&EPA
United States
Environmental Protection
Agency
Industrial Environmental Research EPA-600/7-79-063a
Laboratory February 1979
Research Triangle Park NC 2771 1
Approach to Level 2
Analysis Based on Level 1
Results, MEG Categories
and Compounds, and
Decision Criteria
Interagency
Energy/Environment
R&D Program Report
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RESEARCH REPORTING SERIES
Research reports of the Office of Research and Development, U.S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
gories were established to facilitate further development and application of en-
vironmental technology. Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The nine series are:
1. Environmental Health Effects Research
2. Environmental Protection Technology
3. Ecological Research
4. Environmental Monitoring
5. Socioeconomic Environmental Studies
6. Scientific and Technical Assessment Reports (STAR)
7. Interagency Energy-Environment Research and Development
8. "Special" Reports
9. Miscellaneous Reports
This report has been assigned to the INTERAGENCY ENERGY-ENVIRONMENT
RESEARCH AND DEVELOPMENT series. Reports in this series result from the
effort funded under the 17-agency Federal Energy/Environment Research and
Development Program. These studies relate to EPA's mission to protect the public
health and welfare from adverse effects of pollutants associated with energy sys-
tems. The goal of the Program is to assure the rapid development of domestic
energy supplies in an environmentally-compatible manner by providing the nec-
essary environmental data and control technology. Investigations include analy-
ses of the transport of energy-related pollutants and their health and ecological
effects; assessments of, and development of, control technologies for energy
systems; and integrated assessments of a wide'range of energy-related environ-
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EPA REVIEW NOTICE
This report has been reviewed by the participating Federal Agencies, and approved
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This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161.
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EPA-600/7-79-063a
February 1979
Approach to Level 2 Analysis
Based on Level 1 Results, MEG
Categories and Compounds, and
Decision Criteria
by
LE. Ryan, R.G. Beimer, and R.F. Maddalone
TRW, Inc.
Defense and Space Systems Group
One Space Park - ••
Redondo Beach, California 90278
Contract No. 68-02-2613
Task No. 6
Program Element No. EHE623A
EPA Project Officer: Walter B. Steen
Industrial Environmental Research Laboratory
Office of Energy, Minerals, and Industry
Research Triangle Park, NC 27711
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office of Research and Development
Washington, DC 20460
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SUMMARY
This report has been prepared as a requirement of Contract 68-02-2613,
Task 6 to document a proposed approach for the interpretation of environ-
mental assessment data and identification of additional analytical require-
ments. Volume I describes the general approach to Level 2 analysis and
Volume II, a companion to this document, is the application of the approach
to a set of samples. Addressed are the decision criteria needed to proceed
from the initial emission screening analysis phase (Level 1) to the detailed
emission characterization phase (Level 2) and the Level 2 analytical approach.
This stepwise phased approach to environmental assessment has been shown to
be significantly cost effective compared to a direct approach of obtaining
the needed information by sampling all streams and analyzing them for all
suspected pollutants (1).
In the phased approach to environmental assessment, Level 1 is the
initial survey method by which hazardous streams are distinguished from
those less hazardous or innocuous. Level 1 sampling and analysis have been
designed to generate semiquantitative (±3X) information about the organic
and inorganic elements of interest in the sampled stream so that a dominant
offender does not go undetected (2). This information can then be used to
prioritize the detailed and specific analysis required in Level 2.
The decision criteria developed in this report provide a basis which
can be used for proceeding to a Level 2 emission characterization. However,
this study has been reduced somewhat in scope by limiting the number of
specific pollutants of interest to a chemical correlation with those identi-
fied as the Multimedia Environmental Goals (MEG) (3) compounds as defined by
the EPA and detailed by Research Triangle Institute. The decision criteria
presented here consider only the available Level 1 chemical data. The
contributions from the bioassay results to the choice of Level 2 samples is
not part of this data evaluation. The possibility of negative chemical
results (that in which individual components do not exceed a toxic concen-
tration) occurring with positive biological toxicity is highly probable.
Therefore, consideration by the analysts of the bioassay results is an
important part of a Level 1 environmental assessment and could result in a
iii
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Level 2 effort to detect synergistic agents. In recent environmental assess-
ments (4) the correlation between chemical data and bioassay tests has been
excellent though the entire biological test matrix must be conducted.
Section 2 of this document discusses the types of field samples,
retainable samples, and chemical data avialable from a Level 1 Evironmental
Assessment which can be prioritized for the MEG based Level 2 plan. Retained
Level 1 samples are collected from each of the Source Assessment Sampling
System (SASS) components, either in the form of solids, water samples, or
methylene chloride washings. The samples collected are analyzed either in
the neat or subsequently prepared form. These retained Level 1 samples are
addressed as valid Level 2 samples. Any MEG organic categories or inorganic
elements requiring a Level 2 sampling are discussed and some preliminary
sampling recommendations made. Complete resampling, therefore, becomes
unnecessary under this Level 2 approach, providing the uncertainty in the
Level 1 sampling is tolerable for the required environmental assessment.
A feature of the Level 1 analysis is that the data can be identified by
the analyst when resampling is necessary. This is discussed in Section 4
where a logic flow is presented for establishing the need for a Level 2
sampling effort.
The sampling procedure for Level 1 Environmental Assessment recommends
use of the Source Assessment Sampling System (SASS). This system consists
of the following components:
• 1, 3, and 10 micron particulate cyclones
• Filter
t XAD-2 sorbent trap resin
• XAD-2 sorbent module condensate
t Impingers
t Probe and connecting lines
In the case of a low amount of collected particulate matter all solids may
have been used during Level 1 activities. Therefore, Level 2 analyses can-
not be performed on those neat samples. However, it is possible to proceed
into this Level 2 approach with Level 1 retained prepared samples.
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Section 3 presents the transitional details which start with Level 1
data and arrive at the decision to conduct Level 2 analyses. In this deci-
sion format Level 2 is only required at the specific Level 1 reporting
points containing yg/m^ (yg/fc or yg/g) concentrations which exceed Minimum
Acute Toxicity Effluent (MATE) guidelines. The MEG compounds, decision
criteria MATE, Level 1 reporting points, and generalized Level 2 tests are
presented as usable Level 1 -Level 2 data reduction tables (Appendix A),
Level 1 reporting points are given in Table 2-5 and specifically detailed
in Table A-l. The decision to conduct a Level 2 analysis is then made based
on Level 1 data and MATE concentrations within a specific MEG category.
Section 4 presents decision criteria for Level 2 sampling. If a Level
2 sampling effort is necessary, the SASS may not be the most viable train.
This section, therefore, contains some preliminary suggested Level 2 sam-
pling methods.
In Section 5 an integrated approach to Level 2 inorganic compound
analysis, which is also being developed under Contract 68-02-2165, is pre-
sented. This identification scheme consists of:
• Initial sample characterization, where elemental composition,
sample stability, and bulk morphological structure are
determined.
• Bulk composition characterization, where qualitative and
quantitative am"on, oxidation state, and X-ray diffraction
information are derived.
• Individual particle characterization, where single particle
elemental composition, X-ray diffraction pattern and mor-
phology are measured.
Detailed logic networks are also included to provide direction to the
analyst during the identification process. The analysis of solid and liquid
samples for organic compounds is discussed in Section 6- Combined gas chro-
matography and mass spectrometry is the main technique used to identify
organic compounds in this plan. Direction is provided to the analyst by
means of flow charts and written explanation on such items as:
• Sample size '*
• Mass ranges to be scanned
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• GC columns to be used
• Estimated GC conditions for complete separation
Under EPA Contract 68-02-2150 a procedures manaual (5) is being pre-
pared for Level 2 organic sampling and analysis. It should be referred
to by the Level 2 analyst as a more complete compendium on organic compound
identification methodologies.
The Level 2 approach presented here has been used to access Level 1
data reported by Battelle Columbus Laboratory from run #2 of a 6" Fluidized
Bed Combustor Unit, EPA Contract No. 68-02-1409, Task No. 33. Level 2 anal-
yses of these retained Level 1 samples has been conducted and reported (6)
under EPA Contract No. 68-01-3152, Tasks 2, 3 and 4. The report from this
analytical effort should be referred to for examples of specific method
applications.
VI
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CONTENTS
Summary iii
Figures ix
Tables x
Acknowledgments xi
1. INTRODUCTION 1
2. LEVEL 1 SAMPLES, NATURE OF RETAINED SAMPLES AND
LEVEL 1 DATA 3
2.1 Level 1 Samples 3
2.1.1 Level 1 Home-Site Samples 5
2.2 Nature of Retained Level 1 Samples 10
2.3 Level 1 Data on Home-Site Samples 13
3. MEG CATEGORIES AND COMPOUNDS AT MATE CONCENTRATION AS
DECISION CRITERIA 19
3.1 MEG Categories, Compounds and Elements 19
3.2 MATE Concentrations 20
3.3 Level 1 - Level 2 Data Reduction and Decision
Charts 20
4. SUGGESTED APPROACHES FOR LEVEL 2 SAMPLING AND ON-SITE
ANALYSES 22
4.1 Decision Criteria for Level 2 Sampling 22
4.2 Suggested Level 2 On-Site Tests for Problematic
MEG Compounds 24
5. LEVEL 2 INORGANIC ANALYSES 28
5.1 Inorganic Compound Identification 28
5.2.1 Initial Sample Characterization 29
5.2.2 Bulk Composition Characterization 46
5.2.3 Individual Particle Characterization ... 53
6. LEVEL 2 ANALYSIS OF RETAINED SASS SAMPLES FOR ORGANIC
COMPOUNDS 56
6.1 Hardware Requirements and Options for Level 2
Analysis ^ 57
6.1.1 GC/MS. . . / 57
6.1.2 Chemical lonization (CI) Mass
Spectrometry 58
vii
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CONTENTS (Continued)
6.1.3 Multiple Ion Detection Mass
Spectrometry ............... 59
6.1.4 High Resolution Mass Spectrometry (HRMS). 60
6.1.5 Infrared Spectroscopy .......... 61
6.1.6 High Pressure Liquid Chromatography
(High Resolution Liquid Chromatography,
HPLC) .................. 61
6.1.7 Capillary GC/MS ............. 61
6.2 Sample Preparation and Extraction Procedures .... 62
6.2.1 Probe Wash, Cyclones, and Filter SASS
Train Samples .............. 62
6.2.2 XAD-2 Sorbent Trap ............ 62
6.2.3 Extraction of the Condensate ....... 64
6.3 Analysis of the Extracts for Volatile Components . . 64
6.3.1 GC/MS Analysis of the Probe Wash,
Cyclones, and Filter Extract ....... 64
6.3.2 GC/MS Analysis of the XAD-2 Module
Extract ................. 65
6.3.3 GC/MS Analysis of the Condensate
Extract ................. 66
6.4 Liquid Chroma tographic (LC) Separation ....... 68
6.5 GC/MS Analysis of the LC Fractions ......... 70
6.5.1 Fraction A (1) .............. 70
6.5.2 Fraction B (2 and 3) ........... 71
6.5.3 GC/MS Analysis Fraction C (4 and 5) ... 72
6.5.4 GC/MS Analysis of Fraction D (6 and 7). . 72
6.5.5 GC/MS Analysis of Fraction E (8) ..... 75
6.6 Level 2 Analysis of Water Samples .......... 76
6.6.1 Direct Aqueous Injection GC/MS ...... 76
6.6.2 Purge and Trap Concentration
Technique ................ 78
6.6.3 Extraction of Water Sample for GC/MS
Analysis ................. 79
Appendices
A Level 1 Data Reduction and Decision Charts 80
B Liquid Chromatography Separation Procedure 108
C MEG Organics/Major Mass Peaks Ill
References 151
viii
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FIGURES
Number Page
2-1 SASS Train Schematic 11
2-2 Decision Logic for Phased Level 1-Level 2 Analysis 15
4-1 Decision Logic for Level 2 Sampling 23
5-1 Initial Sample Characterization 31
5-2 Bulk Composition Characterization 33
5-3 Individual Particle Characterization. 35
5-4 Logic Flow Chart for Initial Sample Characterization. ... 36
5-5 Logic Flow for Bulk Composition Characterization 37
5-6 Logic Flow for Individual Particle Characterization .... 38
5-7 Level 2 Liquid Sample Compound Analysis Scheme 39
6-1 General Logic Flow Chart for Level 2 Organic SASS
Component Analysis 63
6-2 Logic Flow Chart for Level 2 Organic Aqueous Samples. ... 77
ix
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TABLES
Number
2-1
2-2
2-3
2-4
4-1
5-1
5-2
5-3
5-4
5-5
6-1
6-2
Level 1 Analytical Categories
MEG Compounds Not Contained in Level 1 Samples
MATE Level 2 Triggering Values for C1-C6
General Level 1 Reporting Points .
Reactive Organic and Inorganic Compounds Capable of
Being Identified by Specific Test Kits (8).
Summary of Recommended Procedures for Anion Analysis ....
Useful IR Bands
Listing of Assigned Infrared Bands Observed in
Particulate Samples
Infrared Bands of Some Common Nitrates (cm" )
Infrared Bands of Some Common Sulfates (cnf )
LC Fraction Blending
Solvents Used in Liquid Chroma tographic Separations
Page
4
6
12
16
26
42
47
48
50
51
69
69
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ACKNOWLEDGMENTS
This document has been prepared under Task 6 of EPA Contract
No. 68-02-2613. The EPA program manager was Mr. Joseph McSorley and the
EPA project officer was Mr. Walter Steen of EPA IERL-RTP. The TRW program
manager was Mr. I. Zuckerman and the task manager was Mrs. Lorraine Ryan.
The Level 2 inorganic procedures discussed in this document are being
developed under EPA Contract 68-02-2165. The project officer on that con-
tract is Mr. Frank Briden, EPA IERL-RTP. Major contributions to the direc-
tion and review of this effort have been provided by several members of the
IERL technical staff particularly Gene Tucker and James Dorsey. In addition
to the principal authors, substantial inputs to individual sections of this
document have been made by Dr. D.G. Ackerman, and Mrs. M.M. Yamada.
Dr. Philip Levins of Arthur D. Little (ADL) contributed to the development
of the Level 1 to Level 2 transition in the organic area sponsored by EPA
under Contract 68-02-2150. Dr. Larry Johnson, EPA IERL-RTP, is the project
officer directing ADL.
XI
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1. INTRODUCTION
This document has been prepared as a requirement of Task 6, Preparation
of a Draft and Final Report on a Level I/Level 2 Analysis Scheme, of EPA
Contract 68-02-2613, Non-Personal Quick Reaction Engineering and Technical
Services. The approach presents a detailed, but preliminary, Environmental
Assessment Plan for characterization of the emissions from an energy process
based on Multimedia Environmental Goal (MEG) organic and inorganic chemical
species. The MEG compounds are potentially hazardous compounds which can
be emitted from a variety of energy conversion processes under certain pro-
cess conditions at concentration levels which could cause an environmental
insult. The emissions characterized by compound class and elemental screen-
ing methods (Level 1) are used to identify those stream samples which may
offer specific pollutant emission problems. The Minimum Acute Toxicity
Effluent (MATE) values are used as the concentration decision criteria for
determining whether additional detailed emission characterization (Level 2)
should be performed. The Level 2 characterization is considerably more
accurate and quantifies specific MEG inorganic and organic compounds. The
v
Level 2 analysis plan presented here is considered to be preliminary because
the information used to test and evaluate the decision criteria was not
based on a recommended Level 1 analysis scheme (e.g.» field test data were
not obtained and provisions for stabilizing the low molecular weight species
were not utilized). The value of the work reported henre is (1) the genera-
tion of a practical reporting format, (2) the logic,.path network to make
decisions for proceeding to Level 2 analysis, and (3) the initial approach
at multimedia Level 2 analysis. Retained Level 1 samples have been the
focal point of the Level 2 approach developed. Level 2 on-site analysis
schemes are recommended for future programs to study the cbmplexity of
on-site volatile and reactive species identification. However, some
approaches to Level 2 on-site compound identification are included as sug1-
gestions to the performing analyst.
The Level 2 analysis of retained Level 1 samples is complex. Deci-
sions requiring analytical expertise follow every Level 2 data generation
effort. Therefore, after each Level 2 analysis step the information
obtained must be evaluated and the list of MEG compounds identified,
quantified, tabulated, and MEG list closure established, the analysis is
1
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continued until an acceptable closure is reached and the total sample
composition is reduced to a list of MEG compounds with their u9/m3 effluents,
This document is based on the currently available MEG and MATE values.
These are both evolving lists and, consequently, the data reduction and
decision tables presented in Appendix A are not fixed.
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2. LEVEL 1 SAMPLES, NATURE OF RETAINED SAMPLES
AND LEVEL 1 DATA
In the phased approach to environmental assessment, Level 1 is the
initial survey method by which hazardous streams are distinguished from
those less hazardous or relatively innocuous. Level 1 sampling and analysis
have been designed to generate semiquantitative (±3X) information about the
organic and inorganic species of interest in the sampled stream so that pol-
lutants do not go undetected. Level 1 data, therefore, consist of identi-
fied organic classes of compounds and inorganic elements. These data can
then be used to prioritize the detailed and specific analysis required in
Level 2.
This section discusses the types of field samples, retained prepared
samples and data available from a Level 1 Environmental Assessment which
can be prioritized for the MEG based Level 2 plan. Retained Level 1 samples
are addressed as valid Level 2 samples. Any MEG organic categories or inor-
ganic elements requiring a Level 2 sampling are discussed. Preliminary
sampling recommendations are made in Section 4. Complete resampling, there-
fore, becomes unnecessary under this Level 2 approach providing the Level 1
sampling effects on quantisation are tolerable for the required environ-
mental assessment.
2.1 LEVEL 1 SAMPLES
Level 1 samples can be separated into two distinct categories based
on where they are analyzed in Level 1. These analytical categories are
designated here as on-site and home-site. Logically the on-site Level 1
samples are reactive and/or volatile and are more suited for real time
analyses. Retention of these materials for complex characterization would
require special sampling equipment or a highly instrumented field laboratory.
The home-site samples can be easily retained. Table 2-1 lists the Level 1
on-site and home-site samples and the MEG categories found in each.
The Level 1 on-site analyses, as listed in Table 2-1, lack specific
tests for some MEG compounds, e.g., ozone and speciation on the C1-C7 cate-
gory' (Section 2.2). The Level 1 home-site samples, although they contain
all MEG categories, do not contain some of the MEG compounds (Section 2.2).
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Table 2-1. Level 1 Analytical Categories
Level 1
General Category
Air
Water
Solids
Level 1
General Category
Air
Water
Solids
On-Site Determinations
• NOx
• C1-C7
• C02, CO, Oe, N2,
H20, S02, H2S
• H2S, S02, COS, CH3SH,
CH3CH2SH, etc.
• Total parti cul ate,
yg/m3 (samples retained)
• PH, acidity, alkalinity,
BOD, COD, dissolved oxy-
gen, conductivity, dis-
solved and suspended
solids, specific anions
(samples retained)
t Total output,
kg/hour (samples
retained)
Home Site Samples
• SASS components
• Retained aqueous sam-
pling, e.g., evapora-
tion pond, cooling
tower, etc.
• Retained bulk solid
samples, e.g., feed
materials, overflow
bed materials, etc.
MEG Category
(Environmental Impact)
47
1, 2, 4, 5, 7, 8, 9,
10, 11, 13, 15, 24,
25, 26
42, 47, 52, 53
13, 53
(Data recorded)
(Data recorded for
general water quality
parameters - most
analyses require
24 hour turnaround)
(Data recorded for
mass emission calcu-
lations and total
particulate emissions)
MEG Categories
(Environmental Impact)
All categories
All categories
All categories
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These home-site samples are fully characterized for inorganic elements and
organic functionality. Level 2 sampling and analysis are, therefore,
required for some MEG compounds (Table 2-2).
2.1.1 Level 1 Home-Site Samples
The home-site emission samples generally consist of a Level 1 catch
taken with the Source Assessment Sampling System (SASS) (shown schematically
in Figure 2-1) consisting of the following components:
t 1, 3, and 1.0 micron particulate cyclones
• Filter
• XAD-2 sorbent trap resin
• XAD-2 sorbent module condensate
t Impingers
• Probe and connecting line washings
These SASS components and the retained water and solid samples can, depend-
ing on the total quantities obtained from the Level 1 sampling effort, be
retained as neat or as Level 1 prepared samples (e.g., in the case of a low
particulate catch where all solids may have been prepared as organic and
inorganic aliquots during Level 1 activities). Level 1 prepared samples
consist of:
1. Inorganic aliquots:
• SASS cyclones, filter particulates and XAD-2 sorbent and
bulk solids dissolved in an acidic media through Parr bomb
combustion over nitric acid
• SASS impingers: H202 and APS (silver catalyzed ammonium
persulfate), diluted to two liters
• Bulk liquid samples: Cooling tower water, feed materials,
etc.
2. Organic aliquots:
• SASS cyclones, filter, particulates and bulk solids
extracted and concentrated in methylene chloride
• SASS XAD-2 sorbent extracted and concentrated in methylene
chloride
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Table 2-2. MEG Compounds Not Contained in Level 1 Samples
Category
Compound
Rationale for Compound Loss
1. ALIPHALIC
HYDROCARBONS
All < C7
On-site analysis is not com-
pound specific. Butadienes,
Pentenes, Cyclohexadiene,
Acetylene, Propyne and Butyne
are reactive.
2. HALOGENATED
ALIPHALIC
HYDROCARBON
• Methyl Iodide
• 1,1,2-Trichloro-
ethane
t Carbon
Tetrachloride
• Methyl bromide
t 1,2-Dichloro-
ethane
• Methyl chloride
• Dichloropropane
• 1,2-Dichloro-l,
2-difluoroethane
t Dichlorodifluoro-
methane
• Trichlorofluoro-
methane
f Bromodichloro-
methane
• Chloroethane
t Dichloropropenes
• 1,1-Dichloro-
ethane
t 1,2-Dichloro-
ethane
On-site analysis is not com-
pound specific. These are
reported as C1-C7 species.
Hexachlorobutadiene and Hexa-
chloroCyclopentadiene are
reactive.
4. HALOGENATED
ETHERS
• Chloromethyl
methyl ether
• 2-Chloroethyl
methyl ether
On-site analysis is not com-
pound specific. Chloromethyl
methyl ether is reactive.
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Table 2-2. MEG Compounds Not Contained In Level 1 Samples (Continued)
Category
5. ALCOHOLS
7. ALDEHYDES,
KEYTONES
8. CARBOXYLIC
• ACIDS
9. NITRILES
10. AMINES
Compound
• 1-Propanol
• Methanol
t Ethanol
• 2-Butanol
• 2-Propanol
• Tertiary
Pentanol
• Acrolein
• Formaldehyde
t Propionaldehyde
• Butyraldehyde
• Acetaldehyde
t 3-Methylbutanol
• Acetone
• Bu tan one
t Methyl
Methacrylate
• 1-Cyanoethane
t Tetramethyl-
succinom'trile
• Butyronitrile
• Benzonitrile
t Acetonitrile
• Butyl amines
• Ethyl ami ne
• 3-Aminopropene
• Ethyl eneinrine
• Dimethylamine
t Diethylamine
• Ethyl methyl -
amine
Rationale for
On-site analysis
pound specific.
On-site analysis
pound specific.
reactive.
Compound Loss
is not corn-
is not com-
Acrolein is
This compound is reactive and
may not be present in its
emitted state.
• „*
On-site analysis
pound specific.
is reactive.
On-site analysis
pound specific.
„
is not com-
1-Cyanoethane
is not com-
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Table 2-2. MEG Compounds Not Contained In Level 1 Samples (Continued)
Category
11. AZO
COMPOUNDS
13. MERCAPTANS,
SULFIDES
15. BENZENE
SUBSTITUTED
BENZENE
17. AROMATIC NITRO
COMPOUNDS
22. FUSED NON-
ALTERNATE
POLYCYCLIC
HYDROCARBONS
24. HETEROCYCLIC
NITROGEN
25. HETEROCYCLIC
SULFUR
'26. ORGANOMETALLICS
42. CARBON
43. SILICON
Compound
All compounds
• Perchloromethyl
Mercaptan
• Benzenthiol
• l-Anthranth1ol
• Methyl Disulfide
• Benzene
• l-Chloro-2-
Nitrobenzene
• l-Chloro-4-
Nitrobenzene
• Dicyclopentadiene
• Furan
• Thiophene
0 Alkyl Mercury
• Tri methyl Arsine
• = CO, Carbonyl
• Si lane
Rationale for Compound Loss
All azo compounds are reactive
and may not be present in
their emitted states.
These compounds are reactive
and may not be present in their
emitted states.
On-site analysis is not com-
pound specific.
These are reactive and may not
be present in their emitted
states.
This is reactive.
On-site analysis is not com-
pound specific.
On-site analysis is not com-
pound specific.
On-site analysis is not com-
pound specific.
Metal carbonyl compounds are
not included in Level 1 on-
site samples. They will be
detected as metallic cations
only.
Not included in Level 1 on-
site samples.
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Table 2-2. MEG Compounds Not Contained In Level 1 Samples (Continued)
Category
Compound
Rationale for Compound Loss
47. NITROGEN
• Hydrazine
Not included iniLevel 1
on-site samples.
48. PHOSPHORUS
t Phosphine
Not included in Level 1
on-site samples. It will be
detected as total P.
49. ARSENIC
• Arsine, AsH,
Not included in Level '1
on-site samples. It will be
detected as total As.
50. ANTIMONY
• Stibine,
Not included in Level 1
on-site samples. It will
detected as total Sb.
be
52. OXYGEN
• Ozone
Not included in Level 1
on-site samples.
53. SULFUR
• Sulfer Dioxide,
so2
• Sulfer Trioxide,
SO,,
SASS metallic composition
catalized S02 indeterminately
to S03, S04. (7) However,
S02 is measured by Field
Gas Chromatograph.
54. SELENIUM
• Hydrogen
Selenide, HpSe
• Carbon
Diselenick, CSe2
Not included in on-site
samples. These are determined
as total Se.
56. FLUORINE
t HF
Not included in on-site
samples. Reactive with SASS,
57. CHLORINE
• C12
• HC1
t COC1,
C12 and COClp not included in
on-site samples. HC1 is
reactive with SASS.
58. BROMINE
t Br2
t HBr
Br2 and HBr are not included in
on-site samples. HBr is
reactive with SASS
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Table 2-2. MEG Compounds Not Contained In Level 1 Samples (Continued)
Category
Compound
Rationale for Compound Loss
59. IODINE
68. CHROMIUM
t I,
Not included in on-site
samples.
• Chromium
Carbonyl,
Cr(CO)c
Not included in on-site
samples. It will be
determined as total Cr.
72. IRON
• Iron Carbonyl,
Fe(CO)5 Fe(CO)9,
Not included in on-site
samples. It will be
determined as total Fe.
76. NICKEL
t Nickel Carbonyl,
Ni(CO)4
Not included in on-site
samples. Decomposed above
50°C and determined as
total Ni.
83. MERCURY
• HgCl
Not included in on-site
samples. It will be
determined as total Hg.
• Bulk liquid samples extracted and concentrated in methylene
chloride
• The subsequent liquid chromatographic aliquots of these
organic extracts
Level 2 environmental assessment can precede from both neat and prepared
Level 1 samples. However, the obtainable Level 2 information will vary
according to the sample's starting condition. Unprepared samples are pre-
ferred. (See the respective inorganic and organic Level 2 analytical
schemes, Sections 5 and 6.)
2.2 NATURE OF RETAINED LEVEL 1 SAMPLES
Level 1 samples retained-for any period of time can undergo species
loss, chemical rearrangement, or surface/interior changes. These can
result from volatilization, decomposition, free radical initiated reactions,
and loss of surface coatings through sample agitation. The extent of these
10
-------
200'C MAX.
"I
1
1 PROBE
11
1 1
1
1
1
CYCLONE
CYCLONE
CYCLONE
Fl
CON
LTER
MNS>
C
ME|—
HjO
OOLIN
(20 -9
n
G
XAD-2
SORBENT
i
IMPINGERS
H-O. APS APS SiC
C-EL"
Figure 2-1. SASS Train Schematic
-------
changes, their kinetics or their effect on the validity of generated Level 2
data are unknown. However, if the samples have been carefully stored (cool,
dark, sealed, limited access storage), they should be reasonably representa-
tive of the site effluents for a period up to six months.
Retained Level 1 samples do not contain some of the MEG compounds of
interest. In some cases they have not been included in the on-site sample
activity; e.g., ozone; or they have reacted with the SASS contruction mate-
rials and are not sampled, e.g., HF; and in other cases, they have been
sampled but altered in composition and their compound origin can no longer
be distinguished, e.g., AsHs. Table 2-2 lists the MEG categories, the com-
pounds in each category not present or distinguishable in retained Level 1
samples, and the rationale for their absence.
Although this listing of MEG compounds not distinguishable or present
in a Level 1 sampling and analysis activity is extensive, it does not
impact the validity of the phased approach. The presence of most of the
listed organic compounds, with the exception of 19 reactive species, is
detectable in the C1-C7 as a total yg/m3 concentration emitted for a specific
boiling point range. If this total quantity exceeds the most toxic MATE
value for that range, then a Level 2 sampling, followed by a compound spe-
cific analytical technique, would be initiated (Section 4). The MATE trig-
gering values for the C1-C7 on-site samples are listed in Table 2-3.
Table 2-3. MATE Level 2 Triggering Values for C1-C6
BOILING POINT RANGE
Cl
C2
C3
C4
C5
C6
MATE VALUE, pg/M3
3.27 x 106
5.31 x 106
3.3 x 102
1.8 x 104
2.5 x 102
3.17 x 10
1
COMPOUND
Methane
Acetylene
Ethyleneimine
Ethyl ami ne
Acrolein
M-Dimethylhydrazine
—
12
-------
The 19 reactive organic compounds are generally dispersed throughout
the MEG categories. Even though these reactive compounds will not be
detected, other nonreactive compounds in these categories will trigger a
Level 2 analysis because of their conservative MATE values. These 19
reactive organic compounds must have specific sampling and analysis systems
designed for Level 2 on-site use. Suggested approaches for Level 2 C1-C7
and reactive organic compounds are presented in Section 4.
Of the inorganic compounds listed, silane, ozone, hydrazine, chlorine
(C12), phosgene (COC1.2), iodine (12). and bromine (8r2) are compounds not
identified by Level 1 on-site sampling analyses and not collected as inor-
ganic elements. The remaining inorganic species are detected in Level 1,
but their emitted compound origin can not be retraced in home-site samples.
If the Level 1 data indicate that a category, e.g., chlorine or antimony,
exceeds the most conservative MATE value for any compound in that category,
then Level 2 on-site activities must design protocol for these listed com-
pounds. Suggested approaches for Level 2 on-site tests for inorganics are
discussed in Section 4.
2.3 LEVEL 1 DATA ON HOME-SITE SAMPLES
In Level 1 methodology the inorganic elements, with the exception of
As, Sb, and Hg are determined by Spark Source Mass Spectroscopy (SSMS).
These data are comprehensive (anion and cation information is present) and
they are determined for all home-site samples. Data are reportable as ug/m3,
yg/1 and ug/g when combined with on-site sample times, flows, and total
catch data. These inorganic elemental values can easily be tabulated and
compared to the MATE concentrations presented in the tables.
In the Level 1 analysis scheme, the samples are apportioned for inor-
ganic and organic analysis. The portions for organic analysis are extracted.
An aliquot is taken for the C7-C12 GC analysis, and one is taken for gravi-
metric and infrared (IR) analyses. If the gravimetric analysis indicates
sufficient concentration of organic material, an aliquot of the extract is
taken so that a minimum of 50 mg of residue results. This residue is then
separated by liquid chromatography (LC). The eight LC fractions are analyzed
by gas chromatography for volatiles and are evaporated for nonvolatiles,"
which are reportable as yg/m3, yg/1 and yg/g and can be compared with MATE
13
-------
values as tabulated in Section 3. If any fraction produces a residue that
is calculated (from the sample size and volume of gas sampled) to exceed
0.5 mg/m3, then a low resolution mass spectra (LRMS) is also obtained. For
the 30 m3 stack sample a fraction weight must exceed 15 mg. Data are then
reduced to yg/m3 for each organic SASS reporting point. The numerical cri-
teria, which would require that a LRMS be conducted, are 0.1 mg/1 for bulk
water samples and 1 mg/kg for bulk solid samples.
A Level 1 IR spectrum is interpreted in terms of the presence of func-
tional groups. That is, the presence of an absorption corresponding to a
carbonyl stretch is taken as indicative of the presence of a carbonyl (cate-
gories 5, 6, 7, and 8) compound. Detection limits vary widely since the
strengths of characteristic absorptions and ionization patterns vary widely
in both the IR and LRMS techniques. Typically, no quantitation is performed.
However, semiquantitative information is obtainable and providing that
detection limits are lower than MATE requirements, MEG categories can be
eliminated from consideration in the Level 2 analysis scheme.
A typical LRMS detection limit is about 1 percent of a 0.1 mg sample.
Thus, about 1 yg of material should be detectable. Again providing that the
detection limit in ug/m3 for the specific MEG category on the specific
instrument in use is lower than the MATE requirements, then specific cate-
gories can be eliminated from Level 2 consideration. A note can be placed
on the Level 1 - Level 2 data presentation table (Appendix A) that the com-
pound was not detectable in the Level 1 IR or LRMS.
The details of Level 1 - Level 2 decision criteria are contained in
Section 3. Generally, any Level 1 reporting point (organic or inorganic)
which exceeds the most conservative MATE concentration value in a given
category will require Level 2 analysis on the particular Level 1 sample
aliquot representative of that reporting point. Figure 2-2 depicts the
Level 1 - Level 2 transition and Table 2-4 lists in general the Level 1
reporting points.
14
-------
LEVEL!
SAMPLES
LEVEL!
ANALYSIS
ON EACH
SAMPLE
LEVEL 1
REPORTING
POINTS
EACHB^
POINT
^ANALYSIS
OF EACH POINT
IN TERMS Of MEG
COMPOUNDS
AND
.MATE
/
EXCEEDS
MATE
LEVEL 2 ANALYSIS
MATE
FINISHED
Figure 2-2. Decision Logic for Phased Level 1-Level 2 Analysis
-------
Table 2-4. General Level 1 Reporting Points
General Level 1
Sample Classes
Level 1
Reporting Point
Inorganics
• SSMS data in yg/m for each element
3
• Hg, As, Sb data in yg/m
Organics
C1-C7 on site in yg/m for each
boiling point range
C7-C12 in yg/m for each boiling
point range
LC1-LC8 in yg/m3 for each MEG
category
LC Fraction
1
MEG Category Present
1. Aliphatic Hydrocarbons (HCs)
2. Halogenated Aliphatic HCs
2, Halogenated Aliphatic HCs
15. Benzene, Substituded Benzene HCs
16. Halogenated Aromatic HCs
21. Fused Aromatic HCs
22. Fused Nonalternate Polycylic HCs
15. Benzene, Substituted Benzene HCs
16. Halogenated Aromatic HCs
21. Fused Aromatic HCs
22. Fused Nonalternate Polycyclic HCs
23. Heterocyclic Nitrogen Compounds
16
-------
Table 2-4. General Level 1 Reporting Points (Continued)
LC Fraction
MEG Category Present
3. Ethers
4. Halogenated Ethers
9. Nitriles
17. Aromatic Nitro Compounds
21. Fused Aromatic HCs
22, Fused Nonalternate Polycyclic HCs
23. Heterocyclic Nitrogen Compounds
25. Heterocyclic Sulfur Compounds
7. Aldehydes, Ketones
9. Nitriles
13. Mercaptans
17. Aromatic Nitro Compounds
18. Phenols
24. Heterocyclic Oxygen Compounds
5. Alcohols
7. Aldehydes, Ketones
8. Carboxylic Acids, Derivatives
9. Nitriles
1Q-. Amines
18. Phenols
19. Halophenols
8. Carboxylic Acids, Derivatives
10. Amines
11. Azo Compounds, Hydrazine Derivatives
17
-------
Table 2-4. General Level 1 Reporting,Points (Continued)
LC Fraction
MEG Category Present
18. Phenols
20. Nitrophenols
8*
8. Carboxylic Acids, Derivatives
14. Sulfuric Acid, Sulfoxides
Recent studies have shown that fraction 8 does not actually contain these
theoretically predicted categories. Sulfuric acid and sulfoxides may not
be removed from the samples by the original extraction process.
18
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3. MEG CATEGORIES AND COMPOUNDS AT MATE CONCENTRATION
AS DECISION CRITERIA
This section presents the transitional details which start with Level 1
data and arrive at the decision to conduct Level 2 analyses. In this deci-
sion format Level 2 is only required at the specific Level 1 reporting
points containing compound concentrations which exceed Minimum Acute Toxi-
city Effluent (MATE) guidelines. The MEG compounds, decision criteria MATE,
Level 1 reporting points and generalized Level 2 tests are presented here
as usable Level 1 -Level 2 data presentation tables.
