# United States

Environmental Protection

Agency



# Occurrence of Contaminants of Emerging

Concern in Wastewater From Nine Publi c ly

Owned Treatment Works

August 2009

# U.S. Environmental Protection Agency

Office of Water (4303T)

1200 Pennsylvania Avenue, NW

Washington, DC 20460

EPA-82 1 -R-09- 009

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# i CONTENTS

Page

1. I NTRODUCTION 

# .................................................................................................................... 1

2. B ACKGROUND 

# ...................................................................................................................... 2

3. S TAGED 

# S TUDY 

# .................................................................................................................... 4

3.1 Stage 1 (200 5-2 006)................................................................................................ 4

3.2 Stage 2 (2007-2008)................................................................................................ 6

4. S AMPLE 

# C OLLECTION 

# ........................................................................................................ 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. S UMMARY OF 

# O CCURRENCE 

# D ATA 

# .................................................................................... 26

5.1 PPCPs.................................................................................................................... 27

5.2 Sterols and Hormones........................................................................................... 33

5.3 Alkylphenols, APEs, and BPA ............................................................................. 35

5.4 PBDEs................................................................................................................... 36

5.5 Pesticides............................................................................................................... 37

6. R EFERENCES 

# ...................................................................................................................... 40

Appendix A: Contaminants of Emer ging Concern (CECs) Analyte list

Appendix B: Analytical Methods Overview

Appendix C: CECs An alytical Results

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 1 1. I NTRODUCTION



# The primary objective of EPA’s Nine POTW Study (the Study) was to investigate the

occurrence of Contaminants of Emerging Con cern (CECs) in untreated and fully treated

wastewater at publicly owned treatment works (P OTWs). EPA also initially investigated the

occurrence of conventional, non- conventional, and toxic pollut ants, 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 th at 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 develo ped enough to meet the needs of the Study. As a

result, prior to collecting samples for the rema ining POTWs, EPA devel oped three analytical

methods to detect the occurrence of CECs in PO TW 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 met hods, 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 cont ain higher concentrations of CECs.

This report presents the findings from the Nine POTW Study for informational purposes.

Caution should be used in interpreting the re sults. For seve ral 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 statistical ly representative of all POTWs in the country, nor would they be expected

to statistically represen t 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 concen tration levels of many CECs

was observed in the effluent, the data are not su fficient to draw any conclusions about treatment

effectiveness.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 2 2. B ACKGROUND



# In 2005, EPA began studying environmental contamination by pharmaceuticals,

detergents, natural and synthetic hormones, a nd other chemicals. These contaminants are

commonly referred to collectively as contaminants of emerging concern.

Many CECs are believed to enter munici pal wastewater through bathing, cleaning,

laundry, and the disposal of unused pharmaceuticals and human waste. Municipal wastewater is

treated by POTWs, which typically employ biolog ical 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 pathoge ns in the treated wastewater discharged to the environment;

however, POTW treatment systems are not design ed to specifically remove CECs. Thus, any

removals of CECs which may occur are incidental to th ese treatment processes.

To assess the occurrence of CECs in POTW influent and effluent, a nd to test and develop

new analytical methods with which to m easure 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 PO TW 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 meta bolized, so a portion is excreted,

unmetabolized, in urine or feces. Metabolized and unme tabolized 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 widespectrum antibacterial and antifungal agent. Personal care produc ts enter domestic

wastewater from bathing, la undry, 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 ar e 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 choleste rol, 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 concen trations by binding to a stereospecific

target-cell receptor to activate a resp onse. Some hormones are classified by

chemical structure as steroids. Steroid hormones include the sex hormones, which

are, among others, natural estrogens, synt hetic estrogens such as EE2 (17 alpha-

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 3 ethinyl estradiol), progesterone, a nd testosterone. Other hormones are

polypeptides or amino acid-derived compounds. Plant steroids can mimic animal

sex hormones.

• 

# Alkylphenols and Alkylphe nol 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 alklyphe nol. Octylphenol ethoxylates (OPEs),

derived from octylphenol (OP), are also common.

• 

# Bisphenol A (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, automo tive primers, and printed

circuit boards.

• 

# Polybrominated Diphenyl Ethers (PBDEs) – Polybrominated diphenyl ethers

(PBDEs) are structurally similar to Po lychlorinated 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 drap eries and upholstery (e.g., decaBDE), and

plastics for personal computers and sm all appliances (e.g., octaBDE). These

chemicals slow ignition and rate of fire growth.

• 

# Pesticides – Pesticides are any of a large num ber of unrelated chemicals that are

used to prevent, destroy, or repel a liv ing 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, rodentic ides, fungicides). Pesticides include

organochlorine, organophosphorus, tria zine, and pyrethroid pesticides.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 4 3. S TAGED 

# S TUDY



# During this Study, EPA collected samples fr om 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 pro cess, including some degr ee 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 harmfu l compounds. After sampling these first four

POTWs in 2005 and 2006, EPA concluded that it need ed 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 developmen t of better analytical methods well underway,

and with changes in both POTW site selection cr iteria 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 (200 5-2 006)

The first stage of the Study was designed to determine the occurrence of pollutants at

POTWs based on one day of sampling. In addi tion to obtaining this relatively limited

information on pollutant occurrence, EPA anticip ated that the Study results would identify

candidate POTWs for future perf ormance sampling should such a decision be made to do so in

the future. Samples taken during this first stage we re analyzed for priority pollutants in order to

build on the information collected during EPA’s 1982 “50-POTW Study 1

1 

# The focus of this report is on CECs and information collected on the priority pollutants is not presented. 

# .” During Stage 1,

EPA also evaluated the available analytical methods for detecting CECs in wastewa ter.

During Stage 1, EPA sampled POTWs with a high proportion of fl ow from industries

believed to be discharging high concentrations of PPCPs. EPA used the 2004 Clean Watershed

Needs Survey (CWNS), the 2004 Permit Complia nce System (PCS) database, and the 2002

Toxic Release Inventory (TRI) to gather inform ation on influent contributions, treatment unit

operations, and performance. EPA verified info rmation about selected POTWs gathered using

these data sources through discus sions with the facilities them selves. Using this information,

EPA identified facilities with av erage influent loadings and typical discharg e patterns. The four

POTWs sampled during Stage 1 were selected be cause they met some or all of the following

criteria:

• 

# Influent flow greater than 1 million gallons per day (MGD).

• 

# High industrial wastewater flow contributi on from a variety of different industries

as well as targeted industries that were expected to contribute CECs. Targeted

industries include: manufactur e of organic chemicals, plastics, and synthetic

fibers; pharmaceutical manufacturing and testing; meat and poultry processing;

dairy products processing; hos pitals and health care facilities; and landfills.

• 

# Adequate POTW performance (effluent BOD 5 

# concentration less than 20 mg/L).

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 5 • 

# Use of a variety of treatment technologies including, technol ogies for nutrient

(total nitrogen and total phosphorus) rem oval, various disinfection technologies

(ultraviolet (UV) light, ozona tion and chorine disinfection).

During Stage 1 of the Study, EPA monitored fo r 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 semivol atile 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 de tail below. Table 3-1

found at the end of this section summarizes the unit process desc riptions and operating

characteristics of all nine PO TWs participating in the Study.

Plant A treats a relatively large proportion of i ndustrial 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 MGD.

Plant A is a conventional activated sludge f acility with powdered activated carbon (PAC)

addition. The wastewater treatment process cons ists of mechanical bar screening at the

comminutors, grit removal, ferric chloride addition for phosphorus precipitation, primary

clarification, PAC addition to remove refr actory organic compounds , aeration, secondary

clarification, sand filtration, chlorine disinf ection using chlorine gas, and dechlorination using

bisulfite. Final treated effluent is discharged to a river.

Plant B receives flow from a variety of sour ces that potentially contribute CECs and

other pollutants. The facility receives approxima tely 10 to 15 percent of influent flow from

industrial sources and comme rcial facilities, as well as wastew ater from three hospitals, domestic

septage, and landfill leachate. The to tal flow to Plant B is 27 MGD.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 6 Plant B is a conventional activated sludge facility. Wastewater treatment includes

screening, grit removal, primar y clarification, aeration, and se condary clarification. After

secondary clarification, the fac ility conducts chlorine disinfection using sodium hypochlorite and

dechlorination using sodium bisulfite, and the final tr eated effluent is discha rged to a river. This

plant does not use any biological nutrient rem oval or other more advanced processes.

Plant C receives significant industrial flow from sources that potential ly contribute both

CECs and other pollutants. The facility receives approximately five to seven percent of influent

flow from industrial sources and commercial faci lities and treats domestic wastewater, landfill

leachate, and septage from local haulers. The total flow to Plant C is 17 MGD.

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 disi nfection. The final effluent is

discharged into a lake.

Plant D receives wastewater from multiple target ed industries and uses a wide variety of

treatment processes. This POTW receives appr oximately 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 MGD.

Plant D is an advanced secondary and tertia ry treatment facility, us ing several treatment

unit operations in two treatment trains. Wastewat er enters the facility and undergoes screening,

grit removal, and primary clarifi cation. 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, tertia ry clarification, and mi xed media denitrification

filters before mixing with the secondary effluent from Train 2 prior to disinfection. Train 2 (44

percent of flow) treatment c onsists of biological phosphorus removal aeration basins with

aluminum sulfate addition to assi st in phosphorus removal, secondary clarifiers, and sand filters.

The Train 1 and Train 2 effluent s are mixed prior to ozone disi nfection. 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 underwa y, Stage 2 sampling resumed during 2007-2008.

By this time, there was more interest in direc ting 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 a ny 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 cr iteria from facilities

with higher industrial flow to thos e with higher residential flow.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 7 To identify the populations of interest for St age 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 gi ven week, over 80 percent of adults in the United States take at

least one medication (pre scription or nonprescription drug, vita min/mineral, or herbal/natural

supplement). Medication use varies consider ably by age. People ove r 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 influe nt 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 horm one medications. In that study, 21 percent of women aged 45 to

65 and 17 percent of women over 65 used conjugat ed estrogens, presumably as part of hormone

replacement therapy (HRT). Sin ce 1998, the use of HRT has declin ed 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 grea ter 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 medicati ons 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 act ive ingredient in birth control pills (Kauffman,

2002). Data published by the National Center for H ealth Statistics show that 32 percent of all

women between the ages of 20 and 24 used th e birth control pill for contraception in 2002

(Chandra, 2005). According to the 2000 Census, 21 percent of college stude nts are women in this

age group compared to 6.5 to 6.8 percent of the general population (Censu s, 2007). As a result,

the use of birth control pills among the college population may be greate r than among the general

population.

For Stage 2 site selection, EPA identified ar eas with high concentra tions 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 popul ations by county) and the U.S. News and

World Report (college settings a nd student populations). EPA selected five facilities for Stage 2

sampling using the following criter ia, 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 larg e college (at leas t 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 desc riptions and operating

characteristics of the nine POTWs participating in the Study.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 8 Plant E receives wastewater from a large uni versity and surrounding towns. The POTW

diverted town flow to another nearby POTW dur ing the sampling episode, so samples collected

represent only university-derive d wastewater. Flow from the to wn was diverted far enough in

advance of EPA’s sampling, to allow for the syst em to treat and discha rge all non-university

flow prior to the sampling episode. The plan t receives approximately 2 MGD from the

university.

Plant E is a multi-train secondary treatmen t facility that operates three secondary

treatment trains and disinfects using chlorine ga s. The influent passes through grit removal, rag

removal, primary aeration, and primary clarificat ion. 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 percen t of flow), which passes through an anoxic tank

before joining Train 1 wastewater. The combin ed 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 r eaeration in the inner zone and cl arification 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 w ith an above-average percentage of population over age

65. Twenty-two percent of the popul ation in the county is over ag e 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 Un ited States to use a five-stage BardenphoTM

treatment system with only bar screening and gr it removal prior to the process. The BardenphoTM

system consists of five zones: anaerobic, anoxi c, aerobic, anoxic, and r eaeration. This process is

designed to provide efficient, economical removal of BOD 5 

# , TSS, nitrogen, and phosphorus. The

BardenphoTM system is followed by clarification, sand filters, and UV disinfection. Final effluent

is either discharged to a river or reused for i rrigation 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 signific antly during and after ra in events; therefore,

EPA planned and conducted the sampling episode to take place during a dry time of the year to

prevent loadi ng dilution.

Plant G has an oxidation ditch system (an extended aeration activated sludge process)

with final discharge to a river. Treatment consists of bar screen ing, grit removal, fine screening,

oxidation ditch treatment, secondary clarificati on, chlorine disinfecti on (sodium hypochlorite),

and dechlorination (s odium bisulfite).

Plant H is located in a community with an above-average pe rcentage 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 ar ea is home to many active adult communities and retirement

homes. Total flow to the facility is approximately 2 MGD.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 9 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 hypochlor ite. The facility maintains chlo rine 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 per centage of population

over age 65. According to the 2000 U.S. Census da ta, 25 percent of the p opulation in the county

where the POTW is located is over age 65, compar ed to the national average of 12.4 percent. The

site contact noted that approximately 50 to 75 per cent 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 reac tors (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 perm itted to discharge to a swamp, but rarely does so.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 10 Table 3-1. Descriptions of Participating POTWs

Plant Primary

Treatment Secondary Treatment Sludge

Retention

Time

(SRT) Nitrification Sand

or

Media

Filters Type of

Disinfection

A Clarification

with ferric

chloride

addition Conventional activated sludge and

PAC addition 20 days Yes Yes Chlorine

B Clarification Conventional activated sludge 12 days Yes No Chlorine

C Clarification

with ferric

chloride (as

necessary) Conventional activated sludge 3.5 days Yes No UV

Train 1: Chemical phosphorus

removal and pure oxygen

activated sludge (with separate

stage nitrification and

denitrification) (56% flow) 2.1 days Yes Yes D Clarification

Train 2: Activated sludge with an

anoxic zone for biological

phosphorus removals and

chemical phosphorus removal

(44% flow) 0.1 days No Yes Ozone

Train 1: Trickling filters (25%

flow)

Train 2: Anoxic tank (25% flow) N/A Yes

Step 1:

19.4 days E Aeration and

clarification

Train 3: 2-step activated sludge

(50% flow)

Step 2:

5.4 days Yes No Chlorine

F None 5-stage Bardenpho process

(anaerobic, anoxic, aerobic,

anoxic, aerobic) 16 days Yes Yes UV

G None Oxidation ditch 26.5 days Yes No Chlorine

H None Oxidation ditch 12.4 days Yes Yes Chlorine

I None SBRs 14.2 days Yes Yes Chlorine

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 11 4. S AMPLE 

# C OLLECTION



# 4.1 Sampling Locations and Procedures

During Stage 1, EPA collected samples of infl uent, 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 sample s of influent and final effluent only. EPA’s

objective during Stage 2 was to id entify POTWs with hi gh influent concentra tions of CECs, not

to estimate daily influent load. POTW influent flows follow a char acteristic diurnal pattern, with

lowest flows in the very early morning hours and peak flows in mid-morning. Influent BOD 5 

# concentration follows the flow variation (Met calf and Eddy, 1978), and EPA assumed that CECs

concentrations, like the BOD 5 

# concentrations, peak with the flow. EPA decided it could identify

POTWs with high influent concen trations 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 comp osite samples. EPA did not collect any sludge

samples during Stage 2.

