ MS(LC/ APCI-MS) analysis
E6
B[ a] P isotope dilution B[ a] P analysis using a benchtop GC/ MS E7
PAHs and
nitro-PAHs
direct screening of aerosol filter samples using laser desorption-time-of-flight-MS
(LD-TOFMS)
E8
PAHs grease-coated Denuder sampling for the determination of phase-distributed PAHs E9
nitro-PAHs extraction of particulate-associated nitro-PAHs, reduction of nitro-PAH to amino-PAH,
and derivatization of the amino-PAH followed by GC/ ECD analysis at the picogram level
E10
PAHs method was developed for LC/ APCI-MSanalysis of particulate-associated high molecular
weight PAHs (MW>300)
E11
PAHs and
thiaarenes
workplace air of an aluminum reduction plant was analyzed using GC-AED; running
GC-AED in sulfur-selective mode allowed the analysis of thiaarenes without prior
separation of PAH from thiaarenes
E12
PAHs PAHs in gasoline and diesel fuels and emissions from engine exhaust were
characterized and quantitated at mg/ L and g/ kg levels
E13
NIST 1649
PAH SRM
microscale sealed vessel (MSSV) thermal extraction-GC/ MSand MSSV-pyrolysis-
GC/ MSmethods were evaluated using the SRM and found to be useful for the
characterization of PM
10 organics.
E14
mass spectrometer (E17). A novel application using GC/ electron
capture negative ion MS (GC/ ECNI-MS) for the analysis of
airborne toxaphene congeners was investigated (E18). Finally,
an SBSE sampling TD-GC/ MSand TD-GC-nitrogen phosphorus
detector (TD-GC-NPD) method was developed for the monitoring
of airborne nicotine at the 5-250 g/ m
3
level (E19).
InorganicCompounds. The sample preparation and analysis
of inorganic compounds including metals, mercury, and volatile
and nonvolatile organometallics were reported in several publica-
tions. Analytical technologies include IC, inductively coupled
plasma-optical emission spectrometry (ICP-OES), ICPMS, X-ray
fluorescence (XRF), AA, and AES. Methods were also developed
for the introduction of samples and calibration standards to ensure
the precision and accuracy of the analysis. For example, Woskov
demonstrated amicrowave-sustained atmospheric plasmaequipped
with an attached source of real-time calibration of metal standards
that was capable of providing the highly sensitive and accurate
data required for on-line continuous emission monitoring (F1).
Using ICP-OES, a method was developed for the elemental
analysis of size-segregated particles ranging from 0.03 to 10 m
(F2). ICPMS instrumentation has had a wide acceptance in
inorganic analysis, and several methods were developed for trace
element analysis of airborne particles using ICPMS-based instru-
mentation, summarized in Table 5 (F3-F7) according to analytes,
analytical methods, and applications. In addition, a method was
developed using laser-induced plasmaspectroscopy (LIPS) for the
on-line monitoring of chromium aerosols of an industrial waste
stream (F8). Laser ablation-based ICPMS(LA-ICPMS) methods
were also developed for the direct analysis of airborne particulate
collected on poly(tetrafluoroethylene) membrane filters (F9) and
the high-resolution, rapid quantitative chromium analysis at a
detection limit of 0.05 g/ filter (F10). Combining instrument
neutron activation analysis and ICPMS, concentrations of metal
collected by PM
10
and PM
2.5
filters were quantified for various
metals with comparable results (F11).
Table 5. Inorganic Applic ations and Methods
analytes methods/ comments refs
ICPMS-Based Methods
206
Pb,
207
Pb,
208
Pb Pb isotope ratio analysis of size-fractionated aerosols for source apportionment applications F3
Pt, Pd, Rh method performance for the analysis of airborne Pt, Pd, and Rh from vehicles catalytic converters F4
235
U,
238
U using
235
U/
238
U ratio obtained from tree bark for the discrimination of nuclear and nonnuclear
emission sources
F5
NiCl2, NiO, NiCO3 method performance for the analysis soluble and insoluble Ni compounds in airborne particulate matter F6
Mn, Fe, Co, Ni, Ag,
Cd, Sn, Sb, Pb
determination of size-fractionated particles from arctic air for trace metal monitoring F7
Chromatography-Assisted Methods
Zn, Co, Fe
2+
, Fe
3+
,
Mn, Cd, Pb
isocratic ion chromatography separation, postcolumn derivatization, UV detection at detection limits
of 10-60 ppb
F12
Zn, Cu, CO, Fe, Cd capillary electrophoresis separation and direct UV detection at detection limits 0.5- 3 ppb F13
Be micellar electrokinetic chromatography analysis of Be in airborne particulate at 1 ppm detection limit F14
Ni(CO)4, Fe(CO)5,
Mo(CO)6, W(CO)6
cryotrapping-GC/ ICPMSanalysis of sewer gas of analytes as a fermentation byproducts F15
Sb(CH3)3, Sn(CH3)4,
Sn(CH3)2(C2H5)2,
Bi(CH3)3
GC/ ITMSan GC/ ICPMSanalysis of volatile organometals in land fill and fermentation gases F16
butylated trimethyl-,
dimethyl-, triethyl-,
diethyllead
GC/ ICPMSanalysis of organolead compounds using tetraethyllead as internalstandard
with detection limits of 2-9 fg for a 1-mL injection
F17
arsenic speciation of arsenic in coarse and fine urban aerosols using sequential extraction and
LC-atomic fluorescence detection with comparable results obtained from INAA analysis
F18
Sb(CH
3)3, Sb LC/ ICPMSanalysis of analytes in airborne particulate F19
XRF-Based Methods
Ca, Cu, Fe, Mn, Ni,
Pb, V, Zn
XRF analysis of aerosol filters of 150-mm diameter with comparable quantitative
results from AA and ICP-OES
F20
silicon XRF analysis of silicon in airborne-particulate matter with quantitative results validated by LA-ICPMS F21
S, Ca, K, Ti, V, Cr, Mn,
Fe, Ni, Cu, Zn, Pb
performance of chemical speciation of analytes in airborne dust by sequential leaching
and XRF was validated by NIST 1648 CRM
F22
lead performance evaluation of portable XRF instrument for analyzing dust wipe samples
with results validated by AA
F23
S, Ca, Cr, Mn, Fe,
Ni, Cu, Zn, Pb
XRF analysis of analytes in particulates of emissions from two disel fuels with different sulfur content F24
As, Ca, Co, Cd, Cr,
Fe, Ga, Ni, Pb, Pt,
V, Zn
comparison of sample preparation methods using oxygen-plasma ashing on sapphire
carriers and acid digestion for XRF analysis of analytes
F25
Hg silver-coated filter sampling followed by XRF analysis of mercury in flue gases F26
Pb evaluation of portable XRF for the determination of analyte in workplace air F27
Mercury Analysis
analysis of ambient Hg
2+
using KCl-coated denuders followed by TD and cold vapor
atomic fluorescence analysis at detection limit of <3 pg
F28
performance evaluation of a hybrid sampling train for simultaneously sampling and
analysis of Hg and other trace elements
F29
method development and performance for Hg speciation applicable to both fossil fuel
and waste combustion processes
F30
method development and performance evaluation for the sampling and analysis of
reactive gaseous mercury using cold vapor atomic fluorescence analysis
F31
Applications of various chromatographic techniques for the
analysis of inorganic compounds are summarized in Table 5
(F12-F19). X-ray fluorescence instrumentation remains the
method of choice for the determination of trace elements on
aerosols loaded filter or particulate samples because of its
reliability, operational efficiency, portability, and ability to produce
data that can meet different data quality objectives. Table 5
summarizes eight XRF applications for the analysis of metals in
airborne particulates (F20-F27). Mercury continued to be an
important area of environmental air analysis, and five selected
applications are documented in Table 5 (F26, F28-F31). Using
ultraviolet spectrometry, asimple, selective, and sensitive method
was developed for the analysis of lead (F32). A critical evaluation
of three sampling and analytical methods was carried out for the
determination of airborne hexavalent chromium (F33). Long-term
biomonitoring of Ba, Cu, Fe, Mn, Zn, and Pb in Quercusilexleave
and analysis of PM
10
fractions of atmospheric particulate were
performed to determine the main metal pollutants emitted by
vehicles. Results ruled out Baand Zn as valid tracers of automobile
traffic and the phase-out of leaded gasoline has resulted in the
decrease of Pb concentration by 20%/ year (F34). Hlavay
demonstrated the use of sequential leaching for the distribution
of metals as a function of particle size in aerosol samples (F35).
A selective stopped-flow injection method for the spectrophoto-
metric determination of palladium in hydrogenation and automo-
bile exhaust gas converter catalysts was also developed (F36).
Chemometrics and Real-Time Monitoring. This section
emphasizes the development of monitoring methods using optical
instruments such as UV, IR, and laser spectroscopy, mass
spectrometry, and the application of dataprocessing and reduction
methods for the interpretation of monitoring data. Modern
instrumentation, for example, Fourier transform infrared spec-
troscopy (FT-IR) and time-of-flight MS (TOF-MS), is capable of
generating massive amounts of data which can be stored in low-
cost storage devices. The availability of powerful desk top PCs
and graphics software has also revitalized interest in mathematic
processes that allow processing analytical data in an efficient and
consistent manner. With this massive amount of data and many
datainterpretation tools, one can increase not only the confidence
of unknown identification but also data quality. Optical spectros-
copy remote sensing has been greatly benefited from these
developments.
A paper examining the sampling and analytical requirements
for the observation of statistically significant temporal trends of
concentrations of atmospheric SVOCs was published (G1).
Statistical considerations in determining the health significance
of the constituents of air particulate matter were also reported
(G2). Examples of spectroscopic data needs for atmospheric
optical remote sensing to achieve the ultimate accuracy for the
measurement were discussed (G3). Fundamental studies on the
use of dispersion modeling and a differential optical absorption
spectroscopy (DOAS) monitor for improving pollution prevention
procedures (G4), experimental evaluation of a radial beam
geometry for mapping air pollutants using computer tomography
(G5), and the application of dataquality objective process for toxic
emission monitoring around a petroleum refinery using multi-
beam, real-time optical remote sensing (G6) have also been
published.
Optical remote sensing is usually done by FT-IR, DOAS, and
tunable diode laser spectroscopy (TDL). Details of applications
of optical spectroscopy-based remote sensing methods, including
an intercomparison of optical remote sensing systems such as
FT-IR, TDL, and DOAS (G7) were compared. Quality assurance
procedures were described to ensure data quality (G8). General
applications of open-path FT-IR experiment, including a data
reduction algorithm with atmospheric absorption corrections to
remove atmospheric interference to achieve a good background
(G9) and the application of the shifting method as a technique to
correct for the quantitative analysis of open-path FT-IR(G10), were
published. The capability of a portable FT-IRgas analyzer for the
measurements of air toxics in pollution prevention applications
(G11) and the detection of airborne chemical reagents by passive
FT-IR remote sensing (emission measurement) and library
searching (G12) were demonstrated.