3.1 MEG CATEGORIES, COMPOUNDS AND ELEMENTS
The Multimedia Environmental Goals (MEG) program concept examines the
pollution potential of fossil fuel conversion processes. The results of
this examination are currently presented in a listing of compounds and ele-
ments associated with coal and oil that could, based on free energies and
the conversion conditions, be liberated to the environment. This is an
evolving data base, changing as more biological data become available.
These data include threshold limit values (TLV), median lethal dose (LDsg);
median lethal concentrations (LCsg), median toxic dose (TDsg), and median
tolerance limit (TLm); and carcinogenic, mutagenic and teratogenic data.
The biological data are then used to determine the elements and compounds
targeted for control technology. The Level 1 environmental assessment
methodology has been designed to identify inorganic elemental composition
and organic compound categories of the sampled stream using the combination
of Spark Source Mass Spectroscopy (SSMS), a sensitive (0.1 ppm) multi-
element analytical technique, and one element specific instrumental tech-
nique for Hg, As, and Sb. Mercury, arsenic, and antimony are volatile spe-
cies with high and indeterminant limits of detection by SSMS. Organic
functional groups are sought using methods such as gas chromatography,
gravimetric analysis, infrared, and mass spectrometry. The inorganic or
organic compounds listed in the MEG charts would not be sought by the Level
1 scheme. However, should an inorganic element or organic class exceed an
EPA concentration guideline, then in the phased approach to environmental
assessment, a Level 2 assessment would be required to identify and quan-
tify the compound forms. Level 2 would be conducted to specifically seek
the MEG compounds.
19
-------
The MEG list provides a guide for the Level 2 analyst. The Level 2
plan developed (Sections 5 and 6) has as its basis the ability to distin-
guish MEG categories in the complex Level 1 samples and the overlapping
Level 1 sample aliquots. The MEG compounds function as a list which the
Level 2 analyst uses to produce analytical standards for verification of
procedures and constantly refers to during the Level 2 analytical effort.
3.2 MATE CONCENTRATIONS
The MEG charts, as originally constructed, do not contain information
on the concentration levels of interest. Concentration guidelines are
necessary for the decision making process. The analyst must know the con-
centration at which Level 1 data trigger the Level 2 activities and the
detection limits for each compound of interest in the Level 2 plan. The
MATE values take into consideration a variety of factors, including the
biological data listed in Section 3.1, half-lives, cumulative tendencies,
and relationships between human and animal toxicity data. The MATE levels
are those permissible for continuous exposure in an ambient media. Levels
exceeding the MATE are, therefore, of environmental concern. MATES will be
refined as more biological data and better models become available.
A decision to conduct a Level 2 analysis can now be made based on
Level 1 data and MATE concentrations and their presences in a specific
MEG category.
3.3 LEVEL 1 - LEVEL 2 DATA REDUCTION AND DECISION CHARTS
The data presented in Table A-l (Appendix A) have been formulated to
function for:
• Level 1 and Level 2 reporting
• Level 2 decision making based on MEG categories, compounds,
and elements at MATE concentrations
t Generalizations on the applicable Level 2 techniques
The table key, which codes the analytical methodology, expectations,
and cost requirements, was meant as a generalization (Sections 5 and 6 con-
tain the specific technical analytical information). For example, GC/MS
is the chosen analytical technique for all the organic categories; pre-
treatment, volume, GC conditions, and MS detection technique are details
20
-------
not meant to be part of the table key. An inorganic Level 2 Test Method
example would be for soluble Fe where 1-C,A would indicate extraction (C)
followed by AAS (A); another 1-C for arsenic would indicate a colorimetric
determination for total As. These tables have been constructed to stand
alone as decision guidelines in the Level 1 — Level 2 approach based on
MEG and MATE. They list MEG compounds with their MATE in order of decreasing
toxicity in each of the MEG categories, where in the Level 1 data the MEG
compound of interest is found, the ratio of the specific Level 1 concentra-
tion to MATE value, if Level 2 is required, and generalizations on the
applicable Level 2 methodology. A decision to conduct Level 2 tests for a
specific MEG category is triggered if the Level 1 report point exceeds the
most toxic MATE for that category. Level 1 bibassay results are not consi-
dered in this decision format.
21
-------
4. SUGGESTED APPROACHES FOR LEVEL 2 SAMPLING AND ON-SITE ANALYSES
This section contains suggested Level 2 on-site tests for the
problematic MEG compounds listed in Table H-2. These are suggested as
starting points only. Where Level 1 data have clearly indicated the require-
ment for Level 2 sampling and analysis then a specific sampling and analy-
tical plan must be generated. In the on-site Level 2 plan specific hard-
ware (e.g., all glass sampling systems, organic impinger systems, inorganic
glass impingers, and particulate samplers, etc.) is to be taken back to the
field along with compound specific test apparatus (e.g., nondispersive
infrared analyzers, NDIR). The planning activity at that time should in-
clude specific analysis techniques and the laboratory backup, checkout and
supportive data, e.g., the details of the total sample required for a suc-
cessful Level 2 test.
4.1 DECISION CRITERIA FOR LEVEL 2 SAMPLING
Figure 4-1 presents a decision flow diagram to be implemented after
conducting the Level 1 environmental assessment and before proceeding onto
a Level 2 sampling and analysis effort. It addresses the questions the
analysts must answer before establishing that the already acquired Level 1
samples are valid for Level 2. It has been designed to be a cost effective
approach requiring Level 2 sampling only to acquire those data necessary for
a reasonable environmental assessment. Complete resampling is not necessary.
The first criterion examines the integrity of the Level 1 tests and
gathered samples. The Level 1 sampling team, home-site analytical crew,
and project monitor evaluate the quality of the Level 1 samples and gene-
rated analytical data. In some cases repeat Level 1 tests would be more
appropriate. Questions to be asked at this evaluation point would be:
• Was the Level 1 test statistically representative of site
operating conditions?
t Has operator or instrumental error resulted in any suspect
samples or data?
• Was the Level 1 representative of others conducted at similar
industries and under similar conditions?
22
-------
LEVEL I
ENVIRONMENTAL
ASSESSMENT
ASSESSMENT OF
LEVEL I SAMPLING
AND ANALYTICAL
QUALITY
DID
LEVEL I PROVIDE
ADEQUATE EFFLUENT
CHARACTERIZATION
SPECIFIC EQUIPMENT
AND PROCEDURES
LIST Of COMPOUNDS
EXCEEDING MATES
IS
LEVEL 2
SAMPLING REQUIRED
ASSESSMENT OF LEVEL 2
DETECTABILITY FOR EACH
INDICATED MEG COMPOUND
IS
SUFFICIENT
SAMPLE PRESENT
F0« LEVEL 2
ANALYSIS
CONDUCT LEVEL 2
COMPOUND
IDENTIFICATION
VEAL
COMPOUNDS
EXCEEDING MATES
KEN FOUND ?
(CLOSURE TO
LEVEL 1)
LEVEL 2
ENVIRONMENTAL
ASSESSMENT
COMPLETED
REASSESSMENT OF SAMPLE
INTEGRITY AND LEVEL 1 DATA
IS
THE LEVEL I
DATA CLOSURE
RESOLVABLE
WITH SAMPLING
AND ANALYTICA
NCE8TAINTY
IS
LEVEL I
SAMPLE ADEQUATE
IN LIGHT OF LEVEL 2
OBTAINED
DATA
'LIST OF LEVEL 2 MEG
COMPOUNDS EXCEEDING
MATES AT LEVEL 2
DETERMINED
CONCENTRATIONS
LEVEL 2
ENVIRONMENTAL
ASSESSMENT
COMPLETED
r
•~i
KEY FOR
SPECIFIC
QUESTIONS:
YES ANSWERS TRIGGER LEVEL 2 SAMPLING
• ARE VOLATILE/REACTIVE ORGANICS OR
INORGANICS INDICATED?
. IS THERE A MORE EFFICIENT TRAIN THAN
THE 5ASS FOR SITE AND SPECIES
INDICATED?
• ARE FURTHER GENERAL SAMPLING
E.A. MORE PARTICULATE FRACTION,
COMPOSITE WATER SAMPLES ETC.
NECESSARY TO DEFINE EFFLUENT?
I J
Figure 4-1. Decision Logic for Level 2 Sampling
23
-------
After this data validation step, the assessment of the Level 1 chemical
results can be conducted according to the decision criteria presented in
Section 3 and contained on the appended Level 1 - Level 2 transition tables.
Once the probable MEG compound list has been generated, Level 2 sampling
requirements' are clearly discernible. For example, only volatile organic
compounds (-160°C to + 100°C, the C1-C6 compounds) may require Level 2
identification and quantisation and the entire Level 2 effort would consist
of a grab gas sampling followed by gas chromatography/mass spectrometry.
In many cases the Level 1 samples will be suitable for the Level 2 program.
Specific questions are given on Figure 4-1. When the quantity remaining
may not be sufficient, then a Level 1 sampling, if less costly, can provide
acceptable Level 2 samples. The analyst then follows the analytical
approaches given in Sections 5 and 6. As each MEG compound triggered by
Level 1 is identified and quantified, closure to the Level 1 data is
checked. When successful agreement is obtained, the Level 2 assessment is
completed. Some conjectural problems which the analyst could face in
obtaining a reasonable closure to Level I involve the sample's integrity
(storage changes, e.g., contamination, loses, surface oxidation) and the
Level 1 uncertainty factor(quantitation factor ±3X, e.g., some inorganic
elements are less reliably quantitied by the Level 1 SSMS) • If the sample
is contaminated to the extent that the Level 2 data obtained are scrambled,
then Level 2 sampling for a higher quality sample may be more reasonable
and cost effective than the identification of the interfering species.
Where quantitation is problematic and multiple analyses by complimentary
techniques have not resolved the closure problem, Level 2 resampling can.
By employing a more efficient sampling system for the species of interest
followed by the most precise analytical techniques, the analyst will resolve
effluent quantitation problems. The Level 2 environmental assessment can
then be reliably completed.
4,2 SUGGESTED LEVEL 2 ON-SITE TESTS FOR PROBLEMATIC MEG COMPOUNDS
The problematic MEG compounds not retained in Level 1 samples are sum-
marized as follows:
• C1-C6 compounds, e.g., methane
• Reactive organic and inorganic compounds, e.g., acrolein and
hydrogen fluoride
24
-------
t Volatile inorganic compounds, e.g., phosgene
t Sampled but altered inorganic compounds, e.g., stibine
Two suggested approaches exist for C1-C6 nonreactive hydrocarbon com-
pounds and both are complimentary:
1. Integrated Tedlar bag (glass or stainless steel sample bomb)
for Level 2 resampling
• Collect 10 liter bag sample
t Concentrate (condense) 0.1 - 1.0 liter in laboratory
t Conduct Gas Chromatography/Mass Spectrometry (GC/MS)
using: a) 6 ft ss, Poropak Q
b) 3 percent OV-101 on Chromasorb W-AW-DMCS
c) any suitable column optimized for separation
of categories 1 and 2 specifically
2. Solid absorbent method
• Collect several 0.1 and 1.0 liter samples on a solid
absorbent capable of being thermally desorbed, e.g., Tenax
t Thermally desorb
• Conduct GC/MS using columns suggested above
Nonreactive compounds detected in the C1-C6 range are best analyzed by
direct GC/MS. Samples will need to be collected specifically for this pur-
pose and shipment and storage should not exceed 24 hours. Two alternatives
are available for these materials, and it is not possible to state a prefer-
ence for one or the other at this time. (Gas sample bags and stainless
steel bombs have been successfully used for direct GC/MS analysis on EPA
Contract No. 68-02-2197.) A gas sample may be collected in a 10-liter bag
and returned to the laboratory where 0.1-1.0 liter of the sample can be
condensed (concentrated) in a manner similar to the Kaiser tube approach
and then introduced into the GC/MS for analysis. Alternatively, several
0.1 and 1.0 liter samples can be collected on Tenax and returned to the
laboratory for thermal desorption and GC/MS. This latter approach is
attractive in terms of the analysis, but it is uncertain as to whether the
Tenax trap is capable of retaining all of the volatile species in the C1-C6
range. Therefore, these methods are recommended as concurrent efforts.
n
25
-------
The reactive organic compounds are best analyzed on-site as they are
emitted. Some reasonable simple tests kits are available for preliminary
screening during the Level 1 effort. MEG category 1 reactive compounds may
also be detected in the integrated bag sample. Table 4-1 lists some reactive
organic and inorganic gases which can be sampled and analyzed by use of
Mine Safety Appliances (MSA) or other test kits and their range of detec-
tion. Although this is not a recommended Level 2 analysis method, it can
indicate if these compounds should be considered for a more suitable Level 2
analytical method, e.g., NDIR. Judgment must be exercised with the use of
these predesigned systems and interferences, reliability, and detection
limits and conversion to yg/m^ volumes made for each kit used.
Table 4-1. Reactive Organic and Inorganic Compounds
Capable of Being Identified by Specific Test Kits (8)
Compound
Acetylene
Hydra zine
Mercaptans
Butanethiol
Phosphine
Arsine
Stibin
Ozone
Sulfur Dioxide
Hydrogen Fluoride
Chlorine
Hydrogen Chloride
Phosgene
Bromi ne
Mercury
Category
1
11 & 47
13
13
48
49
50
52
53
56
57
57
57
58
83
Detection Range (PPM)
3-600
0.5-20
0.5-100
0.5-100
0.025-10
0.025-10
0.025-1.0
0.05-5.0
1-400
0.5-5.0
0.5-20
2-250
0.1-10
5-75
0.5-2.0
26
-------
NDIR (or remote FTIR which is now under development) techniques are
applicable to metal carbonyls (categories 42, 68, 72, and 76), silane (cate-
gory 43) and halide gases (categories 56, 57, and 58). Identification of
interferences, gas conditioning requirements, and sensitivity must be
assessed in the presite activities for these techniques.
Tests for the reactive organic compounds cannot be discussed in gen-
eralized terms. In the phased approach, when a category is implicated, a
presite literature search, choice of analytical method and presite analy-
tical checkout should be conducted. In these cases, as well as some inor-
ganic areas, EPA literature and the Federal Register may contain specific
test methods.
27
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5. LEVEL 2 INORGANIC ANALYSES
Samples for Level 2 analysis may have either been retained from previous
Level 1 analyses, or are new samples that have been obtained specifically
in a Level 2 sampling effort. In general, the sampling systems used produce
particulate matter samples from probe, cyclones, probe washings, filters,
impingers, and the gas conditioner module and module condensate. Additional
organic or inorganic solids, such as feed materials, both solid and liquid
portions of slurries, and liquids — including leachates of selected solids,
are also possible Level 2 samples.
Level 2 inorganic analysis is primarily concerned with compound iden-
tification and consequently the emphasis is placed on the analysis of solid
materials. Analysis of liquid samples for inorganic material is concerned
with the precise elemental composition, oxidation state of free or com-
plexed elements, and the anion content of the sample. The following sec-
tions discuss the preparation, analysis, and correlation of data for Level
2 inorganic analysis. The approach presented here has been under develop-
ment on EPA contract 68-02-2165. Preliminary details were applied and
further expanded for this presentation.
5.1 INORGANIC COMPOUND IDENTIFICATION
The analysis of inorganic compounds requires the coordinated use of a
variety of analytical techniques. Some techniques, such as XRD, TEM-SAED
and ESCA, have the potential for direct compound identification, but only
for selected compounds. The approaches described in Figures 5-1 through
5-3 are of increasing analytical complexity, designed to be cost and time
effective. The identification scheme consists of:
t Initial Sample Characterization - elemental composition, sam-
ple stability, and bulk morphological structure are deter-
mined.
• Bulk Composition Characterizations —qualitative and quanti-
tative anion, oxidation state, and X-ray diffraction infor-
mation are derived.
• Individual Particle Characterization — single particle ele-
mental composition, X-ray diffraction pattern and morphology
are measured.
28
-------
The degree to which each method can be applied will vary considerably
with the experience, sample quantity and equipment available to the analyst,
It is recommended that continued use of any one method be evaluated in
light of the information derived. In general, it is far better to use a
variety of instruments operated in the most efficient manner rather than
pushing a single instrument or technique to the limit of its capabilities.
Figures 5-4 through 5-6 describe a logic path for identification of
inorganic compounds in a solid matrix using the methods from Figure 5-1.
A similar approach for liquid samples is described in Figure 5-7. In both
approaches emphasis is placed on reaching an accurate closure to the MEG
compounds which exceed MATE values. After a method or series of methods
has been applied, a comparison is made of lists of identified to potential
MEG compounds for elements which exceed their MATE values. A satisfactory
analysis will depend upon a variety of factors:
• Number of compounds identified versus MEG compounds exceeding
MATE values
• Interest in identifying the remaining compounds for those ele-
ments that have exceeded MATE values
t Cost/availability of necessary equipment
The analyst must decide what method will be applied and how much more infor-
mation can be obtained by each additional analysis. In many cases some
methods can be bypassed because of results from previous tests, e.g., quan-
titative anion analysis may provide sufficient information and FTIR would
only be repetitious. In other cases efforts may direct the analyst to a
specific method when it would be best to analyze for a given compound. The
following sections provide a discussion of the proposed methodology and
information derived. By understanding the output from each technique, the
analyst will be better able to select the appropriate combination of tech-
niques to determine the compounds present in the environmental sample of
interest.
5.2.1 Initial Sample Characterization
Initially, information from all sources (Level 1 field and analytical
data) concerning the composition of the sample is pooled, assessed, and
29
-------
ANALYSIS PROCEDURE FLOW
PRINCIPLE OF OPERATION
LEVEL 1 SPARK SOURCE
MASS SPECTROMETRY
(SSMS) DATA
i
1
THERMOORAVIMETRIC
ANALYSIS (TGA)/
DIFFERENTIAL
SCANNING
CALORIMETER (DSC)
r
POLARIZED LIGHT
MICROSCOPE (PLM)
t MICRO-SOLUBILITY
* TESTS
/ANALYSIS
\ CHARACTI
ATOMIC ABSORPTION
/ SPECTROSCOPY (AAS)
; y i
•
^^"^v QUANTITATIVE
CONTINUES \ CATION
OMPOSITION 1 ANALYSIS
RF POTENTIAL USED TO BREAKDOWN SAMPLE PLACED IN
TWO ELECTRODES
RESULTANT IONS ACCELERATED OUT OF SOURCE THROUGH
ELECTROSTATIC AND ELECTROMAGNETIC ANALYZERS
(SIMILAR TO ORGANIC MASS SPECTROMETRY)
DETERMINE MASS DISTRIBUTION IN RESULTANT ION
BEAM. USE DETECTION SYSTEM THAT PROVIDES REQUIRED
SENSITIVITY AND PRECISION
• PHOTOGRAPHIC PLATE SYSTEM. USED FOR TOTAL
CHARACTERIZATION OF SAMPLE SINCE ENTIRE
PERIODIC TABLE IS EXAMINED AND POSSIBLE
INTERFERRING IONS ARE RESOLVED
• ELECTRICAL DETECTION SYSTEM. GOOD FOR SINGLE
ELEMENT DETERMINATION
TGA RECORDS WEIGHT LOSS OR GAIN AS MATERIAL
IS HEATED
DSC MEASURES HEAT EVOLVED OR ABSORBED AS SAMPLE
IS HEATED
PARTICLES ARE COLLECTED FROM VARIOUS SOURCES,
CRUSHED TO 0.05 MM, AND EXAMINED WITH MICRO-
SCOPE. OF SPECIAL IMPORTANCE ARE OBSERVATIONS
OF:
• REFRACTIVE INDEX (RELIEF)
• ISOTROPY OR ANISOTSOPY
• BIREFRINGENCE
• PIEOCHROISM
• FRACTURE
• COLOR
• CRYSTAL HABIT
VIEW SMALL AMOUNTS OF SAMPLE UNDER HM WHILE
ADDING COLD WATER, HOT WATER, DILUTE HCI, AND
DILUTE BICARBONATE SOLUTIONS
RECORD INFORMATION ON INDIVIDUAL PARTICLE
SOLUBILITIES
ISOLATE SINGLE PARTICLES ON STAGE OF PLM:
• MICRO-SPOT TEST FOR SPECIFIC ANIONS
(soj, NOj, NO;;, coj, cr>
• COMPARE TO QUANTITATIVE STANDARDS
INTRODUCE SAMPLE INTO AAS AND DECOMPOSE WITH
30
-------
INFORMATION DERIVED
COMPOUND IDENTIFICATION PROCEDURE
LIMITATIONS
PROVIDES ELEMENTAL CONCENTRATION DATA ON ELE-
ME NTS
CAN DETERMINE 1RACE ELEMENTS IN QUANTITIES AS
LOW AS 0.01 PPM
ABSOLUTE SENSITIVITIES RANGE FROM 1 THROUGH 400 NO
NEED ELEMENTAL DISTRIBUTION DATA TO REDUCE
COMPOUND CHOICES
ELEMENTAL INFORMATION ESPECIALLY USEFUL IN
INTERPRETING IR AND XRD DATA
ACCURACY OF ANALYSIS TYPICALLY 100 TO 500%.
IF ONLY LEVEL 1 DATA IS USED, COULD ALLOW A
YES OR NO ANSWER TO THE PRESENCE OF POSSIBLE
COMPOUNDS
TGA PROVIDES SPECIFIC INFORMATION ON THERMAL
STABILITY OF SAMPLE; WEIGHT LOSS CAN SOMETIMES
BE CORRELATED WITH DECOMPOSITION Of SPECIFIC
COMPOUNDS
DSC DATA GIVES INFORMATION ON PHASE TRANSITIONS
OR CHEMICAL REACTIONS IN SAMPLE
TGA/DSC NORMALLY CANNOT DETERMINE COMPOUNDS
PRESENT IN COMPLEX MIXTURES WITHOUT INFORMATION
ON ELEMENTAL AND ANION COMPOSITION
PRIMARY USE IN THIS IDENTIFICATION SCHEME IS TO
PROVIDE STABLE DRYING TEMPERATURES AND IDENTIFY
ANY REACTIVE OR VOLATILE MATERIALS PRESENT
SINCE SMALL SAMPLE SIZES ARE NORMALLY USED,
CHEMICAL STABILITY OF LOW CONCENTRATION
MATERIALS IS NOT SEEN
THE MAXIMUM TEMPERATURE OF MOST INSTRUMENTS
IS 1000-C, WHICH IS BELOW DECOMPOSITION POINT
OF MANY COMPOUNDS
AT LOW MAGNIFICATION, GENERAL APPEARANCE OF
SAMPLE IS NOTED FOR QUALITY CONTROL OF SAMPLE
HANDLING/STORAGE
AT HIGHER MAGNIFICATION, CRYSTAL STRUCTURE,
COLOR, REFRACTIVE INDEX ARE MEASURED FOR
SINGLE PARTICLES
INITIAL VIEW INDICATES MINIMUM NUMBER OF DIFFER-
ENT PARTICLES AND THEIR POTENTIAL COMPOUNDS
ALL CRYSTALLINE COMPOUNDS HAVE SPECIFIC REFRACTIVE
INDEXES WHICH CAN BE USED TO IDENTIFY THE COMPOUND
AMORPHOUS MATERIALS CAN SOMETIMES BE IDENTIFIED
BY COMPARISON TO KNOWN SUBSTANCES VIA PARTICLE
ATLAS
LIMITED TO SINGLE PARTICLE ANALYSIS
TRACE CONSTITUENTS ADSORBED ON PARTICLES OR EX-
TREMELY SMALL PARTICLES (040 MUST BE MEASURED WITH
ANOTHER TECHNIQUE (SEM-EDX)
HOMOGENEITY IMPORTANT FOR CORRECT IDENTIFICATION
RESULTS DIFFICULT TO QUANTITATE
SOLUBILITY OF PARTICLES IN SPECIFIC SOLVENTS
INDICATE THE CLASS Of COMPOUNDS PRESENT
USE SOLUBILITY DATA TO VERIFY LATER RESULTS
USE SOLUBILITY DATA IN CONJUNCTION WITH ANION
MICRO-SPOT TESTS TO REDUCE NUMBER OF POSSIBLE
COMPOUND CHOICES
MICRO-TESTS ON A MICROSCOPE STAGE REQUIRE GOOD
TECHNIQUE AND EXTREME CARE
RESULTS REFLECT COMPOSITION OF SINGLE PARTICLES
AND NOT THE BULK OF THE SAMPLE
REVEALS PRESENCE OR LACK OF SPECIFIC ANIONS
COMBINATION ON ANION AND SOLUBILITY INFORMA-
TION LIMITS THE NUMBER OF CATIONS PRESENT IN
SAMPLE AND AIDS IN SINGLE PARTICLE COMPOUND
IDENTIFICATION
MICRO-TESTS ON MICROSCOPE STAGE REQUIRE GOOD
TECHNIQUE AND EXTREME CARE
RESULTS DIFFICULT TO QUANTITATE
PROVIDES CONCENTRATION DATA ON METALS
WITH FLAMELESS TECHNIQUES, DETECTION LIMITS BE-
TWEEN 0.001 AND I NG ARE FOSSIIBE FOR VARIOUS
ELEMENTS
SPECIFIC CATIONS CAN BE IDENTIFIED AND QUANTITATCD
THESE METALS CAN BE CORRELATED WITH SPECIFIC
PARTICLE TYPES
CATION INFORMATION CAN BE COUPLED WITH SOLU-
BILITY AND ANION CONTENT INFORMATION TO AID IN
COMPOUND IDENTIFICATION
ANALYSES OF NON-METALS AND METALLOIDS CANNOT
BE PERFORMED
Figure 5-1.
Initial Sample
Characterization
31
-------
ANALYSIS PROCEDURE FLOW
USING THE INFORMATION FROM THi TGA'DSC, DRY THE
SAMPLE At A TEMPERATURE HIGH ENOUGH TO REMOVE
WATER BUT BELOW ANY DECOMPOSITION OR VOLATILI-
ZATION POINT
PRINCIPLE OF OPERATION
ANALYSIS CONTINUES
WITH INDIVIDUAL PARTICLE
CHARACTERIZATION
ELECTRON 5PECTRCSCOPY
FOR CHEMICAL ANALYSIS
(ESCA)
QUANTITATIVE
ANION TESTS
MANY INORGANIC ANIONS HAVE SPECIFIC ABSORPTION
BANDS IN INFRARED AND FAR INFRARED. THESE BANDS
CAN BE USED TO IDENTIFY AND QUANTIFY THE ANIONS
PRESENT
EITHER WET CHEMICAL OR QUANTITATIVE IR TECHNIQUES
DIRECTED TOWARD SPECIFIC ANIONS
SAMPLE IS IRRADIATED WITH X-RAYS, CAUSING INNfR
SHELL ELECTRONS TO BE EJECTED:
« ENERGY OF THESE EJECTED ELECTRONS IS A MEASURE
OF THE BINDING ENERGY OF ELECTRONS AS MODI-
FIED BY THE CHEMICAL SURROUNDINGS OF THE
EMITTING ATOM
• ENERGY SHIFTS IN THE BINDING ENERGY OF ELEC-
TRONS EMITTED FROM SAME ELEMENT INDICATE
DIFFERENT CHEMICAL ENVIRONMENTS
POWDER SAMPLE DIFFRACTS A PRIMARY X-RAY BEAM INTO
A SES1ES OF DIFFRACTION LINES CHARACTERISTIC OF A
GIVEN CRYSTALLINE SUKIANCE
QUANTITATIVE COMPOUND DETERMINATIONS ARE
MADE, COMMONLY USING AN INTERNAL STANDARD
WITH SUBSEQUENT QUANTIFICATION BY COMPARISON
TO STANDARD CORVES
AT THIS POINT, THE QUANTITIES OF THE COMPOUNDS
DETERMINED SHOULD BE COMPARED TO THE SSMS, AAS,
AND PLM DATA
IF THERE IS REASONABLE MEG CLOSURE (±30%) WITH
PREDICTED ELEMENTAL DATA, THE VALUE OF FURTHER
WORK SHOULD BE EVALUATED IN LIGHT OF THE POTENTIAL
USEFULNESS AND THE COST OF THE ADDITIONAL DATA
THAT COULD BE OBTAINED
32
-------
INFORMATION DERIVED
COMPOUND IDENTIFICATION
PROCEDURE
LIMITATIONS
USED TO DETERMINE PRESENCE OF SPECIFIC ANIONS
SUCH AS MnO£ PO£ OR CiO|
CONFIRMATION AND QUANTITATION OF SPECIFIC
ANIONS
ONLY SMALL SHIFTS ARE SEEN IN THE SPECTRA WITH
DIFFERENT CATIONS. ANION INFORMATION IS ESSEN-
TIAL FOR INTERPRETING XRD DATA TO ELIMINATE
POTENTIAL COMPOUNDS
RATIO'S OF ANION'CATIONS USED TO PREDICT POTEN-
TIAL COMPOUNDS
INORGANIC HALOGENS HAVE NO BANDS IN THE IR
SPECTRA CAN CHANGE DEPENDING ON MOISTURE
CONTENT OF SAMPLE
TIME CONSUMING, SINCE DIRECTED TOWARD SPECIFIC
ANION
ELEMENTAL CHARACTERIZATION DETERMINES OXIDATION
STATE OF ELEMENTS PRESENT IN SAMPLE
CAN DETERMINE BULK CONCENTRATIONS OF HOMOGEN-
EOUS SAMPLES AT OR ABOVE 0.1%
THOUGH ESCA IS EXTREMELY SURFACE LIMITED SINCE
ELECTRONS HAVE SHALLOW {3 TO 20A") ESCAPE DEPTH,
THIS MAKES THE ESCA A VERY USEFUL TOOL FOR
STUDYING ABSORPTION PHENOMENA SUCH AS SO-
ON SOOT OR FLYASH z
MOST COMMERCIAL INSTRUMENTS HAVE ION (Art)
BEAM FOR SEQUENTIAL REMOVAL OF ATOMIC LAYERS
FOR DEPTH PROFILE ANALYSIS
DIRECT COMPOUND IDENTIFICATION NOT NORMALLY
POSSIBLE SINCE THERE ARE USUALLY ONLY SMALL SHIFTS
IN BINDING ENERGY OF ELEMENTS IN THE SAME
OXIDATION STATE ASSOCIATED WITH ANIONS OR
CATIONS
INTERPRETATION AND QUANTITATION OF DATA IS
DIFFICULT AND REQUIRES STANDARDS MATCHING THE
MATRIX
INTERPRETATION OF DIFFRACTION PATTERN PROVIDES
QUALITATIVE INFORMATION ON CRYSTALLINE
MATERIALS PRESENT. DIFFRACTION LINES ARE MATCHED
WITH SPECTRA OF PURE COMPOUNDS IN THE ASTM
POWDER DIFFRACTION TABLES
THE DIFFRACTION LINES ARE STUDIED AND POTENTIAL
COMPOUND DIFFRACTION SPECTRA ARE COMPARED TO
LINES IN SAMPLE SPECTRA
POTENTIAL COMPOUNDS ARE ELIMINATED OR PROPOSED
BASED ON INFORMATION FROMSSMS OR AAS (ELEMEN-
TAL DISTRIBUTION), ESCA (OXIDATION STATE) AND
IR (ANIONS PRESENT)
STATE OF THE ART SENSITIVITY IS LIMITED TO -0.05%
DEPENDING ON COMPOUND AND MATRIX. ROUTINE'
SENSITURE IS CLOSER TO 0.5%
ONLY CRYSTALLINE MATERIALS CAN 8E SEEN
Figure 5-2.
Bulk Composition
Characterization
33
-------
ANALYSIS PROCEDURE FLOW
PRINCIPLE OF OPERATION
INFORMATION DERIVED
/•""RESULTS OF BULKS.
(SAMPLE CHARACTERIZATION)
SCANNING EIECRON
MICROSCOPY OEM)/
ENERGY DISPERSIVE
X-RAY SPECTROMETER (EDX)
NO-.
ELECTRON PROBE
MICROANALYSIS
(EPMA)
'
r
I COMPOUND I YES
I IDENTIFIED
NOJ
TRANSMISSION ELECTRON
MICROSCOPY (TEM) -
SELECTED AREA ELECTRON
DIFFRACTION (SAED)
ANALYSIS
MAGNETIC DENSITY
GRADIENT SELECTIVE
DISSOLUTION
SEPARATIONS
RE PEAT ABOVE STEPS
IN SEMf
- THE SPECIMEN IS SWEPT BY ELECTRON BEAM
- SECONDARY ELECTRON EMISSION INTENSITY IS
RECORDED
- THE SIGNAL MODULATES BRIGHTNESS OF
OSCILLOSCOPE BEAM, PRODUCING AN IMAGE
-MORPHOLOGICAL CHARACTERISTICS OF THE SPECIMEN
ARE DETERMINED FROM THE IMAGE
USING SEM IN CONJUNCTION WITH EDX;
- THE SECONDARY X-RAYS PRODUCED ARE MONITORED
AND INDIVIDUAL ELEMENTS PRESENT IN THE SAMPLE
ARE IDENTIFIED AND QUANTIFIED
EPMA IS USED FOR ELEMENTS ABOVE ATOMIC NUMBER 6
SMALL ENERGETIC ELECTRON BEAM IMPINGES ON
SURFACE OF SPECIMEN, CAUSING CHARACTERISTIC X-RAY
EMISSIONS WHICH ARE ANALYZED BY WAVELENGTH
DISPERSION TECHNIQUES
WAVELENGTH POSITIONS
FOR QUALITATIVE ANALYSIS:
ARE USED
FOR QUANTITATIVE ANALYSIS! PEAK HEIGHTS (INTENSITY
RATIOS) ARE MEASURES ON BOTH THE UNKNOWN AND
ON A STANDARD OF KNOWN COMPOSITION
IN TEM, ELECTRON BEAM IS IMPINGED ON A THIN FILM
Of SAMPLE AND THE RESULTANT TRANSMITTED ELECTRON
BEAM IS OBSERVED AND RECORDED
QUANTITATIVE ANALYSIS USING TEM IS SUPERIOR TO
SEM BECAUSE:
• SMALLER SAMPLES CAN BE OBSERVED AND IDENTIFIED
• CHEMICAL SPECIES SUCH AS ASBESTOS ARE MORE
RELIABLY IDENTIFIED, (TEM'S SELECTED AREA ELECTRON
DIFFRACTION ANALYSIS IS MORE DEPENDABLE THAN
SEM'S ELEMENTAL ANALYSIS)
AT THIS POINT, IF ALL PARTICLES ARE NOT IDENTIFIED,
THE ANALYST MUST DECIDE WHETHER FRACTIONATION
OF THE SAMPLE WOULD IMPROVE THE IDENTIFICATION
OF MATERIALS PRESENT
IF SEPARATION STEP IS EMPLOYED, EXTREME CARE MUST
BE TAKEN TO PREVENT SAMPLE ALTERATION OR COM-
POUND SCRAMBLING
MAGNETIC SEPARATION IS USED TO REMOVE ANY MAG-
NETIC MATERIAL FROM REST OF SAMPLE
IN DENSITY GRADIENT SEPARATIONS, PARTICLES ARE
FLOATED IN SOLVENTS OF KNOWN DENSITY. PARTICLES
ARE SEPARATE BY DIFFERENCES IN THEIR DENSITY
SAMPLE IS EXTRACTED USING SELECTIVE DISSOLUTION
(WITH DIFFERENT SOLVENTS)
SEM SYSTEM PROVIDES HIGH RESOLUTION MORPHOLOGI-
CAL INFORMATION ON INDIVIDUAL PARTICLES
THE EDX ATTACHMENT ALLOWS IDENTIFICATION OF
INDIVIDUAL ELEMENTS IN THE PARTICLE
SPECIFIC X-RAY FLUORSCENT WAVELENGTHS CAN BE
MONITORED TO PRODUCE ELEMENTAL DISTRIBUTION
OF THE ELEMENT (NOTE: THESE PLOTS ARE ESPECIALLY
USEFUL FOR PARTICLES COMPOSED OF VARIOUS
OCCLUDED MATERIALS)
SEM INFORMATION IS A VALUABLE ADJUNCT TO THE
PLM, ESPECIALLY FOR PARTICLES < 0.5*1 (SEM MAGNIFI-
CATIONS ARE ROUTINELY IN EXCESS OF 50.000X)
OBTAINS SINGLE PARTICULATE ELEMENTAL
COMPOSITION OF ELEMENTS FROM CARBON AND ABOVE
MANY INSTRUMENTS USE WAVELENGTH DISPERSIVE
X-RAY SPECTROMETERS AND CAN RESOLVE ELEMENTS
S THROUGH Ni
PROVIDES HIGH RESOLUTION PHOTOGRAPHS
PRODUCES SINGLE PARTICLE XHtAY DIFFRACTION
PATTERN
DETERMINES PARTICLES SPECIFIC DENSITY, MAGNETIC
CHARACTERISTICS, AND SOLUBILITY IN SOLVENTS
MAIN USE IS TO REDUCE COMPLEX SYSTEMS
34
-------
COMPOUND IDENTIFICATION PROCEDURE
LIMITATIONS
SEM'S HIGH RESOLUTION IMAGES OFTEN ALLOW PAR-
TICLE IDENTIFICATION
THE EDX INFORMATION CAN BE USED TO DETERMINE
ELEMENTAL RATIOS AND THE EXACT COMPOSITION OF
THE PARTICLE
RELATIVELY LONG COUNTING TIMES ARE REQUIRED FOR
TRACE ELEMENTS, BUT THE EDX INSTRUMENT STABILITY
LIMITS COUNTING TIME TO 10 OR IS MINUTES
AT HIGH COUNT RATES, PEAKS MAY BROADEN
PARTICLES IN CLOSE PROXIMITY MAY INTERFERE AND
PRECLUDE UNAMBIGUOUS ANALYSIS
EDX DOES NOT RESOLVE ELEMENTS FROM S TO Ni
VERY WELL
QUANTITATIVE WORK DEPENDS ON HAVING SUITABLE
STANDARDS
COMPOUND IDENTIFIED BY ELEMENTAL RATIOS
EPMA ESSENTIAL WHEN ELEMENTS C THROUGH No ARE
PRESENT SINCE SEM-EDX DOES NOT SEE THOSE
ELEMENTS
IDENTIFICATION POSSIBLE ONLY FOR PARTICLES CON-
TAINING DISCRETE COMPOUNDS RATHER THAN A
HOMOGENEOUS MIXTURE
BETTER QUANTITATIVE RESULTS WHEN STANDARDS ARE
USED WHOSE COMPOSITION CLOSELY MATCHES THE
SPECIMEN
IDENTIFIES CRYSTALLINE COMPOUNDS BY THEIR
CHARACTERISTIC DIFFRACTION PATTERNS
ONLY CRYSTALLINE MATERIAL CAN BE IDENTIFIED
SEPARATING COMPLEX MIXTURE INTO SIMPLER FRACTIONS
AIDS COMPOUND IDENTIFICATION
CAN USE INFORMATION ON PARTICLE DENSITY, SOLU-
BILITY, AND MAGNETIC PROPERTIES TO IDENTIFY
COMPOUNDS
DENSITY GRADIENT WILL ONLY SEPARATE DISCRETE
PARTICLES; OCCLUDEp MATERIAL WILL HAVE AN AVERAGE
DENSITY
MANY COMPOUNDS HAVE SOLUBILITIES IN ORGANIC
SOLVENTS USED IN DENSITY COLUMN
SELECTIVE DISSOLUTION SCRAMBLES THE COMPOUNDS
UNLESS SPECIFIC COMPOUND SOLVENT SYSTEMS CAN
BE FOUND
Figure 5-3.