During Stage 2 there was a seasonal com ponent to scheduling sampling events. The

targeted populations were anticipated to have predictable seasonal mi gratory patterns. EPA

sampled POTWs with large college populations dur ing the school year, in order to get flow

associated with their student population. Similarly, EPA sampled PO TWs 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 summe r months and major holidays, when the

populations may travel to escape warm summer climates or visit family.

EPA reviewed historical monthly flow patte rns for the Stage 2 facilities in order to

determine when the daily flow to the specifi c POTWs declined, indicating that the target

populations may have left the area. All of the sa mpling 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

Plant

A B C D E F G H I a



# Sampling

Date 9/23/2005 6/21/2006 8/9/2006 9/13/2006 11/12/2007 11/15/2007 4/8/2008 4/10/2008 7/29/2008

a 

# While this sampling event took place during summer mont hs, the historical informatio n indicated flow remained

fairly consistent during the summer with peaks in Octo ber and drops off in November and December, two major

holiday months.



# 4.1.1 Sampling Locations

At four plants, EPA collected influent samp les after bar screening and grit removal, but

before primary treatment and recycle stream mixi ng when feasible (Plants A, B, D, and H). At

the remaining plants, EPA collected influent samp les prior to the grit chamber (Plants E, F, and

G) or influent channel bar screen (Plants C and I).

# Occurrence of Contaminants of Emerging Concern in Wastewater from 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 treatme nt units, EPA collected samples at several

intermediate points.

Due to the long SRT of the tw o-step activated sludge treatment system at Plant E, EPA

chose to sample the influent to and effluent fr om the activated sludge treatment system at this

facility.

Figures 4-1 through 4-9 present process sc hematics for each POTW. Sampling points are

noted on each of the plant schematics.

Figure 4-1. Process Schematic of Plant A

Figure 4-2. Process Schematic of Plant B

12

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009

Influent

Channel Bar

Screen Grit

Chamber

Grit Primary

Clarifier

Primary

Sludge Aeration

Basins Secondary

Clarifier

WAS RAS

Screenings Discharge to Lake Ferric Chloride

(as necessary) UV

Disinfection

Sampling

point location



# Figure 4-3. Process Schematic of Plant C

Figure 4-4. Process Schematic of Plant D

Figure 4-5. Process Schematic of Plant E

13

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# Figure 4-6. Process Schematic of Plant F

Figure 4-7. Process Schematic of Plant G

Influent

Channel Bar

Screen Grit

Chamber

Grit Screenings Secondary

Clarifier

WAS RAS Oxidation

Ditch Chlorine

Contact

Tank Tertiary

Media Filters

Filter

Backwash Discharge to

River (optional)

Percolation

Beds Sodium

Hypochlorite

Sampling

point location



# Figure 4-8. Process Schematic of Plant H

14

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 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 sample s collected over a specific period of time (e.g.,

24 hours) intended to represent th e characteristics of the flow at the sampling point over the

entire sampling period.

To collect a representative sample of the va rying influent flow to POTWs, EPA used one

of the following techniques:

• 

# Time-weighted sampling: aliquots collected at 15-minute intervals;

• 

# Flow-weighted sampling: automatic com positors connected to flow meters,

aliquots collected after predetermi ned amount of flow passed; or

• 

# Manual time-/flow-weighted sampling: typi cal 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 composito rs were programmed to collect

sample aliquots every 15 minutes throughout th e entire 24-hour sampling period. The time-based

schedule was intended to reflect the cha nging 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 aliquo ts 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 Wastewater from Nine POTWs August 2009



# 16 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 pe riods of higher flow. This sampling technique

required EPA to adjust the sampling interval on th e automatic compositors four times within the

24-hour sampling period. Sampling aliquot interv als were calculated prior to the sampling

episode. When possible, time-/flow-weighted sa mpling intervals were adjusted on site, as

updated flow data were pr ovided by POTW personnel.

The automatic compositors dispensed samples into multiple 10-liter jars over the 24-hour

sampling period. The contents of the multiple ja rs were poured into a large 15-gallon plastic

container lined with Teflon® bag(s). The samp le was mixed with a Teflon® stirring rod and

pumped into the sample contai ners using a peristaltic pump.

Because automatic sampling equipment could in terfere with analyte recoveries for some

of the non-CEC methods, a subset of these samp les were collected directly into sample

containers. Grab samples were collected four times (at 6-hour interval s) 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 gr ab sample collection at Plants G and H.

Grab sampling was based on the premise th at CECs concentrations, like the BOD 5 

# concentrations, peak with the flow. EPA deci ded it could identify POTWs with high influent

concentrations of CECs by co llecting 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 percen tage of human derived wa ste in the influent. The

one-time grab samples were collected directly in to 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 e ffluent flow is not cons tant, 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 sa mple jar. At the end of the compositing period,

the mixed sample was poured from the 10-L jar dir ectly into sample bottles. At the effluent, EPA

used a bottle dipper to collect sa mple aliquots into a sample bo ttle. 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 samp le bottles. EPA’s sample collection procedures

are summarized in Table 4-2.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 17 Table 4-2. Sample Collection Procedures

Plant Influent Intermediate Sampling

Point(s) Final Effluent Sludge

A Time-weighted 24-hour

composite and 4-interval

grab None Time-weighted 24-hour

composite and 4-interval

grab One-time

grab

B Flow-weighted 24-hour

composite and 4-interval

grab Flow-weighted 24-hour

composite and 4-interval grab Flow-weighted 24-hour

composite and 4-interval

grab One-time

grab

C 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

D Time-/flow-weighted 24-

hour composite and 4-

interval grab 5 time-/flow-weighted 24-hour

composites and 4-interval grabs Time-/flow-weighted 24-

hour composite and 4-

interval grab One-time

grab

E Time-/flow-weighted 24-

hour composite and 4-

interval grab 2 time-/flow-weighted 24-hour

composites and 4-interval grabs Time-/flow-weighted 24-

hour composite and 4-

interval grab None

F Time-/flow-weighted 24-

hour composite and 4-

interval grab None Time-/flow-weighted 24-

hour composite and 4-

interval grab None

G One-time grab None One-time grab None

H One-time grab None One-time grab None

I Time-weighted, 3-hour grab

composites None Time-weighted, 40-minute

grab composites None



# 4.2 Quality Assurance

EPA wrote a Quality Assurance Project Plan (QAPP) to document the project-specific

policies, organization, objectives , functional activities, and speci fic quality assurance/quality

control (QA/QC) procedures fo r the Nine POTW Study. EPA deve loped 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 re view the sampling data collected in the Study.

4.3 Quality Control Procedures

Quality assurance/quality control (QA/QC) pr ocedures 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 coll ecting and analyzing the following:

• 

# Equipment blanks;

• 

# Field duplicates;

• 

# Laboratory QC volumes; and/or

• 

# Trip blanks.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 18 4.3.1 Equipment Blanks

To assess contamination from sampling equi pment in the field, EPA collected equipment

blanks for the automatic compositors and bottl e dippers used at each sampling episode.

For the automatic compositor, EPA collected an equipment blank by pumping Ultra Pure

Blank Water DI+TM through the entire automatic compositor system directly into sample

containers; the automatic compositor system incl uded tubing, a 15-gallon pl astic tank lined with

Teflon® bag(s), a Teflon® stir r od, and, in some cases, a strainer. The tubing was purged prior to

the collection of equipment blan ks. EPA also used Ultra Pure Blank Water DI+TM to collect

bottle dipper equipment blanks by placing the samp le container into the bottle dipper apparatus

as is done during field sampling and pouring the Ultra Pure Blank Water DI+TM directly into the

sample containers.

EPA analyzed equipment blanks for sele ct 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 a ssociated 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 th e variability in samp le collection, handling,

preparation, and analysis. Dupli cate 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. Labor atory 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 leas t 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

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 19 with Ultra Pure Blank Water DI+TM and shipped w ith 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 fo r 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 bl ank for every 10 samples collected, but no less

than one per sampling episode. EPA collected 19 to tal 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 fo r each target analyte family at each POTW

sampled during the program.

Table 4-3. QC Samples at each POTW for each CECs Analyte Family

Plant Analyte

Family A B C D E F G H I

PPCPs MS/MSD MS/MSD

EfDup MS/MSD

EfDup MS/MSD EfDup

EEBlank

InDup

IEBlank EfDup

EEBlank

InDup

IEBlank EEBlank EEBlank EEBlank



# Steroids and

Hormones MS/MSD MS/MSD

EfDup MS/MSD

EfDup MS/MSD EfDup

EEBlank

InDup

IEBlank EfDup

EEBlank

InDup

IEBlank EEBlank EEBlank EEBlank



# Alkylphenols,

APEs, and BPA EfDup EfDup MS/MSD

EfDup

EEBlank

InDup

IEBlank

Trip B MS/MSD

EfDup

EEBlank

InDup

IEBlank

Trip B MS/MSD

EEBlank MS/MSD

EEBlank MS/MSD

EEBlank



# PBDEs InDup InDup EfDup

InDup EfDup

InDup EEBlank EEBlank EEBlank



# Pesticides MS/MSD

InDup MS/MSD

InDup MS/MSD MS/MSD

EfDup

EEBlank

InDup

IEBlank MS/MSD

EfDup

EEBlank

InDup

IEBlank MS/MSD

EEBlank MS/MSD

EEBlank MS/MSD

EEBlank



# MS/MSD – Matrix spike/matrix spike duplicate.

EfDup – Effluent duplicate.

EEBlank – Effluent equipment blank. InDup – Influent duplicate.

IEBlank – 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, a nd storing wastewater samples.

These specifications are designed to prevent degradation and loss of the target analytes. Several

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 20 methods direct samplers to maintain samples at a certain temperature or to treat samples with

preserving chemicals. For example organic analyt es containing chlorine are preserved with

sodium thiosulfate (Na 2 

# S 2 

# O 3 

# ). Dissolved thiosulfate converts hypochlorite to chloride ion and

prevents oxidation of the orga nic analytes in the sample. Fo r the CECs analytical methods,

preservation and storage requi rements and recommendations are still under development.

Because EPA was continuing to develop an alytical methods during the Nine POTW

Study, sample preservation and storage specificati ons were in flux. The methods used by EPA to

detect PPCPs, steroids/hormones an d pesticides suggest some of th e target analytes may degrade

rapidly in aqueous samples. The methods reco mmended beginning sample extraction within 7

days of collection (within 48 hours is strongly encouraged). Extrac ts 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 fr eezer. Samples should arrive at the laboratory at

≤ 6°C.

Both methods used to analyze for nonylphe nols and alkylphenol ethoxolates required that

samples analyzed for alkylphenols, APEs, and BP A be stored between 0 and 4°C from the time

of collection to extraction. Samples must be extracted within 28 da ys of collection and

completely analyzed within 40 days of extractio n. All samples met the hold times for extraction

and analysis. The laboratory did not re port sample temperatures upon receipt.

EPA Method 1614 does not specify holding time s 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 co llection, preservation, a nd storage conditions

used for samples analyzed for CECs:

• 

# Table 4-4: PPCPs;

• 

# Table 4-5: Steroi ds and Hormones;

• 

# Table 4-6: Alkylphenol s, APEs, and BPA;

• 

# Table 4-7: PBDEs; and

• 

# Table 4-8: Pesticides and Herbicides.

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# 21Table 4-4. PPCPs: Sample Collection, Preservation, and StoragePlantABCDEFGHIMethodAXYS MLA-052Rev. 2AXYS MLA-052Rev. 2AXYS MLA-052Rev. 2AXYS MLA-052Rev. 2EPA 1694EPA 1694EPA 1694EPA 1694EPA 1694Sample Containerfor Collection1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L plastic withTeflon lid1-L plastic withTeflon lid1-L amber plasticwith Teflon lid1-L amber plasticwith Teflon lid1-L silanized,amber glass withTeflon lidField PreservationCool, 0-4°CCool, 4°CCool, 4°CCool, 4°CCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentTemperature UponReceipt at Lab3-9°C9 – 12°C5-11°C,12-14°C2°C2°C4°C11°C5°CLab PreservationNH4-EDTANoneNoneNoneNoneNoneNoneNoneNoneStorage ProcedureSampletransferred to 4-Lbottle to preventbreakage andstored frozenRefrigeratedRefrigerated4°CStored frozen for50 days prior toextractionStored frozen for45 days prior toextractionStored frozen for5 days prior toextractionNot frozen;extracted uponreceiptUNKTime fromCollection toExtractionUNKSamplesextracted12 days afterreceiptSamples extracted3 days afterreceiptSamples extracted3 times,70 days89 days98 days aftercollectionSamples wereextracted within48 hours of thawSamples wereextracted within48 hours of thawSamplesextractedimmediately afterthawingSamples intransit 5 daysbefore extract; nolab storageSamples wereextracted twodays aftercollectionTime fromExtraction toAnalysisUNK7 to 29 days1 to 6 days5 to 43 daysUNKUNKUNKUNKWithin methodspecified timeUNK – Unknown. Not reported by laboratory or not recorded in data review narrative.aFor Plants E and F, EPA received verbal confirmation fromthe laboratory that samples arrived at or below 6°C.

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# 22Table 4-5. Steroids and Hormones: SampleCollection, Preservation, and StoragePlantABCDEFGHIMethodAXYS MLA-057Rev. 01AXYS MLA-057Rev. 01AXYS MLA-057Rev. 01AXYS MLA-057Rev. 01EPA 1698EPA 1698EPA 1698EPA 1698EPA 1698Sample Container1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L plastic withTeflon lid1-L plastic withTeflon lid1-L amberplastic withTeflon lid1-L amberplastic withTeflon lid1-L silanized,amber glasswith Teflon lidField PreservationNo headspace; cool,4°CCool, 4°CCool, 4°CCool, 4°CCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentTemperature UponReceipt at Lab3-9°C9 – 14°C9 –11°C15 – 16°C2°C2°C3°C16°C4°CStorage ProcedureStored frozenUNKUNKUNKStored frozenStored frozenStoredat -20°CStored at -20°CUNKTime fromCollection toExtraction5 months34 days4–5 days60 days57 days(extractedwithin 48 hoursafter thaw)52 days(extractedwithin 48 hoursafter thaw)Within methodspecified timeWithin method-specified timeWithincontractspecified timeTime fromExtraction toAnalysis≤40 days18 days8–17 days8 daysUNKUNKWithin methodspecified timeWithin method-specified timeWithincontractspecified timeUNK – Unknown. Not reported by laboratory or not recorded in data review narrative.

