U.S. Department of the Interior

U.S. Geological Survey

Scientific Investigations Report 2008–5173

In cooperation with the Ohio Water Development Authority; National Park Service; Cities of Aurora, 

Bedford, Bedford Heights, Solon, and Twinsburg; Portage and Summit Counties; and in collaboration 

with the Ohio Environmental Protection Agency

Occurrence of Organic Wastewater Compounds in the 

Tinkers Creek Watershed and Two Other Tributaries 

to the Cuyahoga River, Northeast Ohio
Cover image: View of Tinkers Creek near Dunham Road, Cuyahoga County, Ohio (photograph by John S. Tertuliani, 

U.S. Geological Survey).
Occurrence of Organic Wastewater 

Compounds in the Tinkers Creek 

Watershed and Two Other Tributaries to 

the Cuyahoga River, Northeast Ohio

By J.S. Tertuliani, D.A. Alvarez, E.T. Furlong, M.T. Meyer, S.D. Zaugg, 

and G.F. Koltun

In cooperation with the Ohio Water Development Authority; National Park Service; 

Cities of Aurora, Bedford, Bedford Heights, Solon, and Twinsburg; Portage and 

Summit Counties; and in collaboration with the Ohio Environmental Protection Agency

Scientific Investigations Report 2008–5173

U.S. Department of the Interior

U.S. Geological Survey
U.S. Department of the Interior

DIRK KEMPTHORNE, Secretary

U.S. Geological Survey

Mark D. Myers, Director

U.S. Geological Survey, Reston, Virginia: 2008

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reproduce any copyrighted materials contained within this report.

Suggested citation:

Tertuliani, J.S., Alvarez, D.A., Furlong, E.T., Meyer, M.T, Zaugg, S.D., and Koltun, G.F., 2008, Occurrence of organic 

wastewater compounds in the Tinkers Creek watershed and two other tributaries to the Cuyahoga River, Northeast 

Ohio: U.S. Geological Survey Scientific Investigations Report 2008–5173, 60 p.
iii

Contents

Abstract...........................................................................................................................................................1

Introduction.....................................................................................................................................................2

Purpose and Scope ..............................................................................................................................2

Study Area..............................................................................................................................................5

Methods...........................................................................................................................................................5

Passive Sampling Technology ............................................................................................................5

Polar Organic Chemical Integrative Samplers (POCIS) ........................................................7

Semipermeable Membrane Devices (SPMDs).......................................................................8

Sampling-Site Selection and Sampler Deployment........................................................................8

Streambed-Sediment Sampling .......................................................................................................10

Laboratory Analyses....................................................................................................................................11

Reporting of Data.........................................................................................................................................11

Quality Control..............................................................................................................................................12

Trip Blanks............................................................................................................................................12

Field Replicates...................................................................................................................................13

Reagent and Matrix Spikes...............................................................................................................13

Method Blanks and Surrogate and Internal Standards ...............................................................14

Results. ...........................................................................................................................................................14

Compounds in Water..........................................................................................................................15

Antibiotic Compounds...............................................................................................................15

Pharmaceutical Compounds....................................................................................................16

Wastewater Compounds ..........................................................................................................16

Hydrophobic Compounds .........................................................................................................16

Compounds in Streambed Sediments .............................................................................................18

Pharmaceutical Compounds....................................................................................................18

Wastewater Compounds ..........................................................................................................19

Summary and Conclusions.........................................................................................................................20

References Cited..........................................................................................................................................21

Appendix A. Detailed Analytical Methods and Passive Sampling Theory........................................24

POCIS and SPMD Media Preparation and Extraction..................................................................24

Chemical Analysis of POCIS and SPMD Extracts .........................................................................24

Chemical Analysis of Streambed Sediments .................................................................................25

Passive Sampling Theory ..................................................................................................................26

Estimation of Ambient Water Concentrations.......................................................................26

References Cited.................................................................................................................................27

Appendix B. Organic Wastewater Compound Analytes and Reporting Levels, by Sample 

Media and Analytical Method......................................................................................................28

References Cited.................................................................................................................................36

Appendix C. Quality-Control Data ............................................................................................................37

Appendix D. Organic Wastewater Compounds in Polar Organic Chemical Integrative 

Sampler (POCIS) Extracts .............................................................................................................43

Appendix E. Organic Wastewater Compounds in Semipermeable Membrane Device 

(SPMD) Extracts .............................................................................................................................51

Appendix F. Organic Wastewater Compounds in Streambed Sediments .........................................54
iv

Figures

1–3. Maps Showing—

1. Locations of sampling sites within the Tinkers Creek watershed...............................3

2. Locations of reference sampling sites relative to the Tinkers Creek watershed .....4

3. Land cover in the Tinkers Creek watershed....................................................................6

4. Photographs of passive-sampler canister in stream and with polar organic 

integrative sampler (POCIS) disks removed.............................................................................7

5. Component view of a POCIS disk...............................................................................................7

6. Photograph of lipid-filled polyethylene membrane tube from a semipermeable 

membrane device (SPMD)..........................................................................................................8

7. Schematic of sampling-site locations near the Bedford Heights wastewatertreatment-plant outfall ...............................................................................................................10

8. Graph showing numbers of detections of antibiotic, pharmaceutical, wastewater, 

and hydrophobic compounds in water (as determined by analysis of POCIS and 

SPMD media) upstream and downstream from wastewater treatment plants in the 

Tinkers Creek watershed...........................................................................................................15

9. Graph showing numbers of detections of pharmaceutical and wastewater 

compounds in streambed sediments upstream and downstream from wastewatertreatment plants in the Tinkers Creek watershed .................................................................19

Tables

1. Land-cover percentages in the Tinkers Creek watershed based on 1992 National 

Land Cover Dataset......................................................................................................................5

 2. Wastewater-treatment-plant (WWTP) information and passive-sampler locations........9

3. Matrix of quality-control measures used as a function of media and analytical 

method..........................................................................................................................................12

4. Numbers of detections of chemical compounds in water (as determined by analysis 

of POCIS and SPMD media) and streambed sediments in the Tinkers Creek 

watershed and two other tributaries to the Cuyahoga River, 2006 ....................................14

5. Organic wastewater compounds detected most frequently (>50 percent detections 

in one or more groupings) in water (as determined by analysis of POCIS and SPMD 

media) in the Tinkers Creek watershed and two other tributaries to the Cuyahoga 

River, 2006............................................................................................................................................17

6. Organic wastewater compounds detected most frequently (>50 percent detections 

in one or more groupings) in streambed sediments in the Tinkers Creek watershed 

and two other tributaries to the Cuyahoga River, 2006.........................................................18

B1. Antibiotic method for POCIS extracts, including compound names, uses, classes, 

and Chemical Abstract Service registry numbers for antibiotic compounds ..................28

B2. Pharmaceutical method for POCIS extracts, including compound names, uses, 

classes, and Chemical Abstract Service registry numbers for pharmaceutical 

compounds ..................................................................................................................................29

B3. Wastewater method for POCIS extracts, including compound names, suspected 

endocrine disruptor, CAS number, and possible compound uses......................................30

B4. Hydrophobic method for SPMD extracts, including compound names, types, and 

Chemical Abstract Service registry numbers for hydrophobic compounds ....................32
v

B5. Pharmaceutical method for streambed-sediment samples, including compound 

names, uses, classes, and Chemical Abstract Service registry numbers for 

pharmaceutical compounds .....................................................................................................33

B6. Wastewater method for streambed-sediment samples, including compound 

names, endocrine-disrupting potential, and possible compound uses.............................34

C1. Summary of results for analysis of Polar Organic Chemical Integrative Sampler 

(POCIS) extracts by the antibiotic, pharmaceutical, and wastewater methods in 

trip blanks collected in Tinkers Creek and its tributaries and two other tributaries 

of the Cuyahoga River in 2006...................................................................................................37

C2. Summary of results for analysis of Semipermeable Membrane Device (SPMD) 

extracts by the hydrophobic method in trip blanks collected in Tinkers Creek and 

its tributaries and two other tributaries of the Cuyahoga River in 2006 ............................37

C3. Results for analysis of Polar Organic Chemical Integrative Sampler (POCIS) extracts 

by the antibiotic, pharmaceutical, and wastewater methods for replicate POCIS 

deployed in Tinkers Creek in 2006............................................................................................38

C4. Results for analysis of Semipermeable Membrane Device (SPMD) extracts by the 

hydrophobic method for replicate SPMDs deployed in Tinkers Creek in 2006 ................39

 C5. Summary of results for analysis of streambed-sediment replicates by the pharmaceutical and wastewater methods for samples collected in Tinkers Creek in 2006 .......40

C6. Summary of reagent-water spike-recovery data for wastewater compounds ...............41

C7. Summary of spike-recovery data for pharmaceutical compounds in streambedsediment samples collected in Tinkers Creek and its tributaries and two other 

tributaries to the Cuyahoga River in 2006 ...............................................................................42

D1. Results of analysis of POCIS extracts by the antibiotic method for POCIS deployed 

in Tinkers Creek and its tributaries and two other tributaries to the Cuyahoga River 

in 2006 ...........................................................................................................................................43

D2. Summary of results for analysis of POCIS extracts by the antibiotic method for 

POCIS deployed in Tinkers Creek and its tributaries and two other tributaries to the 

Cuyahoga River in 2006..............................................................................................................44

D3. Results for analysis of POCIS extracts by the pharmaceutical method for POCIS 

deployed in Tinkers Creek and its tributaries and two other tributaries to the 

Cuyahoga River in 2006..............................................................................................................45

D4. Summary of results for analysis of POCIS extracts by the pharmaceutical method 

for POCIS deployed in Tinkers Creek and its tributaries and two other tributaries 

to the Cuyahoga River in 2006...................................................................................................46

D5. Results for analysis of POCIS extracts by the wastewater method for POCIS 

deployed in Tinkers Creek and its tributaries and two other tributaries to the 

Cuyahoga River in 2006..............................................................................................................47

D6. Summary of results for analysis of POCIS extracts by the wastewater method 

for POCIS deployed in Tinkers Creek and its tributaries and two other tributaries 

to the Cuyahoga River in 2006...................................................................................................49

E1. Results for analysis of SPMD extracts by the hydrophobic method for SPMDs 

deployed in Tinkers Creek and its tributaries and two other tributaries to the 

Cuyahoga River in 2006..............................................................................................................51

E2. Summary of results for analysis of SPMD extracts by the hydrophobic method for 

SPMDs deployed in Tinkers Creek and its tributaries and two other tributaries 

to the Cuyahoga River in 2006...................................................................................................53
vi

Tables—Continued

F1. Results for analysis of streambed-sediment samples by the pharmaceutical 

method for samples collected in Tinkers Creek and its tributaries and two other 

tributaries to the Cuyahoga River in 2006 ...............................................................................54

F2. Summary of results for analysis of streambed-sediment samples by the pharmaceutical method for samples collected in Tinkers Creek and its tributaries and 

two other tributaries to the Cuyahoga River in 2006.............................................................55

F3. Results for analysis of streambed-sediment samples by the wastewater method 

for samples collected in Tinkers Creek and its tributaries and two other tributaries 

to the Cuyahoga River in 2006...................................................................................................56

F4. Summary of results for analysis of streambed-sediment samples by the wastewater method for samples collected in Tinkers Creek and its tributaries and 

two other tributaries to the Cuyahoga River in 2006.............................................................59

Conversion Factors and Abbreviations

Multiply By To obtain

Length

millimeter (mm) 0.03937 inch (in.)

centimeter (cm) 0.3937 inch (in.)

mile (mi) 1.609 kilometer (km)

Area

square centimeter (cm2

) 0.155 0 square inch (in2)

square mile (mi2

) 2.590 square kilometer (km2)

Volume

liter (L) 0.2642 gallon (gal)

Flow rate

million gallons per day 

(Mgal/d)

 0.04381 cubic meter per second 

(m3

/s)

cubic foot per second (ft3

/s) 0.02832 cubic meter per second 

(m3

/s)

Mass

gram (g) 0.03527 ounce, avoirdupois (oz)

kilogram (kg) 2.205 pound avoirdupois (lb)

Pressure

pascal (Pa) 0.0001450 pound-force per square inch 

(lbf/in2

)

Temperature in degrees Celsius (°C) may be converted to degrees Fahrenheit (°F) as follows:

°F = (1.8 × °C) + 32

Concentrations of compounds in polar organic chemical integrative sampler (POCIS) extracts 

are given in nanograms (ng) per POCIS. Concentrations of compounds in semipermeable 

membrane device (SPMD) extracts are given in nanograms per liter (ng/L). Estimated 

concentrations of compounds in water are given in milligrams per liter (mg/L). Concentrations 

of compounds in sediment are given in micrograms per kilogram (μg/kg). There are 1,000 

micrograms in a gram and 1,000 nanograms in a microgram. 

Amounts and concentrations of analytical reagents are given in milliliters (mL), microliters (μL), 

and nanograms (ng) and as micrograms per liter (μg/L), nanograms per microliter (ng/μL), and 

millimolar (mM). 
Occurrence of Organic Wastewater Compounds in the 

Tinkers Creek Watershed and Two Other Tributaries to the 

Cuyahoga River, Northeast Ohio 

By J.S. Tertuliani, D.A. Alvarez, E.T. Furlong, M.T. Meyer, S.D. Zaugg, and G.F. Koltun

Abstract 

The U.S. Geological Survey—in cooperation with the 

Ohio Water Development Authority; National Park Service; 

Cities of Aurora, Bedford, Bedford Heights, Solon, and Twinsburg; and Portage and Summit Counties—and in collaboration 

with the Ohio Environmental Protection Agency, did a study to 

determine the occurrence and distribution of organic wastewater compounds (OWCs) in the Tinkers Creek watershed in 

northeastern Ohio. In the context of this report, OWCs refer 

to a wide range of compounds such as antibiotics, prescription 

and nonprescription pharmaceuticals, personal-care products, 

household and industrial compounds (for example, antimicrobials, fragrances, surfactants, fire retardants, and so forth) and 

a variety of other chemicals.

Canisters containing polar organic integrative sampler 

(POCIS) and semipermeable membrane device (SPMD) 

media were deployed instream for a 28-day period in May and 

June 2006 at locations upstream and downstream from seven 

wastewater-treatment-plant (WWTP) outfalls in the Tinkers 

Creek watershed, at a site on Tinkers Creek downstream from 

all WWTP discharges, and at one reference site each in two 

nearby watersheds (Yellow Creek and Furnace Run) that drain 

to the Cuyahoga River. Streambed-sediment samples also were 

collected at each site when the canisters were retrieved. 

POCIS and SPMDs are referred to as “passive samplers” 

because they sample compounds that they are exposed to 

without use of mechanical or moving parts. OWCs detected 

in POCIS and SPMD extracts are referred to in this report 

as “detections in water” because both POCIS and SPMDs 

provided time-weighted measures of concentration in the 

stream over the exposure period. Streambed sediments also 

reflect exposure to OWCs in the stream over a long period of 

time and provide another OWC exposure pathway for aquatic 

organisms. 

Four separate laboratory methods were used to analyze 

for 32 antibiotic, 20 pharmaceutical, 57 to 66 wastewater, 

and 33 hydrophobic compounds. POCIS and streambedsediment extracts were analyzed by both the pharmaceutical 

and wastewater methods. POCIS extracts also were analyzed 

by the antibiotic method, and SPMD extracts were analyzed 

by the hydrophobic-compound method. Analytes associated 

with a given laboratory method are referred to in aggregate by 

the method name (for example, antibiotic-method analytes are 

referred to as “antibiotic compounds”) even though some analytes associated with the method may not be strictly classified 

as such. In addition, some compounds were included in the 

analyte list for more than one laboratory method. For a given 

sample matrix, individual compounds detected by more than 

one analytical method are included independently in counts 

for each method.

A total of 12 antibiotic, 20 pharmaceutical, 41 wastewater, and 22 hydrophobic compounds were detected in water 

at one or more sites. Eight pharmaceutical and 37 wastewater compounds were detected in streambed sediments. The 

numbers of detections at reference sites tended to be in the low 

range of detection counts observed in the Tinkers Creek watershed for a given analytical method. Also, the total numbers of 

compounds detected in water and sediment at the reference 

sites were less than the total numbers of compounds detected 

at sites in the Tinkers Creek watershed.

With the exception of hydrophobic compounds, it was 

common at most sites to have more compounds detected in 

samples collected downstream from WWTP outfalls than in 

corresponding samples collected upstream from the outfalls. 

This was particularly true for antibiotic, pharmaceutical, and 

wastewater compounds in water. In contrast, it was common to 

have more hydrophobic compounds detected in samples collected upstream from WWTP outfalls than downstream.

Caffeine, fluoranthene, N,N-diethyl-meta-toluamide 

(DEET), phenanthrene, and pyrene were detected in water 

at all sites in the Tinkers Creek watershed, irrespective of 

whether the site was upstream or downstream from a WWTP. 

Some, but not all of these compounds, also were detected in 

water at the reference sites; however, concentrations generally 

were at the low end of the range of concentrations observed in 

the Tinkers Creek watershed.

Carbamazepine, sulfamethoxazole, trimethoprim, and 

hexahydrohexamethylcyclopentabenzopyran (HHCB) were 

detected in water at 100 percent of the sites downstream 

from WWTP outfalls, yet their frequency of detection at sites 
2 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

upstream from outfalls was statistically smaller (occurring 

in about 29 percent or less of the samples). None of these 

compounds were detected in water at the Yellow Creek reference site, and only two of the compounds (carbamazepine 

and sulfamethoxazole) were detected at the Furnace Run site. 

HHCB, a synthetic musk used in some personal care products, 

has been shown to demonstrate antiestrogenic activity and is 

thought to disrupt endocrine function in fish.

Fifteen wastewater compounds (2,6-dimethylnaphthalene, 2-methylnaphthalene, 3-methyl-1H-indole, anthraquinone, acetophenone, benzo[a]pyrene, β-sitosterol, bis(2-ethylhexyl) phthalate, carbazole, cholesterol, fluoranthene, indole, 

naphthalene, p-cresol, and pyrene) were detected in streambed 

sediments at all sites in the Tinkers Creek watershed, irrespective of whether the site was upstream or downstream from 

a WWTP. Three of the fifteen compounds (benzo[a]pyrene, 

bis(2-ethylhexyl) phthalate, and p-cresol) are known or suspected endocrine disruptors.

Many of the pharmaceutical compounds detected in sediment also were detected in water. One notable exception was 

miconazole, which was detected in more than a quarter of the 

streambed-sediment samples yet never detected in water. In 

contrast, some pharmaceutical compounds (such as trimethoprim and carbamzepine) that were detected in water at all sites 

downstream from WWTP outfalls were either not detected or 

detected at a much lower frequency in streambed sediments. 

Introduction

Treated wastewater commonly contains organic wastewater compounds (OWCs) such as antibiotics, prescription 

and nonprescription pharmaceuticals, personal-care products, 

household and industrial compounds (for example, antimicrobials, fragrances, surfactants, fire retardants, and so forth) and 

a variety of other chemicals (Spongberg and Witter, 2008). 

Some of the same OWCs present in treated wastewater are 

also delivered to streams and lakes through other environmental pathways. Many OWCs are characterized as “contaminants 

of emerging concern” because they currently are not included 

in routine monitoring programs but may be candidates for 

future regulation once more becomes known about their toxicity and health effects (Glassmeyer, 2007). 

OWCs frequently are present in streams receiving discharge from wastewater-treatment plants (WWTPs) (Ashton 

and others, 2004; Glassmeyer and others, 2005; Herberer, 

2002; Kolpin and others, 2002) and some OWCs are sufficiently persistent that they, or their degradates, are being 

found in ground water, lakes, and reservoirs in the United 

States (Barnes and others, 2008; Focazio and others, 2008; 

Herberer and others, 2001; Kolpin and others, 2002, 2004). In 

fact, Kolpin and others (2002) reported detections of at least 

one OWC in 80 percent of 139 streams sampled in 30 U.S. 

states. Urban streams and ground water may be particularly 

vulnerable to OWC contamination because of the myriad of 

potential sources of OWCs in such highly engineered systems 

(Sprague and Battaglin, 2004). For example, Rowe and others 

(2004) reported that low concentrations of at least one OWC 

were present in 76 percent of the shallow urban water wells 

sampled in the Great and Little Miami River Basins in Ohio. 

In addition, that study concluded that the number of OWCs 

detected increased with increasing amounts of urban land use 

(Rowe and others, 2004).

