DRAFT ANALYTICAL REPORT
ORLEANS AREA WATER SUPPLY STUDY
PREPARED AND SUBMITTED BY
LOWER MISSISSIPPI RIVER FACILITY
SLIDELL, LOUISIANA
SURVEILLANCE AND ANALYSIS DIVISION
REGION VI
U, S, ENVIRONMENTAL PROTECTION AGENCY
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DRAFT ANALYTICAL REPORT
NEW ORLEANS AREA WATER SUPPLY STUDY
/
Prepared and Submitted by
Lower Mississippi Rive_r Facility
SIidell, Louisiana
Surveillance and Analysis Division
Region VI
U.S. Environmental Protection Agency
Dallas, Texas
with Technical Assistance as Noted
This document is a preliminary draft. It
has not been formally released by EPA and
should not at this stage be construed to
represent Agency policy. It is being circu-
lated for comment on its technical accuracy
and policy implications.
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TABLE OF CONTENTS
Acknowledgement of Technical Assistance 1
Introduction 2-3
Summary of Experimental Methods 4-15
Analytical Results 18-20
Current Project Status 29-30
LIST OF TABLES
Page
TABLE 1. Distribution of Work Operations
New Orleans Area Water Supply Study 16-17
TABLE 2. Organic Compound Identifications
New Orleans Area Water Supply Study .21-26
Key to Symbols Used in Table 2 27-28.
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ACKNOWLEDGEMENT OF TECHNICAL ASSISTANCE
Valuable technical assistance in the performance of this project
has been provided by staff chemists and other personnel of the following
groups within the U. S. Environmental Protection Agency.
Analytical Chemistry Branch
Southeast Environmental Research Laboratory
NERC-Corvallis
U. S. Environmental Protection Agency
Athens, Georgia
Water Supply Research Laboratory
NERC-Cincinnati
U. S. Environmental Protection Agency
Cincinnati, Oh-io
Robert S. Kerr Environmental Research Laboratory
NERC-Corvallis
U. S. Environmental Protection Agency
Ada, Oklahoma
Houston Facility
Region VI Surveillance and Analysis Division
U. S. Environmental Protection Agency
Houston, Texas
We also wish to acknowledge the participation of the following
individuals or groups outside the Agency.
Mr. Gregor Junk
USAEC - Ames
Ames, Iowa
Gulf South Research Institute
New Orleans, Louisiana
The staff of the Lower Mississippi River Facility particularly wish
to express their grateful appreciation for the assistance extended in
the sampling operation by all plant personnel at the Carroll ton Water
Plant (City of New Orleans), the Jefferson Parish No. 4_Water Plant
(Metairie) and the Jefferson Parish No. 2 Water Plant (Marerro).
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INTRODUCTION
In July 1974, representatives of the State of Louisiana and the
City of New Orleans tendered a request to the Region VI Administrator,
United States Environmental Protection Agency (EPA), that the agency
undertake a sampling and analytical survey designed to determine, to the
extent possible, uie identities and quantitative concentrations Df trace
organic compounds which might be present in the finished water of the
i
Carroll ton Water Plant (City of New Orleans), Jefferson Parish No. 1
Water Plant (Metairie), and the Jefferson Parish No. 2 Water Plant
(Marerro). The request was accepted and agreed to by the EPA Region VI
;
Administrator. Immediately thereafter, a plan and schedule were formulated
for conducting the necessary sampling and'an assignment was made of an
analytical coordinator to make arrangements for the required analytical
assistance. The assignment for sampling and analytical coordination was
given to the Lower Mississippi River Facility, Slidell, Louisiana, a
field facility of the Region VI Surveillance and Analysis Division.
This facility was instructed to have sampling operations completed by
mid-August 1974, and an analytical report issued by the end of October
1974. The present report is the Draft Analytical Report for this project.
It cannot be considered a final report as some phases of the analytical
work are incomplete. However, sufficient information is on record to
warrant issuing this report as scheduled. This analytical study did not
encompass an evaluation of the public health significance of the results
presented herein.
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A very comprehensive sampling and analytical program was developed
and placed in operation, as is illustrated in Table I and described in
some detail in the Summary of Experimental Methods. It may be necessary,
however, to explain one thing here. The carbon adsorption methods
sampling program was established on the assumption that a person would
normally consume one liter of water (approximately one quart) per day.
Thus the use in Table 1 of the terms 70 year equivalent, 10 year equivalent,
1 year equivalent, etc. has reference to the volume of water sampled
equivalent to the amount a person might consume in that period of time
t
at the one liter per day rate. The other sampling methods were added
to the project to provide.a means of detecting compounds of a type
i
undeterminable by the carbon adsorption-chloroform extraction methods
>
or to provide some comparative evaluation of sampling methods'in an
as yet experimental stage of development.