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# 23Table 4-6. Alkylphenols, APEs, and BPA: Sample Collection, Preservation, and StoragePlantABCDEFGHIMethodCRL-MS004CRL-MS004CRL-MS004CRL-MS004CRL-MS004;ASTM D 7076-06aCRL-MS004;ASTM D 7076-06aCRL-MS004;ASTM D 7076-06aCRL-MS004;ASTM D 7076-06aCRL-MS004;ASTM D 7076-06aSample Container1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lidField PreservationCool, 4°C; HCl topH <2Cool, 4°C; H2SO4to pH <2Cool, 4°C; H2SO4to pH <2Cool, 4°C; H2SO4to pH <2Cool,≤6°C;H2SO4to pH <2Cool,≤6°C;H2SO4to pH <2Cool,≤6°C;H2SO4to pH <2Cool,≤6°C;H2SO4to pH <2Cool,≤6°C;H2SO4to pH <2Temperature UponReceipt at LabUNKUNKUNKUNKUNKUNKUNKUNKUNKStorage ProcedureRefrigeratedRefrigeratedRefrigeratedRefrigeratedRefrigeratedRefrigeratedRefrigeratedRefrigeratedUNKTime fromCollection toExtractionWithin the 28-dayhold timeWithin the 28-dayhold timeWithin methodspecified timeWithin method-specified timeWithin method-specified timeWithin method-specified timeAll arbitrary holdtimes were metAll arbitrary holdtimes were met7 daysTime fromExtraction toAnalysisWithin 45 days ofextractionWithin the 40-dayhold timeWithin methodspecified timeWithin the 40-day hold timeWithin the 40-day hold timeWithin the 40-day hold timeAll arbitrary holdtimes were met. Ithas been shownin cases where reextraction wasdone, theconcentrationdoes not changenoticeably withina 2-4 week periodif preservedproperly.All arbitrary holdtimes were met. Ithas been shownin cases where reextraction wasdone, theconcentrationdoes not changenoticeably withina 2-4 week periodif preservedproperly.19 daysUNK – Unknown. Not reported by laboratory or not recorded in data review narrative.aASTM D 7076-06used on selected samples.

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# 24Table 4-7. PBDEs: Sample Collection, Preservation, and StoragePlantABCDEFGHIMethodEPA 1614 draftEPA 1614 draftEPA 1614 draftEPA 1614 draftEPA 1614EPA 1614EPA 1614EPA 1614EPA 1614Sample Container1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lidField PreservationCool, 0-6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool, 0-6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool, 0-6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool, 0-6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool, 0-6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool, 0-6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool, 0-6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool, 0-6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresent;Cool, 0-6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentTemperature UponReceipt at LabUNK9-14°C8-11°C14°C3°C4°C3°C11°CUNKStorage ProcedureNo storagerequired;extracted andanalyzedimmediately atlabNo storagerequired;extracted andanalyzedimmediately atlabNo storagerequired;extracted andanalyzedimmediately atlabNo storagerequired;extracted andanalyzedimmediately atlabStored frozenStored frozenUNKUNKUNKTime fromCollection toExtractionWithin methodspecified timeWithin method-specified timeUNKUNK63days(extracted within48 hours of thaw)63 days(extracted within48 hours of thaw)Within contractspecified timeWithin contract-specified timeWithin contract-specified timeTime from Extractionto AnalysisWithin methodspecified timeWithin method-specified timeUNKUNKUNKUNKWithincontract-specified timeWithin contract-specified timeWithin contract-specified timeUNK – Unknown. Not reported by laboratory or not recorded in data review narrative.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# 25Table 4-8. Pesticides: Sample Collection, Preservation, and StoragePlantABCDEFGHIMethodAXYS MLA035and MLA 037AXYS MLA035and MLA 037AXYS MLA035and MLA 037AXYS MLA035and MLA 037EPA 1699EPA 1699EPA 1699EPA 1699EPA 1699Sample Container1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber glasswith Teflon lid1-L amber plasticwith Teflon lid1-L amber plasticwith Teflon lid1-L amber glasswith Teflon lidField PreservationCool, 0-4°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool, 4°CCool, 4°CCool, 4°CCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentCool,≤6°C; 80mg/L (8 mL/L)Na2S2O3whenchlorine waspresentTemperature UponReceipt at Lab3-9°C9-14°C3-8°C14-16°C3°C1°C2°C12°C3-5°CStorage ProcedureTransferred to 4Lglass jar andstored frozen4°C4°C4°CStoredfrozen;extracted within48 hr of thawStored frozen;extracted within48 hr of thaw4°C4°CUNKTime from Collectionto ExtractionApprox 6 months7 days3 days35 days56-58 days aftercollection53-55 days aftercollectionaWithin methodspecified timeWithin method-specified timeUNKTime from Extractionto AnalysisLess than 40days8 days8 days26 daysUNKUNKWithin 40 daysof extractionWithin 40 daysof extractionbUNKUNK – Unknown. Not reported by laboratory or not recorded in data review narrative.aSample 71322 reanalysis extracted 76 days after collection.bSample 71470: heptachlor, dacthal, simazine, hexazinone, and chlorpyriphos re-analyzed diluted 50 days past extraction.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 26 5. S UMMARY OF 

# O CCURRENCE 

# D ATA



# This section summarizes the occurrence of CE Cs in POTW influent and effluent samples

collected in this study. With each analytical method the labo ratory could detect, but not

necessarily quantify, several CECs. Results for which an analyte wa s detected but failed to meet

method QC specifications are reporte d as DET. No numerical value is associated with detected

(DET) results. Numerical values are associated with quantifiable results, which are CECs

detected at concentrations great er than the laboratory’s reporti ng limits, and for which there were

no laboratory or data quality problems.

Several classes of CECs were detected a nd quantified in POTW influents. Quantifiable

amounts of PPCPs, sterols, alky lphenol ethoxylates (APEs), flam e retardants (PBDEs), and

pesticides were detected in treated effluent. Hormones and BP A were not quantified in any

effluent sample.

Table 5-1 presents the analytes detected and quantified in the Ni ne POTW Study and the

percent of sampled POTWs in which they were de tected or quantified in influent and effluent.

Because of the ongoing development of the analytic al methods, not all of the same CECs were

analyzed for in every POTW. Thus, the denominat or in the tables can vary from analyte to

analyte.

The remainder of this section is divided in to subsections for the following CECs analyte

classes:

• 

# PPCPs;

• 

# Sterols and hormones;

• 

# Alkylphenols, APEs, and BPA;

• 

# PBDEs; and

• 

# Pesticides.

These subsections present the compounds de tected 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 ge neral difference between the concentrations

quantified. Analytes are placed into one of the three following categories:

1. Detected or quantified in at least one in fluent sample and no effluent samples;

2. Quantified 2 

# in at least one influent sample a nd one or more effluent samples at

concentrations at least one order of ma gnitude less than at least one influent

sample; and

3. Quantified 3 

# in at least one influent sample a nd 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 thes e comparisons. For example,

the pharmaceutical albuterol was quantif ied in five influent samples and detected but failed to meet QC

specifications (DET) in effluent sample s. Albuterol is not included in Ta ble 5-2 which compares pharmaceutical

influent and effluent concentrations.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 27 For example, the pharmaceutical acetaminophe n, 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 comp arison is not based on the difference between

influent/effluent pairs, and is pr esented only to indicate the CECs for which concentrations in the

effluent were less than those in the influent. EPA did not design these sa mpling episodes with the

intention of determining trea tment effectiveness of the PO TWs, nor were sludge samples

analyzed for this study. Consequently, the extent that the concentrati on differences represent

biological and/or chemical degradation vers us partitioning to sludges is not known. More

information on the analytical methods us ed in this study is in Appendix B.

5.1 PPCPs

Of the 72 PPCPs in the Nine POTW Study, 44 we re detected in at least one sample of

POTW influent collected. Of the 44 PPCPs detect ed, 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 quantifie d 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 concentrati ons at least one order of magnit ude less than influent samples.

Seven PPCPs were quantified in at least one influe nt 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.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 28 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) 100% (5 of 5) 0% (0 of 5)

Chlorotetracycline (CTC) 11% (1 of 9) 11% (1 of 9)

Doxycycline 67% (6 of 9) 11% (1 of 9)

Minocycline 20% (1 of 5) 0% (0 of 5)

Tetracycline (TC) 78% (7 of 9) 11% (1 of 9)

Sulfadiazine 20% (1 of 5) 20% (1 of 5)

Sulfadimethoxine 25% (2 of 8) 13% (1 of 8)

Sulfamerazine 50% (4 of 8) 0% (0 of 8)

Sulfamethazine 38% (3 of 8) 13% (1 of 8)

Sulfamethizole 13% (1 of 8) 13% (1 of 8)

Sulfamethoxazole 100% (8 of 8) 88% (7 of 8)

Sulfathiazole 25% (2 of 8) 0% (0 of 8)

Ciprofloxacin 78% (7 of 9) 44% (4 of 9)

Clarithromycin 100% (5 of 5) 60% (3 of 5)

Erythromycin 89% (8 of 9) 56% (5 of 9)

Ofloxacin 100% (5 of 5) 20% (1 of 5)

Tylosin 0% (0 of 9) 11% (1 of 9)

Azithromycin 100% (5 of 5) 40% (2 of 5)

Cefotaxime 0% (0 of 5) 20% (1 of 5)

Cloxacillin 20% (1 of 5) 0% (0 of 5)

Lincomycin 56% (5 of 9) 22% (2 of 9)

Penicillin V 40% (2 of 5) 0% (0 of 5)

Trimethoprim 100% (9 of 9) 33% (3 of 9)

Virginiamycin 22% (2 of 9) 0% (0 of 9)

PPCPs: Group 1, other than Antibiotics

1,7-Dimethyl xanthine 100% (9 of 9) 11% (1 of 9)

Acetaminophen 100% (9 of 9) 0% (0 of 9)

Caffeine 100% (9 of 9) 0% (0 of 9)

Carbamazepine 100% (5 of 5) 80% (4 of 5)

Codeine 63% (5 of 8) 13% (1 of 8)

Cotinine 89% (8 of 9) 33% (3 of 9)

Dehydronifedipine 80% (4 of 5) 60% (3 of 5)

Diltiazem 100% (9 of 9) 44% (4 of 9)

Diphenhydramine 60% (3 of 5) 40% (2 of 5)

Fluoxetine 78% (7 of 9) 56% (5 of 9)

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# Table 5-1 (Continued)

29 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 

# )

Miconazole 100% (5 of 5) 0% (0 of 5)

Thiabendazole 80% (4 of 5) 80% (4 of 5)

PPCPs: Group 3

Gemfibrozil 100% (9 of 9) 78% (7 of 9)

Ibuprofen 100% (9 of 9) 0% (0 of 9)

Naproxen 100% (5 of 5) 20% (1 of 5)

Triclocarban 100% (5 of 5) 80% (4 of 5)

Triclosan 100% (5 of 5) 0% (0 of 5)

Warfarin 44% (4 of 9) 0% (0 of 9)

PPCPs: Group 4

Albuterol 67% (6 of 9) 22% (2 of 9)

Cimetidine 100% (9 of 9) 22% (2 of 9)

Metformin 88% (7 of 8) 88% (7 of 8)

Ranitidine 100% (8 of 8) 25% (2 of 8)

Sterols

Beta Sitosterol 100% (9 of 9) 44% (4 of 9)

Beta Stigmastanol 100% (5 of 5) 40% (2 of 5)

Campesterol 100% (5 of 5) 40% (2 of 5)

Cholestanol 100% (9 of 9) 78% (7 of 9)

Cholesterol 100% (9 of 9) 67% (6 of 9)

Coprostanol 100% (9 of 9) 89% (8 of 9)

Desmosterol 100% (9 of 9) 44% (4 of 9)

Epicoprostanol 100% (9 of 9) 67% (6 of 9)

Ergosterol 88% (7 of 8) 50% (4 of 8)

Stigmasterol 100% (9 of 9) 67% (6 of 9)

Hormones

17 Alpha Estradiol 22% (2 of 9) 0% (0 of 9)

17 Alpha-Dihydroequilin 22% (2 of 9) 0% (0 of 9)

17 Beta Estradiol 33% (3 of 9) 0% (0 of 9)

Alpha-Zearalanol 50% (2 of 4) 0% (0 of 4)

Androstenedione 60% (3 of 5) 0% (0 of 5)

Androsterone 100% (5 of 5) 0% (0 of 5)

Beta Estradiol 3-Benzoate 33% (3 of 9) 0% (0 of 9)

Equilin 22% (2 of 9) 0% (0 of 9)

Estriol 100% (5 of 5) 0% (0 of 5)

Estrone 56% (5 of 9) 0% (0 of 9)

Mestranol 11% (1 of 9) 0% (0 of 9)

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# Table 5-1 (Continued)

30 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 

# )

Norethindrone 33% (3 of 9) 0% (0 of 9)

Norgestrel 22% (2 of 9) 0% (0 of 9)

Progesterone 20% (1 of 5) 0% (0 of 5)

Testosterone 89% (8 of 9) 0% (0 of 9)

Alkylphenols and APEs

Nonylphenol Diethoxylates (NP2EO) 22% (2 of 9) 0% (0 of 8)

Nonylphenol Monoethoxylates

(NP1EO) 22% (2 of 9) 11% (1 of 9)

Octylphenol (OC) 44% (4 of 9) 0% (0 of 9)

Nonlyphenols (NP) 100% (9 of 9) 11% (1 of 9)

PBDEs

PBDE-28+PBDE-33 100% (9 of 9) 44% (4 of 9)

PBDE-47 100% (9 of 9) 89% (8 of 9)

PBDE-99 100% (9 of 9) 89% (8 of 9)

PBDE-100 100% (9 of 9) 78% (7 of 9)

PBDE-153 100% (9 of 9) 67% (6 of 9)

PBDE-154 100% (9 of 9) 56% (5 of 9)

PBDE-183 100% (9 of 9) 22% (2 of 9)

PBDE-209 100% (8 of 8) 33% (3 of 9)

Pesticides: Organochlorine

2,4'-DDD 22% (2 of 9) 0% (0 of 9)

2,4'-DDT 11% (1 of 9) 0% (0 of 9)

4,4'-DDD 22% (2 of 9) 0% (0 of 9)

4,4'-DDE 89% (8 of 9) 0% (0 of 9)

4,4'-DDT 22% (2 of 9) 0% (0 of 9)

Aldrin 11% (1 of 9) 0% (0 of 9)

Alpha-BHC 11% (1 of 9) 0% (0 of 9)

Alpha-chlordane 89% (8 of 9) 0% (0 of 9)

Beta-BHC 11% (1 of 9) 0% (0 of 9)

Chlorothalonil 17% (1 of 6) 0% (0 of 7)

Cis-Nonachlor 33% (3 of 9) 0% (0 of 9)

Dieldrin 89% (8 of 9) 56% (5 of 9)

Endosulphan I 11% (1 of 9) 11% (1 of 9)

Endosulfan sulfate 0% (0 of 9) 11% (1 of 9)

Gamma-BHC 44% (4 of 9) 33% (3 of 9)

Gamma-chlordane 89% (8 of 9) 11% (1 of 9)

Heptachlor 11% (1 of 9) 0% (0 of 9)

Heptachlor Epoxide 44% (4 of 9) 11% (1 of 9)

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# Table 5-1 (Continued)

31 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 

# )

Hexachlorobenzene 25% (2 of 8) 0% (0 of 8)

Methoxychlor 11% (1 of 9) 44% (4 of 9)

Perthane 33% (3 of 9) 0% (0 of 9)

Trans-Nonachlor 78% (7 of 9) 0% (0 of 9)

Pesticides: Organophosphorus

Chlorpyriphos 67% (6 of 9) 0% (0 of 8)

Chlorpyriphos-oxon 11% (1 of 9) 22% (2 of 9)

Diazinon 67% (6 of 9) 56% (5 of 9)

Diazinon oxon 0% (0 of 9) 22% (2 of 9)

Disulfoton sulfone 11% (1 of 9) 0% (0 of 9)

Malathion 22% (2 of 9) 0% (0 of 9)

