United States 

Environmental Protection 

Agency

Occurrence of Contaminants of Emerging 

Concern in Wastewater From Nine Publicly 

Owned Treatment Works 

August 2009 

U.S. Environmental Protection Agency 

Office of Water (4303T) 

1200 Pennsylvania Avenue, NW 

Washington, DC 20460 

EPA-821-R-09-009

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

i

CONTENTS 

Page 

1. INTRODUCTION .................................................................................................................... 1 

2. BACKGROUND...................................................................................................................... 2 

3. STAGED STUDY.................................................................................................................... 4 

3.1 Stage 1 (2005-2006)................................................................................................ 4 

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

4. SAMPLE COLLECTION ........................................................................................................ 11 

4.1 Sampling Locations and Procedures..................................................................... 11 

4.1.1 Sampling Locations .................................................................................. 11 

4.1.2 Sampling Procedures ................................................................................ 15 

4.2 Quality Assurance................................................................................................. 17 

4.3 Quality Control Procedures................................................................................... 17 

4.3.1 Equipment Blanks..................................................................................... 18 

4.3.2 Field Duplicates ........................................................................................ 18 

4.3.3 Laboratory Quality Control Volumes ....................................................... 18 

4.3.4 Trip Blanks................................................................................................ 18 

4.3.5 Quality Control Sample Summary............................................................ 19 

4.4 Sample Collection, Preservation, and Storage...................................................... 19 

5. SUMMARY OF OCCURRENCE DATA .................................................................................... 26 

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

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

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

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

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

6. REFERENCES ...................................................................................................................... 40 

Appendix A: Contaminants of Emerging Concern (CECs) Analyte list 

Appendix B: Analytical Methods Overview 

Appendix C: CECs Analytical Results 

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

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1. INTRODUCTION

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

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

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

occurrence of conventional, non-conventional, and toxic pollutants, including many of the 

pollutants in EPA’s 1982 “50-POTW Study” (EPA, 1982). For the first four POTWs in this 

Study, EPA selected facilities that treated industrial discharges because POTWs receiving 

significant volumes of discharges from pharmaceutical or other manufacturing facilities might be 

expected to receive a significant quantity and variety of CECs. 

 After reviewing analytical data from the first four POTWs, EPA realized that the 

available analytical methods were not developed enough to meet the needs of the Study. As a 

result, prior to collecting samples for the remaining POTWs, EPA developed three analytical 

methods to detect the occurrence of CECs in POTW wastewaters. These three methods are: EPA 

1694 for pharmaceuticals and personal care products, EPA 1698 for steroids and hormones, and 

EPA 1699 for pesticides. 

 During the development of these three methods, EPA reevaluated the design of the Study 

and decided to focus the remaining resources on documenting the occurrence of CECs in 

wastewater, and ceased collecting data for the other non-CEC parameters previously analyzed. 

EPA also revised the POTW selection criteria to focus on facilities with specific sources of 

residential flow expected to contain higher concentrations of CECs. 

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

Caution should be used in interpreting the results. For several reasons, the study does not lend 

itself to national conclusions. The Study had two very distinct stages, each with different 

analytical methods, sampling techniques and POTW selection criteria. The nine POTWs in this 

study are not statistically representative of all POTWs in the country, nor would they be expected 

to statistically represent particular subpopulations of POTWs. The analytical methods were under 

development during much of this study, which resulted in certain data quality issues during 

laboratory analysis. Additionally, sample collection efforts were not designed to calculate 

removal of CECs from POTWs. Although some reduction in concentration levels of many CECs 

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

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

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2. BACKGROUND

 In 2005, EPA began studying environmental contamination by pharmaceuticals, 

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

commonly referred to collectively as contaminants of emerging concern. 

 Many CECs are believed to enter municipal wastewater through bathing, cleaning, 

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

treated by POTWs, which typically employ biological treatment and disinfection processes and, 

in some instances, a form of advanced treatment. These processes are designed to reduce the load 

of organic pollutants and pathogens in the treated wastewater discharged to the environment; 

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

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

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

new analytical methods with which to measure these emerging contaminants, between 

September 2005 and July 2008, EPA collected samples for one day at each of nine POTWs. This 

study is referred to in this report as the “Nine POTW Study”, or “the Study.” The CECs in this 

study include the following classes of chemicals: 

• Pharmaceuticals and Personal Care Products (PPCPs) – A variety of 

pharmaceuticals and personal care products are used by individuals for personal 

health or cosmetic reasons. Pharmaceuticals include over-the-counter medication 

(e.g., aspirin, acetaminophen, and pseudoephedrine) as well as medications 

prescribed by a physician (e.g., Lipitor®, albuterol, amoxicillin). Most ingested 

pharmaceuticals are only partially metabolized, so a portion is excreted, 

unmetabolized, in urine or feces. Metabolized and unmetabolized pharmaceuticals 

are discharged in domestic sewage. 

Personal care products include chemicals such as soaps, detergents, shampoo, 

cosmetics, sun-screen products, fragrances, insect repellants, and antibacterial 

compounds. An example of a personal care product is triclosan, a potent widespectrum antibacterial and antifungal agent. Personal care products enter domestic 

wastewater from bathing, laundry, and household cleaning. 

• Steroids and Hormones (S/H) – Steroids and hormones include both naturally 

occurring compounds and synthetic analogues that are structurally related to one 

another. Hundreds of distinct steroids are found in plants and animals. Sterols, 

which are steroid-based alcohols, are the most abundant of the steroids. The most 

common sterol in vertebrates is cholesterol, which is found in cell membranes and 

also serves as a central intermediate in the biosynthesis of many biologically 

active steroids, including bile acids, corticosteroids, and sex hormones. 

Hormones are intercellular chemical messengers. They are synthesized and 

secreted from a cell and act in low concentrations by binding to a stereospecific 

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

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

are, among others, natural estrogens, synthetic estrogens such as EE2 (17 alpha-
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

3 

ethinyl estradiol), progesterone, and testosterone. Other hormones are 

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

sex hormones. 

• Alkylphenols and Alkylphenol Ethoxylates (APEs) – Alkylphenol ethoxylates 

(APEs) are synthetic surfactants used in some detergents and cleaning products. 

The most common APEs are nonylphenol ethoxylates (NPEs), derived from 

nonylphenol (NP), which is an alklyphenol. Octylphenol ethoxylates (OPEs), 

derived from octylphenol (OP), are also common. 

• 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, automotive primers, and printed 

circuit boards. 

• Polybrominated Diphenyl Ethers (PBDEs) – Polybrominated diphenyl ethers 

(PBDEs) are structurally similar to Polychlorinated biphenyl. PBDEs are major 

components of commercial formulations often used as flame retardants in 

furniture foam (e.g., pentaBDE), plastics for TV cabinets, consumer electronics, 

wire insulation, back coatings for draperies and upholstery (e.g., decaBDE), and 

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

chemicals slow ignition and rate of fire growth. 

• Pesticides – Pesticides are any of a large number of unrelated chemicals that are 

used to prevent, destroy, or repel a living organism that occurs where it is not 

wanted (i.e., a pest). Pesticides are often referred to according to the type of pest

they control (e.g., insecticides, rodenticides, fungicides). Pesticides include 

organochlorine, organophosphorus, triazine, and pyrethroid pesticides. 
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

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3. STAGED STUDY

 During this Study, EPA collected samples from nine POTWs located in eight states. 

These POTWs are referred to in this report as Plants A through I. All of the sampled POTWs 

used variations of the activated sludge process, including some degree of nitrification. All 

POTWs disinfected some or all of their treated effluent prior to discharge or land application. 

 The Study was carried out in two stages. In the first stage (Plants A through D), EPA 

examined the occurrence of contaminants of emerging concern (CECs), including endocrine 

disrupting compounds and other potentially harmful compounds. After sampling these first four 

POTWs in 2005 and 2006, EPA concluded that it needed more sensitive and selective analytical 

methods. Method development took place from 2006-2008. See Appendix B for an overview of 

EPA’s CECs analytical methods. With development of better analytical methods well underway, 

and with changes in both POTW site selection criteria and sampling approach (as described in 

Section 3.2 of this report), EPA began the second stage of the Study in September 2007 (Plants E 

through I). 

3.1 Stage 1 (2005-2006)

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

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

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

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

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

build on the information collected during EPA’s 1982 “50-POTW Study1

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 wastewater. 

 

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

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

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

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

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

these data sources through discussions with the facilities themselves. Using this information, 

EPA identified facilities with average influent loadings and typical discharge patterns. The four 

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

criteria: 

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

• High industrial wastewater flow contribution from a variety of different industries 

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

industries include: manufacture of organic chemicals, plastics, and synthetic 

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

dairy products processing; hospitals and health care facilities; and landfills. 

• Adequate POTW performance (effluent BOD5 concentration less than 20 mg/L). 
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

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• Use of a variety of treatment technologies including, technologies for nutrient 

(total nitrogen and total phosphorus) removal, various disinfection technologies 

(ultraviolet (UV) light, ozonation and chorine disinfection). 

During Stage 1 of the Study, EPA monitored for a lengthy list of pollutants including: 

• Pollutants that were part of the 1982 50-POTW Study, including: 

— Volatile and semivolatile organic compounds, 

— Metals (total and dissolved) and, 

— Classical pollutants. 

• Additional organic compounds: 

— Other volatile and semivolatile organic compounds, 

— Polybrominated diphenyl ethers (PBDEs), 

— Polychlorinated dioxins and furans, and 

— Chlorinated biphenyl congeners (PCBs); 

• Microbiological pollutants; and 

• Analytes for which methods were under development, including: 

— Pharmaceuticals and personal care products, 

— Steroids and hormones, 

— Alkylphenol ethoxylates (APEs), and 

— Pesticides and herbicides. 

Stage 1 Facilities 

 Each of the four POTWs selected for Stage 1 is described in more detail below. Table 3-1 

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

characteristics of all nine POTWs participating in the Study. 

Plant A treats a relatively large proportion of industrial wastewater (18 percent of total 

flow is from industrial sources) and receives 3.5 million pounds per year of TRI-listed chemicals, 

the majority of this industrial flow coming from a pharmaceutical manufacturer. Sources of 

domestic wastewater treated at the plant include two colleges with on-campus housing (a 

university with 28,600 students and a college with 1,300 students). The total flow to Plant A is 

26 MGD. 

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

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

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

clarification, PAC addition to remove refractory organic compounds, aeration, secondary 

clarification, sand filtration, chlorine disinfection using chlorine gas, and dechlorination using 

bisulfite. Final treated effluent is discharged to a river. 

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

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

industrial sources and commercial facilities, as well as wastewater from three hospitals, domestic 

septage, and landfill leachate. The total flow to Plant B is 27 MGD. 
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

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

screening, grit removal, primary clarification, aeration, and secondary clarification. After 

secondary clarification, the facility conducts chlorine disinfection using sodium hypochlorite and 

dechlorination using sodium bisulfite, and the final treated effluent is discharged to a river. This 

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

Plant C receives significant industrial flow from sources that potentially contribute both 

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

flow from industrial sources and commercial facilities and treats domestic wastewater, landfill 

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

discharged into a lake. 

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

treatment processes. This POTW receives approximately 17 percent of flow from industrial 

sources and commercial facilities, as well as wastewater from two hospitals and several 

universities, septage, and landfill leachate. The total flow to Plant D is 34 MGD. 

Plant D is an advanced secondary and tertiary treatment facility, using several treatment 

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

grit removal, and primary clarification. After primary treatment, the wastewater is split into two 

treatment trains. The wastewater in Train 1 (56 percent of flow) first undergoes aluminum sulfate 

addition for phosphorus removal, then passes through pure oxygen aeration basins, secondary 

clarification, nitrification aeration basins, tertiary clarification, and mixed media denitrification 

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

percent of flow) treatment consists of biological phosphorus removal aeration basins with 

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

The Train 1 and Train 2 effluents are mixed prior to ozone disinfection. The final effluent is 

discharged to a creek. 

3.2 Stage 2 (2007-2008)

 During Stage 1 of the Study, EPA determined that the analytical methods needed further 

development. This development took place during 2006-2008, and resulted in three new 

analytical methods, EPA Methods 1694, 1698, and 1699. 

 With method development well underway, Stage 2 sampling resumed during 2007-2008. 

By this time, there was more interest in directing available resources to document occurrence of 

CECs in POTW influent and effluent with the use of single-day (screening) sampling episodes. 

