xvEPA
United States
Environmental Protection
Agency
Occurrence of Contaminants of Emerging
Concern in Wastewater From Nine Publicly
Owned Treatment Works
August 2009
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U.S. Environmental Protection Agency
Office of Water (4303T)
1200 Pennsylvania Avenue, NW
Washington, DC 20460
EPA-821-R-09-009
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
CONTENTS
Page
1. INTRODUCTION 1
2. BACKGROUND 2
3. STAGED STUDY 4
3.1 Stage 1 (2005-2006) 4
3.2 Stage 2 (2007-2008) 6
4. SAMPLE COLLECTION 11
4.1 Sampling Locations and Procedures 11
4.1.1 Sampling Locations 11
4.1.2 Sampling Procedures 15
4.2 Quality Assurance 17
4.3 Quality Control Procedures 17
4.3.1 Equipment Blanks 18
4.3.2 Field Duplicates 18
4.3.3 Laboratory Quality Control Volumes 18
4.3.4 Trip Blanks 18
4.3.5 Quality Control Sample Summary 19
4.4 Sample Collection, Preservation, and Storage 19
5. SUMMARY OF OCCURRENCE DATA 26
5.1 PPCPs 27
5.2 Sterols and Hormones 33
5.3 Alkylphenols, APEs, andBPA 35
5.4 PBDEs 36
5.5 Pesticides 37
6. REFERENCES 40
Appendix A: Contaminants of Emerging Concern (CECs) Analyte list
Appendix B: Analytical Methods Overview
Appendix C: CECs Analytical Results
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Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009
1. INTRODUCTION
The primary objective of EPA's Nine POTW Study (the Study) was to investigate the
occurrence of Contaminants of Emerging Concern (CECs) in untreated and fully treated
wastewater at publicly owned treatment works (POTWs). EPA also initially investigated the
occurrence of conventional, non-conventional, and toxic pollutants, including many of the
pollutants in EPA's 1982 "50-POTW Study" (EPA, 1982). For the first four POTWs in this
Study, EPA selected facilities that treated industrial discharges because POTWs receiving
significant volumes of discharges from pharmaceutical or other manufacturing facilities might be
expected to receive a significant quantity and variety of CECs.
After reviewing analytical data from the first four POTWs, EPA realized that the
available analytical methods were not developed enough to meet the needs of the Study. As a
result, prior to collecting samples for the remaining POTWs, EPA developed three analytical
methods to detect the occurrence of CECs in POTW wastewaters. These three methods are: EPA
1694 for pharmaceuticals and personal care products, EPA 1698 for steroids and hormones, and
EPA 1699 for pesticides.
During the development of these three methods, EPA reevaluated the design of the Study
and decided to focus the remaining resources on documenting the occurrence of CECs in
wastewater, and ceased collecting data for the other non-CEC parameters previously analyzed.
EPA also revised the POTW selection criteria to focus on facilities with specific sources of
residential flow expected to contain higher concentrations of CECs.
This report presents the findings from the Nine POTW Study for informational purposes.
Caution should be used in interpreting the results. For several reasons, the study does not lend
itself to national conclusions. The Study had two very distinct stages, each with different
analytical methods, sampling techniques and POTW selection criteria. The nine POTWs in this
study are not statistically representative of all POTWs in the country, nor would they be expected
to statistically represent particular subpopulations of POTWs. The analytical methods were under
development during much of this study, which resulted in certain data quality issues during
laboratory analysis. Additionally, sample collection efforts were not designed to calculate
removal of CECs from POTWs. Although some reduction in concentration levels of many CECs
was observed in the effluent, the data are not sufficient to draw any conclusions about treatment
effectiveness.
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Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009
2. BACKGROUND
In 2005, EPA began studying environmental contamination by pharmaceuticals,
detergents, natural and synthetic hormones, and other chemicals. These contaminants are
commonly referred to collectively as contaminants of emerging concern.
Many CECs are believed to enter municipal wastewater through bathing, cleaning,
laundry, and the disposal of unused pharmaceuticals and human waste. Municipal wastewater is
treated by POTWs, which typically employ biological treatment and disinfection processes and,
in some instances, a form of advanced treatment. These processes are designed to reduce the load
of organic pollutants and pathogens in the treated wastewater discharged to the environment;
however, POTW treatment systems are not designed to specifically remove CECs. Thus, any
removals of CECs which may occur are incidental to these treatment processes.
To assess the occurrence of CECs in POTW influent and effluent, and to test and develop
new analytical methods with which to measure these emerging contaminants, between
September 2005 and July 2008, EPA collected samples for one day at each of nine POTWs. This
study is referred to in this report as the "Nine POTW Study", or "the Study." The CECs in this
study include the following classes of chemicals:
• Pharmaceuticals and Personal Care Products (PPCPs) - A variety of
pharmaceuticals and personal care products are used by individuals for personal
health or cosmetic reasons. Pharmaceuticals include over-the-counter medication
(e.g., aspirin, acetaminophen, and pseudoephedrine) as well as medications
prescribed by a physician (e.g., Lipitor®, albuterol, amoxicillin). Most ingested
pharmaceuticals are only partially metabolized, so a portion is excreted,
unmetabolized, in urine or feces. Metabolized and unmetabolized pharmaceuticals
are discharged in domestic sewage.
Personal care products include chemicals such as soaps, detergents, shampoo,
cosmetics, sun-screen products, fragrances, insect repellants, and antibacterial
compounds. An example of a personal care product is triclosan, a potent wide-
spectrum antibacterial and antifungal agent. Personal care products enter domestic
wastewater from bathing, laundry, and household cleaning.
• Steroids and Hormones (S/H) - Steroids and hormones include both naturally
occurring compounds and synthetic analogues that are structurally related to one
another. Hundreds of distinct steroids are found in plants and animals. Sterols,
which are steroid-based alcohols, are the most abundant of the steroids. The most
common sterol in vertebrates is cholesterol, which is found in cell membranes and
also serves as a central intermediate in the biosynthesis of many biologically
active steroids, including bile acids, corticosteroids, and sex hormones.
Hormones are intercellular chemical messengers. They are synthesized and
secreted from a cell and act in low concentrations by binding to a stereospecific
target-cell receptor to activate a response. Some hormones are classified by
chemical structure as steroids. Steroid hormones include the sex hormones, which
are, among others, natural estrogens, synthetic estrogens such as EE2 (17 alpha-
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
ethinyl estradiol), progesterone, and testosterone. Other hormones are
polypeptides or amino acid-derived compounds. Plant steroids can mimic animal
sex hormones.
Alkylphenols andAlkylphenol Ethoxylates (APEs) - Alkylphenol ethoxylates
(APEs) are synthetic surfactants used in some detergents and cleaning products.
The most common APEs are nonylphenol ethoxylates (NPEs), derived from
nonylphenol (NP), which is an alklyphenol. Octylphenol ethoxylates (OPEs),
derived from octylphenol (OP), are also common.
BisphenolA (BPA), also known as 4,4'-isopropylidenediphenol, is an organic
compound used primarily to make polycarbonate plastic and epoxy resins.
Polycarbonate is used in eyeglass lenses, medical equipment, water bottles, CDs,
DVDs, and many other consumer products. Among the many uses for epoxy
resins are can coatings, industrial floorings, automotive primers, and printed
circuit boards.
Polybrominated Diphenyl Ethers (PBDEs) - Polybrominated diphenyl ethers
(PBDEs) are structurally similar to Poly chlorinated biphenyl. PBDEs are major
components of commercial formulations often used as flame retardants in
furniture foam (e.g., pentaBDE), plastics for TV cabinets, consumer electronics,
wire insulation, back coatings for draperies and upholstery (e.g., decaBDE), and
plastics for personal computers and small appliances (e.g., octaBDE). These
chemicals slow ignition and rate of fire growth.
Pesticides - Pesticides are any of a large number of unrelated chemicals that are
used to prevent, destroy, or repel a living organism that occurs where it is not
wanted (i.e., a pest). Pesticides are often referred to according to the type of pest
they control (e.g., insecticides, rodenticides, fungicides). Pesticides include
organochlorine, organophosphorus, triazine, and pyrethroid pesticides.
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Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009
3. STAGED STUDY
During this Study, EPA collected samples from nine POTWs located in eight states.
These POTWs are referred to in this report as Plants A through I. All of the sampled POTWs
used variations of the activated sludge process, including some degree of nitrification. All
POTWs disinfected some or all of their treated effluent prior to discharge or land application.
The Study was carried out in two stages. In the first stage (Plants A through D), EPA
examined the occurrence of contaminants of emerging concern (CECs), including endocrine
disrupting compounds and other potentially harmful compounds. After sampling these first four
POTWs in 2005 and 2006, EPA concluded that it needed more sensitive and selective analytical
methods. Method development took place from 2006-2008. See Appendix B for an overview of
EPA's CECs analytical methods. With development of better analytical methods well underway,
and with changes in both POTW site selection criteria and sampling approach (as described in
Section 3.2 of this report), EPA began the second stage of the Study in September 2007 (Plants E
through I).
3.1 Stage 1 (2005-2006)
The first stage of the Study was designed to determine the occurrence of pollutants at
POTWs based on one day of sampling. In addition to obtaining this relatively limited
information on pollutant occurrence, EPA anticipated that the Study results would identify
candidate POTWs for future performance sampling should such a decision be made to do so in
the future. Samples taken during this first stage were analyzed for priority pollutants in order to
build on the information collected during EPA's 1982 "50-POTW Study1." During Stage 1,
EPA also evaluated the available analytical methods for detecting CECs in wastewater.
During Stage 1, EPA sampled POTWs with a high proportion of flow from industries
believed to be discharging high concentrations of PPCPs. EPA used the 2004 Clean Watershed
Needs Survey (CWNS), the 2004 Permit Compliance System (PCS) database, and the 2002
Toxic Release Inventory (TRI) to gather information on influent contributions, treatment unit
operations, and performance. EPA verified information about selected POTWs gathered using
these data sources through discussions with the facilities themselves. Using this information,
EPA identified facilities with average influent loadings and typical discharge patterns. The four
POTWs sampled during Stage 1 were selected because they met some or all of the following
criteria:
• Influent flow greater than 1 million gallons per day (MGD).
• High industrial wastewater flow contribution from a variety of different industries
as well as targeted industries that were expected to contribute CECs. Targeted
industries include: manufacture of organic chemicals, plastics, and synthetic
fibers; pharmaceutical manufacturing and testing; meat and poultry processing;
dairy products processing; hospitals and health care facilities; and landfills.
• Adequate POTW performance (effluent BODs concentration less than 20 mg/L).
1 The focus of this report is on CECs and information collected on the priority pollutants is not presented.
4
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Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009
• Use of a variety of treatment technologies including, technologies for nutrient
(total nitrogen and total phosphorus) removal, various disinfection technologies
(ultraviolet (UV) light, ozonation and chorine disinfection).
During Stage 1 of the Study, EPA monitored for a lengthy list of pollutants including:
• Pollutants that were part of the 1982 50-POTW Study, including:
— Volatile and semivolatile organic compounds,
— Metals (total and dissolved) and,
— Classical pollutants.
• Additional organic compounds:
— Other volatile and semivolatile organic compounds,
— Polybrominated diphenyl ethers (PBDEs),
— Polychlorinated dioxins and furans, and
— Chlorinated biphenyl congeners (PCBs);
• Microbiological pollutants; and
• Analytes for which methods were under development, including:
— Pharmaceuticals and personal care products,
— Steroids and hormones,
— Alkylphenol ethoxylates (APEs), and
— Pesticides and herbicides.
Stage 1 Facilities
Each of the four POTWs selected for Stage 1 is described in more detail below. Table 3-1
found at the end of this section summarizes the unit process descriptions and operating
characteristics of all nine POTWs participating in the Study.
Plant A treats a relatively large proportion of industrial wastewater (18 percent of total
flow is from industrial sources) and receives 3.5 million pounds per year of TRI-listed chemicals,
the majority of this industrial flow coming from a pharmaceutical manufacturer. Sources of
domestic wastewater treated at the plant include two colleges with on-campus housing (a
university with 28,600 students and a college with 1,300 students). The total flow to Plant A is
26 MOD.
Plant A is a conventional activated sludge facility with powdered activated carbon (PAC)
addition. The wastewater treatment process consists of mechanical bar screening at the
comminutors, grit removal, ferric chloride addition for phosphorus precipitation, primary
clarification, PAC addition to remove refractory organic compounds, aeration, secondary
clarification, sand filtration, chlorine disinfection using chlorine gas, and dechlorination using
bisulfite. Final treated effluent is discharged to a river.
Plant B receives flow from a variety of sources that potentially contribute CECs and
other pollutants. The facility receives approximately 10 to 15 percent of influent flow from
industrial sources and commercial facilities, as well as wastewater from three hospitals, domestic
septage, and landfill leachate. The total flow to Plant B is 27 MOD.
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Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009
Plant B is a conventional activated sludge facility. Wastewater treatment includes
screening, grit removal, primary clarification, aeration, and secondary clarification. After
secondary clarification, the facility conducts chlorine disinfection using sodium hypochlorite and
dechlorination using sodium bisulfite, and the final treated effluent is discharged to a river. This
plant does not use any biological nutrient removal or other more advanced processes.
Plant C receives significant industrial flow from sources that potentially contribute both
CECs and other pollutants. The facility receives approximately five to seven percent of influent
flow from industrial sources and commercial facilities and treats domestic wastewater, landfill
leachate, and septage from local haulers. The total flow to Plant C is 17 MOD.
Plant C is also a conventional activated sludge facility. Wastewater treatment consists of
screening, grit removal, ferric chloride addition to remove phosphorus (as necessary), primary
clarification, aeration, secondary clarification, and UV disinfection. The final effluent is
discharged into a lake.
Plant D receives wastewater from multiple targeted industries and uses a wide variety of
treatment processes. This POTW receives approximately 17 percent of flow from industrial
sources and commercial facilities, as well as wastewater from two hospitals and several
universities, septage, and landfill leachate. The total flow to Plant D is 34 MOD.
Plant D is an advanced secondary and tertiary treatment facility, using several treatment
unit operations in two treatment trains. Wastewater enters the facility and undergoes screening,
grit removal, and primary clarification. After primary treatment, the wastewater is split into two
treatment trains. The wastewater in Train 1 (56 percent of flow) first undergoes aluminum sulfate
addition for phosphorus removal, then passes through pure oxygen aeration basins, secondary
clarification, nitrification aeration basins, tertiary clarification, and mixed media denitrification
filters before mixing with the secondary effluent from Train 2 prior to disinfection. Train 2 (44
percent of flow) treatment consists of biological phosphorus removal aeration basins with
aluminum sulfate addition to assist in phosphorus removal, secondary clarifiers, and sand filters.
The Train 1 and Train 2 effluents are mixed prior to ozone disinfection. The final effluent is
discharged to a creek.
3.2 Stage 2 (2007-2008)
During Stage 1 of the Study, EPA determined that the analytical methods needed further
development. This development took place during 2006-2008, and resulted in three new
analytical methods, EPA Methods 1694, 1698, and 1699.
With method development well underway, Stage 2 sampling resumed during 2007-2008.
By this time, there was more interest in directing available resources to document occurrence of
CECs in POTW influent and effluent with the use of single-day (screening) sampling episodes.
Thus, in Stage 2 EPA did not analyze for any pollutants beyond what had been identified
as CECs in Stage 1.
In Stage 2 EPA also changed the selection criteria for POTWs. Because CEC discharges
can result from excretion of ingested CECs, EPA changed the selection criteria from facilities
with higher industrial flow to those with higher residential flow.
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Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009
To identify the populations of interest for Stage 2, EPA reviewed literature on the use of
medications that may be found in wastewater. The Slone Epidemiology Center at Boston
University has conducted an annual survey of medication use in the United States since 1998.
The surveys indicated that in a given week, over 80 percent of adults in the United States take at
least one medication (prescription or nonprescription drug, vitamin/mineral, or herbal/natural
supplement). Medication use varies considerably by age. People over 65 are the largest
consumers of medication. Of this age group, 57 to 59 percent take at least five medications in a
week, and 17 to 19 percent take at least 10 (Slone, 2006). Thus, higher influent concentrations of
Pharmaceuticals may be found at POTWs that serve a higher than average proportion of
population age 65 or older.
The Slone survey conducted in 1998-1999 (Kaufman, 2002) identified two population
groups that frequently use hormone medications. In that study, 21 percent of women aged 45 to
65 and 17 percent of women over 65 used conjugated estrogens, presumably as part of hormone
replacement therapy (HRT). Since 1998, the use of HRT has declined dramatically, but as of
2004, 12 percent of women over 50 continued to use this therapy. Higher POTW influent
concentrations of estrogens may be found at POTWs serving a greater than average population of
women over 50, though this effect may have decreased with the decline of HRT use.
The second population group that frequently uses hormone medications is women aged
18 to 44. In the 1998-99 Slone survey, 14 percent of this group used EE2 (17 alpha-ethinyl
estradiol), the synthetic hormone that is the active ingredient in birth control pills (Kauffman,
2002). Data published by the National Center for Health Statistics show that 32 percent of all
women between the ages of 20 and 24 used the birth control pill for contraception in 2002
(Chandra, 2005). According to the 2000 Census, 21 percent of college students are women in this
age group compared to 6.5 to 6.8 percent of the general population (Census, 2007). As a result,
the use of birth control pills among the college population may be greater than among the general
population.
For Stage 2 site selection, EPA identified areas with high concentrations of college-aged
populations or populations over 65. To identify such areas, EPA used information from the U.S.
Census Bureau (population by age and total populations by county) and the U.S. News and
World Report (college settings and student populations). EPA selected five facilities for Stage 2
sampling using the following criteria, in no particular order:
• Use of selected advanced treatment technology;
• Use of separate sewers, which segregates stormwater away from sewers directing
wastewater to the POTW; and
• Service area includes a large college (at least 10,000 students) or more than 15
percent of population 65 or over.
Stage 2 Facilities
The five facilities selected for sampling during Stage 2 are described below. Table 3-1,
found at the end of this section, summarizes the unit process descriptions and operating
characteristics of the nine POTWs participating in the Study.
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Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009
Plant E receives wastewater from a large university and surrounding towns. The POTW
diverted town flow to another nearby POTW during the sampling episode, so samples collected
represent only university-derived wastewater. Flow from the town was diverted far enough in
advance of EPA's sampling, to allow for the system to treat and discharge all non-university
flow prior to the sampling episode. The plant receives approximately 2 MOD from the
university.
Plant E is a multi-train secondary treatment facility that operates three secondary
treatment trains and disinfects using chlorine gas. The influent passes through grit removal, rag
removal, primary aeration, and primary clarification. From here, treatment is split into three
trains. The wastewater in Train 1 (25 percent of flow) is passed through trickling filters prior to
rejoining with Train 2 wastewater (25 percent of flow), which passes through an anoxic tank
before joining Train 1 wastewater. The combined secondary effluent from Trains 1 and 2
undergo secondary aeration and clarification with poly-aluminum chloride addition for
phosphorus removal. Train 3 (50 percent of flow) is a two-step conventional activated sludge
treatment process. The first step is a two-ring activated sludge basin; the inner zone provides
aeration and the outer zone provides anoxic conditions. The second step, also a two-ring
activated sludge basin, provides reaeration in the inner zone and clarification in the outer zone.
Combined secondary effluent from Trains 1 and 2 and secondary effluent from Train 3 are all
combined prior to disinfection using chlorine gas. The final effluent is used for spray irrigation
on agricultural fields.
Plant F is located in a county with an above-average percentage of population over age
65. Twenty-two percent of the population in the county is over age 65, compared to the national
average of 12.4 percent. Total flow to Plant F is 6.7 MGD.
Plant F is one of a few POTWs in the United States to use a five-stage Bardenpho™
treatment system with only bar screening and grit removal prior to the process. The Bardenpho™
system consists of five zones: anaerobic, anoxic, aerobic, anoxic, and reaeration. This process is
designed to provide efficient, economical removal of BOD5, TSS, nitrogen, and phosphorus. The
Bardenpho™ system is followed by clarification, sand filters, and UV disinfection. Final effluent
is either discharged to a river or reused for irrigation and cooling in the plant's service area.
Plant G treats flow mainly from a university and the off-campus student population for a
total of 1.5 MGD. Plant G's flow spikes significantly during and after rain events; therefore,
EPA planned and conducted the sampling episode to take place during a dry time of the year to
prevent loading dilution.
Plant G has an oxidation ditch system (an extended aeration activated sludge process)
with final discharge to a river. Treatment consists of bar screening, grit removal, fine screening,
oxidation ditch treatment, secondary clarification, chlorine disinfection (sodium hypochlorite),
and dechlorination (sodium bisulfite).
Plant His located in a community with an above-average percentage of population over
age 65. According to the 2000 U.S. Census data, 73 percent of the population served by Plant H
is over age 65. The surrounding area is home to many active adult communities and retirement
homes. Total flow to the facility is approximately 2 MGD.
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
Plant H also uses an oxidation ditch system. Treatment consists of screening, grit removal,
oxidation ditch treatment, secondary clarification, tertiary media filters, and chlorine
disinfection using sodium hypochlorite. The facility maintains chlorine residual in the treated
effluent because it is discharged to groundwater percolation beds. The facility is permitted to
discharge to a river, but rarely does so.
Plant I is also located in a community with an above-average percentage of population
over age 65. According to the 2000 U.S. Census data, 25 percent of the population in the county
where the POTW is located is over age 65, compared to the national average of 12.4 percent. The
site contact noted that approximately 50 to 75 percent of the influent flow to Plant I is possibly
from persons over 65. The surrounding area is home to many active adult communities and
retirement homes. Total flow to the facility is approximately 1 MGD.