Individual Particle
Characterization
35
-------
( SOLID ^
V SAMPLE J
\ ELEMENTAL LEVEL 1 /
/ DATA /
< MATE /^yHAT \s^
/ELEMENTS A»-C E*«ED ?
f NOT EXCEEDING/ \ MATE /
I MATE VALUES J N.VALUES /
/LIST ELEMENTS /
EXCEEDING MATE /
VALUES /
i
AVAILABLE ^/^
T
MES LIST POTENTIAL
COMPOUNDS "*• f||sENTUNI>S
/ THESE \
/ LIST UNSTABLE / /CTTAi|iNl)S\
/C^r,UNDS ANT*-<^NDE« WOCESSOR>
/ CONDITIONS /Mn N! 5iUW|Mr. /
SCONDIT-/
VlONS/
/UP-DATE POTENTIAL /
COMPOUND LIST /
t
STUDY GENERAL
CHARACTERISTICS
OF PARTICLES
\
| ^
UPIU I 1 \ TGA/DSC
KLM 1 1 [ (NjORAIR)
* *
iSr^SKS^0^ ^"5«ZE
1 NDEX WEI GMT GAI N/ LOSS.
t REACTION IbMPtRAIURbS,
PHASE CHANGES
\
MICROSOIUBILITY MICRO-SPOT TEST
J*515 . „ ON SPECIFIC
(ACID, BASE, AKlinKK/riTinkic
NEUTRAL ANION5/CATIONS i i
'
1 STABLE DRYING /
/»SS?SKS; / /zSsrssMgarss;/
/ ^a.T£,°, / /DECOMPOSITION POINTS/
/ OF PARTICLES / /AND AIR STABILITY /
. < ,
•>,
J*
1 LISTS OF /
/ ANION VS /
f SOLUBILITY J
\
UP-DATE LIST OF
POTENTIAL
COMPOUNDS
\
SELECTS SPECIFIC ANION/
CATION TESTS FOR
K3TENTIAL ELEMENTS
(f>
\
LWET CHEMICAL
OR INSTRUMENTAL
ANION TESTS
\
1 ' . ' I / /
/ COMPOSITION / / COMPOSITION /
' / 1 '
1
RATIO CATION/
ANION VALUES
*
/UPDATE POTENTIAL /
COMPOUND LIST /
WITH WEIGHT /
INFORMATION /
XHASN.
^CLOSURE OF\ / "" IDENTIRED
/MEG COMPOUNDS^ _/ COMPOUNDS
\EXOSEDING MATEy._*/ WITH ESTIMATED
\VALUES BEEN/ «S / CONCENTRATIONS,
\ATTAI NED/ / /
Nj£
/" LIST POSSIBLE /
/ ASSIGNED COM - /
/POUNDS AT SUSPECTED/
/ LEVELS /
r
Figure 5-4. Logic Flow Chart for Initial Sample Characterization
36
-------
i
STUDY BULK
CHEMICAL
COMPOSITION
ASSIGN PROBABILITY TO
SEE POTENTIAL COM-
POUNDS WITH SPtqFtC
METHOD
ALLOWS
MATCH UP OF
METHOD WITH COMPOUNDS
BASED ON CONCENTRATION
FTIR
ESCA
PERFORM FAR IR SCAN FOR
TRANSITION ELEMENT
ANIONS IN BULK OF SAMPLE
RECORD
SPECTRA
IN FAR IR
SUtTRACr INSOLUBLES
SPECTRA FROM
ORIGINAL SAMPLE
\
STUDY SURFACE TRACE
ELEMENT COMPOSITION
OXIDATION STATES,
CHEMTCAL
ENVIRONMENT
I
XRD
OIREO ID
OF CRYSTALLINE
COMPOUNDS
AT 0.1% OR GREATER
CONCENTRATION
liSSSSSnS* 1 I"•**«* <* 1 /
/EutME5NTT'AN.ONS/ / ABSORBED SPECIES / /
LIST OF SPECIFIC
COMPOUNDS
QUANTITATE
SPECIFIC
ANIONS
WET CHEMICAL OR
INSTRUMENTAL
ANION TESTS
1
/LIST POSSIBLE NEW /
COMPOUNDS /
FOUND I
L
7
LIST IDENTIFIED
COMPOUNDS WITH
ESTIMATED
CONCENTRATION
HAVE
ALL MEG
COMPOUNDS
EXCEEDING MATE
VALUES BEEN
FOUND
LIST ASSIGNED
ELEMENTS EXCEEDING
MATE VALUES
IS FURTHER
NALYSIS COST
JUSTIFIED FOR
UNASSIGNED
ELEMENTS
Figure 5-5. Logic Flow for Bulk Composition Characterization
37
-------
PERFORM SINGLE
PARTICLE ANALYSIS
SEM-EDX
OBTAIN DETAILED MORPHOLOGICAL
INFORMATION, SINGLE
PARTICLE ELEMENTAL
SCAN AND ELEMENTAL RATIOS
J_
/ESTABLISHED ELEMENTAL/
' RATIOS FOR SINGLE /
PARTICLE /
I LIST COMPOUNDS '
WITH CONCENTRATION
ESTIMATE BASED ON ._,
ELEMENTAL VALUES /YES
VEA
SSIGNED
G COMPO
CEEDING MAT
ALUES BEE
FOUND
IS
FURTHER
ANALYSIS COS
JUSTIFIED FOR
UNASSIGNED
ELEMENTS
ELEMENTAL
RATIOS ESTABLISHED
FOR SINGLE PARTICLES
FOR ELEMENTS t C
/ LIST COMPOUNDS
' WITH CONCENTRATION
ESTIMATE BASED ON
ELEMENTAL VALUES / YES
CAN
UN AS-
SIGNED MATE
POUNDS BE
DENTIRED WIT
THESE
RATIOS
DETERMINE XRD SPECTRA
OF SINGLE PARTICLE OR
AREA IN PARTICLE
SPECIFIC COMPOUND!* .
IDENTIFIED /
ELEMENTAL
DATA USED TO
QUANTIFY
VE ALL
UNASSIGNED
EG COMPOUN
CEEDING MA
ALUES DEE
FOUND
%ES
IS
FURTHER
RACTERIZATIO
JUSTIFIED
LIST UNASSIGNED
FRACTION OF
KNOWN ELEMENTAL
COMPOSITION
BASED ON SOLUBILITY
AND ELEMENTAL DATA
SELECT SEPARATION
SCHEME
SELECTIVE
DISSOLUTION
SEPARATION
DENSITY
GRADIENT
SEPARATION
MAGNETIC
SEPARATION
LESS COMPLEX
MATRIX
SSMS
OF FRACTIONS
DOES
FRACTION
CONTAIN
UNASSIGNED
MATE
ELEMENT
Figure 5-6. Logic Flow for Individual Particle Characterization
38
-------
pheochroistn, fracture, color, and crystal habit. Microspot tests for com-
mon anions and tests of the solubility of the particles in water, acid, and
base can be performed directly on the sample as it is being examined under
the microscope. These microtests will alert the analyst to perform quanti-
tative analyses for the anions detected and they will also provide infor-
mation about the potential success of full scale dissolutions and separation.
At this stage in the analysis, quantitative analysis of anions identi-
fied in the microspot tests will most probably be performed using classical
wet test methods, e.g., titrimetric, colorimetric, or specific ion electrode
tests. A summary of the Level 1 and 2 analytical methods used for the more
common anions is presented in Table 5-1. It is meant to serve as a starting
point for the analyst, as other methods may be substituted for those sug-
gested. Level 2 am"on methods can be chosen by the analyst from Standard
Methods (Water and Wastewater), ASTM, or other EPA procedures.
Also, during this initial sample characterization, the analyst may
choose to supplement the SSMS semiquantitative cation data by analyzing
fractions of the samples using such quantitative techniques as atomic
absorption spectrometry (either flame or fTameless), Induction Coupled
Plasma Optical Emission Spectroscopy (ICPOES), Proton Induced X-Ray Emission
(PIXE), or X-ray fluorometry.
In conjunction with the PLM work a TGA/DSC scan of the sample should
be made. This test is used primarily to determine 1) the stability of the
sample, and 2) an appropriate temperature at which to dry samples to be used
in later tests. In a few cases it is possible to determine the compounds
present by the weight loss at specific temperatures. Elemental information
from SSMS and anion information from PLM (and later IR) can be combined to
give a list of potential compounds that exhibit decomposition points at the
weight loss points in the TGA or the exotherms and endotherms of the DSC.
At the end of the initial sample characterization, information will
have been obtained in the following areas:
1. General appearance of a sample
2. Number of different particles present
3. Index of refraction and crystal structure
41
-------
Table 5-!. Summary of Reconmended Procedures for Anion Analysis
ANALYSIS
AREA
Ammonia
Arsenate
Arsenite
Bromide
Carbonate
(Bicar-
bonate)
LEVEL 1
RECOMMENCE
ANALYTICAL
METHOD
Color-
imetric
SSMS/AAS
SSMS
Titri-
metric
SELECTION
RATIONALE
Rapid and simple
method.
Elemental anal-
ysis provides
upper concen-
tration limit
for anions.
SSMS has multi-
component
capability.
As for arsenate
Method provides
a rapid, and
simple analysis
technique.
SPECIAL SAMPLING
AND ANALYTICAL
REQUIREMENTS
As specified by
reagent test kit
*
Aqueous samples:
slurry with
graphite and
briquette. Solid
samples: see
element anal-
ysis. Level 2
technique is
applied to
most Level 1
samples.
As for arsenate
As specified by
reagent test kit.
REFER-
ENCES
LEVEL 2
RECOMMENDED
ANALYTICAL
METHOD
Color-
imetric
(0.05-1
ppm)
Titri-
netric
1.0-25
ppm)
Spectro-
roetric
Titri-
metric
Titri-
metric
SELECTION
RATIONALE
Method provides an
accurate technique
for analysis of
ammonia in water.
EPA method.
Standard Method
132.
Method provides an
accurate, fairly
rapid technique
for measuring
arsenic. ASTM
method.
Method provides an
accurate, fairly
rapid technique
for measuring
bromide. ASTM
method,
Method provides an
accurate technique
for measuring
total carbonate
present. ASTM
method.
SPECIAL SAMPLING
AND ANALYTICAL
REQUIREMENTS
Sample is buffered at
pH 9.5 and distilled
into a solution of
boric acid. The
ammonia in the dis-
tillate can be deter-
mined coloriroetri-
cally by nessleriza-
tion (Hgl2, Kl, NaOH)
or titrimetrically
with H2S04 using a
mixed indicator
(rcethyl red/
methyl ene blue).
25 ml of sample is
acidified with HC1,
mixed with HI and
SnCl2- 3 g of zinc
are added and the
arsine generated is
bubbled through a
silver diethyldithio-
carbamate-pyridi ne
solution. Absorbance
is measured at 540 rnn
within 30 minutes.
Sufficient NaCl is
added to 100 ml of the
sample to produce a 3g
chloride content.
KC10 is added to
oxidize bromide to
bromine (excess is
destroyed with
NaCH02). KI is added
and liberated 12 is
titrated with 0.01N
Apparatus is described
in reference. C02 is
'liberated by acidify-
ing and heating the
sample in a closed
system. COj is
absorbed in a barium
hydroxide solution.
Excess barium hydrox-
ide is titrated with
0.04 N HC1.
ASTM
D1426
D2972
D1246
0513
REMARKS
(LEVELS 1 AND 2}
Volatile organic
alkaline compounds may
cause an off color in
the nesslerization
procedure .
Measurement of arsenic
by AAS is also an
acceptable technique
and may be subject to
fewer interferences.
This method measures
bromide and iodide:
thus, this method is
to be used in conjunc-
tion with iodide +2
determination. Fe ,
«n+2 interfere., but
may be removed by
treatment with CaO.
Sulfides, (H2S)
interfered but are
removed by scrubbing
with iodine solution1,
other interferences
are removed by scrub-
bing with chromic acid.
From pH measurement
HjCOa, HC03, C0§2
concentrations may be
estimated.
-------
Table 5-1. Summary of Recommended Procedures for Anion Analysis (Continued)
ANALYSIS
AREA
Chloride
Cyanide
Fluoride
Iodide
LEVEL 1
RECOMMENDED
ANALYTICAL
METHOD
SSMS
Colori-
rtetric
SSMS
SSKS
SELECTION
RATIONALE
As for arsenate.
Method provides
a rapid, simple
analysis
technique.
As for arsenate.
As for arsenate.
SPECIAL SAMPLING
AND ANALYTICAL
REQUIREMENTS
As for arsenate.
As specified by
reagent test
kit.
As for arsenate.
As for arsenate.
REFER-
ENCES
LEVEL 2
RECOMMENDED
ANALYTICAL
METHOD
Titri-
rcetric
Titri-
metric/
Spectro-
inetric
Specific
Ion
Electrode
(SIE)
Spectro-
metric
SELECTION
RATIONALE
Method provides an
accurate technique
for measuring
chloride content
of industrial
wastewater.
ASTM method.
Method provides an
accurate technique
for measuring
cyanide. ASTM
method.
Method provides an
accurate, rapid,
simple technique
for analysis of
fluoride.
Method provides an
accurate technique
for analysis of
iodide. ASTM
method.
SPECIAL SAMPLING
AND ANALYTICAL
REQUIREMENTS
50 ml sample is titra-
ted with 0.025 N sil-
ver nitrate to a
potassium chromate
endpoint. Sulfites
are oxidized to sul-
fates by Hz02
addition.
500 ml of sample is
refluxed under acidic
conditions with CuCl?.
HCN liberated is
absorbed in NaOH,
Titration: titration
with AgN03 to rhoda-
mine endpoint.
Spectrometric:
neutralize absorption
solution with acetic
acid to pK 6.5 - 8.0
0.2 ml of chloramine
T solution is added.
Absorbance measured
at 620 nm after
20 minutes.
pH is adjusted to
5.2 - 5.5 with 0,5 N
H2S04. CQz is
removed by heating
on a hot water bath.
Buffer is added (pH
6.3, IK sodium
citrate - citric
acid - 0.2 M KNOs)
and fluoride is mea-
sured by known addi-
tion method.
Iodide is determined
by oxidation to iodate
with saturated bromine
water in acid solution.
Excess bromine Is de-
stroyed by addition of
sodium formate. Sam-
ple is titrated with
0.01 N sodium thlo-
sulfate solution.
ASTM
D512
D2036
SIE
9
01246
REMARKS
(LEVELS 1 AND 2)
Phosphates (>250 ppm)
interfere. Iodine and
bromide may also inter-
fere with visual end-
point; potentiometric
titration may solve
this problem.
Titration method
applies when cyanide
concentration >1 ppm;
spectrometric method
for <1 ppm.
Selective ion electrode
(SIE) is more accurate
and simpler than distil-
lation - spectrometric
method (SPADNS).
Effects of Fe+3, Mn+2,
and organic matter are
removed by treatment
with CaO.
This method is used in
conjunction with bro-
mide determination.
CO
-------
Table 5-1. Summary of Recommended Procedures for Anion Analysis (Continued)
ANALYSIS
AREA
Nitrate
Nitrite
Ortho-
Phosphate
LEVEL 1
RECOMMENDS
ANALYTICA
METHOD
Color-
imetric
Co\or~
imetrlc
'alar-
metric
SELECTION
RATIONALE
Method provides
a rapid and
simple analysis
technique.
Method, provides
a rapid, simple
analysis
technique.
Method provides
a rapid, simple
analysis
technique.
SPECIAL SAMPLING
AND ANALYTICAL
REQUIREMENTS
As specified by
reagent test kit
-
As specified by
reagent test kit
As specified by
reagent test .kit.
REFER-
ENCES
LEVEL 2
RECOMMENDED
ANALYTICAL
METHOD
Spectro-
metrlc
Spectro-
metric
Spectro*
metric
SELECTION
RATIONALE
Method provides an
accurate technique
for analysis of-
nitrate. ASTM
method.
Method provides an
accurate technique
for analysis of
nitrite. ASTM
method.
Method provides an
accurate technique
for analysis of
phosphate.
SPECIAL SAMPLING
AND ANALYTICAL
REQUIREMENTS
5 ml of sample 1$
mixed with brucine-
sulfanilic acid
solution then nixed
with 10 ml of. 15.6 M
H2S04. Color is
developed for 10
±1 minute in a dark
area; absorbance is '
measured at 410 nm.
pH is adjusted to 7
with CH3COOH. If
sample has appreci-
able color, filter
with A1{OH)3 9el.
EDTA is added to com-
plex cations. 2 ml
of sulfanilic acid
solution and 2 ml of
a naphthylamine
hydrochloride are
added to the sample,
solution is buffered
at pH 2.0 - 2.5 with-
NazC2H302 solution.
allowed to stand
30 minutes, and
absorbance measured
at 515 nm.
If pH >7, sample is
neutralized with
H2S04. Molybdate
reagent and stannous
chloride reagent are
added. Absorption
is measured at 690 nm
between 10-12 minutes
after reagent
addition.
ASTM'
D992
D1254
D515
REMARKS
(LEVELS 1 AND 2) «
Color does not follow
Beer-Lambert relation;
however, plotting
absorbance vs. concen-
tration yields a smooth
curve. Turbid or
colored -samples Inter-
fere, but may be
removed by filtration
and treatment with
•ftleOj and activated
carbon.
Mercury (II) causes
high results while cop-
per (II) catalyzes the
decomposition of the
diazonium salt and thus
leads to low results.
Certain bacteria uti-
lize nitrites in thefr
metabol i sm. Storage
at low temperature
minimizes this effect.
Color intensity Is
time and temnerature
dependent. Solution
may be extracted with
benzene- isobutanol
solvent to remove
interferences and
increase sensitivity.
-------
Table 5-1. Summary of Recommended Procedures for Am'on Analysis (Continued)
ANALYSIS
AREA
Sulflde
Sulfite
Sulfate
LEVEL 1
RECOMMENDED
ANALYTICAL
METHOD
SSMS
Color-
imetric
Turbid-
imetric/
Color-
imetric
SELECTION
RATIONALE
As for arsenate.
Method provides
a rapid, simple
analysis
technique.
Method provides
a rapid, simple
analysis
technique.
SPECIAL SAMPLING
AND ANALYTICAL
REQUIREMENTS
As for arsenate.
As specified by
reagent test kit.
As specified by
reagent test kit.
REFER-
ENCES
LEVEL 2
RECOMMENDED
ANALYTICAL
METHOD
Titri-
metric
Titri-
metric
Gravi-
metric
SELECTION
RATIONALE
Method provides a
rapid and accurate
technique for
measurement of
sulflde.
Method provides a
rapid and accurate
technique for
measurement of
sulflte. ASTM
method.
Method provides an
accurate technique
for measurement of
sulfate. ASTM
method.
SPECIAL SAMPLING
AND ANALYTICAL
REQUIREMENTS
Sample is acidified
and stripped with an
Inert gas and col-
lected in a zinc
acetate solution.
Iodine solution is
added to collection
vessels, acidified
with HC1 and back
titrated with
0.025 N sodium
thiosulfate solution.
A1r is excluded
while sample 1s
being taken by use
of apparatus
described in refer-
ence. HC1, KI and
KIOs are added.
Excess iodine
chloride formed is
titrated with 0.01 N
Na2S?03 using a dead
stop endpoint -
indicating
apparatus.
Sample is filtered,
pH adjusted to 4.5
with HC1, hot Bad 2
added, allowed to
stand for 2 hours,
filtered and ignited
at 800°C.
ASTM
00745
D1139
D516
REMARKS
(LEVELS 1 AND 2)
Manual for Chemical
Analysis of Water
and Waste Water
Starch indicator may
be used,
A titrimetric method
may also be used
with BaCl2,
titrating in an
alcoholic solution
to a thorin endpoint.
•p"
in
-------
4. Individual particle anion composition
5. Individual particle solubilities
6. Weight loss with respect to temperature
7. Bulk elemental distribution
Having completed the initial elemental and anion screening tests, primary
compound identification methodology can now be applied.
5.2.2 Bulk Composition Characterization
It is expected that the samples will have to be dried to a constant
water content to improve both IR and XRD spectra. Information from the
TGA/DSC step will be used to select a drying temperature that provides water
removal without sample decomposition. Further sample preparation will vary
with the requirements of the specific analysis method.
For IR analysis, the KBr pellet technique for qualitative analysis is
not recommended due to ion exchange possible during the pelletizing process.
It is recommended that a Nujol mull of the sample and AgCl (1333-400 cm )
and polyethylene (600-45 cm ) windows be used. Interpretation of the
infrared spectra on the basis of characteristic frequencies can provide the
identity of specific anions and some individual compounds. General absorp-
tion regions for several anions are given in Table 5-2, and specific absorp-
tion bands, which have been observed in particulate samples, are listed in
Table 5-3.
Several investigators have done extensive work with inorganic com-
pounds and have been able to produce specific correlations between observed
spectra and individual compounds. Tables 5-4 and 5-5 list the characteris-
tic bands for several nitrates and sulfates which could be present in envi-
ronmental samples. There are definite analytical frequencies which can be
used to identify compounds .^particularly when supporting elemental analysis
information is available.
Electron spectroscopy for chemical analysis (ESCA) will be performed
on both loose particulates and particles collected on filters. Loose
46
-------
Table 5-2. Useful IR Bands
Am'on
Absorption Bands (cm" )
SO,
NO,
co:
SiO,
610 - 690 (m)
1080 - 1130 (s)
610 - 640 (m, sp)
1350 - 1370 (s)
650 - 680 (m)
1430 - 1450 (s)
0,900 - 1100 (vs)
participate samples can be attached to a sample holder using an approach
called the "sticky gold" technique. This technique was devised to over-
come the conductivity problem and securely mount the sample. It sandwiches
f"'"'"
the sample between two layers of sputtered gold. The first layer applied
to the scotch tape does not change the tackiness of tape, which allows
loose particles to be stuck to the surface. Another layer of gold is
deposited to assure that all the particles are near a conductive surface.
Filter pieces can be clamped directly onto the sample holder after the
the bottom layers of the filter have been peeled off.
47
-------
Table 5-3. Listing of Assigned Infrared Bands Observed
in Parti oil ate Samples
Frequency, cm"
3140
3020
2920
2860
2800
1768
1720
1620
1435
1400
1384
1360
1190
1140
Species
NH/
4
NH. +
4
HYDROCARBON (C-H)
HYDROCARBON (C-H)
NH/
N02~(BULK)
NH^ (HAL IDE)
H20
co32-
NH4+
N03" (SURFACE)
N03" (BULK)
P043-(2)
po3-<2>
4
48
-------
Table 5-3. Listing of Assigned Infrared Bands Observed
in Particulate Samples (Continued)
Frequency, cm
1120
1110
1035
980
880
840
800
780
728
670
627
620
600
470
Species
P043"(2>
so42-
Si044"
so42"
co32"
N03-(BULK)
Si044'
sio44-
co32-
po43'
' P043-
so42"
po43-
Si044"
49
-------
Table 5-4. Infrared Bands of Some Common Nitrates (cm"1)
Compound
NaN03
KN03
Ca(N03)2'XH20
Fe(N03)3'9H20
Ca(N03)2'3H20
Pb(N03)2
Band Category^3'
VW
2428
1044
.
2431
W
807
M
836 sp
824 sp
820 sp
835 sp
836 sp
726
836 sp
S
M430
M640
1615
1587
VS
1358
1790
1380
1767
M350
1361
-x/1785
1378
1790
1373
W = Weak, M = Medium, S = Strong, V • Very, SP • Sharp, B = Broad
-------
Table 5-5. Infrared Bands of Some Common Sulfates (cm" )
Compound
Na2S04
K2S04
CaS04'2H20
MnS04*2H20
FeS04'7H20
CuS04
PbS04
Band Cateaorv'3'
VW
990
W
645
1010 (sh)
1670
510 (vb)
607
. 1150 (sh)
1020 (sp)
1600 (sh)
M
318
2200 (b)
660
1025
1625
680
805
860
592 (sp)
623 (sp)
S
620
603
667
1630 (sp)
3410 (b)
825
3225 (b)
611 (vb)
3330 (b)
1200
^3300 (b)
VS
1110
1110
620
1130 (vb)
1135 (vb)
1090 (vb)
1090 (vb)
en
(a) V = Very, W = Weak, M = Medium, S = strong, SH = shoulder, B - Broad, SP = sharp
-------
ESCA is employed in this step of the analysis to provide information
on the oxidation state of the elements present on the surface of the sample,
as well as on the change in elemental composition as various monolayers of
sample material are removed through ion etching.
Knowing the oxidation state of elements such as Cl, S, V, Mo, and Si
provides indications to the presence or absence of specific compounds. Once
ESCA has qualitatively established the presence of a species, specific
quantitative wet chemical tests can be made. In some cases the chemical
shift information has been correlated with specific compounds.^ ' In this
case direct determination of a compound is possible. It should be noted
that ESCA is limited to bulk concentrations of 0.1 percent or more. How-
ever, it is an extremely sensitive surface technique which is capable of
seeing a monolayer of a given element. Ar etching can be used to verify
the homogeneous composition of the sample, or to perform elemental depth
profile analysis.
The performance of specific anion tests, IR analysis, and ESCA estab-
lishes substantial information on the concentrations of a variety of cations
and anions in the sample. This information simplifies interpretation of
the XRD spectra, and provides an independent quantification of the species
present. In X-ray diffraction (XRD) analysis, approximately 100 mg of
material are ground in an agate mortar, ultrasonically dispersed with a
1:4 mixture of collodion with alcohol and then evenly spread over a glass
support. Mounting in this fashion will produce the highest sensitivity at
low 20 values. The major disadvantage of XRD as an analytical tool is its
inability to detect noncrystalline materials. In many environmental sam-
ples, the crystal structure of a compound could be grossly affected by the
conditions at the source or those during sampling. For example, As?0q can
be amorphous or crystalline depending on its temperature history. Further-
more, the sensitivity of XRD is normally limited to 1 percent or higher
although new computer averaging techniques enable materials to be detected
in concentrations as low as 0.05 percent.
52
-------
Having completed these analyses, information will have been obtained
on the following:
1. Anions present
2. Valence state of elements present
3. Elemental depth profile
4. Major compounds present
At this point the analyst must correlate all data and determine if a
reasonable (based on the analyst's judgment) agreement has been reached
with the MEG elements exceeding their MATE values. If there is reasonable
agreement between the elemental data obtained from quantitative techniques
and the compounds determined in this characterization, further work should
be carefully evaluated in terms of potential needs and end use.
5.2.3 Individual Particle Characterization
It should be emphasized that this phase of the analysis should be
carried out at the analyst's discretion. The analyst should consider the
sample, its source, the information already available, the type of informa-
tion which is lacking, the instrumental techniques available, and analysis
cost before proceeding.
Analytical techniques which are suggested for identification of
individual particles include Scanning Electron Microscopy with Energy
Dispersive X-ray spectrometry (SEM--EDX), Electron Probe Microanalysis
CEPMA) and Transmission Electron Microscopy with Selected Area Electron
Diffraction (TEM-SAED),
In SEM the sample specimen is swept by an electron beam and the vari-
ation of the secondary electron emission intensity is recorded. This sig-
nal simultaneously modulates the brightness of an oscilloscope beam,
producing an image of the sample surface on the oscilloscope screen. Since
the secondary electron beam is localized in the area impacted by the
incident radiation, images of relatively high resolution are achieved which
can provide morphological characteristics of individual particles. When
SEM is used in conjunction with an energy dispersive X-ray spectrometer
(EDX), the secondary X-rays produced can be monitored, thereby allowing
53
-------
identification and quantification of individual elements present in the
sample. Determining the elemental distribution of a particle is particu-
larly useful for those particles composed of various occluded materials; the
high resolution and magnification of the SEM can produce images distinctive
enough to identify the particle. As such, the SEM information is a valu-
able adjunct to the PLM, especially for particles smaller than 0.5y.
In order to reduce the mounting time for both SEM and EPMA (electron
probe microanalysis), particles should be mounted on a gold stage to pro-
vide a conductive surface. Normally, a carbon film would be deposited on
the sample to ensure its conductivity. If the sample is reasonably conduc-
tive and long analysis times are not necessary, then the carbon film may
be omitted. Mounting samples in this fashion will not interfere with later
EPMA analysis.
Disadvantages of the method include the inability of SEM-EDX to detect
the elements in the periodic table between carbon and sodium. Also,
resolution of the elements between sulfur and nickel is limited. Although
relatively long counting times are required for elements present in trace
amounts, the stability of the EDX instrument limits counting time to 10 to
15 minutes. Peak broadening, interference from neighboring particles and
difficulties in obtaining suitable matching standards can also limit the
certainty of an analysis. The result is generally a bulk composition cor-
related with each particle type present in the sample matrix.
In EPMA a small energetic electron beam impinges the surface of the
particulate specimen and produces characteristic X-ray emissions. EPMA can
be used to qualitatively and quantitatively determine the elemental com-
position of particles ranging in size from 20y down to about 0.2y for most
of the elements of atomic numbers above that of carbon. Instruments using
wavelength dispersive X-ray spectrometers can resolve spectra of elements
sulfur through nickel in atomic number. Using this detection, qualitative
analyses are possible. Peak heights, or intensity ratios, are measured on
samples and standards to provide a quantitative analysis.
54
-------
To achieve the best accuracy, it is necessary to do a considerable
amount of sample preparation. In most cases it is necessary to have stan-
dards similar in particle size and composition to the sample being analyzed.
Further, identification is possible only for particles containing discrete
compounds rather than a homogeneous mixture.
Transmission Electron Microscopy with Selective Area Diffraction
(TEM-SAED) also involves the impingement of an electron beam on a thin
film (~1500A) of sample. The resulting single particle X-ray diffraction pat-
tern permits identification of crystalline compounds. The qualitative and
quantitative data obtained are excellent because 1} individual particles
and fibers can be observed and identified, and 2) the use of selected area
electron diffraction is a dependable technique for identification of such
chemical species as asbestos and silica.
Combining the information derived from TEM-SAED and EPMA can aid the
analyst in assembling the total nature of the various species present.
Many substances which appear essentially identical in elemental composition
as measured with the electron probe, will be determined by TEM-SAED to have
a unique morphology and, therefore, their emitted nature and source clearly
indicated.
At this point, if all the compounds for MEG elements exceeding their
MATE values have not been found, then the analyst might choose to reduce
the sample matrix into simple mixtures. He can either run magnetic density
gradient, or selective dissolution studies. In magnetic separation, mag-
nets are used to remove the magnetic fraction from the sample. In density
gradient separation, particles are floated in organic solvents of known
density. Considerable care must be used in selecting solvents because
many compounds could be soluble in the solvents. This procedure can be
used to obtain gross separations by density or can be used to determine
individual particle densities. Selective dissolution uses a variety of
solvents to remove more and more of the sample and in the process simplify-
ing the composition of the residue.
In all these techniques care must be taken to, avoid contamination
and scrambling of compounds. Also, reasonably large quantities of sample
are necessary. The end result of these separations is to provide less
complex fractions which can be studied starting at the bulk characteriza-
tion level.
55
-------
6.
LEVEL 2 ANALYSIS OF RETAINED SASS SAMPLES FOR ORGANIC COMPOUNDS
This Level 2 organic analysis plan is based on Level 1 analysis data
and is intended for use on retained SASS samples. The plan assumes that
Level 1 analysis has been completed and that this information is available.
The techniques discussed should be implemented by a skilled mass spectrom-
etrist, since at several points in the analysis, judgement and even modi-
fications may have to be made to the procedures, depending on sample source
or what compounds are identified during the course of the analysis.
Combined gas chromatography and mass spectrometry (GC/MS) is central
to this analysis plan. GC/MS combines the separation power of the gas
chromatograph with the unexcelled identification potential of the mass
spectrometer. The incorporation of a computer based data handling system
with the GC/MS provides the most powerful compound identification tech-
nique available to the analyst. The technique is cost effective but
requires an experienced spectrometrist to suitably apply it to environ-
mental samples and analyze the data generated. Judgements as to sample
size, depending on instrument sensitivity, and mass range to be scanned,
depending on instrument resolution, as well as selection of an alternate
GC column for a specific sample, are at the discretion of the analyst.
General direction is given in this report; however, a total analysis to
identify every compound present in a complex mixture requires on-the-spot
modification of procedures. The molecular weights and necessary M/e values
for most of the MEG organic compounds are given in Appendix C.
The most cost effective Level 2 analysis scheme would be a specific
analysis based on category data obtained from Level 1. This information
would provide data for GC column selection and would generally simplify
the overall analysis. The analysis scheme as outlined is for all cate-
gories of compounds on the MEG list with the exception of those compounds
which are volatile and are analyzed by the field GC technique and those
which are reactive and chemically modified by sampling or storage.
This Level 2 analysis plan incorporates wet chemical separations,
including sample extractions and liquid chromatography, and instrumental
analysis using primarily GC/MS. Other techniques are discussed which may
be applied in special cases but require further research Into their
56
-------
application. These include high resolution mass spectrometry (HRMS),
chemical ionization mass spectrometry (CIMS), gas chromatography, with
selective detectors, and capillary column GC/MS. The proposed analysis
plan is patterned after Level 1. It was designed to provide information
on total compound identity and yet ease the total sample burden imposed by
the analysis of every Level 1 organic sample fraction. Specific GC col-
umns are described together with appropriate conditions for their use in
identifying the appropriate MEG compounds sought in each fractionated sam-
ple extract. If a category is known to be absent in a specific sample,
based on information from Level 1, it is expected that this knowledge will
be used to modify the analysis. If specific compounds are expected at very
low concentrations, they should be analyzed separately since, in general, low
levels of materials will be lost in the analysis plan as outlined. Typical
sensitivites for various analysis steps are given as a part of the overall
method discussion. It is important that the analyst implementing this
Level 2 plan have a working knowledge of Level 1 organic analysis since
it is not intended to be a step-by-step workbook but rather a logical
sequence of experiments to achieve the goal of compound identification.
The approach presented here has been specifically developed for Task 6
of EPA Contract 68-02-2163. Under EPA Contract 68-02-2150 a procedures
manual is being prepared for Level 2 organic sampling and analysis (5). It
should be referred to by the Level 2 analyst as a more complete compendium
on organic compound identification methodologies.