Methamidophos 11% (1 of 9) 11% (1 of 9)

Methyl-chlorpyriphos 11% (1 of 9) 0% (0 of 9)

Methyl-parathion 11% (1 of 9) 0% (0 of 9)

Pesticides: Pyrethroid

Cis-Permethrin 80% (4 of 5) 0% (0 of 5)

Cypermethrins 78% (7 of 9) 0% (0 of 9)

Permethrin 89% (8 of 9) 22% (2 of 9)

Trans-Permethrin 100% (5 of 5) 0% (0 of 5)

Pesticides: Triazine

Atrazine 89% (8 of 9) 100% (9 of 9)

Cyanazine 0% (0 of 9) 11% (1 of 9)

Desethyl atrazine 89% (8 of 9) 89% (8 of 9)

Hexazinone 11% (1 of 9) 22% (2 of 9)

Metribuzin 0% (0 of 9) 22% (2 of 9)

Simazine 44% (4 of 9) 56% (5 of 9)

a 

# Does not include excluded results. Includes detected (DET) and quantified results. See Appendix C.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 32 Table 5-2. Comparison of PPCPs Detect ed in POTW Influent and Effluent b,c



# 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

Antibiotics

4-Epitetracycline (ETC)

Minocycline a



# Sulfamerazine

Sulfathiazole

Cloxacillin a



# Penicillin V a



# Virginiamycin a 

# Doxycycline

Sulfamethoxazole

Ciprofloxacin

Clarithromycin

Erythromycin-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

Warfarin a 

# 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.

c 

# Eleven pharmaceuticals were de tected in at least one influent and one e ffluent 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 faile d to meet the QC specifications of the

analytical method. Of the 441 results for whic h 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. S ee Table 5-3 for additional st atistics on detections and

quantifications for PPCP samples.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 33 Table 5-3. Numbers of PPCPs Detected in POTW Influent and Effluent

Number of Analytes Detected in at Least One Sample of

POTW Influent POTW Effluent

Analyte Group Number of

Analytes DET a 

# Quantified b 

# Total

Detected DET a 

# Quantified b 

# Total

Detected

Antibiotics 47 6 16 22 5 12 17

Group 1, other than

antibiotics 15 1 11 12 4 5 9

Group 3 6 1 5 6 0 3 3

Group 4 4 0 4 4 1 3 4

Total 72 8 36 44 10 23 33

a 

# Analytes for which all POTW influen t/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 samples 3

3 

# With the exception of one anal yte (ergosterol) at one plant. 

# . Sterols were detected

in fewer samples of POTW effluent than influent , but all evaluated sterol s 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 in fluent 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 sample s (see Tables 5-4).

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 34 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 b



# None Beta Sitosterol

Beta Stigmastanol

Campesterol

Cholestanol

Cholesterol

Coprostanol

Desmosterol

Epicoprostanol

Stigmasterol None

Hormones

17 Alpha-Estradiol a



# 17 Alpha-Dihydroequilin a



# 17 Beta-Estradiol a



# Alpha-Zearalanol a



# Androstenedione

Androsterone

Beta-Estradiol-3-Benzoate a



# Equilin

Estriol

Estrone

Mestranol a



# Norethindrone

Norgestrel a



# 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 reporte d above the laboratoryreported detection limit, 58 percent of the resu lts were not qualifie d in any way and are

considered accurate. The remaining 42 percent of the results were repor ted only as detected

(DET). No numerical value should be attached to these results because of poor spike recovery or

other laboratory problems. S ee Table 5-5 for additional st atistics on detections and

quantifications of Steroid and Hormone samples.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 35 Table 5-5. Numbers of Sterols and Hormones Detected in POTW Influent and Effluent

Number of Analytes Detected in at Least One Sample of

POTW Influent POTW Effluent

Analyte Group Number of

Analytes DET a 

# Quantified b 

# Total

Detected DET a 

# Quantified b 

# Total

Detected

Sterols 10 0 10 10 1 9 10

Hormones 17 6 9 15 0 0 0

a 

# Analytes for which all POTW influen t/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 in fluent or efflue nt 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. Mo reover, 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 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

OP

NP2EO NP1EO

NP 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 a ny 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 qua ntifications of alkylphenols, APEs and BPA.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 36 Table 5-7. Numbers of Alkylphenols, APEs, and BPA Detected in POTW Influent and

Effluent

Number of Analytes Detected in at Least One Sample of

POTW Influent POTW Effluent

Analyte Group Number

of

Analytes DET a 

# Quantified b 

# Total

Detected DET a 

# Quantified b 

# Total

Detected

Alkylphenols,

Alkylphenol

Ethoxylates (APEs),

and Bisphenol A 5 0 4 4 0 2 2

a 

# Analytes for which all POTW influen t/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, 200 7a ). 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 we re 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 Detect ed 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 preparati on blanks was often gr eater 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 met hod 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.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 37 A relatively small percentage of the PBDEs analytical results failed to meet method QC

specifications in comparison to some of the othe r CECs analyte families. Of the 156 results for

which the concentration was repor ted above the laboratory-reported detection limit, 87 percent of

the results were not qualified in any way and are considered a ccurate. The remaining 13 percent

of the results were reported only as detected (D ET). 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

Number of Analytes Detected in at Least One Sample of

POTW Influent POTW Effluent

Analyte Group Number of

Analytes DET a 

# Quantified b 

# Total

Detected DET a 

# Quantified b 

# Total

Detected

PBDEs 8 0 8 8 0 8 8

a 

# Analytes for which all POTW influen t/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 PO TW influent collected

in this study. Eighteen (18) pestic ides were detected in at leas t one sample of POTW effluent

(Table 5-1).

Twenty-three (23) pesticides were detected or quantified in at leas t one influent sample

and no effluent samples. Five pesticides were qu antified in at least one influent sample and one

or more effluent samples at c oncentrations at least one order of magnitude less than influent

samples. Five pesticides were quantified in at le ast 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.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 38 Table 5-10. Comparison of Pesticides De tected in POTW Influent and Effluent b,c



# 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

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 cyanizin e were detected in POTW ef fluent and no samples of

POTW influent. They are not included on this table.

c 

# 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 pestic ides 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 a ny 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.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 39 Table 5-11. Numbers of Pesticides Detect ed in POTW Influent and Effluent

Number of Analytes Detected in at Least One Sample of

POTW Influent POTW Effluent

Analyte Group Number of

Analytes DET a 

# Quantified b 

# Total

Detected DET a 

# Quantified b 

# Total

Detected

Organochlorine 34 3 18 21 0 7 7

Organophosphorus 17 4 4 8 1 3 4

Pyrethroid 4 0 4 4 0 1 1

Triazine 7 0 4 4 1 5 6

Total 62 7 30 37 2 16 18

a 

# Analytes for which all POTW influen t/effluent sample results were DET.

b 

# At least one sample of POTW influent/effluent was detected with no QC issues.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 40 6. R EFERENCES



# ASTM, 2006. ASTM International. Standard Te st Method for Determination of Nonylphenol,

Bisphenol A, p-tert-Octylphenol, Nonyl phenol Monoethoxylate and Nonylphenol

Diethoxylate in Environmental Waters by Gas Chromatography Mass Spectrometry,

ASTM D7065 – 06. 2006.

Census, 2007. U.S. Census Bureau. School Enrolm ent, Table A-5a. The Population 14 to 24

Years Old by High School Gra duate Status, College Enrollment, Attainment, Sex, Race,

and Hispanic Origin: October 1967 to 2005. http://www.census.gov/population/socdemo/

school/TableA-5a.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.” Nationa l Center for Health Statistics. Vital and Health

Statistics 23 (25). http://www.cdc.gov/nchs/produ cts/pubs/pubd/series/sr23/pre1/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 Agen cy, Office of Science and Technology. Method

1614: Brominated Diphenyl Ethers in Wa ter, Soil, Sediment and Tissue by

HRGC/HRMS, EPA 821-R-07-005. August 2007.

EPA, 2007b. U.S. Environmental Protection Agen cy, Office of Science and Technology. Method

1694: Pharmaceuticals and Personal Care Products in Water, Soil, Sediment, and

Biosolids by HPLC/MS/MS, EP A 821-R-08-002. December 2007.

EPA, 2007c. U.S. Environmental Protection Agen cy, 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 Agen cy, 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.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# 41 Kaufman, 2002. D.W. Kaufman, J. P. Kelly, L. Rosenberg, T.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: McGraw Hill. 1978.

Slone, 2006. Slone Center for Epidemiology at Bost on University. Patterns of Medication Use in

The United States, 2006: A Report from the Slone Survey.

http://www.bu.edu/slone/SloneSurvey/Sl oneSurvey.htm. Accessed 15 October 2007

.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# Appendix A

CONTAMINANTS OF EMERGING CONCERN (CEC s ) ANALYTE LIST

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# A-1 Table A-1. 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) Chlorotetracycline degradate x

4-Epianhydrotetracycline (EATC) Chlorotetracycline degradate x

4-Epichlortetracycline (ECTC) Chlorotetracycline degradate x

4-Epioxytetracycline (EOTC) Oxyetracycline degradate x

4-Epitetracycline (ETC) Tetracycline degradate x

Anhydrochlortetracycline (ACTC) Chlorotetracycline degradate x

Anhydrotetracycline (ATC) Chlo rotetracycline degradate x

Chlorotetracycline (CTC) Tetracycline antibiotic x x

Demeclocycline Tetracycline antibiotic x

Doxycycline Tetracycline antibiotic x x

Isochlortetracycline (ICTC) Chlorotetracycline degradate x

Minocycline Tetracycline antibiotic x

Oxytetracycline (OTC) Tetracycline antibiotic x x

Tetracycline Tetracycline antibiotic x x

Sulfachloropyridazine Sulfonamide antibiotic x x

Sulfadiazine Sulfonamide antibiotic x

Sulfadimethoxine Sulfonamide antibiotic x x

Sulfamerazine Sulfonamide antibiotic x x

Sulfamethazine Sulfonamide antibiotic x x

Sulfamethizole Sulfonamide antibiotic x x

Sulfamethoxazole Sulfonamide antibiotic x x

Sulfanilamide Sulfonamide antibiotic x

Sulfathiazole Sulfonamide antibiotic x x

Ciprofloxacin Fluoroquinolone antibiotic x x

Clarithromycin Macrolide antibiotic x

Clinafloxacin Quinoline antibiotic x

Enroflaxacin Fluoroquinolone antibiotic x x

Erythromycin Macrolide antibiotic x x

Lomefloxacin Quinoline antibiotic x

Norfloxacin Quinoline antibiotic x x

Ofloxacin Quinoline antibiotic x

Roxithromycin Macrolide antibiotic x x

Sarafloxacin Fluoroquinolone antibiotic x x

Tylosin Macrolide antibiotic x x

Ampicillin ß-lactam antibiotic a a



# Azithromycin Macrolide antibiotic x

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# Table A-1 (Continued)

A-2 Analyte Classification AXYS

Method

MLA-052

(Plants

A,B,C,D) EPA

Method

1694

(Plants

E,F,G,H,I)

Carbadox Quinoxaline antibiotic x x

Cefotaxime Cephalosporin antibiotic x

Cloxacillin ß-lactam antibiotic x

Flumequine Quinolone antibiotic x

Lincomycin Lincosamide antibiotic x x

Ormetoprim Macrolide antibiotic x

Oxacillin ß-lactam antibiotic x

Oxolinic acid Quinolone antibiotic x

Penicillin G ß-lactam antibiotic x

Penicillin V ß-lactam antibiotic x

Trimethoprim Pyrimidine antibiotic x x

Virginiamycin Macrolide antibiotic x x

Analytical Group 1, other than antibiotics

1,7-Dimethylxanthine Antispasmodic, caffeine metabolite x x

Acetaminophen Antipyretic, analgesic x x

Caffeine Stimulant x x

Carbamazepine Anticonvulsant x

Codeine Opiate x b



# x

Cotinine Nicotine metabolite x x

Dehydronifedipine Nifedipine metabolite x

Digoxigenin Immunohistochemical marker steroid x x

Digoxin Cardiac glycoside x x

Diltiazem Antihypertensive x x

Diphenhydramine Antihistamine x

Fluoxetine SSRI antidepressant x x

Miconazole Antifungal agent x

Norgestimate Hormonal contraceptives x b



# x

Thiabendazole Fungicide and parasiticide x

Analytical Group 3

Gemfibrozil Antilipemic x x

Ibuprofen Analgesic x x

Naproxen NSAID x

Triclocarban Antimicrobial x

Triclosan Antimicrobial x

Warfarin Anticoagulant x x

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# Table A-1 (Continued)

A-3 Analyte Classification AXYS

Method

MLA-052

(Plants

A,B,C,D) EPA

Method

1694

(Plants

E,F,G,H,I)

Analytical Group 4

Albuterol Antiasthmatic x x

Cimetidine Anti-acid reflux x x

Metformin Anti-diabetic drug x x

Ranitidine Anti-acid reflux x x

Total 40 73

a 

# Although listed in Method 1694, ampicillin was not includ ed in either Stage 1 or Stag e 2 of the Nine POTW Study.

b 

# Codeine and norgestimate were included in AXYS Met hod 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-1 are pharmaceuticals with the exception of

triclosan and triclocarban, both antimicrobial compounds. Samples from Plants E – I were

analyzed for triclosan and triclocarban, while sa mples from Plants A, B, C, and D were not.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# A-4 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 x x

Beta Stigmastanol x

Campesterol x

Cholestanol x x

Cholesterol x x

Coprostanol x x

Desmosterol x x

Epi-coprostanol x x

Ergosterol x x

Stigmasterol x x

Hormones

17 Alpha-Dihydroequilin x x

17 Alpha-Estradiol x x

17 Alpha-Ethinyl Estradiol a 

# x

17 Beta-Estradiol x x

Alpha-Zearalanol x

Androstenedione x

Androsterone x

Beta-Estradiol-3-Benzoate x x

Desogestrel x b



# x

Equilenin x

Equilin x x

Estriol x

Estrone x x

Ethynylestradiol a 

# x

Mestranol x x

Norethindrone x x

Norgestrel x x

Progesterone x

Testosterone x x

Total 21 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, or D.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# A-5 Table A-3. Alkylphenols, AP Es, and BPA Analyte List

Method Number Full Name Abbreviated Name

Nonylphenols a 

# NP

Nonylphenol Monoethoxylates a 

# NP1EO

Nonylphenol Diethoxylates a 

# NP2EO

Octylphenol OP MS004 (Plants A-I) and

ASTM Method D 7065-06

(Plants E-I)

Bisphenol A 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 Analyt e List (Plants A-I)

Full Name Abbreviated Name Number

2,4,4'-Tribromodiphenyl ether plus

2',3,4-Tribromodiphenyl ether 2,4,4'-TrBDE plus

2',3,4-TrBDE PBDE-28 + PBDE-33 a



# 2,2',4,4'- Tetrabromodiphenyl ether 2,2',4,4'-TeBDE PBDE-47

2,2',4,4',5- Pentabromodiphenyl ether 2,2',4,4',5-PeBDE PBDE-99

2,2',4,4',6-Pentabromodiphenyl ether 2,2',4,4',6-PeBDE PBDE-100

2,2',4,4',5,5'- Hexabromodiphenyl ether 2,2',4,4',5,5'-HxBDE PBDE-153

2,2',4,4',5',6- Heptabromodiphenyl ether 2,2',4,4',5',6-HxBDE PBDE-154

2,2',3,4,4',5',6- Heptabromodiphenyl ether 2,2',3,4,4',5',6-HpBDE PBDE-183

Decabromodiphenyl ether DeBDE 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, th e concentration of PBDE 28 + PBDE 33 presented in this report represents

the total concentration for th ese two TrBDE congeners.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# A-6 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 - I