To perform the necessary analytical work for this project, the
analytical coordinator through the Regional Administrator requested
and was granted the technical assistance of several groups within the
Environmental Protection Agency's research centers having highly
developed and competent analytical expertise and the necessary instru-
mentation to perform the required analytical operations. While their
assistance has been acknowledged in a previous section, it should be
stated here that the actual analytical results presented herein represent
the efforts predominantly of the Analytical Chemistry Branch, Southeast
Environmental Research Laboratory (EPA), Athejjs, Gepjcgia, and the Water
Supply Research Laboratory, NERC-Cincinnati (EPA), Cincinnati, Ohio.
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SUMMARY OF EXPERIMENTAL METHODS
Shown In Table I is a distribution of work operations for the New
Orleans water supply study as developed. This table provides in shcrt
form information on the sampling methods employed, the specific water
.plants sampled, inclusive dates sampling was performed, the group
*
performing the sampling'operation, water volume sampled, group preparing
the sample for analysis, and finally the group performing the analysis.
*
Below is a brief description of the various sampling, sample preparation,
and analytical methods used.
Sampling Methods
Carbon Adsorption. Three types of carbon adsorption units were
employed. The Mega sampler is a relatively large scale trailer mounted
unit obtained for the purpose of this project from NERC-Cincinnati. It
consists of four cylindrical columns which can be packed with activated
carbon (approximately 22 pounds of carbon per unit) and connected in
series. In this study only two of these columns in series were used.
The Mega sampler, was employed only at the Carrollton water plant.
The CAM sampler- is a Pyrex cylinder "3" diameter by 18" length of
sufficient capacity to contain approximately 12 ounces of granular
activated carbon. These units are outfitted with various fluid flow
control and measuring devices. In collecting the 70-year equivalent
samples, two packed columns connected in series were employed at each
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plant. In collecting the ten-year and one-year equivalent samples, only
one unit per sample was employed.
The Mini-sampler is a miniaturized version of the CAM sampler. The
sample column is of Poly Vinyl Chloride (PVC) construction and of
sufficient capacity to contain 70 grams of 14 x 40 mesh activated
carbon. Like the CAM sampler, this unit is outfitted with fluid flow
measuring and control devices. The two-month equivalent samples and
*
one-day equivalent samples were obtained with one unit per sample at
each water plant.
In all carbon adsorpotion samplings, EPA personnel were assisted by
water plant personnel.
Precise details on the carbon adsorption sampling procedures may be
obtained by contacting
Mr. Ernest Doug!as_
U. S. Environmental Protection Agency
Lower Mississippi River .Facility
P. 0. Drawer N
Slidell, Louisiana 70458
XAD Resin Adsorption. This method developed by Mr. Gregor Junk,
USAEC-Ames, uses a macro-reticular synthetic resin (Rohm and Haas XAD-2)
contained in a miniature scale column. Its connections allow it to be
quickly connected to a small diameter water line. The unit consists
solely of the sample column not equipped with fluid flow control or
measuring devices. The sampling operations were performed by Mr. Junk
assisted by EPA-LMF personnel. Precise details on the XAD resin adsorp-
tion method may be obtained from:
Mr. Gregor Junk
USAEC-Ames
Ames, Iowa
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Liquid-Liquid Contact Extraction. This sampling method was adopted
by general agreement among the analysts with the intention that it-would
facilitate the recovery and analysis of highly volatile organics which
it was feared might be lost in the sample processing procedures associated
with the-adsorption techniques. At each plant tripli-cate one liter
samples of finished water were extracted in separatory funnels with 2 ml
m
of tetralin (a high boiling tetrahydronaphthalene). The immiscible
liquid phases were allowed to separate, ,the water drained and discarded,
*
and the tetralin recovered Tnto septum vials (Teflon-lined septums),
sealed and delivered to Southeast; Environmental Laboratory for analysis.
i
Precise details concerning the Liquid-Liquid extraction sampling method
may be obtained from:
Mr. John Pope
Analytical Chemistry Branch
Southeast Environmental Research Laboratory
U. S. Environmental Protection Agency
Athens, Georgia
Reverse Osmosis. This semi-permeable membrane water purification
method is as yet in an experimental stage of development for use as a
solute concentration method to facilitate trace organics analysis. Its
use for this purpose is undergoing evaluation at the EPA Water Supply
Research Laboratory, NERC-Cincinnati, which requested its inclusion in
the project with sampling performed by Gulf South Research Institute.
No analytical data from this technique have been derived for inclusion
in this report; con'sequently it will not be considered further at this
time. Details concerning this sampling method may be obtained from:
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Dr. Frederich Kcpfler
Water Supply Research Laboratory
NERC-Cincinnati
U. S. Environmental Protection Agency
Cincinnati, Ohio
Volatile Stripping (Volatile Organics Analysis, VGA; Bellar
Technique). This relatively direct sampling and analytical technique
employs helium gas stripping of volatile organics from a small water
sample with entrapment of organics on a Tenax or Chromosorb 101 column.
*
This column is then attached to the injection port of a gas chromato-
graph, and at elevated temperature with carrier gas flow the components
i
are desorbed directly into the analytical instrument.