Plant I operates three sequencing batch reactors (SBRs) to achieve secondary treatment.
Treatment consists of screening, grit removal, SBR activated sludge treatment, sand filtration,
and chlorine disinfection with elemental chlorine. The final effluent is disposed of on on-site
spray irrigation fields. The facility is also permitted to discharge to a swamp, but rarely does so.
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table 3-1. Descriptions of Participating POTWs
Plant
A
B
C
D
E
F
G
H
I
Primary
Treatment
Clarification
with ferric
chloride
addition
Clarification
Clarification
with ferric
chloride (as
necessary)
Clarification
Aeration and
clarification
None
None
None
None
Secondary Treatment
Conventional activated sludge and
PAC addition
Conventional activated sludge
Conventional activated sludge
Train 1 : Chemical phosphorus
removal and pure oxygen
activated sludge (with separate
stage nitrification and
denitrification) (56% flow)
Train 2: Activated sludge with an
anoxic zone for biological
phosphorus removals and
chemical phosphorus removal
(44% flow)
Train 1: Trickling filters (25%
flow)
Train 2: Anoxic tank (25% flow)
Train 3 : 2-step activated sludge
(50% flow)
5-stage Bardenpho process
(anaerobic, anoxic, aerobic,
anoxic, aerobic)
Oxidation ditch
Oxidation ditch
SBRs
Sludge
Retention
Time
(SRT)
20 days
12 days
3.5 days
2.1 days
0.1 days
N/A
Step 1:
19.4 days
Step 2:
5.4 days
16 days
26.5 days
12.4 days
14.2 days
Nitrification
Yes
Yes
Yes
Yes
No
Yes
Yes
Yes
Yes
Yes
Yes
Sand
or
Media
Filters
Yes
No
No
Yes
Yes
No
Yes
No
Yes
Yes
Type of
Disinfection
Chlorine
Chlorine
UV
Ozone
Chlorine
UV
Chlorine
Chlorine
Chlorine
10
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
4.
SAMPLE COLLECTION
4.1 Sampling Locations and Procedures
During Stage 1, EPA collected samples of influent, final effluent, and at intermediate
points in the treatment process. The wastewater was sampled periodically over a 24-hour period
and the samples were composited for analysis. EPA also collected grab samples of either primary
or combined sludge.
During most of Stage 2, EPA collected samples of influent and final effluent only. EPA's
objective during Stage 2 was to identify POTWs with high influent concentrations of CECs, not
to estimate daily influent load. POTW influent flows follow a characteristic diurnal pattern, with
lowest flows in the very early morning hours and peak flows in mid-morning. Influent BOD5
concentration follows the flow variation (Metcalf and Eddy, 1978), and EPA assumed that CECs
concentrations, like the BOD5 concentrations, peak with the flow. EPA decided it could identify
POTWs with high influent concentrations of CECs by collecting one-time grab samples during
periods of peak flow. For this reason, during the last three sampling episodes, samples were
collected as grab samples or manual grab composite samples. EPA did not collect any sludge
samples during Stage 2.
During Stage 2 there was a seasonal component to scheduling sampling events. The
targeted populations were anticipated to have predictable seasonal migratory patterns. EPA
sampled POTWs with large college populations during the school year, in order to get flow
associated with their student population. Similarly, EPA sampled POTWs with a high percentage
of populations over 65 during times this population was anticipated to be at their residences.
EPA avoided sampling these POTWs during summer months and major holidays, when the
populations may travel to escape warm summer climates or visit family.
EPA reviewed historical monthly flow patterns for the Stage 2 facilities in order to
determine when the daily flow to the specific POTWs declined, indicating that the target
populations may have left the area. All of the sampling in Stage 2 took place outside periods of
reduced flow. See Table 4-1 for the sampling dates.
Table 4-1. POTW Sampling Episode Dates
Sampling
Date
Plant
A
9/23/2005
B
6/21/2006
C
8/9/2006
D
9/13/2006
E
11/12/2007
F
11/15/2007
G
4/8/2008
H
4/10/2008
Ia
7/29/2008
a While this sampling event took place during summer months, the historical information indicated flow remained
fairly consistent during the summer with peaks in October and drops off in November and December, two major
holiday months.
4.1.1 Sampling Locations
At four plants, EPA collected influent samples after bar screening and grit removal, but
before primary treatment and recycle stream mixing when feasible (Plants A, B, D, and H). At
the remaining plants, EPA collected influent samples prior to the grit chamber (Plants E, F, and
G) or influent channel bar screen (Plants C and I).
n
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
At Plants A, F, G, H, and I, EPA collected samples only at the influent and final effluent
locations.
At Plants B and C, EPA collected samples of intermediate secondary effluent in addition
to samples of influent and final effluent. Secondary effluent samples were collected directly after
secondary clarification but before disinfection.
Because Plant D uses a variety of treatment units, EPA collected samples at several
intermediate points.
Due to the long SRT of the two-step activated sludge treatment system at Plant E, EPA
chose to sample the influent to and effluent from the activated sludge treatment system at this
facility.
Figures 4-1 through 4-9 present process schematics for each POTW. Sampling points are
noted on each of the plant schematics.
Bar Screens
Grit
and Chamber
Communitors
Grit
Ferric
Chloride
Ferric
Chloride PAC
Chlorine Bisulfite
Contact
| Chloride PAC ^ Sand Contact I
Primary Aeration Secondary Chloride Filters Cl2 , , f
Clarifier Y Y Basins Clarifier I f , Gas w , , Dechlorinatii
Primary
Sludge
WAS
T
Filter
Backwash
Discharge
to River
(O) Sampling
point location
Figure 4-1. Process Schematic of Plant A
Influent
Channel Bar
Screen
M.
Grit
Chamber
Screenings
Grit
Primary
Clarifier
Aeration Secondary Sodium
Basins Clarifier Hypochlorite
Chlorine
Contact
Tank
Sodium
Bisulfite
Primary
Sludge
WAS
Discharge to River
Figure 4-2. Process Schematic of Plant B
12
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Influent
Channel Bar
Screen
"f
Screenings
Ferric Chloride
(as necessary) Primary
Grit | Clarifier
Grit
Primary
Sludge
Aeration
Basins
Secondary
Clarifier
UV
Disinfection
WAS
Discharge to Lake
JO) Sampling >
point locationj
Figure 4-3. Process Schematic of Plant C
Screenings Grit
Biological
Phosphorus
Removal Aeration
Basins
Aluminum
Sulfate Secondary
Primary
Clarifier
Primary
Sludge
Pure Oxygen Secondary
Nitrification
Ozone from On-Site
Generation
Tertiary
_______ ,
Aeration Basins Clarifier Aeration Tanks C|arifier
Aluminum
Sulfate
RAS
WAS
WAS
Mixed Media
Denitrifi cation
Filters
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Influent
Channel Bar /^ 1
Screen Gri( I V Anc
//// Chamber / A Zo
A If Anc
T 1 ^B_ Zo
Screenings Grit
Anaerobic
Zones
F
Influent
Channel Bar |
Sc.reen Grit Scr
//// x~x Chamber ^
/7f T
Screenings Grit Scr«
F
Influent
Ch^rT'Bar Oxida
Screen Grit Ditc
//// Chamber ^ 1
//// w| ^—6?) J
//// '^®'L
1 1
Screenings Grit
' f Aerobic Zone \ •>* Y'T'-rmndir-
XIC( ") lAnoxic VV C|arifior'
V East J J ;-( )_
A Aerobic Zone "\ J\ ^ J
xicl J JAnoxic /
ne V West y Zone /
5-Stage Bardenpho™ Process
RAS
WAS
Sand uv ^ Discharge
Filters Disinfection i — ^ tn RJUPI-
^ ;:;:;:;:;:;:;:;:; ^1 ^—Lgi-
1 1 — ^ Reuse
Filter
Backwash
((g Sampling ^
1 point locationj
igure 4-6. Process Schematic of Plant F
Chlorine
Contact Sodium
:ine Oxidation Secondary Sodium Tank Ri<,,,|fito
eening Ditch Ciarifier Hypochlorite
^ > i / ") r
m U V ii
f V T
^ RAS ^
senings WAS
igure 4-7. Process Schematic of Plant (
c
<
[ion Secondary Tertiary sodium
h Harifi°r Medla Fllters Hypochlorite
\ C\ '• % '
W I hi • ^ hi
J >1) >.....g
1
RAS | |
WAS Filter
Backwash
~|
1 — (^~^ Discharge to River
Jj_
r&\ Sampling ^
^ po nt locationj
-~~i
Chlorine
Contact
Tank Discharge to
1 — | 1 River (optional)
II —®
IIIH
Peicolalion
^*" Beds
[jQQQc)
{fa Sampling ^
^ point locationj
Figure 4-8. Process Schematic of Plant H
14
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Influent
Channel Bar
Screen Grit
//// Chamber
0 '//// "^ '
Grit
or ^
-2!->
Set
SBR1
SBR3
fencing Batch
Reactors
i
\Nl
k Elemental
* band niters chlorine
^J "p
\S Filter
Backwash
Chlorine
Contact
Tank .qpray
1 1 Irrigation
fk> Sampling ^
^ point locationj
Figure 4-9. Process Schematic of Plant I
4.1.2 Sampling Procedures
EPA collected samples over a 24-hour period at Plants A through F, as one-time grab
samples at Plants G and H, and as multiple-hour manual grab composites at Plant I.
24-Hour Sampling Episodes
At Plants A, B, C, D, E, and F, EPA collected samples over a 24-hour sampling period.
Samples were collected using either an automatic compositor or a grab sampling bottle dipper. A
composite sample is a mixture of discrete samples collected over a specific period of time (e.g.,
24 hours) intended to represent the characteristics of the flow at the sampling point over the
entire sampling period.
To collect a representative sample of the varying influent flow to POTWs, EPA used one
of the following techniques:
• Time-weighted sampling: aliquots collected at 15-minute intervals;
• Flow-weighted sampling: automatic compositors connected to flow meters,
aliquots collected after predetermined amount of flow passed; or
• Manual time-/flow-weighted sampling: typical flow pattern determined, aliquots
collected at intervals ranging from 10 to 20 minutes based on high-, medium-, and
low-flow periods.
Time-weighted sampling. At Plant A, automatic compositors were programmed to collect
sample aliquots every 15 minutes throughout the entire 24-hour sampling period. The time-based
schedule was intended to reflect the changing wastewater stream as flow changed.
Flow-weighted sampling. Because the time-based schedule used at Plant A did not seem
to reflect periods of high flow, EPA used a flow-weighted sampling strategy at Plant B.
Automatic compositors collected sample aliquots when a preset volume of sample passed
through the influent channel, as signaled by a flow meter. However, the flow meters used at
POTW B were sometimes unreliable, and the signal was not always constant.
15
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
Manual time-/flow-weighted sampling. For sampling at Plants C, D, E, and F, EPA used
historical daily flow data and trends to create a manual time-/flow-weighted sampling scheme. A
larger volume of sample was collected during periods of higher flow. This sampling technique
required EPA to adjust the sampling interval on the automatic compositors four times within the
24-hour sampling period. Sampling aliquot intervals were calculated prior to the sampling
episode. When possible, time-/flow-weighted sampling intervals were adjusted on site, as
updated flow data were provided by POTW personnel.
The automatic compositors dispensed samples into multiple 10-liter jars over the 24-hour
sampling period. The contents of the multiple jars were poured into a large 15-gallon plastic
container lined with Teflon® bag(s). The sample was mixed with a Teflon® stirring rod and
pumped into the sample containers using a peristaltic pump.
Because automatic sampling equipment could interfere with analyte recoveries for some
of the non-CEC methods, a subset of these samples were collected directly into sample
containers. Grab samples were collected four times (at 6-hour intervals) during the 24-hour
sample collection period using a bottle dipper. The grab samples were physically composited by
the analytical laboratory prior to analysis.
One-Time Grab Sampling Episodes
EPA changed from composite sampling to grab sample collection at Plants G and H.
Grab sampling was based on the premise that CECs concentrations, like the BODs
concentrations, peak with the flow. EPA decided it could identify POTWs with high influent
concentrations of CECs by collecting one-time grab samples during periods of peak flow.
EPA identified the peak POTW flow periods (the one to two hours during which POTW
flow was at its highest) to get the highest percentage of human derived waste in the influent. The
one-time grab samples were collected directly into the sample containers using a bottle dipper
when the plant influent flow was at its peak.
Manual Grab Composite Episodes
At Plant I, EPA collected time-weighted, manual grab composite samples at the influent
and effluent. Because Plant I operates SBRs and effluent flow is not constant, EPA chose not to
collect one-time grab samples similar to POTWs G and H. Influent and effluent samples were
collected as time-weighted, manual composite aliquots over one SBR fill period and decant
period, respectively. The sampled SBR fill period occurred during the peak POTW flow period.
At the influent, the manual composite samples were collected into a sample bottle from a
sample tap then poured into a 10-L composite sample jar. At the end of the compositing period,
the mixed sample was poured from the 10-L jar directly into sample bottles. At the effluent, EPA
used a bottle dipper to collect sample aliquots into a sample bottle. These bottle aliquots were
poured into two 10-L composite sample jars. At the end of the compositing period, mixed sample
was poured directly from the 10-L jars into sample bottles. EPA's sample collection procedures
are summarized in Table 4-2.
16
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table 4-2. Sample Collection Procedures
Plant
A
B
C
D
E
F
G
H
I
Influent
Time-weighted 24-hour
composite and 4-interval
grab
Flow-weighted 24-hour
composite and 4-interval
grab
Time-/flow-weighted 24-
hour composite and 4-
interval grab
Time-/flow-weighted 24-
hour composite and 4-
interval grab
Time-/flow-weighted 24-
hour composite and 4-
interval grab
Time-/flow-weighted 24-
hour composite and 4-
interval grab
One-time grab
One-time grab
Time-weighted, 3 -hour grab
composites
Intermediate Sampling
Point(s)
None
Flow-weighted 24-hour
composite and 4-interval grab
Time-/flow-weighted 24-hour
composite and 4-interval grab
5 time-/flow-weighted 24-hour
composites and 4-interval grabs
2 time-/flow-weighted 24-hour
composites and 4-interval grabs
None
None
None
None
Final Effluent
Time-weighted 24-hour
composite and 4-interval
grab
Flow-weighted 24-hour
composite and 4-interval
grab
Time-/flow-weighted 24-
hour composite and 4-
interval grab
Time-/flow-weighted 24-
hour composite and 4-
interval grab
Time-/flow-weighted 24-
hour composite and 4-
interval grab
Time-/flow-weighted 24-
hour composite and 4-
interval grab
One-time grab
One-time grab
Time-weighted, 40-minute
grab composites
Sludge
One-time
grab
One-time
grab
One-time
grab
One-time
grab
None
None
None
None
None
4.2 Quality Assurance
EPA wrote a Quality Assurance Project Plan (QAPP) to document the project-specific
policies, organization, objectives, functional activities, and specific quality assurance/quality
control (QA/QC) procedures for the Nine POTW Study. EPA developed the initial QAPP at the
start of Stage 1 (QAPP Versions 1 and 2), and revised it prior to the start of Stage 2 sampling
(QAPP Version 3). The QAPP complies with EPA Requirements for QA Project Plans (QA/R-5)
(EPA, 2001) and presents the criteria used to review the sampling data collected in the Study.
4.3 Quality Control Procedures
Quality assurance/quality control (QA/QC) procedures applicable to the nine sampling
episodes are outlined in the Quality Assurance Project Plan for the POTW Study (ERG, 2006;
ERG, 2008). QC practices include collecting and analyzing the following:
• Equipment blanks;
• Field duplicates;
• Laboratory QC volumes; and/or
• Trip blanks.
17
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
4.3.1 Equipment Blanks
To assess contamination from sampling equipment in the field, EPA collected equipment
blanks for the automatic compositors and bottle dippers used at each sampling episode.
For the automatic compositor, EPA collected an equipment blank by pumping Ultra Pure
Blank Water DI+™ through the entire automatic compositor system directly into sample
containers; the automatic compositor system included tubing, a 15-gallon plastic tank lined with
Teflon® bag(s), a Teflon® stir rod, and, in some cases, a strainer. The tubing was purged prior to
the collection of equipment blanks. EPA also used Ultra Pure Blank Water DI+™ to collect
bottle dipper equipment blanks by placing the sample container into the bottle dipper apparatus
as is done during field sampling and pouring the Ultra Pure Blank Water DI+™ directly into the
sample containers.
EPA analyzed equipment blanks for select analytes during each sampling episode.
Equipment blanks collected at Plants A, B, C, and D were analyzed for semivolatile organic
compounds and metals. Equipment blanks at Plants E, F, G, H, and I were analyzed for the CECs
target analytes. EPA compared the concentrations of CECs detected in the equipment blanks to
the concentrations of CECs detected in the associated samples. See Appendix C for details of
how EPA adjusted the sample results based on the significance of blank contamination.
4.3.2 Field Duplicates
EPA collected duplicate samples to assess the variability in sample collection, handling,
preparation, and analysis. Duplicate samples were collected from the same location, at the same
time, and stored and analyzed independently.
EPA collected field duplicates using separate automatic compositors or duplicate grab
samples collected at the same time as other grab samples. Field duplicates were not collected at
Plants A, D, G, H, and I. Field duplicates collected at Plants B, C, E, and F were analyzed for all
CECs target analytes. Results of analysis of duplicate samples have been averaged for
presentation in Appendix C of this report.
4.3.3 Laboratory Quality Control Volumes
As part of standard laboratory QC, matrix effects on analytical performance are assessed
through the analysis of matrix spikes and laboratory duplicates. For nonisotope dilution
procedures, these analyses are conducted on 10 percent of the samples from a given matrix (e.g.,
aqueous, sludge) within a sampling event. Laboratory QC volumes were taken from composite
volumes collected and poured into separate sample bottles at the same time as sample aliquots
were prepared, or they were collected as grab samples.
EPA collected laboratory QC volumes for at least some of the CECs target analytes at all
nine POTWs.
4.3.4 Trip Blanks
At some POTWs, trip blanks were collected and analyzed for select analytes to evaluate
possible contamination during shipment and handling of samples. Sample containers were filled
18
-------
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs
August 2009
with Ultra Pure Blank Water DI+™ and shipped with empty sample containers to the POTW and
then with the collected samples to the analytical laboratories. Trip blanks collected at Plants A,
B, C, and D were analyzed for volatile organic compounds. Trip blanks collected for Plants E
and F were analyzed for alkylphenols, APEs, and BPA.
4.3.5 Quality Control Sample Summary
Samplers were to collect one equipment blank for every 10 samples collected, but no less
than one per sampling episode. EPA collected 19 total equipment blanks for 31 total samples in
the Nine POTW Study, and met the QAPP QC requirements.
In addition, samplers were to collect one duplicate sample per 10 samples collected for
the program. EPA collected 10 duplicate samples for the 31 total samples, and met the QAPP
requirements.
Table 4-3 lists the QC samples collected for each target analyte family at each POTW
sampled during the program.
Table 4-3. QC Samples at each POTW for each CECs Analyte Family
Analyte
Family
PPCPs
Steroids and
Hormones
Alkylphenols,
APEs, and BPA
PBDEs
Pesticides
Plant
A
MS/MSD
MS/MSD
B
MS/MSD
EfDup
MS/MSD
EfDup
EfDup
InDup
MS/MSD
InDup
C
MS/MSD
EfDup
MS/MSD
EfDup
EfDup
InDup
MS/MSD
InDup
D
MS/MSD
MS/MSD
MS/MSD
E
EfDup
EEBlank
InDup
lEBlank
EfDup
EEBlank
InDup
lEBlank
MS/MSD
EfDup
EEBlank
InDup
lEBlank
TripB
EfDup
InDup
MS/MSD
EfDup
EEBlank
InDup
lEBlank
F
EfDup
EEBlank
InDup
lEBlank
EfDup
EEBlank
InDup
lEBlank
MS/MSD
EfDup
EEBlank
InDup
lEBlank
TripB
EfDup
InDup
MS/MSD
EfDup
EEBlank
InDup
lEBlank
G
EEBlank
EEBlank
MS/MSD
EEBlank
EEBlank
MS/MSD
EEBlank
H
EEBlank
EEBlank
MS/MSD
EEBlank
EEBlank
MS/MSD
EEBlank
I
EEBlank
EEBlank
MS/MSD
EEBlank
EEBlank
MS/MSD
EEBlank
MS/MSD - Matrix spike/matrix spike duplicate.
EfDup - Effluent duplicate.
EEBlank - Effluent equipment blank.
InDup - Influent duplicate.
lEBlank - Influent equipment blank.
Trip B - Trip blank.
4.4 Sample Collection, Preservation, and Storage
Analytical methods used to measure pollutants in the wastewater samples collected in this
study typically include instructions for collecting, preserving, and storing wastewater samples.
These specifications are designed to prevent degradation and loss of the target analytes. Several
19
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
methods direct samplers to maintain samples at a certain temperature or to treat samples with
preserving chemicals. For example organic analytes containing chlorine are preserved with
sodium thiosulfate (^28203). Dissolved thiosulfate converts hypochlorite to chloride ion and
prevents oxidation of the organic analytes in the sample. For the CECs analytical methods,
preservation and storage requirements and recommendations are still under development.
Because EPA was continuing to develop analytical methods during the Nine POTW
Study, sample preservation and storage specifications were in flux. The methods used by EPA to
detect PPCPs, steroids/hormones and pesticides suggest some of the target analytes may degrade
rapidly in aqueous samples. The methods recommended beginning sample extraction within 7
days of collection (within 48 hours is strongly encouraged). Extracts should be analyzed within
40 days of extraction. Freezing of aqueous samples is encouraged to minimize degradation
(especially if extracting within 48 hours is not practical), in which case samples should be
extracted within 48 hours of removal from the freezer. Samples should arrive at the laboratory at
<6°C.