6.1 HARDWARE REQUIREMENTS AND OPTIONS FOR LEVEL 2 ANALYSIS
The primary tool for Level 2 analysis is a high sensitivity GC/MS
instrument. A discussion of corollary GC/MS techniques, expected to be
useful during the course of this analysis, is given as well as where their
use is appropriate. Other instrumental methods are briefly discussed,
however, further work is needed before they may be routinely applied.
6.1.1 GC/MS
In order to apply GC/MS and obtain reliable data it is necessary to
have a spectrometer which is capable of high speed scanning (i.e., record-
ing a full mass spectrum in 3 seconds or less) with resolution that will
57
-------
allow separation nominal mass peaks to at least mass 600. The gas
chromatograph should be capable of using glass columns since many of the
materials to be analyzed are sensitive to metal surfaces. The mass spec-
trometer should be capable of chemical ionization with a variety of reagent
gases such as methane or isobutane. The ability to use capillary columns
may be useful in many of the analyses which are anticipated. The incor-
poration of a computer based data handling system lessens the labor involved
in acquiring mass spectral data, and reduces the time for data reduction and
interpretation. The computer does not eliminate the need for an experienced
mass spectroscopist; it merely provides a more cost effective means of
handling large columns of mass spectral data.
6.1.2 Chemical lonization (CI) Mass Spectrometry
Normal mass spectrometry is accomplished by bombarding the sample with
70 eV electrons. The tonization process produces a spectrum which contains
characteristic fragment ions from the molecule under study. In most cases
a molecular ion is produced (i.e., the ion representative of molecular
weight) and its identification is unambiguous', however, in some cases, no
molecular ion is produced or it is present at such a low level that it
cannot be identified. The most important peak in any mass spectrum is the
molecular ion since a knowledge of molecular weight reduces the total num-
ber of organic compound possibilities by a substantial amount. Electron
ionization does provide a great deal of compound structure information, but
when the molecular ion is absent much information is lost, making spectral
interpretation difficult.
Chemical ionization incorporates a reagent gas to perform the ioniza-
tion process. The use of methane or isobutane for the chemical ionization
process is most common. When these reagent gases are used, the energy of
ionization is reduced from 70 to about 7 eV. The result is ionization of a
sample without sufficient excess energy to cause significant fragmentation
and, in most cases, the pseudomolecular ion dominates the spectrum yield-
ing molecular weight information. The CI process involves a transfer of a
proton from the reagent gas to the sample when ionization occurs. The
resulting spectrum is a pseudomolecular ion at 1 mass unit higher than the
molecular weight of the compound. Chemical ionization should always be
used in conjunction with electron ionization for spectral interpretation.
58
-------
As is true with most analytical techniques, chemical ionization is not
without its difficulties. The ionization of some materials such as alco-
hols, causes a protonation of the hydroxyl group followed by a loss of water
from the pseudomolecular ion by a thermal process. An example of this type
of ionization is given below:
CH3 CH., CH,
X 4- \ + \
HC-OH + CH5 (Reagent Gas) -HC-OH2 + CH4-^—HC+ + H20
CH3 CH3 CH3
The loss of water from the pseudomolecular ion is primarily dependent on
source temperature, and is increased with higher temperatures. This frag-
mentation process may not take place when electron ionization is used and
in many cases causes confusion in the interpretation of the molecular
weight. Similar occurrences take place when amines are being studied,
showing a loss of ammnonia from the pseudomolecular ion, and to a les-
ser extent acids, ethers, esters, and halogenated compounds. Hydro-
carbon samples are typically not sensitive to chemical ionization. This
is especially true of normal hydrocarbons. Under CI conditions, straight
chain hydrocarbons often show a loss of 1 from the molecular ion rather
than an addition, together with a significant reduction in overall sensi-
tivity. Materials which contain heteroatoms such as nitrogen, oxygen, and
sulfur, generally show an increase in sensitivity relative to their
electron ionization spectra. This variation in sensitivity is useful in
identifying heteroatom structures In complex hydrocarbon samples using
chemical ionization. Other reagent gases are available (e.g., ammonia,
nitrous oxide, and hydrogen), however, less work has been done with these
reagent gases and their use should be limited to those experienced in their
application.
6.1.3 Multiple Ion Detection Mass Spectrometry
Multiple ion detection mass spectrometry (MID) is a technique to
improve the sensitivity and selectivity of the mass spectrometer as a GC
detector. To use MID the GC retention time of the compound of interest
must be known in advance and this, together with the appearance of a peak
59
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at that retention time, is used as confirmation of the presence of a material
To use the technique, the mass spectrometer is set up to monitor a specific
set of masses, typically a number from 1 to 8. The sensitivity of the mass
spectrometer is increased by increasing the amount of time spent on selected
mass peaks. The signal to noise is improved as a square root of 2 for every
doubling of the time spent at a given mass number. This specifically is
achieved by selecting only a small number of mass peaks to be monitored
specifically for the compound of interst. The resultant data is a chroma-
togram for a specific set of masses. When an inflection occurs at a point
consistent with the retention time of the compound of interest, that mate-
rial has been identified and can be quantified providing standards are
available. It is not practical to perform multiple ion detection for
several components in a single mixture, however, if a particular compound
such as a nitrosoamine is suspected to be present in a sample at very low
levels, the technique can be invaluable. Standards should be run to deter-
mine the retention time on the column used for the analysis. Any inter-
ferences should also be noted.
6.1.4 High Resolution Mass Spectrometry (HRMS)
The techniques discussed to this point require that the compound of
interest be amenable to gas chromatography. Many materials, of course, can
not be chromatographed and therefore do not lend themselves to GC/MS. High
resolution mass spectrometry is a technique by which one can analyze low
volatility residual materials. Total compound identification may not be
possible in all cases depending on mixture complexity; however, functional
groups and heteroatoms can generally be identified unambiguously. The
technique as discussed employs the direct insertion probe which is used to
introduce the sample into the ion source of the mass spectrometer. The use
of a high resolution data system, together with the high resolution mass
spectrometer, is important in obtaining useful data in a reasonable time.
Full spectra should be recorded and the computer used to reduce the data to
element maps for selected mass peaks. The element maps will give the
elemental composition for mass peaks and an experienced mass spectrometrist
can use this information to determine the compound types in the sample.
The sophistication of a high resolution mass spectrometer is much greater
than GC/MS and the sophistication of the operator must also be greater.
60
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This technique should be applied when it is evident that significant
quantities of organic compounds have not been chromatographed and, there-
fore, are unidentified through the application of GC/MS.
6.1.5 Infrared Spectroscopy
Infrared spectroscopy is useful in determining compound functionality.
The technique is not applied directly in this Level 2 plan since it is
assumed that IR spectra have previously been recorded on all liquid
chromatography fractions in Level 1. It is also assumed that this infor-
mation is available and is used by the analyst to select appropriate GC
columns and to ensure that he has analyzed all materials which are present
in Level 1 by this Level 2 plan.
6.1.6 High Pressure Liquid Chromatography (High Resolution Liquid
Chromatography, HPLC)
High pressure liquid chromatography is not discussed in detail in this
analysis plan. This is not to say the technique is not useful; in fact, it
may be the most important technique to be ultimately used for Level 2
analysis. HPLC does not suffer from the need for volatility of a sample as
is true with gas chromatography. It is a very powerful separation tool,
superior to the extraction techniques which are used in this plan to grossly
separate organic compounds. It may be possible through research to use
HPLC as a screening tool to provide compounds class information.
Further work must be done before the technique can be universally
applied to a Level 2 analysis scheme. In the future, it may be possible to
take fractions from a high resolution liquid chromatograph for direct probe
analysis and mass spectrometer identification or ultimately an interface
between the liquid chromatograph and the mass spectrometer in much the same
way as a gas chromatogaph. Until further work is done using HPLC on
Level 2 type samples, it remains a highly probable technique rather than a
highly useful one.
6.1.7 Capillary GC/MS
It may be found in many cases, that packed columns cannot provide the
chromagraphic resolution necessary to obtain good mass spectral data. It
is expected that this will be especially true in the direct analysis of the
extracts prior to concentration or liquid chromatographic fractionation.
61
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A wide variety of capillary columns are available, including standard open
tubular wall coatee columns, SCOT columns, and micropacked columns. For
the beginner, the use of a SCOT column is recommended since it is more
tolerant of temperature and sample size while providing increased resolu-
tion over its packed column counterpart. The liquid phase chosen for a
capillary column is generally based on information obtained using packed
columns. A wide variety of liquid phases are available, however, due to
their expense, only a selected few columns are expected to be used
routinely. For general application in Level 2 analysis, it is recommended
that a laboratory have available an 0V - 17 SCOT column and a Carbowax 20M
SCOT column, which are between 50 and 100 feet in length. These two
columns will satisfy 90 percent of the requirements for capillary column
GC.
6.2 SAMPLE PREPARATION AND EXTRACTION PROCEDURES
The preparation and extraction procedures described in this section
are very similar to those used in the Level 1 analysis plan. For those
analysts familiar with Level 1 analysis, the only modification is in the
extraction of the condensate of the XAD-2 sorbent trap. Level 1 prepared
samples should be used where possible without further work.
6.2.1 Probe wash, Cyclones, and Filter SASS Train Samples
The probe wash, cyclones, and filter samples should be analyzed as
shown in Figure 6-1 starting with a methylene chloride extraction. The
extractions should be made using a Soxhlet apparatus for 24 hours. For
particulate samples, the Soxhlet cup should have been previously extracted
following the established procedures outlined for Level 1 analysis to remove
contamination which would lead to erroneous results.
6.2.2 XAD-2 Sorbent Trap
The XAD-2 resin from the sorbent trap should be extracted with
methylene chloride using a glass cup and a large Soxhlet apparatus.
62
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GC/MS ON ALIQUOT
OV-17 COLUMN
DATA SIMPLE x Nn
WELL RESOLVED
AND EASY TO
INTERPRET
©
Cl MAY BE USEFUL TO EASE
SPECTRAL INTERPRETATION
SULFUR COMPOUNDS AftE REACTIVE AND
MAY REQUIRE SPECIAL CARE
NITROSOAMINES ARE EXPECTED ONLY
AT LOW CONCENTRATIONS, IF PRESENT
SPECIAL PREPARATION WILL BE REQUIRED
FOLLOWED BY GC/MS ANALYSIS USING
CARBOWAX 20 M AND MULTIPLE ION
DETECTION (MJD)
Figure 6-1. General Logic Flow Chart for Level 2 Organic SASS Component Analysis
-------
6.2.3 Extraction of the Condensate
The condensate from the sorbent trap should first be extracted with
methylene chloride after the pH has been adjusted to 11 or greater with 6N
sodium hydroxide. This base/neutral extract should be set aside for sub-
sequent analysis. The solution pH is then adjusted to less than 2 using 6N
hydrochloric acid and the extraction with methylene chloride repeated. This
division of the condensate sample into two extracts may eliminate the need
for the liquid chromatographic (LC) separation step making the overall
analysis less expensive.
6.3 ANALYSIS OF THE EXTRACTS FOR VOLATILE COMPONENTS
Concentration of extracts prior to analysis causes the loss of most
materials with boiling points below about 220°C (C12). To obtain data on
low boiling extracted compounds from the SASS train samples, GC/MS analysis
is run on the sample prior to concentration. A 2 ml aliquot of the extract
should be saved for this analysis. One GC/MS run on each sample is made
using a general purpose column, e.g., 0V - 17. If specific classes of
compounds were found to be present from the Level 1 data for a given
extract, a repeat analysis of the uncondensed extract may be necessary
to determine if more volatile materials in the same compound class are
present. Column selection for the rerun of a sample should be based on
the categories identified from the GC/MS analysis of the LC fractions.
6.3.1 GC/MS Analysis of the Probe Wash, Cyclones, and Filter Extract
The GC/MS analysis of the probe wash, cyclones and filter extracts
should be run using chromographic conditions given below:
• Liquid phase: OV-17
• Liquid loading: 3 percent
• Solid support: Chromasorb W - AW - DMCS
• Column type: glass
t Column size: 2 mm ID x 2 meters long
• Temperature program: 50°C for 5 minutes, 50°-280°C at 6°C
per minute
64
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t Hold at maximum until all peaks elute
t Injector temperature: 280°C
• Detector and transfer line to separator temperature: 280°C
t Flow rate of helium: 30 cc per minute
• Sample size: 1 to 5 (j.1
• Sensitivity: approximately 30 nanograms per p.1 injected
This set of chromatographic conditions is very general and is designed
to separate and quantify most organic compounds suspected to be present in
a sample. Specific categories and concentrations determined from the LC
fractionation step may dictate the use of an alternate column and/or
modification of the conditions for this column. This judgement can be made
only by the analyst based on his ability to interpret the GC/MS data. The
complexity of this extract is expected to vary widely depending on the
source. When a sample is highly complex, the use of chemical ionization
mass spectrometry is recommended, chemical ionization may aid in the inter-
pretation of individual mass spectra especially if no molecular ion is
present in the El spectrum. The application of chemical ionization was
described in Section 6.1.2.
When problems of chromatographic resolution are present due to sample
complexity the use of capillary GC/MS may aid compound identification.
Liquid phase selection should be made based on the LC fraction data. A
good starting column would be a 50-foot OV-17 SCOT column. The application
of capillary GC/MS is discussed in Section 6.1.7.
6.3.2 GC/MS Analysis of the XAD-2 Module Extract
The procedure outlined for the probe, cyclones, and filter extract,
Section 6.3.1, is adequate for the methylene chloride extract of the XAD-2
sorbent material. No special precautions other than those discussed above
are necessary. The sensitivity of this analysis is also expected to be
30 nanogram per HL! injected.
65
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6,3.3 GC/MS Analysis of the Condensate Extract
The condensate extract consists of two parts, a base/neutral fraction
and an acid fraction. The GC/MS analysis of these fractions.is based on
the polarity of compounds expected to be present. The separation of the
condensate into two parts may possibly eliminate the need for an LC
fractionation step on this sample. The base/neutral fraction may be some-
what complex but the acid fraction should be relatively clean. If the
chromatograms are not too complex, it is advisable to concentrate the
samples hundredfold and repeat this analysis to increase the overall sensi-
tivity without the necessity of LC fractionation. A probe HRMS run on the
residue of the sample will provide information on the compounds which are
not amenable to GC/MS (see Section 6.1.4 for high resolution mass spectrom-
etry techniques). If both fractions are complex, the samples should be
blended prior to LC fractionation, however, if only one fraction is complex,
only that fraction need be submitted for further workup.
GC/MS Analysis of the Base/Neutral Fraction of the Condensate __
The same procedure outlined for the probe, cyclones, and filter
extracts is applied to the base/neutral fraction of the condensate. Sensi-
tivity of this analysis is expected to be 30 nanograms per microliter
injected.
GC/MS Analysis of the Acid Fraction of the Condensate
Due to the polarity and the acidic nature of the acid fraction a
polar column is used for this analysis. The exact column to be used
requires some additional information or the use of two columns for
analysis. If phenols are expected, for instance, a Tenax GC column would
be chosen. If carboxylic acids are expected, a phosphoric acid treated
carbowax 20M column would be the best choice. The use of both Tenax and
phosphoric acid treated carbowax will give results on all acidic species
which could be present in the sample. When using the carbowax column,
phosphoric acid treated glass wool should be used to plug the column ends.
This will minimize adsorption of acidic species. The gas chromatographic
procedure for each of the columns is given below:
• Column type: Tenax GC
t Column material:. glass
66
-------
• Column size: 2 mm ID x 2 meter long
t Temperature program: 50°C for 5 min, 50°-300°C at 6° min; hold
at maximum until all peaks elute
• Injector temperature: 280°C
• Detector and transfer line to separator temperature: 280°C
• Flow rate of helium: 30 cc per minute
• Sample size: 1 to 5 jil
• Sensitivity: 100 nanograms per jj.1 injected
Tenax GC is a gas-solid chromatographic material. It does not contain
a liquid phase and has very good temperature stability. It tends to elute
polar materials with ease, however, nonpolar compounds are likely to be
retained on the column. The ultimate sensitivity achieved with this
column is somewhat Tower than many others due to its absorbtive character.
The following chromatographic conditions a^e for the phosphoric acid
treated carbowax 20M column:
t Liquid phase: 3 percent phosphoric acid and 10 percent carbowax
20M
t Solid support: Chromasorb W-AW
t Column type: glass
• Column size: 2 mm ID x 2 meter long
• Temperature program: 50°C for 5 minutes; 50°-180° at 4°C
per minute. Hold at maximum until all
peaks elute
• Injector temperature: 190°C
• Detector and transfer line to separator temperature: 190°C
• Flow rate of helium: 30cc per minute
t Sample size: 1-5 nl
0 Sensitivity: 50 nanograms per |al injected
Alternate column for acid fraction of condensate extract:
• Liquid phase: FFAP (Free Fatty Acid Phase)
• Liquid loading: 10 percent
67
-------
• Solid support: Chromasorb W-AW
t Column type: glass
• Column size: 2 mm ID x 2 meter long
• Temperature program: 50°C for 5 minutes, 50°-230° at 6 per
minute; hold at maximum until all peaks
elute
• Injector temperature: 240°C
• Detector and transfer line to separator temperature: 240 C
• Flow rate of helium: 30cc per minute
• Sample size: 1-5 pi
• Sensitivity: variable with sample from 30 to 100 nanograms per
jil injected
The conditions specified for the various columns may be modified to improve
a specific analysis. When extracts are found to be relatively clean, a
faster temperature program will result in less analysis time per sample.
This judgement must be made by the operator at the time of analysis.
6.4 LIQUID CHROMATOGRAPHIC (LC) SEPARATION
Once the preliminary GC/MS work has been completed on the extracted
samples, a general idea of compound type or class is available. The next
step is to separate the various extracts after they have been condensed
to identify specific compounds by GC/MS. The purpose of this LC procedure
is to separate the samples into approximate classes based on polarity
using a gradient elution LC technique. The detailed procedure for the LC
fractionation is given in Appendix B. The LC separation is not a high
resolution technique therefore overlap in the compound classes in many of
the fractions is common. The procedure for Level 1 is followed even
though several of the fractions are blended after separation prior to
analysis. The blending of fractions is due to compound class similarity
and allows a more cost effective GC/MS analysis. Table 6-1 gives the
blending of the fractions following the LC separation using the solvent
gradient outlined in Table 6-2. (Unblended aliquots can be analyzed if
the analyst decides complexity warrants it.)
68
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Table 6-1. LC Fraction Blending
LC Fraction
1
2
3
4
5
6
7
-8
Blend
— A
Table 6-2. Solvents Used in Liquid Chromatographic Separations
Fraction No.
Solvent Composition
1
2
3
4
5
6
7
8
Pentane
20% Methylene Chloride in Pentane
50% Methylene Chloride in Pentane
Methylene Chloride
5% Methanol in Methylene Chloride
20% Methanol in Methylene Chloride
50% Methanol in Methylene Chloride
5/70/30, Cone. HC1/Methanol/Methylene Chloride
69
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6.5 GC/MS ANALYSIS OF LC FRACTIONS
Each of the blended LC fractions are concentrated to a volume of less
than 10 ml using an air drying technique. Once this has been achieved,
1 ml of the internal standard is added and diluted to exactly 10 ml using
methylene chloride in a volumetric flask. In specific cases, where sensi-
tivity is very important, a smaller volume may be used-as long as it is
known exactly. The GC analysis of the individual fraction blends is dis-
cussed below.
6.5.1 Fraction A (1)
Fraction A contains the compounds that generally fall in categories
1 and 2 of the MEG list (see Table 2-5). These include aliphatic hydro-
carbons and alkyl halides. These are the least polar compounds to be
analyzed and are well-suited to low polarity silicon liquid phase GC
columns. The column conditions given below provide complete analysis of
this fraction.
• Liquid phase: OV-101
• Liquid loading: 3 percent
• Solid support: Chromasorb W-AW-DMCS
• Column type: glass
t Column size: 2 mm x 2 meters long
• Temperature program: 50°C for 5 minutes, 50°-280° at 6° per
minute. Hold at maximum until all peaks
elute
• Injector temperature: 290°C
• Detector and transfer line to separator temperature: 290°C
• Flow rate of helium: 30 cc per minute
• Sample size: 1-5 (j.1
• Sensitivity: 30 to 50 nanograms per ^1 injected
Because of the nature of the compounds found in fraction A, the use
of chemical ionization is not recommended to improve sample identification.
The loss in sensitivity and the confusion resulting from a mixed ionization
process suggests that electron ionization is the method of choice.
70
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6.5.2 Fraction B (2 and 3)
Fraction B has been blended and contains categories 2, 15, 16, 21,
and 22 as outlined in Figure 6-1. These compounds can normally be classi-
fied as unsaturated hydrocarbons and halogenated species. In general,
these classes produce strong molecular ions in the electron ionization mode
of operation resulting in spectra which are easy to interpret.
The GC separation is best conducted on a high temperature nonpolar
chromatographic column such as Dexil 300. The conditions for a typical
analysis are given below.
• Liquid phase: Dexil 300
• Liquid loading: 3 percent
t Solid support: Chromasorb W-AW-DMCS
• Column type: glass
• Column size: 2 mm ID x 2 meters long
• Temperature program: 50°C for 5 minutes, 50°-300°C at 6° per
minute. Hold at maximum until all peaks
elute
• Injector temperature: 300°C
• Detector and transfer line to separator temperature: 290°C
• Flow rate of helium: 30 cc per minute
• Sample size: 1-5 |j.l
• Sensitivity: 10-30 nanograms per |il injected
The compounds generally found in LC fractions 2 and 3 are also not
amenable to chemical ionization, and electron ionization spectra of these
materials should be sufficient for compound identification.
If the mixture is exceedingly complex such that chromatographic
resolution is insufficient, the use of a silicon liquid phase OV-17
capillary column is recommended.
71
-------
6.5.3 GC/MS Analysis Fraction C (4 and 5)
Fraction C represents classes of compounds with increased polarity
over the previous fractions. Several intermediate polarity nitrogen,
sulfur, and oxygen containing compounds elute in these fractions. Analy-
sis of this material is best suited to an intermediate polarity silicon
column of which any one of several can be chosen. The chromatographic
conditions given below represent a compromise for this class of materials.
• Liquid phase: OV-17
t Liquid loading: 3 percent
• Solid support: Chromasorb W
• Column type: glass
t Column size: 2 mm ID x 2 meters long
• Temperature program: 50°C for 5 minutes; 50°-290°C at 6°C
per minute. Hold at maximum until all
peaks elute
• Injector temperature: 290°C
• Detector and transfer lines to separator temperature: 290°C
• Flow rate of helium: 30 cc per minute
• Sample size: 1 to 5 pi
• Sensitivity: 20 to 50 nanograms per microliter injected
Due to the nature of these classes of compounds and the fact that they
generally contain heteroatoms, chemical ionization is recommended as a
supplemental technique to aid in the interpretation of the mass spectral
data.
6.5.4 GC/MS Analysis of Fraction D (6 and 7)
LC fractions 6 and 7 represent complex mixtures of compounds which
are rather polar in nature and have widely varying acidities. In these
two fractions both basic and acidic compounds elute together, and such
mixtures are not amenable to a single gas chromatographic column.
Without previous information as to the nature of compounds present, it
is necessary to run this fraction on at least three different GC columns
in order to ensure that all materials in the sample have been identified.
72
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The columns selected for these analyses, given below, include an inter-
mediate polarity silicon column, a column designed to elute free fatty
acids and glycols and another to elute free amines. A class of compounds
known as nitrosoamine elute in this fraction. These materials are very
toxic even at low concentrations. An attempt to analyze for nitrosoamines
in this mixture, without special care would be virtually impossible. If
nitrosoamines are expected, special precautions should be taken;
specifically designed cleanup steps should be used followed by chromato-
graphic analysis with a column such as carbowax 20M which is especially
good for nitrosoamines at low concentration. The use of multiple ion
detection mass spectrometry for the determination of nitrosoamines would
be logical for this type of sample. The three columns used for the analysis
of fractions 6 and 7 are given below together with chromographic
conditions:
• Liquid phase: OV-17
• Liquid loading: 3 percent
• Solid support: Chromasorb W
• Column type: glass
• Column size: 2 mm ID x 2 meters long
• Temperature program: 50°C for 5 minutes, 50°-300°C at 6
per minute. Hold at temperature maximum
until all peaks elute
• Injector temperature: 290 C
t Detector and transfer line to separator temperature: 290 C
• Flow rate of helium: 30cc per minute
• Sample size: 1 to 5 microliters
• Sensitivity: 20 to 50 nanograms per microliter injected
This column is designed to elute those compounds with intermediate
polarity such as esters, ketones, and nitrogen heterocycles. The more
polar materials are better suited to an FFAP column described below.
• Liquid phase: FFAP (Free Fatty Acid Phase)
• Liquid loading: 10 percent
73
-------
• Solid support: Chromasorb W-AW
• Column type: glass
• Column size: 2 mm ID x 2 meters long
• Temperature program: 50°C for 5 minutes; 50°-230°C at 6° per
minute. Hold at temperature maximum until
all peaks elute
• Injector temperature: 240 C
• Detector and transfer line to separator temperature: 250 C
• Flow rate of helium: 30 cc per minute
• Sample size: 1 to 5 til
t Sensitivity: 50 to 100 nanograms per microliter injected
The basic compounds, such as amines, are better suited to columns
specific for basic materials. The following set of conditions will provide
good chromatographic separations for basic compounds.
t Liquid phase: 10 percent carbowax 20M-3 percent KOH
• Solid support: Chromasorb W
• Column type: glass
• Column size: 2 mm ID by 2 meters long
• Temperature programs: 50°C for 5 minutes 50°-180°C at 6°C per
minute. Hold at temperature maximum
until all peaks elute
• Injector temperature: 180°C
• Detector and transfer line to separator temperature: 190°C
• Flow rate of helium: 30 cc per minute
• Sample size: 1 to 5 jj]
• Sensitivity: 50 to 100 nanograms per microliter injected
The use of these three columns should provide compound identification
on fractions 6 and 7. Alternate columns may be used if information from
the GC/MS analysis of the original extracted material shows specific cate-
gories present. One alternate column would be Tenax GC, which is
especially suited for analysis of glycols and amides, while Chromasorb
103 can be used as a substitute for the amine column KOH-carbowax.
74
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6.5.5 GC/MS Analysis of Fraction E (8)
LC fraction 8 contains the most polar materials in the sample such as
carboxylic acids and sulfonic acids. These compounds are not particularly
well-suited to chromatographic analysis. Specific columns such as FFAP
or phosphoric acid treated carbowax (SP-216-PS) can be used to run the
lower boiling acidic species. However, the high boiling materials can
only be analyzed by direct insertion probe mass spectrometry, preferably
using high resolution. The GC analysis conditions using FFAP have prev-
iously been given and conditions for the other acid column are given below.
• Liquid phase: 10 percent Carbowax 20M-3 percent H-PO.
»5 T1
• Solid support: Chromasorb W AW
• Column type: glass
• Column size: 2 mm ID x 2 M long
t Temperature program: 50°C for 5 minutes; 50°-180°C at 6°C/min.
Hold at temperature maximum until all peaks
elute
• Injector temperature: 190°C
• Detector and transfer line to separator temperature: 190°C
• Flow rate of helium: 30cc/min
• Sample size: 1-5 ^1
Acid fraction 8 is particularly well-suited for chemical ionization
and, if high resolution mass spectrometer is not available for running the
solids probe on the residue, a solids probe analysis using chemical ion-
ization may aid in identification of some components.
An alternative to direct analysis of acidic species is derivation.
Several methods of derivation are available. However, the two most common
are the formation of trimethylsilyl esters of the acids or methylation to
form the methyl esters. The trimethylsilyl esters are the easiest to
form, although GC/MS identification of these materials can be quite diffi-
cult. GC/MS analysis of this derivative generally results in the TMS
fraction of the molecule dominating fragmentation such that the spectrum is
a function of the derivation rather than the molecule itself. The result
is a confusing, uninformative spectrum that is difficult to interpret.
75
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Chemical ionization is not particularly well-suited to any IMS
derivative.
The formation of methyl esters of carboxylic acids and sulfonic acids
is a more tedious process requiring considerably more chemistry and care.
The derivatization is usually conducted with diazomethane which is a rather
explosive substance. However, once the derivatives are formed, chromato-
graphic separation is trivial and mass spectral identification is usually
positive. Chemical ionization is well suited for mass spectral analysis
of methyl esters. If trimethylsilyl derivatives or methyl esters are
formed, the GC separation should be performed using a OV-101 column and
the conditions outlined in Section 6.5.1.
6.6 LEVEL 2 ANALYSIS OF WATER SAMPLES
This Level 2 plan for analysis of water samples is taken from the
"Sampling and Analysis Procedures for the Survey of Industrial Effluents
for Priority Pollutants," published by the Environmental Protection Agency,
Cincinnati, Ohio. Figure 6-2 is a schematic diagram of the plan. The
analysis is divided into three parts, the first is a direct injection of
the aqueous sample for the determination of very high concentrations of
organic materials and those compounds which are not amenable to the
Bellar purge and trap technique. The second step is the purge and trap
technique where an aqueous sample is purged with an inert gas and the
water immiscible volatile organic compounds are trapped on a Tenax solid
adsorbent prior to GC/MS analysis. Finally the sample is extracted, first
at an alkaline pH followed by an acidic pH extraction to separate the
higher boiling and water miscible organics both basic and acidic.
6.6.1 Direct Aqueous Injection GC/MS
When impurities in the water are present at very high concentration, they
can be most easily determined both qualitatively and quantitatively by direct
aqueous injection of the water sample. Typically a 5 micro!iter sample
of the water is injected onto an appropriate column such as Tenax for
polar compounds and Porapak Q for nonpolar compounds using the conditions
given below. The direct injection technique is also useful for the analy-
sis of extremely volatile impurities which cannot be determined by the
purge and trap technique.
76
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DIRECT AQUEOUS INJECTION GC/MS®
ANALYSIS FOR HIGH CONCENTRATION
AND HIGHLY VOLATILE MATERIALS
TENAXGC^ PORAPAK Q
POLAR COMPOUNDS NON-POLAR COMPOUNDS
- MOST CATEGORIES -
SENSITIVITY 100 NG/tL INJECTED
. HIGH CONCENTRATION
/STOP! AND HIGHLY VOLATILE
1 JMMEG COMPOUNDS
IDENTIFIED
WATER IMMISCIBLE
f STOPl MEG COMPOUNDS
IDENTIFIED
PURGE AND TRAP CONCENTRATION
FOR WATER IMMISCIBLE
VOLATILE (~BP-1M°C) ORGANICS
®
GC/MS
0.2% CAR8OWAX 1500 .
ON CARBOPAK C
CATEGORIES
I, 2, IS, 16 (LOW BOILERS ONLY)
RERUN SAMPLE USING
CAPILLARY COLUMN GC/MS
METAL OR GLASS COLUMN
OV-17 OR CARBOWAX 20 M
SAME DATA OBTAINED AS
BEFORE EXCEPT IMPROVED
CHROMATOGRAPHIC RESOLUTION
WATER IMMISCIBLE
MEG COMPOUNDS
IDENTIFIED
BASE/NEUTRAL
„ EXTRACTABLE
STOPl MEG COMPOUNDS
IDENTIFIED
BASE/NEUTRAL EXTRACTION
PH >ll
Me CI2
CONCENTRATE
GC/MS
OV-17 CATEGORIES^
©
Cl MAY 8E USEFUL TO EASE
SPECTRAL INTERPRETATION
USE H3P04 GLASS WOOL PLUGS
FOR COLUMN TERMINATORS WHEN
•JSING COLUMNS FOR ACIDIC SPECIES
{ ) INDICATES CATEGORIES WHICH
MAY EXIST IN BOTH FRACTIONS DUE
TO ACIDITY (PKo)
ALL COLUMNS GLASS UNLESS
OTHERWISE SPECIFIED.
,,,., '
10,11,12, (13), 15,16,17,21,
22,23,24,(25)
CHROMASORB 103
MAY BE USEFUL FOR
AMINES IF PRESENT
CATEGORIES 10, 12
GC/MS®®
TENAX GC
OR (g
H3 PO4 TREATED CARBOWAX 20 M^
CATEGORIES
(5,A), 8, (13). 14, IB, 19, K. 2-
CONCENTRATE FOR
LC SEPARATION
AS FOR SA5S SAMPLES
GO TO LC SEPARATION
SCHEME ON SASS COM-
PONENT aow CHART
Figure 6-2. Logic Flow Chart for Level 2 Organic Aqueous Samples
-------
Tenax GC
GC conditions for Tenax have been previously given.
Porapak Q
Porapak Q is a porous polymer which is a gas solid absorbent, and
will elute most nonpolar compounds with good resolution.
• Column type: Porapak Q
• Column length: 4 mm ID by 2M long
• Temperature program: Room temperature to 240°C at 6 C per
minute. Hold at maximum until all peaks
elute.
• Sample size: 3 to 10 (j.1
t Sensitivity: 100 nanograms per ^1 injected.
6.6.2 Purge and Trap Concentration Technique
The purge and trap technique is designed to concentrate those organic
compounds from water which are immiscible and having a boiling range up to
about 130°C, very low boiling immiscible materials are not trapped by this
technique. The apparatus used for this analysis consists of a purging
chamber in which the sample is placed. The chamber -is purged with an
inert gas such as helium at a flow rate of 40 cc per minute. The purge
time is approximately 12 minutes and the organic vapors are trapped on a
Tenax and silica gel column which is subsequently heated and the desorbed
gases injected into a gas chromatograph followed by separation on a carbo-
wax 1500 column.
• Liquid phase: 0.2 percent Carbowax 1500
• Solid support: Carbopak C
t Column type: glass
• Column size: 2 mm ID by 3 meters long proceeded by a short column
of 3 percent Carbowax 1500 on Chromasorb W
• Helium flow rate: 30 cc per minute
• Temperature program: room temperature during trap desorption
followed by rapid heating to 60°C hold for
4 minutes then program at 8°C per minute to
170°C, and hold for 12 minutes or until all
compounds have eluted.
78
-------
• Sensitivity: variable depending on trapping efficiency, must be
determined daily when analysis technique is used.
The column used in this analysis has very high resolution for nonpolar
materials which are low boiling. These include categories 1, 2, 15, and
16. If the sample is highly contaminated and chromatographic resolution
is insufficient for compound identification, a capillary column, either
OV-17 or Carbowax 20M, may be used as a substitute in this analysis.
When using the purge and trap technique, it is necessary to run blank
water samples between each analysis sample. It is also necessary to bake
the trap during the course of the GC run to remove all possible inter-
fering organic substituents which may cross over from one sample to the
next due to insufficient trap heating.
6.6.3 Extraction of Water Sample for GC/MS Analysis
The extraction of water samples for subsequent analysis by GC/MS is
identical to the procedure outlined for the condensate sample from the
SASS train. If the chromatographic analysis of the extracts is complex
and incomplete compound analysis results, the LC fractionation step should
be implemented as outlined in Figure 6-1.
79
-------
APPENDIX A:
LEVEL 1 DATA REDUCTION AND DECISION CHARTS
80
-------
Level 1 Data Reduction and Decision Charts
Level 1 Data Reduction and Decision Charts
00
CATEGORY
1 . ALIPHATIC
2. HALOGEHATED
ALIPHATIC
HTDMCARBOD
A. SATURATED
AlKYL
HAL IDES
COMPOUND
Hexanes
Nonanes
Cyclohexane
Butanes
Octanes
Heptanes
Pentanes
Methane
Ethane
Propane
Cyclapetane
Alkalies (C>9)
Cyclopentadtenes
Cyclohexene
Hexenes
Butadienes
Ethyl ene
Propylene
Butylenes
Pentenes
Cyclohexadiene
Heptenes
Propyne
Acetylene
Butyne
Hexachlorocyclo-
hexane (Undone)
Metnyl 1mHde
HATE 1
AIR '
ug/m3 (pp«) '
3.6 x 10s (100)
1.05 x 1C* (MO) •
1.05 x ID* (300) T
1.4 « 106 (600) .
1.45 x 106 (300) '
1.6 x 106 (400)
1.8 x 10« (600)
3.3 x 106 (sooo)
S.12 x ID6 (5000)
9.0 x 106 (5000)
N
N
2.0 x 105 (75)
1.0 x ID* (300)
1.02 x 106 (300)
2.Z x 106 (1000)
5.71 x 106 (5000)
8.59 x 10' (5000)
K
N
N
N
1.65 x 106 (1000J
5.31 x 106 (5000)
N
5.0 x It?
8.54 r. 102
MUTE
HATER
.9/1
HEALTH
5.4 x 106
1.57 « 107
1.58 x 107
2.1 x 10'
2.18 x 10'
2.4 x 10'
1,7 x 107
4.91 x 10'
9.18 x 107
1.35 » to8
N
N
3.0 x 106
1.5 x 107
1.53 x 10'
3.3 x !07
8.57 x !07
1.29 x 10«
It
N
N
N
2.48 » 10?