 Thus, in Stage 2 EPA did not analyze for any pollutants beyond what had been identified 

as CECs in Stage 1. 

 In Stage 2 EPA also changed the selection criteria for POTWs. Because CEC discharges 

can result from excretion of ingested CECs, EPA changed the selection criteria from facilities 

with higher industrial flow to those with higher residential flow. 
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

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 To identify the populations of interest for Stage 2, EPA reviewed literature on the use of 

medications that may be found in wastewater. The Slone Epidemiology Center at Boston 

University has conducted an annual survey of medication use in the United States since 1998. 

The surveys indicated that in a given week, over 80 percent of adults in the United States take at 

least one medication (prescription or nonprescription drug, vitamin/mineral, or herbal/natural 

supplement). Medication use varies considerably by age. People over 65 are the largest 

consumers of medication. Of this age group, 57 to 59 percent take at least five medications in a 

week, and 17 to 19 percent take at least 10 (Slone, 2006). Thus, higher influent concentrations of 

pharmaceuticals may be found at POTWs that serve a higher than average proportion of 

population age 65 or older. 

 The Slone survey conducted in 1998-1999 (Kaufman, 2002) identified two population 

groups that frequently use hormone medications. In that study, 21 percent of women aged 45 to 

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

replacement therapy (HRT). Since 1998, the use of HRT has declined dramatically, but as of 

2004, 12 percent of women over 50 continued to use this therapy. Higher POTW influent 

concentrations of estrogens may be found at POTWs serving a greater than average population of 

women over 50, though this effect may have decreased with the decline of HRT use.

 The second population group that frequently uses hormone medications is women aged 

18 to 44. In the 1998-99 Slone survey, 14 percent of this group used EE2 (17 alpha-ethinyl 

estradiol), the synthetic hormone that is the active ingredient in birth control pills (Kauffman, 

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

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

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

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

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

population. 

 For Stage 2 site selection, EPA identified areas with high concentrations of college-aged 

populations or populations over 65. To identify such areas, EPA used information from the U.S. 

Census Bureau (population by age and total populations by county) and the U.S. News and 

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

sampling using the following criteria, in no particular order: 

• Use of selected advanced treatment technology; 

• Use of separate sewers, which segregates stormwater away from sewers directing 

wastewater to the POTW; and 

• Service area includes a large college (at least 10,000 students) or more than 15 

percent of population 65 or over. 

Stage 2 Facilities 

 The five facilities selected for sampling during Stage 2 are described below. Table 3-1, 

found at the end of this section, summarizes the unit process descriptions and operating 

characteristics of the nine POTWs participating in the Study. 
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

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Plant E receives wastewater from a large university and surrounding towns. The POTW 

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

represent only university-derived wastewater. Flow from the town was diverted far enough in 

advance of EPA’s sampling, to allow for the system to treat and discharge all non-university 

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

university. 

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

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

removal, primary aeration, and primary clarification. From here, treatment is split into three 

trains. The wastewater in Train 1 (25 percent of flow) is passed through trickling filters prior to 

rejoining with Train 2 wastewater (25 percent of flow), which passes through an anoxic tank 

before joining Train 1 wastewater. The combined secondary effluent from Trains 1 and 2 

undergo secondary aeration and clarification with poly-aluminum chloride addition for 

phosphorus removal. Train 3 (50 percent of flow) is a two-step conventional activated sludge 

treatment process. The first step is a two-ring activated sludge basin; the inner zone provides 

aeration and the outer zone provides anoxic conditions. The second step, also a two-ring 

activated sludge basin, provides reaeration in the inner zone and clarification in the outer zone. 

Combined secondary effluent from Trains 1 and 2 and secondary effluent from Train 3 are all 

combined prior to disinfection using chlorine gas. The final effluent is used for spray irrigation 

on agricultural fields. 

Plant F is located in a county with an above-average percentage of population over age 

65. Twenty-two percent of the population in the county is over age 65, compared to the national 

average of 12.4 percent. Total flow to Plant F is 6.7 MGD. 

 Plant F is one of a few POTWs in the United States to use a five-stage BardenphoTM 

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

system consists of five zones: anaerobic, anoxic, aerobic, anoxic, and reaeration. This process is 

designed to provide efficient, economical removal of BOD5, TSS, nitrogen, and phosphorus. The 

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

is either discharged to a river or reused for irrigation and cooling in the plant’s service area. 

Plant G treats flow mainly from a university and the off-campus student population for a 

total of 1.5 MGD. Plant G’s flow spikes significantly during and after rain events; therefore, 

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

prevent loading dilution. 

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

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

oxidation ditch treatment, secondary clarification, chlorine disinfection (sodium hypochlorite), 

and dechlorination (sodium bisulfite). 

Plant H is located in a community with an above-average percentage of population over 

age 65. According to the 2000 U.S. Census data, 73 percent of the population served by Plant H 

is over age 65. The surrounding area is home to many active adult communities and retirement 

homes. Total flow to the facility is approximately 2 MGD. 
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 hypochlorite. The facility maintains chlorine residual in the treated 

effluent because it is discharged to groundwater percolation beds. The facility is permitted to 

discharge to a river, but rarely does so.

 Plant I is also located in a community with an above-average percentage of population 

over age 65. According to the 2000 U.S. Census data, 25 percent of the population in the county 

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

site contact noted that approximately 50 to 75 percent of the influent flow to Plant I is possibly 

from persons over 65. The surrounding area is home to many active adult communities and 

retirement homes. Total flow to the facility is approximately 1 MGD. 

 Plant I operates three sequencing batch reactors (SBRs) to achieve secondary treatment. 

Treatment consists of screening, grit removal, SBR activated sludge treatment, sand filtration, 

and chlorine disinfection with elemental chlorine. The final effluent is disposed of on on-site 

spray irrigation fields. The facility is also permitted to discharge to a swamp, but rarely does so. 
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

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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) 

D Clarification 2.1 days Yes Yes 

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. SAMPLE COLLECTION

4.1 Sampling Locations and Procedures

 During Stage 1, EPA collected samples of influent, final effluent, and at intermediate 

points in the treatment process. The wastewater was sampled periodically over a 24-hour period 

and the samples were composited for analysis. EPA also collected grab samples of either primary 

or combined sludge. 

 During most of Stage 2, EPA collected samples of influent and final effluent only. EPA’s 

objective during Stage 2 was to identify POTWs with high influent concentrations of CECs, not 

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

lowest flows in the very early morning hours and peak flows in mid-morning. Influent BOD5

concentration follows the flow variation (Metcalf and Eddy, 1978), and EPA assumed that CECs 

concentrations, like the BOD5 concentrations, peak with the flow. EPA decided it could identify 

POTWs with high influent concentrations of CECs by collecting one-time grab samples during 

periods of peak flow. For this reason, during the last three sampling episodes, samples were 

collected as grab samples or manual grab composite samples. EPA did not collect any sludge 

samples during Stage 2. 

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

targeted populations were anticipated to have predictable seasonal migratory patterns. EPA 

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

associated with their student population. Similarly, EPA sampled POTWs with a high percentage 

of populations over 65 during times this population was anticipated to be at their residences. 

EPA avoided sampling these POTWs during summer months and major holidays, when the 

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

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

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

populations may have left the area. All of the sampling in Stage 2 took place outside periods of 

reduced flow. See Table 4-1 for the sampling dates. 

Table 4-1. POTW Sampling Episode Dates 

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 months, the historical information indicated flow remained 

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

holiday months. 

4.1.1 Sampling Locations 

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

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

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

G) or influent channel bar screen (Plants C and I). 
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 treatment units, EPA collected samples at several 

intermediate points. 

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

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

facility. 

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

noted on each of the plant schematics. 

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

Screenings Grit

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 samples collected over a specific period of time (e.g., 

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

entire sampling period. 

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

of the following techniques: 

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

• Flow-weighted sampling: automatic compositors connected to flow meters, 

aliquots collected after predetermined amount of flow passed; or 

• Manual time-/flow-weighted sampling: typical flow pattern determined, aliquots 

collected at intervals ranging from 10 to 20 minutes based on high-, medium-, and 

low-flow periods. 

Time-weighted sampling. At Plant A, automatic compositors were programmed to collect 

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

schedule was intended to reflect the changing wastewater stream as flow changed. 

Flow-weighted sampling. Because the time-based schedule used at Plant A did not seem 

to reflect periods of high flow, EPA used a flow-weighted sampling strategy at Plant B. 

Automatic compositors collected sample aliquots when a preset volume of sample passed 

through the influent channel, as signaled by a flow meter. However, the flow meters used at 

POTW B were sometimes unreliable, and the signal was not always constant. 

15 
Occurrence of Contaminants of Emerging Concern in 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 periods of higher flow. This sampling technique 

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

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

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

updated flow data were provided by POTW personnel. 

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

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

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

pumped into the sample containers using a peristaltic pump. 

 Because automatic sampling equipment could interfere with analyte recoveries for some 

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

containers. Grab samples were collected four times (at 6-hour intervals) during the 24-hour 

sample collection period using a bottle dipper. The grab samples were physically composited by 

the analytical laboratory prior to analysis. 

One-Time Grab Sampling Episodes 

 EPA changed from composite sampling to grab sample collection at Plants G and H. 

Grab sampling was based on the premise that CECs concentrations, like the BOD5

concentrations, peak with the flow. EPA decided it could identify POTWs with high influent 

concentrations of CECs by collecting one-time grab samples during periods of peak flow. 

 EPA identified the peak POTW flow periods (the one to two hours during which POTW 

flow was at its highest) to get the highest percentage of human derived waste in the influent. The 

one-time grab samples were collected directly into the sample containers using a bottle dipper 

when the plant influent flow was at its peak. 

Manual Grab Composite Episodes 

 At Plant I, EPA collected time-weighted, manual grab composite samples at the influent 

and effluent. Because Plant I operates SBRs and effluent flow is not constant, EPA chose not to 

collect one-time grab samples similar to POTWs G and H. Influent and effluent samples were 

collected as time-weighted, manual composite aliquots over one SBR fill period and decant 

period, respectively. The sampled SBR fill period occurred during the peak POTW flow period. 

 At the influent, the manual composite samples were collected into a sample bottle from a 

sample tap then poured into a 10-L composite sample jar. At the end of the compositing period, 

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

used a bottle dipper to collect sample aliquots into a sample bottle. These bottle aliquots were 

poured into two 10-L composite sample jars. At the end of the compositing period, mixed sample 

was poured directly from the 10-L jars into sample bottles. EPA’s sample collection procedures 

are summarized in Table 4-2. 
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 specific quality assurance/quality 

control (QA/QC) procedures for the Nine POTW Study. EPA developed the initial QAPP at the 

start of Stage 1 (QAPP Versions 1 and 2), and revised it prior to the start of Stage 2 sampling 

(QAPP Version 3). The QAPP complies with EPA Requirements for QA Project Plans (QA/R-5) 

(EPA, 2001) and presents the criteria used to review the sampling data collected in the Study. 

4.3 Quality Control Procedures

 Quality assurance/quality control (QA/QC) procedures applicable to the nine sampling 

episodes are outlined in the Quality Assurance Project Plan for the POTW Study (ERG, 2006; 

ERG, 2008). QC practices include collecting and analyzing the following: 

• Equipment blanks; 

• Field duplicates; 

• Laboratory QC volumes; and/or 

• Trip blanks. 
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

18 

4.3.1 Equipment Blanks 

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

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

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

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

containers; the automatic compositor system included tubing, a 15-gallon plastic tank lined with 

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

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

bottle dipper equipment blanks by placing the sample container into the bottle dipper apparatus 

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

sample containers. 

 EPA analyzed equipment blanks for select analytes during each sampling episode. 

Equipment blanks collected at Plants A, B, C, and D were analyzed for semivolatile organic 

compounds and metals. Equipment blanks at Plants E, F, G, H, and I were analyzed for the CECs 

target analytes. EPA compared the concentrations of CECs detected in the equipment blanks to 

the concentrations of CECs detected in the associated samples. See Appendix C for details of 

how EPA adjusted the sample results based on the significance of blank contamination. 

4.3.2 Field Duplicates 

 EPA collected duplicate samples to assess the variability in sample collection, handling, 

preparation, and analysis. Duplicate samples were collected from the same location, at the same 

time, and stored and analyzed independently. 

