GC/MS (Gas Chroraatography-Mass Spectrometry)
Analysis of Organises in Drinking Water
Concentrates and Advanced Waste Treatment
Concentrates. Volume 1
Battelle Columbus JUabs., OH
Prepared for
Health Effects Research Lab.
Research Triangle-Park, NC
Nov 84
U.S. DEPARTMENT OF COMMERCE
National Technical Information Service
NTIS
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PEB5-128221
EPA-600/l-84-020a
November 1984
GC/MS ANALYSIS OF ORGANICS IN DRINKING
WATER CONCENTRATES AND ADVANCED
WASTE TREATMENT CONCENTRATES
Volume 1
Analysis Results for 17 Drinking
Wc'.ter, 16 Advanced Waste Treatment
and 3 Process Blank Concentrates
by
Samuel V. Lucas
Battelle
Columbus Laboratories
coiumbus, Ohio jS ep/v,NEIC UBRARY
Denver Federal Center
Building 25, £nt. E-3
PO Box 25227
Oenver, CO 80225-0227
Contract No. 68-03-2548
Project Officer
Frederick C. Kopfler
U.S. Environmental Protection Agency
Health Effects Research Laboratory
Cincinnati, Ohio 45268
HEALTH EFFECTS RESEARCH LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
RESEARCH TRIANGLE PARK, NORTH CAROLINA 27711
REPRODUCED BY
NATIONAL TECHNICAL
INFORMATION SERVICE'
U.S. OEPARTMENt OF COMMERCE
SPRINGFIELD. V*. 221&I
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TPCMNICAI. KEPORT DATA
n,l In::: i, I.,-in nil /In rn,rsc hi Inn n
. Htl'UHT NO
EPA-600/l-84-020a
> TITLL-ANO^UUTITLE GC/MS ANALYSIS 0? ORGANICS IN DRINKING
WATER CONCENTRATES AND ADVANCED WASTE TREATMENT CONCEN-
TRATES: VOLUME 1. Analysis Results for 17 Drinking
Water, 16 Advanced Waste Treatment and 3 Process
3 ncClfiLNT 5 ACCL.. O'. '-C
?33S 128221
'j REI'GHT DATE
November 1934
6 PLnr-onMiNG GHG.V.IZA .
7. AUTHORS) Blank Concentrates
Samuel V. Lucas
8 PERFORMING CJHGANiZATICf.
f PERFORMING ORGANISATION NAME AND
Battelle
Columbus Laboratories
505 King Avenue
Columbus, Ohio 43201
10 P h O G R A M E L E M L i.
CBMCIA
II C O r. T R A C T - C i > '• ' • T 11 O
Contract No. 68-03-2548
12. SPONSORING ACL'JC't NAME AND ADDRESS
Health Effects Research Laboratory
Office of Research & Development
U.S. Environmental Protection Agency
Research Triangle Park, NC 27711
13 TYPE OF REPOPT AN D PE P I C D C ^ .'L P E :
Final Report
SPONSORING AGENCY CODE
EPA-600/11
Mi. SUPPLEMENTARY NOTES
Project Officer: Dr. Frederick C. Kopfler, TMD, HERL (Cl)
16. ABSTRACT
The goal of this research program was to provide a detailed chemical char-
acterization of organic material concentrated from large volumes (1,500 liters to
15,000 liters) of finished drinking water (DW) and finished water from advanced waste
treatment (AWT) plants. The approach used was organic compound identification based on
glass capillary gas chromatography-mass spectrometry (GC-MS) analysis of the frac-
tionated concentrate. The purpose of the research program was to enable EPA scientists
to correlate the results of the detailed chemic;! characterization with those from
other research programs testing the potential biological activity (i.e., mutagenicity)
of the concentrates. Fifteen DW concentrates, sixteen AWT concentrates and five
concentrate production method blanks were analyzed.
The cities represented by the DW samplings were Cincinnati, Miami, New Orleans,
Ottumwa (Iowa), Philadelphia and Seattle. Most of the unrecovered organic portion and
the extracted material not amenable to GC-MS analysis appeared to be humic substances.
In the 15 DW concentrates, 1091 organic compounds were identified in a total of 2383
detection instances.
The AWT plans sampled were located at Escondido, Lake Tahoe, Orange County and
Pomona (all in California), Dallas, and Washington, D.C. (Blue Plains site). In the 16
AWT concentrates, 991 organic compounds were identified in a total of 2097 detection
instancer . ^____
KEY WOllUD AND DOCUMl NT ANALYSIS
IJLLCnil'TOML,
Organic Contaminants
Drinking Water
Advanced Waste Treatment
Municipal Wastewater
11 IDLNIIMLHS/OI'I N f NUE n T t MM
cor,AT i I ic'J
la Ulil MILU I I0'« ST A 1 LMLTj I
Unlimited Distribution
EP*
I 'I jt (_ u M I 1 Y C L A;.b f I tin A'I I'.-r 11
Unclass i fi ed
32/
70 GlCuHilv CL AjS i 7/i/i
Unclassi f ied
uS C Ci 1 ION ' » O»-iCLI_Tr
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NOTICE
This document has been reviewed in accordance with
U.S. Environmental Protection Agency policy and
approved for publication. Mention of trade names
or commercial products does not constitute endorse-
ment or recommendation for use.
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FOREWORD
The many benefits of our modern, developing, industrial society are
accompanied by certain hazards. Careful assessment of the relative risk of
existing and new man-made environmental hazards is necessary for the estab-
lishment of sound regulatory policy. These regulations serve to enhance the
quality of our environment in order to promote the public health and welfare
and the productive capacity of our Nation's population.
The complexities of environmental problems originate in the deep inter-
dependent relationships between the various physical and biological segments
of man's natural and social world. Solutions to these environmental problems
require an integrated program of research and development using input from a
number of disciplines. The Health Effects Research Laboratory-, Research
Triangle Park, NC and Cincinnati, OH conducts a coordinated environmental
health research program in toxicology, epidemiology and clinical studies
using human volunteer subjects. Wide ranges of pollutants known or suspected
to cause health problems are studied. The research focuses on air pollutants,
water pollutants, toxic substances, hazardous wastes, pesticides and non-
ionizing radiation. The laboratory participates in the development and
revision of air and water quality criteria and health assessment documents
on pollutants for which regulatory actions are being considered. Direct
support to the regulatory function of the Agency is provided in the form of
expert testimony and preparation of affidavits as well as expert advice to
the Administrator to assure the adeq'uacy of environmental regulatory decisions
involving the protection of the health and welfare of all U.S. inhabitants.
The purpose of this research program was to enable EPA scientists to
correlate the results of the detailed chemical characterization with those
from other research programs testing the potential biological activity (i.e.,
mutagenicity) of the concentrates.
F. Gordon Hueter, Ph.D.
Director
Health Effects Research Laboratory
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ABSTRACT
The goal of this research, program was to provide a detailed chemical
characterization of organic material concentrated from large volumes (1,500
liters to 15,000 liters) of finished drinking water (DW) and finished water
from advanced waste treatment (AWT) plants. The approach used was organic
compound identification based on glass capillary gas chromatography-mass
spectrometry (GC-MS) analysis of the fractionated concentrate. The complex
organic concentrates were partitioned into less complex fractions by liquid-
liquid partitioning, methylation of acidic components and fractionation of
neutral species on silica gel. The purpose of the research program was to
enable EPA scientists to correlate the results of the detailed chemical char-
acterization with those from other research programs testing the potential
biological activity (i.e., mutagenicity) of the concentrates. Fifteen DW
concentrates, sixteen AWT concentrates and five concentrate production method
blanks were analyzed.
The cities represented by the DW" samplings were Cincinnati, Miami, New
Orleans, Ottumwa (Iowa), Philadelphia and Seattle. For DW concentrates, only
20 percent of the organic material in the concentrates for a given sampling
was recovered in analyzed fractions, and only one half of that material was
of a chemical type suitable for GC-MS analysis. Most of the unrecovered
organic portion and the extracted material not amenable to GC-MS analysis
appeared to be humic substances. In the 15 DW concentrates, 1091 organic
compounds were identified in a total of 2383 detection instances.
The AWT plants sampled were located at Escondido, Lake Tahoe, Orange
County and Pomona (all in California). Dallas, and Washington, D.C. (Blue
Plains site) . Less humic material was present in the AWT concentrates with
the result that about 50 percent of the organic material was recovered in
the GC-MS analyzed fractions. In the 16 AWT concentrates, 991 organic com-
pounds were identified in a total of 2097 detection instances.
The GC-MS data were surveyed by computer for 53 compounds which might
have health effect significance. For DW concentrates, 31 of these compounds
were found to be present in a total of 108 detection instances. For the AWT
concentrates, 33 compounds were found in a total of 117 detection instances.
The DW concentrates uniformly exceeded the AWT concentrates in containing
more and higher concentrations of materials attributable to either pollution
from the organic chemical industry or consumer use of products containing
chemicals. This.difference was probably due to the use of granular activated
carbon (GAG) or reverse osmosis RO as a final treatment step in the AWT plants
but not the DW treatment plants. All DW samples contained some indicators of
water re-use (i.e., drugs or metabolites) ranging from very slight (Seattle)
to substantial (Miami).
IV
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Small volume samples (10 to 30 liters) were also analyzed to study the
effectiveness of the RO and GAG treatments in retaining organic molecules.
These results together with some of the DW concentrate results indicate that
RO membranes do not effectively retain apolar organic molecules.
This report was submitted in fulfillment of U.S. EPA Contract 68-03-2548
by Battelle Columbus Laboratories and covers the period June, 1977 to
November, 1980. Work was completed as of November, 1980.
v
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VOLUME 1
CONTENTS
_ , - . iii
Foreword . . . -
Abstract . 1V
Figures v111
Tables «
Abbreviations and Symbols ^1
Brief Description of All Volumes of the Final Report xiv
Acknowledgments xvl
1. Introduction 1
2. Conclusions 3
3. Recommendations 5
4. Background Information on the Organic Concentrates 7
Concentrate Production Methods ......... 7
The RO Method Blank. 11
The Water Used for Concentrate Production 11
5. Analytical Scheme 13
Rationale for the Analytical Scheme 13
Internal Standards 16
Partitioning of the Concentrates 16
Residue Weight Analysis 21
Gas Chromatographic Analysis 21
Glass Capillary GC-MS Analysis 24
GC-MS Data Processing 28
Archival 28
Correction for the Process Blank 29
Compound Identification and Confirmation . 29
Computerized Data Searching for Specified Compounds 31
Quantification of Identified Compounds 33
Data Management 36
Report Generation 38
Suggestions for Improvements to the Analytical Scheme 42
6. Results and Discussion 44
Organization of the Presentation 44
- Overview of the Results 44
Comparison of Residue Weights and Compound
Identification Statistics 44
Detection of Special Interest Compounds 48
Tables of Identified Compounds 49
Use of the Molecular Weight Table 53
Additional Listings of Compound Identification Results ... 53
Number of Identified Compounds .....'•••• 53
Results of Analysis of Blank Concentrates • 5^
Discussion of DW Concentrate Analysis Results 55
Summaries of the Results for Each Sampling 55
VI
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Volume 1
CONTENTS (Continued
Cincinnati, Ohio, October 17, 1978 55
Cincinnati, Ohio, January 14, 1980 62
Miami, Florida, February 3, 1976 65
New Orleans, Louisiana, January 14, 1976 68
Philadelphia, Pennsylvania, February 10, 1976 70
Ottumwa, Iowa, September 10, 1976 74
Seattle, Washington, November 5, 1976 77
Comparison and Discussion of DW Concentrate Analysis
Results 83
Discussion of AWT Concentrate Analysis Results 98
Summaries of the Results for Each Sampling 98
Lake Tahoe, California, October 24, 1974 99
Pomona, California, September 25, 1974 101
Pomona, California, October 2, 1974 103
Pomona, California, June 17, 1975 104
Orange County, California, January 27, 1976 105
Orange County, California, February 3, 1976 106
Escondido, California, July 8, 1975 108
Dallas, Texas, November 11, 1974 109
Blue Plains, Washington, D.C., September 20, 1974 .... 110
Blue Plains, Washington, D.C., May 31, 1975 113
Comparison and Discussion of AWT Concentrate Analysis
Results 114
Comparison of DW and AWT Concentrate Compound
Identification Results 129
References 225
Appendices
A. Deliverables 226
Deliverables Required by the Contract 226
Additional Deliverables Provided by Battelle 232
B. System for Naming GC-MS Data Files 236
C. Publications and Presentations Resulting from the Contract
Work 241
D. Identified Compounds Listed by Molecular Weight 243
E. HERL Procedures for the Preparation of the Cincinnati, Ohio,
October 17, 1978 Concentrates 292
F. Contents and Lists of Tables for Volumes 2 and 3 293
vii
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VOLUME 1
FIGURES
Number Page
1 Schematic diagram of the reverse osmosis concentrator used
by GSRI ............................ 10
2 Partial gas chromatogram (FID) of a typical unpartitioned
water concentrate sample ................... 14
3 Analytical scheme for the analysis of water concentrates ..... 15
4 Partitioning scheme for water concentrates derived from solvent
extraction of reverse osmosis concentrates .......... 18
5 Partitioning scheme for water concentrates derived from XAD-2
extraction of reverse osmosis concentrates .......... ' 19
6 Typical column evaluation chromatogram for a 30M SP2100 (.apolar)
capillary column ....................... 23
7 Typical column evaluation chromatogram for a 40M SP1000 (polar)
capillary column ..... .................. 23
8 Typical GC-MS daily performance verification test chromatogram
for the SP2100 (apolar) capillary column ........... 26
9 Typical GC-MS daily performance test chromatogram for the
SP1000 (polar) capillary column. ...... ......... 27
viii
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VOLUME 1
TABLES
Number Page
1 Source Water, Sampling and Concentrate Production Information
for Drinking Water Concentrates 8
2 Source Water, Sampling and Concentrate Production Information
for Advanced Waste Treatment Concentrates 9
3 Deuterium-labeled Compounds Used as Internal Standards 17
4 List of the 53 Compounds for which GC-MS Data were Searched ... 32
5 GC Peak Relative Size (RS) Values for Semi-quantitative
Estimation of Compound Concentrations 35
6 Contents of the Individual Reports for DW and AWT Concentrates. . 39
7 Pertinent Concentrate Data for Drinking Water 45
8 Pertinent Concentrate Data for Advanced Waste Treatment Water . . 46
9 Combined Listing of Identified Compounds Found in DW
Concentrates 133
10 Combined Listing of Identified Compounds Found in AWT
Concentrates 163
11 Combined Listing of Identified Compounds Found in DW and AWT
Concentrates 188
12 Special Interest Compounds Found in DW Concentrates 87
13 Occurrence of Molecular Functional Group Types in DW
Concentrates, Showing the Number of Occurrences as a
Percentage of the Total Number of Identified Compounds .... 90
14 Occurrence of Molecular Functional Group Types in DW
Concentrates, Showing the Total GC Peak Size for Each
Group on Both GC Columns 93
15 Special Interest Compounds Found in AWT Concentrates 118
IX
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VOLUME 1
TABLES (Continued)
Number Page
16 Occurrence of Molecular Functional Group Types in AWT
Concentrates, Showing the Number of Occurrences as
a Percentage of the Total Number of Identified Compounds. . . . 122
17 Occurrence of Molecular Functional Group Types in AWT
Concentrates, Showing the Total GC Peak Size for Each
Group on Both GC Columns 123
18 Distribution of Compound Identification Instances for DW
and AWT Concentrates 132
APPENDIX A
Al Analysis Reports for Drinking Water Concentrates. „-. . » ... . .. . 227
A2 Analysis Reports for Advanced Waste treatment Water Concentrates. . 228
A3 Analysis Reports for Process Blank Concentrates .......... 229
APPENDIX D
Dl Compounds in the Chemically Descriptive Level of the Identified
Compound Data Base—Listed by Increasing Molecular Weight . . . 245
x
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ABBREVIATIONS AND SYMBOLS
ABBREVIATIONS IN THE TEXT
(See also, Appendix B)
AWT — advanced waste treatment
BOD — biological oxygen demand
CA — cellulose acetate (RO membrane)
CAS — Chemical Abstracts Service
COD — chemical oxygen demand
DFTPP — decafluorotriphenylphosphine
DW — drinking water
EICP — extracted ion current profile
FC-43 — perfluorotributylamine
GAG — granular activated carbon
GC — gas chromatography
GC-FID — GC analysis with flame ionization detection
GC-MS — gas chromatography-mass spectrometry
GSRI — Gulf South Research Institute
HEB — hexaethylbenzene
HERL-CI — Health Effects Research Laboratory, U.S.
EPA, Cincinnati, Ohio
IFSS — data acquisition program for the System/150 GC-MS
data system
IS — internal standard
K-D — Kuderna-Danish, solvent evaporation apparatus
m/e — mass Catomic mass units) to charge (electronic charge
units) ratio
}ig/l — microgram per liter
ng/1 — nanogram per liter
NTIS — National Technical Information Service
NYL — nylon hollow fiber (RO cartridge)
ppb — part per billion (1 pg/1)
ppt — part per trillion 01 ng/1)
RF — response factor
RO — reverse osmosis
RS — relative size; a designator of the size of GC-MS peaks
relative to the internal standard, HEB
SGCSM — standard GC separation mixture
SIS — selected ion search; an EXCP computer program
SP1000 — a polar GC liquid phase consisting of Carbowax 20M
(.polyethylene glycol) terminated with
nitroterephthalic acid
SP2100 — a nonpolar GC liquid phase consisting of methylsilicone
fluid
TOG — total organic carbon
Xl
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ABBREVIATIONS AND SYMBOLS (Continued)
XAD-2 — a macroreticular adsorption polymer of polystyrene/2%
divinylbenzene copolymer, Rohm and Haas Co.
THREE-DIGIT CONCENTRATE CODE IN THE TEXT AND
COMPUTER-PRINTED TABLES
DW Concentrates
M2C — Miami, Florida, combined solvent extract, 2/3/76
M2X — Miami, Florida, XAD-2 extract, 2/3/76
N2C — New Orleans, Louisiana, combined solvent extract, 1/14/76
N2X — New Orleans, Louisiana, XAD-2 extract, 1/14/76
02C — Ottumwa, Iowa, combined solvent extract, 9/10/76
02X — Ottumwa, Iowa, XAD-2 extract, 9/10/76
P2C — Philadelphia, Pennsylvania, combined solvent extract, 2/10/76
P2X — Philadelphia, Pennsylvania, XAD-2 extract, 2/10/76
S2C — Seattle, Washington, combined solvent extract, 11/5/76
S2X — Seattle, Washington, XAD-2 extract, 11/5/76
TIC — Cincinnati, Ohio, combined solvent extract, 10/17/78
T1X — Cincinnati, Ohio, XAD-2 extract, 10/17/78
T1Y — Cincinnati, Ohio, direct XAD-2 extraction, 10/17/78
T4C — Cincinnati, Ohio, combined solvent extract, 1/14/80
T4X — Cincinnati, Ohio, XAD-2 extract, 1/14/80
VIC — Poplarville, Mississippi, combined solvent extract, 3/2/79
— Poplarville, Mississippi, XAD-2 extract, 3/2/79
AWT Concentrates
B1M — Blue Plains, Washington, D.C., 9/19/74, CH2C12 extract, cellulose
acetate RO brine
BIN — Blue Plains, Washington, D.C., 9/19/74, CHaCl2 extract, acidic
cellulose acetate RO brine
B2C — Blue Plains, Washington, D.C., 5/29/75, combined solvent extract
C1P — Pomona, California, 9/25/74, pentane extract, cellulose acetate
RO brine
C1M — Pomona, California, 9/25/74, CH2C12 extract, acetate RO brine
"C1N — Pomona, California, 9/25/74, CH2C12 extract, acidic cellulose
acetate RO brine
C2N — Pomona, California, 10/2/74, CH2C12 extract, acidic cellulose
acetate RO brine
C3C — • Pomona, California, 6/17/75, combined solvent extract
D2N — Dallas, Texas, 12/10/74, CH2C12 extract, acidic cellulose
acetate RO brine
E1C — Escondido, California, 7/8/75, combined solvent extract
L2P — Lake Tahoe, California, 10/24/74, pentane extract, cellulose
acetate RO brine
L2M — Lake Tahoe, California, 10/24/74, CH2C12 extract, cellulose
acetate RO brine
L2N — Lake Tahoe, California, 10/24/74, CH2C12 extract, acidic
cellulose acetate RO brine
xii
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THREE-DIGIT CONCENTRATE CODE IN THE TEXT AND
COMPUTER-PRINTED TABLES (Continued)
AWT Concentrates (Continued)
L2D — Lake Tahoe, California, 10/24/74, CH2C12 extract, acidic
cellulose acetate RO brine
R1C — Orange County, 'California, 1/27/76, combined solvent extract
R2C — Orange County, California, 2/3/76, combined solvent extract
Blank Concentrates
T2B — XAD-2 resin elution with diethyl ether
X1C — evaporated extraction solvent Cpentane and methylene chloride)
XIX — XAD-2 resin elution with ethanol
ABBREVIATIONS IN THE COMPUTER-PRINTED TABLES
CAS NO. — numbers with five or more digits: Chemical Abstracts Service
compound registry number; numbers with four or fewer digits
are Battelle numbers
MW — molecular weight
DW — drinking water
AWT — advanced waste treatment
T4 — data set for samples reported in Volume 3
T5 — data set for samples reported in Volume 3
RS — relative size; a designator of the size of GC-MS peaks
relative to the internal standard, HEB
SYMBOLS IN THE COMPUTER-PRINTED TABLES
The following four symbols may appear to the left of the compound name:
* — designates a compound on the list of 53 compounds (.see Table 4,
Volume 1) for which, the GC-MS data was specifically searched
+ — designates a compound which, is on EPA's Consent Decree Priority
Pollutant list Csemi-volitile compounds)
$ — designates a compound which is on the Chemical Indicators of
Industrial Pollution list (Federal Interium Primary Drinking
Water Regulations, February 9, 1978)
% — designates a compound which is an entry in the EMIC database of
compounds on which, bioactivity data is available from Oak
Ridge National Laboratory
xiii
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BRIEF DESCRIPTION OF ALL VOLUMES OF THE FINAL REPORT
There are three volumes of this Final Report on EPA contract 68-03-2548.
Each is briefly described below and the Tables of Contents of Volumes 1 and 3
are reproduced in Appendix B.
VOLUME 1
Volume 1 covers all aspects of analysis of the concentrates produced
from large volumes (greater than 1415 liters (400 gallons)) of drinking water
(DW) and advanced waste treatment (AWT) water. Eight key computer-printed
tables which show organic compound identification results in integrated list-
ings for the related sets of concentrates (DW and AWT) are contained in
Volume 1. All discussion of the analysis results for large-volume DW and AWT
concentrates as well as a complete description of the analytical scheme, com-
puterized data management and accounting of all contract deliverables are
contained in Volume 1.
VOLUME 2
Volume 2 contains 22 computer-printed tables which comprise the com-
plete set of compound identification results covering the DW and AWT large-
volume concentrates. Eight of these 22 tables are also incorporated in
Volume 1 as the "core" set of information. The 14 computer-printed tables of
Volume 2 which do not appear in Volume 1 provide the following additional in-
formation:
I. Identification status (.confirmed or tentative) for all instances
of compound identification in concentrates.
2. Systematic names, molecular formulas and molecular weights of all
identified compounds.
3. Functional group information for each concentrate showing the total
relative size values for each functional group on each of the two
GC columns (SP1000 and SP2100).
VOLUME 3
Volume 3 covers the analysis of all small volume (.10 to 30 liters)
samples. These samples comprise the following sets:
1. A group of 13 samples of DW associated with granular activated
carbon (GAG) contact treatment using unit "A" at the Cincinnati
Waterworks„
xiv
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2. A group of 7 samples, analogous to No. 1, above, associated with
GAG contactor unit "D".
3. A group of 9 samples produced to monitor the reverse osmosis pro-
cessing of DW sampled at Jefferson Parrish (New Orleans) Louisiana.
4. A group of 4 10-liter samples consisting of two reagent water
blanks and two Cincinnati DW samples of which one was processed by
lyophylization.
All of the compound identifications results for the above four sets of
samples are presented and discussed in Volume 3. In addition, the modified
analytical scheme used for these samples is presented in detail and compared
to that used for the large-volume samples (Volume 1).
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ACKNOWLEDGMENTS
Through the course of this three-year research program, many members of
Battelle's technical staff have made significant contributions to the high
quality of the results that were obtained. Denis C.K. Lin deserves special
recognition for his major contribution to the conceptualization and develop-
ment of the analytical scheme, results report format and computerized manage-
ment of the extremely large database. His incorporation of glass capillary GC
columns and a large number of deuterated internal standards were definitely
"state of the art" at that time (1977). Other Battelle scientists and their
contributions to this work include:
Laurence E. Slivon—Design and validation of the computer search and
quantification capability; System/150 to INCOS data transfer; EPA/NIH/NSRDS
library search implementation; high-density 9-track taping of GC-MS data;
numberous utility programs for System/150; mass spectral data interpretation
Bruce A. Petersen—Analytical scheme design, quality control development,
and mass spectral data interpretation
Roderick G. Warren—Implementation of the NUCLEUS data management and
report production systems
Roger L. Foltz and Richard M. Thompson—Mass spectral data interpretation
Susan G. Watson—Confirmation of compound identification and mass spectral
data interpretation
Timothy L. Hayes—GC-MS data processing, 10-liter extraction, data
acquisition
Vanessa R. Goff—GC-MS data acquisition, quality control, and mass spec-
tral data interpretation
Denise A. Contos—Concentrate partitioning, residue weight determinations,
standards preparation, sample analysis tracking, and GC-MS data searching and
quantification
Daniel G. Aichele—NUCLEUS system interaction and operation, report genera-
tion and coordination
Patricia P. Kelley—Report system development and production, NUCLEUS
interaction
Joseph P. Tabor—GC-MS data screening for artifacts
Cynthia A. Schweiger and Bruce E. Urbschat—Assistance with NUCLEUS
operations
The author, as senior team member in the early stages and principal in-
vestigator since 1979, was involved in all of the above cited activities
except the development of System/150 operation programs.
xvi
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SECTION 1
INTRODUCTION
Assessing the health effects of trace (part per billion, ppb) levels of
organic material in water is an important, if not determining, factor in
establishing maximum permissible contamination levels for drinking water (DW)
and finished water from advanced waste treatment (AWT) plants. The issue of
trace level organic chemical contamination of DW will continue to receive
major emphasis in pollution health effect research. However, in the western
states, potable usage or other high quality usage of AWT finished water is
certain to assume a major role. Pilot and production scale AWT plants are al-
ready providing high quality water for use in ground water injection—either
to prevent sea water intrusion into coastal aquifers or simply as aquifer re-
plenishment. In addition, direct potable reuse of AWT finished water is now
in the planning stages for some municipalities for which unlimited supplies of
fresh surfacewater or groundwater are not presently assured. With respect to
potential health effects, detection and control of trace level organic contam-
ination in these AWT reuse waters is obviously important for the ultimate
protection of DW sources.
The Health Effects Research Laboratory of the U.S. EPA in Cincinnati,
Ohio (HERL-CI) is pursuing a research program to characterize the trace level
organic materials in DW and AWT water, and to test the biological activity of
these materials as an indication of their potential health effects. Ongoing
work in the HERL-CI laboratories as well as other research projects contracted
through HERL-CI has been concerned with the biological testing of the organic
concentrates. The goal of Battelle's research effort under EPA Contract
68-03-2548 has been to characterize the organic materials present in sufficient
detail to enable EPA to correlate the compound identification results with the
biological test results. This correlation may suggest which of the organic
compounds, or classes of compounds, have sufficient potential health effect
significance to warrant future regulation and/or monitoring.
In HERL-CI's approach to this research problem, large quantities C1500 to
15,000 liters) of DW and AWT water were concentrated, principally by reverse
osmosis techniques, to yield gram-quantity amounts of concentrated organic
material. The concentrate production work was performed by another contractor
(see Section 4). Eighty percent of each organic concentrate was reserved for
biological testing. Half of the remaining 20 percent was analyzed for organic
compounds by glass capillary gas chromatography-mass spectrometry (GC-MS).
Thus, the sample aliquot analyzed represents between 150 and 1500 liters of
the original water for a theoretical concentration factor of 150,000:1 to
1,500,000:1. This extremely high concentration factor, coupled with fraction-
ation of the sample into five separately analyzed organic polarity groups
-------
(.thereby adding another order of magnitude to the concentration factor), al-
lowed for a more detailed characterization of the portion of organic material
amenable to GC-MS analysis in these clean waters than any previous approach.
Theoretical sensitivities for some identified compounds reached below the 0.1
part per trillion, ppt, level (0.1 nanogram per liter).
The following is a brief description of the analytical scheme employed;
• Fractionation of the concentrate into five different polarity groups
• Glass capillary GC-MS analysis of four of the fractions on two differ-
ent GC phases with all generated data archived on 9-track magnetic tape
• Residue weight analysis of the unpartitioned concentrate and the five
fractions
• Attempted identification based on mass spectra of all chromatographic
peaks and shoulders in the GC-MS data
• Automated searching of GC-MS data files for 53 high-interest compounds
and quantification of those found
• Confirmation of tentative identifications by comparison with GC-MS data
generated from commercially obtained reference compounds
• Entry of compound identification results and other pertinent concen-
trate, information into Battelle's mainframe computer for automated
data management and generation of tabular listings of results
• Concentrate analysis report generation.
-------
SECTION 2
CONCLUSIONS
The results of this research program have shown fractionation of complex
organic concentrates followed by glass capillary. GC-MS analysis enables the
identification of hundreds of organic compounds present in these samples.
Moreover, the use of concentration techniques in which thousands of liters of
water are used to produce the analyzed sample together with computerized GC-MS
data searching have enabled theoretical sensitivities toward individual pol-
lutant species which, extend well below the part per trillion (nanogram per
liter) level. Thus, results of this research have produced chemical charac-
terizations of very clean drinking waters and advanced waste treatment fin-
ished waters in greater detail than previously possible.
The results for drinking water (W) provide the following conclusions:
• Most of the organic material in the analyzed concentrates
consisted of humic-related substances which are not amenable
to GC-MS analysis. On the average, more than 90 percent of
the organic material present in the concentrates was not
recovered through the fractionation scheme. Part of the
recovered material is not suitanle for characterization by
GC-MS analysis, and it is estimated that only 30 to 60
percent of the material recovered into fractions (i.e.,
3 to 6 percent of the original concentrates) can be
characterized by GC-MS analysis.
• All of the DW sampled (except one case which served as a
blank) contained many identified organic compounds,
generally between 150 and 4QQ different species.
• The species identified at the highest levels and greatest
numbers were non-aromatic and aromatic carboxylic acids.
• All DW concentrates contained some evidence of the
presence of re-use water via the identification of drug
metabolites and other materials expected to originate from
domestic sewage. The level of re-use water ranged from very
slight for Seattle to a significantly high level for Miami.
• All DW concentrates showed some evidence for contamination
by organic compounds from industrial discharges (organic
solvents and chemical industry commodities, intermediates
and wastes), and consumer use of organic chemical-containing
products including herbicides and pesticides. Concentrates
3
-------
from Cincinnati, Philadelphia and New Orleans contained
the highest levels of these substances.
• All DW concentrates contained halogenated species which
probably originated from the chlorination of naturally
occurring organic material in the source water. This
result was the most pronounced for the Seattle and
Miami concentrates.
• A tentative conclusion that the reverse osmosis membranes
used for pre-concentration did not effectively retain
Cor, perhaps, absorbed) highly apolar species was based
on'a comparison of the RO-produced concentrates from a
Cincinnati sampling with the concentrate produced by direct
XAD-2 adsorption/elution prepared from the same volume of
identical water. Based on the limited evidence, RO was
more effective for recovering highly polar, water soluble
materials, especially humic material.
The central conclusion to be made concerning the AWT concentrate analysis
results was that the use of contact with granular activated carbon (GAC) in
these plants was obviously effective in reducing the amount of organic mate-
rial recoverable in the final concentrate,. Almost without exception, the AWT
concentrates contained less organic material in the analyzed fractions and
resulted in fewer identified compounds and lower detected levels than the DW
concentrates. For some of the AWT concentrates, these comparative differences
were substantial. However, the sampled finished AWT water contained higher
total organic carbon (TOG) levels than the sampled finished DW and, therefore,
the conclusion is that the finished AWT water contained higher levels of
material not recoverable by RO and/or not suitable for GC-MS analysis than
did the finished DW. Assuming that the AWT influent contained organic mate-
rial suitable for GC-MS analysis at levels at least as high as those for the
finished DW', one must conclude that the GAC contact step in the AWT process
was effective in reducing the levels of GC-MS analyzable organic substances
to below those for the sampled DW. Compared to the DW concentrates, the AWT
concentrates contained higher levels of fatty and other acids, phthalates,
and poly glycol ethers (relatively polar species) but generally lower levels
of apolar species attributable to the use or production of industrial organic
chemicals. This observation supports the conclusion, above, concerning the
effectiveness of GAC contact stages in the AWT plants. Higher efficiency for
removing the apolar species (which, are more suitable for GC-MS analysis) than
the polar, more highly water soluble species is consistent with chemical
expectations. One AWT plant (Escondido, California) employed RO rather than
GAC contactor treatment. Since the Escondido concentrate contained less
organic material and fewer species identifiable by GC-MS, the tentative con-
clusion is that RO is highly effective for final treatment for AWT systems.
However, insufficient data are available to compare RO effectiveness to GAC
treatment.
-------
SECTION 3
RECOMMENDATIONS
Future work in attempting to correlate potential health effects of
organic contamination in DW and AWT water with the nature of the organic
materials present should employ biological testing of individual chemical
group fractions of the organic concentrates rather than bulk concentrates.
Such a strategy coul.d greatly reduce the amount of chemical analysis required.
Results from the DW concentrates indicated that more than 80 percent of the
organic material present was humlc material which was not suitable for
characterization by GC-MS yet these materials may be responsible for a sig-
nificant amount of biological activity. Standard methods are available for
isolating the humlc materials in concentrates. Separate biological testing
of a humic/fulvic acid fraction as well as the fractions isolated for GC-MS
analysis would greatly simplify the task of attempting to correlate the
organic compounds present in the concentrate with the biological testing
results. For example, the polar neutral fraction always contained a plethora
of alcohols, ketones, diester plasticizers and mixed functionality species
many of which are difficult to identify by GC-MS analysis. Certainly, many
of these compounds are biologically inactive, and if this polar fraction
consistently failed to show biological activity, GC-MS analysis could be
omitted. The opposite case may be true for the aromatic fraction which
represented only 0.05 to 1.0 percent of organic material in the concentrate.
Comparison of analysis results for concentrates prepared from identical
DW samples by the RO-based method and by the direct XAD-2 adsorption/elution
method suggested that much and possibly most of the apolar anthropogenic
species present in the sampled water were not recovered by RO. These anthro-
pogenic species are of the highest interest group for potential health effect
investigation. On the other hand, direct. XAD-2 adsorption/elution did not
recover ionized, highly polar and macromolecular species such as humic/fulvic
acids and poly glycols as well as the method employing RO pre-concentration.
Development of a combination of these two methods could provide a concentrate
more representative of the organic material present in the original water so
that more reliable health, effect conclusions could be made.
The compound identification results represented in this work constitute
the most detailed chemical characterization of a wide variety of clean waters
such as DW and finished AWT water from various sources. However, the results
also show that only a small fraction of the organic material recovered into
the concentrate is suitable for characterization by GC-MS methods. Detailed
characterization of the major part of the organic material which was not suit-
able for direct GC-MS analysis should be performed to complete this work.
-------
While these incomplete aspects have high importance for the health effects
evaluation goal, their intrinsic scientific value alone justifies a
continuation of the present work.
In future analytical work of this type, some minor modifications to the
analytical scheme requiring further method development work can provide
a more cost effective analysis:
• The use of polar capillary GC columns that are
capable of higher temperature limits could eliminate
the necessity for analyzing the high polarity, medium
polarity and acid fractions on the apolar phase
• GC-MS analysis of the aromatic fraction should be
restricted to th.e apolar GC column
• Based on the compound identification results of this study.
additional compounds could be selected for computerized
data searching. These compounds could be selected to
profile different characteristics of source waters.
-------
SECTION 4
BACKGROUND INFORMATION ON THE ORGANIC CONCENTRATES
CONCENTRATE PRODUCTION METHODS
Although none of the organic concentrates were produced by Battelle under
the subject contract, some discussion of the concentrate production methodo-
logy is necessary to provide context to the discussions that follow.
All but four of the 36 DW and AWT concentrates were produced by Gulf
South Research Institute (GSRI) under contracts 68-02-2090 (AWT) and
68-03-2367 (DW). The remaining four concentrates were produced in the EPA
HERL-CI laboratory. Two of these four concentrates were produced by reverse
osmosis (RO) procedures corresponding to those used by GSRI. The remaining
concentrates (of which one was a process blank) were produced by direct XAD-2
adsorption with diethyl ether elution. In producing these concentrates at
HERL-CI, half of a split stream was used to fill the reservoirs for RO pro-
cessing while the other half was acidified to pH 2 in the flowing stream and
passed directly over a column of XAD-2 resin. Elution of the XAD-2 resin with
diethyl ether and subsequent concentration yielded the Cincinnati I XAD/DIRECT
concentrate, code T1Y (the XAD-2 process blank was coded T2B), and RO process-
ing of the other half of the sample provided the other two concentrates (coded
TIC and T1X) by a procedure adapted from that used by GSRI, below (see
Appendix E). Tables 1 and 2 list the DW and AWT samples, respectively, and
also details concerning the sampling, source water and treatment plant.
The RO concentrate production methodology has been reported previously
(1,2) and is only briefly summarized here. A schematic diagram of the RO pro-
cessing unit is shown in Figure 1 (2). Sample water was processed batchwise
at pH 5.5 through- a cellulose acetate membrane. The permeate water was pro-
cessed after pH adjustment to 10.0 through a second RO unit equipped with a
DuPont Permasep® nylon fiber cartridge. The separate RO brines were recycled
(with all cellulose acetate permeate being used as Permasep® feed) until the
brine volumes were reduced to about 38 liters, or until salt precipitation be-
came a problem. The two RO brines were sequentially extracted with pentane
and methylene chloride. After acidification the extraction with methylene
choride was repeated. Thus, after solvent evaporation, six separate organic
extracts were obtained. For some samples, including all of the DW samples, the
six solvent extracts were combined and analyzed as a composite concentrate.
For some of the AWT samples, one or more of the six individual solvent extracts
was selected for analysis individually (see Table 2).
The extraction of organic compounds from the RO brine was carried one step
7
-------
CO
TABLE 1. SOURCE WATER, SAMPLING AND CONCENTRATE PRODUCTION INFORMATION FOR DRINKING WATER
CONCENTPJ^TES
City
Cincinnati, OH
Cincinnati, OH
Miami, FL
New Orleans, LA
Date
Sampled
10-17-78
01-14-80
02-03-76
01-14-76
Volume
Sampled
(liters)
1,460
7,110
2,270
6,620
Water Source (description; sampling location)
Ohio River (containing contributions from industrial,
chemical, agricultural a,nd treated and untreated
sewage; tap water, EPA Laboratories at 26 W.
St. Clair Street)
Ohio River (as above; Kellogg Ave. Treatment Plant)
Shallow Well (swamp-fed aquifers vulnerable to waste-
disposal contamination; Preston Water Works)
Mississippi River (as above, for Ohio River, but more
predominantly agricultural run-off; tap water, GSRI
TOCa
(mK/1)
not
determined
1.9
6.4 + 1
1.7 + 1
Name
TIC
T1X
T1Y
T4C
T4X
M2C
M2X
N2C
N2X
Concentrates Analyzed
Method of Production
,d
Solvent Extract
XAD-2 Extract
Direct XAD-2 Extraction/
diethyl ether elution
(no RO processing)
Solvent Extract
XAD-2 Extract
Solvent Extract
XAD-2 Extract
Solvent Extract
XAD-2 Extract
Laboratories)
Ottumwa, IA 09-10-76 5,450 Des Moines River (predominantly agricultural run-off;
Ottumwa Water Works)
2.4 + 1
02C Solvent Extract
02X XAD-2 Extract
Philadelphia, PA 02-10-76
Poplarville, MS 03-02-79
Seattle, WA 11-05-76
5,810 Delaware River (as above, for Ohio River, but more 1.7 + 1
predominantly vulnerable to chemical and industrial
pollution; Torresdale Water Works)
15,100 Deep Well (virtually organic-free; Poplarville Water
Works)
11.750 Pristine Mountain Stream (essentially free of all 1.0 + 1
organic pollutants except those from natural sources;
Distribution System at 2700 Airport Way(Cedar River))
P2C
P2X
VIC
V1X
S2C
S2X
Solvent Extract
XAD-^2 Extract
Solvent Extract
XAD-2 Extract
Solvent Extract
XAD-2 Extract
a) determined by GSRI under EPA Contract 68-03-2367
b) the three digit code is used in the computer-printed tabulations
c) concentrates TIC, T1X and T1Y were produced by HERL-CI. The other concentrates were produced by
GSRI under Contract 68-03-2367.
d) "Solvent extract" denotes a combination of the six solvent extracts of the cellulose acetate and
nylon membrane RO brines produced from the sampled water. "XAD-2 extract" denotes a subsequent
extraction of these two RO brines using XAD-2 resin with ethanol elution.
-------
TABLE 2. SOURCE WATER, SAMPLING AND CONCENTRATE PRODUCTION INFORMATION FOR ADVANCED WASTE
TREATMENT CONCENTRATES
""'
Treatment Plant
Date
Sampled
Influent
Characteristics3 Water Treatment Sequence3
Finished Water
Character! sties3
Disolved
TOCb Solids
(nig/1) (rag/1)
Concentrates Analyzed
Method of
Product ion
Code (RO Brine
Naroec Ext rac t ion ) J . «=
Blue Plains 09-19-74
Washington,D.C.
Blue Plains 05-29-75
Washington, D.C.
Dallas, TX 12-10-74
Eacondido, CA 07-08-75
Lake Tahoe, CA 10-24-74
Orange County.CA 01-27-76
Orange County.CA 02-03-76
Pomona. CA 09-25-74
essentially 100% municipal
(domestic, weak strength;
little industrial waste)
(as above)
88% municipal by volume;
35% BOD, industrial and com-
mercial; medium strength
861 domestic, 14% Industrial
(large electronics industry
component)
essentially 100% domestic of
relatively low strength
30% industrial (predomi-
nantly pretreated metal
plating and refining)
(as above)
90% municipal by volume;
diverse industrial sources
including some paper pro-
duct waste
Pomona, CA 10-02-74 'as above)
Pomona, CA 06-17-75 (as above)
low lime clarification; breakpoint chlorlnation 11.3 544
and neutralization (In parallel); CAC adsorption;
dual media filtration
low lime clarification; activated sludge nitrlfl- 2 n
-------
ar— 1| 1
eve? P^
Con trnl Control
i r
Sump Fill T
I uiup 1<-*VJ |
Control
Valve
-il-U
Cellulose Acetate
Unit Process
Drum
208 liters capacity
(55 gallons)
\Auto
Level
Control
PH
Control
/ Base\
t
Back
Pressure i
Valve
r-A
Module
1
rr~
1
t
;
r
Flow
Meter
( r
< i
• r
1
Nylon
Unit
Process
Drum
r-j
i
208 liters capacity
k (55 gallons)
L
>-
"*
Back
r
Pressure f
Valve
Nylon
Module
rr
i
\
— >To
Sewer
^
•
Higli Pressure
Pump
High Pressure
Pump
Figure 1. Schematic diagram of the reverse osmosis concentrator used by GSRI.
(Taken from EPA publication 600/2-78-016, February, 1978; available through NTIS)
-------
further for the DW concentrates. Following solvent extraction, the reverse
osmosis brine was extracted with XAD-2 resin followed by ethanol elution to
obtain an additional amount of organic material which was generally greater
(on a residue weight basis) than that obtained from solvent extraction. Un-
fortunately, three of these XAD-2 concentrates were seriously contaminated with
artifacts generally described as XAD "resin bleed", and the analysis results of
these concentrates are less useful than those for the others. The XAD-2 arti-
fact problem is addressed in Section 6, Results and Discussion of this report.
THE RO METHOD BLANK
The RO methodology for producing organic concentrates from large volumes
of relatively clean water was an emerging technology when the concentrates
were produced. Progress has been made since then to improve recovery and re-
duce artifact generation, and HERL-CI is currently sponsoring a program to
characterize the performance of various organic concentration techniques from
large volumes of clean water under carefully controlled conditions. As might
be expected, obtaining an ideal RO process blank is very difficult. Previous
attempts have shown that RO processing of very large volumes of high quality
reagent water produced a concentrate that contained numerous compounds (J.).
Moreover, the use of reagent water is inappropriate since the lack of dis-
solved salts might be expected to modify the contribution of the RO apparatus
to the blank. For this reason, the Poplarville, Mississippi, concentrate Csee
Table 11 was used as a blank. The Poplarville water originates from deep wells
tapping an aquifer which is extraordinarily organic-free yet contains dissolved
salts at normal levels. Over 15,000 liters of this water were used to prepare
the Poplarville blank concentrate. This volume is greater than the AWT volumes
by a factor of 10 and greater than the DW volumes by a factor of 1.4 to 10 Csee
Tables 1 and 2). In addition, the Poplarville concentrate represents true
field sampling experimental conditions. Of more concern than the authenticity
of the blank is the lack of knowledge of the efficiency of RO membrane reten-
tion of relatively small organic molecules under conditions of extremely low
concentration and high volumes of processed water. This issue is addressed in
Section 6, Results and Discussion.
In addition to the two Poplarville, Mississippi, RO process blank, samples,
three other blank concentrates were analyzed. The first blank corresponds to
evaporated pentane and methylene chloride as a control for organic materials
present in solvents used to extract the RO brine. This concentrate is desig-
nated by the code, X1C, in the tables of combined concentrate results (Tables
9 through 15). The second blank, designated XIX in the computer-printed tables,
was generated from ethanol elution of XAD-2 resin. The third blank sample
designated by the code, T2B,was also a solvent elution of XAD-2 resin, but in
this case the solvent was diethyl ether. This blank sample was actually a
process blank for one of the three concentrates produced by HERL-CI.
THE WATER USED FOR CONCENTRATE PRODUCTION
With the exception of the three concentrates produced by HERL-CI and the
New Orleans sampling, all of the DW sampling was performed at municipal DW
plants. The three HERL-CI produced concentrates and two New Orleans concen-
trates were generated from DW taken from the tap at the HERL-CI and GSRI
11
-------
laboratories, respectively. Some of the relevant information for the DW sites
is given in Table 1. Similar information concerning the AWT concentrates pro-
duced by GSRI is given in Table 2.
The cities sampled for DW concentrates were chosen by EPA to provide a
typical range in types of raw water and methods of treatment. Results of the
analysis of volatile organics from DW sampled from these cities has previously
been reported (3). Details concerning the DW" treatment plants and the stand-
ard water quality parameters (TOG, pR, hardness) at the time of sampling are
available from U.S. EPA/HERL in Cincinnati. Note that none of the DW concen-
trates were prepared from finished water treated by contact with activated
carbon. In contrast, all but one of the AWT plants (Table 2) incorporated
activated carbon contact as either the last step in the treatment scheme or the
step preceding final chlorination. Detailed descriptions of each of the AWT
plants sampled and pre-treatment and post-treatment data on suspended solids,
BOD, COD, TOG, ammonia, pH, hardness, inorganic anions, and other standard
water quality parameters have been reported previously (2).
12
-------
SECTION 5
ANALYTICAL SCHEME
RATIONALE FOR THE ANALYTICAL SCHEME
The analytical scheme described below was developed during the first year
of the contract through the joint efforts of Battelle researchers and the EPA
Project Officer.
The concentrate samples processed through the analytical scheme were ex-
tremely complex organic mixtures in about 1 to 2 ml of solvent. To illus-
trate this complexity, a partial chromatogram from glass capillary GC
analysis of the unpartitioned Pomona II acidified methylene chloride concen-
trate is shown in Figure 2. A 30 meter (0.26 mm I.D.) SP2100 coated glass
capillary column with relatively high efficiency was used to produce this
chromatogram. The column used had a separation number of 36 between the Ci3
and GI« hydrocarbons of the test mixture. In the partial chromatogram of
Figure 2, over 200 resolved and partially resolved GC peaks were obtained
between 60°C and 150°C. The baseline rise between 130°C and 210°C is
due to mixture component co-elution rather than detector drift. Identification
of a significant number of the multitude of species in Figure 2 would be diffi-
cult even with glass capillary GC-MS. The analytical scheme shown in Figure 3
was specifically designed to enable the identification of a maximum number of
the organic species present in these complex organic mixtures.
The analytical scheme includes addition of deuterated internal standards
to the concentrate, fractionation of the concentrate through a combination of
extraction under both acidic and basic conditions, partitioning of neutral
compounds on a short silica gel column, and, analysis of the partitioned frac-
tions as well as the unpartitioned concentrate by glass capillary GC-MS.
Analysis of the unpartitioned concentrate was omitted for the DW concentrates
produced by XAD-2 extraction of RO brine. The GC-MS analyses were conducted on
two types of wall-coated open-tubular glass capillary GC columns, one contain-
ing a non-polar liquid phase SP2100) and the other a polar liquid phase
(SP1000).
Process blank samples were produced simultaneously during concentrate
partitioning. Also, the performance of each analytical instrument was moni-
tored daily to ensure the reliability of the analytical data.
Each aspect of the analytical scheme is described in detail in the sec-
tions that follow. Quality control features are described in the context of
this section and are not presented separately.
13
-------
nn
50
SP2100 (30 M, 0.26 I.D.)
SPLITLESS INJECTION
HEPTANE FOR SOLVENT EFFECT
2 pi SAMPLE (CH2C!2)
50° (6') -> 280°. 2°/MIN
INJECTION TEMPERATURE 280°
GC-FID OF A TYPICAL CONCENTRATE SAMPLE (CZN)
70
90
no
Temperature
130
ISO
170
190
_J
210
_!
16
26
36
46
Time in Minutes
56
66
76
66
Figure 2. Partial gas chromatogram (FID) of a typical unpartitioned water concentrate sample.
-------
ADD DEUTERATED
INTERNAL STANDARDS
PARTITION INTO
FIVE FRACTIONS
RESIDUE WEIGHT
ANALYSIS
GC-MS ANALYSIS
UNPARTITIONED CONCENTRATE
AND FRACTIONS ON
SP1000 AND SP2100
SEARCH AND
QUANTIFICATION
OF SPECIFIC
COMPOUNDS
COMPOUND IDENTIFICATION
BASED ON MASS SPECTRA
CONFIRMATION OF COMPOUND
IDENTIFICATIONS
DATA ENTRY INTO
MAINFRAME COMPUTER
REPORT GENERATION
Figure 3. Analytical scheme for the analysis of water concentrates
15
-------
INTERNAL STANDARDS
Thirteen deuterium-labeled compounds (Table 3) were added to the concen-
'trate before partitioning to serve as internal standards. In addition,
hexaethylbenzene was added to each fraction prior to analysis by GC-MS.
These internal standards served three purposes:
1. Monitoring fractionation recoveries. The deuterium-labeled
internal standards were selected so that at least one compound
was partitioned into each fraction (Table 3). Recoveries of
internal standards in the various fractions could be deter-
mined from the GC-MS data with any significant departure from
the normal recoveries indicating abnormal performance of the
partitioning scheme.
2. Calculation of relative retention values. A relative retention
value was calculated for each GC peak by dividing the absolute
retention time by that of the internal standard, hexaethylbenzene.
Relative retention values were required for confirmation of ten-
tative identifications of compounds based on mass spectra.
3. Quantification. The amounts of specific search compounds found
in the unpartitioned concentrate and the partitioned fractions
were calculated from GC peak areas in the extracted ion current
profile (EICP) chromatogram relative to those of appropriate
deuterated internal standards. In addition, comparison of the
size of the hexaethylbenzene GC peak to those of the identified
components was used to provide a less accurate but more easily
accomplished quantitative estimation for every identified
component.
PARTITIONING OF THE CONCENTRATES
The partitioning scheme was designed to separate the complex concentrates
into acidic, basic, and neutral compounds by aqueous/organic liquid-liquid
partitioning. The neutral compounds were further partitioned with silica gel
chromatography. The scheme is a modification of the procedure reported by
Ishiwatari and Hanya (4) . Not only does the scheme separate the concentrate
.into fractions more suitable for GC-MS analysis, it also isolates the organic
acids and phenols into a fraction which, can be conveniently converted into
methyl esters or ethers by treatment with diazomethane. The methylated acids
and phenols exhibit better chromatographic properties than the corresponding
free acid compounds.
A schematic representation of the originally developed partitioning pro-
cedure for concentrates produced by solvent extraction of RO brine is shown
in Figure 4. A modified procedure for partitioning the concentrates produced
by XAD-2 resin extraction of the DW RO brines is shown in Figure 5. Modifi-
cation of the original scheme was necessary for these samples because of the
extremely high level of acidic material (apparently humic substances) which
made the original extraction of the bases with small volumes of 5% H2SO<, (as
16
-------
TABLE 3. DEUTERIUM-LABELED COMPOUNDS USED AS INTERNAL STANDARDS
Compound
Fractions in Which
Compound is Recovered a
Pyridine-D-
Aniline-D
Benzoic acid-D
Phenol-D5
Eicosane-D,„
42
Bromobenzene-D
1,4-Dibromobenzene-D
Naphthalene-D
8
Chrysene-D
Perylene-D12
Nitrobenzene-D
Nitronaphthalene-D_
Dimethylterephthalate-D
12
Combined
Combined
Derivatized Acids
Derivatized Acids
Aliphatic Hydrocarbons c
Aromatic
Aromatic
Aromatic
Aromatic
Aromatic
Aromatic and Combined"
Aromatic and Combined^
High Polarity
a) See Figures 4 and 5 for production details of the analyzed fractions.
b) Extracted bases combined with medium polarity neutrals.
c) This fraction is not analyzed by GC-MS.
17
-------
CONCENTRATE DILUTED
TO S ml WITH CH2CI2
5% HjSO* 1 ml x 3
CH2CI2
SOLUTION
5% NaOH. 1 ml x 4
3 ml Na2SO4 (SAT.)
40%KOHtopH12-13
CH2CI2.1 ml K 3
WASH WITH 2 ml
DISTILLED WATER
NEUTRALS IN
CH2CI2
SOLUTION
STRONG AND WEAK
ACIDS AND PHENOLS
IN AQUEOUS SOLUTION
00
CH2CI2 ELUTION
FRACTION COMBINED
WITH BASE FRACTION
DRY WITH Na2SO4 ANHYDROUS
EVAP. TO 100/Jl
ADD HEXANE TO 500 |
-------
CONCENTRATE ADDED
TO 76 ml of 5% NaOH
CH2CI2. IS ml x 3
STRONG AND WEAK
ACIDS AND PHENOLS
IN AQUEOUS SOLUTION
K.D. EVAP. CH2CI2 EXTRACT
TRANSFER TO 13 ml TUBE
5.0 ml FINAL VOLUME
7 gm Na2S04. ANHYDROUS
6 M H2SO4. until pH 1
CH2CI2, IS ml x 3 or 4
ACIDS AND PHENOLS
IN
CH2CI2 SOLUTION
5% H2SO4, 1 ml x 3
WASH WITH 2 ml
DISTILLED WATER
K.D. EVAPORATE TO 0.6 ml
TRANSFER TO MICRO TUBE
EVAPORATE TO 50 u\
ADO HEXANE TO 500 pi
EVAPORATE TO SO pi
ADD 450 pi EI2O and 50 pi CH3OH
DIAZOMETHANE
DERIVATIZATION
EVAP. TO 100pi
ADD 2 pg INT. STD. (HEBI
ADD 100 pi CH2CI2
BASES IN
AQUEOUS
SOLUTION
DRV WITH Na2SO4 ANHYDROUS
EVAP. TO 100 pi
ADD HEXANE TO 500 pi
EVAP. TO 100 pi
ADD HEXANE TO 1.0 ml
SILICA GEL COLUMN
(STEP GRADIENT ELUTION)
2.75 ml HEXANE
4mlHEXANE/BENZENE 11:1)
4 ml CH2CI2
4 ml
QC-MS ANALYSIS
DERIV. ACIDS
3 ml Na2SO4 (SAT.)
40%KOHlopH 12-13
CH2CI2. 1 ml x 3
CH2CI2 ELUTION
FRACTION COMBINED
WITH BASE FRACTION
EVAP. TO 200 pi
ADD 2 pg INT. STD. (HEB)
GC-MS ANALYSIS
AROMATIC: HEX/BENZ
HIGH POLARITY: CH3OH
MEDIUM POLARITY
4
BASES
Figure 5. Partitioning scheme for water concentrates derived from XAD-2 extraction of
reverse osmosis concentrates.
-------
in Figure 4) impossible. These two partitioning schemes yield fractions
which are essentially equivalent.
In partitioning the solvent extract concentrates (Figure 4), the bases
were first extracted from the concentrate'with 5% H2S04. After adjusting the
solution to pH 12-13, the bases were back-extracted into methylene chloride.
'The volume of the methylene chloride solution of the bases was then
reduced to about 500 yl. Since this fraction containing extracted bases was
usually not very complex, it was combined with another fraction from the
silica gel chromatography of the neutrals, the methylene chloride fraction,
which also was generally less complex than other analyzed fractions. This
combined fraction was reduced to about 200 yl and 2.0 yg of the internal
standard, hexaethylbenzene (HEB), was added. Analysis of these two fractions
as a combined fraction resulted in a significant savings in time with vir-
tually no loss of compound identification capability.
The acidic and phenolic compounds were extracted from the methylene chlo-
ride solution with 5% NaOH. In the case of XAD-type drinking water concen-
trates (Figure 5), the partitioning of the acids into 5% NaOH preceded the
base extraction step above, and was done on a much larger scale to accommo-
date the relatively high concentration of extractable acidic material. The
remaining base/neutral fraction was" reduced in volume to allow proceeding on a
scale similar to that of Figure 4. The extracted acids were back-extracted
with methylene chloride after acidification to pH 1 to 2 and addition of
Na2SOi,. Prior to derivatization with diazomethane, the methylene chloride
solvent was removed by solvent exchange to hexane. Without the solvent ex-
change, the diazomethane was found to react with the methylene chloride to
generate a homologous series of chlorinated hydrocarbons which unacceptably
complicated identification of the methylated acids and phenols.
The neutral compounds remaining after removal of the acids and bases were
further partitioned into four fractions using a modification of an accepted
pesticide micro-column separation procedure (5,6) employing open-column
chromatography on 5% deactivated silica gel (Woelm type 02747, 70-150 mesh).
Three identical silica gel columns (MD.55 x 7 cm in a 6-inch disposable
Pasteur pipette with, a glass wool plug in the bottom and 6 to 8 mm of anhydrous
granular Na2SO<. at the top) were prepared in a paralled fashion. Two columns
were used for preparation of the sample and process blank fractions. The
third column was used only to check the accuracy of the silica gel deactiva-
tion which was indicated by the volume of hexane required to elute anthracene
from the column. The anthracene elution volume was monitored visually by a
UV lamp of long wavelength (366 nm). One hundred micrograms of anthracene in
30 jjl of hexane was applied to the column. Using hexane as the elution sol-
vent, correct deactivation of the silica gel (5% water, by weight) was indi-
cated by anthracene elution beginning after 7 +0.5 ml of hexane had passed
through the column. For 7% and 3% deactivation the volume of hexane used to
eluate anthracene was found to be 11 +0.5 and 5.5 +0.5 ml, respectively.
Four elution solvents were used to partition the neutral compounds on
silica gel (Figures 4 and 5) - These solvents were applied to the column in the
following sequence: 2.75 ml of hexane, 4 ml of hexane/benzene (1:1), 4 ml of
20
-------
methylene chloride, and 4 ml of methanol. After elution, the first 2.75 ml
of hexane contained mostly alkanes and alkenes and only a small proportion of
other compounds of interest, such as hexachlorobenzene. Since alkanes and
alkenes are not considered potentially hazardous chemicals, this aliphatic
hydrocarbon fraction was not analyzed except for the determination of its
residue weight.
All of the volume reductions except for one Kuderna-Danish (K-D) distil-
lation shown in Figure 5 were performed using an N-EVAP® Analytical Concentra-
tor, Model 111 (Organomation Associates, Northborough, Main). Sample volumes
were reduced'in 4.0 ml capacity Chromaflex® tubes (Kontes, Vineland, New Jersey)
which were tightly capped with aluminum foil. Ultra-pure nitrogen (99.999%,
Matheson) was introduced to the tube with a blunt 18 guage needle inserted to
just below the foil cap. The Na flow was controlled at 1.5 to 2.5 ml/min while
the bottom of the tube was immersed in a water bath maintained at the boiling
point (+ 3°C) of the primary solvent consitituent of the sample. Under these
conditions, very gentle, nearly unobservable solvent refluxing was maintained
in the upper part of the tube during solvent evaporation. These very mild
conditions allowed reduction of a 3.5 ml sample to about 200 yl in 6 to 14
hours, depending on the vapor pressures, heats of vaporization and boiling
points of the solvent constituents. This sample evaporation was used at the
direction of the Project Officer with very little modification or attempts at
further recovery optimization. It should be noted that this extremely slow
solvent evaporation does not correspond to the usually encountered procedure of
solvent blow-down under N2.
RESIDUE WEIGHT ANALYSIS
In order to determine the quantities or organic material partitioned into
the fractions, an aliquot of each fraction and process blank was evaporated
to constant weight on a 12 mm square of aluminum foil, and the residues were
accurately weighed to the nearest 2 yg on a Mettler ME30 microbalance. Re-
sidue weights were also determined for the unpartitioned concentrates. A
sufficient volume of sample was evaporated to result in a minimum of about
20 yg of residue although no more than one half of a given sample was con-
sumed for this purpose. Generally, only the process blank aliquots eva-
porated to net weights of less than 20 yg.
GAS CHROMATOGRAPHIC ANALYSIS
The partitioned fractions were very complex and required the use of
high resolution gas chromatography to resolve the individual components.
Wall-coated open-tubular glass capillary GC columns were used for these anal-
yses with two different liquid phases: SP1000 (polar) and SP2100 (non-
polar) . These two types of coatings effectively complemented each other so
that compounds which co-eluted on one column were usually well-separated on
the other column. Also, high boiling or high polarity compounds which did not
elute from the polar column could be observed on the non-polar column. The
columns used in the initial stages were purchased from the J & W Scientific
Company. For the final year of GC-MS analysis activity, columns of both
polarities were made at Battelle.
21
-------
Before a capillary GC column was accepted for analytical use, it had to
meet the following minimum performance requirements:
• For SP2100 columns (30 M, 0.25 mm I.D.) operated at 100°C with
a helium carrier velocity of 23 cm/sec:
(1) Neff= 80,000 (Ci<,)> minimum
(2) SN = 35 (Cl3-CiJ, minimum
(3) Decylaldehyde, no tailing
(4) Decanol tailing: peak base =4.00 times the peak
base of Ci3, miximum
(5) Acid/base ratio: 2,6-dimethylphenol:2,4-dimethylaniline
ratio of 0.5 to 2.0, peak height basis
(6) Sample capacity: 50 ng of CK., no fronting
• For SP1000 columns (40 M, 0.25 mm I.D.) operated at 125°C with
a helium carrier flow velocity of 23 cm/sec:
(1) Neff= 100,000 (C18). minimum
(2) SN = 25 (C17-Cia), minimum
(3) Decylaldehyde, no tailing
(4) Decanol, no tailing
(5) Acid/base ratio: 0.5 to 2.0, as above
(.6) Sample capacity, 50 ng of Ci8j no fronting
Examples of GC-FID chromatograms resulting from analysis of the GC test mix-
ture on acceptable SP2100 and SP1000 glass capillary columns are shown in
Figures 6 and 7, respectively.
In initial stages of the work, all partitioned fractions and corre-
sponding blank samples as well as unpartitioned concentrates, were analyzed
by GC-FID on both capillary column phases prior to analysis by GC-MS. This
preliminary analysis provided both a screening function to assess the sensi-
tivity that would be required for GC-MS analysis, and also a quality control
measure to ensure that GC-MS chromatography was performing optimally and that
there were not significant amounts of late-eluting material. As experience
was gained with the samples and GC-MS performance aspects, this preliminary
screening was no longer required and, thus, was performed only as necessary.
The following chromatographic analysis conditions were used for both the GC-
FID screening analyses and the GC-MS analyses:
22
-------
2,6-Dimethylphenol
Inj
Figure 6.
2,4-Dimethyloniline
Oeconol
Decytalde-
hyde
SP2IOO (30M)
Neff = 91000 (C)4)
SN = 36(C|3-C|4)
Sample Size = I /j.L
Flow Vel = 20 cm/sec
Inj T • 275
Oven T = 100 iso
FID Sens = 32x1
Split = 20:1
'14
Typical column evaluation chromatogram for a 30M
SP2100 (apolar) capillary column.
Inj.
L
Figure 7,
Methylnonyl ketone
'17
Decylaldehyde
SPIOOO (40 M)
Neff = 110,000 (C,7)
SN=34(C|7-C,8)
Sample Size: .5/i i.
Flow Vel = 23 cm/sec
Inj T=275°
Oven T =125° iso
FID Sens = 8x I
Split =20 = 1
Decanol
2,6-Dimethylphenol
2,4-Dimethylaniline
Typical column evaluation chromatogram for a 40M SPIOOO (polar)
capillary column.
23
-------
GC-FID Operating Conditions
Instrument: Carlo Erba Model 2150
Injector temperature
Initial column temperature (hold)
Program rate
Upper temperature limit
Injection volume (splitless)
Detector temperature
Helium flow velocity
SP1000 (40 M,
0.25 mm I.D.)
250°
50°(6 min)
SP2100 (30 M,
0.25 mm I.D.)
275°
RT C3 min)
50 "(3 min)
2° /min
280°
2°/min
225°
2 yl sample plus 2 yl sample
1 pi heptane
250°
23 to 25 cm/sec
at 125°C
275°
23 to 25 cm/sec
at 100°C
GLASS CAPILLARY GC-MS ANALYSIS
Mass Spectrometer Performance Quality Assurance
GC-MS analysis of the partitioned fractions and the unpartitioned concen-
trates, as well as corresponding blank samples, provided the primary basis
for identification and quantification of organic compounds in the concen-
trates. In order to ensure that all GC-MS data acquired were of high quality,
the total GC-MS system performance was rigorously evaluated each day before
undertaking analysis of concentrate samples. The GC-MS performance evalua-
tion included the following operations:
(1) A check of the mass calibration by acquiring a spectrum of
perfluorotributylamine (FC-43) using signal sampling at 0.1 amu
intervals.
(2) An evaluation of the mass spectrometer resolution and mass
discrimination by analysis of decafluorotriphenylphosphine
(DFTPP) according to the recommendations of Eichelberger,
Harris, and Budde (7).
C3) GC-MS analysis of a test mixture referred to as the Standard GC
Separation Mixture (SGCSM). This mixture was designed to evalu-
ate the following performance characteristics:
• Proper MS sensitivity, resolution, and high-mass/low-mass
ion sensitivity ratio
• Proper functioning of the splitless injection system
24
-------
• Adequate capillary GC column efficiency
• Suitable capillary GC column neutrality (neither acidic
nor basic), and activity toward polar materials
• Absence of adsorptive sites or cold spots in the GC
column and transfer line.
Typical GC-MS reconstructed gas chromatograms of the SGCSM test mixtures
for the SP2100 and SP1000 columns are shown in Figures 8 and 9, respectively.
The components of each mixture are labeled on the chromatogram. The mass
spectrometer operating conditions and data acquisition parameters used for
this test are identical to those used for sample analyses. The chromatogra-
phic conditions for the SGCSM test of both columns are as follows:
Sample: 5 ng/pl, each component in 90% n-decane
Injection: 2 yl; splitless
Carrier: He at 23 cm/sec
Program: 140°C 3 min; 140 to 200° at 20°C/min;
isothermal at 200°C
Data acquisition: Start data acquisition at 8 min (SP2100)
or 10 min (SP1000)
The chromatographic features which were monitored to detect degradation of
the chromatographic and mass spectrometric systems are noted on the test
chromatograms. Generally, failure of SP2100 columns was indicated by decanol
tailing and acid-base ratio failure in advance of loss of coating efficiency
while the opposite was true for the SP1000 column which was much more resis-
tant to performance degradation.
Mass Spectrometer Operating Conditions
Instrument: GC: Finnigan 9500 with a Grob-type split/
splitless injector (identical to that of
the Carlo Erba 2150 GC) and a direct intro-
duction (no separator) transfer line (.fused
silica in final year of work only)
MS: Finnigan 3200
Data System: Systems Industries System/150
with Battelle-modified software and equipped
with a real-time clock.
lonization: 70 eV electron impact at 150 to 350 uA total
emission
Source Voltages: Ion energy: 2 to 8 Volts Cscan programmed)
Extractor/repeller: 2 to 11 Volts
Lens: '\—80 Volts
25
-------
CHROMATOGRAM FOR SP2IOO
Each component: 10 ng injected
-2-Naphthylamlne
Area ratios used to determine
the acid/base ratio
to
CTv
The degree of tailing Indicates
adsorption towards polar compounds
Separation number
visualization
Documents
"correctness"
of ion source
tuning
Pyrene
indicates anomalous
behavior of PNA s
Methyl stearate
Peak area Indicates
system sensitivity
Adequate efficiency requires
baseline resolution
20
6.0
100
11.3
Spectrum Number
Time (mln)
200
15.5
300
19.7
Figure 8. Typical GC-MS daily performance verification test chromatogram for the SP2100
(apolar) capillary column.
-------
2-Methyl Ce I
Methyl myristal*
2,6- Dimethyl ph.nol | Areo ,„„„ „.,„ |ffl de(efmln.
2,4-Dlethylanollne I acid/base ratio
C2i CHROMATOGRAM FOR SPIOOO
Each component- 10 ng Injected
Documents
"correctness"
of Ion source
tuning
DFTPP
Peak area Indicate*
overall system
sensitivity
Methyl stearate
Adequate efficiency requires baseline resolution
mniimiiii
2O
IIO
14.3
Spectrum Number 2
Time (min) 18.5
300
22.7
Figure 9.
Typical GC-MS daily performance test chromatogram for the SPIOOO (polar)
capillary column.
-------
Data Acquisition: Mass range: 40 - 450 amu
IFSS data acquisition parameters;
Maximum repeat count: 5
Samples/amu: 1
Repeat count before checking lower
threshold: 2
Integration time: 2 x 10~3 sec
Lower threshold: 3
Upper threshold: 1
(The above conditions give a slightly
variable scan time—depending on
collected ion current—of 2.4 + 0.3
sec/scan)
Signal Amplification: Preamplifier: 10~8 Amp/Volt
Electron multiplier voltage: sufficient
for 101* gain.
Controlled Temperatures: Separator oven and transfer line:
250° to 265°C for the SP1000 column
and 265° to 285°C for the SP2100
column.
Analyzer manifold: 85° to 100°C
GC-MS DATA PROCESSING
Archival
All GC-MS data associated with concentrate analysis were archived on 9-
track magnetic tape. The archived GC-MS data files include those for all
system performance- verifications (JC-43 calibration check, DFTPP check, and
SGCSM check), analyses (including all replicate analyses) of concentrates,
fractions, process blanks, and confirmation and quantification standards. A
total of 89 2400-foot 9-track magnetic tapes were used for this purpose. The
MS data system used for data acquisition was limited to a maximum of six digits
for each file name. A file naming system was designed which prevented any
redundant usage of file names and also coded the identifying characteristics
of each sample. The coded characteristics were:
• The sampled city
• The sampling sequence of the city
• The type of concentrate (i.e., how it was produced)
• The GC column used
• The identity of the sample (i.e., unpartitioned concentrate
and the various fractions)
• Whether the sample was a process blank
• Identification of each of the three GC-MS performance verifi-
cation checks and the data file to which it corresponded
28
-------
• Identification of an analysis of a standard mixture
Since use of the data file naming system is required in accessing the data on
the 9-track tapes, it was fully described in each of the concentrate analysis
reports and in Appendix C of this volume. Only the first three characteris-
tics above (city, sequence, and type of concentrate), are used in discussions
of the results in this Final Report. The tape-handling software which was
written for this purpose has been supplied to the Project Officer (see
Appendix A).
Correction for the Process Blank
Concentrate samples were partitioned individually rather than in batches,
and a set of process blank samples were generated simultaneously in parallel
fashion. The process blank samples were analyzed by GC-MS in sequence with
the corresponding sample fractions and the blank data were processed exactly
as the sample data. Components of the sample fractions that were present as
fractionation artifacts were identified by correlating the blank data with the
sample data. In this correlation, the analyst attempted to find every dis-
cernible component of the corresponding process blank in the sample data by
comparing chromatographic retentions and mass spectral characteristics. Sample
constituents which were thereby identified as artifacts due to the partitioning
process were not reported as being present in the sample. The only exceptions
to this rule occurred for compounds which were present at higher concentrations
(by at least a factor of 5 to 10) in the sample and which were not unexpected
sample components (for example, plasticizers). Borderline cases were indicated
"partially in the blank" in the tables of the individual concentrate reports
which identified the GC peaks, but these compounds were not entered in the
computer-managed data base of identified compounds.
Compound Identification and Confirmation
Tentative Identification of Sample Components —
Generally, compounds were tentatively identified based on a computerized
or manual comparison of the compound mass spectrum with a library of refer-
ence mass spectra. In some cases, identification by manual interpretation
was performed if it could be done cost-effectively. Appropriate background
spectra were subtracted from the sample constituent mass spectra used for
identification. Background corrected mass spectra normally corresponded to
the top of each discernible GC peak.
Three different mass spectral matching computer programs were available
for use in this work: two used a Systems Industries System/150 data system
and Battelle-developed software and one used a Finnigan/INCOS 2400 data sys-
tem. Since the Finnigan/INCOS mass spectral matching program correctly
identified mass spectra more reliably than the other two programs and pro-
vided the most convenient data output format, the System/150 processing
New software was written to enable the transfer of background corrected mass
spectra from the System/150 data system to the INCOS data system (Appendix A).
The data base for the computer matching system included the most recently
29
-------
released mass spectral library from the National Bureau of Standards (31,357
spectra) . In addition, software was written to bring each new version of the
library into use in advance of commercial availability through the Finnigan
Corporation (Appendix A)-
Confirmation of Tentative Identifications—
A compound identification was considered tentative unless it could be
confirmed by comparison of mass spectrum and relative retention time with
the corresponding data obtained on an authentic reference sample analyzed
under the same GC-MS conditions. The status of a compound identification
is indicated in the tabular computer output with either a "T" (for tenta-
tively identified) or a "P" (for positively identified, i.e., confirmed).
Tentative identifications had to meet the following criteria to qualify
for confirmatory activity:
1. The compound was not a known artifact of sample processing.
2. Identification confidence level of the senior analyst was
about 80 percent or greater.
3. The compound was commercially available for about $15 or
less. In the case of compounds with higher interest func-
tional groups, the upper price limit was in the $20 to $30
range. For compounds of probable health effect significance,
there was no upper price limit. (The decision to purchase
compounds at greater than $20 per sample was made by the
project principal investigator with input from the Project
Officer in special cases.)
Sources were sought for tentatively identified compounds which met the
first two criteria above. Battelle's in-house sources were searched before
resorting to commercial suppliers. The main approach for commercial procure-
ment was to request quotations for the minimum quantity from the most likely
possibilities listed in the current volume of Chem Sources-USA (Directories
Publishing Co., Inc., Ormond Beach, Florida). The Chem Sources-USA editions
published in 1978, 1979, and 1980 were used for this work. Reference com-
pounds were purchased according to the third criterion above.
Neat reference standards were used as received without first checking
purity or verity. In general, purity was not a primary concern since the
data generated were not to be used for quantitative purposes. When the GC-MS
data indicated problems with purity or verity the compound was either rejec-
ted from the confirmation database, or further work was done to establish the
verity of the data for compound identification confirmation purposes. Solu-
tions of neat reagents were prepared individually at 5 mg/ml in methylene
chloride or hexane, depending on compound polarity. Free acids and other
high polarity compounds were dissolved in methanol. Other solvents were used
only as required by solubility problems. Aliquots of 30 to 50 individual
standards were mixed using microsyringes and diluted with hexane or methy-
lene chloride to a concentration of 10 to 20 pg/ml. Mixtures of free acids
including phenolic compounds were methylated before GC-MS analysis using
30
-------
diazomethane exactly as for concentrate acid fractions. Internal standard
(2.0 ug hexaethylbenzene) was added, and the mixture was analyzed by GC-MS
exactly as for the concentrate sample fractions and blanks.
Background subtracted spectra of all discernible GC peaks and shoulders
were, plotted and library matched (using Finnigan INCOS software) . The data
were correlated with the known composition of the mixture. Discrepancies with
INCOS match results, ambiguities concerning isomer assignment or other indi-
cations of questionable purity or verity of individual compounds were recon-
ciled by using the compound in question in a subsequent mixture of different
composition. Often, chemically related species were used in the same mixture
at concentrations different by integer factors to aid in assignment of compo-
nent identities. The resulting standard mass spectra were catalogued for
future reference and the GC and other relevant parameters were entered into
the computerized database. In all, GC data for 1050 individual compounds
were entered in the mainframe computer database. Software was written which
supplied listings of these compounds and the corresponding retention data or-
dered by four different criteria:
• Increasing Molecular Weight
• Increasing Relative Retention on the SP1000 GC Column
• Increasing Relative Retention on the SP2100 GC Column
• Increasing Inventory Index Number of the EPA Reference
Standard Repository
A set of these four listings in their final form constituted one of the de-
liverables required by the contract (see Appendix A).
In confirmation of tentative identifications, the acceptance criteria for
GC retention was correspondence of relative retentions within 0.1 percent to
1 percent, depending on the proximity of elution to that of the internal
standard, hexaethylbenzene. Generally, GC relative retentions over the range
0.3 to 1.8 agreed with reference data within about 0.5 percent. In some
cases, GC retention data for concentrate samples showed a systematic drift
in the GC retentions for the deuterated internal standards and/or other com-
ponents identified at high confidence levels. This drift was taken into
account when comparing sample GC retention with the confirmation database.
Aliquot for EPA's GC-MS Reference Standard Repository—
A portion of each neat standard was reserved to establish an EPA GC-MS
reference standard repository. Screw-cap vials (2.75 ml) with Teflon-lined
septa seals were filled at least half full or with half of the total material
purchased (whichever was greater) and labeled with the compound name, formula,
commercial source, and an inventory index number. Compounds indicated to be
temperature sensitive were stored at -10° until transferred to U.S. EPA HERL-
CI. Compounds of known health hazard were stored separately from the others.
Computerized GC-MS Data Searching for Specified Compounds
In addition to identifying the mass spectra obtained for discrete GC peaks
and shoulders, a more sensitive computer search system was used to detect the
presence of 53 specific compounds (.listed in Table 4) considered by the
31
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TABLE 4. LIST OF THE 53 COMPOUNDS FOR WHICH GC-MS DATA WERE SEARCHED
Compounds Listed by Increasing Molecular Weight
Chloroprene
Aniline
Phenol a
Diethylnitrosamine
Styrene
4-Methylphenol
2-Methyl styrene
2,4-Diamino toluene
2,4-Dimethylphenol
Nitrobenzene
2-Chlorotoluene
2-Chloroaniline
3-Nitroaniline
4-Chloropheno1b
2-Naphthylamine
1,4-Dichlorobenzene
p-Nitrophenolb
4-Chlorophenyl methyl ketone
2-Chloronaphthalene
Diphenylamine
4-Phenylaniline
2,4-Dichlorophenolb
1,2,4-Trichlorobenzene
2,4-Dichloronaphthalene
Fluoranthene
2,4,6-Trichlorophenolb
2-Methyl-4-chlorophenoxyacetic acidb
N-Phenyl-1-naphthylamine -
Chrysene
2,4-Dichlorophenoxyacetic acid b
1,4-Dibromobenzene
Benzo(a)pyrene
Benzo(b,k)fluoranthene
Hexachloro-1,3-butadiene
Pentachloroaniline
2,4,5-Trichlorophenoxyacetic acid
Hexachlorocyclopentadiene
Benzo(ghi)perylene
Indeno(1,2,3-cd)pyrene
Pentachlorophenolb
Hexac hlo robenz ene
Lindane
Tetrachlorobiphenyls
Pentachloronitrobenzene
Pentachlorobiphenyls
Triphenyl phosphate
DDT
Hexachlorobip heny1s
Aldrin
Tri-(m)-cresyl phosphate
Heptachlor
Dieldrin
Hexabromo bip henyl
a) Searching for both the free acid and the methyl ether was performed.
b) Searching for the methyl ether or methyl ester only was performed.
32
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Project Officer as possibly significant health risks. For this purpose, a
highly sensitive and specific computer search program was developed for use
with the System/150 GC-MS data system. In this program the technique of
selected ion summation (SIS) was used to search for each of the 53 compounds
within specified relative retention time windows (8) . The program was very
effective at detecting and locating the specified compounds in the GC-MS data
even when the compound mass spectra were hidden by ion current signals from
background and co-eluting compounds. The main features of the SIS program
are given in Appendix A.
An important quality assurance measure was that mass spectra of SIS
search "hits" were always manually verified before the data were reported to
insure against false positives due to co-elution interference. The SIS
search compounds (Table 4) which were detected appear in all computer-printed
tables with an asterisk flag (*) in front of the compound name and a concen-
tration entry in ng/1 which replaces the "P" or "T" indicator in the tables
showing compound identification status as confirmed or tentative.
Quantification of Identified Compounds
In principal, each of the 521 individual compounds for which compound
identifications in DW and AWT concentrates have been confirmed (and, there-
fore, for which a reference standard of the compound was on hand) could have
been quantified using ordinary response factor/internal standard methodology.
However, such an approach would not be cost-effective since many of these
compounds with confirmed identification have little or no known health effect
significance. Nevertheless, it was important to have some basis for approxi-
mating the concentrations of each of the 1641 individual tentatively and
positively identified compounds. Two approaches to quantitative approxima-
tion were used as the best compromise for this problem:
(1) The 53 compounds of Table 4 which were detected by the SIS
specific search software were quantified using deuterated
internal standards, extracted ion current profiles (EICPs)
and response factors generated from GC-MS analysis of
standards.
(2) The concentrations of all other tentatively or positively
identified compounds were approximated by comparing the
size of the GC peak in the total ion chromatogram with that
of the pre-analysis internal standard, hexaethylbenzene, to
generate a relative size (RS) parameter.
Quantification of Specific Search Compounds—
Response factors (RFs) were generated, as required, for the 53 compounds
of Table 4 using the data from GC-MS analyses of standard mixtures of these
compounds which were processed through the concentrate partitioning scheme.
Equation 1 shows the formula used to generate the response factors for the
component "A" relative to an internal standard (IS):
33
-------
Amount A pig in std)
£-, _ EICP area (A in std) Eq. 1
A ~ Amount IS (yg in std)
EICP area CIS in std)
Quantification of component "A" in the GC-MS sample data was then performed
using equation 2:
A ... A r • i \ EICP area (A, sample)
Amt. A dig in sample) = ____ 77^ v ,\ x
6 v EICP area (IS, sample)
RF x [Amt. IS (yg in sample)] Eq. 2
Equation 2 is equivalent to the use of a one-point plus the origin standard
curve, and it requires that the same EICP masses used to determine the re-
sponse factor (RF, eq. 1) also be used to generate the EICP peak areas in the
GC-MS data for the concentrate. Note also that best results are be obtained
when the instrument high mass/low mass response characteristics are identical
for both the concentrate and standard mixture data acquisitions. As mention-
ed above, this tuning characteristic was checked using DFTPP prior to every
GC-MS acquisition. In addition, care was also taken to ensure that none of
the ion current signals used in the area calculations were saturated.
In theory, optimal quantification would result from analysis of the un-
partitioned concentrate since ambiguities due to the nonreproducibility of
losses of the designated analyte and/or deuterated internal standard in the
partitioning scheme are automatically avoided. In practice, however, the
high dilution factor and extremely complex composition of the concentrate, as
received, always resulted in more sensitive detection and higher quality data
for SIS specific search and quantification on the fractions. Nevertheless,
the GC-MS data from all the analyzed unpartitioned concentrates (which ex-
cludes the concentrates produced by XAD-2 extraction of RO brine) were search-
ed for the compounds of Table 4 using the SIS software, and quantification
was performed using that data whenever possible. Response factors generated
from an unpartitioned standard were used in these cases. Often, the quanti-
tative data from the unpartitioned analysis were too weak to serve any purpose
other than a confirmatory one for the results from the fractions, and in
these cases quantification was performed using the fraction data.
Semi-quantitative Estimation by Relative Size (RS) of the GC Peak—
The relative size (RS) parameter was developed as a somewhat imprecise
but extremely cost-effective method for estimating the amount of every iden-
tified component. It is a logarithmic scale spanning four orders of magni-
tude. Assignment involved visually estimating the size of each GC peak
in the total ion current chromatogram relative to that of hexaethylbenzene,
an internal standard of which 2 yg were added to every sample immediately be-
fore GC-MS analysis. Thus, each GC peak corresponding to an identified com-
pound was assigned an RS value consisting of an integer from 1 to 9 on the
basis shown in Table 5.
The computer report-generation software normalized all RS values (before
outputting) to a typical 1514-liter sample according to equation 3:
34
-------
RS (output) = 2 logl(
antilogy o[RS(input)/2]
(.liters sampled)/(1514 liters)
Eq. 3
Thus, computer output RS values in Tables 9, 10, and 11 are directly compar-
able from one concentrate to another in terms of being representative of con-
centrations in the original water. Generally, the output RS values ranged
between 0 and 9. However, when the sampled water volume exceeded 1514 liters,
it was possible for the RS (output) value, Eq. 3, to become negative for the
smallest RS (input) values since the scale is logarithmic. The RS value was
designed to provide approximate quantification for every water concentrate
sample component identified. While it might be tempting to assign the cor-
responding value in nanograms per liter of original water to each compound
(as indicated in Table), such an assignment would not be scientifically well
founded, and it also could be misleading and easily misinterpreted. If the
following conditions prevailed, then the RS criteria would have provided exact
quantification:
• The sample component and internal standard had the same
response factor for mass spectrometric detection
• Instrument response was linear through the entire 10,000
fold RS range
TABLE 5. GC PEAK RELATIVE SIZE (RS) VALUES FOR SEMI-QUANTITATIVE
ESTIMATION OF COMPOUND CONCENTRATIONS
GC Peak Size
Relative to the Approximate
RS Value Internal Standard3 Concentration^
9
8
7
6
5
4
3
2
1
Greater than 100X
30 to 100
10 to 30
3 to 10
1 to 3
1/3 to 1
1/10 to 1/3
1/30 to 1/10
1/100 to 1/30
>1300 ng/1
.
•
,
13 ng/1
•
•
•
0.13 ng/1
1.3 ppb
•
•
•
13 ppt
•
•
•
0.13 ppt
a) The ranges are half orders of magniture so the RS value numbers span a
"linear" log range. Technically, they should be 1-3.16, ...31.6-100,
etc., but for visual comparison purposes only one significant figure is
more appropriate.
b) Assuming the GC-MS response factor for the analyte to be equal to that of
the Internal Standard and a 1514 liter (400 gallon) water sample. See
text for other precautions concerning the use of the RS value.
c) ppb: parts per billion; ppt: parts per trillion.
35
-------
. Neither the identified component nor internal standard
GC peaks were broadened due to chromatographic over-
loading
The sample component was recovered quantitatively through
the partitioning scheme and suffered the same relative
chromatographic losses as the internal standard
. The component was removed from the original water into
the concentrate quantitatively.
Clearly the preceding conditions were never met. However, since detection of
the internal standard was probably acceptably reproducible, direct comparison
of RS values for the same component from one concentrate to another can be
made with relative confidence. While it is known that RO recovers many or-
ganic species nearly quantitatively Cespecially those of high molecular weight)
it may be somewhat less efficient for others. In addition, the residue weight
results of Tables 7 and 8 (see Section 5, Results and Discussion) indicate
that significant amounts of organic material were not recovered in the parti-
tioning scheme. These and other factors giving rise to the underestimation
of concentration based on the RS value (as per Table 5) are expected to gen-
erally outweigh other factors which cause overestimation. Thus, the
correlation of concentration with RS value as indicated in Table 5 should be
taken as a lower bound only.
DATA MANAGEMENT
The enormous bulk of compound identification results and other data gen-
erated by analyses of the DW and AWT concentrates could not be managed effi-
ciently by manual means. An existing system of Battelle-written software
described as a numerical classification and evaluation system (NUCLEUS) for
large bodies of related information, was modified for this purpose. The
NUCLEUS software was operated on three CDC computers (Control Data Corpora-
tion; Cyber 6500, Cyber 73, and Cyber 74) in Battelle's central computing
facility. This software featured:
• A structured programming language
• Dynamic simulation modeling
• Data base management
• Report generation
• Conversational programs
• Batch or on-line access (via remote terminal in the
laboratory) for program modification and data entry
or editing.
The NUCLEUS data management system provided a number of extremely valu-
able capabilities:
• Flexibility in the way all lists of identified
compounds could be ordered
36
-------
• Combining, non-redundantly, related lists of
identified compounds for a concentrate
• Combining, non-redundantly, lists of compounds
for up to 27 concentrates
• Tabulating occurrence and concentration (RS
value) statistics of 25 types of molecular
functional groups for individual fractions,
combinations of fractions and combinations of
concentrates
• Incorporating useful, descriptive information
about the individual compounds.
These capabilities were necessary for the achievement of the project goal of
enabling interpretation of the biological activity testing results in terms
of the chemical composition of the concentrate. A further benefit was the
ability to produce error-free listings of compound identification results
which were organized in multiple, useful formats. With over 2100 different
identified compounds entered in the data base, it is clear that a computer-
assisted data management and report generation system was the only reasonable
approach to this problem.
The data base stored the following information relevant to each compound
identification:
• Fraction and concentrate in which identification occurred
• GC phase used
• Retention time
• Relative retention value
• Spectrum number
• Relative size of the GC peak
• Concentration (ng/1 in original water), if available
• Status of the identification (tentative or confirmed)
• Description of the compound including:
1. Systematic name
2. Common name
3. CAS number
4. Molecular weight
5. Molecular formula
6. Industrial source and/or use
7 - Classification as one of ten chemical types
8. Functional groups contained in the molecule.
Once these eight items describing the compound have been entered, identifica-
tion in subsequent concentrates require entry of only the CAS number and the
other non-compound descriptive items listed above.
37
-------
In addition to the above listed information relative to each identified
compound, the following general information was also entered into the data-
base:
• Descriptive data for the concentrate (city, date of
sampling and volume of water, date received, date of
partitioning and name of the person who partitioned
the concentrate, the volume, color and solvent of
the concentrate, as received, and the amount of the
concentrate reserved for unpartitioned analysis)
• Residue weight analysis data for the fractions and
unpartitioned concentrate
• Conditions used for the GC-MS analysis.
The above items provided the necessary information for computer data pro-
cessing and generation of the computer-printed tables contained in the in-
dividual concentrate analysis reports and those presented in this Final
Report.
REPORT GENERATION
Concentrate Analysis Reports
Separate reports on the GC-MS analysis results for each DW and AWT con-
centrate were prepared and delivered to the Project Officer. These reports,
along with other relevant information, are tabulated in Tables 1A and 2A of
Appendix A. Each complete concentrate analysis report consisted of seven
volumes produced in various numbers of copies. The contents of each volume
are described in Table 6. Volume 1 was designed to contain the core material
of the concentrate analysis report. The computer-printed tables selected for
inclusion in that volume were the following:
• All compounds found in all four of the GC-MS analyzed
fractions in non-redundant listings of three tables:
1. by decreasing size of the GC peak (RS value) showing
the fraction(s) and GC column(s) where the identifi-
cation was made, the status of the identification
(tentative or confirmed), the RS value and when known
the concentration in ng/1.
2. ordered as in 1 above, but showing both systematic and
common names, industrial source or use, molecular
weight and RS value.
3. ordered by increasing molecular weight showing molecu-
lar formula.