Frequency modulation and several signal-processing tech-
niques were described for the enhancement of the signal-to-noise
ratio SNR of open-path FT-IR measurement (G13, G14). The
capability of open-path FT-IR to measure and map air emissions
from volume sources (G15) and emission rate assessments of
industrial area sources during winter conditions (G16) were also
demonstrated. The capability of difference-frequency-based TDL
spectroscopy for the monitoring of atmospheric formaldehyde was
demonstrated with a detection limit of 7.7 ppbv and precision as
low as 0.24 ppbv (G17). Using a TDL spectrometer and a near-IR
laser, Schiff demonstrated the unique ability of the system in
measuring anumber of gases including HCl, C
2
H
2
, HCN, and H
2
S
with low-ppb sensitivity (G18).
Several publications relate to data-processing applications and
real-time measurements using MS equipment. By using a fuzzy
clustering algorithm, a general solution to processing the large
number of mass spectra obtained from on-line monitoring of
aerosols using laser desorption TOF-MS, so the chemical com-
position of particle classes, particle distribution, size distribution,
and time courses can be rationalized, was reported (G19). Using
the multivariate patch algorithm for the analysis of LA-ITMS
spectra obtained from individual airborne microparticles, the
capability for real-time detection and classification of samples was
demonstrated (G20). Details of seven MS-based real-time monitor-
ing applications are summarized in Table 6 (G21-G27). Finally,
on-line monitoring of chromium aerosols in industrial exhaust
streams and real-time monitoring of airborne metals were dem-
onstrated by LIPS(G28) and spark-induced breakdown spectros-
copy (G29).
Automated Analysis. Automated analysis of ambient VOCs
and polar VOCs was developed in the early 1990s to meet the
need of Photochemical Assessment Monitoring Stations (PAMS).
PAMSwas required by the U.S. 1990 Clean Air Act Amendments
(CAAA) for the enhanced monitoring of ozone, oxides of nitrogen
(NO
x
), and VOCs to obtain more comprehensive and representa-
tive data on ozone air pollution. For VOC analysis, PAMS have
been employing automated gas chromatography in 7 24 mode,
producing hourly monitoring data of 56 VOCs and 3 polar VOCs.
The concept of automated analysis has gained wide acceptance
and been applied to different areas of environmental monitoring
programs using various analytical technologies since the last
review in this series. Eleven publications, including PAMS and
continuous emission monitoring, are summarized in Table 7
according to analytes, analytical technologies, and the nature of
the application (H1-H11).
Deposition and Atmospheric Transport. The precision of
precipitation chemistry measurements in the Canadian Air and
Precipitation Monitoring Network was estimated for inorganic ions
such as Na
+
, Ca
2+
, Mg
2+
, and K
+
, to range from 10 to 35%(I1).
Using a benzylhydroxyloxime-based derivatization scheme, a
method was developed for the determination of R-hydroxylcar-
bonyls and -hydroxylcarbonyls and dicarbonyls in snow and rain
samples by GC-FID and GC/ MS instrumentation (I2). A new
method developed for the analysis of volatile and extractable
organohalogen compounds using GC-AES and GC/ MS has led
to the discovery of a compound new to environmental investiga-
tion, dichloronitromethane (I3). The detection of chlorodifluoro-
acetic acid (CDFA) in precipitation was analyzed using GC/ MS
and confirmed by
19
F nuclear magnetic resonance. The possibility
that CDFA was a fluorocarbon degradation byproduct was also
speculated (I4). A new screening method for the speciation of
inorganic lead and alkyllead by GC/ MS in rainwaters was
developed with detection limits of 1-4 ng/ L (I5). The transient
isotachophoresis procedure was developed to resolve the problem
of transition metals comigration during electrokinetic injection
of capillary electrophoresis analysis of trace ions in rainwater (I6).
A new method was developed for the monitoring of methylmer-
cury in rainwater samples using in situ ethylation followed by GC-
atomic fluorescence spectroscopy (GC-AFS) analysis at adetection
limit of 0.32 ng/ L (I7). Using a water surface sampler, concentra-
tions of PAHs were measured for dry deposition and gas exchange
of PAHs at the air-water interface (I8).
IncinerationandMiscellaneous. (A) Incineration. On-line
emission monitoring of PAHs from stack gas using a mobile
resonance-enhanced laser ionization TOF-MS at detection limits
of pptv levels was described (J1). Off-line monitoring of PAH
emissions from domestic activities using LC-FL was also carried
out (J2). High cost is usually associated with the measurement
of dioxins/ furans (hence, toxic equivalent quantity, TEQ) in stack
gas emissions from wasteincineration facilities. As chlorobenzenes
(CBs) may be used as a substitute index to the dioxin TEQ, the
efficiency of a sampling train for the collection and analysis of
CBs was critically evaluated (J3). A multidimensional GC(MDGC)
is capable of separating target compounds from complicated
organic mixtures for an unambiguous qualitative and quantitative
analysis. By operating an MDGC/ MS system under sequential
repetitive heart-cutting mode, the capability of the analytical
system for the characterization of unknown, trace amounts of
organic contaminants in a complex sample matrix was demon-
strated (J4). The capability of an argon/ air ICP-OES doing real-
time analysis of metals in stack gas was demonstrated at detection
limits from 0.1 to 20 g/ dry m
3
(J5).
Table 6. MS Instrumentation-Based Ambient Air Real-Time Monitoring Methods
VOCs requirements, design, calibration, and use of a sampling inlet/ quadrupole
mass spectrometer system for on-line monitoring
G21
paraquat laser desorption/ ionization tandem MSreal-time monitoring of paraquat
on the surface of airborne soil particles
G22
organic aerosols real-time, thermal desorption particle beam MSanalysis of organic aerosols
was demonstrated using tridecanoic acid, 1-tetradecene, and ozone
G23
benzene, toluene, xylenes,
acetone, methyl methacrylate
low-pressure ionization or atmospheric pressure ionization coupled to an
ITMSfor real-time, continuous monitoring of airborne VOCs
G24
PAHs real-time, simultaneous multiphoton ionization and laser-induced fluorescence
analysis at a detection limit of 1 mg/ m
3
G25
VOCs real-time, on-line VOC monitoring using proton-transfer-reaction MSat
detection limits of pptv
G26
atmospheric particles single aerosol particle analysis using transportable laser ionization MS
system and postdata processing to achieve a time course resolution of 1 h
G27
Table 7. Method Development and Applic ations of Automated Analysis
C2-C10 VOCs in situ VOC measurements above a Sierra Nevada ponderosa pine plantation
at 40-min interval over 2 months
H1
carbonyl VOCs solid-phase extraction of air samples followed by elution/ in situ derivatization
using 2,4-dinitrophenylhydrazine and GC/ MSanalysis at detection limits of 2-3 pptv
H2
formaldehyde direct measurement of atmospheric formaldehyde using GC-pulsed discharge
ionization detection at detection limt of 32 pptv using 0.2-L air sample
H3
C
3-C12 VOCs multisorbent sampling followed by flash heating desorption to avoid the use of
cyrofocusing prior to GC analysis
H4
formaldehyde and
acetaldehyde
atmospheric HCHO and CH3CHO sampling using an annular diffusion scrubber,
in situ derivatization using 2,4-dinitrophenylhydrazine, and HPLC-UV analysis
H5
VOCs performance evaluation of an automated GC/ ITMSsystem for field VOC
measurement activities
H6
55 PAMSVOCs PC-based program for the statistical analysis of PAMSdata H7
limonene and
p-cymene
on-line GC/ MSsystem for the monitoring of tracers (limonene and p-cymene) of
odor at g/ m
3
detection limit
H8
C2-C7 VOCs, HCHO,
CH3CHO
on-line automated TD-GC/ MSanalysis of target compounds of biogenic and
anthropogenic sources
H9
particulate-bound
metals
energy-dispersive X-ray-based continuous sampling/ analysis of metals in flue
gas emissions
H10
Pb continuous emission monitoring of Pb using laser-induced breakdown spectroscopy H11
(B) Miscellaneous. With proper calibration, aerosol TOF-MS
is a powerful tool capable of providing not only chemical composi-
tion but also the size of single aerosol particles, thus providing
qualitative description of a single particle. A side-by-side study
on the particle detection efficiency of three aerosol TOF-MS
systems was carried out and compared to colocated, conventional
referencesamplers (J6). Utilizing muramic acid and concentrations
of three fatty acids (C
12:0
, C
14:0
, C
16:0
), a prototype study on the
ability of a GC/ tandem MS system to measure total and viable
airborne bacterial loadings in two different agricultural environ-
ments was reported. Results from GC/ tandem MSwere compared
to conventional culture data and suggested that these two
approaches provided complementary but independent measure-
ment of airborne biopopulation (J7).
Three PIXE methods were developed and applied to the
identification of air pollution sources by single aerosol fingerprints
via a pattern recognition algorithm (J8). The integration of real-
time PIXE and DOAS data and off-line measurement of IC and
ICPMS data was reported to expand the scientific scope of
environmental studies (J9). By combining PIXE and plasma
desorption MS data, the possibility of determining the chemical
compounds with which elements areassociated in aerosol particles
was demonstrated (J10). A quartz crystal microbalance-based
analytical method was developed for the determination of nitro-
aromatics in landfill gas (J11). Finally, the chemical composition
of organic aerosols formed from biogenic hydrocarbon oxidation,
primarily R-pinene ozonolysis, was characterized using atmo-
spheric pressure chemical ionization mass spectrometry (J12).
WATER ANALYSIS APPLICATIONS
In contrast to previous years, this section is organized by order
of steps in the sample analysis process. This organization was
chosen to emphasize the similarity of the techniques used for
analyte determinations in different water matrixes and to facilitate
a discussion of current trends. However, the authors admit that
the dividing lines between sample collection, extraction, separa-
tion, and detection have become blurred as integrated analytical
systems are developed and used for environmental studies. As in
past reviews, we emphasize methods that lead to an understanding
of the environmental concentrations, transport, and fate of trace
pollutants. Responding to the request of the editors to write a
concise and critical review, we have chosen to focus on current
trends and new developments in water analysis. Thus, we do not
include applications of well-established techniques such as liquid-
liquid extraction, gas chromatography coupled with conventional
detectors, liquid chromatography coupled with conventional
detectors, and most references to inductively coupled plasmamass
spectrometry.