Under the direction of the Water Supply Research Laboratory,
Cincinnati, samples for this technique were collected from a tap in the
Carroll ton water plant on September 23, 1974, by personnel of the Gulf
South Research Institute. Several 50 ml serum vials specially prepared
to eliminate any possible organic contamination were provided by WSRL.
Samples collected in a carefully prescribed manner were pre-chilled in
crushed ice and shipped by air freight in a styrofoam container to WSRL
in Cincinnati for analysis. Details of this procedure may be obtained
from:
Dr. Robert Melton
Water Supply Research Laboratory
NERC-Cincinnati
U. S. Environmental Protection Agency
Cincinnati, Ohio
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Sample Preparation Methods
This description of sample preparation methods is devoted .primarily
to the process operations which followed the Porous Solid Media Adsorp-
tion methods of sample collection.
Mega Carbon Processing. Immediately following its use in sample
collection at the Carrollton Water Plant, the Mega sampler was trans-
£
ported to the EPA-LMF labora'tories where the activated carbon was
removed, distributed in trays in a forced draft convection oven equipped
«
with an activated carbon intake air filter to prevent laboratory air
contamination and dried Tor~TO days at 40°C. At the end of that time
•
the carbon was sealed in new, precleaned, five-gallon metal cans and
*
taken to the Robert A. Taft Center in Cincinnati for solvent extraction.
Using the large scale permanently installed extraction unit specifically
fabricated for Mega-sampler carbon reflux extraction, the carbon was
extracted for 40 hours with 50 gallons of Analytical Reagent grade
redistilled chloroform. Following the 40 hour reflux extraction, the
extract was concentrated by conversion of the unit to a distillation
mode and distillation of excess solvent until a volume of approximately
1/2 gallon remained in the kettle. The concentrated chloroform extract
was then recovered and transported in sealed Teflon bottles to the
Southeast Environmental Research Laboratory for analysis. Precise
details on the Mega carbon sample processing may be obtained from:
Dr. William D. Larrgley or
Mr. Luther Hunt
U. S. Environmental Protection Agency
P. 0. Drawer N
Slide!!, Louisiana 70458
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CAM Carbon Processing. On removal from the sampling sites, the
CAM carbon cylinders were drained of excess water, sealed, and shipped
by commercial air carrier to Oklahoma City where they were claimed by
personnel of the Robert S. Kerr Environmental Research Center, Ada,
Oklahoma, and transported to the Center by private aircraft. The
columns were stored at 4°C until carbon processing could be initiated.
Columns were opened in a special carbon handling room designed to
minimize the potential for contamination. The carbon was transferred to
Pyrex glass dishes and dried at 35-38°C. for 48 hours under a gentle
/
•
flow of clean air in a mechanical convection oven. _The oven air inlet
was equipped with a~ carbon filter to prevent atmospheric contamination.
r
\
The dried carbon was transferred to 2200 ml Soxhlet extrators and
»
extracted for 48 hours with chloroform. The chloroform extracts were
filtered through solvent-extracted glass fiber filters to remove carbon
fines and then vacuum concentrated at temperatures not exceeding 27°C.
in rotary evaporators to final volumes of 30-60 ml. The concentrated
extracts were transferred quantitatively to 10 ml ampules, several
ampules being required to accommodate each extract. The ampules were
purged with dry, clean nitrogen and sealed while the contents were held
at -50°C. in a cold bath. The filled ampules were maintained under
refrigeration (4°C) until shipment to the Southeast Environmental
Research Laboratory by air mail. Further details on CAM carbon processing
can be provided by:
Dr. William Dww4ap
Robert S. Kerr Environmental Research Laboratory
U. S. Environmental Protection Agency
Ada, Oklahoma
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Mini-sampler Carbon Processing. The exposed Mini-sampler units,
drained and sealed, were forwarded by air express to the IP A "Region VI
Houston Laboratory facility (HNF). The carbon was removed and oven-
dried at 39.5°C for a period of 48 hours. The dried carbon was trans-
ferred to Soxhlet extractors equipped with fritted glass disc thimbles
and extracted for a period of 48 hours with spectrophotometric quality
chloroform.
Each of the two-month equivalent sampler extracts were split in a
t
1:1 proportion with one portion being evaporated to dryness at 70°C
for carbon chloroform extract residue determination and the other
t
portion reduced in volume in Kuderna-Danish, evaporative concentrators,
quantitatively transferred to 25 ml volumetric flasks and made up to
volume with chloroform. The one-day equivalent sample extracts were not
split for residue determination but the concentrative evaporation proce-
dures were followed.
The 25 ml extracts were later transferred into vials, sealed, and
shipped to Southeast Environmental Research Laboratory for analysis.
Further details on the sample preparation methods employed with the
mini-sampler may be obtained from:
Mr. Medardo Garza
I). S. Environmental Protection Agency
Houston Laboratory Facility
Houston, Texas
XAD Resin Samples
The XAD resin units were hand carried or sent by air carrier to
Mr. Gregor Junk at Ames, Iowa. The samples were extracted with redis-
tilled ethyl ether according to Mr. Junk's established technique on
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arrival at Ames. The ether was dried and concentrated to 1 ml in a
micro Kuderna-Danish evaporator for GC and GC-MS analysis at Ames. One
fourth of each extract was carried to Southeast Environmental Research
Laboratory for analysis. All extracts were refrigerated until tiwe for
analysis.