 EPA collected field duplicates using separate automatic compositors or duplicate grab 

samples collected at the same time as other grab samples. Field duplicates were not collected at 

Plants A, D, G, H, and I. Field duplicates collected at Plants B, C, E, and F were analyzed for all 

CECs target analytes. Results of analysis of duplicate samples have been averaged for 

presentation in Appendix C of this report. 

4.3.3 Laboratory Quality Control Volumes 

 As part of standard laboratory QC, matrix effects on analytical performance are assessed 

through the analysis of matrix spikes and laboratory duplicates. For nonisotope dilution 

procedures, these analyses are conducted on 10 percent of the samples from a given matrix (e.g., 

aqueous, sludge) within a sampling event. Laboratory QC volumes were taken from composite 

volumes collected and poured into separate sample bottles at the same time as sample aliquots 

were prepared, or they were collected as grab samples. 

 EPA collected laboratory QC volumes for at least some of the CECs target analytes at all 

nine POTWs. 

4.3.4 Trip Blanks 

 At some POTWs, trip blanks were collected and analyzed for select analytes to evaluate 

possible contamination during shipment and handling of samples. Sample containers were filled 
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

19 

with Ultra Pure Blank Water DI+TM and shipped with empty sample containers to the POTW and 

then with the collected samples to the analytical laboratories. Trip blanks collected at Plants A, 

B, C, and D were analyzed for volatile organic compounds. Trip blanks collected for Plants E 

and F were analyzed for alkylphenols, APEs, and BPA. 

4.3.5 Quality Control Sample Summary 

 Samplers were to collect one equipment blank for every 10 samples collected, but no less 

than one per sampling episode. EPA collected 19 total equipment blanks for 31 total samples in 

the Nine POTW Study, and met the QAPP QC requirements. 

 In addition, samplers were to collect one duplicate sample per 10 samples collected for 

the program. EPA collected 10 duplicate samples for the 31 total samples, and met the QAPP 

requirements. 

 Table 4-3 lists the QC samples collected for each target analyte family at each POTW 

sampled during the program. 

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

Analyte Plant

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, and 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 analytes containing chlorine are preserved with 

sodium thiosulfate (Na2S2O3). Dissolved thiosulfate converts hypochlorite to chloride ion and 

prevents oxidation of the organic analytes in the sample. For the CECs analytical methods, 

preservation and storage requirements and recommendations are still under development. 

 Because EPA was continuing to develop analytical methods during the Nine POTW 

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

detect PPCPs, steroids/hormones and pesticides suggest some of the target analytes may degrade 

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

days of collection (within 48 hours is strongly encouraged). Extracts should be analyzed within 

40 days of extraction. Freezing of aqueous samples is encouraged to minimize degradation 

(especially if extracting within 48 hours is not practical), in which case samples should be 

extracted within 48 hours of removal from the freezer. Samples should arrive at the laboratory at 

≤6°C. 

 Both methods used to analyze for nonylphenols and alkylphenol ethoxolates required that 

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

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

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

and analysis. The laboratory did not report sample temperatures upon receipt. 

 EPA Method 1614 does not specify holding times associated with PBDEs in aqueous 

sample matrices. The method notes that, if stored in the dark at <6°C, aqueous samples may be 

stored for up to one year. 

 The following tables present the sample collection, preservation, and storage conditions 

used for samples analyzed for CECs: 

• Table 4-4: PPCPs; 

• Table 4-5: Steroids and Hormones; 

• Table 4-6: Alkylphenols, APEs, and BPA; 

• Table 4-7: PBDEs; and 

• Table 4-8: Pesticides and Herbicides. 
21 

Table 4-4. PPCPs: Sample Collection, Preservation, and Storage 

Plant A B C D E F G 

Method 

AXYS MLA-052 

Rev. 2 

AXYS MLA-052 

Rev. 2 

AXYS MLA-052 

Rev. 2 

AXYS MLA-052 

Rev. 2 EPA 1694 EPA 1694 EPA 1694 E

Sample Container for Collection 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L plastic with Teflon lid 

1-L plastic with Teflon lid 

1-L amber plastic with Teflon lid 

1-L awith 

Field Preservation Cool, 0-4°C Cool, 4°C Cool, 4°C Cool, 4°C Cool, ≤6°C; 80 

mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Cool, ≤6°C; 80 mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Cool, ≤6°C; 80 mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Coolmg/L Na2S

chlorprese

Temperature Upon Receipt at Lab 

3-9°C 9 – 12°C 5-11°C, 12-14°C 2°C 2°C 4°C 11°C 

Lab Preservation NH4-EDTA None None None None None None None Storage Procedure Sample 

transferred to 4-L bottle to prevent breakage and stored frozen 

Refrigerated Refrigerated 4°C Stored frozen for 

50 days prior to extraction 

Stored frozen for 45 days prior to extraction 

Stored frozen for 5 days prior to extraction 

Not fextrarecei

Time from Collection to Extraction 

UNK Samples extracted 

12 days after receipt 

Samples extracted 3 days after receipt 

Samples extracted 3 times, 70 days 89 days 98 days after collection 

Samples were extracted within 48 hours of thaw 

Samples were extracted within 48 hours of thaw 

Samples extracted immediately after thawing 

Samptransbeforlab st

Time from Extraction to Analysis 

UNK 7 to 29 days 1 to 6 days 5 to 43 days UNK UNK UNK UNK 

UNK – Unknown. Not reported by laboratory or not recorded in data review narrative. a For Plants E and F, EPA received verbal confirmation from the laboratory that samples arrived at or below 6°C. 
22 

Table 4-5. Steroids and Hormones: Sample Collection, Preservation, and Storage 

Plant A B C D E F G 

Method 

AXYS MLA-057 

Rev. 01 

AXYS MLA-057 

Rev. 01 

AXYS MLA-057 

Rev. 01 

AXYS MLA-057 

Rev. 01 EPA 1698 EPA 1698 EPA 1698 

Sample Container 1-L amber glass 

with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L plastic with Teflon lid 

1-L plastic with Teflon lid 

1-L amber plastic with Teflon lid 

1-plT

Field Preservation No headspace; cool, 

4°C 

Cool, 4°C Cool, 4°C Cool, 4°C Cool, ≤6°C; 80 

mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Cool, ≤6°C; 80 mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Cool, ≤6°C; 80 mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

CmN

chpr

Temperature Upon Receipt at Lab 

3-9°C 9 – 14°C 9 –11°C 15 – 16°C 2°C 2°C 3°C 16

Storage Procedure Stored frozen UNK UNK UNK Stored frozen Stored frozen Stored at -20°C StTime from Collection to Extraction 

5 months 34 days 4–5 days 60 days 57 days 

(extracted within 48 hours after thaw) 

52 days (extracted within 48 hours after thaw) 

Within methodspecified time W

sp

Time from Extraction to Analysis 

≤40 days 18 days 8–17 days 8 days UNK UNK Within methodspecified time W

sp

UNK – Unknown. Not reported by laboratory or not recorded in data review narrative. 
23 

Table 4-6. Alkylphenols, APEs, and BPA: Sample Collection, Preservation, and Storag

Plant A B C D E F G 

Method CRL-MS004 CRL-MS004 CRL-MS004 CRL-MS004 

CRL-MS004; 

ASTM D 7076-

06 a

CRL-MS004; 

ASTM D 7076-

06 a

CRL-MS004; 

ASTM D 7076-

06 a

CR

AST

Sample Container 1-L amber glass 

with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L awith T

Field Preservation Cool, 4°C; HCl to 

pH <2 

Cool, 4°C; H2SO4

to pH <2 

Cool, 4°C; H2SO4

to pH <2 

Cool, 4°C; H2SO4

to pH <2 

Cool, ≤6°C; H2SO4 to pH <2 

Cool, ≤6°C; H2SO4 to pH <2 

Cool, ≤6°C; H2SO4 to pH <2 

Cool, H2SO

Temperature Upon Receipt at Lab 

UNK UNK UNK UNK UNK UNK UNK UNK 

Storage Procedure Refrigerated Refrigerated Refrigerated Refrigerated Refrigerated Refrigerated Refrigerated RefrigTime from Collection to Extraction 

Within the 28-day hold time 

Within the 28-day hold time 

Within methodspecified time Within method- specified time Within method- specified time Within method- specified time All arbitrary hold times were met All ar

times 

Time from Extraction to Analysis 

Within 45 days of extraction 

Within the 40-day hold time 

Within methodspecified time Within the 40- day hold time Within the 40- day hold time Within the 40- day hold time All arbitrary hold times were met. It 

has been shown in cases where reextraction was done, the concentration does not change noticeably within a 2-4 week period if preserved properly. 

All artimes has bin casextracdone, concedoes nnoticea 2-4 if preprope

UNK – Unknown. Not reported by laboratory or not recorded in data review narrative. a ASTM D 7076-06 used on selected samples. 
24 

Table 4-7. PBDEs: Sample Collection, Preservation, and Storage 

Plant A B C D E F G 

Method EPA 1614 draft EPA 1614 draft EPA 1614 draft EPA 1614 draft EPA 1614 EPA 1614 EPA 1614 E

Sample Container 1-L amber glass 

with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L awith 

Field Preservation Cool, 0-6°C; 80 

mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Cool, 0-6°C; 80 mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Cool, 0-6°C; 80 mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Cool, 0-6°C; 80 mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Cool, 0-6°C; 80 mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Cool, 0-6°C; 80 mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Cool, 0-6°C; 80 mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Coolmg/L Na2S

chlorprese

Temperature Upon Receipt at Lab 

UNK 9-14°C 8-11°C 14°C 3°C 4°C 3°C 11°C 

Storage Procedure No storage 

required; extracted and analyzed immediately at lab 

No storage required; extracted and analyzed immediately at lab 

No storage required; extracted and analyzed immediately at lab 

No storage required; extracted and analyzed immediately at lab 

Stored frozen Stored frozen UNK UNK 

Time from Collection to Extraction 

Within methodspecified time Within method- specified time UNK UNK 63 days (extracted within 

48 hours of thaw) 

63 days (extracted within 48 hours of thaw)

Within contractspecified time With

speci

Time from Extraction to Analysis 

Within methodspecified time Within method- specified time UNK UNK UNK UNK Within contract- specified time With

speci

UNK – Unknown. Not reported by laboratory or not recorded in data review narrative. 
25 

Table 4-8. Pesticides: Sample Collection, Preservation, and Storage 

Plant A B C D E F G 

Method 

AXYS MLA035 

and MLA 037 

AXYS MLA035 

and MLA 037 

AXYS MLA035 

and MLA 037 

AXYS MLA035 

and MLA 037 EPA 1699 EPA 1699 EPA 1699 E

Sample Container 1-L amber glass 

with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber glass with Teflon lid 

1-L amber plastic with Teflon lid 

1-L awith 

Field Preservation Cool, 0-4°C; 80 

mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Cool, 4°C Cool, 4°C Cool, 4°C Cool, ≤6°C; 80 

mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Cool, ≤6°C; 80 mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Cool, ≤6°C; 80 mg/L (8 mL/L) Na2S2O3 when 

chlorine was present 

Coolmg/L Na2S

chlorprese

Temperature Upon Receipt at Lab 

3-9°C 9-14°C 3-8°C 14-16°C 3°C 1°C 2°C 12°C 

Storage Procedure Transferred to 4L 

glass jar and stored frozen 

4°C 4°C 4°C Stored frozen; 

extracted within 48 hr of thaw 

Stored frozen; extracted within 48 hr of thaw

4°C 4°C 

Time from Collection to Extraction 

Approx 6 months 7 days 3 days 35 days 56-58 days after 

collection 

53-55 days after collection a

Within methodspecified time With

spec

Time from Extraction to Analysis 

Less than 40 days 

8 days 8 days 26 days UNK UNK Within 40 days 

of extraction 

Withof ex

UNK – Unknown. Not reported by laboratory or not recorded in data review narrative. a Sample 71322 reanalysis extracted 76 days after collection. b Sample 71470: heptachlor, dacthal, simazine, hexazinone, and chlorpyriphos re-analyzed diluted 50 days past extraction. 
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

26 

5. SUMMARY OF OCCURRENCE DATA

 This section summarizes the occurrence of CECs in POTW influent and effluent samples 

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

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

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

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

detected at concentrations greater than the laboratory’s reporting limits, and for which there were 

no laboratory or data quality problems. 