Both methods used to analyze for nonylphenols and alkylphenol ethoxolates required that
samples analyzed for alkylphenols, APEs, and BPA be stored between 0 and 4°C from the time
of collection to extraction. Samples must be extracted within 28 days of collection and
completely analyzed within 40 days of extraction. All samples met the hold times for extraction
and analysis. The laboratory did not report sample temperatures upon receipt.
EPA Method 1614 does not specify holding times associated with PBDEs in aqueous
sample matrices. The method notes that, if stored in the dark at <6°C, aqueous samples may be
stored for up to one year.
The following tables present the sample collection, preservation, and storage conditions
used for samples analyzed for CECs:
Table 4-4: PPCPs;
• Table 4-5: Steroids and Hormones;
• Table 4-6: Alkylphenols, APEs, and BPA;
• Table 4-7: PBDEs; and
• Table 4-8: Pesticides and Herbicides.
20
-------
Table 4-4. PPCPs: Sample Collection, Preservation, and Storage
Plant
Method
Sample Container
for Collection
Field Preservation
Temperature Upon
Receipt at Lab
Lab Preservation
Storage Procedure
Time from
Collection to
Extraction
Time from
Extraction to
Analysis
A
AXYS MLA-052
Rev. 2
1-L amber glass
with Teflon lid
Cool, 0-4°C
3-9°C
NH4-EDTA
Sample
transferred to 4-L
bottle to prevent
breakage and
stored frozen
UNK
UNK
B
AXYS MLA-052
Rev. 2
1-L amber glass
with Teflon lid
Cool, 4°C
9-12°C
None
Refrigerated
Samples extracted
12 days after
receipt
7 to 29 days
C
AXYS MLA-052
Rev. 2
1-L amber glass
with Teflon lid
Cool, 4°C
s-irc,
None
Refrigerated
Samples extracted
3 days after
receipt
1 to 6 days
D
AXYS MLA-052
Rev. 2
1-L amber glass
with Teflon lid
Cool, 4°C
12-14°C
None
4°C
Samples extracted
3 times,
70 days
89 days
98 days after
collection
5 to 43 days
E
EPA 1694
1-L plastic with
Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3when
chlorine was
present
2°C
None
Stored frozen for
50 days prior to
extraction
Samples were
extracted within
48 hours of thaw
UNK
F
EPA 1694
1-L plastic with
Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3when
chlorine was
present
2°C
None
Stored frozen for
45 days prior to
extraction
Samples were
extracted within
48 hours of thaw
UNK
G
EPA 1694
1-L amber plastic
with Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
4°C
None
Stored frozen for
5 days prior to
extraction
Samples
extracted
immediately after
thawing
UNK
H
EPA 1694
1-L amber plastic
with Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3when
chlorine was
present
11°C
None
Not frozen;
extracted upon
receipt
Samples in
transit 5 days
before extract; no
lab storage
UNK
I
EPA 1694
1-L silanized,
amber glass with
Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3when
chlorine was
present
5°C
None
UNK
Samples were
extracted two
days after
collection
Within method-
specified time
1
•a,
i1
I
1
§
UNK - Unknown. Not reported by laboratory or not recorded in data review narrative.
a For Plants E and F, EPA received verbal confirmation from the laboratory that samples arrived at or below 6°C.
-------
Table 4-5. Steroids and Hormones: Sample Collection, Preservation, and Storage
Plant
Method
Sample Container
Field Preservation
Temperature Upon
Receipt at Lab
Storage Procedure
Time from
Collection to
Extraction
Time from
Extraction to
Analysis
A
AXYS MLA-057
Rev. 01
1-L amber glass
with Teflon lid
No headspace; cool,
4°C
3-9°C
Stored frozen
5 months
<40 days
B
AXYS MLA-057
Rev. 01
1-L amber glass
with Teflon lid
Cool, 4°C
9 - 14°C
UNK
34 days
18 days
C
AXYS MLA-057
Rev. 01
1-L amber glass
with Teflon lid
Cool, 4°C
9-ll°C
UNK
4-5 days
8-17 days
D
AXYS MLA-057
Rev. 01
1-L amber glass
with Teflon lid
Cool, 4°C
15-16°C
UNK
60 days
8 days
E
EPA 1698
1-L plastic with
Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3when
chlorine was
present
2°C
Stored frozen
57 days
(extracted
within 48 hours
after thaw)
UNK
F
EPA 1698
1-L plastic with
Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
2°C
Stored frozen
52 days
(extracted
within 48 hours
after thaw)
UNK
G
EPA 1698
1-L amber
plastic with
Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3when
chlorine was
present
3°C
Stored at -20°C
Within method-
specified time
Within method-
specified time
H
EPA 1698
1-L amber
plastic with
Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
16°C
Stored at -20°C
Within method-
specified time
Within method-
specified time
I
EPA 1698
1-L silanized,
amber glass
with Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3when
chlorine was
present
4°C
UNK
Within
contract-
specified time
Within
contract-
specified time
1
•a,
i1
I
1
§
to
to
UNK - Unknown. Not reported by laboratory or not recorded in data review narrative.
-------
Table 4-6. Alkylphenols, APEs, and BPA: Sample Collection, Preservation, and Storage
Plant
Method
Sample Container
Field Preservation
Temperature Upon
Receipt at Lab
Storage Procedure
Time from
Collection to
Extraction
Time from
Extraction to
Analysis
A
CRL-MS004
1-L amber glass
with Teflon lid
Cool, 4°C; HC1 to
pH<2
UNK
Refrigerated
Within the 2 8- day
hold time
Within 45 days of
extraction
B
CRL-MS004
1-L amber glass
with Teflon lid
Cool, 4°C; H2S04
to pH <2
UNK
Refrigerated
Within the 2 8- day
hold time
Within the 40- day
hold time
C
CRL-MS004
1-L amber glass
with Teflon lid
Cool, 4°C; H2S04
to pH <2
UNK
Refrigerated
Within method-
specified time
Within method-
specified time
D
CRL-MS004
1-L amber glass
with Teflon lid
Cool, 4°C; H2S04
to pH <2
UNK
Refrigerated
Within method-
specified time
Within the 40-
day hold time
E
CRL-MS004;
ASTM D 7076-
06"
1-L amber glass
with Teflon lid
Cool, <6°C;
H2S04topH<2
UNK
Refrigerated
Within method-
specified time
Within the 40-
day hold time
F
CRL-MS004;
ASTM D 7076-
06"
1-L amber glass
with Teflon lid
Cool, <6°C;
H2S04topH<2
UNK
Refrigerated
Within method-
specified time
Within the 40-
day hold time
G
CRL-MS004;
ASTM D 7076-
06"
1-L amber glass
with Teflon lid
Cool, <6°C;
H2S04topH<2
UNK
Refrigerated
All arbitrary hold
times were met
All arbitrary hold
times were met. It
has been shown
in cases where re-
extraction was
done, the
concentration
does not change
noticeably within
a 2-4 week period
if preserved
properly.
H
CRL-MS004;
ASTM D 7076-
06"
1-L amber glass
with Teflon lid
Cool, <6°C;
H2S04topH<2
UNK
Refrigerated
All arbitrary hold
times were met
All arbitrary hold
times were met. It
has been shown
in cases where re-
extraction was
done, the
concentration
does not change
noticeably within
a 2-4 week period
if preserved
properly.
I
CRL-MS004;
ASTM D 7076-
06"
1-L amber glass
with Teflon lid
Cool, <6°C;
H2S04topH<2
UNK
UNK
7 days
19 days
1
•a,
i1
I
1
§
to
UNK - Unknown. Not reported by laboratory or not recorded in data review narrative.
a ASTM D 7076-06 used on selected samples.
-------
Table 4-7. PBDEs: Sample Collection, Preservation, and Storage
Plant
Method
Sample Container
Field Preservation
Temperature Upon
Receipt at Lab
Storage Procedure
Time from
Collection to
Extraction
Time from Extraction
to Analysis
A
EPA 1614 draft
1-L amber glass
with Teflon lid
Cool, 0-6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
UNK
No storage
required;
extracted and
analyzed
immediately at
lab
Within method-
specified time
Within method-
specified time
B
EPA 1614 draft
1-L amber glass
with Teflon lid
Cool, 0-6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
9-14°C
No storage
required;
extracted and
analyzed
immediately at
lab
Within method-
specified time
Within method-
specified time
C
EPA 1614 draft
1-L amber glass
with Teflon lid
Cool, 0-6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
8-ll°C
No storage
required;
extracted and
analyzed
immediately at
lab
UNK
UNK
D
EPA 1614 draft
1-L amber glass
with Teflon lid
Cool, 0-6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
14°C
No storage
required;
extracted and
analyzed
immediately at
lab
UNK
UNK
E
EPA 1614
1-L amber glass
with Teflon lid
Cool, 0-6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
3°C
Stored frozen
63 days
(extracted within
48 hours of thaw)
UNK
F
EPA 1614
1-L amber glass
with Teflon lid
Cool, 0-6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
4°C
Stored frozen
63 days
(extracted within
48 hours of thaw)
UNK
G
EPA 1614
1-L amber glass
with Teflon lid
Cool, 0-6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
3°C
UNK
Within contract-
specified time
Within contract-
specified time
H
EPA 1614
1-L amber glass
with Teflon lid
Cool, 0-6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present;
11°C
UNK
Within contract-
specified time
Within contract-
specified time
I
EPA 1614
1-L amber glass
with Teflon lid
Cool, 0-6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
UNK
UNK
Within contract-
specified time
Within contract-
specified time
1
•a,
i1
I
1
§
to
UNK - Unknown. Not reported by laboratory or not recorded in data review narrative.
-------
Table 4-8. Pesticides: Sample Collection, Preservation, and Storage
Plant
Method
Sample Container
Field Preservation
Temperature Upon
Receipt at Lab
Storage Procedure
Time from Collection
to Extraction
Time from Extraction
to Analysis
A
AXYS MLA035
and MLA 037
1-L amber glass
with Teflon lid
Cool, 0-4°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
3-9°C
Transferred to 4L
glass jar and
stored frozen
Approx 6 months
Less than 40
days
B
AXYS MLA035
and MLA 037
1-L amber glass
with Teflon lid
Cool, 4°C
9-14°C
4°C
7 days
8 days
C
AXYS MLA035
and MLA 037
1-L amber glass
with Teflon lid
Cool, 4°C
3-8°C
4°C
3 days
8 days
D
AXYS MLA035
and MLA 037
1-L amber glass
with Teflon lid
Cool, 4°C
14-16°C
4°C
35 days
26 days
E
EPA 1699
1-L amber glass
with Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
3°C
Stored frozen;
extracted within
48 hr of thaw
56-58 days after
collection
UNK
F
EPA 1699
1-L amber glass
with Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
1°C
Stored frozen;
extracted within
48 hr of thaw
53-55 days after
collection a
UNK
G
EPA 1699
1-L amber plastic
with Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
2°C
4°C
Within method-
specified time
Within 40 days
of extraction
H
EPA 1699
1-L amber plastic
with Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
12°C
4°C
Within method-
specified time
Within 40 days
of extraction b
I
EPA 1699
1-L amber glass
with Teflon lid
Cool, <6°C; 80
mg/L (8 mL/L)
Na2S2O3 when
chlorine was
present
3-5°C
UNK
UNK
UNK
1
•a,
i1
I
1
§
to
UNK - Unknown. Not reported by laboratory or not recorded in data review narrative.
a Sample 71322 reanalysis extracted 76 days after collection.
b Sample 71470: heptachlor, dacthal, simazine, hexazinone, and chlorpyriphos re-analyzed diluted 50 days past extraction.
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
5. SUMMARY OF OCCURRENCE DATA
This section summarizes the occurrence of CECs in POTW influent and effluent samples
collected in this study. With each analytical method the laboratory could detect, but not
necessarily quantify, several CECs. Results for which an analyte was detected but failed to meet
method QC specifications are reported as DET. No numerical value is associated with detected
(DET) results. Numerical values are associated with quantifiable results, which are CECs
detected at concentrations greater than the laboratory's reporting limits, and for which there were
no laboratory or data quality problems.
Several classes of CECs were detected and quantified in POTW influents. Quantifiable
amounts of PPCPs, sterols, alkylphenol ethoxylates (APEs), flame retardants (PBDEs), and
pesticides were detected in treated effluent. Hormones and BPA were not quantified in any
effluent sample.
Table 5-1 presents the analytes detected and quantified in the Nine POTW Study and the
percent of sampled POTWs in which they were detected or quantified in influent and effluent.
Because of the ongoing development of the analytical methods, not all of the same CECs were
analyzed for in every POTW. Thus, the denominator in the tables can vary from analyte to
analyte.
The remainder of this section is divided into subsections for the following CECs analyte
classes:
PPCPs;
• Sterols and hormones;
• Alkylphenol s, APEs, and BPA;
• PBDEs; and
• Pesticides.
These subsections present the compounds detected in POTW influent and effluent
samples. These subsections also present tables comparing the compounds detected and quantified
in the influent and effluent based on the general difference between the concentrations
quantified. Analytes are placed into one of the three following categories:
1. Detected or quantified in at least one influent sample and no effluent samples;
2. Quantified2 in at least one influent sample and one or more effluent samples at
concentrations at least one order of magnitude less than at least one influent
sample; and
3. Quantified3 in at least one influent sample and one or more effluent samples at
concentrations similar to influent samples.
2> 3 Only analytes quantified in both influent and effluent samples are included in these comparisons. For example,
the pharmaceutical albuterol was quantified in five influent samples and detected but failed to meet QC
specifications (DET) in effluent samples. Albuterol is not included in Table 5-2 which compares pharmaceutical
influent and effluent concentrations.
26
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
For example, the pharmaceutical acetaminophen, which was detected in all influent
samples and no effluent samples, was placed in the first category. The pharmaceutical
ciprofloxacin was quantified in five influent samples, one of which was 15,100 ng/L, and three
effluent samples, one of which was 36.7 ng/L. Ciproflaxin was placed in the second category.
EPA cautions that this influent/effluent comparison is not based on the difference between
influent/effluent pairs, and is presented only to indicate the CECs for which concentrations in the
effluent were less than those in the influent. EPA did not design these sampling episodes with the
intention of determining treatment effectiveness of the POTWs, nor were sludge samples
analyzed for this study. Consequently, the extent that the concentration differences represent
biological and/or chemical degradation versus partitioning to sludges is not known. More
information on the analytical methods used in this study is in Appendix B.
5.1 PPCPs
Of the 72 PPCPs in the Nine POTW Study, 44 were detected in at least one sample of
POTW influent collected. Of the 44 PPCPs detected, 27 were in 75% or more of the samples in
which the particular PPCP was analyzed (see Table 5-1).
In POTW effluent samples, 33 PPCPs were detected in at least one sample. Of the 33
PPCPs detected, 16 were detected in less than 25% of the effluent samples analyzed for the
PPCP (see Table 5-1).
Thirteen PPCPs were detected or quantified in at least one influent sample and no
effluent samples. Thirteen PPCPs were quantified in at least one influent sample and one or more
effluent samples at concentrations at least one order of magnitude less than influent samples.
Seven PPCPs were quantified in at least one influent sample and one or more effluent samples at
concentrations similar to influent samples. Table 5-2 compares the PPCPs detected in POTW
influent and effluent samples.
27
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table 5-1. Analytes Detected in POTW Influent and Effluent
Analyte
Percent Occurrence in Sampled
POTW Influent
(Number of POTWs at which
analyte was detected
of
Number of POTWs for which
analyte was analyzed a)
Percent Occurrence in Sampled
POTW Effluent
(Number of POTWs at which
analyte was detected
of
Number of POTWs for which
analyte was analyzed a)
PPCPs: Antibiotics
4-Epitetracycline (ETC)
Chlorotetracycline (CTC)
Doxycycline
Minocycline
Tetracycline (TC)
Sulfadiazine
Sulfadimethoxine
Sulfamerazine
Sulfamethazine
Sulfamethizole
Sulfamethoxazole
Sulfathiazole
Ciprofloxacin
Clarithromycin
Erythromycin
Ofloxacin
Tylosin
Azithromycin
Cefotaxime
Cloxacillin
Lincomycin
Penicillin V
Trimethoprim
Virginiamycin
100% (5 of 5)
Il%(lof9)
67% (6 of 9)
20% (1 of 5)
78% (7 of 9)
20% (1 of 5)
25% (2 of 8)
50% (4 of 8)
3 8% (3 of 8)
13% (1 of 8)
100% (8 of 8)
25% (2 of 8)
78% (7 of 9)
100% (5 of 5)
89% (8 of 9)
100% (5 of 5)
0%(0of9)
100% (5 of 5)
0%(0of5)
20% (1 of 5)
56% (5 of 9)
40% (2 of 5)
100% (9 of 9)
22% (2 of 9)
0%(0of5)
Il%(lof9)
11% (1 of 9)
0%(0of5)
Il%(lof9)
20% (1 of 5)
13% (1 of 8)
0% (0 of 8)
13% (1 of 8)
13% (1 of 8)
88% (7 of 8)
0%(0of8)
44% (4 of 9)
60% (3 of 5)
56% (5 of 9)
20% (1 of 5)
Il%(lof9)
40% (2 of 5)
20% (1 of 5)
0%(0of5)
22% (2 of 9)
0%(0of5)
33% (3 of 9)
0% (0 of 9)
PPCPs: Group 1, other than Antibiotics
1,7-Dimethyl xanthine
Acetaminophen
Caffeine
Carbamazepine
Codeine
Cotinine
Dehydronifedipine
Diltiazem
Diphenhydramine
Fluoxetine
100% (9 of 9)
100% (9 of 9)
100% (9 of 9)
100% (5 of 5)
63% (5 of 8)
89% (8 of 9)
80% (4 of 5)
100% (9 of 9)
60% (3 of 5)
78% (7 of 9)
11% (1 of 9)
0%(0of9)
0%(0of9)
80% (4 of 5)
13% (1 of 8)
3 3% (3 of 9)
60% (3 of 5)
44% (4 of 9)
40% (2 of 5)
56% (5 of 9)
28
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table 5-1 (Continued)
Analyte
Miconazole
Thiabendazole
Percent Occurrence in Sampled
POTW Influent
(Number of POTWs at which
analyte was detected
of
Number of POTWs for which
analyte was analyzed a)
100% (5 of 5)
80% (4 of 5)
Percent Occurrence in Sampled
POTW Effluent
(Number of POTWs at which
analyte was detected
of
Number of POTWs for which
analyte was analyzed a)
0%(0of5)
80% (4 of 5)
PPCPs: Group 3
Gemfibrozil
Ibuprofen
Naproxen
Triclocarban
Triclosan
Warfarin
100% (9 of 9)
100% (9 of 9)
100% (5 of 5)
100% (5 of 5)
100% (5 of 5)
44% (4 of 9)
78% (7 of 9)
0%(0of9)
20% (1 of 5)
80% (4 of 5)
0%(0of5)
0%(0of9)
PPCPs: Group 4
Albuterol
Cimetidine
Metformin
Ranitidine
67% (6 of 9)
100% (9 of 9)
88% (7 of 8)
100% (8 of 8)
22% (2 of 9)
22% (2 of 9)
88% (7 of 8)
25% (2 of 8)
Sterols
Beta Sitosterol
Beta Stigmastanol
Campesterol
Cholestanol
Cholesterol
Coprostanol
Desmosterol
Epicoprostanol
Ergosterol
Stigmasterol
100% (9 of 9)
100% (5 of 5)
100% (5 of 5)
100% (9 of 9)
100% (9 of 9)
100% (9 of 9)
100% (9 of 9)
100% (9 of 9)
88% (7 of 8)
100% (9 of 9)
44% (4 of 9)
40% (2 of 5)
40% (2 of 5)
78% (7 of 9)
67% (6 of 9)
89% (8 of 9)
44% (4 of 9)
67% (6 of 9)
50% (4 of 8)
67% (6 of 9)
Hormones
17 Alpha Estradiol
17 Alpha-Dihydroequilin
17 Beta Estradiol
Alpha-Zearalanol
Androstenedione
Androsterone
Beta Estradiol 3-Benzoate
Equilin
Estriol
Estrone
Mestranol
22% (2 of 9)
22% (2 of 9)
33% (3 of 9)
50% (2 of 4)
60% (3 of 5)
100% (5 of 5)
33% (3 of 9)
22% (2 of 9)
100% (5 of 5)
56% (5 of 9)
Il%(lof9)
0%(0of9)
0%(0of9)
0%(0of9)
0%(0of4)
0%(0of5)
0%(0of5)
0%(0of9)
0%(0of9)
0%(0of5)
0%(0of9)
0%(0of9)
29
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table 5-1 (Continued)
Analyte
Norethindrone
Norgestrel
Progesterone
Testosterone
Percent Occurrence in Sampled
POTW Influent
(Number of POTWs at which
analyte was detected
of
Number of POTWs for which
analyte was analyzed a)
33% (3 of 9)
22% (2 of 9)
20% (1 of 5)
89% (8 of 9)
Percent Occurrence in Sampled
POTW Effluent
(Number of POTWs at which
analyte was detected
of
Number of POTWs for which
analyte was analyzed a)
0%(0of9)
0%(0of9)
0%(0of5)
0%(0of9)
Alkylphenols and APEs
Nonylphenol Diethoxylates (NP2EO)
Nonylphenol Monoethoxylates
(NP1EO)
Octylphenol (OC)
Nonlyphenols (NP)
22% (2 of 9)
22% (2 of 9)
44% (4 of 9)
100% (9 of 9)
0%(0of8)
Il%(lof9)
0%(0of9)
Il%(lof9)
PBDEs
PBDE-28+PBDE-33
PBDE-47
PBDE-99
PBDE-100
PBDE-153
PBDE-154
PBDE-183
PBDE-209
100% (9 of 9)
100% (9 of 9)
100% (9 of 9)
100% (9 of 9)
100% (9 of 9)
100% (9 of 9)
100% (9 of 9)
100% (8 of 8)
44% (4 of 9)
89% (8 of 9)
89% (8 of 9)
78% (7 of 9)
67% (6 of 9)
56% (5 of 9)
22% (2 of 9)
33% (3 of 9)
Pesticides: Organochlorine
2,4'-DDD
2,4'-DDT
4,4'-DDD
4,4'-DDE
4,4'-DDT
Aldrin
Alpha-BHC
Alpha-chlordane
Beta-BHC
Chlorothalonil
Cis-Nonachlor
Dieldrin
Endosulphan I
Endosulfan sulfate
Gamma-BHC
Gamma-chlordane
Heptachlor
Heptachlor Epoxide
22% (2 of 9)
Il%(lof9)
22% (2 of 9)
89% (8 of 9)
22% (2 of 9)
Il%(lof9)
Il%(lof9)
89% (8 of 9)
Il%(lof9)
17% (1 of 6)
33% (3 of 9)
89% (8 of 9)
Il%(lof9)
0%(0of9)
44% (4 of 9)
89% (8 of 9)
Il%(lof9)
44% (4 of 9)
0%(0of9)
0%(0of9)
0%(0of9)
0%(0of9)
0%(0of9)
0%(0of9)
0%(0of9)
0%(0of9)
0%(0of9)
0%(0of7)
0%(0of9)
56% (5 of 9)
Il%(lof9)
Il%(lof9)
33% (3 of 9)
Il%(lof9)
0%(0of9)
Il%(lof9)
30
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table 5-1 (Continued)
Analyte
Hexachlorobenzene
Methoxychlor
Perthane
Trans-Nonachlor
Percent Occurrence in Sampled
POTW Influent
(Number of POTWs at which
analyte was detected
of
Number of POTWs for which
analyte was analyzed a)
25% (2 of 8)
Il%(lof9)
33% (3 of 9)
78% (7 of 9)
Percent Occurrence in Sampled
POTW Effluent
(Number of POTWs at which
analyte was detected
of
Number of POTWs for which
analyte was analyzed a)
0%(0of8)
44% (4 of 9)
0%(0of9)
0%(0of9)
Pesticides: Organophosphorus
Chlorpyriphos
Chlorpyriphos-oxon
Diazinon
Diazinon oxon
Disulfoton sulfone
Malathion
Methamidophos
Methyl-chlorpyriphos
Methyl-parathion
67% (6 of 9)
Il%(lof9)
67% (6 of 9)
0%(0of9)
Il%(lof9)
22% (2 of 9)
Il%(lof9)
Il%(lof9)
n%(iof9)
0%(0of8)
22% (2 of 9)
56% (5 of 9)
22% (2 of 9)
0%(0of9)
0%(0of9)
Il%(lof9)
0%(0of9)
0%(0of9)
Pesticides: Pyrethroid
Cis-Permethrin
Cypermethrins
Permethrin
Trans-Permethrin
80% (4 of 5)
78% (7 of 9)
89% (8 of 9)
100% (5 of 5)
0%(0of5)
0%(0of9)
22% (2 of 9)
0%(0of5)
Pesticides: Triazine
Atrazine
Cyanazine
Desethyl atrazine
Hexazinone
Metribuzin
Simazine
89% (8 of 9)
0%(0of9)
89% (8 of 9)
Il%(lof9)
0%(0of9)
44% (4 of 9)
100% (9 of 9)
Il%(lof9)
89% (8 of 9)
22% (2 of 9)
22% (2 of 9)
56% (5 of 9)
' Does not include excluded results. Includes detected (DET) and quantified results. See Appendix C.