38
-------
TABLE 6. CONTENTS OF THE INDIVIDUAL REPORTS FOR DW AND AWT CONCENTRATES
Number of
Delivered
Volume Contents Copies
1 Short summary of the results 15
Analytical scheme
Residue weight results for fractions and
the unpartitioned concentrate
Discussion of the results
Labeled GC-MS chromatograms for the
unpartitioned concentrate (both GC columns)
Key computer-printed listings of compound
identification results
2 Complete set of computer-printed listings 3
of compound identification results3
Labeled GC-MS chromatograms of the four
fractions (both GC columns)
3 Mass spectra of compounds with confirmed 3
identification and tentative identifica-
tion found on the SP1000 GC column
4 Mass spectra of compounds with confirmed 3
identification and tentative identifica-
tion found on the SP2100 GC column
5 Mass spectra of the deuterated internal 3
standards from the analyzed fraction data
GC-MS chromatograms of a standard run of
the compounds for specific search on
SP1000 and mass spectra of specific
search "hits" on SP1000
GC-MS chromatograms of a standard run of
compounds for specific search on
SP2100 and mass spectra of the specific
search "hits" on SP2100
6 Mass spectra of decafluorotriphenylphosphine 1
(DFTPP) ion source tuneup verification
Standard GC separation mixture (SGCSM)
GC-MS system performance verification
chromatograms
Labeled GC-MS chromatograms for analyses of
fractions of the partitioning process blank
7 Real time total ion chromatograms of 1
concentrate fractions on SP1000 and
SP2100 GC columns
a) See text for an itemized listing of these tables.
39
-------
• Functional group listings for all four, analyzed fractions
combined as follows:
1. all results from the SP1000 GC column showing total,
ma* 1 mi im and minimum RS values
2. all results from the SP2100 GC column showing total,
maximum and minimum RS values
3. results from both columns combined without"RS value
information
• Identified compound listings for the four fractions,
individually, but showing combined results from analysis
on both GC columns; ordered by decreasing RS value
• Functional group listings for the four fractions, individ-
ually, but showing combined results from both GC columns.
These tables were also included in the second volume along with the following
tables which comprised the entire set of computer-produced tabulations:
• Identified compounds for each of the four fractions on each
of the two GC phases (eight sets of tables) with each list
ordered three different ways:
1. alphabetically; showing molecular formula, molecular
weight, identification status (tentative or confirmed)
and concentration in ng/1, if known
2. by increasing relative GC retention; showing GC retention
time, relative GC retention, spectrum number, RS value,
and identification status
3. by decreasing RS value; showing RS value, identification
status and concentration in ng/1, if known
known
• Functional group listings for each of the four fractions on
each of the two GC phases (eight tables).
Combined Concentrate Analysis Reports
Whenever a concentrate report was the final one of a series of related
concentrates, all the results of the related series were integrated by the
NUCLEUS data processing software into a single, tabular output for presenta-
tion as a composite report. These non-redundant listings were produced in
two correlated tables. The first table displayed all results in a listing of
common names ordered by decreasing relative GC peak size. For each entry,
this table showed:
40
-------
• the concentrate in which the detection occurred
• the status of the identification (confirmed or
tentative) in each concentrate
• the concentration (ng/1) results, if known
• the largest relative GC peak size found for the
compound in each concentrate
• an indicator symbol marking compounds of special
interest.
Whenever the number of combined concentrates exceeded six, this first table
was presented in two parts. The second correlating table showed, for each
entry of the first table, the corresponding systematic name, CAS number, mo-
lecular formula and molecular weight. The concentrate reports which contain-
ed these special, combined reports as well as the concentrates which have
been combined, are designated in Tables 1A, 2A, and 3A of Appendix A. In all,
15 such combined reports were produced for inclusion in the regular concen-
trate reports.
Special Listings of the Databases
The NUCLEUS software for data management also provided facile production
of highly useful listings of the entire identified compound database. These
listings did not indicate the concentrate in which detection occurred, but
instead, they showed chromatographic and other information. These lists were
useful in determining whether compounds identified in concentrates were al-
ready in the database. They were also useful for comparing GC retention val-
ues to those previously observed. The identified compound listings were pro-
duced in two formats: (.1) all compounds ordered by increasing molecular
weight, and (2) all compounds ordered by increasing relative GC retention.
The latter was produced in two sets of tables—one set for each GC phase
(SP1000 and SP2100). Each of these sets were, in turn, composed of two
tables: (1) compounds that were identified in the derivatized acid fractions,
and (.2) compounds that were identified in the other three GC-MS analyzed frac-
tions (i.e., base-neutrals).
The database of compounds identified in concentrate samples was distinct
from the database of compounds analyzed as reference standards for confirma-
tion of identifications. This confirmation database was also listed for util-
ity purposes in four tables which are described earlier.
Since these utility listings of the two databases were valuable beyond
the scope of this work as general reference collections, they were provided
to the Project Officer in updated versions through the course of the project
work. These listings are tabulated and described in more detail in Appendix
A. The identified compound database listing ordered by molecular weight is
included as Appendix D. This list has been correlated with the key tables
which show the occurrence of the compounds in the samples.
41
-------
SUGGESTIONS FOR IMPROVEMENTS TO THE ANALYTICAL SCHEME
Some minor modifications to the Analytical Scheme presented above can be
recommended based on the two years of experience with this program.
Internal Standards
At the beginning of the research program all commercially available and
applicable deuterated internal standards were obtained. In addition, one
internal standard, dimethyl terephthalate-D<,, was synthesized since there was
no commercially available deuterated standard of correct polarity for recovery
in the high polarity fraction. Future applications of the analytical scheme
should incorporate some of the additional deuterated compounds which have re-
cently become available. In particular, additional compounds with a variety
of functional groups should be selected to provide more internal standards in
the medium and high polarity fractions. Nitriles, alcohols, esters, amides,
amines, ketones aldehydes and non-aromatic acids are recommended to fill these
internal standard gaps.
Concentrate Fractionation
The low number of basic substances found in the concentrates suggests
that the separate step of extraction of these species should be omitted. More-
over, modern glass capillary GC columns allow gas chromatography of these
materials without derivatization in nearly all cases. Good recovery of the
bases from the silica gel column could be assured by a small amount of methyl
amine modifier in the methanol used to elute the high polarity fraction.
Derivatization of the acids using gas phase delivery of diazomethane was
excellent with respect to minimizing the introduction of impuritites via the
derivatization reagent. However, in situ formation of chloroalkanes (appar-
antly due to multiple CH2 insertions on an active precurser) was a poorly
understood and controlled problem. Solvent exchange removal of methylene chlo-
ride solvent and addition of a trace quantity of mineral acid prior to deriva-
tization appeared to be a reliable solution, but more work should be performed
to refine this critical step.
Final sample evaporation on the N-Evap® apparatus was tedious, time con-
suming and difficult to maintain at optimum conditions. This procedure should
be replaced with another which is better optimized regarding reliability and
speed.
GC-MS Data Acquisition
Newer GC-MS equipment is capable of faster, more reliable scanning of the
mass range. This capability can be exploited through the use of H2 GC carrier
gas and marginally faster temperature programming (perhaps 3°C/min) without
any detriment to the chromatography or quality of the mass spectral data. Ex-
perience suggests that a shorter scan range (40 amu to 350 amu) would also
enable higher quality mass spectral data with almost no loss of compound ident-
ification capability. Repeating an occasional analysis whenever the data
42
-------
suggested higher mass ions were present would probably still allow a cost-
effectiveness improvement.
Data Processing
Improvements in mass spectrometry data systems now allow the flexible
creation of specialized GC-MS data processing routines. Two recommended
improvements to the analytical scheme which this new capability would enable
are the following:
• Capability to build a mass spectral library of the unidentified
mass spectra of each analysis would enable the accurate and
facile updating of compound identification results once recurring
unidentified mass spectra are successfully interpreted. In
addition, the cataloguing of occurrences of such unidentified
mass spectra would provide the necessary occurrence frequency and
concentration level information on which to base decisions con-
cerning the investment of resources in pursuing manual inter-
pretation
• A valuable automated QC step should be incorporated in which, at
the end of each GC-MS data acquisition, a search routine would
generate raw areas of all the pre-fractionation deuterated in-
ternal standards and any pre-analysis internal standards and
calculate the appropriate ratios between the former and the
latter. This hard-copy QC report would allow essentially "real-
time" QC monitoring of both, the GC-MS system performance and the
recovery effectiveness of the fractionation scheme.
43
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SECTION 6
RESULTS AND DISCUSSION
ORGANIZATION OF THE PRESENTATION
Presentation and discussion of the analysis results for the DW and AWT
concentrates is organized in four sections:
1. A general overview of the analysis results, approach
to the concentrate production process blank problem
and summary of the available tabulations (Tables 7 and 8)
2. Discussion of the DW results (Table 9)
3. Discussion of the AWT results (Table 10)
4. Comparison of DW and AWT results (Table 11).
Items 2, 3, and 4 each have an associated computer-printed listing of the
identified compounds showing the concentrates where detection occurred, the
relative size of the GC peak for each detection and an indication of the
compounds which should be considered as attributable to the RO processing
blank or the XAD-2 resin adsorption/elution blank. These tables are very
long (30, 35, and 37 pages for DW (Table 9), AWT (Table 10), and combined DW
and AWT (Table 11) , respectively) and have been placed together at the end of
this section to facilitate referral by the reader.
OVERVIEW OF THE RESULTS
Comparison of Residue Weight Results and
Compound Identification Statistics
Distribution of Organic material in the Analyzed Factions—
Residue weight analysis results and compound identification statistics
are shown for DW concentrates in Table 7 and for AWT concentrates in Table 8.
Comparison of the residue weight results in Tables 7 and 8 shows a similar
predominance in both types of water sources of acidic and highly polar
neutral materials in the recovered fractions. Composited values for the four
Lake Tahoe, three Pomona (9/25/74) and two Blue Plains (9/20/74) concentrates,
Table 8, have been taken for these three samplings as approximations of the
total organic material recoverable from the RO brines by solvent extraction.
Concentrates C3C, R1C, R2C, E1C, and B2C consisted of composites of all RO
brine solvent extracts (see Section 2 and Table 2). Thus, concentrates C2N
and D2N, Table 8, are the only sets of data not useable for comparison as a
combined solvent extract of the RO brine produced by a given sampling.
44
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TABLE 7. PERTINENT CONCENTRATE DATA FOR DRINKING WATER
City
Poplarvllle,
Mississippi
Poplarvllle,
Mississippi
Code*
Name
VIC
V1X
XAD-2 Dlethyl Ethar T28
Elution Blank
Cincinnati,
Ohio
Cincinnati,
Ohio
Cincinnati,
Ohio
Cincinnati,
Ohio
Cincinnati,
Ohio
Miami.
Florida
Miami,
Florida
New Orleans,
Louisiana
New Orleans,
Louisiana
Philadelphia.
Pennsylvsnia
Philadelphia,
Pennsylvania
Ottumwa,
Iowa
Ottunwa,
Iowa
Seattle,
Washington
Seattle.
Washington
Extraction
Solvent Blank
XAD-2 Cthanol
Elutlon 3 lank
TIC
T1X
T1Y
T4C'
T4X
M2C
M2X
N2C
N2X
P2C
P2X
02C
02X
S2C
S2X
X1C
XIX
a) The three digit code IU
b) The amount of
c) The amount of
polarity, and
d) Includes the
e) The value in
Date and
Sampled
(Liters)
> 3/2/79 J
1 (15,100)
)
(k)
10/17/78 •>
(1,460)
(5,300)
• 2/3/76J
1 (2,280)
• l/u/76:l •
(6.620)
2/10/76 J •
(5.810)
,
9/10/76 3 ^
(5,450)
11/5/76 1
(11.750)
(k)
(k)
ne is used in
organic material in the
the recovered fractions
high polarity fractions
recovered
slkane/alkene
Residue Weight Analysis
Fractions, Jc
s! r . £ 1 '" s
5 T, a .25 * •; S
8 Z 1 12 5 31
0.6 2.4 0.6 4.1 11 22
17 1.8 21 1.0 1.8 38
— 0.07* 0.07* 0.02 l 0.04 Z —
143 32 0.05 1.6 18 52
397 11 0.0 0.2 1 12
540 17 0.0 0.6 5.5 23"
527 23 0.2 1.3 16 41
115 26 0.1 0.3 10 36
745 10 0.03 0.1 0.6 11
Ti"
527 38 0.1 0.3 11 50
2,100 11 0.4 0.2 0.6 13
TO"
217 31 0.5 6.0 16 53
949 9 0.3 0.2 0.7 10
IS*
177 31 0.3 0.6 32 65
'1,006 5 0.1 0.4 2 7.7
19°
139 39 0.1 0.5 17 57
775 6 0.1 0.1 0.5 6.7
— *
37 30 0.4 1.5 20 53
99 8 0.1 0.1 3.3 12
13 n,
— 0.05* O.OO1 0.02* 0.031 —
— 0.04' 0.09* 0.08 10.091 —
the computer generated listings.
Identification Results
Number
of Compounds
Status
41
E
e
o
19
60
42
66
35
126
112
96
77
66
101
75
125
96
83
70
120
70
19
27
V
1
c
V
l-
31
98
57
85
42
117
81
85
143
173
148
158
167
125
150
161
269
101
33
31
'-
4*
0
H
50
158
99
151
(140)
77
(66)
243
(211)
193
(165)
181
(113)
220
(208)
239
(106)
249
(231)
233
(144)
292
(279)
221
(114)
233
(213)
231
(142)
389
(361)
171
(140)
52
58
v
u
C
V
I
33
41
110
123
74
52
152
53
69
32
121
99
73
64
64
73
84
42
99
47
55
59
180
114
51
46
61
33
52
57
49
37
68
50
60
28
28
29
80
62
Special
Compounds
00
—
« U
U k.
u •
Q. V
V) VI
k
3
2
6
1
19
16
7
6
2
12
3
10
4
6
3
11
7
0
0
«
« «
• W
s!
9
6
7
7
5
13
13
7
12
a
15
10
11
11
8
6
12
8
2
U
• k.
— 0
II
c c
9
6
11
9
2
24
17
5
13
6
15
8
18
a
12
7
15
12
5
2
concentrate expressed as uR/1 (ppb) in the original water sample.
f expressed as a percentage of the concentrate (residue basis). The
are the hexane: benzene, methylene chloride, and
fraction (hexane silica gel eluate) which is not
parentheses excludes compounds attributable to the RO process blank
f) Unidentified components are listed separately for each GC phaae. Upper number:
methanol silica gel
analyzed by
GC-MS.
aromatic, medium
eluates respectively
or XAD-2 resin (see discussion
S?1000
in Volume
1).
Lower number: SP2100.
g) The 53 compounds for which the data are specifically searched are listed in Table 4 (Volume
1).
h) The EPA "Consent Decree" list of priority pollutants (semi-volatile compounds) .
1) The "Chemical
Indicators of Industrial Pollution" list (Federal Interim Primary
J) Concentrates which were derived from
k) A blank which
does not
t) The value shown is the
the same water sample or s duplicate water
Drinking Wster Regulations
sample
. February 9
. 1978).
correspond to s water sampling.
fraction weight (mg) rather than the percentage of the concentrate.
•) The vslue shown Is composited from Che vslues for the solvent extract and XAD-2
45
-------
TABLE 3. PERTINENT CONCENTRATE DATA FOR ADVANCED WASTE TREATMENT WATER
Residue Weight Analysis
Fractions.
Identification Results
Number of Compounds
Status
Special
Compounds
Code3
City Name
Extraction Solvent X1C
Blank
Lake Tahoe, L2P
California
Lake Tahoe, L2M
California
Lake Tahoe, L2N
California
Lake Tahoe, L2D
California
Pomona, C3C
California
Pomona, C1F
California
Pomona, C1H
California
Pomona, CIS
California
Pomona, C2N
California
Orange County, R1C
California
Orange County, R2C
California
Escondido, E1C
California
Dallas, Texas D2N
Blue Plains, B2C
Washington, D.C.
Blue Plains, B1M
Washington, D.C.
Blue Plains, BIN
Washington, D.C.
Date and
Volume
Sampled
(Liters)
(k)
10/24/74J
(1,500)
6/17/75
(1,500)
9/25/74J
(1,500)
10/2/74
(1,500)
1/27/76
(1,500)
2/3/76
(1,500)
7/8/75
(1,500)
11/11/74
(1,500)
5/31/75
(1,500)
9/20/74 J
(1,500)
S" 25 x^ 3j
c a w B £ •* 11
1) flj 3 14 U ^* >
U T3 B -• «J J= « tU 0
C -rt O -O -4 00 iH 4J (J
O O M 11 O -M O O 11
o •< < sa.xo.HK
— 0.05 £ 0.00 l 0.02 * 0.03 l —
51 7.4 1.2 2.7 77 89
52 65 0.02 4.9 20 90
153 16 2.4 2.6 60 81
50 39 0.01 0.8 21 61
306 27 1.4 2.7 50 81""
87 7.7 1.2 3.0 34 46
197 0.99 1.8 1.5 23 28
104 22 0.96 1.9 13 38
69 83 0 1.1 3.3 88
370 22 1.2 1.5 17 42m
37 5.7 5.4 1.9 5.6 20
104 6.6 0.7 0.5 28 37
144 9.0 1.1 1.8 37 50
18 2.3 0.7 0.2 20 23
18 33 3.2 0.1 13 62
46 12 1.1 1.4 63 79
23 26 0.2 1.0 13 41
21 59 1.4 1.7 20 83
44 42 0.8 1.3 16 60m
-------
Averaging the total recovery percentages for each of these eight AWT composite
concentrates or equivalent composite concentrate groups of Table 8 and
similarly averaging these values for the seven DW solvent extract concentrates
of Table 7, the same value (52 percent) is obtained for the AWT and DW concen-
trates. The majority of the recovered material for both DW and AWT concen-
trates was found in the two most highly water soluble fractions (acidic and
high polarity) with the eight AWT composite concentrates (and groups, as
above) averaging 94 percent of the recovered material in these two fractions
and the seven DW composite concentrates yielding a corresponding value of
97 percent. However, the distribution of these highly water soluble organic
materials between acidic and neutral species is reversed for AWT versus DW
concentrates: of the organic material in the AWT concentrates, averages of 16
and 33 percent were recovered in the acid and high polarity fractions, respec-
tively, while, for the DW concentrates, these averages were 32 and 18 percent
for the same fractions.
Comparison of the Amounts of Organic Material
Present in DW and AWT Concentrates—
As cited above, only 5 of the 16 AWT concentrates shown in Table 8 were
composites prepared by combining all six of the solvent extracts of each RO
processing (sampling event). The other 11 AWT concentrates were individual
solvent extracts which represent only part of the total material recoverable
by solvent extraction of RO brine. Comparison of these AWT solvent extract
composite concentrates (C3C, R1C, R2C, E1C, and B2C, Table 8) with the 7 DW
solvent extract composite concentrates (TIC, T4C, M2C, N2C, P2C, 02C, and
S2C, Table 7) shows that., generally, the sampled drinking water contained a
higher concentration of organic material recoverable by the RO/solvent
extraction procedure than did the AWT water. The average values in Tables 7
and 8 under "Concentration, ug/1" are 81 for the five AWT concentrates and
183 for the seven DW concentrates. Adding composite values for the Lake
Tahoe, Pomona (6/25/74) and Blue Plains (9/29/74) samplings to the five AWT
concentrates (as above) results in a somewhat higher average value of
140 ug/1 although this value is still significantly less than the average
for the seven DW concentrates. It cannot, however, be concluded that, on the
average, the sampled AWT water contained less organic content than the
sampled DW since additional concentrates of the RO brines were not produced
using XAD-2 adsorption/elution for the AWT samplings. Indeed, the TOC data
shown in Tables 1 and 2 are uniformly higher for the AWT samplings (Table 2)
than for the DW samplings (Table 1) by a factor of two to four. Thus, the
distribution of molecular polarities or other properties which have an impact
on recovery by RO and/or solvent extraction of the organic species present
must have been significantly different for these two water types. The
tentative conclusion is that the AWT water contained higher relative amounts
of more highly water soluble organic material with lower extraction effic-
iency than did the DW.
This conclusion seems to be supported by the statistics for the number
of identified compounds for each concentrate in Tables 7 and 8. The average
number of identified compounds for the 5 AWT composite solvent extract
concentrates was 116 while the corresponding average for the 7 DW composite
solvent extract concentrates was 228. This trend may also be explained simply
47
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by considering that, in all but one case (TIC, T1X, and T1Y; see Tables 7 and
8), the DW samplings involved greater volumes of water than those for AWT by
factors ranging from 1.5 to 7.8. A larger volume of sampled water might be
expected to yield detection limits at lower concentrations, and, indeed, the
largest number of compounds (361) were detected for the concentrate with the
greatest DW volume sampled (11,750 liters for Seattle, Washington, code S2C) .
XAD-2 Resin Extraction Effectiveness/Humic Materials—
The DW concentrates produced by XAD-2 resin extraction of the RO brine
contained a significantly greater amount of organic material than those pro-
duced by solvent extraction of RO brine. In Table 7, three digit code names
ending in "C" designate concentrates produced by solvent extraction of the RO
brine while those ending in "X" correspond to subsequent XAD-2 resin extraction
of the RO brine. Comparison of the concentration values for corresponding
concentrate pairs illustrates the higher efficiency of XAD-2 resin extraction,
especially since solvent extraction was performed on the RO brine prior to
XAD-2 resin extraction. The experimental observations indicate that much of
the additional organic material recovered by XAD-2 resin extraction was humic-
related substance. These observations indicating the presence of large
amounts of humic materials include the following:
• The color (aqueous, high pH) was amber-brown and the
UV spectrum showed a very broad maximum in the
250 ran region
• Aqueous solubility was greatly enhanced at high pH
• Extraction efficiency from aqueous media at low pH
with methylene chloride was poor resulting in low
total recoveries
• GC-MS analysis of the derivatized acid fraction always
resulted in a broad, late-eluting range of unresolved
components generally attributable to oligomeric
humic materials
« GC injections of this fraction always resulted in a
significant amount of a dark brown residue of pyrolized,
nonvolatile material in the quartz injector liner.
The effectiveness (greater than 90 percent at low pH) of XAD-2 resin in
removing humic and fulvic acids from dilute aqueous solution has been
demonstrated by Mantoura and Riley who show this resin to have a capacity
exceeding 20 mg/gm before the onset of recovery degradation (9).
Detection of Special Interest Compounds
The numbers of "Special Compounds" shown for the concentrates in Tables
7 and 8 roughly correlate with the total number of compounds detected, as
might be expected. One-half to two-thirds of the detections enumerated under
the "Specific Search" heading would not have occurred without the computerized
GC-MS data searching which was developed for this work and is described in
Section 5 and Appendix A. "Specific Search" detection instances in Tables 9 and
10 with RS values 1.0 or less generally were not detectable without the use of
this special GC-MS data searching software. Note that many of the compounds
48
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on the "Specific Search" list (these 53 compounds are listed in Table 4) are
also members of the other two lists that are tabulated. Thus, there is appre-
ciable redundancy in the numbers shown in these three columns in Tables 7 and 8,
Tables of Identified Compounds
Description of the Tables—
Identified compounds for the DW and AWT concentrates are listed in
Tables 9 and 10, respectively, and as a combined DW and AWT listing in
Table 11. These tables show in which concentrate each of the compounds were
identified by indicating the RS value for the GC-MS peak. The compounds are
arranged in decreasing order of the largest RS value found for each compound.
In addition, instances of detection which were judged to be attributable to
the blank are designated with an asterisk in these tables. The criteria used
to attribute detected compounds to the blank is described and discussed in
this section under "Screening Compound Identification Results for the RO
Process/Concentrate Production Blank".
Selection of Concentrates for Inclusion
in the Combined Results Tables—
The computer software which produced the combined concentrate report
tabulations (Tables 9 and 10 for DW and AWT, respectively) allowed the results
of a maximum of 18 concentrates to be displayed in one table. Since there
were only 16 AWT concentrates (Table 8) and 2 relevant blanks (concentrates
VIC and X1C), it was not necessary to omit any of the AWT concentrates from
that combined results table (Table 10). However, in the case of the DW
concentrates (Table 7), there are 15 concentrates and 5 relevant blanks
(concentrates VIC, V1X, T2B, X1C, and XIX). Thus, it was necessary to omit
two concentrates from the combined DW results (Table 9), and the Miami II XAD
and New Orleans II XAD concentrates (M2X and N2X, respectively. Table 7) were
omitted since these two concentrates were heavily contaminated by XAD-2 resin
bleed artifacts. For example, of the 204 neutral compounds identified in the
M2X concentrate, 133 (65 percent) were attributable as artifacts due to XAD-2
resin bleed, and the corresponding result for concentrate N2X was 90 of 181
neutral compounds (50 percent) attributable as XAD-2 resin artifacts. For
completeness, compound identification results for these two concentrates are
presented in Volume 2, Appendix A.
The computer software which produced the DW plus AWT combined concentrate
report tabulation (Table 11) allowed the results for a maximum of 27 concen-
trates to be displayed. With a total of 36 concentrates (16 AWT, 15 DW, and
5 "Blanks"; see Tables 7 and 8), it was necessary to exclude 9 of these
concentrates from Table 11:
• The two solvent blanks, X1C and XIX, were excluded
• The two contaminated XAD DW samples, M2X and N2X,
were excluded as for Table 9
• Concentrate L2M was chosed as representative of the
Lake Tahoe II samples, thereby excluding concentrates
L2P, L2N, and L2D (see Table 8)
49
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. Concentrate C1M and C1N were chosen as representative
of the Pomona I samples, thereby eliminating concentrate
C1P
• The B1M and BIN concentrate results were combined as a
new concentrate named B3C in the database.
Screening Compound Identification Results for the
RO Process/Concentrate Production Blank—
The method of data correction for artifacts introduced during concentrate
partitioning and sample analysis has been addressed in Section 5. In summary,
this procedure effectively eliminated the possibility of introduction of
concentrate partitioning artifacts into the computer-managed database.
Concentrate production from the sampled water was performed by other
laboratories under separate contracts (see Section 4) and, thus, monitoring
and characterization of artifacts due to concentrate production procedures
was not under Battelle's direction. Because of this circumstance and also
because the concentrates functioning as blanks for these processes were not
available at the beginning of the research program, screening of artifacts
due to the concentrate production process could not be performed prior to
introduction of compound identification results into the computer-managed
database. Thus, this blank screening has been performed manually after
computer processing of the compound identification analysis results.
The blank concentrates—To allow some degree of control against reporting
artifacts due to the concentrate production procedure, five concentrates were
analyzed as blanks:
. VIC: Poplarville I Composite Concentrate (Table 1)
• V1X: Poplarville I XAD Concentrate (Table 1)
. X1C: Composite solvent extract blank (Table 3A, Appendix A)
« XIX: XAD-2 resin elution blank using ethanol (Table 3A, Appendix A)
• T2B: XAD-2 resin elution blank using diethyl ether (Table 3A,
Appendix A).
Blank concentrate T2B corresponds as a simultaneous concentration production
blank to concentrate T1Y, the only concentrate produced by direct adsorption/
elution using XAD-2 resin (i.e., RO preconcentration was not used). Therefore,
T2B is the only blank concentrate which corresponds uniquely to a sampling
incident.
In screening the compound identification results for possible artifacts
due to the concentrate production methodology, criteria based on RS values of
GC-MS peaks, (described below) were applied to Tables 9 and 10. The blank
screening results obtained were added to Table 11.
Screening criteria for DW concentrates—XAD-2 resin bleed artifacts were
identified in the T1Y, T1X, T4X, P2X, 02X, and S2X concentrates based both on
the results of the T2B, V1X, and XIX blanks (shown in Table 9) and on experi-
ence with samples heavily contaminated with XAD-2 resin bleed artifacts.
50
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(See, for example, the analysis results for concentrate M2X in Volume 2,
Appendix A, Table 1A, and the discussion of the XAD-2 resin bleed artifact
problem in Volume 3.) The main criterion for designation of identified
compounds as XAD-2 artifacts was the compound class. The observed relative
concentrations of these XAD-2 resin artifacts were consistent with the usual
pattern. The absolute level of concentrate contamination, however, varied
widely among the XAD-2 concentrates.
The results from concentrates VIC, V1X, X1C, and XIX were used to screen
the compounds identified in the DW concentrates for artifacts attributable to
sources other than XAD-2 resin bleed. In this case, the RS value was the
main criterion used to judge whether a compound which was found in the blank
concentrates, VIC, V1X, X1C, and XIX, should be disregarded when found in one
of the DW concentrates. If, for a given compound, the RS value for detection
in the blank was exceeded by the RS value for detection in a sample concen-
trate by 2.0 or more units (i.e., a factor of 10 difference in relative size
of the GC-MS peak), then the sample concentrate detection was considered gen-
uine (i.e., not an artifact). Since levels of artifacts introduced by RO
processing and solvent and XAD-2 extraction of the RO brine might be expected
to be independent of the volume of water sampled, the RS values used for this
blank screening test should be those originally resulting from comparison of
the GC-MS peaks with the internal standard according to Table 5. The RS values
appearing in Table 9 were obtained by normalizing the original RS values
to the "standard" 1514-liter sample volume using Equation 3 of Section 5.
Thus, the RS values of Table 9 had to be converted before volume normalization
so that the 2.0 RS value increment criterion could be applied. Because RS
values span a logarithmic scale, this adjustment to the pre-normalized value
involved only adding an appropriate constant to the RS values in Table 9.
These constants were: VIC and V1X, 2.0; T4C and T4X, 1.1 (applied after the
correction noted in Table 9); M2C, 0.4; N2C, 1.3; P2C and P2X, 1.2; 02C and
02X, 1.1; S2C and S2X, 1.8. Since the water volume for TIC and T1X was about
the same as that taken as the "standard" volume, these two concentrates re-
quired no RS value adjustment before comparison to the blank RS values. In
addition, the blanks, X1C, XIX, and T1Y, were considered to correspond to the
"standard" 1514-liter sample; thus, no adjustment in RS values was made before
blank screening comparisons.
Screening criterion for AWT concentrates—All of the AWT concentrates
were prepared from approximately 400 gallons (1500 liters) which corresponds
to the "standard" volume to which RS values were normalized. Thus, adjustments
to RS values in Table 10 prior to application of the 2.0 RS value increment
criterion was required only for the VIC concentrate RS value (2.0).
Results of artifact screening—For the DW results (Table 9) , 119 compounds
detected had 238 detection instances for XAD-2 produced concentrates classi-
fied as artifacts due to XAD-2 resin bleed. In addition, another 68 compounds
detected in the 15 DW concentrates had 266 detection instances classified as
concentrate production artifacts from sources other than XAD-2 resin. Thus,
a total of 187 compounds with 504 detection instances have been designated
as artifacts in Table 9. Since none of the AWT concentrates were prepared
by XAD-2 extraction of the RO brine, only the compound identification results
51
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for the blank concentrates VIC and X1C were appropriate for screening artifacts
in AWT concentrate results, and 274 detection instances of 65 compounds in
Table 10 were thereby attributable to non-XAD-2 sources of" contamination.
The results of screening the compound identifications for artifacts
attributable to the concentrate production process should be considered
tentative. The absence of results for analysis of replicate blank concentrates
together with the unavailability of a definitive demonstration of the appro-
priateness of the blanks that were analyzed and reported here prevent assign-
ment of high levels of confidence in some of the listings of Tables 9, 10,
and 11. Indeed, compounds listed in these tables which were detected both at
very low levels (generally at RS values of less than 2.0) and in isolated
instances (i.e., detection occurred in only one or two concentrates) should
be regarded as more tentative than others.
Some considerations which should have a bearing on the interpretation of
the results of artifact screening in Tables 9, 10, and 11, include the
following:
• Except for the XAD-2 artifacts, screening of most
compounds was due to detection in concentrate VIC.
Since this concentrate (as well as concentrate V1X)
corresponds to a sampling of an extremely large volume
of DW, many of the compounds detected and assumed to
be artifacts may have been present in the water.
Examples include the compounds pentachlorophenol,
2,4,6-trichlorophenol, p-cresol, 2,4,6-trichloroaniline,
tributyl phosphate, benzthiazole, 2,6-di-t-butyl-p-
benzoquinone, and dehydroabietic acid.
. There are many compounds in Tables 9, 10, and 11 for
which the RS value criterion resulted in the classification
of numerous, but not all, identifications as artifacts.
For those compounds with RS values large enough not to
be classified as an artifact, it is possible that the
compound was actually present as an artifact at a higher
than usual level. Of course, the greater the ratio for
a given compound of detection instances classified as
artifacts to those not so classified, the greater the
probability may be that more of the detection instances
should have been classified as artifacts.
« It is possible that all artifacts due to concentrate
preparation were not detected in the five blank concen-
trates. Thus, compounds with molecular functionality
closely related to a class of compounds generally designated
as artifactual may also be artifacts. This possibility is
particularly noteworthy in the case of fatty acids, fatty
alcohols, and common plastizers, especially diesders of
phthalic and alkanedioic acids.
• Most of the compounds detected in the blank concentrates
(except for the XAD-2 artifacts and those clearly related
to extraction solvent impurities) are ubiquitous in the
52
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environment and, thus, even though detected in a blank
concentrate, there remains a reasonable probability that
these compounds were indeed present in the DW and AWT water
samples. Again, fatty acids, fatty alcohols, and plasticizers,
as well as polyglycol ethers, are primary chemical classifica-
tions for this consideration.
Use of the Molecular Weight Table
In order to determine whether a given compound was found in any of the
DW and AWT concentrates, it was necessary to produce a listing of the
identified compounds, ordered by molecular weight, which was correlated with
Tables 9 and 10. The required listing is presented in Appendix D of this
volume, and the structure and use of this listing and the significance of
listed compounds which are not indicated as having been found in any of the
concentrates are also discussed here.
Additional Listings of Compound Identification Results
Volume 2 contains the complete set of computer-printed tables for DW and
AWT concentrates. Tables 9, 10, and 11 of Volume 1 which list the identified
compounds for DW concentrates, AWT concentrates, and 24 selected DW and AWT
concentrates, respectively, are, individually, the first parts of three-part
tables. The second and third parts of these tables containing information
not discussed in Volume 1 appear only in Volume 2. Four of the twelve
available tables summarizing occurrences of functional groups appear in
Volume 1. The computer-printed tables which appear in Volume 1 are also
presented in Volume 2 in order to present the complete set of results in that
Volume. The additional information provided by the complete set of listings
is the following:
1. Identification status (confirmed or tentative) for all
compounds identified in concentrates
2. Systematic names, molecular formulas and molecular
weights of all identified compounds
3. Functional group information for each concentrate
showing the total relative size values for each
functional group on each of the two GC columns
(SP1000 and SP2100).
The reader is referred to Appendix F which contains the Table of Contents and
List of Tables for both Volume 2 and Volume 3.
Number of Identified Compounds
Tables 9, 10, and 11 list the following numbers of unique organic
compounds:
Table 9-13 DW concentrates: 1091 compounds
Table 10 - 16 AWT concentrates: 991 compounds
Table 11 - 24 DW and AWT concentrates: 1423 comoounds.
53
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Compounds that were detected in one or more of the blank concentrates (VIC,
V1X, X1C, XIX, and T2B) but not in any other concentrate are not included in
the above totals; there are 87, 25, and 49 of these compounds in"Tables 9,
10 and 11, respectively. Compounds for which more than half of the entries
in a given table are attributed to the blank are also not included in these
totals; 138, 58, and 143 such compounds were found in Tables 9, 10, and 11,
respectively. Tentatively identified compounds which appear in these three
tables that were later confirmed to be absent have a line drawn through them
to indicate that status. There are 21, 32, and 26 such corrections in Tables
9, 10, and 11, respectively.
Results of Analysis of Blank Concentrates
The Poplarville, Mississippi DW concentrates, VIC and V1X, resulted in
the largest numbers of compounds among the 5 concentrates analyzed that
served as blanks. These two concentrates were prepared from the same RO brine
with the VIC concentrate being produced by solvent extraction of the RO brine
and the V1X concentrate being produced by re-extraction of this same RO brine
using XAD-2 resin, as per Table 1 and the discussion in Section 4, Concentrate
Production. The results of the V1X concentrate provided only additional data
on the nature of XAD-2 resin bleed artifacts since 133 of the 158 compounds
identified (84 percent) qualify as such. Of the 55 largest GC peaks (RS values
3.0 or greater) for both of these concentrates, 52 were found exclusively in
V1X, and all but two of those 52 compounds, which were both phthalates, were
XAD-2 resin bleed artifacts. Except for the small volume samples associated
with Jefferson Parrish (Volume 3) , the V1X concentrate was the most heavily
contaminated by XAD-2 resin bleed materials of all the concentrates analyzed.
Only 9 of the 208 different compounds were identified in both the VIC and V1X
concentrates. This surprising agreement disparity between the results of
these two concentrates is probably the result of both the dominance of the
XAD-2 resin artifacts in concentrate V1X and the extremely low level of
organic contamination of the water. For example, only two compounds of
concentrate VIC have RS values greater than 2.0, none have RS values greater
than 3.0, and 60 percent of the identifications have RS values of 0.0 or -1.0.
Only 59 compounds were identified in concentrate VIC. The predominant species
in concentrate VIC were fatty acids (9 compounds), fatty acid methyl esters
(9 compounds), plasticizers (6 phthalates and 1 adipate), resin acids (3
compounds), and alcohols (8 compounds).
Blank concentrates X1C and XIX were intended to reveal artifacts other
than those associated with the RO apparatus. Concentrate X1C was a com-
posite of K-D distilled solvent of the type used for RO brine extraction
while XIX was K-D distilled ethanol which had been used to elute a blank
column containing XAD-2 resin. Only 50 compounds were identified in
concentrate X1C, and, as expected, these compounds were predominantly
solvents: chloroalkanes, alcohols, and ketones. Phthalates and other
plasticizers were identified at lower levels, and fewer were found than for
other concentrates. However, fatty acids (8 compounds) were identified with
RS values in the 2.0 to 5.0 range.
54
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Similarly to concentrate V1X, the XIX concentrate predominantly contained
species ascribable as XAD-2 resin bleed artifacts (about 30 of 58 compounds).
In contrast, however, these artifacts were found at substantially lower
concentration for concentrate XIX than for concentrate V1X, above. Only nine
compounds were found with RS values greater than 3 and only two of these
compounds had RS values of 4.2. Aside from the XAD-2 artifacts, the predomi-
nant species were fatty acids, aleohols, and ethyl esters (presumably produced
by reaction with the ethanol solvent) and ketones.
Concentrate T2B was the only blank concentrate which was processed as a
blank for a specific concentrate, corresponding to concentrate T1Y. Concen-
trate T2B was a blank elution of XAD-2 resin using diethyl ether eluent. The
T2B concentrate contained .few organic compounds and most of the identified
compounds are expected for an XAD-2 resin elution. Only 13 of the 99
identified compounds had RS values greater than 3.0. Moreover, 56 of the
130 identifications in the eight fraction analyses were assigned the RS value
of 1; however, many of these peaks were actually smaller than this size range.
Most of the aromatic or partially reduced aromatic materials identified are
probably XAD-2 resin bleed artifacts. All of these artifacts, however, have
very low RS values of 2 or 1. In addition, only 21 of the 99 compounds shown
in Table 9 for T2B have been classified as XAD-2 resin bleed artifacts. The
T2B concentrate contained the lowest levels of XAD-2 resin bleed artifacts of
the XAD concentrates that were analyzed. High levels of benzoic acid and
methyl benzoate (RS values 5.0 and 7.0, respectively) were found. While
benzoic acid was often found at relatively high levels in XAD concentrates,
the concentrations did not correlate with the much more predominant artifacts,
the alkyl and alkenyl arenes. In addition, benzoic acid was always found in
the corresponding solvent extract concentrate. In contrast, methyl benzoate
was identified only in concentrate T1Y (for which T2B is the process blank).
High levels of these two compounds in T2B is, therefore, considered to be an
isolated instance. Predominantly, the non-XAD artifact compounds included
alcohols, ketones, fatty acids, esters (both alkyl and aryl, mostly methyl),
and diester plasticizers.
DISCUSSION OF DW CONCENTRATE ANALYSIS RESULTS
Summaries of the Results for Each Sampling
Poplarville, Mississippi, March 2, 1979—
The analysis results for the two Poplarville concentrates, VIC and V1X,
which function as concentrate production method blanks in this work but,
nevertheless, were prepared from finished DW are presented in this section
under Results of Analysis of Blank Concentrates.
Cincinnati, Ohio, October 17, 1978—
TIC: combined solvent extract of RO brine—There are three main features
of the TIC concentrate results that distinguish this DW concentrate from all
the others:
55
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1. Sixteen species of alkylated pyridines were identified in
the fraction containing the extracted bases. Most of
these compounds were found at moderately low concentrations
(RS values I'.O to 3.0). Compounds of this functionality
have rarely been identified in DW concentrates from other
samplings.
2. Dichloroaniline, trichloroaniline, and tetrachloroaniline
were identified in the aromatic fraction. Compared to
the other constituents in this fraction, the amount of
dichloroaniline (RS value 3) was surprising. Chloroanilines
were not often encountered in other concentrates at levels
this high. Both 2-chloroaniline and pentachloroaniline
are compounds "for which the data were specifically searched
(Table 4). However, neither of those two members of the
chloroaniline series were detectable by specific search of
the TIC concentrate data.
3. Relatively high levels of chloroalkanes and chloroalkenes were
identified in the aromatic fraction. In particular, the
1,2,3-trichloropropane component was present at high
concentration (RS value 6.0). Usually, aromatic materials
constitute the bulk of the identified compounds in this
fraction. However, in the case of concentrate TIC, C3
halo-hydrocarbons and haloforms are the principal constituents.
In addition to this very large component, 1,1,2-trichloropropane,
1,1,2-trichloropropene, 1,1,3-trichloropropene, two isomers of
bromodichlofopropane, bromoform, dibromochloromethane, and
bromodichloromethane were also identified. All of these halo-
hydrocarbons should have been predominantly in the alkane
fraction which was not analyzed by GC-MS. Indeed, the
residue weight results suggests that the presence of these
compounds in the aromatic fraction is overlap from unusually
high levels in the alkane fraction, since the alkane fraction
contained about eight times as much material as the aromatic
fraction. For most DW and AWT concentrates, the alkane
fraction contained less or a comparable amount of material
compared to the aromatic fraction. Thirteen of seventeen
compounds (76 percent) identified in the aromatic fraction
contained halogen. The most probable conclusion is that
either the sampled DW was unusually contaminated with
halogenated solvents or that the solvent used to extract
the RO brine was contaminated with these halogenated materials.
The compounds identified in the derivatized acid fraction were not
surprising. Fatty acids from C$ to C^ were present at high relative
amounts with a significant absence of unsaturated members of the series.
Methylethylmaleic acid and dimethylmaleic acid were among the largest peaks.
Salicylic, clofibric, and benzoic acids were detected as expected water
re-use indicators. The aromatic acids detected include a number of alkylated
benzoic acids, phenylacetic acids, and phenoxyacetic acids (including 2,4-D
and 2,4,5-T). The presence of 2-aminobenzoic acid and 3,6-dichloro-2-
methoxybenzoic acid (the herbacide, dicamba) may be noteworthy. The dichloro-
acetic, trichloropropenoic, and dichlorobutenoic acids detected may indicate
56
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the presence of other polychloro carboxylic acids which are not recovered
due to high acidity (I.e., trichloroacetic acid). The only phenols identified
were three compounds which are on the specific search list: phenol, 4-chloro-
phenol, and pentachlorophenol.
The medium polarity fraction contained, in addition to the large number
of pyridine compounds noted above, the following nitrogen-containing species:
phenyl acrolein, a C6 amide, N-acetyl morpholine, phenyl acetonitrile,
nicotine, and five quinoline isomers.
One of the largest components of the high-polarity fraction was 1,3,5-
trimethyltriazine-2,4,6-trione (Trimethylisocyonurate), frequently detected
at moderately high levels in concentrates from DW with sources similar to
the Ohio River. A variety of ketones, alcohols, alcohol-ethers, phthalic
diesters and alkane-dioic diesters have been identified in the high polarity
fraction and are probably attributable to the RO process blank. N,N'-dimethyl
urea, triethyl phosphate, tributyl phosphate and N-acetyl morpholine (the
latter also identified in the medium polarity fraction) may be noteworthy
identifications in this fraction.
T1X; XAD-2 extract of RO brine—A smaller portion, 4 percent instead of
10 percent, of the total T1X concentrate was partitioned into fractions for
GC-MS analysis; thus, all potential detection limits for this analysis were
higher by a factor of 2.5. In agreement with the Project Officer, it was
judged not cost effective to repeat analysis on this sample. Inspection of
the GC-MS chromatograms of the fractions revealed excellent signal to noise
with regard to detection of the internal standards. Thus, the relatively
smaller number of identifications for concentrate T1X compared to concentrate
TIC (66 versus 140, respectively) are ascribable to the nature of the sample
rather than to the amount of concentrate which was analyzed. RS values of
identified components were adjusted to account for this factor of 2.5.
Comparison of the identification results for concentrates TIC and T1X
clearly indicates that the solvent extraction of the RO brine (TIC) which
preceded the XAD extraction of that same RO brine (T1X) was very effective
in removing most of the less polar components. This conclusion is easily
verified by comparing RS values of compounds found in both concentrates
(Table 9). Generally, only the alcohols, ketones, and acids are reported in
concentrate T1X with RS values as high or higher than the corresponding values
for TIC. Furthermore, Table 7 indicates that only 12 percent of the concen-
:trate was recovered into fractions and that more than 90 percent of that
recovered material was in the acid fraction. Thus, concentrate T1X consisted
principally of humic-related materials which were not solvent extractable
from the RO brine.
The acid fraction contained some interesting chlorinated acids: 2,4-
dichlorobenzoic acid, tetrachloroterephthalic acid (probably from the pre-
emergence herbicide, chlorthal-dimethyl which has a half-life towards
hydrolysis to the free acid of 100 days in soil), trichloropropenoic acid,
dichloroacetic acid, 2,2-dichloropropanoic acid (the herbicide, dalapon) and
2,2-dichlorobutanoic acid. Identification of N-hydroxyphthalimide, a hydroxamic
acid, may be noteworthy. Benzoic acid and methylethylmaleic acid were the
57
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largest components of the acid fraction. However, results from the blank
T1Y, indicate most of the benzoic acid is probably an artifact. The o-ften
encountered salicylic, benfceneacetic, phthalic, and dimethylmaleic acids
were also identified in the acid fraction.
Concentrate T1X had distinctly fewer aromatic organic compounds than
the other DW concentrates. No residue weight was detected after correction
for the blank, and 3 of the 4 compounds found (naphthalene, 2-methylnaphthalene
and phenanthrene) may be attributable as XAD-2 resin bleed artifacts. Few
noteworthy compounds were detected in the other two fractions (medium and
high polarity). This result is consistent for the very low relative recov-
eries shown in Table 7. Phenol (possibly an XAD-2 artifact in this case),
isophorone and the relatively high polarity compounds, benzaldehyde (at
least partially attributable to XAD-2 resin bleed) and nicotine may be of
some interest.
T1Y; direct XAD-2 extraction with diethyl ether elution—Concentrate
T1Y is unique among all the concentrates analyzed since it is the only one
produced without any use of RO pre-concentration. This concentrate contained
an unusual set of industrially-related organic compounds of which many were
halogen substituted. Of the 211 compounds identified (Table 7), 87 (41 per-
cent) contained one or more halogen atoms. For the aromatic fraction, the
percent of halogen containing compounds is 84 percent with 18 percent of the
identifications containing one or more bromine atoms. Chlorine and bromine
were the only halogen substituents found. The total of 17 specific search
compounds found in the T1Y data are listed in Table 17. This concentrate
contains the highest number of identifications of specific search compounds
of the DW concentrates and is exceeded by only one of the AWT concentrates
(Tables 7 and 8). Moreover, of these 17 specific search compounds, 12 (71
percent), contained chlorine. The number of- identified compounds (24) on
the "Chemical Indicators of Industrial Pollution" list was the highest
number identified in any concentrate. In addition, the number (13) of
Consent Decree compounds was equalled only by concentrate T4C and exceeded
only by concentrate N2C (15 compounds) . A further indication of the high
levels of halogenated compounds was that 140 (64 percent) of the unidentified
mass spectra of GC-MS peaks showed the presence of one or more halogen atoms,
and 53 percent of these unidentified mass spectra were from components in the
aromatic fraction.
The level of contamination of the source water by haloforms and halogen-
ated industrial solvents is actually greater than indicated by the results
in Table 9. Analysis of the unpartitioned concentrate showed that the
dominant constituents of the concentrate were CH2ClBr, CHCl2Br, CHClBr2,
bromo and chloro ethers, and other halo-hydrocarbons. These compounds would
be predominantly recovered in the alkane fraction which was not analyzed by
GC-MS, and detection in the aromatic fraction is due to overlap between
these two silica gel elutions. Another observation for which concentrate
T1Y was unique among the DW and AWT concentrates was a very pronounced late
eluting range of poorly separated sample components in the high polarity
fraction.
58
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Another observation which distinguished the partitioned fractions of
concentrate T1Y from most of the others analyzed is the absence of sample
components which are present at significantly higher concentration than the
majority of the other sample components. None of the GC-MS chroma to grains for
the partitioned fractions showed this often observed "tree stump" effect. In
fact, the number of sample components and their relative concentrations were
distributed among the various fractions in an almost optimal fashion for the
analytical scheme. As noted above, however, there were "tree stump" compo-
nents in the GC-MS chromatograms of the unpartitioned concentrate. These
dominant components partitioned into the alkane fraction which was not
analyzed by GC-MS.
The broad range of interesting and possibly significant compounds
identified in concentrate T1Y is too lengthy to list as individual species.
The following is a short summary of the more interesting types of compounds
found:
• Phenols - 6 halophenols plus phenols
• Acids - chloro C2, C-$, and C^; numerous chlorobenzoic acids
• Herbicides and pesticides - 2,4,5-T, tetrachloroterephthalic
(indicator of chl or thai-dime thyl ), lindane and 2,4-D methyl
and ethyl esters
• Halo/nitro aromatics - 18 halobenzenes and naphthalenes,
4 nitro benzenes, 4 chloro nitro benzenes, 3 chloro anilines,
and PCEs (Cl and
• Re-use indicators - clofibric acid, salicylic acid
• Other halo compounds - 5 chloro butenes and butadienes
(including hexachloro) , tetrachloropropane, 3 halo ethers.
Concentrate T1Y contained few XAD-2 resin bleed artifacts with only 21 of
243 identified compounds classified as such. This result is consistent with
those for concentrates T1Y and T1X which used the same batch of carefully
prepared XAD-2 resin.
Comparison of concentrates TIC, T1X, and T1Y — The water from which these
three concentrates were derived was drinking water obtained during the period
of October 16, 17 and 18, 1978. The water was sampled directly from a tap at
the US EPA/HERL Laboratory in Cincinnati, Ohio. The sampled water was split
into two streams of equal flow with each stream contributing a 1460-liter
(387-gallon) sample. One stream was acidified to pH 2 with a metered flow
of 6 N hydrochloric acid and immediately passed through an XAD-2 column. Sub-
sequent elution with diethyl ether followed by volume reduction produced the
T1Y concentrate. The other stream was used to fill a reservoir for the RO
apparatus. Treatment of the RO brine by solvent extraction produced the TIC
concentrate, while subsequent XAD-2 extraction of the RO brine produced the
T1X concentrate (see Appendix E) . Corrections in Table 9 for compounds which
may have originated from the concentrate production method and which are based
on the blank concentrates VIC, V1X, X1C, and XIX may be less valid for these
three Cincinnati concentrates than for the other DW and AWT concentrates. Note,
59
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however, that blank T2B does correspond directly to concentrates T1X and T1Y
with respect to artifacts due to the XAD-2 resin.
Focusing on a comparison of the residue weight results and compound
identification results in Table 7 for concentrate T1Y and the composited
values for concentrates TIC and T1X (hereafter referred to as T1C/T1X)
reveals some interesting observations. If the process of reverse osmosis
followed by solvent and then XAD-2 extraction of the RO brines (used for TIC
and T1X) recovered organic materials equivalently to the process of direct
XAD-2 adsorption/diethyl ether elution (used for T1Y), then the values for
residue weight analysis in Table 9 ought to be comparable for T1Y and the com-
posite T1C/T1X. Indeed, the amounts of material in the concentrates (expressed
as "Concentration, yg/1") are essentially identical, at 540 and 527 yg/1 for
T1C/T1X and T1Y, respectively. However, comparison of the distribution of
material in the recovered fractions (Table 7) and the numbers and identities
of the identified compounds (Tables 7 and 9, respectively) shows substantial
differences between T1Y and T1C/T1X.
Overall, the organic material of T1Y was recovered nearly twice as
effectively through the partitioning scheme (Figure 4) as that of T1C/T1X
(41 percent versus 23 percent, respectively). Enhancement (expressed as a
percentage increase above T1C/T1X for T1Y) of recovery of concentrate material
into the partitioned fractions was seen for all except the alkane fraction:
acid, 35 percent; alkane, -22 percent (not shown in Table 7); aromatic,
M.800 percent (not calculable from Table 7, due to rounding); medium polarity,
130 percent; high polarity, 190 percent. In addition, T1X concentrate was a
distinctly darker brown color than the T1Y concentrate. Optical densities
were not measured, but if one assumes the brown color to be due principally
to humic-related material in both concentrates, then T1X probably contained
more than T1Y by a factor of 2 to 5.
There were more organic compounds identified in T1Y than in T1C/T1X.
Enumeration of the listings of Table 9 shows that 154 compounds were identi-
fied in T1Y but not in T1C/T1X. Thus, only 55 of the 211 compounds (26 per-
cent) identified in T1Y were also detected in T1C/T1X. There were 117
compounds identified in T1C/T1X but not in T1Y. For some of these compounds,
a chemical explanation is readily apparent. The large number of nitrogen
bases (23 compounds, mostly alkylated pyridines and quinolines or related
species) detected in TIC and noted in the discussion above for that concen-
trate, undoubtedly were unretained by the XAD-2 resin since at pH 2 these
compounds would be in the form of the ionic conjugate acids. Of the 97
other compounds detected in T1C/T1X but not T1Y, 80 (81 percent) had
molecular functionality which would enhance water solubility and, thus,
decrease recovery effectiveness by XAD-2 resin: 33 compounds were alcohols
or poly glycol ether/alcohols; 16 compounds were low'molecular weight ketones;
11 compounds were fatty or aromatic carboxylic acids; 12 compounds were
relatively strong acids (chloro, ketq, or hydroxy substituted or dicarboxylic);
and 8 neutral compounds had exceptional polarity (i.e., amides, ureas, polar
substituted esters or low molecular weight diesters). Only 17 of the 109
compounds do not have a polar molecular functionality reason for poor recovery
by XAD—2, and 9 of these compounds may actually be RO process artifacts (3
plasticizers and 6 possible solvent impurity species).
60
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Many of the 154 compounds identified in concentrate T1Y but not in TIC/
T1X can be classified as the most hydrophobic/lipophilic materials among
those identified. There are few acids and alcohols among this list (chloro-
benzoic acids and halo phenols are exceptions). Most of the 154 compounds
are low polarity aromatic compounds or have moderate polarity such as fatty
acid methyl esters and ethers. Reinforcing these observations is the result
that, for polar or moderately polar compounds found in both T1Y and T1C/T1X,
the RS values for detection in T1Y are less (sometimes substantially) than
those for detection in T1C/T1X. Moreover, the opposite is often true for
polar compounds detected in both T1Y and T1C/T1X. Many of the compounds
which are exception to the above observation are attributable as concentrate
production method artifacts.
Since this set of concentrates are the only ones for which direct
comparison of RO-based concentration technique (T1C/T1X) can be compared
with the direct adsorption/elution technique (T1Y), it is not possible to
propose a definitive explanation for the results. However, the following
seems to be consistent with both the observations and chemical expectations:
• Poor recovery of small and moderate sized apolar species
(i.e., substituted benzenes) is due to permeation by
these species of the RO membranes. In aqueous solution,
these molecules exist as non-solvated species in a hydro-
phobic "shell" so that their sizes are not enlarged above
the molecular size by a tightly associated solvation
sphere. Thus, diffusion of these materials into membrane
pores requires no de-solvation energy, and, indeed, this
process is thermodynamically driven by the "hydrophobic
energy" released when water molecules in the solvent shell
become fully solvated in the bulk solvent. Of course, this
thermodynamic driving force would have to be repaid for the
hydrophobic species to appear in the permeate water, but
only after the membrane capacity for these apolar materials
was exceeded, and that point may often not be reached for
DW samples. XAD-2 resin would, of course, have very high
capacities for these apolar species.
• Highly polar, especially oxygen and nitrogen containing
species, and/or ionized species would have a substantially
larger size in aqueous solution than their actual molecular
sizes due to tightly bound, multiple layered solvation
spheres. Thus, these species should be retained well by the
RO membranes, and the nonionic and ionization suppressable
species can, of course, be recovered by solvent extraction
or XAD-2 extraction of the RO brines. In contrast, due to
the enhanced water solubility of these polar materials, they
would not be retained as well by the XAD-2 resin as more
apolar species.
. Macromolecular hydrophilic materials such as humic-related
substances and poly glycols would be very effectively
retained by the RO membranes. Solvent extraction of the
RO brines effectively recovers the poly glycols but not the
61
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humic-related materials. However, as pointed out above, the
analysis results definitely indicate that the humic-related
material is recovered better by XAD-2 extraction of the RO
brine than by XAD-2 extraction of the water directly. Since
the volume of the RO brine was about 0.05 percent of the
starting water (see Appendix E), the k1 values for the humic-
related material may not be exceeded in XAD-2 resin extraction
of RO brine (approximately 4 bed volumes of RO brine passed
through the column) whereas they may be considerably exceeded
in the direct XAD-2 extraction (approximately 8000 bed volumes
passed through the column).
The essentially equal recoveries into T1Y and T1C/T1X from
the starting water (Table 7) is apparently coincidental:
the recovery losses of the direct XAD-2 resin adsorption
technique for the more water soluble materials including
humic-related substances are approximately equal to the
recovery losses of the RO membrane for apolar materials.
In summary, the results definitely indicate that direct XAD-2 extraction
of DW is superior to RO pre-concentration methods when the target compounds
are relatively apolar organic materials of the type usually encountered as
organic industrial effluents. The opposite is true for strong acids, alcohols,
humic-related material and other highly water soluble and/or macromolecular
organic materials.
Cincinnati, Ohio, January 14, 1980—•
T4C; combined solvent extract of RO brine—Residue weight analysis of
concentrate T4C (Table 7) yielded a value of 115 ug/1 as the concentration
in the original water which the organic material recovered into this concen-
trate represents. This value is lower than corresponding values for all
other DW concentrates except for Seattle, Washington (37 ug/1) and Poplarville,
Mississippi (0.6 yg/1) which serves as the blank in this work. For comparison,
the prior sampling (October 17, 1978) of Cincinnati DW gave a solvent extract
of RO brine concentrate representing 143 vg/1 of organic material in the
original water (Table 7).
Only 36 percent of the original concentrate material was recovered in
the analyzed fractions, and 71 percent of this recovered material was in the
acid fraction. This low overall recovery (of all DW solvent extract concen-
trates, only that for Poplarville was lower) and relatively high percentage
of recovered acids is indicative of humic-related species as the predominant-
organic material present. This indication is confirmed by the presence of
the usual range of unresolved GC-MS peaks in the chromatograms of the unpar-
titioned concentrate and the acid fraction.
Although the acid fraction contained substantially more material than
any other analyzed fraction, there was no highly dominant set of compounds
in this fraction or any other fractions as is often the case for phthalates,
polyglycols or fatty acids. DimethyImaleic acid and ethylmethylmaleic acid
were among the components present in the highest concentrations in the acid
62
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fraction. However, RS values for thses two compounds were about average as
compared to other DW concentrates (entries 14 and 7, Table 9, respectively).
In addition, about as many aliphatic and unsaturated carboxylic acids were
present as phenyl substituted carboxylic acids, with the aromatic species
at slightly lower concentrations.
There were nine specific search compounds identified in the acid
fraction (concentration, ng/1, shown in parentheses): 4-chlorophenol (46),
2,4-D (44), 2,4,6-trichlorophenol (31), phenol (18), 2,4,5-T (4.7), 4-methyl-
phenol (3.0), 2,4-dimethylphenol (2.8), pentachlorophenol (2.6), and 2,4-
dichlorophenol (2.5). These nine acidic compounds were found with higher RS
values than all of the non-acidic specific search compounds found (concentra-
tion, ug/1, shown in parentheses): nitrobenzene (3.3), 2-chloroaniline (1.6),
2-chlorotoluene (1.6), styrene (0.8), 1,4-dichlorobenzene (0.4), 2-methyl-
styrene (0.1), and fluoranthene (0.1). These sixteen specific search
compounds were second in number only to concentrate T1Y among the DW
concentrates.
The usual water reuse indicators have also been found: clofibric acid,
salicylic acid and caffeine at comparatively high concentrations and nicotine
at substantially lower concentration. A number of phenolic antioxidants,
probably originating as food preservatives, were also identified.
A few compounds which may be indicative of contamination from industrial
sources are noteworthy: pyridine and five alkyl pyridine isomers; N,N-
dimethyltoluyl amine; dimethylformamide; nitrobenzene, nitrotoluene and
dinitrotoluene; three orgahophosphates (triethyl, tributyl and tris-2-
chloroethyl); a variety of chlorinated propanes, propenes, ethanes, and
ethylenes; and 2-chloroaniline, 2,4-dichloroaniline and 2,4,6-trichloroaniline.
Also found at relatively high concentration was l,3,5-trimethyl-l,3,5-triazine-
2,4,6-trione (trimethylcyanurate). This compound (entry 53, Table 9)'was
identified in three other DW concentrates: TIC and T1Y (Cincinnati) and N2C
(New Orleans). It has also been identified in a number of the Cincinnati
small-volume samples described in Volume 3.
T4X; XAD-2 resin extract of RO brine—Concentrate T4X contained XAD-2
resin bleed artifacts in amounts which, relative to the other XAD-type
concentrates analyzed, can be described as moderately high. Of the 181
compounds listed for T4X in Table 9, 56 have been classified as XAD-2 resin
bleed artifacts and 12 have been attributed as concentrate production
artifacts from other sources. Thus, the net number of identifications for
this concentrate is 113. The lower overall recovery of material into the
analyzed fractions, as compared to the solvent extracted concentrate, T4C,
is consistent with similar results for the other pairs of DW concentrates
(Table 7).
Of the 48 compounds identified in the aromatic fraction, only 2 have not
been classified as XAD-2 artifacts. Undoubtedly, the high XAD-2 artifact
background prevented identification of some apolar species present at low
concentrations. Most of the apolar compounds in the RO brine should have
been recovered in the solvent extract concentrate, T4C, and, thus, little
information was lost due to the XAD-2 artifact interference.
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The acid fraction contained a distribution of fatty and aromatic
carboxylic acids plus a relatively large number of strong acids (dicarboxylics
and chloro or keto substituted). Water reuse indicators in the acid fraction
included salicylic acid, saccharin, and ethosuximide. The herbicide, dicamba
and tetrachloroterephthalic acid (degradation product of the herbicide
chlorthai-dimethyl), were also detected. Phenol, p-cresol and 2,4-dimethyl-
phenol were the only phenolics found, and the latter two were at very low
concentrations.
Noteworthy compounds found in the medium polarity fraction include the
following nitrogen containing compounds: pyridine, aniline, 2-chloroaniline,
dichloroaniline, diphenylamine, benzylamine, N,N-dimethylbenzylamine, caffeine,
nicotine, N-methyl-y-butyrolactam, and diethylformamide.
The methanol silica gel eluate, Fraction 7, contained poly glycol
materials as the predominant species. Three homologous series of these
compounds were identified as the major constituents of the fraction. Note-
worthy compounds identified included DMF, caffeine, acetanilide, 3-acetyl-
aniline, N-methyl-Y-butyrolactam and isophorone.
Comparison of concentrates T4C and T4X—The T4C and T4X concentrates
were prepared from about 7,570 liters C2000 gallons) of finished drinking
water. The organic material was pre-concentrated by reverse osmosis (RO)
using cellulose acetate and DuPont Permasep® nylon hollow fiber RO units as
described in Section 4. The water was sampled at the Cincinnati, Ohio
waterworks on January 14, 1980, and was taken from the process stream at a
point just prior to treatment by contact with a one million gallon per day
granular activated carbon (GAG) unit. A number of relatively small volume
samples (corresponding to 10 to 30 liters) were taken at various stages of
the RO processing scheme. Analysis results for these 13 small volume
samples, associated with GAG contactor "A", are presented and discussed in
Volume 3. Although 7,570 liters of DW were RO processed by GSRI, 70 percent
instead of 100 percent of the RO brine produced was used by GSRI to generate
concentrates T4C and T4X. This information was not conveyed to Battelle
until analysis work was completed. Thus, the GC-MS analyzed portion of the
material recovered from the sampled DW was 7 percent rather than the usual
10 percent. The water volume shown in Table 7 for concentrates T4C and T4X
is 70 percent of that volume actually sampled since that is the volume of
water actually corresponding to the results obtained for these two concen-
trates.
As usual, the XAD-2 resin produced concentrate, T4X, contained consider-
ably more organic material than the composite solvent extraction concentrate,
T4C, with 745 ug/1 and 115 yg/1 for T4X and T4C, respectively. The material
left in the RO brine after extraction of the T4C concentrate was, as usual,
relatively more polar. Thus, the T4X concentrate was not as well recovered
into the partitioned fractions as the T4C concentrate: 23 percent for T4X
compared to 11 percent for T4C. The higher range of polarities expected in
the T4X concentrate also accounts for the greater portion of recovered
material that the acidic fraction represents: 91 percent for T4X versus
72 percent for T4C.
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It is also noteworthy, in comparing the T4C and T4X results, that fewer
specific search compounds were found in T4X (seven compounds) than in T4C
(sixteen compounds). Five of the seven specific search compounds found in
T4X were also found in T4C: phenol, 4-methylphenol, 2,4-dimethylphenol,
2-chloroaniline, and fluoranthene. In each case, the quantitative results
for the two concentrates agreed within a factor of three.
Comparing the acid fractions of concentrates T4C and T4X, the following
observations are noteworthy:
• T4X contains stronger acids. For example, dichloroacetic
acid, three chlorinated acrylic acid isomers, dichloro-
propionic acid and two isomers of dichlorocrotonic acid
were found only in concentrate T4X. In addition, three
dicarboxylic acids (phthalic, suberic and sebacic) were
found only in T4X while a fourth (azelaic) was found at
three to five times higher concentration in T4X than in
T4C.
• The strong acid herbicide 2-methoxy-3,6-dichlorobenzoic
acid (dicamba) and the degradation product of the herbicide
chlorthal-dimethyl, tetrachloroterephthalic acid (chlorthal)
were found in T4X. Chlorthal was not found in T4C, and
dicamba was found in both concentrates but at substantially
higher concentration (more than one order of magnitude) in
T4X than in T4C.
• Saccharin and ethosuximide, both relatively strong acids,
were found in T4X but not T4C.
• The phenoxy herbicides C2,4-D and 2,4,5-T), clofibric acid
and four chlorinated phenols were found in T4C but not T4X.
• Both concentrates contained about equal amounts of salicylic
acid and the usually encountered maleic acids.
• The T4X acid fraction chromatograms displayed a more distinct
chromatographic profile of humic material than the corresponding
T4C chromatograms. This result is consistent with all other
solvent extracted and XAD-2 extracted DW concentrate pairs
analyzed.
Miami, Florida, February 3, 1976—
M2C; combined solvent extract of RO brine—There are four main features
which distinguished concentrate M2C:
1. The concentrate contained a relatively higher portion of
humic-related materials than all of the other drinking
water concentrates prepared by solvent extraction of
RO brine.
2. There was a relatively large number of halogenated
hydrocarbons present.
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3. A number of sample components were present which clearly
must originate from waste waters (water re-use indicators).
4. Di-n-butylphthalate was.present at very high (and probably
anomalous) levels.
Very prominent in the RGCs of the methylated acid fraction of M2C concen-
trate was the typical large, broad profile of unresolved middle to late
eluting material which is characteristic of samples containing a high percent-
age of humic-related material. In addition, of the material recovered into
the five fractions, 77 percent was in the acid fraction. This predominance
of material in the acid fraction was not exceeded by any DW solvent extract
type concentrates. The Cincinnati (T4C) and Ottumwa (02C) concentrates were
second and third at 72 percent and 68 percent, respectively.
The aromatic fraction contained an unusually large amount of halpgenated
material with 65 percent of the compounds identified in this fraction contain-
ing halogen. Tetrachloroaniline, bromoform, dibromochloromethane, chloro-
cyclohexane, bromocyclohexane, and iodocyclohexane, five chlorinated benzenes
and 12 chlorinated hydrocarbons (C2 to GS) were identified in the aromatic
fraction.
In the acid fraction, amobarbital, pentobarbital, iclofibric acid and
salicylic acid have been identified. These materials probably arise from
wastewater sources since these compounds are all drugs or drug metabolites.
All of these materials were found at surprisingly high levels considering
the source of the Miami DW is groundwater.
It is readily apparent from the chromatograms of the unpartitioned
concentrate that di-n-butylphthalate is the predominant constituent of the
material in concentrate M2C. Based on the unpartitioned sample chromatograms,
this n-butylphthaiate component represented between 10 and 20 percent of the
total GC-MS peak area. Since much of the ion current under the dibutyl-
phthalate peaks probably saturated the signal electronics, the amount of this
compound may actually be greater. Since many underivatized acids and humic-
related materials undoubtedly did not elute in these unpartitioned chromato-
grams, it is not possible to approximate what percentage of the concentrate
this di-n-butylphthalate represents. Similar concentrations of di-n-butyl-
phthalate were observed in the Philadelphia and New Orleans solvent extract
concentrates (P2C and N2C). Since all three concentrates were prepared about
the same time (January 14, 1976 to February 3, 1976). the most reasonable
explanation for the high levels of butylphthalate is that some change in the
concentrate production procedure had occurred or contaminated extraction
solvent was used over that short period of time. In addition, the XAD-2
extracts of RO brine for these cities (M2X, N2X, and P2X) contained either
moderate amounts of dibutylphthalate or none at all. Thus, the artifact
was probably not introduced during RO processing, but rather at or after
the RO brine extraction sequence. There is no evidence to suggest that these
phthalate components are not artifacts since other plasticizers were not
present at even close to comparable levels.
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Six compounds on the specific search list were found: phenol, 2,4,6-
trichlorophenol, o-chlorotoluene, p-dichlorobenzene, 1,2,4-trichlorobenzene,
and fluoranthene (see Table 17). However, based on the RS values of the GC
peaks and occurrence in the blank, trichlorophenol and fluoranthene are
possibly attributable as concentrate production artifacts, as indicated in
Table 9.
M2X: XAD-2 extract of RO brine—As explained elsewhere, the M2X concen-
trate was excluded from Table 9 because of space limitations. The reason
M2X was chosen for omission was that it was badly contaminated with XAD-2
resin bleed artifacts. Of 204 non-acidic compounds identified in concentrate
M2X, 133 (65 percent) were XAD-2 resin bleed artifacts. In addition, 89 of
the 100 largest GC-MS peaks were identified as XAD-2 artifacts. Since the
M2X results were omitted from Table 9, they have been included in Appendix B
of Volume 2.
Although the XAD-2 artifacts dominated the chromatograms for concentrate
M2X, this material was not the predominant substance present. Most of this
artifact material was recovered in the aromatic fraction which accounted for
only 0.4 percent of the organic material present in the concentrate. In
agreement with all of the other XAD-2 produced DW concentrates, M2X consisted
of predominantly humic-related material which is not recovered well in the
partitioning scheme, and the humic material that is recovered appears pre-
dominantly in the acid fraction. For M2X, 88 percent of the material recov-
ered in the fractions was in the acid fraction.
Fluoranthene was the only specific search compound found and may be
attributable as an artifact (see discussion of M2C, above). Two isomers of
DDE, probably degradation products of DDT, were also identified in M2X.
Relatively large components of salicylic acid, dimethyImaleic acid and
methylethylmaleic acid were the only other noteworthy compounds found. All
four of these compounds were also identified in concentrate M2C. The majority
of the non-artifact compounds identified were a large variety of oxygenated
compounds (ketones, alcohols, ethers, furans, and furanones).
Comparison of concentrates M2C and M2X—The water from which the Miami
concentrates were prepared was a 2280-liter (600-gallon) sample of finished
drinking water taken at the Miami waterworks on February 3, 1976. Two
features of these two concentrates are in apparent contradiction to the fact
that the raw water source was groundwater:
• The finished DW apparently contained higher concentrations
of humic-related material than any other DW sampling
• A number of water re-use indicators (salicylic acid, clofibric
acid, amobarbital and pentabarbital) were identified.
Humic-related material results from degradation of the lignin substance
of plant debris, especially leaves. Thus, it is not surprising to find this
material in surface water. Generally, one would expect ground water to be
relatively free of these materials. The Miami XAD-2 extracted concentrate,
M2X, indicates that the sampled water contained a higher concentration of
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humic-related material (by factors ranging from 2.0 to 5.3) than the DW from
cities with surface water sources expected to contain humic material
(Cincinnati, Philadelphia, New Orleans, and Ottumwa). This result is under-
scored by the unusually high concentrations of humic-related material in the
solvent extraction produced concentrate, M2C. No other solvent extract type
concentrate approached the levels of humic-related materials that M2C con-
tained. Presumably, this anomaly was caused by an equilibrium displacement
effect of the very high levels of this material present in the RO brine
during solvent extraction. The relatively high concentration of humic-
related material in the sampled water obviously indicates that the DW source
groundwater aquifier is not well protected from direct surfacewater intrusion.
The detection of the two drugs (pentabarbital and amobarbital) and two drug
metabolites (salicylic acid and clofibric acid) support this contention that
the groundwater source is not protected from intrusion by contaminated surface-
water and add to it a suggestion that the aquifier is vulnerable to treated
or untreated sewage.
New Orleans, Louisiana, January 14, 1976—
N2C: combined solvent extract of RQ brine—The dominant species of
concentrate N2C was di-n-butylphthalate. This material was probably present
as a concentrate production artifact. The specific search compounds and
other high interest species detected in concentrate N2C require some comment.
The controversial herbicides, 2,4-D and 2,4,5-T, have been found in relatively
high, concentrations (54 and 11 tig/1, respectively). Only concentrate 02C
contained comparable concentrations of these two herbicides (entries 427 and
190, Table 9, for 2,4-D and 2,4,5-T, respectively). A 2,4,5-T isomer was
identified at about the same concentration (RS value 3.7), and an even higher
concentration (RS value 4.7) of a 2,4-D isomer was also detected. Although
not a specific search compound another herbicide, atrazine, has also been
detected at relatively high levels (RS value 5.7). Again, 02C was the only
other DW concentrate in which atrazine was found. The herbicide, dicamba,
was also identified at relatively high concentrations (RS value 4.7). In
addition, the pesticides heptachlor and lindane (two isomers) as well as DDE
(which may indicate the presence of DDT) were also found by the specific
search software. Other highly chlorinated specific search compounds found
were pentachlorophenol, 2,4-dichlorophenol, hexachlorobenzene, and hexa-
chlorobutadiene. Phenol, diphenylamine and triphenyl phosphate were the
other specific search compounds found. In all, twelve specific search
compounds were found in the N2C concentrate (see the discussion, Special
Interest Compounds, which appears later in this section). This concentrate
contained the third highest number of specific search compounds for DW con-
centrates. A number of water re-use indicators were identified in the N2C
data: clofibric acid, salicylic acid, caffeine, benzoic acid, and BHT.
In the acid fraction, 67 carboxylic acids, of which 44 were aliphatic,
were identified. This number of carboxylic acids is second only to concen-
trate S2C, and the total RS value in N2C for compounds containing the carbox-
ylic acid group is also the second highest among the DW concentrates, 8.5
versus 8.8 for M2C (see the discussion, Occurrence of Molecular Functional
Groups, which appears later in this section). The two maleic acids, dimethyl
and methyl ethyl, were dominant components in the acid fraction.
68
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Of 73 compounds, identified in the aromatic fraction, 30 contained at
least one halogen atom and 7 contained bromine. Except for chloroform, all
of the possible bromo chloro haloforms were detected. Halogenated hydro-
carbons (GI to Cit, 17 compounds) were present at higher concentrations than
the halogenated aromatics. Most of the other compounds identified were
alkyl substituted benzenes, naphthalenes and partially reduced naphthalenes.
Compounds and their relative amounts in the medium polarity and high
polarity fractions were not distinctly different from the other two solvent
extract concentrates with similar raw water sources (i.e., Philadelphia, P2C
and Cincinnati, TIC'and T4C). The identified compounds were mostly diester
plasticizers, alcohols and alcohol-polyethers, ketones and a few esters and
amides. Atrazine, three phosphate esters (triphenyl, tributyl (possibly an
artifact) and diethyl pentyl (tentatively identified)), and hexanedinitrile
were found in these two fractions.
N2X; XAD-2 resin extract of RO brine—Because of space limitations, the
results of two concentrates were omitted from Table 9. Concentrates N2X and
M2X were the ones omitted due to heavy contamination from XAD-2 resin bleed
materials. For completeness, the identified compounds for these two concen-
trates are presented in Appendix A of Volume 2. The level of contamination
of N2X was somewhat less than that for M2X, but it was so severe that the
aromatic fraction required dilution by a factor of 10 to avoid gross satura-
tion of ion current signals. Of 181 non-acidic compounds in concentrate N2X,
90 are XAD-2 resin bleed artifacts, and 71 of 76 compounds identified in the
aromatic fraction were artifacts.
The distribution of material among the fractions for concentrate N2X
(Table 7) was typical of XAD-2 extracted concentrates and is reflected by
the low overall recovery into the fractions (10 percent) and the predominance
of the acid fraction in the recovered material (90 percent).
The herbicides, 2,4-D, an isomer of 2,4-D, and dicamba were identified
in the acid fraction at comparable concentrations to those found in concen-
trate N2C. Somewhat surprisingly, 2,4,5-T and an isomer, found in N2C, were
not found in N2X. Other acids found in both N2C and N2X include 2 isomers
of dichlorobenzoic acid, p-chlorobenzoic acid, methylethylmaleic acid,
dimethylmaleic acid and salicylic acid. Three chlorinated acids, dichloro-
acetic, chlorobutenoic and dichlorobutenoic, were found in N2X but not in
N2C, in agreement with the usual trend that relatively stronger acids are
more effectively recovered in the XAD-2 extracted concentrate.
The only other noteworthy compounds found in concentrate N2X are
a-chloro-acetophenone (phenacyl chloride) which is a lacrimator used in tear
gas and chemical mace, bischloroethyl ether, BHT and two isomers of DDE (also
identified in N2C). Three specific search compounds were found: phenol,
2,4-D and fluoranthene. The fluoranthene was measured at such a low level
(RS value of -0.3) that it would have been attributed to the blank in Table 9
(see entry 933). Phenol was quantified at 11 ng/1 in N2X and at 7 ng/1 in
N2C. Since the quantification is based on the internal standard, phenol-D5,
the difference in these values is probably real and the conclusion is either
that the XAD-2 resin contributed phenol as an artifact, or that XAD-2 resin
69
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is more effective for the extraction of phenol from RO brine than is solvent
extraction. Since phenol was found at comparable levels in the blank XAD-2
concentrate, V1X, which contained very high levels of resin artifacts, the
former explanation is probably correct. TIC and T1X are the only concentrate
pairs for which phenol was identified in both concentrates and little XAD-2
resin contamination was found. In this case, the solvent extract .concentrate,
TIC, contained higher levels than the XAD-2 extract concentrate, T1X (see
entry 156, Table 9).
Comparison of concentrates N2C and N2X—Concentrates N2C and N2X were
prepared from 6620 liters (1750 gallons) of DW sampled at the GSRI labora-
tories in New Orleans, Louisiana. The amounts of organic material in these
two concentrates and the distribution of that material in the partitioned
fractions is consistent with other DW concentrate pairs with similar surface
water sources. Also consistent with other DW solvent extract and XAD-2
extract concentrate pairs, the N2C and N2X compound identification results
have little in common. Omitting compounds attributable as artifacts to
XAD-2 resin, only 48 of the 326 different compounds found in these two
concentrates were found in both concentrates. Of these 48 compounds, 29
were acids. All of the non-artifact compounds found exclusively in N2X were
also polar materials: 23 acids, 14 alcohols, 18 ketones, 3 highly polar
neutrals (for example, N-hydroxyphthalamide), and 22 medium polarity neutrals
(for example, esters, ethers, and amides). In contrast, many highly apolar
neutrals were identified in concentrate N2C (for example, 73 compounds in
the aromatic fraction).
The levels of herbicides found in these two concentrates is consistent
with the agricultural drainage into the Mississippi River. While there are
several chemical industry sources of organic pollution of this source water,
indicative compounds are relatively few compared to those for DW concentrates
from Cincinnati and Philadelphia.
Philadelphia, Pennsylvania, February 10, 1976—
P2C; solvent extract of RO brine—With respect to organic material
recoverable by solvent extraction of RO brine, the DW sampled at Philadelphia
was about average, with the concentrate reflecting a concentration of 177 ng
per liter of sampled DW (Table 7). The organic material in concentrate P2C
was, however, somewhat different from the other concentrates in the amount
which was recoverable as the high polarity fraction. This fraction represented
32 percent of that present in the P2C concentrate. Values for other solvent
extract type concentrates ranged from 10 percent for T4C to 20 percent for
S2C and averaged 15.3 percent. Thus, the P2C concentrate contained a signif-
icantly higher relative amount of these high polarity materials than compa-
rable concentrates. The relative amounts of the concentrate recovered in
the other fractions (Table 7) were not significantly different from those
for other solvent extract concentrates.
The types of molecules found in the high polarity fraction are not
significantly different from those found for comparable concentrates. The
percentages of the identified compounds in which the usual functional groups
70
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were found are as follows: 38 percent contained the hydroxyl group, 29 percent
contained the keto group, 23 percent contained the ether group, 5 percent
contained the aldehyde group, and 15 percent contained a ring hetero atom.
Only five diester plasticizers were identified. Dibutyl phthalate was found
at very high concentration and is judged to be an artifact introduced during
concentrate preparation at some point following RO processing. Nearly
identical contamination was found for concentrates M2C and N2C.
Four species of isopropylidine derivatives of sugars (entries 12, 13,
238, and 502, Table 9) were identified at high levels (up to the RS value
6.8) in the high polarity fraction. These compounds occurred in two other
cases (the DW concentrate, 02C, and the AWT concentrate, R2C, Table 10).
However, detection of one of these (entry 12, Table 9) in the extraction
solvent blank (TIC) makes interpretation difficult.
Another distinguishing characteristic of the high polarity fraction of
P2C is that it contained higher levels of poly glycol ethers than any other
DW concentrate. A measure of the amounts of these materials present can be
taken from the RS values for the entries for tripropylene glycol methyl ether
isomers in Table 9 (entries 101, 102, 203, 204, 243, and 581). This class
of compound is usually present as oligomers of poly ethylene and poly
propylene glycol with a range of ethers as the terminal group. Thus, the
set of tripropylene glycol methyl ether isomers is only a minor component.
Usually, these oligomeric species could not b.e identified specifically for
entry into the database as a molecular structure, and, therefore, few appear
in Table 9. Thus, occurrence in P2C of these species at the highest levels
seen in DW concentrates is based on th.e GC-MS chromatograms of the high
polarity fraction rather than the results shown in Table 9. Certainly, the
relatively higher levels of these materials in P2C must partially account
for the higher recovery into this fraction for concentrate P2C.
The acid fraction had the following distinguishing features:
• Benzoic acid, clofibric acid and salicylic acid (water
re-use indicators) were among the components identified
at higher concentrations (RS values of 5.8, 5.8, and
4.8, respectively)
. DimethyImaleic acid and methylethylmaleic acid were found
at relatively high concentrations (RS values of 5.8 and
4.8, respectively)
• Five multichlorinated, low carbon number acids were
identified (dichloroacetic, dichloroacrylic, trichloro-
acrylic, dichlorobutenoic and pentachloropentadienoic
which is a degradation product of hexachlorocyclopentadiene)
• p-Chlorophenol, 2,4-dichlorophenol, 3,5-dichlorophenol and
2,4,6-trichloro phenol were identified
• Fatty acids above C12 were absent. The carboxylic acids
were about evenly distributed both in numbers and total
amounts between aromatic and nonaromatic species.
71
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The aromatic fraction contained a large number of halogenated materials
(24 compounds, 34 percent of the total), most of which were non-aromatic.
Some of the noteworthy identifications are:
• Bromocyclohexane, iodocyclohexane, 1-iodopentane and
2-iodopentane
• Trichloroaniline and two isomers of dichloroaniline
* Ortho, meta and paradichlorohenzene and hexachlorobenzene
. Styrene, 2-methylstyrene, and 2-chloronaphthalene.
The above compounds strongly indicate contamination from chemical industry
sources. However, only one of the above compounds had an RS value greater
than 1.8 (iodocyclohexane at 2.8), so the level of contamination may not be
objectionable.
The medium polarity fraction also contained some chemical industry
pollution indicators: phenylacetonitrile, benzonitrile, ethyl and dimethyl
pyridine, isophorone, DMF, diphenylamine, and four aldehydes. As usual, the
balance of the compounds were ketones, alcohols, esters and plasticizers.
P2X; XAD-2 extract of RO brine—Among the XAD-2 produced concentrates,
P2X had next to the lowest overall recovery of material into the fractions
at 7.7 percent. This value would have been even lower had it not been for
a relatively higher amount of material in the high polarity fraction. This
result mirrors that for the solvent extract concentrate, P2C, which had the
highest relative recovery for this fraction of all the DW solvent extract
concentrates (Table 7).
Concentrate P2X was substantially contaminated with material attributable
as XAD-2 resin bleed but less contaminated than the two concentrates, M2X and
N2X, which were omitted from the listing of Table 9 on that basis. Of the
XAD-2 produced concentrates listed in Table 9, concentrate P2X had the most
compounds (86) classified as XAD-2 resin bleed. For comparison, the numbers
of identifications classified as artifacts for concentrates 02X, T2X, S2X,
T1X, and T1Y were 60, 56, 12, 2, and 22, respectively. Thus, the P2X results
in Table 9 give the most representative characterization of what chemical
species constitute XAD-2 resin bleed material. See also Appendix A of Volume
2 and discussion of the Jefferson Parrish results in Volume 3 for similar
information.
Four specific search compounds (Table 4) were identified in P2X. Styrene
is without doubt an XAD-2 resin artifact even though it was also found in
concentrate P2C. Fluoranthene, which was not found in P2C, should also be
classified as a resin bleed artifact since it was also detected in the blank
concentrate, V1X, which was very heavily contaminated with XAD-2 resin bleed
artifacts. Trichlorophenol was identified in P2C at a concentration about
30 times higher than in P2X while pentachlorophenol (found at 0.6 ng/1 in
P2X) was not found in P2C. It is somewhat surprising that extraction effi-
ciencies would favor recovery of trichlorophenol but not pentachlorophenol
72
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in P2C, and the possibility remains that the pentachlorophenol. in P2X is
actually an artifact.
In the acid fraction of P2X, the strong acid herbicide, dicamba, was
identified. This compound was not identified in concentrate P2C. Some of
the stronger or more polar acids identified in P2C were also identified in
P2X: trichloroacrylic, dichloroacetic, dichlorocrotonic, phthalic, azelaic,
suberic, sebacic, salicylic, o-anisic, and anisic. The number of non-
aromatic acids identified exceeded the aromatic acids by about 3 to 2.
Essentially all of the 90 compounds identified in the aromatic fraction
can be classified as definite or probable XAD-2 resin bleed artifacts. For
the medium polarity fraction, 17 of the 42 identified compounds (40 percent)
also must be classified as XAD-2 resin artifacts. In this case, 7 of the
artifacts are ethyl esters of fatty acids and, thus, do not originate from
the resin but from esterification of fatty acids in the sample with the
ethyl alcohol solvent. Bischloroethyl ether is the only noteworthy compound
detected in this fraction.
The XAD-2 resin artifact interference extends even to the high polarity
fraction with 10 of the 37 compounds (27 percent) attributable as resin bleed.
Most of these compounds are arene substituted acetophenones with ethyl stryene
and proprophenone also present. Isophorone is the only noteworthy compound
found in this fraction. The balance of the non-artifact compounds are
alcohols (7 compounds), ketones (8 compounds), and poly glycol ethers (9
compounds). A number of poly glycol oligomers were also identified generi-
cally, but these were not added to the database since not enough was known
about their molecular structures.
Comparison of concentrates P2C and P2X—The concentrates P2C and P2X
were prepared from 5810 liters of DW sampled at Philadelphia's Torresdale
Waterworks on February 10, 1976. As for other solvent extract and XAD-2
extract pairs of DW concentrates, the compound identification results for
P2C and P2X have little in common. Omitting the compounds attributable
to XAD-2 resin bleed in the P2X concentrate, only 15 percent (56 ot 370)
of the compounds identified in these two concentrates were found in both
concentrates. The correspondence between these two concentrates would be
somewhat better if the large amount of XAD-2 resin bleed artifacts did not
present such a high level of interference. Consistent with the other
corresponding DW concentrate pairs, most of the compounds found exclusively
or at significantly higher concentrations in the XAD-2- produced concentrate
(P2X) are relatively stronger acids or more polar materials.
The total amount of organic material in the P2C and P2X concentrates
(equivalent to 1,180 pg per liter of original water) was about midway in the
range for the samplings shown in Table 7 (136 yg/1 for Seattle to 2630 pg/1
for Miami). The distribution of the concentrate material among the fractions
was also fairly typical for these two concentrates. Concentrate P2X had the
lowest percentage of material recovered in the acid fraction for all DW XAD-2
extracted concentrates suggesting that humic-related material may have been
73
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present in this concentrate at slightly higher levels than in other XAD-2
extracted concentrates. In addition, concentrate P2C yielded the highest
recovery observed in the high polarity fraction while the P2X recovery for
this fraction was the second highest. This result was apparently due to
higher relative amounts of poly glycol oligomers and non-aromatic alcohols
and ketones. *
In summary, the compound identification results for concentrate P2C
indicate the presence of chemical industry effluents in the source water
although the levels of these materials are not higher than those for
comparable samplings (for example, Cincinnati and New Orleans).
Ottumwa, Iowa, September 10, 1976—
02C; combined solvent extract of RO brine—The concentration of organic
material which the 02C concentrate represented in the sampled DW was 139 yg/1.
This concentration is somewhat lower than the average (163 yg/1) for the other
DW concentrates with a reasonably similar surface water source (143, 115, 217
and 177 yg/1 for TIC, T4C, N2C, and P2C, respectively, Table 7). The overall
recovery of concentrate 02C into the analyzed fractions was 57 percent, the
second highest recovery obtained for solvent extract concentrates. However,
this recovery was not significantly different from the other solvent extract
concentrates (except the highest, 65 percent, for P2C; see Table 9).
The identified compounds with the largest GC-MS peaks in the acid
fraction were the ubiquitous dimethyl- and methylethylmaleic acids. However,
these two substances may have been present in the concentrate predominantly
as the anhydrides, with the methyl ethyl species being the largest GC-MS
peak found on GC-MS analysis of the unpartitioned concentrate. Whether the
free acids of these two anhydrides were also present in the unpartitioned
concentrate is not known since the gas chromatographic or mass spectrometric
characteristics for the free acids were not investigated. However, the
anhydrides were not found in any of the analyzed fractions, and the fraction-
ation pH extremes would be expected (based on the reported data for maleic
anhydride) to convert all of the anhydride to the free acid. The nitrogen
analogues to these two maleic anhydrides were also detected in the unparti-
tioned concentrate. Presumably, the maleimides would hydrolize to the
corresponding acid-amide species during partitioning. However, no specific
attempt was made to find these materials in the GC-MS data. These four
species (two anhydrides and two imides) were added to the computer database
even though they were not found in the acid fraction since they were found
in the original concentrate.
Concentrate 02C also contained the highest level of 2,4,5-T (15 ng/1)
seen for the DW solvent extract concentrates. A smaller quantity of 2,4-D
(4 ng/1) was also detected. For comparison, the relative levels of 2,4,5-T
and 2,4-D were reversed in T4C at 5 and 44 ng/1, respectively, and in N2C
at 11 and 54 ng/1, respectively, while in TIC (the only other solvent extract
in which the two phenoxy herbicides were found) the levels were in the same
order at 5 and 2 ng/1 for 2,4,5-T and 2,4-D, respectively. Another herbicide
74
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identified in 02C was atrazine with an RS value of 2.9 (entry 91, Table 9).
The only other concentrate in which this compound was found was the New
Orleans concentrate, N2C, with an RS value of 5.7.
Pentachlorophenol, p-chlorophenol and phenol were found in the acid
fraction with the RS values 3.9, 1.9 and 0.9, respectively. The detection
of phenol here is low enough to be attributable to the blank. A number of
alkylbenzoic acids were found (2-methyl, 5 isomers of dimethyl and 4 isomers
of trimethyl). Two isomers of clofibric acid and salicylic acid were
detected at levels comparable to those for other concentrates. The ratio.
of non-aromatic species to aromatic species in the acid fraction was about
4 to 3.