SampleCollection. Over the past decade, sampling strategies
have evolved from simply placing water in a bottle to collecting,
and, in the process, concentrating, analytes on an appropriate solid
medium. There are avariety of commercial materials, for example,
graphitized carbons and polystyrene-divinylbenzene resins, avail-
able for the collection of both organic and inorganic analytes. The
advantages of collecting contaminants on solid media include the
ease of transporting the sample to the laboratory and, in many
cases, the increased stabilities of the analytes on the solid medium
compared to an aqueous sample. For example, many insecticides
collected on graphitized carbon black were stable for 2 months
when stored at -20 C(K1). There are increasing uses of passive
samplers and in situ measurements to replace sample collection.
PassiveSamplers. Passive samplers are used to measure time-
averaged concentrations of organic pollutants. Because they are
deployed over long time intervals (days, weeks, or months),
passive samplers more accurately reflect the average conditions
of a water system than grab samples, which might be affected by
short-term fluctuations in analyte concentrations. One type of
passive sampler is a semipermeable membrane device (SPMD).
A SPMD is alipid-filled membranestypically asealed, low-density,
polyethylene tube filled with triolein. SPMDs mimic bioconcen-
tration of analytes in fat tissue and allow the detection of low
concentrations of semivolatile organic compounds. SPMDs were
used to monitor avariety of persistent organic pollutants in rivers
(K2), and in the study of PAHs in groundwater, PAH concentra-
tions of 0.1-100 g/ L were observed (K3). Another type of passive
sampler uses membranes of polysulfone (for the collection of polar
compounds) or polyethylene (for the collection of nonpolar
analytes) to control the accumulation of analytes on aC
18
Empore
disk. Diuron and Irgarol 1051 were collected with this sampler
and measured, at detection limits of 5-10 g/ L, in natural waters;
measured concentrations of diuron and Irgarol 1051 were com-
parable, but slightly lower than, concentrations measured for grab
samples (K4).
InSituMeasurements. Despite the care with which one collects
a sample, there always exists the question of whether the sample
collection process alters analyte concentrations. To alleviate this
concern, the best strategy might be to make in situ, and real-
time, measurements. A membrane probe coupled with MS was
used to characterize and quantify, in real-time, chlorinated and
nonchlorinated hydrocarbons in the subsurface. A detection limit
of 200 g/ L makes this instrument a useful tool for quickly
mapping high concentrations of volatile organic compounds in
groundwater (K5). An in situ sampler, based on a miniature Ag/
Ag
2
S electrode, was used to measure sulfur species in sediment
porewaters. This sensor could be used to map depth versus
concentration profiles of sulfur with submillimeter resolution and
a detection limit for S
2-
of 10
-20
M (K6). To monitor the
composition of porewaters at different depths in a salt marsh,
porewater concentrations of several sulfur species and metal ions
were determined by voltametry (K7).
Extraction and Sample Preparation. Most routine extrac-
tions of organic compounds in water, including many USEPA
methods, are performed by SPE. SPE has, for the most part,
replaced traditional liquid-liquid extraction because of its ease
of use and the fact that it requires much less hazardous solvent
than liquid-liquid extraction. SPE is amenable to automation and
coupling with on-line detection methods; this will be discussed
in detail later. New SPE materials, such as immunosorbents and
molecularly imprinted polymers (MIP) are being used in sample
cleanup. The use of SPME in water analyses has increased
dramatically over the past several years; its contribution to the
field of environmental analysis has been described in a previous
section.
Solid-PhaseExtractionof OrganicCompounds. Results obtained
by liquid-liquid extraction, off-line SPE, and on-line SPE showed
good agreement in an interlaboratory study; SPE disks collected
sufficient quantities of analytes, present at submicrogram per liter
concentrations in water, to allow their identification by GC/ MS
(K8). In addition to exploiting conventional reversed-phase and
ionic interactions in SPE, researchers are using the formation of
ion-pair complexes to extract organic compounds from water.
Linear alkylbenzenesulfonates wereused as acounterion to extract
alkylbenzyldimethylammonium chlorides from water and onto an
octadecyl material; elution, derivatization, and GC/ MSyielded 0.1
g/ L detection limits (K9). Dynamic ion exchange was used to
extract acidic herbicides (recoveries ranging from 50 to 70%) from
water and effectively removed long-chain fatty acids and other
interferences (K10).
Solid-Phase Cleanup with Tailored Materials. Various solid
phases, for example, silica and Florisil, have traditionally been
used to separate interferences from sample extracts. Recently,
antigen-antibody interactions and molecularly imprinted polymers
have been used to specifically retain target analytes, separating
them from interfering compounds. Immunoaffinity extraction was
applied to the analysis of polycyclic aromatic hydrocarbons in
wastewaters and sludges. This cleanup strategy aided in the
identification of polycyclic aromatic hydrocarbons; however,
analyte losses of 50%were observed (K11). Glyphosate and
atrazine were concentrated from water using immunoaffinity
extraction. In this study, only the antibody used for glyphosate
showed compound-specific, rather than class-specific, binding,
recovered 90%of theglyphosateintroduced, and afforded detection
limits of 0.5 g/ L (K12). MIP were synthesized for enrichment
of chlortriazine herbicides. Recoveries for most herbicides were
80%, which allowed detection limits of 50-200 ng/ L (K13). The
use of MIP sorbents in environmental applications is scarce, and
the technique is still under development and not well understood
on afundamental level. The concept of tailoring cleanup materials
to specific compounds is promising. However, at present, both
immunoaffinity and MIP sorbents tend to exhibit class-specific,
rather than analyte-specific, behavior and also show some non-
specific binding interactions with nontarget analytes.
Inorganic Analytes. Large-volume ultrafiltration of more than
1000 L of water was used to concentrate colloid-bound radio-
nuclides; colloidal concentrations of radionuclides from nuclear
power plants were measured, at detection limits of 10 fg/ L, in
water from the Rho ne River (K14). Commercially available SPE
materials for collecting Sr and Tc were used to study Hanford
groundwater; these materials afforded better detection limits than
with standard analytical methods (K15). Commercially available
cartridges used in series were used for a simplified scheme to
extract Pu, Am and Cu, and Sr from apower station effluent (K16).
An anion-exchange resin coupled with an octadecyl hydrophobic
phase was used to extract Se
4+
, Se
6+
, and various organoselenium
compounds from natural waters; this preconcentration permitted
1-900 ng/ L detection limits (K17). A semiautomated procedure
was developed to preconcentrate and determine, with a low-
background proportional counter,
226
Ra in water; a detection limit
of 0.012 Bq was achieved and 3 samples/ h could be processed
(K18). A MnO
2
film on polyamide was used to absorb 80%of
Rapresent in awater sample; high-resolution R-spectrometry was
used to detect 1 Bq/ L (K19). A procedure using MnO
2
to
preconcentrate Pu in 200 L if water prior to separation with aresin
column improved sample throughput to 1 sample/ day (K20).
IntegratedExtractionandDetection. Over the past several
years, there has been an increased use of automated systems that
integrate the extraction, separation, and detection processes. Some
systems, such as thosethat incorporateSPE, areattractivebecause
they reduce workload and permit hands-off operation. Other
systems, for example, those based on membrane extraction, allow
near-real-time analyses.
Membrane Extraction Coupled with Detection. The use of
membranes for the extraction of volatile organic compounds
coupled with mass spectrometric detection is increasing. Mem-
brane extraction is also amenable to field analyses. Membrane
introduction mass spectrometry (MIMS) was successfully used
to detect 100 ng/ L methyl tert-butyl ether in water, with a total
analysis time of 5 min (K21). Because of its rapid response time,
MIMS was used to study chloroform formation during the
chlorination of phenol and di- and trihydroxybenzenes used as
surrogates for humic acids (K22).
Membrane introduction can suffer from low selectivity if there
is no chromatographic separation prior to detection. Membrane
introduction, followed by a quick separation of analytes with a
5-m, capillary, GC column and MS detection allowed the deter-
mination of trihalomethanes in water. Detection limits were
compound dependent and ranged from 2 to 8 ng/ L; 20 samples/ h
could be analyzed (K23). Membrane extraction with a sorbent
interface (MESI), purge and trap, and thermal membrane desorp-
tion (TMDA), all connected to amobile GC/ MS, were compared.
TMDA had the advantages of excluding water from the detection
system, could be operated at a high cycle time, and could detect
a broad range of polar and nonpolar volatile organic compounds;
MESI and purge and trap were amenable to nonpolar volatile
organic compounds only (K24). MESI, coupled with aChrompack
micro-GC system, allowed the detection of less than 1 g/ L
chloroform in tap water (K25). Various membranes and hollow
fibers were investigated for use with a mobile GC system; a
silicone hollow fiber provided the best extraction efficiency for
BTEXcompounds and afforded detection limits of 100 ng/ L (K26).
A flow-through silicone hollow-fiber membrane inlet was devel-
oped for the measurement of semivolatile organic compounds,
including halogenated benzoic acid, halogenated phenols, and
dimethyl sulfoxide, by rapid GC/ MS. Detection limits for this
system ranged from 6 to 500 g/ L (K27).
Automated SPE and Detection. Over the past several years,
there has been an increase in the use of instruments that integrate
sampling, solid-phase extraction, and analyte detection. These
automated instruments are used for the analyses of organic and
inorganic compounds. Recent examples of coupled extraction and
detection systems are described in Table 8.
SeparationandDetection. Mass spectrometry is a standard
tool for the analyses of both organic and inorganic analytes. GC/
MShas long been used by the USEPA and the USGSfor routine
monitoring and environmental surveys of volatile and semivolatile
organic compounds. With the recent availability of rugged,
commercial LC/ MS systems, LC/ MS has also become a more
routine analytical toolsallowing the detection of thermal-labile,
polar, and nonvolatile compounds. LC/ MS instrumentation and
use were recently reviewed (K44, K45). LC/ MSused with toxicity
testing has proven to be a powerful tool in the identification of
toxicants in wastewaters (K46). ICPMSis a standard tool for the
measurement of inorganic compounds. ICPMS detection limits
are sufficiently low that laboratory blanks, and not the instrumen-
tation itself, often determine method detection limits. Because the
use of mass spectrometry in environmental analyses has been
reviewed recently (K47), we will not discuss it here. We will,
instead, describe recent trends in the detection of analytes in
water.
CapillaryElectrophoresis(CE). There continues to be interest
in CE, which provides excellent separation of compounds in
relatively short times (seconds to minutes). A major disadvantage
of CE is the difficulty of interfacing CE, which produces very
narrow chromatographic peaks, with conventional detectors, such
as organic and inorganic mass spectrometers. However, CE has
found several environmental applications. Solid-phase extraction
followed by CE with diode array detection afforded detection limits
of 20-40 g/ L for vinyl sulfone and chlorotriazine dyes in
wastewater (K48). Anilines were derivatized with fluorescamine,
separated with micellar electrokinetic chromatography, and de-
tected by fluorescence detection; the total analysis time was 4 min
and detection limits of 1 g/ L were obtained (K49). CE/ MS, with
detection limits of 0.1-0.1 mg/ L, was used to detect aromatic
sulfonates from wastewater treatment plants (K50).