Further details on XAD resin processing may be obtained from:
Mr. Gregor Junk
USAEC-Ames
Ames, 'Iowa
Analytical Meth'ods
Southeast Environmental Research Laboratory
GC and GC-MS (Gas Chromatograph-Mass Spectrometry)
Gas chromatography was performed using*a Varian 1400 GC with a
flame ionization detector. Typical GC conditions were:
Column: 101 x 1/8" i.d. glass
Packing: 3% SP-2100 on 80-100 mesh Supelcoport
Program: 6 min. initial hold; then from 40°—280°
at 6°/min.
Carrier gas: helium at 20 ml/min.
Sample size: 2 ul
For the tetralin extracts, the temperature program was usually a 1
min. hold at 35° (with the oven door open) followed by an increase to
210° at 10°/min.
GC-MS instrumentation was a Finnigan 1015 system interfaced via a
Gholke separator to a modified Varian 1400 GC. This system was inter-
faced to a Systems Industries System 150 computer for data acquisition,
data storage, and data reduction and manipulation.
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Some initial GC-MS work was done on a Varian MAT CH5/DF system
interfaced to a Varian 2740 GC via a Watson-Biemann separator and to a
Varian SS-100 Data System. This instrument was later used for confir-
mation of the presence of Atrazine in the Carrollton 70-year CCE by
accurate mass measurement at a resolution of about 5000 amu.
Gas chromatography on these GC-MS systems was performed using a
•
similar column and conditions to those employed in the GC runs described
above. Mass spectrometer electron voltage was 70.
• - »
Mass spectra stored on disks from the Finnigan CG-MS runs were
compared via acoustacoupler connection with spectra in the EPA-Battelle
t
computer files at Battelle (Columbus).
Quantitative Analysis
- The Perkin-Elmer PEP-1 Data System, interfaced to a Varian 1400 GC
containing a SP-2100 column and operated under the conditions described
above, was used for computerized quantitation and retention time measure-
ments. Since Atrazine was present in all extracts of New Orleans samples,
it was chosen as an internal standard. A stock solution of 5 parts-per-
thousand of Atrazine (99.7% pure) in chloroform was the reference for
quantity of all identified compounds for which standards were obtained.
Standards, obtained from the laboratory supply or from commercial
sources, if time permitted, were mixed in known concentrations with
other standards and with a known amount of the Atrazine reference stock
solution. Mixtures were designed so as to obtain good GC peak resolution.
The Atrazine was assigned a flame response of 1.000 and, since its
concentration was known, the computer system was able to calculate the
flame response, as well as the relative retention time, of each standard.
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After tentative identification of compounds by GC-KS, a PEP-1
computer program was written for the GC-computer run of each extract,
allowing the computer to use the known flame responses to calculate
concentrations. In some cases, the flame response calculated for a
standard was also used for other compounds of the same chemical class.
The relative retention times, calculated for all compounds and printed
out by the computer, were then manually compared with those of the
available standards. It was necessary to dose the blanks with Atrazine
as an internal standard, since it was ascertained that Atrazine was not
*
present in them.
If time permitted, mass spectra of the standards were obtained on
the Finnigan GC-MS system for visual comparison with those of the
compounds.
Further details on the-analytical methods employed at SERL may be
obtained from:
Dr. A. W. Garrison, or
Dr. Larry Keith
Analytical Chemistry Branch
Southeast Environmental Research Laboratory
U. S. Environmental Protection Agency
Athens, Georgia
Water Supply Research Laboratory
Volatile Organics Analysis
The following instruments were used:
Perkin-Elmer Model 900 GC
Finnigan 1015[T- System Industries 150 GC/MS
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The volatile organics were purged from aliquots of the water and
adsorbed on a small column containing either Tenax or Chromosorb 103 as
described by Bellar and Lichtenberg. Qualitative analysis was accomplished
by GC/MS using a Chromosorb 101 column and operating the mass spectrometer
in the electron impact ionization mode.
Quantitative analysis of the major components of the volatile
•
organics was accomplished*by gas chromatography using the Perkin-Elmer
gas chromatograph filtered with 6 foot column of chromosorb 101 and
*
flame ionization detectors.
Standards of chloroform and dtchloroethane were prepared by introducing
i
5 Pi and 2.5 yl respectively into one liter of distilled water with a 5 Pi
*
syringe. This was thoroughly shaken until dissolution was complete.
This stock solution was theji diluted 100 fold resulting in concentrations
(calculated from literature values of the densities) of 78 ug/1 chloroform
and 31 ug/1 of dichloroethane.
The GC/MS was calibrated according to EPA (J. W. Eichelberger, L.
E. Harris, and W. L. Budde, Anal. Chem., 45^ 227 (1974) standard proce-
dures .