The aromatic fraction contained few of the chlorinated aliphatic and
aromatic hydrocarbon and other species which have been taken to indicate
the presence of contamination from chemical industry sources. The five
halogenated species found were two isomers of trichloropropene, a dichloro-
pentane isomer, iodocyclohexane and o-dichlorobenzene. The other 42 compounds
identified were alkylated and/or alkenylated benzenes (28 species), naphtha-
lenes (5 species), partially reduced naphthalenes, indenes and azulenes
(6 species), biphenyls (2 isomers) and stilbene. This set of compounds is
similar in both type and relative concentrations to a subset of compounds
that are usually ascribed to XAD-2 resin bleed artifacts, with the most
abundant species being the diethylbenzenes, ethyl styrenes and naphthalene.
However, concentrate production did not involve contact with XAD-2 resin.
Furthermore, the many biphenyl, and bisphenyl C^ and €2 species always
observed in the XAD-2 artifact profile were not detected. If these materials
were not artifacts, then a reasonable explanation might be contamination of
the source water by diesel fuel and/or g'asoline (explaining the presence of
some of the substituted benzenes and partially reduced naphthalenes) as well
as contamination from a polystyrene/divinylbenzene source (explaining the
relatively high concentrations of ethyl styrenes and related species).
The high polarity fractions contained an isopropylidine derivative of
a sugar (furanose) which gave the largest GC-MS peak. Four such components
were also identified as major compounds in the P2C concentrate but not in
any other concentrates. Isophorone, atrazine, triethylphosphate and diethyl
sulfite, and 7 aldehydes were detected in this fraction also. Comparatively,
plasticizers and poly glycols were not major constituents of this fraction.
Most of the identified compounds contained the hydroxyl (18 species) and/or
the keto C28 species) functional group.
The medium polarity fraction contained diethylformamide, 2,4,6-collidine
and six aldehydes. There were also six ethyl esters of fatty acids, com-
pounds which are usually associated with XAD-2 resin produced concentrates.
02X: XAD-2 resin extract of RO brine—Although concentrate 02X resulted
in the lowest overall recovery of material into the analyzed fractions
(6.5 percent, Table 7), it should not be considered atypical. The low overall
recovery into fractions (6.7 percent), the predominance of acid fraction among
the others (90 percent of the recovered material) and the pronounced, late
75
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eluting profile of unresolved material in the GC-MS chromatogram of the acid
fraction on the SP2100 column were typical among the XAD-2 prepared DW
concentrates.
(
As with all XAD-2 resin produced concentrates (except T1X, T1Y, and S2X) ,
02X contained a significant amount of artifact material attributable to the
XAD-2 resin. These artifacts constituted a major portion of the material in
the concentrate identifiable by GC-MS analysis. Of the 231 compounds listed
in Table 7, 60 were attributable to XAD-2 resin bleed and 29 to other concen-
trate production method sources. Only 5 of the 61 compounds identified in
the aromatic fraction were not probable XAD-2 resin artifacts. In this
instance, however, the relative amounts of lower molecular weight material
(substituted benzenes) and higher molecular weight material (bisphenyl
species) was the opposite of that observed for the M2X, N2X, and P2X concen-
trates. In the present case (02X), the bisphenyl species were the predomi-
nant ones. Also in contrast to the results for M2X, N2X, and P2X, naphthalene
(as an artifact) was observed at a concentration about 5 to 8 times that of
the predominant bisphenyl species and about 15 to 50 times those for the
substituted benzene species.
In the acid fraction, two specific search compounds were found: phenol
and 2,4-D. Since phenol was found at about 10-fold higher concentration in
02X compared to 02C, it should probably be considered present in 02X as an
artifact. Results from other XAD-2 prepared concentrates have suggested
phenols as a possible resin bleed artifact also. The two maleic acids
(dimethyl and methylethyl) which were the most concentrated components of
the 02C acid fraction were among the largest GC peaks of 02X also. Other com-
pounds of interest include salicylic acid and ethosuximide as water re-use in-
dicators. The strong acids usually more prominant in XAD-2 prepared concen-
trates included four chlorinated acids (Ca through C<.) and six alkanedioic
acids (C2, Cfc, Ca, C9, C10, and Cn).
The high polarity fraction contained nicotine, isophorone and the usual
array of alcohols and ketones. While the usual diester plasticizers were
present, they were at lower levels than often encountered. The medium
polarity fraction contained some noteworthy nitrogen containing compounds:
nicotine, 2,6-lutidine, 5 quinoline/isoquinoline species, and N,N-dimethyl-
benzylamine.
Comparison of concentrates 02C and 02X—The water from which the 02C
and 02X concentrates were prepared was a 5450-liter ("1440-gallon) sample
of finished DW" taken on September 10, 1976, at the Ottumwa, Iowa, waterworks.
The source water was the Des Moines River for which the city of Des Moines,
about 90 to 120 miles upriver, is presumed to be the only significant non-
agricultural source of pollution. The results of analysis of the 02C and
02X were consistent with reasonable expectations of the source water:
• Herbicides 2,4-D, 2,4,5-T, and atrazine were found at
levels comparable to the highest observed in other DW
concentrates from agricultural drainage surface water
(New Orleans, Cincinnati, and Philadelphia).
76
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• In comparison with other DW concentrates from surface
water sources, few compounds were found indicating
significant pollution from chemical industry sources
. Most of the organic material present in the XAD-2 produced
concentrate, 02X, was humic-related
• Some of the standard water reuse indicators (salicylic
acid, clofibric acid, ethosuximide and nicotine) were
present at relatively moderate levels while other reuse
indicators (benzoic acid, phthalates and poly glycol
ethers) were found at levels lower than those found for
other concentrates with surface water sources.
A particularly curious aspect of the 02C and 02X compound identification results
was that the set of compounds found in the aromatic fractions for both concen-
trates constituted a reasonable representation of the usual spectrum of XAD-2
resin artifact compounds) however, the lower molecular weight substances (sub-
stituted benzenes and partially reduced naphthalenes) were predominantly in
the 02C concentrate while the higher molecular weight materials (bisphenyl
compounds) were predominantly in the 02X concentrate. The nature of this
anomaly can easily be visualized by scanning the entries for 02C and 02X in
Table 7 and comparing occurrence and RS values of compounds designated as
XAD-2 artifacts for these two concentrates with other solvent extract and XAD-2
extract pairs (T4C, T4X; P2C, P2X; and S2C, S2X). One possible explanation is
that the substituted styrene species might be from the effluent of a poly-
styrene plant upriver and the other species were due to gasoline or fuel oil
contamination. However, another curious aspect is that 02C contained .6 ethyl
ester species which are usually ascribed as artifacts due to esterification
from the ethanol solvent of XAD-2 type concentrates. Ethyl esters were rarely
found in solvent extract concentrates. Without further information regarding
the source water, these observations will have to remain engmatic.
Comparison of the identified compounds for these two concentrates
indicates the usually observed mutual exclusivity for solvent extract/XAD-2
resin concentrate pairs.. Enumeration of the results shown in Table 7 for
02C and 02X shows that only 43 of 309 compounds (14 percent) were detected
in both concentrates. The compound occurrence data is generally consistent
with the usual characterization that the most polar compounds are recovered
more efficiently by XAD-2 extraction of the RO brine while the least polar
compounds are nearly exclusively recovered by solvent extraction of the RO
brine.
Seattle, Washington, November 5, 1976—
S2C: combined solvent extract of RO brine—Concentrate S2C represented
the lowest concentration of organic material in the corresponding source
water (37 ug/1, Table 7) of all the non-blank concentrates that were analyzed.
However, since a very large volume of DW (11,750 liters) was sampled to
produce this concentrate, the 10 percent of the concentrate that was used for
77
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analysis, at 44 mg of-material, exceeded ay a factor of two that for concen-
trate TIC, at 21 mg of material. The amount of material in the analyzed
aliquot is equal to 0.1 times the product of the concentration and the volume
shown in Table 7. The average for the 7 solvent extract concentrates of
Table 7 was 81 mg of organic material in the analyzed aliquot. For concen-
trate S2C, the distribution of organic material among the fractions and the
overall recovery (53 percent) were consistent with the other solvent extract
type concentrates of Table 7. In striking contrast,-however, is the number
of identified compounds shown for S2C, 361 after correction for the blank,
compared to an average of 206 for the other solvent extract concentrates of
Table 7. Comparing the numbers of compounds identified in the individual
fractions of S2C (90, 81, 85 and 160 for acid, aromatic, medium polarity and
high polarity, respectively) with the averages for the other six solvent
extract type concentrates (73, 49, 45 and 71, respectively, as above), it
is clear that, while there was somewhat more identifiable material in the
acid and aromatic fractions of S2C, the medium and high polarity fractions
contained distinctly more identifiable material than the other solvent
extract type concentrates. Comparing the numbers of confirmed versus tenta-
tive identifications for the solvent extract concentrates in Table 7, it
is obvious that a smaller portion of the identified compounds have confirmed
status in S2C. The confirmed:tentative ratio for S2C is 1:2.24 while the
average of the other 6 solvent extract concentrates is 1:1.4. The explana-
tion for this apparent anomaly is that only a few of the abnormally high
number of identifications in the medium and high polarity fractions of S2C,
cited above, have been confirmed. For example, of the 160 compounds identi-
fied in the high polarity fraction, only 7 (4 percent) had confirmed identi-
fications. For the medium polarity fraction, only 28 percent of the identi-
fications were confirmed. In contrast, 50 and 41 percent of the compounds
identified in the acid and aromatic fractions, respectively, were confirmed.
Alcohols and ketones make up the bulk of these excess compounds, and this
result can be easily visualized by scanning the listings under the S2C
heading in Table 9 and noting the types of compounds that were either found
exclusively in S2C or only in S2C and one or two other concentrates. Of
160 compounds found in the high polarity fraction, there were 108 alcohols
and/or ketones. These 108 compounds consisted of 26 saturated alcohols,
10 unsaturated alcohols, 9 alcohols with other functional groups, 20
saturated ketones, 23 unsaturated ketones, 12 ketones with other functional
groups and 8 compounds with the furan-2-one moiety. The source of this
plethora of compounds may be related to the conifer forested watershed
which is the source of the raw water since 5 compounds related to oxygenated
diterpenes were identified: camphor, pinacol, fenchone, citronellol and
farnesol. The above noted alcohols and ketones, in the many unsaturated
and alicyclic variations identified, are definitely suggestive of what one
might expect for breakdown products of diterpene-related compounds. The
mass spectra for these compounds almost never contain the molecular ion as
a significant fraction of the ionization. As a result, many identifications
of these alcohol/ketone compounds have been made with a significantly lower
level of confidence than was possible for other types of functional groups.
Since most of these compounds were considered to be relatively innocuous
and/or possibly isolated instances of occurrence, identification confirmation
was not pursued.
78
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The most distinguishing characteristic of the acid fraction was the
relatively higher numbers and concentrations of fatty acids: 38 non-aromatic
carboxylic acids with many isomeric forms were identified. Alkyl benzoic
acids were also in relatively high abundance with 13 species identified:
benzoic; monomethyl, all 3 iscrmers; dimethyl, all 6 isomers; trimethyl,
2 isomers; and one isopropyl isomer. As usual, methylethyl- and dimethyl-
maleic acids were among the species present at highest concentration. The
chlorinated materials identified were the search compounds 2,4,6-trichloro-
phenol and pentachlorophenol (1.6 and 0.9 yg/1, respectively) and some
chlorinated carboxylics (RS values are in parentheses): dichloroacetic
(3.2), trichloroacetic (4.2), dichloropropanoic (3.2), 2-chlorobenzoic
(3.2), 2,4-dichlorobenzoic (2.2), 3,4-dichlorobenzoic (2.2), and 2,5-
dichloro-4-methylbenzoic (2.2) acids; the herbicides amiben (3.2; 3-amino-
2,5-dichlorobenzoic acid) and dicamba (2.2; 2-methoxy-3,6-dichlorobenzoic
acid), and pentachloropentadienoic acid (3.2; oxidative degradation product
of hexachlorocyclopentadiene). As for the other concentrates, methylethyl-
maleic acid and dimethyImaleic acid were predominant components, with the
former appearing as one of the largest GC peaks in the acid fraction. Two
resin acids, dehydroabietic acid and deoxypodocarpic acid, were also
identified.
In the aromatic fraction, a greater than normal portion of the compounds
contained chlorine (28 of 80 compounds, 35 percent), but only two compounds
contained bromine or iodine (dibromochloromethane and iodocyclohexane). Half
of the identified compounds contained a discrete benzene nucleus. The
specific search compounds found in the aromatic fraction were the following
(concentrations, ng/1, are shown in parentheses): lindane (15.), o-chloro-
toluene (0.07), p-dichlorobenzene (1.7), 1,2,4-trichlorobenzene (0.04),
PCB (Cls) (not quantified), styrene (0.09), o-methylstyrene (0.1) and
diphenyl amine (0.2). Other noteworthy compounds found were dichloroaniline,
trichloroaniline and dichloronitrobenzene. While the above compounds seem
to suggest contamination from industrial sources, the concentrations found
were quite low with the following numbers of compounds having the indicated
RS values: one compound at 3.2, 7 at 2.2, 16 at 1.2, 23 at 0.2, and 33 at
-0.8.
As noted above for the S2C concentrate, the medium polarity fraction
contained more identifiable compounds than usual. Most of these materials
were alcohols and ketones with the alcohols more prevalent in the high
polarity fraction and the ketones more prevalent in the medium polarity
fraction. Of the 85 compounds identified in the medium polarity fraction,
32 contained a ketone group and 15 contained an alcohol group. Three of
the four largest GC-MS peaks in the fraction were chlorinated alcohols
and ketones. The only specific search compound identified in the medium
polarity fraction was 2-chloroaniline at 3 ng/1. Other noteworthy compounds
included (RS values are in parentheses): methyl isocyanate (2.2), DMF (1.2),
phenylacetonitrile (1.2), and dimethyl sulfone (2.2).
The analysis results for concentrate S2C can be summarized as follows:
The RS values of the identified compounds were uniformly
lower than those for other concentrates. This result
79
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was principally attributable to the very large volume
of the sampling.
An unusually large number of ketone and alcohol compounds
were identified and these two classes of compounds
account for the comparatively larger number of compounds
identified in the concentrate. Most of these ketone and
alcohol compounds were in the C6 to C10 range and may be
related to breakdown products of oxygenated diterpenes.
• Considering the source of the water, many of the non-
aromatic chlorinated compounds probably originated
from chlorination at the treatment plant rather than
contamination from anthropogenic sources.
. Some of the ubiquitous water re-use indicators (for
example, clofibric acid and salicylic acid) were not
detected in concentrate S2C, consistent with expectations
based on the source of this water. Other water re-use
indicators such as plasticizers and poly glycols were
found at lower levels and in few cases.
S2X: XAD-2 extract of RO brine—The usual late eluting profile of humic-
related material in the acid fraction GC-MS chromatogram on the SP2100
column was distinctly less pronounced for the S2X concentrate than for most
of the other XAD-extracted concentrates. However, the overall recovery of
12 percent of the concentrate material into the fractions was comparable to,
but at the upper range of, the other 6 XAD-2 concentrates. Thus, it appears
that either the nature of the humic-related material or the relatively lower
total amount that was present in the partitioned aliquot (about one fourth
the average for T4X, M2X, N2X, P2X, and 02X) resulted in less interference
in the acid fraction than usual. Another characteristic of concentrate S2X
that enhanced the quality of the GC-MS data was that few XAD-2 resin bleed
artifacts were present. Only 12 of the 171 compounds detected for S2X are
indicated in Table 9 as possible or probable XAD-2 resin bleed artifacts.
Only one concentrate showed fewer XAD-2 artifacts CT1X, produced by the
HERL laboratory staff), and the others were at least an order of magnitude
worse in this respect.
The most concentrated components of the acid fraction were a series of
dihydroxy-alkyl-benzoic acids which probably originate from degration of
lignin in the extensive forested watershed of the source water. Some
analogues with one or more methoxy groups substituted for hydroxyl groups
were probably from the same source. Salicylic acid and ethosuximide were
the only water re-use indicators identified in the acid fraction. The
chlorinated herbicides dicamfaa and dalapon, also identified in S2C, were
the only herbicides detected. Consistent with essentially all the other
concentrates, methylethylmaleic acid was among the most abundant materials
identified, and dimethylmaleic acid was also identified but at a substantially
lower concentration. In proportion to the total number of compounds identi-
fied in th.e acid fraction, a relatively large number of chloro non-aromatic
carhoxylic acids were identified: chloroacetic, dichloroacetic, 2-chloro-
propenoic, trichloropropenoic, 2,2-dichloropropanoic (dalapon), 2,2-dichloro-
80
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butanoic and 4,4-dichlorobutenoic acids. p-Nitrobenzoic, phthalic, tere-
phthalic and 2-chlorobenzoic acids (relatively stronger and more polar
species) were found at moderate levels while the less polar fatty acids
(predominant in S2C) were only minor components. A relatively large amount
of benzoic acid was probably at least partially attributable as an XAD-2
resin bleed artifact. Three isomers of methylbenzoic acid and three isomers
of dimethyIbenzoic acid, detected at lower concentrations than for S2C, may
not be attributable as XAD-2 artifacts.
All seven of the specific search compounds detected were found in the
aromatic fraction (concentrations, ng/1, are shown in parentheses):
p-dichlorobenzene (0.7), lindane (0.3), pentachlorobiphenyl and other PCBs
(less than 0.1), o-chlorotoluene (0.06), trichlorobenzene (0.02), diphenyl-
amine (0.02), and fluoranthene (less than 0.01, possibly an XAD-2 resin
bleed artifact). All of these specific search compounds were also found in
concentrate S2C. Only about three of the 44 compounds found in this fraction
were attributable as XAD-2 resin bleed artifacts. Similarly to S2C, nearly
half (19) of the compounds contained halogen, and 13 of these were non-
aromatic. Typical compounds were three isomers of trichloropropene, three
isomers of dichloroisopentane, bromocyclohexane and chlorocyclohexane. Most
of these compounds, and other similar ones, were also identified in concen-
trate S2C at about the same concentrations. Since these compounds should
have been nearly completely recovered from the RO brine by solvent extraction
(and, therefore, in concentrate S2C), they should have been absent or present
at far lower concentrations in concentrate S2X. Since this was not the case,
the possibility remains that they may be artifacts. In support of the postu-
lated lignin breakdown products found in the acid fraction, three substituted
naphthalene compounds which could have originated from resin acid decomposi-
tion were identified in the aromatic fraction. Two other compounds of
interest are 2,4,6-trichloroaniline and dichlorocyclooctadiene. The latter
compound may be a dimerization product of chloroprene.
The medium and high polarity fractions present no anomalies or other
unexpected results. The numbers of alcohols and ketones identified are
essentially normal in contrast to the plethora of these species in S2C, but
this is the expected result based on the solvent extractability of these
materials. Plasticizers and poly glycols were fewer in number and lower in
concentration compared to the low levels found in S2C, as would be expected.
There were more XAD-2 resin bleed artifacts identified in the medium and
high polarity fractions than in the acid and aromatic fractions. A total of
7 and 6 XAD-2 resin bleed artifacts were identified for the medium and high
polarity fractions, respectively, in addition to 4 fatty acid ethyl esters
arising from the ethanol solvent. Nicotine, isophorone, 1-methylisoquinoline
and diethylformamide were the only compounds of potential interest which
were identified.
Comparison of concentrates S2C and S2X—The S2C and S2X concentrates
were prepared from 11,750 liters (3100 gallons) of finished DW sampled on
November 5, 1976, at the distribution system at 2700 Airport Way in metro-
politan Seattle. The raw water source for the sampled DW was reported to
be the Cedar River.
81
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There was the usual high, degree of mutual exclusivity in the identi-
fication results for S2C and S2X which was consistent with that observed for
other solvent extract/XAD-2 extract pairs of DW concentrates. In this case,
only 61 of the 441 compounds identified in these two concentrates (14 percent)
were identified in both concentrates. Corresponding values for the other
concentrate pairs ranged from 12 to 20 percent.
The distribution of recoveries into the fractions for these two concen-
trates were not significantly different from those of the other concentrate
pairs. The values for S2X indicate the typical poor overall recoveries due
to the presence of humic-related material. However, in this case, the
presence of the humic-related material did not result in the usual quantities
of interfering material in the acid fraction. In addition, the near absence
of XAD-2 resin bleed artifacts in S2X also enhanced the ability to detect
sample constituents at low levels. The result of these two factors was that
a relatively higher number of the S2X identifications were also found in
S2C: 61 of 140 compounds (44 percent). The corresponding values for the
other 6 concentrate pairs ranged from 24 percent to 37 percent and averaged
33 percent.
No water re-use indicators were identified in concentrate S2C, as
expected, based on the source of the water. However, three high polarity
re-use indicators were identified in concentrate S2X C.RS values are in
parentheses): salicylic acid (3.2), ethosuximide (_3.2), and nicotine CP.2).
With one exception, ethosuximide has been identified only in XAD-2 produced
concentrates. Similarly, in 4 of 6 identification instances, nicotine was
found only in the XAD-2 produced concentrate, and in the one case of
identification in both the solvent extract and XAD-2 extract concentrates
(TIC and T1X), the XAD-2 produced concentrate contained a significantly
higher level. Salicylic acid was found in all the XAD-2 produced concentrates
and all solvent extract concentrates except for S2C. There is no readily
apparent explanation for this anomaly other than the S2X detection was as an
artifact or detection in S2C was obscured by interfering materials.
In summary, the results for these two concentrates suggest the following
characteristics for the original water:
. The low levels and numbers of drugs, drug metabolites,
plasticizers and poly glycol species indicate the
presence of a small but distinct component of re-use
water.
• Chlorination has apparently given rise to a substantial
number of non-aromatic chlorine containing species of
relatively low molecular weight. In this context, the
lack of companion brominated species probably derives
from the assumed extremely low level of bromide ion in
the source water.
. Most of the organic material in the water can be
attributed to non-anthropogenic sources in the forested
watershed as indicated by the variety of oxygenated
diterpene-related and resin-related species detected.
82
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The very large number of alcohols and ketones found
were postulated to be breakdown products of oxygenated
diterpene-related materials.
• There was only a slight indication of the presence of
industrial chemicals although there was evidence of the
use of pesticides and herbicides in the watershed
(dicamba, dalapon, amiben and lindane).
Comparison and Discussion of DW
Concentrate Analysis Results
The Degree to Which the GC-MS Analysis Results
Characterize the Organic Concentrates—
A central conclusion of this work is that most of the organic material
present in the concentrate was not accessible to the type of detailed
molecular characterization provided by GC-MS analysis. The recovery results
for partitioning of the concentrates prior to GC-MS analysis (Table 7) clearly
show that most of the organic material present in the concentrate was not
recovered into the four fractions on which essentially all of the compound
identification results were based. The average recoveries were 52 percent
and 10 percent for the 7 solvent extract and 7 XAD-2 extract concentrates,
respectively. Combining recoveries for each pair of solvent extract and
XAD-2 extract concentrates yields composited recoveries for each sampling
which range from 14 percent (Ottumwa, Iowa) to 25 percent (Cincinnati, Ohio,
January 14, 1980) and average 20 percent. Evidence is presented in the
section "Results and Discussion, Overview", which support the contention
that most of the approximately 80 percent non-recovered material was humic-
related substance. Certainly, other classes of compounds, such as quaternary
ammonium ions, mono- and diphosphoric esters, organosulfonic acids, poly-
hydroxy species (for example, glycerol and manitol) and other highly polar
and/or ionizable species (for example, citric acid and ethanolamine)
represent a portion of the 80 percent which was not recoverable through the
partitioning scheme, but the limited evidence, cited above, indicates that
humic-related materials are the major fraction of these non-recoverable
substances. Thus, one must remain cognizant that the compound identification
results presented here represent less than 20 percent (as the average) of the
organic material that was present in the originally sampled DW. Actually,
the fraction of organic material which the identified compounds represent
may be significantly less than 20 percent since CD there is good reason to
believe that the RO process failed to retain many GC-MS analyzable species,
and (2) it is clear that a major portion of the recovered material in the
acid fraction was not sufficiently volatile for gas chromatographic analysis.
Failure of the RO process to recover many GC-MS analyzable organic species
was addressed in the discussion section in which the T1Y results were
compared with the combined results of TIC and T1X. Based on that comparison,
and assuming that the lost organic material escapes into the RO permeate
rather than being lost to absorption on the membrane surfaces, a more
effective method for preparation of representative organic concentrates
would be RO concentration followed by direct XAD-2 adsorption of the RO
permeate water at both acidic and basic pH.
83
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Compounds Identified in Most of the Concentrates—
Inspection of Table'9 conveniently visualizes the frequency with which
compounds were found in the DW" concentrates. Not surprisingly, compounds
which were identified in most of the concentrates were usually found, in at
least one of the detection instances, with RS values at the upper end of the
range. Thus, these compounds appear toward the beginning of Table 9.
Depending on the molecular properties, a compound might be exclusively
recovered into either the solvent extract concentrate or the XAD-2 extract
concentrate or both. This factor must be kept in mind when scanning Table 9
for frequently identified species.
Some of the frequently detected compounds in Table 9 are itemized below.
Numbers in parentheses following compound names designate the entry sequence
number in Table 9.
. Ethylmethylmaleic acid (7) was found at or near the
highest levels observed for identified components in
the acid fractions of every DW concentrate except the
Poplarville, Mississippi, blank. The related compound,
dimethylmaleic (14), was also present at about one-third
to one-tenth the level of the ethylmethyl species. That
these materials were not artifacts is confirmed by their
absence from all of the analyzed blank concentrates
(VIC, V1X, X1C, XIX, and T2B) and their presence in non-
RO produced small-volume samples of the Cincinnati,
January 14, 1980, set (reported in Volume 3). These
two acids are probably related to environmental degrada-
tion of polyester (alkyd) resins widely used in paints
and other polymer applications. The remarkable ubiquity
of their detection and both the uniformity of the concentrations
observed and the relative amounts of the two species in
each concentrate suggest that they may be highly refractory
toward biodegradation in surface waters.
• Fatty acids were always present as a fairly standard set
of species but often at different levels from one concen-
trate to another. Since fatty acids were also often
detected in concentrate blanks and partitioning blanks,
many of the detection instances of Table 9 for these
species (especially ones between C^ and C}8) have been
attributed to the blank. It is reasonable that in most
cases some portion of the fatty acid actually came from
the sampled water. The fatty acids detected with the highest
frequencies were: stearic,C18 (52); oleic, C18-ene (88);
palmitic, C16 (4), myristic, C14. (18); lauric, C12 (86);
capric, C10 (82); pelargonic, C9 (51); caprylic, C8 (48);
2-ethylhexanoic (.71); heptanoic (.158); caproic, C6 (155);
2,3-dimethylbutyric (517); valeric, C5 (95); isovaleric,
3-methylbutyric (63); 2-methylbutyric (22); and butyric (24).
Two alkanedioic acids frequently found were suberic, C8 (87),
and azelaic, C9 (84). Three oxygen substituted acids were
also identified with higher frequency: levulinic, C5-4-keto
84
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(267); 2-methoxy-4-methyl-2-pentenoic C299) and 2-methoxy-
3-methyl-2-pentenoic (587). Possibly, the latter two
compounds were actually present as the 2-keto species and
were formed by methylation of the enol tantomer during
diazomethane derivatization of the acid fraction.
Eight aromatic carboxylic acids were identified in a
majority of the concentrates: benzoic (17); ortho-,
meta- and para-toluic (221, 72, and 73, respectively);
2,3-, 2,4-, and 3,5-dimethylbenzoic (189, 64, and
216, respectively); 2,4,6-trimethylbenzoit (219);
phenylacetic (49); and phthalic (85).
The most frequently identified water re-use indicators
were salicylic (47) and clofibric (74) acids both of
which are metabolites of the common high dosage drugs
asprin and clofibrate (ethyl 2-(4-chlorophenoxy)-2-
methylpropanoate), respectively. Other frequently
identified water re-use indicators were nicotine (684),
ethosuximide (298), BHT (1084) and oligomers of poly-
ethylene and polypropylene glycol ethers. The latter
compounds were not molecularly characterized in enough
detail for entry in the computer managed database.
However, they were always present in solvent extract
type concentrates of DW which had vulnerable surface-
water sources. The levels of these oligomeric materials
were commensurate with th.e expected degree of re-use
of the source water. These poly glycol compounds are
commonly used in soaps, shampoos, cosmetics, ointments,
paints and fabric softeners. Thus, it is not unexpected
that they would be so commonly encountered, especially
since they are known to be highly refractory toward
biological or environmental degradation.
Frequently identified compounds which can be classified
as industrial solvents include: dichloroacetic acid (96),
cyclohexanone (16), 2,5-hexanedione (202), isophorone (75),
3-methyl-2-cyclohexen-l-one (450) (similar to isophorone),
2,2,6-trimethylcyclohexanone (516), 3-methyl-2-cyclohexene-
1-one (450), 3-hydroxy-3-methyl-2-butanone (427), diethyl-
formamide (270), and lower molecular weight poly glycols
such as propylene glycol methyl ether (45) , diethylene -
glycol butyl ether (79) and dipropylene glycol methyl ether
(126),
Frequently identified nonsolvent industrial compounds
include acetophenone (67), p-dichlorobenzene (340),
trichlorobenzene (354), and phenylacetonitrile (346).
Most of the compounds which could be classified as
chemical industry effluents were identified in too few
concentrates for inclusion in this listing of frequently
identified compounds.
85
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• Other compounds frequently detected included common
plasticizers such as di-n-butylphthalate (10, di-
isobutylphthalate (20), diethylphthalate (37), and
triethyl phosphate (97); the herbicides, 2,4-D (427).
2,4,5-T (190), and dicamba (112); bromodichloromethane
(33), probably produced by chlorination at the waterworks?
and phenol (156) and benzaldehyde (115) which could
originate from a number of sources.
Special Interest Compounds—
Computer software (described in Appendix A) was developed to search the
GC-MS data for the 53 compounds- of Table 4. Results of the GC-MS data
search are shown in Table 12. Also shown in Table 12 are other special
interest compounds which were identified in the normal course of GC-MS data
interpretation. These additional compounds are the semivolatile consent
decree priority pollutants and the compounds on the EPA "Chemical Indicators
of Industrial Pollution" list. The organization of Table 12 is parallel to
Table 9 with both tables indicating specific search, consent decree and
industrial indicator compounds with the symbols *, +, and $, respectively.
In addition, quantification results in ng/1 for the specific search compounds
(not shown in Table 9) are shown in parentheses below the RS value entry in
Table 12. Phthalates are listed separately in Table 12 to facilitate
visualization of occurrence patterns for these high interest compounds.
Clearly visible in the pattern of occurrences in Table 12 are the more
frequent instances and higher levels for concentrates from Cincinnat,
Philadelphia, and New Orleans which is consistent with expectations based
on the source water. The relatively high number of specific search compound
detection instances for S2C was principally attributed to higher sensitivity
due to the very large volume sampled (11,750. liters), and the consistently
lower RS values and concentrations shown in Table 12 are in agreement with
this hypothesis. One noticeable aspect of Table 12 is the distinctly enhanced
recoveries of these special interest compounds (except for the phthalates)
shown for concentrate T1Y (direct XAD-2 extraction/diethylether elution)
versus the concentrates TIC and T1X (RO pre-concentrated). This difference in
recovery performance on identical water samples has been discussed in the
sections covering these concentrates.
Some of the identifications of specific search compounds found in XAD-2
produced concentrates are in contradiction with expectations based on solvent
extraction efficiencies: p-dichloroBenzene (S2X), 1,2,4-trichlorobenzene (S2X),
fluoranthene (P2X and S2X), and diphenylamine (T4X). Note, however, that the
detection of a moderately high, level of aniline in concentrate T4X and the
absence of this compound in concentrate T4C is not anomalous since none of
the RO brine solvent extractions are performed at basic pH. There are 108
detection instances for the 31 specific search compounds shown in Table 12.
The 7 most frequently detected compounds account for 50 (46 percent) of the
108 detection instances. These compounds (and the number of times detected)
are: phenol (9), p-dichlorobenzene (8), styrene (7), pentachlorophenol (7),
trichlorophenol (6), and fluoranthene (6 of which some may be as an artifact).
86
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TABLE 12. SPECIAL INTEREST COMPOUNDS FOUND IN DW CONCENTRATES
CD
Seq.
Ho.*
Compound
Special
Intereat Relative Slrp' of GT Pc«k
Llatb VIC V1X T2B TIC T1X T1Y T4C
COMPOUNDS ON THE SPECIFIC SEARCH LIST (TABLE 4J
36
130
144
156
190
340
352
354
357
423
427
468
471
582
649
632
810
817
871
882
933
949
1081
1107
1165
1166
2,4.6-Ttlcblorophenol
Styrena
Uexachloro-1. 3-butadlena
Phenol
2.4,5-T
p-Dlchlolob«nier.a
Pentachloroanl Una
1.2, 4-Tt Ichlorobanzana
Pantachloronltrobencana
Pentachlorophenol
2,4-D
p-Chlorophenol
2.4-Dlchlorophenol
Anlllna
2,4-Dlchloronaphthalana
Trlphenyl phoaphate
o-Chloro toluene
o-Chloroanllina
Pentachloroblphenyla
Fluoranthene
Llndane
Dlphenylaalne
Ueptachlor
Tecrachloroblphenyl
Peatachloroblphenyl
• + t -2.0 6.0 3.6
(0.3) (58) (31)
• $ 0.0 1.0 5.0 -1.4t
(3.6) (0.4) (44) (0.8)
• + $ S.O
(1.6)
• + 2.0 5.0 4.0 3.0 3.6
(3.3) (7.5) (5.1) (20) (18)
* 1.0 3.0 -0.4
(4.8) (31) (4.7)
• + » 1.0 1.0 4.0 -0.4
(0.1) (0.3) (86) (0.4)
• 4.0
(8.2)
• + > 4.0
(18)
* 4.0
(0.4)
• •» ) 0.0 1.0 2.0 1.6t
(0.2) (1.0) (4.1) (2.6)
• 1.0 3.0 2.6
(2.3) (28) (44)
• $ 2.0 3.0 2.6
(0.5) (45) (46)
• + » -0.4
(2.5)
*
• 3.0
(0.8)
* -*• 4 1 fi 1 L
™ T 9 J .U 1 . *
(8.4) (3.3)
•
* 1.0 -0.4
(2.0) (1.6)
• -0.4
(1.6)
• + $ -2.0 2.0 -0.4t
(0.3) (0.9) (0.1)
* J 2.0
(0.8)
*
* "*" $
* $ 1.0
• 5 1.0
(0.4)
for Detection in the Indicated Concentrate11
T4X M2C N2C P2C P2X 02C
0.6t 4.8 -0.2
(2.7) (29) (0.8)
-0.2t 0.3t 3.9
(0.2) (1.9) (8.4)
0.7
(2.7)
3.6 2.6 3.7 0.9
(51) (6.1) (7.0) (1.6)
3.7 4.9
(U) (15)
1.6 3.7 -0.2
(4.9) (6.9) (0.2)
1.6 -0.2
(0.3) (0.2)
3.7 -0.2 3.9
(0.6) (0.7) (0.1)
3.7 3.9
(54) (4.3)
3.8 1.9
(0.6) (3.1)
2.7 3.8
(2.1) (27)
3.6
(23)
2.7
(0.1)
2.6
(1.2)
0.6
(3.9)
-0.4 0.6t 0.8
(0.1) (0.3) (3.7)
1.7
(0.4)
-0.4 1.7 -0.2
(0.2) (0.3) (0.1)
1.7
(0.2)
02X S2C S2X X1C XIX
2.2
(1.6)
0.9t 0.2t
(— ) (0.1)
3.9
(10)
-0.8 2.2
(1.7) (1.7)
-0.8 2.2
(0.01X0.01)
1.2t
(0.9)
2.9
( — )
-0.8 0.2
(0.1X0.2)
2.2
(3.1)
1.2 2.2
(— ) (0.3)
-0.8
(0.0)
1.2 0.2
(1.5) (0.8)
1.8 1.2
(0.2) (0.01)
-------
TABLE 12. (continued)
00
00
Special
Seq. Interest
No . * Compound
1248 Hexachlorobenzene *
1255 p-Creaol •
1294 2-Hethylatyrene *
1301 2-Chloronaphthalene *
1305 2.4-Diaethyl phenol •
Relative Size' of GC PeaV for Detection In the Indicated Concentrate11
Uet» VIC V1X T2B
+ $
0
(0
+ »
2 0.0
01) (0.2)
TIC T1X TH T4C T4X
-0.4t -0.4t
(3.0) (9.9)
-0.4
(0.1)
-0.4 -0.4
(2.8) (1.7)
M2C M2C P2C P2X 02C 02X S2C S2X X1C XIX
0.7 -0.2
(0.3) (0.1)
-0.2
(0.1)
-0.2
(0.01)
-0.8
(0.1)
COHPOUUDS NOT OH THE SPECIFIC SEARCH LIST
2 Naphthalene
62 Toluene
75 laophorone
141 m-Xylene
143 o-Dichlorobeniene
157 1.1.2.2-Tetrachloroethane
332 1.2-Dlchloroethane
335 Blachloroethyl ether
417 p-Xylena
651 a*-Dlchlorobeniene
702 Fhenaothrene
776 o-Xylene
944 Fluorene
995 Acenaphthalene
1198 Pyrene
1203 Ciuwne
1213 n-Fropylbencene
1226 DDE
PHTHALIC ACID DIESTEBS
1 Dl-n-butyl phthalate
20 Dl-laobutyl phthalate
37 Dl-ethyl phthalate
76 n-Butyl leobiityl phthalate
134 Dioctyl phthalate
245 Bla(2-ethylhe*yl) phthalate
265 Dlhexyl phthalate
292 Butyl benzyl phthalate
345 Dimethyl phthalate
703 Dicyclohexyl phthalate
849 Di-n-propyl phthalate
a) The aequence number correaponde to
•»
S
•fr
$
•fr.
•fr
•fr $
* -1.
$
•fr
+
+
•fr
$
+ $
t 8 2.
$
•fr $
$
+ S
+ $ 2
+ $
+ $
$
$ 3.
$
the entry in
b) The three apeclal interest liata are coded: ±:
5.1 1.0
5.0
5.0
-1.0
3.0
0 3.0 1.0
2.0
1.0
1.0
0 1.0 3.1
1.0
2.0
3.0 2.0
6
0
Table 9.
5.0t 0.6 3.6t
3.6
3.0 1.0 2.6 2.7
5.0 0.6
5.0
5.0t 4.0t 0.6t
3.0 2.0
4.0
3.3t
3.0
l.Ot 2.0t
0.6
2.0
-0.4
-1.4
5.0 5.0 0.6t
5.0
5.0 3.0 6.0 1.6t 3.6
5.0t
3.0t 4.6t
4.0 4.0
2.6t 0.6t
2.6
list of 53 compounds for which the GC-MS was
Decree Priority Pollutants." £1 Hat of "Chemical Indicators
1978).
c) See Section 5, Analytical Scheme/Quantification
d) See Tablea 7 and 1 for translation
to the concentrate generation blank
of the three
.
of Identified
4.8
5.8
2.6 0.8
1.6t
-0.2
0.6t 0.7t
2.8
0.8
-0.2
0.7
8.7 8.3 8.1
6.6 6.0 3.8
4.6 4.7
5.6 3.7 5.8
l.lt
4.6t 4.7t 4. It
4.6
4.6 3.7
7.8t 4.9 7.9t 2.2 2.2
5.9 2.2 3.0
3.8 1.9 3.9 1.2 2.2
1.9 2.2
0.9 2.2
0.2t 1.2t 5.0
1.4
O.St -0.lt
1.9 1.2 2.2 4.0
2.8t 1.9t 0.2t 1.2t -0.8
2.2 2.2
-0.8 2.0
O.Bt
0.9
0.9 0.2
0.8
4.0t 2.5t 1.21 . 1.4
3.9 1.2t 1.0
2.9
2. 8t
2.3t 3.9t 4.0t 3.Z
2.9t
apeclfically aearched (aee Table 4). +: Hat of "Consent
of Industrial Pollution" Federal Interim Primary
Compounds for an exolanatlon o
Drinking Water Regulations (February 9
digit concentrate code names. The symbol, t, deaignstea a detection instance that may be attributable
-------
Occurrence of Molecular Functional
Groups in the Identified Compounds—
Associated with each identified compound entered in the computer-managed
data base are a set of molecular functional group descriptors. A tabulation
of the occurrences of the 25 functional groups in the DVT concentrate results
is presented in Tables 13 and 14. Percentages which each of the 25 functional
group classes represent of the total number of identified compounds are shown
in Table 13. Display of the percentage of the total parameter in Table 13
was chosen to facilitate comparison of the relative distribution of the
functional groups among the analyzed concentrates. Thus, Table 13 provides
comparative information on the numbers (but not the amounts) of compounds
with the various'function groups. Total RS values for each functional group
are shown in Table 14, and this parameter reflects the amounts of material
for each functional group (rather than the number of occurrences). Thus,
these two tables are complimentary in the nature of the information provided.
Note that the total number of identified compounds for each concentrate has
been added to .Table 13 to enable computation of the number of functional
group occurrences from the percentages shown. Since these computer-printed
tables (Tables 13 and 14) are generated, from the data base before correction
for the blank, the total number of identified compounds shown in Table 13
are also uncorrected for the blank. In the following discussion of Table 13,
most of the conclusions are based on the results shown for the solvent
extract concentrates since the values in the Table-reflect a large contribu-
tion from XAD-2 resin bleed artifacts in concentrates T4X, M2X, N2X, P2X,
and 02X.
Ten of the functional group types in Table 13 need no discussion due to
a low or uniform distribution across the concentrates shown. These are:
unsubstituted aliphatic, unsubstituted alicyclic, substituted alicyclic,
halogenated PNA, substituted PNA, amide group, amine group, ether group,
phenol group, and sulfur- atom. Observations concerning the remaining 15
functional group types are the following:
• Halogenated species (aliphatic, alicyclic, and aromatic)
have relatively higher detection frequency in three of
the four surface waters mos-t vulnerable to chemical
industry pollution (TIC, T1Y, T4C, and N2C). M2C, which
is not high, as expected, in halogenated aromatics is
nevertheless high in halogenated aliphatics and
halogenated alicyclics which probably results from
chlorination of the high background of natural (humic-
related) organic material in this concentrate. The
average chloro compound frequencies for P2C is
unexpected since the water source is similar to that
for T1C/T1Y, T4C, and N2C.
• Comparing occurrence frequency values for the
substituted aliphatic group with those for the
substituted aromatic group shows that more of the
nonhalogenated species were nonaromatic with the
ratio of substituted aliphatic to substituted aromatic
compounds averaging 1.6:1 for the solvent extract
concentrates. The opposite, however, is true for
89
-------
TABLE 13. OCCURRENCE OF MOLECULAR FUNCTIONAL GROUP TYPES IN DW CONCENTRATES, SHOWING THE
NUMBER OF OCCURRENCES AS A PERCENTAGE OF THE TOTAL NUMBER OF IDENTIFIED COMPOUNDS
OCCURRENCE OF FUNCTIONAL GROUPS AMONG THE IDENTIFIED ORGANICS
PERCENT OF TOTAL*
VIC X1C tflX T2B XIX TIC TlX TlY
H2C H2X N2C N2X P2C P2X 02C 02X S2C S2X
3
0
51
0
0
7
10
r
27
5
2
2
22
2
0
5
25
3
13
i»
1
1
15
12
6
2
13
2
3
8
1
158
0
t)
It It
3
0
6
20
1
25
16
0
3
16
3
2
0
13
28
5
3
<»
1
3
1
1
99
2
0
26
5
0
7
36
0
26
2<»
a
5
10
3
2
2
lit
16
5
5
7
0
3
0
0
58
1
7
3<»
1
0
9
7
7
25
1
1
3
19
1
3
6
25
9
13
16
15
1
3
5
2
151
0
3
W9
0
0
16
i.
i«
l<»
It
0
1
38
1
1
1
36
8
<»
3
18
3
1
5
0
77
2
12
38
0
2
<«
1<«
21
26
5
1
1
10
1
0
3
19
25
9
2
8
3
2
2
243
2
7
31
1
1
7
13
9
30
6
1
2
21
1
1
5
27
6
13
10
12
<*
2
1
193
3
2
31
i*
1
8
26
2
26
12
0
1
16
5
2
it
27
7
10
5
15
2
2
1
181
3
9
36
1
2
9
5
It
l
-------
halogenated aromatics detected compared to halogenated
aliphatics.
Comparison of unsubstituted PNA, unsubstituted aromatic,
and unsubstituted alicyclic values show the effect of
XAD-2 resin bleed artifacts since most of these artifacts
are classified in these three categories (compounds having
only alkyl substitutents are considered unsubstituted in
this work).
The alcohol group does not show significant variation except
for a lower value for concentrate T1Y (compared to T1C/T1X)
in agreement with the earlier conclusion concerning the
reduced effectiveness of the direct XAD-2 adsorption
method for highly polar species.
Consistently higher detection frequencies of the
aldehyde group in the XAD-2 prepared concentrates is
due to various alkyl benzaldehydes which may be present
as a resin bleed artifact. Although it seems unreasonable
that benzaldehydes would be present as a polystyrene
impurity, air or peroxide oxidation at the styrene vinyl
group could be responsible for these aldehydes.
Except for two cases (T1Y and S2C) carboxylic acids
were the most frequently encountered groups. For
solvent extract concentrates, this functional group was
present in an average of 23 percent of the compounds
identified in solvent extract produced concentrates.
Alcohols exceeded carboxylic acids in concentrate S2C;
this result has already been discussed. For T1Y,
carboxylic acids were exceeded in number by ester groups
("see Below).
The range of ester group detection frequencies varied little
except for concentrate T1Y which, at 25 percent, was about
3-fold higher than the average for the solvent extract
prepared concentrates. Most of these species were methyl
and ethyl esters of both aromatic and non-aromatic acids.
Since these results differ markedly from those for concen-
trates TIC and T1X (prepared from identical water), these
esters must be suspected as artifacts. High levels of
methanol and ethanol in the concentrate during storage
could account for this anomalous result but should be
discounted since the XAD-2 adsorption column was eluted
with unpreserved, "distilled-in-glass" grade diethyl ether.
The higher value of concentrate TIC for the heteroatom in
ring group is the result of the large number of alkylated
pyridines, quinolines, and isoquinolines found in that
concentrate.
91
-------
• Little variation in the frequency of. detection of ketones
was observed except for concentrate S2C. The relatively_
large number of ketones detected in this concentrate has
Been discussed earlier in Section 6. The relatively low
value shown for T1Y as compared with T1C/T1X is in
parallel with the similar observation for the alcohol
group discussed above, and the same explanation applies
in this case.
• The five Cincinnati concentrates show slightly higher
frequencies for the nitro-group compared to other
concentrates. This result is consistent with the
observation that the Cincinnati concentrates contained
more pronounced indications of chemical industry pollution
than the other concentrates. The distinction, however,
is not a marked one with respect to the Philadelphia
concentrates.
• Phthalate diester identifications were slightly more in
evidence in the Cincinnati, Miami, and New Orleans
concentrates. It was surprising to find Miami included
in and Philadelphia excluded from this group.
Since RS values span a logarithmic scale, the total RS value shown in
Table 14 is not an arithmetic sum of the individual RS values since such a
sum of logarithmic scale values would be mathematically related to the
product of individual GC peak heights rather than the sum of them. For
example, 10 GC-MS peaks, each with an RS value of 1.0 would give a total
RS value of 3.0, and two peaks with RS values 2 and 8 would yield a total
RS value of 8.0009. The mathematical basis of the GC-MS peak RS parameter
is detailed in Section 5, Analytical Scheme. For the purposes of inter-
preting Table 14, it suffices that an an arithmetic difference of 1.0 between
two total RS values in the table under comparison corresponds to a factor of
one-half of an order of magnitude (.3.16) change in the amount of material
represented; a difference of 2.0 in total RS values corresponds to a factor
of one order of magnitude Q.0.0), and so forth.
The DW concentrate functional group results expressed as total RS value
for each, classification category are shown in Table 14. These results are
consistent with the conclusions made above concerning the frequency of
occurrence of functional groups among the identified compounds as expressed
in Table 13. The information in Table 14 allows some additional conclusions
to be drawn concerning the relative amounts of organic material belonging
to these classes of compounds. Again, attention is focused on the 7 solvent
extract type concentrates plus concentrate T1Y since the amount of XAD-2
resin bleed artifacts- in the XAD-2 resin produced concentrates does not allow
a valid comparison. Concerning the type of molecular nucleus (i.e., the
first 12 categories in Table 14) only three concentrates (M2C, N2C, and P2C)
have the substituted aromatic nucleus representing the greatest amount of
the identified organic material. However, after adjusting for the extremely
high artifact levels of butyl phthalate in these concentrates, the substituted
aliphatic nucleus assumes the highest ranking as for the other concentrates
92
-------
TABLE 14. OCCURRENCE OF MOLECULAR FUNCTIONAL GROUP TYPES IN DW CONCENTRATES, SHOWING THE
TOTAL GC PEAK SIZE FOR EACH GROUP ON BOTH GC COLUMNS
OCCURRENCE OF FUNCTIONAL GROUPS AMONG THE IDENTIFIED ORGANICS
TOTAL RS
VIC X1C W1X T2B XIX TIC T1X MY T«,C T«»X M2C N2X N2C N2X P2C P2X 02C 02X S2C S2X
1. UNSUBSTITUTEO ALIPHATIC 1.2 - <».2 - 1.2 "..6 - <».6 3.3 ",.2 6.8 6.2 6.2 <«.9 5.9 6.3 3.9 6.0 5.6 2.5
2. HALOGENATEO ALIPHATIC - 2.2-1.0 - - 6.<» i«. 3 7.6 3.6 <•. 3 7.5 i».3 6.6 «.. 5 5.9 3.5 6.9 6.6
16. UNSUBSTITUTEO PNA 0.3 5.5 2.1
15. AHIDE CiiOUP - - -i.O 2.6 0.2 5.i» (,.0 2.0 3.2 <,. 0 5.3 - 5.<« <«. 8 3.9 3.8 5.7 3.6 3.<« 1.2
16. 4MINC GROUP 1.2 - 0.0 - 0.2 <*.8 3.0 5.<« 3.<« k.k 2.7 3.6 5.9 3.0 3.3 0.8 it.2 3.5 !..<• 2.1
17. CARBOXYLIC ACID 2.3 6.1 <».7 5.1. 1..5 8.<* 7.0 7.8 7.3 7.5 8.8 7.9 8.5 7.5 8.1. 6.8 7.9 7.5 7.<» 7.1
18. ESTER GROUP <».0 *i.9 5.0 7.2 <«. 1 7.2 «».I 7.7 5.1. 1..6 8.9 7.5 8.7 6.5 8.", 6.0 6.2 5.9 6.3 3.6
19. ETHER GROUP 2.2 "..9 5.3 5.2 3.3 7.6 6.2 7.0 5.7 6.i» 7.9 7.1 7.3 6.3 8.6 6.7 7.2 5.8 7.3 5.6
20. HETEKOATOM IN RING 2.<» 1..9 2.2 3.7 1.6 6.5 <».3 5.<» 5.2 <.. 9 7.5 6.7 6.7 6.0 7.7 <«.5 7.3 <>.3 6.3
-------
and the substituted aromatic nucleus represented the second highest amount
of material for these 8 concentrates. The high levels of chlorinated material
in concentrates TIC, T1Y, T4C, M2C, N2C, and P2C is mirrored in the third
(TIC and T1Y) and fourth (M2C, N2C, and P2C) highest ranking for the halo-
genated aliphatic nucleus and the fourth highest ranking (TIC, T1Y, TAG,
and P2C) for the halogenated aromatic nucleus.
The quantitative rankings for substituent types (categories 13 to 25
in Table 14) shows acids and alcohols taking the highest and next highest
rankings exclusively (5 concentrates show the acid group highest, 2 show
it second highest, and P2C shows acids and alcohols at equal levels). The
ether functional group ranked third highest in 5 (TIC, T4C, M2C, P2C, and
S2C) of the 8 concentrates. In two cases, M2C and S2C, the levels of ethers
and ketones were equal to this third highest level. This surprising level
of ethers is due to poly glycols which were usually observed as major peaks,
and, since these species usually have a terminal alcohol group, they
undoubtedly contribute to the high (first or second) ranking for the alcohols
noted above. Ketones and esters both ranked fifth for three concentrates
(T4C, P2C and 02C; and M2C, N2C and S2C, respectively) with ketones ranking
third once (.N2C) and equal to ethers for third and fourth ranking in three
concentrates Ctwo with ethers, noted above, and one (T1Y) with esters). The
fourth rank for the heteroatom in ring group in concentrate TIC was due to
the large numbers of substituted pyridines, quinolines, and isoquinolines
already discussed. The surprising second/third ranking of the heteroatom
category for concentrate 02C is due to the high levels of dimethyl- and
methylethylmaleic anhydrides and imides (four species) which were discussed
earlier in the section covering that concentrate. Note that the high total
RS values C8.8 to 8.2) for phthalic digesters in concentrates M2C, N2C, and
P2C were not considered in the preceeding discussion since they result
principally from the high levels of dibutyl phthalate present in these
concentrates as artifacts.
For the 7 solvent extract concentrates, the functional groups which
represented the three lowest level categories were the following: nitro group,
6 concentrates Call but T4C); sulfur atom, 6 concentrates Call but P2C);
amine group, 4 concentrates (T4C, M2C, P2C, and 02C); amide group, 3 concen-
trates CT4C, P2C, and S2C); aldehyde group, 2 concentrates CT1C and N2C);
and phthalic diester, 1 concentrate (S2C). The main contributors to the
sulfur atom total. RS value were benzthiazole and benzenesulfonamides.
Compounds contributing to the nitro-group total RS value were almost exclu-
sively nitro aromatics. The nitro functional group is probably the most
unambiguous indicator of chemical industry pollution of all the listed
functional groups since it is the least likely to arise from natural
organic material or the use of consumer products. In agreement with previous
conclusions, the nitro group results of Table 14 indicate Cincinnati,
Philadelphia, and New Orleans DW as containing more of these chemical
industry indicators. The S2C total RS value C2.3) for the nitro group is
due mostly to a questionable identification of l-nitro-2-octanone at RS 2.2
Four additional functional group tables are presented in Volume 2.
Three of these tables show the number of occurrences, the total RS parameter
94
-------
for SP1000 GC-MS analysis and the total RS parameter for SP2100 GC-MS analysis
using a format identical to Tables 13 and 14. The fourth table shows all five
parameters for each concentrate (i.e., those of Table 13 and Table 14 plus the
other three cited above) in close proximity groupings for each concentrate to
facilitate simultaneous comparison of all five parameters between concentrates.
The Effect of Concentrate Production
Methodology on the Compound
Identification Results—
The three types of concentrate production methodology used to produce
the DW concentrates are described in some detail in Section 4. Two methods
are based on sequential extraction of the RO brine in which solvent extraction
of the brine is followed by XAD-2 adsorption and ethanol elution. Thus, two
concentrates were prepared from each sampling. The third method (used to
produce only one concentrate, T1Y) involved direct XAD-2 resin adsorption/
diethyl ether elution without RO pre-concentration. Individual observations
of the consistency of the identified compound results with chemical expecta-
tions based on the concentrate method are interspersed throughout the sections
which, discuss the results for each concentrate, and these will not be repeated
here.
The following summarizes those observations:
• RO pre-concentration either allowed apolar species (such
as substituted benzenes) to escape into the permeate
water or absorbed them. The RO process was, however,
apparently effective at recovering macromolecular
materials (such as humic substances and poly glycols)
ionic species (such as carboxylic acids) and highly
polar species (such as alcohols, ketones, amides,
ureas, sulfones, lactones, and others with similar
polarity and/or hydrogen bonding capability).
• Solvent extraction of the RO brine removed most of the
apolar and moderately polar species including the
carboxylic acids which have normal acid strengths and
lacked high polarity substitution. Since none of the
solvent extractions were performed at strongly basic
pH, strong bases were probably not recovered well.
Humlc species were also not recovered well but poly
glycols were partially recovered.
• After solvent extraction, the RO brine contained the
more water soluble species as evidenced by the compounds
identified in the XAD-2 recovered concentrates. About
90 percent of the XAD-2 recovered organic material was
humic substance. The identified compounds reported
for XAD-2 generated concentrates were predominantly
acids (especially dicarboxylics and polar-substituted
acids) and the more polar substituted neutrals.
95
-------
• Direct XAD-2 extraction apparently recovered apolar
neutral compounds with greater efficiency than the
methods based on RO precancentration. However, the
direct, acidic pH XAD-2' adsorption method performed
less effectively than RO for the recovery of bases,
highly polar neutrals Cespecially alcohols and ketones),
higher strength acids (i.e., dicarboxylics and halo-
aliphatic acids), humic substances and poly glycols.
One aspect of the concentrate production methodology which cannot be
assessed with the information presently available is the adequacy of the
performance toward strong bases. Aliphatic amines were so rarely identified
in the concentrates that their few detection instances should perhaps be
suspected as artifacts. In two cases CT1C and 02C), a variety of pyridines,
quinolines, and isoquinolines were found. However, aniline, which is a
specific search compound and, thus, could be detected with very high sensi-
tivity, was identified in only one concentrate (T4X). Moreover, aniline-D5
was one of the deuterated internal standards and its consistent recovery
in the fractions and blanks indicates that basic compounds would have been
detected had they been recovered in the concentrates at the 50 to 100 yg
level (i.e., 30 to 60 ng/1 for a 1500-liter sampling). Note that chloro-
anilines (mono through pentachloro species;) were detected with some regularity,
but these materials have such, low base strengths that some of them are well
extracted at acidic pH.
Another possible deficiency in the concentrate production methodology is
suggested by the compound identification results for anhydrides, imides,
lactones and lactames. DimethyImaleic acid and methlyethylmaleic acids were
identified at relatively high levels in all of the concentrates. The detec-
tion of the anhydrides of these acids as major constituents of the unparti-
tioned concentrate for 02C has been discussed earlier. These anhydrides were
also found in other unpartitioned concentrates, but they could not have been
present in the original water since they readily hydrolyze in the neutral pH
range. A possible explanation is that dehydration of the free acid occurred
during solvent evaporation steps of concentrate production, and this dehydra-
tion to the anhydride could have been enhanced by concomitant azeotropic water
removal. Frequent detection of Y-lactones (2-furanones) and occasional detec-
tion of Y-lactames may also have been due to a similar dehydration of Y-hydroxy
or Y-amino acids. These species hydrolyze less readily and, thus, could have
partially escaped hydrolysis at the pH extremes of the partitioning scheme.
The frequent detection of f-hydroxy acids in the derivatized acid fraction
may support this hypothesis. An alternative explanation is that these
dehydrated species were formed during GC injection which, for the splitless
GC-MS injection conditions,had durations of about 45 seconds. A definitive
explanation of these observations would require additional experimental work.
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Effect of the Raw Water Source
on the Analysis Results—
Two samplings were of DW with a groundwater source (Poplarville, Mississ-
ippi, and Miami, Florida). As noted in Section 4, Poplarville was sampled
because its source water Ca deep aquifer) was extraordinarily organic-free
and, thus, this sampling was appropriate as a. field sample RO method blank
(see Table 9 and the discussion of the Poplarville results earlier in this
section). Just the opposite was the case for the Miami groundwater as noted
in the earlier discussion of the M2C and M2X concentrate results. To
summarize, one or more of the aquifers for raw Miami DW was, at the time of
sampling, apparently vulnerable to intrusion of surface water with high levels
of humic substances and was also vulnerable through the same or other routes
to contamination with treated or untreated municipal wastes and/or solid waste
leachate. Thus, the analysis results for these two DW samplings appear to
span the entire water quality spectrum for groundwater sources and are not
useful for making general inferences about groundwater DW sources.
In contrast to the lack of representative data for groundwater, above,
the DW samplings with surfacewater sources provide an appropriate spectrum
for comparison. Seattle represented source water with the lowest anthropogenic
component of organic material but with a broad spectrum of natural organic
materials expected from a conifer forested watershed. The concentrate analy-
sis results were in agreement with reasonable expectations of the source
water in a number of areas:
• Many of the identified compounds (alcohols and ketones)
could have originated from natural degradation of
oxygenated diterpenes which were also identified
compounds of the concentrate
« There was minor evidence of the use of pesticides
and herbicides but almost no evidence of water
re-use indicators (i.e., those certain to have
originated from domestic municipal wastes)
• The wide range of very low level hydrocarbons
found were probably from air pollution in the
Seattle metropolitan area which is transported
and deposited as precipitation by the normal
meteorologic patterns of the area
' The many non-aromatic chlorinated species
observed probably were produced from naturally
occurring organic material during chlorine
disinfection and, thus, cannot be taken as
representative of the source water although the
high levels of these materials compared to the
relatively lower levels of humic material may
indicate unusually vigorous chlorination conditions
at the treatment plant.
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The Ottumwa, Iowa, and New Orleans, Louisiana, concentrates represent
source surfacewaters with principally agricultural drainage components.
Somewhat higher levels of materials reflecting water re-use and chemical
industry effluents were expected and found in the New Orleans concentrates.
However, concentrates from these two cities were the only ones in which the
agricultural herbicide atrazine was found. Other herbicides and pesticides
were also relatively predominant in the concentrates for these two cities.
Significantly higher levels of humic-related material, as compared to the
Seattle concentrates, was also in agreement with expectations based on the
source water.
The Cincinnati, Ohio, and Philadelphia, Pennsylvania, concentrates
represent surfacewater sources which are relatively more vulnerable to
chemical industry effluents than those for Ottumwa and New Orleans. The
higher levels and more numerous detection instances of compounds indicative
of chemical industry effluent in concentrates from these two cities have been
discussed earlier and can easily be visualized from the results shown in
Table 12. Somewhat higher concentrations of typical water re-use indicators
for th.ese two cities compared to Ottumwa and New Orleans is in agreement with
the higher population densities for the drainage basins in the former case.
Since Cincinnati was the only city for which the analyzed concentrates
represented more than, one sampling, the analysis results for those concen-
trates are the only ones which could reflect a potential effect of the sampling
time of year. The first Cincinnati sampling (concentrates TIC, T1X, and T1Y)
was performed on October 7, 1978, and the second sampling (T4C and T4X) was
performed on January 14,. 1980. The only aspect of the analysis results for
these two concentrates which might be relevant to the time of year of the
sampling is the apparently lower levels of humic-related material in the 1978
sampling as indicated by the residue weight analysis results shown in Table 7.
The 1978 concentrate reflected a lower level of organic material (540 ug/1 for
TIC plus T1X compared to 860 ug/1 for T4C plus T4X) and also gave a higher
percentage of material recovered in the fractions (23 percent for T1C/T1X
compared to 14 percent for T4C/T4X). The former result indicates higher
concentration of humic substances in th.e 1980 water while the latter result
indicates humic substances represented a lower fraction of the material in
the concentrate for 1978. The observed effect is in opposition to that which
would be expected based on the marked reduction in surface runoff in January
due to the large percentages of frozen ground in the Ohio River drainage
basin upstream from Cincinnati. No explanation of these apparently anomalous
results can be offered at this time.
DISCUSSION OF AWT CONCENTRATE ANALYSIS RESULTS
Summaries of the Results for Each Sampling
All of the AWT plant samplings, for which discussions of the concentrate
analysis results are presented individually below, were of a nominally 1500-
liter (400-gallon) volume of finished AWT water taken on the plant site. In
contrast to the DW concentrates, XAD-2 resin was not used to produce an
98
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additional extract of the RO brine. Instead, some of the six solvent extracts
of the two RO brines produced (see Section 4) were analyzed separately or all
six were combined for analysis as a composite concentrate. The third letter
of the three-digit concentrate code name signifies the type of solvent
extract:
Third Letter
of Code Name Concentrate Type
P Pentane extract of cellulose acetate
RO brine
M Methylene chloride extract of
cellulose acetate RO brine
N Methylene chloride extract of
cellulose acetate RO brine at pH 2
D Methylene chloride extract of
nylon RO brine at pH 2
C Combination of all six solvent
extractions of RO brine
A listing of the treatment steps for each AWT plant is given in Table 2
and complete descriptions of the plants have previously been reported (2).
Thus, no further details of the AWT process for each plant is given in the
discussion which follows.
Lake Tahoe, California,
October 24, 1974—
Four Lake Tahoe concentrates were analyzed; L2P, L2M, and L2N represent
the cellulose acetate RO brine and L2D was produced from the nylon RO brine.
L2D was the only extract of nylon RO brine analyzed separately from the
cellulose acetate RO brine extracts.
The residue weight analysis results of Table 8 show that these four
Lake Tahoe concentrates represented about 300 pg/1 of organic material in
the original water. The four-concentrate composited value for the overall
recovery into fraction (81 percent) was the highest such value found. The
values for concentration and percent recovery in fractions for the individual
concentrates show some inconsistences:
• The level of 50 pg/1 for L2D is surprisingly high
since only material which permeated the cellulose
acetate RO membrane can be recovered in concentrate
L2D. Results for the DW concentrates T1C/T1X and
T1Y indicated that highly apolar species can permeate
the RO membranes. However, concentrate L2D should
have contained only the most polar and acidic species
remaining in the nylon RO brine after pentane and
99
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methylene chloride extraction, and there should have
been only a small amount of these materials in the
RO brine.
• Based on reasonable chemical expectations, concentrates
L2M and L2N probably have reversed identities. Since
L2N is an extract from acidic brine, a relatively higher
amount of acids can be expected in it. In addition,
since extraction of L2M preceded extraction of L2N, a
higher relative amount of the high polarity species
would be expected in concentrate L2M. The results for
percentage recovery into fractions in Table 8 contradicts
both of these expectations. The L2M versus L2N comparison
also contradicts the corresponding values for fraction
recovery for the Pomona concentrates C1M and C1N which
are in agreement with the above stated chemical expectations.
Thirteen specific search compounds were found in the four Lake Tahoe
concentrates (see Table 15): diphenylamine (L2P and L2M), pentachlorophenol
(L2P and L2D), o-chloroaniline (L2P and L2D), phenol (L2M, L2N, and L2D),
p-chlorophenol (L2M, L2N, and L2D), fluoranthene (L2P), styrene (all four
concentrates), 2,4-dimethylphenol (L2D), crysene (L2P), 2-methylstyrene
(L2M, L2N, and L2D), and hexachlorobenzene (L2N). Crysene was not detected
in any other DW or AWT concentrate. In contrast to many concentrates, the
four Lake Tahoe concentrates contained few chlorinated species (only 24
compounds after correction for the blank). The total number of compounds in
Table 10 which have at least one detection instance for these four concen-
trates was 486. Since the sum of the numbers of identified compounds shown
individually in Table 8 for each, of the four concentrates is 647, it is clear
that few compounds were identified in all or most of the four concentrates.
Inspection of Table 10 shows that only 13 compounds were identified in all
four concentrates and only 25 compounds were identified in any three concen-
trates. Certainly an appreciable degree of mutual exclusivity is expected
between the classes of compounds that are extracted well by the two solvents,
pentane and methylene chloride. A second factor which also has some effect
is that the L2P, L2M, and L2N concentrates were the first three to be analyzed
in this research program, and the GC-MS data interpretation activity for these
three lacked the extensive experience that the analysts had gained with DW and
AWT concentrates during the 22 month period preceding analysis of the L2D
concentrate (34th in the series). In addition, the computer mass spectrum
matching capability had been substantially improved in the interval between
these analyses.
Most of the compounds identified in the acid fraction of L2P were fatty
acids. Identification of pentachlorophenol at relatively high levels in L2P
and at a low level in L2D but not in L2M or L2N was unexpected based on this
compound's acid strength. Non-aromatic acids were more numerous than aromatic
acids in L2M and L2N but the opposite was true for L2D. Clofibric acid was
found at high levels in L2M, L2N, and L2D (in which it was the largest GC
peak) and at lower levels in L2P. Ethosuximide, three barbituates, salicylic
acid, and saccharin were also identified in some of the Lake Tahoe acid
fractions.
100
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In the aromatic fractions, 153, 10, 47, and 26 compounds were identified
in L2P, L2M, L2N, and L2D, respectively. The large disparity for L2P was due
to a high hydrocarbon component which was recovered from the RO brine essen-
tially exclusively into the pentane extract. These compounds account for part
of the lack of correspondence in identified compounds among the Lake Tahoe
concentrates. Among these hydrocarbons were 15 compounds with fused ring
systems larger than naphthalene, and this complement of polynuclear aromatic
material constitutes the largest found for AWT and DW concentrates. Most of
the identified compounds were alkylated benzenes, naphthalenes, tetralins,
indenes, and indans. The RS values for these compounds ranged between 5 and
1, and 65 species had RS values of 3 or greater. Except for hexachlorobenzene,
pentachloropyridine (both, in L2N) and styrene and diphenylamine Cboth in L2M),
the other aromatic fractions from the other three concentrates contained no
compounds meriting discussion.
In the medium and high polarity fractions, poly glycols and phthalates
(especially butyl phthalate) were the dominant species. L2P, as expected,
contained almost no poly glycols, but the other three concentrates contained
many of these oligomeric species at moderately high levels. RS values for
these poly glycols ranged up to 7 for species identified sufficiently well
enough for entry into the data base. Other AWT concentrates contained more
or these materials by as much as an order of magnitude. Oxygenated diterpenes
(17 species) were identified in L2P, L2M, and L2N, and these Lake Tahoe
concentrates are unique among both the DW and AWT concentrates in this respect.
Other compounds identified in the medium and high polarity fractions which may
be of interest include caffeine (L2M, L2N, and L2D), nicotine (L2P and L2N),
DMF (L2N), diethyl and dibutyl formamide (L2P), isophorone and two isomers of
isophorone (L2N), 8 detection instances of alkyl phenols (for instance,
nonylphenol), tris-2-chloroethylphosphate (L2M), and three polar anilines
(chloro-, chloronitro, and nitroaniline, L2D).
Pomona, California,
September 25, 1974 (Pomona I)—
Three samplings were performed at the Pomona AWT plant. From the first
sampling on September 25, 1974 (designated Pomona I), three of the RO brine
solvent extract concentrates were analyzed: C1P, C1M, and GIN.
The composited residue weight results in Table 8 show that these three
Pomona I concentrates CC1P, C1M, and GIN) represented the highest concen-
tration C370 ug/1) of organic material in the original water of all the AWT
composite concentrates or related sets of concentrates from a single sampling.
The overall recovery of concentrate material into the analyzed fractions was
42 percent. This recovery value was about half that for the four Lake Tahoe
concentrates C.81 percent). The principal reason for the large difference
between these two concentrates was the presence of a large amount of poly
glycol materials in the Pomona I concentrates. On extraction of the RO brine,
most of the poly glycols were apparently recovered in the pentane (C1P) and
methylene chloride (C2M) concentrates. However, these moderately water
soluble species are not recovered well through the fractio'nation scheme,
and the lower recovery for C1P and C1M (compared to GIN) of concentrate
material into the analyzed fractions is the result. The percentages shown
101
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in Table 8 for recoveries into fractions for the three Pomona I concentrates
is completely consistent with chemical expectations based on the sequence of
solvent extraction of the RO brine and the concentrate partitioning scheme.
A total of 348 different compounds (not counting compounds attributed to
the blank) are listed in Table 10 as having been detected in concentrates
ClP, C1M, and C1N, and 70 of these compounds (20 percent) were identified
either in two of the concentrates or in all three. For comparison, only 25
of the 647 compounds (4 percent) identified in the four Lake Tahoe concen-
trates were identified in three or four of them.
As expected, the principal contributing factor to the lack of corre-
espondence between the three concentrates in the identified compounds is
attributable to the solvent extraction sequence. Concentrate C1P resulted
in 77 identified compounds in the aromatic fraction while 34 and 56 compounds
were identified in this fraction for C1M and C1N, respectively. Also, the
acid fractions of concentrates C1M and GIN resulted in 84 and 63 identified
compounds, respectively, while the C1P acid fraction yielded only 31 identi-
fied compounds. The Pomona I concentrates resutled in 31 identifications of
chlorinated compounds and eleven of the 16 specific search compounds detected
for C1P, C1M, and GIN were chlorinated compounds. The 16 specific search
compounds which were detected for the Pomona I concentrates were: diphenly-
amine, pentachlorophenol, phenol, styrene and 2-methylstyrene (detected in
all three concentrates); 2-chloroaniline and fluoranthene (C1P and C1M);
4-chlorophenol (C1M and C1N); 2,4,6-trichlorophenol and 1,2,4-trichlorobenzene
(C1P and GIN); 2,4-dichlorophenol and p-chloroacetophenone (C1M); and 2,4-D,
hexachlorobenzene, and 1,4-dichlorobenzene (C1N). Detection of p-chloro-
acetophenone in C1M was the only detection instance for this compound in
the TKf and AWT concentrates.
In addition to the above listed specific search compounds, a number of
noteworthy compounds were identified in the four analyzed fractions for these
three concentrates:
• Acid fraction: four barbiturates (C1M plus phenobarbital,
GIN), ethosuximide
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• Medium and high polarity fractions: the most predominant
components of the medium and high polarity fractions were
poly glycol oligomers (jnoted above) which represented at
least three distinct homologous series. Tris-2-chloroethyl
phosphate was found at very high levels in C1M and somewhat
lower levels in C1P and C1N, and the amount of this compound
in the sampled water reflected by these three detections far
surpassed amounts detected for any other sampling. Caffeine
and dimethylsulfone were identified in concentrate C1N. DMF
was identified in C1M and C1N. Benzonitrile, an aminomethyl-
pyridine isomer, a trimethylpyridine isomer, and nicotine
were also found in C1M. Large components of dioctyl phthalate
and dioctylsebacate along with numerous fatty acid methylesters
were identified in C1P.
Pomona, California,
October 2, 1974 (Pomona II)—
The only concentrate analyzed of the six RO brine extracts produced from
the second Pomona sampling (Pomona II) was the methylene chloride extract of
the acidified cellulose acetate brine (C2N). Concentrate C2N contained about
half as much, organic material, at 37 pg/1, as the other comparable Pomona con-
centrate C69 pg/1, C1N), Table 8. In addition, the overall recovery of C2N
into the fractions was distinctly different from C1N at 20 and 88 percent for
C2N and C1N, respectively. Compared to corresponding values in Table 8, the
acid and aromatic fractions of C2N are apparently the source of this deviation.
These two fractions and their corresponding blanks (but not the other fractions
and blanks) inadvertantly evaporated to dryness during storage at -10°C before
residue weights were determined. Thus, the comparative recovery differences
in Table 8 for C2N are not considered significant.
The 106 compounds identified in concentrate C2N are listed in Table 10.
Only 5 of those compounds contained chlorine. The 7 specific search compounds
found in C2N are listed, with quantification results, in Table 15. The 7 com-
pounds are: pentachlorophenol, 2,4,6-trichlorophenol, phenol, 2-methylstyrene,
hexachlorobenzene, 1,4-dichlorobenzene and 1,2,4-trichlorobenzene. Only penta-
chlorophenol, at 11 yg/1, was found at a comparably high level. Consistent
with other acidified brine methylene chloride extracts, relatively small
amounts of the ubiquitous poly glycols and phthalate esters were identified.
In addition to the results noted above, the analyzed fractions can be charac-
terized as follows:
• Acid fraction: clofibric acid was the largest identified GC-MS peak
(.two other GC-MS peaks of comparable size could not be identified) .
Phthalic acid monobutyl ester was also a major component indicating
that a large amount of dibutyl phthalate was probably present in
the other (non-analyzed) Pomona II concentrates. The usual array
of dicarboxylic acids, generally present at higher levels in acid-
ified RO brine methylene chloride extracts than other extracts, were
present, and 7 of these species were identified including the
ubiquitous substituted maleic acids. Saccharin was also identified
with an RS value of 5.
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• Aromatic fraction: Only 11 compounds were identified, and most of
these had RS values of 2 or less. The lack of Appreciable material
in this fraction is in agreement with all other results for brine
extracts of this type. In addition to the specific search compounds
listed above, the only noteworthy compounds identified were three
phenyl substituted quinolines and isoquinolines two of which had
RS values of 3.0.
• Medium polarity fraction: Most of the 24 compounds identified in
this fraction had RS values of 2 or less, and, thus, this fraction
was comparatively "clean". Three phthalates, benzaldehyde, benz-
thiazole, dimethylsulfone and DMF were also identified.
• High polarity fraction: The largest GC-MS peak was identified as
tris-2-chloroethyl phosphate. This compound was also found at
high levels in the Pomona t and Pomona III concentrates, but the
level in C1M was distinctly higher than that for GIN. This re-
sult implies that the Pomona II concentrate produced by methylene
chloride extraction of neutral pH RO brine (not analyzed in this
work) may have contained even higher levels of this compounds
than the level found in C2N. Other than 4 phthalate esters at
moderately low levels, the only noteworthy compounds identified
in this fraction were five non-aromatic nitrogen heterocyclics
Cpiperidines,pyrimidines and pyrrolidines) none of which have
confirmed identifications (.see Table 10) .
Pomona, California,
June 17, 1975 (Pomona III) —
All six solvent extracts of RO brines were combined for analysis as the
composite concentrate, C3C. This concentrate represented only 87 ug/1 of
organic material in the sampled water and this amound is only 24 percent of
the corresponding amount for the three Pomona I concentrates (Table 8). This
rather large disparity between these two Pomona samplings is somewhat sur-
prising. Consistent with the relatively lower amount of material present in
concentrate C3C is the relatively low number of compounds (104) identified
(see Table 10). Of these 104 compounds, 11 contained halogen and 9 were com-
pounds, on the 53-compound specific search, list (Table 4). These 9 specific
search, compounds were: diphenylamine, 2,4,6-trichlorophenol, o-chloroaniline,
phenol, tricresylphosphate (2 isomersl, styrene, 2-methylstyrene and 1,4-
dichlorobenzene. The levels for phenol, 2,4,6-trichlorophenol and 2-chloro-
aniline C39, 10 and 5 ug/1, respectively) were significantly higher than those
for the other detections (see Table 151. The dominant characteristics of con-
centrate C3C were high, levels of poly glycol oligomers and a high concentration
of dibutyl phthalate. As visualized from the GC-MS chromatogram on SP2-100 of
the unpartitioned C3C concentrate, 60 to 80 percent of the concentrate mater-
ial amenable to GC-MS analysis (before methylation of the acids) consisted of
these high concentration materials. Although the separately analyzed concen-
trates (C1P, C1M and C1N) of Pomona I do not allow an exact comparison to this
C3C chromatogram the separate chromatograms indicate that Pomona I was similar
to Pomona III in the level of the poly glycol components. In addition to the
compound identification results described above, the results for the four
GC-MS analyzed fraction were as follows:
104
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• Acid fraction: Surprisingly, clofibric acid was not identified
in CSC although it was found at relatively high levels in all of
the other Pomona I and Pomona II concentrates. 2,4,6-trichloro-
phenol, noted above, was one of the largest GC-MS peaks (RS
value of 5) in this fraction. Many of the 34 compounds identi-
fied were acids containing phenyl substitution, and relatively
fewer fatty acids were present. The largest identified GC-MS
peak was phthalic acid monobutyl ester which was not unexpected
based on the very large amount of dibutyl phthalate present in
the concentrate.
• Aromatic fraction: The compound identification results for the
aromatic fraction were similar to those for concentrate C1P ex-
cept that most of the compounds were present at somewhat lower
levels (i.e., 47 of the 56 compounds had RS values of 1.0).
Most of the identified compounds were alkyl benzenes and
naphthalenes. All three isomers of dichlorobenzene were iden-
tified Cl,4-dichlorobenzene was noted above). Also present
were 2,4,6-trichloroaniline and l-chloro-3-nitro benzene
(tentatively identified).
• Medium and high polarity fractions: These two fractions con-
tained few identifiable compounds beyond the large complement
of poly glycols and dibutyl phthalate. Only 7 compounds were
identified in the medium polarity fraction, and only 2-chloro-
aniline (a search compound, noted above), 3-chloroaniline and
2,6-dimethylpyridine are noteworthy identifications. Only 16
compounds were identified in the high polarity fraction. In
addition to the poly glycols and dibutylphthalate, a relatively
high level of tris—2-chloroethyl phosphate was noteworthy.
Similarly high levels of this compound, which is used as a
flame retardant plasticizer and copolymer, were also found in
the concentrates for Pomona I and Pomona II.
Orange County, California,
January 27, 1976—
The Orange County AWT plant, designated "Water Factory 21", which pro-
duced the sampled water has been the subject of a number of published studies
on the development AWT techniques CIO). All six solvent extracts of RO brines
for this sampling were combined for analysis of the composite concentrate, R1C.
This concentrate represented 104 yg/1 of organic material in the sampled water
(see Table 8) and this value was in the middle of the range observed for AWT
concentrates. The values in Table 8 for the recoveries into the fractions are
somewhat diminished for the acid fraction and somewhat enhanced for the high
polarity fraction compared to average values, but both are well within the
wide ranges observed. The moderately high recovery in the high polarity frac-
tion was principally the result of such an anomalously high level of dibutyl
phthalate that it is nearly inconceivable that this compound was not present
as an artifact. Inspection of the unpartitioned GC-MS chromatograms suggests
that 50 to 70 percent of the organic material in the concentrate which was
amenable to GC-MS analysis (before derivatization of the acids) was dibutyl
phthalate. Other major constituents of these unpartitioned chromatograms were
105
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the plasticizers di-iso-octyladapate and di-iso-actylazelate and a lower than
usual level of poly glycols. Overall, the R1C concentrate can be described as
containing lower concentrations and fewer potentially noxious materials than
most of the analyzed concentrates. In particular, it was nearly pristine in
comparison to the Orange County II concentrate (R2C) which was prepared from a
sampling taken only 6 days following that for RIG (see below). The lack.of
potentially noxious materials is underscored by the result that only one of
the 53 specific search compounds was found in R1C (trichlorobiphenyl, 0.3 ng/1) .
Some possibly noteworthy findings from each of the analyzed fractions are the
following:
• Acid fraction: Nearly every fatty acid from C3 through C2a plus a
number of isomeric fatty acids were detected. A number of benzoic
acid species were also detected: methyl, dimethyl and trimethyl
isomers plus 3-chlorobenzoic acid. Significantly, no phenolic
compounds were identified, although some BHT and BHA related species
were found in the medium and high polarity fractions, and tri-
chlorophenol methyl ether was detected in the aromatic fraction.
• Aromatic fraction: Only 19 compounds were identified in the aro-
matic fraction and all but one of these had RS values of 2.0 or
less. The identified compound with the highest RS value (3.0)
was the methanoindene pesticide, nonachlor. An apparent octa-
chloro analogue of nonachlor was also found but could not be
identified as a specific molecular species. 2,4,5-Trichloro-
aniline, BHT, fluoranthene and fluorene were also identified,
and most of the other species were substituted naphthalenes.
• Medium and high polarity fractions: Many of the compounds
identified in these two fractions C26 and 42 compounds for the
medium and high polarity fractions, respectively, were phthalates
or poly glycols.
Some of the more interesting compounds which contained nitrogen or sulfur
were: dimethyl, trimethyl and dimethyldihydroxy pyridines, trichloroaniline
(also identified in the aromatic fraction), trimethyl-N-nitrosourea, cyclic
maleic diamide, diethyl formamide, an isopropanolyl substituted isoxolidinone,
N-butyl and N-methyl benzene sulfonamide, benzthiazole, isopropyl thiophene,
tetrahydrothiophene dioxide (the solvent sulfolane) and dimethyl sulfone.
Caffeine was the only drug or drug metabolite related material which was
identified.
Some comparitive discussion of the analysis results for the Orange County I
sampling (R1C) with those from the Orange County II sampling (R2C) can be found
in the discussion, below, covering that concentrate.
Orange County, California,
February 3, 1976 (Orange County II)—
The Orange County II sampling was performed at the AWT plant, "Water Fac-
tory 21", only six days after the Orange County I sampling (R1C) which is ad-
dressed in the immediately preceding discussion. As for R1C, all six solvent
extracts of RO brines from Orange County II were combined for analysis as the
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composite concentrate, R2C. This concentrate represented 144 ug or organic
material in the sampled water (Table 8).
The distribution of concentrate material recovered into the fractions for
'.y
R2C appears similar to that observed for RIG except that the values are uni-
formly higher. Upon closer inspection a somewhat curious result in the rela-
tionship between these concentrates becomes clear. The ratio, R2C:R1C, for
the concentration value is 1.38. The corresponding values for the fractions
are 1.36, 1.57, 3.6, and 1.32 for the acid, aromatic, medium polarity and high
polarity fractions, respectively, and the ratio for the overall recoveries is
1.35. Thus, the difference between these two concentrates seems to be that
the approximately 35 percent additional material in the R2C concentrate (com-
pared to R1C) was not only all recovered into the fractions, but it was also
distributed into them in a fashion such that the R2C fraction distribution
was the same as that for RIG. A completely equivalent rationalization would
be that R1C and R2C contained similar recoverable material but that R1C con-
tained relatively less of it (and a correspondingly greater amount of unrecov-
erable material) than did R2C. There are, of course, many other possible
explanations, but examination of the GC-MS chromatograms and the compound
identification results (Table 10) indicate that there are, indeed, some dis-
tinct similarities in chemical makeup between these concentrates, as one might
expect for samplings separated in time by only 6 days. Comparing the compound
identification results (excluding those attributable to the blank) for R1C and
R2C in Table 10 shows that 22 of the 59 compounds (37 percent) identified in
both concentrates had larger RS values for R2C than for RIG while the reverse
was true in only 12 instances (20 percent). Including the possible artifact
compounds yields 32 of 71 (45 percent) detection instances with R2C RS values
greater than those for R1C with 12 instances of the reverse (17 percent).
Certainly the most significant disparity between concentrates R1C and R2C
is the number of identified compounds. Table 8 shows that 234 compounds were
identified in R2C while only 106 were identified in R1C. This disparity is
underscored by the specific search results (Tables 8 and 15) which show that
22 of the 53 search compounds were detected in R2C, but only one of them was
detected in R1C. This detection of 22 compounds exceeded in number that for
any other DW or AWT concentrate. The quantification results in Table 15 for
these 22 search compounds shows that they were all detected at low levels re-
lative to values shown for other AWT concentrates. 2,4,6-Trichlorophenol and
4-chlorophenol were both found at 9 ng/1, and 2,4-dichlorophenol, 2,4-D, and
tricresylphosphate (2.4, 1.6 and 3.9 ng/1, respectively) were the only other
compounds detected at greater than 1 ng/1. The other search compounds found
were pentachlorophenol, 2-chloroaniline, fluoranthene, styrene, 2-methylstyrene,
hexachlorobenzene, 1,4-dichlorobenzene, 1,2,4-trichlorobenzene, triphenyl-
phosphate, 2,4,5-T, lindane, 2-chlorotoluene, heptachlor, tetra-, penta-,
and hexachlorobiphenyls and DDT.
The chromatograms for these two concentrates were similar with the most
noticable differences being distinctly higher levels of poly glycol compounds
and lower levels of fatty acids (relative to aromatic acids) in R2C compared
to R1C. Some of the other differences between the two concentrates involving
specific compounds were:
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• In the acid fraction of R2C, three often encountered water
re-use indicators were identified: salicylic acid, penta-
barbital and phenobarbital. These compounds were not
identified in RIG. While nicotine was also found in R2C
but not R1C, the opposite was true for caffeine
• More organophosphates were found in R2C than in R1C, and
they were found in higher concentrations
• While a.few alkyl-aromatics and halo-aromatics were found
in the aromatic fraction of RIG, a considerably higher
number of these compounds were found in R2C
• In the medium polarity fraction of RIG, three alkyl
pyridines were identified. In contrast, the same fraction
of R2C contained thirteen pyridine isomers (including
pyridine) as well as four quinoline isomers.
Escondido, California,
July 8, 1975—
All six solvent extracts of RO brines for the Escondido sampling were
combined for analysis as the composite concentrates E1C. The values in Table 8
for residue weight analysis of concentrate E1C show that it represents one of
the two lowest concentrations of organic material in the originally sampled
water at 18 yg/1. The extremely low recovery (2.3 percent) into the acid frac-
tion was a distinct departure from the results for other solvent extract
composite concentrates. The only comparably low values were obtained for the
pentane extracts (L2P and C1P) which would be expected to contain very few
acidic species. Inspection of the GC^IS chromatograms of the unpartitioned
concentrate reveals that most (80 to 90 percent) of the material amenable to
GC-MS analysis (before derivatization of the acids) consisted of dibutyl-
phthalate and numerous poly glycols oligomers. This result is in agreement
with the recovery shown for the high polarity fraction (which represents 87
percent of the recovered material) since these materials appear in that
fraction.
The 5 specific search, compounds that were detected were all quantified at
levels ranging from less than 0.1 ng/1 to 0.6 ng/1 (see Table 15). The five
compounds were: pentachlorophenol, 2-chloroaniline, 4-chlorophenol, 2-chloro-
toluene and 4-nitrophenol. In addition, E1C resulted in the fewest number of
identified compounds (40, Table 8) and the lowest levels of these materials
(aside from the butyl phthalate and poly glycols) of all the concentrates
analyzed. The main features of the analyzed fractions were the following:
• Acid fraction: All but 3 of the 24 identified compounds had RS values
of 3 or less. In addition to the specific search compounds, above,
noteworthy identifications were (RS values shown in parentheses):
clofibric acid (4.0), salicylic acid (3.0), phenobarbital (2.0),
phenyldichloroacetic acid (2.0) and 4-chlorobenzoic acid (2.0)
• Aromatic fraction: There were so few sample constituents -at detect-
able levels that the GC-MS chromatograms for this fraction were
108
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essentially indistinguishable from the blank, and the only
compound identified was the specific search compound, 2-
chlorotoluene, cited above
• Medium polarity fraction: 2,5-Hexanedione (RS 4.0), ben-
zaldehyde (RS 3.0) and 2-chloroaniline (RS 1.0, a search
compound, cited above) were the only noteworthy compounds
among the 11 identified. Similarly to the aromatic fraction,
the GC-MS chromatograms were nearly indistinguishable from
the blanks
• High polarity fraction: Beyond the high levels of butyl
phthalate and poly glycols, none of the'23 compounds
identifies warrants discussion. Two isomers of chloro-
alkyl phosphates were found at moderately high levels, but
these two species were not sufficiently well identified for
entry into the data base.
The E1C concentrate was the only one of the AWT series for which the prin-
cipal treatment phase of the AWT plant was the use of RO. The uniquely low
level of acidic materials in E1C was not surprising since RO is expected to
retain ionized species with high efficiency. However, the very high levels of
butyl phthalate and poly glycols found in the concentrate seem inconsistent with
correct performance of the RO unit and, thus, the possibility remains that
these materials may have been present as artifacts.
Dallas, Texas,
November 11, 1974—
Only one of the six solvent extracts of the two RO brines produced from
the Dallas sampling was analyzed. This concentrate, D2N, was the methylene
chloride extract of the acidified cellulose acetate RO brine. The D2N concen-
trate represented 18 pg/1 of organic material in the originally sampled water.
Only the composite concentrate, E1C, contained organic material representing
such a low concentration (see Table 8), although the two concentrates from
Blue Plains I approached that level at 23 and 21 yg/1 for B1M and BIN, respec-
tively.
As expected for an extract from acidified RO brine, most (over half in
this case) of the organic material was recovered in the acid fraction. In
contrast to many of the other AWT concentrates, D2N contained relatively low
levels of poly glycols and phthalates, and this result is reflected by the
somewhat lower relative recovery in the high polarity fraction. This result
was not unexpected, since most of the phthalates and poly glycols should have
been removed from the RO brine during extraction with pentane and neutral
methylene chloride which preceded D2N. The results for these solvent extracts
of the Lake Tahoe and Pomona I samplings (L2P and C1P, respectively) are con-
sistent with this prediction. Thus, the low levels of the nearly ubiquitous
poly glycols and phthalates in D2N cannot be interpreted to mean that they
were not present in the originally sampled AWT finished water.