Time-of-Flight Mass Spectrometry. Because of its high mass
accuracy and the ability to collect a full mass spectrum almost
instantaneously, TOF MS is being explored for use in the
environmental field. Unlike conventional sector or quadrupole MS,
TOF MS does not sequentially scan a mass spectrum. TOF MS
can provide detection limits comparable to those obtained by
selected ion monitoring, while retaining a full mass spectrum for
each analyte. Because it is not a scanning instrument, TOF MS
is compatible with fast GC and CE, both of which produce
extremely narrow chromatographic peaks and are difficult to
interface to conventional MS. GC/ TOF MS, combined with
appropriate extraction methods, provided detection limits of 0.1
g/ L for various organophosphorus pesticides, triazine herbicides,
and PAHs; deconvolution algorithms enabled the calculation of
spectra from overlapping chromatographic peaks (K51). GC
combined with hyperthermal surface ionization/ TOF MS was
developed for use in the detection of PAHs in water; a detection
limit of 1 ng/ L analyte should be achievable with only 5 mL of
water (K52). SPE coupled with surface-assisted laser desorption/
ionization and TOF MS detected low, microgram per liter,
concentrations of phenolic compounds in water (K53). TOF
ICPMS was used to measure 0.5-30 ng/ L Cu, Ni, Sb, Co, Ag,
Cd, Mo In, and Pb in natural waters (K54).
Immunoassays. Immunoassays are desirable tools for the
detection of pollutants because they are easy to use, provide rapid
results, and do not require expensive analytical instrumentation.
However, immunoassays suffer the limitations of cross-reactivity
with nontarget analytes and are only compatible with a limited
number of solvent systems. In an interlaboratory comparison study
with LC/ MS, ELISA proved to be a good screening tool to detect
nonylphenol polyglycol ether (and, presumably other similar
surfactants) spiked in municipal wastewater at 2 mg/ L (K55).
ELISA was used to detect glyphosate (detection limit of 70 g/ L
after sample concentration) in water; however, the glyphosate
metabolite aminomethylphosphonic acid and the herbicide gly-
phosine were found to cross-react with the glyphosate polyclonal
antisera (K56). Immunoassay, with a detection limit of 0.1 g/ L,
was used to detect triazine herbicides in surface waters (K57).
InductivelyCoupledPlasma/ High-ResolutionMassSpectrometry
(ICP/ HRMS). To eliminate interferences, for example, argon
oxides and chlorides, that pose problems at low (unit) mass
resolution, HRMS is being used with ICP. Klaue and Blum
discovered that, while ICP/ HRMS eliminated interferences en-
countered during arsenic analyses, the use of HRMS raised
detection limits to 300 ng/ L. In this study, a hydride generation
sample introduction method used with ICPMS (low resolution)
Table 8. Integrated (and Automated) Extrac tion and Detec tion Systems Used for Analyses of Aqueous Samples
a
detector extraction/ coupling method analyte
sample
size (mL)
DL
(g/ L) ref
GC/ FID open-tubular traps with CP Sil-5 misc organic compds 20-200 0.1-1 K28
GC/ MS PLRP-S pesticides, herbicides 2 <1 K29
LC/ UV various sorbents tested; PLRP-Sand
Hysphere-1 in series was optimal
polar and acidic
organics
40-50 0.001-0.05 K30
LC/ UV or LC/ FL immunosorbents benzidines, PAH 10-20 0.02-5 K31
LC/ fast-scanning FL ion-pair SPE with PLRP-S naphthalenesulfonates 20 0.01-3 K32
LC/ MS ion-pair SPE with PLRP-S naphthalenesulfonates 15 0.05-1 K33
LC/ MS PLRP-S herbicides 100 0.005 K34
LC/ MS/ MS PLRP-S pesticides 10 0.1-10 K35
ICPMS 8-hydroxyquinoline resin Mn, Ni, Cu, Zn, Pb 3 0.0003-0.01 K36
ICPMS retained as pyrrolidinecarbodithioate
complex in PTFE knotted reactor
Fe(II), Fe(III) 2.5 0.08 K37
ICPMS field-flow fractionation 28 elements d50 0.0004-1 K38
ICP-AES retained as diethyldithiocarbamate
complex in knotted reactor
Pb 10 0.2 K39
ET-AAS Chelex-100 and octadecyl silica Cd (speciation studies) 5 0.01 K40
ET-AAS pyrrolidine dithiocarbamate complex
on octadecyl silica
Se (speciation studies) 4 0.005 K41
ET-AAS electrochemical reduction on tungsten Pb 2 0.2 K42
conductometric dialysis coupled with ion
chromatography
Cl
-
, NO3
-
, NO2
-
,
PO4
3-
, SO4
2-
1 5-10 K43
a
AES, atomic emission spectrometer; SPE, solid-phase extraction; DL, detection limit; UV, ultraviolet absorbance detection; ET-AAS, electrothermal
atomic adsorption spectrometer; FL, fluorescence; GC, gas chromatography; FID, flame ionization detection; ICP, inductively coupled plasma; LC,
liquid chromatography; MS, mass spectrometry.
removed argon chlorideinterferenceand improved detection limits
to 0.3 ng/ L; however, only ICP/ HRMS provided reliable quanti-
tation of arsenic concentrations below 1000 ng/ L (K58). The use
of different nebulizers with ICP/ HRMS was studied; the Micro-
Mist nebulizer provided subpicogram per liter detection of
radionuclides (K59). ICP/ HRMS was used to determine V, Cr,
Mn, Fe, Co, Ni, Cu, Zn, Cd, and Pb in seawater; 50 L of sample
and 6 min were required for each analysis (K60). ICP/ HRMSwas
found to be reliable for the determination of Ag, Cd, V, Cr, As,
and Se in 14 mineral waters; using 10 mL of sample, detection
limits ranged from 0.3 to 80 ng/ L (K61). Rh, Pd, and Pt in melted
snow samples from Greenland, Antarctica, and the Alps were
measured by ICP/ HRMS to establish past natural background
concentrations; detection limits ranged from 0.008 to 0.08 ng/ L
and ultraclean laboratory conditions and procedures were adopted
to enable the analyses (K62). ICP/ HRMS was used to measure
boron isotope ratios; these ratios were used to identify anthropo-
genic inputs of boron from detergents (K63).
Miscellaneous Analytical Techniques. Several unconventional
detection techniques have been developed for the determination
of pollutants in water that might eventually be applied to
environmental studies. These techniques are summarized in Table
9.
Analytes of Interest. Over the past few decades, analytes
having acute toxic or carcinogenic effects and that are persistent
in the environment as aresult of anthropogenic activity have been
widely studied. Examples of these compounds include benzene,
lead, polycyclic aromatic hydrocarbons, and chlorinated biphenyls.
While toxic, carcinogenic, and persistent compounds will always
be of concern, the last several years have brought an increased
interest in endocrine disruptorsscompounds that interrupt normal
hormone function and cause adverse biological effects. Endocrine
disruptors might cause adverse affects in living organisms when
present at part-per-trillion concentrations in water. These com-
pounds do not need to be persistent in the environment to cause
damage because they may be continually released into the
environment. Examples of endocrine disruptors are hormones
from birth control pills and surfactants. A review discussing the
origin, occurrence, and effects of endocrine disruptors has been
recently written (K78). Selected analytes of current environmental
interest are shown in Table 10.
SOLID SAMPLE TYPES ANALYSIS APPLICATIONS
Soils and Sediments: Metals. Although we found many
citations concerning the determination of metals in soils and
sediments, fewrepresented real breakthroughs. Theuseof ICPMS
Table 9. Misc ellaneous Tec hniques Developed for the Detec tion of Analytes of Environmental Interest in Water
a
technique application
DL
(g/ L) refs
chemically selective scintillating
microspheres
scintillating microspheres with selective uptake, separation,
and radiometric detection integrated into sensor for
99
Tc(VIII);
applied to analyses of Hanford groundwater
0.01 K64
Cherenkov light
90
Sr measured in 800 mL of groundwater; detection of
Cherenkov light produced when high-energy -particles from
90
Y
passed through sample
10 pCi/ L K65
compound-specific carbon isotope
measurement
determine origin and fate of organic compounds in groundwater
(only standards analyzed) with SPME and GC/ isotope ratio MS
130 K66
diffusive gradients in thin
films (DGT)
developed for in situ measurement of Cu speciation; first direct,
in situ, measurement of both labile inorganic and labile organic
trace metals in natural waters
K67
immunosensor, fluorescence
detection
detection of TNT and RDX; tested at 3 military bases; in general,
results correlated well with LC method; 3 min/ sample
10 K68
LC/ GC/ NPD off-line SPE and on-line LC/ GC (interface based on programmed
temperature vaporizer injector packed with sorbent) for detection
of pesticide residues in spiked river water
<0.001 K69
molecularly imprinted sensor used with fluorescence and mass-sensitive detectors; applied to
polycyclic aromatic hydrocarbons in water
<1 K70
NMRcoupled with LC LC NMRin combination with LC/ MSaided identification of polar,
nonvolatile compounds (review article); detection limits of 5 g on
column; detection limits might improve to 10 ng with future
cryoprobes and new capillary flow-through cells
K71
optical immunosensor coupled
to FIA system
developed to monitor isoproturon in river water; some cross-
reactivity with linuron, diuron, and chlortoluron; 15 min/ assay
0.1 K72
positive thermal ionization
isotope dilution MS
SPE preconcentration of 500 mL of seawater allowed
dimethylthallium to be detected at <0.4-3 ng/ L in the Atlantic
Ocean; this compound is suspected to have a biogenic origin
0.0004 K73
SPE and room-temperature
phosphorimetry
100 mL of water extracted with C
18-bonded silica membranes and
screened for chlorinated dioxins; nondestructive technique;
analysis time is 10 min/ sample
<1 K74
two-step laser MS analysis of carbaryl, phenol, and polycyclic aromatic compounds
in rainwater
1-10 K75
voltammetry on gel-integrated,
microelectrode (GIME) array
developed for determining Cu, Pb, Cd, and Zn speciation; GIME
with square wave anodic stripping voltammety discriminated
between mobile and colloidal metals
0.01 K76
voltammetry with
microfabricated
gold ultramicroelectrode
on-site, As measurement in groundwater using square wave
anodic stripping voltammetry
0.05 K77
a
DL, detection limit; LC, liquid chromatography; SPE, solid-phase extraction; FIA, flow injection analysis; MS, mass spectrometry; SPME,
solid-phase microextraction; GC, gas chromatography; NPD, nitrogen-phosphorus detector.