Organochlorine

2,4'-DDD x x x

2,4'-DDE x x x

2,4'-DDT x x x

4,4'-DDD x x x

4,4'-DDE x x x

4,4'-DDT x x x

Aldrin x x x

Alpha-BHC x x x

Alpha-chlordane x x x

Beta-BHC x x x

Captan x x x

Chlorothalonil x x x

Cis-nonachlor x x x

Dacthal x x x

Delta-BHC x x x

Dieldrin x x x

Endosulfan I x x x

Endosulfan II x x x

Endosulfan sulfate x x x

Endrin x x x

Endrin Ketone x x x

Gamma-BHC x x x

Gamma-chlordane x x x

Heptachlor x x x

Heptachlor Epoxide x x x

Hexachlorobenzene x x x

Methoxychlor x x x

Mirex x x x

Octachlorostyrene x x x

Oxychlordane x x x

Pentachloronitrobenzene x x x

Perthane x x x

Tecnazene x x x

Trans-nonachlor x x x

Organophosphorus

Azinphos-methyl x x x

Chlorpyriphos x x x

Chlorpyriphos-oxon x x x

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# Table A-5 (Continued)

A-7 Analyte AXYS Method

MLA-035 Rev 04

Plant A AXYS Method

MLA-035 Rev 04

Plants B- D EPA Method 1699

Plants E - I

Diazinon x x x

Diazinon-oxon x x x

Disulfoton x x x

Disulfoton sulfone x x x

Ethyl-parathion x x x

Fenitrothion x x x

Fonofos x x x

Malathion x x x

Methamidophos x x x

Methyl-chlorpyriphos x x x

Methyl-parathion x x x

Phorate x x x

Phosmet x x x

Pirimiphos-methyl x x x

Pyrethroid

Cis-permethrin x

Cypermethrins x x x

Permethrin x x x

Trans-permethrin x

Triazine

Ametryn x x x

Atrazine x x x

Cyanazine x x x

Desethyl atrazine x x x

Hexazinone x x x

Metribuzin x x x

Simazine x x x

Other Compounds (not included in EPA Method 1699)

Alachlor x x

Benzonitrile, 3,5-Dibromo-4-Hydroxy- x

Butralin x x

Butylate x x

Dimethenamid x x

Dimethoate x x

Ethalfluralin x x

Ethion x x

Fluazifop x

Flufenacet x x

Flutriafol x x

Linuron x x

MCOA x

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# Table A-5 (Continued)

A-8 Analyte AXYS Method

MLA-035 Rev 04

Plant A AXYS Method

MLA-035 Rev 04

Plants B- D EPA Method 1699

Plants E - I

Methoprene x x

Metolachlor x x

Pendamethalin x x

Tebuconazol x x

Terbufos x x

Triallate x x

Trifluralin x x

Total 79 78 62

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# Appendix B

ANALYTICAL METHODS OVERVIEW

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# B-1 The analytical methods used to measure CE Cs 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-1.

Table B-1 Analytical Methods by POTW

Plant PPCP Method S/H Method Pesticide Method PBDE Method APEs Method

A Laboratory SOP AXYS Method MLA057 Rev 01 a 

# AXYS Method MLA035 Rev. 04 a 

# Draft EPA Method 1614

(August 2003) CRL-MS004 Rev #2

B AXYS MLA052 a 

# AXYS Method MLA057 Rev 01 a 

# AXYS Method MLA035 Rev. 04 a 

# Draft EPA Method 1614

(August 2003) CRL-MS004 Rev #2

C AXYS MLA052 a 

# AXYS Method MLA057 Rev 01 a 

# AXYS Method MLA035 Rev. 04 a 

# Draft EPA Method 1614

(August 2003) CRL-MS004 Rev #2

D AXYS MLA052 a 

# AXYS Method MLA057 Rev 01 a 

# AXYS Method MLA035 Rev. 04 a 

# Draft EPA Method 1614

(August 2003) CRL-MS004 Rev #2

E EPA Method

1694 EPA Method 1698 EPA Method 1699 EPA Method 1614

(August 2007) CRL-MS004 Rev #2

and

ASTM Method D

7065-06

F EPA Method

1694 EPA Method 1698 EPA Method 1699 EPA Method 1614

(August 2007) CRL-MS004 Rev #2

and

ASTM Method D

7065-06

G EPA Method

1694 EPA Method 1698 EPA Method 1699 EPA Method 1614

(August 2007) CRL-MS004 Rev #2

and

ASTM Method D

7065-06

H EPA Method

1694 EPA Method 1698 EPA Method 1699 EPA Method 1614

(August 2007) CRL-MS004 Rev #2

and

ASTM Method D

7065-06

I EPA Method

1694 EPA Method 1698 EPA Method 1699 EPA Method 1614

(August 2007) CRL-MS004 Rev #2

and

ASTM Method D

7065-06

a 

# AXYS Analytical Services, Si dney, 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 se nsitive and selective analytical methods for three

groups of CECs: PPCPs, steroids and hormone s, 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-labor atory 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 multilaboratory validated and published in August 2007; EPA made some additional refinements

during this study to improve the detection of certain PBDEs.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# B-2 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 Analyte Group Method Type Method Status During

Stage 1 Date Published

1614 PBDEs HRGC/HRMS Under development August 2007

1694 PPCPs HPLC/MS/MS Un der development December 2007

1698 Steroids and Hormones HRGC/H RMS Under development December 2007

1699 Pesticides HRGC/HRMS Under development 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, EP A analyzed samples of POTW influent and

effluent for alkylphenols, APEs, and BPA usi ng methods recently developed by the EPA Region

5 Chicago Regional Laboratory (CRL). During Stag e 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 Analyte Group Method Type Date

Published

MS004 Short chain alkylphenol ethoxylates and bisphenol A GC/MS-SIM, highvolume injection May 2007

ASTM D 7065-06 Short chain alkylphenol ethoxylates and bisphenol A GC/MS-SIM, lowvolume injection 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 ar e discussed below. Table B-1 lists the version

of the method used to analyze sample s 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 we re 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 si ngle-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 di vided into four groups (1 thr ough 4). Each group represents

an LC/MS/MS run. Groups 1, 2, and 3 are extrac ted under acidic (pH 2) conditions. Groups 1

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# B-3 and 2 are run in the positive elec trospray 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 in cluded 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 anti biotics and Analytical Group 2):

2. Analytical Group 1, othe r 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 th e 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 vali dation 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 targ et analytes are deriva tized 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 th e 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 cong eners such as congener 209. Subse quent to analysis at Plants

A, B, C and D, the method was modified to in corporate a temperature programmable injector

(TPI) and a 15-meter short column to mitigate de gradation of PBDE 209. After multi-laboratory

validation and peer review, Method 1614 was re vised and published in August 2007. Samples

from Plants E, F, G, H, and I were analyzed using the 2007 version of 1614.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# B-4 Pesticides

AXYS Method MLA-035 Rev. 04 (a preliminary laboratory procedure) was used to

analyze for pesticides in Plants A, B, C, a nd D. An EPA method was under development at the

Axys laboratory during the analysis of samples collect ed at Plants A, B, C, and D. Subsequent to

analysis at Plants A, B, C, and D, organonitr ogen pesticides were removed from the method by

EPA because they demonstrated thermal instabi lity and poor response under the conditions used

in EPA Method 1699.

After single-laboratory validation and p eer 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/H RMS. 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 in cludes two analytes not included in

AXYS Method MLA-035 Rev. 04.

Alkylphenols, APEs, and BPA

EPA analyzed samples for alkylphenols, APEs, and BPA using methods developed by the

EPA Region 5 CRL. Certain samples were al so analyzed using ASTM Method D 7065-06.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# Appendix C

CEC s ANALYTICAL RESULTS

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# C-1 This appendix presents the results of EPA’ s analysis of POTW influent and effluent

samples collected during the Ni ne POTW Study; sludge sampling e fforts were dropped after the

first stage because the analytical methods need ed more development. Tables C-1 through C-10

present the results of sample analys is 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 infl uent, sludge and effluent. It is difficult to

optimize analytical procedures for a large numbe r of diverse analytes. Procedures that are

optimal for one analyte may be less suitable fo r other analytes. As a result, many of the

analytical results failed to meet method quali ty 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 fl ags or other data interpretation issues were:

PPCPs 54 percent (441 detected results)

Sterols and hormones 58 percen t (240 detected results)

Alkylphenols, APEs, and BPA 65 pe rcent (31 detected results)

PBDEs 87 percent (156 detected results)

Pesticides 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 det ected with QC flags or other data

interpretation issues are reported as detected (DET) with no numeric

concentration. “DET” indicates that the an alytes 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 ve rification (CCV);

b. Other matrix interference issues;

c. Calibration issues; and

d. Blank contamination.

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# C-2 3. Results for which an analyte was not dete cted at or above th e laboratory-reported

quantitation limit are reported as not quan tified (NQ) with the laboratory-reported

quantitation limit in parentheses.

Results of analysis of duplicate sample s have been averaged for presentation in

Tables C-1 through C-10. All results are presen ted in ng/L (parts per trillion (ppt)). The

following designations and footnotes are used throughout the tables:

NA Not analyzed.

NQ() Not measured above the, laboratory- reported quantitation level with said

level reported in parentheses.

DET Detected but has associated QC flags

EXCLUDE Excluded due to crit ical QC failure including: no/low recovery in matrix

spikes and other laboratory spikes; ma trix-specific effect on LCR; and no

OPR performed.

< For duplicate samples, an NQ result was averaged with a quantified result.

a 

# 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.

b 

# For duplicate samples, an NQ result was averaged with a DET result.

c 

# Sample result set to NQ due to field blank contamination (sample result

less than five times the field blank re sult). For duplicate samples, one or

both sample results may have been set to NQ.

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-3Table C-1. Occurrence of PPCPs in POTW Influent (ng/L)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant IAntibiotics4-Epianhydrochlortetracycline(EACTC)NANANANANQ(519)NQ(472)NQ(2,860)NQ(2,890)NQ(560)4-Epianhydrotetracycline(EATC)NANANANANQ(130)NQ(118)NQ(1,340)NQ(204)NQ(140)4-Epichlortetracycline(ECTC)NANANANANQ(313)NQ(272)NQ(194)NQ(204)NQ(140)4-Epioxytetracycline (EOTC)NANANANANQ(51.9)NQ(104)NQ(288)NQ(297)NQ(189)4-Epitetracycline (ETC)NANANANADETDETb412475206Anhydrochlortetracycline(ACTC)NANANANANQ(462)NQ(464)NQ(768)NQ(751)NQ(140)Anhydrotetracycline (ATC)NANANANANQ(130)NQ(118)NQ(1,070)NQ(757)NQ(140)Chlorotetracycline (CTC)NQa434NQaNQ(684)NQ(51.9)NQ(47.2)NQ(77.7)NQ(81.8)NQ(56.0)DemeclocyclineNANANANANQ(130)NQ(118)NQ(194)NQ(204)NQ(140)DoxycyclineNQa2,970NQa2,540DETNQ(47.2)724341176Isochlortetracycline (ICTC)NANANANANQ(51.9)NQ(47.2)NQ(77.7)NQ(81.8)NQ(56.0)MinocyclineNANANANADETNQ(1,020)NQ(3,090)NQ(3,520)NQ(2,270)Oxytetracycline (OTC)NQ(997)NQ(169)NQaNQ(326)NQ(51.9)NQ(47.2)NQ(77.7)NQ(81.8)NQ(56.0)Tetracycline (TC)DETNQ(329)NQa234DETDET368490231SulfachloropyridazineNQ(59.2)NQ(16.0)EXCLUDENQ(130)NQ(13.0)NQ(11.8)NQ(19.4)NQ(20.4)NQ(14.0)SulfadiazineNANANANANQ(13.0)31.1NQ(19.4)NQ(20.4)NQ(14.0)SulfadimethoxineDETDETEXCLUDENQ(24.0)NQ(26.4)NQ(9.09)NQ(16.8)NQ(23.7)NQ(10.0)SulfamerazineDET12.5EXCLUDENQ(65.0)NQ(5.19)12.6NQ(7.77)15.3NQ(5.60)SulfamethazineDETDETEXCLUDENQ(26.0)8.94NQ(4.72)NQ(7.77)NQ(79.0)NQ(5.60)SulfamethizoleDETNQ(3.00)EXCLUDENQ(24.0)NQ(5.50)NQ(4.72)NQ(7.77)NQ(8.18)NQ(5.60)SulfamethoxazoleDETDETEXCLUDE1,500DETDETDETDET2,620SulfanilamideNANANANANQ(276)NQ(118)NQ(194)NQ(204)NQ(140)SulfathiazoleDETNQ(6.00)EXCLUDENQ(56.0)NQ(13.0)NQ(11.8)NQ(19.4)212NQ(14.0)CiprofloxacinDETNQ(300)DETNQa1,44080359115,1001,530ClarithromycinNANANANA748384DETDET292ClinafloxacinNANANANANQ(123)NQ(47.2)NQ(77.7)NQ(334)NQ(244)EnrofloxacinNQaNQ(649)NQ(690)NQ(331)NQ(26.0)NQ(23.6)NQ(38.9)NQ(40.9)NQ(28.0)

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-4Table C-1 (Continued)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant IErythromycinNQa126119DET5295862,330280202LomefloxacinNANANANANQ(26.0)NQ(23.6)NQ(38.9)NQ(40.9)NQ(28.0)NorfloxacinNQ(33.8)NQ(1,270)NQ(1,350)NQ(650)NQ(130)NQ(353)NQ(194)NQ(204)NQ(140)OfloxacinNANANANA1475054293,240DETRoxithromycinNQaNQ(4.00)NQ(4.00)NQ(2.00)NQ(5.50)NQ(2.36)NQ(3.89)NQ(27.0)NQ(2.80)SarafloxicinNQ(51.2)NQ(32.0)NQaNQ(16.0)NQ(119)NQ(403)NQ(777)NQ(818)NQ(560)TylosinNQ(79.7)NQ(16.0)NQ(18.0)NQ(17.0)NQ(256)NQ(47.2)NQ(744)NQ(2,480)NQ(661)AzithromycinNANANANADETDETDETDET669CarbadoxNQ(50.0)NQ(3.00)NQ(4.00)NQ(3.00)NQ(59.1)NQ(25.7)NQ(19.4)NQ(180)NQ(14.0)CefotaximeNANANANANQ(1,240)NQ(1,150)NQ(786)NQ(1,600)NQ(858)CloxacillinNANANANADET bNQ(123)NQ(38.9)NQ(146)NQ(28.0)FlumequineNANANANANQ(13.0)NQ(11.8)NQ(19.4)NQ(20.4)NQ(14.0)LincomycinDETDETNQ(89.0)19.1NQ(102)DETDETNQ(40.9)NQ(28.0)OrmetoprimNANANANANQ(5.19)NQ(4.72)NQ(7.77)NQ(8.18)NQ(5.60)OxacillinNANANANANQ(54.5)NQ(50.1)NQ(38.9)NQ(40.9)NQ(28.0)Oxolinic AcidNANANANANQ(21.1)NQ(10.0)NQ(7.77)NQ(8.18)NQ(5.60)Penicillin GNANANANANQ(26.0)NQ(23.6)NQ(38.9)NQ(40.9)NQ(28.0)Penicillin VNANANANANQ(109)NQ(47.2)DETDETNQ(56.0)TrimethoprimDET195498DETDETDETDETDET418VirginiamycinDETNQ(8.00)NQ(8.00)NQ(8.00)DET bNQ(332)NQ(205)NQ(2,300)NQ(148)Analytical Group 1, other than antibiotics1,7-Dimethyl xanthineDETDETDETDET62,60019,400DETDET4,860AcetaminophenDETDETDETDET79,30054,400129,000340,00040,200CaffeineDETDETDET42,10068,20052,500DETDET13,300CarbamazepineNANANANADETDETDETDET163CodeineNANQ(664)NQ(706)NQ(904)DETDETDETDET345CotinineDETDETDET2,9405352,820NQ(490)DET2,980DehydronifedipineNANANANADETDETDETDETNQ(5.60)DigoxigeninNQaNQ(126)NQ(134)NQ(134)NQ(553)NQ(431)NQ(605)NQ(516)NQ(215)DigoxinNQaNQ(1,330)NQ(1,410)NQ(1,410)NQ(757)NQ(630)NQ(194)NQ(2,530)NQ(140)DiltiazemDETDETDETDETDETDETDETDET1,490DiphenhydramineNANANANADETDETNQ(7.77)aNQ(40.9)a1,440FluoxetineDETNQ(15.0)DETDET24.758.7NQ(38.9)DET56.1