Similarly to concentrate E1C, described above, concentrate D2N yielded
relatively few identified compounds and low detected levels. While the number
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of identified compounds for D2N was about twice that for E1C, the total amount
of material recovered into the fractions was higher by about a factor of three,
The low levels of materials amenable to GC-MS analysis in D2N is further ex-
emplified by the specific search results. Only two search compounds were
found, and they were both at relatively low levels: 2,4-D and styrene at 1.6
and 1.4 ng/1, respectively (see Table 15). Not surprisingly, more than half
of the compounds were identified in the acid fraction. The following summar-
izes the compound identification results for each fraction of concentrate D2N:
• Acid fraction: Of the 60 identified compounds, 44 had RS values
of 3.0 or less. The largest number of identified compounds were
saturated or unsaturated fatty acids with dimethyl and methyl-
ethyl maleic acids present at a relatively high level. Benzoic
acid was among the components present at the highest levels, and
a number of alkylbenzoic acids were also identified at substan-
tially lower levels. All three isomers of chlorobenzoic acid
C4-chlorobenzoic acid at RS 4.0 as well as 3,4-dichlorobenzoic
acid were also detected. Salicylic acid and clofibric acid were
also identified, but these were present at lower levels than
usually encountered
• Aromatic fraction: The GC-MS chromatograms for this fraction
were nearly indistinguishable from the blanks. Although 19
compounds were identified, 16 of them had RS values of 1.0 or
0.0. Styrene (noted above), phenanthrene, (1,2-dichloro-
ethyDbenzene (probably from chlorination of styrene), and 1,2-
dichlorobenzene were among the identified compounds
• Medium polarity fraction: As for the aromatic fraction, the
chromatograms for the medium polarity fraction were nearly
indistinguishable from those for the blanks, and 11 of the 42
identified compounds had RS values of 1.0 or 0.0. BHT, di-t-
butyl quinone, and dimethylsulfone were among the identified
compounds
• High polarity fraction: Dibutyl phthalate (RS value 5.0) was
the largest identified GC peak, and 26 of the 29 compounds had
RS values of 3.0 or less. Other phthalates and plasticizers,
fatty alcohols, DMF and tris-2-chloroethyl phosphate (RS value
3.0) were also identified.
The very low levels of organic material in the aromatic and medium polar-
ity fractions, noted above, are not unexpected for a concentrate such as D2N
produced by extraction of RO brine after prior extraction steps with pentane
and methylene chloride.
Blue Plains, Washington, B.C.,
September 20, 1974 (Blue Plains I) —
Of the six solvent extracts of RO brine produced from the Blue Plains I
sampling, only two were analyzed in this work: the methylene chloride extract
of cellulose acetate RO brine, B1M, and the subsequent methylene chloride ex-
tract of the same RO brine after acidification, BIN. The Blue Plains I
110
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sampling is not related to the Blue Plains II sampling on May 31, 1975 (dis-
cussed separately, below) since these two samplings are associated with
significantly different AWT schemes Csee Table 2).
The B1M and BIN concentrates represent about the same amount of organic
material in the original water at 23 and 21 yg/1, respectively, but the values
for recovery of the concentrate materials into the fractions (Table 8) indi-
cate some significant differences between these concentrates. BIN contained a
greater relative amount of acidic material, as would be expected based on the
acidic conditions under which it was extracted from the RO brine. B1M resulted
in a lower overall recovery, and this result can be attributed to higher levels
in this concentrate of poly glycols which are not recovered well through the
fractionation scheme. This effect has been observed for other similar concen-
trate pairs (i.e., C1M and C1N) and is supported by the GC-MS analysis results
which show relatively higher amounts of these poly glycol materials in the un-
partitioned concentrate and high polarity fraction for B1M as compared to BIN.
Although the values for residue weight analysis in Table 8 indicate that
there are some significant differences between B1M and BIN, there are far more
similarities than differences with respect to the nature of the organic mater-
ial amenable to GC-MS analysis. This result can be seen both in the compound
identification results and in some distinct similarities between the corres-
ponding chromatograms for these two concentrates for the acid and high polarity
fractions. Comparison of the compound identification results in Table 10 for
B1M and BIN shows that 47 of the 177 compounds (27 percent) were identified in
both concentrates. For comparison, the corresponding value for the concentrates
C1M and C1N was 17 percent.
The relative similarity in the identified compounds for B1M and BIN is
also demonstrated in the specific search compound results. Of the 7 search
compounds identified, 4 were identified in both B1M and BIN: pentachloro-
phenol, phenol, p-cresol and 2,4-dimethylphenol (found in both concentrates);
fluoranthene and hexachlorobenzene (B1M); and 2,4-dichloronaphthalene (BIN).
The quantitative results for these 7 compounds are presented in Table 15.
Examination of the compound identification results of Table 10 shows that most
of the disparities in the results for B1M and BIN are consistent with expecta-
tions based on the sequence of the extraction from the brine (B1M was extracted
first) and the pR of the extraction (unbuffered for B1M and acidic for BIN).
Some of the features of the compound identification results which may be
of interest are listed below:
B1M:
Acid fraction: Normal and isomeric fatty acids were the
largest group of compounds identified. Clofibric and
salicylic acids were identified at moderate levels.
Methylethylmaleic and dimethylmaleic acids were present
at relatively high levels along with the related compound,
methylethyLmaleamide. Phenol and five alkylated phenols
were detected with all three isomers of cresol found at
unusually high levels. Other noteworthy compounds include:
111
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2-aminobenzoic acid, 2-amino-5-chlorobenzoic acid,
p-aminophenylacetic acid and 2,4-dichlorobenzoic acid.
There were relatively few halogenated compounds
identified in the acid fraction.
Aromatic fraction: Only 12 compounds, all at relatively
low levels, were detected, including hexachlorobenzene,
fluoranthene, acenaphthalene and 2-methylnaphthalene.
Medium polarity fraction: Of 22 compounds, 19 had RS values
of 3 or less. Terpin, diethylcarbonate, dimethylsulfone,
acetamide and quinoline were identified .
High polarity fraction: Tris-2-chloroethylphosphate was
found at relatively high levels. Many species of plas-
ticizers (phthalates and others) and poly glycols were
identified at moderately high levels.
BIN:
Acid fraction: The predominant species identified were
nonaromatic carboxylic acids (.18 unsubstituted fatty
acids and 10 unsaturated and/or keto and methoxy fatty
acids). Palmitic, oleic, linoleic and linolinic acids
were the four largest GC peaks. The typical aromatic acids
were also present: benzoic, phenylacetic, salicylic,
phthalic and 2,4-dichlorobenzoic acids. The amino and
amino-halo aromatic acids identified in B1M were not de-
tected. However, six halo-substituted and, therefore,
relatively stronger acids were identified which were
not seen in B1M: chloroacetic, 2,2-dichloropropanoic,
2,2-dichlorobutanoic, trichloroacrylic, 4,4-dichloro-2-
butenoic and 4-chloro-2-butenoic acids .
Aromatic and medium polarity fractions: These two fractions
contained almost no material at all. The highest level
compounds of the medium polarity fraction were ketonesi
some of which remain unidentified but are probably diterpene
related. A number of lactones were also found (N-methyldelta;
N-methy1-gamma; delta; and epsilon) .
High polarity fraction: The usual di-ester plasticizers and
polyglyols were identified, but these were present at dis-
tinctly lower levels than for B1M. A relatively large
number of gamma-lactones, furans, and other cyclic and/or
unsaturated ketones were also detected as well as the natural
product terpin. Tris-chloroethyl phosphate was also identi-
fied but at a far lower level than for B1M.
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Blue Plains, Washington, D.C.,
May 31, 1975 (Blue Plains II) —
All six solvent extracts of RO brines for the Blue Plains II sampling
were combined for analysis of the composite concentrate, B2C. An earlier
sampling at this AWT plant (Blue Plains I, B1M and BIN, see previous dis-
cussion section) was concerned with a different treatment plant sequence, and,
thus, is not related to concentrate B2C. The 46 yg/1 of organic material
which the B2C concentrate represented in the originally sampled water was
comparable to the corresponding composite value (44 yg/1 for concentrates B1M
and BIN (Table 8). However, the distribution of recoveries of the organic
material into the fractions was substantially different for B2C compared to
B1M/B1N .with the B2C acid fraction recovery equal to about one fifth of that
for B1M/B1N and the high polarity fraction recovery for B2C higher by more
than three times that for B1M/B1N. The very high levels of dibutyl phthalate
and poly glycols present in B2C easily account for the predominance of the high
polarity fraction among the others. This results is graphically illustrated
by the strong similarities in appearance of the high polarity fraction chroma-
tograms with those for the unpartitioned concentrate. The chromatograms of
the unpartitioned concentrate suggest that these anomalously high levels of
phthalate and poly glycols account for 70 to 90 percent of the organic material
in the concentrate which was amenable to GC-MS analysis (before derivatization
of the acids).
Six of the specific search compounds were found in concentrate B2C:
pentachlorophenol, 2,4,6-trichlorophenol, tricresyl phosphate, p-cresol and
styrene. Tricresyl phosphate was quantified at 130 ng/1, and this was the
highest level determined for all search compound detections in both DW and
AWT concentrates. The presence of p-cresol in B2C may be related to the high
level of tricresyl phosphate as a hydrolysis degradation product of tricresyl
phosphate either before or after preparation of the concentrate. This hypo-
thesis may be supported by the detection of o-cresol and m-cresol at levels
similar to those for the search compound, p-cresol.
In addition to the distinguishing feature of the tricresyl phosphate, was
the detection of a number of chlorinated and brominated species in the acid
fraction (described below). This array of halo-acids was unique among the AWT
concentrates analyzed. The main characteristics of the analyzed fractions
were the following:
• Acid fraction: Significantly more compounds C83) were
identified in the acid fraction than in the other three
fractions. The most predominant materials were fatty
acids, benzoic acid, and phenyl substituted aliphatic
acids. There were a surprising number of bromo, chloro,
and bromochlorobenzoic acids and phenols detected:
chlorobenzoic, dichlorobenzoic, bromochlorobenzoic,
bromobenzoic and dibromobenzoic acids were identified as
well as dichlorophenol, trichlorphenol, pentachlorophenol,
and tribromophenol. Moreover, an additional 8 bromo, 3
chloro, and 2 bromochloro compounds were detected but it
was not possible to identify these compounds with enough
specificity to enable entry in the data base.
113
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• Aromatic fraction: This fraction contained so few compounds
that the chromatograms were nearly indistinguishable from
the blank. The only two compounds identified were trichloro-
aniline and bromochloroaniline
• Medium polarity fraction: Dibutyl phthalate was the only
compound of the 18 identified that had an RS value greater
than 3.0, and 16 of these 18 compounds had RS values of 2.0
and 1.0. Phenylacetonitrile and di-t-butyl quinone were
the only noteworthy compounds found
• High polarity fraction: Phthalates and poly glycols were
the compounds identified at the highest levels in this
fraction. Tricresyl phosphate, discussed above was the only
other noteworthy compound identified.
Comparison and Discussion of AWT Concentrate Analysis Results
The degree to which the GC-MS Analysis Results Characterize the Sampled
AWT Water—
The degree to which the compound identification results correctly reflect
the organic material present in the sampled water is principally dependent on
three factors: 1. The completeness of recovery of organic material from the
sampled water, 2. The completeness of recovery of the concentrate material
into the analyzed fractions and, 3. The percentage of the material recovered
in fractions which can be successfully analyzed by GC-MS. The effect of each
of these factors is addressed in the discussion below.
In contrast to the DW samplings, extraction of the AWT RO brines with
XAD-2 resin was not performed following the solvent extractions. Thus, no
conclusions can be made concerning the nature of the organic material not re-
covered from the AWT RO brines. However, it can be concluded that most of the
organic material present in the sampled AWT water was not recovered in the
concentrates. Some of the factors which relate to this conclusion are the
following:
• TOG values in Tables 1 and 2 indicate that the sampled AWT
water contained distinctly more organic material (by factors
ranging from 2 to 10) than the sampled DW
« The concentrations which the DW and AWT concentrate material
represented in the sampled water (Tables 7 and 8, respectively)
were, on the average, significantly lower for AWT solvent ex-
tract concentrates than for this type of DW concentrate
• In the corresponding section of the discussion covering the
DW concentrates the conclusion was made (based on the amounts
of material in solvent extract and XAD-2 extract concentrate
pairs) that only 15 to 25 percent of the organic material
contained in the RO brine was recoverable by solvent extraction.
114
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Thus, an even lower fraction of the organic material present in the sampled
AWT water was recovered into the AWT concentrate than was recovered from the
DW source water into the DW solvent extract type concentrates. Taking 6 mg
of carbon per liter as a typical TOC value for AWT water, 0.6 as an approxi-
mate 'weight fraction that carbon represents in the organic material, and
100 yg/1 as a representative value for the concentration of organic material
in the original water represented by an AWT concentrate, the calculated re-
sult is that the organic concentrate represents only 1 percent of the organic
material in the sampled water.
In comparison of the values for overall recovery of AWT concentrate mater-
ial into the fractions (Table 8), no pattern emerges which is dependent on
the type of concentrate or the source of the sampled water. The range of
total percent recovery values for composited extract concentrates and the
composited values for the sets of individually analyzed extract concentrates
(Lake Tahoe, Pomona I and Blue Plains I) ranged from 23 percent for concen-
trate E1C to 81 percent for the four Lake Tahoe concentrates. The presence of
high levels of poly glycol oligomers has been found to reduce overall recov-
eries. This reduction has been attributed to the water solubility of these
materials and their partial loss during aqueous/organic partitioning steps of
the fractionation scheme. Only the concentrates representing Blue Plains I
(B1M and BIN) and Lake Tahoe (L2P, L2M, L2N and L2D) contained low amounts of
these poly glycols, and the recovery values for these two concentrates were at
the upper range of the values found (60 and 81 percent for Blue Plains I and
Lake Tahoe, respectively). In contrast, all of the poly glycol dominated
composite concentrates or sets of concentrates except one (B2C) had overall
recoveries which were lower than the Lake Tahoe and Blue Plains I values but
the percentage recoveries did not correlate well with the relative amounts of
poly glycol material present. In the case of DW concentrates, \ov recovery
into fractions usually correlated with the presence of high levels of humic
material, and this condition was always apparent in the GC-MS data for the
acid fraction as a broad, late eluting profile of unresolved peaks in the
chromatogram. No comparable results were observed for the AWT concentrates
which could be correlated with the results for overall recovery into the frac-
tions. Thus, the extent to which the presence of humic material effected re-
coveries of AWT concentrate material into fractions cannot be assessed.
Certainly, there are other classes of organic material in the concentrates
which are not recovered well in the concentrate fractionation scheme, and the
relative levels of these probably varied widely among the concentrates depend-
ing on variations in the AWT plant feed water and differences in the treatment
modules used at each plant. Thus, the data presently available do not permit
speculation on the nature of the AWT concentrate material which was not recov-
ered in the fractions except that for certain concentrates, part of that
material was probably poly glycols.
It is not possible to unambiguously determine what portion of the AWT con-
centrate fractions was amenable to GC-MS analysis. However, based on the
types of compounds identified, the residue weight results and their corres-
pondence to GC-MS chromatographic profiles, and the residues left on the GC
injector liner following sample injection, the acid fraction was the only
fraction which contained appreciable but highly variable amounts of material
which was not amenable to GC-MS analysis. In contrast to the DW concentrates,
115
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no pattern was observed for the AWT concentrates, and the relative amounts of
material recovered in the fractions which was not represented in the compound
identification results can be estimated to range from a small portion for
some concentrates to less than about one half for certain concentrates con-
taining high levels of acidic material (BIN, D2N, GIN and possibly L2N) .
Compounds Identified in most of the AWT Concentrates—
Table 10 conveniently displays the frequency with which compounds were
detected in the AWT concentrates. As expected, the most frequently detected
compounds are located near the beginning of Table 10. The 16 AWT concentrates
for which Table 10 presents the identified compound results were produced from
10 samplings, as noted in Table 8. For 991 of the 1107 compounds shown in
Table 10, more than half of the detection instances among the 16 AWT concen-
trates were not attributable to the blank. The number of compounds for which
detection instances not attributable to the blank were shown for 5 or more
of the 10 samplings was 65, and, except for 4 compounds, they appear among
the first 390 compounds in Table 10. These 65 frequently identified compounds
can be taken as indicative of the average chemical profile of the AWT concen-
trates, and they are listed below by catagories with the entry sequence number
of each compound in parentheses:
• Methylethyl maleic acid (17) and dimethyl maleic acid (50) were
not successfully identified until after the completion of anal-
ysis of concentrates L2P, L2M, L2N, C3C and C1P. Thus, these
two compounds are not shown as having been detected in those
concentrates. Inspection of some of the acid fraction chroma-
tograms shows these compounds probably were present in a few
cases. This result is not surprising since these compounds
were detected in most of the other AWT and all of the DW con-
centrates. These compounds are monomers used in polyester
(alkyd) resins used in paints and other polymer applications,
so their nearly ubiquitous detection is not surprising
• Although many of the longer chain (C10 to Cia) fatty acids in
Table 10 have been designated as attributable to the blank,
9 shorter chain fatty acids qualify for listing here: valeric,
C5 (204); 2-methylbutyric C202); caproic, C« (71); 2,2-dimethyl-
butyric C102); n-heptanoic (120); caprylic, Ca (33); 2-ethyl-
hexanoic (9); and the alkane diacid, subereric, C8 (91)
• Of the 13 acids containing a phenyl moiety, most were substituted
benzoic acids: benzoic (10); o-, m-, and p-toluic (.30, 15 and
43, respectively); 2,4-, 2,5- and 3,5-dimethylbenzoic (12, 37 and
42, respectively); 2,4,5-trimethylbenzoic (125); o-, m- and
p-chlorobenzoic (53, 123 and 44, respectively); phenyl acetic
C36); 2-phenylbutyric (100); phthalic (111), and monobutyl phthalic
(.36) . The frequent detection of monobutyl phthalic acid should
probably be disregarded since it correlated with the detection of
very high levels of dibutyl phthalate which was suspected as an
artifact. Phenol (208) and p-chlorophenol (209) also qualify as
frequently detected compounds. Other phenols, in particular the
chlorinated phenol search compounds, were also frequently detected,
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but, due to low RS values, most detection instances were
attributed to the blank (see the discussion concerning the
specific search results, following section).
• The list of frequently detected plasticizers was dominated
by phthalates: dibutyl (3), dioctyl (8), methyl butyl (57),
di-isobutyl (81), n-butyl-isobutyl (94) and dimethyl C197).
Di-isobutyl and n-butyl-isobutyl phthalates probably would
not have been classified as frequently detected if the very
high levels of di-n-butyl phthalate had not been present
(see above). The fire retardant plasticizer, tris-2-chloro-
ethyl phosphate (.13) was also frequently detected at high
levels.
• Glycol ethers and poly glycol oligomers were frequently
detected, and 9 species (sequence numbers: 4, 11, 18, 19,
21, 61, 63, -148, and 371) detected in more than half the
samplings.
• 6 Compounds can be classified as organic solvents although
some may have other industrial uses: n-butanol (22), 3-
hexanol (214), benzyl alcohol (268), 2-cyclohexanone (369),
2,5-hexanedione C370) and dimethyl sulfone (.387) .
• 7 Aromatic hydrocarbons, generally found at low levels, may
be due to the presence of fuel oil or other petroleum dis-
tillates in the original water: psendocumene (.337) , naph-
thalene (92), 1-methylnaphthalene (517), 2-methylnaphthalene
(340), l,6-dimethyl-4-isopropylnaphthalene (566), biphenyl
(.346) and fluorene (753).
• 5 Compounds were possibly attributable as chemical industry
effluents: benzoldehyde (160), n-butylbenzene sulfonamide
(131), 2-chloroaniline (186), styrene (334) and 2-methyl-
styrene (802).
• Not surprisingly, 5 domestic sewage indicators were found
among the frequently identified compounds: clofibric acid
(1), salicylic acid (110), ethosuximide (39), phenobarbital
(101) and BHT (34).
Special Interest Compounds—
Computer software (described in Appendix A) was developed to search the
GC-MS data for the 53 compounds of Table 4. Results of the GC-MS data search
for the AWT concentrates are shown in Table 15. Also shown in Table 15 are
other special interest compounds which were identified in the normal course
of GC-MS data interpretation. These additional compounds are the semi volatile
consent decree priority pollutants and the compounds on the EPA "Chemical
Indicators of Industrial Pollution" list. The organization of Table 15 is
parallel to Table 10 with both tables indicating specific search, consent
decree and industrial indicator compounds with the symbols *, +, and $, re-
spectively. In addition, quantification results in ng/1 for the specific
117
-------
TABLE 15. SPECIAL INTEREST COMPOUNDS FOUND IN AWT CONCENTRATES
oo
Seq.
No."
Special
Interest Relative Slzec of GC Peak
Compound
Llstb VIC X1C L2P L2M L2N L2D
C3C
for Detection in the Indicated Concentrate11
C1P
cut
C1N C2N
R1C R2C E1C
D2N B2C BID BIN
COMPOUNDS ON THE SPECIFIC SEARCH LIST (TABLE 4)
(Values In parentheses are ng per liter of original water)
7
162
163
186
208
209
250
270
308
322
334
422
Dlphenylamine
Pentachlorophenol
2,4, 6-Trichlorophenol
o-ch loroanlllne
Phenol
p-Chlqrophenol
Tricresyl phosphate
2,4-D
p-Cresol
Fluoranthene
Styrene
2 ,4-Dlchlorophenol
* 5.2 1.6
(1.5) (0.01)
* + $ 0.0 5.0 l.Ot
(0.2) (17) (5.2)
* •»• $ -0.2 l.Ot
(0.3) (3.9)
* 3.2 2.0
(0.6) (2.7)
* + 4.0 4.0 5.0
(1.1) (8.5) (23)
* $ 1.0 1.0 3.0
(1.6) (8.1) (100)
A
*
* 0.2
(0.01)
* + $ -2.0 l.Ot
(0.3) (0.2)
* $ 4.0 2.0 1.0 '0.0
(0.9) (1.0) (0.4) (— )
* + $
1.
(0.
0
1)
8
(9
4
.0
.8)
.Ot
(44)
5.
(9.
2.
(4.
3.
0
6)
0
5)
0
(39)
2.
(1.
1.
(0.
0
7)
0
8)
3
(1
3
(3
2
(4
4
(3
2
(0
.0
.6)
.0
.9)
.0
.8)
.0
.4)
.0
.7)
3.1
(2.2)
4.0t
(10)
5.0
(25)
5.0
(20)
5.0
(16)
l.Ot
(0.2)
1.0
(1.4)
4.0
2.0
(0.1)
4.0t 5.0
(6.8) (11)
2.0t 4.0
(2.4) (1.3)
5.0 5.0
(11) (4.6)
4.0
(55)
5.0
(70)
1.
(0.
4.
(9.
1.
(1.
1.
(9.
1.
(3.
1.
(1.
2.
Ot l.Ot
1) (0.0)
0
1)
0 1.0
0) (0.6)
0 2.0
0) (0.3)
0
9)
0
6)
Ot
(0.8)
2.0
(0.6)
1.0
(0.5)
1.0
(— ) (2.4)
591
775
802
821
834
2 , 4-Dloethylphenol
Chrysene
2-Hethyl styrene
Hexachlorobenzene
p-Dlchlorobenzene
* + 1.0
(2.0)
* + 2.0
(5.1)
* 1.0 1.0 1.0
(0.01H0.6) (0.1)
* + $ 1.0
(0.1)
* + $
1.
(0.
0
1)
1
(0
.0
.6)
2.0
(0.6)
1.0
(0.01)
836
Tri-m-cresyl phosphate
*
1.0 1.0
(0.3) (0.1)
2.0 1.0
(3.4) (1.6)
2.0
(0.6)
l.Ot l.Ot l.Ot
(0.7) (0.2) (0.4)
l.Of
(0.2)
3.0 3.0 3.0
(3.6) (0.6) (6.7)
5.0
(130)
2.0
(1.6)
4.2t 4.0t 3.0t
(16) (79) (49)
l.Ot
(0.9)
1.0
(1.4)
1.0
(0.8)
3.0 1.0
(8.9X1.0)
1.0
(0.1)
1.0
(0
1
(0
.6)
.0
.2)
1.0
(0.7)
2.0
(0.8)
840
996
1014
1017
1034
1 , 2 ,4-Trichlorobenzene
H-nltroanlline
Trlphenylphosphate
p-Chloroacetophenone
2,4,5-T
* *• 5
* 1.0
(0.5)
*
*
*
2
(0
1
(1
.0
.7)
.0
•3)
1.0
(7.5)
1.0
(0.1)
1
(0
1
(3
1
.0
.1)
.0
.4)
.0
(0.5)
1035
Trlchloroblphenyl
ft
1.0
(0.3)
(continued)
-------
TABLE 15. (Continued)
Seq.
No.*
1037
1038
1039
1040
1041
1042
1044
1069
1082
26
77
92
164
172
173
306
324
380
511
523
528
616
620
621
649
744
750
753
951
1043
3
8
41
57
69
81
82
Compound
Llndane
o-Chlorotoluene
Heptachlor
Tetrachloroblphenyl
Pentachloroblphenyl
Hexachloroblphenyl
DDT
p-Nltrophenol
2 , 4-Dlchloronaph thalene
COMPOUNDS HOT ON THE SPECIFIC
1,1,2,2- Te trachloroe thane
Phenanthrene
Naphthalene
Pyrene
Ethylbenzene
p-Xylene
1,2-Dlchloroethane
Toluene
Anthracene
m-Xylene
Cumene
o-Dichlorobenzene
i»-Dlchlorobenzene
2,3, 4 ,6-Te t rachlorophenol
2,4, 5-Trichlorophenol
o-Chlorophenol
Acenaph thalene
o-Xylene
Fluorene
n-Propylbenzene
DDE
PHTHAL1C ACID DIESTERS
Dl-n-butyl phthalate
Dloctyl phthalate
Butyl butoxyethyl phthalate
Butyl methyl phthalate
Dlethyl phthalate
Diisobutyl phthalate
Dlcyclohexyl plithalate
Special
Interest
Listb VIC lie
* $
*
* + $
* + $
* + $
* + s
* + $
*
*
SEARCH LIST
$ 5.0
+ -1.0
$ 4.0
$ 4.0
$
$ 3.0
+
$
$
+ $
+ $
$
$
$
+ 2.0
$
•i
5
+ $
+ $ 2.0
+ $
$
$
+ $ 1.0
$
$ 3.0
Relative Size' of fir Peak for Detection In the Indicated Concentrate1'
L2P L2M L2N L2B C3C C1P C1M C1N C2N R1C R2C E1C D2N
1.0
(0.2)
1.0 1.0
(0.2) (0.2)
1.0
(0.5)
1.0
(0.1)
1.0
(0.2)
1.0
(0.1)
1.0
(0.2)
1.0
(0.1)
3.0t 3.0t 7.0t 6.0t 6.0t o.Ot
2 Ot l.Ot O.Ot 6.0 2.0t 2.0t 2.0t 3.0t 3.0t
1 o 4.0 6.0 6.0 1-0 1.0
3.0 5.0 l.Ot
5.0t 2.0t O.Ot 1-°t
5.0t 2.0t O.Ot 1-°t
A n
4.6 *-°
4.0t l.Ot *-°t 4'°t
1.0 1.0 4.0
•> n 3 O 3 0 1.0
3.0 j.uj."
3.0 1.0 1.0
2.0 1.0 3.0
1.0 3.0
3.0
3.0
O.Ot 1-Ot !-°t O.Ot
i n
2.0 1-°
1.0 1.0 1.0 2.0 2.0
1'° i.o i.o
9.0 5.0t 7.0 5.0t 9.1 3.0t 3.6t 8.1 7.1 7.0 5.0t
,- f. n 8070
6.0 6-0 "•" '•"
7.0
4.0 3.0 7.0 4.0 4.0 3.0 1.0
3 ot 2.0t 5.0 6.0 3.0t
5.0 4.0t 6.0 2.0 3.0t 5.1 6.0 3.0t
2.6 1 6'°
B2C B1M BIN
1.0
(0.9)
4.0t O.Ot
1.0
l.Ot
o-.et o.ot
2.0
8.1 6.0t 5.0t
2.0
4.0
6.0
5.0
5.0t 5.0t
(continued)
-------
TABLE 15. (Continued)
Seq.
No > Compound
83 Bls(2-ethylhexyl) phthalate
94 n-Butyl Isobutyl phthalate
97 Methyl ethyl phthalate
158 Butyl benzyl phthalate
197 Dimethyl phthalate
332 Butyl butoxycarbonyl phthalate
368 Dimethyl terephthalate
396 t-Butyl methyl phthalate
678 Dl-n-propyl phthalate
1091 Dlhexyl phthalate
a) The sequence number corresponds to
Special
Interest
List"
+ $
$
$
•*• 5
$
$
$
$
$
$
the entry
:e coded:
f
VIC X1C UP
2.6
5.0
5.0
5.0
4.0
0.0
in Table 10.
*: list of 53 com
L2M L2N L20 C3C C17 CLM C1N C2N R1C R2C E1C D2N B2C B1M BIN
2.0 2.0 6.0 1.0 6.0 2.0 3.0 5.0
6.0 3.0 6.0 3.0 6.0
6.0
S.O 1.0 4.0 2.0 5.0
4.0 1.0 4.0 4.0 2.0 4.0 4.0
4.0
4.0 2.0
4.0
3.0
DOunda for which the GC-MS waa fioeciflcallv searched fsee Table 41. +: licit of "Consent
c)
d)
Decree Priority Pollutants." £: list of "Chemical Indicators of Industrial Pollution" Federal Interim Primary Drinking Mater Regulations (February 9
1978).
See Section 5, Analytical Schema/Quantification of Identified Compounds for an explanation of the Relative Size Parameter.
See Tablea 8 and 2 for translation of the three digit concentrate code names. The symbol, t. designates a detection instance that may be attributable
to the concentrate generation blank.
N5
O
-------
search compounds (not shown in Table 10) are shown in parentheses below the
US value entry in Table 15. Phthalates are listed separately in Table 12 to
facilitate visualization of occurrence patterns for these high interest com-
pounds .
The three samplings which reflected the highest levels of organic com-
pounds in the sampled water (Pomona I, Lake Tahoe, and Orange County II at
370, 306 and 144 yg/1, respectively) also resulted in the detection of the
highest number of search compounds at 16, 13 and 22 detections, respectively,
as above. There are 117 detection instances shown for the 33 search compounds
listed in Table 15; 10 of the 33 compounds account for 78 (67 percent) of
those 117 detection instances; and 14 of the compounds were detected in only
one concentrate. Table 15 also shows the specific search results for the
Poplarville, VIC, DW concentrate since it functioned as the RO process blank.
The detection of four compounds in concentrate VIC has resulted in the class-
ification of 20 of the AWT concentrate detection instances as possibly
attributable to the RO process blank, as indicated by the symbol, t. Since
concentrate VIC does correspond to a sampling of finished DW instead of
reagent water the possibility remains that these 4 search compound detections
in VIC were present in that sampled water rather than introduced by the RO
process. Thus, the 14 compounds designated as possibly due to the blank may,
indeed, represent genuine detection instances. The search compounds for which
some of the detection instances were at relatively high levels (10 ng/1 or
higher) were diphenyl amine, pentachlorophenol, 2,4,6-trichlorophenol,
2-chloroaniline, phenol, tricresyl phosphate and 2,4-D. In the section of
Table 15 showing the detection instances for phthalates, those concentrates
showing extremely high levels of dibutyl phthalate are L2P, L2N, C3C, R1C,
R2C, E1C and B2C. In preceding discussions, the dibutyl phthalate detections
in these-concentrates were noted as probably artifacts. Since the source of
the dibutyl phthalate contamination was probably an impure one, some of the
other phthalate detections listed (especially iso-butyl and mixed, monobutyl
ones) are probably also artifacts.
Occurrence of Molecular Functional
Groups in the Identified Compounds—
Associated with each identified compound entered in the computer-managed
data base are a set of molecular functional group descriptors. Tabulations
of the occurrences of the 25 functional groups in the AWT concentrate results
is presented in Tables 16 and 17. Percentages which each of the 25 function-
al group classes represent of the total number of identified compounds are
shown in Table 16. Display of the percentage of the total parameter in Table
16 was chosen to facilitate comparison of the relative distribution of the
functional groups among the analyzed concentrates. Thus, Table 16 provides
comparative information on the numbers but not the amounts of compounds
with the various function groups. Total RS values for each functional group
are shown in Table 17, and this parameter reflects the amounts of material
for each functional group rather than the number of occurrences. Thus,
these two tables are complimentary in the nature of the information provided.
Note that the total number of identified compounds for each concentrate has
been added to Table 16 to enable computation of the number of functional
group occurrences from the percentages shown. Since these computer-printed
tables (Tables 16 and 17) are generated from the data base before correction
121
-------
S3
Ni
TABLE 16. OCCURRENCE OF MOLECULAR FUNCTIONAL GROUP TYPES IN AWT CONCENTRATES, SHOWING THE
NUMBER OF OCCURRENCES AS A PERCENTAGE OF THE TOTAL NUMBER OF IDENTIFIED COMPOUNDS
OCCURRENCE OF FUNCTIONAL GROUPS AMONG THE IDENTIFIED ORGANICS
PERCENT OF TOTAL
1. UNSUBSTITUTED ALIPHATIC
2. HALOGENATEO ALIPHATIC
3. SUBSTITUTED ALIPHATIC
4. UNSUSBSTITUTEO ALICVCLIC
5. HALOGENATEO ALICVCLIC
6* SUBSTITUTED ALICVCLIC
7. UNSUBSTITUED AROMATIC
a. HALOGENATEO AROMATIC
9. SUBSTITUTED AROMATIC
10. UNSUBSTITUTEO PNA
11. HALOGENATEO PNA
12. SUBSTITUTED PNA
13. ALCOHOL GROUP
lit. ALDEHYDE GROUP
15. AMIDE GROUP
16. AMINE GROUP
17. CARBOXVLIC ACID
18. ESTER GROUP
19. ETHER GROUP
20. HETEROATOH IN RINS
21. KETONE
22. NITRO GROUP
23. PHTHALIC DI-ESTER
2<.. PHENOL GROUP
25. SULFUR ATOM
TOTAL NUMBER OF IDENTIFIED
COMPOUNDS
VIC X1C L2P L2N L2N L20 C3C C1P C1H C1N C2N RtC R2C E1C D2N B2C BIN BIN
3
0
51
0
0
r
10
7
27
5
2
2
22
2
0
5
25
3<.
3
8
10
10
3
0
It
5<»
0
0
12
a
0
12
6
0
2
25
2
0
0
25
10
10
4 9
Ic
15
2
0
0
1
2
19
3
0
7
55
2
15
35
0
2
13
1
0
2
7
13
6
%
3
J»
0
2
2
It7
0
0
lit
6
2
29
it
0
3
20
2
0
1
29
17
16
t.
*»
16
5
2
1
11
1
31
5
0
9
20
it
29
12
0
3
17
1
1
2
26
6
11
8
2
8
3
3
2
3
-------
TABLE 17. OCCURRENCE OF MOLECULAR FUNCTIONAL GROUP TYPES IN AWT CONCENTRATES, SHOWING THE
TOTAL GC PEAK SIZE FOR EACH GROUP ON BOTH GC COLUMNS
OCCURRENCE OF FUNCTIONAL GROUPS AMONG THE IDENTIFIED ORGANICS
1. UNSUBSTITUTEO ALIPHATIC
2. HALOGENATEO ALIPHATIC
3. SUBSTITUTED ALIPHATIC
-------
for the blank, the total numbers of identified compounds shown in Table 16 are
also uncorrected for the blank.
For 13 of the functional group classifications of Table 16, the percent
occurrence values are either low or there is not sufficient variation in them
among the AWT concentrates to require any discussion. These 13 classifications
are: unsubstituted aliphatic, halogenated aliphatic, unsubstituted alicyclic,
halogenated alicychic, halogenated PNA, substituted PNA, aldehyde group, ester
group, amide group, amine group, nitro group, phenol group, and sulfur atom.
Observations concerning the remaining functional group types are the following:
• Comparing the molecular nucleus classifications, substituted
aromatic, substituted alicyclic and substituted aliphatic,
shows that, for the non-halogenated species, non-aromatic
molecular nuclei! were more numerous than aromatic molecular
nuclei! in all concentrates except E1C and C3C. Large
numbers of phthalates, which are classified as containing
an aromatic nucleus, partially explain the exceptions for
E1C and C3C (see the discussion, below, on the phthalate
functional group) .
• The high values shown for unsubstituted aromatic and unsub-
stituted PNA for concentrates L2P, C3C and C1P are related to
the high numbers of alkyl benzenes and naphthalenes that were
identified in the aromatic fractions of these three concen-
trates. In the assignment of functional groups, molecules
with only alkyl (or alkenyl) substitution are classified as
unsubstituted, and aromatic ring systems larger than benzene
are classified as a PNA molecular nucleus .
• Concentrates R1C and E1C have marginally higher occurrence
percentages for the halogenated molecular nucleus, and the
Lake Tahoe and Blue Plains I concentrate sets are somewhat
below average for this value .
• Little variation was observed for 'the relative numbers of
identified alcohols except for the Blue Plains I and II
concentrates (B2C, B1M and BIN) which are significantly above
the average. The higher proportion of alcohols for these
three concentrates can partially be attributed to a greater
variety of poly glycols among the identified compounds .
• The carboxylic acid substituent group was the predominant
one found for all concentrates except the two prepared by
pentane extraction of the RO brine (L2P and C1P). This re-
sult was not surprising based on the polarities of the
extraction solvent. In two of the three cases for which both
the unbuffered methylene chloride and the acidified methylene
chloride extracts were analyzed (L2M/L2N, C1M/C1N and B1M/B.1N)
a slightly higher proportion of carboxylic acids were identified
in the concentrate from the unbuffered extract (L2M and C1M) .
124
-------
This result is in contradiction to the expected one, and is
addressed in a subsequent section of this volume .
• Slightly elevated detection frequencies for the heteroatom in
ring functionality in concentrates C1M, C1N and C2N reflect
detection of the following materials: barbiturates (four
species in C1M, one in C1N), saccharin (C2N), ethosuximide
(C1M), pentachloropyridine (C1N), caffeine (GIN), nicotine
(C1M), quinolines (C2N), isoquinolines (C2N), pyridines (C1M
and C2N), piperidines (C2N), pyrimidines (C2N), and pyrroli-
dines (C2N).
• The percentages of compounds with the ketone goup were
slightly elevated for about half the concentrates (L2M, L2D,
C1M, GIN, E1C, B1M, and BIN).
• The two concentrates (C3C and E1C) in which the artifact
level of dibutyl phthalate was the highest show distinctly
higher percentages of the identified compounds were phtha-
lates (i.e., in addition to dibutyl phthalate). This results
from two effects: 1. The dibutyl phthalate concentration
was so high that the accompanying impurity levels of seldom
encountered phthalates were at easily detectable levels, and
2. The phthalate chromatographic overloading resulted in
less effective identification of other compounds, reducing
the total number of identifications.
Since RS values span a logarithmic scale, the total RS value shown in
Table 17 is not an arithmetic sum of the individual RS values since such a sum
of logarithmic scale values would be mathematically related to the product of
individual GC peak heights rather than the sum of them. For example, 10 GC-MS
peaks, each with an RS value of 1.0 would give a total RS value of 3.0, and
two peaks with RS values 2 and 8 would yield a total RS value of 8.0009. The
mathematical basis of the GC-MS peak RS parameter is detailed in Section 5,
Analytical Scheme. For the purposes of interpreting Table 17, it suffices
that an arithmetic difference of 1.0 between two total RS values in the table
under comparison corresponds to a factor of one-half of an order of magnitude
(3.16) change in the amount of material represented; a difference of 2.0 in
total RS values corresponds to a factor of one order of magnitude (10.0), and
so forth.
The AWT concentrate functional group results, expressed as the total RS
value for each classification catagory, are shown in Table 17. Some of the
characteristics of the AWT concentrates which the values in Table 17 reflect
are discussed below.
The predominant type of molecular nucleus (catagories 1-12, Table 17) were,
as expected, the substituted aliphatic and substituted aromatic catagories with
these taking the highest and second highest total RS values for each concen-
trate. Although 10 of the 16 concentrates have the substituted aliphatic cat-
agory with highest total RS value (an eleventh, C1P, had equal total RS values
125
-------
for the two nucleus types) this predominance probably does not reflect the
organic material present in the original water since 8 of those 10 concentrates
are the separate methylene chloride extracts of RO brine (C2N, D2N, L2M/L2N,
C1M/C1N and B1M/B1N) and the prior extraction of RO brine with pentane had re-
moved a significant portion of the aromatic material. For 3 of the 4 composi-
ted concentrates (B2C, E1C and R1C), the substituted aromatic nucleus had the
highest total RS value. For the 2 pentane extract concentrates, L2P had the
substituted aromatic nucleus with the highest total RS and C1P had the sub-
stituted aliphatic and aromatic nucleii with equal total RS values. On the
other hand, high levels of dibutyl phthalate (classified as containing the
substituted aromatic molecular nucleus) exerted a controlling influence on
concentrates R1C, E1C, B2C and L2P. The high levels of poly glycols (classi-
fied as the substituted aliphatic nucleus) exerted a similar controlling effect
for concentrates L2M, L2N, C1M, C2N, R2C, D2N, B1M and BIN. If both the butyl
phthalate and poly glycols were present as artifacts, no conclusion concerning
the predominant type of molecular nucleus in the original water can be made.
The halogenated aromatic nucleus was ranked with the third highest total RS
value in 7 cases (L2M, C1M, GIN, C2N, R1C, E1C and D2N) and fourth highest in
3 cases (L2D, C3C and BIN).
In the 13 catagories of substituent groups (13 through 25 in Table 17),
the presence of very high levels of butyl phthalate and poly glycols exerts an
obscuring effect similar to that noted above for the type of molecular nucleus.
Butyl phthalate contributed to the total RS values for the ester and phthalate
groups, and these two groups have the highest two RS value rankings for con-
centrates L2P, R1C, E1C and B2C which contained dibutyl phthalate at high,
artifact levels. Poly glycol compounds were classified as containing the ether
and alcohol functional group, and these two groups were among the 5 highest
total RS values for all concentrates except C1P. Eight concentrates (L2M, L2N,
C2D, C1M, GIN, C2N, B1M and BIN) had the alcohol and ether group as two of the
3 highest total RS value substituent groups, and, in all but one case (L2N) ,
the carboxylic acid substituent was the other group of the three. The carbo-
xylic acid group was among the 5 with highest RS values for all concentrates
except C1P and C3C. Ketones had the fourth highest total RS value for 5 con-
centrates (.L2M, L2D, GIN, B1M and BIN) and the fifth highest in one case (C1M) .
The heteroatom in ring group had the fourth highest total RS value in concen-
trate C1M and the fifth highest value in concentrates C1P, GIN and C2N. The
compounds which contributed significantly to the heteroatom in ring total RS
values for these four concentrates were (in decreasing order of RS values):
benzthiazole (all four concentrates), barbiturates (C1M and C1N), saccharin
(GIN, C2N), dimethyldihydroacridine (.C1P), methoxbenzis:othiazole (C1M), benz-
isothiazolone (C1M), a reduced keto-azepine (GIN, quinolines and isoquinolines
(C2N and C1P), ethosuximide (C1M), caffeine (C1N), nicotine (C1M), dimethyl-
indole (C1M), a reduced pyridine (C2N), and N-propyl succinamide (C1P).
The substituent groups which were among the three for each of the 16 con-
centrates with the lowest total RS values were distributed as follows:
126
-------
Number of Concentrates for which the
Indicated Functional Group was Found
Functional Group Among the Three Lowest Total RS Value
amide 14
aldehyde 13
amine 11
sulfur atom 5
phthalic diester 3
nitro 2
ketone 2
ether 1
ester 1
Four additional functional group tables for the AWT concentrates are pre-
sented in Volume 2. Three of these tables show the number of occurrences, the
total RS parameter for SP100Q GC-MS analysis and the total RS parameter for
SP2100 GC-MS analysis- using a format identical to Tables 16 and 17. The fourth
table shows all five parameters for each concentrate (i.e., those of Table 16
and Table 17 plus the other three cited above) in close proximity groupings
for each concentrate to facilitate simultaneous comparison of all five para-
meters between concentrates.
The Effect of Concentrate Production Methodology on the Compound Identifica-
tion Results—
The 16 AWT concentrates analyzed were produced using RO preconcentration
as the first step (with cellulose acetate and nylon units processing the water
in series) followed by liquid-liquid solvent extraction of the two RO brines
produced for each concentrate (see Section 4). Four of the concentrates were
a composite of all six solvent extracts of RO brine (C3C, R1C, E1C and B2C)
and the other 12 concentrates were individual extracts of RO brine. Based on
the compound identification results, some conclusions can be made regarding
the types of compounds that can be recovered in the separate RO brine extracts.
Concentrate L2D was the only separate RO brine extract analyzed that was
produced from the nylon unit RO brine. If the cellulose acetate RO unit had
retained all of the organic materials in the sampled water, concentrate L2D
should have been devoid of organic compounds. The listings of Tables 7, 9 and
17 show that just the opposite was the result, and concentrate L2D contained
comparable amounts of material (relative to L2M and L2N) amenable to GC-MS
analysis. Analysis of additional concentrates enabling comparison of cellu-
lose acetate' and nylon RO extract pairs would be required to determine whether
the anomalous L2D results were caused by some malfunction of the cellulose
acetate RO module or whether they correctly reflect a very poor performance
capability for the cellulose acetate RO unit. Obviously, correctness the
latter possibility would have a serious impact on this work.
127
-------
As expected, the first RO brine extract, using pentane, contained more
apolar materials (especially aromatic hydrocarbons) and less strongly polar
material, (especially carboxylic acids) compared to the two methylene chloride
extracts. The pentane concentrates (L2P and GIF), nevertheless, contained sur-
prisingly high levels of many moderate polarity neutrals. Comparison of the
total RS values for concentrates L2P and C1P in Table 17 with other methylene
chloride extract concentrates adequately illustrates this point. These sur-
prisingly high, recoveries of polar species'may have been due to the strong
salting out effect of the. RO brine ionic strength combined with the mass action
effect of the high levels of organic material present in the aqueous phase.
Addition of an ethanol or methanol back extraction of the partially concen-
trated pentane extract with re-combination of the alcohol phase and the RO
brine would have produced a pentane concentrate containing lower levels of
polar species.
The compound identification results indicate that the RO brine extraction
procedure of unbuffered methylene chloride extraction failed to produce the
expected result of recovery of acidic materials preferentially into the latter
extract. The concentrate pair B1M/B1N illustrates this failure clearly, and
comparison of the other pairs, L2M/L2N and C1M/C1N, give essentially the same
results. The GC-MS chromatograms of the acid, medium polarity and high polar-
ity fractions of B1M and BIN were so similar that they could almost be super-
imposed in most regions. Not surprisingly, there was a high degree of cor-
respondence between the sets of compound identification results for B1M and
BIN. The principal differences were that the pH 2 extract, BIN, contained
more or higher concentrations of higher strength or more polar acids. Sur-
prisingly, many acids were recovered better or exclusively in the unbuffered
extract, B1M (for example, clofibric acid, 2-ethylhexanoic acid and ethosuxi-
mide). One explanation for these results would be that the unbuffered pH was
more acidic than the pE 5.5 reported for cellulose acetate RO processing (pH
10 was used for the nylon RO unit). An uncontrolled pH for the first
methylene chloride extraction would account for the variability of acid species
enhancement for the pH 2 extract (compare total RS values in Table 17 for the
carboxylic acid group and the identified compounds in Table 10 for concentrate
pairs L2M/L2N, C1M/C1N and B1M/B1N).
The near exclusion of basic species from the compound identification re-
sults probably was due to a failure of the concentrate production system to
recover these species. Most of the compounds which contributed to the amine
group total RS values in Table 17 were of very low base strength (for example,
diphenylamine was found with RS value 8.1 in concentrate C1P1. While the pro-
tonated bases would probably have been retained efficiently by the cellulose
acetate RO unit (operated at pH 5.5), these species would have been very poorly
recovered by extraction from the cellulose acetate RO brine since no extrac-
tions were performed at basic pH. Bases which permeated the cellulose acetate
membrane and were retained by the nylon membrane (operated at pH 10) could
have been recovered by the first and second extractions (pentane and unbuffered
methylene chloride), and these circumstances may account for the small number
of basic species that were, observed. An alternative recovery mechanism would
be an ion pair extraction mechanism during the unbuffered cellulose acetate
methylene chloride extraction.
128
-------
One unfortunate effect of the concentrate production method had on the
analysis results was the apparant contamination of certain concentrates
(Pomona I, P.omona III, Escondido, Orange County I and Blue Plains II) with
very high levels of dibutyl phthalate. The presence of similarly high levels
of poly glycol materials in some of the concentrates did not correlate with
the phthalate artifact, but the levels of these poly glycol materials varied
over such an extremely wide range that they must also be considered as possible
artifacts. However, since use of these materials in soaps, cosmetics and oint-
ments is common, they are expected at relatively high levels in sewage, and
the variability of their levels in the concentrates might be explainable in
terms of variations in AWT plant performance. Since these poly glycols are
hydrophilic, they might be among the first of the organic materials to break
through a GAG contactor as the adsorption capacity is consumed.
Effect of the Raw Water Source on the Analysis Results—
Apparantly, the effectiveness of the AWT plant exerted a greater control-
ling influence on the organic material present in the AWT concentrates than
did the nature of the plant influent water since there are no obvious correla-
tions between the source water (described in Table 2) and the compound identi-
fication results. In addition, no conclusion can be made concerning the
effect the time of year of sampling had on the nature of the concentrate since
all of the multiple samplings at significantly different times of year at a
given site (Pomona and Blue Plains) corresponded to a change in the AWT plant
design. The only noteworthy observation in this regard was that a variety of
oxygenated diterpene compounds were found in the Lake Tahoe concentrates
(especially L2P), but these compounds are probably more related to precipita-
tion run off than wastewater discharges. With regard to the AWT plant effect-
iveness, the analysis results indicate that the Escondido AWT plant, which was
based on RO treatment rather than GAG contactor treatment as for all the other
plants (.see Table 2) , produced product water containing substantially less
organic material than the other plants. Comparison of the results shown in
Table 8 for E1C with those of the other AWT concentrates adequately documents
this conclusion.
COMPARISON OF DW AND AWT CONCENTRATE COMPOUND
IDENTIFICATION RESULTS
In Section 6, Overview, some conclusions regarding the comparison of DW
and AWT concentrates were reached on the basis of the information presented
in Tables 7 and 8. Those conclusions are briefly summarized below:
• Of the organic material recovered in the analyzed fractions, most
was contained in the acid and high polarity fractions (averages of
94 and 97 percent for DW and AWT concentrates, respectively).
• The percentage of the original concentrate material which could be
recovered into the analyzed fractions was about the same for DW
and AWT concentrates, averaging 52 percent for both.
• The relative amounts of the material (versus the original concen-
trate) recovered in the acid and high polarity fractions for DW
and AWT concentrates was substantially different, with DW
129
-------
concentrates averaging 32 and 18 percent in the acid and high
polarity fractions, respectively, and AWT concentrates aver-
aging 16 and 33 percent for the acid and high polarity fractions,
respectively.
• On the basis of the concentration in the original water that the
concentrates represented, the DW concentrates were consistantly
and, in some cases, higher than the AWT concentrates.
Comparison of the tables listing the total RS values for 25 functional
groups for the DW and AWT concentrates (Tables 14 and 17, respectively) shows
that carboxylic acids and phenols represented higher concentrations of com-
pounds in DW concentrates than these functional groups did in AWT concentrates.
The average values are 8.1 versus 7.0 for carboxylic acids and 5.6 versus 5.02
for phenols for the 7 composited solvent extract type DW concentrates versus
the 5 composited solvent extract type AWT concentrates. Thus, these compari-
sons agree with the relatively higher amount of material in the DW concentrate
acid fraction compared to the AWT concentrate acid fraction.
A predominant feature of the AWT concentrates was a variable but usually
very high level of poly glycols. This class of compounds was recovered in the
high polarity fraction, accounting for the higher portion of the AWT concen-
trates, relative to the DW concentrates, recovered in that fraction. While
poly glycol species were usually represented in the DW concentrates, none of
them approached the very high levels observed for the AWT concentrates. The
total RS values for the ether functional group in Tables 14 and 17 reflect the
higher amounts of these poly glycols in the AWT concentrates. The average
total RS values for the ether group were 7.5 and 7.2 for the AWT and DW con-
centrates, respectively, as above. The ether group is less sensitive for
demonstrating the presence of poly glycols than is the carboxylic acid group
for the amount of material in the acid fraction since other compounds commonly
encountered at high levels (for example, clofibric acid) also contain the ether
linkage. The significance of the ether group total RS values cited above is
reinforced by similarly comparing the ketone functional group which is also
encountered predominantly in the high polarity fraction. The average total RS
values for the ketone group are 4.9 and 6.9 for the AWT and DW concentrates,
respectively. Note also that the poly glycol compounds that are identified
specifically enough for entry into the data base are lower molecular weight
oligomers which represent only 5 to 10 percent of the GC-MS peak areas of the
higher molecular weight poly glycol oligomers. Although these higher molecular
weight oligomers were observed in the GC-MS data, they were not specifically
identified, on a molecular basis and, thus, did not contribute to the ether
group total RS values in Tables 14 and 17-
The compound identification results for both the DW and AWT concentrates
are shown is a single, integrated listing in Table 11 (note, some of the con-
centrates have been omitted from Table 11 due to space limitations; see the
relevant discussion .in Section 6, Overview). Table 11 facilitates the com-
parison of DW and AWT compound identification results on the basis of frequency
and levels of detection for each compound. Most of the compounds listed in
Table 11 have relatively isolated detection instances which cannot reasonably
be used to infer a pattern of occurrence in the sampled water. The compounds
130
-------
which- do have a sufficient number of detection instances in Table 11 to just-
ify classification as predominantly occurring in either DW or AWT water or
both have been assembled in Table 18 to further facilitate comparison of the
types of compounds identified in DW and AWT concentrates. The compounds
shown in Table 18 have been listed in the order that they appear in Table 11
and arranged on the page to spatially approximate the position of occurrence
in Table 11. In addition, the glycol ethers and poly glycol compounds have
been omitted from Table 18 since there are so many of these species and care-
ful attention was not taken to maintain consistency in their identification
assignments (all of which were intentionally left tentative). Some of the
conclusions which can be drawn from Table 18 are the following:
• DW concentrates show a greater tendency for recurring detections
of compounds with 39 compounds indicated as identified principally
in DW concentrates and only 12 compounds indicated as identified
principally in AWT concentrates.
• A higher portion of recurring identifications in AWT concentrates
are for materials related to domestic sewage. Examples are drug
related compounds (phenobarbital, clofibric acid, salicylic acid
and ethosuximide) and food related materials (saccharin, benzoic
acid,, caffeine and BHT) . Nicotine is the only compound qualify-
ing for this class of substances among the 39 compounds shown
for DW concentrates.
• Bromohaloforms were detected nearly exclusively in DW concentrates.
• Non-aromatic halogen containing compounds (12 species) are found
in Table 18 only as predominantly DW identification occurrences.
• There was a somewhat greater tendency for aromatic compounds to
be found in AWT concentrates. The relative amounts of compounds
with an aromatic moiety were 67, 73 and 28 percent for the AWT
only, both AWT and DW and DW only groupings in Table 18. This
result is also reflected by comparing the listings in Tables 16
and 13 of the percentage of identified compounds in AWT and DW
concentrates which contained the substituted or unsubstituted
aromatic nucleus. The averages for the 5 AWT and 7 DW concen-
trates (as above) are 50 and 3A percent, respectively.
131
-------
TABLE 18. DISTRIBUTION OF COMPOUND IDENTIFICATION INSTANCES FOR DW AND AWT CONCENTRATES
ro
Sequence
Number*
34
42
46
56
57
72
80
81
129
135
148
149
150
163
142
197
211
240
320
332
343
345
363
364
365
384
454
472
494
499
528
617
689
690
752
786
837
1092
1350
* The se
Compounds Identified Principally
in DU Concentrates
cyclohexanone
butyric acid
dichloroacetone
bromodlchlorotte thane
broaofora
phenylacetic acid
2-pentanol
3-penten-2-ol
acetophenona
laophorone
valeric acid
trichloroacetlc acid
trlethylphoephatq
dicamba (3.6-dichloro-2-
nethoxylbenzoic acid)
dlbroaochloroae thane
o-dlchlorobenzene
trlchloropropenolc acid
2,3-dimethylbeozolc acid
2.4,5-T
veratrlc acid
2,2, 6- trine thy 1-1 , 4-cyclohexanedlone
laohexaaolc acid
anisic acid
tetrahydrotriaethylbenzofuranone
l,3-dlchloro-2-aethylbutanoic acid
dlethylfornamlde
2,3-dlchloroanillne
2-methyl-2-pencanol
dalapon(2,2-dlchloropropanoic acid)
4,4-dlchlorobucenoic acid
3-methyl-2-cyclohexen-l-one
1,1, 3-trlchloropropene
2,2, 6- 1 rime thy Icyclohexanone
2,3-dlmethylbutyrlc acid
3-Bethylcyclopentenone
3-hydroxy-3-aethyl-2-butanone
nicotine
1,1, 2-trlchloropropene
1,1,2,3, 3-pentachloropropene
quence nunber corresponds to each coi
Sequence
Number*
1
14
35
70
95
133
134
193
239
243
250
254
331
419
444
451
456
464
507
523
535
538
785
845
848
860
872
1031
1032
1368
Compounds Identified in Both DU and
AUT Concentrates
clofibrlc acid
methylethylmalelc acid
benzole acid
salicylic acid
ethosiuclaide
at-tolulc acid
p-toluic acid
cyclohexenone
p-chlorophenoi
2.4-D .
o-toluic acid
2,5-dlaethylbentotc acid
2,5-hexanedione
5-aethylhexanolc acid
dlaethylfara»ide
p-dlchlorobencene
phenylacetonitrile
caffeine
p-chlorobenzolc acid
2,4-dlchlorophenol
2,2-dlnethylbutyrlc acid
dlphenylamlne
2,6-dimethylpyridine
2,4,6-triuethylpyrldlne
BUT
paeudocuaene
l,6-diiBethyl-4-ifiopropylnaphthalene
1 , 2 , 3-triuethylbenzene
2,3,6-trloiethylnaphthalene
Sequence Coapounda Identified Principally
Number* in AUT Concentratea
6 tris-2-chloroethyl phosphate
107 phenobarbital
258 2-chloroaniline
260 saccharin
297 2,5-dlmethylphenylbutanolc
341 3,5-dluthylbenzoic acid
455 dimethyl phtbalata
531 at-chlorobenzolc acid
561 dimethyl aulfone
886 2,6-dlaethylheptanoic acid
1160 fluorene
1215 2-methylstyrene
acid
mpound location in Table 11.
-------
TABLE 9. COMBINED LISTING OF IDENTIFIED COMPOUNDS
FOUND IN DW CONCENTRATES
COMBINED CONCENTRATE REPORT (PART I.AI
EPA 18 CONCENTRATES PAGE \
CONNON NAME
1 XttOI-N-BUTrtPHTHALATE
2 XtNAPHTHALENE
3 2-ETHYL-l.l-BIPHENVL
<• ZPALHITIC ACID
5 Xl-BJTANOL
6 2-HrDROXY-2-HETHVLPROPANOIC ACID
7 2-ETHYL-3-HETHTLHALEIC AGIO
8 l-U-HETHYLPROPOXVI-2-PROPANOL
9 XhETHYL BENZOATE
10 XCTCLOMEXANOL
11 XHONOauTYL PHTHALATE
12 1.2 5,6-BIS-O-ISOPROPYLlDENE-BETA-O-TALO
13 Ii2 <.,5-01-0-ISOPROPYLIOEHE-ALPHA-O-FSJC
U 2.3-DIHETHYLMALEIC ACID
15 PHTHALIC ANHYDRIDE
16 XCYCLOHEXANONE
17 XBENZOIC ACID
18 ZMYRISTIC ACID
19 PENTADECANOIC ACIO
20 ZIOI-ISOBUTYLPHTHALATE
21 TRANS-2-NCTHVLCVCLOPENTANOL
22 2-NLTHYLBUTYRIC ACID
23 2,2,<«. XBJTfRIC ACID
25 MARtARIC ACIO
26 1.2-PROPYLENE GLVCOLt DINETHYL ETHER
27 2-HEPTENE
28 1.1-DICHLOROACETONE
29 3-ErHYL-'i-l1ETHVL-2i5*>FURANOIONE
30 2-HITOROXY-3-METHYL-2-CYCV.OPENTEN-1-ONE
31 H-IH£XYLOXY)-1-BUTANOL
32 6-BROHO-2-HEXANONc:
3) XBROHODICHLOROMEIHA>4E
3<> XBROMOFORn
35 ".-MtTHYL-2-PENTANOL
36 X*»«2.ii,6-TRICHt.OROPHCNOL
37 XXOIETHYL PHTHALATE
38 2.V.6-TRIBROMOPHENOL
39 AMVLENE OICHLORIOE
<>0 X9.1Q-ANTHRACENEDIONE
1.1 7,7-OIMETHYL-2-OXOBICYCLOt2.2.1lHEPTANE-
<>2 3-r1ETHOXY-3-HETHYL-2-BUTANONE
<> XT^ICHLOROPROPANE
<»S l-METHOXY-2-PROPANOL
CAS NO.
91203
1812517
57103
71363
591.616
53907952
93583
13170".
23262795
20880937
488211
BS«.<.9
1089i>l
51. 1.638
10028<»2
25 1 H*»0 V 1
3302123
107926
506127
7778850
592778
513882
3552338
80717
10226296
7527*
75252
66062
2001
8<>651
31«. <.169
36687946
2
-------
TABLE 9. (Continued)
EPA !• CONCENTRATES PAGE 2
COMBINED CONCENTRATE REPORT(PART I.At
COHNON NAHE
46 3-HEXANOL
47 XSALICVLIC AGIO
48 XCAPRYLIC ACID
49 XPHENYLACETIC ACID
SO a,»-BIM£TH«hNAU£IC A6IB SEE NO. 14
51 XPELARGONIC ACID
52 ZSTE&RIC ACID
53 1,3,5-TRIHETHVLCYANURIC AGIO
54 1-HETHYLBUTYLALCOHOL
55 3-PENTEN-2-OL
56 2-HETHYL-3-HEXANOL
57 2-ETHVLBUTANAL
58 X4»-ETHYLACETOPHENONE
59 OEHYDROABIETIC ACID
60 3(4-DIETHYLaiPHENVL
61 1-HETHYL INOENE
62 ZSTOLUENE
63 ISOVALERIC ACID
64 2,4-DINETHYLBENZOIC ACID
65 3-PENTEN-2-ONE
J-1 66 HEXtHYOROTOLUENE
^ 67 XACETOPHENONE
68 6-NETHYL-5-HEPTEN-2-ONE
69 2-ETHYL-l-HEXANOL
70 2»-ETHYLACETOPHENONE
71 2-ETHYLHEXANOIC AGIO
72 H-TOLUIC AGIO
73 P-TOLUIC AGIO
74 CLOFIBRIC AGIO
75 «ISOPHORONE
76 SN-BUTYL-ISOBUTVLPHTHALATE
77 2,6-OINETHYLBENZOIC ACID
78 1.5-HEPTAOIENE-3.I.-DIOL
79 2-U-BUTOXYETHOXVIETNANOL IA DIETHYLE
80 3-NETHYL-2-8UTEN-1-OL
81 BtNZORESORCINOL
82 XCAPRIC ACID
83 XTRIBJTYL PHOSPHATE
84 XAZELAIC AGIO
85 XPHTHALIC AGIO
66 XLAURIC AGIO
87 SUBERIC AGIO
86 XOLEIC ACID
69 2-CYCLOPETEN-l-ONE
90 OICYANOHEXANE
CAS NO.
623370
69727
124072
103822
112050
RELATIVE SIZE
* VIC V1X T2B TIC
6.0
4 0
6.0
T1X T1V
6.0
57114 6.0*
827167
6032297
1569502
617298
97961
937304
5155704
61141660
767599
108883
503742
611018
625332
108872
98862
110930
104767
2142645
149575
99047
99945
•82097
78591
17851535
632462
51945983
112345
556821
131566
334485
126738
123999
88993
143077
505486
112801
930303
111693
6.0
3.0 3.6
A 4.0
1.9 o.o 2.0
A 5.3
a i.o
5.0
4.0
3.1
-1.1 4.0
A 2.0
-1.1 5.0
t.O
4.0
S.O
0.0 4.0
1.0 1.0 3.0
2.0 1.0 5.0
0.0
4.0
s.a
T4CtT*XtH2C
S.6
5 fi L t
3.6*
3.6
S.7
H2C
4.7
3.7*
4.7
6.0
P2C
Z.6
4.9
4.0* 2.6*
3.0
5.0
3.0
3.0
4.0
9.0
3.0 1.0
5.0
4.0
3.1
4.0*
3.0*
3.6*
Z. 6*
3.6
Z.6
4.2 4.6
5. 2.6 3.6
2. 2.6
2. 2.6
4. S.6
2. 2.7
S.6
S.
3.6 4.
3.6* 4.
3.6 4.6*3.
3.6*
3. &
3.6
2. '
1.
0.
1.
4.7
4.7
3.7
1.7
4.7
S.7
5.7
*5.7
S.7
1.6
h.O
3.6
5.
S.
S.
S.
S.
S.
4.6
h.6
4.6
PZI OZC
2.6
g 9
4.1*
4.0
1.8*
5.9*
S.9
S.9
2.9
5.9
5. 9
S.6*
3.4
4.9
3.9
3.9
3.«*3.9
02X S2C
2.9 1.2
3.2
S.2*
4.5
4.S*
Z.2*
S.9*
1.9*
S.9
S.9 4.2
2.2
4.9*
2.9 4.2
1.9 4.2
4.2
2.9
S.2
4.2
1.2
4.2
3.2
4.9*
5.7
S.7
S.7
5.7
5.7
2.6*3.1*3.9*3.9*5.2
2.6 2.9
2.9
3.2
S2X X1C
3.2
2.2
S.O
3.0
6.0
1.2*
1.0
2.2 3.0
4.2
2.2
1.0
3.2
3.2
2.2
1.0
* 2.0
2.2*2.0
2.2
4.2 3.0
XIX
1.2
4.2
"
-0.4
1. 1
* SEE LAST PAGE OF TABLE
(Continued)
-------
TABLE 9. (Continued)
EPA 18 CONCENTRATES
COMBINED CONCENTRATE REPORT(PAR! l.AI
COMMON NAME
CAS NO.
U)
Ln
91 XATRAZINE
92 lM-IMIOAZOLE-2-CARBOXALOEM»DE
93 XN-OCTANOL
9<> CIS-2-METHYLCfCLOPENTAMOL
95 XVALERIC AGIO
96 X8ICHLORACETIC AGIO
97 XTRIETMYL PHOSPHATE
98 5,b,7,7A-TETRAHYO*0-i.,i.,7A-TRIMETHYL-2li.
99 3-METHYL-2-8UTENOIC ACIO
100 3-METHOXYPENTANt
101 T*IPROPYLtNE GLYCOL, METHYL ETHER
102 TRIPROPVLENE GLYCOL. METHYL ETHER
103 6-METHYL-2-HEPIANONE
10<> XPROPYL ALCOHOL
105 2t2-OIETHYLPROPYLENE GLYCOL
106 AHVL CHLORIDE
107 3.5-OIMETHYLCYCLOHEXAN0L
108 l-METHYL-3-CYCLOMEXEN-l-OL
109 CYCLOHEXVL FORMATE
110 ltl,l-TRICHLORO-2-PROPANONE
111 X2-CHLORO-1.1-OIETHOXYETHANE
112 XOICAHBA
113 XISOSUTYRIC ACID
11V 2-METHYL-3-8UTEN-2-OL
115 XBENZALDEHVOE
116 OIETHYLENE GLYCOL, BUTYL ETHER
I IT 3,3.3-TRICHLOROPROPENE
110 2-ETHYL-3-HETMYLFUMARIC ACIO
119 ETHYL LACTATE
120 OIACETYLBENEZENE
121 ALOOL
122 Xl-IETHENYLDXYIBUTANE
123 6-P30PYL-8ETA-RESORCYLIC ACID
12<« i.-ISOPROPYL-0-PYROCATECMUIC ACIO
125 N-TRIETHYLENE GLYCOL. HONOETHYL ETHER
126 OIPROPYLENE GLVCOL, METHYL ETHER
127 METHYL MYRISTATE
120 METHYL STEARATE
129 OIOCTYL AOIPATE
130 X'tSTYRENE
131 1,3-DIETHYL BENZENE
132 1.I.-OIETHYL BENZENE
133 1,2-OIETHYL BENZENE
131, XMOIOCTYLPHTHALATE
135 ETHYL PALMITATE
RELATIVE SIZE
MIX T28 TIC T1X TIY H,CtT»XtN2C N2C C2C PZX 020 BIX S2C SIX X1C XIX
191221,9
10111087
111875
25H.I.OS2
10952*
791.36
78<>00
1535671.*
36839675
1,00
928687
71238
115761.
51.3599
51.1.1521
330611620612
112505
121,107
11261*
123795
1001.25
11.1935
105055
135013
117*1,0
62*977
$.7 2.9
-1.1 f
3.0 5
1..0 5.0 f
3.0 <>.0 1.6 i
3.0 S
2.8 3.6 5
2.6 5
0.6 5
$
$
5
^
5
5
J
3.8 1.9
t.8 0.9
3.8 1.9
01 9. 4
• » £• T
3.8
*.( 3.9
t.8
1.7 2.9
1.8
5.6
0.0 %.0 2.6 $.6 V.f 1.1
S.6 3.)
2.6 t.6 5.3 k.8 3.9
1.0 1.7 3.1
•0.* 3.9
3.8
1.0 0.6 1.8 S.I 1.9
1.0 1.0 5.0 2.1*
1.9 2.0 2.0*5.0
0.0 0.0 2.0*5.0*0.«i*2.6*3.6* 3.8* 1. *0.9
0 0 1.0 5.0-l.i>* -0.2*0 *3.
A 3 0 3.0 5.0* 2.6* 1 **. -(.1
A i, 0 3.0 5.0* 2.6* 1 *•». 0.9
A I 0 2.0 5.0* 1.6* 1 *)>. 0.9
3 0 2.0 5.0* 1.7* 2 *
A 30 1.0 5.0*1.% 2.6*. % * «.9
*
0.2
s. z
2.2
Z.2
2.2
2.2 3.
5.2
$.
5.2 i>.
5.2
5.2
5.2
5.2
S.
f.
*
o.z*
1.
2
2
2
2
2
2
2
2
3.6
O.Z
* SEE LAST PAGE OF TABLE
(Continued)
-------
TABLE 9. (Continued)
EPA IS CONCENTRATES PACE
COHBINEO CONCENTRATE REPORT(PART t.AI
COMMON NAHE
CAS NO.
RELATIVE SIZE
* me V1K TZB TIC T1X TIY ThCtfkXtNZC NZC PZC PZ X OZC OZX SZC SZX X1C XIX
U)
136
137
13ft
139
K.O
K.1
l«
1<»3
!<>%
11,5
H.6
U7
11.8
109
150
151
152
153
151.
155
156
157
158
159
160
161
162
163
16".
165
166
167
168
169
170
171
172
173
171.
175
176
177
| yg
179
180
HETHYL-3.S-OINETHYL BENZOATE
Z-HETHOXY-3-NETHYLCROTONIC ACIO
XOIBRQ HOC HLORO HE THANE
2-CTCLOHEXENONE
2.3,$,6-TETRACHLOROTEREPMTHALIC ACIQ
X«H-X»LEN£
X3-CHLORO-2-METHYL PROPENE
X»tO-OlCHLORO BENZENE
X*»SHEXACHLORO-li 3- BUTADIENE
P-HETHYLSULFONYL TOLUENE
1.1.3.3-TETRANETHYL-Z-INOANONE
2>3-OIHETHrL-2-BUTANOL
HtTNYL HEPTANOATE
PHENYL ACETIC ACID. NETHYL ESTER
DI-12-BRONOETHVLI ETHER
l-ISOCVANO-<»-HETHYLBENZE*E
SULFONYLBISU-CHLOROBENZENEI
2-ETHVL-i»-HETHVL-l-PENTANOL
3-NETHVLCYCLOPENTANONE
XCAPROIC ACIO
X»*PHENOL
XS1.1.2,2-TETRACHLORO£THAN|
XN-HEPTANOIC ACIO
2<3,3-TRICHLORO-2-PROPENOIC ACIO
N-HTOROXVPHTHALANIQE
1-ETNOXV-l-HETHOXVETHANE
1-1-OIHETHOXYPROPANE
2 3 OIHETHVLHALCIC AC13 SEE NO 11
ISOPROPYL BENZOATE
1.1-BISU-ETHVLPHtNVLIETHANE
O*ETH VLSTVRENE
XSTILBENE (CIS OR TRANS. SEE NO. 411)
2-HEPTENYLBENZENE
X2-HETHYLNAPHTHALENE
XBIPHENYL
Z-HETHYL aiPHENYL
3.<«t-OIHETHYL-l.l»-BIPHENYL
XSTILBENE OXIDE
1.1-BISIH-ETHYLPHENYLt ETHANE
XCYCLOPROPYL METHYL KETONE
2-HETHYLCYCLOPENTANOL ICEONETRV UNKNOHNI
XHETHYL UUTVLKETONE
CARBOH1C ACIO
2-HEXANEAHINE
Zi<»>HEXAOIEN-l-OL
Z50B139<>
5*973115
4 9 J.4.H a
IcHHO 1
930617
Z136790
108313
5631)73
95501
87613
3185997
56891Z3
S9<>605
106730
101H17
5i.li.197
7175V75
80079
10667Z
17S7I.ZZ
108952
79345
Hll
-------
TABLE 9. (Continued)
EPA 1* CONCENTRATES PACE *
COMBINED CONCENTRATE REPORT(PART X.AI
CONNON NAME
181 OIETHVL CARBINOL
182 XBENZYL ALCOHOL
113 2,3-OlHYDRO-<.-HETrtrLFURAN
18". ETMYLBENZALOEHYDE
115 2».3»-OIMETHYLACErOPiiENO*E
186 3-EfHVLSTYREN£
187 ETHYL NY*ISTATE
161 OECAHYORO-2,3-OINcTHVLNAPHTHALENE
189 2,3-DINETHYLBENZOIC ACIO
190 X»<2,I.,5-TRICMLOROPMENOXY>ACETIC ACIO
191 3,.0* 1.6*
2.0 3.0
d.O
1.0 3.0-0.%
Z.6
3.6*0.6
%.9
%.0 3.0
2.6 3.6 t.fc
1 0 1.6
% D 1.0* 0.6*
1. 0
% 0 1.0 3.0*
1 0
%. 0* 1.6*
2. *
1.0 1.0 2. 2.6
2.0
3 A 7 ? 7 k fc
• II t • £••.
%.
It.
2.8 •
2.
%.
3.
5
Z
2
2»
2
8
Z
2
Z
2
2
Z
S2I
1.
0.
1.
1.
3.
B •
z.
3.
0.
2.
2.
Z.
•
3.
1.
Z
1*
Z*
2*
Z*
Z
.
z
z
z
2
2
Z*
2
2
X1C XIX
2.0
• (.1
0.2
-1.8
3.2
1.0
1.2
* SEE LAST PAGE OF TABLE
(Continued)
-------
TABLE 9. (Continued)
EPA It CONCENTRATES PASE 6
U)
00
COMBINED CONCENTRATE REPORT(PART I.A I
COMMON NAME
CAS NO.
RELATIVE SIZE
VIC MX T28 TIC T1X T1V TkCtT^XtN2C N2C P2C PZX OZC P2X S2C S2X X1C XIX
ZZ6
zz?
2Z1
2Z9
y\n
C-JU
Z31
Z3Z
Z33
23Z-FURANONE
XTCA (TRICHLOROACETIC ACID)
DICHLOROPHENOXYACETIC ACIO (ISOHER UNKHO
PIVALIC ACIO
3-CHLOROCYCLOPENTENE
6-IACETYLOXYI-2-HEXANONE
6.7-OOOECANEDIONE
OIETHYL PENTYL PHOSPHATE
7-TR10ECANONE
vi Aiifivi_ AI rnwni
ALHUf^ 1U MUlfUnUL.
N.N.4-TRIHETHYLBEMZENESULFONAHIOE
ISOPROPTL MYOROPEROXIDE
OIISOOCTYLPHTHALATE
3.I.-EPOXY-2-HEXANONE
x*«ointxYL PHTHALATE
Xl.ii-OIOXANE
LEVULINIC ACIO
l-HEPTEN-«.-OL
2-METHYL-1-PENTEN-3-OL
N.N-OIETHYL FORM* HIDE
6179*7 3.6 %.7 k.
20324327 2.7 k
1561111 k
15877573 k
23701Z9 k
55956221. k
53636<.<> It
1632731 k
19711 k
15120997 k
507700 k
20»810<,3 k
5932796 k
55332020 k
874,12 k
527131.31, k
<,0<. k
31Z397S 2.6 2
117117 2.6 1.0 k. * k.6*k.7*k
100091. 0.0 k. 0 3. 3.6 .7 3
3622K.2 -1.0 Z.O .7 3
17092921 5.0 3. .7 3
23010073 1. k.6 .7 3
2001961.1 2. k.6 .7
76039 .7
711 .7
75919 .7 Z.
96<,02 .7
1.305261. .7
13757909 .7
20195011 .7
1.62110 .7
1 1 ?f*t A k 7 9
I L £*3 Q * • f C a
599699 k.7
3031752 k.7
Z7S5I.263 k.7
17257417 2.0 .6*
81.753 0.0 .6
123911 3.0* . *3.7*
123762 2.0 k.O 3.0 3.6 . 2.7 I.
3521913 3.0 .
2088075 k.O .
61781.5 2.6 2.6 k.
3.8
0.9 2.2
-0.8
2.9 "..2
2. a
2.) k.l 3.2
*2^*3.»*k.O* 3.2
2.1* Z.9*2.Z
3.1 3.2
8 0.2 2.2
3.2
I..2
a i>.2
-O.I
k.Z
Z.2*2.Z*
1.9*1.9* k.8
1 Z.I 2.9 2.9 3.2 4.2
3.2
4.Z
0.9 3.Z 1.2
(Continued)
-------
TABLE 9. (Continued)
•PA 1* C9NCENTRATES PACE T
COMBINED CONCENTRATE REP3RHPART I.AI
CONMON NAME
271 2-HETMYL-2-HEPTANOL
272 3,5-OIMETHOXYPHENOL
273 XAHOBARBITAL
27d XPENfABARBITAL
27S TRANS-9-H£XAOtCENOIC AGIO
276 PETROSEL1NIC ACIO
277 XCYCLOHEXYC 8ROHIOE
278 5-METMYL-3-HEXANOL
279 2-NETMYL-2-BUTEN-1-OL
280 S-ErHYL-2-HEPTANOL
Z81 3-METMOXY-1.3,d-H£XATRlEI»E
212 2-METMYL-2-ISOBUTYLOXIRANE
213 1-HETHYLHEXYLHYOROPEROXIDE
28d 2-BUTYL-3-NETHYLOXIRANE
28S 2-METHOXY-d-METHYL-2-PENTENOIC ACID, MET
286 2,3,d-TRIHETHYL-3-P£NTA»L
287 1-ISOCYANONAPHTHALENE
288 N-TERT-BUTYL-3-NETHYLBENZAMIDE
289 dt5-OIETHVL-2,3-DIHYORO-2,3-DIHETHYLFURA
290 d,7-DIMETHYL-lt3-IS09ENZOFURANOIONc
291 2.5-OINETHVL-2-HEXANOL
292 X»»BUTYL BENZYL PHTHALATE
293 PROPYLOXIRANE
29d XCYCLOHEXYL ACETATE
29$ XIETHOXVHETHVLIOXIRANE
296 d-HEPTANONE
297 PHENOXY ACETIC ACID
298 XETHOSUXIHIOE
299 2-HETHOXY-I.-HETHVL-2-PENTENOIC ACID
300 P-CFHYLBENZOIC ACID
304 1,1-OIPHENYLETHANE
306 HETHYL ANYL CARBINQL
307 XETHYL CARBONATE
308 S-METHYL HEXANDIC ACIO
309 2-BUTYL THF
310 ^,5-DIHETHYL-2-HEPTEN-3-OL
311 5-HETHYL-2-MEPTANONE
312 1.3,3,7-TETRAMETHYL-2-OXOBICYCLO(2.2.1lH
313 BJTYL IS08UTYRATE
31". 2-ErHYLCYCLOHtXANON£
31S OIETHYLEN£ SLYCOL, HETHYL ETHYL OIETHER
CAS NO.
625252
S00992
S7<>32
767".!.
373*99
593395
108850
623S52
S675870
19780<>06
53783883
53897317
7631.69
1<«92S963
56009360
305<,920
198<.0<«9
i»2 (.98339
5XtN2C N2C P2C P2X 02C 02X S2C S2X X1C Xl<
0.6
1.2
3.2
1.1
1.1
2.2
1.2
2.2
3.7
d.6 1.7
d.6
d.6*
3.1
1.2
2.»*I.9*1.Z*
d.6
2.6 d.6
0 d.6 2.6
d.6
3.6 d.6
d.6
d.6*
3.7*
1.9
1.0 2.9 3.9 •
3.2
•,.2
1.0
3.0
2.0
1.7
1.1'
3.8
2.7 1.8
0.8*0. 1-0. P
-I.*
2.6
1.6
3.6
3.8
2.8
2.9
3.9
2.2
2.2*
d.2*
d.2
d.2
d.2 2.2
d!z
d.2
d.2
d.2
d.2
d.8
' SFF I AST PAHF OF TABLE
(Continued)
-------
TABLE 9. (Continued)
IPA 18 CONCENTRATES PACE.I
COMBINED CONCENTRATE REPORTIPART I.A I
COMMON NAME
CAS NO.
RELATIVE SHE
* V16 WIX T2B TIC T1K TtV T4Ct UXt NZG N2C P2C P2K 02C 02X SZC S2X XiC XIX
316
317
318
319
321
322
323
324
325
326
327
328
329
330
331
332
33]
334
335
336
337
338
339
340
341
342
34]
344
345
34A
""W
347
341
349
350
351
352
353
354
355
356
357
358
359
360
2-HETHYLHEPTANOIC ACIO
1,6-HEXANEOIOL
2,3-OIHYORO-4-ll-NETHVLETHVLIFURAN
CYCLOHEXANEHEXANOL
2.2,5.5-TETRAMETHYL THF
X4I1HI-PVRIHIDINONE
3.S-NONADIEN-7-YL-2-OL
4,4.5,S-TETRAMETHYL-1.3-OIOXOLAN-2-ONE
2-(l-NETHVLETHYLIOENE>CVCLOHEXANONE
OXACYCLOTETRAOECAN-2-ONE
l.l-OICHLORO-2-HEXANONE
4.4-OICHLORO-3-HEXANONE
OIHYDRO-5-METHYL-2(3HI-FURANONE
C3-DIHYOROXYBENZOIC ACIO
4-BUTOXV8UTYRIC ACIO
XI1.2-OICHLOROETHANE
PENTAETHYLBENZENE
0-ETHYLBENZOIC ACIO
Z*IOICHLORO£THYL ETHER
XETHYL BENZOATE
ETHYL PENTAOECANOATE
ETHYL STEARATE
ANTEISOPENTAOECANOIC ACID
X»»»P-OICMLOROBENZENE
OIHEXYLADIPATE
METHYL LAURATE
HETHYL-Z.4-OIMETHYL BEMZDATE
2.3-OICHLOROANILINE
XSOIHETHVL PHTHALATE
XBENZYL CYANIDE
3-HEPTANOL
l-CHLORO-2-METHVL-2-BUrEHE
NEOPENTVL CHLORIDE
1-BROMO-4-ETHYL BENZENE
2,4,5-TRICHLOROANZLINE
«PENTACHLO*OANILINE
1,2,2,3-TtTEACHLOROPROPANE
X»**l, 2. 4-TRICHLORO BENZENE
2,4-OICHLORO-l-NITROBENZENE
+XLINDANE IBETA ISOMERI
x»PtNfACHLORONiTROBENZENE
DIMETHYL AZELATE
4-TERT-BUTYL- 2- METHYL PHENOL
4-METHYLPHENYLSULFONYL ACETIC ACID. HETH
1188029
629118
4354589
15045439
4562270
19424294
137477)4
1725048
2648591
2648604
108292
1016
557247)7
107062
605016
28134318 A
111444
93890 A
41114005 A
111615 A
5502943
106467
110388
111820 a
23617712 a
608275
131113
589822
13417431
753899
1585075
636306
527208
131165)5
120821
611063
3198S7
82688
1732101
98271
50397643
4.2
4^2
4.2
4.2
4.2
4.2
4.2
4.2
4.2
4.2
4.2
4.2
4.2
4.2
i.O 2.0 4.1
4.1
3.0 .0* 3.6*
-1.1 .0 0.8* -O.t*
4.0 1.0 .0* 1.8*1.9
2.0 .0* 1.6* 2.8* l.i*
z.o i, a .0* 1.6* 2.8* 2.9*
1.0 4.0
1.0 1.0 4.0-0.4 l.i $.7-8.2 -0.8 2.2
1.0 4.0
3.0 4.0* •
2.0 4.0*
I.O 4.0 1.6 1.0 1.2
4.0 4.0
1.0 4.0 -0.8
4.0
4.0 1.6
4.0
4.0 1.2
4.0
4.0 1.6
4.0 1.6 -0.2 -0.8 2.2
4.0 9.2
4.0 2.7
4.0
4.0
4.0-0.4 S.9 2.2
4.0
1.8
1.2
0.2
SFF I AST PAGF OF TABLE
(Continued)
-------
TABLE 9. (Continued)
EPA l« CONCENTRATES PACE «
COMBINED CONCENTRATE REPORT (PART I.AI
COMMON NAHE
361 <»-METHYL-l-PHTMALAZINONE
362 2-METHYL-2-PENTANOL
363 XCAMPHOR
36<> 2-KETOISOCAPROIC AGIO
369 PENTYLENETETRAZOLE
366 SUCCINIC AGIO. DIMETHYL ESTER
367 XOIETHYL SUCCINATE
36« 2.2-OIMETHYLGLUTARIC ACID
369 1-ETHANONE
370 METHYLSULFONYL BENZENE
371 ALLYL-1.3-OIOXANE
37Z METHYL CAPROATE
373 METHYLCAPRYLATE
370 HETHYL PELARGONATE
375 ETHYLNONENOATE
376 MITrtYL CAPRATE
377 BENIONITRILE
371 PMENYLPROPIONIC AGIO,METHYL ESTER
379 2.<«.5-TRICHLOROPHENOXV ACETIC ACIDt NETH
3aO 2.2-DIMETHYL-3-PENTANOL
381 I1-ETMOXYETHYLI8ENZENE
382 l,2-OIMETHYL-<«-Nm08ENZENE
383 METHYL HEPTADECANOATc (METHYL MARCARAT
3«<> l-<2-8UTOXYETMOXYI ETHANOL
385 2-MExENOIC AGIO
3S6 METHYL N-ANYL KETONE
387 XOALAPON
J»4 HENEICOSANIC ACID
389 HEPFYL ALCOHOL
390 XBISI2-ETHVLHEXVLI AOIPATE
391 ADIPIC AGIO. OIHEXYL ESTER
392 6-UNOECANOL
393 P-ISOPROPYL 9ENZOIC ACID
39<« <>.<.-DICHLOROBUTENOIC ACID
39S XANTHRANILIC AGIO
396 2-HETHYL-<»-<2t5-XYLVL>BUTANOIC ACID
397 2-(2*HYOROXYPROPOXri-l>PROPANOL IA OIPRO
398 2-PMENOXYETHANOL
399 CYCLIC TETRAHETHYLENE AOIPATE
•,00 1-CYCLOPENTYLETHANONe
1,01 (2-ETHOXY-l-METHOXYETHOXYI-ETHENE
<>02 NiNf-OIHETHYLUREA
||03 OIPNENYLHETHANE
<,0<> 1,2-OINYDRONAPHTMALENE
•.OS TETRAETHYLBCNZENE
CAS NO.
RELATIVE SIZE
* VIC V1X T2B TIC FIX T1V T«,CtUXtM2C N2C P2C P2X 02C 021 S2C S2X XIC XIX
500<.<.S8
590363
76222
816660
106650
123251
681572
26<,199 A
31128S<»
1,528261
106707
111115
17316<>6
3519<>399
1101,29
1004,70
103253
353891, <>0
3970625
3299056 a
995K,
1731926
5<><, 1,6785
11910K<,
1101,30
75990
2363715
111706
103231
110338
23708567
536663
16502888
118923
303161', «.
106627
122996
777957
6001,600
S<>063182
96311
101815 A
1,1,7530 A
33637206 A
k. 0
k.a
.0
.0
.0
.0
. 0
.0
.0*
. 0
d. 0
k.a
k.a
k.a
k.a
k.a
k.a
k.a
k. a
k.a
<,. o*
k. a
k. 0
2.0 d.l -0.%
k.a k.a 3.0
k.a -i.%
k.a 3.0
k.a
k.a 1.6
3.1 *.0«
3.0 k. 0*2.0*
k.a 3.0
k.a 2.6
k.a
k.a
k.a
k.a
k.a
k.a 3.6
k.a
k.a
k.a
k.a
k.a
k.a
3.6 3.7 0.9 2.2
2.2
2.6 0.8
2.9
1.6* 1.9*
1.1
1.9* -I.I
1.8 3.9 2.2 1.2*
1.8
3.6 3.7 1.2
2.6 3.2 3.2
3.6*2.7* 3.9*3.9*
2.9*
2.8 -O.I
1.8 3.2
2.6 3.1 1.8 3.2
1.6 3.6
1.9 3.5
2.6* 2.t* 2.9*
2.8* 0.9*
2.6* 3.8* 2.9*
1.2
• SFE LAST PAGE OF TABLE
(Continued)
-------
TABLE 9. (Continued)
EPA It CONCENTRATES PACE 10
COMBINED CONCENTRATE REP3RTIPART I.AI
COMNON NAME
-P-
N5
1.06 1-EfHYLNAPHTHALENE
407 l-METM»L-7-ISOPfiOPYL NAPHTHALENE
408 X3-HETHVLPHENANTHRENE
1.09 1-PHENYL TETRALIN
410 1.1-BIS(0-ETHYLPHEN»LIETHANE
411 XSTILBENE (TRANS OR CIS. SEE NO. 167)
1.12 2-PHENYL TETRALIN
413 3-ETHYLACETOPHENONE
•.I". 2-(ETHYLPHENYLIPROP»L METHYL ETHER
415 XETHYLENE TETRACHLORIDE
416 SETHYLBENZENE
417 ZtP-XYLENE
418 3S OIOCTVL SEBACATE
1.36 2-METHOXY-3.5.5-TRIMETHYL-2-CYCLOHEKENE-
1.37 PIPERIOINONE
1.38 TETKAHYDRO-2-HETHYL-2-FURANOL
4.39 XSUCCINIC ACID
'.'•O 2-ETHOXYNAPHTHALENE
".1.1 ZN-DECYL ALCOHOL
442 1.2,1,-TRIETHYLBENZENE
41.3 TETRALIN
444 OIVINYLBENZENE
44S P-ETHYLBENZALDEHYOE
446 2*-HETHYLACETOPH£NONE
447 1-METHYL TETRALIN
448 1,1-OIMETHYL INDAN-4-CARIOXYL1C ACID. ET
449 2-ACETYLOXYACETOPHENONE
450 3-NETHYL-2-CYCLOHEXEN-1-3NE
CAS NO.
RELATIVE SIZE
* VIC VIX T2B TIC T1X TIY I4CtT%XtN2C N2C P2C P2X 02C 02X S2C S2X X1C KM
1127760 A
490653 A
832713 a
3016200 A
1023 A
103300
29422137 A
22699703 A
667
127184
100414
106423
13703521
123422
432257
112356
1422260 -1.1
87865 0.0
102250
1618220
96480
94757
111206
2142769 a
528905
1961724
G 7 Q7EQ
9 1 VI 9^
1669449
122623
41654277
27154434
7326467
110156
93185
112301
877441
119642
1321740
4748781
577162
1559815
55591123
2243358 a
1193186
k.
t.
4.
%.
t.
4.
4.
4.0
4.0
4.0
2.0
3.0
1.0
3.1
1.0
3.0
1.0
211
. 0
3.0
3.0 1.0
2.0
2.0
1.0
2.0
1.0
2.0
2.3
3.1* 1.9*
i.a*
0.6* 2.8* 1.9*
3.8* 1.9*
0.6* 2.1* 1.9*
2.6* 3.9*
2.6
l.b* 1.9* 2.5*2.2*4.
3.3* 1.9 1.2 2.2 4.
4.
k.O 3.8 2.5 3.
3.9
3.9
1.6*3.
2.0 1.6* S.f -0.2 3.
2.6* 3.8*2.
3.
3.
3.0 2.6 3.7 3.
2.6 2. >
1.6*
2.6 3.8 .
i.r .
2.8
I. 8
.
.
.