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

amounts of PPCPs, sterols, alkylphenol ethoxylates (APEs), flame retardants (PBDEs), and 

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

effluent sample. 

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

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

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

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

analyte. 

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

classes: 

• PPCPs; 

• Sterols and hormones; 

• Alkylphenols, APEs, and BPA; 

• PBDEs; and 

• Pesticides. 

 These subsections present the compounds detected in POTW influent and effluent 

samples. These subsections also present tables comparing the compounds detected and quantified 

in the influent and effluent based on the general difference between the concentrations 

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

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

2. Quantified2

 in at least one influent sample and one or more effluent samples at 

concentrations at least one order of magnitude less than at least one influent 

sample; and 

3. Quantified3

 in at least one influent sample and one or more effluent samples at 

concentrations similar to influent samples. 

 

2, 3 Only analytes quantified in both influent and effluent samples are included in these comparisons. For example, 

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

specifications (DET) in effluent samples. Albuterol is not included in Table 5-2 which compares pharmaceutical 

influent and effluent concentrations. 
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

27 

 For example, the pharmaceutical acetaminophen, which was detected in all influent 

samples and no effluent samples, was placed in the first category. The pharmaceutical 

ciprofloxacin was quantified in five influent samples, one of which was 15,100 ng/L, and three 

effluent samples, one of which was 36.7 ng/L. Ciproflaxin was placed in the second category. 

EPA cautions that this influent/effluent comparison is not based on the difference between 

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

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

intention of determining treatment effectiveness of the POTWs, nor were sludge samples 

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

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

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

5.1 PPCPs

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

POTW influent collected. Of the 44 PPCPs detected, 27 were in 75% or more of the samples in 

which the particular PPCP was analyzed (see Table 5-1). 

 In POTW effluent samples, 33 PPCPs were detected in at least one sample. Of the 33 

PPCPs detected, 16 were detected in less than 25% of the effluent samples analyzed for the 

PPCP (see Table 5-1). 

 Thirteen PPCPs were detected or quantified in at least one influent sample and no 

effluent samples. Thirteen PPCPs were quantified in at least one influent sample and one or more 

effluent samples at concentrations at least one order of magnitude less than influent samples. 

Seven PPCPs were quantified in at least one influent sample and one or more effluent samples at 

concentrations similar to influent samples. Table 5-2 compares the PPCPs detected in POTW 

influent and effluent samples. 
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 Detected in POTW Influent and Effluentb,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 detected in at least one influent and one effluent sample but were not quantified in 

both influent and effluent samples. Consequently, their influent and effluent concentrations could not be compared 

and they are not included on this table. 

 Many of the PPCPs laboratory results failed to meet the QC specifications of the 

analytical method. Of the 441 results for which the concentration was reported above the 

laboratory-reported detection limit, 54 percent of the results were not qualified in any way and 

are considered accurate. The remaining 46 percent of the results were reported only as detected 

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

other laboratory problems. See Table 5-3 for additional statistics on detections and 

quantifications for PPCP samples. 
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 influent/effluent sample results were DET. 

b

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

5.2 Sterols and Hormones

 All evaluated sterols were detected in all POTW influent samples3

3

 With the exception of one analyte (ergosterol) at one plant. 

. Sterols were detected 

in fewer samples of POTW effluent than influent, but all evaluated sterols were detected in at 

least one sample of effluent (see Table 5-1). 

 Concentrations of all evaluated sterols were much lower in the POTW effluent samples 

than in the influent samples (see Table 5-4).

 Hormones were detected in fewer POTW influent samples than sterols, and when 

detected, the concentrations of hormones were typically much lower than concentrations of 

sterols. Evaluated hormones were not detected in any effluent samples (see Tables 5-4). 

 
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 

Sterolsb 

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 reported above the laboratoryreported detection limit, 58 percent of the results were not qualified in any way and are 

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

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

other laboratory problems. See Table 5-5 for additional statistics on detections and 

quantifications of Steroid and Hormone samples. 
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 influent/effluent sample results were DET. 

b

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

5.3 Alkylphenols, APEs, and BPA

 BPA was not detected in the influent or effluent of any sampled plant. NP was detected in 

each plant influent, additionally, the reporting limits for NP were significantly lower than the 

EPA Water Quality Criteria of 6,600 ng/L. Moreover, nonlyphenol monoethoxylates (NP1EO), 

nonlyphenol diethoxylates (NP2EO), and octylphenol (OP) were occasionally detected. OP and 

NP2EO were never detected in the effluent (see Tables 5-6). 

Table 5-6. Comparison of Alkylphenols, APEs, and BPA Detected in POTW Influent and 

Effluent 

Detected in at Least One Influent 

Sample AND

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 any way and are considered accurate. The remaining 

35 percent of the results were reported only as detected (DET). No numerical value should be 

attached to these results because of poor spike recovery or other laboratory problems. See Table 

5-7 for additional statistics on detections and quantifications of alkylphenols, APEs and BPA. 
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 influent/effluent sample results were DET. 

b

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

5.4 PBDEs

 There are 209 PBDE congeners. For the Nine POTW Study, results were reported for 

nine PBDEs of interest (EPA, 2007a). Note that PBDE-28 and PBDE-33 are treated as one 

analyte in this report because the analytical laboratory reported results for PBDE-28 + PBDE-33. 

 All PBDE congeners evaluated in this study were detected in all POTW influent samples. 

The concentrations of the analyzed congeners are very similar plant to plant, despite the 

differences in the populations served by the POTWs. Concentrations of all congeners of interest 

are much lower in the samples of POTW effluent than in samples of POTW influent (Table 5-8). 

Table 5-8. Comparison of PBDEs Detected in POTW Influent and Effluent 

Detected in at Least One Influent 

Sample AND

Quantified in at Least One Influent Sample 

AND

No Effluent Samples 

One or More Effluent Samples at 

Concentrations at Least One Order of 

Magnitude Less than at Least One 

Influent Sample 

One or More Effluent 

Samples at Concentrations 

Similar to Influent Samples 

None PBDE-28 + PBDE-33 

PBDE-47 

PBDE-99 

PBDE-100 

PBDE-153 

PBDE-154 

PBDE-183 

PBDE-209 

None 

 The concentration of PBDE-209 in preparation blanks was often greater than the method 

quantitation levels (EPA Method 1614 quantitation level of 2 ppt). Because PBDE-209 sample 

results for POTW effluents are close to the method quantitation level, for effluent samples from 

four plants, it was impossible to determine if PBDE-209 detected in the effluent was the result of 

contamination. Consequently, the effluent sample concentrations were reported as not-quantified 

at the quantitation level, adjusted for sample size. See Appendix C. 
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 other CECs analyte families. Of the 156 results for 

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

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

of the results were reported only as detected (DET). No numerical value should be attached to 

these results because of poor spike recovery or other laboratory problems. See Table 5-9 for 

additional statistics on detections and quantifications of PBDEs. 

Table 5-9. Numbers of PBDEs Detected in POTW Influent and Effluent 

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 influent/effluent sample results were DET. 

b

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

5.5 Pesticides

 Of the 62 pesticides, 37 were detected in at least one sample of POTW influent collected 

in this study. Eighteen (18) pesticides were detected in at least one sample of POTW effluent 

(Table 5-1). 

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

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

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

samples. Five pesticides were quantified in at least one influent sample and one or more effluent 

samples at concentrations similar to influent samples. Table 5-10 compares the pesticides 

detected in POTW influent and effluent samples. 
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

38 

Table 5-10. Comparison of Pesticides Detected in POTW Influent and Effluentb,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 cyanizine were detected in POTW effluent 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 pesticides analytical results failed to meet method 

QC specifications in comparison to some of the other CECs analyte families. Of the 238 results 

for which the concentration was reported above the laboratory-reported detection limit, 81 

percent of the results were not qualified in any way and are considered accurate. The remaining 

19 percent of the results were reported only as detected (DET). No numerical value should be 

attached to these results because of poor spike recovery or other laboratory problems. See Table 

5-11 for additional statistics on detections and quantifications of pesticides. 
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

39 

Table 5-11. Numbers of Pesticides 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

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 influent/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. REFERENCES

ASTM, 2006. ASTM International. Standard Test Method for Determination of Nonylphenol, 

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

Diethoxylate in Environmental Waters by Gas Chromatography Mass Spectrometry, 

ASTM D7065 – 06. 2006. 

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

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

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

school/TableA-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.” National Center for Health Statistics. Vital and Health 

Statistics 23 (25). http://www.cdc.gov/nchs/products/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 Agency, Office of Science and Technology. Method 

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

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

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

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

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

EPA, 2007c. U.S. Environmental Protection Agency, Office of Science and Technology. Method 

1698: Steroids and Hormones in Water, Soil, Sediment, and Biosolids by HRGC/HRMS, 

EPA 821-R-08-003. December 2007. 

EPA, 2007d. U.S. Environmental Protection Agency, Office of Science and Technology. Method 

1699: Pesticides in Water, Soil, Sediment, Biosolids, and Tissue by HRGC/HRMS, EPA 

821-R-08-001. December 2007. 

ERG, 2006. Eastern Research Group, Inc. Quality Assurance Project Plan for the POTW Study. 

19 May 2006. 

ERG, 2008. Eastern Research Group, Inc. Quality Assurance Project Plan for the POTW Study. 

13 June 2008. 
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 Boston University. Patterns of Medication Use in 

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

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

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

Appendix A 

CONTAMINANTS OF EMERGING CONCERN (CECs) 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) Chlorotetracycline 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 xb 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 xb 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 included in either Stage 1 or Stage 2 of the Nine POTW Study. 

b Codeine and norgestimate were included in AXYS Method MLA-052 for the analysis of Plant B, C, and D 

samples, but not for Plant A samples. 

 

 Note all compounds listed in Table A-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 samples 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, APEs, 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 Analyte 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-33a 

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, the concentration of PBDE 28 + PBDE 33 presented in this report represents 

the total concentration for these 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 CECs in the Nine POTW Study were developed 

and revised throughout the course of this study. The version of the method used to analyze 

samples from each plant is listed in Table B-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 aDraft EPA Method 1614 

(August 2003) 

CRL-MS004 Rev #2

B AXYS MLA052 a

AXYS Method MLA057 Rev 01 aAXYS Method MLA035 Rev. 04 aDraft EPA Method 1614 

(August 2003) 

CRL-MS004 Rev #2

C AXYS MLA052 a

AXYS Method MLA057 Rev 01 aAXYS Method MLA035 Rev. 04 aDraft EPA Method 1614 

(August 2003) 

CRL-MS004 Rev #2

D AXYS MLA052 a

AXYS Method MLA057 Rev 01 aAXYS Method MLA035 Rev. 04 aDraft 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, Sidney, British Columbia, Canada. 

 Samples collected during Stage 1 of the Study (September 2005 – September 2006) were 

analyzed with draft methods based on procedures developed at contract laboratories. EPA used 

the results of these analyses to develop more sensitive and selective analytical methods for three 

groups of CECs: PPCPs, steroids and hormones, and pesticides. Three new EPA methods 

resulted from this work (EPA 1694, 1698 and 1699). These methods were designed to screen for 

a large number of analytes in a broad range of POTW matrices including influent, effluent, and 

sewage sludge. After single-laboratory validation and peer review, three methods were published 

in December 2007, and EPA used the published methods to analyze samples collected in Stage 2 

of the Nine POTW Study (November 2007 through September 2008). 

 The PBDE (flame retardants) analytical method (EPA Method 1614; EPA, 2007a) was 

developed before the Nine POTW Study began. Although EPA Method 1614 was 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 Under development December 2007

1698 Steroids and Hormones HRGC/HRMS 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, EPA analyzed samples of POTW influent and 

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

5 Chicago Regional Laboratory (CRL). During Stage 2, some samples were also analyzed using 

ASTM Method D 7065-06 (ASTM, 2006), which is based on the EPA Region 5 methods. Table 

B-3 lists these methods. 

Table B-3. CRL Analytical Methods for Alkylphenol-Related Compounds 

CRL Method 

Number 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 are discussed below. Table B-1 lists the version 

of the method used to analyze samples collected during the Nine POTW Study. 