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-5Table C-1 (Continued)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant IMiconazoleNANANANADETDETbDETDET114NorgestimateNANQ(16.0)NQ(17.0)NQ(8.00)NQ(78.8)NQ(104)NQ(38.9)NQ(40.9)NQ(113)ThiabendazoleNANANANANQ(13.0)12.4DETDET34.0Analytical Group 3GemfibrozilDETDETDET1,3705394,260DETDET6,630IbuprofenDETDET7,36011,60018,90016,80020,500DET13,400NaproxenNANANANA11,30014,800DETDET18,800TriclocarbanNANANANA1875714,27013,7003,100TriclosanNANANANA9962,4204,11012,0002,810WarfarinNQ(10.6)DETNQ(53.0)DETNQ(13.0)NQ(11.8)NQ(19.4)DETDETAnalytical Group 4AlbuterolDETNQ(31.0)NQ(121)22.56.4030.6NQ(24.2)75.668.9CimetidineDET46145222773.133012011,7001,100MetforminDETNQ(326)EXCLUDEDET17,40029,40036,500248,00011,100RanitidineDET496EXCLUDEDET1,6105511,87016,800784

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-6Table C-2. Occurrence of PPCPs in POTW Effluent (ng/L)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant IAntibiotics4-Epianhydrochlortetracycline(EACTC)NANANANANQ(494)NQ(555)NQ(1,780)NQ(1,800)NQ(502)4-Epianhydrotetracycline(EATC)NANANANANQ(124)NQ(342)NQ(470)NQ(483)NQ(125)4-Epichlortetracycline(ECTC)NANANANANQ(124)NQ(296)NQ(125)NQ(125)NQ(125)4-Epioxytetracycline (EOTC)NANANANANQ(49.4)NQ(120)NQ(190)NQ(49.8)NQ(267)4-Epitetracycline (ETC)NANANANANQ(49.4)NQ(206)NQ(50.0)NQ(168)NQ(226)Anhydrochlortetracycline(ACTC)NANANANANQ(124)NQ(586)NQ(465)NQ(477)NQ(125)Anhydrotetracycline (ATC)NANANANANQ(124)NQ(313)NQ(510)NQ(515)NQ(125)Chlorotetracycline (CTC)NQ(34.4)<462aNQaNQ(673)NQ(49.4)NQ(55.5)NQ(50.0)NQ(169)NQ(50.2)DemeclocyclineNANANANANQ(124)NQ(139)NQ(125)NQ(125)NQ(125)DoxycyclineNQ(372)a<284aNQaNQ(641)NQ(49.4)NQ(55.5)NQ(50.0)NQ(49.8)NQ(50.2)Isochlortetracycline (ICTC)NANANANANQ(49.4)NQ(55.5)NQ(50.0)NQ(49.8)NQ(50.2)MinocyclineNANANANANQ(494)NQ(1,940)NQ(2,620)NQ(2,180)NQ(2,080)Oxytetracycline (OTC)NQ(460)NQ(160)NQaNQ(320)NQ(49.4)NQ(55.5)NQ(50.0)NQ(49.8)NQ(50.2)Tetracycline (TC)NQ(104)568NQaNQ(320)NQ(49.4)NQ(55.5)NQ(50.0)NQ(49.8)NQ(50.2)SulfachloropyridazineNQ(5.86)NQ(14.5)EXCLUDENQ(16.0)NQ(12.4)NQ(13.9)NQ(12.5)NQ(12.5)NQ(12.5)SulfadiazineNANANANANQ(12.4)<14.2NQ(12.5)NQ(12.5)NQ(12.5)SulfadimethoxineNQ(0.885)DETEXCLUDENQ(3.00)NQ(2.47)NQ(2.78)NQ(2.50)NQ(2.49)NQ(2.51)SulfamerazineNQ(0.245)NQ(7.50)EXCLUDENQ(8.00)NQ(4.94)NQ(5.55)NQ(5.00)NQ(4.98)NQ(5.02)SulfamethazineNQ(10.6)DETbEXCLUDENQ(3.00)NQ(4.94)NQ(5.55)NQ(5.00)NQ(19.9)NQ(5.02)SulfamethizoleNQ(1.31)NQ(3.00)EXCLUDENQ(3.00)NQ(4.94)NQ(5.55)33.5NQ(4.98)NQ(5.02)SulfamethoxazoleDETDETEXCLUDE9.542761,490DETDETNQ(5.02)SulfanilamideNANANANANQ(124)NQ(139)NQ(125)NQ(125)NQ(125)SulfathiazoleNQ(1.52)NQ(6.00)EXCLUDENQ(7.00)NQ(12.4)NQ(13.9)NQ(12.5)NQ(12.5)NQ(12.5)CiprofloxacinNQaNQ(284)DETNQ(301)36.7161NQ(219)53.0NQ(20.0)ClarithromycinNANANANA89.723.9DETNQ(12.5)NQ(12.5)ClinafloxacinNANANANANQ(49.4)NQ(55.5)NQ(345)NQ(49.8)NQ(50.2)EnrofloxacinNQaNQ(614)NQ(627)NQ(326)NQ(24.7)NQ(27.8)NQ(100)NQ(24.9)NQ(25.1)

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-7Table C-2 (Continued)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant IErythromycinNQ(4.99)a114115NQ(9.00)16791.8418NQ(2.49)NQ(2.51)LomefloxacinNANANANANQ(24.7)NQ(27.8)NQ(25.0)NQ(24.9)NQ(25.1)NorfloxacinNQ(1.21)NQ(1,210)NQ(1,230)NQ(640)NQ(124)NQ(139)NQ(1,170)NQ(125)NQ(125)OfloxacinNANANANANQ(12.4)162NQ(12.5)NQ(12.5)NQ(12.5)RoxithromycinNQ(0.203)aNQ(4.00)NQ(4.00)NQ(2.00)NQ(2.47)NQ(2.78)NQ(2.50)NQ(2.49)NQ(2.51)SarafloxicinNQ(9.80)NQ(31.0)NQaNQ(16.0)NQ(113)NQ(290)NQ(1,060)NQ(498)NQ(502)Tylosin45.1NQ(15.5)NQ(16.0)NQ(17.0)NQ(49.4)NQ(55.5)NQ(307)NQ(317)NQ(50.2)AzithromycinNANANANADETDETNQ(12.5)NQ(12.5)NQ(12.5)CarbadoxNQ(13.5)NQ(3.00)NQ(3.00)NQ(3.00)NQ(12.4)NQ(13.9)NQ(12.5)NQ(12.5)NQ(12.5)CefotaximeNANANANADETbNQ(846)NQ(361)NQ(450)NQ(698)CloxacillinNANANANANQ(93.9)NQ(100)NQ(25.0)NQ(24.9)NQ(25.1)FlumequineNANANANANQ(12.4)NQ(13.9)NQ(12.5)NQ(12.5)NQ(12.5)LincomycinDETNQ(22.0)NQ(91.5)NQ(11.0)NQ(24.7)DETNQ(25.0)NQ(24.9)NQ(25.1)OrmetoprimNANANANANQ(4.94)NQ(5.55)NQ(5.00)NQ(4.98)NQ(5.02)OxacillinNANANANANQ(24.7)NQ(27.8)NQ(25.0)NQ(24.9)NQ(25.1)Oxolinic AcidNANANANANQ(10.6)NQ(5.55)NQ(5.00)NQ(4.98)NQ(5.02)Penicillin GNANANANANQ(24.7)NQ(27.8)NQ(25.0)NQ(24.9)NQ(25.1)Penicillin VNANANANANQ(49.4)NQ(55.5)NQ(50.0)NQ(49.8)NQ(50.2)TrimethoprimNQ(1.14)NQ(15.0)385NQ(16.0)NQ(41.1)DET293NQ(12.5)NQ(12.5)VirginiamycinNQ(1.11)NQ(7.50)NQ(8.00)NQ(8.00)NQ(109)NQ(187)NQ(25.0)NQ(85.4)NQ(25.1)Analytical Group 1, other than antibiotics1,7-Dimethyl xanthineNQ(13.1)NQ(1,320)DETbNQ(700)NQ(1,240)NQ(1,390)NQ(1,250)NQ(1,250)NQ(1,250)AcetaminophenNQ(27.3)NQ(32.5)NQ(129)NQ(343)NQ(494)NQ(555)NQ(500)NQ(498)NQ(502)CaffeineNQ(79.4)NQ(303)NQ(309)NQ(322)NQ(124)NQ(139)NQ cNQ cNQ(125)CarbamazepineNANANANADETDET598487NQ(12.5)CodeineNANQ(628)NQ(642)NQ(890)NQ(24.7)DETNQ(25.0)NQ(24.9)NQ(25.1)CotinineNQ(1.41)DETNQ(722)NQ(72.0)46.0NQ(127)NQ(83.7)NQ(61.5)20.7DehydronifedipineNANANANANQ(4.94)DETNQ(5.00)44.716.5DigoxigeninNQ(1,080)NQ(120)NQ(122)NQ(132)NQ(186)NQ(406)NQ(50.0)NQ(49.8)NQ(50.2)DigoxinNQaNQ(1,260)NQ(1,280)NQ(1,390)NQ(124)NQ(139)NQ(125)NQ(125)NQ(125)DiltiazemDETNQ(2.00)DETNQ(2.00)DETDETNQ(5.00)NQ(4.98)NQ(5.02)DiphenhydramineNANANANADETDETNQ(5.00)aNQ(4.98)aNQ(5.02)FluoxetineNQ(4.26)DETbDETNQ(8.00)14.724.7NQ(25.0)DETNQ(25.1)

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-8Table C-2 (Continued)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant IMiconazoleNANANANANQ(12.4)NQ(13.9)NQ(12.5)NQ(12.5)NQ(12.5)NorgestimateNANQ(15.0)NQ(15.0)NQ(8.00)NQ(98.0)NQ(104)NQ(25.0)NQ(24.9)NQ(91.2)ThiabendazoleNANANANA<12.819.8DETDETNQ(12.5)Analytical Group 3GemfibrozilDETDETDETNQ(35.0)18.9259DETDETNQ(12.5)IbuprofenNQ(34.6)NQ(87.0)NQ(690)NQ(358)NQ(124)NQ(139)NQ(125)NQ(125)NQ(125)NaproxenNANANANA75.3NQ(27.8)NQ(25.0)NQ(24.9)NQ(25.1)TriclocarbanNANANANA15445.440.676.4NQ(25.1)TriclosanNANANANANQ(494)NQ(555)NQ(500)NQ(498)NQ(502)WarfarinNQ(0.797)NQ(1.00)NQ(6.00)NQ(7.00)NQ(12.4)NQ(13.9)NQ(12.5)NQ(12.5)NQ(12.5)Analytical Group 4AlbuterolDETNQ(30.0)NQ(125)NQ(31.0)NQ(2.83)DETNQ(5.01)NQ(4.92)NQ(5.03)CimetidineNQ(0.0453)NQ(41.0)374NQ(21.0)NQ(5.66)DETNQ(5.01)NQ(4.92)NQ(5.03)MetforminDETDETEXCLUDEDET5,4201,2503,650826NQ(252)RanitidineNQaNQ(7.00)EXCLUDENQ(8.00)NQ(5.66)DET7.22NQ(4.92)NQ(5.03)

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-9Table C-3. Occurrence of Sterols and Hormones in POTW Influent (ng/L)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant ISterolsBeta SitosterolDET271,000DET239,000DETDETDETDETDETBeta StigmastanolNANANANA34,00027,300DETDET46,000CampesterolNANANANADET46,600DETDETDETCholestanolDET39,70018,40035,800DET45,700DETDETDETCholesterolDET636,000590,000745,000DETDETDETDETDETCoprostanolDET496,000470,000366,000DETDETDETDETDETDesmosterolDET2,3201,3301,3702,8702,210DET7,03011,100EpicoprostanolDET20,1009,37019,9005,78021,400DETDETDETErgosterolDETDETNQ(5,230)EXCLUDE4,4902,820DETDETDETStigmasterolDET17,40014,80014,900DET37,200DETDETDETHormones17 Alpha EstradiolDETNQ(253)NQ(256)NQ(314)NQ(10.9)NQ(10.9)DETNQ(11.9)NQ(44.4)17 Alpha EthinylEstradiolNQ(351)NQ(253)NQ(256)NQ(628)NQ(13.0)NQ(13.0)NQ(5.07)aNQ(11.9)NQ(3.93)a17 Alpha-DihydroequilinDETNQ(285)NQ(289)NQ(354)DETbNQ(59.3)NQ(33.2)NQ(75.1)NQ(91.0)17 Beta EstradiolDETNQ(283)NQ(286)NQ(351)NQ(10.9)NQ(10.9)DETDETNQ(38.9)Alpha-ZearalanolNQ(347)DETDETNQ(317)NANANANANAAndrostenedioneNANANANA510380864NQ(378)NQ(1,640)AndrosteroneNANANANADETDET2,910661DETBeta Estradiol 3-BenzoateDETNQ(263)NQ(266)NQ(653)DETDETNQ(5.07)NQ(11.9)NQ(3.93)DesogestrelNQ(3,510)NANANANQ(75.0)NQ(71.5)NQ(91.1)NQ(125)NQ(459)EquileninNANANANANQ(5.22)NQ(5.24)NQ(5.07)NQ(11.9)NQ(13.6)EquilinNQ(150)NQ(251)NQ(254)NQ(311)<12.7NQ(10.7)NQ(17.2)28.9NQ(101)EstriolNANANANADETDET2121,000DETEstroneDETNQ(256)NQ(259)NQ(317)DET54.163.398.9NQ(89.2)MestranolNQ(417)NQ(266)DETNQ(329)NQ(48.9)NQ(12.3)NQ(5.07)NQ(11.9)NQ(3.93)Norethindrone<810DETNQ(80.5)NQ(396)NQ(11.2)DETbNQ(5.07)NQ(125)NQ(28.3)

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-10Table C-3 (Continued)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant INorgestrelNQ(509)DETDETNQ(395)NQ(606)NQ(21.8)NQ(36.3)NQ(95.2)NQ(62.1)ProgesteroneNANANANANQ(212)118NQ(191)NQ(489)NQ(349)TestosteroneDETDETDETNQ(659)917831DETDET2,650Note - To analyze influent samples, EPA’s contract laboratorysplit the sample extract into two portions for analysis of sterols and hormones. The contractlaboratory used a small portion for sterol analysis and the remaining portion for hormone analysis. The extract is split in this manner to accommodate theanticipated high sterol levels in samples and preserve the laboratory-reported detection limits of the hormone analyses. The laboratory did not split the effluentsamples in this manner because sterolsconcentrations were anticipated tobe much lower in treated effluent.