7.97 x 10?
N
7.50 x 103
1.28 x 10'
NATE
MATER
U9/1
ECOLOGV
1.0 x 105
N
1.0 x 103
-1.0 x 105
N
1.0 x 10*
1.0 x 103
>1.0 x 105
N
>1.0 x 105
>).0 x 10s
s
ri
n
»
1.0 x SO3
1.0 x ID*
1.0 x ID5
N
H
II
l.Dx 10>
1)
II
II
1.0 x 102
n
NATE
LAND
"9/9
HEALTH
1.1 x 10«
3.2 x 10"
3.2 x to"
4.2 x 1(4
4.4 x 104
4.S » 10<
5.4 x 10*
9.8 x 10«
1.8 x 105
?.8 x 105
1.1 x 10*
n
$.0 x 103
3.0 x 104
n
6.6 x 10^
1.7 x !05
2.6 x 105
N
N
II
N _
5.0 x 10<
1,6 x 10s
N
1.5 x 10'
2.6 x 101
HATE
LAM)
c9/9
ECOLOSY
.2.0 x 10?
N
2.0
=2.0 x 10?
K
Z.O x 102
2-0
=2.0 x 10?
N
.2.0 x 10?
>2.0 x 10*
d
K
II
n
2.0
2.0 x 10
2.0 x 102
N
II
n
^0_x Ig
H
n
n
2.0 x ICr'
H
KHEBE FOUND
IN
LEVEL I
GAS, FIELD, C6
SASS, Lflfl, C9
GAS. FIELD, C6
SAS, FIELD, C4
SASS, LAB, C8
GAS, LAB, 07
GAS, FIELD, C5
GAS, FIELD. Cl
GAS, FIELD. C2
GAS, FIELD, C3
GAS, FIELD, CS
SAS, LAB, C10-
12, LCI
T GAS, FIELD, C5
GAS. FIELD, C6
GAS, FIELD, C6
GAS, FIELD, C3
GAS. FIELD, Cl
SAS, FIELD, C2
OAS, FIELD, C3
6AS, FIELD, C5
GAS, FIELD, C5
GAS^FIELD^ C6
GAS, FIELD, C3
SAS, FIELD, C2
GAS, FIELD, C3
SUSS, LAB, Cll
6AS, FIELD, CS
SANPLE
W/m3
U9/9
UJ/1
RATIO
SAMPLE
MATE
LE»EL 2
REQUIRED
V'YES
N=NO
TEST
METHOD1
1
TEST
EXPEC-
TATIONS^
!
:
1 ^EST
• COST3
1 SAMPLE
J ALIQUOT4
',
\
I
TASLE KEY:
. TEST METHOD
1. STAHDAP.D
2. DEVELOP-
MENTAL
3. UNKNOWN
A. AAS
£.. XRD
C. KEt
CHEMICAL
D. ESCA
E. GC/HS
. EXPECTED TEST
SUCCESS:
1. NIGH
2. MODERATE
3. UNKNOWN
. TEST COST
1. REASON-
ABLE
2. MODERATE
3. HIGH
SANPLE
ALIQUOT
1. ADEQUATE
2. MARGINAL
3. INADEQUATE
4. RESAHPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reduction and Decision Charts (Continued)
00
CATEGORY
B. UHSATUKD
ALKYL
HALIDES
3. ETHERS
COMPOUND
THbrommiethane
Kexachloroetrtane
1,1.2-Trichlorti-
ethane
Carbon tetra-
eMorJde
Hetfeyl bromide
Chloroform
l,2-D1cMoroett>ane
Hetltyl chloride
Dichloropropanes
DidilonMe thane
Brcmchloramethaiw
l.2-Wchloro-l,2-
difluoroethaiK
Dlchlorodifluord-
methane
Trichlorofluoro-
ffithane
Bramsdichloro-
ntthaiw
DlbroKKflcMoro-
me thane
BronobEitanes
1»Ch1oroD£tane
Hexachlorocyclo-
pentadiena
Chlaroethene
Hexachloro-
butadlene
D1 chloropropenes
1,1-OicMoroetheiie
Tetrachloroethene
l.Z-DlchloroetheM
Z-e«ty1-4-*tf»yl-
1,3-Dloxolines
1,3>Dfoun
1 ,4-01oxine
tiopropyl ether
2-Hettoxybiplienyl
HATE
AIR
M9/m3 (ppm)
5.0 > ID3 (0.5)
1.0 X 10' (!)
4.5 x 10* (10)
5.98 » 10*
6.0 x 10* (15)
l.Z x 10s (25)
2.0 x to5 (SO)
2.1 x 105 (100)
3,5 i 105 (75)
1,1 x 105 (£00)
1.1 x IB6 (200)
4.95 x 106 (1000)
4.95 x 106 (1000)
5.6 x 106
H
H
K
N _ _
1.1 x Id2 (0.01)
2.SS x 103 (1)
4.0 x 103
1.12 x 10*
2.59 X 105
6.7 * 105 (100)
7,0 x 105 (ZOO)
2.25 x 10*
1.8 x 105 (50)
1.8 X 105
1.05 x 10s (250)
N
HATE
UATEfi
wg/i
HEALTH
7.5 K 10*
1.5 It !05
6.75 x 105
8,97 x 105
9.0 « 105
6,0 » 105
3.0 x 106
3.15 x Id6
5.25 x 10'
1.08 x 107
1,7 x 107
7.43 x 107
7.43 x 107
8.4 It 106
N
N
N
N
1.6S x ID3
3.83 x 10*
6.07 x 10*
1 .68 x 105
3.88 x 106
1.01 x !07
1.10 x 107
3.38 x 10s
1.7 x 10«
1.7 x 10*
1.58 x 107
N
MUTE
UHTER
ug/l
ECOLOGY
II
N
1.0 « 103
1.0 x 103
>1.0 x IDS
X
1.0 x 10*
>1.0 x 1«5
1.0 x 103
4.5 x 103
N
K
>1.0 x 105
f,
N
N
N
N
It
>71.0 x 105
N
1.0 X 103
4.5 x 103
1.0 x 103
1.0 x 10*
N
N
1.0 x 10«
1.0 x 10*
N
MATE
LAND
-9/9
HEALTH
1.5 x 10?
3.0 x 10?
1.4 x 103
1.8 x 10?
1.8 x 103
1.2 x 103
6.0 x 103
S.4 x 103
1.1 x 10*
3.* x 10*
1 .5 x 105
1.5 x 105
1.7 x IDS
K
N
K
K
3.4
7.6 x 101
1.2 x 10*
3.4 x 102
2.0 x 10*
2.2 x 10*
6.8 x 10Z
5.4 x 103
5.4 x 103
3.1 x 104
N
MATE
LAND
U4/9
ECOLOGY
N
N
2.0
2.0
72.0 x 102
It
2.0 » 10'
Z.O x 10?H
J.O
N
H
72.0 x IQ2
N
N
N
N
N
H
Z.O x 102
N
?.o
2.0
2.0 x Ifll
N
2.0 x 101
Z.O x 101
Z.O x 10<
K
MHERE FOUND
IN
LEVEL I
SASS, LAB, CIO
SA55, LAfl, Cll
SAS. FIELD, CS
GAS, FIELD, C5
GAS. FIELD, M
GAS. FIELD, «
GAS, FIELD, CS
GAS, FIELD, C3
GAS, FIELD, C6
SASS, LAB, C8
SAS, FIELD, C6
GAS. FIELD, C5
GAS, FIELD, C3
GAS, FIELO, C4
WS, FIELO, C6
GAS, FIELO, C9
.SASS, LAS, C7
SASS, LAB, Cll
SASS, LAB, LCZ
GAS, FIELD, C3
SASS, LAB, LC2
GAS, FIELO, C6
GAS. FIELD, CS
SASS. LAB, CS
GAS, FIELD. CS
SASS, LAB, C8
SASS, LAB, C7
SASS, LAB, C7
SASS, LAB, C7
SASS, LAB, C7
SAMPLE
Bg/m3
W9/9
ug/l
RATIO
5AH?LE
HATE
LEVEL 2
REQUIMD
Y-YES
N'NC
TEST
METHOD1
TEST
EXPEC-
TATIONS2
TEST 1 SAMPLE
COST3 ALIQUOT*
|
1
j
^
1
TA6LE KEY:
TEST HETHOD
1. STANDARD
2. DE»ELOf>-
HENTAL
3.
A. AAS
B. XRD
C. HET
CHEMICAL
0. ESCA
E. GC/MS
EXPECTED
TEST SUCCESS:
1. HIGH
2. MODERATE
3. UNKNOWN
TEST COST
1. REASON-
ABLE
2. MODERATE
3. HIGH
. SAMPLE
ALIQUOT
1. ADEQUATE
2. MARGINAL
3. INADEQUATE
4. RESAMPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reduction and Decision Charts (Continjed)
GO
00
CATEGORY
4. HALOSENATEO
ETHERS
5. ALCOHOLS
K. PRIHARY
ALCOHOLS
8. SECONDARY
ALCOHOLS
COMPOUND
1,1-Wchlorodt-
rthyl etlwr
l.2*D1chloro-
sthyl ether
2,2-01 cWorodl-
ethyl ether
Chlorcmethyl
methyl ether
1,1-trtchloro-
methyl etiwr
2-Olloro-l,2
epoxypfopane
2-Chloroethyl
aetliyl other
l-CMoro-1,2-
metane
Chloroetfiylethyl
ether
1,2-DichlOroethyl
ethyl ether
u*Chlorabutyl-
ethyl ether
bis-{1-Chloroiso-
propyl) ether
Bronuphenyl
phenyl ether
a-Hydroxytholyene
Isobutylalcohol
Pentanols (Primary)
1-PropMiol
Butanols (Urinary)
N-Butanol
Nethanol
Ethano!
Phenyl Ethanol
Benzyl
Borneol
2,6-B1methyl-4-
h»pt»no1
HATE
AIR
ug/ffl3 (ppnt)
3.0 x 104 (5)
3.0 « 10* (5)
3.0 x 10* (5)
3.68 x 10*
N
N
N
n
N
N
N
N
N
S.S x 10-*
1.5 x 105 (50)
3.6 « 10S (100)
5.0 x 10s
1.5 x 105 (50)
2.6 x 10s (200)
1.9 s loMlOOO)
1.8 x lO4""^
- S.54 « 10*
9.0 x 10* •
1.6 x 105
MATE
HflTIR
1.9/1
HEALTH
«.5 x 105
4.S » 105
4.5 x 105
5.52 x 10^
N
N
N
N
N
n
N
N
N
. 8.3 » 105
2.3 x 106
5.4 x 106
7.S x 106
Z.25 x 106
3.9 x 106
Z.8S x 107
2.7 x 10*
S.31 x 105
1.35 x 106
2.1 x 106
NATE
UATER
ug/1
ECOLOGY
N
4.5 « 103
1.0 x 10*
4.5 x 1C3
N
»
N
U
K
N
K
N
N
1.0 x 104
1.0 x 10*
1.0 x 10*
1.0 * 10*
>1.0 x 10s
>I.O K 106
=1.0 x 106
N
1.0 x 10*
N
N
WTE
LAND
.-9/9
HEALTH
9.0 x 102
K
9.0 x 102
1.1 x 103
K
N
N
K
N
N
N
N
11
1.7 x 103
4.5 X 103
1.1 X 10*
1.6 X 10*
4.5 « 103
7.8 x 103
s.a x 10*
5.4 x 10?
4.S x 103
4.8 x 103
IWTE
LAND
•i9/9
ECOLOGY
N
N
2.0 x 101
9.0
N
N
K
tl
N
»
N
N
N
2.0 x 10'
2.6 x 10'
2.0 x !0'
2.0 x 101
2.0 * 10!
2.0 x 102
2.0 x 102
K
N
N
WHERE FOUND
IN
LEI/EL 1
SASS. LAB, C7
SASS, LAB. C9
SASS, LAB, CIO
GAS, FIELD, C5
SASS, LAB, C7
SASS. LAB, LC4
GAS, FIELD, C6
SASS, LAB, C7
SASS. LAB, C7
SASS, LAB, C9
SASS, LAB, CIO
SASS, LAB, Cll
SASS, LAB, LC4
SASS, LAB, C12
SASS, LAB, C7
SASS, LAB, C8
GAS, FIELD, C6
SASS, LAB, C8
GAS, FIELD, C6
GAS, FIELD, C6
SASS, LAB, LC6
SASS. LAB, ,LC6
SASS, LAB, LC6
SASS, LAB, C6
SAMPLE
u9/m3
a«/9
U9/1
W1Q
^E1
LEVEL 2
REOU1REO
Y*YES
N=NO
TEST
METHOD1
i
i
TEST
EXPEC-
TATIONS2
TEST
COST3
SAMPLE,
ALiQUOT*
TABLE KE»:
1. TEST *THOO
1. STANDARD
2. DEVELOP-
MENTAL
3. UNKNOWN
A. AAS
B. XflO
C. MET
CHEMICAL
D. ESCA
E. GC/HS
2. EXPECTED
TEST SUCCESS:
1. HIGH
2. MODERATE
3. UNKROMN
3. TEST COST
1. REASON-
ABLE
2. MODERATE
3. HIGH
t. SAMPLE
ALIQUOT
1. ADEQUATE
2. MARGINAL
3. INADEQUATE
4. RESAMPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
L*nl 1 fttta Reduction and Decision Charts (Continued)
00
CATEGORY
C. TERTIARY
ALCOHOLS
6. SLYCOLS,
EPOXIOFS
A. GLYCOLS
B EPOXIDES
7. ALDEHYDES,
ICETONE5
A. ALDEHYDES
B. KETONES
COMPOUND
PentOTlol s
(secondary)
2-81.0 x SO5
1.0 x 10* ,
>1.0 x 10S^
N
>1.0 x 106
n
1.0 x 10*
>!.0 x 10s
1.0 x 103
«
<1.0 x 10J
1.0 x 103
1.0 x 10*
N
1.0 X 102
N
1.0 x 1C3
N
N
N
•1.0 x 105
>1.0 x 105
N
11
H
N
MATE
LAND
US/ 9
HEALTH
1.1 x 10*
1.4 x 10*
3.0 x 10*
1.4 x 103~1
5.8 x 103
9.0 x 103
H
3.0 x 10J
1.1 x 10*
4.8 x 10Z
5.2 x 103
7.5
4.8 x 101
1.1 X 103
1 .8 x 103
3.3 x 103
5,4 i 103
1,2 « 10*
3,6 x 10r
7.5 x 102
1.2 x 1C3
7.2 x 10*
1.8 x 10*
N
N
N
N
MATE
LAND
»S/3
ECOLOGY
N
Z.Q x 10?
2.0 x 10
2.0 x ID?"
N
2,0 x 10J
N
2.0 x 101
2.0 * 102
3.0
n
2.0 x 10-'
2.0
2.0 x 10
n
1.0 x 10-'
N
2.0
N
N
N
>2.0 x 10?
>2.0 x 102
N
N
N
N
UHCRC FOUND
IN
LEVEL I
SASS, LAB, CS
|_ GAS, FIELD, C6
GAS, FIELD. CS
SIS, FIELD, C6
SASS, LAB, LCG
SASS, LAB, LC6
SASS, LAB, C11
SASS, LAB, C11
SASS, LAB, C8
SASS, LAB, CIO
GAS. FIELD, C5
6AS, FIELD, C3
BAS, FIELD, C5
SASS, LAB, CIO
GAS, FIELD, C6
GAS, FIELD, C4
GAS, FIELD, C6
SASS, LAB, LC4
SASS, LAB, LC4
SASS, LAS. LC4
GAS, FIELD, C5
6AS, FIELO, C6
SASS, LAB, Cll
SASS, LAB. LC4
SASS, LAB, LC4
SASS, LAB, LC4
SAMPLE
ug/m3
»«/9
us/1
RATIO
SAHPLE
HATE
LEVEL 2
REQUIRED
Y-YES
«*m
TKT
METHOD'
f ~ •
TEST
EXPEC-
TATIONS2
TEST,
COST1
SAHH.E.
ALIQUOT*
TABLE KEY:
1. TEST HETHOD
1. STANDARD
2. DEVELOP-
WINTAL
3. UNKMMN
A. AAS
B. XRD
C. UET
CHEKICAL
D. ESCA
E. GC/HS
2. EXPECTED
TEST SUCCESS:
1. HIGH
2. MODERATE
3. UNKNOWN
3. TEST COST
1. REASON-
ABLE
2. MODERATE
3. HIGH
4. SAHPLE
ALIQUOT
I. ADEQUATE
2. MARGINAL
3. INADEQUATE
4. RESAHPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reduction and Decision Crurts (Continued)
00
tn
CATEGORY
8. CARBOmiC ACIK
A. CARBOXVLIC
ACIDS
B. CABBOXYLIC
ACIDS U1TH
ADDITIONAL
FUNCTIONAL
C. ABIDES
D. ESTERS
g. NITRILES
COMPOUND
Hal el c
Phthal 1c
Formic
Acetic
Benzole
Long Chain
3-Hydroxypropanoic
Acid Lactone
B-Propiolactone
Hydroxybenzaic Aclij
Hydroxyacetlc Acid
6-Hevane1actam
Fonunride
Acetanlde
6-Aflrinc-hexano3c
Acid
Phthalates
Methyl Hethicry-
late
Adipstes
Methyl Benirate
Phenyl Benzoate
Di-2-ethylnexyl
ptithalste
Long chain esters
1-Cyanoethane
Tetr»«ethy1-
succlnonftrlle
Butyronltrile
Benionitrile
AcrylonitHle
Acetonltrlle
Kaphtlranttrlles
HATE
AIR
^g/m3 {ppn)
1.0 X 103 (O.ZS)
6.0 X 103 (1.0)
9,0 t 10J (5.0)
2.5 x 10* (10)
1.4 x 10*
N
3.17 x 102
3.2 x IOZ
«.01 x 104
8.78 x 10"
1.0 x 103
3.0 x 10* (ZO)
4,5 x 105
2.33 x 106
5.0 x !03
4.1 x 105 (100)
1.89 x W4
1.5 x K>5
N
N
«
1,76 x 103
3,0 x 103 (0.5)
E.Z5 x 104
3,24 x Id*
4.5 x 10< (20)
7,0 x 10* (40)
N
HATE
HATER
69/1
HEALTH
1,5 X iO*
9.0 ( 10*
3.4 x 10s
3.B x 105
2.1 x lo6
N
4.76 x 103
1.6 x 103
6.01 K 105
1.13 x 106
1.5 x 10*
4.5 x 105
6.75 x I06
3,5 x 107
7,5 x ID4
6.2 > 106
2.83 X 105
2.25 x 106
N
K
N
2.64 x 104
4.5 x 104
3.37 x 105
4.86 x I05
6.8 x 105
l.OS x 1fi6
N
NATE
MATER
ug/l
ECOLOGY
N
N
N
1.0 x 103
H
N
1.0 x 104
N
N
N
1)
It
N
N
1.5
1 .0 x 104
N
K
«
N
N
N
fl
N
N
1.0 X 103
1 .0 X 10s
H
HATE
LAND
-S/9
HEALTH
3.0 X 10'
1.8 x 102
Z.7 x I0?
7.6 x 102
4.2 x 103
N
9.6
3.2
1.2 x 103
2.6 11 103
3.0
9.0 x 10*
1.4 x 104
N
l.S x 102
1.2 x 10*
5.6 x 10?
4.6 x 103
N
«
N
5.4 X 10
9.0 x 10
6.8 x 102
l.t X 103
1.4 x 103
2.1 x 103
»
HATt
LAND
•-9/S
ECOLOGY
N
N
N
2.0
N
N
2.0 x 10
»
N
N
N
«
N
N
-3.0 x 10-3
2.0 x 10
II
tt
N
N
N
N
N
2.0
2.0 x 102
N
HHERE FOUND
IN
LEVEL I
SASS, LAB, C8
5ASS, LAB,
LC7 « 8
SASS. LAB, C8
SASS, LAB,
LC7 t 8
SASS, LAB, C8,
8 t LC7
SASS, LAB, CB,
3 1 LC7
SASS, LAB, CIO
SASS, LAB, C7
SASS, LAB, LC7
SASS. LAS, C7
SASS, LAB, LC7
r SASS, LAB, LC7
SASS, LAS, US
SASS, LAB. LC6
SASS, LAB, C7
SASS, LAS, C8,
9810
SASS. LAB, CIO
SASS, LAB, LC6
SASS, LAB, LC6
SASS, LAB, LC6
GAS, FIELD, C6
SASS. LAB. LC4
SASS. LAJ. LC4
SASS, LAS
SASS, LAS, C11
CAS, FIELD, C6
SASS, LAB. LC4
SAMPLE
US/"5
vl/9
van
RATIO
SAMPLE
HATE
=
LEVEL 2
REQUIRED
T'YES
h=«0
TEST ,
HETHOD1
»
TEST
EXPEC-
TATIONS2
TEST
COSTJ
SAMPLE
ALIQUOT
1
2.
J.
TABLE KEY:
1. TEST HETHOD
1. STABOASD
2. DEVELOP-
MENTAL
3. UNKNOWN
A. AAS
B. XRD
C. WET
CHEMICAL
0. ESCA
E. GC/MS
. EXPECTED
TEST SUCCESS:
1. HIGH
2. MODERATE
3. UNKNOWN
TEST COST
1. REASONABLE
2. MODERATE
3. HIGH
SAHPLE
ALIQUOT
1. ADEQUATE
2. MARGINAL
3. INADEQUATE
4. RESAMPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reduction and Decision Charts (Continued)
CD
(ft
CATEGORY
1<1. AMINES
A. PRIMARY
B. SECONDARY
C. TERTIARY
MINES
11. AZO
COMPOUNDS
COMPOUND
i-Afflinaiuphulene
Nethylamine
4-Affliniblphenyl
Etnanolanrfne
Butylaifflnes
Ethyl anijne
1,2-Diamlnoe thane
Cyclohexylamine
Propanolaflilne
3-Airinopro£ene
Ett>y1eneirajne
Dimethylanslne
MorphoHne
Dfethylanfne
EtnylroethylaminE
Anlnotolijenes
2-Aminonaptithjlenc
4,4l-Methylene-
b1s-(2-cliloro-
anlllne
AMsldlnes
4-Am1n1b1phenyl
1 ,4-Diurlnobenzene
3,3'-D1diloro-
benzidlne
Benzidfne
'Aniline
Dlwthylaniline
N,H-tH«tnyl-
anltlne
M'-DlrwthyV
hydrajine
Mnoetnyl-hydrazlne
Olazomethwie
N,H-01methyl-
hydnzlne
Hydrazobenzene
Diphcnjrlhydrazlnes
HydrazfM
HATE
AIR.
ug/n.3 (ppm)
5.5 x !02
1,81 x !03
1,2 x 103 (SO)
6.0 x ID3 (3)
1.5 x 10* (5)
1.8 x 10* (ibj
2.5 x 104 (10)
4.0 x 10* (10)
1.27 x 105
N
3.33 i 108
1.8 « 104 (10)
7.0 x 104 (20)
7.5 x 104 (25)
N
1.1 x 105
1.7 x ID2
2.18 x 102
5.0 x 102 (0,1)
1.3 x 103
4.5 x 103
6.6 x 103
1.4 x 104 -
1.9 x 10* (5)
2.S x 104 (5)
2.5 x 10* (5)
3.17 x 10
3.S x 102 (0.2)
4.0 x 10* (0.2)
1.0 x 103 (0.5)
! .35 x Id4
1.4 x 10*
N
WTE
WATER
ug/i
HSALTH
8,5 x I03
f.7? x 10'
1.8 x 10*
S.O x 10*
2.25 x ID5
2.? x 10s
3.75 x 10*
6.0 i 105
1.9 x 10«
N
5.0 x 103
2.7 x 105
l.OS x ID6!
1.13 x ifl*"1
N
1.7 x 103
Z.5 x 103
3.27 x 103
7.5 x 103
2.0 x 10*
6.75 x 10*
9.S x 10*
2.1 t 105
2.85 x 105
3.75 x !05
3.83 x 10s
4.76 x 102
5.25 x 103
6.0 x 1Q3
1.5 x 10*
2.0? x 105
Z.O x 105
n
HATE
HATER
US/1
ECOLOGY
.0 x 1D?
N
.0 x 103
.0 » 10*
> .0 x 105
.0 x 103
.0 x 103
.0 x 104
Pf
It
1.0 x !03
1.0 x 10"
1.0 x 103
N
N
1.0 x 1C2
K
N
N
N
N
1.0 x 102
1.0 x 103
N
N
H
n
N
H
N
N
N
MATE
LAUD
ug/g
HEALTH
3.6 x 10
1.8 x 10Z
4.5 I 10Z
5.4 x Id2
7.6 x 102
1.2 x 103
3.8 x 103
N _
1,0 x 10 .
5.4 x 10?
2.1 x 303
2.2 x 103
N
3.0
5.0
6.0
1.5 x 10
4.0
1.4 » 103
2.0 x 10?
4,2 x 102
6.0 x 10?
7.5 x 102
7.5 x 10Z
).o
1.1 x 10
1.2 x 10
3.0 x 10
4.0 x W2
mil
LAND
ug/fl
ECOLOGY
t.a
2.0 x 10
2.0 x 102
2.0
2.0
2.0 x 10
N
N
N
, 2.0
2.0 > 10
2.0
H
N
2.0 x 10-1
K
«
N
1— "
H
2.0 x 10"'
2.0
N
N
K
N
N
N
N
UHEitE FOUND
IN
LEBEL I
SASS, LAB, LC7
SASS, LAB, LC6
GAS, FIELD, C6
SASS. LAB, CIO
GAS, FIELD, C6
GAS, FIELD, C4
SASS, LAB, CS
SASS, LAB, CS
SASS. LAB, C9
GAS^FIELC^S
GAS. FIELD, C3?
GAS, FIELD, C3?
SASS, LAB, LC6?
OAS, FIELD, C3?
GAS, FIELO, W
SASS, LAB, Cll
SASS, LAB, LC6
SASS, Lfte, LC7
SASS, \M, Lee
SASS, LAB, LC6
SASS, LAB, LC6
SASS, LAB, LC7
SASS, LAS, LC7
SASS, LAB, Cll
SASS, LAB, Cll
SASS, LAB, LC6
OAS, FIELD, C6
MS. FIELD. C6
SAS, FIELD, C3
SASS, LA3, CS
SAS. FIELD. C6
SASS, LAB. LC7
SASS, LAB, C8
SAMPLE
ug/m3
u9/g
U9/1
RATIO
SAMPLE
-R5TT
LEVEL 2
REQUIRED
Y=YES
K«NO
TEST
METHOD1
TEST
EXPEC-
TATIONS2
_
TEST
COST3
!
SAMPLE
ALIQIXIT*
1.
2.
3.
4,
TABLE KEY:
TEST HETHOD
1. STANDARD
2. DEVELOP-
MENTAL
3. UNKNOWN
A. AAS
B. IRQ
C. OTT
CHENICAL
D. ESCA
E. GC/NS
EXPECTED
TEST SUCCESS:
1. HIGH
2. MODERATE
3. UNKNOWN
TEST COST
1. REASONABLE
2. MODERATE
3, HIGH
. SAMPLE
ALIOUOT
1. ADEQUATE
2. MAXIMAL
3. INADEQUATE
4. RESAHPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Seduction and Decision Charts (Continued;'
OO
-•4
CATEGORY
12. NITROSAMIES
13. MERCAPTANS,
5ULFIDES
A. MERCAPTASS
B. SULflDES
DISULF1DES
14. SULfONIC ACIDS,
. SULFOXIOES
A. SULFONIC
ACIDS
6. SULFOXIOW
COMPOUND
S-mtroso-
Dimethylasiine
K-Nltroso-
!H ethyl anrine
N-ltethyl-S-
NitrosoAm1l1ne
H-mtroso-Qi-
propylaime
N-mtroso-01-
phenylanine
N-Nltnreo-Oilso-
propylamine
N-Hitroso-01-
pentylamine
Perchloromethyl
Mercaptan
Hettiyl tercaptan
Ethyl Htrcaptan
Butyl Mercaptans
Benzwthlol
Propyl Mercaptans
l-Antt™th1ol
Dimethyl Sulfide
ptienyl Sulfide
Methyl Sulfide
Methyl Dliulfide
8enzensulfon1c
Atid
9,10-Anthraqui-
none-D4sulfon1c
Acid
Dimethyl Sulf oxide
HATE
AIR
ig/rn3 (ppm)
f
1.2 i
1
1.21 x IflZ
1.29 x 103
2.41 x 103
7.4 x 10*
3.83 x 10*
N
8.0 x 102 (0.11
1.0 x 103 (0.5)
1.0 x 103 (0.5)
1,5 x 103 (0.5)
2.07 x Io3
8.06 x 10*
N
Z.41 X 104
9.63 x 10*
H
«
4.01 x 10*
«
.8.14 x 102
WTE
HATER
-S/l
HEALTH i
1,8 J 10
1.92 x ID3
1 .94 x !0<
3.62 x 10*
1.1 l 10*
5.75 x 10s
1
1.2 x 10*
1.5 x 10*
1.5 x 10*
2.25 » 10<
3.10 x 10*
1.21 x 106
N
3.61 x 105 ^
1.44 x 106
N
N
6.01 x 105
N
1.22 x TO3
HATE
WATER
-g/1
ECOLOGY
It
N
N
N
S
N
N
N
N
N
N
N
n
It
n
B
N
N
N
N
»
WffE
L,WC
-9/9
HEALTH
3.6 x 10-2
3,6
3-8 X 10
7.2 > 10
2.2 x 10J
1.2 x 103
N
2.4 x 10
3.0 x 10
3.0 x 10
4.5 x 10
6.2 X 10
2.4 x 103
II
7.2 X 102
2.9
N
»
1.2 x 103
N
2.4
NftTE
LAND
-9/5
ECOLOGY
N
»
N
H
N
N
N
N
n
«
N
N
N
N
N
N
N
N
N
N
WHERE FOUND
IN
LEVEL 1
5ASS, LAB. C9
SASS. LAB. CIO
SASS, LAS. IC5
SASS, LAB, C12
i LCS
SASS, LAB, LCS
SASS, LAB. Cll
SASS, LAB, LCS
SASS, LAB, LC6
GAS. FIELD, SGC
GAS, FIELD. S6C
MS, HELD, SQC
SASS, LAB, LC6
GAS. FIRD. SGC
SASS, LAB, LCS
GAS, FIELD, SGC
SASS, LAB, C9
t LCS
GAS, FIELD, SGC
SASS, LAB. C3
SASS. LAB. LCS
SASS, LAB, LCS
SASS, LA6, Cll
SAMPLE
ag/m3
uJ/9
H9/1
„
RATIO
SAMPLE
NATE
LEVEL 2
REQUIRED
V=VES
N-NO
TEST
HETHOO1
TEST
, EXPEC-
• TATIONS*
^ ~1
TEST ' SAMPLE,
cosT3 ; ALiouor
i
i
!
!
1
TABLE KEY:
1. TEST METHOD
1. STANDARD
2. DEVELOP-
MENTAL
3. UNKNOWN
A. AAS
B. XRD
C. MET
CHEMICAL
D. F.SCA
E. GC/MS
2. EXPECTED
TEST SUCCESS:
1. HIGH
2. TODERATE
3. UNKNOWN
3. TEST COST
1. REASON-
ABLE
2. MODERATE
3. HIGH
4. SAMPLE
ALIOUOT
1, ADEQUATE
2. MARGINAL
3. INADEQUATE
4. RESAMPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reduction and Decision Charts (Continued)
00
00
CATEGORY
1$. BENZENE,
SUBSTITUTED
BENZENE
16. HALOGENATED
AROMATIC
HYDROCARBONS
A. RING
StflSTITUED
AROMAT1CS
COMPOUND
Biphenyl
Benzene
Terphenyls
Indene
Isopropyl Benzene
THmethyl Benzenes
Dlhydronaphtha-
lenes
Tetrahydro-
naphthalenes
Pfopy) Benzene
Dialkyl -Benzene
Butyl Benzene
Indane
Toluene
Styrene
Ethyl Benzene
Xylenes
4.41-Ofplsenyl-
biphenyl
Tetrmetnjrl
Benzenes
Polychlorlnated
b-tpnenyls
Polychlorlnited
Chloronaphthalenes
2-Chlorotol uene
1,2-D1chloro-
benzene
Cnlonbenzene
1.4-Wchloro-
bertzene
MATE
AIR
yg/n3 (ppm)
1.0 X 103 (0.2)
3.0 x 103 (10)
9.0 x 103 (1)
4.5 x I01 (10)
6.3 x 104
1.2 x 10s (25)
1.27 x 105
1.29 x 10s
2.17 x I05
2.25 x 10S
2.25 x 10s
2.3 x 106
3.75 x 10s (100)
4.2 x 105 (100)
4.35 x 10$ (too)
4.35 x 106 (100)
N
n
5.0 x 102
3.4 x 10*
6.93 x 10*
2.5 x 10s (50)
3.0 x 105 (50)
3.5 x 105 (75)
4.75 x 105 (76)
MATE
HflTiR
ug/1
HEALTH
1.5 x 104
4.5 x 10«
1.35 x 105
6.6 x 10s
9.45 x 105
1 .8 x 10*
1.91 x 106
1 .94 x 106
3.2S x 106
3.38 x 106
3.38 x 1C6
3.4 x 10«
5.63 x 106
6.3 x SO6
6.53 x !06
6.53 x 106
*
H
7.5 x ID3
5.1 x 105
1.04 x 106
3.75 x 10*
4.5 x lO6
6.J5 x 106
6.8 x 10*
HATE
WATER
ug/l
ECOLOGY
II
1.0 103
1.0 103
4.5 102
1.0 x 103
1.0 x 103
1.0 x 103
1.0 x 103
N
N
1,0 x 103
1.0 x 103
1.0 x 1C3
1.0 x ID3
N
1.0 x 104
5.0 x 10-3
1.0 x 10Z
N
N
1.0 x ID*
1.0 x ID?
1.0 x 10*
HATE
LAND
HEALTH
3.0 x 10
9.0 x 10
2.8 x 10Z
1.4
1.9 x 103
3.6 x 103
4.0 > 103
4.0 x 103
6.6 x ID3
6.8 x 103
6.8 x 103
6.8 x 103
1.1 x 10*
1.3 x 104
1.3 x ID4
1.3 x 10*
N
N
1.0 x 103
1.5 x 10
7.5 x 103
9.0 x 103
1.1 x 104
1.4 x 104
MATE
LAND
ECOLOGY
H
2.0
N
N
2.0
N
2.0
2.0
2.0
2.0
N
N
2.0
2.0
?.o
2.0
N
2.0 x 10
2.0 x 10-'
1,0 x 10-5
N
2.0 x 10-'
2.0 x 10-'
2.0 x 10-1
HHESE FOUND
III
LEVEL I
SASS, LAB, LC2
GAS. FIELD. C6
SA5S, LAB, LC3
SASS, LAB, LC3
SASS, LAB, C9
SASS, LAB, CIO
SASS, LAB. LC2
SASS, LAB, CU,
LC2
SASS, LAB, C9
SASS, LAB, CIO.
11, 12
SASS, LAB, Cll
SASS, LAB, LC2
SASS. LAB, C8
SASS, LAB, C9
SASS, LAB, C8
SASS, LAB, C9
SASS, LAB, LC2
t 3
SASS, LAB, Cll
SASS, LAB, LC2
t 3
SASS, LAB, LC2
SASS, LAB, LC2
1 3
SASS. :AB. CO
SASS, LAB, CIO
SASS, LAB, C8
SASS, LAB, CIO
SAMPLE
ug/m'
RATIO
SAHPLE
HATE
LEVEL 2
REQUIRED
Y-YES
N=NO
TEST
METHOD1
TEST
EXPEC-
TATIONS?