Further details on the analytical procedures employed at the Water
Supply Research Laboratory may be obtained from:
Dr. Robert Melton, or
Dr. Fredrich Kopfler
Water Supply Research Laboratory
NERC - Cincinnati
Ur~S. Environmental Protection Agency
Cincinnati, Ohio •
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Processing of Blanks
The foregoing discussion of sampling, preparation, and analytical
methods has been concerned with the processing of actual ScmrplBS.
However, to assure that components identified were actually derived from
the original samples and were not artifacts, contaminants, or inherent
components deriving from the sampling method itself, the sampling
media, commercial,solvents, or the sample preparations, it was necessary
t
to process blank samples taken through all stages of the operations in
parallel with the actual samples. The one exception to this was that no
sample blank was developed for the reverse osmosis sampling operation.
As a consequence of this; processing of blanks through the analytical
stage no components could be accepted .as deriving from the finished
water samples unless these components were not present at a significant
level in the blanks relative to the samples or unless they were identified
independently in one or more of the other methods. The details of blank
preparation, processing and analysis may be obtained from the individuals
previously referred to in discussion of the various methods.
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TABLE I
DISTRIBUTION OF WORK OPERATIONS
NEW ORLEANS AREA WATER SUPPLY STUDY
Sampling Method
Method Modification Plants Sempled Dates Sampled Sampled By Water Volume Sample Prepared By Analysis By
Carbon Adsorption
with Chloroform
Extraction
Mega Sampler
CAM 70 yr. equlv.
CAM 10 yr. equlv.
CAM 1 yr. equlv.
Mini-Sampler
2 Mo. equlv.
Mini-Sampler
Carroll ton
Car roll ton
Jefferson No. 1
Jefferson No. 2
Carroll ton
Jefferson No. 1
Jefferson No. 2
7/17-24/74
7/18-24/74
7/24-8/2/74
7/24-8/2/74
Carroll ton 8/6-7/74
Jefferson No. 1 8/6-7/74
Jefferson No. 2 8/6-8/74
8/13/74
8/13/74
8/13/74
Carrollton 7/30-31/74
Jefferson No. 1 7/31-8/1/74
Jefferson No. 2 8/1-2/74
Carrollton (repeat)8/6-8/74
Carrollton 8/6/74
Jefferson No. 1 8/6/74
Jefferson No. 2 8/6/74
LMF
LMF
LMF
LMF
LMF
LMF
LMF
LMF
LMF
LMF
LMF
LMF
LMF
LMF
LMF
LMF
LMF
300,000 Gals.
6,750 Gals.
6,759 Gals.
6,707 Gals.
963 Gals.
965 Gals.
1,300 Gals.
74 Gals.
90 Gals.
97.5 Gals.
62 liters
65 liters
60 liters
58 liters
1 liter
1 liter
1 liter
LMF
RSKERL
RSKERL
RSKERL
RSKERL
RSKERL
RSKERL
RSKERL
RSKERL
RSKERL
HNF
HNF
HNF
WSRL
HNF
HNF
HNF
SERL
SERL
SERL
SERL
stored in
sealed vials
at RSKERL
stored In
sealed vials
at RSKERL
HNF-SERL
HNF-SERL
HNF-SERL
WSRL
HNF-SERL
HNF-SERL
HNF-SERL
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Sampling Method
XAO Resin Adsorp.
with Ethyl Ether
Extraction
Liquid-Liquid
Contact Extract.
Reverse Osmosis
Volatile
Stripping
TABLE I (CONTINUED)
DISTRIBUTION OF WORK OPERATIONS
NEW ORLEANS AREA WATER SUPPLY STUDY
Method Modification Plants Sampled Dates Sampled Sampled By Water Volume Sample Prepared By Analysis By
Developed by Greg Junk
Tetralln Solvent
Cellulose Acetate
Membrane in Series
with Dupont Permasep
Membrane
Bellar Technique for
Volatile Organlcs
Analysis (VOA)
Carroll ton
Jefferson No. 1
Jefferson No. 2
Carrollton
Jefferson No. 1
Jefferson No. 2
Carrollton
Carrollton
7/30-8/1/74
7/30-31/74
7/31-B/1/74
7/31-8/1/74
7/31/74
7/30/74
!LMF-Junk
LMF-Junk
LMF
SERL-LMF
SERL-LMF
LMF
318 liters
365 liters
275 liters
3 ea. X 1 lit.
3 ea. X 1 lit.
3 ea. X 1 lit.
Junk-SERL
Junk-SERL
Junk-SERL
SERL
SERL
SERL
SERL
SERL
SERL
SERL
SERL
SERL
8/7-9/74
9/23/74
GSRI Approx. 400 Gals.