1.2*
1.9*
2.9
19 9 9
• C £• C
3.9
1.9*
3.2
1.9 2.2
3.9
3.9
1.8 1.9 2.2
2.6* 3.1*1.9 2.9*
2.0* 1.6* 1.7-0.2 3.0*1.9 2.9*0.8
1.6* 3.8*1.9
3.6* 3.6*2.9 -0.8*
2.7 3.8* 1.9
1.6* -0.2 3.6* -0.0
3.8* 2.9*
3.8*
2.6 0.8 3.8 1.9 2.2 2.2
0.2.
-0.8
1.2
2«?
0
0
0
a
-o.a
-a.t
3.2
* SEE LAST PAGE OF TABLE
(Continued)
-------
TABLE 9. (Continued)
EPA II CONCENTRATES PAGE 11
COMBINED CONCENTRATE REPORT IPART I.AI
COMMON NAHE
451 2».4»-DINETHVLACETOPHENONE
452 X2-ETHYL NAPHTHALENE
•.53 3-NETHVL VALERIC ACID
454 2-NETMYL INOAN
455 2,2-DIMETMYL-3t5-OECAOJVNE
456 5-HETHYL INOAN
457 2.5-CYCLOHEXAOIENYLBENZEME
458 ALPHA-NETHYLSTILBENE
459 2.3.4.S.6-PENTAFLUORO-N-I2-PHENVLETHYLIB
1,60 4.4»-OIETHYLBIBENZVl
461 OIPROPYLENE GLYCOL METHYL ETHER -OICHLOROPHENOL
472 lt2t3.3-T£TRACHLORa-l>PROPENE
473 1-METHYL-4-U-HETHYLETMYH-7-OXABICYCLOI
474 XCAFFEINE
475 2'HETHYL VALERIC ACID
476 l-<4.5-OIETHYL-2-NETHYL-l-CVCLOPENrEN-l>
477 FENCHONE
47» 3-OCTENOIC ACID
479 1-PHENVLBUTVRIC ACID
460 2-HYOROXYTETRAOECANOIC ACID
481 3-METHYLPHTHALlC AGIO
4»2 4-HETHYL-3-PENTENAL
483 XCINEOLE
4«4 3-ErHOXY-3-HETHYL-2-BUTANONE
485 ISOPROPENYLBENZENE
486 6-HETHOXY-2-HEXANONE
487 2.4-HEPTANEOIONE
488 2-CYCLOOCTYL-2-PROPANOL
489 METHYL 2. 2, 3-TRIMETHYLCYCLOPENTVL KETOME
490 TNIOHEKANOIC ACID, S-BUTVL ESTER
491 3-ETHOXY-3-METHVL-1-BUTYNE
492 5-(P£NTYLOXYI-2-PENIENt
493 2-ETHYL-3-NETHYLOXETANE
494 2-NETHYL-2-PROPYL-l,3-DIOXOLANE
495 2-ErHYL-l,3.2-OIOXABOROLtNE
CAS NO.
89747
939275
10S431
824635
55652730
874351
4794052
833818
38842147
57364791
13429077
34067759
1653301
112425
6789884
2049969
95169
106489
4316238
93094
120832
20589859
470677
58082
97610
62338243
1195795
1577191
1821121
2507553
37102742
5362505
470826
36687997
98839
29006006
7307020
16624069
17983221
2432793
7740694
56052858
53778624
4352981
10173383
RELATIVE SIZE
• VIC V1X T2B TIC T1X T1V T4CtT%XtH2C N2C P2C P2< 02C 02X S2C S2X X1C XIX
3.0<
1.6
1.6*
1.7
2.S*
2.9*
2.9
0.$*
P.2
'1.9
-0.8
1.9
i.g
2.1
3.0 2.6'
3.B 2.6
1.6
-0.4
-1.4
1.6
3.6
3.7 2.8
1.7
Z.7
Z.7
3.7
3.7
1.6
3.7
2.2
3.2*
2.2
2.2
1.2
2.9
1.1
3.2
* SfE LAST PAGE OF TABLE
(Continued)
-------
TABLE 9, (Continued)
EPA II CONCENTRATES PACE 12
COMBINED CONCENTRATE REPORT(PART I.AI
1,96
1.97
1,98
1.99
500
501
503
503
Sod
505
506
507
508
509
510
511
512
513
51".
515
516
517
518
519
520
521
522
523
52".
525
526
527
526
529
530
531
532
533
531,
535
536
537
538
539
5i»0
COMMON NANE
CAS NO.
RELATIVE SUE
VIC Vl( T2B TIC TIX TIY T%Ct T*Xt N2C N2C P2C P2X 02C OZX S2C S2X X1C XIX
BORNYL 2,5-OIKETONE
7i7-OINETHVL-ll-OODECEN-Z-ONE
NETMYL 9-OXOOECANOATE
CYCLOOCTANEPROPANOl
CYCLOHEXYL HETHVL KETONE
P-ISOPROPYLBENZALOEHYDEt CUHINALDCHYDE
2,3 5, 6-01-0- ISOPROPYLIDENE-ALPHA-0-TALO
1-TERT-BUTYL-1.-ETHOXYBENZENE
5-METHYL-K3HI-ISOBENZOFURANONE
9-OCTAOECENAL
«,-NETHYL-3-HEPTEN-2-ONE
6-METHOXT-2-NETHYL-3-MEXANONE
2.6-OIMETHYL-3-HEPTANOL
2-(2-HETHO«Y-l-HETHVlETHOXVI-l-PROPANOL
AHYL BUTYL PHTHALATE
2-ErHYL-2-ISOBUTYL-li3-DIOXOLANE
ELAIOIC ACIO
P-ll-HYDROXY-l-HETHVLETHYLIACETOPHENONE
ZP-CHLOROBCNZOIC ACID
3,<.-OICHLOROBENZOIC ACIO
2,2,6-TRIHETHVLCVCLOHEXAMONE
2|3-OINETHVLBUTYRIC ACIO
OICHLOROISOPROPYL ETHER
PENTACHLOROCYCLOPROPANE
2.3-OCTANEOIONE
BUTYLBENZOATE
2-PHENYLBUTYRIC ACIO
3-HETHOXYBENZOIC ACI3
2.6-OICHLOROBENZOIC ACID
UNDECANEOIOIC ACID
XCHLDROBROMOHETHANE
TRICHLOROPHENOXVACETIC ACIO IISONER UNKN
3-B*OMO-l,l-DICHLOROPROPANE
XTERT-PENTVL ALCOHOL
S-NETHYLHEXANOL
CIS-3,<»,i.-T«IMETHYL-5-OXD-2-HEXENOIC ACI
ETHYLENE GLYCOL, MONOHETKYL ETHER
I.-ISOPROPYLCVCLOHEXANOL
l.-HETHYL-3-HEPTANOL
SEC-BUTYLISOPROPYL ETHER
X2-PROPENYL HEXANOATE
CVCLOPENTANONE
VINYL BUTYRATE
TETRAHYORO-5-HETHYL-2-FURANHETHANOL
1206li8
50901.15
22319251
171.29059
1951.9736
55956213
1018
9J51.55
112798 ?ol i.fi
51.51.9723 0.0
74113 1.0 3.0
51V.5 0.0 3.0
108601 1.0
6262517 1.6
585251 2.6 2.6
136607 Z.6
90277
586389
50793
185201,6
7«»975
713
366681,58
75851.
1860395
1<.9195<.1
109861,
1,62101,9
11,979396
1861,1811
123682
120923
123206
51,771,286
"
.7*
.7
.1
.7
.7
.7
.7
V
.7
.7
.7
.7
.7
.7
.7
.7
.7
.7
.7
.7
.7
.7
.7
.7
.7
.7
•
•
•
•
0.9
. Z.» 0.2
•
•
3.2
•
2.2
•
•
•
!.
1.
3.2*lel
2.2
t.8
2.2
1,9 -8aS
I • 6
1.8
2.1 £.8
2,»
3
2»2
(Continued)
-------
TABLE 9. (Continued)
EPA II CONCENTRATES PACE 13
COMBINED CONCENTRATE REPORMPARF I.At
5*1
5*2
5*1
5**
5".5
5*6
5*7
5*8
5 ".9
550
551
552
553
550
sss
556
557
558
559
560
561
563
563
56<>
565
566
567
561
569
570
571
572
573
57*
575
576
577
579
579
580
561
5«2
583
58<>
585
COMMON NAME
OCTYL ACRYLATE
VlJ^MPTUVI *9*PVCAI THAUP
AH NCI H f L t ™ I ™U HUUHt
*-KETOISOHEPTANOIC ACID
3-N£THYL-*-PENTEN-2-ONE
2-NETHYL-2-PROPYLMEXANDIC AGIO
J».nTMF THV 1 AIIT VP TP APTM
• O m U &nL 1 n T LD Ul IK1U HwAU
CHRYSANTHEHIC ACID
CIS-1.3-OICHLOROC»CLOH£K»NE
3, t-OIHVORO-6 -METHYL- 2M-PVRAN
5-NETHOXY-2*HETHYL-2-PENTANOL
2-VINYLCROTONALOEHTOE
(1-METHYLBUTYLIOXIRANE
2-HYOROXVCYCLOHEX»NONE
5-NETHVL-l-HEXANOL
2-T-8urYU-2-METMYL-l,3-OIOKOLANE
J-CMLORO-2-CYCLOPENTEN-l-ONE
<»6f6-TRIHETHYLT£rRAHYDRO-2-PYRANONE
3.7-OCIAOIEN-2-ONE
2-HEPTENOL
2-BJTOXYPENTANE
ALPHA-ACETVLBUTVROLACTONE IGANHA LACTONE
2-0:TEN-l-OL
CHLOROACETONITRILE
XTERPIN
2-NETHYLENEBUTYRIC ACID
XETHYLENE GLYCOL MONOETHYL ETNERI (OXITOL
3i6-DIMETHYLOCTANOIC ACID IAN ISODECANOI
3-METMYL-<.-PHENYLBUTYRIC ACID
OCT*HYDRO-l,<»A-OIH£THYL-l-PHENANr»4RENE C
1.3-OIHETHYL-2-I2-ISOPROPYLPHENYLIETHVLC
X7-OXABICYCLOI <>. 1. 01 HEPTANE
X PVRIOINE
Xl,2-OIHYORO-3,6-PVRIOAZINEOIONE
3-HYOROXYOCTANOIC ACID
3,i.-OIHVDROXYBEN;«LOEHYO-
2.3-DICHLOROACRYLlC ACIO
5-OXO-HkXANOIC ACIO
2-IHYOROXVMETHVLIBEN7.0IC ACIO
TftlPROPYLENE GLYCOL, METHYL ETHER
X'ANILINE
X2,2,2-rRICHLOROETH«NOL
<<-ACEIYLHORPHOLINE
2-HETHYLPHENYLPROPANOIC ACIO
CAS NO.
51.832836
2<.99S4<.
A T 9KA LL
Of £9\t H
i.lbS'.O'.O
758872
31080372
1 A 7 A A 1 Y
1 U f UO JJ
101.53891
2 ".955633
16015115
55721,01. <•
20521<.20
53229393
533608
627985
613551.2
531021*0
20628368
25172069
33<.6776<>
62238022
517237
18<. 09171
107K.2
80535
3586581
110805
1.812297
7315616
36500<.2
6080
28620%
110861
123331
1<>29227<.
8897
8896
1128061
612201.
20321.338
62533
115208
1696201.
22080895
RELATIVE SIZE
tlC V1X T28 TIC T1X T1V UCt T»Xt N2C N2C P2C P2X 02C 02X S2C S2X X1C XIX
3.7
1.7 3.2
1.0 1.0 3.0 2.6 1.6*1
3.0 1
2.0 1
1
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
Z.r 2.6* 2.9*2.2 3.2*
2.2
1.2
2.8
1.9
3.0
1.}
6
6
6
1.6 2.1 0.6 2.8
1.0 1.6 1.1 1.9 Z.» 2.2
0.9
2.6
0
1.9
0.2
3.1
3.3
•1.0 1.2
(Continued)
-------
TABLE 9. (Continued)
EPA It CONCENTRATES PACE 1%
COMBINED CONCENTtAU REPORT (PART I.A)
586
567
588
569
590
591
593
593
59".
595
596
597
598
599
600
601
60Z
601
60<.
605
606
607
608
609
610
611
612
611
6m
615
616
617
611
619
620
621
622
623
62-OINETHVL-2-P£NTENE
ACETYL ISOBUTYRYL
1.2-OIHETHYLCYCLOHEXENE
PiHf YL TRIMiTHYLENi
*»-H£THOXV-l-8UTANOL
3,<.-OlHYDRO-2,5-OIMETM»L-2H-PYRAN-2-CAIlB
2-BUTYL-N-BUTVRATE
N-BENZOYLGLYCINE, METHYL ESTER
CUHENE ISOPROPYL ETHER
1.3-OIMETHOXY-2-PROPANOL
2-ISOPROPYL-l .3-010X0 LANE
1-OXIRANYLETHANONE
6,6-DINETHYL-3.<.-UNDECADIENE-2tlO-OIONE
TEREPHTHALIC ACID
3-HETHOXY-2-NETHYL-2-PENTENOIC AGIO
3-HETHOXY-1.2-BENZISOTHIAZOLE
1-MET HYL-%-11 -METHYL- 2-BUTENYLI NAPHIN ALE
CYCLOPcNTYL BROHIDE
2. 2-0 ICHLORO-3-HETHYL BUTANE
SYN-OIPHENYLETHANE OIBENZYLI
3-HYDROXY-3-NETHYL-2-BUT»NONE
CAS NO.
t
75650
1006
116912
610720
2756161
1951.9770
5731.5309
(•536236
56S9<>16
2231931.0
1192627
56961252
6299667
13390V
693721
623563
109675
2313657
23799259
625650
7 <»935B5
167(tl06
3il 191 1
111320
17257626
192021<>
619976
1205069
2W1I.2776
623696
622633
1.1.01110
S2566760
100210
101 1.0 1.9* 3.2
SEE LAST PAGE OF TABLE
(Continued)
-------
TALBE 9. (Continued)
COMBINED CONCENTRATE REP3RMPART I.it
COMMON NAME
631 METHYL PENTAQECANOATE
632 METHYL PALHITATE
611 METHYL ISOPALNITATE
63". OIBiNZOFURAN IOIPHENYLENE OXIDE)
635 2,2-DICMLOROBUTYRIC AGIO
616 2-ETHYLHEPTANOIC AGIO
637 H-CHLOROBENZOIC ACID
618 0-CHLOROPHENYL ACETATE
639 2.3.0,6-TETRACHLOROPHENOL
600 XCHL3ROBENZENE
6ii CHLOROVINYLBENZENE
60S SI.2. 3-TRICHLOROBENZENE
61.6 3.5-DIBRONOTOLUE.NE
607 U.2-OICHLOROETHYLI8ENZENE
601 XM-CMLORONITROBEKZENt
609 »Z.O-DICHLORONAPHTHALENE
650 CYCLOPENTENE
651 X»tM-OICHLOROBENZENE
652 X*»SNITROBENZCNE
653 l-CHLOROTRICYCLOm.3.1.13.11UNOECANE
650 OECANETHYLCYCLOPENTASILOXANE
655 2-CHLORO-1.3.5-TRIMETHYLBENZENE
656 1-CHLORO-ZIPHENVLETHYNVLI BENZENE
657 Z'METHYLBENZOTRIAZOLE
656 XETHYLENE 6LVCOL, BIS 12-CHLOROETHTU ETHE
659 CYCLOOOOECANOL
660 DIMETHYL SUBERATE
661 METHYL SUCCINATE.DIMETHYL ESTER
662 N-METHYL ETHENAMINE
663 XHEPTANOIC ACIO.ETNYL ESTER
660 2-12-CHLOROETHOXYIETHAMOL
665 UNOECANOIC ACIO.METHYL ESTER
666 XBENZENEACETIC ACIO.ETHYL ESTER
667 MET1YL P-ETHYLBENZOATE
668 XCLOFIBRATE
669 X9H-FLUOREN-9-ONE
670 X1-HETHYL>2.0-OINITROBENZENE
671 2.0-OICHLOROPHENOXY ACETIC ACIO. METHYL
672 METHYL ISONONANOATE
673 XETHYL CAPRYLATE
670 2-KETOPENTANEOIOIC ACID. DIMETHYL ETHER
675 CLOFIBRIC ACID,METHYL ESTER
CAS NO.
7132601
149 1Q A
1 1 £ J^f U
5129602
132609
13023002
3270291
535808
876277
938227
108907
89963
67721
1973220
622253
87616
1611923
1070119
121733
Z198756
102290
501731
98953
Z7011067
501026
1667005
10271575
13351730
112265
830137
1732098
1600111
38239279
106309
628897
1731868
101973
0306183
637070
086259
121102
50571088
2177868
106321
13192006
55162019
RELATIVE SIZE
*IC V1K T2B TIC Tl« T1Y TOCtTtXtNZC NZC PZC P2«
1.1 1.0 3.0*
0.0 3.0
1.0 3.0 -1.2
Z.I 3.0
3.0
3. 0 2. ft
3.0 2.6
3.0
3.0-0.% 0.7
3.0
3.0 1.8
3.0
3.0
3. 0
3.0
3.0
3.0 2.7
3. 0
3.0
3.0 -1.2
3.0-1.0
3.0
3.0 1.7
3.0
3. 0
3.0
3.0 t.l
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.8
3.0
3.0
3. 0
3.0-0.0
3.0
3.0
3.0
3.0
3.0
EPA It CONCENTRATES PAGE 15
026 OZX SZC SZX K1C IU
I.*
O.Z'
2.2
-o.» o.z
z.z
2.1
O.Z
(Continued)
-------
TABLE 9. (Continued)
EPA It CONCENTRATES PACE U
00
COMBINED CONCENTRATE REPORT(PART I.At
COMMON NAME
CAS NO.
VIC
RELATIVE SIZE
V1X T2B TIC T1X T1V T*Ct T%Xt HZC MZC PZC P2X 02C 02X SZC SZX SIC XIX
676
677
6/8
679
680
681
61Z
683
f.mi.
OB*>
685
616
687
688
689
690
691
69Z
693
69%
695
696
697
69S
699
700
701
703
70*
70S
706
707
708
709
710
711
712
713
71".
715
716
717
718
719
720
METHYL ISOTRIOECANOATE
ETHYL 7-NETHYLHYRISTATE
METHYL PENTACOSANOATE
l-H£XANOL
XHEKYL METHYL KETONE
2.5-HEXANEOIOL
5-HEXEN-2-OL
XN-AMVL ALCOHOL
¥uTr*nT TUF
Aitiuu I JNC
3-HETHYL-<»-HEPTANONE
Z-OOOECANOL
2-HYOROXY-6-METHYLBENZOIC ACID
t-OXO-NONANOIC ACIQ
Z-BROHO-1, 2-0 ICHLOROPRO PANE
1-BROHO-ZiI-OICHLOROPROPANE
1-U.3-OIHETHVLBUTOXVI-2-PROPANOL
TRIPROPYLENE GLYCOL
BUTYL BENT. VLPHTHAL ATE
X2.6-LUTIDINE
X2.H-LUTIDINE
2t3-LUTIOENE
Z,<>.6-COLLIOINE
3,<,,i.-TRIMETHYL-2-C»CLOHEXEM-i-ONE
2-PHENYL ACROLEIN
I-METHYLISOQUINOLINE
2-3-OIMETHYL QUINOLINE
y«PUpUA|jTUDpUC
**rncrmni nitric
XSOICYCLOHEXYL PHTHALATE
1.2-OIHYDRO-I.-PHENYLNAPNTHALINE
H-OIETHENVLBENZENE
1-PMENYL-3-BUTEN-2-ONE
3-7,ll-TRIMETHYL-3-OOOECANOL
XCETVL ALCOHOL
ZiZ*-BI-l,3-OIOXOLANE
N-PROPOXY ETHANOL
2-METHYLCYCLOPENTANONE
PHOSPHORIC ACIQ
0-ALLYLTOLUENE
P-ETHYL-ISOPROPYLBENZENE
H-ETHYLISOPROPYLBENZENE
(1,1 -DIMETHYL PR OPYL) BENZENE
1-HETHVL INDAN
1-ETHYL INDAN
l-HETHYL-ltZ-OIPHENVLETHANE
HEXAN-3-ONE
17318*0
17670756
55373892
111273 O.Z
111137 0 0
29357<.
563619
108758
17299'tll
1.95103
17219J3
1721897
81.617 S.l 0.0
7i.69i.01 a 1.0
108576 A 3.0 I'll
371.1.2550 a 3.9
7278651 3.0
36653821. 3.0
6705891 3.0
2607309 3.0
1120725
15870I.C a 1.0 I.I
<>218<.88 A 1.0
1.920991. A 0.0
20<.995« A 1.0
767588 0.0
1.830993 A -1.0
5811.657 A 1.0
589388
3.0
3.0
3.0
3.0
3.0 0.6* 2.Z
1.0 3.0
!.0 3.0 2.6
.0 3.0 1.6 1.9 l.Z
3.0
3.0
.0 2.9
.0
.0 Z.7
.0 1.7
.0
.0
.0
.0 0.6 -1.1
. -O.t l.t
-o.%
. 9.9
1.9 2.Z
•
Z. 9.2
1.0 -0.
A* 9 A* ft t* • T* • fc* 11 * H 91l t Mt
. • O* £» 8* •• • •• » ••* ••• " B» €, 1 oC
2.6*0.6* Zo *
1.1* -1. *
2.6* 2.9*
1.9*
0.6* 1.0* 1.9*2.2*
1.9*0.9*
2.6* -0.2*2.9 2.9*
0.6* 0.1*2.9
-fl.«.* 2.9-0.1*
0.6* l.S*2.9 0.9*
l.f 0.6* 2.9* 1.2*
2.1* 2.9*
2.8* 2.9*
-0.6 2.1 2.0 2.9
«^9
• C
IB A ft
"Hoi
•O.I
2*1
3,0
1.2"
l.Z
* SEE LAST PAGE OF TABLE
(Continued)
-------
TABLE 9. (Continued)
EPA II CONCENTRATES PACE I?
COMBINED CONCENTRATE REPORTIPART I.II
721
7ZZ
723
72*
725
726
727
721
729
730
731
732
733
73*
735
736
» 1 7
f Jf
731
739
7*0
7*1
7*2
7*3
7**
7*5
7*6
7*7
7*1
7*9
750
751
752
753
75*
755
756
757
751
759
760
761
762
Tt I
/ b J
76*
765
COMMON NANE
6-METMYL TETRALIN
Z.3.*-TRIHETHVLBENZOIC AGIO
2-HETHVL-2-NONEN-t-ONE
XCHLOROACETIC ACID
P-DIISOPROPYL BENZENE
1-HEPTENYL8ENZENE
2.3.6-TRIMETHYL 8ENZOIC ACID
3-METHYL-2, 2-01 OXIDE- 1X-Z .1. 3-BENZOTHIAP
XCHLOROACETONE
ISOPROPYL ACETATE
.8ETA.-OKO-8ENZENEACETIC ACID. ETHYL EST
1.3-OlHYORO-2.2-DIOXIDE-Ztlt3,BENZOTMIAO
HETHYLISOBUTYL BENZENE
SEC-BUTYL ALCOHOL
3,S,5-TRIHETHVL-2I5HI-FIMANONE
2-PROPVLCYCLOHEXANONE
S-METHYL-5-PHENYL-Z-MEXANONE
TETRAMETHYL8EN/ENE PROfANOIC ACID
2.2-DIHETHYLPROPANOIC ACID. 2 .* ,6-TRIMET
6-UNDECANONE
2.6-OIHETHVLCYCLOHEXANDL
HEXAHYDRO-3-I2-PROPENYLI-2H-AZEPIN-Z-ONE
ll2.6-OIHYDROXV-*-NETHOXYPHENVLIETHANONE
XMNDELIC ACID
(2-CHLORO-2-PROPENYL) OXVBENZENE
OECYL VINYL ETHER
. ALPHA. -HYOROXY-. ALPHA. -NETMYL BENZENE A
*-BUTVL-1.3-CVCLOPENTAMEPIONE
PHTHIOCOL
P-ISOBJTYLTOLUENE
XORCINOL
DIBUTYL-3-NETHYLGLUTARATE
7-METHYL-7-HEPTAOECANOL
CVCIOHEXYL CHLORIDE
1-PMENYLNAPHTHALENE
2-PHENVLNAPMTHALENE
2-EFHYL TETRALIN
X2-HETHYLANTHRAQUINONE
".-METHYL INDAN
BENJILIOENEACETONE
2,i.-DIMETMYL-l-SEC-BilTYLB£NZENE
Th^BA N SEE NO. 565
*-ElMYL8ENZYL ALCOHOL
VER«TRALOEHYDE
CAS NO.
< VIC VIX TZB TIC T1X
1611519
1076*77
2903233
79111
100115
129992
252936*
Z225*03
71955
10121*
61*277
1615061
100
71922
51591500
9*655
1*121611
55613101
5*6***05
927*91
533772*
295593*0
7507893
906*2
53299539
765059 a
515300
5*2**723
•.63556
51610*6
50*15*
56051606
55723938
5*2117
605027 A 21
6129*2 A 10
323675*7 A 11
1*5*1 a 10
12*226 A -10 1.0
122576 A 0.0
1*83609 A
* AC 1 t
O • i 3 J
768592 a
1201*9
RELATIVE SIZE
T1Y TtCtTkXtNZC NZC PZC PZ<
02C OZX S2C SZX X1C XU
1.7 2.8* Z.9*
1.1
Z.I
I.I
1.1
1.1
Z.9 1.7
Z.
2.
1.6* Z.
2.
2.6* Z.
Z.
1.6* 2.
*£ y
TTW CD O
2.
2.
Z.9
Z.
1.
Z.
Z.
Z.
2.
2.
2.
2.
2.
2.
2.
2.
2.
2.
2.
2.
2.
Z.9 Z.Z
-O.I
Z.9
I.)
Z.)
Z.9
Z.9
Z.9
Z.9*
Z.9
Z.9
2.9
Z.9
Z.9
Z.9
Z.9
1.2 Z.Z
-O.I*
1.9*
I.Z
1.9*
1.9 1.9*
* 1.9*
Z.Z
SEE LAST PAGE OF TABLE
(Continued)
-------
TABLE 9. (Continued)
EPA II CONCENTRATES PAGE t*
COHBINEO CONCENTRATE REPORT(PART I.A I
CONNON NANE CAS NO.
*
766 1,3-OINETHVNAPHTHALENE 575<»17 »
767 I2-HETHVL-1-PROPENYLI BENZENE 768<>90 A
768 P-DIPROPYLBENZENE <»81557fl A
769 (1,1-OINETHVLBUTVLl BENZENE 1985575 A
770 XAZULENE 27551". a
771 1-HETHVLFLUORENE 1730376 a
772 5-HETHYL-2-HEXANOL 627598
773 3,5,5-IRIHETHYt.-Z-CYCLOPENTEN-l-ONE Z7
778 IOOOCVCLOHEXANE 626620
779 2,2-OINETHYLSUCCINIC ACID 5971.33
780 TRANS-3-BUTYLTETRAHVORO-2-HETHVLFURAN 16712206
781 <>-HYDROXY-3-NETHYL-2-l2-PROPENYLt-2-CVCL 5511.51
782 OCTAHYORO-0
79>> 2.I.-OIMETHYL HEXANOIC ACID %2329908
795 1-ETHYL-3-NETHYL BENZENE 6201't'.
796 1>6 OINETHYL-1.-ISOPROPYL-NAPHTHALENE 1.83783
797 1.2.3-TRIHETHVL BENZENE 526738
798 l-(3.3-DIHETHYLOXIRANVL)ETHANONE %<«78631
799 2,2-OIMETHYL BUTYRIC AC 10 595379
800 2-ETHYLBUTYRIC ACI3 88095
801 <>,i.-OIMETHYL-l(3-DIOXANE 766151.
802 X3.I.-OICHLOROPHENOXYACETIC ACID 588227
803 D30ECAMETHYLCYCLOHEXASIL0XANE 51.0976
801. X2.6-DIMETHYLNAPHTHILENE 5811.20
80S XO-C-iLORONITROBEMZENE 88733
806 XNESITVLENE 108678
807 l-OICHLOROH£THYL)-%-ETHYLBENZENE S<»789296
808 1,1-OIBUTOXY-BUTANE 5921802
809 CIS-9-OCTADECbNAHIOE 301020
810 X*TRIPHENYL PHOSPHATE 115866
RELATIVE SIZE
VIC V1X T28 TIC T1X T1V UCtUXtNZC NZC P2C P2K 02C 02X S2C S2X XIC XIX
2.«*
2.8*0.9 1.** t.2*
2.
2.0
2.0
O.b
-1.1
-1.8 1.0
2.t
2.0
2.0
l.b*
i.r*
i
2
1.7 2
t
t
2
2
t
2
I
2
t
t
t
2
2.7*1
2.
2.
2.
,2.
2.
2.
2.
1.9*
1.2
1.9
z.a
i.o
i.o
0.6
-0.%
1.6
1.6
2.
2.
2.
2.
g.6 z.
1.6 2.
2.
2.
1.6 2.
2.
2.
2.
2.
t.
2.
2.
2.
2.
2.
0.2*
2.2 Z.2
1.9
1.8
l.B-O.t
1.9
0.9
t.l
-0.8
2.2
0.2*1.2
1.2*
Z.2
0.2
1.2
Z.2
Z.2
0.2
0.2 2.2
* SEE LAST PAGE OF TABLE
(Continued)
-------
TABLE 9. (Continued)
COMBINED CONCENTRATE REPORT (PAR? I.At
COHNON NAME CAS NO.
811 3.3.5-TRIHETHVCVCLOHEXANONE 8739*9
• 12 d-ISOPROPYLACETOPHENONE 6d5136
• II 2-NETHYL-3-OXOHEXANOIC ACIO. ETHYL ESTER 2930dd03
aid 3-OCTANONE 186683
815 DIAHYLPHTHALATE 131180
816 <>,7,7-TRIHETHVLBICVCLOIZ.Z.llNEPTAN-Z-ON 10292985
817 X»0-CHLOROTOLUENE 951.98
818 1.1,2,3-TETRACHLOROPROPAHE 181.95302
819 ETHYL BUTYL KETONE 10635d
820 XH-ANINOACETOPHENONE 99036
•21 ALPHA-CHLOROPROPIONIC ACID 598787
• 22 Z.3-OIMETHYL-2-PENTANOL 1.911700
•23 3-CHLORO-Z-METHYL-1-8UIENE 5166358
• 21. 2,3-OICHLOROISOBUTANAL 1011,1227
•25 l-CHLORO-3-ICHLOROHETHYL)BENZENE 620202
826 l.d-DIMYORO-1-NETMYL-d-OXONICOTINONITRIl. 767986
827 Z,d.d-TRIHETHYL-Z-PEMTENAL 53907612
828 1-NETHYL-d-ISOPROPYL-l.Z-CYCLOHEXANEOIOL 33669760
•29 X3-HETHYL-1-BUTANOL ACETATE 123922
• 30 TIG»LO£HYOE <>97030
831 TRIHETHYLOXIRANE 5076197
832 l-HYOROXV-3-HETHVL-Z-BJTANONE 36960222
833 CIS-Z.3-EPOXYHEXANE 61Zd909
• 3", Z,
-------
TABLE 9. (Continued)
COMBINED CONCENTRATE REPORT (PART I.II
Ef A It CONCENTRATES PACE ZO
COMMON NAME
CAS NO.
RELATIVE SIZE
tflX T2B TIC Tin Tit TkCtTkXtNZC MZC P2C P2I 02G 02X SZC S2K XtC XIX
856
857
858
859
860
861
862
863
864
865
866
867
868
869
870
871
872
873
874
875
876
877
878
879
880
881
882
883
884
845
886
887
888
889
890
891
892
893
894
895
896
897
898
899
900
TETRAETHYLENE GLVCOL DINETHVLETHER
TETRAPROPVLENE GLYCOL METHYL ETHER
4-CHLOROCROTONIC ACID
XSACCHARIN
H-OI-SEC-BUTYLBENZENE
P-Ol-SEC-BUTVLBENZENE
X2-METHVL-Z-PHENYLOXIRANE
6,6-DIHETHYL-2.5.10-UNDECANETRIONE
2-METHYL-2-CYCLOPENTEN-1-ONE
3,4-OIHETHYLBENZALDEHVOE
3-BROMOHEPTANE
N-BENZOYL-L-ALANINE. METHYL ESTER
1-HEPTAOECANOL
1.1.2-TRICHLORO-l-PROPENE
3-METHYL-Z-HEPTANOL
X»0-CHLOROANILINE
2-ETHVLACETOACETIC AGIO
TRIDECYLIC ACID
5-HETHYL-3-HEXEN-2-ONE
4.4-OIMETHYLHEXANAL
TETRAHYORO-2H-PYRAN-Z-ONE
2-OECANOL
XP-TERT-BJTYL PHENOL
2.S-OICHLORO-4-HETMVLBENZOIC ACIO
1-NAPHTHOIC ACID
2-CHLORO-3-HETHVL-2-BUTENE
•*1PENTACHLOROBIPHENYL » OTHER PCBS
2.4-DICHLOROPENTANE
3.6-DIMETHYL-3-HEPTANOL
l-ETHOXY-2-HEPTANONE
3-CYCLOHEXYL-4-PENTEN-Z-ONE
3-METHYL-li2,4-CYCLOPEMTANETRIONE
3-ETHOXYPROPANAL
1-ll-CYCLOHEPTEN-l-YDETHANONE
4,4fS>5-TETRAMETHYL-2l7-OCTANEOIONE
XBETA-CITRONELLOL
3-ETHYL-4-METHYL-3-PENT£N-2-ONE
4,4-OIHETHYLCYCLOHEXENE
l-NITRO-2-OCTANONE
5.5-DIETHOXY-3-PENTYN-Z-ONE
3-ALLYL-Z.4-PENTANEDIONE
2,2-OIMETHYL-3-PRaPYLOXIRANE
7-METHYL-3-OCTEN-2-ONE
HENTHYL ACETATE
143248
20324349
16197903
81072
1079965
1014411
2085883
50464965
1120736
5973717
1974056
7Z44679 1.1
1454859
21400259
31367461
95512
4433856
638539
5166530
5932912
542289
1120065
98544
21460888
86555
17773658
800
625673
1573Z80
51149703
55702540
4505548
2806851
14377118
17663273
106229
22287112
14072867
16067019
55402045
3508789
17612350
33046810
16409453
-0.4 2.6
2.6
2. 0.8
2.
2.
2.
2.
2. 2.2
2. l.J 2.2 1.2
2. l.»
2.3
2.2
2.0 2*2
t.O 1.6 1.7 2.2
1.6 2.2
-0.4 0.6 2.2
0.8 1.1 2.2
1.9 2.2 S..2
l.i 2.2
8.9 2.2
2.2
2.2
2.2
2.2
2.2
2.2
1.2 2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
(Continued)
-------
TABLE 9. (Continued)
COMBINED CONCENTMTE REPORTIPARr I.It
EPA It CONCENTRATES PAGE 21
901
902
903
90*
905
906
907
906
909
910
911
912
913
91*
915
916
917
916
919
920
921
922
923
92*
925
926
927
926
929
Qlfl
7 JU
931
932
933
93*
935
936
937
936
939
9*0
9*1
9*2
9*3
9**
9*5
COMMON NAME
3-HETHVL-3-OECEN-2-ONE
6-HETHVL-3I2HI-BENZOFURANONE
OI-SEC-BUTOXYHETHANE
XANTHENE
6-DOOECANOL
2-METHVL-2-HEXANOL
5-M£THYL-3-HETHVLENE-2-H|XANONE
CYCLODECANOL
1-IETHNYLOXYIPENTANE
CIS-3,*-OIHETHYL-l-HEXCN-2-ONE
PHENYLBUTANAL
CIS-5 -BUT YLDI HYDRO- I,-NETHYL-2I3HI-FUR«NO
2,6-DIISOPROPYLPHENOL
ALPHA-FARNESAL
3A.i.,5,7A-TETRAHYDRO-*-HYOROXY-3A,7A-OIM
BUTYL CVANATE
ETHYL AHYL KETONE
3.6-NONAOIEN-2-ONE
3A,i,,7,7A-TETRAHYORO-2-P»OPYL-lH-ISOINOO
2-HEXEN-l-OL
ISOCYANOETHANE
*-PENT£N-2-OL
3-CHLORO-3-BUTEN-2-ONE
1 Z-l PENT YLOKTI ETHYL 1C YCLOHEXANE
OIHETHYLSULFONE
2, *-OI-TERT-8UTYL PHENOL
2-CHLORO-2-PROPENOIC ACI9
BETA-RESORCYLIC AGIO
XP-NITROBENZOIC ACID
TETRAHYOROFURFURYL ALCOHOLI THFA
LOLIOLIOE
(•tSFLUORANTHENE
HETHVL HEPTAOECANOATE
XPROPIOPHENONE
11-NITROETHYLI BENZENE
2,3,*,5-TETRACHLOROANILlNE
tO-CNLOROPHENOL
2-HETHYL-l-NAPHTHALENOL
2.3-OICHLOROBUTENE
1-BROHO-2-CHLORO-2-BUTENE
2.*-OICHLORO-l- (CHLOROHETHVL) BENZENE
1.2-OICMLORO-*- BENZENE
X»9H-FLUORENE
P-BROHOTOLUENE
CAS NO.
S**ll039
20(95*1*
2566925
92631
6636360
625230
1187677
1502052
5363633
20665*5*
16326115
55013326
20765*6
*9S5322
5*31,606*
17662*7
5*1655
55262901
2021207
2*9169
62*793
625310
663705
5*65275*
67710
9676*
596796
69661
62237
9799*
1133035
206*1,0
1731936
93550
721*611
63*633
95576
7*69771,
7561977
5**106*3
9*995
102*76
66737
106367
RELATIVE SIZE
VIC VtX T28 TIC TIX T1Y UCtUXtNZC N2C
-2.1 2.0-0.*l*0.* 1.6*
-1.1 2.0
0.0 2.0
1.0 2.0
1.0 2.0 0.6
2.0
2.0
2. 0
2.0
2.0
2.0
2.0
2.0
P2C P2I 02C 02X S2C S2X XtC XI*
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2 2.2
2.
2.
2.
2.
2.
2.2
2.2
?•*
5.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
2.2
O.I -0.6
1.9*
(Continued)
-------
TABLE 9. (Continued)
EpA 18 CONCENTRATES PACE ZZ
COMBINED CONCENTRATE REPORT(PART I.AI
COMMON NAME
Ln
-P-
946 l.Z-DICMLORO-3-NITRDBENZENE
947 2-CHLORO-P-CYHENE
941 2-CHLORO-1-U-ETHYI.PHENYLI-2-HETHYL-1-PR
949 + X*SLINPANE
950 HETHYL OICHLOROACETATE
951 XUKETMANE (ETHVLCARBAHATEI
952 4-CHLOROPHENVL ACETIC AGIO. METHYL ESTER
953 METHYL ANTEISOPENTAOECANOATE
954 P-CHLORO-2-NITROANILIHE
955 2,4-D.ETHYL ESTER
956 ALPHA-KETOGLUTARIC ACID
957 METHYL PROPENYLOXY KETONE
958 4-HYOROXY-4-HETHYLCYCL3HEXANONE
959 3.4.5-TRIHETMYL-2-CYCLOPENTEN-1-ONE
960 XETHYLENE GLYCOL
961 GAMMA-PICOLINE
962 2.5-LUTIDINE
963 2.3,6-TRIMETHVLPYRIDINE
96% 5-ETHYL-2-PICOLINE
965 2t3,4-TRIMETHYLPYRIDINE
966 2,HENYLETHYL> ACETATE
981 Z-XYLYLETHANOL
982 XCINNAMALDEHYOE
993 ACETYl 8IPHENYL
98<> <>-OCTANONE
985 3-BUTEN-2-OL
916 0-ETHVLSTVRENE
987 1-HEPTADECENE
988 3.5-OIMETHYL-2-CYCLOHEXEN-1-ONE
989 OODCCANAMIDE
990 METHYL-2t3-OIHETHVL BENZOATE
CAS NO.
RELATIVE SIZE
VIC VIX T2B TIC TIX T1Y TdCt TltXt MZC NZC C2C P2X 02C OZX SZC S2X X1C XIX
3209221
".395793
55012696
51899
11651.1
51796
31.01.061.7
5129661
8963".
51.5711.99
321507
17257793
171.29026
55683211
107211
108891,
519935
1<>628<>6
lOf.905
2233296
1122390
1122696
17<>29297
51. 11.68
91225
91634
110915
19730042
130381,51. 0.0
130314,76 1.1
3177191 A
767602 A
300 A
2K,1620
1031.57
27577961,
104552
91,7911
519639
591323
7564631 A
6765395
1123097
1120167
15012369
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.9
2.0
2.0
2.0
2.0
Z.l
2.0
2.0
2.0
2.0
2.0
2.0
2.0
Z.O
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
1.2
1.7
-0.1
0.6
1.9
2 t.
2
2.0
1.9 1.9
-O.I.
0.6
0.6
1.1*
1.9'
1.6*
1.6*
1.6
-a.
.9*
0.7
o.z
-0.1
l.Z
0.2
* SEE LAST PAGE OF TABLE
(Continued)
-------
TABLE 9. (Continued)
EPA II CONCENTRATES PAGE 21
Ul
COMBINED CONCENTRATE REPORTIPART I.A I
COMMON MAKE
CAS NO.
RELATIVE SHE
* vie vix TZB ric TIX TIV n.ctuxt«c NZC PZC PZ« 020 otx szc szx xic xix
991
992
993
99<>
995
996
997
991
999
1000
1001
1002
1003
1001,
1005
1006
1007
1001
1009
1010
1011
1012
1013
1011,
1015
1016
1017
1010
1019
1020
1021
1 OZZ
1023
1021,
1025
1026
1027
1028
1 t\ >Q
1 U c »
1030
1031
1032
1033
103<>
1035
HETHYL-11-OCTADECENOATE
METHYL-9,12, 15-OCTAOECATRIENOATE
ZN.II-OIHETHYLBENZENESULFONAHIOE
3-NETMYL-l-PENTANOL
X»ACENAPHTHALENE
OCTADECANOL
ANTEISOHEPTADECANOIC ACID
<•--NETHYLCVCLOHEXANE CARBOXVLIC ACID
PSEUD OCUNENE
ACETOACETIC ACID
1. ".-DIMETHYL- 2-ISOBUTYL BENZENE
2,3,1,-TRIMETHYL-Z-CYCLOPENTEN-l-ONE
5-NETHYLFURFURAL
1,1-OIHETHVL INDENE
2-PENTENOIC ACID
1,-OCTENOIC ACIO
XN-UNOECYLIC ACID
CLOFIBRIC ACIO, N-SHLORO ISONER
7-OKO-OCTANOIC ACIO
1,Z,3,3A-TETRAHYORO AZULENE
7-OCTEN-Z-ONE
6-NETHYL-BICYCLOU.l.OIHCPTANONE
XFURFURAL
6-METHYL-3.5-HEPTAOIEN-Z-ONE
Z-METNYL-Z-d-NETHYLPROPYLI-OXIRANE
XOIEfHYL SULFITE
3-ISOPROPYL-Z.I.-PENTANEOIONE
MEXAHYDRO-I.-METHYL-2H-AZEPIN-Z-ONE
2-METHLY-5-ISOPROPYLCYCLOHEXANONE
2-BUTYL-2-OCTtNAL
3,3-OIM£THYL-2(3H»-FURANONE
3-H»DROXY-2,l,-PENTANEOIONE,BENZOATE
5Z380333 Z.O
301001 Z.O
61,0619 Z.O
509355 Z.O
83329 -0.% -I.I 2
267621,1,7 1.6* 2
-.57 2
31963916 2
1651921,7 2
5009325 2
20193231 -1.1 1.9*
827521 A i.o 1.6* 1.1* 1.9* 1.2
539822 0.0 1.9
1Z3660 0.0 l.i
51,789150 A -1.0 1.6* l.»* 1.9* -I.I
ZS55013*. A 1.0 1.0 1.7 1.9
1750512 1.0 ' 1.9
1125800 1.1 1.9
1,33151,8 0.6 1.9
5(,1SO<> 1.6 1.9
55669000 A -0.%* 1.9*
21790065 1.6 1.9
620020 0.6 1.
10636550 I.I 1. -I.I
626982 1.1 1.9
18291.898 1.
112378
171,13739 .
1<«1 1298 2 .
33877871
366<>606 .
11,01,51,1 .
90011 .
lbbl.70',1. .
1,23201,30
623811,
151,0381
3623050
1.99707
13019161. .
13521,760 .9
i,6ZOi,77 .9
* SEE LAST PAGE OF TABLE
(Continued)
-------
TABLE 9. (Continued)
EPA IS CONCENTRATES PACE 2%
COMBINED CONCENrRArE REPORT I PART I.A)
COMMON NAME CAS NO.
1036 2.2-DIHETHYLHEXANEOIOIC ACID. OINETHYL E 17219215
1037 VINYL CHLORIDE 75014
1038 XCROTONIC ACID 3724650
1039 3-PENTENOIC ACID 5204648
1040 XOXALIC ACID 144627
1041 7-NONCNOIC ACID 1022
1042 l-ErHYL-2.3-DIMETHYL BENZENE 933982
1043 U-ETHYL-2-PROPENYLI-BENZENE 19947229
1044 2.6-DIMETHYLSTYRENE 2039909
1045 8IS(3-H£rHYLPHENVLIMETHANONE 2852688
1046 1-ACETVf.PIPERIOINE 618428
1047 CIS-2.3-DIHYORO-2-HErHYL-lH-INOENE-l.2-0 56588400
1048 2.3-OIHYORO-3.3-OINErHYL-lH-INOEN-l-OL 38393929
1049 5-ETHENYL TETRAHYORO-.»Li»HA... ALPHA. ,5-T 5989333
1050 1-ll-CVCLOHEXCN-l-YLIETHANONE 932661
1051 H-HENTH-K7I-ENE ««•-«-» 13837713
1052 1.7.0IHYORO-2-IHETHYLAItlNOI-6H-PURIN-GON 10030781
M 1053 1-ALLYLBENZENE 637503
<-" 1054 2(3H)-BENZOTHIAZOLONE 934349
^ 1055 XP-TOLUQUINONE 491350
1056 4-METHYLPHENANTHRENE 832644
1057 3*|itt-DIHYDROXYACETOPHENI}NE 1197097
1058 TAANS-3-HETHYL-3-PENTENOIC ACIO 41653934
1059 5-ETHYLOIHYDRO-2C3HI-FURANONE 695067
1060 0-CRESOTIC ACID 83409
1061 PMLOROL 90006
1062 2.3-DIHETHVL TETRALIN Z1564921
1063 OCTYL BENZENE 2189606
1064 2.4,5-TRIHETHYLBENZALDEHYOE 5779726
1065 3-METHYLSTILBENE 14064483
1066 BENZIL 134816
1067 2-C1-I2-HETHOXVETHOXYIETHOXV1ETHANOL 1017
1068 XP-CYNENE (P-ISOPROPVL FOLUENEI 9967,6
1069 ltli2t3.3-PENTACHLOROPROPANE 15104617
1070 XOHF (DIMETHYLFORMAMIDE) 66122
1071 1.6-DIIt£rHYLNAPHTHAL£NE 575439
1072 5-HETHYL TETRALIN 2609645
1073 2-PROPYLHEPTANOIC ACID 31080394
1074 X3.5-DICHLOROPHENOL 591355
1075 0-ISOPROPYL8ENZOIC ACIO Z438042
1076 0-EFHYL 70LUENE 611143
1077 l-METHYL-2-CYClOHEXEN-l-OL Z3756272
1078 TRI-N-PROPYLENE GLYCOL, NETHYL EfHER 13133294
1079 4-ETHYLPYRIOINE 536754
1060 Xl,3,6-TftIMETHYL-2,4llH,3H)-PYRINIDINEDIO 13509529
* SEE LAST PAGE OF TABLE
RELATIVE SIZE
* VIC V1K T28 TIC T1X T1Y TtCtUXtNZC N2C PZC P2« 02C 02X S2C SZX XIC MIX
l.»
1.9
t
1.2
O.Z
o.o
1.6
•O.I,
1.6
1.6
t.r
1.7
0.7
-0
I*
a*
-S.I
Sot
•0.2
•0.2
-0.1
0.2
i.2
-a.i
l.g
(Continued)
-------
TABLE 9. (Continued)
EfA It CONCENTRATES PAGE
COHBINED CONCENTRATE REPORT(PART I.A)
COMMON NAME
CAS NO.
RELATIVE SIZE
* vie vix TZB ric MX TIV ucmxtuzc «c PZC PZ< oz: ozx szc szx xtc xix
1061
1082
1063
1061.
1085
1086
1087
1 AAA
1 UOO
1 AAQ
1 If 07
1090
1091
1092
1093
1091.
1095
1096
1097
1096
1099
1100
1101
1102
1103
I IQi.
1106
1107
1108
1109
1110
till
1112
1113
till.
1115
1116
1117
1118
1119
1120
1121
1122
1123
1121.
1125
XCAPRALOEHVOE
3*.t»-OINETHOXYACETOPHENONE
X'OIPHENYLAHINE
BUTYLATtO HYOROXV TOLUENE IBHTI
XPHENYL ETHER
Z-METHYL-3-PENTANONE
Z-ETHYL PENTANOIC ACIO
UUO ~ C. J.ME
1-EFHYL-3.5-OIMETHYL BENZENE
I.-ETHYL-1.2-OIMETHYL BENZENE
liOOURENE
l.Z-OIMETHYL INOAN
Xl.t-OIMETHYLNAPHTHALENE
P-CHLORONITROBENZtNE
2, 3, 6-TRI METHYL NAPHTHALENE
1.6.7-TRlHETHYLNAPHTHALENE
1.I..6-TRIHETHYL NAPHTHALENE
5-CHLORO-Z-HETMVLBENZOFURAN
CIS-l.Z,3-TRIN£THYL-i»-PROPENYLNAPhTNALEN
CHLOROFLUOROBENZENE
1.1.3-TRICHLORO-2-KETHYL-1-PROPENE
PENTACHLOROBENZENE
Z-T-BUTYL NAPHTHALENE
I.-PHENVLBICYCLOHEXYL
X* + (HEPrACHLOR
NITROCVCLOHEXANE
2.6-OIMETHYLCVCLOHEXANONE
METMOXYCYCLOHtXANE
3-ETHYLHEXAWIC ACIO
P-ETHVL TOLUENE
ACETOIN
2-METHVL-2-ISOPROPYL-1.3-DIOXOLANE
I.-PHENYL PENTANOIC ACID
DIMETHYL ISOPROPYL BENZENE
(.-HYDRO* V-I.-HETHYL-Z-PE NT ANONE
1-INDANONE
2,Z*METHYLENEBISI6-
-------
TABLE 9. (Continued)
EPA II CONCENTRATES PAGE 26
Ln
00
COMBINED CONCENTRATE REPDRMPARI I.At
COMMON NANE CAS NO.
1126 5-HEXENOIC ACID 1577336
1127 2,6-DINETHYLHEPTANOIC ACID 601".19<,9
1121 3,3-OINETHYLBUTVNE 917920
1129 SEC-ISOAMYL ALCOHOL 5917SI,
1110 7-BCTEN-I.-OL 53907725
1131 2-METMYLCYCLOPENTANOL ACETATE 1,0991933
1132 2,1,-OIISOPROPYLPHENOL 293<>056
1133 ETHYL i»-HYOROXYPHEN»LACETATE 17131212
us*. OIOITYL AZELATE io32<,2
1135 TRIETHVLENE GLYCOL. PHENYL ETHER 720<>162
1136 2-ErHYL-3-PROPYLOKIRANE 53*97328
1137 ONU (DIMETHYL UREA) 53362I1-ETHYLPROPVL>TOLUENE 22975512
1139 2-METHYL-l-DOOECANOL 572A9266
1K.O 2-HETHYLENE-l-BUTANOL ACETATE 55670092
TETRAHYDROFURFURYL ACETATE 63767 5-NONANOL 62393A
ll1261
Il99
115<> OIPROPYL CARBINOL 519559
1155 XGUAIACOL 90051
1156 SPIROOOOECANE 111157
1157 l*PHENYL-lt2-PROPANEOIONE 579077
1151 FARNESOL 379071*.
1159 l-IBROMOHETHYLI-'.-METHYLBENZENE 104.111,
1160 P-CHLOROANISOLE 623121
1161 1.2,4.5-TETRACHLOROBENZENE 9591,3
1162 H-CHLOROeTHVLIOlN£THVLBENZENE 54(1,11211
1163 2-BIOHO-ifHETHYL-l-ISOPROPVLBENZENE 4,1,71106
116l( 1-ICHLOROMETHVLINAPHrHALENE 16522
1165 MTETKACrtLOROBIPHENYL 26914330
1166 *SPENTACHLOROBIPHENYL 251,29292
1167 3-HEXYL BROMIDE 3377175
1161 1.1,2-TRICHLOROPROPANE 591776
1169 5.8-DIMETHVLQUINOLINE 2623509
1170 2,3,5-COLLIOINE 695917
VIC K1X T2B TIC Tl«
RELATIVE SIZE
T1V
N2C »2C P2« 02C 02X
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
l.t
S2C S2X
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.2
.2
.2
.2
.2
.2
.2
.2
X1C MIX
-0.1
1.2
(Continued)
-------
TABLE 9. (Continued)
COMBINED CONCENTRATE REPORT (PART I.»l
COHNON NAME
1171 *-ETHYL-2,6-OINETHYL PYHI DINE
117Z 3-ETHYL-Z,*,S-TRIMtTHYL-lH-PYRROLE
1171 XZ,*-OIMETHYLQUINOLlNE
ll/i, TRIETHYLENE GLYCOL N-BUTYL ETHER
117S NETNYL OLEATE
1176 l.Z-BENZISOTMIAZOLE
1177 9,12-OCTAOECAOIENOIC AC IB
1178 *-ETH£NYL BENZOIC ACIO
1179 *-HYOROXVACETOPH£NONE
1180 2-HYOROXV OECANOIC ACIO
1181 XMETA-CRESOL
1182 1-N»PHTHALENOL
1183 OIETHVL PHENOL.(l-HETHYLETHYL)-BENZENE
1210 2.<,-OIHETHYLISOPROPYLB£NZENE
1211 3-PHENYLPENTANE
1212 3.5i5-TRIHETHYLCYCLOHEK-3-EN-l-ONE
1213 $N-PROPri BENZENE
121<» l.J-QIHdTHrL INOAN
1215 <.,i.-OIHETHYL*2>PENTeNOIC ACIO
CAS NO.
36917369
SZ069*
1198371,
11.3226
1 1 2629
272162
60333
1075".9b
7339879
S393817
10839",
90153
26967657
100663
605390
76937
610<.80
6137117
55*121
1Z2009
1667012
6630019
5830*0
*0133«,7
91190
1*010232
119619
129000
758*3
2679870
*087696
167*7506
98828
622322
1120258
1*171892
5*0631*8
110383
*706905
1,706892
1196583
1.71012
103651
*175535
69*5353
RELATIVE SIZE
* VIC V1X TZB TIC T1K T1V T*CtT»XtNZC
1.0
1.0
1.0
1.1
1.1
1.1
1.)
A 1.0
1.0
1.0
1.0
1.0
1.0
1.0
A 1.0
1.0
1.0
1.0
1.0
a 1.0
a i.o
A i.o
a l.
a l.
1.
A 1.
a 1.
0.0 >0
.0
.0
.0
.0
.0 -1.%
.0
.0
-0.*
0.6
a -0.**
0.6
EPA II CONCENTRATES PAGE 17
NZC PZC PZ« OZC Ott S2C SZX XtC IU
-0.*
o.»*
0.8*
1.8
-0.2
-I.Z
0.1
0.*
0.1*0.9
0.9
0.9
0.)
0.9
1.9
0.9
0.2
0.2
* SEE LAST PAGE OF TABLE
(Continued)
-------
TABLE 9. (Continued)
EPA 11 CONCENTRATES PAGE 21
COMBINED CONCENTRATE REPORMPART I.»l
COMMON NAHE
1216 C6-3ENZENE
1Z17 Z-METHYL-2-BUTENAL
1211 3-FUROIC ACID
1219 TETRAHYDRO-3,6-OII1ETHYL-2M-PYRAN-Z-ONE
1220 Z.3-DIHETHYL-1.I.-HEXADIENE
1221 2-METHYL-CVCLOHEXANEHETHANOL
1222 XMETrtYLPHENYL CARBINOL
1222 3.1.-OIHYORO-1CZMI-NAPHTHALENONE
122<> PENTAMETHYLBENZENE
1Z25 XIS03UINOLINE
1226 X+SDOE
12Z7 Z.I.-DIMETHYLPENTANOL
1221 3,3-OIMETHYLBUTANANINE
1229 Z.7-OINETHYL TETRALlN
1230 2t<>-OIHETHYLHEPTANE
1231 2,6-OIMETHYLHEPTANE
1232 2-I2-NETMOXYPROPOXYI-1-PROPANOL CA OIPR
1233 ETHYL BENZOPHENONc
1231, 2,*-OICHLOROANILIN£
1235 Z3.it-OICHLOROANII.INE
1236 2-IOOOPENTANE
1237 Z-NETHYLTHIOPHENE
1231 1,1,3-TRICHLORO-l-BUTENE
1239 1-ETHYL-2.I.-OINETHYL BENZENE
121.0 l,6-DINETHVL-«-ISOPR0PYL TETRALlN
I2«.l 2-ETHYL-l,3-D:METHYL BENZENE
1242 TRIPROPYLENE CLYCOLi METHYL ETHER IISONE
12<.3 2-IMETHYLTHIOIBENZOTHIAZOLE
121.lt NONANAL
127 l.>t-OIHYDRO-2.5.1-TRIHETH\rLNAPHTHALENE
121.8 Z*»SHEX»CHLOROBENZENE
12W l-HETHYL"t-PROPYLBENZENE
12SO 3,3,3-TRICHLORO'Z-NETHYLPROPENE
1251 COTININE
1252 CYCLOHEPTANONE
1253 BENZYLAHINE
1251. Z-NETHYL-2,lt-PENTANEOIOL
1255 X»P-CRESOL
1256 1.6-OICHLORO-1.5-CYCLOOCTAOIENE
1257 t96117
i. i.8941.3
30316199
11871.1
1071.551
(.71.9273
1.86566
5021.21
8891,
1071.15
lObi.i.5
Z9i.80i.30
6682719
21693516
2521.9392
95932
RELATIVE SIZE
* vie *ix TZB ric TIX TIT TtcmxtNzc NZC PZC PZX ozc ozx szc szx xic xix
0.9
O.f
1.9
0.9
0.9
0.9
0.9
0.9
0.3
t.7
-0.%
-0.%
o.z
0.7
0.7
0.7
0.7-0.2
0.6
0.6
O.Z
1.2
•0.*
-0.1
0.6
O.Z 0.0
0.6
0.6
0.6
-1.2
O.Z
O.Z
o.z
O.Z
O.Z
* SEE LAST PAGE OF TABLE
(Continued)
-------
TABLE 9. (Continued)
EM II CONCENTRATES PACE Z»
COMBINED CONCENTRATE REPORMPART I.A)
COMMON NAHE
1261 CIS-<.-PHENYL6lCYCLOHEXYL
1262 t-NETHYLENECVCLOHEXANENErHANOL
1261 2.6.6-TRIMETMYL-BICYCL3C3.1.1IHEPTAN-3-0
1261. 3-BUTYL-1.2i-TETRAHETHVL BENZENE
1270 l-ECMYL-1-METMYL INQAN
1271 1-CHLOROTETRAOECANE
1272 1.1-OIPHENYLCVCLOHEIUNE
1271 8ICYCLOC2.2.2IOCTANE-1,%-OIOL. HONOACETA
1271. (.-METHYL BIPHENVL
127$ ARACHIDVL ALCOHOL
1276 2-I4ETHOXV-1-PROPANOL
1277 ISOHYRISTIC ACID
127S ISOPENTADECANOIC ACIO
1279 ABIETIC ACIO
1280 OIOEHYOROGENATEO ABIETIC ACIO
1211 P-PNENYLACETOPHENONE
1262 M-HETHOXYPHcNYL ACETATE
1283 METHYL 3-HYOROX VPHENVLICtTATE
128% X2-HETHYL ANTHRACENE
128$ 2-(PHENYLNETHYLI NAPHTHALENE
1286 PHENYL P-PYRIOYL KEF ONE
1287 7-ETHYLQUINOLINE
1288 D3DCCYL PHENOL
1289 DIMETHYL ETHYL BENZENE
1290 l-PHENYL-2>CYCLOPENrEN-l-OL
1291 0-TOLUALDEHYOE
1292 2.3-BISTRIHETHYLKAPHTHALENE I3.I..5-TR
1301. l-£rHYL-l-NETHYLCYCL3PtNr ANE
1305 X«*2.i.-OIHETHYLPHENOL IXYLENOLI
CAS NO.
214.81.127
1006
5I.760*.
1.6005098
93561
$0639026
26532277<.9<.6
6<< <>366
629969
15191.75
51.3
5«.<.
62<»
625
«.96
102<.
1,2058593
613127
613592
$6771507
766 !<.?<.
27193868
200
$6667106
52920<.
I.9I265I.2
1071267
611151.
626171
1756689
95136
$320<>572
26715266
1.506369
91587
3031061
3676979
37261.7'.
105679
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
RELATIVE SIZE
VIC V1X T2B TIC Til TIT UCtTkltNZC N2C P2C PZ< 02C
-0.%
OZX S2C
• 2
.2
.2
.2
.2
.2
.2
.*
X1C XIX
0.2
0.2
•0.1
-1.
-1.
-1.2
-0.2
-0.2
-0.2
-0.2
-0.2
-0.2
-0.2
-0.2
-0.2
-0.2
I
2
-1.1
-1.1
-O.I
-O.I
-0.1.-0.".
(Continued)
-------
TABLE 9. (Continued)
EPA It CONCENTRATES PAGE 30
COMBINED CONCENTRATE REPORMPART I.AI
COMMON NAME
1306 DIMETHYL ISOPROPVL BENZENE
1307 COUMARONE
1308 1,,6-QIISOPROPYL-M-XXLENE
1309 7-NETHYLBENZOFURAN
1310 TRICHLOROHEPTAFLUOROBUTANE
1311 DIMETHYL ISOPROPYL BENZENE
1312 1.2,3-TRIETHYLBENZEME
1311 XBENZYL CHLORIDE
131V <>-METHYLSTYRENE
1315 2-PHENYLHEXANE
1316 1.0,6-TRiMETHYL TETRALIN
1317 O-ISOPROPYL-ALPNA-NETHYL STYRENE
1311 M-TERPHENYL
1319 OECAHYDRO-liOA-OIHETHVL-7-U-METHYLETHYL
1320 1-CHLORO-O-Cl-CHLOROcTHENYHCYCLOHEXENE
1321 2tO,6-TR:«ETHYLBIPMENYL
1322 0-PHENYLBICYCLOHEXYL
1323 2,0,5,7-TETRAMETHYLPHENAHTHRENE
132". (l.K-BICYCLOPEMTVLI-2-OME
1325 0-TERT-BUTYLPHENOL
1326 P-U-ETMYL-1-METMYLMEXYLI PHENOL (A NONV
1327 P-<2,2.3f3-TETRAN£THVLBUTYLIPHENOL
1321 ETHYL NONADECANOATE
1329 S-OECANONE
1330 ISOPALHITIC ACIO
1331 OIBROMOPHENOL
1332 2-(ii-H£THYL-3-CYCLOHEXENYLIISOPROPANOL
1333 1,2-CYCLOHEXANEOIOL
133V BUTYL. THIAZOLE
1335 2-MYDROXY-5-ISOPROPYL-Z,0.6-CYCLOMEPTATR
1336 ACEULDEHYOE OIETHYL ACETAL
1337 7-MEfHYL-3I2MI-BENZOFURANONE
1338 0-NITROTOLUENE
CAS NO.
105
271196
5186615
1891
219132i>
238011,9
92061
15i.0i.63i,
1I5<>7063
1976350
20273272
7396385
1.861,21,6
88186
52027131
51,932781.
1828101,1,
120291
51,5
5
-------
TABLE 10. COMBINED LISTING OF IDENTIFIED COMPOUNDS
FOUND IN AWT CONCENTRATES
EPA 1C CONCENTRATES PACE 1
COMBINED CONCENTRATE REPORT(PART I.A I
COMMON NANE CAS NO.
i CLOFIBRIC ACIO t 882097
2 OIOCTYL SEBACATE 122623
3 X»*OI-N-8UTYLPHTHALATE 8676Z
6 Z-(2-BUTOXVETHOXYIETHANOL (A OIETHYLE 11Z365
5 OIETHYLENE GLYCOL. 6-METHOXYBUTYL BUTYL 1002
6 OIETHYLENE GLYCOL. Z-HCTHOXVBUTVL BUTYL 1003
7 X
-------
TABLE 10. (Continued)
EPA 18 CONCENTRATES PACE 2
COMBINED CONCENTRATE REPORMPART I.AI
COMMON NAME
<(6 <»>HETHYLHEXANOIC AGIO
1,7 6-NONENOIC AGIO
<•• 0-ETHYL8ENZOIC AGIO
>t<) BETA.BETA-OIHETHYLBENZENEPROPIONIC ACID
BO 2,3-OINETHYLMALEIC ACID
51 1-PHENYL9UTYRIC ACID
52 XHANOELIC ACID
53 O-CHLOROBtNZOIC AGIO
5 XLAURIC ACID
85 i»-(1.6-OIHETHYL-3-OXOHEXVLICVCLOHEXANECA
86 2-ETHYLBUTANAL
87 2-H.ETHYL-3-HEXANOL
88 XPELARGONIC ACID
89 P-T-BUTYLPHENOXY ACETIC ACID
90 8-NONENOIC ACID
CAS NO.
RELATIVE SIZE
VIC X1C L2P L2H L2N L20 C3C C1P C1N C1N CZN R1C R2C EtC OZN B2C BIN BIN
1561111
31502235
2813<>3ia
10101.86
1021121
90642
118912
51446
Z495394
1781. ',07',
I** A (1 ftTf. 1
-------
TABLE 10. (Continued)
EPA It CONCENTRATES PACE 1
COMBINED CONCENTRATE REPORT(PART I.A I
COHMON NAME
91 SUBERIC AGIO
93 X»NAPHTHALENE
93 9.10-OIHYORO-9.9-DINETHYL ACRIOINE
9". IN-BUTVL-ISOauTVlPHTHALATE
95 ACETYL BIPHENYL
96 (.-ETHOXYBUTYL BUTANOATE
97 tHETNVL ETHYL PHTHALATE
98 2-BUTOXYETHYL BUTANOATE
99 XHETMYL PROPYL KETONE
100 2-PHENYLBUTYRIC AGIO
101 XPHENOBARBITAL
102 2,2-OIMETHYL BUTYRIC AGIO
103 l-HETHOXY-2-PROPANOL
10
70553
51.889981.
1<.800169
RELATIVE SIZE
VIC X1C L2P L2N LZN L2D C3C C1P C1H C1M C2N RIG R2C E1C 02N B2C B1H BIN
2.
1.
4.
5.
6.
6.0
5.0
6.0
2.0
4.0 6.0
6.0
6.0
5.0
5.1
4.0 3.0 6.0 3.0
6.0 6.0
3.0 6.0
6.0 6.1
2.0 3.0 6.0
6.0
4.0 5.1 6. 0
5.0
4.0 6.0
2.0 6.0
4.0 2.0
3.0
3.0
5.0 6.0
6.0
6.0
2.0 3.0
2.0
.0
.0
.0
.0
. 0
. 0
A
• u
. 0
.0
.0
3. 0
3.0
6.0
3.0
6.0
5.0
6.0
6.0
3. 0
6.0
6.0
5.0 4.0
2.1 4.1
4.1 4.0
4.1
5.1
6.0
2.0 3.1
3.0
5.0
6.0
6.0
5.0
6.0
4.0
6.0
1.1 1.1
3.0 2.0
3.1 2.1
5.1 9.0
5.0
6.0
3.1
5.1
6.1 3.0 2.0 4.0 5.1
3.0
211 7.0
. u c • •
3.1
5.0
5.1 6.1
5.0
3.1 6.1 6.0 4.1 2.0 2.1
3.1 4.0 1.0
3.1
3.0 4.1
1.0 3.1
4.0 3.0 5.0
1.0
2.1
(Continued)
-------
TABLE 10. (Continued)
EPA 18 CONCENTRATES PAGE
COMBINED CONCENTRATE REPORMPARI I.A I
COMMON NAME
CAS NO.
RELATIVE SIZE
VIC X1C LZP LZH L2N L20 C1C C1P C1M C1N C2N R1C R2C E1C D2N BZC B1M BIN
136
137
138
139
140
142
143
144
145
146
147
150
151
152
153
154
155
156
157
158
159
161
163
164
165
166
167
168
169
170
172
173
174
175
176
177
178
179
180
4-TERPINEOL ISOMER
N.N-OINETHYLHEPTANAMIOE
METHYL ELIAOATE
nETHYLTRIDECYLOCTANOATE
BUTYL METHOXYBUTYRATE
2.4-OICHLOROBENZOIC AGIO
XOLEIC AGIO
3.7-OIMETHYL-6-OCTENOIC ACID
THIS (CMLOROPROPVLIPHOSP HATE
TETRAMYORO-2-METHVI-2-FURANOL
2-HETHYL-2,4-PENTANEOIOL
HEXAN-3-ONE
4-ISOPROPYLACETOPHENONE
6-METHYL-5-HEPTEN-2-ONE
2.5-HEXANEOIOL
TETRAHYDRO-l.l-OIOXIDE TrtlOPHENE
BENZOTHIAZOLE
DIPROPVLENE GLVCOL HETHVL ETHER ll-<2-
AOIPIC ACID. DIHEXYL ESTER
Z+SBUTYL BENZYL PHTHALATE
2>6-BIS(l,l-OIHETHYLETHVLI-4-ETHYLPHENOL
ISOPENTAOE.CANOIC ACID
X»»»2t 4. 6-TRICHLORO PHENOL
XtPVRENE
XTRIBUTYL PHOSPHATE
METHYL PALHITATC
HETHYL STEARATE
2-ETHYL-l-HEXANOL
2>6-OI-T-8UTYL-P-BENZOQUINONE
CARBONIC ACID
fETHVLBENZENE
ZtP-XYLENE
XAZELAIC AGIO
ANTEISOHEPTAOECANOIC ACID
HARGARIC AGIO
4-MtTHYL-2-P£NTANOL
2-HEXANOL
3-METHYLCYCLOPENTANONE
2-HEXANEAHINE
526
1115964
1937628
55193798
1010
50840
112801
2006
995
7326467
107415
589388
645136
110930
2935446
126330
95169
13429077
110338
85687
4130421
544
88062
1Z90GO
126738
112390
112618
104767
719222
100414
106423
123999
457
506127
108112
626937
1757422
5329793
1.9
-2.D
0.0
1.0 2.0
2.0
1.0
-1.0
-1.0
% 0
4.0
4.0
2.0
2.0
1.0
1.0
5.0
5.0
5.1
5.1
2.0
5.0
3.0
4.0*
5.0*
4.0
2.&*Z.O*
5.0*2.0*
S.O*Z.O*
5.0
Z. 0*5.0
t.o*
6.0
6.0 5.0
6.0
6.0
6.0
6.0 4.0 3.0
4.9 6.0 5.0 6.0
3.0 6.0
6.0
6.0
5.4 3.2
5 Z 50 ft.O
4.0 4.0
5.1 Z.O
1.0 5.1 Z.O
4.J S.I
s.o'
4.0 3.0 S.O
S.O 1.0 4.0 Z.O 5.0
4.1
S.O 3.0
1.0*5.0 3.0 Z. 0*4.0 Z.I 4.0 t.O*
3.0 1.0*
4.1*5.0*1.0* 5.0*
S.O* Z.O* Z.O*
0.0* S.O*
1.0* S.O 3.0*2.0* 3.0*4.0 3.Z*3.6
2.0*5.0 4.0 2.0* 3.0* 1.0*2.0*2.0*
0.0* 1.0* • I.I*
0.0* 1.0*
5.0 4.0*5.0 3.0*4.0*3.0*
S.O
Z.O* 1.0* 4.0
1.0*
(Continued)
-------
TABLE 10. (Continued)
EPA !• CONCENTRATES PAKE 9
COMBINED CONCENTRATE REPORTIPART I.A I
COMMON NAME
1*1 2i<>-HEXAOIEN-l-OL
182 5-PnENYL PENTANOIC ACID
113 Itl-OIHETHVU TETRALIN
14
1091.33
7l3518115
131113
527
2017831.1
19*3959
501520
11 653 0
88095
i n ony i*
1U TI9CH
1051.31
112367
20'tVOOO
1 A jt QC 9
10 0 ?9c
10680637
f y 1 » y H
b£ J J r u
108101
1313329>32<.8
123861.
55956213
13877935
lJi.Oi.9
100210
SOi.991,
1733V553
X1C L
5.0
I.
5
5
5
3
5
5
5
5
3
5
5
5
5
5
5
5
5
5
2P
.0
.0
.0
.0
.2
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
L
5
3
S
<>
%
3
S
9
1
5
I.
3
2
•>
5
3
3
S
2
RELATIVE SIZE
2H L2N L20 C3C CIP C1N C1N C2N R1C R2C E1C
.0
1.0 3.0
1.0
2.0 2. « 3.0 5.0 1.0
2.0
1.0 3.0
2.0 1.0 5.0
3.0
t.O 1.0 t.O *.0 Z.I
5.0
1.0
1.1
.0 3.0 5.0
01& A
*»• 0
.0 <*.0 $.0
.0 5.0 t.O
.0 3.1
.0 t.O 3.0
.0 1.0 1.0 5.0 t.l 2.0
.0
.0 5.0
.0 5.0 «.0
.0 5.0
Of B L • 9 9
£• i %••£•£
.0 5.0
.0
.0 5.0
.0 5.0 3.0 2.1
.0
.0 5.
5.
2. S.O
3. 5.0
5.
5.
02N B2C BIN BIN
«..0 4.1
1.0
2.0
2.0
IA t. g ?»•
• H %• V C • V
2.0 1.0
S.7
3D t. • 1 B
• U <*• • w • V
3.4
1.0
2.0
1.0
(Continued)
-------
TABLE 10. (Continued)
EPA I« CONCENTRATES PAGE 6
COMBINED CONCENTRATE REPORT (PART I.Al
COMMON NAME
CAS NO.
RELATIVE SIZE
226
227
228
229
230
231
232
233
231
235
236
237
238
239
210
211
242
213
211
215
216
217
218
219
250
251
252
253
251
255
256
257
258
259
261
262
263
261
265
266
267
268
2b9
271
2f6-NAPHTHALIC ACIO
5-EPIDEOXYPOOOCARPIC ACID
CLOVE NE
IM-CHLOROPHENOL
«ISOPHORONE
XN-NITROSO-3-HETHVL PIPERIOINE
NONYLPHENOL
XMESITYL OXIDE (3-ISOHEXEN-2-ONE!
P-(2,2.3.3-TETHANETHYLBUTYLIPHENOL
2-ETHVLVALERIC ACIO
2-HETHYLGLUTARIC ACIO
5-METHYL HEXANOIC ACIO
2.6-OIHETHYL8ENZ.OIC ACIO
2,3,6-TRIHETHYL BENZOIC ACIO
XDICAMBA
1-NAPHTHOIC ACIO
3-13,1-OIMETHOXVPHENYLI-Z-PROPENOIC ACIO
2-METHYLCAPROIC ACIO
BETA.BETA-DIMETHYLPHENYLACETIC ACIO
ALPHA-METMYLENE BENZENE PROPANOIC ACIO
12,5-OIMETHYLBENZENEI BUTANOIC ACIO
PHTHALIOE
2,2 »1 tl-TETRA METHYL PENTANOIC ACIO
3-METHOXV-l,2-BENZISOTHIAZOLE
•TRICRESYL PHOSPHATE IISOHER UNKNOWN)
OECYLENE
1-UNOECENE
ALPHA -OOOECYLENE
XCVCLOHEXENE
2.3.6-TRIMETHVLNAPHTHALENE
1, 3, 6-TRI METHYL NAPHTHALENE
P-ISOPROPVLOIPHCNVL AHINE
9,10-OIHVOROPHENANTHRENE
2.2,S.7-TETRAMETHVL-1,5-OCTAD!ENE-3-ONE
HETHYL N-AMVL KETONE
2-METHOXY-1-METHYL-Z-PENTENOIC ACIO
XN-UNOECYLIC ACIO
TRANS -9-HEXAOECENOIC ACID
1.2-BENZISOTHIAZOL-3I2HI-ONE
1.3-DIMETHVL BUTABARBITAL
l-PHENYL-1.2. 3-PROPANETRIOL
X6ENZVL ALCOHOL
1-HEPTAOECANOL
X»2,1-OICHLOROPHENOXYACETIC ACIO, (2.4-D)
1111381
57315309
169921
108130
78591
13603071
25151523
111797
51932781
2005
617629
628466
632462
2529361
1918009
66555
2316369
4536236
826551
5078
1453061
87412
1 1 n 9i 91
i iu£l£ J
40991386
1330785
872059
821954
112414
110838
829265
3031081
5650102
776352
19377970
110430
1009
112378
373499
2634335
77281
16354953
100516
1454859
94757
VIC XIK L2f> L2N LZN LZO
5.0
5.0
5.1
4.0
5.0
5.0
5.0
5.0
3.0
S.O
S.O
S.O
5.0
S.O
5.0
5.0
5.0
5.0
5.0
5.0
4.0
4.0
C3C C1P C1N C1N C2N
Z.O 4.0
5.0
5.0
4.0
2.0
4.0 S.O
4.0 S.O
4.0 5.0
2.0
5.0
5.
5.
5.
5. 1.0 1.0
S. Z.O t.O
5.
S.O
S.O
4.0
S.O 4.0
3.0
4.0 S.O
S.O
5.0
S.O
2.0
S.O
S.O
R1C RZC E1C OZN BZC BIN BID
4.0
Z.O Z.O
Z.I 4.0 Z.O
2.1
4.0
4.1 4.0 1.8 3.0 S.t
Z.O Z.O
1.1 S.I
1.0
Z.O
2.2 5.0
3.0 4.1
5.1 4.0 3.0
3.0
4.1 5.1 3.Z 3.3 4.3 Z.Z.
t.O
1.0 2.0
(Continued)
-------
TABLE 10. (Continued)
COMBINED CONCENTRATE REPORT(PART I.»l
EPA 14 CONCENTRATES PACE T
COMMON NAME
CAS NO.
RELATIVE SIZE
VIC X1C L2P L2N L2N L20 C3C C1P C1N C1N C2N R1C R2C E1C 02N B2C 81H BIN
271
272
273
270
276
277
279
280
281
282
283
280
285
286
287
288
289
290
291
292
293
290
295
296
297
298
299
300
301
302
303
300
305
306
307
•I fin
3 It 9
309
310
311
312
313
310
315
XBICHLORACETIC ACIO
2-(2-METMOXYPROPOXY)-l-PROPANOL IA DIPR
3-METHYL-2-HEPTANOL
2-(2-HYOROXYPftOPOXYI-l-PROPANOL (A OIPRO
XMETHYL CHLOROFORM
2.2-OINETHYL-l-BUTANOL
2-TERT-BUTYLCYCLOHEXANOL
CHRYSANTHEMIC ACIO
2-ETHYL-3-METHYLFUHARIC ACIO
ETHENYL CYCLOPENTANEACETATE
XARA:HIOONIC ACIO
ANTEISOPcNTADECANOIC ACID
TRIPROPYLENE GLVCOLt METHYL ETHER
XP-METHOXY-T-BUTYL PHENOL
3-BUTYL-6-HETHYL-2.0-PVRIOINEOIOL
2-HVOROXY DECANOIC ACID
1-1 I2,6.6-TRIHETHYL*1-CVCLOHEXEN-1-YLIOX
TETRAETHYLENE GLYCOL HONOBUTYL ETHER
8,11-OCTAOECAOIENOIC ACID
LIGNOCERIC ACIO
1,2 OiS-OI-O-ISOPROPVLIOENE-ALPHA-D-FRUC
HYRISTYL ALCOHOL
3-METHOXY-2-BUTANOL
CYCLOHEXYL FORMATC
XMCTA-CRESOL
1.5-BIS(T-auTYLI-3,3-OIHETHYL BICYCLOC3.
OIOCTYL AZELATE
OCTADECATRIENOIC ACIO
ACENAPHTHYLENE
PIPERIDINOL
XMETMYLPHENYL CAR8INOL
1-CYCLOP£NTYLETHANONE
7-OCTEN-2-ONE
Xf 1. 2-0 1C HLOROE THANE
0-HVOROXY-O-METHVLCYCLOHEXANONE
XCVCLOHEXANOL
1.2 5.6-BIS-O-ISOPROPYLIOENE-BETA-O-TALO
BUTYL CLOFIBRATC
2-BUTYL THF
XCAFFEINE
XDnF (OIHETHYLFORHAMIDE)
PHT-4ALIC ANHYDRIDE
79036
13588288
31367061
106627
71556
1185337
2916O5 — — — • — ~
13091797
10053891
28098808
OS955666
506309
5502903
10213771
25013165
6967700
539381 7
250
218
2197526
557595
20880937
112721
53778720
035151,6
108390
1977968
103202
0906916
208968
6859990
988S1
6000600
3660606
107062 0.6
17029026
i n in 1*1* *i n >
1 U D HH y V * C
108910 0.2 2.0*
23262795 0.2
1713100 0.2
1000291
58082 0.0 0.0 0. 1
68122 2.0
85009 3.0
S.O 5.0
1.0 S.O 3.0
S.O 3.0
5.0 2.0
5.0
S.O
5.0 .
S.O
S.O
S.O 3.0
3.) 5.0
3.1 5.0 3.0
5.1 3.0
S.O
5.0
5
5
5 5.0
5
5
5.0
S.
1. 5.0
2. 5.0
S.
5.
5.0
5.0
5.0
5.0
0.0
0.6
0.0* 2.1* 0.0
0.2 2.0
3.0 3.1
0. 1 2.0 3.2 2.0
0.1 1.0
3.0
S.O
3.0
S.O
2.0
S.O
S.O
0.6
•3.0 •
(Continued)
-------
TABLE 10. (Continued)
EPA 18 CONCENTRATES PACE •
COMBINED CONCENTRATE REPORT(PART I.A)
COMMON NAME
CAS NO.
RELATIVE SIZE
VIC X1C L2P L2H L2N L20 C3C C1P C1H C1N C2N R1C R2C E1C 02N B2C BIN BIN
316
317
318
319
320
321
322
323
320
325
326
327
328
329
330
331
332
333
335
336
t IT
JJf
334
339
300
301
302
303
300
305
11.C.
JHO
307
308
309
350
351
352
353
350
355
356
357
358
359
360
N-ACETYLCYCLOHEXYLAHINE
0.0-DIMETHYLOIHYOROFURANONE
2-METHOXY-l-PROPANOL
1SOMYRISTIC ACID
9-KETOCAPRIC ACID
ISOPALMITIC ACID
X*»SFLUORANTHENE
3.0-EPOXY-2-HEXANONE
XSTOLUENE
OIACETONE ALCOHOL
XCETYL ALCOHOL
METHYL AMYL CARBINOL
0-HEPTANONE
(1,0-CYCLOHEXAOIEN-l-VLI BENZENE
0-HETHYL OIOXANE
2-ACETYL-O-HETHYL-O-PENTENOIC ACID
XIBUTYLCBUTOXY CAR80NYL) METHYL PHTHALATE
0-ETHYL TOLUENE
X*ISTVRENE
(1.1-OIHETHYLBUTVLI BENZENE
6-METHYL TETRALIN
PSEOOOCUMENE
2-ETHYL-1.3-DIHETHYL BENZENE
1-METHVL INOAN
X2- METHYL NAPHTHALENE
1-ETHYL-3.5-OINETHYL BENZENE
2-BUTYLNAPHTHALENE
P-OIISOPROPVL BENZENE
C5 BENZENE
2-METHYL TETRALIN
XBIPHENVL
DIMETHYL NAPHTHALENE
XO-CRESOL
1-METHYLPYRENE
TERPHENYL
2.3,5-TRINETHYL PHENANTHRENE
1-HETHYL ANTHRACENE
2-OCTYLPHENOL
EXO-90RNEOL
XENOD-BORNtOL
XCAHPHOR
FENCHYL ALCOHOL
DI-T-BUTYL ETHER
CIS-1.2-CIS-2.3-PLINOL
2-I2-ISOPROPYLPHENVLI-1-PROPANOL
1120530
13861977
1589075
503
1022260
505
206000
17257817
108883
123022
36653820
503097
123193
13703521
1120970
1005
85701
611103
1 0 0*»25
1985575
1680519
2870000
767588
91576
930707
1130629
100185
120
3877198
Q 9K9 It
Tf £y£ **
300
95087
2381217
26100603
3670735
610080
909133
120765
507700
76222
1632731
6163662
11039728
58003826
O.I
0.1 1.0
0.0 O.I* Z.O*
0.0 •••«*
-1.0 3.0*0.0 2.0*0.0 3.0*
-1.0 O.O
-2.0 1.0* 0.0 1.0* 2.0* 1.0*
2.0 0.0* 3.0*
3.0 0.0*1.0* 0.0* 0.0*
3.0 2.0* 3.0* O.J* Z.O*
2.0 *.0*
0.0 2.0* 0.0*3.0*
0.0 3.0* 3.0* Z.O*
0.0
0.0
3.0 0.0
0.0 ».0
0.0 2.0 3.0 2.0 Z.O
k.O 1.0
o.o
o.o
0.0 1.0 3.0
1.0 1.0 0.0 1.0
0.0
0.0
o.o
3.0 1.0 1.0 0.0 Z.O
2.0 2.0 2.0 0.0
0.0
0.0
0.0
2.0 0.0
0.0 2.0 0.0
2.0 0.0
0.0 3.0
0.0
0.0
0.0
0.0
0.0
(Continued)
-------
TABLE 10. (Continued)
EPA 10 CONCENTRATES PACE 9
COMBINED CONCENTRATE REPORMPART I.AI
COMMON NAME
CAS NO.
RELATIVE SIZE
VIC X1C L2P L2H L2N L20 C3C C1P C1N C1N C2N R1C R2C E1C 02N B2C BIN BIN
361
362
363
361.
365
366
367
366
369
370
371
* 7 9
ore
373
375
376
377
376
379
360
362
383
3o<.
385
366
386
369
390
391
392
393
390
395
396
397
398
399
1.00
001
1,02
<>03
004
1.05
CIS-2-NETHYLCVCLOPENTANOL
TRIOCTYL PHOSPHATE
HETHYL HENEICOSANOATE
HiTMYLDEHYDROABIEUTE
BENZOFURANONE
HETHYL OCTENOATE
3-OCTENOIC ACIO
tOIHETHYL TEREPHTHALATE
2-CYCLOHEXENONE
2,5-HtXANEOIONE
OIETHYLENE GUY COL, HONONETHVL ETHER 1C
3C CwTOTMfTMVI PVPl rtUCV • V •Fkl« 4 • ftH T
• .>• 9 • i Nine I n TLU TULUniii^j "tn™ l~Unt
OICVCLOHEXVtAOIPATE
P» 1 1 • 1 I vTf TO A ttf Tw VI BUT VI IQUFkm
•tltlt-JtJ'ltl KAHL 1 flTLDUl TL IK fit HUL
CHLOR09ENZOIC ACID ISOMER
ALPHA -CAR YOPHYLLENE
ISO-HEXANOIC ACIO
<>,5-OIMETHYL-l-HEXENE
2,3-OlNETHYLBUTVRIC ACIO
X»ANTHRACENE
l-SEC-BUTOXY-2-METHOXYPROPANE
3-HETHVL-2-CYCLOHEXEN-1-ONE
<.,"., 5-TRIMETHYL-2-CYCLOHEXEN-1-ONE
VINYL CYCLOHEXVLF04NATE
P-(l-ETHYL-l-METHYLHEXYL) PHENOL (A NONV
ftTMFTMVi Clll EflilF
ui nc. i ni L juir unt
2-l2-HETHOXY-l-H£THYLETHOXY)-2-PROPANOL
XBUTYRIC ACIO
<..<.-OIMETHYL-2-PENTENOIC ACIO
4-OCTENOIC ACIO
N-BENZOVLGLVCINt IHIPPURIC ACIDI
V,6,6-TRIMETHYLTETRAHYORO-2-PYRANONE
S-aUTYLOIHVORO-2-FJRANON-
TRIETHYLENE GLYCOL. DIMETHYL ETHER
STERT-BUTVL HETHYL PHTHALATE
OIMETHYLNAPHTHALENE
1.5,6-TRIMETHYL TETRALIN
X2*HVOROXYBIPHENYL
3-OCTANUNE
1-OCTENE
1-NONYLENE
SEB4CIC ACIO
1-TRIOECENE
1-TETRAOECENE
25H.I.052
160651,6
6061,900
123571.1
716931,6
700
1577191
120616
930667
110131.
111900
1,7101 2
61.9990
140669
706
6753966
6
-------
TABLE 10. (Continued)
EPA II CONCENTRATES PAGE 1C
COMBINED CONCENTRATE REPORT(PART I.A I
COMMON NAME
CAS NO.
RELATIVE SIZE
VIS XIC L2P L2H L2N L20 C3C C1P CIM C1N CZN R1C RZC E1C OZN BZC BIN BIN
406
407
408
409
410
411
412
413
414
415
416
417
418
420
421
422 *
423
424
425
426
427
428
429
430
431
432
433
434
435
436
437
438
440
441
442
443
44*
445
446
447
448
449
450
1-PtNTADECENE
CETENE
2-NETHYL-2-PROPYLHEXANOIC ACIO
2. 6-0 IISOPROPYL PHENOL
X3,4-OICHLOROANILIN£
1, 3. a-TRlMETHYL NAPHTHALENE
l,2,3-TRIMETHYL-4-P*OPENYLNAPHTHALENE IT
1,4,6-TRlMETHYL NAPHTHALENE
BUTYLATEO HYOROXY ANISOLE IBHAI
1,4.6-TRIHETHYL TETKALIN
N-P*OPYLSUCCI NAMIOE
METHYL PALMITCLEATE
XISOBUTYRIC ACID
2-METHOXV-3-NETHYL-2-PENTENOIC ACIO
CIS-2,5-OIHETHYLTETRAHYDROFURAN
N-METHYLETHOSUXIHIDE
*+S2,4-OICHLOROPHENOL
4-TERT-BUTYL-0-PHtNYL£NE CYCLIC CARBONAT
BUTABARBITAL
ANISOLE-2-ACETIC ACIO
BETA,3,4-TRINETHYLBENZENEPROPANOIC ACID
2-IPHENYLHETHYLIBENZOIC ACIO
2,2-OIMETHYLGLUTARIC ACID
XP-TERT-BUTYL PHENOL
1.3-OIHETHOXY-2-PROPANOL
1,3-PROPYLENE GLYCOL, BUTYL METHYL DIETH
XCHLOROBENZENE
3-METHOXY-2-NETHYL-2-PENTENOIC ACIO
ALPHA.ALPHA-OICHLOROPHENYLACETIC ACIO
l-(2-BUTOXY-l-METHYLETHOXY)-2-PROPANOL 1
6-NETHYL-TETRAHYORO-2-PYRANONE
HEXAHYORO-4-HETHYL-2H-AZEPIN-2-ONE
6-METHYL-3I2HI-BENZOFURANONE
l-METHOXY-2-HEXENE
OI-N-HEXYL ETHER
ACETOACETIC ACIO
l-METHOXY-2-BUTANOL
2.3-OIMETHYL- 3-PENTANOL
2,6-OIMETHYLPHENOXV CARBONIC ACIO
2-METHYLCfCLOPENTANOL {GEOMETRY UNKNOHNI
X6-HYOROXYCAPROIC ACIO LACTONE
2-»HYOSOXYMETHYL)BENZOIC ACID
TRIOECYLIC ACIO
UNOECANEOIOIC ACIO
13360617
629732
31080372
2078548
95761
17057919
26137531
Z131422
15359996
2Z824324
3470971
1120250
79312
1008
2144414
13861999
120832
54815213
125406
93254
1011
612351
681572
98544
623698
1012
100907
1014
61031729
29911282
823223
3623050
20895414
56052836
112583
541504
53778737
595*,15
1013
24070777
502443
612204
638539
1852046
4.0
4.0 2.0
3.0 4.0
4.0
4.0
4.0
4.0 2.0 1.0
4.0 3.0
4.0
4.0
4.0
4.0
4.0 4.0
4.0 3.0 *•• 3.0
4.0
4.0
4.0 1.0 l.fl
4.0
4.0
4.0
4.0
t.O
4.0 4.0
4.0
4.0
4.0
4.0 0.0
4.0
4. iei
4.
4.
4.
4. 3.0
4.
4.