as the technique of choice for the final analysis has become
widespread, although new methods based on atomic absorption
spectroscopy (AAS) are still reported. Considerable research is
ongoing with respect to the sample preparation steps prior to
ICPMSor AASanalysis. Microwave extraction methods have not
yet achieved their promise of the definitive sample dissolution
technique, but steady progress is being made. A microwave-
assisted method for sample evaporation has been reported, where
analyte losses due to volatilization have been minimized (L1). For
the sample digestion of sediments, Scancar found that significantly
lower results were obtained for Cr, Ni, and Cd when aqua regia
digestion was employed, compared to total acid dissolution and
Table 10. Analytes of Interest in Environmental Waters
a
analyte comment
DL
(ng/ L) ref
anatoxin A SPE, derivatization with fluorenyl methylchloroformate, and
electrospray MS
2 K79
anionic surfactants ditallowdimethylammonium chloride and substitution products determined
by microbore LC/ MSat 0.4-140 g/ L in surface waters
K80
arsenic method for on-site speciation of As; membrane filtration, SPE, and hydride
generation atomic fluorescence detection used
50 K81
cyanazine amide,
cyanazine acid, cyanizine
SPE, LC/ MS; detection of these compounds in groundwater from New York
indicate these compounds leach into groundwater
2-5 K82
disinfection byproducts
(brominated)
MSand IRused to identify DBP in ozonated water treated with secondary
chlorine or chloramine; previously unreported bromo- and
chlorobromopropanones identified
K83
disinfection byproducts
(haloacetic acids)
different analytical methods discussed; electrospray MSprovided
sufficient detection limits to analyze drinking water
70 K84
estrogens partitioning of estrogens between sediment and water studied; synthetic
estrogens were removed more easily from water than natural estrogens
K85
17(-ethynylestradiol,
17
2
-estradiol)
SPE of 25 L of water, conversion to trimethylsilyl derivatives, GC/ MS;
1-13 ng/ L found in wastewater treatment plant effluents
1 K86
17(-ethinyl estradiol,
17
2
-estradiol)
ELISA-detected hormones, at concentrations sufficient to cause
vitellogenesis in fish in municipal wastewater treatment plant effluents;
ELISA had lower detection limits than GC/ MS/ MSand was less
susceptible to matrix interferences
K87
fragrance materials extraction with C18 disk, GC/ MS; wastewater treatment plant influent
concentrations were 0.3-150 g/ L and effluent concentrations
were 0.005-2 g/ L
0.5-40 K88
herbicides SPE with LC/ MSused to determine diuron, Irgarol, and
chlorothalonil in seawater
5 K89
ibuprofen GC/ MSdetected 3000 ng/ L in wastewater treatment plant influents;
8 ng/ L found in rivers and lakes
1 K90
methyl tert-butyl ether purge and trap, GC/ MSin selected ion monitoring mode; no MTBE
detected in old groundwater, <20-1000 ng/ L MTBE measured
in shallow groundwater
20 K91
microcystins collision-induced dissociation to MS
3
afforded tentative identification;
full scan electrospray MSdata could be collected for 250 pg of material
K92
nonylphenol ethoxylates flow injection, atmospheric pressure ionization MSand MS/ MS
methods developed to screen sewage treatment plant effluents
50 K93
nonylphenol ethoxylates
(and metabolites)
reversed-phase LC/ MSused after extraction; metabolite concentrations
of 1-300 ng/ L detected in water from Jamaica Bay, New York
1 K94
nonylphenol ethoxylates 100 L of sample injected, separated with poly(vinyl alcohol) gel
column, and analyzed by electrospray MS
200 K95
perchlorate extraction as ion pair followed by electrospray MS 300 K96
perchlorate direct injection, electrospray MS/ MS; <0.5-35 g/ L perchlorate found
in local groundwaters
500 K97
steroids SPE, derivatization, GC/ MSused to measure steroids in spiked
effluent samples
1 K98
strontium four different methods used to determine
90
Sr in 45 groundwater
samples were compared; detection limits for these methods ranged
from 40 to 150 Bq/ m
3
K99
sulfonamide drugs SPE, LC electrospray MS; detected at 10-100 ng/ L in surface waters
and 10-2000 ng/ L in municipal wastewater treatment plant effluents
200-4000 K100
sulfonated naphthalene-
formaldehyde condensates
(SNFC)
ion-pair SPE, ion pair chromatography, and fluorescence detection;
SNFC ranged from 1 g/ L in groundwater to 200 g/ L in treated effluent
3-8 K101
surfactants 99%of linear alkylbenzenesulfonates and other compounds were
removedduring sewage treatment; concentrations of surfactants in
treated sewage were 5-200 g/ L
K102
technetium
99
Tc biosensor and direct analysis methods reviewed with 53 refs K103
thallium ion-exchange and atomic absorption spectroscopy; contrary to
thermodynamic prediction, Tl(III) was the most dominant form of
Tl in the Great Lakes
0.7 K104
tin preconcentration, derivatization, GC/ ICPMSdetected 1-100 pg/ L Sn
in seawater
0.00001 K105
volatile fatty acids SPME/ GC/ MSapplied to raw sewage; headspace SPME minimized
interferences
2000-6000 K106
a
APEO, alkylphenol ethoxylates; DBP, disinfection byproducts; DL, detection limit; ECD, electron capture detector; GC, gas chromatography;
IR, infrared absorption spectroscopy; LC, liquid chromatography; MS, mass spectrometry; SPE, solid-phase extraction.
acetic acid extraction methods (L2). Another study comparing
various digestion methods found that the mildest method useds
sodium acetateattackswas most effectivein enhancing differences
between polluted and nonpolluted sediments (L3). Microwave
digestion of soils and sediments was found to give better than
80%accuracy for awide group of metals (L4). Ultrasound-assisted
extraction gave a2-fold better precision and better detection limits
compared to microwave-assisted digestion of biological and
sediment samples (L5).
Improved methods for Hg determination continues to be the
subject of great interest. In one novel application, samples of mine
tailings could be analyzed directly for Hg by X-ray absorption
spectroscopy (XAS) if concentrations were 100 ppm or greater
(L6). Speciation data were obtained by comparing XAS spectra
with those from spectral databases. Aqueous distillation is
sometimes used in the determination of monomethyl Hg (MMHg),
even though this technique can result in overestimating concen-
trations because MMHg can be generated from inorganic Hg
during the distillation (L7). This problem can be overcome by
headspace determination of MMHg, but detection limits may not
be as good. Hintelmann also examined the formation of MMHg
during sample preparation and found that artifacts could be
eliminated by leaching using a H
2
SO
4
/ KBr/ CuSO
4
mixture (L8).
By steam distillation of sediments followed by aqueous-phase
derivatization and GC-atomic fluorescence spectroscopy, Bowles
achieved detection levels of 0.01 ng/ g for 1 g of wet sediment
(L9). A rapid field screening method for elemental Hg in soil
samples was reported by Easterling, which involved thermal
desorption of Hg onto gold, followed by thermal desorption from
the gold to a gold film Hg vapor analyzer (L10). Good precision
for the determination of total Hg in solid sample types was
achieved by slurry sampling combined with flow injection-cold
vapor-AAS (L11). Ultrasonic pretreatment of slurries was neces-
sary to improve the low Hg recoveries obtained.
Citations were found for all of the typical metals of environ-
mental interest, but we have selected a few we consider to be
representative of the direction in which the environmental analysis
field is headed. Kingston reported that the Cr in solid samples
can undergo bidirectional transformations between the VI and III
oxidation states during sample preparation and storage (L12). To
correct for this, he developed an isotopic dilution (ID) method
capable of monitoring and correcting for such changes by spiking
samples with a
53
Cr(VI) spike (enriched in
53
Cr) and a
iso
Cr(III)
spike (enriched in
50
Cr). Without the application of spike correc-
tions, biases as high as 163%were observed. An electrothermal
AAS method for total Cr in sediments provided detection limits
from 23 to 45 ng/ L (L13). For the determination of total Sn in
sediments, Yoshinaga found ID-ICPMS to be the most precise,
when combined with alkali fusion sample decomposition (L14).
Prohaska combined GC and HPLC with hydride generation
introduction to ICPMSfor the speciation determination of arsenic
in soil samples (L15). An inexpensive microwave-assisted pro-
cedure for the quantitative determination of inorganic As in soils
employed atomic fluorescence detection (L16). A detection limit
of 0.006 g of As/ g of soil with good precision was obtained.
Extractable As was also determined by slurry sampling-on-line
microwave extraction and hydride generation AAS(L17). Separa-
tion of arsenic species from soil solutions can be performed in
under 5 min by using capillary electrophoresis, with detection
limits of 0.1-0.5 mg/ L (L18). A simple and highly selective
method for trace Pb in environmental samples was reported, based
on selective preconcentration of Pb on amicrocolumn packed with
a macrocycle immobilized on silica gel (L19).
Soils and Sediments: Organics. Hyphenated chromatog-
raphy-mass spectrometry techniques are still the methods of
choice for the determination of trace organic analytes in environ-
mental samples. In fact, many of these methods have reached an
advanced stage of maturity and no real new breakthroughs have
been observed in the past few years. The combination of fast GC
coupled with TOFMS may be one exception to this statement,
and many more applications of fast GC/ TOFMSare expected in
the next few years. Capillary electrophoresis coupled to MS is
another possibly powerful technique that is at an early stage of
development. Comprehensive reviews of recent developments in
environmental MS are given in Table 1. Only a few applications
representative on the current state of the art will be presented
here.
Much work over the past two years was in the area of sample
extraction. A simple, rapid method for extraction of PAHs from
soils, sediments, and air particulates involved the coupling of static
subcritical water extraction with styrene-divinylbenzene extrac-
tion disks (L20). After extraction, sorbent disks can be stored in
autosampler vials with no loss of PAHs, which provides a
convenient method of shipping samples from the field to labora-
tory. Di Corcia used subcritical water (phosphate-buffered) extrac-
tion and a graphitized carbon black cartridge to recover terbuth-
ylazine and its metabolites from soil (L21). In another study,
continuous subcritical water extraction was combined with solid-
phase cleanup/ preconcentration and HPLC separation with post-
column fluorometric detection for the determination of PAHs in
soil (L22). Hot phosphate-buffered water extractions for polar and
medium polar analytes in soil (L23) and subcritical water extrac-
tion followed by sorbent trap for mutiresidue herbicide analysis
(L24) have also been reported. Pressurized liquid extraction,
although a relatively new technique, has rapidly become an
effective and widely accepted extraction method for trace organics
in environmental samples. Ding achieved quantitative extraction
of 4-nonylphenols from sediments with shorter extraction times
and with less solvent use by employing pressurized liquid
extraction, compared to other standard extraction techniques
(L25). A miniaturized pressurized liquid extraction method was
reported by Ramos for PAHs in soils and sediments, where only
100 L total of solvent was needed for a 10-min extraction (L26).
Linear alkylbenzenesulfonates in sediments (L28), PAHs in marine
sediments (L30), and PAHs in contaminated soils (L31) have all
been efficiently recovered by using pressurized liquid extraction.