PPCPs 

 A preliminary laboratory procedure (AXYS Method MLA-052) was used to analyze 

samples from Plant A. Plants B, C, and D were analyzed using a more refined laboratory 

procedure (AXYS Method MLA-052 ). An EPA method was under development at the Axys 

laboratory during the analysis of samples collected at Plants B, C, and D. After single-laboratory 

validation and peer review, the method was published as EPA Method 1694 in December 2007 

(EPA, 2007b), and samples from Plants E, F, G, H, and I were analyzed using the published 

method. 

 EPA Method 1694 is designed to identify 73 PPCPs in POTW wastes. The 73 target 

analytes in EPA Method 1694 are divided into four groups (1 through 4). Each group represents 

an LC/MS/MS run. Groups 1, 2, and 3 are extracted under acidic (pH 2) conditions. Groups 1 
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

B-3 

and 2 are run in the positive electrospray ionization (ESI+) mode, but with differing run profiles. 

Group 3 is run in the negative electrospray ionization (ESI-) mode. Group 4 is extracted under 

basic pH 10 conditions and run in the ESI+ mode. Quantitation is achieved using isotope dilution 

and internal standard techniques. 

EPA Method 1694 includes all analytes included in AXYS Method MLA-052 as well as 

an additional 33 analytes. 

 In this report, the PPCP analytes are organized by following groups: 

1. Antibiotics (Analytical Group 1 antibiotics and Analytical Group 2): 

2. Analytical Group 1, other than antibiotics; 

3. Analytical Group 3; and 

4. Analytical Group 4. 

Steroids and Hormones 

 AXYS Method MLA-057 Rev 1 (a preliminary laboratory procedure) was used to 

analyze samples from Plants A, B, C, and D; the procedure consisted of low resolution gas 

chromatography mass spectrometry (GC/MS). 

 An EPA method was under development at the Axys laboratory during the analysis of 

samples collected at Plants A through D, and consisted of gas chromatography combined with 

high resolution mass spectrometry. After single-laboratory validation and peer review, the 

method was published as EPA Method 1698 (EPA, 2007c) in December 2007. Samples from 

Plants E, F, G, H, and I were analyzed using the published method. 

 EPA Method 1698 is designed to identify 27 steroids and hormones in POTW wastes. 

The method requires solvent extraction of the sample, followed by cleanup with a layered 

alumina/florisil column. Following cleanup, the target analytes are derivatized and analyzed by 

GC/HRMS. Quantitation is achieved with isotope dilution and internal standard techniques. 

 One analyte included in AXYS Method MLA-057 Rev 1 is not included in EPA Method 

1698: alpha-zearalanol, an anabolic agent. EPA Method 1698 includes seven analytes not 

included in AXYS Method MLA-057 Rev. 1. 

PBDEs 

 EPA analyzed samples collected during the Nine POTW Study for 8 PBDEs using EPA 

Method 1614 which is HRGC/HRMS. Prior to analysis of samples collected at Plants A, B, C, 

and D the method utilized a 30-meter GC column that, when heated, was suspected to degrade 

several high-molecular-weight congeners such as congener 209. Subsequent to analysis at Plants 

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

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

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

from Plants E, F, G, H, and I were analyzed using the 2007 version of 1614. 
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, and D. An EPA method was under development at the 

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

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

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

in EPA Method 1699. 

 After single-laboratory validation and peer review, EPA published Method 1699 (EPA, 

2007d) in December 2007. Samples from Plants E, F, G, H, and I were analyzed using the 

published method. 

 EPA Method 1699 was initially designed to identify 60 pesticides in the following 

chemical groups: 

• 34 Organochlorine Pesticides; 

• 17 Organophosphorus Pesticides; 

• 7 Triazine Pesticides; and 

• 2 Pyrethroid Pesticides. 

 Method 1699 requires solvent extraction of the sample, followed by cleanup. After 

cleanup, the target analytes are derivatized and analyzed by GC/HRMS. Quantitation is achieved 

with isotope dilution and internal standard techniques. 

 The AXYS Methods MLA-035 Rev. 04 and MLA-037 Rev. 03 analyte lists differed 

between Plant A and Plants B, C, and D. AXYS Method MLA-035 Rev. 04 includes 20 analytes 

not included in EPA Method 1699. EPA Method 1699 includes two analytes not included in 

AXYS Method MLA-035 Rev. 04. 

Alkylphenols, APEs, and BPA 

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

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

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

Appendix C 

CECs 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 Nine POTW Study; sludge sampling efforts were dropped after the 

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

present the results of sample analysis for the following types of CECs: 

• PPCPs; 

• Sterols and hormones; 

• Alkylphenols, APEs, and BPA; 

• PBDEs; and 

• Pesticides. 

 EPA developed Methods 1694, 1698, and 1699 to identify a large number and variety of 

analytes in three complex matrices, POTW influent, sludge and effluent. It is difficult to 

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

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

analytical results failed to meet method quality control (QC) specifications. For each analyte 

family, the percentage of the detected results (i.e., where the concentration was reported above 

the laboratory-reported detection limit) with no QC flags or other data interpretation issues were: 

PPCPs 54 percent (441 detected results) 

Sterols and hormones 58 percent (240 detected results) 

Alkylphenols, APEs, and BPA 65 percent (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 detected with QC flags or other data 

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

concentration. “DET” indicates that the analytes are present in the samples, but 

that the measured concentration was not considered reliable. Results are qualified 

because of QC issues including the following: 

a. Poor spike recoveries including: 

i. Labeled compound recovery (LCR), 

ii. Matrix spike (MS) recovery, 

iii. Initial precision and recovery (IPR), and 

iv. Ongoing precision and recovery (OPR); 

v. Continuous calibration verification (CCV); 

b. Other matrix interference issues; 

c. Calibration issues; and 

d. Blank contamination. 
Occurrence of Contaminants of Emerging Concern in Wastewater from Nine POTWs August 2009 

C-2 

3. Results for which an analyte was not detected at or above the laboratory-reported 

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

quantitation limit in parentheses. 

 Results of analysis of duplicate samples have been averaged for presentation in 

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

following designations and footnotes are used throughout the tables: 

NA 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 critical QC failure including: no/low recovery in matrix 

spikes and other laboratory spikes; matrix-specific effect on LCR; and no 

OPR performed. 

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

both sample results may have been set to NQ. 
C-3 

Table C-1. Occurrence of PPCPs in POTW Influent (ng/L) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

Antibiotics4-Epianhydrochlortetracycline (EACTC) 

NA NA NA NA NQ(519) NQ(472) NQ(2,860) N

4-Epianhydrotetracycline (EATC) 

NA NA NA NA NQ(130) NQ(118) NQ(1,340) 

4-Epichlortetracycline (ECTC) 

NA NA NA NA NQ(313) NQ(272) NQ(194) 

4-Epioxytetracycline (EOTC) NA NA NA NA NQ(51.9) NQ(104) NQ(288) 4-Epitetracycline (ETC) NA NA NA NA DET DET b 412 Anhydrochlortetracycline (ACTC) 

NA NA NA NA NQ(462) NQ(464) NQ(768) 

Anhydrotetracycline (ATC) NA NA NA NA NQ(130) NQ(118) NQ(1,070) Chlorotetracycline (CTC) NQ a 434 NQ a NQ(684) NQ(51.9) NQ(47.2) NQ(77.7) Demeclocycline NA NA NA NA NQ(130) NQ(118) NQ(194) Doxycycline NQ a 2,970 NQ a 2,540 DET NQ(47.2) 724 Isochlortetracycline (ICTC) NA NA NA NA NQ(51.9) NQ(47.2) NQ(77.7) Minocycline NA NA NA NA DET NQ(1,020) NQ(3,090) NOxytetracycline (OTC) NQ(997) NQ(169) NQ a NQ(326) NQ(51.9) NQ(47.2) NQ(77.7) Tetracycline (TC) DET NQ(329) NQ a 234 DET DET 368 Sulfachloropyridazine NQ(59.2) NQ(16.0) EXCLUDE NQ(130) NQ(13.0) NQ(11.8) NQ(19.4) Sulfadiazine NA NA NA NA NQ(13.0) 31.1 NQ(19.4) Sulfadimethoxine DET DET EXCLUDE NQ(24.0) NQ(26.4) NQ(9.09) NQ(16.8) Sulfamerazine DET 12.5 EXCLUDE NQ(65.0) NQ(5.19) 12.6 NQ(7.77) Sulfamethazine DET DET EXCLUDE NQ(26.0) 8.94 NQ(4.72) NQ(7.77) Sulfamethizole DET NQ(3.00) EXCLUDE NQ(24.0) NQ(5.50) NQ(4.72) NQ(7.77) Sulfamethoxazole DET DET EXCLUDE 1,500 DET DET DET Sulfanilamide NA NA NA NA NQ(276) NQ(118) NQ(194) Sulfathiazole DET NQ(6.00) EXCLUDE NQ(56.0) NQ(13.0) NQ(11.8) NQ(19.4) Ciprofloxacin DET NQ(300) DET NQ a 1,440 803 591 Clarithromycin NA NA NA NA 748 384 DET Clinafloxacin NA NA NA NA NQ(123) NQ(47.2) NQ(77.7) Enrofloxacin NQ a NQ(649) NQ(690) NQ(331) NQ(26.0) NQ(23.6) NQ(38.9) 
C-4 

Table C-1 (Continued) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

Erythromycin NQ a 126 119 DET 529 586 2,330 Lomefloxacin NA NA NA NA NQ(26.0) NQ(23.6) NQ(38.9) Norfloxacin NQ(33.8) NQ(1,270) NQ(1,350) NQ(650) NQ(130) NQ(353) NQ(194) Ofloxacin NA NA NA NA 147 505 429 Roxithromycin NQ a NQ(4.00) NQ(4.00) NQ(2.00) NQ(5.50) NQ(2.36) NQ(3.89) Sarafloxicin NQ(51.2) NQ(32.0) NQ a NQ(16.0) NQ(119) NQ(403) NQ(777) Tylosin NQ(79.7) NQ(16.0) NQ(18.0) NQ(17.0) NQ(256) NQ(47.2) NQ(744) NAzithromycin NA NA NA NA DET DET DET Carbadox NQ(50.0) NQ(3.00) NQ(4.00) NQ(3.00) NQ(59.1) NQ(25.7) NQ(19.4) Cefotaxime NA NA NA NA NQ(1,240) NQ(1,150) NQ(786) NCloxacillin NA NA NA NA DET b NQ(123) NQ(38.9) Flumequine NA NA NA NA NQ(13.0) NQ(11.8) NQ(19.4) Lincomycin DET DET NQ(89.0) 19.1 NQ(102) DET DET Ormetoprim NA NA NA NA NQ(5.19) NQ(4.72) NQ(7.77) Oxacillin NA NA NA NA NQ(54.5) NQ(50.1) NQ(38.9) Oxolinic Acid NA NA NA NA NQ(21.1) NQ(10.0) NQ(7.77) Penicillin G NA NA NA NA NQ(26.0) NQ(23.6) NQ(38.9) Penicillin V NA NA NA NA NQ(109) NQ(47.2) DET Trimethoprim DET 195 498 DET DET DET DET Virginiamycin DET NQ(8.00) NQ(8.00) NQ(8.00) DET b NQ(332) NQ(205) NAnalytical Group 1, other than antibiotics1,7-Dimethyl xanthine DET DET DET DET 62,600 19,400 DET Acetaminophen DET DET DET DET 79,300 54,400 129,000 Caffeine DET DET DET 42,100 68,200 52,500 DET Carbamazepine NA NA NA NA DET DET DET Codeine NA NQ(664) NQ(706) NQ(904) DET DET DET Cotinine DET DET DET 2,940 535 2,820 NQ(490) Dehydronifedipine NA NA NA NA DET DET DET Digoxigenin NQ a NQ(126) NQ(134) NQ(134) NQ(553) NQ(431) NQ(605) Digoxin NQ a NQ(1,330) NQ(1,410) NQ(1,410) NQ(757) NQ(630) NQ(194) NDiltiazem DET DET DET DET DET DET DET Diphenhydramine NA NA NA NA DET DET NQ(7.77) a NFluoxetine DET NQ(15.0) DET DET 24.7 58.7 NQ(38.9) 
C-5 