4.0
4.0
4.0
4.0
4.0 3.0
4.0
4.0 2.0
3.1 4.0 2.0
4.1 4.0 4.0 3.0
(Continued)
-------
TABLE 10. (Continued)
EPA II CONCENTRATES PAGE 11
COMBINED CQNCEMTRATE REPORT(PART I.A I
COHNON NAME
d51 d-BUTOXVBUTYRIC AGIO
d52 3-HEPTANOL
d53 2,3-DIhtTHYLTETRAMYDRO-2-FURANOL
d5d 6-BROMO-2-HEXANONE
d55 XiaiMETHYL NITROSO UREA
d56 3, "t-OIHTOROXr-6-METHOXY-1-NAPHTHA LE NONE
d57 BUTYLBENZYLPHTHALATE
458 XBENZYL CYANIDE
dS9 PIPERIOINONE
1,60 1-ETHOXY OECALIN
d61 d-OXO-NONANOIC AGIO
d62 VACCENIC AGIO
d63 NONAOECANOIC ACID
d6d BEHENIC AGIO
d65 1.3.6-TRIOXOCANE
d66 Z-ETHYL-1.3-HEXANEOIOL
d67 2-ETHYL-5-HETHYLOIOXANE
d68 X PVRIQINE
d69 ETHYL PALMITATE
1,70 d-HEXEN-2-ONE
d71 5-METHYL-2-HEXANOL
d72 3-HYOROXY-1.2-BENZISOTHIAZOLE
d73 2,6-OICHLOROBENZOIC AGIO
474 0-PROPIONYL BENZOIC AGIO
1.75 2-METHYL-4-OIflRONON£THVL BENZOIC AGIO
476 3-HYOROXYTETRADECANOIC AGIO
1.77 XANTHRANILIC AGIO
478 2-AHINO-5-CHLOROBENZOIC AGIO
d79 4-HYOROXY-4-M£THYL-2-PENrANON£
480 2.2.3-TRIMETHYL-3-CYCLOPEKTENE-1-ACETALO
4«1 2,3-BUTANEDIOL
442 0-AN1SIC AGIO
483 3-METHOXYBENZOIC AGIO
484 TERPIN
4«5 DICVCLOHEXYL SEBACATE
486 XCINNAMALOEHYOE
487 XN-METHYL-2-PYROLIOONE
448 MKftt'IN SEE NO. 484
489 BUTYLBEN/OATE
490 OIOEHVOROGENATEO ABIETIC ACID
491 3-NETHYLPENTAN-3-OL
492 P-I1-HYOROXY-1-H£TMYLETMYL(ACCTOPMENONE
493 METHYL HYRISTATE
49-. 1,2-BENZISOTHIAZOLE
495 N-PROPYL-1-MEXANAHINE
CAS NO.
RELATIVE SIZE
55724737
589822
61142776
10226296
3475636
1078199
38*11120
140294
51953107
6064524
693721
646300
25378261
1779197
94962
53907918
110861
628977
25659227
627598
50793
4219550
129
1961724
118923
89543
123442
4501580
513839
579759
586389
80535
366
104552
872504
136607
625
77747
54549723
124107
272162
VIC X1C L2P L2M L2N L20 C3C ClP Clli C1N C2N RIG R2C E1C
3.
3.
3.
3. 3.0
die
d.O 3.0
d.O
d.O
d!o
4.0
d.O
d.O
d.O
d.O
d.O
d!o
3.6
1.0
3.0 3.1 3.0
0.0
0.0 1.0* 2.0*
0.0 3.0*
1.0 3.0* 3.0* 2.0*
t.l 3.0*
02N B2C BIN BIN
d.O
d.O 2.0
4.0
d.O
1.0
2.0
3.0
d.
d.
d.
d.O
d.O
d.O 2.0
d.O
d.
d.
d.
3.2 d.
d.
2.0 3.2
2.0
1.0*3.0* 3.0*
20193231 -1.0
3.0*
(Continued)
-------
TABLE 10. (Continued)
EPA II CONCENTRATES PAGE 1Z
COMBINED CONCENTRATE REPORT(PART I.A I
COMMON NAME
CAS NO.
RELATIVE SIZE
VIC X1C L2P L2M LZN LZO C3C CIP CtN CtN CZN R1C RZC E1C OZN BZC BIN BIN
tto
497
498
499
500
501
502
503
504
505
506
507
soa
509
510
511
512
513
51*
515
516
517
518
519
520
521
522
523
521.
525
526
527
524
529
530
531
532
533
534
535
536
537
538
539
540
3-PENTEN-2-OL
2-METHYLCYCLOPENTANONE
11 -METHYL BUTYLIOXIRANE
OCTAOECANOL
8-NONENE-2-ONE
XCHLOROBRO HOME THANE
2(4t6-TRIMETHYLUNDECANOIC ACID
10-UNDECEHOIC ACID
3-METHYLCYCLOHEXENE
X3-CHLORO-2-METMYL PROPENE
li2-OICHLOROPENTANE
1-CHLOROHEPTANE
ACETALOEHYOE OIETHVL ACETAL
3-PHENYL-3-NETHVLHEXANE
XSH-XYLENE
4-PHENYLCYCLOHEXENE
1.2.3-TRIMETHYL BENZENE
XMESITYLENc
l-METHYL-2-PROPYL BENZENE
4-METHYL INOAN
Xl-METHYLNAPHTHALENE
X2-ETHYL NAPHTHALENE
Xl,t-DIMETHYLNAPHTHALENE
1.6,7-TRIMETHYLNAPHTHALENE
l-eiHYL-2i4-DlMETnYL BENZENE
1-EIHYL-2.3-OIMETHYL BENZENE
XSCUMENE
1-METHYL-d-PROPYLBENZENE
N-BUTYL8ENZENE
2-PHENYLPENTANE
C5 BENZENE
X*tO-OICHLORO BENZENE
DIMETHYL INOAN
DIMETHYL ISOPROPYL BENZENE
. ETHYL TRIMETHYL BENZENE
%.7-OIMETHYL INDAN
DIMETHYL INOAN
2, /-DIMETHYL TETRALIN
1-PHENYL NONANE
X2.6-DIMCTHYLNAPHTHALENE
1.6-OIMETHYLNAPHTHALENE
1-PHENYL UNOECANE
OIISOPROPYL PHENOL
TRIMETMYLNAPHTHALENE
1569502
1120725
53229393
26762<<
-------
TABLE 10. (Continued)
EPA II CONCENTRATES PAGE II
COMBINED CONCENTRATE REPORTIPART I.A)
Ln
Sol
51,2
51.3
SHO
5<.S
5-.6
Si.7
5*8
51,9
550
551
55Z
SS3
SSi.
SSS
SSb
557
SSS
559
560
561
562
563
56*
56S
566
567
568
569
570
571
572
673
57",
575
576
577
578
579
580
581
5«2
563
58<.
585
COMMON NAME
CAS NO.
RELATIVE SIZE
VIC XIC L2P LZM LZN LZO C3C C1P C1N C1N CZN R1C RZC E1C OZM BZC BIN BIN
TRINETHYLNAPHTHALENE
TRIHETHYLNAPHTHALENE
DIMETHYL BIPHENVL
< 1. 1 -DIMETHYL PR OPYLI BENZENE
1-ETHVL-3-HETHYL BENZENE
2-ISOPROPYLNAPHTHALENE
XRETINE
2-IPHENYLHETMYLI NAPHTHALENE
DUAENE
DIMETHYL ETHYL BENZENE
DIMETHYL ETHYL BENZENE
XCINEOLE
XMETHYL BENZOATE
S-PICOLINE
N.N-OIETHYL FORHAMIDE
FENCHONE
Z-£tHOXY£THYL-Z-BUTOXYETM»L ETHER
XTRICHLOROPROPANE
v AT f T nPufuntjf
(Abe. i ufntnunc
DIHVORO FARNESOL
XNICOTINE
2-NETHYL VALERIC ACIO
ISOPROPYL BENZOATE
3-NETHYL-I.-PHENYLBUTYRIC ACIO
1.6 DIMETHYL-".- ISOPROPYL- NAPHTHALENE
XTRIETHYL PHOSPHATE
XCYCLOHEXANONE
VINYL ACETATE
HENTHONE
COTININE
ANISIC ACIO
XGLUTARIC ACIO
AMINOPHTHALAZINE
J-METHYLGLUTARIC ACIO
XOALAPON
T— frifr M¥lTOTfii'flAtl> —
1 • ' r *tttw TLffKlULU**HC.' . ...—
1.1.3-TRIMETHYL-3-PHENYL INOAN
TAICOSANE
TrT-r'f.O'^AHF
IctTnOUliAriL ...—--.
P" |J T A Pflt- ' t tiC
tnt*IUV3*lnc •• "
TCTRAHYOROLINALOOL
METHYL HEPTADECANOATE (METHYL HtR&ARAT
5, 5- DIM ETHYL- 2- FUR* NONE
31 Z
313
600
ZO
ZOZ7170
1.83658
613592
95932
ZOO
Z01
".70826
93S83
108996
61784,5
1195795
3*95178
96181.
Q A Aft 9
yoooc
1 33 51.8 «.
51.115
97610
939<.«0
7315686
1.83783
781,00
10891.1
10805-.
101.5811,7
1,86566
100091.
11091,1
19061,698
626S17
75990
i •?? f.c t \
ILL JW •!
3910358
638675
f ± f < \ a
O^O 311
rf.PQQQP'
« t Tf-J f.
78b93
1731926
2001961,1
3
3
3
3
1
3
3
3
1
Z
1
3
2
3
1
3
3
3
3
3
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
3.0
2.0
3.0
3.0
2.0
2.0
1.0
3.0
3.0
1.0
Z
Z
3
3
Z
]
3
3
3
3
3
J
3
3
J.
J.
3
3
2
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z.o
2.0 3.0 1.0
3.0
.0
1.0 3.0 l.t 1.0
3.0
3.0
3.0
.0
3.0
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3.0 1.0
.0 0.0 1.0 Z.O Z.O 1.0
3.0
1.0 3.0 2.0
3.0
.0 1.0 2.0 2.0
.0
.0
.0
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.0
a
TH • — —
Q
.0 1.0
.0
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(Continued)
-------
TABLE 10. (Continued)
EM 18 CONCENTRATES PACE It
COMBINED CONCENTRATE REPORTIPART I.A I
COMMON NAME
CAS NO.
RELATIVE SIZE
VIC XtC L2P LZN LZN L20 C3C CtP CIH C1N CZN R1C R2C E1C OZN BZC B1M BIN
586
587
568
689
590
591
592
593
594
595
596
597
594
599
600
bOl
602
603
60<>
605
606
607
608
609
610
611
612
613
614
615
616
617
616
619
620
621
622
623
£.?lt
DcH
625
£ yf
oco
627
628
629
630
3,5-OIHETHYL-2-CVCLOHEXEN-l-ONE
1-INOANONE
JSONONTL PHENOL IISONER UNKNOWN)
P-lt-HETHYLOCTVLIPHENOL (A NONYL PHENOL
TRIETHVLENE GLYCOL METHYL ETHER
X*»2,4-OIMETHYLPHENOL (XVLENOL)
2-HEXENOIC ACID
OIETHYL KETONE
METHYL ISOPENTYL KETONE
l-il-CYCLOHEXEN-l-LYI-2-PROPANONE
2-BUTVL-3-HETHYLOXIRANE
3,5,S-TRIMETHYL-2-CYCLOPENTEN-l-ONE
5-ETHVLOIHYORO-2I3HI-FURANONE
6-HETHYL-3-ISOPROPYL-2-CYCLOHEXEN-1-ONE
5-PMENYL-2-PENTANONE
OCTYL PHENOL
5-CPENTYLOXYI -2-PENTENE
. ALPHA. -HYOROXV-. ALPHA. -METHYL BENZENE A
l-PHENYL-2-BUTANONE
2-BUTYLOCTANOL
5-HETHYL-l 1 3H I-ISOBENZOFURANONE
ISOVALEftAMIOE
HEXAHVDRO-2H-AZEPINE-2-ONE
P-CHORO-2-NITROANILINE
ETHYL PHENOXYBENZENE
XHALONIC ACID
<.-HETHYLPHENYLPENTANOIC ACID
SISOBUTYL METHYL PHTHALATE
«SEC-BUTYL METHYL PHTHALATE
2-ETHYL-l.it-OlMETHVL BENZENE
X+IH-OICHLOROBENZENE
METHYL HETHOXYMETHYL FORMAL
%2,6-LUTIDINE
7.M-CHLOROANILINE
XS2i3(ki6-TETRACHLOROPHENOL
Xf 2 i15695<»
695067
49971(1
2235636
500
56052856
515300
1007325
3913026
54120646
541466
10560Z
69634
634140
141622
59094712
1004
1006
1756869
541731
626900
106465
106429
58902
96954
585342
109864
111697
6765395
112809
107880
4799626
3.0 3.0
3.0
3.0
3.0
3.0
1.0
3.0
3.0
3.0
3.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
1.0
1.0
3.0
3.0
3.0
3.0 1.0
3. a
1.0 1»0 2.0 2«t
3.1
3.0
3.0
3.0
3.0
3.0
1.0 3.0
1.0 3.0
3.0
2.0 3.9 2.0 1.0
3.0 3.0
3.0
3.0
3.0
3.0 Z.fl 3.0
3.0
3.0
3.0 2.0
3.0
3.0
(Continued)
-------
TABLE 10. (Continued)
COMBINED CONCENTRATE REPORT(PART I.AI
EpA II CONCENTRATES PAGE 15
COMMON NAME
CAS NO.
RELATIVE SIZE
VIC X1C L2P 12N LZN LZO C3C CtP C1H C1N C2N R1C RZC E1C D2N BZC BIN BIN
631
632
633
63i«
635
636
637
638
639
61,0
61,1
6<>3
61,1.
6i>5
61,6
6*7
61.8
6«.9
650
651
652
653
651.
655
656
657
658
659
660
661
662
1 1 »
DO J
665
666
667
668
669
670
671
672
673
671.
675
METH Y L-N- PROP YL BENZENE
METHYL-N-PROPVLBCNZENE
2.7-OINETHYLNAPMTHALENE
1,2.8-TRIMETHYLNAPHTHALtNE l3,i»,S-TR
OIMETHYLNAPHTHALENE
1.3-OIMETHYNAPHTHALENE
OCTENAL (ISOMER UNKNOWN)
0-CYCLOHEXYLPHENOL
XBORNVL ACETATE
X2,6>OIMETHYLQUINOLINE
SEC-BUTYLISOPROPYL ETNER
2.6-OIMETHYLHEPTANOIC ACIO
2-METHOXY-3-METHYLCROTONIC ACIO
3,6-OIHETHVLOCTANOIC ACID IAN ISOOECANOI
LEVULINIC ACIO
X2.2.2-TRICHLOROETHANOL
9-OOOECENOIC ACIO
2.3.3-TRIMETHVL-3M-INOOLE
SO-CHLOROPHENOL
XTETRAMETMYLUREA, TNU
2.2.5,5-TETRAHETMYL THF
1,-KETOISOHEPTANOIC ACIO
ALPHA-NETHYL-ALPHA-ACETVLOXYBENZENEACETI
2,5,6-TRIMETHYL-l-NAPHlMOL
2,5-OIMETMYL STYRENE
1-I3-BUTOXYPROPOXYI-2-PR3PANOL (A OIPROP
ALPHA-PICOLINC
X2-ACCTYLFURAN
3-METHYL PHTHALIOE
7-HETHYL-3I2HI-BENZOFURANONE
BUTYL M-TOLYL SULFIOE
TCTRAHYOROPYRAN-2-METHANOL
2.2-OICHLORO-3-METMYLBUTANE
1,6-HEXANEOIOL
2-NORBORNENE-7-OL
2-HEXENAL
2.6-OIMETHYL-2-MEPTEN-1.-ONE
2.2-OINETHYL-3-PENTANOL
.0 1.0
2.0
1.0 2.0
!.0
1.0
'. 0
.0
.0
.0
.0
.0
.0
.0
.0 3.0
.0
.0 3.0
.0
.0
.0
.0
.0
.0
1.0
0
0
0
0
0
0
1.1
Z.I
2.0
Z.I
Z.I
Z.I
3.1
(Continued)
-------
TABLE 10. (Continued)
EPA It CONCENTRATES PACE 16
00
COMBINED CONCENTRATE REPORT(PART I.A»
COMMON NAME
676 1-ACETYL-1.2.3.1.-TETRANYOROPYRIOINE
677 OIETHYLENEGLYCOL, CYCLDHtXYL ETHER
678 JOl-N-PROPYL PHTHALATE
679 7-NONENOIC ACID
680 ISOINOOLE-lt3-DIONE
641 2-ETHYL-3-METHYL-2-BUTENEOIOIC ACID
682 TRICOSANOIC ACID
683 NONACHLOR
68". 1-HETHYLBUTYLALCOHOL
605 XN-OCTANOL
686 X2-PHENYLISOPROPANOL
687 Xl,2-OIMYDRO-3.6-PYRIOAZINEOIONE
608 5,6,7,7A-T£TRAHYORO-iitt,7A-TRIH£THirL-2(l>
689 3-tTHOXY-lI3HI -IS08ENZOFURANONE
690 2-ISOPROPYLTH10PHENE
691 3-<2-HYOROXYPROPYL>-5-NErHYL-2-OX»ZAL10I
692 3-METHYLOCTAH YDROPENTALENE-1-CARBOXYLIC
693 i.-HYDROXY-OCTAHYDRO-1-NAPHTHALENONE
696
5638120
3121
1201i»9
2363715
506387
5061.67
510371.2
7581.3
7180623
91,699
15677573
112538
201.9969
1377
1378
1379
78955
5325202
627985
98S95
693232
110805
33796871
5B6765
611007
RELATIVE SIZE
VIC X1C L2P L2M L2N L20 C3C C1P C1N C1N C2N R1C R2C E1C 02N 82C BIN BIN
1.0
3.0
1.0
.1
.1
.0
.1
.0
.0
.0
.1
.0
.0
3.0
2.0
2.0
3.1
.0
.0 1.0
3.0
.0
.D
.0
.0
.0
.0
.0
.0
.0
.0
.0
2.0
3.0
3.0
3.0
2.0
2.0
3.0
i.a
3.0
3.0
3.0
3.0
(Continued)
-------
TABLE 10. (Continued)
EM 1* CONCENTRATES PACE 17
COMBINED CONCENTRATE REPORT(PART t.AI
COMMON NAME
721 2.<».6-TRiaROMOPHENOL.
722 "•-PHENYL-'.-OXO-BUTYRIC AGIO
723 <,(2,5-XYLYL>BUTVRIC ACID
72<» 2,S-OI(CHLOROMETHYL>-3-ETMYL BENZOIC ACI
729 N-ETHYL-<,-HETHYL-2-PENTANEAMINE
726 0-CRESYL ACETATE
727 5-HEXEN-2-OL
728 OIHYORO-S-H£TMYL-2t3HI-FURANONE
729 2,2-OIETHYLPROPYLENE GLYCOL
730 1,-ETHYLPMENOL
731 ALPHA-OXOBENZENEACETIC ACID, ETHYL ESTER
732 3-DICMLOPOrtETHYL-i»,6-OI-T-BUTYL-0-BENZOQ
733 2,2I6-TRIHETHYL-1,<,-CYCLOHCXANEOIONE
73", CYCLOPENTANE CAR30XYLIC ACID, VINYL ESTE
735 2,2-OICHLOROBUTYRIC ACIO
736 2.3.3-TRICHLORO-2-PROPENQIC ACIO
737 2-METHOXY-2-HIXENOIC ACID
731 2-HEPTENOL
739 1-I2-HETHOXY-1-NETHYLETHOXY1-2-PROPANOL
7«,0 ABIETIC ACIO
71.1 2,<»,6-TRICHLOftOANILlNE
7<«2 METHYL PENTAOECANOATE
7s3 AMYLENE OICHLORIDE
7<<-T£TRAMETHYL BENZENE
755 2-HETHYL 8IPHENYL
766 HETHYLIS03UTVL BENZENE
757 C5 BENZtNE
75« Cb-BENZENE
759 C5 BENZENE
760 ETHYL TRIHETHVL BENZENE
761 OlETHYL TOLUENE
762 DIMETHYL ISOPfcOPYL BENZENE
763 DIMETHYL ISOPROPVL BENZENE
76<< DIMETHYL INOAN
765 5-METHYL TETKALIN
2001
3333
127
128
1,296661.3
533186
51,771,275
108292
11576<,
123079
1603798
26i»
2051,7993
16523061
13023002
2257351,
331,67761,
2032<>327
621,
631,935
713261.1
507".S9
83329
581.021
531,225
1651921,7
3027576<>
H99752
95<,76
11961,2
1,90653
86737
•,88233
61,3583
100
118
250
119
113
108
IQi.
105
617
2809645
0.0
-1.0
1.0 2.0*
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
1.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
CAS NO. RELATIVE SIZE
VIC X1C L2P L2M LZN L20 C3C C1P C1N C1N C2N R1C RZC E1C 02N B2C BIN BIN
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.1
3.0
3.1
3.0
1.0*
1.0*
0.0*
1.0*
1.0
2.0*
0.0*
1.0*
2.6
2.0*
0.0*
0.0*
0.0*0.0 *
1.0
1.1
1.0
2.0
1.0
2.8 2.0
0.0
2.0
2.0
(Continued)
-------
TABLE 10. (Continued)
EPA 18 CONCENTRATES PAGE it
COMBINED CONCENTRATE REPORMPART I.A)
COMMON NAME CAS NO.
766 2-PHENYL UNOECANE ".536883
767 C3 NAPHTHALENE 316
768 TRIMETHYLNAPHTHALENE 316
769 P-ETHYL TOLUENE 622968
770 2.6-OIMETHYLSTYRENE 2039909
771 INOAN 096117
772 1,3-OIETHYL BENZENE 101935
773 2-PHENYLHEXANE 6031023
770 1.2.3.I.-TETRAHYORO-0.9-OIHETHYL ACRIOINE 55030650
775 X»+CHRYSENE 318019
776 (2,2-DIHETHYLBUTYLI BENZENE 28080866
777 1.0-OIETHYL-2.3.5.6-TETRAMETHYL BENZENE 33962139
778 1-BUTYLNAPHTHALENE 1630099
779 1.5.7-TRIHETHYL INDAN 5030088O
780 1.1.0.7,7,8-HEXAHETHYL-S-HYDRINOACENE 17O6S586
781 BENZOFLUORANTHENE 203123
782 OIPHENYLMETHANE 101615
743 SEC-BUTYL BENZENE 135988
780 X2.3-OIMETHYLNAPHTHALENE 581008
., 785 TRIHETHYLNAPHTHALENE 317
00 786 C3 NAPHTHALENE 318
O 787 2-MtTHYL FLUORENE 1O30973
788 X2-METHYL ANTHRACENE 613127
789 1-TERT-BUTVLNAPHTHALCNE 17065915
790 XMENTHOL 89781
791 XN-auTYLETHER 102961
792 3,3,5-TRIMETHYCYCLOHEXANONE 873909
793 XTHUJVL ALCOHOL 513235
79* TERPENYL ACETATE 08210O9
795 OIACETYLBENEZENE 1009616
796 HEX-3-ENE-2.5-OIOL 7319235
797 o.ot-OIHETHOXYSTlLBENE 0705300
798 0-TERT-BUTYLPHENOL 88186
799 HETHYL ANTEISOHEPTAOECANOATE 2090095
800 2-HETHYL-1-PENTEN-3-OL 2088075
801 METHOXYNAPHTHALENE 2216695
802 *Z-HETHYL STYRENE 611150
803 TETRAPROPYLENE GLYCOL HETHYL ETHER 20320309
800 M-METHOXYPHENYL ACETATE 1020
605 3,3,0-TRIHETHYLOECANE 09622186
806 N-TSIETHYLENE GLYCOL. HONOETHYL ETHER 112505
807 N-METHYL SACCHARIN 15008990
808 Z-KETO-3-rtETHYL VALERIC ACIO 1060300
809 TRANS-3-HEPTENOIC ACIO 29901857
810 PENTACHLOROPYRIOINE 2176627
VIC X1C
RELATIVE SIZE
I C1N C2N R1C R2C E1C 02N
0.0
0.0
L2P
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
1.0
2.0
2.0
2.0
2.0
2.0
1.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
L2M L2N L2D C3C C1P C1N C1N C2N
1.0 1.0
2.B 1.0
2.0
0.0
2.0
2.0
1.0
1.0
2.0
1.0 2.0
2.0
1.0 1.0 1.0 1.0 1.0 2.0 1.0 1.0
2.0
2.0
2.0
2.0 2.0
2.0
2.0
2.0
1.0 2.0 2.0
1.0
1.0
1.0
(Continued)
-------
TABLE 10. (Continued)
EPA II CONCENTRATES PACE 19
COMBINED CONCENTRATE REPORT(PART I.At
COMMON NAME
CAS NO.
RELATIVE SIZE
VIC XtC LZP LZH LZN L20 CJC C1P C1H C1N CZN R1C RZC E1C
BZC B1H BIN
Oil
A 1 >
O 1 C
All
O 1 J
815
A 1 ft
O IO
817
818
A 1 4
O 17
821
822
A? 1
0€ J
A ?/.
O fc*»
825
826
827
828
829
M 830
2 "l
M 832
833
83H
835
836
837
838
839
8i.O
em
8i>2
81.3
8 <•<•
81.5
8 -.6
807
81.8
8i<9
850
851
852
853
850
855
••C.H IHUC.UH1E
1-ISOBUTYLNAPHTHALENE
1.1.2-TRIMETHYL-3-PHENVL INOAN
1,2.3-TRIHETHYL-l-PHENYL INOAN ISTERIOIS
1,2,3-TRIMETHYL-l-PHENYL INOAN (STEREOIS
X*»SHEX«CHLOROBENZENE
3.I..1.-TRIHETHVL-Z-CYCLOHEXEN-1-ONE
XH-ACETOTOLUIOE
NONYL PHENOL ISOHER
XGLYCIOYL PHENVL ETHER
<.(7-OlMETHYLBENZOFURAN
11, 2-0 ICHLOROETHVLI BENZENE
2-CYCLOHEXENOL
XCLOFIBRATE
XETHYLENE GLYCOL
1.3.5-TRICHLORO-Z-NETHOXYSENZENE
X»»IP-OICHLOROBENZ£N£
METHYL I.-BUTOXY8UTYRATE
•TRI-M-CRESYLPHOSPHATE
3-HETHYL AOIPIC ACIO
CYHENE IISOHER UNKNOWN)
CYHENE (ISOHER UNKNOWN)
X»»Sl,2.i<-TRICHLOROB£NZENE
l.Z.<>-TRINETHYL ETHYL BENZENE
Z.I..5-TRIHETHVLETHYL BENZENE
OIETHVL TOLUENE
Z.I..6-COLLIOINE
BENZONITRILE
Z-AMlNO-5-PICOLlNE
TRANS-2-ETHYL -3-PROPYLOXI RANE
P-HETHYLANISOLE
2.3.I.-TRIMETHYLOXETANE
2,5-DIMETHYL THF
l.-BROHO-3-PHENYLSYONONE
3.8-OIHETHYL-5-ISOPROPYL-lt2-NAPHTHOQUlN
CHLOROIOOOMETHANE
l-HETHYL-i.-11-HETHYLETHENYLI-CYCLOHEXENE
l-12-BROHOETNYLI-i.-CHLOROBENZENE
oeivc-i
16727916
33508020
33603393
33611161.
1187
-------
TABLE 10. (Continued)
EPA II CONCENTRATES PAGE 20
COMBINED CONCENTRATE REPORMPART I.AI
856
• 57
•58
859
860
• 61
862
663
864
• 65
• 66
• 67
• 64
869
• 70
• 71
• 72
873
• 7<>
«76
«"
878
• 79
880
• 81
882
• 83
sew
885
886
• 87
888
• 89
• 90
• 91
892
• 93
89<>
8 95
• 96
• 97
898
899
900
COMMON NAME
3,-TETRACHLOROBUTANE
X3-METHYLPHENANTHRENE
XN'AMYL ALCOHOL
XMETHYLAL
<.-PENTEN-2-OL
2,2-OIMETHYL-l, 3-CYCLOPEMTANEDIONE
S-OODECANONE
ZQUINOLlNE
CAS NO.
73<>3068
7396385
3661702
820291
26118317
tl9572
2311.785
106707
6181.28
-------
TABLE 10. (Continued)
It CONCENTRATES PACE
COMBINED CONCENTRATE REPORf(PART I.A)
00
U)
COMMON NAME
901 TETRAPROPYLENE GLYCOL
90Z N-ETHYL-Z-BENZOTHIAZOLANINE
903 N.N-OIHETHVL8ENZYLAMINE
90* OIMETHYLCYCLOHEXANE OIONE
905 2.Z.1.-TR1METMYL-1.3-PENTAKEOIOL
906 METHYL LAURATE
907 ETHYL NYRISTATE
90S 6-METMOXY-2-HEXANONE
909 6-METHYL-2-HEPTANONE
910 1.2-OIAZABICYCLOC2.Z.Z. IOCTAN-1-ONE
911 2-HCTHOXY-10-UNOECENOIC AGIO
91Z 5.6,7,7A-TETRAHYORO-i»t'..7A-TRIHETMTL-ZI*
911 l-PROPOXY-2-PROPANOL
91i> 2-ETHYLHEPTANOIC AGIO
915 5-METHVL-5-ETHYL-2ti>-OXAZOLIDINEDIONE
916 X3.5-OICHLOROPHENOL
917 aROHOCHLOROBENZOIC AGIO
911 16-HYOROXY PALMITIC ACIO
919 OCTAHYOHO-l,i.A-DIH£THYL-l-PHENANTHRENE C
920 I..6-OIMETHVL OCTANOIC ACIO
921 5-NETHYL-2-HEPTANONE
922 2-METHYL£NEBUTYRIC ACID
923 P-AHINOBENZENc-T-BUTYRIC ACIO
921. 5-ETHENYL TETRAHYOSO-.ALPHA.,.ALPHA. ,5-T
926 6-NETHYL-3.5-HEPTAOIEN-2-ONE
92b TRIMETHYL-6-VINYLTETRAMYOROPYRAN-3-OL
927 2-METMYL-2-HEPTEN-I.-ONE
924 3,".-OIHETHYL-2,5-FURANOIONE
929 XETHYL CARBONATE
930 <.,)>-OICHLOROauTENOIC ACIO
931 BARBITAL
932 Z-BROHO-1.2-OICHLOROPROPAME
933 METHYL OICHLOROACETATE
93<« 3-OCT£N-2-ONd
935 2>3.<»-TRIMETHYL-2-CVCLOPENTEN-l-ONE
936 S.5-OIMETH.YLFURANONE
937 5-HEPTEN-2-ONE
938 N-nETHYL'2-PIPERIOINONE
939 3.1.-OIMETHYL-3-PENTEN-2-ONE
9<>0 hETHYL-l.ll-OCTAOtCAOIENOATE
9<.l N-6ENZOTL-L-ALAKINE, METHYL ESTER
9. 1,1,2,3-TETRACHLOROPROPANE
9<.S 6-PHENYL-2-HEXANONE
CAS NO.
1376
28291692
103133
126814
111120
12<>061
29006006
921617
163226t
21<>
153567m
1569013
327<«291
115673
591355
Z56311<>6
506138
365001.2
2553960
1121712I.
35*6581
15118602
5989333
166<.70<><.
UO-.9117
2231921.0
766392
105588
16502888
25187Z1
17759885
11651.1
1669V1.9
28790865
137
6711.007
93120<>
681.91.6
130381.76
721.1.679
60333
111271
181.95302
U171892
RELATIVE SIZE
VIC X1C LZP LZM LZN LZD C3C C1P C1N C1N C2N R1C
R2C E1C
Z.O
2.0
2.8
Z.O
Z.O
Z.O
Z.O
Z.O
Z.O
Z.O
OZN B2C B1M BIN
Z.O
2.9
Z.O
2.
2.
2.
2.
2.
2.
2.
Z.
2.
1.0
Z.O
Z.O
Z.O Z.I
Z.O
Z.O Z.O
Z.O
2.0
Z.O
Z.
Z.
Z.
Z.
Z.
Z.
Z.
Z.
Z.
Z.
1.0
1.0
1.0
0.2 1.0 *
1.0
1.0
1.1*
(Continued)
-------
TABLE 10. (Continued)
EPA 16 CONCENTRATES PA6E Z2
COMBINED CONCENTRATE REPORT IPART I.A I
COMMON NAME
CAS NO.
RELATIVE SIZE
VIC KIC LZP LZM LZN LZO CIC C1P C1H CtN CZN R1C RZC ElC OZN BZC 81M BIN
91.6
9*7
9»8
9*9
950
951
952
953
9S*
955
956
QC7
^ y t
958
959
960
961
96Z
963
96<>
|-i 965
00 96o
*- 967
968
969
970
971
97Z
973
97*.
975
976
977
978
979
980
981
9«2
983
98<»
98S
966
987
984
989
990
3-PENTEN-Z-ONE
3-METHYL-2-BUTEN-1-OL
<>I-TRIMETHVL PHENANTHRENE
3,9,10-TRIMETHYL ANTHRACENE
OCTYL BENZENE
1,1,3-TRIMETHYL INOAN
X9-METHYL ANTHRACENE
IS08UTYL BENZENE
HETA-CYMENE IM-ISOPROPYL TOLUENE*
DIMETHYL ETHYL BENZENE
1.8-OIMETHYL TETRALIN
1,2-DIMETMYL NAPHTHALENE
METHYL ACENAPHTHENE IISOHER UNKNOWN)
XOI-N-BUTYLNITROSAHINE
3,3,3-TKICHLOROPROPENE
TERT-BUTYLBENZENE
<>f6-OIMtTHYL PYRIMIOINE
2.3-OIMETHYL PVRAZINE
PYRAZOLE
N-PROPYL NAPHTHALENE
TRIMETHYLNAPHTHALENE
METHYL NONAOECANOATE
KCINNAMYL ALCOHOL
Z-T-BUTYL NAPHTHALENE
Z-METHYL-1-PROPYLNAPHTMALENE
6ZS33Z
556821
5<,0fc31i,8
1.920950
56667017
103651
6682060
55 669680
827521
1127760
1<»60022
l7*»65597
1007267
19262205
S't'il07<>l
19219853
367i!757
17059462
17057626
5*31.0873
2318961.2
6301891.0
2189606
2613765
779022
63(932
535773
202
25-.1933'.
573968
5851.8362
92<.163
2233003
96066
155617'.
5910691.
286131
325
319
173191.8
10<>5i.l
2876359
5i.77i.899
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
In
. u
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
1.0
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
(Continued)
-------
TABLE 10. (Continued)
EPA IB CONCENTRATES PACE ZI
COMBINED CONCENTRATE REPORT(PART I.At
00
Ul
COMHON NAME
CAS NO.
VIC XIC L2P L2N
RELATIVE SIZE
L2D C3C CIP C1N CtN
R1C RZC EtC OZN BZC Bin BIN
991
992
993
991.
995
996
997
991
999
1000
1001
1002
1003
100<.
1005
1006
1007
i Ann
1 U UO
1 009
1010
1011
1012
1013
lOli,
1015
1016
1017
1011
1019
1020
1021
1022
1023
102<.
1025
i n ?A
1 U cO
1027
1021
1029
1030
1031
1032
1033
103%
1035
NONVL PHENOL ISOHER
XINOENE
CHLOROVINYLBENZENE
GAHHA HETHYLBENZENEBUTANOIC AGIO, HETHYL
2-HETHYLBENZAHIOE
X*M-NITROANILINE
i.-TERT-BUTYL-2-HETHYLPMENOL
l-HETHYL-3-PROPYL BENZENE
3-HETHYL-3-HEXANOL
1-ALLYLBENZENE
OIETHYLHETHYLVINYLSILANE
XH-CHLORONITRO BENZENE
2-PMENYL-1.1.-CYCLOHEXAOIENE
1.1.-OIHETHYL-S-OCTYLNAPHTHALENE
1-ALLYLNAPHTHALENE
3,i.»-OIHETMYL-ltlt-8lPMENYL
ETHYLBENZYL BENZENE (ISOMER UNKNOMN1
OIMETHVLOIPHENYLNETHANE
AMYL BENZENE
5-NETHYL INOAN
1-HETHYL TETRALIN
X«TRIPHENYL PHOSPHATE
PARA- MET HOXYSTILBENE
1.2.1.-TRITERTIARY BENZENE
*P-ChLOROACETOPHENONE
3-METHYL-2-MEXANOL
P-EFHYL-ISOPR OP YL BENZENE
2,6-OI-TERT-BUTYL TETRALIN
1,1.3-TRICHLORO-l-PROPENE
l-BROnO-2-CHLOROCYCLOPENTANE
7-ETHYLQUINOLINE
etT*. BETA-DIMETHYL HISTAHINE
3-CYCLOHEXYL-i.- PENT EN-Z -ONE
OIISOBUTYL KETONE
5-METMYL-5-PHENYL-2-HEXANONE
t-DECANONE
b-METHYL*2-PHENYLQUINOLINE
HEXtMETHYLENE ACEUNIOE
l.-HETHYL-3-HEXANOL
HEXYL BUTVRATE
X*(2,i.,5-TRICHLOROPHENOXYIACETIC ACID
•TRICHLOROBIPHENYL
511 1.0
95136 1.0
622253 0.0 *•>
21.306238 1.0
6016 1.0
99092 1.0
91271 1.0
1071.1.37 .1
597966 .0
637503 .0
11292290 .0
121733 .0
1370521 .0
55000531 .0 1.0
21.19163 .0 1.0
7383906 .0
i«2550<.5i»l .0
1351.0562 1.0
538611 1.0
171.351 1.0 1.0
1559115 1.0 1.0
115166 l.« 1.0
111.2150 1.0
11.59116 1.0
99912 1.0
2313657 1.1
1.21 8488 1.1
1.2981760 .1
256711.1 .«
11.376820 .0
766 H. 71. .1
21150016 .0
5570251.0 .0
101838 .0
11.128611 .0
6?i.l68 1.0
273561.63 1.0
50091.16 1.0
615292 1.0
2639636 1.0
93765 1.1
25323616 1.1
(Continued)
-------
TABLE 10. (Continued)
EPA IS CONCENTRATES PAGE Z«.
COMBINED CONCENTRATE REPORHPART I.AI
CONNON NAME
CAS NO.
RELATIVE SIZE
VIC X1C L2P IZN L2N L20 C3C CtP C1H C1N CZN RlC RZC EtC OZN B2C B1H BIN
1036
1037
1034
1039
10".0
1041
tO 1.2
10H3
101.1.
101,5
101.6
10*7
10<.8
101.9
1050
1051
CO l052
0? 1153
1051.
1055
1056
1057
1058
1059
1060
1061
106Z
1063
1061.
1065
1066
1067
1068
1069
1070
1071
1072
1073
1071.
1075
1076
1077
1078
1079
1080
2.3,6-TRIMETHYLHEPTANE
+ ZMLINOANE
X*0-CHLOROTOLUENE
X»»$HEPTACHLOR
•tTETRACHLOKOBIPHENVL
••1PENTACHLOROBIPHENYL » OTHER PCBS
•SHEXACHLOR08IPHENYL
X*»ODE
X»»»OOT
OIBENZOTHIOPHENE
icHETHYLQIBENZOTHIOPHENE
XETHYLENE TETRACHLORIOE
0-ETHYLSTYRENE
1.1,2.3.3-PENTACHLOROPROPANE
l.b-OICHLORO-l.S-CrCLOOCrAOIENE
2-ETH YL-1 . 1-BIPMI- NYL
1-METHTLFLUORENE
METHri.atNZACRIOIN£
3-HYDPOXV-3-HETHVL-2-BUTANONE
XZ.iftUTIOINE
Z.5-LUTIOINE
2.1..5-COLLIOINE
«.-ETHYL-Z,6-OIMETMYL PYRIOINE
Z.3.5-COLLIOINE
3-ETHYL-5-NETHYLPYRIOINE
2.3.6-TRIMETHYLPYRIOINE
N.N-OIETHYLANILINE
3-OOOECANONE
<.*ACETYLHORPHOLINE
XQUINAIOINE
2.3.I.-TRIMETHYLQUINOLINE
TRINETHYLQUINONE
HEXANEOIOIC ACID. OIHEXYL ESTER
Z*P-NITRO PHENOL
3-CHLORO-2-BUTANOL
7-OXO-OCTANOIC ACID
3-METHVLPIPERIOINE-Z.8-OIONE
S-PROPYLOIHYORO-2-FURANONE
3A.7A-OIHETHYL OCTAHYORO-I.-ISOBENZOFURAN
UtiO^CAN£
3-METHYL-3-OCTANOL
BROMOOICHLORO ANILINE
HEPTYLPROPIONATE
ACETAMIOE
XCHLORQACETIC ACID
1.032933
58899
951.98
761.1.8
26911.330
800
2660161.9
72559
50293
132650
7372865
127191.
7561.638
1510<>617
Z91.8 01.20
1812517
1730376
3519877
115220
1081.71,
589935
1122390
36917369
695987
3999788
ti.6281,6
91667
1531.276
1696201.
91631.
2it37721
1361.
1759
100027
56381.8
11,112982
29553513
105215
51.382580
jlCO^llr
531.0363
739
2216811
60355
79118
1.1
.0
.0 1.0
.0
.0
.0
.0
.0
1.0
1.0
1.0
1.0
1.0
1.0
1.1
1.0
1.0
1.0
1.0
1.0
1.0
1.0
.0
.0
.0
.0
.0
.0
.0 1.1
.0
.0
1.0
1.0
1.8
1.1
1.0
1.0
1.0
1.0
— trj
l.Q
1.0
1.0
1.0
1.1
(Continued)
-------
TABLE 10. (Continued)
EPA It CONCENTRATES PAGE Z»
00
COMBINED CONCENTRATE RE PORT (PART I.At
RELATIVE SIZE
VIC X1C LZP LZN LZN LZO C3C C1P C1N
C1N CZN RlC RZC EtC OZN BZC BIN BIN
COMMON NAME CAS NO.
1081 t-CHLOROCROTONIC ACID
108Z "Z.I.-DICMLORONAPMTHALENE
1093 SEC-ISOAMYL ALCOHOL
106<. 5-UCETYLOXY)-Z-PENTANON£
1085 3,<,,5-TRIMETMYL-Z-CYCLOPENTEN-l-ONE
1086 OIETHYLENE GLTCOL, MONOMETHYL ETHER
1047 N-BUTYLAMINE
1088 Zt077 0.0
1097 3,3-OIMETHYL-Z<3HI-FURANONE 1352<.760 0.0
1098 FLUOROIOOOBENZENE (ISOME* UNKNONN) 1111 0 0
1099 J-NETHYL-Z-FURANONE
1100 1.-..5-TRIMETHYL NAPHTHALENE
1101 3-HETHOXY-3-HETHYL-Z-BUTANONE
1102 DIBROMOPHENOL
1103 1H-INIOAZOLE-Z-CARBOXALDEHVQE
110". 2-U-METMYL-3-CYCLOHEXENYLI ISOPROPANOL
1105 1,2-CYCLOHEXANEOIOL
1106 METHYL HEPTAOECANOATE
1107 BUTYL THIAZOLE
< RS ENTRIES LABELED WITH AN ASTERISK ARE PROBABLY ATTRIBUTABLE TO THE BLANK ASSOCIATED WITH CONCENTRATE GENERATION. SEE DISCUSSION IN TEXT OF VOLUME 1.
16197903
Z19>7S6
59875<.
5185977
55683211
111773
109739
2931,056
1303«<.5«
5129b02
81.753
1809105
622855
95156
203805
3-.5i.077
1352<.760
1111
22122367
Z131i.ll
36687966
5 -.6
10111087
101.62561
931179
1731936
6086222
0.0
0.0
0.0
-1.0
-1.0
-1.0
-1.1
-1.0
-1.0
0.0
0.0
0.0
-------
TABLE 11. COMBINED LISTING OF IDENTIFIED COMPOUNDS FOUND
IN DW AND AWT CONCENTRATED
oo
oo
PAGE 1
COMMON NAME
FINAL REPORT (PART I)
RELATIVE SIZE MD CONCENTRATE WHERE DETECTED
1 CLOFIBRIC ACID t
2 X*SOI-N-BUTYLPHTHALATE
3 2-U-BUTOXYETHOXVIETHAN[)L (A OIETHVLE
1.2,2-TETRACHLOROETHANE
20 OIHEXYLAOIPATE
21 XHETHYL BENZOATE
22 XSTEARIC ACIO
23 DIETHYLENE GLYCOL, BUTYL ETHER
2
-------
TABLE 11. (Continued)
PAGE z
COMMON NAME
<>6 1,1-OICMLOROACETONE
9
251
6
566
6
1 6
6
6
5
3 i,
5
t
1
0
3*
2 2
1 t'
S
2
C
2
6
6
2
3
»
1
3
2
Ii
3
i,
it
3
i.
2
S L C C C U K
2211121
X H C M N N C
3
6 5 i. 3 5
6 5 k
5
5
5
5
it
1
3* 6
3
0
5 5
2 2
32 5
Zc c
3 y
It '» 6
5
5
5
I* 2*
<.<,<.
1* 3* it*
3* <.*
6 5* 5*
2* 3* 5*
it
(Continued)
-------
J.O.. (.Continued)
PAGE 3
COMMON NAME
FINAL REPORT (PART II
RELATIVE SIZE »NO CONCENTRATE HHERE DETECTED
91
92
93
95
96
97
96
99
100
101
102
103
10
OEHYDROABIcTIC AGIO 102
3tit-DIETHYLBIPHENYL A 5
1-HETHYL INOENE a 3
ZtTOLUENE 5
ISOVtLERIC ACID *
2tit-DIHETHYLBENZOIC ACID
3-PENTEN-2-ONE
HEXAHYDROTOLUENE
XACETOPHENONE a 322
6-METHYL-5-HEPTEN-2-ONE 3
2-ETHYL-l-HEXANOL -1 li 5
2'-ETHYLACETOPHENONE A 2
M-TOLUIC ACID it
P-TOLUIC AGIO it
HSOPHORONE 3
T T T H
Y C X C
3* 6
It*
i 5 it it
3 5
-------
PAGE «.
COMMON NAME
FINAL REPORT (PART I)
RtLATIWE SIZE AND CONCENTRATE WHERE DETECTED
116
117
118
119
1VO
I'll
11.2
1<>1
1 VV
11.5
IV6
1 Vf
1 <>8
1 V9
150
151
152
151
1 5<<
155
156
157
158
159
160
161
162
161
161.
165
166
167
1 fr. A
1 DO
169
170
171
172
171
1 7<<
75
76
77
78
79
180
2.6-OIHETHYLBENZOIC ACID
l,5-H£PTAOIENE-l.
-------
TABLE 11. (Continued)
PASE 5
COMMON NAME
161 TETR*HYORO-1<1-OIOKIDE THIOPHENE
182 N-TRIETHYLENE GLYCOL> MONOETHVL ETHER
183 METHYL NYRISTATE
18* METHYL STEARATE
185 X'tSTYRENE
186 1.3-DIETHYL BENZENE
187 l.it-DIETHYL BENZENE
188 1,2-DIETHYL BENZENE
189 ETHYL PALNITATE
190 METHYL-3,5-OIHETHYL BENZOATE
191 2-METHOXV-3-NETHVLCROTOMIC AGIO
192 XOIBROHOCHLOROHETHANE
193 2-CVCLOHEXENONE
19S 2,3,5,6-TETRACHLOROTEREPMTHALIC AGIO
195 XfH-XVLENE
196 X3-CHLORO-2-METH»L PROPENE
197 X»10-DICHLORO BENZENE
198 X»»SHEXACHLORO-li3-BUTADIENE
199 P-METHYLSULFONYL TOLUENE
200 lil.3,3-TETRAMETHYL-2-INDANONE
201 2.3-DIMETMYL-2-BUTANOL
202 METHYL HEPTANOATE
203 PHENYL ACETIC AGIO. METHYL ESTER
20 y 33
3
3
3* 5* 5* 5* 3* 2*
3 5
5 V 2 5
5 3
it* U* 5 1* t* i*
5 3 it
(Continued)
-------
TABLE 11. (Continued)
PAGE 6
COMMON N«H£
FINAL REPORT (PART II
RELATIVE SIZE AND CONCENTRATE HHERE OtTECfEO
226 XMETA-CRESOL
227 3tit-OICHLOROBENZOIC ACID
22« 2-HEPTENYLBENZENE
229 X2-METHYLNAPHTHALENE
230 XBIPMENYL
231 2-METMYL BIPHENVL
232 3fit»-OIMETHYL-ltl»-BIPHENYL
23) XSTILBENE OXIDE
23<, 2-<2-HYDROXYPROPOXYI-l-PROPANOL 248 Z-HETHOXY-i.-METMYL-2-PENTENOIC ACID
2".9 2t>ti6-TRIMETHYLBENZOIC ACID
250 ORTHO-TOLUIC ACIO
251 2-PHENYLPROPIONIC ACIO
252 XHYDROCINNANIC ACIO
253 3,
-------
TABLE 11. (Continued)
PAGE 7
COMMON NAME
FINAL REPORT (PAST II
RELATIVE SIZE MO CONCENTRATE WHERE DETECTED
I/ \l T T T
1 1 2 I 1
* C X B C X
T T T M N F POOSSLCCC
l
C**C
293
294
295
296
297
296
299
300
301
30Z
303
30".
305
306
107
306
309
310
311
312
313
31<.
315
7-OCTEN-Z-ONE
XCHLORO FORM
XMETHYLPHENVL CARBINOL
OIOCTYL AZELATE
3-HETHOXY-1.2-BENZISOTHIAZOLC
2-NETHYL-J-HEXENOIC ACID
5-PHENYL PENTANOIC ACIO
TETRAHYDROFURAN-Z,5-DICARBOXYLIC ACIO
XETHYL ACETATE
ZHETHYL IS08UTYL KETONE
N-BUTYL ACtTATE
^-ETHOXYBUTYL BUTANOATE
•TRICRESYL PHOSPHATE IISONER UNKNOWN)
SH-CHLOROPHENOL
'•-I1.5-OIHETHVL-3-OXOHEXVLICVCLOHEXANECA
li2-BENZISOTHIAZOL-3(2HI -ONE
1,3-OIHETHYL BUTABAitBITAL
1-PHENYL-1.2.3-PROPANETRIOL
N.N-OIHETHYLHEPTANANIOE
XHETHYL CHLOROFORM
2.2-OINETHYL-l-BUTANOL
— trUULKA nt
Z-TERT-BUTYLCYCLOHEXANOL
ZAOIPIC ACIO
Z.2-OIHETHYLVALERIC ACID
ETHENYL CYCLOPENTANEACEFATE
12.5-OIHETHYLBENZENEIBUTANOIC ACIO
XARACHIOONIC ACID
TRIPROPYLENE GLYCOL, METHYL ETHER
XP-HETMOXY-T-BUTYL PHENOL
3-BUTVL-6-HETHVL-Zil>-PVRIDINEDIOL
1-(CZ, 6,6-TRIMETHYL-l-CYCLOHEXEN-l-YLIOX
ANTEISOHEPTAOECANOIC ACIO
TETRAETHYLENE GLYCOL MON09UTYL ETHER
6.11-OCTAOECAOIENOIC ACIO
LIGNOCERIC ACIO
HYRISTVL ALCOHOL
3-METHOXY-2-BUTANOL '
1,5-8IS(T-8LITYL» -3,3-DINEfHYL BICYCLOC3.
OCTAOECATRIENOIC ACID
ACENAPHTHYLENE
PIPERIDINOL
OIETHYL CARBINOL
2,3-DIHYDRO-<.-HETHYLFURAN
ETHYLBENZALDEHYDE A "i 2
2 5
to t
• £ P
1 5
1 5
3 ii 5
2 5
5
5 3
5
5
5
S
Z 15
5
5 <•*
5 3
5
5
5
5
5
<3
5
5
5 3
"• <• 1 3 5
3 5
5 3
5
5
5
5
S
5 5
5 3
5
5
5
5
5
5
Z* 3* 5
3 Z 52
<.* i»* 5* 1 i^ I*
* SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
COMMON NAME
TABLE 11. (Continued)
FINAL ?EPO*T (PART II
RtLATIVE SIZE AND CONCENTKATE MHERE DETECTED
PAGE 8
316
317
31S
319
320
321
322
323
32<>
325
326
327
326
329
330
331
332
333
33",
335
336
337
338
339
3«,0
3<»1
31.2
31.3
3<«<»
I6
3<.7
3«.8
31.9
J50
352
353
35«,
355
356
357
358
359
360
11211
«C X B C X
2»tJ»-OIN£TMYLACETOPHENON£ A
3-ETHYLSTYRENE A <• 2
ETHYL MYRISTATE A <,
DEC AHYORO-2t 3-01 METHYL NAPHTHALENE 2
X* 12, 1,,5-TRICHLOROPHENOXYI ACETIC ACID 1
3,<.-OIMETMYL-2,5-FURANDIONE
l,2,3-TRIMETHYL-«.-PROPENYLNAPMTHALENE 2 3
-------
TABLE 11, (Continued)
PAGE 9
COMMON NAME
FINAL REPORT JPART II
RELATIVE SIZE AMD CONCENTRATE WHERE DETECTED
361 OCTAHYORO-'t-HEXATRIENE
39<« 2-M£rHVL-2-ISOBUTVLOXIRANE
395 1-METHYLHEXVLHVOROPEROXIOE
396 2-BUTYL-3-HETHVLOXIRANE
397 2-HETHOXV-<>-METHYL-Z-PENTENOIC ACID, NET
398 2.3.<>-TRIMETHVL-3-PENTANOL
399 1-ISOCVANONAPHTHALENE
".00 N-TERT-BUTYL-3-METHYLBENZAHIDE
<«01 <,,5-OIETHYL-2. 3-DIHYORO-2t 3-OIMETHYLFURA
i»02 il>7-OIMETHVL-li3-ISOB£NZOFURANDION£
".03 Zt5-DIHETHYL-2-HEXANOL
H0<. PROPYLOXIRANE
".05 XCYCLOHEXYL ACETATE
11211
c x a c x
0
3
2
0
3
i,
1 it It 2
Y C X C
I, it it
it
2 5
2 l(
-------
COMMON NAME
TABLE 11. (Continued)
FINAL AEPORF (PART II
RELATIVE SIZE AND CONCENTRATE WHERE DETECTED
PACE 10
•.06
1(06
1.09
1,10
1.11
•,12
413
414
415
416
417
416
419
•,20
421
4ZZ
423
424
425
426
427
4Z8
4Z9
it *I ft
H J U
-.31
43Z
1,33
434
435
436
437
438
439
440
441
442
•,43
444
445
446
447
448
449
1,50
11Z11144ZZ2
*CXBCXYCXCCC
X(ETHOXYHETHYL) OXIRANE 5
4-HEPTANONE S *
4,6-DIMETMYL OCTANOIC ACID 5
0-CRESYL ACETATE 4 5
3-HYpROXVNONANOIC ACID 5
XZ.4-DIMETHOXYBENZOIC ACID A 5
P-ETMYLBENZOIC ACID 5*
4-HrOROXY-4-HETHYLCYCLOHE«ANONE 2
X»P-CRESOL 00 0* 0*
1.1-DIPHENVLETHANE A 4 4* 2
2-BUTYL THF -1 3
HETHYL AHYL CARBINOL 1 4*
XETHVL CARBONATE 3 4
5-METHYL HEXANOIC ACID 2 34
4.5-OIHETMYL-Z-HEPTEN-3-OL 2
5-METHYL-Z-HEPTANONE 4
1,3.3, 7-TETRAMETHYL-2-0«OaiCYCLOIZ. 2.1 IH 4
BUTYL ISOBUTYRATE 3
2-ETHVLCYCLQHEXANONE
OIETHYLENE GLYCOL, HETHYL ETHYL DIETHER
2-MEFMYLHEPTANOIC ACID
1.6-HEXANEOIOL
Zt3-OIHYORO-<.-ll-METHYLETHYLIFURAN
CYCLDHEXANEHEXANOL
Z,Z,5,5-TETRANETHYL TMF
X4I1HI -PrRIMIOI NONE
3.5-NONADIEN-7-YL-Z-OL
4,4,5.5-TETRAMETHYL-t.3-OIOXOLAN-Z-ONE
Z-U-METHYLETHYLIOENEICYCLOMEXANONt
OXACYCLOTETRAOECAN-Z-ONE
1,1-OICHLORO-Z-HEXANONE
4.4-DICHLORO-3-HEXANONE
OIHYORO-5-METHYL-Zt3HI -FURANONE
C3-OIHYDROXYBENZOIC ACID
4-BUTOXYBUTYRIC ACID
XS1.2-DICHLOROETHANE 3 2
PENTAETHYL8ENZENE 4
XDMF (D1METHYI FORMAMIDE) Z Z
N-ACETYLCVCLOHEXVLAniNE
D-ETHYLBtNZOIC ACID A3 4* 4*
X»tOICHLOROETHYL ETHER -1 4
XETHYL 8EN70ATE A 4 1 4*
ETHYL PENTADECANOATE A 2 4* 2*
ETHYL STEARATE A 2 1 4' Z*
POOSSLCCCCKKtUBO
Z2ZZZZ31121Z1ZZ3
XCXCXMCMNNCCCNCC
Z
3
3
Z
5
4* 4*
1* 0 0* 2*
<( 2 i H
4
4
4 3
4
4
4 3
li
I,
4
4
4
4
4
4 3
4
4 I 4
l. ii
1 4 Z 3 Z
i,
1* 0*
2* 2
3* i"
3* 3*
* SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE 11. (Continued)
PAGE 11
FINAL REPORT (PART I)
COMMON NAME RELATIVE SIZE AND CONCENTRATE WHERE DETECTED
VVTTTTTTMNPPOOSSLDCCCRREOBB
1121lli.it222222222Jll2121223
*CXBCXYCXCCC XCXCXMCMNNCCCNCC
«51 X»»»P-OICHLOROBENZENE 11 itO 21(0 -12 1 2 1
1.52 METHYL LAURATE a 3 3 1
".57 3-HEPTANOL 3 * -1 3*2
1.58 1-CHLORO-2-METHYL-2-BUTENE <•
i.59 NEOPENTYL CHLORIDE it 2
1.60 l-BROMO-*-ETHYLBENZEN£ i|
1.61 2.I..S-TRICHLOROANILINE <• 12
1.62 'PENTACHLOROANILINE It
1.63 1.2,2>3-TETEACHLOROPROPANE U 2
it6>t X*+fl,2,t • 12
00 .7<, PENTYLENETETRAZOLE It J
-------
TABLE 11. (Continued)
PAGE 12
COMMON NAME
i.9b HEPTVL ALCOHOL
BUTANOIC AGIO
502 2-PHLNOXVETHANOL
50J (2-ETHOXV-l-HETHOXrETHOXri -ElHENE
S0
-------
TABLE 11. (Continued)
PAGE 13
COMMON NAME
FINAL jiEPORT (PART II
RELATIVE SIZE UNO CONCENTRATE WHERE DETECTED
5*1
Sift
5*3
5**
51,5
5*6
5*7
5*8
5*9
550
551
552
553
55*
555
556
557
55»
559
560
K> 56t
0 562
O 563
56*
565
566
567
568
569
570
571
572
573
57*
575
576
577
578
579
580
561
562
583
c a *.
9 OH
585
TERPIN
3-HETNYL VALERIC ACID
3-HETHOXYBcNZOIC ACID
3-HYDROXYTETRAOECANOIC ACID
2.6-OICHLOROBENZOIC AGIO
UNOECANEOIOIC ACID
5-EPIDEOXYPOOOCARPIC ACID
DIACETONE ALCOHOL
3-OCTANONE
3-OCTENOIC ACID
0-ANISIC ACID
OICYCLOHEXYLAOIPATE
S-METHYL-2-HEXANOL
PIPERIDINONE
TRIOECYLIC ACID
HEXAHYDRO-*-HETHVL-2H-AZEPIN-2-ONE
XP-TERT-BUTVL PHENOL
VACCENIC ACID
6-METHVL-3(2H) -BENZO FUR* NONE
1.3-OIHETHOXY-2-PROPANOL
OIMETHYLSULFONE
P-l 1,1, 3, 3-TETRAMETHYLBUTYLI PHENOL
3-METMOXY-2-METHYL-2-PENTENOIC ACID
3.3 DIHETHVLGLUTARIC ACID
XSBUTYLIBUTOXY CARBONYLI METHYL PHTHALATE
fOIHETHYL TEREPHTHALATE
STERT -BUTYL METHYL PHTHALATE
X2-HYDROXY8IPHENYL
CIS-2. 5-OIMETHYLTETRAHYORO FURAN
N-METHYLETHOSUXIMIDE
*-TERT-BUTYL-O-PMENYLENE CYCLIC CARBONAT
BUTABARBITAL
2,6-8IS(i,l-OIMETHYLETHYLI-*-ETHYLPHENOL
ANISOLE-2-ACETIC AGIO
BETA.3.*-TRIMETHVLBENZENEPROPANO!C ACID
*- d *
* *
* 3 3 * * * 3
233 <
** 22* J**- 2*
311 0 *
* *
* 2 * 3 *
31 *
3 4
* * 2
22 3
-------
TABLE 11. (Continued) O.rc
PA&c
FINAL REPORT (PART II
COMMON NANE RELATIVE SIZE AND :t>NCENTRATE HHERE DETECTED
VVTTTTTTHNPFOOSSLCCCCRREDBB
112111<><>2222222223112121223
•CxecxYCXccc XCXCXMCMNNCCCNCC
586 OI-N-HEXTL ETHER - li
5*7 l-HETHOXY-2-BUTANOL "i
588 2t3-OIM£THYL-J-PENTANOL <>
589 2-METHYLGLUTARIC ACID <•
590 2-ACETYL-V-METHYL-I.-PENTENOIC ACID <•
591 2.6-DIMETHYLPHENOXY CARBONIC AGIO *•
592 X6-MYOROXYCAPROIC ACID LACTONE 3-HYDROXV-l,2-BEN;iSOrHIAZOLE <•
60S 0-PROPIONYL BENZOIC ACID <.
606 2-HETHYL- lt3t5-TRIETHYLBENZENE a 3 3* •.* 3 I. *
615 2,6-OIMETHYL OLCALIN 1 <•
616 XBUTROLACTONE 3 < ^ >• *, i Z I
618 SEBACIC ACIO 3 3 i, 3
619 2,6-DlHETHYL ACETOPHENONE a 2* <.*
620 3-OCTEN-2-ONE J % 2
621 2-M£rMOXY-3,5,5-TRIMEIH»L-2-C»CLOM£XENE-
623 2-ETHOXYNAPHTHALENE "«
62<> XN-DECYL ALCOHOL -. . 2 3«
626 TETRALIN A 31 2* 2* 2 0 <. « 2 3A • 1
627 OIVINYLBENZENE A 2 2* <• » 2
628 P-ETHYLBENZALDEHYDE A 2 «•• «. • 3 -1»
629 2»-METHYLACETOPHENONE A 1 3 <. . 2 »
630 1-METHYL TETRALIN A 2 2« 0 ".» -I I
• SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE 11. (Continued)
PAGE IS
Ki
O
COMMON NAME
FINAL REPORT (PART I>
RELATIVE SIZE AND CONCENTRATE WHERE DETECTED
V V
1 1
* c x
8C
CCC
631 1,1-OIHETHYL INOAN-t-CARBOXYLIC ACID, ET A
632 2-ACETYLOXYACETOPHENONE a
633 2»,i,»-DIMETHYLACETOPHENONE A
63*. XZ-ETHYL NAPHTHALENE A
635 2-METHYL INOAN A
636 Z.Z-DIMETHYL-3.S-OECADIYNE
637 5-HETHYL INOAN A
638 2,5-CYCLOHEXAOIENYLBENZENE
639 ALPHA-HETHYLSTILBENE a
6<>0 Z,3,i»,5,6-PENTAFLUORO-N-(2-PHENYLErHVLIB
6<>1 <«,i,»-OIETHYLaiBENZYL a
6*2 OIPROPYLENE 6LYCOL METHYL ETHER (l-(2-
6i.3 3-PRDPYLCVCLOPENTENE
fc«,H 2-HENDECANOL
6*5 1-UNOECANOL
6<>6 HEXVL BENZOATE
61.7 PENTYL BENZOATE
6*8 *-HETHYLPHTHALIC ACID
61,9 X2-NAPHTHOIC ACID
650 1,2.3,3-TETRACHLORO-l-PftOPENE
651 l-NETHVL-
-------
TABLE 11. (Continued)
SJ
o
U)
676
677
678
679
6*0
681
68Z
683
68<>
665
686
687
688
689
690
691
69Z
o93
69«
695
696
697
698
699
700
701
702
703
70<«
/05
706
707
708
709
710
711
71Z
713
71*
715
7 It,
717
718
719
720
COMMON NAHE
FINAL *£PO«T (PART II
RELATIVE SIZE A NO CONCENTRATE NNERE DETECTED
V V
1 1
c x
TTTTTTMNPPOOSSL
211 1I.I.222222222
BCXYCXCCCXCXCXM
c c
1 2
N N
R R
1 2
C C
E 0
1 Z
C N
PAGE 16
B B
2 3
C C
CYCLOHEXYL METHYL KETONE
P-ISOPROPYLBENZALDEMYOE! CUMINALOEHYDE
2.3 5.6-OI-O-ISOPROPVLIOENE-ALPHA-O-TALO
1-TERT-BUTVL-t-ETHOXYBENZENE
S-HETHYL-H3HI-XSOBENZOFURANONE
9-OCTAOECENAL
li-MErMYL-3-HEPTEN-2-ONE
6-METHOXY-Z-METHYL-3-HEXANONE
2.6-OIMETHYL-3-HEPTANOL
Z-<2-HETHOXY-l-HETHYLETHOXY»-l-PROPANOL
AHYL BUTYL PHTHALATE
2-ETHYL-2-IS06UT \TL-t, 3-D 10KOLANE
P-ll-HYOROXY-l-METHYLETHYLIACETOPHENONE 0
2tZt6-TRIH£THVLCYCLOHEXANONE
2,3-OIHETHYLBUTVRIC ACID
OICHLOROISOPROPVL ETHER
PENTACHLOROCYCLOPROPANE
2.3-OCTANEOIONE
l-CTMYL-J.i •OIMClHYLOCLOHiKANE
<, I
it 21.1.332220
Z «3
-------
TABLE 11. (Continued)
PAGE IT
722
723
725
726
727
728
729
730
731
732
733
731.
735
736
737
738
739
71,0
7it3
71.5
71,6
71.8
71.9
750
751
752
753
75it
755
756
757
754
759
760
761
762
763
76
-------
TABLE 11. (Continued)
PAGE 1»
COMMON NAME
FINAL REPORT IPART II
RELATIVE SIZE ANO CONCENTRATE WHERE DETECTED
766
7 *, 7
• O f
760
7 to
f O 7f
770
771
772
773
7 7 it
r f H
775
776
777
778
779
780
7 A 1
• O 1
78Z
783
78*
785
786
787
788
789
790
791
79Z
793
79",
795
796
797
798
799
800
801
80Z
803
80",
805
806
8 07
808
809
8 10
ACETYL IS08UTYRYL
OCCAL I N
l.Z-OIHETHYLCVCLOHEXENE
nf |^| y yi TRI HE TH YL.ENE
i.-METHOXY-1-BUTANOL
3,"»-£POXY-3-£THYL-Z-BUTANOhE
" 7 01 HE TH YLQCTAMC
3,i,-OIHYORO-Z,5-DIM£THYL-ZH-PVRAN-Z-CA*B
N-BENZOYLGLYCINE. METHYL ESTER
CUMENE ISOPROPYL ETHER
2-ISOPROPYL-l. 3-OIOXOLANE
1-OXIRANVLETHANONE
6,b-OIh£THYL-J,<.-UNOECADIENE-Z, 10-01 ONE
TEREPHTHALIC AGIO
l-METMYL-<.-U-METHYL-Z-BUT£NYL»NAPHTMALE
CYCLOPENTYL BROMIDE
Z,2-DICHLORO-3-HETHYLBUTANE
•4*OIPHENVLAMINE
3-HYOROXY-3-METHYL-Z-BUTANONE
METHYL PENTAOECANOATE
METHYL PALMITATE
METHYL ISOPALMITATE
OIBENZOFURAN IOIPHENYLENE OXIOEI
Z.Z-DICHLOROBUTYRIC ACID
Z-ETHYLHEPTANOIC ACID
i>*CHLOROPHENYL ACETATE
Z.3.I..6-TETRACHLOROPHENOL
1-CHLORO-Z -ETHYL BENZENE
PERCHLOROETHANE
1-BROMO-Z-ETHYLBENZENE
CHLOROVINYLBENZENE
Sl,Zi3-TRICHLOROBENZENE
3,5-DIBROMOTOLUENE
I1.Z-OICHLOROETHYLI BENZENE
XH-CHLORONITROBENZENE
•Z,i«-DICHLORONAPHTHALENE
CYCLOPENTENE
X •»M-OICHLOROBENZENE
!•-• »SNITRQBENZ£NE
l-CHLOROTRICYCLOm.3.1 .13. aiUNOECANE
DECA ME THYLCYCL OPEN TASILO KANE
Z-CHLORO -1,3, 5-TH METHYL BENZENE
1-CHLORO-ZCPHENYLETHYN YD BENZENE
1 1 Z 1 1 1 <>
C X 8 C X Y C
3 1
11 3«
Z Z Z* 3*
0 3
1 3
Z 3
3
3
3
3
3
3
3
3
3
3
3
3
3
-I
TMNPPODSSLC
<>ZZZ2Z2ZZZ3
X C C C XCXCXHC
3
3
3
3
3
j
3
3
3
3
3
3
3
3
3
0 Z 0 Z 1 Z 1
Z3 13Z1ZO
0* 3* 0*
0
1 Z
3
1
-I 0
3 1
Z
0 1
Z
CCCRREDBB
1 1 Z 1 Z 1 Z Z 3
MNNCCCNCC
j
Z
3
3 Z
1
Z* Z*
3
Z
1
Z 1
3
(Continued)
-------
TABLE 11. (Continued)
PAGE 19
COMMON NAME
FINAL REPORT (PART II
RELATIVE SIZE AND CONCENTRATE WHERE DETECTED
811 2-NETHYLBENZOTRIAZOLE
812 XETHYLENE GLVCOL. BIS12-CM.OROETHVLI ETHE
813 CYCLOOODECANOL
3 I". DIMETHYL SUBERATE
815 METHYL SUCCINATE.DIMETHYL ESTER
816 N-HETHYL ETHENAMINE
917 XHEPTANOIC ACID.ETHYL ESTER
818 2-(2-CHLOROETHOXVIETHANOL
819 UNOECANOIC ACIO.METHYL ESTER
820 XBENZENEACETIC ACID,ETHYL ESTER
821 METHYL P-ETHVLBENZOATE
822 XCLOFIBRATE
823 X9H-FLUOREN-9-ONE
82>< Xl-METHYL-2,«,-DINITROBENZENE
825 2.<>-DICHLOROPH£NOXY ACETIC ACID. METHYL
826 METHYL ISQNONANOATE
827 XETHYL CAPRYLATE
828 2-KETOPENTANEDIOIC ACID. DIMETHYL ETHER
829 CLOFIBRIC ACIO,METHYL ESTER
830 METHYL ISOTRIDECANOATE
^j 831 ETHYL 7-KETHYLMVRISTATE
O 832 METHYL PENTACOSANOATE
°^ 833 1-HEXANOL
838 2.<,.6-COLLIOINE
8«,9 3,i,,i,-TRIMETHYL-2-CYCLOHEXEN-l-ONE
850 2-PHENYL ACROLEIN
851 1-METHYLISOQUINOLINE
852 2-3-OIMETHYL QUINOLINE
853 DIDEHYOROGENATEO ABIETIC ACIO
851, XtPHtNANTHRENE
855 1,2-BENZISOTHIAZOLE
\l
c
0
X B C X
)
0 3
223
3 3
2 3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
1 it >t 2 2 2 2
V C X C C C X
3
3 3
3
3
3
3
3
3
3
3
3
3
3
3 0
3
3
3
3
3
3
3
3
1 *
3
2
0 2
3
2
1
0 1
0
0
-1
1
0 0 S S
2222
c x c x
L C
2 3
H C
C C
1 I
R R
1 2
N N C
B B
2 3
C C
1* 2*
1*1*
3*
2 2
2* 0*1*
2*
3
2 1
1
2 2
2 2
2* 3*
3*
1* 3* 3 *
3* 1*
(Continued)
-------
COMMON NAME
TABLE 11. (Continued)
FINAL REPORT (PART II
RELATIVE SIZE AND CONCENTRATE MHERE DETECTED
PA&d 3D
856
857
858
859
860
861
862
863
86<«
865
866
867
868
869
870
871
872
873
87<>
875
S76
S •"
^j 874
879
880
881
862
883
86<*
885
866
ft A 7
O o /
888
889
690
891
892
893
89<.
895
896
897
898
899
900
.
* C X B C *
N-PROPYL-1-HEXANAHINE -1
1.2-DIHYORO-I.-PHENYLNAPMTHALENE a 3
M-OIETHENVLBENZEKiE A 31
1-PHENYL-3-BUTEN-2-ONE a 3
BUTYLATEO HYOROXY TOLUENE IBHTt 1 I
ACETtLOEHYOE OIETHYL ACETAL -1
7-METHYL-3I2HI-BENZOFURANONE -1
NEOPENTYL ALCOHOL 1
3-7.11-TRIMETHYL-3-OOOECANOL 3
2.2*-BI-1.3~OIOXOLANE 3
N-PROPOXY ETHANOL 3
ALPHA-PICOLINE 2
ISOV&LERAMIOE 2
tO-CHLORO PHENOL
I01-N-PROPYL PHTHALATE
X ••Z.'.-OIMETHYLPHENOL IXYLENOLI
PSEUDOCUMENE
1-INDANONE
OCTAOECANOL
COTININE
TETRtETHYLENE CLVCOL OINETHYLE THER
1,1.,6-TRIMETHYL NAPHTHALENE
HENTHONE
5-ETHYLOIHYORO-2(3HI-FURANONE
VERATRALOEHYDE
TRIETHYLENE CLYCOL. DIMETHYL ETHER
<>,<>-OIMETHVL-2-PENTENOIC ACID
J.-OCTENOIC AGIO
ZCHLOROACETONE
7-NONENOIC AGIO
2,6-OIMETHYLHEPTANOIC AGIO
j t Q j **£• THVI HCNANE
VINYL ACETATE
XHALONIC AGIO
1.-METHYLPHENYLPENTANOIC AGIO
fISOBJTYL METHYL PHTHALATE
ISEC-BUTYL METHYL PHTHALATE
HETHYL METHOXVMETHYL FORMAL
XM-CHLOROANILINE
9-OOOECENOIC AGIO
2.3. 3-TRIMETHYL-3H-INOOLE
2,5-OI-T-AMYL QUINONE
XTETRAMETHYLUREA, TMU
P-METHYLANISOLE
AL PMA - MET HYL-ALPHA -ACE T YLOXY BENZENE ACE T I
Sit FOOTNOTE ON LAST PAGE
1^^2222222223112121223
YC xccc XC*CXN:NNNCCCNCC
2 3*
2* 0*
3» 3.
2*
2 21 312111
3
3 3
3
3 5
3
2 3
3 3
00 3
0 221 2 1 3 2 Z 1 1
2 3
2* 3* 2*
1 1 3
03 3 23
2 0 3
3 3
2 3 13
32 3
3 3 2
1 3
2 3
3 3
2 32
1 332 1
3
3
J
3
3
3
3
3
3
3 I
3 2
Z 3
3
(Continued)
-------
TABLE 11. (Continued)
PAGE 21
COMMON NAME
FINAL REPORT (PART II
RELATIVE SIZE AND CONCENTRATE WHERE DETECTED
ro
o
oo
901
902
903
900
9m
91.2
9
9>,5
2(5i 8-TRINETHYL-l-NAPHTHOL
2,5-DIHETHVL STYRENE
1-I3-BUTOXYPROPOXYI-2-PROPANOL «A OIPROP
3-METHYL PHTHALIDE
BUTYL H-TOLYL SULFIDE
TETRAHYOROPVRAN-2-HETHANOL
S^C"TM¥ i — Ai. •MFTH VI HFMAUF
c f ft T t *i ™nc I H TLnc. K ANC.
2-NORBORNENE-7-OL
2-HEXENAL
2(6-OIMETHYL-2-HEPTEN--HETHVL-3-CYCLOHEXENE-l-CARBOXVLIC ACID
2-ETHYL-2-HETHVLBUTYRIC AGIO
<»-METHYL-2-PHENYLQUINOLINE
1-(PHENYLHETHYL»ISOQUINOLINE
lt2.i>-TRIHETHVL-l>3-OIAZOCYCLOHEX-l-ENE
1-ACETYL-lf 2i3.<»-TETRAHYOROPYRIOINE
VINYL CYCLOHEXYLFORMATE
DIETHYLENEGLYCOL. CYCLOHEXVL ETHER
ISOINOOLE-1.3-OIONE
2-ETHYL-3-HETHYL-2-BUTENEOIOIC AGIO
TRICOSANOIC AGIO
NONACHLOR
3-ETHOXY-1C3HI-ISOBENZOFURANONE
2-ISOPROPVLTHIOPHENE
3-(2-HYOROXYPROPVLI-5-METHYL-2-OXAZALIOI
3-METHYLOCTAHVOROPENTALENE-t-CARBOXVUC
it-HYDROXY-OCTAHYORO-1-NAPHTHALENONE
2.2-OIMETHYL-3-I2-METHYL-1-PROPENYLICYCL
-nENZOTHIAZIN-3-ONE
8-NONENE-2-ONE
CXBCXYCXCCCXCXCXHCMNNCCC'NC
3
3
)
3
3
3
3
3
]
3
3
3
3
3
3
2
3
3
3
2 3
3 2
3
3
3 3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3 2
3*
a
3
C
3
3
3*
(Continued)
-------
TABLE 11. (Continued)
PAGE 22
ro
o
COMMON NAME
906 OOOECANEOIOIC ACID
9*7 P-BROHOBENZOIC AGIO
9<.l 2,9 aENZENE
963 1-METHYL INDAN
96". 1-ETHYL INOAN
965 1-METHYL-1.2-DIPHENYLETMANE
966 6-METHYL TETRALIN
967 2.3.I.-TRIHETHVLBENZOIC ACIO
964 2-NETHYL-2-NONEN-1.-ONE
969 XCHLOROACETIC ACIO
970 P-OIISOPROPYL BENZENE
971 1-HEPTENYL8ENZENE
972 2.3,6-TRIMEIHYL BENZOIC ACIO
973 3-METHYL-2.2-OIOXIOE-IH-2,1,3-BENZOTHIAP
97«, ISOPROPVL ACETATE
975 .BETA.-OXO-BENZENEACETIC ACIO. ETHVL EST
976 l,3-DlHVORO-2.2-DIOXIOE>2,l,3,BENZOTHlAO
977 METHYLISOBUTYL BENZENE
97« SEC-BUTYL ALCOHOL
979 3i5,5-TRIMETHYL-2l5H)-FURANONE
960 2-PROPYLCYCLOHEXANONE
9«1 5-MErHYL-5-PHENYL-2-HEXANONE
982 TETRAHETHYLBENZENE PROPANOIC ACIO
981 2.2-OIMETHYLPROPANOIC ACID. 2, I. ,6-f RIMET
98<, 6-UNOECANONE
985 2.6-OIMETHYLCYCLOHEXANOL
986 HEXAH»ORO-3-(2-PROPENYL»-2H-AZEPIN-2-ONE
987 K2.6-DIHYOROXY-<.-MErHOXVPH£NYL)ETHANONE
988 XHANOELIC ACIO
989 (2-CMLORO-2-PROPENYL»OX»8ENZENE
990 DECYL VINYL ETHEK
" Sit FOOTNOTE ON LAST PAGE
FINAL REPORT (PART I)
RELATIVE SIZE AND CONCENTRATE WHERE DETECTED
11211
* C X 8 C X
a 11
A 1
A 0
A 1
0
A -1
A 1
A
d
1<>'>22222
rcxcccxc
3 * 0*3
1 * 1*3
0 « 3
1 * 2*3
2 * 1*
3*
3*
2 3»
2 3
3 3
2 2
2 3
2
3
3
3
3
3
3
3
3
3
3
3
3
3
3
0 S
2 2
X C
3*
0
1
3
3
3
3
3
-1
3
2
3
3
3
3.
SLCCCCRREOBB
223112121223
XMCMNNCCCNCC
3
3
3
3
3
3
3
3
3
3
3
3
3
1
0«
2 1
1
(Continued)
-------
TABLE 11. (Continued)
PAGE 23
COMMON NAME
FINAL REPORT (PART I)
RELATIVE SIZt AND C3NCENTRATE NHERE DETECTED
V V T T T
11211
* c x a c x
T T
1 <•
Y C
991 .ALPHA.-HYOROXY-.ALPHA.-METHYL BENZENE A
992 ".-BUTVL-1.3-CYCLOPENTANEDIONE
993 PHTHIOCOL
99<> P-ISOBUTVLTOLUENE
995 XORCINOL
996 OI8UTYL-3-METHYLGLUTARATE
997 7-METHYL-7-HEPTAOECANOL
998 CVCLOHEXVL CHLORIDE
999 1-PHENVLNAPHTHALENE A
1000 2-PHENVLNAPHTHALENE A
1001 2-ETHYL TETRALIN A
1002 X2-METHYLANTHRAQUINONE a
1003 6-TRICHLOROANILINE -1
1029 2,".-DIMETHYL HEXANOIC ACIO
1030 1-ETMYL-3-METMYL BENZENE
1031 1,6 DIMETHYL-<»-ISOPROPYL-NAPHTHALENE
1032 1,2.3-TRIHETHVL BENZENE
1033 1-13,3-OIMETHVLOXIRANYLIETHANONE
103<> -OIMETHYL-l,3-OIOXANE
1035 X3,<.-OICHLOROPH£NOXVACETIC ACID
* SEE FOOTNOTE ON LAST PAGE
M
2
C
N
2
C
P
2
C
F
2
X
0
2
C
0
Z
X
3
S
2
C
S
2
X
L
2
H
C
3
C
C
1
H
C
1
N
C
2
N
R
1
C
R
2
C
E
1
C
0
2
N
6
2
C
B
3
C
2
1
1
1
-1
0
2*
2*
3*
3*
3*
3*
3*
3*
3* 2
3*
3*
3* 1
3*
3*
3*
3*
3
3*
3
I
323 2
3
3
0*
2*
0
2*
2*
2*
2*
2*
1
2
0
0*
1*
0*
2
3
3
3* 2*
3
3
3 2
3 2
3
3
3
1*
Z 1
2 1
2 2
t*
2 1
0
(Continued)
-------
TABLE 11. (Continued)
PAGE 2+
COMMON NAME
FINAL REPORT (PART II
RELATIVE SIZE AND CONCENTRATE WHERE DETECTED
1036 OOOECAHETHYLCYCLOHEXASILOXANE
1037 Z2t6-OIHETHYLNAPHTHALENE
103« XO-CHLORONITROBENZENE
1039 XICSITYLENE
10
-------
TABLE 11. (Continued)
PAGE. 25
COMMON NAME
FINAL RECOIU (PART II
RELATIVE SIZE AND CONCENTRATE HHESE DETECTED
VVTTTTTTMNP
1121tlt»<»2Z2
CXBCXYCXCCC
POOSSLCCCCRREOBB
Z2Z2223112121223
XCXCXHCMNNCCCNCC
1061
loez
1063
108<.
1065
1086
1067
1086
1089
1090
1091
1092
1093
109<<
1095
1096
1097
1098
1099
1100
11 01
1102
1103
HO't
1105
1106
1107
1108
1109
1110
1111
1112
1113
4 4 | j.
A i AH
1115
1116
1117
1118
1119
1120
1121
1122
1123
1121,
1125
TETRAPROPYLENE CLYCOL METHYL ETHER
•.-CHLOROCROTONIC ACID
M-DI-SEC-BUTVLBENZENE
P-D1- SEC-BUTYL BENZENE
X2-METHYL-2-PHENYLOXIRANE
6,6-DIMETHYL-Z,S,10>UND£CANETRIONE
2-MtTHVL-2-CYCLOPENT£N-l-ONE
3 ,<>-OIHETHYLBENZ ALDEHYDE
SETHYLBENZENE
3-BROHOHEPTANE
N-BENZOYL-L-ALANINE. METHYL ESTER
ItltZ-TRICHLORO-l-PROPENE
2-ETHYLACETOACETIC ACID
5-METHYL-3-HEXEN-2-ONE
<.,i»-DIHETHYLHEXANAL
TETRAHYORO-2H-PVRAN-2-ONE
2-OECANOL
2.5-DICHLORO-4-HETHYLBENZOIC ACID
1-NAPHTHOIC ACID
2-CHLORO-3-HETHVL-2-BUTENE
•»tPENTACHLOROBIPHENYL » OTHER PCBS
2,<,-OICHLOROPENTAN£
3.6-DIHETHVL-3-HEPTANQL
l-ETHOXY-2-HEPTANONE
3-CYCLOHEXYL-<.-PENTEN-2-ONE
3-METHYL-1.2.<>-CYCLOPENTANETRIONE
3-ETHOXYPROPANAL
1-«1-CYCLOHEPTEN-1-YL)£TH»NONE
<•,«., 5, 5-TETRAHETHYL-2.7-OCTANEOIONE
XBETA-CITRONELLOL
3-ETHYL-i»-METHYL-3-PENTEN-2-ONE
-------
COMMON NAME
TABLE 11. (Continued)
FINAL REPORT (PART II
RELATIVE SIZE AND CONCENTRATE WHERE DETECTED
PAGE 36
1126
1127
112*
1129
1130
1131
1132
1133
11 3".
1135
1136
1137
1138
1139
HdO
11 1.1
11 1.2
11 1.3
11<><>
11 ">b
11 <>6
1 1 1* 7
!!<,«
111.9
1150
1151
1152
1153
11 51.
1155
1156
1157
1168
1159
1160
1161
1162
1163
lib-.
1165
1166
1167
1168
11 69
1170
11211
c x a c x
CYCLODECANOL
1-IETHNYLOXYIPENTANE
CIS-J.1.-OIMETHYL-3-HEXEN-2-ONE
PHENYLBUTANAL
CIS-5-BUTVLDIHYORO-d-HETHYL-Z(3HI-FURANO
2,6-OIISOPROPYLPHENOL
ALPHA-FARNESAL
3A,ii(Sl7A-TETRAHVORO-d-HYOROXY-3Ai7A-DIM
BUTYL CYANATE
ETHYL AMVL KETONE
J.8-NONAOIEN-2-ONE
3A,d.7,7A-TETRAHYORO-2-PROPYt.-lH-ISOINDO
2-HEXEN-1-OL
ISOCYANOETHANE
•.-PENTEN-2-OL
3-CHLORO-3-BUTEN-2-ONE
I2-IPENTYLOXVI ETHYLICYCLOHEXANE
2.I.-OI-TERT-BUTYLPHENOL
2-CHLORO-2-PSOPENOIC ACID
BETA-RESORCYLIC ACID
P-NITROBENZOIC ACID
HEPTANE
TETRAHYOROFURFURYL ALCOHOL! THFA
LOLIOLIOE
K" »»FLUORANTHENE -2
METHYL HEPTAOECANOATE -1
XPROPIOPHENONE 0
(1-NITROETHYL) BENZENE 1
2.3.1..5-TETRACHLOROANILINE 1
2-METHYL-l-NAPHTHALENOL
2,3-OICHLOROBUTENE
1-BRONO-2-CHLORO-2-BUTENE
2. i.-DICHLORO-1-ICHLOROMETHYLI BENZENE
1,2-0 1 CHLORO-i,- ( CHLOROMETH YD BENZENE
X»9M-FLUORENE
P-BRQHOTOLUENE
1,2-D I CHLORO- 3 -NITROBENZENE
2-CHLORO-P-CYMENE
2-CHLDRO-l-«".-ETMYLPHENYL> -2-METHYL-l-PR
*X'tLINOANE
METHYL OICHLOROACETATE
XURETHANE (ETHYLCARBAMATE)
<.-CHLOROPHENYL ACETIC ACID. METHYL ESTER
HETHVL ANTEISOPENTAOECANOATE
P-CHLORO-2-N1TROAN1L INE
1 «. d
Y C X
2 0* 0
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2 1
2
2
2
HNPFOOSS
22222222
CCCXCxCX
2
2
2
2
2
2 2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
^
2
2
1» 1 -1
1
1
1
0
2 10
1
2
LCCCCRREOBB
23112121223
NCMNNCCCNCC
Z
|
1» 2* 1*
1 22 2
1
2
(Continued)
-------
TABLE 11. (Continued)
PAGE 27
COMMON NAME
1171 2,4-D. ETHYL ESTER
1172 ALPHA-KETOGLUTARIC AGIO
1173 METHYL PROPENYLOXY KETONE
117<» 3.<>.5-TRIMETHYL-2-CYCLOPENTEN-l-ON£
1175 XETMYLENE GLYCOL
1176 GAMMA-PICOLINE
1177 2.5-LUTIOINE
1178 2,3,6-TRIMETHTLPYRIOINE
1179 5-ETHVL-2-PICOLINE
1160 2,3,1,-TRIMETHVLPVRIDINe
1181 2,<,,S-COLLIOINE
1182 2-ETHVL-6-PICOLINE
1183 <•.<•. 5-TRIMETHYL-2-CYCLOHEKEN-i-ONE
118<« XQUINOLINE
1165 XQUINAIOINE
1186 OIPROPYLENE GLYCOL
1187 2-I1-METHYL-2-PIPERIOINYLI-PYRIDINE
1188 ABIETIC ACID
1189 METHYLOCTAOEC-10-ENOATE
1190 HETHVL-9.11-OCTADECAOIENQATE
1191 M-METHOXYPHENYL ACETATE
1192 2-METHYL TETRALIN
1193 2 2 2
cxvcxccc
2
2
2
2
2
2 0
2
2
2
2
2
2
2
2
2 1
2 1
2
2* 1
2
POOSSLCCCC
22222Z3112
XCXCXHCHNN
2 2
R R E 0 B B
121223
C C C N C C
2*
2*
2*
1*
1 2
-1
2 0
2 1
0
-1
(Continued)
-------
TABLE 11. (Continued)
Pft&t Z»
COMMON NAME
FINAL REPORT (PART II
RELATIVE SIZE AND CONCENTRATE WHERE DETECTED
1216 3,5, 5-TRIMETHYLCYCLOHEX-3-EN-1-ONE
1217 2.3.I.-TRIHETHYL-2-CYCLOPENTEN-1-ONE
Hit 1.6-OIHETHVLNAPHTHALENe
1219 <<-PHENYLBICVCLOHEXYL
1220 X» HHEXACMLOROBENZENE
1221 K3.5-OICMLOROPMENOL
1222 0-ETHYL TOLUENE
1223 "..7-OIMETHYL8ENZOFURAN
122<« 1,3,6-TRIHETHVLNAPHTHALENE
1225 6-NETHYL-3.5-MEPIAOIEN-Z-ONE
1226 2-NETHYLCYCLOPENTANONE
1227 1-ACETYLPIPERIOINE
1224 5-ETHENYL TETRAHVDRO-.ALPNA.,.ALPHA.,S-T
1229 2,'.,5, 7-TETRAMETHYLPMENANTMRENE
1230 DIPROPYL CARBINOL
1231 XCUAIACOL
1232 8-NONENOIC ACID
1233 METHOXYNAPHTMALENE
1231, 3,3,1,-TRIMETHYLOECANE
1235 2-OCTYLPHENOL
1236 l,3,5-TRICHLORO-2-HETHOIIYaENZENE
1237 OIHETHYLNAPHTHALENE
1234 HETHYL «.-BUTOXYBUTYRATE
1239 »TRI-M-CRESYLPHOSPHATE
121 TRANS-2-ETHYL-3-PROPVLOXIRANE
12<>2 PENTACHLOROPYRIDINE
12<<3 2, J.".-TRIM£THYLOXETANE
12^'. 2,5-OIhETHYL THF
1?".5 <,-BROMO-3-PHENYLSYONONE
12".6 3.6-OIMETMYL-5-ISOPROPYL-1.2-NAPHTHOQUIN
121.7 CHLOROIOOONETHANE
12<.» l-METHYL-".-«l-METHYLETH£NYLI-CYCLOHEXENE
12<.9 l-(2-BRONOETHYLI-<»-CHLOi{OBENZENE
1250 3,5,6-TETRAN£THYLPHENANTHRENE
.1251 (Z-BROMOCYCLOPROPYLI BENZENE
1252 OCTAHYOROAZOCINE
1253 PIPERIDOHE
125
-------
TABLE 11. (Continued)
PAGE 29
COMMON NAME
FINAL REPORT IPART I»
RELATIVE SIZE »ND CONCENTKATE WHERE DETECTED
1361
1262
1263
126<>
1 ? fifi
1 C O9
1266
1267
1268
1269
1270
1271
1272
1273
1271.