31
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table 5-2. Comparison of PPCPs Detected in POTW Influent and Effluent
b,c
Detected in at Least One Influent
Sample AND
No Effluent Samples
Quantified in at Least One Influent Sample
AND
One or More Effluent Samples at
Concentrations at Least One Order of
Magnitude Less than at Least One
Influent Sample
One or More Effluent
Samples at Concentrations
Similar to Influent Samples
Antibiotics
4-Epitetracycline (ETC)
Minocycline a
Sulfamerazine
Sulfathiazole
Cloxacillin a
Penicillin V a
Virginiamycin3
Doxycycline
Sulfamethoxazole
Ciprofloxacin
Clarithromycin
Erythromy tin-Total
Oflaxacin
Chlorotetracyline (CTC)
Tetracycline (TC)
Sulfadiazine
Trimethoprim
Analytical Group 1, other than Antibiotics
Acetaminophen
Caffeine
Miconazole
Cotinine
Carbamazepine
Fluoxetine
Thiabendazole
Analytical Group 3
Ibuprofen
Triclosan
Warfarin3
Gemfibrozil
Naproxen
Triclocarban
None
Analytical Group 4
None
Cimetidine
Metformin
Ranitidine
None
a All influent results for which the analyte was detected are DET.
b Tylosin and cefotaxime were detected in POTW effluent and no samples of POTW influent. They are not included
on this table.
0 Eleven pharmaceuticals were detected in at least one influent and one effluent sample but were not quantified in
both influent and effluent samples. Consequently, their influent and effluent concentrations could not be compared
and they are not included on this table.
Many of the PPCPs laboratory results failed to meet the QC specifications of the
analytical method. Of the 441 results for which the concentration was reported above the
laboratory-reported detection limit, 54 percent of the results were not qualified in any way and
are considered accurate. The remaining 46 percent of the results were reported only as detected
(DET). No numerical value should be attached to these results because of poor spike recovery or
other laboratory problems. See Table 5-3 for additional statistics on detections and
quantifications for PPCP samples.
32
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table 5-3. Numbers of PPCPs Detected in POTW Influent and Effluent
Analyte Group
Antibiotics
Group 1, other than
antibiotics
Group 3
Group 4
Total
Number of
Analytes
47
15
6
4
72
Number of Analytes Detected in at Least One Sample of
POTW Influent
DETa
6
1
1
0
8
Quantified b
16
11
5
4
36
Total
Detected
22
12
6
4
44
POTW Effluent
DETa
5
4
0
1
10
Quantified b
12
5
o
J
3
23
Total
Detected
17
9
3
4
33
a Analytes for which all POTW influent/effluent sample results were DET.
b At least one sample of POTW influent/effluent was detected with no QC issues.
5.2 Sterols and Hormones
All evaluated sterols were detected in all POTW influent samples3. Sterols were detected
in fewer samples of POTW effluent than influent, but all evaluated sterols were detected in at
least one sample of effluent (see Table 5-1).
Concentrations of all evaluated sterols were much lower in the POTW effluent samples
than in the influent samples (see Table 5-4).
Hormones were detected in fewer POTW influent samples than sterols, and when
detected, the concentrations of hormones were typically much lower than concentrations of
sterols. Evaluated hormones were not detected in any effluent samples (see Tables 5-4).
1 With the exception of one analyte (ergosterol) at one plant.
33
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table 5-4. Comparison of Sterols and Hormones Detected in POTW Influent and Effluent
Detected in at Least One Influent
Sample AND
Quantified in at Least One Influent Sample
AND
No Effluent Samples
One or More Effluent Samples at
Concentrations at Least One Order of
Magnitude Less than at Least One
Influent Sample
One or More Effluent
Samples at Concentrations
Similar to Influent Samples
Sterols"
None
Beta Sitosterol
Beta Stigmastanol
Campesterol
Cholestanol
Cholesterol
Coprostanol
Desmosterol
Epicoprostanol
Stigmasterol
None
Hormones
17 Alpha-Estradiola
17 Alpha-Dihydroequilina
17 Beta-Estradiola
Alpha-Zearalanola
Androstenedione
Androsterone
Beta-Estradiol-3-Benzoate'
Equilin
Estriol
Estrone
Mestranola
Norethindrone
Norgestrela
Progesterone
Testosterone
None
None
a All influent results for which the analyte was detected are DET.
b Ergosterol was quantified in at least one influent sample but was not quantified in effluent samples. Consequently
its influent and effluent concentrations could not be compared and it is not included on this table.
Many of the sterol and hormone analytical results failed to meet method QC
specifications. Of the 240 results for which the concentration was reported above the laboratory-
reported detection limit, 58 percent of the results were not qualified in any way and are
considered accurate. The remaining 42 percent of the results were reported only as detected
(DET). No numerical value should be attached to these results because of poor spike recovery or
other laboratory problems. See Table 5-5 for additional statistics on detections and
quantifications of Steroid and Hormone samples.
34
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table 5-5. Numbers of Sterols and Hormones Detected in POTW Influent and Effluent
Analyte Group
Sterols
Hormones
Number of
Analytes
10
17
Number of Analytes Detected in at Least One Sample of
POTW Influent
DETa
0
6
Quantified b
10
9
Total
Detected
10
15
POTW Effluent
DETa
1
0
Quantified b
9
0
Total
Detected
10
0
a Analytes for which all POTW influent/effluent sample results were DET.
b At least one sample of POTW influent/effluent was detected with no QC issues.
5.3 Alkylphenols, APEs, and BPA
BPA was not detected in the influent or effluent of any sampled plant. NP was detected in
each plant influent, additionally, the reporting limits for NP were significantly lower than the
EPA Water Quality Criteria of 6,600 ng/L. Moreover, nonlyphenol monoethoxylates (NP1EO),
nonlyphenol diethoxylates (NP2EO), and octylphenol (OP) were occasionally detected. OP and
NP2EO were never detected in the effluent (see Tables 5-6).
Table 5-6. Comparison of Alkylphenols, APEs, and BPA Detected in POTW Influent and
Effluent
Detected in at Least One Influent
Sample AND
No Effluent Samples
OP
NP2EO
Quantified in at Least One Influent Sample
AND
One or More Effluent Samples at
Concentrations at Least One Order of
Magnitude Less than at Least One
Influent Sample
NP1EO
NP
One or More Effluent
Samples at Concentrations
Similar to Influent Samples
None
Some of the analytical results failed to meet method QC specifications. Of the 31 results
for which the concentration was reported above the laboratory-reported detection limit, 65
percent of the results were not qualified in any way and are considered accurate. The remaining
35 percent of the results were reported only as detected (DET). No numerical value should be
attached to these results because of poor spike recovery or other laboratory problems. See Table
5-7 for additional statistics on detections and quantifications of alkylphenols, APEs and BPA.
35
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table 5-7. Numbers of Alkylphenols, APEs, and BPA Detected in POTW Influent and
Effluent
Analyte Group
Alkylphenols,
Alkylphenol
Ethoxylates (APEs),
and Bisphenol A
Number
of
Analytes
5
Number of Analytes Detected in at Least One Sample of
POTW Influent
DETa
0
Quantified b
4
Total
Detected
4
POTW Effluent
DETa
0
Quantified b
2
Total
Detected
2
a Analytes for which all POTW influent/effluent sample results were DET.
b At least one sample of POTW influent/effluent was detected with no QC issues.
5.4 PBDEs
There are 209 PBDE congeners. For the Nine POTW Study, results were reported for
nine PBDEs of interest (EPA, 2007a). Note that PBDE-28 and PBDE-33 are treated as one
analyte in this report because the analytical laboratory reported results for PBDE-28 + PBDE-33.
All PBDE congeners evaluated in this study were detected in all POTW influent samples.
The concentrations of the analyzed congeners are very similar plant to plant, despite the
differences in the populations served by the POTWs. Concentrations of all congeners of interest
are much lower in the samples of POTW effluent than in samples of POTW influent (Table 5-8).
Table 5-8. Comparison of PBDEs Detected in POTW Influent and Effluent
Detected in at Least One Influent
Sample AND
Quantified in at Least One Influent Sample
AND
No Effluent Samples
One or More Effluent Samples at
Concentrations at Least One Order of
Magnitude Less than at Least One
Influent Sample
One or More Effluent
Samples at Concentrations
Similar to Influent Samples
None
PBDE-28 + PBDE-33
PBDE-47
PBDE-99
PBDE-100
PBDE-153
PBDE-154
PBDE-183
PBDE-209
None
The concentration of PBDE-209 in preparation blanks was often greater than the method
quantitation levels (EPA Method 1614 quantitation level of 2 ppt). Because PBDE-209 sample
results for POTW effluents are close to the method quantitation level, for effluent samples from
four plants, it was impossible to determine if PBDE-209 detected in the effluent was the result of
contamination. Consequently, the effluent sample concentrations were reported as not-quantified
at the quantitation level, adjusted for sample size. See Appendix C.
36
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
A relatively small percentage of the PBDEs analytical results failed to meet method QC
specifications in comparison to some of the other CECs analyte families. Of the 156 results for
which the concentration was reported above the laboratory-reported detection limit, 87 percent of
the results were not qualified in any way and are considered accurate. The remaining 13 percent
of the results were reported only as detected (DET). No numerical value should be attached to
these results because of poor spike recovery or other laboratory problems. See Table 5-9 for
additional statistics on detections and quantifications of PBDEs.
Table 5-9. Numbers of PBDEs Detected in POTW Influent and Effluent
Analyte Group
PBDEs
Number of
Analytes
8
Number of Analytes Detected in at Least One Sample of
POTW Influent
DETa
0
Quantified b
8
Total
Detected
8
POTW Effluent
DETa
0
Quantified b
8
Total
Detected
8
a Analytes for which all POTW influent/effluent sample results were DET.
b At least one sample of POTW influent/effluent was detected with no QC issues.
5.5 Pesticides
Of the 62 pesticides, 37 were detected in at least one sample of POTW influent collected
in this study. Eighteen (18) pesticides were detected in at least one sample of POTW effluent
(Table 5-1).
Twenty-three (23) pesticides were detected or quantified in at least one influent sample
and no effluent samples. Five pesticides were quantified in at least one influent sample and one
or more effluent samples at concentrations at least one order of magnitude less than influent
samples. Five pesticides were quantified in at least one influent sample and one or more effluent
samples at concentrations similar to influent samples. Table 5-10 compares the pesticides
detected in POTW influent and effluent samples.
37
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table 5-10. Comparison of Pesticides Detected in POTW Influent and Effluent
b,c
Detected in at Least One Influent
Sample AND
No Effluent Samples
Quantified in at Least One Influent Sample
AND
One or More Effluent Samples at
Concentrations at Least One Order of
Magnitude Less than at Least One
Influent Sample
One or More Effluent
Samples at Concentrations
Similar to Influent Samples
Organochlorine
2,4'-DDD
2,4'-DDT
4,4'-DDD
4,4'-DDE
4,4'-DDT
Aldrin
Alpha-BHC
Alpha-chlordane
Beta-BHC
Chlorothalonil
Cis-nonachlor
Heptachlor a
Hexachlorobenzene
Perthane
Trans-nonachlor
Dieldrin
Gamma-chlordane
Gamma-BHC
Heptachlor Epoxide
Organophosphorus
Chlorpyriphos
Disulfoton sulfone a
Malathion
Methyl-chlorpyriphos a
Methyl-parathion
Diazinon
None
Pyrethroid
Cis-Permethrin
Cypermethrins
Trans -Permethrin
Permethrin (sum of cis and trans)
None
Triazine
Desethyl atrazine
Atrazine
Hexazinone
Simazine
a All influent results for which the analyte was detected are DET.
b Endosulfan sulfate,diazinon oxon, metribuzin, and cyanizine were detected in POTW effluent and no samples of
POTW influent. They are not included on this table.
0 Endosulfan I, metholxychlor, chlorpyrophos oxon, and methamidophos were detected in at least one influent and
one effluent sample. They were not quantified in both influent and effluent samples, however. As a result, their
influent and effluent concentrations could not be compared and they are not included on this table.
A relatively small percentage of the pesticides analytical results failed to meet method
QC specifications in comparison to some of the other CECs analyte families. Of the 238 results
for which the concentration was reported above the laboratory-reported detection limit, 81
percent of the results were not qualified in any way and are considered accurate. The remaining
19 percent of the results were reported only as detected (DET). No numerical value should be
attached to these results because of poor spike recovery or other laboratory problems. See Table
5-11 for additional statistics on detections and quantifications of pesticides.
38
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table 5-11. Numbers of Pesticides Detected in POTW Influent and Effluent
Analyte Group
Organochlorine
Organophosphorus
Pyrethroid
Triazine
Total
Number of
Analytes
34
17
4
7
62
Number of Analytes Detected in at Least One Sample of
POTW Influent
DETa
3
4
0
0
7
Quantified b
18
4
4
4
30
Total
Detected
21
8
4
4
37
POTW Effluent
DETa
0
1
0
1
2
Quantified b
7
3
1
5
16
Total
Detected
7
4
1
6
18
a Analytes for which all POTW influent/effluent sample results were DET.
b At least one sample of POTW influent/effluent was detected with no QC issues.
39
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
6. REFERENCES
ASTM, 2006. ASTM International. Standard Test Method for Determination of Nonylphenol,
Bisphenol A, p-tert-Octylphenol, Nonylphenol Monoethoxylate and Nonylphenol
Diethoxylate in Environmental Waters by Gas Chromatography Mass Spectrometry,
ASTM D7065 - 06. 2006.
Census, 2007. U.S. Census Bureau. School Enrolment, Table A-5a. The Population 14 to 24
Years Old by High School Graduate Status, College Enrollment, Attainment, Sex, Race,
and Hispanic Origin: October 1967 to 2005. http://www.census.gov/population/socdemo/
school/TableA-Sa.xls. Accessed 16 October 2007.
Chandra, 2005. Chandra A, G.M. Martinez, W.D. Mosher, J.C. Abma, J. Jones. "Fertility,
Family Planning, and Reproductive Health of U.S. Women: Data from the 2002 National
Survey of Family Growth." National Center for Health Statistics. Vital and Health
Statistics 23 (25). http://www.cdc.gov/nchs/products/pubs/pubd/series/sr23/pre-
l/sr23_25.htm. Accessed 15 October 2007.
EPA, 1982. U.S. Environmental Protection Agency. Fate of Priority Pollutants in Publicly
Owned Treatment Works. EPA 440/1-82/303. September 1982.
EPA, 2001. U.S. Environmental Protection Agency. EPA Requirements for Quality Assurance
Project Plans, EPA QA/R-5. March 2001. http://www.epa.gov/QUALITY/qs-docs/r5-
final.pdf. Accessed 13 November 2008.
EPA, 2007a. U.S. Environmental Protection Agency, Office of Science and Technology. Method
1614: Brominated Diphenyl Ethers in Water, Soil, Sediment and Tissue by
HRGC/HRMS, EPA 821-R-07-005. August 2007.
EPA, 2007b. U.S. Environmental Protection Agency, Office of Science and Technology. Method
1694: Pharmaceuticals and Personal Care Products in Water, Soil, Sediment, and
Biosolids by HPLC/MS/MS, EPA 821-R-08-002. December 2007.
EPA, 2007c. U.S. Environmental Protection Agency, Office of Science and Technology. Method
1698: Steroids and Hormones in Water, Soil, Sediment, and Biosolids by HRGC/HRMS,
EPA 821-R-08-003. December 2007.
EPA, 2007d. U.S. Environmental Protection Agency, Office of Science and Technology. Method
1699: Pesticides in Water, Soil, Sediment, Biosolids, and Tissue by HRGC/HRMS, EPA
821-R-08-001. December 2007.
ERG, 2006. Eastern Research Group, Inc. Quality Assurance Project Plan for the POTW Study.
19 May 2006.
ERG, 2008. Eastern Research Group, Inc. Quality Assurance Project Plan for the POTW Study.
13 June 2008.
40
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
Kaufman, 2002. D.W. Kaufman, J.P. Kelly, L. Rosenberg, I.E. Anderson, A.A. Mitchell.
"Recent patterns of medication use in the ambulatory adult population of the United
States: The Slone Survey." JAMA 2002; 287:337-44.
Metcalf and Eddy, 1978. Metcalf and Eddy, Inc. Wastewater Engineering: Treatment/
Disposal/Reuse, Second Edition. Boston: McGrawHill. 1978.
Slone, 2006. Slone Center for Epidemiology at Boston University. Patterns of Medication Use in
The United States, 2006: A Report from the Slone Survey.
http://www.bu.edu/slone/SloneSurvey/SloneSurvey.htm. Accessed 15 October 2007.