Table C-1 (Continued) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

Miconazole NA NA NA NA DET DET b DET Norgestimate NA NQ(16.0) NQ(17.0) NQ(8.00) NQ(78.8) NQ(104) NQ(38.9) Thiabendazole NA NA NA NA NQ(13.0) 12.4 DET Analytical Group 3Gemfibrozil DET DET DET 1,370 539 4,260 DET Ibuprofen DET DET 7,360 11,600 18,900 16,800 20,500 Naproxen NA NA NA NA 11,300 14,800 DET Triclocarban NA NA NA NA 187 571 4,270 Triclosan NA NA NA NA 996 2,420 4,110 Warfarin NQ(10.6) DET NQ(53.0) DET NQ(13.0) NQ(11.8) NQ(19.4) Analytical Group 4Albuterol DET NQ(31.0) NQ(121) 22.5 6.40 30.6 NQ(24.2) Cimetidine DET 461 452 227 73.1 330 120 Metformin DET NQ(326) EXCLUDE DET 17,400 29,400 36,500 Ranitidine DET 496 EXCLUDE DET 1,610 551 1,870 
C-6 

Table C-2. Occurrence of PPCPs in POTW Effluent (ng/L) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

Antibiotics4-Epianhydrochlortetracycline (EACTC) 

NA NA NA NA NQ(494) NQ(555) NQ(1,780) N

4-Epianhydrotetracycline (EATC) 

NA NA NA NA NQ(124) NQ(342) NQ(470) 

4-Epichlortetracycline (ECTC) 

NA NA NA NA NQ(124) NQ(296) NQ(125) 

4-Epioxytetracycline (EOTC) NA NA NA NA NQ(49.4) NQ(120) NQ(190) 4-Epitetracycline (ETC) NA NA NA NA NQ(49.4) NQ(206) NQ(50.0) Anhydrochlortetracycline (ACTC) 

NA NA NA NA NQ(124) NQ(586) NQ(465) 

Anhydrotetracycline (ATC) NA NA NA NA NQ(124) NQ(313) NQ(510) Chlorotetracycline (CTC) NQ(34.4) <462 a NQ a NQ(673) NQ(49.4) NQ(55.5) NQ(50.0) Demeclocycline NA NA NA NA NQ(124) NQ(139) NQ(125) Doxycycline NQ(372) a <284 a NQ a NQ(641) NQ(49.4) NQ(55.5) NQ(50.0) Isochlortetracycline (ICTC) NA NA NA NA NQ(49.4) NQ(55.5) NQ(50.0) Minocycline NA NA NA NA NQ(494) NQ(1,940) NQ(2,620) NOxytetracycline (OTC) NQ(460) NQ(160) NQ a NQ(320) NQ(49.4) NQ(55.5) NQ(50.0) Tetracycline (TC) NQ(104) 568 NQ a NQ(320) NQ(49.4) NQ(55.5) NQ(50.0) Sulfachloropyridazine NQ(5.86) NQ(14.5) EXCLUDE NQ(16.0) NQ(12.4) NQ(13.9) NQ(12.5) Sulfadiazine NA NA NA NA NQ(12.4) <14.2 NQ(12.5) Sulfadimethoxine NQ(0.885) DET EXCLUDE NQ(3.00) NQ(2.47) NQ(2.78) NQ(2.50) Sulfamerazine NQ(0.245) NQ(7.50) EXCLUDE NQ(8.00) NQ(4.94) NQ(5.55) NQ(5.00) Sulfamethazine NQ(10.6) DET b EXCLUDE NQ(3.00) NQ(4.94) NQ(5.55) NQ(5.00) Sulfamethizole NQ(1.31) NQ(3.00) EXCLUDE NQ(3.00) NQ(4.94) NQ(5.55) 33.5 Sulfamethoxazole DET DET EXCLUDE 9.54 276 1,490 DET Sulfanilamide NA NA NA NA NQ(124) NQ(139) NQ(125) Sulfathiazole NQ(1.52) NQ(6.00) EXCLUDE NQ(7.00) NQ(12.4) NQ(13.9) NQ(12.5) Ciprofloxacin NQ a NQ(284) DET NQ(301) 36.7 161 NQ(219) Clarithromycin NA NA NA NA 89.7 23.9 DET Clinafloxacin NA NA NA NA NQ(49.4) NQ(55.5) NQ(345) Enrofloxacin NQ a NQ(614) NQ(627) NQ(326) NQ(24.7) NQ(27.8) NQ(100) 
C-7 

Table C-2 (Continued) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

Erythromycin NQ(4.99) a 114 115 NQ(9.00) 167 91.8 418 Lomefloxacin NA NA NA NA NQ(24.7) NQ(27.8) NQ(25.0) Norfloxacin NQ(1.21) NQ(1,210) NQ(1,230) NQ(640) NQ(124) NQ(139) NQ(1,170) Ofloxacin NA NA NA NA NQ(12.4) 162 NQ(12.5) Roxithromycin NQ(0.203) a NQ(4.00) NQ(4.00) NQ(2.00) NQ(2.47) NQ(2.78) NQ(2.50) Sarafloxicin NQ(9.80) NQ(31.0) NQ a NQ(16.0) NQ(113) NQ(290) NQ(1,060) Tylosin 45.1 NQ(15.5) NQ(16.0) NQ(17.0) NQ(49.4) NQ(55.5) NQ(307) Azithromycin NA NA NA NA DET DET NQ(12.5) Carbadox NQ(13.5) NQ(3.00) NQ(3.00) NQ(3.00) NQ(12.4) NQ(13.9) NQ(12.5) Cefotaxime NA NA NA NA DET b NQ(846) NQ(361) Cloxacillin NA NA NA NA NQ(93.9) NQ(100) NQ(25.0) Flumequine NA NA NA NA NQ(12.4) NQ(13.9) NQ(12.5) Lincomycin DET NQ(22.0) NQ(91.5) NQ(11.0) NQ(24.7) DET NQ(25.0) Ormetoprim NA NA NA NA NQ(4.94) NQ(5.55) NQ(5.00) Oxacillin NA NA NA NA NQ(24.7) NQ(27.8) NQ(25.0) Oxolinic Acid NA NA NA NA NQ(10.6) NQ(5.55) NQ(5.00) Penicillin G NA NA NA NA NQ(24.7) NQ(27.8) NQ(25.0) Penicillin V NA NA NA NA NQ(49.4) NQ(55.5) NQ(50.0) Trimethoprim NQ(1.14) NQ(15.0) 385 NQ(16.0) NQ(41.1) DET 293 Virginiamycin NQ(1.11) NQ(7.50) NQ(8.00) NQ(8.00) NQ(109) NQ(187) NQ(25.0) Analytical Group 1, other than antibiotics1,7-Dimethyl xanthine NQ(13.1) NQ(1,320) DET b NQ(700) NQ(1,240) NQ(1,390) NQ(1,250) NAcetaminophen NQ(27.3) NQ(32.5) NQ(129) NQ(343) NQ(494) NQ(555) NQ(500) Caffeine NQ(79.4) NQ(303) NQ(309) NQ(322) NQ(124) NQ(139) NQ c Carbamazepine NA NA NA NA DET DET 598 Codeine NA NQ(628) NQ(642) NQ(890) NQ(24.7) DET NQ(25.0) Cotinine NQ(1.41) DET NQ(722) NQ(72.0) 46.0 NQ(127) NQ(83.7) Dehydronifedipine NA NA NA NA NQ(4.94) DET NQ(5.00) Digoxigenin NQ(1,080) NQ(120) NQ(122) NQ(132) NQ(186) NQ(406) NQ(50.0) Digoxin NQ a NQ(1,260) NQ(1,280) NQ(1,390) NQ(124) NQ(139) NQ(125) Diltiazem DET NQ(2.00) DET NQ(2.00) DET DET NQ(5.00) Diphenhydramine NA NA NA NA DET DET NQ(5.00) a NFluoxetine NQ(4.26) DET b DET NQ(8.00) 14.7 24.7 NQ(25.0) 
C-8 

Table C-2 (Continued) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

Miconazole NA NA NA NA NQ(12.4) NQ(13.9) NQ(12.5) Norgestimate NA NQ(15.0) NQ(15.0) NQ(8.00) NQ(98.0) NQ(104) NQ(25.0) Thiabendazole NA NA NA NA <12.8 19.8 DET Analytical Group 3Gemfibrozil DET DET DET NQ(35.0) 18.9 259 DET Ibuprofen NQ(34.6) NQ(87.0) NQ(690) NQ(358) NQ(124) NQ(139) NQ(125) Naproxen NA NA NA NA 75.3 NQ(27.8) NQ(25.0) Triclocarban NA NA NA NA 154 45.4 40.6 Triclosan NA NA NA NA NQ(494) NQ(555) NQ(500) Warfarin NQ(0.797) NQ(1.00) NQ(6.00) NQ(7.00) NQ(12.4) NQ(13.9) NQ(12.5) Analytical Group 4Albuterol DET NQ(30.0) NQ(125) NQ(31.0) NQ(2.83) DET NQ(5.01) Cimetidine NQ(0.0453) NQ(41.0) 374 NQ(21.0) NQ(5.66) DET NQ(5.01) Metformin DET DET EXCLUDE DET 5,420 1,250 3,650 Ranitidine NQ a NQ(7.00) EXCLUDE NQ(8.00) NQ(5.66) DET 7.22 
C-9 

Table C-3. Occurrence of Sterols and Hormones in POTW Influent (ng/L) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

Sterols Beta Sitosterol DET 271,000 DET 239,000 DET DET DET Beta Stigmastanol NA NA NA NA 34,000 27,300 DET Campesterol NA NA NA NA DET 46,600 DET Cholestanol DET 39,700 18,400 35,800 DET 45,700 DET Cholesterol DET 636,000 590,000 745,000 DET DET DET Coprostanol DET 496,000 470,000 366,000 DET DET DET Desmosterol DET 2,320 1,330 1,370 2,870 2,210 DET Epicoprostanol DET 20,100 9,370 19,900 5,780 21,400 DET Ergosterol DET DET NQ(5,230) EXCLUDE 4,490 2,820 DET Stigmasterol DET 17,400 14,800 14,900 DET 37,200 DET Hor mones17 Alpha Estradiol DET NQ(253) NQ(256) NQ(314) NQ(10.9) NQ(10.9) DET N17 Alpha Ethinyl Estradiol 

NQ(351) NQ(253) NQ(256) NQ(628) NQ(13.0) NQ(13.0) NQ(5.07) a N

17 Alpha-Dihydroequilin DET NQ(285) NQ(289) NQ(354) DET b NQ(59.3) NQ(33.2) N17 Beta Estradiol DET NQ(283) NQ(286) NQ(351) NQ(10.9) NQ(10.9) DET Alpha-Zearalanol NQ(347) DET DET NQ(317) NA NA NA Androstenedione NA NA NA NA 510 380 864 NAndrosterone NA NA NA NA DET DET 2,910 Beta Estradiol 3-Benzoate 

DET NQ(263) NQ(266) NQ(653) DET DET NQ(5.07) N

Desogestrel NQ(3,510) NA NA NA NQ(75.0) NQ(71.5) NQ(91.1) NEquilenin NA NA NA NA NQ(5.22) NQ(5.24) NQ(5.07) NEquilin NQ(150) NQ(251) NQ(254) NQ(311) <12.7 NQ(10.7) NQ(17.2) Estriol NA NA NA NA DET DET 212 Estrone DET NQ(256) NQ(259) NQ(317) DET 54.1 63.3 Mestranol NQ(417) NQ(266) DET NQ(329) NQ(48.9) NQ(12.3) NQ(5.07) NNorethindrone <810 DET NQ(80.5) NQ(396) NQ(11.2) DET b NQ(5.07) N
C-10 

Table C-3 (Continued) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

Norgestrel NQ(509) DET DET NQ(395) NQ(606) NQ(21.8) NQ(36.3) NProgesterone NA NA NA NA NQ(212) 118 NQ(191) NTestosterone DET DET DET NQ(659) 917 831 DET 

Note - To analyze influent samples, EPA’s contract laboratory split the sample extract into two portions for analysis of sterols and horm

laboratory used a small portion for sterol analysis and the remaining portion for hormone analysis. The extract is split in this manner to 

anticipated high sterol levels in samples and preserve the laboratory-reported detection limits of the hormone analyses. The laboratory dsamples in this manner because sterols concentrations were anticipated to be much lower in treated effluent. 
C-11 

Table C-4. Occurrence of Sterols and Hormones in POTW Effluent (ng/L) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G P