TEST
COST3
SAMPLE
ALIQUOT*
TABLE KEY:
TEST METHOD:
1. STANDARD
2. DEVELOP-
MENTAL
3. UNKNOVfH
A. AAS
C'. WET
CHEBICAL
D. ESCA
E. GC/KS
. EKPECTEO TEST
SUCCESS:
1. HIGH
2. MODERATE
3. UHKNOUS
:. TEST COST
1, REASON-
ABLE
^. MODERATE
3. HIGH
I. SAMPLE
AUQUOT
1. ADEQUATE
2. MARGINAL
3. INADEQUATE
4. RESAWLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reduction and Decision Charts (Continued}
00
IO
CATEGORY
B. ARCMATICS
WITH HALO-
GENERATED
ALKYL SIDE
CHAINS
17. AROMATIC
NITRO
13. PHENOLS
A. MONOHYMUCS
COMPOUND
&n»no and
Qibroraobenzenes
Broiwchloro-
benzenes
1 ,3-Ofchlonj-
benzene
a-Chloro toluene
Bls-lchloromsthyl)
Benzene
4-N1trob1phenyl
D1nitroto>uenes
Jtetrqxynitro-
bgnzene
Nitrobenzene
l-CMoro-2-
mtrobMzene
t-Chloro-4-
N1 trobenzene
HHrotoluenes
Z.Z'-Olllydroxy-
dlphenyls
Polyalkyl
Phenol:
Phenol
CreScls
Phenyl Phenols
Alkyl CresoU
2-HetKoxy Phenol
Xylenols
Ethyl phenols
MUTE
AIR
ug/niS (ppm)
K
N
K
5.54 x 10*
N
1.3 x 103
1.50 x 103
4.5 x 103
5.0 X 103 (1.0)
1.3 x 10*
1,89 x 104
3.0 x 10» (it
6.75 x 103
1.49 x 10*
1.9 x 104 (5)
2.2 X 104 (5)
2.3 X 10*
2.39 I 104
3.26 X 10*
1.3 X 10*
K
HATE
WATER
jgyi
HEALTH
N
N
»
8.31 x 10*1
N
2.0 x ID4
J.25 x 10*
«,75 x 104
7.5 x 10*
1.95 x 105
2.84 x 105
4.5 x 105
5.0
5.0
5.0
5.0
5.0
5.0
S.O
5,0
5,0
HATE
WATER
aa/1
ECOLOGY
N
II
n
1.0 x 10?
N
N
1.0 x 103
N
1.0 x 103
1.0 x I04
•1
1.0 x 103
5.0 x ID?
S.O x 102
5.0 x }(?
S.O x Iff
5.0 x 102
5.0 x 10^
S.O x 102
5.0 x 102
5.0 x 102
HATE
LAND
ag/s
HEAtTH
N
N
N
K
4.0 x 10
4.5 x 10
1.4 > 10?
1.5 x 10?
4.0 x 102
5.8 X 10?
9.0 x 10?
1.0 « 10-2
1 .0 x 10-2
1 .0 x 10-J
1.0 x 10-2
1.0 x 10-!
1.0 x 10"z
1.0 x 10-2
1.0 x 10-2
1.0 x 10-2
HATE
LAND
ig/g
ECOLOGY
n
N
N
N
2.0
N
2.0
2.0 x 10
N
2.0
1.0
1.0
1.0
1.0
.0
.0
.0
.0
.0
WERE FOUND
IN
LEVEL 1
SASS, LAB, C9,
12. S LC2
SASS, l»B, C12
1 LCe
SASS, LAB, CIO
SASS, LAB, C11
SASS, LAB, LC2
SASS, LAB, LC4
SASS, LAB, LC5
SASS, LAB, LC5
SASS. LAB, C12
1 LC4
SASS, LAB, LC4
SASS, LAB, LC4
SASS, LAB, LC5
SASS, LAB, LC6
SASS, LAB, LC6
SASS, LAB, Cl!
SASS, LAB, C12
* LC6
SASS, LAB, LC6
SASS, LAB, C12
& Lee
SASS. LAB. LC6
SASS, LAB, LC6
SASS, LAB, LC6
SAHPLE
ug/m3
ag/9
ft/I
RATIO
SAMPLE
TKTT
LEVEL 2
REQUIRED
V=YES
N-NO
TEST
METHOD1
TEST
EXPEC-
TATIONS2
T£Sr SAMPLE
COST3 ALIQUOT4
•
\
|
1
i
j
TABLE KEY:
1. TEST METHOD
1. STANDARD
1, DEVELOP-
MENTAL
3. urra.wi,
A. AAS
g. XRD
C. WET
CHEHICAL
0. ESCA
E. GC/MS
2. EXPECTED TEST
SUCCESS:
1. NIGH
2. MODERATE
3. UNKNOUN
4. T£ST COST
1. REASON-
ABLE
2. MODERATE
3. HIGH
4. SAHPLE
ALIQUOT
1. ADEQUATE
2. KARGIKAL
3. INADEQUATE
4. RESAMPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reduction and Decision Charts (Continued)
CATEGORY
B. DIHYDRICS.
POLYHYDRICS
C. FUSED RING
HYDROXY
COMPOUNDS
19. HALOPHENOLS
20. NITROPHENOLS
21. FUSED
AROMATIC
HYDROCARBONS
COMPOUND
1,4-Othydroxy-
beiuene
Cltehol
1,2,3-THtiydriJxy-
benzenes
1,3-Dihydroxy-
benzene
l-ruphthol
2-Hafitithol
Indanols
Phenanthrols
Acenaphthenols
2-Hydroxyfluorene
2-Hydroxyd 1 benzo-
furan
Pentacnlorophenol
Chlorinated Cresols
2,4-Dichloro$>henol
2-Chlorophenol
Trlnltrophenol
Oinitro-o-cresol
D1nitro-p-creso1
Dinitrophenols
4-Nitrophenql
3-Nltrnpnetiol
2-Anino-4,6-
N1 trophenol
2-N1trophenol
BenzoU)pyrene
D1benzo{3,n)
anthracene
7,12-Dtmethylbeni-
(a)-anthracene
D1benzo(a.j)pyrene
NATE
AIR
ug/m3 (ppm)
2.0 x 103
2,0 x 10* (5)
3.55 x 10«
4.5 x 10* (10)
1.17 x 10s
1.09 x 10s
1.46 x 10*
H
N
N
tl
5.0 x 10?
2.25 x 10*
7.0 » 103
3.02 x 10"
1.0 x 10J (0.011)
2.0 x 102 (0.025)
6.8 x 10?
1.35 x 103
1.53 x 104
2.01 x 104
4.64 x It)4
S.8 x 10"
2.11 x 10-2
9.27 x 10-2
1.6 x 10-'
4.3 » 10
WTE
HATER
MS/!
HEALTH
5.0
5.0
5.0
5.0
s.o
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
r~ s.o
5.0
5.0
5.0
5.0
S.O
5.0
5.0
S.O
3.17 x 10-' ,
1.39
3.91
6.5 x 102
HATE
HATER
»9/n
ECOLOS*
5.0 x 10?
5.0 x 102
S.O x 10?
5.0 x 102
"s.O x 10?
S.O x 10?
5.0 x 10?
5.0 x 102
6,0 x 102
S.O x 102
5.0 x 1112
5.0 x 10?
5.0 x 10?
5.0 x 102
5.0 x 102
5.0 x TO*
5.0 x 10^
5.0 x 10Z
5.0 x 102
5.0 x 10Z
5.0 x 10?
5.0 x 10*
5.0 x 102
N
H
N
n
MUTE
UNO
w/g
HEALTH
1 .0 x 10-2
l.C x 10-2
1 .0 x 10-2
1 .0 x 10-2
1.0 x 10-2
l.C x 10-2
l.C x 10-2
1.0 x 10-2
1 .0 x 10-2
1 .0 x 10-2
1 .C x 10-2
1 .0 x 10-2
l.C x 10-2
l.C x 10-2
1 .0 x 10-2
1 .0 x 10-2
1 .0 x 10-?
1 .0 x 10-2
1 .0 x 10-2
1.0 x 10-2
1 .C x 10-2
1.0 x 10-2
6.0 x 10-2
3.0 x 10-3
8.0 x 10-3
•-.3
HATE
LAND
U9/9
ECOLOGY
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.D
N J
N
N
WHERE FOUND
IS
LEVEL I
SASS, LAB. LC6
SAK, LAB, LC6
SASS, LAB, LC6
SASS, LAB, CIO
SASS, LAB, LC6
SASS, LAB, LC6
SASS, LAB, LC6
SASS, LAB, LC6
SASS, LAB. IC6
SASS, LAB, LC6
SASS, LAB, LC6
SASS, LAB, LC7
SASS, LAB, LC6
SASS, LAB, CI2
SASS, LAB, CIO
SASS, LAB, LC7
SASS, LAB, LC7
SASS, LAB, LC7
SASS, LAB, LC7
SASS. LAB, LC7
SASS. LAB, Cll
S LC7
SASS, LAB, LC7
SASS, LAB, C12
t LC7
SASS, LAS, LC3
SASS, LAS, LC3
SASS, LAB. LC3
SASS, LAB, LC3
SAMPLE
u9/m3
u9/g
ug/1
RATIO
^
LEVEL 2
REWIRED
Y-rES
N»NO
TEST
NETKOC1
TEST
EXPEC-
TATIONS2
TEST
COST'
SAMPLED
ALigUOT4
TABLE KEY:
TEST METHOD:
1. STANDARD
2. OEVELOP-
fEKTAL
3. IMKNOUN
A. AAS
B, MB
C. HET
CHEHICAL
D- ESCA
£. SC/KS
EXPECTED TEST
SUCCESS:
1. HIGH
2. MODERATE
3, UNKNOWN
. TEST COST
1. REASON-
ABLE
2. MODERATE
3. HIGH
. SAMPLE
ALIQUOT
1. ADEQUATE
2. MARGINAL
3. INAOEOUATE
4. RESANPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reduction and Decision Charts (Continued)
CATEGORY
COMPOUND
9.10-Oiaethyl-l .1
2-benzanthracene
Qen*(a)anthracene
Nbenzotb.def)
Chrysene
Beniolg.h.D
perylene
>ibenzo(a,Opyene
*t«nanthreBe
Nethylctirysenes
Chrysene
Plcene
Benzo(e)pyrene
D1benzQ(a,h)pyrene
Dtbenz{a,c)
anthracene
l,J;3,*-Dibenio-
anthracene
BenzoCgJchrysene
flenzci(c)ph«n-
anthrene
Methylphefi-anthrene
naphthalene
Anthraune;Methyl
Anthracene
KmoiUyl
Naphthalenes
Dimethyl
tephthalems
Pyrene
Plwnyl Naphtha-
lenes
Acenaphthene;
Acenaphthylene
J,7-0(mcthy1-
anthracene
Ktphthacene
TMphenylene
HATE
sg/m3 (ppnO |
,96 x 10
4.45 x 10
.32 I 102
5,43 x 10*
.08 x ID3
.59 x 103
\.n x io3
z.z x ia3
2.S x 103
3.04 x !03
3.68 x IO3
9.9 x Id3
1.0 x IO4
1.63 x 10*
2,69 x ID4
3.04 x 10'
5,0 * 10*
5.6 x 10*
2.25 x 10^
2.25 x 105
2.33 > 10s
It
N
N
N
N
NATE
MATER
ug/1
HEALTH
4.44 x IO2
6.72 x !02
4.98 x 103
8.15 x 103
1.6? x 103
2.39 x 10*
2.69 x 104
3.3 x 10*
3.75 X 10*
4.S6 x 104
5.52 x IO4
1.5 x IO5
1.5 » IO5
3.45 x ID'
4.04 x 10s
4.56 x 105
7.5 x 105
8.4 x IO5
3.38 x 106
3.38 x IO6
3.5 x 1<)6
N
N
«
Ij
. X
HATE
HATED
«9/l
ECOLOGY
K
14
N
tl
N
N
N
N
N
X
K
N
N
N
N
N
1.0 X 102
N
N
N
N
N
N
N
N
a
NATE
LAND
»S/9
HEALTH
1.3
N
N
3.2 x 10
4.S x 10
5.4 x 10
6.6 x 10
7.5 x 10
9.1 x 10
1.1 x 102
3.0 x 1C2
4.8 x IO2
8.2'x Id2
9.1 x 102
1.5 x 103
1.7 x 103
6.8 » 10J
6.8 x 103
6.9 x 103
N
N
»
N
N
NATE
LAND
"9/9
ECOLOSY
ft
K
N
«
N
N
ft
tt
N
N
N
N
K
H
Z.O x 10-1
1
N
N
It
N
N
K
h
N
UHERE FOUND
IN
LEVEL I
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SBSS. LAB, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAS, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAS, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAB, Cll
& LC2
SASS, LAB, LC3
SASS, LAB, LC2
SASS, US, LC2
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAS, LC3
SASS, LAB, LCS
SASS, LAB, LC3
SAMPLE
rt/»3
M9/»
U9/1
RATIO
SAMPLE
-rorr
LEWL 2
REQUIRED
Y'TES
N-NO
TEST
METHOD1
1
T
TEST
1 ESI>EC-,
I TAT10MS2
1
i
i
TEST
COST3
!'
• SAMPLE.
; ALIQUOT4
TABLE KEY:
1. TEST HETHOD
1. STABOARC
2. DEVELOP-
WNTAL
3. UNKNOWN
A. AAS
B. XRD
C. MET
CHEHICftL
D. ESCA
£. GC/MS
2. EXPECTED TEST
SUCCESS:
1. HIGH
i. MODERATE
3, UKCH1WN
3. TEST COST
1. REASON-
ABLE
2. HOOERATE
3. HIGH
4. SAMPLE
ALIQUOT
1. ADEQUATE
2. MARGINAL
3. INADEQUATI
4. RESANPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reduction and Decision Charts (Continued)
VD
INJ
CATEGORY
22. FUSED RW-
ALTERHATE
POLrc»CLIC
KYOTOCARBOHS
COMPOUND
1-Hethyl Pyrene
Dimethyl Pyrenes
1,2 BenzMpntM-
cene
Peryleae
Coronene
3-Methyl-
Uolanthrene
Benzo(b)
flinranthene
Benzol k)
fluorantftene
Indeno(1.2.3.c.d)
pyrene
flMzo(4 )
fluoranthene
I,2:S,6-D1l>«ira-
fluorene
Dlcyclopentadtew
Indaiw, Indene
Fluoranthene,
(Tetrafcyd™-
flWH-Mnthene)
Fluorwne
Cyclopentano-
napnthalMW
2,3-Benzofluor-
ene
1,2-Benzofluorene
Cyclopenta(def}-
phenwithrww
Trux«neCrrit*nzyl-
ew Dnzew)
MATE
AIR
ug/n.3 (ppn)
N
H
H
V
H
3.75
8.97 x 1C2
1.63 x 103
1.63 x 103
6.48 x 103
l.X x 104
J.S9 x ID4
4.5 x lO'HlO)
9.0 » 104
H
N
H
N
N
N
HATE
MATEB
!.«/«
HEALTH
N
N
II
N
N
5.63 x 10
1.35 x 104
2.45 x ID4
2.45 < 104
9.72 » 104
1.9B x ID5
2.39 x 10*
6.75 x 10s
1.35 x Id5
a
N
N
N
N
•
NATE
HATER
uq/t
ECOLOGY
K
H
N
H
N
„
«
»
N
»
N
1.0 x 10Z
N
N
N
N
,
N
N
N
KME
LAND
W9/9
HEALTH
K
K
N
H
H
1.1 K 10"1
2.8 x 10
4.9 x 10
4.8 x 10
2.0 x 102
4.0 x 10Z
4.B x 10Z
N
2.8 x 103
N
K
K
It
N
N
MATE
LAUD
ug/g
ECOLOGY
K
K
N
H
K
N
N
N
N
*
N
Z.O X 10"*
K
H
N
N
N
N
N
N
WERE FOUND
IN
LEVEL I
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS. LAB, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAB, LC3
SASS, LAB, CIO
SASS. LAB, Cll
SASS. LAB, LC3
SASS, LAB, LC2
SASS, LAB, LC2
SASS, LAB, LC3
SASS, LAB. LC3
SASS, LAB. LC3
SASS, LW, LC3
SAMPLE
ug/ra3
P9/9
BS/1
BAT 10
SAMPLE
HAYE
LEVEL 2
REQUIRED
Y-YES
H'NO
TEST
METHOD1
TEST
EXPEC-
TATIONS'
-
TEST-
COST3
1
swu.
ALIQUOT4
TABLE KEY:
1. TEST METHOD;
1. STAHDARD
2. DEVELOP-
MENTAL
3. UNKNOWN
A. AAX
B. XRD
C. MET
CHEMICAL
D. ESCA
E. GC/MS
2. EXPECTED TEST
SUCCESS:
1. HIGH
2. MODERATE
3. UNKKOyN
3. TEST COST
1. REASON-
ABLE
2. MODERATE
3. HIGH
4. SAMPLE
ALIQUOT
1. ADEQUATE
2. MARGINAL
3. INADEQUATE
4. RESAHPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Seduction and Decision Charts {Continued)
IO
OJ
CATEGORY
23, KETEROCYCLIC
NITROGEN
A. PVRIOINE S
PYR1DINES
B. FUSED
S-MENBERED
C. PYRROLE AND
RFN5
DERIVATIVES
1
COMPOUND
Pyrtdlne
D1 & pclysubsti- ;
tutfrd pyridlnes
PfcoHnes
Chloropyridlne
CollidiiKS
htodosutistttuted
Alky! Pyridlnes
Dibenzd.h)
acridine
DUienzU.j)
acridine
Benz(c)«ridine
Qulnollne-,
IsoqufflOllne
D1benz{c,n;
acridine
Nithylqulnollnes
Acridine
Dlmethylqulnollnes
Dlhydrojcridine
Benzo(c}qu1nal1n
Benzo(f)qufnol1fie
Benza(rt)qutao1ine
Benzo(a)acrid1ne
Oibetiz B-Indeno
(1 ,Z-cOqiiinol1ne
Indeno (1,2,3,1,.!)
Isoqulnollne
01t.enzo(c,d)
carbazole
Pyrrole
Oibmzo(a.g)
carbwole
rnttole
HATE
AIR
u5/iii3 (pp.)
l.S « 10* (S)
2,7 x 104
3.56 x 10*
4.32 x 103
S.9 x 104
M
2.24 i 102
2.47 x 10Z
!.l s 10*
1.58 « 10*
2.33 X 10*
5.54 X 104
9.0 X 104
II
V
It
B
B
11
N
»
1.05 X ID'
2.75 X 103
6.03 X 103
1.1 )[ 104
1
MUTE
HATER
»9/l
HEALTH
2.25 x 10s
4.05 X 105
5.34 x 10B
7.23 » 104
1.0 x 106
B
3.36 x 103
3.71 x 1Q3
1.6 x 10s
2.37 x 106
3.5 x 105
8.31 x 10s
1.4 » 106
N
N
N
N
- N
N
N
N
1.5B x 103
4.13 x ID*
9. OS x 1C4
1.7 x 105
HATE
UATER
ECOLOSY
1.0 x 10*
N
N
N
N
N
N
N
K
N
N
N
n
N
N
K
»
N
N
N
N
A
N
N
N
HUTE
LAND
U9/9
HEMTK
4.5 x 10?
8.2 x 102
1.1 x 103
1.4 x 102
2.1 x 103
N
6.7
7.4
3.2 x 10*
4.7 X 102
6.9 » ID2
1.7 x 103
2.7 x 103
N
II
N
N
N
N
N
N
3.0
S.I x 10
1.8 x 102
3.3 x 102
MATE
LAND
u«/«
ECOLOGY
2.0 x 10
N
N
N
N
n
"
N
H
N
N
N
N
n
N
N
n
H
N
N
.'1
H
N
N
N
UHERE FOUND
IN
LEVEL 1
SASS, LftB, C8
SUSS, LAB, CIO
SASS, LAD, CG
SASS, LAS. C9
i CIO
SASS, LAB, C8
SLC3
SASS, LAB, LC3
SASS, LAB, LC6
SASS, LAB, LC6
SASS, LAB, LC6
SASS, LAB, U6
SASS, LAS, LC6
SASS, LAS, LC6
'SASS, LAB, LC6
SASS, LAB, LC6
SASS, LAB, LC6
SASS. LAB. LCS
SASS, LAB, LC6
SASS, LAB, LC6
SASS, LAB, LC6
SASS, LAIS, LC6
SASS, LAB, LC6
SSSS, LAB, LC6
SASS, LAB, LC6
SASS, LAB, LC6
SASS, LAB, LC6
SAMPLE
uj/m5
US/8
«g/l
RATIO
SAMPLE
NATE
LEVEL 2
REQUIRED
V-YES
N=NO
TEST .
HETHOD1
TEST
EXPEC-
! TATIONS2
i
TEST
CDST3
!
SAMPLE
ALIQUOT"
;
;
TABLE KEY:
1, TEST METHOD:
1, STANDARD
2. DEVELOP-
MENTAL
3. unKKOWN
A. AAS
B. XRD
C. KEt
CHEMICAL
D. ESCA
t. SC/MS
2. EXPECTED TEST
SUCCESS:
1. HIGH
2. MODERATE
3. UNKNOWN
3. TEST COST
1, REASON-
ABLE
2. MODERATE
3. HIGH
4. SAMPLE
ALIQUOT
1. ADEqUATE
2. HAR5INAL
3. INADEQUATE
4. RESAKPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reduction and Decision Charts (Continued)
vo
CATEGORY
D. NITROGEN
containing
ADDK't HETEROATOHS
24. HETEROCVCIIC
25. HETETOCVCLIC
SULFUR
26. ORSAJiO-NETAUlCS
A. M.KYL or
AKYL
COMPOUND
Dibenzo(a.i)
carbazole
Benzo(a)
carbazole
Carbazole
Methylfndoles
BenzotMazole
Methyl
BenztMazoles
Tetrahydrofuran
Furan
Berzofuran
Dibanzofuran
Methyldlbenzo-
furanes
Naphthofurans
Benzo(b)naphto
(2,3-d)furan
Pnenoantnro(9,
10-b)furan
1.9-Beniox-
antftene
Benzonaphtho-
thlopene
Thiophene
Metnylthlopnenes
B«flzo(b)th1op)iene
Dlmethyl-
tlrlopnenes
Trf; TetraacUiyl
thlophenes
2,2-Bithiophene
Dlbenzthlopnene
Alkyl Mercury
Tstraethyl Lead
Orjanotln
Tetramethyl Lead
Organogernanes
Trlmethyl Arslne
MATE
AIR
ug/«3 SPP»)
1.15 x 10*
1,89 * 10*
2.25 x 10*
4.5 x 10*
a. 28 x 103
4.73 x 103
5.9 x 105 (200!
H
li
n
N
N
N
N
«
9.86 x 10Z
4.5 > 103
2.25 x 10*
2.30 x 10*
N
N
H
K
1.0 I 10 (.001)
1.0 I 102 (.0075)
1.0 x 10?
l.S x 102 {.014!
J.15 x 10*
N
HUTE
WATER
ug/1
HEALTH
1.73 x 10*
2.84 x 10s
3.38 « II)5
6.75 x 10*
6.42 x 104
7.10 x 10*
6.85 x 10<
N
K
n
N
N
K
li
N
1.48 x 10*
6.75 x 10*
3.38 x ID*
3.45 x 10s
N
»
»
N
1.6 x 102
1.6 x 103
1.0 x IflJ
2.25 x 10'
4.73 x 105
N
WTE
WATER
ECOLOGY
N
N
N
N
N
N
N
K
It
It
K
H
II
K
N
II
K
K
N -
N
N
N
N
2.0 x 10-*
«t.5 x 101
N
H
N
"
WTE
LAND
ug/9
HEALTH
3.6 x 102
5.6 x ID?
6.8 x 102
1.4 x 103
6.9 x 10*
1.4 i 102
1.8 x 104
II
N
K
N
N
N
"
N
3.0 I 10
1.4 x 102
7.0 x 1&
7.0 x 102
N
N
N
N
3.0 x 10-1
3.0
4.5
9.4 » 102
NATE
LAND
"t/1
ECOLOGY
N
N
N
N
N
N
N
N
N
II
N
N
N
N
N
N
II
N
H
N
»
N
N
4.0 x 10-5
N
N
N
N
WERE FOUND
[N
LEVEL I
SA5S, LAB, LC6
SA5S, LAB, LC6
SASS, LAB, LC6
SASS, LAB, LC6
SASS. LAB, LC6
SASS. LAB, LC6
SASS, LAB, LC5
GAS, FIELD, C5
SASS, LAB, CIO
SASS, LAB, LC5
SASS, LAB, LC5
SASS, LAB, LC5
SASS, LAB, LC5
SASS, LAB, LC5
SASS, LAB, LC5
SASS. LAB. LC4
GAS. FIELD, CS
SASS. LAB. CB
SASS, LAB. LC4
SASS, LAB, C9
SASS, LAB, CIO
SASS. LAB, IC4
SASS, US, LCI
GAS, FIELD. C6
SASS, LAB, C12
and LCI
_a&+2ttffij*
SASS. LAB. C7
SAS. FIELD. C6
GAS, FIELD. CS
SAMPU
ug/"5
ug/g
ug/l
RATIO
SAKPLE
TtSTT
LEVEL 2
REQUIRED
Y=¥ES
H--WJ
TEST
METHOD1
~]
TEST
EXPEC- |
TATIONS2 i
1
J
TEST
COST3
SAWPLE
ALIQUOT*
TABLE KET:
TEST METHOD:
1. STANDARD
2. DEVELOP-
MENTAL
3.
A. AA5
B. XRD
C. KET
CHEMICAL
D. £SCA
E. GC/MS
EXPECTED TEST
SUCCESS:
1. HIGH
2. MODERATE
3. UNKNOWN
. TEST COST
1. REASON-
ABLE
?. WOOERATE
3. HIGH
. SAMPLE
ALIQUOT
1. ADEQUATE
2. MARGINAL
3. INADEQUATE
4. RESAMPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
L««el 1 tata Reduction and Decision Charts (Continued)
10
CATEGORY
B, SANDHICH
C. HETAL
PORPHYMIS
CHEUTES
COMPOUND
Nickelocene
Ferrocene
D1 benzene
chranium
Caaiplexed
Copper
Complexes
Nickel
Completed Iron
Complexed Tin
Complied Zinc
HATE
AIR
ug/«3 (ppnj
3.5 x 103
5. 84 x 10*
3.52 i 103
N
N |
pi
N
HATE
HATER
1.3/1
HEALTH
5.25 » 10*
8.91 x lt|5
5.28 « I0<
H
«
!i
N
HATE
WATER
u9/)
ECOLOGY
N
N
N
'
N
N
N
HATE
LAND
HE$H
1.0 x 102
1.8 i 103
9.0 x 10
N
N
X
N
MATE
LAM)
ag/g
ECOLOGY
N
"»
N
»
N
H
II
WHERE FOUND
lit
LEVEL I
SASS.LAB.LC4
GAS.FIELO.ce
SAMPLE
t9/3
»g/l
RATIO
^
tElfEL 2
REQUIRED
V«fE5
S=NO
TEST
METHOD1
1
: TEST
• EXPEC-
. TATIONS2
1
i
i
i
. TEST
! COST
•
1
1
1 SAHPLE,
ALIQUOT*
i
"
TABLE KEr:
, TEST METHOD:
1. STANDARD
Z. DEVELOP-
HENTAL
3. LINK NOUN
A, MS
8. IRQ
C. HET
CHEMICAL
0. ESCA
E. GC/HS
. EXPECTED TEST
SUCCESS:
1. HIGH
2, HODEB5TE
3. UNKKOHN
. TEST COST
!. REASON-
ABLE
1. MODERATE
3. HIGH
. SAMPLE
ALIQUOT
1- ADEQUATE
2. MARGINAL
3. INADEQUATE
i. BESAHPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Dm Seduction and Decision Charts (Continued)
CATEGORY
27. LITHIUN
29. SODIUM
29. POTASSIUM
30. RUBlDIun
31. CESIUM
32. BERYLLIUM
33. HASHES [UH
34, CALCIUH
COMPOUND
Li
Li*
L1F (as LI)
LljCOj (as Li)
UH
Hi*
KiOH
ROH
K
K+ (as K)
R6*'
cs*i
Be
Be**
8eO (as 8e)
SeO-AljOvSIOj
(« 84
Hagnesiun, Hg
Hagnesfun Ion, Mg**
Magnesium Oxide.
MgO
Magnesium Fluoride,
H9F2 (as Mg)
Magnesiun Sulfite,
KgSOi (as Kg)
Kagnesite, HgC03
(as Ms)
Dolomite, HgCOs-
CaC03 (as HsJ
Asbestos (as Hg)
Calcium loo, Ca*4
Ciicltm Fluoride,
Cafj
Calcium Carbonate,
CaOOs
Calcfun Sulfitc,
CaSDa
Dolomite', HgCOs-
CaCOj
MATE
AIR
*g/m3 (ppm)
2.2 x 10
2.2 x 10
2.2 x 10
2.2 x 10
2.5 x 10
5.3 x 10s
2.0 » 10.3
?.0 » 10^
K
K
1.21 » 10s
8.19 x 10*
2.0
2.0
2.0
6.0 x 103
6.01 x 10^
1.01 < TO4
6.0 x 103
6.0 x 10-!
6.0 x 103
6.D x 103
6.0 x 103
1.6 « 104
it
ri
N
N
MUTE
UATER
.g/1
HEALTH
3.3 x 1C?
3.3 x 102
3.3 x 102 ,
3.3 x id?"'
3.6 x 10Z
8.0 x 105
3.0 x 10<
3.0 » 10*
rc
N
1.S2 x 106
1.23 « 106
3.0 i 10
3.0 x 10
3.0 x 10
9,0 « ID4
9.0 x 10*
1.5 x 10S
9.0 x 10*
9.0 x" 10*
9.0 x 10*
9.0 X 10*
9.0 x 104
2.4 x 105
«
N
N
N
MATE
aATEB
-•I/I
ECOLOGY
3.8 x 10Z
3.8 x !0J
3.8 x 102
3.8 x 102
N
N
N
N
K
2.3 « 10*
N
N
S.6 x 10
S.5 > 10
5.5 x 10
8.7 » 10*
8.7 x 10*
1.0 x 10S
8.7 x 10*
8.7 x 10*
8.7 » 10*
8.7 X 10*
8.7 x 10*
1,6 x 104
N
N
N
N
MATE
LAND
U9/9
HEALTH
7.0 » 10-1
1.6 x 103
6.0 X 10
6.0 x 10
N
N
3.64 x 103
2.46 x 103
6.0 x 10-z
i.O x 10-*
6.0 x 10"2
1,8 x 102
1.8 x 102
3.0 x 10*
1.8 x 10Z
1.8 x 102
1.8 x 102
1.8 x 102
1.8 x 10?
4.8 x 10Z
N
N
N
K
HATE
LAND
U9/9
F ECOLOGY
7.5 x 10-'
N
N
N
L N
4.6 » 10
N
N
1.1 x 10-1
1.1 x 10-5
I.I x 10"1
1.7 x 102
1.7 x 102
e.o x io2
1.7 x 102
1-7 x 10*
1.7 x 10Z
1,7 x 102
1.7 x 10*
3.2 x 10
N
N
N
N
SAMPLE
»9/«3
U9/9
»9/l
RATIO
SftFFLE
KATE
LEVEL Z
REWIRED
Y=VES
tt'tiR
r
TEST
KETHOD1
TEST
EXPEC-,
T«TIONSJ
TEST
COST3
SAMPLE
ALIQUOT4
TABLE KEY:
. TEST METHOD
1. STANDARD
2. DEVELOP-
MENTAL
3. UNKNOWt
A. MS
B. XRO
C. MET
CHEMICAL
0. ESCA
E. SC/MS
. EXPECTED TEST
SUCCESS:
1. HIGH
2. MODERATE
3. UNKNOWN
. TEST COST
1. REASONABLE
2. MODERATE
3. HIGH
. SAMPLE AUQDOT
1. ADEQUATE
I. ItWIUSAL
3. INADEQUATE
4. flESAMPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reducttonand Decision Charts (Continued)
vo
-•4
CATEGORY
95. STRONTIUM
36. BARIUM
37. BOROH
38. ALUMINUM
39. GALLIUM
COMPOUND
Strontium
Strontium Ion,
Sr+* (as Sr)
Strontium Fluoride,
SrFz Us Sr)
Strontium Sulfate,
SrS04 (as Sr)
Barium, Ba
Barium Ion, Ba++
(as Ba)
Barium Sulflde,
BaS (as Ba)
Sariun Thio-
earbonate. BaCSa
(»s fia)
Barium Fluoride,
B*F2 (« Ba)
Barium Carbonate,
ftaC03 (as Ba)
Barium Sulfate,
BaS04 (as 9a)
Boron, B
Borote, B03 (as 6)
Netaborate, Boy-
Ins 8)
Boron Oxide, B?03
Alunlnw, A!
Aluminum lofl.
Bauxite, AV/h-
3H20 (as Al)
Hydrated Aluminum
Silicate (as Al)
Alums [M A1 ($04)9]
(H20)x (as Al)
Aluminum Oxide,
Alj03
Sa!]1um. Ga
Elemental Species,
Ga
Gallous. 6a+1
(as Ga)
MATE
AIR
uOVi*3 (ppm)
3.1 x !03
3.1 > 103
3.1 < 103
3.1 x 103
S.O X 10?
5.0 n 10Z
5.0 x 102
5,0 x 10!
5.0 x 102
5.0 x 102
5,0 » 102
3.1 x !03
3.1 x 103
3.1 x 103
1.0 x 104
5.2 x 103
5.2 x 1Q3
5.2 x ID3
5.2 x 103
5.2 x ID3
1.0 x 10*
5.0 x 103
5.0 x 103
5.0 x 103
HATE
UATER
ug/I
HEALTH
4.6 X 10*
4.6 x 10<
4.6 x 104
4.6 x 104
5.0 x in3
S.O x 103
5.0 > !03
5.0 x 103
S.O » 103
5.0 x 103
5.0 x 103
'.7 x 10"
4.7 x 10*
4.7 x 10*
1.5 x 105
S.O » 10"
8.0 x 104
8.0 x 104
8.0 x 10*
8.9 x 10*
1.5 x 10s
7.4 x 10'
7.4 x 10"
7.4 x Id4
MATE
HATER
i'9/l
ECOLOGY
H
II
It
K
E.5 x 103
2.5 x 103
J.5 x 103
2.5 x 103
2.5 x 103
8.5 x W3
2,5 x 103
2.5 x 104
2.5 x 104
2.5 x 10"
K
1.0 x 103
1.0 x 1C3
1.0 x 103
1.0 x 103
1,0 x 103
N
N
N
N
MATE
LAND
HEALTH
9.2 x 10
9.2 x 10
9.2 x 10
9.2 x 10
1.0 x 10
1.0 x 10
1.0 x 10
1.0 x 10
1.0 « 10
1.0 x 10
1.0 x 10
9,3 x 10
9.3 x 10
9,3 x 10
3.0 x 10Z
1.6 x ID2
1.6 x 102
1.6 x 102
1.6 x 102
i.e x io2
3.0 x 1C2
1.5 x 10*
1.5 x 102
1.5 x 1^
MATE
LAND
9/g
ECOLOGY
H
u
N
N
6.0
5,0
5.0
5.0
5.0
5,0
5.0
5.0 x 10
5.0 x 10
5.0 x 10
N
2,01
N
2.0
2.0
?,0
N
N
N
N
SWLE
Bg/m3
V9/9
»J/I
RATiO
SAMPLE
SWTE
L(»a 2
WWIRED
V.VES
N-HD
^
TEST
METHOD1
TEST
EXPEC-
TATIONS2
TEST
COST3
SAMPLE,
ALIQUOT4
1. TEST HETHOO
I. STANDARD
I. DEVELOP-
MEKTAL
3. UNKNOUH
A. MS
B. XRO
C. «ET
CHEMICAL
D. ESCA
E. fiC/MS
2. EXPECTED TEST
SUCCESS:
1. HIGH
•2. MODERATE
3.
1. REASONABLE
•2. MOOERATE
3. HIGH
4. SARPLE ALIQUOT
1. ADEQUATE
2. MARGINAL
3. INADEQUATE
4. RESAHPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reduction and Decision Charts (Continued)
to
00
CATEGORY
40. INDIUM
41. THAUIUH
42. CARBON
43. SILICON
44. SERIMNIUM
COMPOUND
Gallic, Ga+3
(as Gal
GdlSlimSesqui-
oxide, CaT^h
(as Ga) 3
Ind3i£n, In
Indium Ion, WJ
Thallium, Tl
Thallous, 11*'
ThalHc, Tl*3
Elemental Carbon
Coal
carbide, c-
Carbcnate. COj-2
Bicarbonate. HCOj
Carbonyl, C0=
Carbon Monoxide
Carbon Dioxide
Si lane, SiH4
Silicon. Si
Qrthosilicate,
S10(-z
Hetasilicite,
SiOj-2
Silicon Dioxide,
Sift!
Silicon Disulfide,
Si 52
silicon Carbide. SIC
Germanium, fie
termanous, Ge<2
(as Ge)
Germanic, Ge**
(as Ge)
Germanous Sulfide.
6e5 (as Ge)
Sermairfc Sutfice,
se$2 (as Se)
Germane, Ge«4
105
8.4 » l63
S.4 x 10'
3.4 x 103
8.4 x 11)3
8.4 x 10.3
8.4 x 103
8.4 x 103
NflTE
UATER
ug/l
ECOLOGY
N
H
N
N
N
H
N
N
N
N
N
N
N
6.0 x 10
N
N
N
N
N
N
H
N
N
N
N
N
N
N
N
HATE
UNO
y9/9
HEALTH
1.5 » 102
1.5 x 11)2
3.0
5.0
3.0
3.0
3.0
1.6 x 10?