Yang reported anovel purge-and-trap method where an attenuated
total reflectance flow cell (ATR) was coated with a hydrophobic
polyisobutylene polymer that acted like an SPME phase (L27).
Semivolatiles in soil could be detected by IRin the 200-300 ppb
range. Microwave extractions of under 30 min were found effective
for the determination of PAHs and PCBs in sediments (L29). In
another study using microwave extraction, samples were slurried
in acetoneand passed through themicrowavecavity (L32). Results
were comparable to the standard EPA method for microwave-
assisted extraction but exhibited much improved precision for
replicate samples. Another extraction/ analysis method reported
involved the determination of organics in sediments by on-line
solid-phase extraction-GC/ MS(L34). The authors feel this method
has good potential for use in rapid screening studies.
A variety of mass spectrometry-based techniques werereported
for the determination of trace organic analytes in soils and
sediments. By using real-time aerosol MS, surface-bound PAHs
in petroleum-contaminated soils were determined with no sample
preparation (L33). Priority pollutants were determined by Fuoco
by using on-line supercritical fluid chromatography cleanup-
cryotrap-GC/ MS(L35). Multistep elution from thecleanup column
was possible by addition of a suitable supercritical CO
2
modifier.
Nitro- and oxy-PAHs in soil and air particulates were determined
by ion trap MS and negative chemical ionization (NCI) (L36).
NCIMS was also used for polar herbicides in soils after HPLC
separation and aparticlebeam HPLC-MSinterface(L37). NCIMS
seems to be an ideal method for several important groups of
environmental compounds but has never developed into a wide-
spread technique. The use of electrospray MSwas also reported
for imidazolinone herbicides in soil (L38) and nonylphenol
polyethoxylate surfactants in marine sediments (L39). GC/ MS
methods were found comparable to EPA 418.1 and a rapid field
method for the estimation of total petroleum hydrocarbons in
sediments (L40). The GC/ MSmethod was advantageous because
of its use of internal standard methods. A novel non-MSmethod
for total PCBs in soil by enzyme immunoassay was developed by
Schuetz, who performed the quantitative dechlorination of all
PCBs to biphenyl before ELISA determination (L41).
Sewage Sludge: Metals. Sequential extraction procedures
were compared to single-metal extractions for metals in sewage
sludge samples by Albores (L42). Comparable results were
obtained for both methods, for most metals studied. Solid sampling
electrothermal vaporization ICPMS was used for the direct
determination of Hg in sludge samples (L43). Pretreatment of
samples was limited to drying, sieving, and homogenization, and
1-mg samples were then inserted into a graphite furnace coupled
to ICPMS. More rapid analysis by slurry sample introduction is
of considerable interest, as illustrated by the determination of Pb
and Cd (L44) and Co (L45) in sewage sludge. In both studies,
results for the analysis of reference materials was good. Capillary
electrophoresis was used by Michalke for the speciation deter-
mination of Sb, by interfacing CE to ICPMS(L46). Detection limits
of submicrograms per liter were achieved.
SewageSludge: Organics. Supercritical fluid extraction was
combined with solid-phase extraction for the determination of
bisphenol A in sewage effluent and sludge (L47). With GC/ MS
detection, detection limits were 0.006 g/ L in wastewater and 0.05
g/ g in sludge. SFE was also used by Berset to extract PAHs,
PCBs, and organochlorine pesticides in sewage sludge (L48). SFE
proved to be efficient, fast, and partially selective for this applica-
tion. Analytes of more recent concern in sewage sludge are anionic
and nonionic surfactants, their degradation products, and endocrine-
disrupting compounds. Petrovic reported a broadly applicable
method for all of these compound classes based on LC/ MS(L49).
Less polar compounds were determined by reversed-phase LC/
atmospheric pressure chemical ionization (APCI)-MS (positive
ionization mode), whereas the more polar analytes were deter-
mined by ion-pair LC/ ESI-MS under negative ionization condi-
tions. Crozier reported a rapid screening procedure for nonyl-
phenol ethoxylates in sewage treatment plant samples based on
flow injection LC/ APCI-MS (L50). By using precursor scanning
and multiple reaction monitoring, total nonylphenol ethoxylates
in samples could be detected at concentrations as low as 50 ng/
L. Sewage sludge samples were subjected to immunoaffinity solid-
phase extraction for the trace determination of PAHs by Miege
(L51). Although PAH recoveries were only 50%, the selectivity
of the immunocleanup used resulted in clean extracts that allowed
easier identification and quantitation of PAHs. The problem of
malodorous volatile compounds from digested sludge was inves-
tigated by Winter, who employed purge-and-trap sampling of
liquefied samples followed by GC/ MS (L52). Most of the odor
problem was accounted for by various sulfides, especially dimethyl
trisulfide. Another group of important fragrance compounds in
liquid sewage sludges are the nitro musks. A method using GC/
(ion trap)MS/ MS for nitro musks and their amino metabolites
was reported by Berset (L53).
OrganometallicAnalytes. Although effective methodologies
for the speciation analysis of organometallics in the environment
have been available for the past several years, significantly fewer
citations in this areahave been found for this review. It is possible
that this is one area where analytical technologies are far in front
of regulatory activity, as other compound classes have been
examined in greater detail to date. However, work to advance the
state of the art continues and is focused principally in improving
compound class speciation. Rajendran reported a quantitative
extraction method for trace concentrations of butyl- and phenyltin
in marine sediments (L54). No cleanup of sample extracts was
necessary, because analyses were conducted by using ICPMS.
One study was reported in which interlaboratory testing of butyl-
and phenyltin in sediments was used to determine and eliminate
pitfalls in routine testing (L55). The results were needed as a
precursor for the development of a freshwater sediment certified
for various organotin compounds. Various hyphenated instrumen-
tal methods were applied to the speciation and quantitation of
organometallics in solid sample types including organotins in
marinemussels by GC/ MS(L56), butyl- and phenyltin compounds
in sediments by LC/ ICPMS after pressurized liquid extraction
(L57), and organotins in sediment by HPLC/ (APCI)-MS (L58).
BIOTA ANALYSIS APPLICATIONS
Few advances in the determination of environmental pollutants
in biota have been reported since the last review in this series.
For metals, most reported applications were for the determination
of Hg or Hg species. One novel application reported the use of a
GC capillary cold trap, where Hg speciation was carried out in
the same capillary as was used for the cryogenic trapping (M1).
The advantage of this arrangement was speed; a complete
chromatogram was obtained in 3 min. Rapid, low detection limit
Hg speciation was also reported by Slaets, who coupled multi-
capillary GCwith ICPMSto achieve absolute detection of 0.08 pg
(M2). The signal intensity of Hg for ICPMS detection can be
enhanced as much as a factor of 10 by adding small amounts of
aqueous ammonia, ethylenediamine, or triethanolamine(M3). Sub-
ppt detection limits for methylmercury in fish were reported by
Palmieri, employing amicrowave-induced plasmaatomic emission
spectrometer (M4). By combining capillary zone electrophoresis
separation with ICPMS detection, absolute detection limits of
various Hg species were in the range of a few picograms (M5).
The advantage of the reported instrumental design was that
sample pretreatment of biological samples involves only digestion
and pH adjustment, without the need for derivatization or extrac-
tion. A low-pressure ICPwas operated in atomic and molecular
modes for the selective determination of various Hg species in
sediments (M6). The ICPresponse depended on operation in pure
He at 9-12 W power (atomic mode) and operation at 5 W power
in the presence of areagent gas (methane, isobutane, or ammonia;
molecular mode). Applications for the determination of other
inorganic species in biota included the following: speciation of
As in mussels by LC-UV irradiation-hydride generation-ICPMS
(M7), speciation of As in edible algae by bidimensional size
exclusion anion-exchange HPLC with dual ICPMS and electro-
spray MS/ MS detection (M8), determination of Al in fish by
graphite furnace AASafter pretreatment with microwave-activated
oxygen plasma (M9), and the determination of a range of heavy
metals in low-weight bird feather samples (M10).
Few studies on the determination of organics in biota were
reported. Medium-chain polychloroalkanes were extracted from
fish by pressurized fluid extraction in one investigation (M11).
Analyte detection and quantitation was performed by using GC/
ECNI HRMS. Compound-specific methods for the extraction and
isolation of linear alkylbenzenesulfonate and its metabolites from
fish were reported by Tolls (M12). Matrix solid-phase dispersion
extraction followed by ion-pair liquid-liquid partitioning was found
to be an efficient sample preparation method. Short-chain poly-
chlorinated paraffins in fish were determined by Coelhan (M13),
who used short-column GC/ electron capture negative chemical
ionization MS. Diarrheic shellfish toxins in mussels and phyto-
plankton were determined by Draisci (M14). LC/ MS with ion
spray ionization were used, with both negative and positive
ionization necessary to perform the complete analysis. A new
cleanup method for the removal of lipids from fish extracts was
reported (M15). LCcolumns of 100%poly(divinylbenzene) packing
were found to be effective for the determination of semivolatile
organics in fish.
RADIONUCLIDES
Uranium determination continues to be of significant interest
in environmental samples. Chelation ion chromatography was
used to separate the uranyl ion from matrix interferences in under
10 min (N1). Isotope dilution sector field ICPMS was used as a
rapid method for
230
Th,
234
U, and
235
U in marine sediments (N2).
Sediments with
230
Th/
232
Th ratios of >10
-6
could be quantified.
Ma proposed the determination of U in tree bark as an indicator
of airborne contamination (N3). Reports of the determination of
U in soil and other solid sample types by a laser fluorometric
method (N4) and the low-level detection of U in aqueous solution
by ion chromatography-ICPMS (N5) have also been published.
ICPMSis rapidly becoming the technique of choice for determi-
nation of radionuclides. Methods using ICPMS have also been
published for Th in soil (N6) and
99
Tc in arange of environmental
samples (N7, N8). Another MS-based technology, microwave
induced plasma-MS, was used for
129
I in environmental samples
(N9). Grahek published a method for semiautomated isolation
and detection of
90
Sr from soil samples (N10). The procedure
included leaching Sr from soil by using a water suspension of
Amberlite IR-20 and then separating Sr from other cations with
Amberlite CG-400 or Dowex. Methods reported for specific
radionuclides included Pu in soil using microwave digestion and
anion exchange (N11),
137
Cs in soil by low-level Compton sup-
pression -counting (N12), and
99
Tc in soil by using acombustion
apparatus (N13). Tamborini characterized radioactive soil particles
by using secondary ion mass spectrometry and obtained good
accuracy and precision with a MS resolution of 1000 (N14).