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-11Table C-4. Occurrence of Sterols and Hormones in POTW Effluent (ng/L)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant ISterolsBeta SitosterolNQ(636)aNQaDET375<988 c<663 cNQ(9.64)aNQ(9.60)aNQ(5.77)aBeta StigmastanolNANANANA117NQ(16.6)NQ(9.64)aNQ(9.60)a19.6CampesterolNANANANA14837.6NQ(16.1)aNQ(16.0)aNQ(9.62)Cholestanol72.1155486NQ(641)52440.6123197NQ(9.62)aCholesterolNQ(916)a2,22015,8004582,080DETDETNQ(16.0)aNQ(9.62)aCoprostanol163699DETNQ(695)7581141,320111103DesmosterolDET<1901,160NQ(594)41.7NQ(31.2)NQ(32.1)NQ(32.0)NQ(19.2)EpicoprostanolNQ(6.84)NQ(252)<195NQ(300)38.58.55DET4.4149.4ErgosterolDETDETDETEXCLUDENQ(30.9)NQ(30.5)DETNQ(80.0)NQ(48.1)StigmasterolDET1,300406414<401 c<287 cNQ(3.21)aNQ(3.20)aNQ(9.05)aHormones17 Alpha EstradiolNQ(2.08)NQ(257)NQ(300)NQ(306)NQ(5.89)NQ(5.82)NQ(3.21)NQ(3.20)NQ(1.92)17 Alpha Ethinyl EstradiolNQ(3.95)NQ(257)NQ(300)NQ(612)NQ(7.03)NQ(6.94)NQ(3.21)aNQ(3.20)aNQ(1.92)17 Alpha-DihydroequilinNQ(7.99)NQ(289)NQ(337)NQ(344)NQ(19.8)NQ(20.8)NQ(11.4)NQ(3.20)NQ(8.96)17 Beta EstradiolNQ(1.55)NQ(287)NQ(334)NQ(341)NQ(5.89)NQ(5.82)NQ(3.21)aNQ(3.20)aNQ(1.92)Alpha-ZearalanolNQ(6.83)NQ(259)NQ(303)NQ(309)NANANANANAAndrostenedioneNANANANANQ(31.8)NQ(31.3)NQ(64.1)NQ(97.1)NQ(95.3)AndrosteroneNANANANANQ(6.44)NQ(6.35)NQ(14.1)NQ(23.3)NQ(11.3)Beta Estradiol 3-BenzoateNQ(1.63)NQ(267)NQ(311)NQ(635)NQ(6.01)NQ(5.93)NQ(3.21)NQ(3.20)NQ(11.9)DesogestrelNQ(44.5)NANANANQ(6.58)NQ(16.0)NQ(16.7)NQ(20.9)NQ(12.7)EquileninNANANANANQ(2.84)NQ(2.80)NQ(3.21)NQ(3.20)NQ(1.92)EquilinNQ(7.85)NQ(254)NQ(297)NQ(303)NQ(5.78)NQ(5.71)NQ(3.21)NQ(3.20)NQ(11.8)EstriolNANANANANQ(19.0)NQ(14.4)NQ(33.1)NQ(21.9)NQ(1.92)EstroneNQ(1.18)NQ(259)NQ(303)NQ(309)NQ(6.58)NQ(6.49)NQ(3.21)aNQ(3.20)NQ(14.2)MestranolNQ(1.77)NQ(269)NQ(314)NQ(321)NQ(6.63)NQ(6.55)NQ(3.21)NQ(3.20)NQ(1.92)NorethindroneNQ(13.7)NQ(80.6)NQ(94.0)NQ(386)NQ(6.12)NQ(6.05)NQ(3.21)NQ(3.20)NQ(7.55)

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-12Table C-4 (Continued)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant INorgestrelNQ(7.65)NQ(80.6)NQ(94.0)NQ(384)NQ(11.6)NQ(11.4)NQ(6.43)NQ(6.40)NQ(30.4)ProgesteroneNANANANANQ(86.0)NQ(29.8)NQ(71.1)NQ(16.0)NQ(99.6)TestosteroneNQ(8.80)aNQ(269)NQ(314)NQ(641)NQ(33.3)NQ(47.8)NQ(36.5)NQ(70.0)NQ(40.1)Note - To analyze influent samples, EPA’s contract laboratorysplit the sample extract into two portions for analysis of sterols and hormones. The contractlaboratory used a small portion for sterol analysis and the remaining portion for hormone analysis. The extract is split in this manner to accommodate theanticipated high sterol levels in samples and preserve the laboratory-reported detection limits of the hormone analyses. The laboratory did not split the effluentsamples in this manner because sterols concentrations are anticipated to be much lower in treated effluent.

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-13Table C-5. Occurrence of Alkylphenols, APEs, and BPA in POTW Influent (ng/L)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant IBPANQ(5,000)EXCLUDENQ(610)NQ(1,200)EXCLUDEEXCLUDENQ(330)NQ(340)NQ(320)NP2EONQ(100,000)NQ(53,000)DET200,000NQ(1,900)NQ(1,950)NQ(2,000)NQ(2,000)NQ(1,900)NP1EONQ(50,000)NQ(19,000)DET100,000NQ(1,250)NQ(1,300)NQ(1,300)NQ(1,400)NQ(1,300)OPNQ(5,000)NQ(2,000)NQ(400)13,000DETDETNQ(220)NQ(230)3,500NP39,70079,00044,00078,000DETDET5,70024,00063,000Table C-6. Occurrence of Alkylphenols, APEs, and BPA in POTW Effluent (ng/L)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant IBPAEXCLUDEEXCLUDENQ(350)NQ(380)NQ(100)NQ(100)NQcNQcNQ(300)NP2EOEXCLUDENQ(1,100)NQ(2,100)NQ(2,200)NQ(1,100)NQ(1,100)NQ(1,100)NQ(1,100)NQ(1,800)NP1EONQ(1,000)1,100NQ(1,400)NQ(1,500)NQ(370)NQ(370)NQ(370)NQ(370)NQ(1,200)OPNQ(100)NQ(40.0)NQ(230)NQ(250)NQ(40.0)NQ(40.0)NQ(40.0)NQ(40.0)NQ(200)NPNQ(500)NQ(250)NQ(1,050)NQ(1,100)NQ(250)<520cNQ(250)NQ(250)NQ(900)

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-14Table C-7. Occurrence of PBDEs in POTW Influent (ng/L)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant IPBDE-28+PBDE-330.6832.171.331.781.111.480.7104.082.96PBDE-47DET97.178.1103DETDET34.0200151PBDE-99DET91.171.396.246.690.518.7155148PBDE-1008.4120.716.623.110.219.34.2635.833.1PBDE-153DET10.67.2410.4DETDET1.5715.814.6PBDE-1542.548.816.088.46DETDETDET11.811.9PBDE-1830.7461.521.112.161.451.550.4852.081.31PBDE-209EXCLUDE211256225260241149119142Table C-8. Occurrence of PBDEs in POTW Effluent (ng/L)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant IPBDE-28+PBDE-33NQ(0.0538)0.06520.0897NQ(0.0593)0.05740.0904NQ(0.153)NQ(0.140)NQ(0.141)PBDE-47NQa1.643.370.967DET0.9541.491.311.98PBDE-99NQa1.313.010.7811.010.4560.7870.5271.63PBDE-100NQ(0.0538)0.2650.6760.1990.2210.1310.180NQ(0.140)0.347PBDE-153NQ(0.0538)0.1380.2970.08100.0763DETNQ(0.153)NQ(0.140)0.142PBDE-154NQ(0.0538)0.1110.2410.07430.06490.0332NQ(0.153)NQ(0.140)NQ(0.141)PBDE-183NQ(0.108)NQ(0.118)NQ(0.125)NQ(0.118)0.05060.0705NQ(0.305)NQ(0.280)NQ(0.281)PBDE-209NQ(2.15)NQ(2.36)DETbNQ(2.37)aNQ(7.65)a<12.0aNQ(6.10)NQ(5.61)DET

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009



# C-15Table C-9. Occurrence of Pesticidesin POTW Influent (ng/L)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant IOrganochlorine2,4'-DDDDET1.83NQ(6.30)NQ(6.32)NQ(1.44)NQ(1.40)NQ(1.44)NQ(1.38)NQ(1.24)2,4'-DDENQ(1.07)NQ(3.43)NQ(6.30)NQ(3.16)NQ(1.44)NQ(1.40)NQ(1.44)NQ(1.38)NQ(1.24)2,4'-DDTNQ(1.29)NQ(3.43)1.00NQ(3.16)NQ(1.44)NQ(1.40)NQ(1.44)NQ(1.38)NQ(1.24)4,4'-DDDDET2.66NQ(6.30)NQ(6.32)NQ(1.44)NQ(1.40)NQ(1.44)NQ(1.38)NQ(1.24)4,4'-DDEDET2.354.003.01<1.502.06NQ(1.44)4.582.764,4'-DDTDETNQ(7.63)2.00NQ(3.16)NQ(1.44)NQ(1.40)NQ(1.44)NQ(1.38)NQ(1.24)Aldrin<0.293NQ(6.87)NQ(6.30)NQ(31.6)NQ(4.05)NQ(3.93)NQ(4.32)NQ(4.13)NQ(3.73)Alpha-BHC0.640NQ(6.87)NQ(6.30)NQ(6.32)NQ(2.89)NQ(2.79)NQ(2.88)NQ(2.75)NQ(2.49)Alpha-chlordane<5.061.89DET12.3<1.763.53NQ(1.44)4.326.64Beta-BHC<0.494NQ(6.87)NQ(6.30)NQ(6.32)NQ(2.89)NQ(2.79)NQ(2.88)NQ(2.75)NQ(2.49)CaptanEXCLUDENQ(21.5)EXCLUDENQ(39.5)EXCLUDEEXCLUDENQ(24.0)NQ(22.9)NQ(20.7)ChlorothalonilEXCLUDE1.04NQ(3.94)NQ(7.90)EXCLUDEEXCLUDENQ(4.80)NQ(4.59)NQ(4.15)Cis-Nonachlor<0.6250.307NQ(3.15)DETNQ(1.44)NQ(1.40)NQ(1.44)NQ(1.38)NQ(1.24)DacthalNQ(0.200)NQ(2.15)NQ(1.97)NQ(3.95)NQ(0.900)NQ(0.873)NQ(0.959)NQ(2.29)NQ(0.830)Delta-BHCNQ(0.474)NQ(6.87)NQ(6.30)NQ(31.6)NQ(2.89)NQ(2.79)NQ(2.88)NQ(2.75)NQ(2.49)DieldrinDET1.441.003.08NQ(1.44)6.983.611.967.09Endosulfan IDETNQ(3.43)NQaNQaNQ(4.50)NQ(4.36)NQ(4.80)NQ(4.59)NQ(4.15)Endosulfan IINQaNQaNQaNQ(31.6)NQ(4.50)NQ(4.36)NQ(4.80)NQ(4.59)NQ(4.15)Endosulfan sulfateNQ(1.20)NQ(3.43)NQ(3.15)NQ(31.6)NQ(1.80)NQ(1.74)NQ(1.92)NQ(1.83)NQ(1.66)EndrinNQ(0.518)NQ(3.43)NQ(0.00)NQ(3.16)NQ(1.44)NQ(1.40)NQ(1.44)NQ(1.38)NQ(1.24)Endrin KetoneNQ(1.14)NQ(3.43)NQ(3.15)NQ(12.6)NQ(1.80)NQ(1.74)NQ(1.92)NQ(1.83)NQ(1.66)Gamma-BHC1.457.141.001.95NQ(2.89)NQ(2.79)NQ(2.88)NQ(2.75)NQ(2.49)Gamma-chlordaneDET2.601.0016.3<2.266.61NQ(2.40)6.9911.8HeptachlorDETNQ(3.43)NQ(3.15)NQ(6.32)NQ(1.44)NQ(1.40)NQ(1.44)NQ(3.44)NQ(1.24)Heptachlor Epoxide<0.4630.291NQ(0.00)1.46NQ(1.80)NQ(1.74)NQ(1.92)NQ(1.83)1.91HexachlorobenzeneEXCLUDE0.425NQ(0.00)1.37NQ(1.80)NQ(1.74)NQ(1.92)NQ(1.83)NQ(1.66)MethoxychlorNQ(3.59)NQ(6.87)DETNQ(15.8)NQ(14.4)NQ(9.44)NQ(8.33)NQ(23.4)NQ(9.05)MirexNQ(0.183)NQ(3.43)NQ(3.15)NQ(63.2)NQ(4.50)NQ(4.36)NQ(4.80)NQ(4.59)NQ(4.15)