Because OWCs are continually released into the environment (frequently in complex mixtures), there is considerable 

concern about the effect of chronic exposure on aquatic biota 

(Sumpter and Johnson, 2005). Several common OWCs are 

known or suspected to disrupt or influence endocrine function in 

fish, which can cause reproductive problems and other anomalies (Sumpter and Johnson, 2005). Some OWCs have been 

shown to survive conventional water-treatment processes and 

persist in drinking-water supplies (Stackelberg and others, 2004, 

2007), yet the prevalence and potential human-health effects of 

consuming low concentrations of mixtures of OWCs is largely 

unknown. Other human-health concerns include the presence of 

antibiotics in water supplies and the potential for the development of antibiotic resistant strains of bacteria (Kummerer, 2004; 

Lee and others, 2004; Sando and others, 2006). 

The U.S. Geological Survey—in cooperation with the 

Ohio Water Development Authority; National Park Service; 

Cities of Aurora, Bedford, Bedford Heights, Solon, and Twinsburg; and Portage and Summit Counties—and in collaboration 

with the Ohio Environmental Protection Agency, investigated 

the occurrence and distribution of OWCs in the Tinkers Creek 

watershed and two other tributaries to the Cuyahoga River. 

The Tinkers Creek watershed was chosen for study in response 

to biological surveys by the Ohio Environmental Protection 

Agency (Ohio EPA). Those surveys indicated that although the 

available habitat in Tinkers Creek and its tributaries was generally adequate, the fish population was impaired (based on 

a comparison of habitat and biological indices to ecoregional 

expectations); yet, conventional water-quality data did not 

fully explain the impairment (Ohio Environmental Protection 

Agency, 2003). Because effluent from WWTPs constitutes a 

continuous and sometimes large proportion of the flow in Tinkers Creek and its tributaries (sometimes greater than or equal 

to 80 percent), there was concern that OWCs in wastewater 

may have contributed to the impairment of the fish population. 

However, no data were available on the occurrence or distribution of OWCs in the Tinkers Creek watershed that could 

support or refute that concern. To address that concern, this 

study focuses primarily on identifying the presence of OWCs 

in streams near WWTP outfalls.

Purpose and Scope

The purpose of this report is to describe the methods and 

results of the USGS study on the occurrence and distribution of 

OWCs in the Tinkers Creek watershed and at reference sites on 

two other tributaries to the Cuyahoga River (figs. 1 and 2). 
Introduction 3

Figure 1. Locations of sampling sites within the Tinkers Creek watershed.
4 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Figure 2. Locations of reference sampling sites relative to the Tinkers Creek watershed.
Methods 5

The water results are based on a 28-day May–June 2006 

exposure period, during which a total of 20 canisters (7 on the 

mainstem of Tinkers Creek, 11 on tributaries to Tinkers Creek, 

and 2 on nearby tributaries to the Cuyahoga River) were 

deployed that contained both polar organic chemical integrative sampler (POCIS; Alvarez and others, 2004) and semipermeable membrane device (SPMD; Huckins and others, 2002) 

passive-sampler media. Streambed-sediment samples also 

were collected at each site when the canisters were retrieved. 

Passive-sampler media and streambed sediments were subsequently analyzed for a 32 antibiotic, 20 pharmaceutical, 57 to 

66 wastewater, and 33 hydrophobic compounds. Considerable 

text is devoted to discussion of POCIS and SPMD technologies, both of which are relatively new technologies for surface-water- and ground-water-quality assessments, particularly 

relating to OWCs. Also, appendixes are provided that contain 

detailed information on analytical methods, passive-sampler 

theory, and quality assurance and laboratory results.

Study Area

Tinkers Creek originates in northwest Portage County 

and flows west to northwest through Summit County and then 

into Cuyahoga County, where it eventually discharges to the 

Cuyahoga River near Independence, Ohio (figs. 1–2). Tinkers 

Creek is the largest tributary to the Cuyahoga River, with a 

drainage area of 96 mi2. Long-term (1963–2006) mean annual 

streamflow for the USGS streamgage on Tinkers Creek at 

Bedford (04207200), located 5.5 mi upstream from the mouth, 

is 137 ft3/s. 

The study focused on the Tinkers Creek watershed in 

which seven WWTPs are located (fig. 1). Several tributaries 

enter Tinkers Creek within this area. Pond Brook, the largest tributary to Tinkers Creek, receives discharge from the 

Aurora Shores WWTP and indirectly (by way of an unnamed 

tributary) from the Aurora Westerly WWTP. Other tributaries include Beaver Meadow Run, which receives discharge 

from the Solon WWTP; Hawthorne Creek, which indirectly 

receives discharge from the Bedford Heights WWTP (the 

WWTP discharges to an unnamed tributary to Hawthorne 

Creek near its confluence with Hawthorne Creek); and Wood 

Creek, which receives discharge from the Bedford WWTP.

Land cover in the watershed varies along the length of 

Tinkers Creek (table 1 and fig. 3). About 47 percent of the 

land in the watershed is classified as wetland or forest, 21 

percent as agricultural, and about 27 percent as residential 

or commercial/industrial/transportation (table 1). Land use 

in the northern half of the watershed tends to be more urban 

and developed than in the southern half (fig. 3). The seven 

WWTPs in the study are in or near one of the larger cities 

in the Tinkers Creek watershed. The population ranges from 

approximately 11,375 people in Bedford Heights to approximately 21,800 people in Solon (U.S. Census Bureau, 2000). 

Like Tinkers Creek, the streams where reference sites were 

established are tributary to the Cuyahoga River (fig. 2). Both 

Furnace Run and Yellow Creek discharge to the Cuyahoga 

River within the boundary of the Cuyahoga Valley National 

Park. Furnace Run, which drains about 20.4 mi2

, flows 

through park lands in the lower third of the watershed. In 

contrast, almost all of Yellow Creek’s 31.0-mi2 drainage area 

is outside of the park. The percentages of the Furnace Run and 

Yellow Creek watersheds classified as residential or commercial/industrial/transportation land covers, 6.8 and 12.4 percent, 

respectively, are less than half that of the Tinkers Creek watershed. The predominant land cover in both watersheds is forest, 

followed by agricultural classes.

Methods

The occurrence of OWCs was assessed by analyzing sequestration media from passive sampling devices and 

by analyzing streambed sediments. The following sections 

describe (1) the passive sampling technologies, (2) site-selection and sampler-deployment criteria, (3) methods used to collect streambed sediments, (4) laboratory analytical techniques, 

and (5) quality-control procedures.

Passive Sampling Technology

Passive samplers are nonmechanical devices consisting 

of an encased medium that can accumulate compounds of 

interest over time (Alvarez and others, 2004, 2008; Chambers 

and others, 2006; Huckins and others, 2002). The advantages 

of the passive-sampler approach include the ability to integrate 

exposure over a range of hydrologic conditions and the ability 

to concentrate ultratrace to trace levels of chemicals, which 

Table 1. Land-cover percentages in the Tinkers Creek 

watershed based on 1992 National Land Cover Dataset1.

[Percentages add up to less than 100 percent because of independent 

rounding]

Land cover Percentage 

of watershed

Open water 1.9

Low-intensity residential 16.1

High-intensity residential 1.8

Commercial/Industrial/Transportation 9.3

Transitional 0.5

Deciduous forest 40.3

Evergreen forest 1.0

Mixed forest 0.5

Grasslands/Herbaceous 0.1

Pasture/Hay 14.0

Row crops 6.9

Urban/Recreational grasses 1.4

Wetlands 5.2

1

U.S. Geological Survey (2000).
6 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Figure 3. Land cover in the Tinkers Creek watershed.
Methods 7

can result in a detectable amount of a compound that might 

otherwise be present in streamwater grab samples at concentrations below detection (Chambers and others, 2006; Alvarez 

and others, 2004). Integrating and accumulating exposure over 

time also increases the likelihood of detecting chemicals that 

are present in the stream only sporadically.

Passive-sampler media were packaged together in a protective plastic canister for deployment in the streams (fig. 4). 

The canisters have slotted openings at both ends to facilitate 

the flow of water over the media.

Polar Organic Chemical Integrative Samplers 

(POCIS) 

The Polar Organic Chemical Integrative Sampler 

(POCIS) is designed to sample water-soluble (polar or 

hydrophilic) organic chemicals from aqueous environments. 

The POCIS is a passive integrative sampler that yields 

time-weighted concentrations of chemicals over deployment 

periods ranging from weeks to months. The POCIS samples 

chemicals in the dissolved phase, mimicking the respiratory 

exposure of aquatic organisms (Alvarez and others, 2004). 

Each POCIS disk consists of a solid-phase sorbent or 

mixture of sorbents sandwiched between two sheets of a 

microporous polyethersulfone membrane (fig. 5). The type of 

sorbent used depends on the specific chemicals or chemical 

classes of interest. The membranes allow water and dissolved 

chemicals to pass through to the sorbent material (where the 

chemicals are sequestered) while excluding particulate matter 

such as suspended detritus and sediment. The membranes are 

resistant to biofouling, which can reduce the amount of chemical sampled. The samplers deployed in this study contained six 

POCIS disks.

Figure 4. Photographs of passive-sampler canister in stream and with polar organic integrative sampler (POCIS) disks removed.

Figure 5. Component view of a POCIS disk.
8 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Two configurations of the POCIS, differing in the type of 

sorbents incorporated, were used in this study. The “pesticide” 

POCIS is the original design optimized for the sampling of 

many pesticides, biogenic and synthetic hormones, wastewater-related compounds, and other water-soluble organic chemicals. The “pharmaceutical” POCIS was designed to permit the 

recovery of certain classes of chemicals that contain multiple 

functional groups (as do many pharmaceuticals). The use of 

both configurations during the Tinkers Creek study permitted 

a broad range of OWCs to be sampled. Some overlap exists in 

the types of chemicals sampled by each configuration (Alvarez 

and others, 2004, 2007; Jones-Lepp and others, 2004; Petty 

and others, 2004), so 11 compounds have more than 1 result 

reported.

Semipermeable Membrane Devices (SPMDs) 

Semipermeable membrane devices (SPMDs) were used 

in conjunction with the POCIS. The SPMD is designed to 

sample lipid or fat-soluble (nonpolar or hydrophobic) semivolatile organic chemicals from water and air (Huckins and others, 2002, 2006). The SPMD is an integrative sampler similar 

in function to the POCIS device. The SPMD consists of a 

small volume of a neutral, high-molecular-weight lipid, such 

as synthetic triolein (as used for this study), which is contained 

in a thin-walled, low-density polyethylene membrane tube 

(fig. 6). The semipermeable membrane allows the nonpolar 

chemicals to pass through to the lipid, where the chemicals 

are concentrated. Larger molecules and particulate matter are 

excluded.

SPMDs were used to gather information on selected 

chemicals that are more hydrophobic than those sampled for 

by POCIS (Alvarez and others, 2004, 2007; Jones-Lepp and 

others, 2004; Petty and others, 2000). Chemicals sampled by 

SPMDs include hydrophobic, bioavailable organic chemicals 

such as polychlorinated biphenyls (PCBs), polycyclic aromatic 

hydrocarbons (PAHs), organochlorine pesticides, dioxins and 

furans, selected organophosphate and pyrethroid pesticides, 

and other nonpolar organic chemicals. 

Sampling rates (the liters of water extracted per day) can 

vary with changes in water flow, turbulence, and temperature 

and as a function of the amount of biofilm on the surface areas 

of the membrane tube. A performance reference compound 

(PRC) approach was used to account for site-specific environmental factors that can affect sampling rates (Huckins and others, 2002). A PRC compound was added to the SPMD during 

its construction. The amount of PRCs lost to the surrounding 

water during deployment was used to adjust SPMD-derived 

sampling rates. 

Sampling-Site Selection and Sampler 

Deployment

Sampling sites were established upstream and downstream from seven WWTP outfalls in the Tinkers Creek watershed (table 2). In one case (at the Bedford Heights WWTP), a 

third site was established to sample a second upstream location. Sampling sites also were established on Tinkers Creek 

at Dunham Road (about 2.4 mi upstream from the mouth of 

Tinkers Creek and downstream from all WWTP inputs (fig. 

1)) and near the mouths of Furnace Run and Yellow Creek 

within the boundary of the Cuyahoga Valley National Park 

(fig. 2). The Furnace Run and Yellow Creek sites were considered reference sites because they were near Tinkers Creek and 

were in similar environmental settings, plus the Ohio EPA had 

determined that both streams had Index of Biological Integrity 

(IBI) scores (a measure of fish species diversity and species 

populations) indicating full attainment of their aquatic life uses 

(Ohio Environmental Protection Agency, 2003).

Several criteria were considered when selecting where 

to deploy the samplers at a given site. Adequate water depth 

was a priority to ensure the sampler remained submerged for 

the entire period of deployment. Exposure to the atmosphere 

was minimized (before, during, and after deployment) because 

Figure 6. Photograph of lipid-filled polyethylene membrane tube from a semipermeable 

membrane device (SPMD).
Methods 9

Table 2. Wastewater-treatment-plant (WWTP) information and passive-sampler locations. 

[Mgal/d, million gallons per day; °, degrees;  ́, minutes;  ̋, seconds; n/a, not applicable]

Location/WWTP County

Permitted 

discharge 

(Mgal/d)

Population 

served

(in 2004) 

Upstream 

sampler

location

Downstream 

sampler

location

Deployment

period

(all dates in 

2006)

Streetsboro Portage 4 18,066 41°14 ́56 ̋

81°23 ́17 ̋

41°14 ́60 ̋

81°23 ́20 ̋ 5/10–6/7

Aurora Westerly Portage 1.4 4,897 41°18 ́45 ̋

81°23 ́03 ̋

41°18 ́32 ̋

81°23 ́30 ̋ 5/9–6/6

Aurora Shores Summit 0.5 2,347 41°20 ́03 ̋

81°24 ́06 ̋

41°19 ́59 ̋

81°24 ́10 ̋ 5/9–6/6

Twinsburg Summit 4.95 19,353 41°19 ́23 ̋

81°26 ́57 ̋

41°19 ́23 ̋

81°26 ́54 ̋ 5/10–6/7

Solon Cuyahoga 5.8 22,000 41°22 ́17 ̋

81°27 ́33 ̋

41°22 ́05 ̋

81°27 ́40 ̋ 5/9–6/6

Bedford Cuyahoga 3.2 15,000 41°23 ́15 ̋

81°33 ́42 ̋

41°23 ́12 ̋

81°33 ́49 ̋ 5/9–6/6

Bedford Heights Cuyahoga 7.5 14,256

41°23 ́09 ̋

81°29 ́57 ̋a 41°23 ́05 ̋

81°29 ́59 ̋ 5/8–6/5 41°23 ́06 ̋

81°29 ́55 ̋b

Tinkers Creek at 

Dunham Road Cuyahoga n/a n/a 41°22 ́30 ̋81°34 ́33 ̋ n/a 5/8–6/5

Furnace Runc Cuyahoga n/a n/a 41°12 ́14 ̋

81° 35 ́08 ̋ n/a 5/10–6/7

Yellow Creekc Cuyahoga n/a n/a 41°09 ́47 ̋

81°35 ́03 ̋ n/a 5/10–6/7

a

Location upstream from outfall on unnamed tributary to Hawthorne Creek.

b

Location on Hawthorne Creek upstream from confluence with unnamed tributary.

c

Reference site.

atmospheric exposure presents a risk of contamination from 

airborne chemicals that can confound the identification and 

quantification of waterborne chemicals. Samplers were placed 

where water would flow over them; however, deployment in 

the fastest or deepest section of the channel was not always 

possible. Protection of samplers from floating debris and vandalism and options for securing the samplers played a major 

role in determining sampler placement. 

Reconnaissance of each sampling site was completed 

in April 2006, during a period of low to moderate flow. Of 

particular interest were the mixing zones below the seven 

WWTP outfalls. The downstream location for a sampling 

site was established where the WWTP effluent was estimated 

to be well mixed with the receiving water. Another concern 

was proximity to the nearest tributary. If any tributaries 

entered close to the WWTP outfall, the sampler preferably 

was positioned between the WWTP outfall and the nearest 

tributary. Three samplers were used to bracket the Bedford 

Heights WWTP because its outfall on an unnamed tributary 

to Hawthorne Creek is so close to the mouth that the effluent 

could not mix completely with the receiving stream before it 

enters Hawthorne Creek (fig. 7). Consequently, one sampler 

was placed in the unnamed tributary above the WWTP outfall, 

the second in Hawthorne Creek above the confluence with the 

unnamed tributary, and the third in Hawthorne Creek below 

the confluence with the unnamed tributary (where it appeared 

that the two streams were fully mixed). 

Streamflow in Tinkers Creek during the passive-sampler 

deployment period can be characterized as being greater 

than normal. Daily mean streamflows determined for the 

USGS streamgage on Tinkers Creek at Bedford, Ohio (station 

04207200), for May 8, 2006, through June 7, 2006, were compared to mean daily streamflows determined for those same 

calendar days based on gage data collected from 1962 to 2007. 

That comparison indicates that the 2006 daily mean streamflows exceeded their corresponding long-term mean daily 

streamflows on 19 of the 31 calendar days and that the average 

streamflow for that period in 2006 (283 ft3

/s) was over twice 

the historical average (127 ft3/s) for the same calendar days.

Passive samplers were deployed for a 28-day period 

beginning in May 2006 and ending in June 2006. Specific 

beginning and ending dates of deployments at each loca-
10 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

tion are listed in table 2. Field personnel were instructed to 

avoid use of compounds that were in the list of analytes being 

measured (both in passive samplers and streambed sediments), 

and basic good field practices were followed (U.S. Geological 

Survey, 2006). So, for example, field personnel did not wear 

insect repellant containing DEET when handling or processing 

samples. Passive samplers were stored in airtight containers on 

ice for transport to and from the study area and to the laboratory.

Streambed-Sediment Sampling

Streamed-sediment samples were collected at each 

sampling location before the passive samplers were retrieved. 

Streambed-sediment samples were collected slightly downstream from the passive samplers, and sediments and samplers 

were collected in a downstream-to-upstream order so as to prevent contamination from upstream disturbances. The top 1 to 2 

cm of streambed sediment was sampled from 5 to 10 depositional zones, and the samples were composited with samples 

from other depositional zones sampled at the same site. The 

number of samples collected from each zone was roughly 

proportional to the relative size of each zone (for example, the 

larger the area of the depositional zone, the larger the number 

of samples collected). The purpose of compositing subsamples 

from different depositional zones was to reduce local scale 

variability and gather samples that were most representative of 

the average contaminant concentration at the site. 

Streambed-sediment samples were collected and processed in the field according to the organic-contaminant 

methods described by Shelton and Capel (1994). Streambedsediment samples from each depositional zone were collected 

with stainless steel spoons, then composited in a basin before 

being poured through a 2-mm stainless steel sieve. Approximately 100 g of material was collected at a sampling site for 

each of the analytical schedules used. Streambed-sediment 

samples were placed in baked amber glass jars and placed on 

ice for transport from the study area and to the laboratory.

Unnamed tributary

Hawthorne Creek

Culvert

Outfall

Solon Road

Above outfall (AO)

Upstream (US)

Downstream (DS)

EXPLANATION

Wastewater outfall

Sampling location

Figure 7. Schematic of sampling-site locations near the Bedford Heights wastewater-treatment-plant outfall.
Methods 11

Laboratory Analyses

The following is a brief overview of the methods used to 

analyze the passive-sampler media and streambed-sediment 

samples. A detailed description of the methods is given in 

Appendix A ,and lists of the analytes by medium and analytical method are given in Appendix B. 

A solvent (or mixture of solvents) was used to extract 

analytes from the POCIS media at the USGS Columbia Environmental Research Center (CERC) in Colombia, Mo. The 

extracts were concentrated, filtered, and sealed in ampoules 

for shipment to the analytical laboratories. Each POCIS 

sample analyzed in the laboratory was a composite of extracts 

from two POCIS disks, which served to increase the total mass 

of sampled compounds and thereby effectively lowered the 

analytical detection limits.

POCIS sample extracts were analyzed for 66 wastewater 

compounds at the USGS National Water Quality Laboratory 

(NWQL) in Denver, Colo., by means of full-scan positiveion gas chromatography (GC)-mass spectrometry (MS), 

operating in electron impact mode (Zaugg and others, 2007). 

POCIS sample extracts were analyzed for pharmaceuticals at 

the NWQL by means of positive-mode electrospray ionization (ESI) high-performance liquid chromatorgraphy (LC)-

mass spectrometry (Cahill and others, 2004). To confirm the 

identity of pharmaceuticals, selected POCIS extracts also were 

analyzed by means of liquid chromatography tandem mass 

spectrometry (LC/MS/MS), operated in multiple-reaction 

monitoring mode.

Antibiotic and degradation products were separated from 

the POCIS extracts by means of a liquid chromatography 

(LC) gradient elution. Individual antibiotic compounds were 

analyzed by means of selected ion monitoring liquid chromatography/tandem mass spectrometry at the USGS Organic 

Geochemistry Research Laboratory (OGRL) in Lawrence, 

Kans. The antibiotic analysis includes some analytes that are 

not antibiotics (such as ibuprofen and carbamazepine); however, the 32 compound analyte list will be referred to generically hereafter as “antibiotic compounds.”