1275
1276
1277
1278
1279
1280
1281
1282
1283
128<«
1285
1286
1287
1288
1289
1290
1291
1292
1293
129t
1295
1296
1297
1298
1299
1300
1301
1302
1303
130i6-OIM£THYLNONANOIC AGIO
OIMETHYLFLUORENE
1,2,3,1,-TETRACHLOROBUTANE
2t2-DIMETHYL-lt3-CYCLOPENTANEDIONE
5-OODECANONE
X2.6-OIMETHYLQUINOLINE
TETRAPROPYLENE GLYCOL
N-ETHYL-2-BENZOTHIAZOLAMINE
OIHETHYLCYCLOHEXANE DIONE
2,2,<.-TRIHETHYL-lt3-PENrANEOIOL
2,2,5,7-TETRAMETHYL-li.S-OCTAOIENE-3-ONE
1.2-QIAZA8ICYCLOI2.2.2.10CTAN-3-ONE
Z-METHOXY-10-UNOECENOIC ACID
CETENE
1-OCTAOECENE
l-PROPOXY-2-PROPANOL
5-HETHVL-5-ETHYL-2t<>-OXAZOLIOINEOIONE
BROMOCHLOROBENZOIC AGIO
16-HYDROXY PALMITIC ACID
P-AMINOBENZENE-T-BUTYRIC AGIO
BAR8ITAL
TRIMETHYL-6-VINYLTETRAHVDROPVRAN>3-OL
5,5-OIMETHYLFURANONE
5-HEPTEN-2-ONE
N-METHYL-2-PIPERIOINONE
3,i«Z22222Z223112121
*CXBCXYCXCCCXCXCXH:M^NCCC
2
2
2
2
1
e
2
2
2 2
2
2
2
2
2
2
2
2
2
2
2
2
A i 2* 2* 2*
0 2
0 2
A -1 2* 2* 2*
At 2*
All 12
1 2
t 2
1 2
A 0* 2*
1 2
DBS
223
N C C
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
* SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
COMMON NANE
TABLE 11. (Continued)
FINAL REPORT IPART II
RELATIVE SIZE AND CONCENTRATE NHERE DETECTED
PACE 30
1306
1307
1301
1309
1310
• ft.
A J 1 I
1312
1313
1311,
1315
| » « t
1 J 1 D
1317
1316
1319
1320
1321
1322
1323
1321,
1325
1326
1327
1328
1329
1330
1331
1332
1333
I33i>
1335
1336
1337
1)38
1339
131,0
131.1
111.2
131.3
131,1,
131.5
131.6
131.7
131.8
131,9
1350
•
1
* C
1.1-OIHETHVL INOENE
2-PENTENOIC ACIO
CLOFIBRIC ACID. M-CHLORO ISOMER
7-OXO-OCTANOIC ACIO
1,2.3,3A-TETRAHYORO AZULENE
? _ f, — fl T HF TM tf 1 fiPTAtJF
E TV wa nt m VL vv frdWt
6-METHVL-aiCVCLOC-PENTANEOIONE
2-METHLV-S-ISOPROPVLCYCLOHEXANONE
2-BUTVL-2-OCTENAL
3.3-DIMETHYL-2UHI-FURANONE
3-HVOROXY-2t
-------
TABLE 11. (Continued)
PACE 31
COMMON NAME
FINAL REP04T (PART II
RELATIVE SIZE AND CONCENTRATE WHERE DEJECTED
1351
1352
135
1365
1366
1367
1368
1369
1370
V V T T T
1 i 2 1 &
* C X B C X
5-METHYL TETRALIN
2-PROPYLHEPTANOIC ACID
0-ISOPROPYLBENZOIC ACID
l-METHYL-2-CYCLOHEXEN-l-OL
4-ETHYLPYRIDINE
X1.3.6-TRINETHVL-2,l>llH.3HI-PVRInIOINEDIO
XCAPRALOEHVOE
3»i,6-TRIHETHYLBENZALDEHYDE a
M-ANISALOEHYOE
DIBROMOCYCLOHEXENE
HETA-CYHENE (H-ISOPROPVL TOLUENE)
2-KErO-3-HETHYL VALERIC ACID
5-HEXENOIC ACIO
3,3-OIMETHYLBUTYNE
SEC-ISOAMYL ALCOHOL
7-OCTEN-I.-OL
T T T H N
V C X C C
1
2
2
•«
2
2
2
2
2
2
2
2
2
2
2
2
2
2
•»
2
2
2
2
2
2
2
2
2
2
2*
2
2
PPOOSSLCCCCRREOBB
2222222311 2121223
C XCXCKMCMNNCCCNCC
2 0
2
2
2
2
2
2
2 0
1
11 1
1 01
-1 1
1
0 -1 111
1 1 I
1
0
1
1 0
01 1
1
1
1
1 1
1
M 1372
0° 1373
137".
1375
1376
1377
1378
1379
1360
1361
1362
1363
136't
1365
1366
1367
1361
1369
1390
1391
1392
1393
139<»
1395
* SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE 11. (Continued)
PAGE. 32
COMMON NAME
FINAL REPORT (PART II
RELATIVE SIZE AND CONCENTRATE WHERE DETECTED
V V T T f T
1 t Z 1 I I
* C X B C X Y
1396 Z-METMYLCYCLOPENTANOL ACETATE
1397 2.0-OIISOPROPYLPHENOL
1398 ETMYL «.-HYDROXYPHENYLACET»TE
1399 TRIETHYLENE tLYCOL. PHENYL ETHER
mOO 2-ETHYL-3-PROPYLOXIRANE
IsOl OHU (DIMETHYL UREA)
1".OZ P-d-ETHYLPROPYLJTOLUENE
11.03 Z-METHYl-1-DQOECANDL
l«.0i. Z-METHYLENE-1-BUTANOL ACETATE
ItOS TETRAHYOROFURFURYL ACETATE
1",06 5-HETHOXY-Z-PENTANONE
1<.07 S-(ACETVLOXYI-Z-PENTANONE
11.08 PINACOL
11.09 1.1-OINETHOXYCVCLOHEXANE
1-.10 HETHYL 3.6-OIHYDRO-<>f5-OinETHYL-ZH-PYRAN
1<.11 5-NONANOL
1«.IZ 1-TERT-BUTOXY-Z-HETMYlCYCLOHEXENE
11.13 0-ISOPROPYLACETOPHENONE
li.li. NONYLPHENOL
1<.1S XZ-FUROIC AGIO
Islb CROTONYLBENZEME
mi7 ALLVLACETONE
K.18 SPIROOOOECANE
11.19 1-PHENYL-l.Z-PROPANEOIONE
IsZO 1-IBROMOMETHTL >-<.-MErHYLBEK!ZENE 1
IsZl P-CHLOROANISOLE
H.ZZ 1,Z,*,5-TETRACHLOROBEMZEME
Is?3 (1-CMLOROETHVLIOIHETHYLBENZENE
m?.Zb »$TETRACHLOROBIPHENYL
11.27 MPENTACHLOROalPHENYL
1I.Z8 3-HEXYL BROMIDE
1<.29 1.1.2-TRICHLOROPROPANE 1
1<.30 5,8-DIMETHVLQUINOLINE 1
1<.31 2,3,5-COLLIDINE 1
m3Z ".-ETHYL-Z.b-DIMETMYL PYRIOINE 1
1«.J3 3-ETMYL-2.I..5-TRINETHYL-1M-PYRROLE 1
1<.3<. XZ.I.-OIMETHYLQUINOLINE 1
1I.3J HETHYL OLEATE 1
l-3b 9.1Z-OCTAOECAOIENOIC AGIO 1
11.37 I.-ETHENYL BENZOIC acia A i
11.38 <.-HVOROXYAC£TOPHtNON£ 1
11.39 1-NAPHTHALENOL 1
1<.<.0 DIETHYL PHENOL , (UNKNOWN ISOMER) 1
• SEE FOOTNOTE ON LAST PAGE
TTMNFPOOSSLCCC
(>
-------
1<,<.1
H.50
1".51
11. 5".
1".56
11.57
11.58
11,59
H.60
1-.61
ti.62
H.63
11.65
li,66
f.67
11,68
11.69
11,70
H.71
11,72
Iit73
11.71.
11,75
1476
11,77
1-.78
1<<79
1-.80
11.81
11,82
11.83
COMMON NAME
TABLE 11. (Continued)
FINAL REPORT (PART II
RELATIVE. SIZE AND CONCENTRATE HHERE DETECTED
11.85
2-ETHYL*li<»-DIMETHYL BENZENE
l,2.t-TRIHETHYLNAPHTHALENE «3,i»,5-TR
1,6-OICHLORO-l.S-CYCLOOCTAOIENE
1,5,8-TRIHETHYL TETRALIN
OURENE
TERT-BUTYL BENZENE
1.,6-DIMETHYL PYRIMIDINE
2.3*DIHETHYL PYRAZINE
PYRAZOLE
l-HETHYL-3-PROPYL BENZENE
N-PROPYLNAPHTHALENE
TRIHETHYLNAPHTHALENE
TRINETHVLNAPHTHALENE
TRIHETHYLNAPHTHALENE
TRIHETHYLNAPHTHALENE
TRIHETHVLNAPHTHALENE
TRIMETHYLNAPHTHALENE
TRINETHYLNAPHTHALENE
X»ANIHRACEN£
TRIOECANE
T T T
B C
HETHOXYBENZENE 1
2,2-DIMETHYL-l.l-BIPHENYL A 1
ALPHA-HYDROXV-ALPHA-PHENYL PHENYL ACETIC 1
1-NETHYL ANTHRACENE 1
<»-HETHYL-3-HEPTANONE 1
HETHYL PROPIONATE 1
P-NETHYL ACETOPHENONE a 1
2X,<»*, 6X-TRIHETHYLACETOPHENONE a 1
1-T-8UTYL-3-ETHYL-5-HETHVL BENZENE A 1
2-ALLYL BENZOATE a 1
1-HETHOXYETHYL8ENZENE a 1
QUINOXALINE 1
ETHYL HARGARATE A 1
BENZOPHENONE a 1
X*PYRENE 0 1
7-ETHYLQUINOLINE 0
2-ETHOxr8UTANE 1
HVOROGENATEO ABIETIC ACID 1
1-ETHYL'HETHVLCYCLOPENTANE 1
XtCUHENE 1
BENZtLDEHVOEOXlHE 1
HETHYL PALMITOLEATE 1
X+ACENAPHTHALENE
1-METHYL-I.-PROPYLBENZENE
THNPPOOSSLCC
I.22222222Z31
xccc XCXCXHCN
-i
i*
i*
-t
i i
0
-I
R R
1 Z
N N C C C
PAGE 33
B B
2 3
C C
1*
1*
1* 0 * 0 *
1
(Continued)
-------
COMMON NAME
11.86 3-NETHYL-3-HEXANOL
11.87 OIETMYLMETHYLVINYLSILANE
K.88 1,1-OISOPROPYL BENZENE
l",89 TETRAHYOROLINALOOL
11.90 2-PHENYL-l..l.-CYCLOrtEXAOIENE
1<.91 C3 NAPHTHALENE
1«.92 l.i.-OIMETHYL-5-OCTYLNAPHTHALENE
H.93 ETMYLBEHZYL BENZENE CISOHER UNKNOWN I
l'.9<> TETRAHETHYL BIPHENYL
11.95 PENTATRIACONTANE
l<«9b 1,3.5-TRI-TERT-BUTYL BENZENE
1W97 OI-P-TOLYLMETHANE
11.98 DIMETHYLOIPHENYLMEIHANE
11.99 X2.3-DIMETHYLNAPHTHALENE
1500 Z-BUTYLNAPHIHALENE
1501 l.Z.O-TRITERTIARY BENZENE
150Z *P-CHLOROACETOPHENONE
1503 2,6-OI-TERT-BUTYL TETRALIN
150-. 1.1.3-TRIMETHYL-3-PHENYL I MOAN
1505 1-BROHO-Z-CHLOROCVCLOPENTANE
1506 BETA.BETA-OIMETHYL HISTAMINE
1507 ".-DECANONE
1508 6-MEIHYL-Z-PHENYLQUINOUNE
1509 K-BUTYL8ENZENE
1510 HEXANETHVLENE ACETAMIOE
1511 <.-HErHYL-3-HEXANOL
1?12 HEXVL BUTYRATE
1513 •TRICHLOR08IPHENYL
151H 2.3,6-TRINETHYLHEPTANE
1515 •ShEXACHLOKOBIPHENYL
1516 X> »(ODT
1517 OIBENZOTHIOPHENE
1518 i.-NErHYLOIBENZOTHIOPHENE
1519 S-ETHYL PHENANTHRENE
1520 METHYLBENZACRIDINE
1521 3-ETMYL-5-METMYLPYRIDINE
1522 N.N-OIETHYLANILINE
152) 3-DOOECANONE
152<. 2.3,<.-TRIHETHYLQUlNOLINE
1525 TRINETHYLQUINONE
1526 HEXANEOIOIC ACID. OIHEXYL ESTER
1527 X»P-NIfRO PHENOL
1526 3-CHLORO-Z-BUTANOL
1529 M-CYCLOHEXYLPMENOL
1530 3-HEIHYLPIPERI 01 NE-2,8-010HE
TABLE 11. (Continued)
FINAL REPORT (PART II
RELATIVE SIZE AND CONCENTRATE WHERE DETECTED
T r
2 1
B C
T It N P
•.222
X C C C
P 0
2 2
x c
S L
2 2
X M
C C
3 1
C N
R R
1 2
C C
E 0
1 2
C N
PACE 3<>
B B
2 3
C C
(Continued)
-------
TABLE 11. (Continued)
PACE 35
K)
K3
K)
COMMON NAME
FINAL REPORT (PART II
RELATIVE SIZE AND CONCENTRATE MHERE DETECTED
V V T T T
11211
c x a c x
TTHNPPOO
t<»222222
C C C
1531 10-UNDECENOIC ACID
1532 5-PROPVLOIHYDRO-2-FURANONE
1633 3A.7A-DINETHYL OCTAHYDRO-I.-ISOBENZOFUR4N
IBS'. 3-HETHYL-3-OCTANOL
1535 BROMOOICHLOROANILINE
1536 6-PHCNYL-2-HEXANONE
1537 METHYL NONAOECANOATE
1536 HEPTYLPROPIONATE
1539 HETHYLCAPRVLIC ACID
15<>0 ACETANIOE
151.1 DIETHVLENE GLYCOL, MONOHETHVL ETHER
151.3 N-BUTYLAHINE
151,3 XETHYL CAPRAT£
151.1, 1,3-DIHETHVL-S-(1-HETHYLETHYLI -BENZENE
151,5 2,«.-DIMETHYLISOPROPYL8ENZENE
151,6 3-PHENYLPENTANE a
151.7 SN-PROPVL BENZENE
151.8 1,3-DIMETHYL I NO AN
151.9 C6-BENZENE
1550 2-METHYL-Z-BUTENAL
1551 3-FUROIC ACID
1552 TErRAHYORO-3.6-OIN£THYL-2H-PVRAN-2-ONE
1553 Z,3-DINETHVL-l,i»-HEXAOIENE
1551. 2-METHVL-CYCLOHCXANEMETHANOL
1555 3.<.-DIHYORO-l(2HI-NAPHTHALENONE
1556 PENTANETHVLBENZENE
1557 XISOQUINOLINE
1558 2,"i-OIHETHYLPENTANOL
1559 3,3-OIMETHYLBUTANAHINE
1560 2.7-DIMETHYL TETRALIN a
1561 2.
-------
COMMON NAME
TABLE 11. (Continued)
FINAL REPORT (PART II
RELATIVE SIZE AND CONCENTRATE MMERE DETECTED
tf V T T
1121
c x a c
T
MNP
222
c c c
1576 l.<>-DIHYDRO-2.5f8-TRIMETHYLNAPHTHALENE
1577 3,3,3-TRICHLORO-2-MErHYLPROPENE
1578 CYCLOHEPTANONE
1679 BENZYLAMINE
1580 «.,/-DIMETHYL INOAN
1581 BISCCHLOROPHENYLIMETHANE
1582 CIS-I.-PMENYL8ICYCLOHEKYL
1583 1,-MElHYLENECYCLOHEXANEMETHANOL
1581. 2.6.6-TRIHETHVL-BICTCLOC 3. 1. 11 MEPTAN-3-0
1585 3-BUTYL-l,2,*-C»CLOPENTAN£TRIONE
1586 XSTYRENE CLYCOL
15«7 Z-HEfHYL-S-UNOECANONE
1568 I3|3-DIHETHYLCYCLOH£XVLIOENE>ACETALOEHVD
1589 1,2, J.1.-TETRAMETHYL BENZENE
1»90 1-ETHYL-l-METMYL INOAN
1591 1-CHLOROTETRAOECANt
1592 1,1-OIPH£NYLCYCLOH£XANE
1593 BICVCLOI2.2.2)OCTANE-l.l>-OIOLt HONQACETA
159<, METHYL 3-HYOROXYPHENVLACErATE
1595 X2-HETHYL ANTHRACENE
1596 2-IPHENYLMETHYLI NAPHTHALENE
1597 PHENYL P-PVRIOVL KETONE
1598 OOOECVL PHENOL
1599 FLUOROIOOOBENZENE USOHER UNKNOMNI
1600 3-METMYL-2-FURANONE
1601 2-PHENVL UNDECANE
160? l,
-------
1622
1623
162<»
1625
1626
1627
1620
1629
1630
1631
1632
1633
1635
1636
1637
1638
1639
16m
COMMON NAME
TABLE 11. (Continued)
FINAL REPORT (PART I)
RELATIVE SIZE AMD CONCENTRATE MHERE DETECTED
PAGE 37
XBENZYL CHLORIDE
PHENOL
ETHYL NONADECANOATE
OIBROHOPHENOL
2-U-HETHYL-3-CVCLOHEXENVL) ISOPROPANOL
li2-CVCLOHEXANEOIOL
BUTYL THIAZOLE
2-HYDROXV-S-ISOPROPYL-2t<»i6-CVCLOHEPTATR
0-NITROTOLUENE
1121
C X B C
lt<»
-------
REFERENCES
1. Kopfler, F. C., W. E. Coleman, R. G. Melton, R. G. Tardiff, S. C. Lynch,
J. K. Smith, "Extraction and Identification of Organic Micropollutants:
Reverse Osmosis Method", Ann. NY Acad. Sci., 298, 20 (1977).
2. Smith, J-. K., A. J. Englande, M. M. McKown, S. C. Lynch, "Characterization
of Reusable Municipal Wastewater Effluents and Concentration of Organic
Constituents", Environmental Protection Technology Series, U. S. EPA
#600/2-78-016, February, 1978.
3. Coleman, W. E., R. D. Lingg, R. G. Melton, F. C. Kopfler, "The Occurrence
of Volatile Organics in Five Drinking Water Supplies Using Gas Chromato-
graphy/Mass Spectrometry" in Identification and Analysis of Organic
Pollutants in Water, L. H. Keith, Ed., p. 305, Ann Arbor Science, 1976.
4. Ishiwatari, R. and T. Hanya, "Gas Chromatographic-Mass Spectrometric
Identification of Organic Compounds in A River Water", in Actes du 6e
Congres International de Geochimie Organique. Rueil-Malmaision, Edition
Technip, 27, Rue Ginous, 7537, Paris, France, 1051, September, 1973.
5. Law, L. M., and D. F. Georlitz, "Microcolumn Chromatographic Clean-up for
the Analysis of Pesticides in Water", Journal of Assoc. of Off. Anal.
Chem., 53, 1276 (1970).
6. Leoni, V., "The Separation of Fifty Pesticide and Related Compounds and
Polychlorobiphenyls into Four Groups by Silica Gel Microcolumn Chromato-
graphy", J. Chromatography, 62, 63 (1971).
7. Eichelberger, J. W., L. E. Harris, and W. L. Budde, "Reference Compound
to Calibrate Ion Abundance Measurements in Gas Chromatography-Mass
Spectrometry Systems", Anal. Chem., 47, 995 (1975).
8. Kuehl, D. W., "Identification of Trace Contaminants in Environmental
Samples by Selected Ion Summation Analysis of GC-MS Data", Anal. Chem.,
49_, 521 (1977).
9. Mantoura, R. F. C. and J. P. Riley, "The Analytical Concentration of
Humic Substances from Natural Waters", Anal. Chem. Acta, 76, 97 (1975).
10. McCarty, P. L., D. Argo, M. Reinhard, "Operational Experiences with
Activated Carbon Adsorbers at Water Factory 21", J. Am. Water Works
Assn., 71, 683 (1979).
225
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APPENDIX A
DELIVEKABLES
DELIVERABLES REQUIRED BY THE CONTRACT
The deliverables required by EPA Contract 68-03-2548 include the follow-
ing items:
• monthly progress reports for the first twelve months covering
analytical scheme development and validation
• separate reports of analysis results for each analyzed concen-
trate
• unused portions of concentrates and fractions
• samples of compounds used for identification confirmation
• magnetic tapes of GC-MS data
• utility listings of the databases
Monthly Progress Reports
Monthly progress reports for the first twelve months of contract activity
were delivered to the Project Officer on approximately the fifteenth day of
the month following the month covered. These reports were dated August 15,
1977 through July 15, 1978.
Concentrate Analysis Reports
Individual reports of concentrate analysis results for DW and AWT concen-
trates are listed in Tables Al and A2, respectively. A description of the
contents of each of the seven volumes of these reports is given in Table 6,
and a description of the material presented in the computer-printed listings
is presented in detail in Section V, Analytical Scheme, under "Report Genera-
tion/Concentrate Analysis Reports". Three of the concentrates analyzed were
process blanks of the concentrate production methodology and are listed in
Table A3.
226
-------
Table Al. Analysis Reports for Drinking Water
Concentrates
Code
Name3 City
TIC Cincinnati, OH
T1X "
T1Y
T4C "
T4X
M2C Miami, FL
M2X "
N2C New Orleans, LA
N2X
02C Ottumwa, LA
02X "
P2C Philadelphia, PA
P2X "
VIC Poplarville, MS
V1X
S2C Seattle, WA
S2X "
Concentrate
Typeb
Combined Solvent Extract
XAD of RO Brine
XAD Direct
Combined Solvent Extract
XAD of RO Brine
Combined Solvent Extract
XAD of RO Brine
Combined Solvent Extract
XAD of RO Brine
Combined Solvent Extract
XAD of RO Brine
Combined Solvent Extract
XAD of RO Brine
Combined Solvent Extract
XAD of RO Brine
Combined Solvent Extract
XAD of RO Brine
Date of
Report
08-28-79
09-12-79
10-29-79
04-30-81
05-04-81
06-07-79
06-26-79
07-10-79
07-18-79
07-27-79
08-03-79
05-21-79
04-20-79
12-14-79
01-07-80
05-09-79
04-20-79
Concentrates
Included in
Comb. Rpts.c
TIC,
T2Bd
TIC,
T4C,
M2C,
N2C,
02C,
P2C,
VIC,
S2C,
T1X
, T1Y,
T1X
T4X
M2X
N2X
02X
P2X
V1X
S2X
a) The code name is used in the computer-printed tables.
b) Combined Solvent Extract: These are extracts of the two RO brines
produced. XAD of RO Brine: XAD-2 extraction was performed on the RO
brines after solvent extraction.
c) Identified by the three-digit code. Reports with no entry in this
column did not contain a combined report.
d) T2B is an XAD-2 resin elution blank, see text.
227
-------
Table A2. Analysis Reports For Advanced-Waste
Treatment Water Concentrates
Code
Name3 City
B1M Blue Plains
(Washington D.C.)
BIN "
B2C
D2N Dallas, TX
E1C Escondido, CA
R1C Orange County, CA
R2C "
C1P Pomona, CA
C1M
C1N "
C2N "
C3C
L2P Lake Tahoe, CA
L2M "
L2N "
L2D
Concentrate
Typefa
CH2CA2 Extract, CA
Acidic CH2CA2 Extract, CA
Combined Solvent Extract
Acidic CH C£2 Extract, CA
Combined Solvent Extract
Combined Solvent Extract
Combined Solvent Extract
Pentane Extract, CA
CH CA Extract, CA
Acidic CH Ci Extract, CA
£* &•
Acidic CH C£ Extract, CA
Combined Solvent Extract
Pentane Extract, CA
CH C£ Extract, CA
Acidic CH CA2 Extract, CA
Acidic CH CA Extract, Nyl.
Date of
Report
04-18-20
11-03-80
04-18-80
04-27-81
01-31-80
11-05-79
04-24-81
01-30-79
02-23-79
04-04-79
04-13-79
01-15-79
11-10-78
12-04-78
12-21-78
04-29-81
Included in
Comb. Rpts.c
B1M and BIN,
B1M,B1N & B2C
C1P,C1M& C1N
C1P,C1M,C1N,
C2N & C3C
L2P,L2M,L2N
L2P,L2M,L2N,
and L2D
a) The code name is used in the computer-printed tables.
b) All extracts are of RO brine. "CA" indicate the RO brine produced by the
cellulose acetate membrane. "Nylon" refers to RO brine produced by the
Permasep R nylon hollow fiber RO unit. "Conbined Solvent Extract"
indicates a combination of all extracts of both the CA and Nylon RO
brines(a total of six extracts).
c) Identified by the three-digit code. Reports with no entry in this
column did not contain a combined report.
228
-------
Table A3. Analysis Reports for Process for Process Blank Concentrates
Code
Namea
X1C
XIX
T2BC
Concentrates
Date of Included in
Sample Description Report Comb. Rpts.b
evaporated pentane and methylene 11-14-79
chloride extraction solvent
evaporated ethanol elution solvent 12-05-79 X1C, XIX
of XAD-2 resin
evaporated diethyl ether eluate of 08-23-79 T1Y, T2BC;
XAD-2 resin0 TIC, T1X, T1Y,
and T2B
a) The code, name is used in the computer-printed tables.
b) Identified by the three-digit code. Reports with no entry in this
column did not contain a combined report.
c) Concentrate T2B is a process blank for concentrate T1Y only
(see table Al)
229
-------
Unused Portions of Concentrates
Unused portions of DW and AWT concentrates were stored at -10°C at
Battelle until the GC-MS analysis tasks were completed. These unused concen-
trate portions were hand-delivered to the Project Officer in May, 1980. The
returned aliquots, except as explained below, consisted of 10 percent and 40
percent of the material originally produced for the solvent extracted and
XAD-2 extracted concentrates, respectively.
Generally, the portion received by Battelle of concentrates produced by
solvent extraction of RO brine was 20 percent of the total produced from the
sampled water. Half of the material submitted (10 percent) was partitioned
into fractions for GC-MS analysis. The remaining material (.10 percent of the
total produced) was used for sample archiving and analysis of the concentrate,
as received; these GC-MS and residue weight analyses consumed only about 1.5
percent of the 10 percent saved. If it became necessary to repeat the frac-
tionation of the concentrate, the entire remaining amount was used, and this
occurred for six concentrates: VIC and V1X (Table 1A) , GIN (Table 2A) , and
X1C, XIX and T2B (Table 3A).
Generally, concentrates produced by XAD-2 resin extraction of RO brine
were supplied for analysis in the amount of 50 percent of the total material.
Use of 10 percent for GC-MS analysis thus left 40 percent of the originally
produced material for sample archiving and repeated analysis, if necessary.
Repeated analyses of concentrates P2X, S2X and 02X (Table 1A) reduced the un-
used portions to 30, 20 and 30 percent of the originally produced material,
respectively.
Three of the AWT concentrates (B2C, E1C and R2C, Table 2A) were incor-
rectly divided into aliquots for biological (toxicity) testing and GC-MS
analysis before being sent by EPA to Battelle. The aliquot received was 16
percent (20 percent of 80 percent) of the original material produced. Parti-
tioning of 10 percent thus left 6 percent remaining for unpartitioned concen-
trate analysis and sample archiving. Fortunately, repeat analysis was not
required for these three samples.
Unused Portions of Fractions
As explained under Section V, Analytical Scheme/Residue Weight Analysis,
a variable amount, ranging from 1Q to 60 percent, of each concentrate frac-
tion and corresponding blank was consumed for the determination of residue
weights. The remainder of each, sample was sealed into a 2.0 ml break-seal
glass ampule for sample archiving and stored at -10°C. These ampules were
delivered to the Project Officer along with, the unused portions of the con-
centrates.
Aliquots of Reference Standards
Compound identifications were confirmed by GC-MS analysis of commercially
obtained standards whenever possible and practical. GC-MS data for 1035 dif-
ferent compounds were obtained for this purpose. An aliquot of each of
these compounds except for those supplied as mixtures was placed in a 1.8 ml
230
-------
Teflon-sealed screw cap bottle and delivered to the Project Officer.
Magnetic Tapes of GC-MS Data
The GC-MS data acquired during the course of the Contract can be classi-
fied as follows:
. GC-MS analysis of unpartitioned concentrates, fractions and
corresponding blanks
• GC-MS analysis of confirmation standards and standard mixtures
of the compounds for specific search
. MS calibration verification and DFTPP ion source tuning verifi-
cation data corresponding to each GC-MS data file described
above
• SGCSM GC-MS performance verification for each day that the above
described data were obtained
All of the above data were stored on 9-track magnetic tape. When repeat anal-
yses were required, the unused, previously acquired data were not deleted
from the tape archive, so that the collection of 89 tapes actually corres-
ponds to all acquired data. The tapes were numbered sequentially and each
tape is accompanied by a computer-printed listing which shows the data files
on the tape (by the 6-digit data system file name) and the amount of storage
space required for it on a magnetic disk in system/150 "block" storage units.
The 6-digit data file naming system used for the analysis of unpartitioned
concentrates, fractions and corresponding method blanks was designed to elim-
inate the possibility of using the same file name for more than one sample
analysis. In addition, the file name readily translates into a complete
description of the sample using the directions included in each concentrate
report and reproduced with some expansion in Appendix B. The 6-digit code
naming system unambiguously identifies the following:
• the city; the sampling sequence number, and the method of organic
extraction from RO brine
• identity of the fraction Cor unpartitioned concentrate)
• the GC phase used for the analysis
• indication as the first, second, etc., time that the analysis had
been performed
• for the mass calibration, DFTPP and SGCSM performance verifications,
the 6-digit name identifies the type of GC-MS quality assurance
check and the data file to which the QA check file corresponds.
231
-------
Utility Listings of the Databases
Computerized data management of both the compound identification results
and the chromatographi.c data from analysis of reference standards allowed the
listing of these databases in multiple orderings that were valuable beyond
their relevance to the contract work. These two sets of listings were pro-
duced in a one-volume format (for each database) and multiple copies deliver-
ed to the Project Officer. The contents of these two special supplementary
reports and a description of the information provided in the listings is given
in Section V, Analytical Scheme in this volume of the Final Report (see
Special Listings of the Database and Compound Identification and Confirma-
tion) . Note that the report volume covering the confirmation standards data-
base also serves as a source guide for EPA users of the GC-MS standards
repository which was created from the set of aliquots of reference compounds
delivered to the Project Officer (.described above in this Appendix under
Aliquots of Reference Standards). The repository is managed by the Environ-
mental Monitoring Support Laboratory (.EMSL) at EPA-Cincinnati, and the com-
puter-printed listing of the confirmation database is available from Dr. Bill
Budde at EMSL-CI.
ADDITIONAL DELIVEEABLES PROVIDED BY BATTELLE
System/150 Data Processing and Utility Programs
In order to make GC-MS.data acquisition and processing on the Systems In-
dustries System/150 GC-MS data system more effective and efficient, develop-
ment of some new software was required. In addition, the existing data
acquisition program (IFSS) was modified to allow the use of a real-time in-
ternal clock for accurate assignment of GC retentions. Two of the new pro-
grams written for this work can be classified as relatively complex data
processing capability providing extracted ion current profile (EICP) data
searching and graphics. The remaining eight are relatively simple data han-
dling programs. All of these programs, listed and described below, were
delivered to the Project Officer on a magnetic disk for distribution to other
EPA GC-MS laboratories.
Data Processing Programs
1. Selected Ion Summation (SIS)—The SIS program provided new and more
powerful EICP processing and convenient, flexible chromatography graphics
display/output capabilities. Some of the capabilities include:
• display of the summed ion current of one to eight ions with the
absence in a given spectrum of any one of the selected ions re-
sulting in the sum for that spectrum to be set to zero
• variable thresholding requiring the least intense of the selected
ions to be a user-selected percent of the most intense
• base peak requirement option which sets the EICP sum to zero unless
the user-designated base peak is the largest of the selected ions
232
-------
. chromatographic display of up to 2047 spectra on one page of
the CRT screen or plotter output with the summed EICP trace
synchronized with Cand appearing above) the total ion chroma-
togram trace
• easy GC peak area determination, chromatographic scale ex-
pansion, and retention time determination using the CRT terminal
cross-hairs; independent vertical scale expansion of EICP
and total ion traces
. automatic queue forming of spectrum-background pairs using the
CRT terminal cross-hairs
• selection of local or global normalization of the total ion
chromatogram trace
2. Selected Ion Summation Data Search for Specified Compounds (QSIS)—
The QSIS program allowed automated searching of GC-MS data for any number of
species. The parameters for the individual compounds (output labeling, re-
tention time, selected EICP ions, etc.) are established by a separate program
(see EDQ, below). The signal level thresholding and EICP zero-set defaulting
described above for the SIS program are incorporated for the EICP data search.
Other features of the QSIS program include:
• searching of a user-specified width GC retention window based on
either relative or absolute retention
• option to pause after searching for each compound for spectrum-
background queuing or area determination, as described for the SIS
program. There is no pause if no EICP peaks are detected
• automatic plotting on one 8 1/2 by 11 inch page of the SIS EICP
trace and the total ion trace (vertically correlated) over the
selected GC retention window. No plot is produced if no EICP
peaks are detected
Utility Data Handling Programs
1. Search Queue Editor (EDQ)—The EDQ program was required to set up a
file of compounds for automated data searching using the QSIS software de-
scribed above. For each search compound entry in the list, the following are
specified: name of the compound; the SIS ions (one to eight); ion threshold-
ing to be used; base peak requirement, if any; and expected retention time
and/or relative retention index. The program allows editing by deletion or
modification of the entries which, are accessed by their sequence numbers.
New entries can also be added to the end of the list, and there is no practi-
cal limit to the number of compounds that can be placed in such a search
queue.
2. Magnetic Tape Storage/Retrieval (MAG150)—The MAG150 program allowed
GC-MS data files to be transfered to and retrived from standard 9-track mag-
netic tape using the System/150 data system. Data are stored on tape in an
industry-standard (800 bits/inch) format using a data file specific dialogue
233
-------
rather than the entire disk image as the storage unit. The software is de-
signed for use with a Digital Equipment Corp. TM-8E-compatible interface and
a Wangco Model 10 tape handling unit. Nine to eleven GC-MS data files and
their associated performance verification checks can be stored on a single .
2400 ft. tape.
3. Spectrum Queue Handling Programs (MERGE. QSORT and BUILDQ)—These
three programs aided in manipulating lists (queues) of spectrum-background
pairs (_Q-files) in preparation for library matching and spectrum plotting.
MERGE allows two or more Q-files to be combined into a new Q-file with a new,
user-specified name. The QSORT program can then be used to sort the spectrum-
background pairs of a Q-file by increasing order of the spectrum number. The
BUILDQ program allows Q-files to be listed on the CRT terminal or printer
showing the number of entries and the spectrum/background numbers in the list.
This program also allows new Q-files to be created by typing in the spectrum/
background pairs at the CRT terminal.
4. Data Interpretation Worksheet (.QFORM)—The QFORM program created a
tabular format for recording mass spectral-based compound identification re-
sults. For each entry of a referenced Q-file, the form shows a sequence
number, the spectrum number, the subtracted background spectrum number, the
retention time, the relative retention index, and designated spaces to record
the compound identity, molecular weight, molecular formula, size of the GC
peak, library match index and confidence level of the analyst. Each page of
the form is labeled with the data file name and the retention time of the
internal standard and a space is provided for the name of the analyst and the
date of completion. The form is printed on standard 15-inch wide z-fold com-
puter form paper with 26 entries per page.
5. Data Transfer from System/150 to INCOS CQSAVE and INCOS4)—Since the
Finnigan INCOS mass spectral library matching software was distinctly super-
ior to that available on the System/150 data system, two new programs were
required to accomplish the transfer of mass spectral data between the two
systems. The. QSAVE program constructs a user-named data file of the back-
ground subtracted mass spectra corresponding to the entries of a Q-file of
interest. This greatly abbreviated data file (.usually 75 to 300 spectra com-
pared to the 2100 to 2800 spectra of the original data file) can then be
transfered directly to the INCOS data system using the INCOS4 software. Spec-
trum library matching can be performed on each spectrum of this abbreviated
data file using standard INCOS software. The hard-copied output of the INCOS
library match, is correlated to the original data via the sequence number of
the abbreviated data file and the sequence number on the Data Interpretation
Worksheet produced by the QFORM program (.see No. 4, above). The INCOS4 pro-
gram can also be used to transfer full (unabbreviated) GC-MS data files.
Retention time information is not retained in the transfered data file.
MASS SPECTRAL LIBRARY IMPLEMENTATION
When the 31,357 EPA/NIH/NSRDS mass spectral library became available from
the National Bureau of Standards, it was immediately implemented at Battelle's
GC-MS facility for the INCOS data system. This implementation was done one
year before the expanded library was made available through the instrument
234
-------
manufacturer CFinnigan Instruments!. The 31,357 spectrum library was sup-
plied to the Project Officer on a standard INCOS data system magnetic disk
for distribution to interested EPA GC-MS facilities.
Preliminary Report on DW Concentrate Analyses for Five Cities
At the conclusion of analyses of the first ten DW concentrates a prelim-
inary combined report of the compound identification results and residue
weight analysis results was prepared at the request of the Project Officer.
These ten concentrates were the five pairs of combined solvent extracts and
XAD-2 extracts of the RO brine produced from the second sampling of five
cities: Miami, Florida; Philadelphia, Pennsylvania; New Orleans, Louisiana;
Ottumwa, Iowa; and Seattle, Washington.
This report contained the following items:
• summary of the special interest compounds found among the total
of 1152 identified compounds
• brief explanation of the analytical scheme
• discussion of the compound identification and residue weight
analysis results and assessment of the problem of artifact
compounds due to XAD-2 resin bleed
• three listings of the 1152 identified compounds in the format
described in this Final Report volume under Section V,
Analytical Scheme Report Generation/Combined Concentrate
Analysis Reports.
This combined report was classified as preliminary due to the following
three circumstances: 1. Analysis of the five Cincinnati DW concentrates had
not been completed and, thus, were not included. 2. Assessment of the RO
method blanks (jthe two Poplarville, Mississippi DW concentrates) had not been
completed. 3. Further compound identification confirmation for the results
of these five cities was anticipated. The Final Report material in this
volume and Volume 2 completes these three requirements, and, thus, supercedes
the preliminary report on the five cities.
Fifty bound copies of the preliminary five cities DW report were deliver-
ed on August 28, 1979 to the Project Officer. This report is available through
U.S. EPA HERL/CI.
235
-------
APPENDIX B
SYSTEM FOR NAMING GC-MS DATA FILES
The Systems Industries System/150 GC-MS data system which was used for
all GC-MS data acquisition in this work allowed a maximum of six digits to be
used for naming GC-MS data files. A naming system was developed which both
eliminated the possibility of replicate use of a data file name and allowed
relatively easy translation of the six digits, in a logical and systematic
fashion, to a completely unambiguous description of the sample.
Only three digits of this 6-digit code (the second, third and fourth) are
used in the Final Report material covering the DW and AWT concentrates. These
three digits code the city, sampling sequence and method of concentrate pro-
duction and, thus, completely identify the concentrate. Four digits (.the
second, third, fourth and fifth) were required to code the twenty small-volume
samples associated with the Cincinnati DW GAC Contactor A and D samplings.
Since these 3- or 4-digit sample identifying codes are always translated in
the accompanying text and/or tables, knowledge of the complete 6-digit coding
system, as presented in this appendix, is not necessary for understanding any
part of the Final Report. Access of the original GC-MS data on 9-track tape
(one of the deliverables listed in Appendix A) does, however, require the use
of the 6-digit file name coding system. For this reason, the following com-
plete explanation has been included here.
Digit One
A number was used to identify the fraction analyzed as follows:
Q = Unprocessed concentrate, as received
1 = Base fraction
2 = Acid fraction (derivatized)
3 = 2.75 ml hexane eluate from silica gel
4 = Neutral compounds (no acids or bases); no other fractionation
5 = 4 ml hexane/benzene eluate from silica gel
6 = 4 ml methylene chloride eluate from silica gel
7 = 4 ml methanol eluate from silica gel
8 = Combination of 1, the base fraction, and 6, the CH2C12 eluate
9 = 4 ml methylene chloride eluate of silica gel following the 2.75 ml
hexane elution (i.e., hexane/benzene elution omitted)
236
-------
Digit Two
A letter was used to indicate the origin of the water sample as follows:
B = Blue Plains, Washington, D. C.(AWT) 0 = Ottumwa, Iowa (DW)
C = Pomona, California (AWT) p = Philadelphia, PA (DW)
D = Dallas, Texas (AWT) R = Orange County, CA (AWT)
E = Escondido, California (AWT) S = Seattle, WA (DW)
J = Jefferson Parrish (New Orleans) T = Cincinnati, Ohio (.DW)
Louisiana (DW)
L = Lake Tahoe, California (AWT) V = Poplarville, MS (DW)
M = Miamia, Florida (DW) X = An extraction solvent blank
N = New Orleans, Louisiana (DW)
Digit Three
Numbers 1 to 6 were used to indicate the sampling sequence of the site.
Digit Four
For large-volume concentrates, a letter corresponding to the method of
extraction of organic material from the. RO brine was used:
C = Combination of all RO brine solvent extracts
D = Acidified methylene chloride extraction of RO brine from the nylon
membrane
P = Pentane extraction of RO brine from the cellulose acetate membrane
M = Methylene chloride extraction of RO brine from the cellulose acetate
membrane
N = Acidified methylene chloride extraction of RO brine from the cell-
ulose acetate membrane
X = XAD extraction of RO brine with ethanol elution
Y = Direct XAD extraction of the sampled water with diethyl ether
elution; RO processing was not used
B. - A blank elution of an XAD column using diethyl ether
For small-volume water samples, letters were used to indicate the point of
sampling for all samples except the Jefferson Parrish XAD/analytical samples:
Q » A "Super-Q" reagent water 10-liter extraction blank
L = 10 liters of water, lyophylized and reconstituted to the original
volume with "Super-Q" reagent water
K. = 1Q liters of water corresponding to L_, above
E = 10 liters of water sampled prior to RO concentration and GAG
contactor treatment
R = Water sampled from various points in the RO concentration process at
a volume approximating 10 liters of unconcentrated water
G = Water following GAG contactor treatment, unconcentrated or concen-
trated 200-fold by RO
Y = A concentrate produced by XAD-2 extraction/diethyl ether elution
237
-------
XAD analytical samples generated from reverse osmosis concentration process
monitoring of the Jefferson Parrish sampling are coded with a number as
follows:
~~~~ pH of Sample
Before XAD-2
Extraction
Sampling Point of the RO Concentrator Acidic Basic
Cellulose Acetate Feed
Cellulose Acetate Permeate (Nylon Feed)
Cellulose Acetate Concentrate
Nylon Concentrate
1
3
5
7
2
4
6
8
The number 9 in the third digit indicates the sample is a blank XAD ,
elution.
Digit Five
For the large-volume DW and AWT concentrates and all small-volume samples
except those corresponding to the Cincinnati GAC contactors A and D, the fol-
lowing letter/number system was used to indicate whether the data file
corresponded to an analysis on the SP1000 or SP2100 GC column as well'as to
indicate the type of GC-MS performance verification, where applicable:
1 = Sample analyzed using the SP1000 GC column
A = FC43 by batch inlet to check mass calibration corresponding to a
sample analysis using SP1000
B = Direct inlet check of DFTPP prior to sample run using SP1000 column
C = GC-MS analysis of the SGCSM system test mixture prior to sample
analysis using SP1QOO column
2 = Sample analyzed using the SP21QO GC column
D = FC43 by batch inlet to check mass calibration corresponding to a
sample analysis using SP2100
E = Direct inlet check of DFTPP prior to sample run using SP2100 column
F = GC-MS analysis of the SGCSM system test mixture prior to analysis
run using SP21QO column
For the twenty small-volume samples corresponding to Cincinnati GAC contac-
tors A and D, a letter/number combination was used for the fourth/fifth
digits, to completely identify the point of sampling. The only GC column used
for all the small-volume samples was SP1QOQ, so this parameter did not need
identification in the fifth digit of the 6-digit code. The second and third
digits for the 13 GAC Contactor A and 7 GAC Contactor D samples are T4 and
T5, corresponding to the fourth and fifth Cincinnati sampling, respectively.
The following is the coding system for the fourth and fifth digits for these
twenty samples:
238
-------
T4 Samples5
Digits
4 and 5 Sample Identity0
Digits
3 and 4
T5 Samplesb
Sample Identity0
El
Rl
R2
R3
R4
R5
R6
Gl
G2
Yl
Y2
Y3
Y4
10 liters, finished DW El
10-fold, CA cone. Rl
100-fold, CA cone. R2
10 liters, CA permeate R3
10-fold, NYL cone. R4
100-fold, NYL cone. Gl
200-fold, CA cone. Yl
10 liters
200-fold, CA cone.
10 liters, XAD-2
permeate, Na2S03 preserved
XAD-2 concentrate
corresponding to Yl
10 liters, XAD-2 permeate,
without Na2S03
XAD-2 concentrate
corresponding to Y3
10 liters, finished DW
10-fold, CA cone.
10-fold, NYL cone.
200-fold, CA cone.
200-fold, CA cone.
10 liters
XAD-2 concentrate
a) Only Gl and G2 are post-GAC samples.
b) Only El and R4 are pre-GAC samples.
c) 10-fold, etc, indicates the degree of RO concentration;
CA cone, and NYL cone, are RO concentrates from cellulose
acetate and nylon membranes, respectively.
Indication of the GC-MS performance verification data for these twenty
small-volume samples was accomplished somewhat differently than as described
above for the large-volume samples:
Correspondence of Letters with the Numbers Used to
Identify the Twenty Small-Volume Samples
Performance
Check.
FC-43
DFTPP
SGCSM
1
A
a
C
2
D
E
F
3
G
a
I
4
J
K
L
5
M
N
0
6
P
Q
R
Digit Six
A number was used corresponding to whether the data file resulted from
the first, second, etc., time analysis was attempted; or, if the sample cor-
responded to a blank, a letter was used. Thus, "A" would indicate the first
239
-------
attempt to analyze a blank sample, "B" the second attempt, and so on.
EXAMPLE TRANSLATIONS
The following examples illustrate the use of the above mechanism for
translating 6-digit GC-MS file names into sample identities:
2L2D2B: The second analysis of the process blank ( B) on the SP2100
GC column (. 2-) of the derivatized acid fraction (2 ) correspond-
ing to the derivatized acid fraction of the AWT concentrate produced from
the second sampling (_—2 ) at Lake Tahoe (-L ) by methylene chloride
extraction of the acidified RO brine produced with the nylon membrane
C D—) .
5P2X11: The first analysis ( D of the hexane/benzene silica gel
eluent (.5 ) of the DW concentrate produced from the second sampling
(—2 ) at Philadelphia (-P ) by XAD-2 extraction of RO brine
C X—) analyzed on the SP1000 GC column C 1-).
7T4CEA: A DFTPP GC-MS performance check C E-) corresponding to the
first analysis (using SP2100 GC column C E-)) of the process blank
G A) methanol elution of silica gel (7 ) generated with the frac-
tionation of the DW concentrate of the fourth sampling (.—4 ) at
Cincinnati (-T ) which, was a composite of all the solvent extracts of
RO brine C C—) .
240
-------
APPENDIX C
PUBLICATIONS AND PRESENTATIONS RESULTING FROM THE CONTRACT WORK
At this writing, five reports containing results of the contracted re-
search have been published in the scientific literature:
1. Lin, D.C.K., R.G. Melton, F.C. Kopfler, and S.V. Lucas, "Chapter 46.
Glass Capillary GC-MS Analysis of Organic Concentrates from Drinking and
Advanced Waste Treatment Water", p. 861, in Advances in the Identifica-
tion and Analysis of Organic Pollutants in Water, Vol. 2. L.H. Keith, Ed.,
Ann Arbor Science Publishers, 1981
2. Melton, R.G., W.E. Coleman, R.W. Slater, F.C. Kopfler, W.K. Allen,
T.A. Aurand, D.E. Mitchell, S.J. Voto, S.C. Watson, and S.V. Lucas,
"Chapter 36. Comparison of Grob Closed-Loop-Stripping Analysis CCLSA) to
Other Trace Organic Methods", p. 597, in Advances in the Identification
and Analysis of Organic Pollutants in Water, Vol. 2. L.H. Keith, Ed.,
Ann Arbor Science Publishers, 1981.
3. Lin, D.C.K., S.V. Lucas, B.A. Petersen, R.G. Melton, and W.E. Coleman,
"Glass Capillary GC-MS Analysis of Organics in Drinking Water Concen-
trates and Advanced Waste Treatment Water Concentrates", in High Resolu-
tion Gas Chromatography. S.P. Cram, Ed., Academic Press, New York.
4. Lin, D.C.K., R.L. Foltz, S.V. Lucas, B.A. Petersen, and L.E. Slivon,
"Application of Deuterated Standards in Analysis of Organics in Water
Concentrates", in Stable Isotopes: Proceedings from Third International
Conference, p. 243, R. Klein and P. Klein, Eds., Academic Press, New York
(1979)
5. Lin, D.C.K., R.L. Foltz, S.V. Lucas, B.A. Petersen, L.E. Slivon, and
R.G. Melton, "Glass Capillary GC-MS Analysis of Organics in Drinking
Water Concentrates and Advanced Waste Treatment Water Concentrates. II.",
in Measurement of Organic Pollutants in Water and Wastewater, p. 68,
E.E. Van Hall, Ed., ASTM Special Technical Publication, No. 686,
Philadelphia, Pennsylvania (1979).
Publications 1 and 2 were presented in lectures given by Lucas and
Melton, respectively at the Symposium on Analysis of Organic Pollutants in
Water at the American Chemical Society meeting, August, 1980 in Las Vegas,
Nevada. Publications 4 and 5 were presented in a talk by Lin at the Third
International Conference on Stable Isotopes in 1978 at Argonne National Lab-
oratory and the ASTM Committee D-19 meeting in June, 1978, at Denver,
Colorado, respectively. The following oral presentations at scientific
241
-------
meetings do not have corresponding written publications. In each case the
first author listed made the oral presentation:
1. Petersen, B.A., R.L. Foltz, S.V. Lucas, and D.C.K. Lin, "Routine Evalua-
tion and Optimization of a Capillary Column GC/Quadrupole MS/COM System
for the Analysis of Complex Environmental Samples", Twenty-Sixth Annual
Conference on Mass Spectrometry and Allied Topics, St. Louis, May 31,
1978.
2. Slivon, L.E., "A Selected Ion Summation Technique Used for Reverse Search
and Quantitation", Twenty-sixth Annual Conference on Mass Spectrometry
and Allied Topics, St. Louis, May 31, 1978.
3. Contos, D.A., V.R. Goff, S.V. Lucas, S.C. Watson, L.E. Slivon, and
D.C.K. Lin, "Glass Capillary GC-MS Analysis of Organic Pollutants in
Water. I. Fractionation and Analysis of Complex Concentrates from
Drinking Water and Advanced Waste Treatment Water," llth Central Region-
al Meeting, American Chemical Society, Columbus, Ohio, May 7, 1979.
4. Goff, V.R., D.A. Contos, S.V. Lucas, S.C. Watson, L.E. Slivon, and
D.C.K. Lin, "Organic Pollutants in Water. II. Quality Assurance, Re-
sults, and Computerized Data Searching for Specific Pollutants in the
Analysis of Complex Concentrates from Drinking Water and Advanced Waste
Treatment Water", llth Central Regional Meeting, American Chemical
Society, Columbus, Ohio, May 7, 1979.
5. Lin, D.C.K., R.L. Foltz, S.V. Lucas, and B.A. Petersen, "Glass Capillary
GC-MS Analysis of Drinking and Advanced Waste Treatment Water Concen-
trates". Presented at the Twenty-seventh Annual Conference on Mass
Spectrometry and Allied Topics, June 4, 1979, Seattle, Washington.
6. Lucas, S.V., B.A. Petersen, R.L. Foltz, and D.C.K. Lin, "Routine Perfor-
mance Monitoring of a Capillary GC/Quadrupole MS/Computer System Used for
the Analysis of Complex Environmental Pollution Samples". Presented at
the Twenty-seventh Annual Conference on Mass Spectrometry and Allied
Topics, June 4, 1979, Seattle, Washington.
In addition, two publications in refereed journals (probably Environmen-
tal Science and Technology and the Journal of the American Water Works
Association) are planned.
242
-------
APPENDIX D
IDENTIFIED COMPOUNDS LISTED BY MOLECULAR WEIGHT
Tables of computer-printed listings of identified compounds accompany the
discussion of the DW and AWT results in this volume. Analogous tables for the
small-volume samples are presented in Volume 3 of this Final Report. All of
these tables list the identified compounds in decreasing order of the size of
the observed GC peak while showing in which of the concentrates identification
occurred. Thus, these tables provide for a convenient comparison of occurrence
in related concentrates as well as an easy visualization of the predominant
chemical species present. However, since these lists are ordered by decreas-
ing size of the GC peak, it is difficult to determine if and where
a specific compound was found. Obviously, the ability to determine whether a
specific compound was found in these concentrates is of critical importance to
the present and future usefulness of this work. To accomplish compound-speci-
fic inspection of the results, Table Dl has been produced. This table lists
all the compounds that have been added to the computer-managed database by
increasing molecular weight, and correlates this listing with the tables show-
ing occurrence of the compounds in the four sets of related samples (DW, AWT,
GAG contactor A and GAG contactor D). Thus, to determine whether a specific
compound was found, the range of compounds in Table Dl which have the correct
molecular weight must be searched. If the compound is found in Table Dl, it
can then be located at the indicated sequence number of the relevant table
showing the concentrates or small-volume samples in which that compound was
found. Tables 9 and 10 of this Final Report volume are correlated in Table Dl
for the DW and AWT concentrates, respectively, and Tables 7 and 8 of Volume 3
are correlated for the GAG contactor A and D samples, respectively.
For a few of the compounds in Table Dl, detection in any of the four
groups of samples is not indicated. A brief description of the structure and
use of the identified compound database provides an explanation for this ap-
parent inconsistency. The database of identified compounds is structured on
two levels. The first level contains information about chemical species; i.e.,
name, CAS registry number, molecular weight, molecular formula, types of func-
tional groups, industrial source and use, etc., but contains no concentrate-
specific information. The second level contains exclusively (.except for the
CAS registry number) concentrate-specific information; i.e., the concentrate
and fraction where identified, size of the GC peak, identification proof
status, retention time, relative retention index, and spectrum number, and it
is linked to the first level of the database only by the CAS registry number.
The listing in Table Dl is of the first, chemically descriptive level of the
database. There are three principal reasons that some entries in Table Dl are
not listed further in the four sample-specific occurrence tables:
243
-------
• The compounds identified in the set of nine Jefferson Parrish
small-volume samples were entered in the database but are not
included in the set of four sample groups. These nine samples
were so grossly contaminated with XAD-2 resin bleed artifacts
that many of the identified species were not found even in
other samples which had substantial XAD-2 resin bleed contami-
nation and are included in the DW sample group. There are 91
compounds in Table ID which were not found in the four data
sets and can unambiguously be attributed to this source. These
materials are typically aromatic hydrocarbons, some of which
contain oxygen.
• Some compounds were deliberately added to the database for con-
vience in anticipation of their detection in samples but were
not subsequently detected in the four sample groups. Isomers
of commonly encountered species or high interest compounds such
as the 53 specific search compounds are included in this cate-
gory. Twenty of the specific search entries in Table Dl were
not found in any sample.
• Preliminary compound identification results were sometimes
added to the first, chemically descriptive level of the data-
base before final review by a senior analyst. In these cases,
compound identifications that were disallowed were, of course,
not entered into the second, concentrate-specific level of the
database. However, these compounds were not removed from the
first level (since the possibility always, existed to correctly
identify the compound in subsequent analyses), so they still
appear in Table Dl.
Of the 2107 entries in Table Dl, 271 are not reported as having been found in
one of the four groups of samples with which the table is correlated.
244
-------
TABLE Dl. COMPOUNDS IN THE CHEMICALLY DESCRIPTIVE LEVEL
OF THE IDENTIFIED COMPOUND DATA BASE—LISTED
BY INCREASING MOLECULAR WEIGHT
MM
55
55
59
6.
60
62
62
62
68
68
72
71
73
7<>
71.
7
85
46
86
86
86
86
86
86
86
66
CAS NO.
621.793
34239279
60355
71238
bl>l*7
117211
751ii.
1.55
230131
I
10711.2
109861.
109475
3031752
581.032
110461
107073
110838
S1792u
531.225
931303
75092
625332
3i.3ii.435
<.97030
12C423
7651.35
11.5113
616V55
104051.
107879
1.675470
556821
625310
m.0.llO
50/6197
115181.
1569502
MATER POLLUTANTS PAGE 1
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTt—THIS LIST HAT CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANT OF THE CONCENTRATES ANALTZEQ
COMMON NAME
1SOCYANOETHANE
N-MIL I NIL tTHENAHlNE
ACETAHIOE
XPROPYL ALCOHOL
ACETIC »C 10
•/.ETHTLENE GLTCOL
VINYL CHLOKIOE
CARBONIC ACID
PTrtA20LE
CTCLOPENTENE
3-aUIEN-c-OL
XOHF (DIMETHYL FORHAMIDE)
N-BUTtLAMlNt
%1-auTANOL
ZTERT-BUTANOL
SEC-BUTYL ALCOHOL
ETHTL FOKMATE
CHLOROACETONITRILE
ETHTLENE GLYCOLi MONOMETfcYL ETHER
XHETHTLAL
ISOPROPYL HTDROPEROXIOE
1.2-3UUNEOIOL
X'PTRIOINt
2-CHLOKOtTHANOL
XCTCLOHEXENE
3.3-OIHETHYLBUTTNE
2-METHYLFUfcAN
2-CYCLOPtTEN-l-ON£
XMETHYLENE CHLORIDE
3-PtNTtN-2-ONE
2.3-OIHYDRO-I.-HETHYLFURAN
TIGALOEHYOE
CYCLOPENIANONE
XCYCLOPKOPYL HETHTL 1C t TONE
2-M£lHTL-2-aUTtNAL
2-PYRROLlDCNt
VINYL ACt-TAIt
XMETHTL PROPTL KETONC
2-Nt!HTL-2-BUT£N-l-OL
3-MEFHYL-2-BUTEN-1-OL
I.-PENTLN-2-OL
1-OXIfeANYLETHANONE
TRIML.IHYLOX1KANE
2-Mi.THTL-3-auT£N-2-OL
3-PtNTtN-2-OL
DATA
OU
921
662
104
580
960
1037
650
985
1070
5
586
734
564
533
602
262
573
1128
851
89
65
183
830
538
175
279
80
922
620
831
114
55
SET CORRELATION
AWT T4
1079
158
832
982
314
1087
22 1)7
623 33
896
468
254
746
946
18
569
99
947
897
497
t
T5
86
87
MOLECULAR FORMULA
C3
C3
C2
C3
C2
C2
cz
Cl
C3
C5
Cd
C3
C".
Ci.
Cl.
Ci.
C3
C2
C3
C3
C3
Cl.
C5
C2
C6
C6
C5
C5
Cl
C5
C5
C5
C5
C5
C5
Ci.
C<>
C5
C5
C5
C5
Cl.
C5
C5
C5
H5 . Nl
H5 . Nl
H5 . Nl
H8 . 01
Hi, . 02
H6 . 02
H3 . CL1
HZ . 33
Hi. . N2
H8
H8 . 01
H7 . Nl
Hil. Nl
HlO. 31
H1G. 01
HlO. Ol
H6 . 02
H2 . NZ
H8 . 02
H8 . N2
H8 . OZ
HlO. 32
H5 . Nl
H5 . 01
HlO
HlO
H6 . Ol
H6 . 01
H2 .CLZ
H8 . Ol
H8 . Ol
H« . 01
H8 . 01
HB . Ol
H4 . 01
H7 . Nl
H6 . OZ
HlO. Ol
HlO. 01
HlO. 31
HID. 01
H6 . 02
HlO. Ol
HlO. 01
Hid. 31
. 01
. 01
.CLZ
.CL1
. 01
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
MATER POLLUTANTS PAGE 2
MM
86
86
86
86
86
8i
88
88
88
88
88
88
88
88
88
88
88
88
88
83
88
89
9.
90
9,
9<
90
9j
90
90
92
9
Si.
Vt
96
9b
CAS NO.
100311.1
1.31038
37^1.650
961.80
96,: 20
11.1786
126998
lc39li
79312
107926
6032297
581.021
/i'.iO
598751.
107891
5i3860
75851.
7581.3
963*1
551.121
62551.7
51796
5631.73
107982
107880
110805
11.1.627
15891.75
513839
50215
108883
131.0337
78955
lt.8996
62533
109068
108891.
108952
67710
79118
1^700 i>
71.839
9.J0687
108971.
IDENTIFIED COMPOUNDS B» MOLECULAR HEIGHT
NOTE—THIS LIST HAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
CONHON NAHE
PROPYLOXIRANE
XOIACETYL
XCROTONIC ACID
XBUTKOLACrONE
OIETHYL KETONE
XETHYL ACc.TATE
X'CHLOrtOPfitNE
XI.I.-OIOXANE
XISCBUTYRIC ACID
XBUTYRIC ACID
1-NETHYLBUTYLALCOHOL
OIETHYL CARBINOL
XN-AMYt ALCOHOL
StC-JSOAMYL ALCOHOL
ALGOL
ACETOIN
XTEST-PENIYL ALCOHOL
NEOPtNTYL ALCOHOL
N.N*-DIM£THYLUREA
METHYL PkOPIONATE
ETHYL ISOPROPYL ETHER
XURETMANE (ETHYLCARBAMATEI
X3-CHLOrtO-2-METHYL PROPENt
l-MtIHOXY-2-PROPANOL
1.3-BUTYLENE GLYCOL
XETHYLENE GLYCOL HONOETHYL ETHERt COXITOL3 CELLOSOLVEI
XOXALIC ACID
2-METHOXY-l-PROPANOL
2. J-BUTANEOIOL
2-HfDROXYPKOPANOIC ACID
XfTOLUcNE
•l-CHLOKO-2 ,3-EPOXYPROPAN£ II CHLOROME THYL8 OXIRANE I
XCHLOROACtTONE
B-PICOLINE
X'ANILINt
ALPHA-PICOLINE
GAHHA-PICOLINE
X»»PH£NOL
QIMtTHYLSULFONL
ZCHLOROACtTIC ACID
l-CHLORO-2-PROPANOL
BROMOME THANE
3-Mt THYLCYCLOHt XENE
2-CYCLOHEXENONE
i,H-PYRAN-<,-ONE
DATA SET CORRELATION t
DU AWT T4 T5
293
1038
426
266
113
24
54
181
683
1129
121
1113
530
402
951
142
45
567
1040
62
729
582
842
961
156
925
724
139
593
210 162
171 114
418
389
684
745
895
1083
703
43
506
103
629
717
318 115
481
324 250
712
554
657
208 163
387
1080 228
160
132
505
369
864
HOLECULAR FORMULA
C5 HlO. 01
H6 . 02
H6 . 02
H6 . 02
C5 HlO. 01
H8 . 02
C". H5 .CL1
H8 . 02
Ci. H8 . 02
Ci. H8 . 02
C5 H12. 02
C5 H12. 02
C5 H12. 01
C5 H12. 01
H8 . 02
H8 . 02
H12. 01
C5 H12. 01
C3 H8 . N2 . 01
CI. H8 . 02
C5 H12. 01
C3 H7 . Nl . 02
CW H7 .CL1
Ci. HlO. 02
Hid. 02
Ci. HlO. 02
C2 H2 . 0 Si
.CL1
H7 . 01 .CL1
H3 .BRt
Hl2
H8 . 31
Hit . 02
+ SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
IH
9b
96
96
96
96
96
93
98
93
98
98
98
98
98
98
93
93
93
93
98
93
98
93
98
98
93
93
93
98
98
93
99
99
99
99
IGU
100
iwo
IOC
100
ll/j
100
100
lOO
lOu
CAS NO.
1120736
2758181
1.562270
10111037
20521<>20
98011
107062
1120725
17571.22
10891.1
H.1797
822673
29161.5
505577
1091.99
758872
1.9607511.
625650
551.11.3
5362505
2501.1.013
16015115
21.97211.
592778
286201.
25659227
l0887t
2008
111281.
1.56
22122367
872501.
176821.7
27151.1.31.
211.1620
25H.1.U52
591786
589388
2088075
108101
198930
211. 1.1.11.
537?S6*3
1003389
11.382 5
HATER POLLUTANTS PAGE 3
IDENTIFIED COMPOUNDS B1 MOLECULAR HEIGHT
NOTE—THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT SEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
DATA SET CORRELATION t
COMMON NAME
I-METHYL-2-CYCLOPENTEN-1-ONE
3-METHYL-2-CYCLOPENTEN-1-ONE
Z «.<1H>-PYRIHI 01 NONE
IN -1MIDAZOLE-3-CARBOXALDEHYDE
2-VINYLCROTONALOEHYOE
t. FURFURAL
X$l,2-OICHLOKOETHANE
2-METHYLCYCLOPENTANONE
3-METHYLCYCLOPENTANONE
7.CYCLOHEXANONE
XMESITYL OXIDE I3-ISOHEXEN-2-ONEI
2-CYCLOHEXENOL
SUBE*ANE
2-HEXENAL
ALLYLACETONE
3-METHYL-1.-PENTEN-2-ONE
1-METHYL-IH-1.2.I.-TRIAZOL-3-AMINE
2t".-OIMfcTHYL-2-PENTENE
2-METHYLTHIOPHENE
i,-METHYL-3-PENTENAL
2-METHYL-1-PENTEN-3-ONE
3.l«-OIHYU*0-&-METHYL-2H-PYkAN
l«-HtXEN-3-ONE
2-HEPTENE
X7-OXABICYCLOII..1.01HEPTANE
. N2
C
-------
TABLE Dl. (Continued)
ho
-P-
00
HH
100
100
lOB
109
110
100
104
100
100
100
100
109
100
100
100
100
1UJ
100
100
100
101
101
101
101
101
102
102
102
102
102
102
102
102
102
102
102
U2
Iy2
102
Iu2
Iu2
102
Iu2
1..2
Ib2
CAS NO.
2
11,173383
5i.77«»275
6121.909
5076200
1501.5600
5b5695
520<<6-METHYL OIOXANE
1-HEXANOL
3-METHYLPENTAN-3-OL
3-HEXANOL
2-HEXANOL
2-METHYLBUTYRIC AGIO
•/.VALERIC ACID
ISOVALERIC ACID
<»-M£THYL-2-PENTANOL
X'OIETHYLNITROSAMINE
2.2-DIMtTHYL-l-BUTANOL
ACETOACETIC ACID
3-HYOROXY-3-METHYL-2-BUT4NONE
TETRAHYDROFURFURYL ALCOHOLS THFA
PIVALIC ACID
2i3-OIMETHYL-2-8UTANOL
3-ETHOXYPROPANAL
2-METHYL-2-PtNTANOL
BUTYL FORMATE
3-METHOXYPENTANE
DM
176
21
566
99
1016
876
122
836
329
229
493
495
682
833
1086
1039
957
57
270
969
179
679
201
46
193
22
95
63
35
1011
630
931
254
147
QQQ
Boo
362
777
100
AWT T4
446
879
922
728
706
727
86
555 147
607
180
302
330
943 183
491
214 25
178
202
204 159
106
177 127
277
442
1054
T5
113
83
98
MOLECULAR
C6 H12.
C6
C5
C5
C5
C5
C6
C6
C5
C6
C6
C<.
C6
C6
C6
C6
C6
C5
C5
C6
C5
C6
C5
C6
C5
C5
C6
C6
C6
Cb
C5
C5
C5
C6
Cl,
C6
Cl.
C5
C5
C5
C6
C5
C6
C5
C6
Hl2.
H8 .
H8 .
H8 .
H8 .
H12.
H12.
H8 .
H12.
H12.
H9 .
H12.
H12.
Hl2.
H12.
H12.
H8 .
H8 .
H12.
Hll.
HIS.
Hll.
HIS.
Hll.
H10.
HI"..
Hit.
H1U.
Hll..
HlO.
HlO.
HlO.
HH..
HlO.
Hll..
H6 .
HlO.
HlO.
Hid.
Hll..
Hia.
Hll..
HlO.
HH.
FORMULA
01
01
02
02
02
02
01
01
02
01
Ol
02
31
01
01
01
01
02
02
01
Nl
Nl
Nl
Nl
Nl
02
01
01
01
01
02
02
02
01
N2
01
03
02
32
02
01
02
01
02
01
. Bl
. 01
. 01
. 01
. 01
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
MATER POLLUTANTS PAGE 5
MM
11.2
11*2
luZ
luZ
10Z
10Z
Iu2
lu2
It3
10".
1L".
10".
1U<>
In".
ill".
10".
in
IL".
ll>".
101.
IbU
ib".
ID*.
101.
1.1.
H.1,
Ub
1.6
Ibb
Ibb
Ibb
106
lib
iLb
Ibb
lOb
lib
1U7
107
n, r
ior
107
1.7
1.9
luS
CAS NO.
36960222
339361. <•
".1/16119
96 1.0 Z
108211.
73Z6I.67
Z679870
589355
10QI.70
1001,25
11.1822
53778737
17773658
111320
6837U5
591.616
5166358
7778850
691.871
2807309
".71,1,109
101.7111. t<
13i.17i.31
53778720
5b9",6d8
35876"<2
951.76
108383
1061.23
10u m i.
10b 627
6Z8900
598798
51.3599
753899
111 1<6F>
539800
1081.85
1081.71,
53675",
583619
569935
ad9i<
1558171,
5910891,
CO
1-
".-
/. (E
3-
IS
TE
2-
3-
BE
X'lST
X.H«
1-
Z-
"<-
3-
Z-
3-
1.
81
N-
1-
1-
1-
3-
1,
X "
•/.to-
X.»M-
•/.IP-
«tl
•/.at
ME
2-
Al
Ni
o:
2
X.2,
xz,
"<•
2
2
ai
i,
2
IDENTIFIED COMPOUNDS BY MOLECULAR WEIGHT
NOTE—THIS LIST HAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
DATA SET CORRELATION t
COMMON NAME
l-HYOROXY-3-NETHYL-Z-BUTANONE
-HYOROXY-J-METHYL-3-BUTANONE
•/. i . 0".
CIS. H12. OZ
CS . H9 .CLl
CS . HlZ. OZ
C<< . H5 . 01
C<< . H8 . 03
CS . H9 .CL1
CS . HlZ. OZ
C8 . H8
CS . HlZ. OZ
CS . Hi2. OZ
CS . HlZ. OZ
CS . H9 .CLl
CS . HlZ. OZ
C". . H6 . 03
CS . HlZ. OZ
C8 . H10
ca . HIO
ca . HIO
ca . HIO
C7 . H6 . 01
C". . HIO. 03
C3 . H3 . OZ
CS . Hit. CLl
CS . H11.CL1
c<* . HID. 03
C7 . H6 . 01
C7 . H9 . Nl
C7 , H9 . Ni
C7 . H9 . Nl
C7 . H9 . Nl
C7 . H9 . Nl
C7 . H9 . Nl
C6 . H8 . HZ
Cb . MS . NZ
.CLl
.CLl
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
MH
109
ioa
ua
109
i.a
169
too
109
106
Iu9
110
li<
liJ
110
lib
ro iiJ
'A ii"
0 110
114
110
110
110
111
lil
112
112
1*2
li.2
112
112
112
112
112
112
112
112
112
112
112
112
112
112
112
1*2
112
CAS NO.
10939*
106*1.5
951.87
100516
1603*1*
598787
111693
100663
5 63 8* a
3014120
1193186
280331
1192627
53783872
3*L 67759
^67*108
1*072867
53783883
93188*
577132*
620020
18669528
629083
6*07358
16106595
200196*1
11166Q
108907
881*2
3*31*8*6
5166530
2511913
77*069*
600*600
80717
3726*7*
23758272
3306116*
1713333
110**1
* 88 93 7
167*7505
123331
68*9*6
671*007
MATER POLLUTANTS PAGE 6
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE—THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
COMMON NAME
XMETA-CRESOL
X»P-CRESOL
XO-CRtSOL
XBENZYL ALCOHOL
2-AMINO-5-PICOLINE
ALPHA-CHLOROPROPIONIC ACID
OICYANOHLXANE
HETHOXYBENZENE
3-CHLORO-i-BUTANOL
OICHLOROACET ONITRILE
3-METHYL-Z-CYCLOHEXEN-l-ONE
9ICYC.LOC2.2.2) OCTANE
X.2-ACETYLFURAN
2-NORBORNENE-7-OL
3-PROPYLCYCLOPENTENE
1,2-DIMETHYLCYCLOHEXENE
*,*-OIHETHYLCYCLOHEXENE
3-METHOXY-l,3,*-HEXATRIENE
CYCLOOCTENE
SPIRO(2.*)HEPTAN-2-:ONE
S-METHYLFUfcFURAL
2,3-DI«ETHYL-l,*-HEXAOIENE
N-HEXYLCYANIOE
N-CYGLOHEXYLIOENE METHAN4MINE
*,5-DIMETHYL-l-HEXENE
5.5-OIMETHYL-2-FURANONE
1-OCTENE
ZCHLOR08ENZENE
X2-FUROIC ACID
2,3-OIHYDRO-i»-ti-METHYLErHYLIFURAN
5-METHYL-3-HEXEN-2-ONE
PENTYL TRIMETHYLENE
S-ETHOXY-J-METHYL-^-BUTY'JE
1-CYCLOPENTYLETHANONE
2-HYDROXY-3-HETHYL-2-CYCLOPENTEN-1-ONE
l-ETHYL-3-METHYLCYCLOPENTANE
l-METHYL-2-CYCLOHEXEN-i-OL
i-METHYL-3-CYCLOHEXEN-l-DL
l-METHYL-7-OXABICYCLO(*.1.0)HEPTANE
XSOR8IU ACID
3-FUROIC ACID
1-ETHYL-METHYLCYCLOPENTANE
Xl,2-OIHYDRO-3,6-PYRIOAZINEOICNE
3i<.-OIHcTHYL-3-PENTEN-2-ON£
5-H£PTtfc-2-ONt
DATA SET CORRELATION t
DW AWT T4 T5
199
182
821
90
450
596
462
608
893
281
1014
251
640
1151
318
874
491
400
30
1077
108
574
297
308
348
268
846
1070
383
658
667
378
585
401
432
304
687
939
937
229
170
100
185
183
132
137
151 115
71
MOLECULAR
C7 H8
C7
C7
C7
C6
C3
C6
C7
C
C7
C7
Ha
H8
Ha
Ha
H5
H8
HB
H9
HI
H10
HI*
H6
HlO
HI*
HI*
HI*
HlO.
Hi*
H13.
H6 .
HI*
H13.
H13.
H16
H8 .
Hl6
H5 .
H* .
H12.
H1Z.
H16
H12.
H12.
Ha .
Hie
H12.
H12.
HI?.
Ha .
H* .
H16
H* .
H12.
H12.
FORMULA
01
01
01
01
N2
02
N2
01
01
Nl
01
02
01
01
01
32
Nl
Nl
02
CL1
03
01
31
01
01
02
01
01
31
02
03
N2
01
01
.CL1
.CL1
.CL2
. 02
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
MM
11Z
113
il3
113
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
lid
ltd
lid
lid
lid
lid
lid
ild
CAS NO.
SOZdZl
1121922
93l20d
105602
589d35
123193
1 lO 1 3 d
3123975
51d5017
110d30
695067
592278
56052950
823223
Id925963
17257817
56052836
dlO 65978
106351.
dl65393d
119lOdd
1577226
623563
d 1.78631
3521913
7d93585
592132
17257828
17612350
53897328
5363633
279dd792
931566
13861977
53229393
53897317
533600
33d6776d
1 8 60 3 9 5
123206
53229«.l7
d2326d38
dSZttjei
598398
HATER POLLUTANTS PAGE 7
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE—THIS LIST HAY CONTAIN COHPOUNOS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
COMMON NAHE
CYCLOHEPTANONE
OCTAHYDROAZOCINE
N-HcTHYL-c-PIPERIDINONE
HEXAHYDRO-2H-AZEPINE-Z-ONE
2,d-OIHETHYL HEXANE
d-HEPTANONE
2.5-HEXANEDIONE
5,5-OIMETHYLDIHYOROFURANONE
3. 5-DIMETMYLOIHYDROFURANONE
METHYL N-AMYL KETONE
5-ETHYLOIHYDRO-2I3HI-FURANONE
Z-McTHYLHEPTANE
TRANS-2-ETHYL-3-PROPYLOXIRANE
6-METHYL-TtTRAHYORO-2-PY|JANONE
2-BUTYL-3-METHYLOXIRANt
3.d-EPOXY-2-HEXANONE
l-HETHOXY-2-HEXENE
<<-METHVLHEXANAL
Z6-HYOROXYCAPROIC ACID LAC TONE
ETHYL BUTYL KETONE
TRANS-3-METHYL-3-PENTENOIC ACID
2-HEXENOIC ACID
5-HEXENOIC ACID
ETHYL ISOBUTYL KtTONt
l-»3,3-DIM£THYLOXIRANYLIETHANON£
l-H£PTtN-i.-OL
ACETYL ISOBUTYRYL
2,5-OIMETHYLHEXANE
3,d-£POXY-3-£THYL-2-BUTANON£
Z.Z-OIMETHYL-3-PROPYLOXIRANE
Z-ETMYL-3-PROPYLOXiaANE
l-<£THNYLOXY»PtNTANE
I, ".-DIMETHYL PENT ANAL
METHOXYCYCLOHEXANE
d,d-oiMETHYLOiHYOROFURANON£
U-METHYLBUTYLIOXIRANE
2-METHYL-2-ISOBUTYLOXIRANE
Z-HYDROXYCYCLOHEXANONE
Z-HEPTENOL
5-MtTHYLHE XANOL
YINYL BUIYKATE
3-METHYL3UTYLOXIRANE
2-MtrHYL-Z-ll-HETH»LPROPYL>-OXIR«NE
ALLYL-1.3-DIOXANL
£.i-OICHLOROETH4NOL
DATA SET CORRELATION t
DW AWT T4 T5
296
202
244
386
1059
859
938
608
328
378
129
130
261
598
130
67
93 64
85
284
264
819
1058
385
1126
601
798
268
606
611
898
1136
909
834
1110
200
553
282
554
560
531
539
1027
371
847
436
596
323
440
867
447
876
592
317
499
738
MOLECULAR FORMULA
C7 . H1Z. 01
C7 . HIS. Nl
C6 . Hll. Nl
C6 . Hll. Nl
C8 . H18
C7 . Hid. 01
C6 . HlO. 02
C6 . HlO. OZ
C6 . HlO. 02
C7 . Hid. 01
C6 . HlO. 02
C8 . Hid
C7 . Hid. 01
C6 . HlO. 02
C7 . Hid. 01
C6 . HlO. 02
C7 . Hid. 01
C7 . Hid. 01
C6 . HlO. 02
C7 . Hid. 01
C6 . HlO. 02
C6 . HlO. OZ
C6 . HlO. OZ
C7 . Hid. 01
C6 . HlO. 02
C7 . Hid. 01
C6 . HlO. 32
C8 . Hid
C6 . HlO. 02
C7 . Hid. 01
C7 . Hid. 01
C7 . Hid. 01
C7 . Hid. 01
C7 . Hid. 01
C6 . HlO. 32
C7 . Hid. 01
C7 . Hid. 01
C6 . HlO. 02
C7 . Hid. 01
cr . Hid. 01
C6 . HlO. 02
C7 . H12. 01
C7 . Hid. 31
C6 . HlO. 02
C2 . Hd . 01
. 01
. 01
.BR1
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
MH
11
11".
111.
116
116
116
116
116
116
116
116
116
116
Ii6
116
Hi
116
116
116
116
116
116
116
116
116
116
116
116
116
116
ii6
116
116
116
116
116
116
116
116
Hi
116
116
116
115
CAS NO.
110123
7379126
598389
1<>36357
1O70833
11.2621
7319235
88095
595379
97610
1231.22
123861.
Iu5it31
6> . 01
H16. 01
H12. 02
H12. 02
H12. 02
H12. 02
H12. 02
H12. 02
H12. 02
H12. 02
H12. 02
H12. 02
H12. 02
H8
H16. 01
H16. 01
HB . 03
H12. N2
H16. 01
H12. 02
H16. 01
H16. 01
H16. 01
H16. 01
H16. Ol
H16. 01
H16. 01
H16. 01
H16. 01
H16. 01
H16. 01
H8
H12. 02
H12. 02
H16. 01
H12. 02
H12. 02
H16. 01
H16. 01
H16. 01
H16. 01
H5 . 01
HI?. 02
.CL2
. 01
.CL1
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
MATER POLLUTANTS PAG£ 9
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE—THIS LIST MAY CONTAIN COMPOUNDS THAT HAYE NOT BEEN FOUND IN ANT OF THE CONCENTRATES ANALYZED
MM
116
116
116
116
lib
116
116
US
117
117
11)
118
119
116
K> its
Oi . ..
CO ll8
119
li.9
119
11)
119
11)
119
118
118
119
119
119
119
118
119
119
11)
12 j
12u
I2il
Itj
12u
120
l£j
l£J
120
1 2.
12ii
CAS NO.
759057
6111,2776
1231,1,2
931179
1,3591,50
21,1,1976
3. 02
HI .CL3
Hli>. 02
HlO
HlO
Hli.. 02
H6 . 01
Hl<>. 02
HH.. 01
H11.CL1
HlO. 03
HlO. 03
Hli.. 02
HlO
HlO. 03
HlO. 03
HlO. 03
HlO. 02
H6 . Oi,
Hli,. 02
Hli,. 02
HlO. 03
HlO
H12
H12
H12
H12
H12
H12
H12
H8 . 01
H12
H12. 03
H5 . 02 .CL1
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (continued)
MATER POLLUTANTS PAGE it,
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE--THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOf SEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
DATA SET CORRELATION t
MM
12)
I2y
120
12j
121
121
121
121
121
121
121
121
121
122
122
It2
122
122
to 122
<•" 122
*• 121
122
122
123
i£<»
12*
121.
12*
121.
12*
12<>
12*
12*
12*
1 i**
12*
12*
12*
125*
125
125
126
126
125
126
CAS NO.
*052903l
52920*
126330
111773
108758
622322
1122390
695987
10*905
1*628*6
2233296
1122696
3999788
65850
105679
958u7
10*93b
90006
98851
10083*
123079
95658
108689
98953
Il23u97
90051
*961U6
2*15695*
23799259
25172069
55683211
28790865
150765
932661
x *t d ^ S'ti
166*70**
50*15*
628397
19615271
60 96222
110576
95*98
110930
12*lia
25**7692
COMMON NAME
i.-CHLORO-3-BUTENOIC AGIO
0-TOLUALDEHYOE
TETRAHYORO-l.l-OIOXIDE THIOPHENE
DIETHYLENt GLYCOLt MONOMETHYL ETHER
2.I..6-COLLIOINE
8ENZALOEHYOEOXIME
2.<.,5-COLLlDINE
2,3i5-COLLlOINE
5-ETHYL-t-PICOLINE
2,3,6-TRIMETHYLPYRIOINE
2,3,I.-TRIMETHYLPYRIDINE
2-tTHYL-6-PICOLINE
3-ETHYL-S-METHYLPYRIOINE
•/.9ENZOIC ACID
X»*2.l>-DIM£THYLPHtNOL (XYLENOL)
/.•2t'.-DIAHINOTOLUENE
P-MtlHYLANISOLt
PHLOROL
ZMETHYLPHtNYL CARBINOL
3-HYDROXYBENZALDEHYDE
II-ETHYLPHENOL
3,1,-DIMETHYLPHENOL
3.S-OIMETHYLPHENOL
/.'UNITROBENZENE
3,5-OIMETHYL-2-CYCLOHEXEN-l-ONE
XGUAIACOL
OCTAHYDROINOENC
3.5.5-TRIMETHYL-2-CYCLOPENTEN-1-ONE
1-MtTHYL-H-METHYLENESUBERANE
3,7-OCTADIEN-2-ONE
J,<»,5-TRIMtTHYL-2-CYCLOPENTtN-l-ONE
2.3,<.-TRIMETHYL-2-CYCLOPENTEN-l-ON£
XP-NETHOXYPHENOL (HYOROQUI NONE, MONOMETHYL ETHER)
1-(l-CYCLOHtX£N-l-YL)ETH»NONE
6-ME THYL-B ICY CLO («..!. 01 HE PTA NONE
6-HETHYL-3.5-HEPTADIEN-2-ONE
XORCINOL
2-(2-CHLOROETHOXYIETHANOL
l-ACETYL-i,2,3,i»-T£TRAHYDROPYRIOINE
BUTYL THIAZOLE
It
-------
TABLE Dl. (Continued)
MATER POLLUTANTS PAGE 11
IDENTIFIED COHPOUNOS 8f MOLECULAR HEIGHT
NOTE--THIS LIST HAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
MM
126
126
IZb
IZb
I2b
I2b
IZb
I2b
lib
l2b
IZb
I2b
12b
12b
12b
IZb
12b
12b
12b
126
i2b
126
12b
126
126
127
127
127
127
127
It7
127
127
120
128
128
121
129
128
128
121
128
128
itl
121
CAS NO.
77781
53517923
100<.
-------
TABLE Dl. (Continued)
MH
123
12S
12»
129
12S
128
123
129
129
128
129
128
123
128
129
N3 129
Ui 128
°" 128
129
129
128
129
129
129
129
128
129
129
123
128
128
129
128
128
128
129
129
129
123
129
129
131,
1J-
130
13u
CAS NO.
Ii)0
111137
5<»1855
55670092
1.361 51.6
6137H7
7317020
15120997
517237
181.09171
533772<.
589639
3720227
21051.00
22lb3i.it
171.29026
15726155
105215
11 22 60 7
119653
169620
-------
TABLE Dl. (Continued)
MM
130
1JO
130
130
134
130
130
130
130
130
130
130
130
130
130
130
130
UO
130
130
13(1
130
130
130
130
130
130
130
130
130
130
130
130
130
13ft
1-NJ
130
1 30
130
l3l
132
13?
1 32
1 3t
132
CAS NO.
816660
6281,66
lllil.8
58973185
3l367i.6l
1185393
19889373
106707
79016
1.1.33856
132171.0
<,i,753u
1561111
-------
TABLE Dl. (Continued)
00
MATER POLLUTANTS PAGE Id
HH
132
132
132
132
132
132
132
132
132
132
132
132
132
132
132
132
132
132
132
132
132
132
132
133
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
CAS NO.
83330
111897
87d35l
537920d
2039896
10d552
71556
1560061
7681.90
2039909
752562d
3d5d077
158701.8
5572dfldd
11576d
762d69
756d638
1195320
202252d5
33*77871
53907952
5()86
8898
13351730
I07dd37
135988
28 70 Odd
93d8Q5
1758889
5278dd
93d7d7
Idl936
107di75
135013
lGd518
87ddl9
105055
d88233
95932
933982
527537
629061
71693d8
98u66
.»»9jJ
C
1
1
5
3
2
XC
•/.Ml
Cl
i,
2
3-
d
0-
5'
2,
i-
0'
p-
2-
1,
1-
PI
7-
2'
1-
SI
2-
d-
2-
2-
1-
1.
1-
li
N-
1-
li
1,
01
1-
i:
i-
BE
T£
0]
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE—THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT 3EEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
11 DATA SET CORRELATION t
COMMON NAME
1-INOANONE
1,5-OIHE THOX» PENTANE
5-METHVL INDAN
3,5-OIMETHYL STYRENE
2.5-OIMETHYL STYRENE
XCINNAHALUEHYOE
'/.METHYL CHLOROFORM
CROTONVLBENZENE
«2-METHYL-l-PROPENYLI BENZENE
2,6-OIN£THYLSTYR£NE
3-ETHYLSTYkENE
d-ETHYLSTYRENE
0-ALLYLTOLUENE
5-METHOXY-2-METHYL-2-PENTANOL
2,2-OIETHYLPROPYLENE GLYC OL
1-MtTHYLHt XYLHYOROPEROXIOE
0-ETHYLSTYRENE
P-ISOPROPENYLTOLUENE
2-ETHYL PENTANOIC ACID
It 2,3,3A-TtTRAHYDRO AZ.JLENE
l-U-METHYLPROPOXYI-2-PROPANOL
PROPYL&NE GLYCOL MONOBUTYL ETHER
7-METHYLBENZOFURAN
2-METHYLBtNZOTRIAZOLE
l-METHYL-3-PROPYL BENZENE
SEC-BUTYL BENZENE
2-ETHYL-1.3-DIMETHYL BENZENE
d-£THYL-l,2-OIMETHYL BENZENE
2-ETHYL-i, d-DIMETHYL BENZENE
2-ISOPROPYL TOLUENE (0-CYMENE>
1-ETHYL-3.5-DIMETHYL BENZENE
1,3-OIETHYL BENZENE
l-METHYL-2-PROPYL BENZENE
1,2-OIETHYL BENZENE
N-8UTYLBENZENE
l-ETHYL-i.d-DIMtTHYL BENZENE
l.d-OIETHYL BENZENE
l,2,3.d-TETRAMETHYL BENZENE
OURENE
l-£THYL-2t3-DIM£THYL BENZENE
ISODURENE
1-CHLOftOHEPTANE
BENZOFURANONE
TERT-BUTYLBENZENE
OIETHYLENE GLYCOL, MONOMETHYL ETHER (CARBITOLI
uw
1118
456
982
1152
767
1044
186
166
713
551
105
283
986
1087
1021
8
657
1091
1090
131
133
132
1042
1092
194
AMI 14 It)
587 42
625
1012 5
132
655
486
276
770
4
1096 233 2
729
1048 27
146
998
783 47
338
184 227 49
615 231
341 222
772 3
515 224
9
525
521 232
187 8
754
549
522
189
508
365
979
371
MOLECULAR
C9 . H6 .
C7 . H16.
ClO. H12
C1U. H12
CIO. H1Z
C9 . H8 .
FORMULA
01
02
01
C2 . H3 .CL3
CIO. H12
ClO. H12
CIO. H12
CIO. H1Z
ClO. H12
ClO. H12
C7 . H16.
C7 . H16.
C7 . H16.
ClO. H12
CIO. H12
C7 . Hid.
CIO. H12
C7 . H16.
C7 . H16.
C9 . H8 .
C7 . H7 .
ClO. Hid
CIO. Hid
ClO. Hid
CIO. Hid
CIO. Hid
CIO. Hid
CIO. Hid
CIO. Hid
CIO. Hid
CIO. Hid
CIO. Hid
ClO. Hid
CIO. Hid.
CIO. Hid
C1C. Hid
ClO. Hid
CIO. Hid
C7 . H15.
C8 . H6 .
CIO. Hid
C6 . Hid.
02
02
02
02
02
02
01
N3
CL1
02
03
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
MM
1 Jd
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
13d
131.
13d
13d
13d
13d
13d
13d
Ud
13d
13d
135
135
135
135
135
135
135
135
136
I3b
136
136
136
136
CAS NO.
536932
I07d551
99876
535773
200
201
202
10d5dl
205
206
20 a
209
87dl2
106627
53951501
1.71.8781
57799d2
d98265d2
103797
577162
767986
2085883
93550
26dddl99
621636
122069
5973717
110985
6628801.
29538770
95158
95169
27216i
99036
103833
369*7369
9d699
10381.1.
6u86
11891)1
93583
10382?
990<.7
999d5
138363
HATER POLLUTANTS PAGE IS
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE—THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
DATA SET CORRELATION t
COMMON NAME
ISOSUTYL BENZENE
1-METHYL-d-PROPYLBENZENE
XP-CYMENE (P-ISOPROPYL TOLUENE)
META-CYMENE (M-ISOPROPYL TOLUENE*
DIMETHYL ETHYL BtNZENE
DIMETHYL ETHYL BENZENE
DIMETHYL ETHYL BENZENE
XCINNAHVL ALCOHOL
METHYL-N-PROPYLBENZENE
ME THYL-N-PROPYLBENZENE
CYMENE IISOMER UNKNOWN!