41
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
Appendix A
CONTAMINANTS OF EMERGING CONCERN (CECs) ANALYTE LIST
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table A-l. PPCP Analyte List
Analyte
Classification
AXYS
Method
MLA-052
(Plants
A,B,C,D)
EPA
Method
1694
(Plants
E,F,G,H,I)
Antibiotics
4-Epianhydrochlortetracycline (EACTC)
4-Epianhydrotetracycline (EATC)
4-Epichlortetracycline (ECTC)
4-Epioxytetracycline (EOTC)
4-Epitetracycline (ETC)
Anhydrochlortetracycline (ACTC)
Anhydrotetracycline (ATC)
Chlorotetracycline (CTC)
Demeclocycline
Doxycycline
Isochlortetracycline (ICTC)
Minocycline
Oxytetracycline (OTC)
Tetracycline
Sulfachloropyridazine
Sulfadiazine
Sulfadimethoxine
Sulfamerazine
Sulfamethazine
Sulfamethizole
Sulfamethoxazole
Sulfanilamide
Sulfathiazole
Ciprofloxacin
Clarithromycin
Clinafloxacin
Enroflaxacin
Erythromycin
Lomefloxacin
Norfloxacin
Ofloxacin
Roxithromycin
Sarafloxacin
Tylosin
Ampicillin
Azithromycin
Chlorotetracycline degradate
Chlorotetracycline degradate
Chlorotetracycline degradate
Oxyetracycline degradate
Tetracycline degradate
Chlorotetracycline degradate
Chlorotetracycline degradate
Tetracycline antibiotic
Tetracycline antibiotic
Tetracycline antibiotic
Chlorotetracycline degradate
Tetracycline antibiotic
Tetracycline antibiotic
Tetracycline antibiotic
Sulfonamide antibiotic
Sulfonamide antibiotic
Sulfonamide antibiotic
Sulfonamide antibiotic
Sulfonamide antibiotic
Sulfonamide antibiotic
Sulfonamide antibiotic
Sulfonamide antibiotic
Sulfonamide antibiotic
Fluoroquinolone antibiotic
Macrolide antibiotic
Quinoline antibiotic
Fluoroquinolone antibiotic
Macrolide antibiotic
Quinoline antibiotic
Quinoline antibiotic
Quinoline antibiotic
Macrolide antibiotic
Fluoroquinolone antibiotic
Macrolide antibiotic
B-lactam antibiotic
Macrolide antibiotic
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
a
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
a
X
A-l
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table A-l (Continued)
Analyte
Carbadox
Cefotaxime
Cloxacillin
Flumequine
Lincomycin
Ormetoprim
Oxacillin
Oxolinic acid
Penicillin G
Penicillin V
Trimethoprim
Virginiamycin
Classification
Quinoxaline antibiotic
Cephalosporin antibiotic
B-lactam antibiotic
Quinolone antibiotic
Lincosamide antibiotic
Macrolide antibiotic
B-lactam antibiotic
Quinolone antibiotic
B-lactam antibiotic
B-lactam antibiotic
Pyrimidine antibiotic
Macrolide antibiotic
AXYS
Method
MLA-052
(Plants
A,B,C,D)
X
X
X
X
EPA
Method
1694
(Plants
E,F,G,H,I)
X
X
X
X
X
X
X
X
X
X
X
X
Analytical Group 1, other than antibiotics
1 ,7-Dimethylxanthine
Acetaminophen
Caffeine
Carbamazepine
Codeine
Cotinine
Dehydronifedipine
Digoxigenin
Digoxin
Diltiazem
Diphenhydramine
Fluoxetine
Miconazole
Norgestimate
Thiabendazole
Antispasmodic, caffeine metabolite
Antipyretic, analgesic
Stimulant
Anticonvulsant
Opiate
Nicotine metabolite
Nifedipine metabolite
Immunohistochemical marker steroid
Cardiac glycoside
Antihypertensive
Antihistamine
SSRI antidepressant
Antifungal agent
Hormonal contraceptives
Fungicide and parasiticide
X
X
X
xb
X
X
X
X
X
xb
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
Analytical Group 3
Gemfibrozil
Ibuprofen
Naproxen
Triclocarban
Triclosan
Warfarin
Antilipemic
Analgesic
NSAID
Antimicrobial
Antimicrobial
Anticoagulant
X
X
X
X
X
X
X
X
X
A-2
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table A-l (Continued)
Analyte
Classification
AXYS
Method
MLA-052
(Plants
A,B,C,D)
EPA
Method
1694
(Plants
E,F,G,H,I)
Analytical Group 4
Albuterol
Cimetidine
Metformin
Ranitidine
Antiasthmatic
Anti-acid reflux
Anti-diabetic drag
Anti-acid reflux
Total
X
X
X
X
40
X
X
X
X
73
a Although listed in Method 1694, ampicillin was not included in either Stage 1 or Stage 2 of the Nine POTW Study.
b Codeine and norgestimate were included in AXYS Method MLA-052 for the analysis of Plant B, C, and D
samples, but not for Plant A samples.
Note all compounds listed in Table A-l are pharmaceuticals with the exception of
triclosan and triclocarban, both antimicrobial compounds. Samples from Plants E - I were
analyzed for triclosan and triclocarban, while samples from Plants A, B, C, and D were not.
A-3
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table A-2. Steroids and Hormones Analyte List
Analyte
AXYS Method
MLA-057 Rev 01
(Plants A,B,C,D)
EPA Method
1698
(Plants E,F,G,H,I)
Sterols
Beta Sitosterol
Beta Stigmastanol
Campesterol
Cholestanol
Cholesterol
Coprostanol
Desmosterol
Epi-coprostanol
Ergosterol
Stigmasterol
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
Hormones
17 Alpha-Dihydroequilin
17 Alpha-Estradiol
17 Alpha-Ethinyl Estradiol a
17 Beta-Estradiol
Alpha-Zearalanol
Androstenedione
Androsterone
Beta-Estradiol-3 -Benzoate
Desogestrel
Equilenin
Equilin
Estriol
Estrone
Ethynylestradiol a
Mestranol
Norethindrone
Norgestrel
Progesterone
Testosterone
Total
X
X
X
X
X
xb
X
X
X
X
X
X
X
21
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
27
a Ethynylestradiol and 17 Alpha-Ethinyl Estradiol are synonyms.
b Desogestrel was included in AXYS Method MLA-057 Rev 01 for the analysis of Plant A samples, but not for
Plants B, C, orD.
A-4
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table A-3. Alkylphenols, APEs, and BPA Analyte List
Method Number
MS004 (Plants A-I) and
ASTM Method D 7065-06
(Plants E-I)
Full Name
Nonylphenols a
Nonylphenol Monoethoxylates a
Nonylphenol Diethoxylates a
Octylphenol
Bisphenol A
Abbreviated Name
NP
NP1EO
NP2EO
OP
BPA
a Nonylphenols, nonylphenol monoethoxylates, and nonylphenol diethoxylates are mixtures of branched isomers.
The concentrations reported are the totals for the isomer mixtures.
Table A-4. PBDE Analyte List (Plants A-I)
Full Name
2,4,4'-Tribromodiphenyl ether plus
2',3,4-Tribromodiphenyl ether
2,2',4,4'- Tetrabromodiphenyl ether
2,2',4,4',5- Pentabromodiphenyl ether
2,2',4,4',6-Pentabromodiphenyl ether
2 2' 4 4' 5 5'- Hexabromodiphenyl ether
2,2',4,4',5',6- Heptabromodiphenyl ether
2 2' 3 4 4' 5' 6- Heptabromodiphenyl ether
Decabromodiphenyl ether
Abbreviated Name
2,4,4'-TrBDE plus
2',3,4-TrBDE
2,2',4,4'-TeBDE
2,2',4,4',5-PeBDE
2,2',4,4',6-PeBDE
2 2' 4 4' 5 5'-HxBDE
2,2',4,4',5',6-HxBDE
2 2' 3 4 4' 5' 6-HpBDE
DeBDE
Number
PBDE-28+PBDE-33a
PBDE-47
PBDE-99
PBDE-100
PBDE- 153
PBDE- 154
PBDE- 183
PBDE-209
a PBDE 28 and PBDE 33 have the same retention time on the DB-5HT gas chromatography column and cannot be
quantified separately. For this reason, the concentration of PBDE 28 + PBDE 33 presented in this report represents
the total concentration for these two TrBDE congeners.
A-5
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table A-5. Pesticides Analyte List
Analyte
AXYS Method
MLA-035 Rev 04
Plant A
AXYS Method
MLA-035 Rev 04
Plants B- D
EPA Method 1699
Plants E - 1
Organochlorine
2,4'-DDD
2,4'-DDE
2,4'-DDT
4,4'-DDD
4,4'-DDE
4,4'-DDT
Aldrin
Alpha-BHC
Alpha-chlordane
Beta-BHC
Captan
Chlorothalonil
Cis-nonachlor
Dacthal
Delta-BHC
Dieldrin
Endosulfan I
Endosulfan II
Endosulfan sulfate
Endrin
Endrin Ketone
Gamma-BHC
Gamma-chlordane
Heptachlor
Heptachlor Epoxide
Hexachlorobenzene
Methoxychlor
Mirex
Octachlorostyrene
Oxychlordane
Pentachloro nitrobenzene
Perthane
Tecnazene
Trans-nonachlor
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
Organophosphorus
Azinphos-methyl
Chlorpyriphos
Chlorpyriphos-oxon
X
X
X
X
X
X
X
X
X
A-6
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table A-5 (Continued)
Analyte
Diazinon
Diazinon-oxon
Disulfoton
Disulfoton sulfone
Ethyl-parathion
Fenitrothion
Fonofos
Malathion
Methamidophos
Methyl-chlorpyriphos
Methyl-parathion
Phorate
Phosmet
Pirimiphos-methyl
AXYS Method
MLA-035 Rev 04
Plant A
X
X
X
X
X
X
X
X
X
X
X
X
X
X
AXYS Method
MLA-035 Rev 04
Plants B- D
X
X
X
X
X
X
X
X
X
X
X
X
X
X
EPA Method 1699
Plants E - 1
X
X
X
X
X
X
X
X
X
X
X
X
X
X
Pyrethroid
Cis-permethrin
Cypermethrins
Permethrin
Trans-permethrin
X
X
X
X
X
X
X
X
Triazine
Ametryn
Atrazine
Cyanazine
Desethyl atrazine
Hexazinone
Metribuzin
Simazine
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
Other Compounds (not included in EPA Method 1699)
Alachlor
Benzonitrile, 3,5-Dibromo-4-Hydroxy-
Butralin
Butylate
Dimethenamid
Dimethoate
Ethalfluralin
Ethion
Fluazifop
Flufenacet
Flutriafol
Linuron
MCOA
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
A-7
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
Table A-5 (Continued)
Analyte
Methoprene
Metolachlor
Pendamethalin
Tebuconazol
Terbufos
Triallate
Trifluralin
Total
AXYS Method
MLA-035 Rev 04
Plant A
X
X
X
X
X
X
X
79
AXYS Method
MLA-035 Rev 04
Plants B- D
X
X
X
X
X
X
X
78
EPA Method 1699
Plants E - 1
62
A-8
-------
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Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
Appendix B
ANALYTICAL METHODS OVERVIEW
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
The analytical methods used to measure CECs in the Nine POTW Study were developed
and revised throughout the course of this study. The version of the method used to analyze
samples from each plant is listed in Table B-l.
Table B-l Analytical Methods by POTW
Plant
A
B
C
D
E
F
G
H
I
PPCP Method
Laboratory SOP
AXYS MLA-
052 a
AXYS MLA-
052 a
AXYS MLA-
052 a
EPA Method
1694
EPA Method
1694
EPA Method
1694
EPA Method
1694
EPA Method
1694
S/H Method
AXYS Method MLA-
057 Rev 01 a
AXYS Method MLA-
057 Rev 01 a
AXYS Method MLA-
057 Rev 01 a
AXYS Method MLA-
057 Rev 01 a
EPA Method 1698
EPA Method 1698
EPA Method 1698
EPA Method 1698
EPA Method 1698
Pesticide Method
AXYS Method MLA-
035 Rev. 04 a
AXYS Method MLA-
035 Rev. 04 a
AXYS Method MLA-
035 Rev. 04 a
AXYS Method MLA-
035 Rev. 04 a
EPA Method 1699
EPA Method 1699
EPA Method 1699
EPA Method 1699
EPA Method 1699
PBDE Method
Draft EPA Method 16 14
(August 2003)
Draft EPA Method 16 14
(August 2003)
Draft EPA Method 1614
(August 2003)
Draft EPA Method 1614
(August 2003)
EPA Method 1614
(August 2007)
EPA Method 1614
(August 2007)
EPA Method 1614
(August 2007)
EPA Method 1614
(August 2007)
EPA Method 1614
(August 2007)
APEs Method
CRL-MS004 Rev #2
CRL-MS004 Rev #2
CRL-MS004 Rev #2
CRL-MS004 Rev #2
CRL-MS004 Rev #2
and
ASTM Method D
7065-06
CRL-MS004 Rev #2
and
ASTM Method D
7065-06
CRL-MS004 Rev #2
and
ASTM Method D
7065-06
CRL-MS004 Rev #2
and
ASTM Method D
7065-06
CRL-MS004 Rev #2
and
ASTM Method D
7065-06
a AXYS Analytical Services, Sidney, British Columbia, Canada.
Samples collected during Stage 1 of the Study (September 2005 - September 2006) were
analyzed with draft methods based on procedures developed at contract laboratories. EPA used
the results of these analyses to develop more sensitive and selective analytical methods for three
groups of CECs: PPCPs, steroids and hormones, and pesticides. Three new EPA methods
resulted from this work (EPA 1694, 1698 and 1699). These methods were designed to screen for
a large number of analytes in a broad range of POTW matrices including influent, effluent, and
sewage sludge. After single-laboratory validation and peer review, three methods were published
in December 2007, and EPA used the published methods to analyze samples collected in Stage 2
of the Nine POTW Study (November 2007 through September 2008).
The PBDE (flame retardants) analytical method (EPA Method 1614; EPA, 2007a) was
developed before the Nine POTW Study began. Although EPA Method 1614 was multi-
laboratory validated and published in August 2007; EPA made some additional refinements
during this study to improve the detection of certain PBDEs.
B-l
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
These four methods (EPA 1614, 1694, 1698 and 1699) are available on the CWA
methods website at http://www.epa.gov/waterscience/methods/method/other.html, and are listed
in Table B-2.
Table B-2. EPA Analytical Methods for CECs
EPA Method
Number
1614
1694
1698
1699
Analyte Group
PBDEs
PPCPs
Steroids and Hormones
Pesticides
Method Type
HRGC/HRMS
HPLC/MS/MS
HRGC/HRMS
HRGC/HRMS
Method Status During
Stage 1
Under development
Under development
Under development
Under development
Date Published
August 2007
December 2007
December 2007
December 2007
HRGC/HRMS - High resolution gas chromatography/high resolution mass spectrometry.
HPLC/MS/MS - High performance liquid chromatography/tandem mass spectrometry.
In both stages of the Nine POTW Study, EPA analyzed samples of POTW influent and
effluent for alkylphenols, APEs, and BPA using methods recently developed by the EPA Region
5 Chicago Regional Laboratory (CRL). During Stage 2, some samples were also analyzed using
ASTM Method D 7065-06 (ASTM, 2006), which is based on the EPA Region 5 methods. Table
B-3 lists these methods.
Table B-3. CRL Analytical Methods for Alkylphenol-Related Compounds
CRL Method
Number
MS004
ASTM D 7065-06
Analyte Group
Short chain alkylphenol ethoxylates and bisphenol A
Short chain alkylphenol ethoxylates and bisphenol A
Method Type
GC/MS-SIM, high-
volume injection
GC/MS-SIM, low-
volume injection
Date
Published
May 2007
December
2006
GC/MS-SIM - Selected Ion Monitoring Gas Chromatography/Mass Spectrometry.
Development of the analytical methods used for these five groups: PPCPs,
steroids/hormones, pesticides, PBDEs and APEs are discussed below. Table B-l lists the version
of the method used to analyze samples collected during the Nine POTW Study.
PPCPs
A preliminary laboratory procedure (AXYS Method MLA-052) was used to analyze
samples from Plant A. Plants B, C, and D were analyzed using a more refined laboratory
procedure (AXYS Method MLA-052 ). An EPA method was under development at the Axys
laboratory during the analysis of samples collected at Plants B, C, and D. After single-laboratory
validation and peer review, the method was published as EPA Method 1694 in December 2007
(EPA, 2007b), and samples from Plants E, F, G, H, and I were analyzed using the published
method.
EPA Method 1694 is designed to identify 73 PPCPs in POTW wastes. The 73 target
analytes in EPA Method 1694 are divided into four groups (1 through 4). Each group represents
an LC/MS/MS run. Groups 1, 2, and 3 are extracted under acidic (pH 2) conditions. Groups 1
B-2
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
and 2 are run in the positive electrospray ionization (ESI+) mode, but with differing run profiles.
Group 3 is run in the negative electrospray ionization (ESI-) mode. Group 4 is extracted under
basic pH 10 conditions and run in the ESI+ mode. Quantitation is achieved using isotope dilution
and internal standard techniques.
EPA Method 1694 includes all analytes included in AXYS Method MLA-052 as well as
an additional 33 analytes.
In this report, the PPCP analytes are organized by following groups:
1. Antibiotics (Analytical Group 1 antibiotics and Analytical Group 2):
2. Analytical Group 1, other than antibiotics;
3. Analytical Group 3; and
4. Analytical Group 4.
Steroids and Hormones
AXYS Method MLA-057 Rev 1 (a preliminary laboratory procedure) was used to
analyze samples from Plants A, B, C, and D; the procedure consisted of low resolution gas
chromatography mass spectrometry (GC/MS).
An EPA method was under development at the Axys laboratory during the analysis of
samples collected at Plants A through D, and consisted of gas chromatography combined with
high resolution mass spectrometry. After single-laboratory validation and peer review, the
method was published as EPA Method 1698 (EPA, 2007c) in December 2007. Samples from
Plants E, F, G, H, and I were analyzed using the published method.
EPA Method 1698 is designed to identify 27 steroids and hormones in POTW wastes.
The method requires solvent extraction of the sample, followed by cleanup with a layered
alumina/florisil column. Following cleanup, the target analytes are derivatized and analyzed by
GC/HRMS. Quantitation is achieved with isotope dilution and internal standard techniques.
One analyte included in AXYS Method MLA-057 Rev 1 is not included in EPA Method
1698: alpha-zearalanol, an anabolic agent. EPA Method 1698 includes seven analytes not
included in AXYS Method MLA-057 Rev. 1.
PBDEs
EPA analyzed samples collected during the Nine POTW Study for 8 PBDEs using EPA
Method 1614 which is HRGC/HRMS. Prior to analysis of samples collected at Plants A, B, C,
and D the method utilized a 30-meter GC column that, when heated, was suspected to degrade
several high-molecular-weight congeners such as congener 209. Subsequent to analysis at Plants
A, B, C and D, the method was modified to incorporate a temperature programmable injector
(TPI) and a 15-meter short column to mitigate degradation of PBDE 209. After multi-laboratory
validation and peer review, Method 1614 was revised and published in August 2007. Samples
from Plants E, F, G, H, and I were analyzed using the 2007 version of 1614.
B-3
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
Pesticides
AXYS Method MLA-035 Rev. 04 (a preliminary laboratory procedure) was used to
analyze for pesticides in Plants A, B, C, and D. An EPA method was under development at the
Axys laboratory during the analysis of samples collected at Plants A, B, C, and D. Subsequent to
analysis at Plants A, B, C, and D, organonitrogen pesticides were removed from the method by
EPA because they demonstrated thermal instability and poor response under the conditions used
in EPA Method 1699.
After single-laboratory validation and peer review, EPA published Method 1699 (EPA,
2007d) in December 2007. Samples from Plants E, F, G, H, and I were analyzed using the
published method.
EPA Method 1699 was initially designed to identify 60 pesticides in the following
chemical groups:
• 34 Organochlorine Pesticides;
• 17 Organophosphorus Pesticides;
• 7 Triazine Pesticides; and
• 2 Pyrethroid Pesticides.
Method 1699 requires solvent extraction of the sample, followed by cleanup. After
cleanup, the target analytes are derivatized and analyzed by GC/HRMS. Quantitation is achieved
with isotope dilution and internal standard techniques.
The AXYS Methods MLA-035 Rev. 04 and MLA-037 Rev. 03 analyte lists differed
between Plant A and Plants B, C, and D. AXYS Method MLA-035 Rev. 04 includes 20 analytes
not included in EPA Method 1699. EPA Method 1699 includes two analytes not included in
AXYS Method MLA-035 Rev. 04.
Alkylphenols, APEs, andBPA
EPA analyzed samples for alkylphenols, APEs, and BPA using methods developed by the
EPA Region 5 CRL. Certain samples were also analyzed using ASTM Method D 7065-06.
B-4
-------
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
Appendix C
CECs ANALYTICAL RESULTS
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs August 2009
This appendix presents the results of EPA's analysis of POTW influent and effluent
samples collected during the Nine POTW Study; sludge sampling efforts were dropped after the
first stage because the analytical methods needed more development. Tables C-l through C-10
present the results of sample analysis for the following types of CECs:
PPCPs;
• Sterols and hormones;
• Alkylphenols, APEs, and BPA;
• PBDEs; and
• Pesticides.
EPA developed Methods 1694, 1698, and 1699 to identify a large number and variety of
analytes in three complex matrices, POTW influent, sludge and effluent. It is difficult to
optimize analytical procedures for a large number of diverse analytes. Procedures that are
optimal for one analyte may be less suitable for other analytes. As a result, many of the
analytical results failed to meet method quality control (QC) specifications. For each analyte
family, the percentage of the detected results (i.e., where the concentration was reported above
the laboratory-reported detection limit) with no QC flags or other data interpretation issues were:
PPCPs
Sterols and hormones
Alkylphenols, APEs, and BPA
PBDEs
Pesticides
54 percent (441 detected results)
58 percent (240 detected results)
65 percent (3 1 detected results)
87 percent (156 detected results)
81 percent (238 detected results)
The majority of the sampling results were in one of three categories
1. Results for which an analyte was detected with no QC flags or other quality issues
are reported as a measured concentration.
2. Results for which an analyte was detected with QC flags or other data
interpretation issues are reported as detected (DET) with no numeric
concentration. "DET" indicates that the analytes are present in the samples, but
that the measured concentration was not considered reliable. Results are qualified
because of QC issues including the following:
a. Poor spike recoveries including:
i. Labeled compound recovery (LCR),
ii. Matrix spike (MS) recovery,
iii. Initial precision and recovery (IPR), and
iv. Ongoing precision and recovery (OPR);
v. Continuous calibration verification (CCV);
b. Other matrix interference issues;
c. Calibration issues; and
d. Blank contamination.