Sterols Beta Sitosterol NQ(636) a NQ a DET 375 <988 c <663 c NQ(9.64) a NBeta Stigmastanol NA NA NA NA 117 NQ(16.6) NQ(9.64) a NCampesterol NA NA NA NA 148 37.6 NQ(16.1) a NCholestanol 72.1 155 486 NQ(641) 524 40.6 123 Cholesterol NQ(916) a 2,220 15,800 458 2,080 DET DET NCoprostanol 163 699 DET NQ(695) 758 114 1,320 Desmosterol DET <190 1,160 NQ(594) 41.7 NQ(31.2) NQ(32.1) NEpicoprostanol NQ(6.84) NQ(252) <195 NQ(300) 38.5 8.55 DET Ergosterol DET DET DET EXCLUDE NQ(30.9) NQ(30.5) DET NStigmasterol DET 1,300 406 414 <401 c <287 c NQ(3.21) a NHormones 17 Alpha Estradiol NQ(2.08) NQ(257) NQ(300) NQ(306) NQ(5.89) NQ(5.82) NQ(3.21) N17 Alpha Ethinyl Estradiol NQ(3.95) NQ(257) NQ(300) NQ(612) NQ(7.03) NQ(6.94) NQ(3.21) a N17 Alpha-Dihydroequilin NQ(7.99) NQ(289) NQ(337) NQ(344) NQ(19.8) NQ(20.8) NQ(11.4) N17 Beta Estradiol NQ(1.55) NQ(287) NQ(334) NQ(341) NQ(5.89) NQ(5.82) NQ(3.21) a NAlpha-Zearalanol NQ(6.83) NQ(259) NQ(303) NQ(309) NA NA NA Androstenedione NA NA NA NA NQ(31.8) NQ(31.3) NQ(64.1) NAndrosterone NA NA NA NA NQ(6.44) NQ(6.35) NQ(14.1) NBeta Estradiol 3-Benzoate NQ(1.63) NQ(267) NQ(311) NQ(635) NQ(6.01) NQ(5.93) NQ(3.21) NDesogestrel NQ(44.5) NA NA NA NQ(6.58) NQ(16.0) NQ(16.7) NEquilenin NA NA NA NA NQ(2.84) NQ(2.80) NQ(3.21) NEquilin NQ(7.85) NQ(254) NQ(297) NQ(303) NQ(5.78) NQ(5.71) NQ(3.21) NEstriol NA NA NA NA NQ(19.0) NQ(14.4) NQ(33.1) NEstrone NQ(1.18) NQ(259) NQ(303) NQ(309) NQ(6.58) NQ(6.49) NQ(3.21) a NMestranol NQ(1.77) NQ(269) NQ(314) NQ(321) NQ(6.63) NQ(6.55) NQ(3.21) NNorethindrone NQ(13.7) NQ(80.6) NQ(94.0) NQ(386) NQ(6.12) NQ(6.05) NQ(3.21) N
C-12 

Table C-4 (Continued) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G P

Norgestrel NQ(7.65) NQ(80.6) NQ(94.0) NQ(384) NQ(11.6) NQ(11.4) NQ(6.43) NProgesterone NA NA NA NA NQ(86.0) NQ(29.8) NQ(71.1) NTestosterone NQ(8.80) a NQ(269) NQ(314) NQ(641) NQ(33.3) NQ(47.8) NQ(36.5) N

Note - To analyze influent samples, EPA’s contract laboratory split the sample extract into two portions for analysis of sterols and hormlaboratory used a small portion for sterol analysis and the remaining portion for hormone analysis. The extract is split in this manner to 

anticipated high sterol levels in samples and preserve the laboratory-reported detection limits of the hormone analyses. The laboratory dsamples in this manner because sterols concentrations are anticipated to be much lower in treated effluent. 
C-13 

Table C-5. Occurrence of Alkylphenols, APEs, and BPA in POTW Influent (ng/L) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

BPA NQ(5,000) EXCLUDE NQ(610) NQ(1,200) EXCLUDE EXCLUDE NQ(330) NNP2EO NQ(100,000) NQ(53,000) DET 200,000 NQ(1,900) NQ(1,950) NQ(2,000) NNP1EO NQ(50,000) NQ(19,000) DET 100,000 NQ(1,250) NQ(1,300) NQ(1,300) NOP NQ(5,000) NQ(2,000) NQ(400) 13,000 DET DET NQ(220) NNP 39,700 79,000 44,000 78,000 DET DET 5,700 

Table C-6. Occurrence of Alkylphenols, APEs, and BPA in POTW Effluent (ng/L) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

BPA EXCLUDE EXCLUDE NQ(350) NQ(380) NQ(100) NQ(100) NQ c NP2EO EXCLUDE NQ(1,100) NQ(2,100) NQ(2,200) NQ(1,100) NQ(1,100) NQ(1,100) NNP1EO NQ(1,000) 1,100 NQ(1,400) NQ(1,500) NQ(370) NQ(370) NQ(370) NOP NQ(100) NQ(40.0) NQ(230) NQ(250) NQ(40.0) NQ(40.0) NQ(40.0) NNP NQ(500) NQ(250) NQ(1,050) NQ(1,100) NQ(250) <520 c NQ(250) N
C-14 

Table C-7. Occurrence of PBDEs in POTW Influent (ng/L) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

PBDE-28+PBDE-33 0.683 2.17 1.33 1.78 1.11 1.48 0.710 PBDE-47 DET 97.1 78.1 103 DET DET 34.0 PBDE-99 DET 91.1 71.3 96.2 46.6 90.5 18.7 PBDE-100 8.41 20.7 16.6 23.1 10.2 19.3 4.26 PBDE-153 DET 10.6 7.24 10.4 DET DET 1.57 PBDE-154 2.54 8.81 6.08 8.46 DET DET DET PBDE-183 0.746 1.52 1.11 2.16 1.45 1.55 0.485 PBDE-209 EXCLUDE 211 256 225 260 241 149 

Table C-8. Occurrence of PBDEs in POTW Effluent (ng/L) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

PBDE-28+PBDE-33 NQ(0.0538) 0.0652 0.0897 NQ(0.0593) 0.0574 0.0904 NQ(0.153) NPBDE-47 NQ a 1.64 3.37 0.967 DET 0.954 1.49 PBDE-99 NQ a 1.31 3.01 0.781 1.01 0.456 0.787 PBDE-100 NQ(0.0538) 0.265 0.676 0.199 0.221 0.131 0.180 NPBDE-153 NQ(0.0538) 0.138 0.297 0.0810 0.0763 DET NQ(0.153) NPBDE-154 NQ(0.0538) 0.111 0.241 0.0743 0.0649 0.0332 NQ(0.153) NPBDE-183 NQ(0.108) NQ(0.118) NQ(0.125) NQ(0.118) 0.0506 0.0705 NQ(0.305) NPBDE-209 NQ(2.15) NQ(2.36) DET b NQ(2.37) a NQ(7.65) a <12.0 a NQ(6.10) 
C-15 

Table C-9. Occurrence of Pesticides in POTW Influent (ng/L) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

Organochlorine 2,4'-DDD DET 1.83 NQ(6.30) NQ(6.32) NQ(1.44) NQ(1.40) NQ(1.44) 2,4'-DDE NQ(1.07) NQ(3.43) NQ(6.30) NQ(3.16) NQ(1.44) NQ(1.40) NQ(1.44) 2,4'-DDT NQ(1.29) NQ(3.43) 1.00 NQ(3.16) NQ(1.44) NQ(1.40) NQ(1.44) 4,4'-DDD DET 2.66 NQ(6.30) NQ(6.32) NQ(1.44) NQ(1.40) NQ(1.44) 4,4'-DDE DET 2.35 4.00 3.01 <1.50 2.06 NQ(1.44) 4,4'-DDT DET NQ(7.63) 2.00 NQ(3.16) NQ(1.44) NQ(1.40) NQ(1.44) Aldrin <0.293 NQ(6.87) NQ(6.30) NQ(31.6) NQ(4.05) NQ(3.93) NQ(4.32) Alpha-BHC 0.640 NQ(6.87) NQ(6.30) NQ(6.32) NQ(2.89) NQ(2.79) NQ(2.88) Alpha-chlordane <5.06 1.89 DET 12.3 <1.76 3.53 NQ(1.44) Beta-BHC <0.494 NQ(6.87) NQ(6.30) NQ(6.32) NQ(2.89) NQ(2.79) NQ(2.88) Captan EXCLUDE NQ(21.5) EXCLUDE NQ(39.5) EXCLUDE EXCLUDE NQ(24.0) Chlorothalonil EXCLUDE 1.04 NQ(3.94) NQ(7.90) EXCLUDE EXCLUDE NQ(4.80) Cis-Nonachlor <0.625 0.307 NQ(3.15) DET NQ(1.44) NQ(1.40) NQ(1.44) Dacthal NQ(0.200) NQ(2.15) NQ(1.97) NQ(3.95) NQ(0.900) NQ(0.873) NQ(0.959) Delta-BHC NQ(0.474) NQ(6.87) NQ(6.30) NQ(31.6) NQ(2.89) NQ(2.79) NQ(2.88) Dieldrin DET 1.44 1.00 3.08 NQ(1.44) 6.98 3.61 Endosulfan I DET NQ(3.43) NQ a NQ a NQ(4.50) NQ(4.36) NQ(4.80) Endosulfan II NQ a NQ a NQ a NQ(31.6) NQ(4.50) NQ(4.36) NQ(4.80) Endosulfan sulfate NQ(1.20) NQ(3.43) NQ(3.15) NQ(31.6) NQ(1.80) NQ(1.74) NQ(1.92) Endrin NQ(0.518) NQ(3.43) NQ(0.00) NQ(3.16) NQ(1.44) NQ(1.40) NQ(1.44) Endrin Ketone NQ(1.14) NQ(3.43) NQ(3.15) NQ(12.6) NQ(1.80) NQ(1.74) NQ(1.92) Gamma-BHC 1.45 7.14 1.00 1.95 NQ(2.89) NQ(2.79) NQ(2.88) Gamma-chlordane DET 2.60 1.00 16.3 <2.26 6.61 NQ(2.40) Heptachlor DET NQ(3.43) NQ(3.15) NQ(6.32) NQ(1.44) NQ(1.40) NQ(1.44) Heptachlor Epoxide <0.463 0.291 NQ(0.00) 1.46 NQ(1.80) NQ(1.74) NQ(1.92) Hexachlorobenzene EXCLUDE 0.425 NQ(0.00) 1.37 NQ(1.80) NQ(1.74) NQ(1.92) Methoxychlor NQ(3.59) NQ(6.87) DET NQ(15.8) NQ(14.4) NQ(9.44) NQ(8.33) Mirex NQ(0.183) NQ(3.43) NQ(3.15) NQ(63.2) NQ(4.50) NQ(4.36) NQ(4.80) 
C-16 