Analytes and performance reference compounds (PRCs) 

were extracted from SPMDs by means of two-stage dialysis 

with a solvent. The extracts were concentrated, and size exclusion chromatography (SEC) was used to separate the compounds into fractions based on their size. Fractions from the 

SEC were further processed by means of gravity-column chromatography to remove potential interferences and to enrich the 

PRCs and analytes. Analysis of SPMD extracts for PRCs and 

33 hydrophobic compounds was done at the CERC by means 

of GC/MS, using positive ion electron-impact ionization in the 

selected-ion mode (Alvarez and others, 2008; Petty and others, 

2000) (table B4).

Pressurized solvent extractions were used to extract 

analytes from streambed-sediment samples. After extraction, 

pharmaceutical analyses (20 compounds) were done at the 

NWQL by means of high-performance LC/MS, using positive 

electrospray ionization operated in the selected-ion monitoring mode (Kinney and others, 2006). Wastewater compounds 

of interest were isolated from potential matrix interferences 

by means of solid-phase extraction (SPE). The SPE cartridges 

were dried with nitrogen gas, and the sorbed compounds were 

eluted with a solvent mixture. The eluate was analyzed for 57 

wastewater compounds at the NWQL by means of capillarycolumn GC/MS (Burkhardt and others, 2006).

Eleven OWCs in passive-sampler extracts were analyzed 

by more than one analytical method. For those compounds, 

concentrations are reported independently for each method 

because sensitivities—and consequently, method detection 

levels—differ by method. Four compounds (azithromycin, carbamazepine, sulfamethoxazole, and trimethoprim) in POCIS 

extracts were analyzed by means of the antibiotic and pharmaceutical methods. Two compounds (caffeine and cotinine) 

were analyzed in POCIS extracts by means of the pharmaceutical and wastewater methods. Five other compounds (2-methylnaphthalene, anthracene, benzo[a]pyrene, naphthalene, and 

pyrene) were analyzed in POCIS extracts by means of the 

wastewater method and also in SPMD extracts.

Reporting of Data

POCIS and SPMD media were processed to determine 

concentrations of target analytes. The resulting raw concentration data are reported in units of nanograms (ng) per unit 

of media (for example, nanograms per POCIS disk or per 

SPMD). If uptake kinetics (sampling rates) of the sampling 

media can be determined, time-weighted water concentrations can be estimated. Unfortunately, a variety of site-specific 

environmental factors (for example, temperature and water 

velocity over the media) can affect sampling rates. Sampling 

rates can be estimated for SPMDs through the use and analysis 

of performance reference compounds (PRCs) embedded in 

the media. (See Appendix A for more details.) Because loss 

and sampling rates are equal (isotropic), the rate of PRC loss 

during field deployment can be used to adjust laboratorydetermined sampling rates to account for site-specific factors. 

Consequently, time-weighted water concentrations are estimated and reported in units of micrograms per liter for SPMD 

analytes. However, the POCIS media are so strongly sorptive 

that the PRC approach does not work. Consequently, concentrations of analytes determined from POCIS must be reported 

in units of nanograms per POCIS disk, and these concentrations cannot be adjusted for variable sampling rates. Because 

the concentrations of analytes from POCIS cannot be adjusted 

for sampling rate, care must be taken in their interpretation. 

For that reason, this report focuses primarily on the detection/

nondetection of analytes in POCIS and assumes (possibly 

incorrectly) that sampling rates were approximately equal at 

all locations.

Each laboratory determined laboratory reporting levels 

(LRLs) for the analytes included in their respective analytical 

schedules. LRLs are the smallest measured concentration that 
12 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

the laboratory could measure reliably for a given analytical 

method. Method detection limits (MDLs) are also determined 

for some analytical methods. MDLs are defined as the minimum concentration of a substance that can be measured and 

reported with 99 percent confidence that the analyte concentration is greater than zero for the given sample matrix. LRLs 

and MDLs (where applicable) are reported in Appendix B.

In some cases, values are reported for compounds 

at concentrations below the LRL. That was done because 

information-rich analytical methods (such as GC/MS and LC/

MS) provide qualifying information that enhances analyte 

identification (Childress and others, 1999). Concentrations 

reported below the LRL and above the MDL (identified in data 

tables by an “e” in front of the concentration) met the same 

criteria for qualitative identification as concentrations above 

the reporting level; however, there is greater uncertainty associated with the calculated concentration. An “e” code may also 

be used for other reasons, such as when results are extrapolated above the calibration curve or when analyte performance 

does not meet acceptable method-specific criteria. For more 

information on reporting procedures, see Childress and others 

(1999). All values qualified with an “e” code in this report 

were counted as detections.

Occasionally, compounds are detected below the average MDL (identified in tables by an “m,” indicating that the 

compound is present but is not quantified). This can happen 

because the low-level sensitivity can vary between analytical 

instrument setups and may at times be more sensitive than 

indicated by the average MDL. When compounds were not 

detected, concentrations were censored at (reported as less 

than) the reporting level.

A detection was censored (identified in tables by a “dc”) 

for a given compound if the concentration in the environmental sample was less than 3 times the concentration in the 

corresponding trip blank. If the concentration of the compound 

in the environmental sample was between 3 and 5 times the 

corresponding concentration in the trip blank, it was footnoted 

to indicate that the compound was also detected in the corresponding trip blank.

The methods used to process and analyze POCIS media 

are still in development and have not been fully validated. 

Consequently, we emphasize that all POCIS results should be 

treated as estimates.

Quality Control

Various quality-control (QC) measures were employed 

in this study to help assess sampling and analytical variability 

and bias and to aid accurate quantification of target analytes. 

As is evident from table 3, the types of QC measures used 

varied as a function of sampling media and analytical method. 

The QC measures are discussed in the sections that follow, 

with detailed information given on trip blanks and replicate 

analyses. 

Trip Blanks

The POCIS and SPMD devices have the potential to 

accumulate airborne contaminants when exposed to the atmosphere. Consequently, at each of the 18 sampling locations, 

trip blanks were used. Trip blanks consisted of deployment 

canisters containing POCIS and SPMD media that were identical in construction to those placed in the water. The trip blanks 

were exposed to the atmosphere at each sampling location 

during the same time and for the same duration that field-deployed canisters were exposed to the atmosphere (as they were 

being deployed into or retrieved from the stream). The trip 

blanks were stored in airtight containers on ice for transport 

to and from the study area. Between deployment and retrieval 

of the field-deployed canisters, trip blanks were stored in their 

airtight containers at less than 0°C. 

No antibiotics were detected in POCIS trip blanks; however, 4 of 20 pharmaceutical compounds and 10 of 66 wastewater compounds were detected (appendix table C1). For most 

compounds, detections occurred at from one to three locations. 

Three compounds, diethylhexyl phthalate (a plasticizer), fluoxetine (an antidepressant), and diphenhydramine (an antihistamine) were found in four or more trip blanks. 

Table 3. Matrix of quality-control measures used as a function of media and analytical method.

[X indicates that a quality-control measure was used; POCIS, polar organic chemical integrative sampler; SPMD, semipermeable membrane device]

Media Analytical method Trip 

blank Replicate Method blank

Reagent 

spike

Matrix 

spike

Surrogate 

standards

Internal 

standards

POCIS Antibiotic X X X X

POCIS Pharmaceutical X X

POCIS Wastewater X X X X X

SPMD Hydrophobic X X X X

Sediment Pharmaceutical X X X X X

Sediment Wastewater X X X X X
Methods 13

Of the 33 hydrophobic compounds analyzed for, 14 

were detected in SPMD trip blanks (appendix table C2). Of 

the 14 compounds, 9 were detected in more than half of the 

samples, and 3 of those 9 (pheanthrene, 1-methylnaphthalene, 

and 2-methylnaphthalene; all fuel-related compounds) were 

detected in 100 percent of the samples.

Field Replicates

Field replicates were collected at two locations (Streetsboro and Twinsburg, both downstream from WWTP outfalls) to assess variability of the environmental data. POCIS 

replicates (appendix table C3) and SPMD replicates (appendix 

table C4) consisted of a second passive-sampler canister (containing POCIS and SPMD media) deployed on the same tether 

side by side with the primary sampler (the designation of one 

sampler as primary and the other as a replicate was done at 

random). A streambed-sediment replicate (appendix table C5) 

consisted of a second sample collected at the same time as 

the environmental sample. Locations downstream from the 

Streetsboro and Twinsburg WWTPs were chosen for replicate 

sampling because each WWTP discharges directly into Tinkers 

Creek, and the likelihood of detecting OWCs was expected to 

be greatest at sites downstream from WWTP outfalls.

Of the 236 environmental replicate pairs of POCIS 

analytes (118 analytes total from three methods × 2 sets of 

replicates = 236), the detection or nondetection of the analyte 

was confirmed in about 94 percent of the pairs. Only in 15 

pairs were there detections in only one of the paired samples 

(appendix table C3). Similarly, for SPMDs and streambed sediments, an analytes’s detection or nondetection was confirmed 

in replicate samples about 97 and 94 percent of the time, 

respectively. In most cases, the concentration of the detection 

was either estimated or near the LRL when an analyte was 

detected in only one of the replicate pairs.

The variability of the results for field replicate samples 

was assessed by calculating the absolute relative percent 

difference (RPD) in concentration for the two environmental 

samples forming the replicate pair. The RPD is calculated as 

follows: 

RPD=100×|(R1 –R2)/(0.5 (R1+R2))|

where

R1 is the concentration of analyte in the first 

sample of the replicate pair, and

R2 is the concentration of analyte in second 

sample of the replicate pair.

RPDs for POCIS replicates ranged from 4.2 to 120 

percent (appendix table C3). Some RPDs were high, and in 

several instances a compound was detected in one sample in 

the replicate but not the other (RPDs were not calculated when 

a compound was detected in only one sample of the replicate pair). This can be expected when comparing chemical 

concentrations at or near detection levels (Sando and others, 

2006). One factor that could result in differing concentrations 

between replicate samples is the slightly different environmental exposures (such as due to each sampler’s position in 

the stream). RPDs for SPMD replicates ranged from 4.3 to 27 

percent (appendix table C4). The largest RPD (27 percent) was 

for phenanthrene, a compound found in 100 percent of the trip 

blanks.

RPDs for streambed-sediment replicates ranged from 0 to 

120 percent. For a given compound, RPDs determined for different replicate pairs could be very different. For example, the 

RPD for β-stigmastanol (a plant sterol) was 9.5 percent in one 

replicate pair and 120 percent in the other replicate pair. This 

difference in variability may reflect the ability to obtain representative streambed-sediment replicates, as well as reflecting 

analytical variability.

Reagent and Matrix Spikes

Reagent spikes consist of analyte-free reagents that 

were “spiked” by adding known concentrations of the target 

analytes. In contrast, matrix spikes consist of environmental 

samples that are spiked with known concentrations of target 

analytes. Reagent and matrix spike samples were used to 

assess analytical bias due to variable analyte recovery and to 

check the performance of an analytical method at the time that 

environmental samples were analyzed, respectively. 

The recoveries of the reagent-water spikes for wastewater 

compounds ranged from 20 percent (for tetrachloroethylene) 

to 107 percent (metalaxyl) (appendix table C6). The median 

reagent-water-spike recovery was 89.5 percent, and about 84 

percent of the recoveries equaled or exceed 60 percent.

The recoveries of pharmaceuticals in reagent spikes for 

sediments ranged from 11 percent (for azithromycin) to 150 

percent (for sulfamethoxazole), with a median recovery of 

68.5 percent (appendix table C7). Recoveries of less than 50 

percent occurred in both sediment reagent spike samples for 

azithromycin and fluoxetine. One of the two sediment reagentspike samples showed greater than 100 percent recovery for 

half of the analytes, whereas the other sediment reagent-spike 

sample indicated recoveries in the range of 61 to 72 percent 

for those same analytes.

The recoveries of pharmaceuticals in matrix spikes for 

two streambed-sediment samples were quite variable (appendix table C7). Recoveries of miconazole and ranitidine were 

consistently low (<10 percent), and percent recoveries for some 

other compounds such as 1,7-dimethylxanthine, cimetidine, and 

dehydronifedipine varied by more than 50 percentage points. 

The poor recoveries for some analytes and high variability for 

others suggests that matrix effects can be significant.
14 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Method Blanks and Surrogate and Internal 

Standards

Method blank samples consisted of analyte-free POCIS 

and SPMD media or reagent-grade sand that were processed 

and analyzed in the laboratory along with the environmental 

samples. 

Surrogate standards are analytically noninterfering compounds that are similar to the target analytes in both physical 

and chemical properties but are not expected to be present in 

the environment. Surrogates are added to environmental and 

quality-control samples immediately prior to analysis and used 

to monitor the recovery efficiency of the analytical method for 

the unique environmental-sample matrix. 

Internal standards are similar in concept and application 

to surrogate standards except that their primary purpose is to 

improve quantification by facilitating corrections for loss of 

analyte. 

Quantitative information about method blank and surrogate and internal standard results is not presented in this 

report; however, those data were examined and used to ensure 

the reporting of valid and accurate data.

Results

The numbers of OWCs detected by sample matrix and 

analytical method are presented in table 4. Numbers of detections downstream from WWTPs are bolded in table 4 if they 

are larger than corresponding upstream numbers. A one-sided 

Fisher’s exact test (Sokal and Rohlf, 1981) was done to determine whether the number of detections at the downstream 

location was significantly greater (at a 5-percent level) than at 

the corresponding upstream location. Those counts that were 

significantly greater at the downstream locations are italicized 

as well as bolded.

For a given sample matrix (that is, water or sediment), 

individual compounds that were detected by more than one 

analytical method are included separately in counts for each 

method. Percentages of detections of the most frequently 

detected compounds in the POCIS and SPMD extracts and in 

bed-sediments samples are presented in tables 5 and 6, and 

numbers of detections by WWTP and analytical method are 

shown in figures 8 and 9, respectively. The minimum, median, 

maximum, and frequency of detection for the individual compounds are presented by sample matrix and analytical method 

in Appendixes D through F. 

Table 4. Numbers of detections of chemical compounds in water (as determined by analysis of POCIS and SPMD media) 

and streambed sediments in the Tinkers Creek watershed and two other tributaries to the Cuyahoga River, 2006.

[Number of analytes for the method shown in parentheses; WWTP, wastewater-treatment plant; US, upstream from WWTP outfall; DS, downstream from WWTP outfall; bold values indicate number of DS detections that were greater than their respective US detections; italicized values 

indicate number of DS detections that were statistically greater (at a 5-percent level) than their respective US detections]

Sample area

Numbers of detections, by indicated media and analytical method

Water Streambed sediment

Antibiotic 

method

(32)

Pharmaceutical 

method 

(20)

Wastewater 

method

 (66)

Hydrophobic 

method

 (33)

Pharmaceutical 

method 

 (20)

Wastewater 

method

 (57)

US DS US DS US DS US DS US DS US DS

Streetsboro 0 7 1 5 9 22 6 4 0 3 23 25

Aurora Westerly 0 7 1 6 9 16 5 3 2 4 24 26

Aurora Shores 0 4 1 4 8 8 4 3 2 2 21 26

Twinsburg 4 5 5 5 13 11 10 10 0 1 24 23

Solon 0 10 1 12 17 20 15 12 1 1 20 31

Bedford 2 7 2 5 23 29 20 17 1 1 29 29

Bedford Heights 0a

 0b 6 2a 1b 5 9a 12b 22 16a 17b 18 2a 1b 4 20a 20b 23

Tinkers Creek at 

Dunham Road 6 10 21 13 2 28

Furnace Run 3 1 5 3 1 20

Yellow Creek 0 2 1 5 2 18

a The number of detections at the unnamed tributary site located upstream from the WWTP outfall.

b The number of detections at the Hawthorne Creek site located upstream from the unnamed tributary.
Results 15

Compounds in Water

The following sections contain information about the 

time-weighted concentrations of OWCs in the water column 

as determined by analyzing extracts from POCIS or SPMD 

passive-sampler media. 

Antibiotic Compounds

Twelve compounds were detected in one or more POCIS 

extracts by means of the antibiotic method (appendix table 

D2). Sulfamethoxazole and trimethoprim (two antibiotics that 

are commonly combined to treat a variety of infections) and 

carbamazepine (an anticonvulsant and suspected endocrine 

disruptor1) were each detected in more than 50 percent of the 

1

 Endocrine disruptors are natural or synthetic compounds that can mimic or 

block the action of an organism’s natural hormones.

samples (table 5). Antibiotic compounds were not detected at 

most sites upstream from WWTPs addressed in this study but 

were detected at all sites downstream from WWTP outfalls 

(table 4 and fig. 8) and at the Furnace Run reference site 

(which has a wastewater source about 5 mi upstream from the 

sampling site). 

Antibiotic compounds were detected at sites upstream 

from the Twinsburg and Bedford WWTP outfalls (table 4 and 

fig. 8). Potential sources of those compounds at Twinsburg 

include the Aurora Westerly, Aurora Shores, and Streetsboro 

WWTPs, all of which discharge to Tinkers Creek or its tributaries upstream from Twinsburg. Three out of four antibiotic 

compounds detected upstream from Twinsburg also were 

detected downstream from all three upstream WWTPs, and the 

fourth (erythromycin-H2O (anhydroerythomycin), an antibiotic degradate) was detected downstream from two of the 

three upstream WWTPs. In both cases where antibiotics were 

detected upstream from WWTPs, the number of detections at 

the corresponding downstream locations was greater.

Streetsboro

Aurora Westerly

Aurora Shores

Twinsburg

Solon

Bedford

Bedford Heights

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30

Detections of Antibiotic Compounds

 Upstream

 Downstream

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30

 Detections of Pharmaceutical Compounds

Streetsboro

Aurora Westerly

Aurora Shores

Twinsburg

Solon

Bedford

Bedford Heights

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30

Detections of Wastewater Compounds

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30

Detections of Hydrophobic Compounds

Figure 8. Numbers of detections of antibiotic, pharmaceutical, wastewater, and hydrophobic compounds in water (as determined by 

analysis of POCIS and SPMD media) upstream and downstream from wastewater-treatment plants in the Tinkers Creek watershed.
16 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Six antibiotic compounds were detected at the Dunham 

Road site (table 4), the most downstream sampling site on Tinkers Creek. By comparison, the median number of antibiotics 

detected downstream from the WWTPs was seven. No antibiotic compounds were detected at the Yellow Creek reference 

site; however, three compounds were detected at the Furnace 

Run site (which has a wastewater source about 5 mi upstream 

from the sampling site). Two of the antibiotic compounds (carbamazepine and sulfamethoxazole) detected at Furnace Run had 

been found downstream from all WWTP outfalls in the Tinkers 

Creek watershed. The third antibiotic compound, ormetoprim 

(commonly used in combination with sulfadimethoxine to treat 

skin and soft-tissue infections in animals), was not detected at 

any other site. 

Pharmaceutical Compounds

Fifteen compounds were detected in one or more POCIS 

extracts by means of the pharmaceutical method (appendix 

table D3). Caffeine (a stimulant), trimethoprim, and carbamazepine were detected in 50 percent or more of the samples 

(table 5). Frequent detections of trimethoprim and carbamazepine had also occurred in samples analyzed by the antibiotic method; however, sulfamethoxazole, which had been 

detected in more than 50 percent of the samples analyzed by 

means of the antibiotic method (table 5), was detected only 

once by means of the pharmaceutical method. The difference 

in frequency of detection between the two analytical methods 

is due in part to the higher reporting level for sulfamethoxazole by the pharmaceutical method (5 ng/POCIS) as compared to the antibiotic method (1 ng/POCIS).

The spatial pattern of pharmaceutical compound detections was similar to that of the antibiotic compounds (fig. 8) 

with exception that at least one pharmaceutical compound 

(caffeine) was detected upstream from each WWTP. Caffeine 

was detected in all but one sample (appendix table D4). The 

number of pharmaceutical-compound detections at sites downstream from WWTP outfalls was greater than at upstream sites 

except at Twinsburg, where the same number of detections 

occurred in both upstream and downstream samples (fig. 8).

Caffeine was detected at both reference sites, although at 

lower concentrations than found in the Tinkers Creek watershed (appendix table D3). Fluoxetine (an antidepressant) also 

was detected at the Yellow Creek reference site. In general, the 

number of detections of pharmaceutical compounds at reference sites was similar in magnitude to the number of detections observed at sites upstream from the WWTP outfalls. 