C-l
-------
Occurrence of Contaminants of Emerging Concern in Wastewaterfrom Nine POTWs
August 2009
3. Results for which an analyte was not detected at or above the laboratory-reported
quantitation limit are reported as not quantified (NQ) with the laboratory-reported
quantitation limit in parentheses.
Results of analysis of duplicate samples have been averaged for presentation in
Tables C-l through C-10. All results are presented in ng/L (parts per trillion (ppt)). The
following designations and footnotes are used throughout the tables:
NA
NQ()
DET
EXCLUDE
<
a
b
c
Not analyzed.
Not measured above the, laboratory-reported quantitation level with said
level reported in parentheses.
Detected but has associated QC flags
Excluded due to critical QC failure including: no/low recovery in matrix
spikes and other laboratory spikes; matrix-specific effect on LCR; and no
OPR performed.
For duplicate samples, an NQ result was averaged with a quantified result.
Sample result set to NQ due to lab blank contamination (sample result less
than five times the lab blank result). For duplicate samples, one or both
sample results may have been set to NQ. A laboratory-reported detection
limit may or may not have been provided.
For duplicate samples, an NQ result was averaged with a DET result.
Sample result set to NQ due to field blank contamination (sample result
less than five times the field blank result). For duplicate samples, one or
both sample results may have been set to NQ.
C-2
-------
Table C-l. Occurrence of PPCPs in POTW Influent (ng/L)
Analyte
Plant A
Plant B
Plant C
Plant D
Plant E
Plant F
Plant G
Plant H
Plant I
Antibiotics
4-Epianhydrochlortetracycline
(EACTC)
4-Epianhydrotetracycline
(EATC)
4-Epichlortetracycline
(ECTC)
4-Epioxytetracycline (EOTC)
4-Epitetracycline (ETC)
Anhydrochlortetracycline
(ACTC)
Anhydrotetracycline (ATC)
Chlorotetracycline (CTC)
Demeclocycline
Doxycycline
Isochlortetracycline (ICTC)
Minocycline
Oxytetracycline (OTC)
Tetracycline (TC)
Sulfachloropyridazine
Sulfadiazine
Sulfadimethoxine
Sulfamerazine
Sulfamethazine
Sulfamethizole
Sulfamethoxazole
Sulfanilamide
Sulfathiazole
Ciprofloxacin
Clarithromycin
Clinafloxacin
Enrofloxacin
NA
NA
NA
NA
NA
NA
NA
NQa
NA
NQa
NA
NA
NQ(997)
DET
NQ(59.2)
NA
DET
DET
DET
DET
DET
NA
DET
DET
NA
NA
NQa
NA
NA
NA
NA
NA
NA
NA
434
NA
2,970
NA
NA
NQ(169)
NQ(329)
NQ(16.0)
NA
DET
12.5
DET
NQ(3.00)
DET
NA
NQ(6.00)
NQ(300)
NA
NA
NQ(649)
NA
NA
NA
NA
NA
NA
NA
NQa
NA
NQa
NA
NA
NQa
NQa
EXCLUDE
NA
EXCLUDE
EXCLUDE
EXCLUDE
EXCLUDE
EXCLUDE
NA
EXCLUDE
DET
NA
NA
NQ(690)
NA
NA
NA
NA
NA
NA
NA
NQ(684)
NA
2,540
NA
NA
NQ(326)
234
NQ(130)
NA
NQ(24.0)
NQ(65.0)
NQ(26.0)
NQ(24.0)
1,500
NA
NQ(56.0)
NQa
NA
NA
NQ(331)
NQ(519)
NQ(130)
NQ(313)
NQ(51.9)
DET
NQ(462)
NQ(130)
NQ(51.9)
NQ(130)
DET
NQ(51.9)
DET
NQ(51.9)
DET
NQ(13.0)
NQ(13.0)
NQ(26.4)
NQ(5.19)
8.94
NQ(5.50)
DET
NQ(276)
NQ(13.0)
1,440
748
NQ(123)
NQ(26.0)
NQ(472)
NQ(118)
NQ(272)
NQ(104)
DETb
NQ(464)
NQ(118)
NQ(47.2)
NQ(118)
NQ(47.2)
NQ(47.2)
NQ(1,020)
NQ(47.2)
DET
NQ(11.8)
31.1
NQ(9.09)
12.6
NQ(4.72)
NQ(4.72)
DET
NQ(118)
NQ(11.8)
803
384
NQ(47.2)
NQ(23.6)
NQ(2,860)
NQ(1,340)
NQ(194)
NQ(288)
412
NQ(768)
NQ( 1,070)
NQ(77.7)
NQ(194)
724
NQ(77.7)
NQ(3,090)
NQ(77.7)
368
NQ(19.4)
NQ(19.4)
NQ(16.8)
NQ(7.77)
NQ(7.77)
NQ(7.77)
DET
NQ(194)
NQ(19.4)
591
DET
NQ(77.7)
NQ(38.9)
NQ(2,890)
NQ(204)
NQ(204)
NQ(297)
475
NQ(751)
NQ(757)
NQ(81.8)
NQ(204)
341
NQ(81.8)
NQ(3,520)
NQ(81.8)
490
NQ(20.4)
NQ(20.4)
NQ(23.7)
15.3
NQ(79.0)
NQ(8.18)
DET
NQ(204)
212
15,100
DET
NQ(334)
NQ(40.9)
NQ(560)
NQ(140)
NQ(140)
NQ(189)
206
NQ(140)
NQ(140)
NQ(56.0)
NQ(140)
176
NQ(56.0)
NQ(2,270)
NQ(56.0)
231
NQ(14.0)
NQ(14.0)
NQ(IO.O)
NQ(5.60)
NQ(5.60)
NQ(5.60)
2,620
NQ(140)
NQ(14.0)
1,530
292
NQ(244)
NQ(28.0)
O
-------
Table C-l (Continued)
Analyte
Erythromycin
Lomefloxacin
Norfloxacin
Ofloxacin
Roxithromycin
Sarafloxicin
Tylosin
Azithromycin
Carbadox
Cefotaxime
Cloxacillin
Flumequine
Lincomycin
Ormetoprim
Oxacillin
Oxolinic Acid
Penicillin G
Penicillin V
Trimethoprim
Virginiamycin
Plant A
NQa
NA
NQ(33.8)
NA
NQa
NQ(51.2)
NQ(79.7)
NA
NQ(50.0)
NA
NA
NA
DET
NA
NA
NA
NA
NA
DET
DET
Plant B
126
NA
NQ(1,270)
NA
NQ(4.00)
NQ(32.0)
NQ(16.0)
NA
NQ(3.00)
NA
NA
NA
DET
NA
NA
NA
NA
NA
195
NQ(8.00)
Plant C
119
NA
NQ(1,350)
NA
NQ(4.00)
NQa
NQ(18.0)
NA
NQ(4.00)
NA
NA
NA
NQ(89.0)
NA
NA
NA
NA
NA
498
NQ(8.00)
Plant D
DET
NA
NQ(650)
NA
NQ(2.00)
NQ(16.0)
NQ(17.0)
NA
NQ(3.00)
NA
NA
NA
19.1
NA
NA
NA
NA
NA
DET
NQ(8.00)
Plant E
529
NQ(26.0)
NQ(130)
147
NQ(5.50)
NQ(119)
NQ(256)
DET
NQ(59.1)
NQ( 1,240)
DETb
NQ(13.0)
NQ(102)
NQ(5.19)
NQ(54.5)
NQ(21.1)
NQ(26.0)
NQ(109)
DET
DETb
Plant F
586
NQ(23.6)
NQ(353)
505
NQ(2.36)
NQ(403)
NQ(47.2)
DET
NQ(25.7)
NQ(1,150)
NQ(123)
NQ(11.8)
DET
NQ(4.72)
NQ(50.1)
NQ(IO.O)
NQ(23.6)
NQ(47.2)
DET
NQ(332)
Plant G
2,330
NQ(38.9)
NQ(194)
429
NQ(3.89)
NQ(777)
NQ(744)
DET
NQ(19.4)
NQ(786)
NQ(38.9)
NQ(19.4)
DET
NQ(7.77)
NQ(38.9)
NQ(7.77)
NQ(38.9)
DET
DET
NQ(205)
Plant H
280
NQ(40.9)
NQ(204)
3,240
NQ(27.0)
NQ(818)
NQ(2,480)
DET
NQ(180)
NQ(1,600)
NQ(146)
NQ(20.4)
NQ(40.9)
NQ(8.18)
NQ(40.9)
NQ(8.18)
NQ(40.9)
DET
DET
NQ(2,300)
Plant I
202
NQ(28.0)
NQ(140)
DET
NQ(2.80)
NQ(560)
NQ(661)
669
NQ(14.0)
NQ(858)
NQ(28.0)
NQ(14.0)
NQ(28.0)
NQ(5.60)
NQ(28.0)
NQ(5.60)
NQ(28.0)
NQ(56.0)
418
NQ(148)
Analytical Group 1, other than antibiotics
1 ,7-Dimethyl xanthine
Acetaminophen
Caffeine
Carbamazepine
Codeine
Cotinine
Dehy dronifedipine
Digoxigenin
Digoxin
Diltiazem
Diphenhydramine
Fluoxetine
DET
DET
DET
NA
NA
DET
NA
NQa
NQa
DET
NA
DET
DET
DET
DET
NA
NQ(664)
DET
NA
NQ(126)
NQ(1,330)
DET
NA
NQ(15.0)
DET
DET
DET
NA
NQ(706)
DET
NA
NQ(134)
NQ(1,410)
DET
NA
DET
DET
DET
42,100
NA
NQ(904)
2,940
NA
NQ(134)
NQ(1,410)
DET
NA
DET
62,600
79,300
68,200
DET
DET
535
DET
NQ(553)
NQ(757)
DET
DET
24.7
19,400
54,400
52,500
DET
DET
2,820
DET
NQ(431)
NQ(630)
DET
DET
58.7
DET
129,000
DET
DET
DET
NQ(490)
DET
NQ(605)
NQ(194)
DET
NQ(7.77)a
NQ(38.9)
DET
340,000
DET
DET
DET
DET
DET
NQ(516)
NQ(2,530)
DET
NQ(40.9)a
DET
4,860
40,200
13,300
163
345
2,980
NQ(5.60)
NQ(215)
NQ(140)
1,490
1,440
56.1
O
-------
Table C-l (Continued)
Analyte
Miconazole
Norgestimate
Thiabendazole
Plant A
NA
NA
NA
Plant B
NA
NQ(16.0)
NA
Plant C
NA
NQ(17.0)
NA
Plant D
NA
NQ(8.00)
NA
Plant E
DET
NQ(78.8)
NQ(13.0)
Plant F
DETb
NQ(104)
12.4
Plant G
DET
NQ(38.9)
DET
Plant H
DET
NQ(40.9)
DET
Plant I
114
NQ(113)
34.0
Analytical Group 3
Gemfibrozil
Ibuprofen
Naproxen
Triclocarban
Triclosan
Warfarin
DET
DET
NA
NA
NA
NQ(10.6)
DET
DET
NA
NA
NA
DET
DET
7,360
NA
NA
NA
NQ(53.0)
1,370
11,600
NA
NA
NA
DET
539
18,900
11,300
187
996
NQ(13.0)
4,260
16,800
14,800
571
2,420
NQ(11.8)
DET
20,500
DET
4,270
4,110
NQ(19.4)
DET
DET
DET
13,700
12,000
DET
6,630
13,400
18,800
3,100
2,810
DET
Analytical Group 4
Albuterol
Cimetidine
Metformin
Ranitidine
DET
DET
DET
DET
NQ(31.0)
461
NQ(326)
496
NQ(121)
452
EXCLUDE
EXCLUDE
22.5
227
DET
DET
6.40
73.1
17,400
1,610
30.6
330
29,400
551
NQ(24.2)
120
36,500
1,870
75.6
11,700
248,000
16,800
68.9
1,100
11,100
784
1
•a,
i1
I
O
1
§
-------
Table C-2. Occurrence of PPCPs in POTW Effluent (ng/L)
Analyte
Plant A
Plant B
Plant C
Plant D
Plant E
Plant F
Plant G
Plant H
Plant I
Antibiotics
4-Epianhydrochlortetracycline
(EACTC)
4-Epianhydrotetracycline
(EATC)
4-Epichlortetracycline
(ECTC)
4-Epioxytetracycline (EOTC)
4-Epitetracycline (ETC)
Anhydrochlortetracycline
(ACTC)
Anhydrotetracycline (ATC)
Chlorotetracycline (CTC)
Demeclocycline
Doxycycline
Isochlortetracycline (ICTC)
Minocycline
Oxytetracycline (OTC)
Tetracycline (TC)
Sulfachloropyridazine
Sulfadiazine
Sulfadimethoxine
Sulfamerazine
Sulfamethazine
Sulfamethizole
Sulfamethoxazole
Sulfanilamide
Sulfathiazole
Ciprofloxacin
Clarithromycin
Clinafloxacin
Enrofloxacin
NA
NA
NA
NA
NA
NA
NA
NQ(34.4)
NA
NQ(372)a
NA
NA
NQ(460)
NQ(104)
NQ(5.86)
NA
NQ(0.885)
NQ(0.245)
NQ(10.6)
NQ(1.31)
DET
NA
NQ(1.52)
NQa
NA
NA
NQa
NA
NA
NA
NA
NA
NA
NA
<462a
NA
<284a
NA
NA
NQ(160)
568
NQ(14.5)
NA
DET
NQ(7.50)
DETb
NQ(3.00)
DET
NA
NQ(6.00)
NQ(284)
NA
NA
NQ(614)
NA
NA
NA
NA
NA
NA
NA
NQa
NA
NQa
NA
NA
NQa
NQa
EXCLUDE
NA
EXCLUDE
EXCLUDE
EXCLUDE
EXCLUDE
EXCLUDE
NA
EXCLUDE
DET
NA
NA
NQ(627)
NA
NA
NA
NA
NA
NA
NA
NQ(673)
NA
NQ(641)
NA
NA
NQ(320)
NQ(320)
NQ(16.0)
NA
NQ(3.00)
NQ(8.00)
NQ(3.00)
NQ(3.00)
9.54
NA
NQ(7.00)
NQ(301)
NA
NA
NQ(326)
NQ(494)
NQ(124)
NQ(124)
NQ(49.4)
NQ(49.4)
NQ(124)
NQ(124)
NQ(49.4)
NQ(124)
NQ(49.4)
NQ(49.4)
NQ(494)
NQ(49.4)
NQ(49.4)
NQ(12.4)
NQ(12.4)
NQ(2.47)
NQ(4.94)
NQ(4.94)
NQ(4.94)
276
NQ(124)
NQ(12.4)
36.7
89.7
NQ(49.4)
NQ(24.7)
NQ(555)
NQ(342)
NQ(296)
NQ(120)
NQ(206)
NQ(586)
NQ(313)
NQ(55.5)
NQ(139)
NQ(55.5)
NQ(55.5)
NQ(1,940)
NQ(55.5)
NQ(55.5)
NQ(13.9)
<14.2
NQ(2.78)
NQ(5.55)
NQ(5.55)
NQ(5.55)
1,490
NQ(139)
NQ(13.9)
161
23.9
NQ(55.5)
NQ(27.8)
NQ(1,780)
NQ(470)
NQ(125)
NQ(190)
NQ(50.0)
NQ(465)
NQ(510)
NQ(50.0)
NQ(125)
NQ(50.0)
NQ(50.0)
NQ(2,620)
NQ(50.0)
NQ(50.0)
NQ(12.5)
NQ(12.5)
NQ(2.50)
NQ(5.00)
NQ(5.00)
33.5
DET
NQ(125)
NQ(12.5)
NQ(219)
DET
NQ(345)
NQ(IOO)
NQ( 1,800)
NQ(483)
NQ(125)
NQ(49.8)
NQ(168)
NQ(477)
NQ(515)
NQ(169)
NQ(125)
NQ(49.8)
NQ(49.8)
NQ(2,180)
NQ(49.8)
NQ(49.8)
NQ(12.5)
NQ(12.5)
NQ(2.49)
NQ(4.98)
NQ(19.9)
NQ(4.98)
DET
NQ(125)
NQ(12.5)
53.0
NQ(12.5)
NQ(49.8)
NQ(24.9)
NQ(502)
NQ(125)
NQ(125)
NQ(267)
NQ(226)
NQ(125)
NQ(125)
NQ(50.2)
NQ(125)
NQ(50.2)
NQ(50.2)
NQ(2,080)
NQ(50.2)
NQ(50.2)
NQ(12.5)
NQ(12.5)
NQ(2.51)
NQ(5.02)
NQ(5.02)
NQ(5.02)
NQ(5.02)
NQ(125)
NQ(12.5)
NQ(20.0)
NQ(12.5)
NQ(50.2)
NQ(25.1)
O
-------
Table C-2 (Continued)
Analyte
Erythromycin
Lomefloxacin
Norfloxacin
Ofloxacin
Roxithromycin
Sarafloxicin
Tylosin
Azithromycin
Carbadox
Cefotaxime
Cloxacillin
Flumequine
Lincomycin
Ormetoprim
Oxacillin
Oxolinic Acid
Penicillin G
Penicillin V
Trimethoprim
Virginiamycin
Plant A
NQ(4.99)a
NA
NQ(1.21)
NA
NQ(0.203)a
NQ(9.80)
45.1
NA
NQ(13.5)
NA
NA
NA
DET
NA
NA
NA
NA
NA
NQ(1.14)
NQ(l.ll)
Plant B
114
NA
NQ(1,210)
NA
NQ(4.00)
NQ(31.0)
NQ(15.5)
NA
NQ(3.00)
NA
NA
NA
NQ(22.0)
NA
NA
NA
NA
NA
NQ(15.0)
NQ(7.50)
Plant C
115
NA
NQ( 1,230)
NA
NQ(4.00)
NQa
NQ(16.0)
NA
NQ(3.00)
NA
NA
NA
NQ(91.5)
NA
NA
NA
NA
NA
385
NQ(8.00)
Plant D
NQ(9.00)
NA
NQ(640)
NA
NQ(2.00)
NQ(16.0)
NQ(17.0)
NA
NQ(3.00)
NA
NA
NA
NQ(ll.O)
NA
NA
NA
NA
NA
NQ(16.0)
NQ(8.00)
Plant E
167
NQ(24.7)
NQ(124)
NQ(12.4)
NQ(2.47)
NQ(113)
NQ(49.4)
DET
NQ(12.4)
DETb
NQ(93.9)
NQ(12.4)
NQ(24.7)
NQ(4.94)
NQ(24.7)
NQ(10.6)
NQ(24.7)
NQ(49.4)
NQ(41.1)
NQ(109)
Plant F
91.8
NQ(27.8)
NQ(139)
162
NQ(2.78)
NQ(290)
NQ(55.5)
DET
NQ(13.9)
NQ(846)
NQ(IOO)
NQ(13.9)
DET
NQ(5.55)
NQ(27.8)
NQ(5.55)
NQ(27.8)
NQ(55.5)
DET
NQ(187)
Plant G
418
NQ(25.0)
NQ(1,170)
NQ(12.5)
NQ(2.50)
NQ( 1,060)
NQ(307)
NQ(12.5)
NQ(12.5)
NQ(361)
NQ(25.0)
NQ(12.5)
NQ(25.0)
NQ(5.00)
NQ(25.0)
NQ(5.00)
NQ(25.0)
NQ(50.0)
293
NQ(25.0)
Plant H
NQ(2.49)
NQ(24.9)
NQ(125)
NQ(12.5)
NQ(2.49)
NQ(498)
NQ(317)
NQ(12.5)
NQ(12.5)
NQ(450)
NQ(24.9)
NQ(12.5)
NQ(24.9)
NQ(4.98)
NQ(24.9)
NQ(4.98)
NQ(24.9)
NQ(49.8)
NQ(12.5)
NQ(85.4)
Plant I
NQ(2.51)
NQ(25.1)
NQ(125)
NQ(12.5)
NQ(2.51)
NQ(502)
NQ(50.2)
NQ(12.5)
NQ(12.5)
NQ(698)
NQ(25.1)
NQ(12.5)
NQ(25.1)
NQ(5.02)
NQ(25.1)
NQ(5.02)
NQ(25.1)
NQ(50.2)
NQ(12.5)
NQ(25.1)
Analytical Group 1, other than antibiotics
1 ,7-Dimethyl xanthine
Acetaminophen
Caffeine
Carbamazepine