Jerome reviewed one of the difficulties of radiochemical analysiss
the need for chemical yield tracers (N15). The discussion includes
when a yield tracer may be required, which radionuclides could
be used, and the possible sources of such materials. Consistently
high recoveries of the actinide elements from soil and sediment
samples was reported by Kim, based on the ion-exchange resin
Diphonix (N16).
QUALITY ASSURANCE, REFERENCE MATERIALS,
AND RELATED TOPICS
Batley stated that published environmental data frequently
shows no evidence of QA, although such datamay form the basis
of costly management decisions (O1). One of the QA areas that
has improved in recent years is the availability of real-matrix
CRMs. Some new CRMs reported recently include industrial
sludge for the determination of acid-extractable metals (O2), trace
elements in marine macroalgae Fucus (O3), and chlorinated
hydrocarbons in river sediment (O4). Another area of significant
recent interest is the expression of uncertainty in environmental
sample analysis. Kucera discussed the 1993 ISO Guide to the
Expression of Uncertainty as applied to neutron activation analysis
(NAA) and presented an example uncertainty calculation for the
NAA determination of Mn in biological materials (O5). Barwick
has reviewed the sources of uncertainty as applied to GC and
HPLCincludingswhere warrantedsquantitative estimates of their
magnitude (O6). The determination of uncertainty as applied to
ICPMSanalysis (O7) and reference materials (O9) has also been
presented. Tirez published a full uncertainty calculation for the
quantitative determination of native calcium and tracer calcium
(
111
Ca) in soil column effluents by ICPMS (O8).
A quick guide to determine how large sample sizes should be
was published (O10). Schnelle-Kreis studied the variability of
pentachlorophenol in indoor environments and found large varia-
tions in measured valuesson the same order as the measured
values (O11). In a large international round-robin study for
organochlorines and petroleum hydrocarbons in a sediment
reference material, the authors concluded that there still remains
some difficulties with the accurate determination of organics such
as pesticides and PAHs (O12). In another interlaboratory study,
60 laboratories from five countries determined halogenated
hydrocarbons in water (O13). Relative standard deviations of up
to 35%, and outlier rates up to 19%, were observed. Robertson
studied various sampling strategies on load estimated for small
streams (O14). For 1-year studies, fixed-period, monthly sampling
supplemented by storm chasing proved to be the best strategy,
while 2-year or longer studies were best served by fixed-period,
semimonthly sampling. In modern environmental trace analysis,
ultradilute solutions are often utilized as the final sample before
analysis. Such solutions may have an associated high intrinsic
variance that restricts the attainable overall analytical precision
obtainable. This difficulty was discussed by Efstathiou (O15).
BIOMONITORING AND BIOMARKERS
One of the difficulties with environmental chemical analysis
is how to relate results to risk. For example, Vincent obtained
gene-response assay data 10
4
times greater than predicted from
the concentration datafrom chemical analysis (P1). Deciding how
to measure biochemical processes in an ecosystem is a daunting
task reviewed by Heath, especially as this task relates to the study
of urban air basins (P2). Several major reviews on biomonitoring
and biomarkers have appeared over the past two years including
the following: established and developmental biomarkers in
mussels responsive to organic contaminants (P3), biomarker
compounds as source indicators and tracers of air pollution (P4),
algae as biomarkers, bioaccumulators, and toxin producers (P5),
molecular probes and biosensors for bioremediation and site
assessment (P6), the use of bioindicators for monitoring heavy
metals (P7), EROD activity in fish as a biomarker of chemical
exposure (P8), and ongoing efforts in small-scale toxicity testing
(P10). Biological monitors may be necessary for exposure as-
sessment tools because they provide a measure of internal dose
integrated over all routes of exposure. However, relating biological
markers to human exposure is complex. Hoppin has published a
conceptual framework for the interpretation of biological markers
for environmental exposure assessment (P9).
Viarengo discussed the problem of management and inter-
comparison of biomarker dataand proposes aweb site as gateway
to an on-line warehouse for biomarker data(P11). In an extensive
review of USEPA methods for identification of hazards to develop-
ing organisms, one conclusion was that methods that the USEPA
currently depends on to identify the developmental toxicity of
chemicals have limitations that impede obtaining complete and
reliable data on which to base regulatory decisions that protect
children (P12). The zebra mussel was found to be a good
bioindicator for PAH contamination in a harbor (P13). The ratios
of selected thiaarenes, when compared to the ratios in source
samples, enabled identification of vehicular emissions and coal
tar-contaminated sediment as two sources of the PAH contamina-
tion. Beckvar used transplanted freshwater mussels to study Hg
contamination at a contaminated site (P14). Native and trans-
planted mosses were also found to be valuable biomonitors of Hg
contamination around an industrial facility (P15). Dendrochemical
analysis was used to monitor historical changes in soil and
atmospheric trace metals by Watmough, who found that not all
tree species are suitable for this purpose, and careful sampling
strategies must be used (P16). Groundwater systems are espe-
cially difficult to monitor, but theanalysis of microbial communities
appears to be an effective tool to collect information on the
ecological status of groundwater systems (P17). New tools for
monitoring the environment include bioluminescent bioreporter
integrated circuits that use light-emitting microorganisms as
sensors (P18), DNA-based biosensors (P19), guppy sexual
behavior as a biomarker for estrogen mimicking xenobiotics
(P20), and magnetic biomonitoring of roadside tree leaves (P21).
Baun studied the toxicity testing of organic chemicals in ground-
water polluted with landfill leachate and found that the direct
testing of whole samples produced toxic responses, but the
complex sample matrix masked the toxicity of the organic
chemicals of interest (P22). Solid-phase extraction was used on-
site to eliminate interferences and resulted in biotest responses
that reflected the toxicity of the nonvolatile organics in ground-
water. Rahn published a graphical technique based on log-log
plots of selected elemental ratios that was used to resolve four
sources of atmospheric deposition in biomonitors (P23). The effect
of sample storage on sediment toxicity was studied by Cole, who
found the toxicity of both a fine and a silty sand remained
essentially constant during storage from 27 to 83 days (P24).
ACKNOWLEDGMENT
The authors are grateful to Ms Barbara Dworak for her
invaluable assistance in the preparation of the manuscript.
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(K90) Buser, H.-R.; Poiger, T.; Mueller, M. D. Environ. Sci. Technol.
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(K91) Koester, C. J.; Davisson, M. L.; Moran, J. E. Proc.-Water Qual.
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(K93) Plomley, J. B.; Crozier, P. W.; Taguchi, V. Y. J. Chromatogr.,
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(K98) Kelly, C. J. Chromatogr., A 2000, 872 (1-2), 309-314.
(K99) Scarpitta, S.; Oldin-McCabe, J.; Gaschott, R.; Meier, A.; Klug,
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(K100) Hartig, C.; Storm, T.; Jekel, M. J. Chromatogr., A 1999, 854
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SOLID SAMPLE TYPES ANALYSIS APPLICATIONS
Soils and Sediments: Metals
(L1) Link, D. D.; Kingston, H. M. S. Anal. Chem. 2000, 72 (13),
2908-2913.
(L2) Scancar, J.; Milacic, R.; Horvat, M. Water, Air, Soil Pollut.
2000, 118 (1-2), 87-99.
(L3) Adami, G.; Barbieri, P.; Reisenhofer, E. Int. J. Environ. Anal.
Chem. 1999, 75 (3), 251-260.
(L4) Falciani, R.; Novaro, E.; Marchesini, M.; Gucciardi, M. J. Anal.
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(L5) Lima, E. C.; Barbosa, F., Jr.; Krug, F. J.; Silva, M. M.; Vale, M.
G. R. J. Anal. At. Spectrom. 2000, 15 (8), 995-1000.
(L6) Kim, C. S.; Brown, G. E.; Rytuba, J. J. Sci. Total Environ. 2000,
261 (1-3), 157-168.
(L7) Baeyens, W.; Leermakers, M.; Molina, R.; Holsbeek, L.; Joiris,
C. R. Chemosphere1999, 39 (7), 1107-1117.
(L8) Hintelmann, H. Chemosphere1999, 39 (7), 1093-1105.
(L9) Bowles, K. C.; Apte, S. C. Anal. Chim. Acta 2000, 419 (2),
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(L10) Easterling, D. F.; Hovanitz, E. S.; Street, K. W. Anal. Lett. 2000,
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(L11) Rio-Segade, S.; Benedicho, C. J. Anal. At. Spectrom. 1999, 14
(12), 1907-1912.
(L12) Huo, D.; Kingston, H. M. S. Anal. Chem. 2000, 72, 5047-
5054.
(L13) Marques, M. J.; Salvador, A.; Morales-Rubio, A.; de laGuardia,
M. Microchem. J. 1999, 62 (3), 363-370.
(L14) Yoshinaga, J.; Nakama, A.; Takata, K. Analyst (Cambridge, U.
K.) 1999, 124 (3), 257-261.
(L15) Prohaska, T.; Pfeffer, M.; Tulipan, M.; Stingeder, G.; Mentler,
A.; Wenzel, W. W. Fresenius J. Anal. Chem. 1999, 364 (5),
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(L16) Barra, C. M.; Cervera, M. L.; de la Guardia, M.; Santelli, R. E.
Anal. Chim. Acta 2000, 407 (1-2), 155-163.
(L17) Gurleyuk, H.; Tyson, J. F.; Uden, P. C. Spectrochim. Acta Part
B 2000, 55B (7), 935-942.
(L18) Naidu, R.; Smith, J.; McLaren, R. G.; Stevens, D. P.; Sumner.;
M. E.; Jackson, P. E. Soil Sci. Soc. Am. J. 2000, 64(1), 122-
128.
(L19) Yan, X.-P.; Sperling, M.; Welz, B. Anal. Chem. 1999, 71(19),
4216-4222.
Soils and Sediments: Organic s
(L20) Hawthorne, S. B.; Trembley, S.; Moniot, C. L.; Grabanski, C.
B.; Miller, D. J. J. Chromatogr., A 2000, 886(1+2), 237-244.
(L21) Di Corcia, A.; Caracciolo, A. B.; Crescenzi, C.; Giuliano, G.;
Murtas, S.; Samperi, R. Environ. Sci. Technol. 1999, 33, 3271-
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(L22) Fernandez-Perez, V.; Luque de Castro, M. D. J. Chromatogr.,
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(L23) Crescenzi, C.; Di Corcia, A.; Nazzari, M.; Samperi, R. Anal.