Wastewater Compounds

Forty-one compounds were detected in one or more 

POCIS extracts by means of the wastewater method (appendix 

table D6). Eleven of the compounds were detected in more 

than 50 percent of the samples (table 5). Caffeine was the most 

frequently detected compound, with detections in all but one 

sample (table 5). Other compounds detected in more than 50 

percent of the samples include atrazine and metolachlor (herbicides), diethyl phthalate (plasticizer), N,N-diethyl-meta-toluamide (DEET) (topical insect repellant), anthraquinone (used 

to produce dyes and occurs naturally in some plants), p-cresol 

(disinfectant and wood preservative), ethanol,2-butoxy-phosphate (fungicide), hexahydrohexamethylcyclopentabenzopyran 

(HHCB) (synthetic musk), and tris(2-chloroethyl)phosphate and 

tris(dicholorisopropyl)phosphate (flame retardants). HHCB, a 

synthetic musk used in some personal care products, has been 

shown to have antiestrogenic activity (Schreurs and others, 

2005) and is thought to disrupt endocrine function in fish. Atrazine and diethyl phthalate are also known or suspected endocrine disruptors (appendix table B6). 

Wastewater compounds generally were detected with 

greater frequency downstream from WWTP outfalls than 

upstream (table 4 and fig. 8). Twinsburg was the only location 

where more compounds were detected upstream from the outfall than downstream. Appreciably fewer detections of wastewater compounds occurred at the reference sites than at sites in the 

Tinkers Creek watershed (table 4).

Hydrophobic Compounds

Twenty-two hydrophobic compounds were detected in 

one or more SPMD extracts (appendix table E1). Ten of the 

compounds were detected in over 50 percent of the samples 

(table 5). Fluoranthene and pyrene (combustion by-products 

and coal tar derivates) were the most frequently detected 

hydrophobic compounds, occurring in 100 percent of the 

samples (appendix table E2). Other compounds detected in 

more than 50 percent of the samples include phenanthrene, 

chrysene, 2-methylphenanthrene, benzo[b]fluoranthene, 

benzo[a]anthracene, benzo[b]naphtha[2,1-d]thiophene, 

benzo[e]pyrene, and benzo[k]fluoranthene. 

Compounds detected more frequently downstream than 

upstream from WWTPs are bolded in table 5. A one-sided 

Fisher’s exact test (Sokal and Rohlf, 1981) was done to determine whether the frequency of detection at the downstream 

location was significantly greater (at a 5-percent level) than at 

the corresponding upstream location. Those detection frequencies that are significantly greater at the downstream locations 

are italicized as well as bolded.

Unlike the antibiotic, pharmaceutical, and wastewater 

compounds, hydrophobic compounds generally were detected 

in about the same or greater numbers at sites upstream of 

WWTP outfalls than at corresponding downstream sites (table 

4 and fig. 8). Many hydrophobic compounds strongly sorb to 

particulate matter such as soils and sludge, which are removed 

during the wastewater-treatment process. Consequently, the 

reason for fewer detections of hydrophobic compounds downstream of WWTP outfalls (relative to upstream) may be due to 

dilution of stream water by the WWTP effluents. 

Hydrophobic compounds were detected at the reference 

sites; however, the frequencies of detection tended to be in the 

lower range of frequencies observed for sites in the Tinkers 

Creek watershed (table 4). 
Results 17

Table 5. Organic wastewater compounds detected most frequently (>50 percent detections in one or more groupings) in water (as 

determined by analysis of POCIS and SPMD media) in the Tinkers Creek watershed and two other tributaries to the Cuyahoga River, 2006.

[US, upstream from wastewater-treatment plant (WWTP); DS, downstream from wastewater-treatment plant; AS, all sites (including reference sites); bold 

values indicate DS detection frequencies that were greater than their respective US frequencies; italicized values indicate DS detection frequencies that were 

statistically greater (at a 5-percent level) than their respective US frequencies]

Compound

Percentage of detections, by indicated media and analytical method

POCIS SPMD

Antibiotic method Pharmaceutical 

method

Wastewater 

method

Hydrophobic 

method

US DS AS US DS AS US DS AS US DS AS

Azithromycin 0 86 39

Carbamazepine (by antibiotic method) 14 100 56

Erythromycin-H2

O 14 86 44

Sulfamethoxazole 29 100 61

Trimethoprim 29 100 56

Lincomycin 0 57 28

Ofloxacin 0 57 22

Caffeine (by pharmaceutical method) 100 86 94

Carbamazepine (by pharmaceutical method) 14 100 50

Diphenhydramine 0 86 39

Thiabendazole 14 71 39

Trimethoprim 29 100 56

N,N-diethyltoluamide (DEET) 100 100 83

Acetyl-hexamethyl-tetrahydro-naphthalene 

(AHTN) 14 86 44

Atrazine 100 86 89

Anthraquinone 71 71 67

Caffeine (by wastewater method) 100 100 94

Diethyl phthalate 86 86 83

Ethanol,2-butoxy-,phosphate 57 71 56

Hexahydrohexamethyl-cyclopentabenzopyran 

(HHCB) 29 100 56

Metolachlor 100 43 72

4-Nonylphenol monoethoxylate (NP1EO; sum 

of all isomers) 29 57 39

4-Octylphenol monothoxylate (OP1EO; sum of 

all isomers) 14 57 33

p-Cresol 86 71 67

p-Nonylphenol, total 29 57 39

3-methyl-1(H)-indole 14 57 28

Tris(2-chloroethyl) phosphate 43 86 56

Tris(dichlorisopropyl) phosphate 43 86 56

2-methylphenanthrene 57 57 61

Benz[a]anthracene 57 57 56

Benzo[b]fluoranthene 71 57 61

Benzo[b]naphtho[2,1-d]thiophene 57 57 56

Benzo[e]pyrene 57 57 56

Benzo[k]fluoranthene 57 57 56

Chrysene 100 71 89

Fluoranthene 100 100 100

Phenanthrene 100 100 94

Pyrene 100 100 100
18 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Compounds in Streambed Sediments

The following sections discuss analytical results for 

streambed-sediment samples. Streambed-sediment chemistry 

can reflect long-term exposure to stream water but also can 

reflect other contaminant sources, such as airborne deposition 

or sediments washed off urban or agricultural landscapes. 

Pharmaceutical Compounds

Eight pharmaceutical compounds were detected in one or 

more streambed-sediment samples (appendix table F1). One 

compound (diphenhydramine, an antihistamine) was detected 

in 50 percent of the samples (table 6). A comparison of pharmaceutical compounds detected in sediment to those detected 

in POCIS extracts indicates that many of the compounds 

detected in sediment also were present in water. One notable 

exception is miconazole (an antifungal compound), which 

was detected in 28 percent of the streambed-sediment samples 

but was not detected in water. Miconazole’s poor solubility in 

water explains why it partitions preferentially onto particulate 

phases. In general, concentrations of pharmaceutical compounds in sediment, when detected, were higher in samples 

collected downstream from WWTP outfalls than in samples 

collected upstream from the outfalls (table 6 and fig. 9). 

Some pharmaceutical compounds (such as trimethoprim 

and carbamazeipine) that were detected in water at all sites 

downstream from WWTP outfalls were either not detected or 

Table 6. Organic wastewater compounds detected most frequently (>50 percent detections in one or more groupings) in 

streambed sediments in the Tinkers Creek watershed and two other tributaries to the Cuyahoga River, 2006.

[US, upstream from wastewater-treatment plant (WWTP); DS, downstream from wastewater-treatment plant; AS, all sites (including reference sites); 

–, not analyzed for with the method; bold values indicate DS detection frequencies that were greater than their respective US frequencies; italicized values 

indicate DS detection frequencies that were statistically greater (at a 5-percent level) than their respective US frequencies]

Compound

Percentage of detections in streambed sediments, by analytical 

method

Wastewater method Pharmaceutical method

US DS AS US DS AS

Diphenhydramine 43 71 50

1-Methylnaphthalene 86 86 67

2,6-Dimethylnaphthalene 100 100 56

2-Methylnaphthalene 100 100 94

3-β-Coprostanol 86 100 83

3-Methyl-1H-indole 100 100 100

4-Nonylphenol 14 57 28

Anthraquinone 100 100 100

Acetophenone 100 100 90

Acetyl-hexamethyl-tetrahydro-naphthalene (AHTN) 29 86 50

Anthracene 100 86 94

Benzo[a]pyrene 100 100 100

β-Sitosterol 100 100 100

β-Stigmastanol 86 100 83

Bis(2-ethylhexyl) phthalate 100 100 94

Carbazole 100 100 94

Cholesterol 100 100 100

4-Nnonylphenol diethoxylate (NPEO2; sum of all isomers) 43 71 44

Fluoranthene 100 100 100

Hexahydrohexamethyl cyclopentabenzopyran (HHCB) 29 86 50

Indole 100 100 100

4-Nonylphenol monoethoxylate (NPEO1; sum of all isomers) 29 71 39

Naphthalene 100 100 94

p-Cresol 100 100 89

Phenanthrene 100 86 94

Phenol 100 86 83

Pyrene 100 100 100
Results 19

Streetsboro

Aurora Westerly

Aurora Shores

Twinsburg

Solon

Bedford

Bedford Heights

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32

Detections of Pharmaceutical Compounds

 Upstream

 Downstream

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32

 Detections of Wastewater Compounds

detected at a much lower frequency in streambed sediments 

(appendix tables D3 and F1). Results such as these reinforce 

the need to sample both sediments and water when assessing 

the occurrence and distribution of OWCs.

Pharmaceutical compounds were detected in sediments at 

the reference sites (table 4). Sulfamethoxazole was detected at 

both reference sites, and erythromycin (an antibiotic) also was 

detected at very low concentration at the Yellow Creek reference site (appendix table F1). 

Wastewater Compounds

Thirty-seven wastewater compounds were detected in 

one or more streambed-sediment samples (appendix table 

F3). Twenty-two compounds were detected in more than 50 

percent of the samples, and 12 of those compounds (2,6-

dimethylnaphthalene, 2-methylnaphthalene, 3-methyl-1Hindole, anthraquinone, benzo[a]pyrene, β-sitosterol, carbazole, 

cholesterol, fluoranthene, indole, naphthalene, and pyrene) 

were detected at all sites (table 6). Fourteen of the wastewater 

compounds detected (three of which were detected in more 

than 50 percent of the samples) are known or suspected endocrine disruptors (appendix table B6). 

Fifteen wastewater compounds (2,6-dimethylnaphthalene, 2-methylnaphthalene, 3-methyl-1H-indole, anthraquinone, acetophenone, benzo[a]pyrene, β-sitosterol, bis(2-ethylhexyl) phthalate, carbazole, cholesterol, fluoranthene, indole, 

naphthalene, p-cresol, and pyrene) were detected in sediments 

at all sites in the Tinkers Creek watershed, irrespective of 

whether the site was upstream or downstream from a WWTP 

(table 6). Sources of those compounds likely are diffuse within 

the watershed. Three of the seventeen compounds (benzo[a]

pyrene, bis(2-ethylhexyl) phthalate, and p-cresol) are known 

or suspected endocrine disruptors. 

In all cases except one (at Solon), the number of detections of wastewater compounds in streambed sediments was 

equal or greater (although generally not statistically greater) 

in samples collected downstream from WWTP outfalls as 

compared to corresponding upstream samples (table 4 and fig. 

9). Three compounds (hexahydrohexamethyl-cyclopentabenzopyran (HHCB), acetyl-hexamethyl-tetrahydro-naphthalene 

(AHTN), and triclosan) were detected in sediments downstream from WWTP outfalls at least 3 times more frequently 

than at upstream sites. 

Concentrations of wastewater compounds in sediments 

downstream from the Aurora Westerly, Aurora Shores, and 

Solon WWTP outfalls tended to be higher than their corresponding upstream concentrations (appendix table F3). In contrast, concentrations of wastewater compounds in sediments 

downstream from the Streetsboro and Twinsburg WWTP 

outfalls tended to be somewhat lower than their corresponding 

upstream concentrations. Higher concentrations of wastewater 

compounds in sediments upstream from Twinsburg are not 

completely unexpected given the number of upstream wastewater sources; however, the reason for the higher concentrations upstream from Streetsboro is not known.

In spite of their low water solubilites, some wastewater 

compounds, such as atrazine and DEET, were not detected 

in streambed sediments in spite of being detected in water 

at most sites downstream from WWTP outfalls (appendix 

tables D3 and F4). Some other wastewater compounds, such 

as AHTN and HHCB, were detected in both water and sediment, with detections in both matrices occurring appreciably 

more frequently downstream from WWTPs as compared 

to upstream. Once again, these results reinforce the need to 

sample both sediments and water when assessing the occurrence and distribution of OWCs.

Figure 9. Numbers of detections of pharmaceutical and wastewater compounds in streambed sediments upstream and downstream 

from wastewater-treatment plants in the Tinkers Creek watershed.
20 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Wastewater compounds were detected in sediments at the 

reference sites (table 4), generally with detection frequencies 

slightly lower than observed for sites upstream from WWTPs 

in the Tinkers Creek watershed. 

Summary and Conclusions

This report presents the results of a study to determine the 

occurrence and distribution of a wide variety of organic wastewater compounds (OWCs) in the Tinkers Creek watershed and 

in reference sites on two other tributaries to the Cuyahoga River. 

The study was done by U.S. Geological Survey in cooperation 

with the Ohio Water Development Authority; National Park 

Service; Cities of Aurora, Bedford, Bedford Heights, Solon, 

and Twinsburg; Counties of Portage and Summit; and in collaboration with the Ohio Environmental Protection Agency. 

Samples were collected at sites in the Tinkers Creek watershed 

upstream and downstream from seven wastewater-treatment 

plants (WWTPs) serving the communities of Aurora, Bedford, 

Bedford Heights, Solon, Streetsboro, and Twinsburg, Ohio, at 

one site downstream from all upstream WWTP inputs, and at 

reference sites outside of the Tinkers Creek watershed near the 

mouths of Furnace Run and Yellow Creek. 

Water-column results were based on a 28-day May–June 

2006 exposure period, during which a total of 20 canisters 

containing passive sampler media were deployed instream. 

The canisters contained both polar organic chemical integrative sampler (POCIS) and semipermeable membrane device 

(SPMD) media. The POCIS and SPMD media are designed 

to sample OWCs in water in a manner that yields a timeweighted concentration for the exposure period. Streambedsediment samples also were collected at each site when the 

passive-sampler canisters were retrieved.

POCIS media extracts were analyzed by means of three 

separate laboratory methods predominately targeting antibiotic, pharmaceutical, or wastewater compounds. SPMD media 

extracts were analyzed by means of a laboratory method 

that targeted hydrophobic compounds. Streambed sediments 

also were analyzed by means of separate laboratory methods 

targeting pharmaceutical or wastewater compounds. Results 

are reported by analytical method and sample matrix (water or 

sediment). 

Analytes associated with a given laboratory method are 

referred to in aggregate by the method name. For example, 

analytes associated with the antibiotic method are referred to 

as “antibiotic compounds.” This is true even though some of 

the analytes quantified with the method (for example, ibuprofen and carbamazepine) are not antibiotics. In addition, 

11 compounds were in the analyte list of more than 1 method. 

Individual compounds that were detected by more than one 

analytical method are included independently in counts for 

each analytical method.

On the basis of an examination of data from all sites, a 

total of 12 antibiotic, 20 pharmaceutical, 41 wastewater, and 

22 hydrophobic compounds were detected in water, and 

8 pharmaceutical and 37 wastewater compounds were detected 

in streambed sediments. The numbers of detections at reference sites tended to be in the low range of detection counts 

observed in the Tinkers Creek watershed for a given analytical method. Also, the total numbers of compounds detected 

in water and sediment at the reference sites (3 antibiotic, 2 

pharmaceutical, 5 wastewater, and 4 hydrophobic compounds 

in water and 2 pharmaceutical and 22 wastewater compounds 

in sediment) were less than the total numbers of compounds 

detected at sites in the Tinkers Creek watershed.

With the exception of hydrophobic compounds, it was 

common at most sites to have more compounds detected in 

samples collected downstream from WWTP outfalls than in 

corresponding samples collected upstream from the outfalls. 

This was particularly true for antibiotic, pharmaceutical, and 

wastewater compounds in water. In contrast, it was common 

to have more hydrophobic compounds detected in samples 

collected upstream from WWTP outfalls than downstream, 

possibly because of dilution of stream water by WWTP 

effluents having lower concentrations of hydrophobic compounds. The numbers of detections of compounds upstream 

and downstream from the Twinsburg WWTP generally 

were about equal. This was attributed to the fact that several 

WWTPs discharge to Tinkers Creek or its tributaries upstream 

from Twinsburg, yielding potential sources for the compounds 

detected at the upstream location.

Caffeine, fluoranthene, N,N-diethyl-meta-toluamide 

(DEET), phenanthrene, and pyrene were detected in water 

at all sites in the Tinkers Creek watershed, irrespective of 

whether the site was upstream or downstream from a WWTP. 

This finding suggests that these compounds were diffuse 

in the Tinkers Creek watershed. Some, but not all of these 

compounds, were also detected in water at the reference sites, 

but at concentrations that generally were at the low end of 

the range of concentrations observed in the Tinkers Creek 

watershed.

Carbamazepine, sulfamethoxazole, trimethoprim, and 

hexahydrohexamethylcyclopentabenzopyran (HHCB) were 

detected in water at 100 percent of the sites downstream 

from WWTP outfalls, yet their frequency of detection at sites 

upstream from outfalls was appreciably smaller (occurring in 

about 29 percent or less of the samples). This pattern suggests 

a strong association between the presence of these compounds 

and wastewater discharges. None of these compounds were 

detected in water at the Yellow Creek reference site, and only 

two of the compounds (carbamazepine and sulfamethoxazole) 

were detected at the Furnace Run reference site. 

Fifteen wastewater compounds (2,6-dimethylnaphthalene, 

2-methylnaphthalene, 3-methyl-1H-indole, anthraquinone, 

acetophenone, benzo[a]pyrene, β-sitosterol, bis(2-ethylhexyl) 

phthalate, carbazole, cholesterol, fluoranthene, indole, naphthalene, p-cresol, and pyrene) were detected in sediments at all 

sites in the Tinkers Creek watershed, irrespective of whether 

the site was upstream or downstream from a WWTP. Sources 

of those compounds likely are diffuse within the watershed. 
References Cited 21

 Many of the pharmaceutical compounds detected in sediment also were present in water. One notable exception was 

miconazole (an antifungal compound), which was detected 

in more than a quarter of the streambed-sediment samples 

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compounds (such as trimethoprim and carbamazepine) that 

were detected in water at all sites downstream from WWTP 

outfalls were either not detected or detected at a much lower 

frequency in streambed sediments. Results such as these 

reinforce the need to sample both sediments and water when 

assessing the occurrence and distribution of OWCs.

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Zaugg, S.D., Smith, S.G., Schroeder, M.P., Barber, L.B., and 

Burkhardt, M.R., 2007, Methods of analysis by the U.S. 

Geological Survey National Water Quality Laboratory—

Determination of wastewater compounds by polystyrenedivinylbenzene solid-phase extraction and capillary-column 

gas chromatography/mass spectrometry (ver. 1.1): U.S. 

Geological Survey Water-Resources Investigations Report 

01–4186, 37 p.
24 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Appendix A. Detailed Analytical Methods and Passive Sampling Theory

Traditional methods for determining organic wastewater 

compounds in natural-water samples generally are optimized 

for one or two classes of compounds and use liquid-liquid 

extraction with an organic solvent followed by analysis with 

gas chromatography (GC) and nitrogen-phosphorus, electroncapture, or mass spectrometry (MS) detection. Analytical 

methods that use solid-phase extraction (SPE) as an alternative 

to liquid-liquid extraction were adopted for this study.

POCIS and SPMD Media Preparation and 

Extraction

A detailed description of the preparation of the POCIS 

is given by Alvarez and others (2004, 2005, 2007). POCIS 

of both the pesticide and pharmaceutical configurations were 

used in this study. The pesticide POCIS disk contained media 

composed of a triphasic admixture of (80:20 w:w) Isolute 

ENV+ and S-X3 dispersed Ambersorb 1500, and the pharmaceutical POCIS disk contained Oasis HLB media. Each 

POCIS disk had an effective sampling surface area of 41 

cm2. The membrane surface area to total sorbent mass ratio 

of POCIS used in this study was approximately 180 cm2/g. 

This ratio conforms to the definition of a standard POCIS as 

defined by Alvarez and others (2004). Three pesticide and 

three pharmaceutical POCIS were placed inside each deployment canister.