Codeine
Cotinine
Dehy dronifedipine
Digoxigenin
Digoxin
Diltiazem
Diphenhydramine
Fluoxetine
NQ(13.1)
NQ(27.3)
NQ(79.4)
NA
NA
NQ(1.41)
NA
NQ( 1,080)
NQa
DET
NA
NQ(4.26)
NQ(1,320)
NQ(32.5)
NQ(303)
NA
NQ(628)
DET
NA
NQ(120)
NQ( 1,260)
NQ(2.00)
NA
DETb
DETb
NQ(129)
NQ(309)
NA
NQ(642)
NQ(722)
NA
NQ(122)
NQ( 1,280)
DET
NA
DET
NQ(700)
NQ(343)
NQ(322)
NA
NQ(890)
NQ(72.0)
NA
NQ(132)
NQ(1,390)
NQ(2.00)
NA
NQ(8.00)
NQ( 1,240)
NQ(494)
NQ(124)
DET
NQ(24.7)
46.0
NQ(4.94)
NQ(186)
NQ(124)
DET
DET
14.7
NQ(1,390)
NQ(555)
NQ(139)
DET
DET
NQ(127)
DET
NQ(406)
NQ(139)
DET
DET
24.7
NQ(1,250)
NQ(500)
NQc
598
NQ(25.0)
NQ(83.7)
NQ(5.00)
NQ(50.0)
NQ(125)
NQ(5.00)
NQ(5.00)a
NQ(25.0)
NQ(1,250)
NQ(498)
NQc
487
NQ(24.9)
NQ(61.5)
44.7
NQ(49.8)
NQ(125)
NQ(4.98)
NQ(4.98)a
DET
NQ( 1,250)
NQ(502)
NQ(125)
NQ(12.5)
NQ(25.1)
20.7
16.5
NQ(50.2)
NQ(125)
NQ(5.02)
NQ(5.02)
NQ(25.1)
O
-------
Table C-2 (Continued)
Analyte
Miconazole
Norgestimate
Thiabendazole
Plant A
NA
NA
NA
Plant B
NA
NQ(15.0)
NA
Plant C
NA
NQ(15.0)
NA
Plant D
NA
NQ(8.00)
NA
Plant E
NQ(12.4)
NQ(98.0)
<12.8
Plant F
NQ(13.9)
NQ(104)
19.8
Plant G
NQ(12.5)
NQ(25.0)
DET
Plant H
NQ(12.5)
NQ(24.9)
DET
Plant I
NQ(12.5)
NQ(91.2)
NQ(12.5)
Analytical Group 3
Gemfibrozil
Ibuprofen
Naproxen
Triclocarban
Triclosan
Warfarin
DET
NQ(34.6)
NA
NA
NA
NQ(0.797)
DET
NQ(87.0)
NA
NA
NA
NQ(l.OO)
DET
NQ(690)
NA
NA
NA
NQ(6.00)
NQ(35.0)
NQ(358)
NA
NA
NA
NQ(7.00)
18.9
NQ(124)
75.3
154
NQ(494)
NQ(12.4)
259
NQ(139)
NQ(27.8)
45.4
NQ(555)
NQ(13.9)
DET
NQ(125)
NQ(25.0)
40.6
NQ(500)
NQ(12.5)
DET
NQ(125)
NQ(24.9)
76.4
NQ(498)
NQ(12.5)
NQ(12.5)
NQ(125)
NQ(25.1)
NQ(25.1)
NQ(502)
NQ(12.5)
Analytical Group 4
Albuterol
Cimetidine
Metformin
Ranitidine
DET
NQ(0.0453)
DET
NQa
NQ(30.0)
NQ(41.0)
DET
NQ(7.00)
NQ(125)
374
EXCLUDE
EXCLUDE
NQ(31.0)
NQ(21.0)
DET
NQ(8.00)
NQ(2.83)
NQ(5.66)
5,420
NQ(5.66)
DET
DET
1,250
DET
NQ(5.01)
NQ(5.01)
3,650
7.22
NQ(4.92)
NQ(4.92)
826
NQ(4.92)
NQ(5.03)
NQ(5.03)
NQ(252)
NQ(5.03)
1
•a,
i1
I
O
I
oo
1
§
-------
Table C-3. Occurrence of Sterols and Hormones in POTW Influent (ng/L)
Analyte
Plant A
Plant B
Plant C
Plant D
Plant E
Plant F
Plant G
Plant H
Plant I
Sterols
Beta Sitosterol
Beta Stigmastanol
Campesterol
Cholestanol
Cholesterol
Coprostanol
Desmosterol
Epicoprostanol
Ergosterol
Stigmasterol
DET
NA
NA
DET
DET
DET
DET
DET
DET
DET
271,000
NA
NA
39,700
636,000
496,000
2,320
20,100
DET
17,400
DET
NA
NA
18,400
590,000
470,000
1,330
9,370
NQ(5,230)
14,800
239,000
NA
NA
35,800
745,000
366,000
1,370
19,900
EXCLUDE
14,900
DET
34,000
DET
DET
DET
DET
2,870
5,780
4,490
DET
DET
27,300
46,600
45,700
DET
DET
2,210
21,400
2,820
37,200
DET
DET
DET
DET
DET
DET
DET
DET
DET
DET
DET
DET
DET
DET
DET
DET
7,030
DET
DET
DET
DET
46,000
DET
DET
DET
DET
11,100
DET
DET
DET
Hormones
17 Alpha Estradiol
17 Alpha Ethinyl
Estradiol
17 Alpha-Dihydroequilin
17 Beta Estradiol
Alpha-Zearalanol
Androstenedione
Androsterone
Beta Estradiol 3-
Benzoate
Desogestrel
Equilenin
Equilin
Estriol
Estrone
Mestranol
Norethindrone
DET
NQ(351)
DET
DET
NQ(347)
NA
NA
DET
NQ(3,510)
NA
NQ(150)
NA
DET
NQ(417)
<810
NQ(253)
NQ(253)
NQ(285)
NQ(283)
DET
NA
NA
NQ(263)
NA
NA
NQ(251)
NA
NQ(256)
NQ(266)
DET
NQ(256)
NQ(256)
NQ(289)
NQ(286)
DET
NA
NA
NQ(266)
NA
NA
NQ(254)
NA
NQ(259)
DET
NQ(80.5)
NQ(314)
NQ(628)
NQ(354)
NQ(351)
NQ(317)
NA
NA
NQ(653)
NA
NA
NQ(311)
NA
NQ(317)
NQ(329)
NQ(396)
NQ(10.9)
NQ(13.0)
DETb
NQ(10.9)
NA
510
DET
DET
NQ(75.0)
NQ(5.22)
<12.7
DET
DET
NQ(48.9)
NQ(11.2)
NQ(10.9)
NQ(13.0)
NQ(59.3)
NQ(10.9)
NA
380
DET
DET
NQ(71.5)
NQ(5.24)
NQ(10.7)
DET
54.1
NQ(12.3)
DETb
DET
NQ(5.07)a
NQ(33.2)
DET
NA
864
2,910
NQ(5.07)
NQ(91.1)
NQ(5.07)
NQ(17.2)
212
63.3
NQ(5.07)
NQ(5.07)
NQ(11.9)
NQ(11.9)
NQ(75.1)
DET
NA
NQ(378)
661
NQ(11.9)
NQ(125)
NQ(11.9)
28.9
1,000
98.9
NQ(11.9)
NQ(125)
NQ(44.4)
NQ(3.93)a
NQ(91.0)
NQ(38.9)
NA
NQ( 1,640)
DET
NQ(3.93)
NQ(459)
NQ(13.6)
NQ(lOl)
DET
NQ(89.2)
NQ(3.93)
NQ(28.3)
O
-------
Table C-3 (Continued)
Analyte
Norgestrel
Progesterone
Testosterone
Plant A
NQ(509)
NA
DET
Plant B
DET
NA
DET
Plant C
DET
NA
DET
Plant D
NQ(395)
NA
NQ(659)
Plant E
NQ(606)
NQ(212)
917
Plant F
NQ(21.8)
118
831
Plant G
NQ(36.3)
NQ(191)
DET
Plant H
NQ(95.2)
NQ(489)
DET
Plant I
NQ(62.1)
NQ(349)
2,650
1
•a,
i1
I
Note - To analyze influent samples, EPA's contract laboratory split the sample extract into two portions for analysis of sterols and hormones. The contract
laboratory used a small portion for sterol analysis and the remaining portion for hormone analysis. The extract is split in this manner to accommodate the
anticipated high sterol levels in samples and preserve the laboratory-reported detection limits of the hormone analyses. The laboratory did not split the effluent
samples in this manner because sterols concentrations were anticipated to be much lower in treated effluent.
1
O
i
o
§
-------
Table C-4. Occurrence of Sterols and Hormones in POTW Effluent (ng/L)
Analyte
Plant A
Plant B
Plant C
Plant D
Plant E
Plant F
Plant G
Plant H
Plant I
Sterols
Beta Sitosterol
Beta Stigmastanol
Campesterol
Cholestanol
Cholesterol
Coprostanol
Desmosterol
Epicoprostanol
Ergosterol
Stigmasterol
NQ(636)a
NA
NA
72.1
NQ(916)a
163
DET
NQ(6.84)
DET
DET
NQa
NA
NA
155
2,220
699
<190
NQ(252)
DET
1,300
DET
NA
NA
486
15,800
DET
1,160
<195
DET
406
375
NA
NA
NQ(641)
458
NQ(695)
NQ(594)
NQ(300)
EXCLUDE
414
<988c
117
148
524
2,080
758
41.7
38.5
NQ(30.9)
<401c
<663c
NQ(16.6)
37.6
40.6
DET
114
NQ(31.2)
8.55
NQ(30.5)
<287c
NQ(9.64)a
NQ(9.64)a
NQ(16.1)a
123
DET
1,320
NQ(32.1)
DET
DET
NQ(3.21)a
NQ(9.60)a
NQ(9.60) a
NQ(16.0)a
197
NQ(16.0)a
111
NQ(32.0)
4.41
NQ(80.0)
NQ(3.20)a
NQ(5.77)a
19.6
NQ(9.62)
NQ(9.62) a
NQ(9.62)a
103
NQ(19.2)
49.4
NQ(48.1)
NQ(9.05)a
Hormones
17 Alpha Estradiol
17 Alpha Ethinyl Estradiol
17 Alpha-Dihydroequilin
17 Beta Estradiol
Alpha-Zearalanol
Androstenedione
Androsterone
Beta Estradiol 3-Benzoate
Desogestrel
Equilenin
Equilin
Estriol
Estrone
Mestranol
Norethindrone
NQ(2.08)
NQ(3.95)
NQ(7.99)
NQ(1.55)
NQ(6.83)
NA
NA
NQ(1.63)
NQ(44.5)
NA
NQ(7.85)
NA
NQ(1.18)
NQ(1.77)
NQ(13.7)
NQ(257)
NQ(257)
NQ(289)
NQ(287)
NQ(259)
NA
NA
NQ(267)
NA
NA
NQ(254)
NA
NQ(259)
NQ(269)
NQ(80.6)
NQ(300)
NQ(300)
NQ(337)
NQ(334)
NQ(303)
NA
NA
NQ(311)
NA
NA
NQ(297)
NA
NQ(303)
NQ(314)
NQ(94.0)
NQ(306)
NQ(612)
NQ(344)
NQ(341)
NQ(309)
NA
NA
NQ(635)
NA
NA
NQ(303)
NA
NQ(309)
NQ(321)
NQ(386)
NQ(5.89)
NQ(7.03)
NQ(19.8)
NQ(5.89)
NA
NQ(31.8)
NQ(6.44)
NQ(6.01)
NQ(6.58)
NQ(2.84)
NQ(5.78)
NQ(19.0)
NQ(6.58)
NQ(6.63)
NQ(6.12)
NQ(5.82)
NQ(6.94)
NQ(20.8)
NQ(5.82)
NA
NQ(31.3)
NQ(6.35)
NQ(5.93)
NQ(16.0)
NQ(2.80)
NQ(5.71)
NQ(14.4)
NQ(6.49)
NQ(6.55)
NQ(6.05)
NQ(3.21)
NQ(3.21)a
NQ(11.4)
NQ(3.21)a
NA
NQ(64.1)
NQ(14.1)
NQ(3.21)
NQ(16.7)
NQ(3.21)
NQ(3.21)
NQ(33.1)
NQ(3.21)a
NQ(3.21)
NQ(3.21)
NQ(3.20)
NQ(3.20)a
NQ(3.20)
NQ(3.20)a
NA
NQ(97.1)
NQ(23.3)
NQ(3.20)
NQ(20.9)
NQ(3.20)
NQ(3.20)
NQ(21.9)
NQ(3.20)
NQ(3.20)
NQ(3.20)
NQ(1.92)
NQ(1.92)
NQ(8.96)
NQ(1.92)
NA
NQ(95.3)
NQ(11.3)
NQ(11.9)
NQ(12.7)
NQ(1.92)
NQ(11.8)
NQ(1.92)
NQ(14.2)
NQ(1.92)
NQ(7.55)
-------
Table C-4 (Continued)
Analyte
Norgestrel
Progesterone
Testosterone
Plant A
NQ(7.65)
NA
NQ(8.80)a
Plant B
NQ(80.6)
NA
NQ(269)
Plant C
NQ(94.0)
NA
NQ(314)
Plant D
NQ(384)
NA
NQ(641)
Plant E
NQ(11.6)
NQ(86.0)
NQ(33.3)
Plant F
NQ(11.4)
NQ(29.8)
NQ(47.8)
Plant G
NQ(6.43)
NQ(71.1)
NQ(36.5)
Plant H
NQ(6.40)
NQ(16.0)
NQ(70.0)
Plant I
NQ(30.4)
NQ(99.6)
NQ(40.1)
1
•a,
i1
I
Note - To analyze influent samples, EPA's contract laboratory split the sample extract into two portions for analysis of sterols and hormones. The contract
laboratory used a small portion for sterol analysis and the remaining portion for hormone analysis. The extract is split in this manner to accommodate the
anticipated high sterol levels in samples and preserve the laboratory-reported detection limits of the hormone analyses. The laboratory did not split the effluent
samples in this manner because sterols concentrations are anticipated to be much lower in treated effluent.
1
O
i
to
§
-------
Table C-5. Occurrence of Alkylphenols, APEs, and BPA in POTW Influent (ng/L)
Analyte
BPA
NP2EO
NP1EO
OP
NP
Plant A
NQ(5,000)
NQ(100,000)
NQ(50,000)
NQ(5,000)
39,700
Plant B
EXCLUDE
NQ(53,000)
NQ(19,000)
NQ(2,000)
79,000
Plant C
NQ(610)
DET
DET
NQ(400)
44,000
Plant D
NQ(1,200)
200,000
100,000
13,000
78,000
Plant E
EXCLUDE
NQ( 1,900)
NQ( 1,250)
DET
DET
Plant F
EXCLUDE
NQ(1,950)
NQ(1,300)
DET
DET
Plant G
NQ(330)
NQ(2,000)
NQ(1,300)
NQ(220)
5,700
Plant H
NQ(340)
NQ(2,000)
NQ(1,400)
NQ(230)
24,000
Plant I
NQ(320)
NQ( 1,900)
NQ(1,300)
3,500
63,000
1
•a,
i1
I
Table C-6. Occurrence of Alkylphenols, APEs, and BPA in POTW Effluent (ng/L)
Analyte
BPA
NP2EO
NP1EO
OP
NP
Plant A
EXCLUDE
EXCLUDE
NQ( 1,000)
NQ(IOO)
NQ(500)
Plant B
EXCLUDE
NQ( 1,100)
1,100
NQ(40.0)
NQ(250)
Plant C
NQ(350)
NQ(2,100)
NQ( 1,400)
NQ(230)
NQ( 1,050)
Plant D
NQ(380)
NQ(2,200)
NQ(1,500)
NQ(250)
NQ(1,100)
Plant E
NQ(IOO)
NQ(1,100)
NQ(370)
NQ(40.0)
NQ(250)
Plant F
NQ(IOO)
NQ(1,100)
NQ(370)
NQ(40.0)
<520C
Plant G
NQC
NQ(1,100)
NQ(370)
NQ(40.0)
NQ(250)
Plant H
NQC
NQ(1,100)
NQ(370)
NQ(40.0)
NQ(250)
Plant I
NQ(300)
NQ( 1,800)
NQ( 1,200)
NQ(200)
NQ(900)
1
§
o
-------
Table C-7. Occurrence of PBDEs in POTW Influent (ng/L)
Analyte
PBDE-28+PBDE-33
PBDE-47
PBDE-99
PBDE-100
PBDE-153
PBDE-154
PBDE-183
PBDE-209
Plant A
0.683
DET
DET
8.41
DET
2.54
0.746
EXCLUDE
Plant B
2.17
97.1
91.1
20.7
10.6
8.81
1.52
211
Plant C
1.33
78.1
71.3
16.6
7.24
6.08
1.11
256
Plant D
1.78
103
96.2
23.1
10.4
8.46
2.16
225
Plant E
1.11
DET
46.6
10.2
DET
DET
1.45
260
Plant F
1.48
DET
90.5
19.3
DET
DET
1.55
241
Plant G
0.710
34.0
18.7
4.26
1.57
DET
0.485
149
Plant H
4.08
200
155
35.8
15.8
11.8
2.08
119
Plant I
2.96
151
148
33.1
14.6
11.9
1.31
142
1
•a,
i1
I
1
O
Table C-8. Occurrence of PBDEs in POTW Effluent (ng/L)
Analyte
PBDE-28+PBDE-33
PBDE-47
PBDE-99
PBDE-100
PBDE-153
PBDE-154
PBDE-183
PBDE-209
Plant A
NQ(0.0538)
NQa
NQa
NQ(0.0538)
NQ(0.0538)
NQ(0.0538)
NQ(0.108)
NQ(2.15)
Plant B
0.0652
1.64
1.31
0.265
0.138
0.111
NQ(0.118)
NQ(2.36)
Plant C
0.0897
3.37
3.01
0.676
0.297
0.241
NQ(0.125)
DETb
Plant D
NQ(0.0593)
0.967
0.781
0.199
0.0810
0.0743
NQ(0.118)
NQ(2.37)a
Plant E
0.0574
DET
1.01
0.221
0.0763
0.0649
0.0506
NQ(7.65) a
Plant F
0.0904
0.954
0.456
0.131
DET
0.0332
0.0705
<12.0a
Plant G
NQ(0.153)
1.49
0.787
0.180
NQ(0.153)
NQ(0.153)
NQ(0.305)
NQ(6.10)
Plant H
NQ(0.140)
1.31
0.527
NQ(0.140)
NQ(0.140)
NQ(0.140)
NQ(0.280)
NQ(5.61)
Plant I
NQ(0.141)
1.98
1.63
0.347
0.142
NQ(0.141)
NQ(0.281)
DET
§
-------
Table C-9. Occurrence of Pesticides in POTW Influent (ng/L)
Analyte
Plant A
Plant B
Plant C
Plant D
Plant E
Plant F
Plant G
Plant H
Plant I
Organochlorine
2,4'-DDD
2,4'-DDE
2,4'-DDT
4,4'-DDD
4,4'-DDE
4,4'-DDT
Aldrin
Alpha-BHC
Alpha-chlordane
Beta-BHC
Captan
Chlorothalonil
Cis-Nonachlor
Dacthal
Delta-BHC
Dieldrin
Endosulfan I
Endosulfan II
Endosulfan sulfate
Endrin
Endrin Ketone
Gamma-BHC
Gamma-chlordane
Heptachlor
Heptachlor Epoxide
Hexachlorobenzene
Methoxychlor
Mirex
DET
NQ(1.07)
NQ(1.29)
DET
DET
DET
O.293
0.640
<5.06
<0.494
EXCLUDE
EXCLUDE
<0.625
NQ(0.200)
NQ(0.474)
DET
DET
NQa
NQ(1.20)
NQ(0.518)
NQ(1.14)
1.45
DET
DET
<0.463
EXCLUDE
NQ(3.59)
NQ(0.183)
1.83
NQ(3.43)
NQ(3.43)
2.66
2.35
NQ(7.63)