GSRI 50 ml vials
WSRL
WSRL
WSRL
WSRL
Key to abbreviations used In Table I
LMF
SERL
RSKERL
WSRL
GSRI
HNF
Lower Mississippi River Facility (Region VI EPA) SUdell, Lou si ana
Southeast Environmental Research Laboratory (EPA; NERC-CorvalUs) Athens, Georgia
Robert S. Kerr Environmental Research Laboratory (EPA; NERC-Corva Us) Ada, Oklahoma
Water Supply Research Laboratory (EPA; NERC-C1nc1nnat1) Cincinnati, Ohio
Gulf South Research Institute, New Orleans, Louisiana
Houston Facility (Region VI, EPA) Houston, Texas
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ANALYTICAL RESULTS
The trace organic compounds or organic isomers of undetermined
specific structure which have been identified by one or more methods
in samples derived from the finished water at the Carrollton Water
Plant (New Orleans, Louisiana), Jefferson Parish No. 1 Water Plant
t
(Metairie, Louisiana), ahd Jefferson Parish No. 2 Water Plant (Marerro,
Louisiana) are listed in Table 2. Supporting data for these identi-
t
fications exist at the Water Supply Research Laboratory (Cincinnati,
Ohio) or at the'Southeast Environmental Research Laboratory (Athens,
i
Georgia).
*
These compounds are listed in Table 2 in the alphabetical order
of their capitalized letter with the single exception of compound 10.
The reason for its listing out of order will be explained below. Each
compound is numbered in the order of its listing in Table 2. Any
reference to a compound in this discussion will be by its assigned
number unless a reason exists to refer to the name.
No specific chemical nomenclature system is used in this list of
compounds. The name used for a specific compound is the name most
generally used for it or by which it might be most readily recognized.
For example, compound 2 is called acetone although it might also be
named dimethyl ketone or propanone.
The chemical composition of compound 10 is closely related to that
of compound 9. Compound 9 is named preferentially by its common name,
but its name in the IUPAC nomenclature system is given in parenthesis.
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The IUPAC name for compound 10 is also given in parenthesis to show its
close relationship to compound 9 and where the difference in chemical
composition exists. Compound 10 is given a coined name derived from the
common name of compound 9 which shows this difference. This discussion
is felt to be necessary to provide assurance that a typographical error
has not been made in the common name given for compound 10 and to explain
its listing out of ^alphabetical order.
Where the name given for a particular compound is followed by the
term isomer, manual or computerized .interpretation of the mass spectral
data did not permit the analysts to determine precisely which one of
more than one possible molecular isomers bearing that name was present.
In some instances, as for example compounds 3 through 8, it was only
possible to distinguish the compound class such that specific names
could not be provided. Where the specific isomer was determined, as for
example compound 43, this was normally confirmed by a gas chromatographic
retention time match of an available standard of the compound with the
subject peak on the sample chromatogram.
Also given for most compounds in Table 2 is a quantitative value
representing the "highest measured concentration"' in micrograms per
liter (ppb). With the exceptions of compounds 18 and 27 (which were
obtained by the Volatile Organics Analysis technique directly from
water) all concentration values were obtained from quantitative analy-
ses of carbon chloroform extracts and related back to the water medium.
This could be done since the precise volumes of water through the carbon
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units was known. That is to say that an expressed concentration value
of 1.0 wg/1 means 1.0 ug/1 in the water from which the sample was derived.
In order to express precise concentration values in the water,
however, it would be necessary to know the efficiency values for every
stage of the sample collection, preparation, and analytical process.
That is, one would have to be able to measure with standards for each
compound the efficiency of the carbon adsorption from water, losses
t
incurred in carbon drying, efficiency of desorption by solvent from
the carbon, and losses incurred in concentrating the solvent to a low
volume. For this project, determination of these efficiencies could
be considered an impossible or, a,t least, infeasible task. Consequently,
it is emphasized by the analysts that the concentration values reported
must not be interpreted as absolute concentration levels present in the
water, but simply represent the highest concentration values measured by
them. The term "highest" is used because when values determined by two
or more different methods gave values which differed to some extent,
the higher or highest of the values was reported in the tabulation.
All values are available in the analysts' records.
The analysts also recognize that all of the specific organic com-
pounds identified and reported herein were, in the final stage of
analysis, analyzed by some modification of gas chromatography. For
a compound to be analyzed by this method, it must have some degree of
volatility under the conditions of analysis. Consequently non-volatile
organic substances would not have been detected under the analytical
conditions employed.
-20-
-------
TABLE 2
ORGANIC COMPOUND IDENTIFICATIONS
NEW ORLEANS AREA WATER SUPPLY STUDY
1
2
3
.4
5
6
7
8
9
10
Highest Measured Concentration
ug/1 (ppb)
Compound
Acetaldehyde
Acetone
Alkylbenzene-C2 tsomer
Al kyl benzene-C2 i somer
Alky1benzene-C2 i somer
Alkylbenzene-Cg i somer
Al kyl benzene-Cj i somer
Alkylbenzene-C3 i somer
Atrazine *
( 2-chl oro-4-e thyl ami no-
6-isopropylamino-
£-triazine)
Deethylatrazine
( 2-chl oro-4-amino-
6-isopropylamino-
£-triazine)
Carroll ton
Water Plant
D-VOA
D-VOA
0.05
0.33
0.11
0.01
0.04
0.02
5.0
0.51
Jefferson i 1
Water Plant
NE
NE
ND
ND
0.03
ND
0.05
ND
4.7
0.27
Jefferson * 2
Water Pla-nt
NE
NE
,ND
ND
ND
ND
0.02
ND
5.1
0.27
-21-
-------
TABLE 2 (Continued)
ORGAN1C^COMPOUND IDENTIFICATIONS
NEW ORLEANS AREA WATER: SUPPLY STUDY ::
11
12
13
14
15
16
* •
17
18
19
— i-
20
21
Highest Measured Concentration
pg/1 (ppb)
Compound
Benzyl butyl phthalate*
Bromodl chl oromethane
Bromoform *
Butanbne.