Procedures for the recovery of the sequestered chemical 

residues from environmental and quality control POCIS are 

described in detail by Alvarez and others (2004). Briefly, the 

POCIS were disassembled, and the sorbent was transferred 

into glass gravity-flow chromatography columns. Chemical 

residues were recovered from the sorbent by organic solvent 

elution. Methanol was used to recover analytes from the pharmaceutical POCIS, and a combination of 1:1:8 (v:v:v) 

methanol:toluene:dichloromethane was used to recover chemicals from the pesticide POCIS. The extracts were reduced in 

volume by rotary evaporation and under a gentle stream of 

nitrogen, filtered through glass-fiber filter, solvent exchanged 

as necessary, and sealed in amber ampoules under nitrogen 

for shipment to the collaborating analytical laboratories. 

Each sample was a composite of extracts from two individual 

POCIS disks to increase the total mass of sequestered residues 

and thereby lower analytical detection limits.

SPMDs were prepared as described by Huckins and 

others (2006) and Petty and others (2000 and 2004). Briefly, 

the SPMD were constructed by adding 59 μL of triolein to 

a 10-cm piece of low-density polyetheleyne (LDPE) tubing (5 cm between the lipid containment seals). A mixture 

of perdeuterated PAHs (500 ng each of acenaphthylene-d10, 

acenaphthene-d10, fluorene-d10, phenanthrene-d10, pyrene-d10

and dibenz[a,h]anthracene-d14) were also added to the SPMDs 

to serve as performance reference compounds (PRCs). PRCs 

are used to correct sampling rate data for the site-specific 

factors such as flow, temperature, and biofouling, which can 

affect the uptake kinetics of passive samplers. A single SPMD 

was added to each deployment sampler.

Recovery of the PRCs and other chemicals of interest 

(that is, PAHs sampled from the study sites) was achieved 

using a two-stage dialysis of the SPMD with hexane. Following dialysis, the extracts were concentrated and the chemicals 

of interest isolated using a size exclusion chromatographic 

(SEC) system. Then, the fractions from the SEC system were 

applied to a gravity-flow chromatographic column containing acidic, basic, and neutral silica gel to remove additional 

potential interferences and to enrich the PAHs and PRCs prior 

to analysis.

Chemical Analysis of POCIS and SPMD Extracts

POCIS extracts were analyzed for compounds in the 

macrolide, sulfonamide, quinoline, and tetracycline classes 

of antibiotics as well as for chlroamphenicol, lincomycin, 

ormetoprim, and trimethoprim and the pharmaceuticals carbamazepine and ibuprofen. Clinafloxacin, demeclocycline, 

erythromycin-13C2, erythromycin-H2O-13C2, simatone, and 

sulfamethoxazole-13C6 were used as internal standards and oleandomycin, meclocycline, nalidixic acid, and sulfamethazine13C6

 as surrogate standards. Samples were analyzed using the 

method of standard addition.

Internal standard and surrogate standard solutions were 

combined and diluted to 0.1 ng/μL solutions with 50 mM 

phosphoric acid (H3PO4) pH 7 to a final volume of 2 mL in a 

2-mL glass chromatography vial. The 1 ng/μl standard mix for 

standard addition also was diluted to 0.1 ng/μL with 50 mM 

H3

PO4 pH 7 to a final volume of 2 mL in a 2-mL glass chromatography vial. A blank solution of methanol and reagent 

water (50/50) was added to a 2-mL glass chromatography vial. 

The internal and surrogate standard solution, standard mix 

solution, and blank solution were added to the liquid-chromatography (LC) auto sampler along with the methanol POCIS 

extracts and reagent water blank.

Each POCIS extract was analyzed two times. The LC 

auto sampler first pulled and mixed 20 μL of sample, 20 μL of 

internal and surrogate standard, and 20 μL of blank solution 

and injected it into the LC auto sampler for analysis. The LC 

then pulled 20 μL of sample, 20 μL of internal and surrogate 

standard, and 20 μL of standard mix and injected it into the LC 

for analysis. The second sample analysis was the equivalent 

of spiking the sample at 100 μg/L. Standard solutions of 1 to 

1,000 μg/L were injected and analyzed by standard addition to 
Appendix A 25

assess the linearity of the concentration range for the standard 

addition and to estimate the analyte detection levels.

The antibiotics were separated using a LC gradient with 

the 0.3 percent formic acid mobile phase A and acetonitrile/

methanol (80/20) mobile phase B. A 3.0 × 150 mm Luna 

C18(2) (Phenonomenex) LC column with 3-μm packing was 

used to separate the antibiotics. The LC column was rinsed 

for 5 minutes with 100 percent mobile phase B at the end of 

the gradient and then equilibrated at initial conditions for 5 

minutes before the next sample analysis.

Individual antibiotic compounds were analyzed using 

selected ion monitoring liquid chromatography/tandem mass 

spectrometry and were identified using retention times and the 

ratios of the quantifying ion to one or two confirming ions. 

Detected antibiotic compounds were quantitated using the 

ratio of the area of the base-peak ion of the analyte to the area 

of the base-peak ion of the internal standard. The antibiotic 

compounds may also have been quantitated by the method of 

standard addition using the following equation:

C=(Rus/(Rsp –Rus))Csp (1)

where

C is the concentration of the analyte in the 

unspiked sample,

Rus is the ratio of area of the quantitation-ion of 

the analyte to the area of the quantitationion of the internal standard in the unspiked 

sample,

Rsp is the ratio of area of the quantitation-ion of 

the analyte to the area of the quantitationion of the internal standard in the spiked 

sample, and

Csp is the concentration of the analytes in the 

spiked sample due to the spike.

The method of standard addition corrects for matrix effects 

and can result in more accurate quantitation of individual 

analytes.

The analytical method for the determination of wastewater compounds in POCIS extracts targets 66 compounds 

typically found in domestic and industrial wastewater. The 

wastewater method is an efficient means of detecting important toxic and estrogenic compounds that otherwise might 

not be reported because they are unregulated or not included 

in other USGS or U.S. Environmental Protection Agency 

methods (Zaugg and others, 2007). Analysis of the alkylphenol ethoxylate nonionic surfactant compounds is particularly 

important because they are persistent indicators of wastewater. 

Other method compounds are representative of fragrances, 

food additives, antioxidants, flame retardants, plasticizers, 

industrial solvents, disinfectants, fecal sterols, PAHs, and 

high-use domestic pesticides.

The POCIS extracts analyzed for organic wastewater 

compounds at the USGS National Water Quality Laboratory 

arrived in sealed ampoules containing methylene chloride, 

approximately 0.5 mL in volume. Each ampoule was opened, 

and 20 μL of a five-compound internal standard mixture [(1,4-

dichlorobenzene-d4 (IS1), naphthalene-d8 (IS2), acenapthened10 (IS3), phenanthrene-d10 (IS4), chrysene-d12 (IS5)] was 

added to the vial before transferring the entire contents using 

a disposable Pasteur pipette to a labeled 2-mL GC/MS vial. To 

ensure complete transfer of sample extracts, an additional 

400 μL of methylene chloride was used to rinse the open 

ampoules and the rinsate was transferred to the GC/MS vial 

using the same pipette. The sample extracts (in 900–1,000 μL 

of methylene chloride) were analyzed by full scan positive-ion 

GC/MS in the electron impact mode (Model 5975 quadrupole mass spectrometer; Hewlett-Packard/Agilent, Palo Alto, 

Calif.), along with a set of multiple-level analytical standard 

solutions; this was the same as the normal analytical schedule 

1433 method (Zaugg and others, 2007).

Each POCIS extract analyzed for pharmaceuticals was 

analyzed first with positive mode electrospray ionization 

interface on a liquid chromatography/mass spectrometer (LC/

MS) system (Model LC/MSD quadrupole mass spectrometer; 

Hewlett-Packard/Agilent, Palo Alto, Calif.), along with a set 

of multiple-level analytical standard solutions. A binary water: 

acetonitrile gradient was used on a reversed phase LC column. The instrument procedure used followed the analytical 

methodology initially described in Cahill and others (2004) 

but included additional pharmaceutical compounds. Selected 

POCIS extracts also were analyzed using a LC/MS/MS 

system, operated in the multiple-reaction monitoring mode, 

to confirm the identity of pharmaceuticals. For the reasons 

described later in this appendix, pharmaceutical concentrations 

are reported as nanograms per POCIS. 

Analysis of the SPMD extracts for hydrophobic compounds (PAHs and PRCs) was done using an Agilent 6890 GC 

(Agilent Technologies, Inc., Wilmington, Del.) coupled to a 

5973N mass selective detector (MSD; Agilent Technologies, 

Inc., Palo Alto, Calif.). An HP–5MS (30 m x 0.25 mm i.d. x 

0.25 -μm film thickness) capillary column (Agilent Technologies, Inc., Wilmington, Del.) was used with the temperature 

program of injection at 50°C, held for 2 min, ramped at 25°C/

min to 130°C, held for 1 minute, then ramped at 6°C/min to 

310°C and held at 310°C for 5 minutes. Detector zone temperatures were set at 310°C for the MSD transfer line, 150°C at the 

quadrupole, and 230°C at the source. Quantitation of the analytes was accomplished using a six-point curve with internal 

calibration. Concentrations of calibration standards bracketed 

the range of 20 to 4,000 μg/L for each of the analytes with the 

2-methylnaphthalene-d10 and benzo[e]pyrene-d12 maintained at 

0.25 μg/mL as the instrumental internal standard. 

Chemical Analysis of Streambed Sediments

Streambed-sediment samples were processed with standard approved and custom laboratory methods (Burkhardt and 

others, 2006). Streambed-sediment samples were analyzed for 

pharmaceuticals and other wastewater compounds at NWQL. 
26 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

The list of targeted pharmaceutical compounds in bed-sediment is presented in table B1, and the wastewater compounds 

are in table B3.

Pharmaceuticals in sediment were determined by the 

method described in Kinney and others (2006a, b) for the 

analysis of soils and biosolids. Briefly, an aliquot of wet sediment, equivalent to 10 g of dry solids, is extracted by using 

pressurized solvent extraction, which minimizes degradation 

of these polar, labile compounds. Five sequential extractions 

were carried out using 70 percent acetonitrile/30 percent 

water at a temperature of 130°C and a pressure of 10.34 x 

107 Pa (15,000 lbf/in2). Typically, the final volume of extract 

was about 20 mL. A 1-mL extract subsample was filtered 

using a 0.20-mm syringe filter into a high-performance liquid 

chromatography (HPLC) vial, and then the acetonitrile was 

evaporated under nitrogen. The concentrated aqueous extract 

volume (approximately 0.3 mL) was increased to 1 mL with 

0.050 mL of a 1.59 x 10-4 mM nicotinamide-2,4,5,6-d4 solution, added as an internal standard, and approximately 0.65 

mL of a 10 mM aqueous ammonium formate buffer. The sediment extracts were analyzed in a similar manner to the POCIS 

extracts, using the method of Cahill and others (2004), but 

including additional pharmaceuticals. As noted in Kinney and 

others (2006a), mean recoveries of individual pharmaceuticals 

in three soil types ranged between 39 and 94 percent. Recoveries of pharmaceuticals from streambed sediment from Tinkers 

Creek were expected to be similar.

Streambed-sediment samples analyzed for wastewater 

compounds were extracted using a pressurized solvent extraction system with water/isopropyl alcohol as the extraction solvent (Burkhardt and others, 2006). Following extraction, the 

compounds of interest were isolated from potentially interfering matrix components using disposable solid-phase extraction 

(SPE) cartridges containing chemically modified polystyrenedivinylbenzene resin. The cartridges were dried with nitrogen 

gas, then sorbed compounds were eluted with methylene 

chloride (80 percent)-diethyl ether (20 percent) through a 

Florisil/sodium sulfate SPE cartridge and then analyzed by 

capillary-column gas chromatography/mass spectrometry (GC/

MS). Initial method reporting levels for single-component 

compounds ranged from 50 to 500 μg/kg.

Passive Sampling Theory

Estimation of Ambient Water Concentrations

SPMD and POCIS uptake kinetic data (sampling rates) 

are required to accurately estimate aquatic concentrations of 

environmental contaminants. Using models previously developed (Alvarez and others, 2004, 2007; Huckins and others, 

2006), data from the analysis of the PRC concentrations and 

from calibration studies (when available), the bioavailable 

(that is, via respiration from the dissolved phase) concentrations of analytes in POCIS and SPMDs deployed in the study 

sites can be estimated for selected chemicals.

 Method detection limits (MDL) and laboratory reporting level (LRL) for SPMD results were estimated from 

low-level standards as determined by the signal-to-noise ratio 

of the response from the instrumental analysis of the sample 

blanks. LRLs were determined as the mean of the response 

of a coincident peak present in the analysis of the blanks plus 

3 standard deviations of the response of the coincident peak 

present during instrumental analysis (Keith, 1991). The LRLs 

were determined as the greater of the mean plus 10 standard 

deviations or the concentration of the low-level calibration 

standard (Keith, 1991). In cases where no coincident peak was 

present, the LRL was set at the low-level calibration standard, 

and the MDL was estimated to be 20 percent of the LRL.

The effects of exposure conditions on SPMD and POCIS 

uptake and dissipation rates are largely a function of (1) facial 

velocity-turbulence at the membrane surface, which in turn is 

affected by the design of the deployment canister, (2) exposure 

medium temperature, and (3) membrane biofouling. PRCs are 

analytically noninterfering organic compounds having a moderate to high fugacity from SPMDs that are added to the lipid 

prior to membrane enclosure and field deployment (Huckins 

and others, 2006). By comparing the rate of PRC loss during field exposures to that of laboratory studies, an exposure 

adjustment factor (EAF) can be derived and used to adjust 

laboratory sampling rates to more accurately reflect actual in 

situ sampling rates. PRCs will undergo increased loss as the 

logarithm of their octanol-water partition coefficient (that is, 

log Kow) value decreases. The loss rate is isotropic, meaning 

the uptake rate is equal to the loss rate, and is dependent on 

the same environmental factors influencing chemical uptake. 

Because of the strong sorptive properties of the adsorbents 

used in the POCIS, attempts to incorporate PRCs into the 

POCIS have failed (Alvarez and others, 2007).

 Uptake of hydrophobic chemicals into SPMDs follows linear, curvilinear, and equilibrium phases of sampling. 

Integrative (or linear) sampling is the predominant phase for 

compounds with log Kow values ≥ 5.0 and exposure periods 

of up to 1 month. During the linear uptake phase, the ambient 

chemical concentration (Cw) is determined by

 

Cw =N/(Rst) (2)

where

N is the amount of the chemical sampled by an 

SPMD (typically in nanograms),

Rs is the SPMD sampling rate (liters per day), 

and

t is the exposure time (days).

Estimation of a chemical’s site-specific Rs in an SPMD and 

its ambient Cw requires the derivation of the EAF as described 

by Huckins and others (2006). A key feature of the EAF is 

that it is relatively constant for all chemicals that have the 

same rate-limiting barrier to uptake, which allows PRC data 
Appendix A 27

to be applied to a range of chemicals. Thus, the in situ or site 

specific sampling rate, Rsi, of an analyte is the EAF times its 

laboratory calibration Rs.

Uptake of hydrophilic organic chemicals by the POCIS is 

controlled by many of the same rate-limiting barriers, allowing the use of the same models to determine ambient water 

concentrations. Previous data indicate that many chemicals 

of interest remain in the linear phase of sampling for at least 

56 days (Alvarez and others, 2004, 2007); therefore, the use 

of a linear uptake model (eq. 2) for the calculation of ambient 

water concentrations would be justified in cases where the Rs

for a chemical was known. Such Rs data for the chemicals targeted in this study are largely unknown; therefore, the POCIS 

data presented in this report are expressed as nanograms of 

chemical sequestered per POCIS disk. In spite of the inability 

to estimate concentrations in the water surrounding each sampler, the data produced are useful for the positive identification 

of target analytes and for comparison of the relative amounts 

of chemicals sampled at each site.

References Cited

Alvarez, D.A., Petty, J.D., Huckins, J.N., Jones-Lepp, T.L., 

Getting, D.T., Goddard, J.P., and Manahan, S.E., 2004, 

Development of a passive, in situ, integrative sampler for 

hydrophilic organic contaminants in aquatic environments: 

Environmental Toxicology and Chemistry, v. 23, no. 3, 

p. 1640–1648.

Alvarez, D.A., Stackelberg, P.E., Petty, J.D., Huckins, J.N., 

Furlong, E.T., Zaugg, S.D., and Meyer, M.T., 2005, Comparison of a novel passive sampler to standard water-column 

sampling for organic contaminants associated with wastewater effluents entering a New Jersey stream: Chemosphere, 

v. 61, no. 5, p. 610–622.

Alvarez, D.A.; Huckins, J.N.; Petty, J.D.; Jones-Lepp, Tammy; 

Stuer-Lauridsen, Frank; Getting, D.T.; Goddard, J.P.; and 

Gravell, Anthony, 2007, Tool for monitoring hydrophilic 

contaminants in water—Polar organic chemical integrative 

sampler (POCIS), in Greenwood, R., Mills, G., and Vrana, 

B., eds., Passive sampling techniques in environmental 

monitoring, v. 48 of Wilson & Wilson’s Comprehensive 

analytical chemistry: Amsterdam, Elsevier, chap. 8, 

p. 171–197.

Burkhardt, M.R., Zaugg, S.D., Smith, S.G., and ReVello, R.C., 

2006, Determination of wastewater compounds in sediment and soil by pressurized solvent extraction, solid-phase 

extraction, and capillary-column gas chromatography/

mass spectrometry: U.S. Geological Survey Techniques and 

Methods, book 5, sec. B, chap. 2, 33 p.

Cahill J.D., Furlong, E.T., Burkhardt, M.R., Kolpin, D.W., 

and Anderson L.G., 2004, Determination of pharmaceutical 

compounds in surface- and ground-water samples by solidphase extraction and high-performance liquid chromatography—Electrospray ionization mass spectrometry: Journal of 

Chromatogography A, v. 1041, nos. 1–2, p. 171–180.

Huckins, J.N., Petty, J.D., and Booij, Kees, 2006, Monitors 

of organic chemicals in the environment—Semipermeable 

membrane devices: New York, Springer, 223 p.

Keith, L.H., 1991, Environmental sampling and analysis—A 

practical guide: Boca Raton, Fla., CRC Press, p. 101–113.

Kinney, C.A., Furlong, E.T., Werner, S.L., and Cahill, J.D., 

2006a, Presence and distribution of wastewater-derived 

pharmaceuticals in soil irrigated with reclaimed water: 

Environmental Toxicology and Chemistry, v. 25, no. 2, 

p. 317–326

Kinney, C.A., Furlong, E.T., Zaugg, S.D., Burkhardt, M.R., 

Werner, S.L., Cahill, J.D., and Jorgensen, G.R., 2006b, 

Survey of organic wastewater contaminants in biosolids 

destined for land application: Environmental Science & 

Technology, v. 40, no. 23, p. 7207–7215.

Petty, J.D., Orazio, C.E., Huckins, J.N., Gale, R.W., Lebo, 

J.A., Meadows, J.C., Echols, K.R., and Cranor, W.L., 2000, 

Considerations involved with the use of semipermeable 

membrane devices for monitoring environmental contaminants: Journal of Chromatography A, v. 879, no. 1, 

p. 83–95.

Petty, J.D., Huckins, J.N., Alvarez, D.A., Brumbaugh, W.G., 

Cranor, W.L., Gale, R.W., Rastall, A.C., Jones-Lepp, T.L., 

Leiker, T.J., Rostad, C.E., and Furlong, E.T., 2004, A holistic passive integrative sampling approach for assessing the 

presence and potential impacts of waterborne environmental 

contaminants: Chemosphere, v. 54, p. 695–705.

Zaugg, S.D., Smith, S.G., Schroeder, M.P., Barber, L.B., and 

Burkhardt, M.R., 2007, Methods of analysis by the U.S. 

Geological Survey National Water Quality Laboratory—

Determination of wastewater compounds by polystyrenedivinylbenzene solid-phase extraction and capillary-column 

gas chromatography/mass spectrometry (ver. 1.1): U.S. 

Geological Survey Water-Resources Investigations Report 

01–4186, 37 p.
28 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Appendix B. Organic Wastewater Compound Analytes and Reporting Levels, 

by Sample Media and Analytical Method 

Appendix B contains CAS Registry Numbers®, which is a Registered Trademark of the American Chemical Society. CAS 

recommends the verification of the CASRNs through CAS Client ServicesSM.

Table B1. Antibiotic method for POCIS extracts, including compound names, uses, classes, and Chemical Abstract 

Service registry numbers for antibiotic compounds.