NQ(6.87)
NQ(6.87)
1.89
NQ(6.87)
NQ(21.5)
1.04
0.307
NQ(2.15)
NQ(6.87)
1.44
NQ(3.43)
NQa
NQ(3.43)
NQ(3.43)
NQ(3.43)
7.14
2.60
NQ(3.43)
0.291
0.425
NQ(6.87)
NQ(3.43)
NQ(6.30)
NQ(6.30)
1.00
NQ(6.30)
4.00
2.00
NQ(6.30)
NQ(6.30)
DET
NQ(6.30)
EXCLUDE
NQ(3.94)
NQ(3.15)
NQ(1.97)
NQ(6.30)
1.00
NQa
NQa
NQ(3.15)
NQ(O.OO)
NQ(3.15)
1.00
1.00
NQ(3.15)
NQ(O.OO)
NQ(O.OO)
DET
NQ(3.15)
NQ(6.32)
NQ(3.16)
NQ(3.16)
NQ(6.32)
3.01
NQ(3.16)
NQ(31.6)
NQ(6.32)
12.3
NQ(6.32)
NQ(39.5)
NQ(7.90)
DET
NQ(3.95)
NQ(31.6)
3.08
NQa
NQ(31.6)
NQ(31.6)
NQ(3.16)
NQ(12.6)
1.95
16.3
NQ(6.32)
1.46
1.37
NQ(15.8)
NQ(63.2)
NQ(1.44)
NQ(1.44)
NQ(1.44)
NQ(1.44)
<1.50
NQ(1.44)
NQ(4.05)
NQ(2.89)
<1.76
NQ(2.89)
EXCLUDE
EXCLUDE
NQ(1.44)
NQ(0.900)
NQ(2.89)
NQ(1.44)
NQ(4.50)
NQ(4.50)
NQ(1.80)
NQ(1.44)
NQ(1.80)
NQ(2.89)
<2.26
NQ(1.44)
NQ(1.80)
NQ(1.80)
NQ(14.4)
NQ(4.50)
NQ(1.40)
NQ(1.40)
NQ(1.40)
NQ(1.40)
2.06
NQ(1.40)
NQ(3.93)
NQ(2.79)
3.53
NQ(2.79)
EXCLUDE
EXCLUDE
NQ(1.40)
NQ(0.873)
NQ(2.79)
6.98
NQ(4.36)
NQ(4.36)
NQ(1.74)
NQ(1.40)
NQ(1.74)
NQ(2.79)
6.61
NQ(1.40)
NQ(1.74)
NQ(1.74)
NQ(9.44)
NQ(4.36)
NQ(1.44)
NQ(1.44)
NQ(1.44)
NQ(1.44)
NQ(1.44)
NQ(1.44)
NQ(4.32)
NQ(2.88)
NQ(1.44)
NQ(2.88)
NQ(24.0)
NQ(4.80)
NQ(1.44)
NQ(0.959)
NQ(2.88)
3.61
NQ(4.80)
NQ(4.80)
NQ(1.92)
NQ(1.44)
NQ(1.92)
NQ(2.88)
NQ(2.40)
NQ(1.44)
NQ(1.92)
NQ(1.92)
NQ(8.33)
NQ(4.80)
NQ(1.38)
NQ(1.38)
NQ(1.38)
NQ(1.38)
4.58
NQ(1.38)
NQ(4.13)
NQ(2.75)
4.32
NQ(2.75)
NQ(22.9)
NQ(4.59)
NQ(1.38)
NQ(2.29)
NQ(2.75)
1.96
NQ(4.59)
NQ(4.59)
NQ(1.83)
NQ(1.38)
NQ(1.83)
NQ(2.75)
6.99
NQ(3.44)
NQ(1.83)
NQ(1.83)
NQ(23.4)
NQ(4.59)
NQ(1.24)
NQ(1.24)
NQ(1.24)
NQ(1.24)
2.76
NQ(1.24)
NQ(3.73)
NQ(2.49)
6.64
NQ(2.49)
NQ(20.7)
NQ(4.15)
NQ(1.24)
NQ(0.830)
NQ(2.49)
7.09
NQ(4.15)
NQ(4.15)
NQ(1.66)
NQ(1.24)
NQ(1.66)
NQ(2.49)
11.8
NQ(1.24)
1.91
NQ(1.66)
NQ(9.05)
NQ(4.15)
1
•a,
i1
I
3
d
I
§
O
o
-------
Table C-9 (Continued)
Analyte
Octachlorostyrene
Oxychlordane
Pentochloronitrobenzene
Perthane
Tecnazene
Trans-Nonachlor
Plant A
NQ(0.272)
NQ(0.630)
NQ(0.363)
NQ(20.4)
NQ(0.333)
<3.46
Plant B
NQ(1.20)
NQ(6.87)
NQ(17.2)
NQ(34.3)
NQ(8.58)
1.50
Plant C
NQ(l.lO)
NQ(6.30)
NQ(7.87)
DET
NQ(7.87)
1.00
Plant D
NQ(ll.l)
NQ(6.32)
NQ(79.0)
NQ(126)
NQ(39.5)
7.86
Plant E
NQ(1.80)
NQ(2.89)
NQ(3.61)
DET
NQ(3.60)
NQ(1.80)
Plant F
NQ(1.74)
NQ(2.79)
NQ(3.49)
30.4
NQ(3.49)
2.01
Plant G
NQ(1.92)
NQ(2.88)
NQ(3.84)
NQ(84.2)
NQ(3.84)
NQ(1.92)
Plant H
NQ(1.83)
NQ(2.75)
NQ(3.67)
NQ(66.0)
NQ(3.67)
2.96
Plant I
NQ(1.66)
NQ(2.49)
NQ(3.32)
NQ(79.2)
NQ(3.32)
4.66
Organophosphorus
Azinphos-methyl
Chlorpyriphos
Chlorpyriphos-oxon
Diazinon
Diazinon oxon
Disulfoton
Disulfoton sulfone
Ethyl-parathion
Fenitrothion
Fonofos
Malathion
Methamidophos
Methyl-chlorpyriphos
Methyl-parathion
Phorate
Phosmet
Pirimiphos-methyl
NQ(38.8)
DET
NQ(2.07)
NQ(4.67)
NQ(1.63)
NQ(26.2)
NQ(0.699)
NQ(7.66)
NQ(3.46)
NQ(1.26)
NQ(70.7)
NQ(62.3)
DET
NQ(38.3)
NQ(5.40)
NQ(8.36)
NQ(0.736)
NQ(10.7)
19.3
NQ(8.58)
8.89
NQ(8.58)
NQ(42.5)
NQ(0.687)
NQ(8.58)
NQ(8.58)
NQ(8.58)
NQ(114)
NQ(60.3)
NQ(10.7)
NQ(25.8)
NQ(17.2)
NQ(21.5)
NQ(8.58)
NQ(19.7)
17.0
NQ(7.87)
DET
NQ(7.87)
NQ(39.0)
NQ(0.630)
NQ(7.87)
NQ(7.87)
NQ(7.87)
NQ(104)
NQ(15.7)
NQ(9.84)
NQ(23.6)
NQ(15.7)
NQ(39.4)
NQ(7.87)
NQ(98.7)
NQ(79.0)
DET
41.0
NQ(158)
NQ(78.2)
DET
NQ(15.8)
NQ(31.6)
NQ(39.5)
DET
DET
NQ(19.7)
94.6
NQ(31.6)
NQ(79.0)
NQ(15.8)
NQ(35.6)
NQ(3.61)
NQ(3.61)
NQ(3.61)
NQ(3.60)
NQ(18.0)
NQ(1.35)
NQ(3.60)
NQ(3.61)
NQ(3.61)
NQ(46.8)
NQ(45.0)
NQ(4.68)
NQ(10.8)
NQ(9.00)
NQ(21.6)
NQ(3.61)
NQ(8.72)
13.0
NQ(3.49)
71.9
NQ(3.49)
NQ(17.5)
NQ(1.31)
NQ(3.49)
NQ(3.49)
NQ(3.49)
NQ(45.4)
NQ(65.2)
NQ(4.54)
NQ(10.5)
NQ(8.72)
NQ(8.73)
NQ(3.49)
NQ(9.59)
NQ(3.84)
NQ(3.84)
NQ(3.84)
NQ(3.84)
NQ(19.2)
NQ(1.44)
NQ(3.84)
NQ(3.84)
NQ(3.84)
NQ(48.0)
NQ(48.0)
NQ(4.80)
NQ(9.59)
NQ(9.59)
NQ(9.59)
NQ(3.84)
NQ(54.6)
262
NQ(3.67)
6.31
NQ(3.67)
NQ(18.3)
NQ(1.38)
NQ(3.67)
NQ(3.67)
NQ(3.67)
NQ(45.9)
NQ(45.9)
NQ(4.59)
NQ(9.17)
NQ(9.17)
NQ(9.17)
NQ(3.67)
NQ(8.30)
64.9
NQ(3.32)
20.9
NQ(3.32)
NQ(16.6)
NQ(1.24)
NQ(3.32)
NQ(3.32)
NQ(3.32)
474
NQ(41.5)
NQ(4.15)
NQ(8.30)
NQ(8.30)
NQ(8.30)
NQ(3.32)
Pyrethroid
Cis-Permethrin
Cypermethrins
Permethrin
Trans-Permethrin
NA
<23.2
DET
NA
NA
26.4
146
NA
NA
52.0
176
NA
NA
70.5
349
NA
25.3
NQ(9.00)
59.0
33.8
155
DET
DET
238
NQ(9.59)
NQ(9.59)
NQ(19.1)
9.26
44.5
DET
104
59.3
306
66.8
689
383
O
-------
Table C-9 (Continued)
Analyte
Plant A
Plant B
Plant C
Plant D
Plant E
Plant F
Plant G
Plant H
Plant I
Triazine
Ametryn
Atrazine
Cyanazine
Desethyl atrazine
Hexazinone
Metribuzin
Simazine
NQ(1.85)
DET
NQ(ll.l)
DET
NQ(6.16)
NQ(3.43)
DET
NQ(8.58)
87.7
NQ(8.58)
27.3
NQ(10.7)
NQ(2.15)
2.67
NQ(7.87)
DET
NQ(7.87)
31.0
NQ(19.7)
NQ(1.97)
DET
NQ(15.8)
DET
NQ(31.6)
4.96
NQ(79.0)
NQ(7.90)
NQ(15.8)
NQ(3.61)
35.9
NQ(15.7)
58.0
NQ(4.68)
NQ(2.70)
6.65
NQ(3.49)
58.9
NQ(17.4)
7.84
7.13
NQ(2.62)
NQ(3.49)
NQ(3.84)
DET
NQ(3.84)
2.65
NQ(4.80)
NQ(2.88)
NQ(3.84)
NQ(3.67)
NQ(13.2)
NQ(3.67)
NQ(1.83)
NQ(11.5)
NQ(2.75)
NQ(9.17)
NQ(3.32)
37.0
NQ(ll.l)
6.11
NQ(4.15)
NQ(2.49)
NQ(3.32)
1
•a,
i1
I
1
o
§
-------
Table C-W. Occurrence of Pesticides in POTW Effluent (ng/L)
Analyte
Plant A
Plant B
Plant C
Plant D
Plant E
Plant F
Plant G
Plant H
Plant I
Organochlorine
2,4'-DDD
2,4'-DDE
2,4'-DDT
4,4'-DDD
4,4'-DDE
4,4'-DDT
Aldrin
Alpha-BHC
Alpha-chlordane
Beta-BHC
Captan
Chlorothalonil
Cis-Nonachlor
Dacthal
Delta-BHC
Dieldrin
Endosulfan I
Endosulfan II
Endosulfan sulfate
Endrin
Endrin Ketone
Gamma-BHC
Gamma-chlordane
Heptachlor
Heptachlor Epoxide
Hexachlorobenzene
Methoxychlor
Mirex
NQ(0.404)
NQ(0.575)
NQ(0.452)
NQ(0.220)
NQ(0.743)
NQ(0.468)
NQ(0.115)
NQ(0.154)
NQ(0.174)
NQ(0.213)
NQ(9.46)
NQ(0.0867)
NQ(0.216)
NQ(0.0867)
NQ(0.233)
NQ(0.102)
2.06
NQ(0.429) a
2.86
NQ(0.229)
NQ(0.369)
NQ(0.244)
NQ(0.186)
NQ(0.0347)
NQ(0.143)
EXCLUDE
DET
NQ(0.0657)
NQ(3.55)
NQ(3.55)
NQ(3.55)
NQ(3.55)
NQ(3.55)
NQ(3.55)
NQ(7.09)
NQ(7.09)
NQ(3.55)
NQ(7.09)
NQ(22.2)
NQ(4.43)
NQ(3.55)
NQ(2.22)
NQ(7.09)
0.273
NQa
NQa
NQ(3.55)
NQ(3.55)
NQ(3.55)
2.45
NQ(3.55)
NQ(3.55)
NQ(3.55)
NQ(3.55)
DET
NQ(3.55)
NQ(3.17)
NQ(3.17)
NQ(3.17)
NQ(3.17)
NQ(3.17)
NQ(3.17)
NQ(6.33)
NQ(6.33)
NQ(3.17)
NQ(6.33)
EXCLUDE
NQ(3.95)
NQ(3.17)
NQ(1.98)
NQ(6.33)
NQ(O.OO)
NQa
NQ(3.17)
NQ(3.17)
NQ(3.17)
NQ(4.73)
1.00
NQ(3.17)
NQ(3.17)
NQ(3.17)
NQ(3.17)
NQ(6.27)
NQ(3.17)
NQ(3.16)
NQ(1.58)
NQ(1.58)
NQ(3.16)
NQ(3.16)
NQ(1.58)
NQ(3.16)
NQ(3.16)
NQ(1.58)
NQ(3.16)
NQ(19.7)
NQ(3.95)
NQ(1.58)
NQ(1.97)
NQ(3.16)
0.589
NQa
NQ(3.16)
NQ(3.16)
NQ(1.58)
NQ(6.32)
3.84
0.863
NQ(3.16)
0.471
NQa
0.416
NQ(6.32)
NQ(0.745)
NQ(0.745)
NQ(0.745)
NQ(0.745)
NQ(0.745)
NQ(0.745)
NQ(2.09)
NQ(1.49)
NQ(0.745)
NQ(1.49)
EXCLUDE
EXCLUDE
NQ(0.745)
NQ(0.466)
NQ(1.49)
NQ(0.745)
NQ(2.33)
NQ(2.33)
NQ(0.931)
NQ(0.745)
NQ(0.931)
NQ(1.49)
NQ(1.16)
NQ(0.745)
NQ(0.931)
NQ(0.931)
NQ(1.63)
NQ(2.33)
NQ(0.699)
NQ(1.48)
NQ(1.48)
NQ(1.48)
NQ(1.48)
NQ(1.48)
NQ(1.97)
NQ(1.40)
NQ(0.699)
NQ(1.40)
EXCLUDE
EXCLUDE
NQ(1.48)
NQ(0.437)
NQ(1.40)
1.64
NQ(2.18)
NQ(2.18)
NQ(0.873)
NQ(0.699)
NQ(0.873)
NQ(1.40)
NQ(1.09)
NQ(0.699)
NQ(0.873)
NQ(0.873)
DETb
NQ(2.18)
NQ(0.657)
NQ(0.657)
NQ(0.657)
NQ(0.657)
NQ(0.657)
NQ(0.657)
NQ(1.97)
NQ(1.31)
NQ(0.657)
NQ(1.31)
NQ(10.9)
NQ(2.19)
NQ(0.657)
NQ(0.438)
NQ(1.31)
0.888
NQ(2.19)
NQ(2.19)
NQ(0.876)
NQ(0.657)
NQ(0.876)
NQ(1.31)
NQ(1.09)
NQ(0.657)
NQ(0.876)
NQ(0.876)
NQ(0.657)
NQ(2.19)
NQ(0.691)
NQ(0.691)
NQ(0.691)
NQ(0.691)
NQ(0.691)
NQ(0.691)
NQ(2.07)
NQ(1.38)
NQ(0.691)
NQ(1.38)
NQ(11.5)
NQ(2.30)
NQ(0.691)
NQ(0.460)
NQ(1.38)
NQ(0.691)
NQ(2.30)
NQ(2.30)
NQ(0.921)
NQ(0.691)
NQ(0.921)
NQ(1.38)
NQ(1.15)
NQ(0.691)
NQ(0.921)
NQ(0.921)
NQ(0.691)
NQ(2.30)
NQ(0.614)
NQ(0.614)
NQ(0.614)
NQ(1.23)
NQ(0.614)
NQ(0.614)
NQ(1.84)
NQ(1.23)
NQ(0.614)
NQ(1.23)
NQ(20.5)
NQ(2.05)
NQ(0.614)
NQ(0.409)
NQ(1.23)
1.40
NQ(2.05)
NQ(2.05)
NQ(0.819)
NQ(0.614)
NQ(0.819)
NQ(1.23)
NQ(1.02)
NQ(0.614)
NQ(0.819)
NQ(0.819)
NQC
NQ(2.05)
O
i
-------
Table C-10. (Continued)
Analyte
Octachlorostyrene
Oxychlordane
Pentochloronitrobenzene
Perthane
Tecnazene
Trans-Nonachlor
Plant A
NQ(0.0662)
NQ(0.184)
NQ(0.0867)
NQ(0.403)
NQ(0.0867)
NQ(0.173)
Plant B
NQ(1.24)
NQ(7.09)
NQ(8.86)
NQ(35.5)
NQ(4.43)
NQ(3.55)
Plant C
NQ(l.ll)
NQ(6.33)
NQ(7.91)
NQ(31.7)
NQ(3.95)
NQ(3.17)
Plant D
NQ(l.ll)
NQ(3.16)
NQ(7.90)
NQ(63.2)
NQ(3.95)
NQ(1.58)
Plant E
NQ(0.931)
NQ(1.49)
NQ(1.86)
NQ(8.78)
NQ(1.86)
NQ(0.931)
Plant F
NQ(0.873)
NQ(2.96)
NQ(1.75)
NQ(2.18)
NQ(1.75)
NQ(0.873)
Plant G
NQ(0.876)
NQ(1.31)
NQ(1.75)
NQ(2.19)
NQ(1.75)
NQ(0.876)
Plant H
NQ(0.921)
NQ(1.38)
NQ(1.84)
NQ(2.30)
NQ(1.84)
NQ(0.921)
Plant I
NQ(0.819)
NQ(1.23)
NQ(1.64)
NQ(2.05)
NQ(1.64)
NQ(0.819)
Organophosphorus
Azinphos-methyl
Chlorpyriphos
Chlorpyriphos-oxon
Diazinon
Diazinon oxon
Disulfoton
Disulfoton sulfone
Ethyl-parathion
Fenitrothion
Fonofos
Malathion
Methamidophos
Methyl-chlorpyriphos
Methyl-parathion
Phorate
Phosmet
Pirimiphos-methyl
NQ(6.45)
NQ(0.817)
NQ(2.04)
NQ(0.610)
NQ(0.479)
NQ(8.84)
NQ(0.345)
NQ(1.48)
NQ(1.66)
NQ(0.207)
NQ(27.2)
NQ(58.6)
NQ(0.0899)
NQ(21.8)
NQ(1.59)
NQ(1.26)
NQ(0.123)
NQ(ll.l)
NQ(8.86)
NQ(8.86)
NQ(8.86)
6.67
NQ(43.9)
NQ(0.709)
NQ(8.86)
NQ(8.86)
NQ(8.86)
NQ(118)
NQ(8.86)
NQ(ll.l)
NQ(26.6)
NQ(8.86)
NQ(22.2)
NQ(8.86)
NQ(9.88)
NQ(7.91)
NQ(7.91)
3.50
NQ(11.8)
NQ(58.6)
NQ(0.944)
NQ(7.91)
NQ(7.91)
NQ(7.91)
NQ(105)
NQ(7.91)
NQ(9.88)
NQ(23.7)
NQ(7.91)
NQ(19.8)
NQ(7.91)
NQ(9.87)
NQ(7.90)
NQ(15.8)
3.84
NQ(15.8)
NQ(39.1)
NQ(0.632)
NQ(7.90)
NQ(15.8)
NQ(3.95)
NQ(105)
DET
NQ(9.87)
NQ(23.7)
NQ(15.8)
NQ(39.5)
NQ(7.90)
NQ(4.65)
NQ(1.86)
NQ(1.86)
<11.9
NQ(1.86)
NQ(9.31)
NQ(0.698)
NQ(1.86)
NQ(1.86)
NQ(1.86)
NQ(24.2)
NQ(34.8)
NQ(2.42)
NQ(5.59)
NQ(4.65)
NQ(4.66)
NQ(1.86)
NQ(4.37)
NQ(1.75)
NQ(1.75)
DET
NQ(1.75)
NQ(18.5)
NQ(0.655)
NQ(1.75)
NQ(1.75)
NQ(1.75)
NQ(48.1)
NQ(21.8)
NQ(2.27)
NQ(ll.l)
NQ(4.37)
NQ(9.27)
NQ(1.75)
NQ(4.38)
NQ(1.75)
NQ(1.75)
2.86
NQ(1.75)
NQ(8.76)
NQ(0.657)
NQ(1.75)
NQ(1.75)
NQ(1.75)
NQ(21.9)
NQ(21.9)
NQ(2.19)
NQ(4.38)
NQ(4.38)
NQ(4.38)
NQ(1.75)
NQ(4.60)
NQ(1.84)
15.9
NQ(1.84)
4.49
NQ(9.21)
NQ(0.691)
NQ(1.84)
NQ(1.84)
NQ(1.84)
NQ(23.0)
NQ(97.4)
NQ(2.30)
NQ(4.60)
NQ(4.60)
NQ(4.60)
NQ(1.84)
NQ(4.09)
EXCLUDE
2.59
NQ(1.64)
NQ(1.64)
NQ(8.19)
NQ(1.23)
NQ(1.64)
NQ(1.64)
NQ(1.64)
NQ(20.5)
NQ(20.5)
NQ(2.05)
NQ(4.09)
NQ(4.09)
NQ(4.09)
NQ(1.64)
Pyrethroid
Cis-Permethrin
Cypermethrins
Permethrin
Trans-Permethrin
NA
NQ(2.82)
NQ(0.775)
NA
NA
NQ(22.2)
<3.34
NA
NA
NQ(19.8)
6.00
NA
NA
NQ(19.7)
NQ(3.95)
NA
NQ(4.65)
NQ(4.66)
NQ(9.26)
NQ(2.33)
NQ(4.37)
NQ(9.27)
NQ(8.69)
NQ(2.18)
NQ(4.38)
NQ(4.38)
NQ(8.71)
NQ(2.19)
NQ(4.60)
NQ(4.60)
NQ(9.16)
NQ(2.30)
NQ(4.09)
NQ(4.09)
NQ(6.14)
NQ(2.05)
O
i
vo
-------
Table C-10. (Continued)
Analyte
Plant A
Plant B
Plant C
Plant D
Plant E
Plant F
Plant G
Plant H
Plant I
Triazine
Ametryn
Atrazine
Cyanazine
Desethyl atrazine
Hexazinone
Metribuzin
Simazine
NQ(0.463)
DET
NQ(2.24)
DET
NQ(1.18)
NQ(1.17)
2.64
NQ(8.86)
60.1
NQ(8.86)
25.0
NQ(ll.l)
NQ(2.22)
2.55
NQ(7.91)
DET
DETb
27.5
NQ(9.88)
DETb
5.00
NQ(7.90)
DET
NQ(15.8)
6.13
NQ(39.5)
NQ(3.95)
NQ(7.90)
NQ(1.86)
32.9
NQ(4.11)
57.2
4.09
NQ(1.40)
5.05
NQ(1.75)
53.8
NQ(4.54)
7.44
DET
1.90
NQ(1.75)
NQ(1.75)
DET
NQ(1.75)
1.63
NQ(2.19)
NQ(1.31)
NQ(1.75)
NQ(1.84)
DET
NQ(1.84)
NQ(0.921)
NQ(2.30)
NQ(1.38)
5.28
NQ(1.64)
26.3
NQ(1.64)
5.83
NQ(2.05)
NQ(1.23)
NQ(1.64)
1
•a,
i1
I
1
o
K>
o
§
------- |