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-16Table C-9 (Continued)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant IOctachlorostyreneNQ(0.272)NQ(1.20)NQ(1.10)NQ(11.1)NQ(1.80)NQ(1.74)NQ(1.92)NQ(1.83)NQ(1.66)OxychlordaneNQ(0.630)NQ(6.87)NQ(6.30)NQ(6.32)NQ(2.89)NQ(2.79)NQ(2.88)NQ(2.75)NQ(2.49)PentochloronitrobenzeneNQ(0.363)NQ(17.2)NQ(7.87)NQ(79.0)NQ(3.61)NQ(3.49)NQ(3.84)NQ(3.67)NQ(3.32)PerthaneNQ(20.4)NQ(34.3)DETNQ(126)DET30.4NQ(84.2)NQ(66.0)NQ(79.2)TecnazeneNQ(0.333)NQ(8.58)NQ(7.87)NQ(39.5)NQ(3.60)NQ(3.49)NQ(3.84)NQ(3.67)NQ(3.32)Trans-Nonachlor<3.461.501.007.86NQ(1.80)2.01NQ(1.92)2.964.66OrganophosphorusAzinphos-methylNQ(38.8)NQ(10.7)NQ(19.7)NQ(98.7)NQ(35.6)NQ(8.72)NQ(9.59)NQ(54.6)NQ(8.30)ChlorpyriphosDET19.317.0NQ(79.0)NQ(3.61)13.0NQ(3.84)26264.9Chlorpyriphos-oxonNQ(2.07)NQ(8.58)NQ(7.87)DETNQ(3.61)NQ(3.49)NQ(3.84)NQ(3.67)NQ(3.32)DiazinonNQ(4.67)8.89DET41.0NQ(3.61)71.9NQ(3.84)6.3120.9Diazinon oxonNQ(1.63)NQ(8.58)NQ(7.87)NQ(158)NQ(3.60)NQ(3.49)NQ(3.84)NQ(3.67)NQ(3.32)DisulfotonNQ(26.2)NQ(42.5)NQ(39.0)NQ(78.2)NQ(18.0)NQ(17.5)NQ(19.2)NQ(18.3)NQ(16.6)Disulfoton sulfoneNQ(0.699)NQ(0.687)NQ(0.630)DETNQ(1.35)NQ(1.31)NQ(1.44)NQ(1.38)NQ(1.24)Ethyl-parathionNQ(7.66)NQ(8.58)NQ(7.87)NQ(15.8)NQ(3.60)NQ(3.49)NQ(3.84)NQ(3.67)NQ(3.32)FenitrothionNQ(3.46)NQ(8.58)NQ(7.87)NQ(31.6)NQ(3.61)NQ(3.49)NQ(3.84)NQ(3.67)NQ(3.32)FonofosNQ(1.26)NQ(8.58)NQ(7.87)NQ(39.5)NQ(3.61)NQ(3.49)NQ(3.84)NQ(3.67)NQ(3.32)MalathionNQ(70.7)NQ(114)NQ(104)DETNQ(46.8)NQ(45.4)NQ(48.0)NQ(45.9)474MethamidophosNQ(62.3)NQ(60.3)NQ(15.7)DETNQ(45.0)NQ(65.2)NQ(48.0)NQ(45.9)NQ(41.5)Methyl-chlorpyriphosDETNQ(10.7)NQ(9.84)NQ(19.7)NQ(4.68)NQ(4.54)NQ(4.80)NQ(4.59)NQ(4.15)Methyl-parathionNQ(38.3)NQ(25.8)NQ(23.6)94.6NQ(10.8)NQ(10.5)NQ(9.59)NQ(9.17)NQ(8.30)PhorateNQ(5.40)NQ(17.2)NQ(15.7)NQ(31.6)NQ(9.00)NQ(8.72)NQ(9.59)NQ(9.17)NQ(8.30)PhosmetNQ(8.36)NQ(21.5)NQ(39.4)NQ(79.0)NQ(21.6)NQ(8.73)NQ(9.59)NQ(9.17)NQ(8.30)Pirimiphos-methylNQ(0.736)NQ(8.58)NQ(7.87)NQ(15.8)NQ(3.61)NQ(3.49)NQ(3.84)NQ(3.67)NQ(3.32)PyrethroidCis-PermethrinNANANANA25.3155NQ(9.59)44.5306Cypermethrins<23.226.452.070.5NQ(9.00)DETNQ(9.59)DET66.8PermethrinDET14617634959.0DETNQ(19.1)104689Trans-PermethrinNANANANA33.82389.2659.3383

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-17Table C-9 (Continued)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant ITriazineAmetrynNQ(1.85)NQ(8.58)NQ(7.87)NQ(15.8)NQ(3.61)NQ(3.49)NQ(3.84)NQ(3.67)NQ(3.32)AtrazineDET87.7DETDET35.958.9DETNQ(13.2)37.0CyanazineNQ(11.1)NQ(8.58)NQ(7.87)NQ(31.6)NQ(15.7)NQ(17.4)NQ(3.84)NQ(3.67)NQ(11.1)Desethyl atrazineDET27.331.04.9658.07.842.65NQ(1.83)6.11HexazinoneNQ(6.16)NQ(10.7)NQ(19.7)NQ(79.0)NQ(4.68)7.13NQ(4.80)NQ(11.5)NQ(4.15)MetribuzinNQ(3.43)NQ(2.15)NQ(1.97)NQ(7.90)NQ(2.70)NQ(2.62)NQ(2.88)NQ(2.75)NQ(2.49)SimazineDET2.67DETNQ(15.8)6.65NQ(3.49)NQ(3.84)NQ(9.17)NQ(3.32)

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-18Table C-10. Occurrence of Pesticides in POTW Effluent (ng/L)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant IOrganochlorine2,4'-DDDNQ(0.404)NQ(3.55)NQ(3.17)NQ(3.16)NQ(0.745)NQ(0.699)NQ(0.657)NQ(0.691)NQ(0.614)2,4'-DDENQ(0.575)NQ(3.55)NQ(3.17)NQ(1.58)NQ(0.745)NQ(1.48)NQ(0.657)NQ(0.691)NQ(0.614)2,4'-DDTNQ(0.452)NQ(3.55)NQ(3.17)NQ(1.58)NQ(0.745)NQ(1.48)NQ(0.657)NQ(0.691)NQ(0.614)4,4'-DDDNQ(0.220)NQ(3.55)NQ(3.17)NQ(3.16)NQ(0.745)NQ(1.48)NQ(0.657)NQ(0.691)NQ(1.23)4,4'-DDENQ(0.743)NQ(3.55)NQ(3.17)NQ(3.16)NQ(0.745)NQ(1.48)NQ(0.657)NQ(0.691)NQ(0.614)4,4'-DDTNQ(0.468)NQ(3.55)NQ(3.17)NQ(1.58)NQ(0.745)NQ(1.48)NQ(0.657)NQ(0.691)NQ(0.614)AldrinNQ(0.115)NQ(7.09)NQ(6.33)NQ(3.16)NQ(2.09)NQ(1.97)NQ(1.97)NQ(2.07)NQ(1.84)Alpha-BHCNQ(0.154)NQ(7.09)NQ(6.33)NQ(3.16)NQ(1.49)NQ(1.40)NQ(1.31)NQ(1.38)NQ(1.23)Alpha-chlordaneNQ(0.174)NQ(3.55)NQ(3.17)NQ(1.58)NQ(0.745)NQ(0.699)NQ(0.657)NQ(0.691)NQ(0.614)Beta-BHCNQ(0.213)NQ(7.09)NQ(6.33)NQ(3.16)NQ(1.49)NQ(1.40)NQ(1.31)NQ(1.38)NQ(1.23)CaptanNQ(9.46)NQ(22.2)EXCLUDENQ(19.7)EXCLUDEEXCLUDENQ(10.9)NQ(11.5)NQ(20.5)ChlorothalonilNQ(0.0867)NQ(4.43)NQ(3.95)NQ(3.95)EXCLUDEEXCLUDENQ(2.19)NQ(2.30)NQ(2.05)Cis-NonachlorNQ(0.216)NQ(3.55)NQ(3.17)NQ(1.58)NQ(0.745)NQ(1.48)NQ(0.657)NQ(0.691)NQ(0.614)DacthalNQ(0.0867)NQ(2.22)NQ(1.98)NQ(1.97)NQ(0.466)NQ(0.437)NQ(0.438)NQ(0.460)NQ(0.409)Delta-BHCNQ(0.233)NQ(7.09)NQ(6.33)NQ(3.16)NQ(1.49)NQ(1.40)NQ(1.31)NQ(1.38)NQ(1.23)DieldrinNQ(0.102)0.273NQ(0.00)0.589NQ(0.745)1.640.888NQ(0.691)1.40Endosulfan I2.06NQaNQaNQaNQ(2.33)NQ(2.18)NQ(2.19)NQ(2.30)NQ(2.05)Endosulfan IINQ(0.429)aNQaNQ(3.17)NQ(3.16)NQ(2.33)NQ(2.18)NQ(2.19)NQ(2.30)NQ(2.05)Endosulfan sulfate2.86NQ(3.55)NQ(3.17)NQ(3.16)NQ(0.931)NQ(0.873)NQ(0.876)NQ(0.921)NQ(0.819)EndrinNQ(0.229)NQ(3.55)NQ(3.17)NQ(1.58)NQ(0.745)NQ(0.699)NQ(0.657)NQ(0.691)NQ(0.614)Endrin KetoneNQ(0.369)NQ(3.55)NQ(4.73)NQ(6.32)NQ(0.931)NQ(0.873)NQ(0.876)NQ(0.921)NQ(0.819)Gamma-BHCNQ(0.244)2.451.003.84NQ(1.49)NQ(1.40)NQ(1.31)NQ(1.38)NQ(1.23)Gamma-chlordaneNQ(0.186)NQ(3.55)NQ(3.17)0.863NQ(1.16)NQ(1.09)NQ(1.09)NQ(1.15)NQ(1.02)HeptachlorNQ(0.0347)NQ(3.55)NQ(3.17)NQ(3.16)NQ(0.745)NQ(0.699)NQ(0.657)NQ(0.691)NQ(0.614)Heptachlor EpoxideNQ(0.143)NQ(3.55)NQ(3.17)0.471NQ(0.931)NQ(0.873)NQ(0.876)NQ(0.921)NQ(0.819)HexachlorobenzeneEXCLUDENQ(3.55)NQ(3.17)NQaNQ(0.931)NQ(0.873)NQ(0.876)NQ(0.921)NQ(0.819)MethoxychlorDETDETNQ(6.27)0.416NQ(1.63)DETbNQ(0.657)NQ(0.691)NQcMirexNQ(0.0657)NQ(3.55)NQ(3.17)NQ(6.32)NQ(2.33)NQ(2.18)NQ(2.19)NQ(2.30)NQ(2.05)

# Occu rrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-19Table C-10. (Continued)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant IOctachlorostyreneNQ(0.0662)NQ(1.24)NQ(1.11)NQ(1.11)NQ(0.931)NQ(0.873)NQ(0.876)NQ(0.921)NQ(0.819)OxychlordaneNQ(0.184)NQ(7.09)NQ(6.33)NQ(3.16)NQ(1.49)NQ(2.96)NQ(1.31)NQ(1.38)NQ(1.23)PentochloronitrobenzeneNQ(0.0867)NQ(8.86)NQ(7.91)NQ(7.90)NQ(1.86)NQ(1.75)NQ(1.75)NQ(1.84)NQ(1.64)PerthaneNQ(0.403)NQ(35.5)NQ(31.7)NQ(63.2)NQ(8.78)NQ(2.18)NQ(2.19)NQ(2.30)NQ(2.05)TecnazeneNQ(0.0867)NQ(4.43)NQ(3.95)NQ(3.95)NQ(1.86)NQ(1.75)NQ(1.75)NQ(1.84)NQ(1.64)Trans-NonachlorNQ(0.173)NQ(3.55)NQ(3.17)NQ(1.58)NQ(0.931)NQ(0.873)NQ(0.876)NQ(0.921)NQ(0.819)OrganophosphorusAzinphos-methylNQ(6.45)NQ(11.1)NQ(9.88)NQ(9.87)NQ(4.65)NQ(4.37)NQ(4.38)NQ(4.60)NQ(4.09)ChlorpyriphosNQ(0.817)NQ(8.86)NQ(7.91)NQ(7.90)NQ(1.86)NQ(1.75)NQ(1.75)NQ(1.84)EXCLUDEChlorpyriphos-oxonNQ(2.04)NQ(8.86)NQ(7.91)NQ(15.8)NQ(1.86)NQ(1.75)NQ(1.75)15.92.59DiazinonNQ(0.610)NQ(8.86)3.503.84<11.9DET2.86NQ(1.84)NQ(1.64)Diazinon oxonNQ(0.479)6.67NQ(11.8)NQ(15.8)NQ(1.86)NQ(1.75)NQ(1.75)4.49NQ(1.64)DisulfotonNQ(8.84)NQ(43.9)NQ(58.6)NQ(39.1)NQ(9.31)NQ(18.5)NQ(8.76)NQ(9.21)NQ(8.19)Disulfoton sulfoneNQ(0.345)NQ(0.709)NQ(0.944)NQ(0.632)NQ(0.698)NQ(0.655)NQ(0.657)NQ(0.691)NQ(1.23)Ethyl-parathionNQ(1.48)NQ(8.86)NQ(7.91)NQ(7.90)NQ(1.86)NQ(1.75)NQ(1.75)NQ(1.84)NQ(1.64)FenitrothionNQ(1.66)NQ(8.86)NQ(7.91)NQ(15.8)NQ(1.86)NQ(1.75)NQ(1.75)NQ(1.84)NQ(1.64)FonofosNQ(0.207)NQ(8.86)NQ(7.91)NQ(3.95)NQ(1.86)NQ(1.75)NQ(1.75)NQ(1.84)NQ(1.64)MalathionNQ(27.2)NQ(118)NQ(105)NQ(105)NQ(24.2)NQ(48.1)NQ(21.9)NQ(23.0)NQ(20.5)MethamidophosNQ(58.6)NQ(8.86)NQ(7.91)DETNQ(34.8)NQ(21.8)NQ(21.9)NQ(97.4)NQ(20.5)Methyl-chlorpyriphosNQ(0.0899)NQ(11.1)NQ(9.88)NQ(9.87)NQ(2.42)NQ(2.27)NQ(2.19)NQ(2.30)NQ(2.05)Methyl-parathionNQ(21.8)NQ(26.6)NQ(23.7)NQ(23.7)NQ(5.59)NQ(11.1)NQ(4.38)NQ(4.60)NQ(4.09)PhorateNQ(1.59)NQ(8.86)NQ(7.91)NQ(15.8)NQ(4.65)NQ(4.37)NQ(4.38)NQ(4.60)NQ(4.09)PhosmetNQ(1.26)NQ(22.2)NQ(19.8)NQ(39.5)NQ(4.66)NQ(9.27)NQ(4.38)NQ(4.60)NQ(4.09)Pirimiphos-methylNQ(0.123)NQ(8.86)NQ(7.91)NQ(7.90)NQ(1.86)NQ(1.75)NQ(1.75)NQ(1.84)NQ(1.64)PyrethroidCis-PermethrinNANANANANQ(4.65)NQ(4.37)NQ(4.38)NQ(4.60)NQ(4.09)CypermethrinsNQ(2.82)NQ(22.2)NQ(19.8)NQ(19.7)NQ(4.66)NQ(9.27)NQ(4.38)NQ(4.60)NQ(4.09)PermethrinNQ(0.775)<3.346.00NQ(3.95)NQ(9.26)NQ(8.69)NQ(8.71)NQ(9.16)NQ(6.14)Trans-PermethrinNANANANANQ(2.33)NQ(2.18)NQ(2.19)NQ(2.30)NQ(2.05)

# Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs A ugust 2009



# C-20Table C-10. (Continued)AnalytePlant APlant BPlant CPlant DPlant EPlant FPlant GPlant HPlant ITriazineAmetrynNQ(0.463)NQ(8.86)NQ(7.91)NQ(7.90)NQ(1.86)NQ(1.75)NQ(1.75)NQ(1.84)NQ(1.64)AtrazineDET60.1DETDET32.953.8DETDET26.3CyanazineNQ(2.24)NQ(8.86)DETbNQ(15.8)NQ(4.11)NQ(4.54)NQ(1.75)NQ(1.84)NQ(1.64)Desethyl atrazineDET25.027.56.1357.27.441.63NQ(0.921)5.83HexazinoneNQ(1.18)NQ(11.1)NQ(9.88)NQ(39.5)4.09DETNQ(2.19)NQ(2.30)NQ(2.05)MetribuzinNQ(1.17)NQ(2.22)DETbNQ(3.95)NQ(1.40)1.90NQ(1.31)NQ(1.38)NQ(1.23)Simazine2.642.555.00NQ(7.90)5.05NQ(1.75)NQ(1.75)5.28NQ(1.64)