N
R|
N
N
II
B/A
N/A
N
3.0 x 10J
Ij
N
3.0 X 102
N
3.0 X 102
1.7 X 10
1.7 x 10
1.7 x 10
1.7 x 10
1.7 x 10
1.7 x 10
1.7 x 10
HATE
LAND
>g/g
ECOLOGY
N
>(
M
K
N
N
N
}f
it
84
X
H
M
N/A
N/A
Z.1 x 10
N
U
H
N
N
H
N
N
N
N
H
N
N
SAMPLE
ul/m3
u9/9
U9/I
RATIO
SAHPLE
TiKTr
LEVEL 2
REQUIRED
Y=YES
B-nO
TEST
METHOD1
TEST
EXPEC-
TATIONSJ
TEST
COST3
SAMPLE.
ALIQUOT*
TABLE KEY:
. TEST HETHOD
1 . STANDARD
2. DEVELOP-
MENTAL
3.
A. AAS
E. XRD
C. WET
CHEMICAL
D. ESDI
E. GC/MS
^. EXPECTED TEST
SUCCESS:
I. HIGH
2. MODERATE
3. UNKNOUIt
3. TEST COST
1. REASONABLE
2. MODERATE
3. HIGH
4. SAHPLE
ALIQUOT
1. ADEQUATE
2. WRGINAL
3. HIAOEQUATE
4, RESAHPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Deduction and Decision Charts (Continued)
UD
IQ
CATEGORY
45. TIN
46. LEAD
47. NITROGEN
COMPOUND
Tin Oxide, SnOj
Tin, Sn
Stannous, Sn*2
Stannic, Sn*4
Lead, f>b
Elemental Led, ft
Plumbous. Pb*2
Plumbic, PbM
(as Pb)
Lead ttonoxide,
PbO (as Pb)
Lead Sulfate,
PbS04 3(>>04)2 Us Pb)
Lead Chraiate,
PbCrOfl (as Pb)
Lead Holybdate,
PbMo04 (as Pb)
Lead Arsenate,
PbHAsOa (as Pb)
Hydrailne
AHaH Cyanides.
NaCH, KCN
Nitric Add, HN03
Nitrogen Oxides,
tbO, HO?, NjOa,
MZ03, N205
Hydrogen Cyanide,
Aniniila, BHj
Cyanogen, CgNa
Nitride, K-
Nitrate, Noj-
Nltrtte, <*>r
Annoniun, NHj*
MATE
AIR
ag/m3 (ppm)
1.0 x !(>4
N
N
it
1.5 X IO2
1.5 I 102
1.5 x 10*
1.5 x 10*
1.5 * 10Z
1.5 * 10Z
l.i x Mil
1.5 x 10s
1.5 > 10?
1.5 x 102
1.5 x I02
1.5 « 102
1.5 x 10Z (.1)
5.0 x 103
5.0 x 103
9.0 x 103
5.1 x 10* (10)
1.8 x 10* (25)
2.0 x 10*
N
N
N
N
KATE
UATER
u9/l
HEALTH
1.5 x 10s
n
n
N
2.5 x I02
2.5 x SO2
2.5 x ID2
2, a x io2
2.B x lO2
2.6 i 10Z
2.5 x 102
2.5 x IO2
2.5 x IO2
Z.5 x 102
2.5 x lO2
Z.5 X IO2
2.3
5.0 x IO2
7.5 i IO4
1.4 x 105
5,0 K 10Z
2.5 x 103
1.0 x 103
n
N
N
"
HATE
UATEIi
1;g/l
ECOLOG*
N
N
N
N
5.0 x 10
5.0 x 10
5.0 x 10
5.0 x 10
5.0 x 10
5.0 x 10
5.0 x 10
5.0 > 10
5.0 x 10
5.0 x 10
5.0 x 10
5.0 x !0
N
2.5 x 10
4.5 x IO2
N
2.5 X 10
5.0 x 10
2.5 X 10
N
N
N
N
MATE
LAND
pg/9
HEALTH
3.0
N
t|
«
5.0 x 10-1
5.0 x lO'1
5.0 x 10-1
5.0 x 10-1
5.0 x 10-1
5.0 x IO-1
5.0 x 10-1
5.0 x 10-1
5.0 x lO"1
5.0 x IO-1
5.0 x Itr1
5.0 x IB"'
4.5
1.0
1.6 x 1Q3
(I/A
1.0
6.0
2.0
K
«
K
M
NATE
LAND
U9/9
ECOLOGY
N
N
N
N
1.0 x 10-1
1.0 x 10-'
1.0 x 10-1
1.0 < 10-'
1.0 x 10-1
1.0 x 10-i
1.0 x 10-1
1.0 x 10-1
1.0 x 10-1
1.0 x 10-1
1.0 x ID'1
1.0 X 10-1
N
5.0 x IO-2
9.0 x 10-'
N/A
5.0 x ID"2
1.0 x ID'1
5.0 x 10-2
M
N
N
M
5AHPLE
,,9/n3
U9/9
ufl/1
PATIO
SAMPLE
MOTE
LEHL 2
REQUIRED
Y-VES
N-BO
TEST
METHOD1
TEST
EXPEC-
TATIONS2
TEST
COST3
SAMPLE
ALIQUOT
T.
?.
3.
4.
TABLE KEY:
. TEST METHOD
i. STANDARD
2- DEVELOP-
MENTAL
3. UNKNOWN
K. AAS
B. XRO
C. HET
CHENICAL
D. ESCA
E. GC/MS
. EXPECTED TEST
SUCCESS
1. HIGH
.2. MODERATE
3. UNKNOWN
TEST COST
1. REASONABLE
2. MODERATE
3. HIGH
SAMPLE ALIQUOT
1. ADEQUATE
^. MARGINAL
3. INADEQUATE
4. RESAMPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reduction and Decision Charts (Continued)
O
o
CATEGORY
48. PHOSPHORUS
19. ARSENIC
SO. AKT!HOHV
51. 8ISHUTK
COMPOUND
Phosphorus, F
Phosphite, PO->-3
(as P! 3
B1 phosphite,
H2P04- (as P)
Phospnine, PH3
Phosphoric Aciq,
H3P04
Phosphorus
Pentasulfide
Phosphate, POn-i
Arsenic, As
Metallic Arsenic
Arsenous, As+3
Arsenic, AstS
Arsenate, AsOa~3
(as As)
ArsenUe, AsOa"3
(as As!
Arsenide, As"3
(u As)
Arsine, AsH^
Arsenic Trioxide,
As203
Antimony Tri-
oxide, SbjOj
Antimony Metal , Sb
Antimnous.
(stibnous) Sb*3
Anjjmnfc (stibnfc)
Stibine. SbHs
(as Sb)
Antitnonous Sul-
flde. SbjS3
Antinony. Sb
Bisnwth. Bi
Elemental Bis-
nuth, 81
BlsmUlous, B1*3
(as B1)
Bfsnuthlc, BI*6
(u Bfl
NATE
A!B
ag/ltl3 (upm)
1.0 * 102
1.0 x 102
t.O x !02
4.0 X 102 (0.3)
1.0 x 103
1.0 X JO3
X
2.0
2.0
?,0 x 10
2.0 x 10
2.0 x 10
2.0 x 10
2.0 x 10
2,0
2.0
5.0 x 101
5.0 x 10?
5.0 > 102
5.0 x 10Z
5.0 X ID2
5.0 x 102
5.0 x 10?
4.1 x 10Z
4.1 x 102
4.1 x 102
4.1 x 102
MATE
1 HATER
I -g/l
HEALTH
1.5 x 104
1.5 x 10'
1.5 x 10<
6,0 x 103
1-5 x 10fl
1.5 . ID4
N
2.5 x 102
2.5 x 10J
2.5 x 102
2.5 x 102
2.5 x 102
2.5 x 102
2.5 x tO2
2.5 x 102
2.5 i SO2
7.5 x 102
7.5 x 1O3
7.5 x lO^
7.5 x 103
7.5 x 103
7.5 x ID3
7.5 x 103
6.1 x 103
6.1 x 103
6.1 i 103
6.1 K 1Q3
HATE
UATER
-9/1
ECOLOGY
5.0 x 10-1
5.0 < 10-1
5.0 x lO-1
N
4.5 x 103
M
N
5.0 x 10'
5,0 x 101
5.0 x 101
5.0 x 101
5.0 x 101
5.0 x )0>
5.0 x tO1
5.0 x 101
5.0 x 101
?.0 x 102
(as Sb)
2.0 X I02
2.0 X 102
2.Q X 102
2.0 X 102
2.0 X 10?
2.0 x lO2
N
It
N
N
MATE
LAUD
ug/g
HEALTH
3.0 x 10
3.0 x 10
3.0 X 10
N/A
3.0 x 10
3.0 x ID
N
5.0 x 10-1
5.0 K 10-'
5.0 « 1C'1
5.0 x 10-'
5.0 > ID'1
5.0 x 10"!
5.0 x 10-1
5.0 x 10-1
5.0 x lO'1
1.5
1.5 X I01
1.5 X 10!
1.5 X 101
1.5 x 10T
1.5 x 10'
1,5 x 10'
1.2 x 101
\.t x 101
1.2 x 101
1.2 x Ifll
NATE
LAUD
1-9/9
ECOLOGY
1.0 » 10-3
5.0 * 10-3
1.0 t 10-3
N/A
9.0
N
rt
1.0 x 10-1
1.0 x 10-'
1.0 x 10-'
1,0 x 10-'
1.0 x 10-'
1.0 x 10-1
1.0 x 10"1
1.0 x 10-'
1.0 x 10-1
4.0 x 10-'
{as Sb)
4.0 x 10-'
4.0 x 10-'
4.0 x 10-1
4.0 x 10-1
4.0 x 10-'
4.0 x 50-1
N
N
K
N
SAMPLE
Lg/m3
1-9/9
,9/1
RATIO
5AHPLE
_.
... _,
h— -|
1
LEI/EL 2 '
REQUIRED
Y=TES
N=NO
TEST
METHOOl
TEST
EXPEC-
TATIONS'
TEST
COST3
SAHPLE
ALI3UOT4
TABLE KE»:
TEST METHOD
1. STANDARD
2. DEVELOP-
HENTAL
3. UNNWUN
A. AAS
B XRO
C, UET
CHEMICAL
D, ESCA
E. OS/MS
EXPECTED TEST
SUCCESS:
1. HIGH
2. NODERATE
3. UNKNOWN
TEST COST
1. REASONABLE
2. MODERATE
3. HISH
SAflPLE ALIQUOT
1. ADEQUATE
?. MARGINAL
3, INADEQUATE
4. RESAMPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Uati deduction and Decision Charts (Continued)
CATEGORY
52. OXYGEN
S3. SULFim
54. SELENIUH
SS. TELIUHIUH
56. FLUORIDE
MATE ! KATF ! "WTE ; WT[
; WTE | IrtTER vlATER ] LAUD • LAND
JIB I .9/1 ; g.-l , ..5/0 ! vn/o
.. . . . , ., fppti) ; HEALTH 1 ECOLOGY j HEALTH j ECOLOGY
Ozone, Oj I 2.0 x 102 (O.I I ' II/A | «V* Vft ' N/A
Rhwfcic Sulfur. S8 ; N ] N •) X , II
Sulflfe. S-2
Sulfite, SD4"2
Sulfltt. SOj-2
TMocyarute, SOT
Sulfur THoxide,
S03
Sulfurlc Acid,
HjSOj
Sulfur Dioxides,
S02
Hydrogen Sulflde,
H2S
Carbon Bisulfide,
CS2
Carbony! Sulflde,
COS
Selenium, Se
Elemental Selenium,
Se
Selenlde, Se-Z
Seletiltes, 5e03-^
(as Se)
SslCTates, Se04-z
(as Se)
Hydrogen sslenide,
H2Se
Carbon Diselenide,
tSe-j (as Se)
Selenium Dioxide,
SeO? (as Se}
Tellurium. Te
Tellurlde. Te"2
Tellurtte, TeOj-*
(«s M
Tell grate, TeOj
(M Te)
Fluorfiie Ion. r
Hydrogen Fluorine,
HF
N : N
!l BIN
N N t N • N
II ! N 1 (1 | B ; N
N
N
11 ' II ^
, , . t . . .
N ; N
N
fl
n
1.0 x 103 i 1.5 x 10" i »,* x 10Z ! J.(! x Id1 i 9.0 > Id?
1.3 K 10< i 2.0 x 10s | N i 4.0 x IOJ I N
1.5 x 10* (10! | 2,3 x 10"
1 .0 X I01 | N/« H/A
6.0 x 104 (!0) ' 9.0 x 105 1.0 x 10*
4.4 x ID5 | N/A j N/A
2.0 x 10Z 1 5.0 x IQl
2.0 x Id2
2.0 x SO2
2.0 x 10Z
2.0 x 10?
2.0 x 102 (.05!
Z.O x 102
J.O x 102
1.0 i 10J
1.0 x HP
1,0 x 10s
1.0 x 102
Z.5 x 103
2.0 x I03
5.0 i 101
5.0 x 10' 1
2.5 x 101
2.5 x 101
»/A | N/A
N/ft
1.0 x 10-1
1.0 x 10-'
2.5 x ID1 ! 1.0 x ID'1
5.0 x 101 2.5 > 10"
S.O x 1Q1
5.0 x-101
(as Se)
5.0 X 10'
5.0 x 101
1.5 < 103
1.5 x 103
1.5 x !03
.1.5 x 103
3.8 » 10*
3.0 « 10<
2.5 x ID1
2.5 x I01
(as Se!
2.5 X Id'
2.5 x 10'
N _|
N
N
n
N
N
1.0 x 1C"1
1.0 x ID'1
!,0 x 10-'
(as Se!
1.0 x 10-'
1.0 K 10"'
3.0
3.0
3.0
3.0
7.5 x 101
U/A
N/A
5.0 x 10-2
5.0 i 10"z
5.0 i 10"2
•5,0 x 10-Z
5.0 x 10"z
5.0 x 10-2
(as Se)
5.0 i 10-2
5.0 « 10-2
11
K
H
N
N
»/
!
SAMPLE i RATIO
ug/fiH 1
W9/9 | SAJgLE
.,5/1 j TSTF
LEVEL 2
REQUIRED
»«YES 1 TEST
«>NO METHOD'
;
•
•
TEST
EXPEC-
TATIONS?
TEST,
COST^
SAMPLE,
ALIQUOT"
i
1
!
^_ : L
:
7
i !
j
i i
i
1
1
1
„
1 -..
!
!
!
i
<
|
TASLE KEY:
1. TEST HETH03
1, STAHuASD
I. OEI/ELOP-
KERTA1.
3. u:it,'Mit'i
A. IAS
B. XRD
C. MET
CHEWCAL
D. ESCA
E. GS/HS
2. EXPECTED TEST
SUCCESS
1. HIGH
2. MODERATE
3, UNKNDUN
3. TEST COST
1. SEASOflABLt
2. HOBERATE
3. HICK
«. SAMPLE ALIQUOT
1. ADEQUATE
2. WRGINAl
3. INADEQUATE
4. RESAHPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Oata Reduction and Decision Charts (Continued)
o
ro
CATEGORY
57. CHLORINE
58. BROMINE
59. IODINE
60. SCANDIUM
61. VTTRIUM
62. TITANIUM
63. ZIRCONIUB
64. HAFNIUM
65. UANAOIUM
COMPOUND
Chloride Ion, Cl"
Hypoehlorite,
cio-
dilorlte. ClOj-
Chlorate, C103
Chlorine Dioxide,
C102
Carbonyl Chloride
(phosgene),
COClz
Hydrogen Chloride.
HC1
Bromide Ion, Br"
Bromide IonT Br~
Hydrogen Bromide,
HBr
Iodide Ion, 1-
Scandfum; Sc
Scandium Ion, Sc*3
Yttrium Ion, f*3
Titanium, Ti
tttanous, Tt*3
(as T1)
Titanic, T1*4
(as Ti)
Titan turn Dioxide,
TiO? (as T1)
Zirconium Ion.
Zirconium Dioxide,
ZrOj (as Zr)
Hafnium Ion, Hf*
Vanadium, V
Elemental
Vanadium, V
Vanadic, ¥*3 (as V)
Vanadyl, W*!
(as f)
DrtAovanadate!
Vod-* Us V)
HATE
AIR
•jg/ml (ppm)
N
N
li
It
N
4.0 X Ifl2
7,0 i id3
N
»
1.0 x ID4
N
S.3 x 10s
5.3 x lO*
1.0 x 103
6.0 » 103
6.0 > 103
6.0 x 103
6.0 x 103
5.0 i 103
S.O < I0>
5.0 x 102
5.0 x !02
5.0 x 102
5.0 x 102
5.0 i 10Z
5.0 x 10?
MATE
MATER
•-«/!
HEALTH
1.3 x 10S n
N
N
14
N
6.0 x 103
1,1 » 10s
N
N
l.S x 10s
11
8,0 x 105
6.0 x 105
1.5 x ID4
9,0 x ID4
9.0 x 10*
9.0 x 10*
9.0 x 104
7.5 x 10*
7.5 X 10*
7.5 x 10*
l.S x 103
2.5 » 103
2.5 x 103
2.5 x ID3
2.5 x 103
KftTE
UATER
:.9/l
ECOLOGY
ft
"
«
N
U
N
N
N
II
N
II
N
«
N
8.2 x W*
(as
Ti[S04]2>
8.2 x 102
8.2 X TO2
8.2 x 102
N
n
N
1.5 x 102
l.S x 102
1.5 x 102
l.S x 102
l.S x 102
HUTE
LAND
HEALTH •
2.6 x 103
N
N
N
N
I»/A
H/A
f(
N
N,'A
H
l.S x 10'3J
1.6 x 10"3
3.0 x 10l
1.8 x IOZ
1.8 x 102
1.8 x 102
1.8 x 102
l.S x 101
1.6 X 101
l.S x 10
5.0 x 10
5.0 x 10
5.0 i 10
S.O x 10
5.0 x 10
MATE
LAND
u9/g
ECOLOGY
K
H
H
H
H
»/fl
N/A
fj
N
N/ft
N
N
N
S
1.5
1.6 x 10
1.6 x 10
1.5 x 10
N
II
N
3.0 x 10-T
3.0 x 10-1
3.0 x 10-1
J.O x 10-'
3.0 x 10-'
sty
3f!
RATIO
w
LEVEL Z
REQUIRED
Y=VES
N=NO
TEST
METHOD"
TEST
EXPEC-
TATIONS2
1
TEST
COST3
SAMPLE
ALIQUOT*
TABLE KEY:
TEST METHOD
1. STAtiOARD
2. DEVELOP-
MENTAL
3. UNKNOWN
A. AAS
6. IRD
C. MET
CHEMICAL
D. ESCA
£. SC/MS
EXPECTED TEST
SUCCESS:
I. HIGH
2. MODERATE
3. UNKNOWti
TEST COST
1. REASONASLE
Z. MODERATE
3. HIGH
. SAMPLE ALIQUOT
1, ADEQUATE
2. MARGINAL
3. INADEQUATE
4. RESAWLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 ilata Reduction and Decision Charts (Continued)
CATEGORY
<-
66. HIDS1UH
67. TAKTHLUd
£8. CHROMIUM
COMPOUND
Metavanadate, ¥03-
<«s V) 3
Vanadyllc, W>*3
10*
Z.5 x 10Z
2.5 x ID?
2.5 x JO2
2.5 x 10Z
7.5 x ID?
Z.5 x 102
2.5 x 102
Z.5 x 102
2.5 x 10?
2.5 i 10?
MUTE
klftTER
..g/1
ECOLOGY
1.5 x 10?
1.5 x !02
1.5 x Kl2
1.5 x H>2
1.5 x Id2
1.5 x 102
l.S « !02
1.5 x 10*
l.S x Id2
1.5 x 10?
II
N
K
II
t.s * lo2
2.5 x 102
Z.S x 102
2.5 X 1C2
2.5 x 102
2.5 x 102
2.5 x 102
2.5 x 1Q2
2.5 x 102
2.5 i 10?
MATE
LAND
19/9
HEALTH
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
6.5 x !02
6.5 x 102
C.i x 102
l.S x Id2
5.0 x ID-'
5.0 » 10-1
5.0 x 10"'
5.0 x JO-'
5.0 x 10-1
5.0 x 10-1
5.0 x 10-'
5.0 x 10-'
5.0 x 10-1
5.0 x 10-1
NATE
LAND
1-9/9
ECOLOGY
3.0 x 10"'
3.0 » 10-1
3.0 x 10-1
3.0 x ID-'
3.0 x 10-1
3.0 x 10-'
3.0 x 10-'
3.0 » 10-'
3.0 » 10-'
3.0 « 10-1
K
K
N
H
5,0 x 10-'
5.0 x 10-'
5.0 x lO'l
5.0 I 10-'
S.O x 10-1
5.0 x 10-1
5.0 x 10-'
5.0 x 10-1
6,0 i 10-1
5.0 x 10-1
SAMPLE
K9/«>5
39/9
»o/l
8AT10
SAWLJ
MUTE
L
LEVEL 2
REQUEUED
V'YES
N-NQ
)
'. TEST
I METHOD'
1
i TEST
EXPEC-
TATIONS2
i
TEST
COST3
SAMPLED
ALIQUOT4
;
. TEST HETHOO
1. STANDARD
2. OEVELOP-
3. UNKNOWN
A. AAS
B. XRD
C. MET
CHEMICAL
D. ESCA
E, SC/MS
. EXWCTEO TEST
SUCCESS:
1. HIGH
2. MODERATE
3. UNKNOWN
. TEST COST
1. REASONABLE
?, MODERATE
3. HIGH
. SAMPLE ALIQUOT
1. ADEQUATE
2. MARGINAL
3. INADEQUATE
4. RESAMPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reduction and Decision Charts (Continued)
CATEGORY
S3. MOLYBBEN
70. TUNGSTEN
71. MANGANESE
72. IRON
COMPOUND
Hydrous Chromium
Phosphate, CrP04
KH20 (as Cr)
Iron Chromate,
FeCrOj (as Cr)
Molybdenum, Ho
NolyMenous. Nn*Z
Holybdic. Ho*3
Molybdate, MoO«-z
(«5Ho)
NolybdBluti Sulfide,
*SJ (as Mo)
Molybdenum Trioxfde,
MaOj (as H>)
Tungsten, H
Tungsten tons, n*2,
H*«. H*5, H*«, KQV2
Tungsten Bisulfide,
USz (is U)
Holframite Mineral ,
FeM04-MnWO< (as U)
Manganese. Nn
ttongjnous. Nn+? .
Manganic, Kn+3
Permanganate, NnOa-
(as Ih)
Manganous Oxide,
NnO (as Ml)
Manganese Dioxide,
MiOz (as Mn)
Manganese Carbonate,
KcCOj (as Hi)
Kinoanous Sulfate,
ItlSO* (as Mn)
Manganese Sulflde,
NaS2 (as Hn)
Iron Carbonyls,
Fe(CO)5. Fe(CO)9.
FE3[CO)1J
Ferrous, Fe*2
Ferric, Fe*3
Ferrous Oxide, FeO
TOTE
AIR
^g/mj (ppm)
1.0
1.0
5.0 X 103
5.0 x 10^
5.0 r, 103
5.0 x 103
5.0 i 103
5.0 x 103
1.0 x TO3
N
1.0 x 103
1.0 x 103
5.0 x 10-1
5.0 x 103
5.0 x 103
5.0 x 10'
5.0 x 103
5.0 K 103
5.0 « 103
5.0 x 103
5.0 x 103
7.0. x 10*
1.0 x 103
1.0 x 103
5.0 I 10s
MATE
UATEB
ug/1
HEALTH
?.5 « 102
Z.i x 10^
7.5 « 10«
7.5 « 10"
7.5 x 104
7-S x 10*
7.5 t 10*
7.5 x 10*
1.5 x 10*
N
1.S X 10*
1.S x 10*
2,5 x 10!
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 Data Reduction ind Decision tnarts (Continued)
o
01
CATtfiORT
n. RUTHENIUM
7*. COMLT
76. RHODIUM
76, NICKEL
COMPOUND
Magnetite.
FeO-FeaOj
ferrocyanlde,
FelCKIr*
Ferr1cy«i1de,
F.(CN>6-3
Ferric Oxide, fejOj
Ferric Hydroxide
(hydrited)
F«203-XHZ0
Iron Sol fides, FeS,
FejS3
Pyrite. FeSz
Potassium Iron Sili-
cate, KFeSlzOe
Ruthenium Ion, «u*3
Cobalt, Co
Cobalttus, Co*2
Cotultic. Co*3
Cobaltous Carbonate.
hydrated. CoCOj>HzD
(as Co)
Cobalt Carbide,
CojC (as Co)
Cobilt Sulfldts, Cos,
C02$3 (as Co)
Cobalt Arsenic '
Sulftde. CoAsS
(ai Co)
Cobalt Arsenide,
CoAsz (is Co)
CobtH Carbonyl,
Co(CO)« (as Co)
Cobaltous (Mde,
CoO (as Co)
Cobaltous Hydroxide,
Co(OH)2 (as Co)
Rhodium Ion, (h*3
Ntckelous, HI*2
Nickeltc. M*3
Nickeloiis Sulflde,
ms (as N1)
Nick«l Arsenide,
N1AS (as ffl>
HATE
AIH
•jg/m3 (ppn)
9.3 x 10'
N
N
N
N
N
N
H
N
5.0 X 10'
5.0 x 10'
5.0 x 10.1
5.0 x 10'
5.0 > 10'
5.0 x Id1
5.0 K lol
$.0 x Id1
5.0 < 1C11
5.0 I 101
5.0 x Id1
1.0 x 10
I.S -x 10'
(,S « 101
1.5 » 10'
1.5 x 1Q<
WTE
UATER
..9/1
HEALTH
t.i » in3
N
K
H
»
N
N
N
N
7.S x 10Z
7.5 x 10?
7.5 x !02
7,5 > 102
7.5 x 102
7.5 « 102
7.5 x 102
7,5 x 10Z
7.S f 102
7.5 x 102
7.5 x 10?
1.5 x 10'
2.3 » 10?
2.3 x 102
2.3 x 102
2.3 x 102
WTE
WATER
^/l
ECOLOG*
N
N
N
n
N
H
>1.0 x 105
N
N
2.5 x 102
2.5 x 102
2.5 t 102
?.5 x 102
Z.5 x 102
2.5 x 102
2.5 x 102
2.5 x 102
2.5 x 10Z
2.5 x ID?
2.S x Id2
N
1.0 » 10'
1.0 x 101
1.0 x 10'
1.0 » 10'
HATt
LAND
A
3.8 x ID'
N
N
N
N
N
«
«
N
1.5
1,5
I.S
1.5
I.S
1.5
1.5
1.5
I.S
I.S
1.5
J.O x 10-2
1.5 x 10-1
4.5 x 10-1
4.5 x 10-'
4.5 x 10-'
HATE
LAND
I&&.T
II
N
»
H
N
N
Z.O x 10?
"" ^
K
5.0 x 10-1
5.0 x 10-1
^S.O x 10'1
5.0 x 10-1
5.0 x 10-1
5.0 x 10-'
5.0 ) 10-'
5.0 x 10-'
S.O x 10-'
5.0 x 10-'
5.0 x 10-'
N
2.0 x 10-2
2.0 x 10-2
2.0 x 10-*
2-0 x 10-2
SAMPLE
wg/i»3
.U9/9
ug/I
DAT10
SAMPLE
KATE
LEVEL Z
REQUIRED
Y-VES
K=NO
1
; TEST
NCTHOO1
TEST
EKPEC-
TATiONS'
TEST
COST3
SAMPLE
ALiquor
|
1
2.
4.
TABLE KEY
. TEST HETHOO
1. STANDARD
2. DEVELOP-
MENTAL
3. tINKTIOWl
A. AAS
B. XRD
C. KET
CHEMICAL
0. ESCA
E. GC/MS
EXPECTED TEST
SUCCESS:
T. HIGH
2. MODERATE
3. UNKNOWN
TEST COST
1. REASONABLE
1. MODERATE
3, HIGH
SAMPLE ALIQUOT
I. ADEQUATE
2, WRGIHAL
3. IMOPJUATE
I. RESAWLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
level 1 Data Seduction and Decision Charts (Continued)
O
cn
CATEGORY
77. PLATINUM
78. COPPER
79. SILVER
81. ZINC
COMPOUND
Nickel Oxide. NiO
(as ill)
NATE
MR
-g/nH tppn)
1.5 x I0l
Kicke) Antimonide, , . .-]
MfSb (as Nf) '-s * !0
Nickel Arsenic Sul- , t ,n|
fide, NiAsS (as Ni) '•* x '°
nickel Carton/I.
Ni(CO)4
Elemental Platinum.
Pt
Copper
Cuprous. Cu*
Cuorfc, Cu+2
Copper Fluoride,
CuFz (as Cu!
Copper Oxides, CuO,
CuzO (as Cu)
Copper Sulfate,
CuSOt (as Cu)
Copper Sul fides, CuS,
Cu2S (as Cu)
Copper Carbonate,
CuCOj (as Cu]
Malachite Mineral,
CuC03-Cu(OH)2 (as Cu)
CftalcopyHte
Mineral , CuFeSj
Silver, Ag
Silver Ion, Ag*
(as Ag)
Silver Chloride,
AgCl (,t Ag)
Silver Cyanide, AgCN
(as Ag)
Silver Sulfide,
AJ2S (as Ag)
Zinc, Zn
Elemental Zinc, Zn
Zinc Ion, Zn+2
Zinc Oxide, ZnO
(as Zn)
S.3 » 10s
2,0 x 10
2.0 x 102
2.0 x 102
2.0 x 102
Z.O x (02
2.0 x 10?
2.0 x 102
Z.O J 102
Z.O x 102
2.0 x 10?
N
1.0 x 10"
1.0 x 101
1.0 x 101
1.0 x 10'
1.0 x 101
4.0 x Ifl3
4.0 x 103
4.0 x 103
4.0 i 103
MATE MITE
HATED WATER
..g/1 uq/l
HEALTH j ECOLOSY
2.S i 1Q2 i 1.0 » I01
HATE
LnllU
VUft
rtbtLTH
4.S x 10-'
2.3 x 102 1.0 x 101 ! 4.S x 10-1
i [
2.3 x 10? ! 1.0 x 101 i 4.S » 10-1
6.5 x 10^
3.0 x 101
1.0 x 101 : , „ ..-1
(as Sit j 1-° * '"
N 6.0 x 10-z
5.0 x 103 S.O » 10' | 1.0 x 101
5.0 x 103
5.0 x ID3
I1ATE 'SAvPlE i RATIO
LAily iid/^ I
*•!/* 9/3 i SAOT-E
ttULObY i,o/l j MATE
2.0 x 10-2
2.0 « lO-?
2.0 x 10"?
2.0 x 20"2
N
1.0 x 10-'
5.0 x 101 1.0 x 101 1.0 x 10-'
5.0 x !0l
5.0 « 103 j 5.0 x 101
5.0 x 103 I 5.0 » 101
•
5.0 x 103
5.0 x 103
5.0 x 103
5.0 x 103
N
2.5 x tO1
2,5 x 102
2.5 x 102
2.5 x 10?
2.5 x 102
2.5 x 104
2.5 x 10*
2.5 x 10'
2,5 x 10*
5.0 x IQl
5.0 x 10'
5,0 x tfll
S.O x lol
N
s.o
5.0
5.0
5.0
5.0
N
1,0 x 10Z
1.0 x 102
1.0 x 102
1.0 x 102
1.0 x 10' 1.0 » 10-1
1.0 x 10>
1.0 x !01
1.0 x 10'
1.0 x 10'
1.0 x I0l
1.0 X 10'
N
5.0 x 10-' J
5.0 x 10-1
5.0 x 10-1
5.0 » lO"1
5.0 x 10-'
- N
5.0 x Id1
6.0 x 10T
S.O x l(ll
5.0 x 10s
1.0 x 10-1
1.0 x 10-5
5,0 x 10-1
1.0 x 10-1
1.0 x 10-1
1.0 x 10-1
N
1.0 x JO"2
1.0 x 10"2
1 0 x 10"2
1.0 x 10"2
1.0 x 10"2
2.0 x 10-1
2.0 x 10-1
2.0 x 10-1
2.0 x 10-1
LEVEL 2
REQUIRED ;
Y=YES : TEST
IW40 ' HETWD1
1
TEST
EXPEC-
TATIONS?
TEST
COST3
SAMPLE
AUQUOT*
; [
i i
,
I
i
j
!
j
t
!
1
1.
2.
3.
4.
TABLE KEY;
TEST METHOD
1. STANDARD
2. DEVELOP-
MENTAL
3. UNKNOWN
A. HAS
XRD
C. WET
CHEMICAL
a. ESCA
E. OC/HS
EXPECTED TEST
SUCCESS:
1. HIGH
2. MODERATE
3, UNKWUK
TEST-COST
1. REASONABLE
2. MOOEMTE
3. HIGH
. SAMPLE ALIQUOT
1. ADEQUATE
2. KftfiGINAt
3. ISADEdUATE
4. RESAMPLE
-------
Level 1 Data Reduction and Decision Charts (Continued)
Level 1 IUU Reduction and Decision Charts (Continued]
CATEGORY
82. CADK1UM
33. MERCURY
St. CERIUM
35. URMIIW
W. THOHIUM
COMPOUND
Zinc Sulfste, ZnSO(
(is En)
Zinc Sulfide. ZnS
(as In)
Udmiim. Cd
Eltmmtal Ctdmlun,
Cd
HATE : >HTE
KATE ! WATER WA7EB
AIR ,f)/l .g/1
-9/m3 (ppm) HEALTH ECOLOGY
4.0 x SO3 ; 2.5 x 10*
4.0 x !03 2.5 x 10*
1.0 x SO' ! 5.0 x 10'
1,0 x 101 5.0 x 10'
Cadmium Ion, Cd*2 1.0 x 10' 5.0 x 101
Cadmium Sulflds. Cits
(as Cd)
Cadmium Oxide, CdO
(as Cd)
Jtrcury, US
Elemental Mercury, Hg
1.0 x 10' 5.0 x I0l
1.0 » 10' 5.0 x 10'
5.0 x 10' , 1.0 x loi
5.0 x 10' ! 1.0 x 101
fcrcurous, Hgj** ,' 6.0 x 101
Wrcurlc, Hg** 5.0 x 10'
Mercuric Sulfide,
1195
Mercuric Chloride,
HgCl2
Dysprosiun, Dy
N
1.2 x 102
1,3 x 10
i WT£
I UUW)
i US/9
2.0 x 10-1
2.0 x 10-1
, 2.0 x 10-3
2.0 x 10-3
2.0 x 10-3
2.0 x 10-3
Z.O x 10-3
5.0 x 10*1
5.0 x 10-1
L 5.0 * 10-1
S.O i 10-1
5.0 x 10-1
5.0 x 10-'
N
II
N
N
N
1.0
II
SAMPLE
,19/m3
: WIO
i LfVEL 2
Y=VES
1
TEST
1 METHOD'
TEST
EXPEC-
TATIONS'
I
I
' TEST
i COST3
;
i
'. SAMPLE,
' AL 191)0.
;
; • ! ;
• " j
1 j
1 :
}
^
?
'
•
i
i |
'
! i
1
2
3.
4.
TABLE KEV:
. TEST HETitOO
1. STASDARD
2. DEVELOP-
MENTAL
3. UKKIWlir:
A. AA5
8.
-------
APPENDIX B
LIQUID CHROMATOGRAPHY SEPARATION PROCEDURE
Column: 200 mm x 10.5 mm ID, glass with Teflon stopcock.
Adsorbent: Divison Silica Gel, 60-200 mesh, Grade 950 (Fisher Scientific
Company). This adsorbent is activated at 100°C for two hours
just prior to use. Cool in a desiccator.
B.I PROCEDURE FOR COLUMN PREPARATION
Dry pack the chromatographic column, plugged at one end with glass
wool, with 6.0 grams of freshly activated silica gel. A portion of prop-
erly activated silica gel weighing 6.0 ±0.2 g occupies 8 ml in a 10 ml
graduated cylinder. Vibrate the column for a minute to compact the gel
bed. Pour pentane into the solvent reservoir positioned above the column
and let the pentane flow into the silica gel bed until the column is homo-
geneous throughout and free of any cracks and trapped air bubbles.* The
total height of the silica bed in this packed column is 10 cm. The solvent
void volume of the column is 2 to 4 ml. When the column is fully prepared,
allow the pentane level in the column to drop to the top of the silica bed
so that the sample can be loaded for subsequent chromatographic elution.
B.2 PREPARATION OF THE SAMPLE
At room temperature evaporate the solvent from an aliquot of solution
containing the sample. The preferred sample weight is 100 mg. Weigh this
sample in a glass weighing funnel. In order to facilitate transfer of the
sample, add 0.5 to 1.0 g of activated silica gel to the sample and care-
fully mix this with the sample using a micro-spatula.
Table B-l shows the sequence for the chromatographic elution. In
order to ensure adequate resolution and reproducibility, the column elution
rate is maintained at 1 ml per minute.