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(L24) Cresenzi, C.; DAscenzo, G.; Di Corcia, A.; Nazzari, M.;
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2163.
(L25) Ding, W.-H.; Fann, J. C. H. J. Chromatogr., A 1999, 866 (1),
79-85.
(L26) Ramos, L.; Vreuls, J. J.; Brinkman, U. A. T. J. Chromatogr., A
2000, 891 (2), 275-286.
(L27) Yang, J.; Her, J.-W. Anal. Chem. 1999, 71 (20), 4690-4696.
(L28) Ding, W.-H.; Fann, J. C. H. Anal. Chim. Acta 2000, 408 (1-
2), 291-297.
(L29) Budzinski, H.; Letellier M.; Thompson, S.; LeMenach, K.;
Garrigues, P. Fresenius J. Anal. Chem. 2000, 367 (2), 165-
171.
(L30) Notar, M.; Leskovsek, H. Fresenius J. Anal. Chem. 2000, 366
(8), 846-850.
(L31) Lundstedt, S.; van Bavel, B.; Haglund, P.; Tysklind, M.; Oberg,
L. J. Chromatogr., A 2000, 883 (1+2), 151-162.
(L32) Cresswall, S. L.; Haswell, S. J. Analyst (Cambridge, U. K.)
1999, 124 (9), 1361-1366.
(L33) Rodgers, R. P.; Lazar, A. C.; Reilly, T. A.; Whitten, W. B.;
Ramsey, J. M. Anal. Chem. 2000, 72 (20), 5040-5046.
(L34) Slobodnik, J.; Ramalho, S.; van Baar, B. L. M.; Louter, A. J. H.;
Brinkman, U. A. T. Chemosphere2000, 41 (9), 1469-1478.
(L35) Fuoco, R.; Ceccarini, A.; Onor, M.; Marrara, L. J. Chromatogr.,
A 1999, 846 (1-2), 387-393.
(L36) Niederer, M. Environ. Sci. Pollut. Res. Int. 1998, 5(4), 209-
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(L37) Jimenez, J. J.; Bernal. J. L.; Del Nozal, M. J.; Martin, M. T. J.
AOAC Int. 2000, 83 (3), 756-761.
(L38) Krynitsky, A, J.; Stout, S. J.; Nejad, H.; Cavalier, T. C. J. AOAC
Int. 1999, 82 (4), 956-962.
(L39) Shang, D. Y.; Ikonomou, M. G.; Macdonald, R. W. J. Chro-
matogr., A 1999, 849 (2), 467-482.
(L40) Xie, G.; Barcelona, M. J.; Fang, J. Anal. Chem. 1999, 71 (9),
1899-1904.
(L41) Schuetz, A. J.; Weller, M. G.; Niessner, R. Fresenius J. Anal.
Chem. 1999, 363 (8), 777-782.
Sewage Sludge: Metals
(L42) Albores, A. F.; Cid, B. P.; Gomez, E. F.; Lopez, E. F. Analyst
(Cambridge, U. K.) 2000, 125 (7), 1353-1357.
(L43) Vanhaecke, F.; Gelaude, I.; Moens, L.; Dams. R. Anal. Chim.
Acta 1999, 383 (3), 253-261.
(L44) Lopez-Garcia, I.; Vinas, P.; Arroyo-Cortez, J.; Hernandez-
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732.
(L45) Conte, R. A.; de Loos-Vollebregt, M. T. C. J. Anal. Chem. 2000,
367 (8), 722-726.
(L46) Michalke, B.; Schramel, P. J. Chromatogr., A 1999, 834(1+2),
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Sewage Sludge: Organic s
(L47) Lee, H.-B.; Peart, T. E. J. AOAC Int. 2000, 83 (2), 290-297.
(L48) Berset, J. D.; Holzer, R. J. Chromatogr., A 1999, 852(2), 545-
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(L49) Petrovic, M.; Barcelo, D. Anal. Chem. 2000, ACS ASAP.
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2000, Proc. Bienn. Int. Conf. Monit. Meas. Environ., 3rd 2000,
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(L51) Miege, C.; Bouzige, M.; Nicol, S.; Dugay, J.; Pichon, V.;
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(L52) Winter, P.; Duckham, S. C. Water Sci. Technol. 2000, 41, 73-
80.
(L53) Berset, J.-D.; Bigler, P.; Herren, D. Anal. Chem. 2000, 72,
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Organometallic Analytes
(L54) Rajendran, R. B.; Tao, H.; Nakazato, T.; Miyazaki, A. Analyst
(Cambridge, U. K.) 2000, 125 (10), 1757-1763.
(L55) Ariese, F.; Cofino, W.; Gomez-Ariza, J. L.; Kramer, G.; Quevau-
viller, Ph. J. Environ. Monit. 1999, 1 (2), 191-196.
(L56) Gallina, A.; Magno, F.; Tallandini, L.; Passaler, T.; Caravello,
G. U.; Pastore, P. Rapid Commun. Mass Spectrom. 2000, 14
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(L57) Chiron, S.; Roy, S.; Cottier, R.; Jeannot, R. J. Chromatogr., A
2000, 879 (2), 137-145.
(L58) Rosenberg, E.; Kmetov, V.; Grasserbauer, M. Fresenius J. Anal.
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BIOTA ANALYSIS APPLICATIONS
(M1) Dietz, C.; Madrid, Y.; Camara, C.; Quevauviller, P. Anal. Chem.
2000, 72, 4178-4184.
(M2) Slaets, S.; Adams, F.; Rodriguez, P. I.; Lobinski, R. J. Anal.
At. Spectrom. 1999, 14 (5), 851-857.
(M3) Shuqin, C.; Hangting, C.; Xianjin, Z. J. Anal. At. Spectrom.
1999, 14 (8), 1183-1186.
(M4) Palmieri, H. E. L.; Leonel, L. V. Fresenius J. Anal. Chem.
2000, 366 (5), 466-469.
(M5) Tu, Q.; Qvarnstrom, J.; Frech, W. Analyst (Cambridge, U. K.)
2000, 125 (4), 705-710.
(M6) Rosenkranz, B.; OConnor, G.; Hywel Evans, E. J. Anal. At.
Spectrom. 2000, 15 (1), 7-12.
(M7) Dagnac, T.; Padro, A.; Rubio, R.; Rauret. G. Talanta 1999,
48 (4), 763-772.
(M8) McSheehy, S.; Szpunar, J. J. Anal. At. Spectrom. 2000, 15
(1), 79-87.
(M9) Ranau, R.; Oehlenschlager, J.; Steinhart, H. Fresenius J. Anal.
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(M10) Vallner, J.; Posta, J.; Szep, T.; Braun, M.; Balogh, A.; Kiss, F.
Toxicol. Environ. Chem. 1999, 70 (3-4), 297-304.
(M11) Tomy, G. T.; Stern, G. A. Anal. Chem. 1999, 71, 4860-4865.
(M12) Tolls, J.; Haller, M.; Sijm, D. T. H. M. Anal. Chem. 1999,
71, 5242-5247.
(M13) Coelhan, M. Anal. Chem. 1999, 71 (20), 4498-4505.
(M14) Draisci, R.; Palleschi, L.; Giannetti, L.; Lucentini, L.; James,
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A 1999, 847 (1-2), 213-221.
(M15) Dodo, G. H.; Knight, M. M. J. Chromatogr., A 1999, 859(2),
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RADIONUCLIDES
(N1) Shaw, M. J.; Hill, S. J.; Jones, P.; Nesterenko, P. N. Chro-
matographia 2000, 51 (11/ 12), 695-700.
(N2) Hinrichs, J.; Schnetger, B. Analyst (Cambridge, U.K.) 1999,
124 (6), 927-932.
(N3) Ma, R.; Bellis, D.; McLeod, C. W. Anal. Chem. 2000, 72(20),
4878-4881.
(N4) Premadas, A.; Srivastava, P. K. J. Radioanal. Nucl. Chem.
1999, 242 (1), 23-27.
(N5) Rollin, S.; Eklund, U.-B. J. Chromatogr., A 2000, 884 (1+2),
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(N6) Zbiral, J.; Medek, P.; Kuban, V.; Cizmarova, E.; Nemec, P.
Commun. Soil Sci. Plant Anal. 2000, 31(11-14), 2045-2051.
(N7) Uchida, S.; Tagami, K.; Ruhm, W.; Steiner, M.; Wirth, E. Appl.
Radiat. Isot. 2000, 53 (1-2), 69-73.
(N8) McCartney, M.; Rajendran, K.; Olive, V.; Busby, R. G.;
McDonald, P. J. Anal. At. Spectrom. 1999, 14 (12), 1849-
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(N9) Uezu, Y.; Morita, S.; Nakano, M.; Matanabe, H.; Katagiri, H.
Radioisotapes 2000, 49(3), 136-139.
(N10) Grahek, Z.; Eskinja, I.; Kosutic, K.; Lulic, S.; Kvastek, K. J.
Radioanal. Nucl. Chem. 1999, 241 (3), 617-626.
(N11) Rubio Montero, M. P.; Martin Sanchez, A.; Crespo Vasquez,
M. T.; Gascon Murillo, J. L. Appl. Radiat. Isot. 2000, 53 (1-
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(N12) Iskander, F. Y.; Landsberger, S.; Warren, S. D. J. Radioanal.
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(N14) Tamborini, G.; Betti, M. Mikrochim. Acta 2000, 132 (2-4),
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(N16) Kim, G.; Burnett, W. C.; Horwitz, E. P. Anal. Chem. 2000, 72
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QUALITY ASSURANCE, REFERENCE MATERIALS, AND
RELATED TOPICS
(O1) Batley, G. E. Mar. Pollut. Bull. 1999, 39 (1-12), 23-31.
(O2) Nagourney, S.; Tummillo, N. J.; Birri, J.; Peist, K.; MacDonald,
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(O3) Caroli, S.; Forte, G.; Iamiceli, A. L. Microchem. J. 1999, 62
(2), 244-250.
(O4) Gawlik, B. M.; Martens, D.; Henkelmann, B.; Schramm, K.
W.; Kettrup, A.; Muntau, H. Fresenius J. Anal. Chem. 2000,
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(O5) Kucera, J.; Bode, P.; Stepanek, V. J. Radioanal. Nucl. Chem.
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(O9) Pauwels, J.; Van Der Veen, A.; Lamberty, A.; Schimmel, H.
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(O10) Sheppard, C. C. R. Mar. Pollut. Bull. 1999, 38(6), 439-447.
(O11) Schnelle-Kreis, J.; Scherb, H.; Gebefugi, I.; Kettrup, A. J.
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(O12) Villeneuve, J.-P.; de Mora, S. J.; Cattini, C.; Carvalho, F. P. J.
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BIOMONITORING AND BIOMARKERS
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