Table C-9 (Continued) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

Octachlorostyrene NQ(0.272) NQ(1.20) NQ(1.10) NQ(11.1) NQ(1.80) NQ(1.74) NQ(1.92) Oxychlordane NQ(0.630) NQ(6.87) NQ(6.30) NQ(6.32) NQ(2.89) NQ(2.79) NQ(2.88) Pentochloronitrobenzene NQ(0.363) NQ(17.2) NQ(7.87) NQ(79.0) NQ(3.61) NQ(3.49) NQ(3.84) Perthane NQ(20.4) NQ(34.3) DET NQ(126) DET 30.4 NQ(84.2) Tecnazene NQ(0.333) NQ(8.58) NQ(7.87) NQ(39.5) NQ(3.60) NQ(3.49) NQ(3.84) Trans-Nonachlor <3.46 1.50 1.00 7.86 NQ(1.80) 2.01 NQ(1.92) Organophosphorus Azinphos-methyl NQ(38.8) NQ(10.7) NQ(19.7) NQ(98.7) NQ(35.6) NQ(8.72) NQ(9.59) Chlorpyriphos DET 19.3 17.0 NQ(79.0) NQ(3.61) 13.0 NQ(3.84) Chlorpyriphos-oxon NQ(2.07) NQ(8.58) NQ(7.87) DET NQ(3.61) NQ(3.49) NQ(3.84) Diazinon NQ(4.67) 8.89 DET 41.0 NQ(3.61) 71.9 NQ(3.84) Diazinon oxon NQ(1.63) NQ(8.58) NQ(7.87) NQ(158) NQ(3.60) NQ(3.49) NQ(3.84) Disulfoton NQ(26.2) NQ(42.5) NQ(39.0) NQ(78.2) NQ(18.0) NQ(17.5) NQ(19.2) Disulfoton sulfone NQ(0.699) NQ(0.687) NQ(0.630) DET NQ(1.35) NQ(1.31) NQ(1.44) Ethyl-parathion NQ(7.66) NQ(8.58) NQ(7.87) NQ(15.8) NQ(3.60) NQ(3.49) NQ(3.84) Fenitrothion NQ(3.46) NQ(8.58) NQ(7.87) NQ(31.6) NQ(3.61) NQ(3.49) NQ(3.84) Fonofos NQ(1.26) NQ(8.58) NQ(7.87) NQ(39.5) NQ(3.61) NQ(3.49) NQ(3.84) Malathion NQ(70.7) NQ(114) NQ(104) DET NQ(46.8) NQ(45.4) NQ(48.0) Methamidophos NQ(62.3) NQ(60.3) NQ(15.7) DET NQ(45.0) NQ(65.2) NQ(48.0) Methyl-chlorpyriphos DET NQ(10.7) NQ(9.84) NQ(19.7) NQ(4.68) NQ(4.54) NQ(4.80) Methyl-parathion NQ(38.3) NQ(25.8) NQ(23.6) 94.6 NQ(10.8) NQ(10.5) NQ(9.59) Phorate NQ(5.40) NQ(17.2) NQ(15.7) NQ(31.6) NQ(9.00) NQ(8.72) NQ(9.59) Phosmet NQ(8.36) NQ(21.5) NQ(39.4) NQ(79.0) NQ(21.6) NQ(8.73) NQ(9.59) Pirimiphos-methyl NQ(0.736) NQ(8.58) NQ(7.87) NQ(15.8) NQ(3.61) NQ(3.49) NQ(3.84) Pyrethroid Cis-Permethrin NA NA NA NA 25.3 155 NQ(9.59) Cypermethrins <23.2 26.4 52.0 70.5 NQ(9.00) DET NQ(9.59) Permethrin DET 146 176 349 59.0 DET NQ(19.1) Trans-Permethrin NA NA NA NA 33.8 238 9.26 
C-17 

Table C-9 (Continued) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

Triazine Ametryn NQ(1.85) NQ(8.58) NQ(7.87) NQ(15.8) NQ(3.61) NQ(3.49) NQ(3.84) Atrazine DET 87.7 DET DET 35.9 58.9 DET Cyanazine NQ(11.1) NQ(8.58) NQ(7.87) NQ(31.6) NQ(15.7) NQ(17.4) NQ(3.84) Desethyl atrazine DET 27.3 31.0 4.96 58.0 7.84 2.65 Hexazinone NQ(6.16) NQ(10.7) NQ(19.7) NQ(79.0) NQ(4.68) 7.13 NQ(4.80) Metribuzin NQ(3.43) NQ(2.15) NQ(1.97) NQ(7.90) NQ(2.70) NQ(2.62) NQ(2.88) Simazine DET 2.67 DET NQ(15.8) 6.65 NQ(3.49) NQ(3.84) 
C-18 

Table C-10. Occurrence of Pesticides in POTW Effluent (ng/L) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

Organochlorine 2,4'-DDD NQ(0.404) NQ(3.55) NQ(3.17) NQ(3.16) NQ(0.745) NQ(0.699) NQ(0.657) 2,4'-DDE NQ(0.575) NQ(3.55) NQ(3.17) NQ(1.58) NQ(0.745) NQ(1.48) NQ(0.657) 2,4'-DDT NQ(0.452) NQ(3.55) NQ(3.17) NQ(1.58) NQ(0.745) NQ(1.48) NQ(0.657) 4,4'-DDD NQ(0.220) NQ(3.55) NQ(3.17) NQ(3.16) NQ(0.745) NQ(1.48) NQ(0.657) 4,4'-DDE NQ(0.743) NQ(3.55) NQ(3.17) NQ(3.16) NQ(0.745) NQ(1.48) NQ(0.657) 4,4'-DDT NQ(0.468) NQ(3.55) NQ(3.17) NQ(1.58) NQ(0.745) NQ(1.48) NQ(0.657) Aldrin NQ(0.115) NQ(7.09) NQ(6.33) NQ(3.16) NQ(2.09) NQ(1.97) NQ(1.97) Alpha-BHC NQ(0.154) NQ(7.09) NQ(6.33) NQ(3.16) NQ(1.49) NQ(1.40) NQ(1.31) Alpha-chlordane NQ(0.174) NQ(3.55) NQ(3.17) NQ(1.58) NQ(0.745) NQ(0.699) NQ(0.657) Beta-BHC NQ(0.213) NQ(7.09) NQ(6.33) NQ(3.16) NQ(1.49) NQ(1.40) NQ(1.31) Captan NQ(9.46) NQ(22.2) EXCLUDE NQ(19.7) EXCLUDE EXCLUDE NQ(10.9) Chlorothalonil NQ(0.0867) NQ(4.43) NQ(3.95) NQ(3.95) EXCLUDE EXCLUDE NQ(2.19) Cis-Nonachlor NQ(0.216) NQ(3.55) NQ(3.17) NQ(1.58) NQ(0.745) NQ(1.48) NQ(0.657) Dacthal NQ(0.0867) NQ(2.22) NQ(1.98) NQ(1.97) NQ(0.466) NQ(0.437) NQ(0.438) Delta-BHC NQ(0.233) NQ(7.09) NQ(6.33) NQ(3.16) NQ(1.49) NQ(1.40) NQ(1.31) Dieldrin NQ(0.102) 0.273 NQ(0.00) 0.589 NQ(0.745) 1.64 0.888 Endosulfan I 2.06 NQ a NQ a NQ a NQ(2.33) NQ(2.18) NQ(2.19) Endosulfan II NQ(0.429) a NQ a NQ(3.17) NQ(3.16) NQ(2.33) NQ(2.18) NQ(2.19) Endosulfan sulfate 2.86 NQ(3.55) NQ(3.17) NQ(3.16) NQ(0.931) NQ(0.873) NQ(0.876) Endrin NQ(0.229) NQ(3.55) NQ(3.17) NQ(1.58) NQ(0.745) NQ(0.699) NQ(0.657) Endrin Ketone NQ(0.369) NQ(3.55) NQ(4.73) NQ(6.32) NQ(0.931) NQ(0.873) NQ(0.876) Gamma-BHC NQ(0.244) 2.45 1.00 3.84 NQ(1.49) NQ(1.40) NQ(1.31) Gamma-chlordane NQ(0.186) NQ(3.55) NQ(3.17) 0.863 NQ(1.16) NQ(1.09) NQ(1.09) Heptachlor NQ(0.0347) NQ(3.55) NQ(3.17) NQ(3.16) NQ(0.745) NQ(0.699) NQ(0.657) Heptachlor Epoxide NQ(0.143) NQ(3.55) NQ(3.17) 0.471 NQ(0.931) NQ(0.873) NQ(0.876) Hexachlorobenzene EXCLUDE NQ(3.55) NQ(3.17) NQ a NQ(0.931) NQ(0.873) NQ(0.876) Methoxychlor DET DET NQ(6.27) 0.416 NQ(1.63) DET b NQ(0.657) Mirex NQ(0.0657) NQ(3.55) NQ(3.17) NQ(6.32) NQ(2.33) NQ(2.18) NQ(2.19) 
C-19 

Table C-10. (Continued) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

Octachlorostyrene NQ(0.0662) NQ(1.24) NQ(1.11) NQ(1.11) NQ(0.931) NQ(0.873) NQ(0.876) Oxychlordane NQ(0.184) NQ(7.09) NQ(6.33) NQ(3.16) NQ(1.49) NQ(2.96) NQ(1.31) Pentochloronitrobenzene NQ(0.0867) NQ(8.86) NQ(7.91) NQ(7.90) NQ(1.86) NQ(1.75) NQ(1.75) Perthane NQ(0.403) NQ(35.5) NQ(31.7) NQ(63.2) NQ(8.78) NQ(2.18) NQ(2.19) Tecnazene NQ(0.0867) NQ(4.43) NQ(3.95) NQ(3.95) NQ(1.86) NQ(1.75) NQ(1.75) Trans-Nonachlor NQ(0.173) NQ(3.55) NQ(3.17) NQ(1.58) NQ(0.931) NQ(0.873) NQ(0.876) Organophosphorus Azinphos-methyl NQ(6.45) NQ(11.1) NQ(9.88) NQ(9.87) NQ(4.65) NQ(4.37) NQ(4.38) Chlorpyriphos NQ(0.817) NQ(8.86) NQ(7.91) NQ(7.90) NQ(1.86) NQ(1.75) NQ(1.75) Chlorpyriphos-oxon NQ(2.04) NQ(8.86) NQ(7.91) NQ(15.8) NQ(1.86) NQ(1.75) NQ(1.75) Diazinon NQ(0.610) NQ(8.86) 3.50 3.84 <11.9 DET 2.86 Diazinon oxon NQ(0.479) 6.67 NQ(11.8) NQ(15.8) NQ(1.86) NQ(1.75) NQ(1.75) Disulfoton NQ(8.84) NQ(43.9) NQ(58.6) NQ(39.1) NQ(9.31) NQ(18.5) NQ(8.76) Disulfoton sulfone NQ(0.345) NQ(0.709) NQ(0.944) NQ(0.632) NQ(0.698) NQ(0.655) NQ(0.657) Ethyl-parathion NQ(1.48) NQ(8.86) NQ(7.91) NQ(7.90) NQ(1.86) NQ(1.75) NQ(1.75) Fenitrothion NQ(1.66) NQ(8.86) NQ(7.91) NQ(15.8) NQ(1.86) NQ(1.75) NQ(1.75) Fonofos NQ(0.207) NQ(8.86) NQ(7.91) NQ(3.95) NQ(1.86) NQ(1.75) NQ(1.75) Malathion NQ(27.2) NQ(118) NQ(105) NQ(105) NQ(24.2) NQ(48.1) NQ(21.9) Methamidophos NQ(58.6) NQ(8.86) NQ(7.91) DET NQ(34.8) NQ(21.8) NQ(21.9) Methyl-chlorpyriphos NQ(0.0899) NQ(11.1) NQ(9.88) NQ(9.87) NQ(2.42) NQ(2.27) NQ(2.19) Methyl-parathion NQ(21.8) NQ(26.6) NQ(23.7) NQ(23.7) NQ(5.59) NQ(11.1) NQ(4.38) Phorate NQ(1.59) NQ(8.86) NQ(7.91) NQ(15.8) NQ(4.65) NQ(4.37) NQ(4.38) Phosmet NQ(1.26) NQ(22.2) NQ(19.8) NQ(39.5) NQ(4.66) NQ(9.27) NQ(4.38) Pirimiphos-methyl NQ(0.123) NQ(8.86) NQ(7.91) NQ(7.90) NQ(1.86) NQ(1.75) NQ(1.75) Pyrethroid Cis-Permethrin NA NA NA NA NQ(4.65) NQ(4.37) NQ(4.38) Cypermethrins NQ(2.82) NQ(22.2) NQ(19.8) NQ(19.7) NQ(4.66) NQ(9.27) NQ(4.38) Permethrin NQ(0.775) <3.34 6.00 NQ(3.95) NQ(9.26) NQ(8.69) NQ(8.71) Trans-Permethrin NA NA NA NA NQ(2.33) NQ(2.18) NQ(2.19) 
C-20 

Table C-10. (Continued) 

Analyte Plant A Plant B Plant C Plant D Plant E Plant F Plant G 

Triazine Ametryn NQ(0.463) NQ(8.86) NQ(7.91) NQ(7.90) NQ(1.86) NQ(1.75) NQ(1.75) Atrazine DET 60.1 DET DET 32.9 53.8 DET Cyanazine NQ(2.24) NQ(8.86) DET b NQ(15.8) NQ(4.11) NQ(4.54) NQ(1.75) Desethyl atrazine DET 25.0 27.5 6.13 57.2 7.44 1.63 Hexazinone NQ(1.18) NQ(11.1) NQ(9.88) NQ(39.5) 4.09 DET NQ(2.19) Metribuzin NQ(1.17) NQ(2.22) DET b NQ(3.95) NQ(1.40) 1.90 NQ(1.31) Simazine 2.64 2.55 5.00 NQ(7.90) 5.05 NQ(1.75) NQ(1.75)