*
A convenient device for the elimination of gel bed cracks and air bubbles
is acetone coolant, which is subsequently referred to as the ACE B method.
It consists of a paper towel wound loosely around the glass column along
the region of the crack or bubble; the paper towel is periodically moist-
ened with acetone. The acetone evaporation cools the region and dissi-
pates the bubble or crack.
108
-------
Table B-l. Liquid Chromatography Elutlon Sequence
No.
Fraction
1
2
3
4
5
6
7
8
Solvent Composition
Pentane
20% Methyl ene chloride in pentane
50% Methyl ene chloride in pentane
Methyl ene chloride
5% Methanol in methylene chloride
20% Methanol in methylene chloride
50% Methanol in methylene chloride
Cone. HC1 /Methanol /Methyl ene
chloride (5 + 70 + 30)
Vol ume
Collected
25 ml
10 ml
10 ml
10 ml
10 ml
10 ml
10 ml
10 ml
B.3 LOADING SAMPLE ON THE COLUMN
Quantitatively transfer the sample into the column via the weighing
funnel used for 'sample preparation; a micro-spatula can be used to aid in
the sample transfer. Rinse the funnel* with a few ml of pentane to com-
plete the quantitative sample transfer. (Note: Do not rinse with methy-
lene chloride because this solvent will cause the aromatics to elute with
the paraffins.) Add the solvent slowly to minimize disturbing the gel bed
and eliminate the trapped air bubbles, particularly in the zone of the
sample-containing silica gel, by using the ACE B approach (see footnote,
preceding page). The chromatographic system is now ready for sample
fractionation.
B.4 CHROMATOGRAPHIC SEPARATION INTO 8 FRACTIONS
The volume of solvents shown in Table B-l represents the solvent vol-
ume collected for that fraction. If the volume of solvent collected is
"save this weighing funnel for subsequent additional rinsing with the sol-
vents used at interim fractions up to methylene chloride.
109
-------
less than volume actually added due to evaporation, add solvent as neces-
sary. In all cases, however, the solvent level in the column should be at
the end of the collection of any sample fraction.
After the first fraction is collected, rinse the original sample
weighing funnel with a few ml of the fraction number 2 solvent (20% methy-
lene chloride/pentane) and carefully transfer this rinsing into the column.
Repeat as necessary for fractions 3 and 4,
B.5 PREPARATION OF XAD-2 RESIN
The XAD-2 resin to be used in the SASS train sorbent trap must be
cleaned prior to use. The resin as obtained from Rohm and Haas is soaked
with an aqueous salt solution. This salt solution plus residual monomer
and other trace organics must be removed before the resin can be used for
sampling trace organics.
Transfer the resin to a large Soxhlet extractor with a 1.5-liter
dumping volume. This requires 2 to 2.5 liters of solvent in the 3-liter
supply flask. The XAD-2 resin is then extracted in sequence with the
following solvents and times:
• Water - 22 hrs
• Methanol - 22 hrs
• Anhydrous ether «• 8 hrs
• Pentane - 22 hrs
The water removes the salt solution and any water soluble organic
material. Methanol removes the residual water from the resin and ether
removes the majority of the polar organic material. Pentane is used as
the final stage because it is the solvent used in the actual extraction
of collected material from the resin.
After the final pentane extraction, transfer the XAD-2 resin into a
clean flask and dry it under a vacuum for 18 hours using mild heat from
a heat lamp.
110
-------
APPENDIX C
MFG. ORGANIC/MAOOR MASS PEAKS
111
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Aliphatic Hydrocarbons
A. Alkanes and Cyclic Alkahes
Methane
Ethane
Propane
Butanes
Pentanes
Cyclopentane
Hexanes
Cyclohexane
Heptanes
Octanes
Nonanes
Alkanes (C>9)
B. Alkenes, Cyclic Alkenes and
Dienes
Ethylene
Propylene
Butylenes
Butadienes
Pentenes
Compound
Detail
N-Butane
N-Pentane
N-Hexane
N-Heptane
N-Octane
N-Nonane
N-Decane
Cis 2-Butene
1,3 Butadiene
1-Pentene
Molecular
Weight
16
30
44
58
72
70
86
84
100
114
128
142
28
42
56
54
70
M/e Values (RI)
16(100), 15(86), 14(16), 13(8)
28(100), 27(33), 30(26), 26(23)
29(100), 28(62), 44(40), 43(34)
43(100), 29(41), 27(31), 28(30)
43(100), 42(60), 41(40), 27(35)
42(100), 70(30), 41(29), 55(29)
57(100), 43(82), 41(74), 29(63)
56(100), 84(73), 41(57), 55(34)
.43(100), 41(52), 57(48), 29(46)
43(100), 41(33), 29(34), 57(34)
43(100), 57(67), 41(40), 29(37)
43(100), 57(82), 41(43), 29(38)
28(100), 27(54), 26(50), 25(7)
41(100), 42(69), 39(61), 27(25)
41(100), 56(48), 39(36), 27(33)
54(100), 39(91), 53(66), 27(46)
42(100), 55(58), 41(45), 39(35)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detai1
Molecular
Weight
M/e Values (RI)
C.
Cyclopentadienes
Hexenes
Cyclohexene
Cyclohexadiene
Heptenes
Al kynes
Acetylene
Propyne
Butynes
1,3 Cyclopentadlene
1-Hexene
1,3 Cyclohexadiene
1-Heptene
2-Butyne
66
84
82
80
98
26
40
54
66(100), 65(65), 39(50), 40(41)
41(100), 56(86), 42(75), 27(68)
67(100), 54(77), 82(40), 41(37)
79(100), 80(57), 77(38), 39(23)
41(100), 56(87), 29(71), 55(60)
26(100), 25(20), 13(6), 24(6)
40(100), 39(92), 38(36), 37(28)
54(100), 27(45), 53(45), 39(26)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Alkyl Hal ides
A. Saturated Alkyl Hal ides
Methyl bromide
Methyl chloride
Methyl iodide
Dichloromethane (methylene
chloride)
Bromodi chloremethane
Dibromochloromethane
Tribromomethane (bromo-
form)
Di bromodi chloromethane
Di chlorodi f1uoromethane
Tri chlorof1uoromethane
Carbon tetrachloride
1,2-dichloroethane
(ethylene chloride)
1,1,1,-trichloroethane
94
50
142
84
162
206
250
240
120
136
152
98
132
94(100), 15(47), 93(21), 91(7)
50(100), 15(83), 52(32), 49(10)
142(100), 127(38), 141(14),
15(13)
49(100), 84(58), 86(36), 51(30)
83(100), 85(64), 47(23), 48(16)
129(100), 127(78), 131(25),
208(14)
173(100), 171(50), 175(49)
93(22)
163(100), 161(62), 165(45),
79(22)
85(100), 87(33), 50(12), 101(9)
101(100), 103(60), 35(16),
66(15)
117(100), 119(97), 121(32),
82(19)
62(100), 27(93), 49(37), 64(32)
97(100), 99(64), 61(50),
117(19)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
l,2-dichloro-l,2-difluoro
Hexachloroethane
Dichloropropanes
Bromobutanes
Hexachlorocyclohexane
(lindane)
1-chlorooctane
B. Unsaturated Alkyi Hal ides
Chloroethene (vinyl
chloride)
1,2-dichloroethene
1,1-dichloroethene (vinyl-
idine chloride)
Tetrachloroethene (per-
chloroethylene)
Dichloropropenes
1,3-Hexachlorobutadi ene
Hexachlorocyclopentadi ene
C2C12F2
1,2-Dichloro-
propanes
1-Bromobutane
2,3 Dichloropene
134
234
112
136
288
148
62
96
96
164
110
258
270
117(100), 119(96), 201(80),
203(51)
63(100), 62(71), 27(57), 41(48)
57(100), 41(49), 29(34), 27(20)
181(100), 183(83), 217(66),
219(65)
91(100), 43(54), 55(39), 41(39)
62(100), 27(67), 64(31), 26(19)
61(100), 96(73), 98(47), 63(32)
61(100), 96(61), 98(32), 63(32)
166(100), 164(79), 129(69),
131(66)
75(100), 39(67), 71(32),
110(23)
225(100), 227(65), 223(63),
190(42)
237(100), 235(64), 239(63),
95(42)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Ethers
2,2'-Oxy bis propane
(Diisopropylether)
2-Ethyl-4-methyl-l,3-
Dioxolane
1,3-Dioxane
1,4-Dioxane
2-Methoxy blphenyl
(0-phenylam'sole)
102
130
88
184
45(100), 43(39), 47(24), 59(11)
28(100), 31(81), 29(79), 87(58)
28(100), 29(37), 88(31), 58(24)
184(100), 169(46), 141(24),
115(10)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Halogenated Ethers
Chloromethyl methyl ether
l,l'-Dichloromethyl ether
2-Chioro-1,3-epoxypropane
(Bepichlorohydri n)
2-Chloroethylmethyl ether
l-Chloro-l,3-oxetane
Chloromethylethyl ether
Chloro ethyl ethyl ether
l.l'-Dichlorodiethyl ether
1.2-Dichlorodiethyl ether
1,2-Dichloroethyl ethyl
1,2-Dichloroethyl ethyl ether
2,2'-Dichlorodiethyl ether
ot-Chlorobutyl ethyl ether
bis-(l-chloroisopropyl) ether
1,2-Dichlorodiisobutyl ether
Bromophenyl phenyl ether
80
114
92
94
92
94
108
142
142
142
142
136
170
248
45(100), 29(43), 15(39), 49(14)
79(100), 49(47), 81(33), 51(16)
93(100), 63(98), 27(75), 95(32)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Alcohols
C.
Primary Alcohols
Methyl alcohol
Ethyl alcohol
1-propanol
1-butanol
1-pentanol
Secondary Alcohols
2-propanol
2-butanol
2-pentanol; 3-pentanol
a-hydroxytoluene (m-cresol)
2,6-dimethyl-4-heptanol
Borneol
Tertiary Alcohols
2-methyl propanol (tert-
butyl alcohol)
a-methyl- hydroxytoluene
2 pentanol
32
46
60
74
88
60
74
88
108
144
154
74
122
31(100), 32(72), 29(42), 28(9)
31(100), 45(35), 29(27), 27(24)
31(100), 27(19), 29(18), 59(12)
31(100), 56(90), 41(74), 43(64)
42(100), 55(74), 41(60), 70(56)
45(100), 43(19), 27(17), 29(12)
45(100), 27(22), 31(22), 59(20)
45(100), 43(16), 55(16), 27(13)
108(100), 107(94), 79(35)
39(32)
69(100), 87(49), 45(43), 43(42)
95(100), 41(30), 27(20), 43(18)
59(100), 31(28), 41(18), 43(12)
122(100), 107(83), 121(38),
77(32)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
a-terplneol
Isoborneol
154
154
59(100), 43(74), 93(72),
121(52)
95(100), 41(42), 27(25), 43(24)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detai1
Molecular
Weight
M/e Values (RI)
to
o
Glycols, Epoxides
A. Glycols
Ethylene glycol
(1.2-Ethanediol)
Propylene glycol
(1.2-Propanediol)
B, Epoxides
2,3-epoxy-l propanol
(glycidol)
l-chloro-2,3-epoxy propane
(a-Epichlorohydrin)
62
76
74
92
31(100), 33(32), 29(14) 32(10)
45(100), 43(14), 31(12), 27(9)
44(100), 43(89), 31(59), 18(44)
57(100), 27(39), 29(31), 49(25)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Aldehydes. Ke tones
A. Aldehydes
Formaldehyde
Acetaldehyde
Propionaldehyde
Acrolein
Butyraldehyde
Bromoform butanol
3-Methylbutanol
Benzaldehyde
B . Ketones
Acetone
Tetrachl oroacetone
Butanone
Isophrone (Isophorone)
Camphor (d)
Acetophenone
Compound
Detail
Molecular
Weight
30
44
58
56
72
?
88
106
58
194
72
138
152
120
M/e Values (RI)
29(100), 30(88), 28(31), 14(4)
29(100), 44(88), 43(50), 42(15)
29(100), 28(69), 27(58), 58(27)
27(100), 56(65), 26(59), 28(53)
44(100), 43(79), 72(73), 41(60)
Improper Name?
41(100), 29(98), 57(83), 31(72)
77(100), 106(91), 105(89),
. 51(58)
43(100), 58(37), 42(7), 27(5)
83(100), 85(65), 111(21),
113(14)
43(100), 72(21), 29(17), 27(9)
82(100), 39(88), 138(17),
41(13)
126(100), 95(97), 41(79),
81(71)
105(100), 77(83), 51(30),
120(25)
ro
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detai1
Molecular
Weight
M/e Values (RI)
Chlorohydroxy benzophenone
5,6-Benzo-9-anthrone
Dihydro(d)carvone
232
152
155(100), 232(58), 105(57),
157(32)
Unknown
81(100), 67(70), 41(59), 39(46)
ro
ro
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
INJ
CO
Carboxylic Acids and
Derivatives
A. Carboxylic Acids
Formic acid
Acetic acid
Maleic acid
Benzoic acid
Phthalic acid
Long chain acids
B. Carboxylic Acids with
Additional Functional
Groups
Hydroxyacetic acid (glylolic
acid)
Hydroxybenzoic acids (p)
3-hydroxypropanoic acid,
(6-lactone)
C. Amides
Formami de
Acetamide
'12
46
60
116
122
166
200
76
138
72
45
59
29(100), 46(61), 45(48), 28(17)
43(100), 60(99), 45(98), 44(34)
18(100), 26(99), 54(77), 25(24)
105(100), 122(78), 77(75),
51(46)
149(100), 121(25), 166(18),
105(16)
73(100), 60(93), 41(42), 43(59)
18(100), 31(79), 32(24), 17(22)
28(100), 121(26), 37(14),
138(21)
47(100), 28(93), 26(28), 43(78)
18(100), 45(56), 28(44), 29(30)
44(100), 59(93), 43(75), 15(48)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detai1
Molecular
Weight
M/e Values (RI)
ro
-fa.
6-aminohexanoic acid
(6-aminocaproic acid)
D. Esters
Methyl methacrylate
Phthalates (Diethyl
phthalate)
Adipates (Diethyl adipate)
Long chain esters
Methyl benzoate
Phenyl benzoate
Di-2-ethylhexyl phthalate
(Dop)
6-Aminohexanoic acid
(e-caprolactam)
131
100
222
202
136
198
392
113
44(100), 59(93), 43(75), 15(48)
41(100), 69(68), 39(38),
100(31)
149(100), 177(28), 150(13),
176(9)
29(100), 55(57), 111(52),
27(50)
Too vague -
105(100), 71(68), 51(38),
136(28)
•105(100), 77(29), 106(8), 51(7)
149(100), 167(41), 57(40),
43(34)
-------
Table C-l. MES Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Nitriles
Acetonitrile
1-Cyanoethane (acrylonltrile)
1,4-Dicyano-l-hydroxy butane
Benzonitrile
Naphthonitriles
41
53
124
103
153
41(100), 40(54), 39(18), 15(1)
26(100), 53(99), 52(75), 51(32)
103(100), 76(32), 50(17),
51(10)
ro
en
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Azo Compounds, Hydrazine, and
Derivatives
Di azomethane
Hydrazi ne
Dimethyl hydrazines
Di pheny1hydrazi nes
42
32
60
184
32(100), 31(44), 29(40), 30(31)
60(100), 42(98), 28(52), 45(52)
169(100), 168(56), 167(32)
51(26)
fs>
at
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
ro
-j
Ami nes
A. Primary Amines
Ethylamine
Ethanolami ne
3-Aminopropene
Propanolamine C iso)
1-Aminobutane
2-Aminobutane
Cyclohexylamine
1,2-Diaminoethane
Aniline
2-Ami notoluene .
Dimethyl aniline ,
Anisidines (p-)
Aminodiphenyl
Aminonaphthaienes (2-)
45
61
57
75
73
73
99
60
93
107
121
123
169
143
30(100,), 28(29), 44(20), 45(19)
42(100), 61(78), 43(49), 44(29)
30(100), 56(80), 28(76), 57(32}
44(100), 42(14), 58(5), 41(5)
30(100), 28(9), 41(6), 27(5)
44(100), 18(15), 58(11), 41(11)
56(100), 43(30), 28(15), 30(14)
30(100), 18(13), 42(6), 43(5)
•93(100), 66(33), 65(18), 39(18)
28(100), 106(84), 107(66),
77(24)
120(100), 121(70), 77(25),
51(16}
108(100), 123(68), 80(41),
53(22)
168(100), 167(56), 51(53),
169(52)
143(100), 115(36), 144(13),
116(13)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Oetai1
Molecular
Weight
M/e Values (RI)
1,4-Diaminobenzene
4,4'-Diami nodiphenyl
3,3'-Dichloroben2idine
4,4'-Methylene bis
(2-chloroaniline)
1 B. Secondary Amines
t Ethyleneimine
^ ; Dimethy1amine
03 I Ethylmethylamine
| Diethyl amine
Morpholine
j C. Tertiary Amines
; N,N-Dimethylaniline
108
184
252
43
45
59
73
87
121
121
108(100), 80(82), 52(39),
28(38)
252(100), 254(67), 126(16),
77(15)
42(100), 28(79), 43(55), 15(36)
44(100), 28(68), 45(51), 15(20)
58(100), 30(98), 28(37), 27(29)
57(100), 29(99), 87(69), 28(69)
120(100), 121(70), 77(25),
51(16)
120(100), 121(68), 77(25),
105(13)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
ro
<£>
Nitrosamines
Dimethylamine-N-Nitroso
Di ethylami ne-N-Ni troso
Dipropylamine-N-Nitroso
Di i sopropylami ne-N-Ni troso
Di pentylami ne-N-Ni troso
Aniline, N-Methy1-N-Nitroso
Di pheny1ami ne-N-Ni troso
74
102
130
130
158
136
198
42(100), 74(88), 43(52), 44(21)
42(100), 44(98), 102(74),
57(48)
43(100), 42(66), 70(66), 41(47)
43(100), 70(33), 42(32), 41(31)
136(100), 107(56), 77(54),
105(38)
169(100), 168(72), 167(50),
51(19)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Mercaptans, Sulfides and
M siilfldes
A. Mercaptans
Methyl mercaptan
Ethyl mercaptan
Propyl mercaptans
Butyl mercaptans
Benzenethlol
1-anthrathiol
Perchloromethyl mercaptan
B. Sulfides, Disulfides
Dimethyl sulfide
Diethyl sulfide
DiPhenyl sulfide
DiMethyl disulfide
43
62
76
90
110
210
150
62
90
186
94
47(100), 48(90), 45(47), 46(12)
62(100), 29(90), 47(80), 27(80)
47(100), 76(88), 43(80), 42(74)
56(100), 41(92), 27(57), 90(51)
110(100), 66(38), 109(25),
51(22)
47(100), 62(83), 45(59), 46(34)
75(100), 47(82), 20(72), 29(63)
186(100), 185(46), 51(26),
184(23)
94(100), 45(63), 79(59), 46(38)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detai1
Molecular
Weight
M/e Values (RI)
Sulfonic Acids. Sulfoxldes
A. Sulfonic Acids
Benzenesulfonic acid
9,10-Anthraqui none-
disulfonic acids
B. Sulfoxides
Dimethyl sulfoxide
158
368
78
158(100), 77(85), 94(74),
51(39)
63(100), 78(68), 15(40), 45(35)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detai1
Molecular
Weight
M/e Values (RI)
Benzene, Substituted Benzene
Hydrocarbons
Benzene
Toluene
Ethyl benzene
Styrene
N-Propyl benzene
Isopropyl benzene (cumene)
N-Butyl benzene
Biphenyl
4,4'-diphenylbiphenyl (P-P,
quaterphenyl)
Xylenes
Dialkyl benzenes
Te trahydronaphthalene
(Tetralin)
78
92
106
104
120
120
134
154
306
106
132
78(100), 52(17), 51(16), 77(15)
91(100), 92(76), 39(19), 65(13)
91(100), 106(31), 51(13),
39(10)
104(100), 103(39), 98(32),
51(30)
91(100), 120(24), 92(11),
65(9)
105(100), 120(26), 77(88),
51(10)
91(100), 92(55), 134(24),
27(12)
154(100), 153(32), 152(24),
76(18)
306(100), 307(26), 153(26),
152(6)
91(100), 106(62), 105(30),
77(12)
Vague description
104(100), 132(64), 91(50),
13(17)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Di hydronaphthalene
Terphenyl
Trlmethyl benzene
Tetramethyl benzene
130
230
120
134
128(100), 130(95), 129(78),
115(70)
230(100), 231(19), 115(15),
228(12)
105(100), 120(59), 119(16),
39(14)
119(100), 134(58), 43(23),
42(17)
CO
CO
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detai1
Molecular
Weight
M/e Values (RI)
CO
Halogenated Aromatic Compounds
A. Ring Substituted Aromatics
Chlorobenzene
dibromobenzenes
Bromochlorobenzenes
1,2-di chlorobenzene
1,3-dichlorobenzene
1,4-dichlorobenzene
Polychlorinated benzenes
Chloronaphthaiene
Polychlorinated biphenyls
Bromo benzene
112
234
190
146
146
146
162
156
112(100), 77(48), 114(32),
51(16)
236(100), 234(51), 238(49),
155(30)
192(100), 190(76), 111(57),
75(28)
146(100), 148(64), 111(36),
75(20)
146(100), 148(65), 111(32),
75(17)
' 146(100), 148(65), 111(32),
75(19)
Strong molecular ion - loss of
Cl
162(100), 126(13), 77(10),
63(10)
Strong molecular ion - loss of
Cl
77(100), 156(77), 158(76),
51(42)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Aromatics with Halogenated
Alkyl Side Chain
a-chlorotoluene (benzyl
chloride)
bi s-(chloromethyl)-benzene
126
174
91(100), 126(28), 65(9), 63(6)
139(100), 141(32), 174(21),
103(18)
CO
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Aromatic Nitro Compounds
Nitrobenzene
4-nitrobiphenyl; nitrobiphenyls
Chioroni trobenzenes
Methoxynitrobenzenes
Dinitrotoluenes
123
199
157
153
182
77(100), 51(59), 123(42),
50(25)
111(100), 157(73), 75(52),
113(32)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Mol ecul ar
Weight
M/e Values (RI)
Phenols
A. Monohydries
Phenol
Methyl phenols (cresols)
(p-cresol)
2-methoxyl phenol
Ethylphenols (0-ethylphenol)
Hydroxybiphenyls
Dimethylphenols (Xylenols)
(2,5)
Polyalkylphenols
B. Dihydrics, Polyhydrics
2,2'-dihydroxydi pheny1s
1,2-di hydroxybenzene
(catechy1)
1,3-di hydroxybenzene
(resorcinol)
1,4-di hydroxybenzene
(hydroquinone)
94
108
124
122
170
122
186
110
110
110
94(100), 66(28), 39(28), 65(22)
107(100), 108(75), 77(30),
79(26)
124(100), 94(57), 81(39),
39(31)
107(100), 122(40), 77(18),
79(9)
170(100), 169(60), 141(24),
115(15)
122(100), 107(87), 121(43),
77(30)
Too vague
186(100), 157(28), 158(23),
131(22)
110(100), 64(39), 63(22),
52(15)
110(100), 81(22), 39(22),
53(19)
110(100), 53(27), 81(22),
55(22)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
1,2,3-tri hydroxybenzenes
C. Fused ring hydroxy
compounds
a-naphthanol
3-naphthanol
Phenthrols (Phenanthrols)
Indanols
Acenaphthenols
2-hydroxyfluorene
2-hydroxydi benzofuran
126
144
144
194
134
170
182
184
126(100), 108(33), 80(30),
52(22)
144(100), 115(74), 116(37),
145(10)
144(100), 115(63), 116(28),
57(15)
43(100), 194(94), 165(78),
39(22)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Halophenols
2-chlorophenol
2,4-dichlorophenol
Pentachlorophenol
Chlorinated cresols
128
162
264
144
128(100), 64(35), 130(32),
63(14)
162(100), 164(63), 63(30),
98(27)
CO
VO
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detai1
Molecular
Weight
M/e Values (RI)
Mltrophenols
2-nitrophenol
3-nltrophenol
4-nitrophenol
01nltrophenols
o-cresol, dinltro
p-cresol, dinltro
2-ami no-4,6-d1nltrophenol
Trinltrophenol
139
139
139
184
198
198
199
229
139(100}, 65(36), 64(22),
63(22)
65(100), 39(88), 139(74),
93(70)
139(100), 65(35), 64(20),
63(21)
198(100), 182(36), 77(35),
51(27)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Fused Polycyclic Hydrocarbons
Naphthalene
Monoalkyl naphthalenes
Phenyl naphthalenes (a)
Dimethyl naphthalenes
Acenaphthene; acenaphthylene
Anthracene
2,7-dimethy1anthracene
Phenanthrene
Methylphenanthrenes
Naphthacene
1,2-benzanthracene
9,10-dimethyl-l,2-benzanthra-
cene
Benzo(c)phenanthrene
128
204
156
154
178
206
178
192
228
228
256
228
128(100), 51(12), 129(11),
64(11)
Too vague
204(100), 203(68), 202(47),
101(34)
156(100), 141(26), 155(30),
153(14)
154(100), 153(95), 152(53),
76(26)
178(100), 176(16), 179(16),
178(100), 179(15), 176(15),
89(14)
228(100), 229(30), 114(29),
226(21)
228(100), 229(19), 226(19),
114(18)
256(100), 241(40), 239(37),
240(24)
228(100), 226(45), 227(34),
118(31)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Chrysene
Methyl chrysenes
Triphenylene (9,10 benzphen-
anthracene
Pyrene
1-methyl pyrene
1 , 2-benzonaphthacene
Benzo(b)chrysene
1,2:3 ,4-di benzanthracene
l,2:5,6-dibenzanthracene
Benzo[a]pyrene
Benzo[e]pyrene
Perylene
Picene (dibenzo(a,i)phenan-
threne)
Compound
Detail
Molecular
Weight
228
242
228
202
216
278
278
278
278
252
252
252
278
M/e Values (RI)
228(100), 226(22), 229(19),
114(16)
242(100), 239(20), 243(20),
241(17)
228(100), 226(22), 229(21),
113(17)
202(100), 101(26), 208(17),
100(17)
216(100), 215(61), 94(26),
217(18)
278(100), 276(81), 138(25),
1 279(22)
278(100), 139(24), 279(24),
276(15)
278(100), 139(24), 279(24),
276(16)
252(100), 126(23), 253(21),
250(16)
252(100), 126(23), 252(21),
250(16)
252(100), 253(22), 126(21),
250(21)
PO
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Dibenzo[a,h]pyrene
Dibenzo[a,i]pyrene
Dibenzo[asj,]pyrene
Benzo[g,h,i]perylene
Coronene
302
302
302
276
300
276(100), 138(37), 277(55)
300(100), 150(78), 149(66),
148(37)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Fused Non-Alternant Polycyclic
Hydrocarbons
Idene and derivatives (alkyl)
Dicyclopentadiene
Fluorene and derivatives (alkyl)
Cyclopentanonaphthalene
2,3-benzofluorene
Fluoranthene
1,2-benzofluorene
4-H^cyclopenta(def)phenanthrene
Benzo(k)fluoranthene
Benzo(e)fluoranthene
Benzo(j)f1uoranthene
1,2:5,6-dibenzof1uorene
3-methyl cholanthrene
Indeno (l,2,3,c,d}pyrene
Indene
Fluorene
116
130
166
216
202
216
252
252
252
266
268
276
116(100), 115(84), 63(14),
39(11)
166(100), 165(81), 163(15),
164(14)
216(100), 215(78), 217(18),
107(16)
202(100), 101(22), 203(17),
200(14)
216(100), 215(62), 107(21),
217(19)
252(100), 253(23), 125(16),
Similar to (k)
Similar to (k)
268(100), 252(39), 253(39),
267(24)
276(100), 138(28), 277(27)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Truxene (tribenzylene benzene)
Tetrahydrof1uoranthene
?
206
178(100), 206(67), 89(28),
76(19)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
4*
0>
Heterocyclic Nitrogen Compounds
A. Pyrldlne and Substituted '
Pyrldines
Pyridine
Monosubstituted alkyl
pyrldines
phenyl pyrldines
Chi oropyri dine
Disubstituted, poly-
substituted pyridines
(dimethyl pyridine)
B. Fused 6-membered Ring
Heterocycles
Quincline, isoquinoline
Methylquinolines,
methylisoquinolines
Dimethylquinolines,
dimethyli soqui nol1nes
Acridine
Dihydroacridine
79
93
155
113
107
129
143
157
179
181
79(100), 52(74), 51(36), 50(26)
93(100), 66(41), 39(31), 92(20)
113(100), 78(49), 115(32),
18(24)
107(100), 106(65), 39(32),
79(29)
129(100), 102(22), 51(18),
128(16)
143(100), 142(43), 28(24),
115(16)
157(100), 156(33), 158(13),
115(10)
179(100), 178(14), 180(14),
89(12)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
c.
Benzo(c)quinoline
Benzo(f)quinoline
Benzo(h}quinoline
Benz(a)acr1dine
Benz(c)acridine
Dibenz(a,j)acridine
Dibenz(a,h)acridine
D1benz(c,h)acridine
Indeno(l,2-b)quinoline
Indeno(l,2,3,i,j)isoquino-
line
Pyrrole and Fused Ring
Derivatives of Pyrrole
Pyrrole
Indole
Methylindoles
Carbazole
179
179
179
229
229
279
279
279
67
117
131
167
179(100), 178(24), 180(16),
151(12)
179(100), 178(24), 151(17),
76(16)
179(100), 178(24), 180(14),
151(11)
67(100), 41(58), 39(58), 40(51)
117(100), 90(40), 89(24),
130(100), 131(59), 77(14),
65(10)
167(100), 166(18), 83(14),
168(13)
-------
Table C-l. MEG Organic/Major Mass Peak
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Methylcarbazoles (9-)
Benzo(a)carbozole
Dibenzo(a,g)carbozole
Dibenzo(a,i)carbozole
Di benzo(c,g)carbozole
Nitrogen Heterocycles
containing additional
Heteroatoms
Benzothiazole
Methyl benzothiazoles
181
231
281
281
281
135
149
135(100), 108(35), 69(27),
63(13)
148(100), 108(32), 69(29),
149(17)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
10
Heterocyclic Oxygen Compounds
Furan
Benzofurans
Dibenzofuran
Methyldi benzofurans
Naphthofurans
Benzo[b]naptho[2,3-d]furan
Phenanthro[9,10-b]furan
1,9-benzoxanthene
68
118
168
182
168
218
218
232
39(100), 68(71), 37(18), 29(16)
118(100), 90(30), 89(29),
63(13)
168(100), 139(23), 169(13),
84(11)
-------
Table C-l. MEG Organic/Major Mass Peaks
Category
Compound
Detail
Molecular
Weight
M/e Values (RI)
Heterocyclic Sulfur Compounds
Thiophene
Methylthiophenes
Dimethylthiophenes
Trimethyl Thiophene
2,2'-Bithiophene
Benzo[b] thiophene
Dibenzothiophene
Benzonaphthathiphene
Tetramethylthiophenes
84
98
112
126
166
134
184
234
140
84(100), 58(65), 45(55), 39(28)
97(100), 98(55), 45(21), 39(17)
111(100), 112(78), 97(58),
59(22)
111(100), 126(12), 125(58),
45(27)
166(100), 121(29), 45(26),
69(16)
134(100), 89(10), 135(10),
63(8)
184(100), 185(14), 139(12),
92(11)
234(100), 235(18), 117(18),
232(9)
-------
REFERENCES
1. J.W . Hamersraa and S.L. Reynolds "Field Test Sampling Analytical
Strategies and Implementation Cost Estimates: Coal Gasification and
Fluid Gas Desulfurization," EPA-600/2-76-0935, April 1976.
2. J.W. Hamersam, S.W. Reynolds, and F.R. Maddalone, "IERL-RTP Procedures
Manual: Level I Environmental Assessment," EPA-600/2-76-16a, June
iy/D.
3* /25ftr!!ep!rl °n *"? Development of a Multimedia Environmental Goals
(MEG) Chart, Battelle Columbus Laboratories, August 31, 1976.
4. J.M Harless, MP. Kilpatrie W.C. Thomas, and G.C. Page, "Summary of
Results from the Holston Gasification Plant Level 1 Pilot Study"
K(,COn^e^!al,D1scussion Draft> 17 -April 1978, Radian Contract
No. 200-143-13-01, Radian DCN No. 78-200-143-58.
5. J.C. Harris and P.L. Levins, EPA/IERL-RTP. "Interim Procedures for
Level 2 Sampling and Analysis of Organic Materials," EPA-600/7-78-016,
February 1978.
6. L.E. Ryan, "Level 2 Results on Fluidized Bed Combustor Samples,"
(Draft) EPA Contract #68-01-3152, March 17, 1978.
7. R. Maddalone, Task 28, EPA 69-02-2165, Monthly Technical Progress
Narratives 9 and 10. February, April, May 1977.
8. Mem" Safety Appliances Company, Technical Bulletin No. 400 Penn Center
Blvd., Pittsburg, Pa. 15235.
9. J. Thomas, Jr. and H.J. Gluskoter, "Determination of Fluoride in
Coal with the Fluoride Ion Selective Electrode," Analytical Chemistry.
46(a), 1321, August 1874
10. Thomas A. Carlson, Photoelectron and Auger Spectrochopy, New Yorj^,
Plenum Press, 1975.
11. Level 1 Pilot Study on Low-BTU Gasifiers at the Holston Army Ammuni-
tion Plant EPA Contract No. 68-02-2165 task 32, Task Manager L.E. Ryan
(Draft Report)
12. "Procedures Manual for Environmental Assessment of Fluidized-Bed
Combustion Procedures," EPA-600/7-77-009, The Mitre Corporation,
January 1977. Table Modification.
13. American Society for Testing and Materials. Gaseous Fuels, Coal and
Coke, Part 19. Philadelphia, Pennsylvania, 1971!
14. R.R. Ruch, H.J. Gluskoter and N.F. Shimp, "Occurrence and Distribu-
tion of Potentially Volatile Trace Elements in Coal," Environmental
Geology Notes, No. 72, August 1974.
151
-------
TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing;
. REPORT NO.
EPA-600/7-79-063a
2.
3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE APPROACH TO LEVEL 2 ANALYSIS
BASED ON LEVEL 1 RESULTS, MEG CATEGORIES
AND COMPOUNDS, AND DECISION CRITERIA
5. REPORT DATE
February 1979
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
L.E.Ryan, R. G. Beimer, and R. F. Maddalone
8. PERFORMING ORGANIZATION REPORT NO
9. PERFORMING ORGANIZATION NAME AND ADDRESS
TRW, Inc.
Defense and Space Systems Group
One Space Park
Redondo Beach, California 90278
10. PROGRAM ELEMENT NO.
EHE623A
11. CONTRACT/GRANT NO.
68-02-2613, Task 6
Li.
12. SPONSORING AGENCY NAME AND ADDRESS
EPA, Office of Research and Development
Industrial Environmental Research Laboratory
Research Triangle Park, NC 27711
13. TYPE OF REPORT AND PERIOD COVERED
Task Final: 12/76 - 12/78
14. SPONSORING AGENCY CODE
EPA/600/13
is. SUPPLEMENTARY NOTES
2825.
project officer fe Waiter B. Steen, MD-61, 919/541-
i6. ABSTRACT Tne report describes an approach to the decision criteria needed to pro-
ceed from the initial emission screening analysis (Level 1) to the detailed emission
characterization (Level 2), and a Level 2 analytical approach. The decision criteria,
considering only the available Level 1 chemical data, provide a basis which can be
used for proceeding to a Level 2 emission characterization based on chemical cor-
relation with compounds identified as Multimedia Environmental Goals (MEGs). The
report discusses the types of Level 1 environmental assessment samples, and the
chemical data available which can be prioritized for a MEG-based Level 2 plan. It
presents a logic network for determining the need for a Level 2 sampling effort. K
also presents an integrated approach to Level 2 inorganic compound analysis, an
identification scheme consisting of characterization of the initial sample, of bulk
composition, and of individual particles. Detailed logic networks are included to
provide direction to the analyst during the identification process. The analysis of
solid and liquid samples for organic compounds is discussed, using mainly combined
gas chromatography/mass spectrometry. A logic network is provided for the organic
analyst.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS
COS AT I Field/Group
Pollution
Assessments
Analyzing
Sampling
Organic Compounds
Inorganic Compounds
Gas Chromato.-
graphy
Mass Spectroscopy
Pollution Control
Stationary Sources
Environmental Assess-
ment
Level 2 Analysis
MEGs
13B
14B
07C
0702
07D
8. DISTRIBUTION STATEMENT
Unlimited
19. SECURITY CLASS (ThisReport)
Unclassified
21. NO. OF PAGES
163
20. SECURITY CLASS (TMspage)
Unclassified
22. PRICE
EPA Form 2220-1 (9-73)
152
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