[ng/POCIS, nanograms per extract for one polar organic chemical integrative sampler disk; CAS, Chemical Abstract Service]

Compound 

name

Laboratory 

reporting level

(ng/POCIS)

Use CAS number

Azithromycin 1.0 Antibiotic (human and veterinary; macrolide class) 83905-01-5

Carbamazepine 1.0 Anticonvulsant, antineuralgic (prescription) 298-46-4

Chloramphenicol 10.0 Antibiotic (veterinary) 56-75-7

Chlortetracyline 5.0 Antibiotic (veterinary; tetracycline class) 57-62-5

Ciprofloxacin 1.0 Antibiotic (human and veterinary; quinolone class) 85721-33-1

Doxycycline 5.0 Antibiotic (human and veterinary; tetracycline class) 564-25-0

Enrofloxacin 1.0 Antibiotic (veterinary; quinolone class) 93106-60-6

Epi-chlortetracycline 5.0 Chlortetracycline degradate 57-62-5

Epi-iso-chlortetracycline 5.0 Chlortetracycline degradate 57-62-5

Epi-oxytetracycline 5.0 Oxytetracycline degradate 79-57-2

Epi-tetracycline 5.0 Tetracycline degradate 60-54-8

Erythromycin-H2

O (Anhydroerythromycin) 1.0 Erythromycin degradate 114-07-8

Ibuprofen 10.0 Anti-inflammatory (nonprescription) 15687-27-1

Iso-chlortetracycline 5.0 Chlortetracycline degradate 57-62-5

Lincomycin 1.0 Antibiotic (veterinary; macrolide class) 154-21-2

Lomefloxacin 1.0 Antibiotic (veterinary; quinolone class) 98079-51-7

Norfloxacin 1.0 Antibiotic (human and veterinary; quinolone class) 70458-96-7

Ofloxacin 1.0 Antibiotic (human and veterinary; quinolone class) 83380-47-6

Ormetoprim 1.0 Antibiotic (veterinary; sulfonamide class) 6981-18-6

Oxytetracycline 5.0 Antibiotic (veterinary; tetracycline class) 79-57-2

Roxithromycin 1.0 Antibiotic (human and veterinary; macrolide class) 80214-83-1

Sarafloxacin 1.0 Antibiotic (veterinary; quinolone class) 98105-99-8

Sulfachlorpyridazine 1.0 Antibiotic (veterinary; sulfonamide class) 80-32-0

Sulfadiazine 1.0 Antibiotic (veterinary; sulfonamide class) 68-35-9

Sulfadimethoxine 1.0 Antibiotic (veterinary; sulfonamide class) 122-11-2

Sulfamethoxazole 1.0 Antibiotic (human and veterinary; sulfonamide class) 723-46-6

Sulfamethazine 1.0 Antibiotic (veterinary; sulfonamide class) 57-68-1

Suflathiazole 1.0 Antibiotic (veterinary; sulfonamide class) 72-14-0

Tetracycline 5.0 Antibiotic (human and veterinary; tetracycline class) 60-54-8

Trimethoprim 1.0 Antibiotic (human and veterinary; sulfonamide class) 738-70-5

Tylosin 1.0 Antibiotic (veterinary; macrolide class) 1401-69-0

Virginiamycin 1.0 Antibiotic (veterinary; macrolide class) 21411-53-0
Appendix B 29

Table B2. Pharmaceutical method for POCIS extracts, including compound names, uses, classes, and 

Chemical Abstract Service registry numbers for pharmaceutical compounds.

[ng/POCIS, nanograms per extract for one polar organic chemical integrative sampler disk; CAS, Chemical Abstract 

Service]

Compound 

name

Laboratory 

reporting 

level

 (ng/POCIS)

Use CAS 

number

1,7-Dimethylxanthine 5.0 Precursor is a stimulant 611-59-6

Acetaminophen 5.0 Analgesic 103-90-2

Albuterol 5.0 Bronchodilator 18559-94-9

Azithromycin 5.0 Antibiotic 83905-01-5

Caffeine 5.0 Stimulant 58-08-2

Carbamazepine 5.0 Antiepileptic 298-46-4

Cimetidine 5.0 Inhibits production of stomach acid 51481-61-9

Codeine 5.0 Opiate agonist 76-57-3

Cotinine 5.0 Naturally occurring alkaloid stimulant 486-56-6

Dehydronifedipine 5.0 Precursor is an antiangial 67035-22-7

Diltiazem 5.0 Antihypertensive 42399-41-7

Diphenhydramine 5.0 Anntipruritic 58-73-1

Erythromycin 5.0 Antibiotic 114-07-8

Fluoxetine 5.0 Antidepressant 54910-89-3

Miconazole 5.0 Antifungal 22916-47-8

Ranitidine 5.0 Antacid 66357-35-5

Sulfamethoxazole 5.0 Antibiotic 723-46-6

Thiabendazole 5.0 Anthelmintic, fungicide 148-79-8

Trimethoprim 5.0 Antibiotic 738-70-5

Warfarin 5.0 Anticoagulant, rodenticide 81-81-2
30 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Table B3. Wastewater method for POCIS extracts, including compound names, suspected endocrine disruptor, CAS number, and 

possible compound uses (modified from Zaugg and others, 2007).

[EDC, known or suspected endocrine disruptor; Y, yes; -; no or status is not known; CAS, Chemical Abstract Service; F, fungicide; H, herbicide; I, insecticide; 

GUP, general-use pesticide; FR, flame retardant; WW, wastewater; Mfr, manufacturing; %, percent; >, greater than; CP, combustion product; UV, ultraviolet; 

ng/POCIS, nanograms per extract for one polar organic chemical integrative sampler disk]

Compound name EDC CAS number Possible compound uses or sources4

Laboratory 

reporting 

level (ng/

POCIS)

1,4-Dichlorobenzene1,5 Y 106-46-7 Moth repellant, fumigant, deodorant 200

1-Methylnaphthalene - 90-12-0 2-5% of gasoline, diesel fuel, or crude oil 200

2-butoxyetanol phosphate - 39454-62-1 Solvent 200

2,6-Dimethylnaphthalene5 - 581-42-0 Present in diesel/kerosene (trace in gasoline) 200

2-Methylnaphthalene - 91-57-6 2-5% of gasoline, diesel fuel, or crude oil 200

3-β-Coprostanol - 360-68-9 Carnivore fecal indicator 200

3-Methyl-1(H)-indole (Skatole) - 83-34-1 Fragrance, stench in feces and coal tar 200

3-tert-Butyl-4-hydroxy anisole (BHA) 1 Y 25013-16-5 Antioxidant, general preservative 200

4-Cumylphenol Y 599-64-4 Nonionic detergent metabolite 200

4-n-Octylphenol Y 1806-26-4 Nonionic detergent metabolite 200

4-tert-Octylphenol Y 140-66-9 Nonionic detergent metabolite 200

5-Methyl-1H-benzotriazole7 - 136-85-6 Antioxidant in antifreeze and deicers 200

Acetophenone - 98-86-2 Fragrance in detergent and tobacco, flavor in beverages 200

Acetyl hexamethyl tetrahydronaphthalene 

(AHTN) Y 21145-77-7 Musk fragrance, persistent and widespread, in ground water, concern for bioaccumulation & toxicity 200

Anthracene5

 - 120-12-7 Wood preservative, component of tar, diesel, or crude oil, 

CP 200

Anthraquinone5 - 84-65-1 Dye mfr and textiles, seed treatment, bird repellant 200

Atrazine5,6 Y 1912-24-9 Selective triazine herbicide 200

Benzo[a]pyrene5

 Y 50-32-8 Regulated PAH, used in cancer research, CP 200

Benzophenone Y 119-61-9 Fixative for perfumes and soaps 200

β-Sitosterol - 83-46-5 Plant sterol 200

β-Stigmastanol - 19466-47-8 Plant sterol 200

Bisphenol A Y 80-05-7 Mfr polycarbonate resins, antioxidant, FR 200

Bromacil5 - 314-40-9 H (GUP), >80% noncrop usage on grass/brush 200

Bromoform1, 5,7 - 75-25-2 WW ozination byproduct, military/explosives 200

Caffeine5,7 - 58-08-2 Beverages, diuretic, very mobile/biodegradable 200

Camphor - 76-22-2 Flavor, odorant, ointments 200

Carbaryl2, 5,7 Y 63-25-2 I, crop and garden uses, low persistence 200

Carbazole - 86-74-8 I, Mfr dyes, explosives, and lubricants 200

Chlorpyrifos5

 Y 2921-88-2 I, domestic pest and termite control (domestic use restricted as of 2001) 200

Cholesterol - 57-88-5 Often a fecal indicator, also a plant sterol 200

Cotinine7 - 486-56-6 Naturally occurring alkaloid stimulant 200

Cumene (Isopropylbenzene) 1 - 98-82-8 Mfr phenol/acetone, fuels and paint thinner 200

Diazinon5

 Y 333-41-5 I, > 40% nonagricultural usage, ants, flies 200

Diethylhexyl phthalate (DEHP) 5,6 Y 117-81-7 Plasticizer for polymers and resins, pesticide inert 200

Diethyl phthalate (DEP) 5,6 Y 84-66-2 Plasticizer for polymers and resins 200

d-Limonene1 - 5989-27-5 F, antimicrobial, antiviral, fragrance in aerosols 200

Ethyl citrate - 77-93-0 Flavoring

Fluoranthene5 - 206-44-0 Component of coal tar and asphalt (only traces in gasoline 

or diesel fuel), CP 200

Hexahydrohexamethylcyclopentabenzopyran (HHCB) Y 1222-05-5 Musk fragrance, persistent and widespread, in ground 

water, concern for bioaccumulation and toxicity 200

Indole - 120-72-9 Pesticide inert ingredient, fragrance in coffee 200

Isoborneol - 124-76-5 Fragrance in perfumery, in disinfectants 200

Isophorone5 - 78-59-1 Solvent for lacquer, plastic, oil, silicon, resin 200

200
Appendix B 31

Table B3. Wastewater method for POCIS extracts, including compound names, suspected endocrine disruptor, CAS number, and 

possible compound uses (modified from Zaugg and others, 2007).—Continued

Compound name EDC CAS number Possible compound uses or sources4

Laboratory 

reporting 

level (ng/

POCIS)

Isoquinoline5 - 119-65-3 Flavors and fragrances 200

Menthol - 89-78-1 Cigarettes, cough drops, liniment, mouthwash 200

Metalaxyl5 - 57837-19-1 H, F (GUP), mildew, blight, pathogens, golf/turf 200

Methyl salicylate - 119-36-8 Liniment, food, beverage, UV-absorbing lotion 200

Metolachlor5 - 51218-45-2 H (GUP), indicator of agricultural drainage 200

N,N-diethyl-meta-toluamide (DEET) - 134-62-3 I, urban uses, mosquito repellent 200

Naphthalene5

 - 91-20-3 Fumigant, moth repellent, major component (about 10%) 

of gasoline 200

4-Nonylphenol diethoxylate (NP2EO; sum 

of all isomers)3 Y 26027-38-3 Nonionic detergent metabolite 200

4-Nonylphenol monoethoxylate (NP1EO; 

sum of all isomers)3,6 Y N/A Nonionic detergent metabolite 200

4-Octylphenol diethoxylate (OP2EO; sum of 

all isomers)3 Y 26636-32-8 Nonionic detergent metabolite 200

4-Octylphenol monoethoxylate (OP1EO; 

sum of all isomers)3 Y 26636-32-8 Nonionic detergent metabolite 200

p-Cresol5

 - 106-44-5 Wood preservative 200

p-Nonylphenol (total)3 Y 84852-15-3 Nonionic detergent metabolite 200

Phenanthrene5

 - 85-01-8 Mfr explosives, component of tar, diesel fuel, or crude oil, 

CP 200

Phenol5

 - 108-95-2 Disinfectant, mfr several products, leachate 200

Polybrominated diphenyl ether Y 5436-43-1 Textiles and electronics, flame retardant 200

Prometon5 - 1610-18-0 H (noncrop only), applied prior to blacktop 200

Pyrene5

 - 129-00-0 Component of coal tar and asphalt (only traces in gasoline or diesel fuel), CP 200

Tetrachloroethylene1, 5,7 - 127-18-4 Solvent, degreaser, veterinary anthelmintic 200

Tris(2-chloroethyl) phosphate - 115-96-8 Plasticizer, flame retardant 200

Tri(1,3-dichloro-2-propyl) phosphate - 13674-87-8 Flame retardant 200

Tributyl phosphate - 126-73-8 Antifoaming agent, flame retardant 200

Triclosan Y 3380-34-5 Disinfectant, antimicrobial (concern for acquired microbial resistance) 200

Triethyl citrate (ethyl citrate) - 77-93-0 Cosmetics, pharmaceuticals 200

Triphenyl phosphate - 115-86-6 Plasticizer, resin, wax, finish, roofing paper, FR 200

Tri(2-butoxyethyl) phosphate - 78-51-3 Flame retardant 200

1

Concentration is always estimated because recovery is less than 60 percent or variability is greater than 25 percent RSD.

2

Concentration is always estimated because of unstable instrument response.

3

Concentration is always estimated because the reference standard is from a technical mixture.

4

Web links to compound uses, URL: http://wwwnwql.cr.usgs.gov/USGS/Reno/lc8033.html; ChemFinder Webserver: http://chemfinder.camsoft.com/; NTP 

National toxicology program health & safety data: http://ntp-server.niehs.nih.gov/Main_Pages/Chem-HS.html; NIST Chemistry WebBook: http://webbook.

nist.gov/; Spectrum Laboratories, Inc.: http://www.speclab.com/compound/chemabc.htm; RxList: http://www.rxlist.com/; EXtension TOXicology NETwork 

(EXTOXNET): http://ace.ace.orst.edu/info/extoxnet/

5

Compound determined by at least one other method at the National Water Quality Laboratory.

6

Compound only available with lab code 8033 or 8050—not approved for schedule 1433.

7

Compound not available with sediment analysis (lab code 8050).
32 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Table B4. Hydrophobic method for SPMD extracts, including compound names, types, and Chemical Abstract 

Service registry numbers for hydrophobic compounds.

[ng/L, nanograms per liter; CAS, Chemical Abstract Service; PAH, polycyclic aromatic hydrocarbon. Water concentrations are 

estimated on the basis of recovery of performance reference compounds]

Compound 

name

Compound

type

CAS

number

Estimated 

method detection level 

(ng/L)

Laboratory 

reporting level

 (ng/L)

1,2-Dimethylnaphthalene PAH 573-98-8 0.5 2.4

1-Ethylnaphthalene PAH 1127-76-0 0.4 2.2

1-Methylfluorene PAH 1730-37-6 0.3 1.5

1-Methylnaphthalene PAH 90-12-0 0.6 4.8

2,3,5-Trimethylnaphthalene PAH 2245-38-7 0.3 1.5

2-Methylfluoranthene PAH 33543-31-6 0.0 1.4

2-Methylnaphthalene PAH 91-57-6 1.3 4.8

2-Methylphenanthrene PAH 2531-84-2 0.1 1.5

3,6-Dimethylphenanthrene PAH 1576-67-6 0.0 1.4

4-Methylbiphenyl Flavoring agent 644-08-6 2.8 6.9

9-Methylanthracene PAH 779-02-2 0.0 1.4

Acenaphthene PAH 83-32-9 0.4 2.7

Acenaphthylene PAH 208-96-8 0.7 3.3

Anthracene PAH 120-12-7 0.3 1.9

Benz[a]anthracene PAH 56-55-3 0.0 1.5

Benzo[a]pyrene PAH 50-32-8 0.0 1.7

Benzo[b]fluoranthene PAH 205-99-2 0.0 1.4

Benzo[b]naphtho[2,1-d]thiophene PAH 239-35-0 0.0 1.4

Benzo[b]thiophene PAH 95-15-8 9.3 46.7

Benzo[e]pyrene PAH 192-97-2 0.1 1.8

Benzo[g,h,i]perylene PAH 191-24-2 0.0 2.3

Benzo[k]fluoranthene PAH 207-08-9 0.0 1.6

Biphenyl PAH 92-52-4 0.9 4.4

Chrysene PAH 218-01-9 0.1 1.4

Dibenz[a,h]anthracene PAH 53-70-3 0.0 1.9

Dibenzothiophene PAH 132-65-0 0.1 2.2

Fluoranthene PAH 206-44-0 1.0 2.6

Fluorene PAH 86-73-7 0.2 2.2

Indeno[1,2,3-c,d]pyrene PAH 193-39-5 0.4 2.1

Naphthalene PAH 91-20-3 2.5 12.3

Perylene PAH 198-55-0 0.3 1.5

Phenanthrene PAH 85-01-8 1.7 4.1

Pyrene PAH 129-00-0 0.5 1.4
Appendix B 33

Table B5. Pharmaceutical method for streambed-sediment samples, including compound names, uses, classes, and 

Chemical Abstract Service registry numbers for pharmaceutical compounds.

[MDL, method detection limit; LRL, laboratory reporting levels determined by using matrix-free ashed sand; CAS, Chemical Abstract Service; 

μg/kg, micrograms per kilogram]

Compound 

name

Use CAS number Estimated 

MDL2

 (μg/kg)

Interim 

LRL3 (μg/kg)

1,7-Dimethylxanthine Precursor is a stimulant 611-59-6 2.03 4.06

Acetaminophen1 Analgesic 103-90-2 0.76 1.52

Albuterol1 Bronchodilator 18559-94-9 1.09 2.18

Azithromycin Antibiotic 83905-01-5

Caffeine Stimulant 58-08-2 1.32 2.65

Carbamazepine Antiepileptic 298-46-4 1.65 3.3

Cimetidine1 Inhibits production of stomach acid 51481-61-9 0.88 1.76

Codeine Opiate agonist 76-57-3 1.32 2.64

Cotinine Naturally occurring alkaloid stimulant 486-56-6 1.3 2.61

Dehydronifedipine Precursor is an antiangial 67035-22-7 1.69 3.38

Diltiazem1 Antihypertensive 42399-41-7 1.48 2.96

Diphenhydramine Antipruritic 58-73-1 1.35 2.71

Erythromycin Antibiotic 114-07-8 1.66 3.32

Fluoxetine1 Antidepressant 54910-89-3 2.17 4.35

Miconazole1 Antifungal 22916-47-8 0.97 1.94

Ranitidine1 Antacid 66357-35-5 1.11 2.22

Sulfamethoxazole Antibiotic 723-46-6 1.58 3.16

Thiabendazole Anthelmintic, fungicide 148-79-8 1.04 2.08

Trimethoprim Antibiotic 738-70-5 1.47 2.95

Warfarin Anticoagulant, rodenticide 81-81-2 1.26 2.53

1

Concentrations of these compounds should be routinely reported as estimates. Qualitative identification of compound meets all identification 

criteria, but recovery falls between 35 and 59 percent.

2

Estimated MDLs determined according to the procedure of U.S. Environmental Protection Agency (2005).

3

Interim LRLs are determined according to the procedure of Childress and others (1999).
34 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Table B6. Wastewater method for streambed-sediment samples, including compound names, endocrine-disrupting potential, and 

possible compound uses (modified from Burkhardt and others, 2006).