Carbon disulfide
Carbon tetrachloride
bis-2-Chloroethyl ether*
Chi ofcbf onto r*"**»*
bi s-2-Chl oroi sopropyl
ether *
n-Decane *
__— — —
Decane-branched isomer
' Carroll ton
Water Plant
0.64
D-VOA
0".57;5?
i
D-VQA'/OA
D-VOA .
D-VOA
: 0.07
133JJ3
0.18 :
0.04
i
0.03
Jefferson # 1
Water Plant
0.81
NE . •
NO
'NE
NE .
NE -
; — _____——
0.16
NE fit
!
0.05
ND
i
ND
Jefferson i 2
Water Plant
0.73
NE
ND ND
NE-NE
i
NE
NE
0.12r>
NENE
4
t
0.03
ND
ND
.22-"
-------
TABLE 2 (Continued)
ORGANIC COMPOUND IDENTIFICATIONS
NEW ORLEANS AREA WATER SUPPLY STUDY
Highest Measured Concentration
ug/1 (ppb)
22
23
24
25
26
27
28
29
30
31
32
Compound
Dibromodichloroethane
i somer
Dibromochlorome thane *
Dibutyl phthalate *
2,6-Di-t-butyl-£-
benzoquinone *
Dichlorobenzene i somer
1,2-Dichloroethane a
Dichloromethane
Dieldrin **
Diethyl phthalate *
Di(2-ethylhexyl) phthalate
Dihexyl phthalate
Carroll ton
Water Plant
0.33
1.1
Of. 10
0.22
0.01
8
D-VOA
0.05
0.03
0.10
0.03
Jefferson 1 1
Water Plant
ND
0.30
0.16
0.19
D-RE
NE
NE
0.07
0.03
0.31
ND
Jeff£rson i 2
Water Plant
0.63
0.60
0.19
0.23
ND
NE
NE
0.05
0.01
0.06
ND
-2s-
-------
TABLE 2 (Continued)
ORGANIC COMPOUND IDENTIFICATIONS
NEW ORLEANS AREA WATER SUPPLY STUDY
Highest Measured Concentration
pg/1 (ppb)
33
34
35
36
37
38
39
40
41 -
42
43
Compound
Dihydrocarvone
i
DiisobutyVphthalate *
Dimethyl phthalate
Dioctyl adipate
Dipropyl phthalate *
n-Dodecane *
Endrin **
Ethanol
o-Ethyl toluene *
£-Ethyl toluene *
1, 2, 3, 4, 5, 7, 7-
Heptachloronorbornene *
Carroll ton
Water Plant
0.14
0.59
0.27
o.io'
0.07
0.01
0.004
D-VOA
ND
0.02
0.06
Jefferson # 1
Water Plant
0.06
ND
0.13
ND
0.13
ND
NYE
NE
0.04
0.03
0.05
Jefferson # 2
Water Plant
0.07
ND
0.18
ND
0.14
ND
NYE
NE
0.02
0.03
0.05
-24-
-------
TABLE 2 (Continued)
ORGANIC COMPOUND IDENTIFICATIONS
NEW ORLEANS AREA WATER SUPPLY STUDY
Highest Measured Concentration
vg/1 (ppb)
44
45
46
47
48
49
50
51
52
53
54
Compound
Heptachloronorbornene *
isomer
Hexachloro-l,3-butadiene *
Hexachloroethane *
Isophorone *
Limonene *
______ —^— — — — " •
Methanol
Methyl benzoate
3-Methylbutanal
2-Methylpropanal
n-Nonane *
. .