CYMENE (ISOHER UNKNOHN)
PHTHALIOE
2- (2-HYDfcOXYPROPOXYI -1-PROPANOL (A OIPROPYLENE GLYCOLI
ETHYLBtNZALOEHYOE
P-ETHYLBENZALOEHYOE
2,5-OIMETHYLBENZALOEHYDE
2,3-BIS(M£IHYLENEI-BICYCLO[3.2.110CTANE
BENZYL METHYL KETONt
2»-M£THYLACETOPHENONE
l.d-OIHYORO-l-M£THYL-d-OXONICOTINONITRILE
X2-METHYL-2-PHENYLOXIRANE
XPROPIOPHcNONE
1- (METHYLPHENYLIETHANONE
2,2-OIETHOXYETHANOL
P-MtTMYL ACETOPHENONE
3,d-OIMETHYLB£NZALD£HYDE
DIPROPYLENE GLYCOL
2-CHLOROCYCLOHEXANOL
FRANS-I.-CHLOROCYCLOHEXANOL
3ENZOTHIOPHENE
BENZOTHIAZOLt
1.2-SENZISOTHIAZOLE
XM- AMI NOACtTOPHE NONE
N, N-OIMtTHYL BENZYL AMI NE
I.-ETHYL-2. 6-DIMETHYL PYRIOINE
N-(2-METHYLPH£NYL»FORMAM10E
N-PHENYL ACETAMIDE
2-MtrHYLBENZAMIDl:
OrtTHO-TOLUIC ACID
'/.METHYL BENZOATt
•/.PHtNYLACtTIC ACID
M-TOLUIC ACID
P-TOLUIC ACID
l-MtIH»L-'t-(l-McTHYLtTHENYLI-CYCLOH£XENE
DM
1068
1124
241
397
184
445
208
214
446
826
862
935
369
840
865
972
467
82U
855
852
221
9
49
72
73
AWT
971
524
188
972
550
551
973
988
631
632
838
839
247
274
1094
155
494
903
1058
705
995
30
553
35
15
42
854
T4
221
225
226
113
157
74
48
13
69
121
128
T5
149
53
188
155
181
120
16
61
103
104
MOLECULAR FORMULA
CIO
CIO
CIO
Clb
CIO
CIO
cm
C9
CIO
CIO
Clb
Clb
C8
C6
C9
C9
C9
etc
C9
C9
C7
C9
C9
C9
C6
C9
C9
C6
C6
C6
C8
C7
C7
C8
C9
C9
C8
C8
C8
C8
C8
C8
C8
ca
C1L
HI,
Hid
Hid
Hid
Hid
Hid
Hid
H10. 01
Hid
Hid
Hid
Hid
H6 . 02
Hid. 33
HlO. 01
H10. 01
HlO. 01
Hid
HlO. 01
HlO. 01
H6 . N2
Hit. 01
HlO. 01
HlO. 01
Hid. 03
HlO. 01
HlO. 01
Hid. N3
Hll. 01
Hll. 01
H6 . SI
H5 . Nl
H5 . Nl
H9 . Nl
H13. Nl
HU. Nl
H9 . Nl
H9 . Nl
H9 . Nl
na . 02
H8 . 02
Ha . 02
H8 . 02
H8 . 02
H16
. 01
.CL1
.CL1
. Si
. SI
. 01
. 01
. 01
. 01
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
MH
136
136
136
136
136
136
136
136
136
137
137
137
137
139
138
138
138
139
138
13»
139
138
139
139
138
138
138
139
138
138
138
139
138
13)
139
139
13)
125
139
Idi
IdO
IdO
idj
Id.
IdO
CAS NO.
764592
6179d7
d3ld2d3d
536505
591311
7339479
d0133d7
998d3
622855
118923
S2069d
88722
9999b
d71t!2
990 98
78591
69727
I7299dll
17d29297
286761
622253
d930l6
137d773d
Id377ll8
55242901
93561
47d680
62381d
5d955
13837713
122996
768503
151140
8997
100027
2115Q016
20189d28
17825864
3717155
I67d335
8739d9
872059
17773669
165 ,-5056
d3d26Q3
HATER POLLUTANTS PAGE 16
IDENTIFIED COHPOUNDS 81 MOLECULAR HEIGHT
NOTE—THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN AN* OF THE CONCENTRATES ANALYZED
DATA SET CORRELATION t
COMMON NANE
d-ETHYLB£NZYL ALCOHOL
Z2-PHENYLISOPROPANOL
3.5-NONA01EN-7-YL-2-OL
P.ALPHA-OIMETHYL8ENZYL ALCOHOL
M-ANISALOtHYOE
I'HEfHOXYETHYLBENZENE
d-MtTHYL£NE-l-U-METHYLETHYL»CYCLOHEX£NE
PHENYLPROPYL ETHER
XANTHRANILIC AGIO
3-ETMYL-2td,5-TRIMETHYL-lH-PYRROLE
0-NITROTOLUENE
P-NITROTOLUENE
3i5,5-TRIHETHYLCYCLOH£X-J-EN-l,-ONE
X*M-NITROANILINE
HSOPHOKONt
^SALICYLIC ACID
3td,d-TRIM£THYL-2-CYCLOHEXEN-l-ONE
!.,<>,S-T«IMtTHYL-2-C»CLOHEX£N-l-ONE
BICYCLO OECANE
CHLOROVINYLBENZENE
OECALIN
2-ll-H£THYLETHYLlOENEICYCLOH£XANONE
1-ll-CYCLOHEPTEN-l-YLIETrlANONE
3.8-NONAOIEN-2-ONE
'/.STYRtNE GLYCOL
1-CYCLOHEXYLIOENE ACETONE
XOIETMYL SULFITE
PENTYLtNETETRAZOLE
M-MENTH-K 71-ENE IRI-I-I
2-PHENOXYETHANOL
l-ll-CYCLOHEXEN-l-LYI-2-PROPANONE
1, J-OIHETHOXY BENZENE
3,d-OIHYOftOXYBENZALOEHYDE
K»P-NITRO PHENOL
BETA, BETA-DIMETHYL HISTAMINE
3-ETHYL-d-«ETHYL-lH-PYRROLE-2« 5-01 ONE
2,3-dimethylmaleimide
(>-HETHYLaENZALD£HYDE OXIME
i,2-OICHLOM>PENTAN£
3.3,5-TKINETHYCYCLOHEXANONE
OECYLcNt
2t2-OICHLORO-3-H£THYL8UTtNE
2,6-OIM£IHYL-2-HEPT£N-<)-ONE
d-METHYL-3-CYCLOHEX£NE-l-CARBOXYLIC ACID
DM
AWT
T4
T5
764
226
323
1122
686
158
182
395
75
47
698
968
644
607
325
889
918
1028
365
1051
398
576
195
196
811
628
1093
477
64 78
194
372
996
230 76
110 143 105
822
384
626
993
595
1069
1024
192
507
792
251
665
609
671
MOLECULAR FORMULA
C9
C9
C9
C9
C8
Ct
C9
CIO
C9
C7
C9
C7
C7
C9
C6
C9
C7
C9
C9
Clt
C8
CIO
C9
C9
C9
C8
C9
C<>
C6
CIO
C8
C9
C8
C7
C6
C7
C7
C6
Ct
C5
C9
CU
C5
C9
C8
H12. 01
Hl<>. 01
H12. 01
H1Z. 01
H8 . 02
HB . 02
H12. 01
H16
H12. 01
H7 . Nl
HIS. Nl
H7 . Nl
H7 . Nl
HI"). 01
H6 . N2
Hl<>. 01
H6 . 03
HI"). 01
HIS. 01
H18
H7 . CL1
H18
Hl
-------
TABLE Dl. (Continued)
HATER POLLUTANTS PAGE 17
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE — THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANV OF THE CONCENTRATES ANALYZED
MM CAS NO. COMMON NAME
11.0 5071,59 AMYLENE OICHLORIDE
11.0 23010073 1.3-OICHLOKO-2-METHYLBUTANE (A OICHLOROPENTANEI
1W 21.03379 2.2,6-TRIHETHYLCYCLOHEXANONE
11.0 625672 2.1.-OICHLOROPENTANE
11.0 3508789 3-ALLYL-2, I.-PENTANEDIONE
11.0 3301.6810 7-METHYL-3-OCTEN-2-ONE
!•*» 192821* 3,.
Hid.
H18.
HI*.
HI, .
HID.
Hl».
HID.
H7 .
CL2
CL2
01
CL2
02
01
02
03
02
01
01
01
CL1
SI
01
02
02
03
31
02
Ni
Nl
Nl
Nl
02
02
01
02
02
01
02
02
01
02
02
01
Oi
01
01
.CL2
.CL2
.CL2
. 02
. 02
. 01
. 01
.CL2
.CL2
.CLZ
.Cll
(Continued)
-------
TABLE Dl. (Continued)
HATER POLLUTANTS PAGE 18
IDENTIFIED COMPOUNDS 8Y MOLECULAR HEIGHT
NOTE—THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
DATA SET CORRELATION t
MH
1*2
1*2
1*2
1*2
1*2
1*2
1*3
1*3
1*3
1*3
1*3
1*3
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
1**
CAS NO.
*62lO*9
1829*898
*3315*8
2051301
15*0381
H032933
3*003775
91598
20193231
1721933
1.91350
1125800
9163*
115673
12*072
1*9575
2233003
101*
706
705
*10659l2
1188029
109217
819976
1008
1009
1121.136
*165*0*0
25671*8
21*00259
18636550
6299667
1573280
19*2*29*
97870
195*9770
6376*9
5185977
933*0*
623938
5320*572
5932796
17*29059
195*9736
19780*06
COMMON NAME
*-ISOPROPYLCYCLOHEXANOL
*-OCTENOIC ACIO
*-M£THYLCYCLOHEXANE CARBOXYLIC ACIO
2.6-DIMETHYLOCTANE
3-ISOPROPYL-2,*-PENTANEOIONE
2,3,6-TRIHETHYLHEPTANE
5-BUTYLOIHYORO-2-FURANONE
X>2-NAPHTHYLAMINE
N- PROPYL-1 -HE XA NAMINE
1- METHYL IS OQUI NOLI NE
XP-TOLUOUINONE
XM-TOLUQUINONE
XQUINAIOINE
5-M£THYL-5-£THYL-2,*-OXAZOLIOINEDIONE
•/.CAPRYLIC ACIO
2-ETHYLHEXANOIC ACIO
3,3,3-TRICHLOROPROPENE
3-METHOXY-2-NETHYL-2-PENTENOIC ACIO
ETHYL HEXANOIC ACID
ETHYL HEXANOIC ACID
3-ETHYLHEXANOIC ACIO
2-HETHYLHEPTANOIC ACID
BUTYL BUTYRATE
2-BUTYL-N-BUTYRATE
2-METHOXY-3-METHYL-2-PENTENOIC ACID
2-METHOXY-*-METHYL-2-PENTENOIC ACID
l.a-CYGLOBUTANEOICAftOOXYl USE CAS HO. 488211, NEXT PAGE
*-KETOISOHEPTANOIC ACID
1,1,3-TRICHLORO-l-PROPENE
1.1,2-TRICHLORO-l-PROPENE
1,1-OIMETHYL INOENE
*-ETHYLH£XANOIC ACID
3.6-DIMETHYL-3-HEPTANOL
*,*,5,5-TETRAHETHYL-l,3-BIOXOLAN-2-ONE
8UTYL ISOBUTYRATE
2, *- DIMETHYL-*- HE PTANOL
TETRAHYOROFURFURYL ACETATE
5-«ACETYLOXY)-2-PENTANONE
1,1-OIMETHOXYCYCLOHEXANE
5-NONANOL
1,2-DIMETHYL INOENE
*-NONANOL
6-METHOXY-2-METHYL-3-HEXANONE
2, 6-OIMETH YL-3-HEPTA NOL
5-ETHYL-2-HEPTANOL
DM
534
1017
1009
1030
1001
700
1055
1008
971
48
71
117
623
1111
316
615
587
299
14
544
428
869
1015
598
884
324
313
591
1141
1143
1145
1147
239
507
508
280
AWT
391
1036
394
495
1065
915
33
9
978
433
107
113
117
70
419
262
«./ J
652
1021
1084
T4 T5
109 184
4 161
133
211
MOLECULAR FORMULA
C9
C8
ce
CIO
C8
CIO
C8
ClO
C9
CIO
ClO
CIO
ClO
C6
C8
C8
C3
C7
C8
ce
C8
C8
C8
C8
C7
C7
C fi.
C7
C3
C3
Cll
C8
C9
C7
C8
C9
C7
C7
C8
C9
Cll
C9
C8
C9
C9
H18. 01
Hit. 02
Hlii. 02
H22
Hli.. 01
H22
HHi. 02
H9 . Nl
H21. Nl
H9 . Nl
H9 . Nl
H7 . Nl
H9 . Nl
H9 . Nl . 03
H16. 02
H16. 02
H3 .CL3
H12. 03
H16. 02
H16. 02
H16. 02
H16. 02
H16. 02
H16. 02
H12. 03
H12. 03
H12. 03
H3 .CL3
H3 ,CL3
H12
H16. 02
H20. 01
H12. 03
H16. 02
H20. 01
H12. 03
H12. 03
H16. 02
H20. 01
H12
H20. 01
H16. 02
H20. 01
H2£. 01
t SEE FOOTNOTE ON LAST PAGE
-------
TABLE Dl. (Continued)
HATER POLLUTANTS PAGE 19
IDENTIFIED COMPOUNDS 61 MOLECULAR HEIGHT
NOTE—THIS LIST HAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANT OF THE CONCENTRATES ANALYZED
MM
Idd
Idd
Idd
Idd
Idd
Idd
Idd
Idd
Idd
Idd
Idd
Idd
Ad5
Idb
Id6
Idb
Idb
Ida
Id6
Id6
11,6
Id6
Id6
Id6
Id6
Id6
Id6
Id6
Idb
Id6
Idb
Idb
Id6
Idb
Idb
Idb
Id6
Id6
Id6
Idb
Id6
Id6
Id6
Id6
Id6
CAS NO.
6l355d2
62238022
",2329908
5dOOdd21
123660
I, 88211
25713375
10673C
90153
531,0363
Idd
5087
I9b6d698
d9l2929
1680519
dl 75535
280961.5
1075225
170591.82
17057828
95501
9618d
3877198
6682719
1061,67
617
616
615
626517
I2d0d9
iOOl
5dl73l
1559815
1012
28715266
617629
1.830993
56ld7638
122576
598776
597d33
526892dd
di. d98d 1
607Z577
3653955
COMMON NAMt
2-T-8UTYL-i-METHYL-l,3-OIOXOLANE
2-8UTOXYPENTANE
2,<(-DIHETHYL HEXANOIC ACID
2,3-OIMETHYL-BUTANOIC ACID, ETHYL ESTER
/.ETHYL HEX A NO ATE
2,3-OIHETHYLHALEIC ACID
a.i-DIMETHYLHAkCIC AGIO USE CAS NO. 488211, ABOVE
METHYL HEPTANOATE
1-NAPHTHALENOL
3-NETHYL-J-OCTANOL
2-METHOXY-2-HEXENOIC ACIP
2-ACETYL-3-METHYLBUTANOIC ACID
AMINOPHTHALAZINE
1,1-OIMETHYLINOAN
6-METHYL TETRALIN
1,3-OIMETHYL INOAN
5-METHYL TETRALIN
5,6-OIMETHYL INOAN
1.6-OIMETHYL INDAN
1.2-oiMETHYL INDAN
XtlO-OICHLORO BENZENE
ZTRICHLOROPROPANE
2-METHYL TETRALIN
l»i 7-OIMETHYL INOAN
•««HP-DICHLOROBENZENE
OIHtTHYL INOAN
DIMETHYL INDAN
DIMETHYL INOAN
3-METHYLGLUTARIC ACIO
XAOIPIC ACIO
1-SEC-BUTOXY-2-HtTHOXYPROPANE
X»»M-OICHLOI
-------
TABLE Dl. (Continued)
MM
ld&
ld&
11.6
ld&
ld&
11.6
Id6
1<>6
11.6
11.6
11.6
Id6
Idb
Id6
1*7
Id*
11.8
Ida
11.8
IdB
i>«a
Id3
ida
Ida
Ida
ids
Ida
Ida
Ida
Ida
Ida
Ida
Id3
Ida
Ida
Ida
ida
Ida
ida
ida
Id3
ida
IdJ
ida
ida
CAS NO.
i99d7229
52931.0
37dd2S50
6705891
5d063ia2
328507
106650
5 dO 63 id 8
Iddl9d
Id6
9d962
5080
769255
1117863
85dl6
98511
538681
20d99d7
3968852
1196583
dl32723
17851273
2555613d
5 dl 20 626
20d9958
1007267
2719520
dd6l305
I3d29o77
55956213
2u32d327
5595622d
d26
d25
100
108
1L5
lOd
103
lid
113
121
i£0
119
118
HATER POLLUTANTS PAGE 2u
IDENTIFIED COMPOUNDS 3V MOLECULAR HEIGHT
NOTE—THIS LIST HAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANr OF THE CONCENTRATES ANALYZED
DATA SET CORRELATION t
COMMON NAMt
U-ETHYL-2-PROPENYLI -BENZENE
3,d-OIHYOR 0-112H> -NAPHTHA LENONE
1-PHENYL-3-BUTEN-2-ONE
2,2*-Bl-i,3-DIOXOLANE
(2-ETHOXY-l-METHOXYETHOXY»-ETHENE
ALPHA-KETOGLUTARIC ACID
SUCCINIC ACIOt DIMETHYL ESTER
d,d,5-TRIMETHYL-l,3-OIOXAN-l-OL
2,2,d-TRIMETHYL-l,3-PENTANEOIOL
d-ISOPROPOXYBUTYRIC ACID
2-ETHYL-l,3-HEXANEDIOL
A PENTENYLBENZENE
2,d,6-TRIMETHYLSTYR£NE
1,2-OCTANEOIOL
ISOINOOLt-1,3-DIONE
i-M£THYL-d-TERT-BUTYLBENZENE
AHYL BENZENE
ISOPENIYLBENZENE
(2-MtTHYLflUTYLI BENZENE
3-PHENYLPENTANE
l,d-OIMETHYL-2-ISOPROPYL BENZENE
2,d,5-TRIMETHYLETHYL BENZENE
DIETHYL TOLUENE
l,2,d-TRIMETHYL ETHYL BENZENE
(It1-DIMETHYLPROPYLl BENZENE
NEOPENTYL BENZENE
2-PH£NYLPENTANE
(1,2-DIMETHYLPROPYLI -BENZENE
DIPROPYLENE GLYCOL METHYL ETHER
-------
TABLE Dl. (Continued)
HATER POLLUTANTS PAGE 21
IDENTIFIED COMPOUNDS BY MOLECULAR WEIGHT
NOTE—THIS LIST HA* CONTAIN COMPOUNDS THAT HAVE NOT BtEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
DATA SET CORRELATION t
MM
mi
11,8
I'll
ma
i*
m)
I5j
15J
1SD
15J
IS,
ISO
ISO
IS.
ISO
ISO
IS*
CkS NO.
115208
13518288
1.2181.86
66901,5
208951)11,
31,5361,3
1371,39
8971,7
1.07683
5779726
579077
937301,
2m26<<5
1002671
51,12061,8
18328115
122032
1,706892
101,1,61
577971,8
851,1,9
1,920991,
1,706905
2t<>2769
22699703
5l610i<6
700129
10751,96
137
1007325
529339
537928
91667
1,99752
11309325
1,99069
501520
6110x8
610720
122601
56531.2
9651.
-------
TABLE Dl. (Continued)
MM
15}
15*
15i<
150
I5u
150
150
151
I5a
150
150
15J
15,
150
151
151
151
151
151
I5l
152
152
152
152
152
152
152
152
152
152
152
i52
152
152
152
152
152
152
152
152
152
152
152
152
l5c
CAS NO.
1.92375
3299356
88186
93890
61901,5
119675
18091U5
28131,318
1011.17
26967657
27577961.
533186
61961,7
590023
2631,335
931,31,9
7211,611
7211.61
995H
27655261
1195795
76222
122598
100091,
16u<>36
221.3983
89816
612201.
831,09
579759
1197697
586389
51,7601.
W695629
2653221.1
1.881.21.6
5511.51
21.955633
15932806
10242985
121335
567613
31600552
1.32257
9061,2
HATER POLLUTANTS PAGE ZZ
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE—THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
COMMON NAME
2-PHENYLPROPIONIC ACID
(1-ETHOKYETHYLI BENZENE
0- TERT-BUTYLPHENOL
XETHYL BENZOATt
3,<.-OIH£THYL8ENZOIC ACID
2-FORMYLBENZOIC ACID
3-BROMOPtNTANE
U-ETHYL8ENZOIC ACID
PHENYL ACETIC ACIO. METHYL ESTER
DIETHYL PHENOL, (UNKNOWN ISCHERI
Z-XYLYLEIHANOL
0-CRESYL ACETATE
P-ETHYLfltNZOIC ACIO
BJTYL CHLOKOACETATE
1,2-BENZISOTHIAZOL-3<2HI-ONE
2(3HI-BENZOTHIAZOLONE
(i-NITROETHYLlBENZENE
U-NITK8LTHYLte£NZEN£ USE CAS NO. 7214611. ABOVE
1,2-OIMETHYL-ii-NITROBtNZENE
3-HYOROXY-1.2-8ENZISOTHIAZOLE
FENCHONE
XCAMPHOK
PHENOXt ACETIC ACID
ANISIC ACIO
1-UNOECYNE
5-UNDECYNE
PIPERIDONE
2-(HYOkOXYM£THYL>BENZOIC ACIO
0-CRESOTIC ACIO
0-ANISIC ACIO
3» ,-2-CYCLOPENT£N-l-ONE
CIS-lti-OICHLOROCYCLOHEXANE
PULEGONt
it, 7,7-rRIM£THYL8ICYCLOC2.2.1)H£PTAN-2-ONE
XVANILLIN
2-HYOROXY-6-METHYLBENZOIC ACIO
METHOXYMETHOXYMETHYLBENZENE
2,6,6-TkIMtTHVL-l-CYCLOHEXtNE-l-CAR80XALOEHYDE
•/.MANOtLIC ACIO
DATA SET CORRELATION t
DW AWT T4 T5
845
381
336
223
334
149
981
301
1054
936
382
477
363
297
246
579
1060
433
1057
524
784
781
549
8)6
420
745
16
798
109
1092
48
726
265
556
356
14
572
823
824
860
448
482
483
52
122
218
7
36
50
111
180
149
112
54
173
89
204
11
121
52
88
107
114
110
109
168
MOLECULAR FORMULA
C9
CIO
CIO
C9
C9
C8
C5
C9
C9
CIO
CIO
C9
C9
C6
C7
C7
C8
ca
ca
C7
CIO
CIO
C8
C8
Cll
Cll
CIO
C8
ca
ca
ca
ca
CIO
CIO
CIO
CIO
C9
C6
CIO
CIO
C8
ca
C9
CIO
ca
HlO.
Hll..
H14.
HlO.
HlO.
H6 .
Hll.
HlO.
HlO.
Hli>.
HH..
HlO.
HlO.
Hll.
H5 .
H5 .
H9 .
H9 o
H9 .
H5 .
H16.
H16.
H8 .
Ha .
H2fl
H20
Hie.
H8 .
H8 .
H8 .
H8 .
Ha .
H16.
H16.
H16.
H16.
H12.
HlO.
H16.
H16.
Ha .
HB „
H12.
H16.
H8 .
02
01
01
02
02
03
BR1
02
02
01
01
D2
02
OZ
Ni
Nl
Ml
Nl
Nl
Nl
01
01
03
03
01
03
03
33
03
03
01
01
01
01
02
CL2
01
31
03
03
02
01
03
0
CL1
01 . Si
01 . SI
02
02
02
01 . SI
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
MM
152
152
152
152
152
152
152
153
153
151.
151.
151.
151.
151,
151,
i5i»
151.
151,
151,
151,
151,
151,
151,
151,
151.
151,
151,
151,
151,
151,
151,
151.
151.
151,
15U
151,
151,
151,
151.
151,
151.
15",
155
155
CAS NO.
621625
208968
1.501580
1,9971,1
2958761
2108921
822866
1981,01.9
2955931,0
92521,
1,70826
121,765
507700
586823
513235
10 i,5-2H-AZEPIN-2-ONE
X.alPHtNYL
'/.CINE OLE.
EXO-BOKNEOL
•/.ENOO-80RNEOL
1-METHtL-it-d-METHYLETHYL • -3-CY CLO HE XE N- 1-OL
XTHUJYL ALCOHOL
MENTHONE
FENCHYL ALCOHOL
1,-TERPINEOL ISOMtR
1,-TERPINEOL ISOMER
CIS-1.2-CIS-2.3-PLINOL
•P-CHLOROACETOPHENONE
VINYL CYCLOHLXYLFORNATE
XtACENAPHTHALENE
1-UNOELENE
XALPHA-TEKPINEOL
ETHtNYL CYCLOPENTANEACETATE
1,,1,-OICHLOROBUTENOIC AGIO
BETA-RtSOKCYLIC AGIO
2. 2,6-TRI MfcTHYL- 1,1,-CYCLO HEX A NEOI ONE
1,3, 3, 7-It TRAMETHYL-2-OXOBICYCLOC i .2 .1 1 HEPTANE
i-HtTHYL-i,-ll-MtTHYLETHYL) -7-OX AB I CYCL 0( 2. 2 .11 HEP T ANE
METHYL 2,2 ,3-TRINETHYLCYCLOPENTYL KETONE
2-M£THYL-2-NON£N-l,-ONE
i,<:-OIMETHYL-3-ISOPROPENYLCYCLOPENTANOL
Xl,3,6-TRIMETHYL-2,i.(lH,3M»-PYRIMIDINEOIONE
3,5-OlMLTHOXYPHtNOL
I..5-OIE THY L-2, 3-01 HYDRO-? , 3-01 ME T H YL FUR A N
OMtGA-CHLOROACETOPHENONE
2-METMLY-5-ISOPROPYLCYCLOHEXANONE
l»-BUTYL-l, 3-CYCLOPtNTANEQIONE
2-CHLORO-l ,3.5-TKlMtTHVLaEN^ENE
^-(l«-MET(1YL-3-CYCLOHEXENYLIISOPROPANOL
N-MLTHYLETHOSUXIMIOE
l-VALEKYLPYRROLIDINL
l,a-DIMEIHYLNAPHTHALENE
DW
111
287
743
170
483
237
787
234
995
394
928
218
312
473
489
723
785
1080
272
289
1032
749
655
AWT T4 T5
301
480
599
24
76 72
239 21
205
346
552
354
355
194
793
570
357 138
198
136
359
1017
385
744
252
282
930
733 155
1104
421
870
196
MOLECULAR FORMULA
C6 . HU. 02
C12. H8
CIO. H16. 01
ClO. H16. 01
Cll. H20
C6 . H10.CL2
C6 . H10-CL2
Cll. H7 . Nl
C9 . H15. Nl
C12. HID
CIO. HIS. 01
CIO. HIS. 01
ClO. Hta. 01
cio. Hia. 01
CIO. HIS. 01
CIO. HIS. 01
CIO. HIS. 31
CIO. HIS. 01
ClO. HIS. 01
CIO. HIS. 01
C8 . H7 . 01
C9 . Hl. 02
C9 . H11.CL1
CIO . HIS. 01
CS . Mil. Nl
C9 . H17. Nl
CIZ. H12
.CL1
. 01
.CL1
.CL2
. 02
.CL1
. 0?
. 01
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
MATER POLLUTANTS PAGE 2<<
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE--THIS LIST HAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
CTi
00
HM
156
156
156
156
i.56
156
156
156
156
156
156
156
156
156
155
156
156
156
156
156
156
156
156
156
156
156
156
156
156
156
156
156
156
156
155
156
156
156
156
156
156
156
156
156
156
CAS NO.
5811.20
57158".
571619
58<;i6i
1127760
1005
3161.2678
89781
939275
581UOIJ
700
5751.39
573988
300
118912
7«.113
7D8
71.1113
5751.17
1370521
301
575371
535808
820291
621.168
131.91797
30 £
13023002
i.79<.052
106229
1502U52
55013326
56052858
112312
Il202l<.
123682
1J22
3112851.
1651921.7
13703521
2518721
1.121.883
31502235
535159
22lO
-------
TABLE Dl. (Continued)
NJ
ON
MM
157
157
157
157
157
157
157
157
157
157
157
157
158
158
154
15»
158
158
159
158
159
158
159
158
159
158
.1.58
158
158
158
i58
159
158
158
i58
158
.•.58
158
158
158
159
159
160
IbO
160
CAS NO.
761659
121733
1771.30
1115461.
7661I.7I)
100005
88733
1721897
2623509
1198371.
31.31.
16627353
<<99<«165
112050
92<>l63
2216695
50<«9989<.9
'.16S'.095
28J 98408
112061
1(305261.
1120065
1.71.9273
5111,9703
1 12301
13279862
9351.55
56009360
31702337
1M12982
3271.291
106309
111115
71.69771.
2007
3001.931
16537125
161*0 397
33758Ub
10 76615
1985597
5i.3i.088i.
HATER POLLUTANTS PAGE 25
IDENTIFIED COMPOUNDS B» MOLECULAR HEIGHT
NOTE—THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
COMMON NAME
N.N-OI-N-BUTYL FORMA HIDE
XH-CMLORO NITROBENZENE
•/.2,6-DIHETHYLQUINOLINE
N.N-OIMETHYLHEPTANAMIOE
7-ETHYLQUINOLINE
P-CHLORONI TROBENZENE
XQ-CHLORONI TROBENZENE
2-3-OIMtTHYL QUINOLINE
5.8-OIHETHYLQUINOLINE
X.2.1.-OIHETH YLQUINOLlNE
3-HYOROXY-1.2-BENZISOTHIAZOLE
N,N-DIETHYL-
-------
TABLE Dl. (Continued)
MH
160
16«
160
160
160
160
160
160
160
IbO
160
160
160
160
160
160
169
16ft
160
160
160
160
160
160
160
160
160
161
0.61
161
161
161
161
162
162
16;
162
162
162
162
162
162
162
i&2
162
CAS NO.
5*3*0873
6682060
827521
<:0**ooo
*839*67
2613765
25*1933*
13065071
61898586
681572
5572*737
56298750
323675*7
22531200
2156*921
23881*9
2568925
913003
620202
*2 7 75 75 7
56282*30
lb**097*
56667108
5*3*0895
900**d8
160*111
1*29227*
95761
608275
55*007
23102025
310 JO 5*3
*377359
1985575
5**1069*
19262205
28080866
5**107*1
19219853
99627
55669880
6031023
6*5136
5***6785
1009616
HATER POLLUTANTS PAGE 26
IDENTIFIED COMPOUNDS B» MOLECULAR HEIGHT
NOTE—THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
DATA SET CORRELATION t
COMMON NAME
1,*,7-TRIMETHYL INOAN
*,5,7-rRIMETHYLINOAN
PHENYLCYCLOHEXANE
TETRAHYDROFURAN-2.5-DICARBOXYLIC A CIO
3.3 OIHETHYLGLUTARIC ACID
1,1,3-TRIMETHYL INOAN
lt8-DIMETHYL TETRALIN
2,7-OIMtTHYL TcTRALIN
3-METHYL AOIPIC ACID
2.2-OIMETHYLGLUTARIC ACID
*-BUTOXY8UTYRIC ACID
1-ETHYL-l-METHYL INDAN
2-ETHYL TETRALIN
6-ETHYL TETRALIN
2,3-OIMEIHYL TETRALIN
"t-ISOPROPYL-ALPHA-METHYL STYRENE
OI-S£C-auTOXYMETHANE
l.l.l-TRICHLORO-2-PROPANONE
l-CHLORO-3- BENZENE
1.3-OISOPROPYL BENZENE
l.*-OIMETHYL-2-ISOBUTYL BENZENE
2-PH£NYLH£XANE
*-ISOPKOPY LACETOPHENONE
1-12-BUTOXYtTHOXY) ETHANOL
OIACETYLBENCZENE
AWT
T5
1002
368
331
758
841
1062
903
110
825
965
952
954
207
211
969
974
534
837
428
451
179
92
197
691
361
661
575
344
769
1012
812
384
120
410 249
121
335
960
959
776
960
961
185
953
773
151
795
108
47
MOLECULAR
C12.
C12.
CIS.
C6 .
C7 .
C12.
C12.
C12.
C7 .
C7 .
C8 .
C12.
C12.
C12.
C12.
ClE.
C9 .
C3 .
C7 .
C12.
C12.
Cll.
Cll.
C9 .
C9 .
C7 .
ca .
C6 .
ce .
C6 .
C6 .
C6 .
C6 .
C12.
Cic.
ClE.
C12.
C12.
C12.
C12.
C12.
C12.
Cll.
C8 .
CIO.
H16
H16
H16
H8 .
H12.
H16
H16
H16
H12.
H12.
H16.
H16
H16
H16
H16
H16
H20.
H3 .
H6 .
H16
H16
H12.
H12.
H20.
H8 .
H12.
H16.
H5 .
H5 .
H5 .
His.
Hll.
H5 .
HIS
H18
HIS
Hia
H18
Hia
Hia
Hia
Hia
HI*.
Hia.
H10.
FORMULA
05
Ok
Ok
fHi
03
02
01
CL2
01
01
02
N2
0
-------
TABLE Dl. (Continued)
MATER POLLUTANTS PAGE 27
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE—THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT SEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
DATA SET CORRELATION t.
HH
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
162
163
1 b1*
1 fal*
16".
16U
16<<
161.
161.
161.
IbU
161.
16<<
CAS NO.
51.115
61.5736
112367
250
101185
11231.6
120832 X
91587 •>.
t3l
1866393
108850
38393929
8771.1.1
102250
55682730
<>8 15570
11.83609
22975582
211.2656
76039
591355
75272205083
1077163
208951. 1,7
1667Q12
13521.760
583d<.0
5u78
2235838
2<«9539i.
583788
95772
521.389
90277
528905
9391.80
536663
112356
1821121
1.80637
1017
22dd>.895
98271
3377875
-TRI£THYLB£NZEN£
1,3.5-TRIETHYL BENZENE
2.2-DIMETHYL-3.5-OECADIYNE
P-DIPROP«LBENZEN£
2,<»-OIMETHYL-l-SEC-BUTYLBENZENE
P- (1-ETHYLPROPYLI TOLUENE
fl-ISOPfcOPYLACETOPHENONE
XTCA (TRICHLOROACETIC ACID)
•/.3,5-OICHLOROPHENOL
XBROMOOICHLOROME THANE
1,2,3-TRIETHYLBENZENE
1-PHENYLHEXANE
««,6-OIMLTHYLBENZOFURANON£
2 «.<.*,&*-TRI METHYL ACE TOPHENONE
3,3-OIMETHYL-2(3HI-FURANONE
2-ALLYL BENZOATE
ALPHA-METHYLtNE BENZENE PROPANOIC ACID
5-PHENYL-2-PENTANONE
2-Bc.NZYLACRYLlC ACID
2.5-OICHLOROPHENOL
3, . 01 .CL2
Cl . HI .BR1 .CL2
C12. HIS
C12. Hia
CiO. HlO. 02
Cll. Hli.. 01
CIO. HlO. 02
CIO. HlO. 32
ClO. HlO. 02
Cll. HIV. 01
CIO. HlO. 02
C6 . H"» . 01 .CL2
C6 . HI. . 01 ,CL2
C8.H5.N1. 03
CIO. H12. 02
CIO. H12. 02
ClO. H12. 02
CIO. H12. 02
C7 . H16. 0<<
Clli. H12. 02
ClL. H12. 02
C7 . H16. 0<«
CIO. H12. 02
Cll. H16. 01
C6 . H13.BR1
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
MH
16<.
16V
16".
161.
16<<
16I>
161.
163aO
-------
TABLE Dl. (Continued)
MM
166
166
166
167
169
163
161
163
168
163
163
169
168
163
168
168
163
168
168
168
168
168
168
163
163
163
168
168
168
169
169
169
170
170
170
170
170
170
170
170
170
170
170
170
170
CAS NO.
1701775
52718".
203805
62237
6,3-PROPANETRIOL
CHRYSANTHEMIC ACID
3-METMYLBIPHENYL
•..8-OIMETHYL-7-NONEN-2-ONE
3-METHYL-3-OECEN-2-ONE
Itl-OICHLORO-2-HEXANONE
<«i
-------
TABLE Dl. (Continued)
MH
170
170
170
170
170
170
170
170
170
170
170
170
170
170
170
M 170
~-J 170
*• 170
170
170
170
170
170
170
170
170
171
171
171
171
172
172
172
172
172
172
172
172
172
172
172
172
172
CAS NO.
28652779
3876979
319
17057919
90«.37
2i310209117
29253369
7 u 61 1.9
5088
5I.38258C
70553
827167
8951.3
1361.
3 3 1.1.8 5
173181.6
31080372
"(812297
2639636
23708567
1 1 i <<2 5
80535
93091.
86555
533621.3
3lC8C39<.
'>506369
HATER POLLUTANTS PAGE 30
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE--THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
COMMON NAME
TRIMETHYLNAPHTHALENE (ISOMER UNKNONN)
l,2,a-TRIMETHYLNAPHTHALENE (3, <«, 5-TRIME.NAP. I
TRINETHYLNAPHTHALENE
1,3,8-TRIMETHYLNAPHTHALENE
X.2-HYOROXY8IPHENYL
1.<..6-TRIMETMYL NAPHTHALENE
l,«t.5-TKIMETHYL NAPHTHALENE
5.5-OIETHOXY-3-PENTYN-2-ONE
METHYL 3,6-OIHYORO-i.,5-DIMETHYL-2H-PYRAN-2-CARBOXYLATE
XPHENYL ETHER
2-CYCLOOCTYL-2-P*OPANOL
CYCLOOCTANEPROPANOL
",-CHLOkOPHENTL ACETATE
CIS-J.. 01
CIO. H20. 02
Cll. H8 . 02
Cll. H8 . 02
C9 . H20. N2 . 01
CIO. H2G. 02
C13. H16
SI
>CL1
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
KJ
~~J
Ln
MM
172
172
172
172
172
172
172
172
172
172
172
172
172
172
172
172
172
172
173
17"»
m
17%
171.
m
171.
171,
17".
171.
171.
171.
171.
171.
171,
176
176
176
176
I7b
17b
176
176
17b
176
176
CAS NO.
33669760
16533J1
30316199
29301, <.03
5 <. 1,66 990
93185
6061.521.
2451016
2177868
106321
I73l8%8
8963%
119619
2216811
2553960
95567
28933597
26896208
16067019
5051.86
55956257
22821.32 %
21693516
29006062
1010
1071.119
2257351.
829992
261.1.7632
261.1,7651.
123251
1319201.6
33796871
2132867
191.3959
1.66566
1191.26
593715
24i.80i.2J
1 J5W063
51.63503
1.1.661.00
14961041
9V3271
HATER POLLUTANTS PAGE 31
80535, PREVIOUS PAGE
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE—THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
COMMON NAHE
l-MErHYL-
-------
TABLE Dl. (Continued)
MM
176
176
176
176
176
178
17*
178
178
178
178
178
178
178
178
178
178
171
178
178
178
179
179
179
179
179
17S
178
178
179
179
178
178
179
179
179
179
179
17J
179
179
180
180
180
180
CAS NO.
1973001,2
86522
1078199
11,171892
6630019
120127
2270201,
161,331,35
51,518115
85018
136607
5669170
7315686
1125)5
520
581, 1,3826
207851,8
1121,92
22<<3358
20589859
293i>u56
2«a"»2776
Si.5',9723
1726991,2
10226296
1603798
611.277
131,85660
1971.056
16821,025
667
3333
1,219550
28291692
1010<<86
821,691
5081
15i»825<,9
89521
3 1,2 63 61, -OXO-BUTYRIC ACID
0-PROPIONVL BENZOIC ACID
N-ETHYL-2-BENZOTHIAZOLAMINE
B£TA,8ETA-OIHETHYL8ENZENEPROPIONIC ACID
l,i»-DICHLOf<0-2,5-DIHYDROXY BENZENE
I,-ETHYL TETRA METHYL PHENOL
2-ACETYL-P-TOLUIC ACID
N-ACETYLANTHRANILIC ACID
3-ETHOXY-l,2-BENZISOTHIAZOLE
P-AMINOBtNZENE-T-BUTYRIC ACID
9-METHYL-9H-FLUORENE
2-METHYL FLUORENE
•/.**$!, 2, it-TRICHLOROBtNZtNE
9.10-OIHYOROPHENANTHfcENE
DATA
DW
973
1164
1115
702
522
847
569
125
913
775
449
472
1132
617
513
503
32
731
198
866
414
SET CORRELATION t
AWT T4 T5
456
945
380 242
182
31
196
77
489 193
37
565
806
539
360
409
395
1088
492
454
731
689
722
474
902
49
137
172
23
125
178
124
354
923
787
840
258
MOLECULAR FORMULA
Cll.
Cll.
Cll.
C12.
C13.
Cl",.
Cll.
Cll.
C12.
cm.
Cll.
Cll.
Cll.
C6 .
C12.
C12.
C12.
C8 .
CIO.
C3 .
C12.
C12.
Cll.
C12.
C6 .
cia.
CIO.
C12.
C7 .
C1C.
C12.
CIO.
Clb .
C9 .
Cll.
C6 .
C12.
C1C.
C9 .
C9 .
Clb.
Cl>>.
Cll,.
C6 .
Cli,.
H16. N2
H9 .CLI
H12. 02
H16. 01
H20
H10
HI!,. 02
HH«. 02
H18. 01
HlO
Hl<>. OZ
Hl<>. 32
HH,. 02
H18. Ol»
H18. 01
H18. 01
H18. 01
HIS. Ol»
HlO. 03
H2 -CH,
H18. 01
H18. 01
Hl<>. 02
H18. 01
Hll. 01
HlO. 03
HlO. 03
H18. 01
H15.B%1
HlO. 03
H18. 01
Hlfl. *3
Hl(). 03
HlO. N2
Hll,. 02
H
-------
TABLE Dl. (Continued)
HM
isii
183
iao
180
18-
18,
181)
181
18,
18?
ISO
18D
181
180
180
18.
I8j
18D
160
181
181
182
18£
182
182
18Z
I8c
182
182
182
18?
182
182
iBi
182
182
182
182
182
182
182
18£
182
182
1B2
CAS NO.
1U87U3
87616
15359996
5it576i.l9
".316238
18495302
103300
1730376
588590
17492921
17138282
<<86259
1131620
3710271.2
6233821.3
153567<«8
530<«83
13116535
25013165
615225
6967700
605390
781.00
600
7383906
2«.3756l
11.376820
1.1651.277
93072
91521
6120QO
1812517
92831
5i.3i.606i.
«.6".5152
1C3297
13ul9l6i,
7507893
830137
12111.2
519531G7
3021736
Cll,. Hl<>
C13. H26
C5 . H8 .BR1
CIO. HIS. 03
C9 . HlO. Oi.
C9 . HlO. 01,
Cll,. Hid
Cll,. Hll,
C13. HlO. 01
CIO. Hid. 03
C12. H22. 01
Cll.. HI".
C12. H22. 01
C9 . HlO. Oi.
C12. H22. 01
C7 . H6 . N2
Cl2. H22. 01
Cll. HIS. 02
C12. H22. 01
C1U. Hid
Cll,. Hll,
. S2
. 02
. Pi
.CLI
•
. 01,
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
MATER POLLUTANTS PAGE 3".
IDENTIFIED COMPOUNDS BY MOLECULAR WEIGHT
NOTE--THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
MM
182
163
183
181.
181.
*84
181.
181.
161.
181.
181.
161.
181.
181.
181.
ho I"
^J 161.
CO 18(,
181.
161.
181.
161.
161.
181.
181.
181.
184
181.
185
18&
186
166
186
18S
186
j.86
166
186
186
185
18&
186
166
166
186
CKS NO.
606202
81072
56771507
1131.629
1631.099
i 8 763 5 9
112389
490653
1.9622186
17085915
16727916
629505
54771,899
51.771.91.6
1.351,589
21.99591.
50639026
765059
3401,061,7
1973224
1585075
104614
27011467
35194399
1978010ft
132650
104676
5305C7
640619
19377970
112378
33583027
112563
112538
1422260
112265
6836380
10203288
110429
1534276
19943716
3913028
10203335
1119637
5601605
Cl
2
•/.s,
PI
2-
1-
2-
11
I-
3,
1-
1-
Tl
2-
8!
C\
0(
2-
Dl
4-
1-
1-
1-
1-
El
5-
01
5-
1,
XN,
2,
XN-
2,
01
XL«
9-
XET
6-
2-
ME
3-
4,
2-
5-
9-
AN
COMMON N«ME
2,6-OINITROTOLUENE
XSACCHARIN
PHENYL P-PYRIDYL KtTONE
2-BUTYLNAPHTHALENE
1-BUTtLNAPHTHALtNE
2-T-BUTYL NAPHTHALENE
It-UNOECENOIC ACID
l-METHTL-7-ISOPROPYL NAPHTHALENE
3.3,i>-TRIMETHYLOtCANE
1-TERT-BUTYLNAPHTHALENE
1-IS08UTYLNAPHTHALENE
TklOECANE
2-METHYL-l-PROPYLNAPHTHALENE
BICYCLOt2.2.2)OCTANE-l.l»-OIOL. MONOACETATE
CYCLOHEXANEHEXANOL
OCTYL ACRYLATE
2-MfcTHtL-5-UNOECANONE
DECVL VINVL ETHER
-CHLOROPHENYL ACETIC ACIO, METHYL ESTER
l-BROMO-2-ETHYLBENZENE
l-BROMO-«i-tTHYL BENZENE
1-(BROMOMETHYLI-I,-METHYLBENZENE
1-CHLOROTRICYCLOI1..3.1.13.61UNOECANE
ETHVLNONENOATE
5-DODECANONE
OIBENZOTHIOPHENE
5-HEPTYL DIHYDRO-2-FURANONE
1.1-OIPHENYLHYORAZINE
XN.it-OIMETHVLSENZENESULFONAMIDE
2,2,5,7-TETRAMETHYL-'»,5-OCTADIENE-3-ONE
XN-UNDECYLIC ACIO
2,5,8-TRIMtTHYL-l-NAPHTHOL
OI-N-HEXYL ETHER
XLAURYL ALCOHOL
9-KLTOCAPRIC ACID
XETHYLENE GLVCOL, DIS (2-CHLOROETHYL I ETHER
6-OOOECANOL
2-DOOECANOL
METHYL CAPKATE
3-OOOECANONE
6-OIMETHYLNONANOIC ACID
2-8UTYLOCTANOL
5-OOOEGANOL
9-METHYLOECANOIC ACIO
ANTEISOUNOECANOIC ACIO
DATA SET CORRELATION t
DU AWT T4 T5
859
1104
407
319
542
747
952
643
350
1159
653
375
993
1018
260
422
658
905
686
376
45
342
778
989
504
752
805
789
814
990
899
1045
887
259
263
654
441
707
320
1063
889
605
22
144
55
214
17
135
120
MOLECULAR FORMULA
C7 .
C7 .
C12.
cm.
Cll..
cm.
Cll.
CH.
C13.
Cll..
Cll..
C13.
Cll..
CIO.
C12.
Cll.
C12.
ciz.
C9 .
C8 .
C8 .
C8 .
Cll.
Cll.
C12.
C12.
Cll.
C12.
ca .
C12.
Cll.
C13.
C12.
C12.
CIO.
C6 .
C12.
C12.
Cll.
C12.
Cll.
C12.
Cl2.
Cll.
Cll.
H6 . N2 . Oi,
H5 . Nl . 03 . SI
H9 . Nl . 01
H16
H16
H16
H20. 02
H16
H28
H16
H16
H28
H16
H16. 03
H2ii. 01
H20. 02
H2t>. 01
H2i>. 01
H9 . 02 .CLI
H9 .B«l
H9 . 8R1
H9, .BU
H17.CL1
H22. 02
H2<». 01
H8 . SI
H20. 02
H12. Hi
Hll. Nl . 02 . Si
H20. 01
H22. 02
Hll,. 01
H26. 01
H26. 01 *
HIS. 03
H12. Q2 .CL2
H26. 01
HZ6. 01
H22. 02
HZ*. 01
H22. 02
H26. 01
H26. 01
H22. 02
H22. 02
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (Continued)
MATER POLLUTANTS PAGE 35
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE—THIS LIST MAT CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
MM
188
148
148
188
IBS
188
188
188
188
188
148
188
188
188
188
189
190
190
190
190
190
190
190
190
190
190
190
190
190
190
190
1.90
190
190
ISO
190
190
191
191
191
192
192
192
192
192
*BUTYL
Ct(S NO.
33931689
20<« 1.2062
123999
2596181.6
2331.2256
21.32793
29518727
1603618
1.201.1.268
1.20 ".1,2 21,
5U789296
1.83556
5689123
5393817
11.292263
1.95692
33962139
3895178
2189608
5081.0
511.1,5
3507521.2
29911282
11.128611
51.789150
33637206
1079965
5280581.2
18335151.
1011.1.11
777220
597637
50793
17759885
33037079
366631.58
5186685
3209221
611063
!.<: 1.96339
613127
779022
6101.80
163b 160
59091.712
ETHER)
CC
i<-
2-
y.Ai
01
2,
Th
1-
(2
6-
2-
1-
Ph
1.
2-
3-
N-
1,
2-
OC
2.
3,
1-
1-
5-
1-
Tf
M-
1-
3-
P-
2-
T(
2,
2-
1-
3-
i.
1
2
N-
'/. i-
X9-
1-
Tl
1.
* it
COMMON NAME
-ETHOXYBUTYL BUTANOATE
2-BUTOXYETHYL BUTANOATE
XAZELAIC ACID
DIETHVLENECLYCOL. CYCLOHEXYL ETHER
2,2,5.7-TETRAMETHYL TETRALIN
THIOHEXANOIC ACID, S-BUTYL ESTER
1-OCTENYL8ENZENE
(2-CYCLOHEXYLETHYLIBENZENE
6-TERT-BUTYL TETRALIN
2-TERT-BUTYL TETRALIN
1- (OICHLOROMETHYL) -<.- ETHYL BENZENE
PHTHIOCOL
l,l,3,3-TETRAM£THYL-2-INOANON£
2-HYOROXY OECANOIC ACID
3-HYOROXYCAPRIC ACID
N-BcNZOYLGLYCIN£ IHIPPURIC ACID)
l,i.-DItTHYL-2,3.5.6-TETR»METHrL BENZENE
2-ETHOXYETHTL-2-BUTOXYETHYL ETHER
OCTYL BENZENE
2.'.-OICHLOkOBENZOIC ACID
3.1.-OICHLOROBENZOIC ACID
l-(3-BUTOXYPROPOXYt-2-PROPANOL (A OIPROPYLENE GLYCOL.*
1-(2-BUTOXY-l-M£THYLETHOKY»-2-PROPANOL (OIPKOPYLENE **
5-MeiHYL-S-PH£NYL-2-HEXANONE
1-U-Ef HYLPROPY LI-2-PROPYL BENZENE
TETR4ETHYLBENZENE
M-OI-SEC-BUTYLBENZENE
l-C5-C2-FUfcANYLMETHYLI-2-FURANYL)ETHANONE
3-PHENYLOCTANE
P-Dl-SEC-BUTYLBtNZENE
2-PHtNYLOCTAN£
TETRAETHVLGERMANE
2,6-OICHLOROBENZOIC ACID
2-BROMO-l, 2-OICHLOROPROP1NE
1-BROMO-2.3-OICHLOROPROP4NE
3-BROMO-i,i-OICHLOROPROPANE
I..6-OIISOPROPYL-M-XYLENE
1.2-OICMi-ORO-3-NITKOaENZ£NE
2,l.-OICHLORO-l-NITROBLNZ£Nt
N-TERT-BUTYL-3-METHYLBENZAMIDE
X2-METHYL AMHRACENc
X9-MLTHYL ANTHhACtNc.
1-MtTHYL ANTHRACENE
TRIPROPYLL N£ GLYCOL
!.-MtTHYLPHtNYLPi.NTANOIC ACIO
GLYCOL,BUT.ET.)
DATA SET CORRELATION t
DW AWT T4 T5
84
213
490
861
525
689
690
529
946
355
288
692
96
98
174
677
807
750
146
848
1063
793
515
738
1005
405
860
288
126
392
777
557
968
142
54
656
435
1028
473
932
788
970
352
114
612
16 159
91
12
247
251
C7
C3
C5
C3
SI
03
MOLECULAR FORMULA
CIO. H20. 03
CIO. H20. 03
C9 . H16. 01.
ClO. H20. 03
Cli«. H20
CIO. H20. 01
Cli.. H20
ClU. H20
cm. H2o
Cli.. H?0
C9 . H10.CL2
Cli. H8 . 03
C13. H16. 01
CIO. H20. 03
Cli. H20. 03
C9 . H9 . Nl
Cli.. H22
CIO. H22. 03
Cli.. H22
C7 . Hi. . 02 .CL2
C7 . Hi. . 02 .CL2
CIO. H22. 03
ClO. H22. 03
C13. HIS. 01
Cli,. H22
Cli.. H22
Cl<.. H22
Cli. H10. 03
Cli.. H22
CU. H22
Cli.. H22
C8 . H2O
Hi. . 02 .CL2
H5 .BR1 .CL2
H5 .BRi .CL2
H5 .8*1 .CL2
Cli,. H22
C6.H3.Nl. 02 .CL2
C6 . H3 . Nl . 02 .CL2
C12. H17. Nl . 01
C15. H12
C15. H12
C15. H12
C9 . H20. 01.
Cl2. Hi6. 02
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE Dl. (continued)
WATER POLLUTANTS PAGE 36
IDENTIFIEC) COMPOUNDS 3» MOLECULAR HEIGHT
NOTE--THIS LIST MAY CONTAIN COMPOUNDS THAT HAUL NOT BEEN FOUND IN ANT OF THE CONCENTRATES ANALYZED
DATA SET CORRELATION t
MM
192
192
192
193
192
192
192
192
193
19J
191.
191.
191.
19*
194
.1.91.
K, 19",
00 191.
O 191,
19<>
191,
191.
195
195
196
195
196
195
196
196
195
196
196
196
19o
196
195
19&
19b
196
196
195
196
196
196
CAS NO.
83261. i.
1011
5I.8.5213
832713
201.9969
11.5 JO 61
127
21.30623d
1205b89
2021207
713U62
120616
53002
131113
933810
11.0 6<> 1.83
51.821.112
91.995
1021.76
31.05600
1.612639
626857
631.935
636306
91.7911
I.821UI.9
08 062 /.
2198756
1351.0562
«.255fli.5<.l
1120361
9595".
761.938
761.93
36617021.
1.95711.6
1.707500
i9i.206i2
1016
1133035
17619975
5811.857
3976350
1015
7180576
COMMON NAME
l»-MtTHYLPHtNANTHRENE
B£TA,3,i.-Tf
-------
TABLE Dl. (Continued)
NJ
00
MATER POLLUTANTS PAGE 17
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE—THIS LIST HAT CONTAIN CONPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
MM
196
197
191
19*
191
199
19ft
191
191
191
198
198
198
198
191
191
191
191
198
199
199
2*A
200
200
201
200
200
200
200
200
200
200
200
20 i
202
202
202
202
202
202
202
202
202
2(i>
CAS NO.
1.96
15)><»899«
1.83783
62959).
2312 <<03
17663273
13757909
16".09".5i
5<.15275>3077
777957
19(191.758
57269266
2575077
50182638
50862616
110363
1731668
586765
676006
6272361.
206<.i.O X
129000
3971333
111206
1.83772
169820*6
5921802
11.629528
17219215
173.2098
11/61772
COMMON NAMt
P-PHENYLACETOPHENONE
CIS-l-BROMO-2-CHLOROCYCLOHEXANE
N-METHYL SACCHARIN
li 6 OlNtTHYL->HETHYLDIBENZOTHIOPHENE
<»,5-OIMElHYLCYCLOOCTANE CARBOXYLIC ACIO
2-CHLORO-P-TERT-BUTYLPHENOL
ETHYLPHENOXVBENZENE
ALPHA,«-OIHYOROXY-3-NETHOXYPHENYLACtTIC ACIO
l-METHYLBARBITAL
N, N,<>-TRIMLTHYLBENZENESULFONAMIDE
OODECANAMIDE
XLAURIC ACIO
CYCLIC UTKANETHYLENE AOIPATE
• METHYL CHLORO PHENOXYACETIC ACID INCPAI
2-MtTHYL-l -OOOECANOL
METHYL 9-OXOOECANOATE
l-BUTYL-2-NAPHTHALENOL
2-BUTYL-l-NAPHTHALENOL
ZETHYL CAPRATE
UNOECANOIC ACIOiHETHYL ESTER
P-BROMOBtNZOIC ACIO
IC-OXO-UNOi-CANOIC ACIO
2.»tFLUORANTHENE
X»PYRENt
2-cTHYLSUBERIC ACIO
SEBACIC ACIO
1.6-OIHETHYL-. H12. 01
C6 . HlO.BRl .CL1
C8 . H7 . Nl . 03
C15. HIS
Cl<>. H30
C12. H22. 02 .
C12. H22. 32
ClZ. H22. 02
Cl2. H22. 02
Cl3. H26. 01
C5 . Hll. II
C5 . Hll. II
C13. H26. 01
C13. HID. 02
Cl3. HlO. Si
Cll. H20. 02
Cll. HIS. 01 .CL1
Cli.. HI".. 01
C9 . HlO. 05
C9 . HI".. N2 . 0]
C9 . H13. Nl . 02
C12. H25. Nl . 01
C12. H2<>. 02
CIO. H16. 0<.
C9 . H9 . 03 .CLI
Cl3. H28. 01
Cll. H20. 03
Cll.. H16. 01
Cm. H16. 01
Cl2. H2ii. 02
C12. H2
-------
TABLE Dl. (Continued)
HATER POLLUTANTS PAGE 3«
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE—THIS LIST MAT CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
DATA SET CORRELATION t
00
to
MH
20*
204
204
£04
20
206
206
206
206
206
206
2C6
206
206
206
206
206
206
206
206
2o6
266
286
206
206
206
206
2D6
206
206
206
lit i] 669
1.06
1,05
lO".
1,10
Cli.. H22. 01
CIO. H22. 04
Cl
CIO. H22. 0
-------
TABLE Dl. (Continued)
HATER POLLUTANTS PACE 39
IDENTIFIED COMPOUNDS Bl MOLECULAR HEIGHT
NOTE--THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
t-0
CO
U)
MH
201
209
209
208
209
208
269
208
208
209
210
211
<-\.
210
210
2la
21|<
210
210
21<
21.
210
210
2 10
219
210
210
211
211
212
21Z
212
21Z
212
212
2lZ
Z1Z
Z1Z
Zl3
Zi1.
211.
2 ill
2l<.
211.
CAS NO.
101.87920
3U18200
291,22137
151.0 1. 63 it
52588780
<.12(1 1.882
51.832836
81.651
2316269
6267023
".920950
871,01
13360617
26137531
111,2150
38171970
131.816
18220901
626620
3519I.Z20
Z852688
6111.1660
2613081.7
51.965536
2726218
55012696
17160266
55030651,
5650102
629629
1Z5I.06
612351
77281
17Z50<.8
660631.1.
6262517
10271575
i.<.7aioa
36ZZJI.Z
9365Z
(182097
15101.617
6J8539
1 31566
DATA SET CORRELATION t
COMMON NAME
ALPHA-METMYL-ALPHA-ACETYLOXYBENZENEACETIC ACID
1-PHENYL TETRALIN
2-PHENTL TETRALIN
OECAHYORO-1.I.A-OIHETHYL-7- (1-ME THYLE THYL INAPHTHAL ENE
6,6-DIMETHYL-3,i.-UNOECADIENE-2,lO-OIONE
b-PMENYL TETRALIN
OCTAHYDRO-Z, 2, <•,<.. 7. 7-HEX AMETHYL-1H-INDENE
Z9f 10-ANTHRACENE 01 ONE
3-
-------
TABLE Dl. (Continued)
HATER POLLUTANTS PAGE
IDENTIFIED COMPOUNDS B1 MOLECULAR HEIGHT
NOTE—THIS LIST HAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANT OF THE CONCENTRATES ANALYZED
DATA SET CORRELATION t
MH
21it-TRIHtTHYL PHENANTHRENE
2,9,10-TkIhETHYL ANTHRACENE
TRIPROPYLCNE GLYCOL, ETHYL ETHER ISOMER
,<.-OICHLOSOPHENOXYACETIC ACIO, (2,i.-D>
NONYLPHENOL
ISONONYL PHENOL (ISOHER UNKNOWN)
P-ll-MtTHYLOCTYL)PHENOL «A NONYL PHENOL)
P- (1-cIHYL-l-METHYLHEXYL) PHENOL (A NONYL PHENOL)
NONYL PHENOL ISOMER
NONYL PHtNOL ISOMER
OICAMBA
JJ3.I.-DICHLOROPHENOX YACETIC ACIO
DM
342
1019
1161
91
526
358
448
914
333
792
1084
427
1150
112
802
AWT T4
906
125
126
911
294
349
226
450 175
548
190
855
290
1030
673
674
351
169
34
966
967
199
270 85
232
588
589
386
826
991
240 88
T5 HOLECULAR FORMULA
C13.
CIO.
C6 .
C13.
CIS.
C13.
C13.
C12.
ci2.
Clii.
C8 .
C17.
C12.
Cll.
C16.
Cll.
C8 .
C17.
C16.
C1Z.
C8 .
Cl
H20. 01.
H9 . 02
Hid
H26
H26. 03
H8 .BR1
H18. 02
H22. 01
H26
H26
H26. 03
H13. Nl
H13. Nl
H13. Nl
H13. Nl
H16
H20. 02
H2U. 01
Hlf>
H16
H2U. 01,
H6 . 03
H2i». 01
H2
-------
TABLE Dl. (Continued)
MH
220
220
220
221
222
222
222
222
222
222
222
ZZZ
ZZZ
ZZ
51.9651,31.
13351.81,
629732
1795160
20195088
5085
571.32
7671,1,
203123
50i.6i.965
7201.162
2363715
218019
28<,8i«222
51,1(638
5571, Jl,5
106332
51.812725
7278651
5039761,3
551621.19
1731880
5 -1 <2H I -NAPHTHA*
OC TAHYDRO- ItA. 5-DIME THYL-J-1SOPROPYL- 2(1H)-NAPHTHALENONE
FARNESOL
3,5-T-8UTYL-<»-HYOROXY-2tt
162 Cd . H2 . 02
Cll. H18. N2
Cll. Hid. N2
C18. HlO
C13. H22. 03
C12. H18. 01,
C21. H<<2. 02
CIS. H12-
Cli.. H28. 02
37 CH. H28. 02
C15. H16. 02
157 Cll.. H28. 32
Cli. H2A. 01.
Cl5. H32. Oi
CIO. H12. 01.
Clt. H13. 03
Cll,. H28. 02
53 CH. H28. 02
ClU. H12. 03
CIS. H32. 31
C6 . H3 . Nl
cm. HH.
C6 . H2 . 01
C18. Hli.
Cll. H18. 05
Cl. . H8 . 01
C6 . H2 . 01
Cl2. H22. 01.
.CL2
. 11
. Pi
.CLI.
. 03
. 03
. SI
.CLI
.CLI.
.CLU
.BR2
. CL4
t SEE FOOTNOTE ON LAST PAGE
(Continued)
-------
TABLE
(Continued)
HATER POLLUTANTS PAGE <)Z
IS3
C»
MH
231
232
232
232
Z32
t32
232
Z3<>
23>t
231.
231.
23V
231.
231.
231.
231.
231.
231,
236
236
23S
236
Z36
236
236
236
236
236
236
236
233
23)
23*
238
238
i.39
233
233
238
239
2i«0
21,0
2M>
2M)
CAS NO.
6006015
50066
1.536883
671.251,7
1003
2ii255ii9
3m BISBENZENE
1,1-BISCO-ETHYLPHENYLlETHANE
, 1-BIS IM-ETHYLPHENYL) ETHANE
HEXAMETHYL 8IPHENYL
1-HEPTADECENE
i, i-BIS (I.-ETHYLPHENYL i ETHANE
,i,t-OIETHYLBI8ENZYL
ASYMMETRICAL BIS IE THYLPHE N YD ETHANE
1, 5-OIKHtNYL-3-PtNTANONE
OIBROMOCYCLOHEXENE
BROMOOICHLOROANILINE
i»,i,»-DIMtTHOXYSTlLBENE
HEPTdOECANE
i.-BROMO-3-PHENYLSYONONE
EXALTOLIOE
DATA
DU
41
642
671
410
174
987
165
460
1123
SET CORRELATION t
AWT T4 T5
81
101
766
538
6
547
159 212 170
856
857
73
917
206
579 248
815
817
818
57
613
614
396
724
298 58
209
950
627
883
1077
797
857
MOLECULAR FORMULA
C16. H2S. Nl
ClZ. HiZ. N2 . 03
C17. H28
C17. H20
Cl3. H28. Oi«
Cl
-------
TABLE Dl. (Continued)
WATER POLLUTANTS PAGE
MH
242
21.2
III
2W2
21.2
2i»2
21.2
21.2
21,2
21.2
21.2
21.2
i>ti
21.3
2i.i.
21.'.
2<>i.
21.'.
21.6
21.6
21.6
2Kb
2Kb
21.6
21,8
2i<9
21.8
21.9
2K8
2'
-------
TABLE Dl. (Continued)
HATER POLLUTANTS PAGE <*
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE—THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN AN* OF THE CONCENTRATES ANALYZED
DATA SET CORRELATION t
IxJ
00
00
MM
£51,
ZSd
251.
251.
251.
25".
25".
£51.
£55
256
£56
256
356
256
256
258
259
£59
£58
253
258
26u
26i,
260
262
£63
26<>
261.
266
£66
266
268
£69
£69
269
269
£68
268
270
270
£70
£70
270
270
£7J
CAS NO.
93765
5931,53
38963916
2091£9«.
3731.99
575893
713
£51,
571«3
713261,1
li.5i.859
121.061
25323686
51.5
1119£06
87663 y.
573i»53d9
305£589i.
105997
56051606
36500 <>£
2326£795
£0890937
23262781.
£7193868
527£09
£032>t3l9
87865 '/.
1£6738
50901.15
107377
629925
7££5663
55000538
1120258
56591.16
353891. ".u
£6£ 65996
771.71. y.<
ll£396>
506i£7
1.11 moo 5
1019
17670756
557£3938
COMMON NAME
X»<£,1.,5-TRICHLOROPHENOXY I ACETIC ACID
OCTAOECANE
I.- (1.5-OIMETHYL-3-OXOHEXYLICYCLOHEXANECARBOXYLIC ACID
PALMITOLtIC ACID
TRANS-9-HEXADECENOIC ACI3
X.£,i.,6-TRICHLOROPHENOXYACETIC ACIO
TRICHLOROPHENOXVACtTIC ACIO (ISOHER UNKNOHN)
i-t(£,6,6-IRIMETHYL-J-CYCLOHEXEN-l-YL)OXY]-l-BUTANOL ACETATE
/.PALMITIC ACIO
METHYL PtNTADtCANOATE
1-HEPTAOECANOL
ETHYL MYRISTATE
•TRICHLOROBIPHENYL
ISOPALMITIC ACIO
01 VINYL MERCURY
>»JHEXACHLORO-1,3-SUTADIENE
5-EPIOtOXYPOOOCARPIC ACI3
POLYFORMALDEHYOE
OIBUTYL AOIPATE
DIBUTYL-3-METHYLGLUTARATE
OCTAHYDRO-l.l.A-DIMETHYL-1-PHENANTHKENE CARBOXILIC ACID,*
1,£ 5,6-BIS-0-ISOPROPYLIDENE-8ETA-D-TALOFURANOS£
1,2 1..5-OI-0-ISOPROPYLIDENE-ALPHA-0-FRUCTOPYRANOSE
2,3 5,6-OI-O-ISOPROPYLIOENE-ALPHA-O-TALOFURANOSE
OOOtCrL PHtNOL
•PENTACHLOROANILINE
TETRAPROPYLENE GLYCOL METHYL ETHER
'»tPENTACHLOROPHENOL
XTRIUUTtL PHOSPHATE
9-OCTAOECENAL
(CHtOROMETHYL) METHYL MERCURY
NONAOECANE
7-HEXYLTRIOECANE
1, i.-OIMETHYL-5-OCTYLNAPHTHALENE
METHYL PALMITOLEATE
2,3,i.,5,5-PENTACHLORO-£,i.-PENTAOIENOIC ACIO
2,1.,5-ThICHLOROPHENOXY ACETIC ACID, METHYL ESTEp
HEPTAOtCANOIC ACIO
ttHEX IHEXACHLOROCYCLOPENT4DIENEI
METHYL PALMITATE
MARGARIC ACIO
ETHYL PENTAOECANOATE
2-KETOPALMITIC ACIC
tTHYL 7-MtTHYLM»f.ISTATE
7-METHYL-7-HEPTAOECANOL
*METHYL ESTER
DM
190
998
215
275
528
4
631
868
187
144
592
753
570
12
13
502
352
857
423
83
505
594
379
632
25
337
677
754
AWT
1034
816
85
79
264
289
28
742
269
1035
321
T4 T5 MOLECULAR
C8 .
C18.
45 127 CIS.
32 Cl6.
C16.
C8 .
C8 .
Cl5.
C16.
C16.
Cl7.
C16.
C12.
87 C16.
86 175 Ci. .
H5 .
H38
H26.
H30.
H30.
H5 .
H5 .
H26.
H32.
H32.
H36.
H32.
FORMULA
03
03
02
02
03
03
03
02
02
01
02
.CL3
.CL3
.CL3
H7 .CL3
H3£.
H6 .
02
HG1
C<> .CL6
227
919
310
293
803
162
165
1004
417
166
176
C17.
ca .
CU.
Clt,.
46 C17.
C12.
C12.
C12.
cie.
C6 .
102 C13.
C6 .
152 44 C12.
CIS.
C2 .
C19.
Cl9.
C20.
C17.
C5 .
C9 .
58 C 17 .
C5 .
219 C17.
C17.
C17.
C16.
(U7.
CIS.
H££.
H18.
H26.
H26.
H2£.
HZO.
H20.
Hze.
H30
H2 .
H28.
HI .
H27.
H3«i.
H5 .
H1.D
Hi.4
H28
H32.
HI .
H7 .
H32.
CL6
H3i<.
H3«t.
H31..
H30.
H3i>.
H38.
02
09
01.
01.
02
06
06
06
Hi
05
01
3
-------
TABLE Dl. (Continued)
HATER POLLUTANTS PAGE
TRICHLOROHtPTAFLUOROBUTANE
tX'tLINOANE
+ X.LINOANt (BtTA ISOMERI
•tTETRACHLOROB IPHENYL
•»«2.2- tETKACHLOROBIPMENYL
AMYL BUTYL PHTHALATE
METHYL-9, 12, 15-OCIAOECAKIENOATE
X •PtNTACHLORONITkOStNZENE
METHtL-9.11-OCTAOECAOItNOATE
(1ETHYLOCTADEC-1G-ENOATE
MtTHtL OLLATc
9-OCrAOECENOAft (GEOMErUY UNKNOWMI
MLTHTL EUAOATt
METHYL-11-OCTAOtCENOATE
DM
633
997
996
76
1
20
809
88
512
600
276
52
853
383
135
242
934
152
949
356
1165
510
992
357
975
974
991
AWT T4
1090
175 57
500
311
918
78
94
3
81
300 75
475
291 106
143 39
821
75
462
29
13
799
584
469 220
1106
885
696
1037
1040
940
1089
80
138
T5 MOLECULAR FORMULA
C17. H3<«. 02
C17. H3I.. 02
C18. H38. 01
Cli>. H19. 03 .CLl
C16. H32. 03
C22. H12
C22. H12
145 C5 . H6 .CL6
C16. H22. 01.
C16. H22. Oil
C16. H22. 01.
CIS. H30. 02
C9 . H8 . 02 .8R2
C18. H32. 02
C18. H35. Nl . 01
C18. H3i«. 02
C6 .CL6
C20. H. 02
CIS. H3i>. 02
C18. H3. 02
C19. H36. 02
C19. H36. 02
C19. HJ6. 32
CIS. H36. 02
C19. H36. 02
t SEE FOOTNOTE ON LAST PAGE
1t 2.4-01BROMOBENZ01C ACID (MW 278):
LISTED IN MH 250 RANGE
(Continued)
-------
TABLE Dl. (Continued)
HATER POLLUTANTS PACE *6
MH
29S
298
29S
298
298
298
JOd
300
302
302
3fl«
302
302
302
302
3fl<»
306tt
311
3lt
312
312
3J.2
312
312
31*
31*
31*
31*
31*
3i5
316
316
322
322
322
32*
32*
32*
32*
326
326
326
328
330
33*
CAS NO.
112618
1*010232
629969
38*11120
625
6*63U(
515570*
57983365
2136790
62*
26*
5835267
795*9
S*3u7*25
6080
*087696
131180
8*9990
629970
506309
17319*8
85687
111615
3121
109*33
4.2357*1
110338
110388
1759
388*21*7
72559
3*2*826
3337*2S6
1020
60333
25*29292
63S675
800
38380028
115S66
182810**
995
20Ci
8*617
8*753
IDENTIFIED COMPOUNDS BY MOLECULAR HEIGHT
NOTE—THIS LIST MAY CONTAIN COMPOUNDS THAT HAVE NOT BEEN FOUND IN ANY OF THE CONCENTRATES ANALYZED
COMMON NAME
METHYL STEARATE
ETHYL MARGARATE
ARACHIOVL ALCOHOL
3UTYLBENZYLPHTHALATE
OIOEHYOROGENATEO ABIETIC AGIO
NONAOECANOIC ACID
OEHYOROABIETIC ACID
3ISI1-METHYLPROPYLI NONANE01 QATE
2,3,5.6-TETRACHLOROTEREPHTHALIC ACID
AaitTIC ACID
3-DICHLOPONETHYL-*.6-01-T-BUTYL-0-BE NZOQUI NONE
ISOPIMARIC ACIO
LEVOPIMARIC ACID
7-ETH£NYLOODECAHYDRO-l,*A,7-TRIMETHYL-l-PHENANTHRENECAR'ir
1.3-OIHETHYL-2-(i-ISOPROPYLPHENYLIETHYLCYCLOHEX«ME CAR-
HYOROGtNATED ABIETIC ACID BOXILIC ACID
OIAHYLPHTHALATE
OICYCLOHEXYLADIPATE
OOCOSANE
XARACHIOONIC ACIO
METHYL NONADtCANOATE
XtlBUTYL BENZYL PHTHALATE
ETHYL STEARATE
ISOEICOSANOIC ACID
OIBUTYL StBACATE
METHYLOEHYOROABIETATE
ADIPIC ACIO. OIHtXYL ESTER
DIHEXYLAOIPATE
HEXANEOIOIC ACIO, DIHEXYL ESTER
2,3,*,5,6-PENTAFLUORO-N-(2-PHENYLETHYLJBENZAMIOE
X.ttDOE
X.O.P-DDt
taUTYL-aUTOXY ETHYL PHTHALATE
3-«2.3-DIBROMOPH£NYLl PROPANOIC ACID
9.12-OCTADtCAOItNOIC ACID
•SPENTACHLOR08IPHENYL
TRICOSANE
*«-$PENT«CHLOROBIPHENYL » OTHER PCBS
2.2*.3,*,S*-PENTACHLOKOBIPHENYL
Z'TRIPrtENYL PHOSPHATE
ETHYL NONADECANOATt
TRIS (CHLOROPROPYLt PHOSPHA TE
2,*,o-rRIBROMOPHENOL.
X.SUICYCLOHEXYL PHTHALATE
Xt$OIHtXYL PHTHALATE
*BOXYLIC ACID
DATA
DM
128
693
59
140
571
815
788
292
338
391
341
459
1166
882
810
38
703
265
SET CORRELATION t
AWT T4 T5
167 235
457
490
463
76 8
740
732
193
171
163
373
283
985
158
59
697
192
364
157 177 33
59
1068
1043
40
942
1041
1014
145
721
82
1091
MOLECULAR FORMULA
C19. H38. 02
C19. H38. 02
C20. H*2. 01
cis. HIS. o>t
C20. H26. 02
C19. H3S. 02
C20. H28. 02
C17. H32. OU
C8 . H2 . 0>> .CL0. 02
CIS. H3
-------
TABLE Dl. (Continued)
HATER POLLUTANTS PAGE.
-------
APPENDIX E
HERL PROCEDURES FOR THE PREPARATION OF THE
CINCINNATI, OHIO, OCTOBER 17, 1978 CONCENTRATES
HERL personnel prepared the three concentrates (TIC, T1X, and T1Y) of the
Cincinnati, Ohio, October 17, 1978 sampling. These three concentrates were
the only ones not produced by GSRI. Since the procedure used by HERL was some-
what different from that used by GSRI, the important differences are summarized
here.
DW sampled from the laboratory tap was split into two streams of essen-
tially equal flow of about 500 ml/min. One of the streams was used to fill
1510-liter capacity stainless steel reservoirs for later RO processing. The
other stream was acidified to pH 2 with a metered flow of 6N HCL immediately
before passage through a 25 cm by 3.2 cm column containing about 190 cc of
XAD-2 resin. The flow rate and bed volume resulted in a mean column residency
time of about 10 seconds. The XAD-2 resin had been prepared for use by con-
secutive Soxhlet extraction with methanol, acetonitrile, ethyl ether and meth-
anol. The sampling at these specified rates required about 50 hours after
which the XAD-2 resin was eluted with 450 ml of unpreserved distilled in glass
grade diethyl ether. Volume reduction to about 10 ml by KD distillation pro-
duced concentrate T1Y.
Before beginning RO processing of the 1510-liter sample, the pH was ad-
justed to 4.3 by the addition of 0.52 I of 6N HC1. In contrast to the GSRI
RO processor (Figure 1) , the HERL system was equipped with only the cellulose
acetate RO unit. RO volume reduction proceeded until the brine was reduced
to about 70 liters. Further volume reduction was accomplished by lyophiliza-
tion to about 800 ml of liquid and about 500 ml of salts. The salts were re-
moved by filtration and subjected to vacuum drying. The dry salts were
extracted with pentane and methylene chloride aliquots that were reused in the
extraction of the liquid. The 800 ml of liquid was extracted in the-usual
sequence (pentane, methylene chloride and, after acidification to pH 2,
methylene chloride again), the extracts were combined and volume reduction to
about 5 ml by KD distillation produced concentrate TIC. The extracted 800 ml
of acidified brine was then passed through an XAD-2 resin column identical to
the one described above for concentration by direct XAD-2 adsorption. The
column was eluted with ethyl alcohol, as above, and final volume reduction to
10 ml produced concentrat T1X.
292
-------
APPENDIX F
CONTENTS AND LISTS OF TABLES FOR VOLUMES 2 AND 3
The contents and lists of tables for the other volumes of this report
are presented here to aid the reader's grasp of the scope of this report in
the absense of these other two volumes.
293
-------
VOLUME 2
CONTENTS
Abstract
Tables -. v
Abbreviations and Symbols viii
Brief Description of All Volumes of the Final Report x
Acknowledgements . xii
1. Introduction 1
2. Guide to the Computer-Printed Listings 2
Selection of Concentrates for Combined Results Tables . 2
DW Results—Tables 3 Through 11 3
AWT Results—Tables 12 Through 20 5
Combined DW and AWT Compound Identification Results—
Tables 21, 22 and 23 5
Compounds in the Database Listed by Molecular Weight—
Table 24 5
Appendices
A. Compound Identification Results for Two Concentrates
Not Included in the Tables of Combined Results ....... 348
B. Tables of Contents of Volumes 1 and 3 372
294
-------
VOLUME 2
TABLES
Number
1 Pertinent Concentrate Data for Drinking Water (DW)
2 Pertinent Concentrate Data for Advanced Waste Treatment (AWT) Water .
3 Combined Listings of Identified Compounds Found in DW Concentrates,
Showing the Size of the GC Peak
4 Combined Listings of Identified Compounds Found in DW Concentrates,
Showing the Identification Status ................. 39
5 Combined Listings of Identified Compounds Found in DW Concentrates,
Showing Molecular Weight and Formula ................ 59
6 Occurrence of Molecular Functional Group Types in DW Concentrates,
Showing the Number of Occurrences ................. 99
7 Occurrence of Molecular Functional Group Types in DW Concentrates,
Showing the Number of Occurrences as a Percentage of the Total
Number of Identified Compounds ................... 100
8 Occurrence of Molecular Functional Gfoup Types in DW Concentrates,
Showing the Total GC Peak Size for Each Group on the SP1000
GC Column ............................. 101
9 Occurrence of Molecular Functional Group Types in DW Concentrates,
Showing the Total GC Peak Size for Each Group on the SP2100
GC Column ............................. 102
10 Occurrence of Molecular Functional Group Types in DW Concentrates,
Showing the Total GC Peak Size for Each Group on Both
GC Columns ............................. 103
11 Occurrence of Molecular Functional Group Types in DW Concentrates,
Showing all Tabulated Parameters ..................
12 Combined Listings of Identified Compounds Found in AWT Concentrates,
Showing the Size of the GC Peak .................. 107
13 Combined Listings of Identified Compounds Found in AWT Concentrates,
Showing the Identification Status ................. 132
295
-------
VOLUME 2
TABLES (Continued)
Number
14 Combined Listings of Identified Compounds Found in AWT Concentrates,
Snowing Molecular Weight and Formula .
15 Occurence of Molecular Functional Group Types in AWT Concentrates ,-
Showing the Number of Occurrences .................. 182
16 Occurrence of Molecular Functional Group Types in AWT Concentrates,
Showing the Number of Occurrences as a Percentage of the Total
Number of Identified Compounds . . <, ................ 183
17 Occurrence of Molecular Functional Group Types in AWT Concentrates,
Showing the Total GC Peak Size for Each Group on the SP1000
GC Column .............................. 184
18 Occurrence of Molecular Functional Group Types in AWT Concentrates,
Showing the Total GC Peak Size for Each Group on the SP2100
GC Column .............................. 185
19 Occurrence of Molecular Functional Group Types in AWT Concentrates,
Showing the Total GC Peak Size for Each Group on Both
GC Columns ....... , . . . . ................. 186
20 Occurrence of Molecular Functional Group Types in AWT Concentrates,
Showing all Tabulated Parameters ... ............... 187
21 Combined Listings of Identified Compounds Found in Both DW and AWT
Concentrates, Showing the Size of the GC Peak ............ 190
22 Combined Listings of Identified Compounds Found in Both DW and AWT
Concentrates, Showing the Identification Status ....... .... 227
23 Combined Listings of Identified Compounds Found in Both DW and AWT
Concentrates, Showing Molecular Weight and Molecular Formula .... 264
24 Compounds in the Chemically Descriptive Level of the Identified
Compound Database — Listed by Increasing Molecular Weight ...... 301
296
-------
VOLUME 2
TABLES (Continued)
Number Page
Appendix A
LA Compounds Identified in the Miami II XAD Concentrate
(Code M2X), Listed by GC Peak"Si2e 349
2A Compounds Identified in the Miami II XAD Concentrate
(CodeM2X), Listed by Molecular-Weight,-,-,- 355
3A Compounds Identified in the New Orleans II XAD Concentrate
(Code N2X), Listed by GC Peak-Size 361
4A Compounds Identified in the New Orleans II XAD Concentrate
(Code N2X), Listed by Molecular Weight 367
297
-------
VOLUME 3.
COHTENTS
Abstract. ...........-••.•-.--•. ............... ii:i-
Figures ..... ............-> ...............
Tables ..... ...... ..... . . «, ...............
Abbreviations and Symbols . ..... « .................
Brief Description of All Volumes of the Final Report ........... xiv
Acknowledgments ..... ......... ............... xvi
1. Introduction. ....... ................... 1
2. Conclusions . ° . ° ........ ............... 3
3. Recommendations . ...... . . ................ 4
4. Description of the Samples. . . ................. 5
Cincinnati GAC Contactor A Samples. .... ......... 5
Cincinnati GAC Contactor D Samples. ... I ......... 8
Samples for Monitoring RO Pre-Concentration of Jefferson
Parrish, Louisiana, and Poplarville, Mississippi ...... 8
Samples for Method Validation of the 10-Liter
Extraction Procedure. .... ............... 10
5. Analytical Scheme . . . . ...... .............. 11
Rationale for the Analytical Scheme . . ........... 11
Distillation of Extraction Solvent .............. 12
Reagent Water ...„...» ................ 13
Liquid-Liquid Extraction of 10-Liter Samples ......... 13
Extraction of Blanks ..... . ............... 16
XAD-2 Resin Extraction of Samples .............. 17
Sample Partitioning ...... ............... 17
GC-MS Analysis ...... . ................. 21
Compound Identification and Confirmation ........... 24
Estimation of Sample Constituent Concentrations ....... 25
Quality Assurance ...................... 27
Data Management ....... ................ 27
6. Results and Discussion. ..... ................ 29
Thirteen Samples Associated with Cincinnati GAC
Contactor A ........................ 29
Seven Samples Associated with Cincinnati GAC Contactor D. . . 46
Comparison of Cincinnati GAC Contactor A and GAC
Contactor D Results .................... 55
Analysis Results for the 10-Liter Extraction Process Blank. . 56
Validation of the 10-Liter Liquid-Liquid Extraction
Procedure .......... . .............. 5-7
Samples for Monitoring RO Pre-Concentration of DW at
Jefferson Parrish, Louisiana, and Poplarville, Mississippi. 65
References
298
-------
VOLUME 3
CONTENTS (Continued)
Appendices
A. The 6-Digit Code Used for Small-VoljMe Water Samples and
Their Fractions rY'7J.N ; 78
B. Compound Identification Results for the Thirteen Cincinnati
GAG Contactor A Samples—Computer-Printed Tables 80
C. Compound Identification Results fof the Seven Cincinnati
GAG Contactor D Samples--—Ccfmputer-Print'ed Tables 97
D. Analysis Results for the Reagent "Water Samples—Labeled GC-MS
Chroma to grams '....... 107
E. Analysis Results for Cincinnati Tap"Water and Lyophilized
Cincinnati Tap Water ...'.' 132
F. Contents and Lists of Tables for Volumes 1 and 2 159
299
-------
TABLES
Number
1 Deuterium-labeled compounds used as internal standards ..... 15
2 GC peak relative uaizB Contactor A ............ 32
5 Compound identification results for. the thirteen samples
associated with Cincinnati GAC Contactor A ........... 36
6 Possible artifact. cpoj.pourid& contributed by the RO apparatus
and other sources* ,>.i ,...,»..,». ................ 45
7 Compound identification statistics?, for the seven samples
associated with Cincinnati GAG "Contractor D ........... 47
8 Residue weight analysis results for unpartitioned extracts
and fractions; Cincinnati ; .GAC •Ccmtaetor D ............ 48
9 Compound identification results, for the seven samples
associated with Cincinnati GAC Contactor D ........... 50
10 GC-MS analysis results of the acid fraction for the
Jefferson Parrish 10-fold cellulose acetate RO concentrate,
acidic XAD-2 extraction. .... ................ 68
11 GC-MS analysis results of the aroajatic/medium polarity
fraction for the Jefferson Parrish 10-fold cellulose
acetate RO concentrate, acidic XAD-2 extraction ......... 73
APPENDIX B
Bl Compound identification results for the Cincinnati GAC
Contactor A sample, T4R5, pre-GAC 100-fold nylon
RO brine ............ ............. ... 81
300
-------
VOLUME 3
TABLES (Continued)
Number Page
B2 Compound identification results for the Cincinnati GAC
Contactor A sample, T4R4 pre-OMJJXr-fold nylon
RO brine .......... ^^^-^. .............. 82
B3 Compound identification results for the Cincinnati GAC
Contactor A sample, T4R3, pre-GAC cellulose acetate
RO permeate .......................... 83
B4 Compound identification results for the Cincinnati GAC
Contactor A sample, T4R1, pr«-eGACLJLO-f old -cellulose acetate
RO brine .......... ^_.,.._,.. ______ _. . .. -».,,... ..... 85
B5 Compound identification results. ;:6or the Cincinnati GAC
Contactor A sample, T4R2, pre-CAC lOOE-fold cellulose
acetate RO brine ....................... 86
B6 Compound identification results. fdr the Cincinnati GAC
Contactor A sample, T4R6, pre-GAC, 200-fold cellulose
acetate RO brine ...... -_- , .... =. . -. ,..;. ........ 87
B7 Compound identification results for the Cincinnati GAC
Contactor A sample, T4E1, pre-GAC>ilO 'liters, no RO
processing ........ •.-.?./.«..-. <. >. •. -.- - ........ 88
B8 Compound identification results ^or. the Cincinnati GAC
Contactor A sample, T4G1, post-rGAC,. 10 liters,- no RO
processing .......................... 89
B9 Compound identification res'ui'tst fdr the Cincinnati GAC
Contactor A sample, T4G2, post-GAC, 200-fold cellulose
acetate RO brine ....... -., .. . . . . -.-- .- . ........ 90
BIO Compound identification results for the Cincinnati GAC
Contactor A sample, T4Y2, pre-iQAC ^10-liter XAD-2
concentrate; sulfite preserved.. ..- ..... .......... 91
Bll Compound identification results for the Cincinnati GAC
Contactor A sample, T4Y4, pr'erGAC 10-liter XAD-2
concentrate ......... • • '•- ............... '-^
B12 Compound identification results for the Cincinnati GAC
Coatactor A sample, T4Y1. pre-GAC 10-liter XAD-2 permeate,
sulfite preserved ....................... 95
B13 Compound identification results for the Cincinnati GAC
Contactor A sample, T4Y3, pre-GAC 10-liter XAD-2 permeate ... 96
301
-------
3
1 TABLES" [l Cont inu ed )
Number
APPENDIX C
Cl Compound Identif icatioit r^ulff "for the Cincinnati GAG
Contactor p sample, T5R4,' pre^-GAC 200- fold cellulose
acetate RO '''
C2 Compound identification results for the Cincinnati GAG
Contactor D sainple^VTSELr prer-GAC,. 10-liters, no RO
processing. . -<_;. r. . _^,-,. -v:iy»« •: ...............
C3- Compound identification .results £f or the Cincinnati GAC
Contactor D sample, TSGl-^, p^st^GAC, 10-liters, no RO
processing. . . . ... ...«._. « ;._•_•_ ..............
C4 Compound identifi/atidn;resiii£sTfpr the Cincinnati GAC
Contactor D sample, T5YI, pdst-GAC, XAD-2 concentrate ..... 102
C5 Compound identification results for the Cincinnati GAC
Contactor D sample, T5R1, post-GACs 10-fold cellulose
acetate RO brine ........................ 104
C6 Compound identification results for the Cincinnati GAC
Contactor D sample, T5R3, post-GAC, 200-fold cellulose
acetate RO brine. ......... ............ „ . , 105
C7 Compound identification results for the Cincinnati GAC
Contactor D sample, T5R2, post-GAC, 10-fold nylon
RO brine ......... , . . .'". . .............. 106
APPENDIX D
Dl GC-MS analysis results for the acid fraction of the
10-J.iter reagent water sample, S1Q ........... . . . . 110
D2 GC-MS analysis results for the aromatic /medium
polarity fraction of the 10-liter reagent water sample, S1Q. . . 113
D3 GC-MS analysis results for the unpartitioned aliquot
of the 10-liter reagent water sample, S1Q ......... ... 117
D4 GC-MS analysis results for the acid fraction of the
10-liter reagent water sample, S2Q ...... . ........ 122
D5 GC-MS analysis results for the aromatic /medium
polarity fraction of the 10-liter reagent water sample, S2Q. . . 125
D6 GC-MS analysis results for the unpartitioned aliquot
of the 10-liter reagent water sample, S2Q ....... ..... 130
302
-------
VOLUME 3
TABLES (Continued
Number £2££
APPENDIX E
El GC-MS analysis results for the acid fraction of the
10-liter Cincinnati tap water sample, T3K ....... ...... 135
E2 GC-MS analysis results for the aroma trie /medium polarity
fraction of the 10-liter Cincinnati tap water sample, T3K. . . . 139
E3 GC-MS analysis results for the unpartitioned aliquot
of the 10-liter Cincinnati tap water 'sample, T?K ........
E4 GC-MS analysis results for the acid fraction of the
lyophilized 10-liter Cincinnati tap water sample, T3L ...... 150
E5 GC-MS analysis results for tHe aromatic /medium polarity
fraction of the lyophilized 10-liter Cincinnati tap
water sample, T3L ......... ...... ........ . 156
'303
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