[EDC, known or suspected endocrine disruptor; Y, yes; -, no or status is not known; CAS, Chemical Abstracts Service; F, fungicide; H, herbicide; I, insecticide; 

FR, flame retardant; GUP, general-use pesticide; WW, wastewater; Manuf, manufacturing; >, greater than; CP, combustion product; PAH, polycyclic aromatic 

hydrocarbon; UV, ultraviolet; NA, not applicable; μg/kg, micrograms per kilogram]

Compound name EDC1 CAS number Possible compound uses or sources2

Long-term 

method 

detection 

level 

(μg/kg)

Laboratory 

reporting 

level 

(μg/kg)

1,4-Dichlorobenzene Y 106-46-7 Moth repellent, fumigant, deodorant 27.6 50

1-Methylnaphthalene - 90-12-0 2-5 percent of gasoline, diesel fuel, or crude oil 

27.8

50

2,2 ́,4,4 ́-tetrabromodiphenyl ether Y 5436-43-1 Flame retardant 19.1 50

2,6-Dimethylnaphthalene - 581-42-0 Present in diesel/kerosene (trace in gasoline) 24.8 50

2-Methylnaphthalene - 91-57-6 2-5 percent of gasoline, diesel fuel, or crude oil 27.8 50

3-β-Coprostanol - 360-68-9 Carnivore fecal indicator 360 500

3-Methyl-1(H)-indole (Skatole) - 83-34-1 Fragrance, stench in feces and coal tar 30.9 50

3-tert-Butyl-4-hydroxy anisole (BHA) Y 25013-16-5 Antioxidant, general preservative 101 150

4-Cumylphenol Y 599-64-4 Nonionic detergent metabolite 33.7 50

4-n-Octylphenol Y 1806-26-4 Surfactant 36.8 50

4-Nonylphenol Y 104-40-5 Surfactant 498 750

4-tert-Octylphenol Y 140-66-9 Nonionic detergent metabolite 22.9 50

Acetophenone - 98-86-2 Fragrance in detergent and tobacco, flavor in 

beverages 100 150

Acetyl hexamethyl tetrahydronaphthalene 

(AHTN) - 21145-77-7 Musk fragrance (widespread use), persistent in ground water; endocrine disruptor 12.5 50

Anthracene3 - 120-12-7 Wood preservative, component of tar, diesel, 

or crude oil, CP 19.8 50

Atrazine Y 1912-24-9 Selective triazine herbicide 58.9 100

Benzo[a]pyrene3 Y 50-32-8 Regulated PAH, used in cancer research, CP 24.6 50

Benzophenone Y 119-61-9 Fixative for perfumes and soaps 31.8 50

β-Sitosterol - 83-46-5 Plant sterol 363 500

β-Stigmastanol - 19466-47-8 Plant sterol 367 500

bis(2-Ethylhexyl) phthalate Y 117-81-7 Plasticizer for polymers and resins, pesticides 138 250

Bisphenol A Y 80-05-7 Manuf polycarbonate resins, antioxidant, FR 31.2 50

Bromacil3 - 314-40-9 H (GUP), >80 percent noncrop usage on 

grass/brush 254 500

Camphor - 76-22-2 Flavor, odorant, ointments 27 50

Carbazole - 86-74-8 I, Manuf dyes, explosives, and lubricants 22.4 50

Chlorpyrifos3 Y 2921-88-2 I, domestic pest and termite control (domestic 

use restricted as of 2001) 33.6 50

Cholesterol - 57-88-5 Often a fecal indicator 168 250

Diazinon3 Y 333-41-5 I, > 40 percent nonagricultural usage, ants, 

flies 48.6 50

Diethyl phthalate Y 84-66-2 Plasticizer for polymers and resins 46.7 100

d-Limonene - 5989-27-5 F, antimicrobial, antiviral, fragrance in aerosols 23.7 50

Fluoranthene3 - 206-44-0 Component of coal tar and asphalt (only traces 

in gasoline or diesel fuel), CP 23.2 50

Hexahydrohexamethylcyclopentabenzopyran (HHCB) - 1222-05-5 Musk fragrance (widespread use) persistent in 

ground water; endocrine disruptor 16.5 50

Indole - 120-72-9 Pesticide inert ingredient, fragrance in coffee 53.5 100
Appendix B 35

Compound name EDC1 CAS number Possible compound uses or sources2

Long-term 

method 

detection 

level 

(μg/kg)

Laboratory 

reporting 

level 

(μg/kg)

Isoborneol - 124-76-5 Fragrance in perfumery, in disinfectants 39.3 50

Isophorone3 - 78-59-1 Solvent for lacquer, plastic, oil, silicon, resin 43.4 50

Isopropylbenzene (cumene) - 98-82-8 Manuf phenol/acetone, fuels and paint thinner 86.6 100

Isoquinoline3 - 119-65-3 Flavors and fragrances 83.1 100

Menthol - 89-78-1 Cigarettes, cough drops, liniment, mouthwash 42 50

Metolachlor3 - 51218-45-2 H (GUP), indicator of agricultural drainage 37.2 50

N,N-diethyl-meta-toluamide (DEET) - 134-62-3 I, urban uses, mosquito repellent 56.2 100

Naphthalene3 - 91-20-3 Fumigant, moth repellent, major component 

(about 10 percent) of gasoline 23.5 50

4-Nonylphenol diethoxylate (NP2EO; sum 

of all isomers) Y 26027-38-3 Nonionic detergent metabolite 161 250

4-Nonylphenol monoethoxylate (NP1EO; 

sum of all isomers) - NA Nonionic detergent metabolite; endocrine 

 disruptor 

20.7 50

4-Octylphenol diethoxylate (OP2EO; sum 

of all isomers) Y 26636-32-8 Nonionic detergent metabolite 38.3 50

4-Octylphenol monoethoxylate (OP1EO; 

sum of all isomers) Y 26636-32-8 Nonionic detergent metabolite 44.2 50

p-Cresol Y 106-44-5 Wood preservative 20.6 50

Anthraquinone - 84-65-1 Dye mfr and textiles, seed treatment, bird 

repellant 24.3 50

Phenanthrene3 - 85-01-8 Manuf explosives, component of tar, diesel 

fuel, or crude oil, CP 39.3 50

Phenol3 - 108-95-2 Disinfectant, manuf several products, leachate 43.4 50

Prometon3 - 1610-18-0 H (noncrop only), applied prior to blacktop 86.6 100

Pyrene3 - 129-00-0 Component of coal tar and asphalt (only traces 

in gasoline or diesel fuel), CP 83.1 100

Tris(2-butoxyethyl) phosphate - 78-51-3 Flame retardant 98.5 150

Tris(2-chloroethyl) phosphate Y 115-96-8 Plasticizer, flame retardant 70.3 100

Tri(1,3-dichloro-2-propyl) phosphate Y 13674-87-8 Flame retardant 73 100

Tributylphosphate - 126-73-8 Antifoaming agent, flame retardant 39.3 50

Triclosan Y 3380-34-5 Disinfectant, antimicrobial (concern for acquired microbial resistance) 49.6 50

Triphenyl phosphate - 115-86-6 Plasticizer, resin, wax, finish, roofing paper, 

FR 46 50

1

World Wildlife Fund Canada (1999).

2

ChemFinder Webserver (2001); National Toxicology Program (2001); National Institute of Standards and Technology (2001); Spectrum Laboratories, Inc. 

(2001); HealthCentral.com (2001); EXtension TOXicology NETwork (2001).

3

Compound determined by at least one other method at the National Water Quality Laboratory.

Table B6. Wastewater method for bed-sediment samples, including compound names, endocrine-disrupting potential, and possible 

compound uses (modified from Burkhardt and others, 2006).—Continued
36 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

References Cited

Burkhardt, M.R., Zaugg, S.D., Smith, S.G., and ReVello, R.C., 

2006, Determination of wastewater compounds in sediment and soil by pressurized solvent extraction, solid-phase 

extraction, and capillary-column gas chromatography/

mass spectrometry: U.S. Geological Survey Techniques and 

Methods, book 5, sec. B, chap. 2, 33 p.

Childress, C.J.O., Foreman, W.T., Connor, B.F., and Maloney, T.J., 1999, New reporting procedures based on longterm method detection levels and some considerations for 

interpretations of water-quality data provided by the U.S. 

Geological Survey National Water Quality Laboratory: U.S. 

Geological Survey Open-File Report 99–193, 19 p.

U.S. Environmental Protection Agency, 2005, Guidelines 

establishing test procedures for the analysis of pollutants (App. B, Part 136, Definition and procedures for the 

determination of the method detection limit): U.S. Code of 

Federal Regulations, Title 40, revised as of July 1, 2005, 

p. 319–322.

Zaugg, S.D., Smith, S.G., Schroeder, M.P., Barber, L.B., and 

Burkhardt, M.R., 2007, Methods of analysis by the U.S. 

Geological Survey National Water Quality Laboratory—

Determination of wastewater compounds by polystyrenedivinylbenzene solid-phase extraction and capillary-column 

gas chromatography/mass spectrometry (ver. 1.1): U.S. 

Geological Survey Water-Resources Investigations Report 

01–4186, 37 p.
Appendix C 37

Appendix C. Quality-Control Data

Table C1. Summary of results for analysis of Polar Organic Chemical Integrative Sampler (POCIS) extracts by the antibiotic, 

pharmaceutical, and wastewater methods in trip blanks collected in Tinkers Creek and its tributaries and two other tributaries of the 

Cuyahoga River in 2006.

[All results are considered estimates because a method validation has not been completed for POCIS extracts. Table lists only those compounds that were 

detected. There were no detections of antibiotic compounds in trip blanks. Concentrations are reported per extract from one POCIS disk. e, estimated concentration]

Compound Number of 

detections

Frequency

of detection 

(percent)

Number of 

environmental 

samples 

censored

 Concentrations of detections, in nanograms per POCIS

Minimum Maximum Median

Pharmaceutical method

Fluoxetine 7 39 0 e0.24 e0.51 e0.34

Diphenhydramine 4 22 1 e0.34 e2.8 e0.58

1,7-dimethylxanthine 1 6 0 e4.2 e4.2 e4.2

Caffeine 1 6 0 e0.32 e0.32 e0.32

Wastewater method

Diethylhexyl phthalate 11 61 11 e48 43,000 e63

Cholesterol 4 22 2 e810 e1,300 e1,100

Diethyl phthalate 3 17 3 e100 3,800 e280

Phenol 3 17 1 410 2,300 770

Bisphenol A 2 11 0 e54 e70 e62

4-Nonylphenol diethoxylate (NP2EO; sum of 

all isomers) 

2 11 0 e3,1001 e3,200 e3,100

3-β-Coprostanol 1 6 0 e640 e640 e640

β-Sitosterol 1 6 0 e730 e730 e730

β-Stigmastanol 1 6 0 e960 e960 e960

4-Octylphenol diethoxylate (OP2EO; sum of 

all isomers) 1 6 0 e150 e150 e150 

1

Rounded to two significant digits.

Table C2. Summary of results for analysis of Semipermeable Membrane Device (SPMD) extracts by the hydrophobic 

method in trip blanks collected in Tinkers Creek and its tributaries and two other tributaries of the Cuyahoga River in 2006.

[Water concentration results are estimated on the basis of recovery of performance reference compounds. Table lists only those compounds that were detected.]

Compound Number of 

detections

Frequency of 

detection (percent)

 Concentrations of detections, in nanograms per liter

Minimum Maximum Median

1-Methylnaphthalene 18 100 0.26 0.82 0.5

2-Methylnaphthalene 18 100 0.48 1.7 0.84

Phenanthrene 18 100 1.1 8.1 2.6

4-Methylbiphenyl 17 94 0.94 10 8.9

Pyrene 17 94 0.67 36 1.5

Fluoranthene 15 83 0.83 7.8 2.4

Chrysene 13 72 0.1 0.55 0.18

Benz[a]anthracene 10 56 0.02 0.11 0.04

Fluorene 10 56 0.2 0.79 0.28

Benzo[e]pyrene 8 44 0.09 0.17 0.12

Acenaphthene 6 33 0.52 0.91 0.62

2-Methylphenanthrene 4 22 0.28 0.52 0.34

Anthracene 1 6 2.7 2.7 2.7

Perylene 1 6 3.2 3.2 3.2
38 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Table C3. Results for analysis of Polar Organic Chemical Integrative Sampler (POCIS) extracts by the antibiotic, pharmaceutical, and 

wastewater methods for replicate POCIS deployed in Tinkers Creek in 2006.

[All results are considered estimates because a method validation has not been completed for POCIS extracts. Results are reported as nanograms per POCIS 

disk. R1, sample 1 of replicate pair; R2, sample 2 of replicate pair; RPD, absolute relative percent difference; e, estimated concentration; –, not detected (less 

than laboratory reporting level); nc, RPD not calculated because compound was not detected in one or both samples of the replicate pair]

Compound Replicate A Replicate B

R1 R2 RPD R1 R2 RPD

Antibiotic method

Azithromycin 12 21 51 2.5 e0.5 130

Carbamazepine 46 56 22 57 130 79

Erythromycin-H2

O 10 12 17 12 13 12

Ibuprofen 30 – nc – – nc

Ofloxacin 1 e0.5 67 – 1 nc

Sulfamethoxazole 3 2 40 3.5 3.5 0

Trimethoprim 9.5 10 5.1 16 19 14

Pharmaceutical method

Caffeine 12 6.3 66 6.4 e4.2 41

Carbamazepine 5.8 e4.6 23 e4.3 e3.4 25

Diphenhydramine e2.5 e3.2 25 e1.3 2.9 74

Erythromycin 7.7 – nc – – nc

Thiabendazole – e1.2 nc e0.87 e0.78 11

Trimethoprim e2.2 e2.5 11 e3.7 e2.7 30

Wastewater method

1,4-Dichlorobenzene e31 – nc – – nc

Acetyl hexamethyl tetrahydronaphthalene (AHTN) e120 e120 0 e85 e88 3.1

Anthraquinone – – nc 210 nc 4.9

Atrazine e130 e150 10 210 250 19

Benzophenone e120 e130 4.7 – – nc

β-Sitosterol e2,100 – nc – – nc

Caffeine e110 e140 23 e160 220 29

Cotinine e30 e30 0 – e30 nc

Diethyl phthalate 340 510 40 – – nc

Ethanol,2-butoxy-,phosphate 420 400 5.7 390 480 21

Hexahydrohexamethylcyclopentabenzopyran (HHCB) 520 610 15 320 410 24

Indole 590 190 100 – – nc

Metolachlor e39 e46 18 e53 e68 25

N,N-Diethyltoluamide (DEET) e180 240 30 270 370 31

4-Nonylphenol monoethoxylate (NP1EO; sum of all isomers) 670 – nc – – nc

4-Nonylphenol diethoxylate (NP2EO; sum of all isomers) e3,000 – nc – – nc

4-Octylphenol diethoxylate (OP2EO; sum of all isomers) e130 – nc – – nc

p-Cresol 3,600 1,200 100 260 – nc

p-Nonylphenol (total) e970 – nc – – nc

Phenol 380 – nc – – nc

Prometon – – nc – e180 nc

3-Methyl-1(H)-indole (Skatole) e26 – nc – – nc

Tris(2-chloroethyl) phosphate e170 e190 13 210 250 18

Tri(1,3-dichloro-2-propyl) phosphate e190 220 14 220 220 0
Appendix C 39

Table C4. Results for analysis of Semipermeable Membrane Device (SPMD) extracts by the hydrophobic method for replicate 

SPMDs deployed in Tinkers Creek in 2006.

[Results are reported as nanograms per liter. -, not detected (less than laboratory reporting level); R1, sample 1 of replicate pair; R2, sample 2 of replicate 

pair; RPD, absolute relative percent difference; nc, RPD not calculated because compound was not detected in one or both samples of the replicate pair. 

Water concentration results are estimated on the basis of recovery of performance reference compounds]

Compound Replicate A Replicate B

R1 R2 RPD R1 R2 RPD

1-Methylfluorene - - nc - 1.9 nc

2-Methylphenanthrene - - nc 2.5 2.2 13

Benz[a]anthracene - - nc 1.9 - nc

Benzo[b]fluoranthene - - nc 3.6 3.0 18

Benzo[b]naphtho[2,1-d]thiophene - - nc 2.0 1.9 5.1

Benzo[e]pyrene - - nc 3.6 3.2 12

Benzo[k]fluoranthene - - nc 2.3 2.4 4.3

Chrysene 5.2 4.7 10 14 12 15

Fluoranthene 20 22 9.5 53 47 12

Phenanthrene 8.4 11 27 15 16 6.5

Pyrene 13 15 14 34 30 12
40 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Table C5. Summary of results for analysis of streambed-sediment replicates by the pharmaceutical and wastewater methods for 

samples collected in Tinkers Creek in 2006.

[μg/kg, micrograms per kilogram; m, compound detected, but value is highly variable by this method; R1, sample one of replicate pair; R2, sample 2 of 

replicate pair; RPD, absolute relative percent difference ; –, not detected (less than laboratory reporting level); e, estimated concentration; m, compound 

presence verified through qualitative criteria, but concentration could not be quantified; nc, RPD not calculated because compound was not detected in one 

or both samples of the replicate pair]

Compound Replicate A Replicate B

R1 R2 RPD R1 R2 RPD

Pharmaceutical method

Dehydronifedipine 12 – nc – 26 nc

Diltiazem – – nc – 5.3 nc

Diphenhydramine 12 14 11 13 26 69

Miconazole 6.1 5.5 9.9 – 3.5 nc

Wastewater method

1-Methylnaphthalene e10 e11 8.6 m e5.0 nc

2,6-Dimethylnaphthalene e40 e30 29 m – nc

2-Methylnaphthalene e20 e16 22 e10 e7.4 29

3-β-Coprostanol e90 e90 0 e60 e57 4.5

3-Methyl-1H-indole 100 62 47 m e7.8 nc

Anthraquinone 71 e46 42 55 e42 27

Acetophenone e20 9.4 72 m e6.8 nc

Acetyl hexamethyl tetrahydronaphthalene 

(AHTN) e20 e11 55 e10 e8.9 12

Anthracene e30 e19 45 60 57 5.8

Benzo[a]pyrene 80 51 45 170 120 33

β-Sitosterol e1,400 e1,500 6.2 e640 e450 34

β-Stigmastanol e380 e420 9.5 e30 e120 120

bis(2-Ethylhexyl) phthalate e50 e36 33 e50 e38 27

Carbazole e40 e30 28 50 e29 53

Cholesterol e870 e910 4.2 e600 e390 42

4-Nonylphenol diethoxylate (NP2EO; sum of 

all isomers) e250 – nc – – nc

Fluoranthene 310 240 26 600 490 20

Hexahydrohexamethylcyclopentabenzopyran 

(HHCB) 70 e38 59 e20 e16 25

Indole 780 430 58 100 94 6.2

4-Nonylphenol monoethoxylate (NP1EO; sum 

of all isomers) e190 – nc – – nc

Naphthalene e20 e22 10 e10 e7.6 27

p-Cresol e120 e46 89 e10 e19 62

Phenanthrene 110 89 21 290 230 22

Phenol e150 – nc – e24 nc

Pyrene 240 180 30 440 350 22

Tris(2-butoxyethyl) phosphate – – nc e30 e30 0
Appendix C 41

Table C6. Summary of reagent-water spike-recovery data for 

wastewater compounds.—Continued

[All results are averages of nine measurements made during the time that 

POCIS samples were being processed]

Compound Recovery 

(percent)

1,4-Dichlorobenzene 51

1-Methylnaphthalene 64

2,6-Dimethylnaphthalene 50

2-Methylnaphthalene 57

3-β-Coprostanol 71

3-tert-Butyl-4-hydroxy anisole (BHA) 52

4-Cumylphenol 90

4-n-Octylphenol 70

4-tert-Octylphenol 89

5-methyl-1H-benzotriazole 67

Acetophenone 104

Anthracene 81

Anthraquinone 93

Benzo[a]pyrene 77

Benzophenone 98

β-Sitosterol 66

β-Stigmastanol 67

Bisphenol A 39

Bromacil 95

Bromoform 61

Caffeine 97

Camphor 95

Carbaryl 60

Carbazole 93

Chlorpyrifos 91

Cholesterol 76

Cotinine 53

Cumene 36

Diazinon 101

d-Limonene 25

Ethanol,2-butoxy-,phosphate 100

Ethylcitrate 96

Fluoranthene 91

Hexahydrohexamethylcyclopentabenzopyran 

(HHCB) 85

Indole 86

Isoborneol 96

Isophorone 99

Isoquinoline 91

Menthol 98

Metalaxyl 107

Methylsalicylate 95

Metolachlor 102

N,N-diethyl-meta-toluamide (DEET) 102

Naphthalene 72

Table C6. Summary of reagent-water spike-recovery data for 

wastewater compounds.—Continued

[All results are averages of nine measurements made during the time that 

POCIS samples were being processed]

Compound Recovery 

(percent)

4-Nonylphenol monoethoxylate (NP1EO; sum of 

all isomers) 80

4-Nonylphenol diethoxylate (NP2EO; sum of all 

isomers) 80

4-Octylphenol monoethoxylate (OP1EO; sum of 

all isomers) 88

4-Octylphenol diethoxylate (OP2EO; sum of all 

isomers) 103

p-Cresol 91

p-Nonylphenol (total) 78

Phenanthrene 87

Phenol 96

Prometon 98

Pyrene 92

3-Methyl-1(H)-indole (Skatole) 91

Tetrachloroethylene 20

Acetyl hexamethyl tetrahydronaphthalene 

(AHTN) 87

Tris(2-chloroethyl) phosphate 99

Tri(1,3-dichloro-2-propyl) phosphate 100

Tributylphosphate 99

Triclosan 89

Triphenyl phosphate 96
42 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Table C7. Summary of spike-recovery data for pharmaceutical compounds in streambed-sediment samples collected in Tinkers 

Creek and its tributaries and two other tributaries to the Cuyahoga River in 2006.

[ng/g (μg/kg), nanograms per gram (micrograms per kilogram); –, not detected; na, not analyzed; <rl, less than reporting level established by the U.S. 