n-Pentadecane *
Carroll ton
Water Planl
0.06
0.16
4.4*
1.5
0.03
D-VOA
ND
D-VOA
D-VOA
0.03
0.02
Jefferson 1 1
Water Plant
0.04
0.27
0.19
»
2.2
ND
NE
D-RE
NE
NE
ND
ND
Jefferson f 2
Water Plant
0.04
0.21
0.16
2.9
ND
NE
ND
NE
NE
ND
ND
-25-
-------
TABLE 2 (Continued)
ORGANIC COMPOUND IDENTIFICATIONS
NEW ORLEANS AREA WATER SUPPLY STUDY
Highest Measured Concentration
pg/i (ppb)
55
56
57
58
59
60
61
62
63
64
65
66
Compound
Tetrachloroe thane
i somer
Tetrachl oroethyl ene
n-Tetradecane *
Toluene *
1 ,1,2-Trichloroethane *
1 ,1 ,2-Trichloroethylene
n-Tridecane *
Trimethyl-trioxo-
hexahydrotriazine
i somer
Triphenyl phosphate *
n-Undecane *
Undecane-branched i somer
Undecane-branched i somer
Carroll ton
Water Plant
0.11
D
»
•
0.02
0.08
0.35
D-VOA
0.01
0.07
0.12
0.02
.0.04
0.06
Jefferson # 1
Water Plant
,-ND
0.5
NO
0.10
0.45
NE
ND
ND
ND
ND
ND
ND
Jefferson # 2
Water Plant
ND
--0.41
ND
ND
0.41
NE
ND
ND
ND
ND
ND
ND
-26-
-------
KEY TO SYMBOLS USED IN TABLE 2
Symbols used in column headed Compound
* While all compounds listed in the table were identifisd by one or
more methods, those marked with this symbol gained added confirma-
tion by gas chromatography retention time match with an available
standard of the compound.
** Compounds marked with this symbol gained further confirmation by
gas chromatography retention time match with available standards on
each of three different columns, polar and non-polar.
t
a The quantitative values for these compounds were obtained on
Volatile Organics Analysis by comparison with standards of known
concentration at the Water Supply Research Laboratory. Compound 18
was detected but not quantified in Tetralin extracts of Carroll ton
water at Southeast Environmental Laboratory, but not in Tetralin
extracts of Jefferson No. 1 or Jefferson No. 2. The latter labora-
tory did not detect compound.' 27.
Symbols used in columns headed Highest Concentration Measured.
D-VOA These compounds were detected by Volatile Organics
Analysis - Bellar Technique only. Quantitative values
have not yet been obtained. This method was performed
only on the Carroll ton water at the Water Supply Research
Laboratory.
D-RE These compounds were detected only on XAD resin
extracts in the specific water for which this symbol
is used. Quantitative values were not obtained from
the resin extracts. The compound may have been detected
and quantified by another method in one or both of the
other waters examined.
D In the one instance where this symbol was used the
compound was detected by both the Water Supply Research
Laboratory and Southeast Environmental Research Laboratory
but not quantified by either laboratory.
NE This symbol means not examined. It is used
exclusively for some compounds reported by the Water
Supply Research Laboratory. This laboratory did not
obtain samples of water from Jefferson No. 1 or Jefferson
No. 2.
-27- .
-------
KEY TO TABLE 2 (CONTINUED)
ND This symbol means the compound was not detected in
that specific water by any of the methods employed.
NYE Compound 39 was confirmed in Carroll ton water carbon
chloroform extracts shortly before preparation of this
report. Jefferson No. 1 and Jefferson No. 2 extracts
have not yet been re-examined specifically for compound 39.
-28-
-------
CURRENT PROJECT STATUS
The sampling program as originally assigned to the Lower
Mississippi River Facility was completed on schedule in mid-August
1974. The time required in processing of samples for analysis
prevented getting the samples to the analysts before mid-August to
early September. Thus, the analysts have had only eight to ten
weeks to perform extremely complex and demanding analyses while
t
maintaining precise control over sample integrity and adhering to
scientifically defensible techniques.. ' Nevertheless, the Analytical
Chemistry Branch of the Southeast Environmental Research Laboratory
which has handled the greatest portion of the analytical work-load,
estimates that their committment is 80% complete and that a final
technical assistance report will be submitted to the Region VI
Administrator by early December 1974.
The SERL staff will continue their work toward obtaining some
additional confirmatory evidence and quantitative estimates on the
carbon chloroform extracts and in particular will examine the 2
month equivalent and 1 day equivalent Mini-sample extracts which they
have had no opportunity to examine as yet.
The Water Supply Research Laboratory, which performed some of
the additional analytical work not in the original program, made no
definite committment to the initial project plan, but has provided
valuable assistance in developing confirmatory evidence for some
-29-
-------
2
compounds identified at SERL and, through the VOA technique, detected
the presence of others which would most likely not have been detected
through the carbon adsorption methods alone for various technical
reasons.
It is doubtful that any analytical data for this project will
be forthcoming from the Reverse Osmosis sampling technique. This
i
technique, still in a developmental stage as a sampling method for
trace organics concentration,will probably require further study and
development at the research level before it can be relied on to
produce the type of valid data required of it.
The Liquid-Liquid contact extraction with tetralin solvent was
also a sparse source of data, although a few confirmatory identifi-
cations were derived from it. No reliable quantitative estimates
were obtained and it is not expected to be a source of any additional
data.
No commitment to the analysis of the CAM 10 year equivalent or
CAM 1 year equivalent samples could be obtained. These samples have
been extracted with chloroform and are at present being stored in
sealed vials under refrigeration at the Robert S. Kerr Environmental
Research Laboratories. If analyses are to be required for these
samples, additional analytical assistance will need to be sought.
-30-
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