Geological Survey National Water Quality Laboratory (NWQL)]

Compound

Set 1

 blank

ng/g 

(μg/kg)

Set 1

reagent spike

recovery 

(percent )

Set 2

blank

ng/g (μg/kg)

Set 2

reagent spike

recovery 

(percent )

Lab-selected 

matrix spike-1 

recovery 

(percent)

Lab-selected 

matrix spike-2

recovery 

(percent)

1,7-Dimethylxanthine – 130 – 65 89 <rl

Acetaminophen – 94 – 120 68 69

Albuterol – 45 – 60 Interference 27

Azithromycin – 17 – 11 na <rl

Caffeine – 93 – 62 100 84

Carbamazepine – 110 – 75 71 69

Cimetidine – 41 – 55 8.6 66

Codeine – 120 – 64 4.6 50

Cotinine – 120 – 72 65 52

Dehydronifedipine – 130 – 68 56 110

Diltiazem – 87 – 66 61 51

Diphenhydramine – 110 – 69 58 68

Erythromycin – 68 – 130 na 38

Fluoxetine – 45 – 44 24 3.8

Miconazole 8.7 94 8.7 21 9.6 <rl

Ranitidine – 78 – 48 <rl 2.9

Sulfamethoxazole – 150 – 68 57 33

Thiabendazole – 130 – 61 83 66

Trimethoprim 2.8 120 2.8 68 44 55

Warfarin – 130 – 67 72 82
Appendix D 43

Appendix D. Organic Wastewater Compounds in Polar Organic Chemical 

Integrative Sampler (POCIS) Extracts

Table D1. Results of analysis of POCIS extracts by the antibiotic method for POCIS deployed in Tinkers Creek and its tributaries and 

two other tributaries to the Cuyahoga River in 2006.

[All results are considered estimates because a method validation has not been completed for POCIS extracts. Street, Streetsboro; Aur W, Aurora Westerly; 

Aur Sh, Aurora Shores; Twins, Twinsburg; Sol, Solon; Bed, Bedford; Bed Hgts, Bedford Heights; DR, Tinkers Creek at Dunham Road; FR, Furnace Run; 

YC, Yellow Creek; US, upstream; DS, downstream; AO, above outfall; <, less than; e, estimated concentration below the reporting level. Data in bold print 

were either not detected or detected at a lower concentration in the upstream sample]

Compound

Concentrations at sampling locations, in nanograms per POCIS

Street Aur W Aur Sh Twins Sol Bed Bed Hgts DR FR YC US DS US DS US DS US DS US DS US DS AO US DS

Azithromycin <1 12 <1 69 <1 e0.5 <1 2.5 <1 260 <1 <1 <1 <1 85 8.0 <1 <1

Carbamazepine <1 46 <1 420 <1 50 36 57 <1 170 <1 200 <1 <1 110 74 1.7 <1

Chloramphenicol <10 <10 <10 <10 <10 <10 <10 <10 <10 <10 <10 <10 <10 <10 <10 <10 <10 <10

Chlorotetracycline <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5

Ciproflaxacin <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1

Doxycycline <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5

Enrofloxacin <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1

Epi-chlorotetracycline <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5

Epi-iso-chlorotetra-cycline <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5

Epi-oxytetracycline <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5

Epi-tetracycline <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5

ErythromycinH2

O <1 10 <1 41 <1 <1 5.5 12 <1 42 <1 15 <1 <1 37 24 <1 <1

Ibuprofen <10 30 <10 <10 <10 <10 <10 <10 <10 <10 <10 89 <10 <10 <10 <10 <10 <10

Iso-chlorotetracycline <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5

Lincomycin <1 <1 <1 16 <1 <1 <1 <1 <1 9 <1 2 <1 <1 1 1.5 <1 <1

Lomefloxacin <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1

Norfloxacin <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1

Ofloxacin <1 1 <1 16 <1 <1 <1 <1 <1 33 <1 7.5 <1 <1 <1 <1 <1 <1

Ormetoprim <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 e0.92 <1

Oxytetracycline <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5

Roxithromycin <1 <1 <1 <1 <1 <1 <1 <1 <1 1 <1 <1 <1 <1 <1 <1 <1 <1

Sarafloxacin <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1

Sulfachloropyridazine <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1

Sulfadiazine <1 <1 <1 <1 <1 <1 <1 <1 <1 12 <1 <1 <1 <1 <1 <1 <1 <1

Sulfadimethoxine <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1

Sulfamethazine <1 <1 <1 <1 <1 <1 <1 <1 <1 1.5 <1 <1 <1 <1 <1 <1 <1 <1

Sulfamethoxazole <1 3 <1 15 <1 2 4 3.5 <1 67 e0.97 4 <1 <1 48 7.5 e0.5 <1

Sulfathiazole <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1

Tetracycline <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 <5

Trimethoprim <1 9.5 <1 22 <5 e0.5 4.5 16 <1 86 1.3 17 <1 <1 34 7.3 <1 <1

Tylosin <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1

Virginiamycin <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1 <1
44 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Table D2. Summary of results for analysis of POCIS extracts by the antibiotic method for POCIS 

deployed in Tinkers Creek and its tributaries and two other tributaries to the Cuyahoga River in 2006.

[All results are considered estimates because a method validation has not been completed for POCIS extracts. –, not 

detected; e, estimated concentration below the reporting level]

Compound Number of 

detections

Frequency 

of

detection 

(percent)

Concentrations of detections, 

in nanograms per POCIS

Minimum Maximum Median

Sulfamethoxazole 11 61 e0.5 67 e4

Carbamazepine 10 56 1.7 420 65

Trimethoprim 10 56 e0.5 86 e13

Erythromycin-H2

0 8 44 5.5 42 20

Azithromycin 7 39 e0.5 260 e12

Lincomycin 5 28 1 16 2

Ofloxacin 4 22 1 33 12

Ibuprofen 2 11 30 89 60

Ormetoprim 1 6 e0.92 e0.92 e0.92

Roxithromycin 1 6 1 1 1

Sulfadiazine 1 6 12 12 12

Sulfamethazine 1 6 1.5 1.5 1.5

Chloramphenicol 0 0 – – –

Chlortetracycline 0 0 – – –

Ciproflaxacin 0 0 – – –

Doxycycline 0 0 – – –

Enrofloxacin 0 0 – – –

Epi-chlortetracycline 0 0 – – –

Epi-iso-chlortetracycline 0 0 – – –

Epi-oxytetracycline 0 0 – – –

Epi-tetracycline 0 0 – – –

Iso-chlortetracycline 0 0 – – –

Lomefloxacin 0 0 – – –

Norfloxacin 0 0 – – –

Oxytetracycline 0 0 – – –

Sarafloxacin 0 0 – – –

Sulfachlorpyridazine 0 0 – – –

Sulfadimethoxine 0 0 – – –

Sulfathiazole 0 0 – – –

Tetracycline 0 0 – – –

Tylosin 0 0 – – –

Virginiamycin 0 0 – – –
Appendix D 45

Table D3. Results for analysis of POCIS extracts by the pharmaceutical method for POCIS deployed in Tinkers Creek and its tributaries and two other tributaries to the Cuyahoga River in 2006.[All results are considered estimates because a method validation has not been completed for POCIS extracts. Street, Streetsboro; Aur W, Aurora Westerly; Aur Sh, Aurora Shores; Twins, Twinsburg; Sol, Solon; Bed, Bedford; Bed Hgts, Bedford Heights; DR, Tinkers Creek at Dunham Road; FR, Furnace Run; YC, Yellow Creek; US, upstream; DS, downstream; AO, above outfall; e, estimated concentration below the reporting level; dc, data censored for quality assurance purposes; lt, less than reporting level of 5 nanograms per POCIS. Data in bold print were either not detected or detected at a lower concentration in the upstream sample]

Compound

Concentrations at sampling locations, in nanograms per POCIS

Street Aur W Aur Sh Twins Sol Bed Bed Hgts DR FR YC US DS US DS US DS US DS US DS US DS AO US DS

1,7-Dimethylxanthine lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Acetaminophen lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Albuterol lt lt lt lt lt lt lt lt lt 13 lt lt lt lt lt e1.9 lt lt

Azithromycin lt lt lt 19 lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Caffeine 5.4 12.4 e3.8 lt 6.8 6.6 11 6.4 15 24 45 8.4 12 16 11 11 e2.6 e0.30

Carbamazapine lt 5.8 lt 28 lt 8.6 e4.5 e4.3 lt 18 lt 2.0 lt lt 7.5 8.3 lt lt

Cimetidine lt lt lt lt lt lt lt lt lt 14 lt lt lt lt lt e1.7 lt lt

Codeine lt lt lt lt lt lt lt lt lt 34 lt 4.2 lt lt lt 12 lt lt

Cotinine lt lt lt lt lt lt lt lt lt lt e3.9 lt lt lt lt lt lt lt

Dehydronifedipine lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Diltiazem lt lt lt lt lt lt lt lt lt 21 lt lt lt lt lt 6.9 lt lt

Diphenhydramine lt e2.5 lt 9.4 lt lt lt e1.3 lt 27 lt e3.3 lt lt e1.4 e2.3 lt dc

Erythromycin lt 7.7 lt 13 lt lt lt lt lt 64 lt lt lt lt lt 23 lt lt

Fluoxetine lt lt lt lt lt lt lt lt lt e0.003 lt lt lt lt lt lt dc e0.16

Miconazole lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Ranitidine lt lt lt lt lt lt lt lt lt 6.8 lt lt lt lt lt lt lt lt

Sulfamethoxazole lt lt lt lt lt lt e0.67 lt lt lt lt lt lt lt lt lt lt lt

Thiabendazole lt lt lt 8.0 lt e1.1 e0.92 e0.87 lt 12 lt lt lt lt e2.5 e1.8 lt lt

Trimethoprim lt e2.2 lt 28 lt e0.16 e1.0 e3.7 lt 120 lt e4.3 e1.8 lt 10 13 lt lt

Warfarin lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt
46 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Table D4. Summary of results for analysis of POCIS extracts by the pharmaceutical method for POCIS deployed 

in Tinkers Creek and its tributaries and two other tributaries to the Cuyahoga River in 2006.

[All results are considered estimates because a method validation has not been completed for POCIS extracts. –, not detected; 

e, estimated concentration below the reporting level]

Compound Number of

detections

Frequency of

detection 

(percent)

Concentrations of detections, 

in nanograms per POCIS

Minimum Maximum Median

Caffeine 17 94 e0.30 45 e11

Trimethoprim 10 56 e0.16 120 e4.0

Carbamazepine 9 50 e2.0 28 e7.5

Diphenhydramine1 7 39 e1.3 27 e2.5

Thiabendazole 7 39 e0.87 12 e1.8

Erythromycin 4 22 7.7 64 18

Codeine 3 17 4.2 34 12

Albuterol 2 11 1.9 13 7.5

Cimetidine 2 11 1.7 14 7.9

Diltiazem 2 11 6.9 21 14

Fluoxetine1 2 11 e0.003 e0.16 e0.08

Azithromycin 1 6 19 19 19

Cotinine 1 6 e3.9 e3.9 e3.9

Ranitidine 1 6 6.8 6.8 6.8

Sulfamethoxazole 1 6 e0.67 e0.67 e0.67

1,7-Dimethylxanthine 0 0 – – –

Acetaminophen 0 0 – – –

Dehydronifedipine 0 0 – – –

Miconazole 0 0 – – –

Warfarin 0 0 – – –

1

Data censored for one station.
Appendix D 47

Table D5. Results for analysis of POCIS extracts by the wastewater method for POCIS deployed in Tinkers Creek and its tributaries and 

two other tributaries to the Cuyahoga River in 2006.—Continued

[All results are considered estimates because a method validation has not been completed for POCIS extracts; Street, Streetsboro; Aur W, Aurora Westerly; Aur 

Sh, Aurora Shores; Twins, Twinsburg; Sol, Solon; Bed, Bedford; Bed Hgts, Bedford Heights; DR, Tinkers Creek at Dunham Road; FR, Furnace Run; YC, Yellow 

Creek; US, upstream; DS, downstream; AO, above outfall; e, estimated concentration less than reporting limit or due to laboratory quality-control factors; dc, data 

censored for quality assurance purposes; lt, less than reporting level of 200 ng/POCIS. Data in bold print were either not detected or detected at a lower concentration in the upstream sample]

Compound

Concentrations at sampling locations, in nanograms per POCIS

Street Aur W Aur Sh Twins Sol Bed Bed Hgts DR FR YC US DS US DS US DS US DS US DS US DS AO US DS

1,4-Dichlorobenzene lt e31 lt lt lt lt 59 lt lt lt lt lt lt 32 lt lt lt lt

1-Methylnaphthalene lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

2,6-Dimethylnaphthalene lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

2-Methylnaphthalene lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

3-β-Coprostanol lt lt lt lt lt lt lt lt lt lt lt e1,300 lt lt lt lt lt lt

3-Methyl-1(H)-indole (Skatole) lt e26 lt e75 lt lt lt lt lt lt e31 e29 lt lt e98 lt lt lt

3-tert-Butyl-4-hydroxy anisole 

(BHA) lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

4-Cumylphenol lt lt lt lt lt lt lt lt lt lt lt lt lt lt e130 lt lt lt

4-n-Octylphenol lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

4-tert-Octylphenol lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

5-Methyl-1H-benztriazole lt lt lt lt lt lt lt lt e24 e22 lt 700 e46 lt e40 lt lt lt

Acetophenone lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Acetyl hexamethyl tetrahydronaphthalene (AHTN) lt e120 lt 550 lt lt e40 e85 lt 560 lt 520 lt lt 280 490 lt lt

Anthracene lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Anthraquinone lt lt e160 200 lt lt e180 210 340 200 520 320 200 230 230 270 lt lt

Atrazine e160 e130 e140 e170 e160 e170 e160 210 280 lt 210 160 e140 e160 e130 330 e100 lt

Benzo[a]pyrene lt lt lt lt lt lt lt lt lt lt lt 160 lt lt lt lt lt lt

Benzophenone e140 e120 lt e180 lt lt lt lt lt e120 lt 160 lt lt lt lt lt lt

β-Sitosterol lt e2,100 lt lt lt lt e1,700 lt lt lt e4,600 e1,900 lt lt lt lt lt lt

β-Stigmastanol lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Bisphenol A lt lt lt 350 lt lt lt lt 340 e140 220 lt lt 230 460 260 lt lt

Bromacil lt lt lt lt lt lt lt lt 2,600 lt lt lt lt lt lt lt 590 lt

Bromoform lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Caffeine e98 e110 e23 e37 e56 e74 e98 e160 260 e65 290 640 e79 e140 e110 450 e18 lt

Camphor lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Carbaryl lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Carbazole lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Chlorpyrifos lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Cholesterol lt lt lt e1,400 lt lt e1,200 lt dc lt e1,900 e2,600 dc lt e1,200 lt lt lt

Cotinine lt e30 lt lt lt lt lt lt lt lt lt lt lt e20 lt 56 lt lt

Cumene lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Diazinon lt lt lt lt lt lt lt lt lt lt lt lt e90 lt lt lt lt lt

Diethylhexyl phthalate 350 dc dc e150 e170 dc 200 dc 280 dc dc dc dc lt 250 dc dc dc

Diethyl phthalate 260 340 e100 e140 e150 e180 dc dc 450 e140 690 280 220 230 e140 dc 280 e72

d-Limonene lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Ethanol,2-butoxy-,phosphate lt 420 lt lt lt lt 480 390 620 690 3,300 27,000 lt 660 660 3,900 lt lt

Ethylcitrate lt lt lt e25 lt lt lt lt lt e23 lt lt lt lt lt 90 lt lt

Fluoranthene lt lt lt lt lt lt lt lt lt lt 250 450 lt lt lt lt lt lt

Hexahydrohexamethylcyclopentabenzopyran (HHCB) lt 520 lt 3,100 lt 310 e140 320 lt 3,800 lt 2,100 e24 lt 580 1,600 lt lt

Indole e88 590 290 lt lt lt lt lt lt lt 38 lt lt lt lt lt lt lt

Isoborneol lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt
48 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Table D5. Results for analysis of POCIS extracts by the wastewater method for POCIS deployed in Tinkers Creek and its tributaries and 

two other tributaries to the Cuyahoga River in 2006.—Continued

[All results are considered estimates because a method validation has not been completed for POCIS extracts; Street, Streetsboro; Aur W, Aurora Westerly; Aur 

Sh, Aurora Shores; Twins, Twinsburg; Sol, Solon; Bed, Bedford; Bed Hgts, Bedford Heights; DR, Tinkers Creek at Dunham Road; FR, Furnace Run; YC, Yellow 

Creek; US, upstream; DS, downstream; AO, above outfall; e, estimated concentration less than reporting limit or due to laboratory quality-control factors; dc, data 

censored for quality assurance purposes; lt, less than reporting level of 200 ng/POCIS. Data in bold print were either not detected or detected at a lower concentration in the upstream sample]

Compound

Concentrations at sampling locations, in nanograms per POCIS

Street Aur W Aur Sh Twins Sol Bed Bed Hgts DR FR YC US DS US DS US DS US DS US DS US DS AO US DS

Isophorone lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Isoquinoline lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Menthol lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Metalaxyl lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Methylsalicylate lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Metolachlor e55 e39 e28 lt e39 e54 e27 e53 91 lt 51 lt e34 e43 lt e120 e24 lt

N,N-Diethyl-meta-toluamide 

(DEET) e140 e180 e140 250 e130 e140 e170 270 e140 500 e170 544 lt e140 210 800 lt lt

Naphthalene lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

4-Nonylphenol diethoxylate 

(NP2EO; sum of all isomers) lt e670 lt lt lt lt lt lt e810 e2,100 e1,700 e1,200 lt lt lt e2,200 lt lt

4-Nonylphenol monoethoxylate 

(NP1EO; sum of all isomers) lt 3,000 lt lt lt lt lt lt 3,900 4,100 4,600 5,500 lt lt 3,400 6,900 lt lt

4-Octylphenol diethoxylate 

(OP2EO; sum of all isomers) lt e130 lt lt lt lt lt lt lt e350 e310 e220 lt lt e200 e580 lt lt

4-Octylphenol monoethoxylate 

(OP1EO; sum of all isomers) lt lt lt lt lt lt lt lt lt lt lt e770 lt lt lt e370 lt lt

p-Cresol 2,900 3,600 3,200 lt 810 700 lt 260 1,000 lt 350 1,200 lt e190 1,800 2,200 lt lt

p-Nonylphenol (total) lt e970 lt lt lt lt lt lt e1,100 e1,200 e1,500 e4,900 lt lt e1,100 e1,400 lt lt

Phenanthrene lt lt lt lt lt lt lt lt lt lt lt e170 lt lt lt lt lt lt

Phenol lt 380 dc lt lt lt lt lt lt lt lt lt lt lt 240 lt lt lt

Polybrominated diphenyl ether lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Prometon lt lt lt 230 e180 200 lt lt lt lt 260 250 160 lt lt 310 lt lt

Pyrene lt lt lt lt lt lt lt lt lt lt e160 350 lt lt lt lt lt lt

Tetrachlorethylene lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt lt

Tris(2-chloroethyl) phosphate lt e170 lt 670 lt lt lt 210 e180 e180 e160 300 lt e140 200 400 lt lt

Tris(dichloroisopropyl) 

phosphate lt e190 lt 650 lt lt e160 220 e150 e180 e160 260 lt lt 220 360 lt lt

Tributyl phosphate lt lt lt lt lt lt lt lt lt e100 lt lt lt lt 400 lt lt lt

Triclosan lt lt lt lt lt lt lt lt lt e140 lt 600 lt lt lt 220 lt lt

Triphenyl phosphate lt lt lt lt lt lt lt lt lt e160 e110 260 lt lt lt lt lt lt
Appendix D 49

Table D6. Summary of results for analysis of POCIS extracts by the wastewater method for POCIS deployed in Tinkers Creek and 

its tributaries and two other tributaries to the Cuyahoga River in 2006.—Continued

[All results are considered estimates because a method validation has not been completed for POCIS extracts. e, estimated concentration less than reporting 

limit or due to laboratory quality-control factors; –, not detected]

Compound Number of 

detections

Frequency of 

detection 

(percent)

Concentrations of detections, 

in nanograms per POCIS

Minimum Maximum Median

Caffeine 17 94 e18 640 e98

Atrazine 16 89 e100 330 e160

Diethyl phthalate1 15 83 e72 690 220

N,N-diethyl-meta-toluamide (DEET) 15 83 e130 800 e170

Metolachlor 13 72 e24 e120 e43

Anthraquinone 12 67 e160 520 220

p-Cresol 12 67 e190 3,600 1,100

Ethanol,2-butoxy-phosphate 10 56 390 27,000 660

Hexahydrohexamethylcyclopentabenzopyran (HHCB) 10 56 e24 3,800 550

Tris(2-chloroethyl) phosphate 10 56 e140 670 e190

Tris(dichloroisopropyl) phosphate 10 56 e150 650 e210

Acetyl hexamethyl tetrahydronaphthalene (AHTN) 8 44 e40 560 390

Bisphenol A 7 39 e140 460 260

p-Nonylphenol (total) 7 39 e970 e4,900 e1,200

4-Nonylphenol monoethoxylate (NP1EO; sum of all 

isomers) 7 39 3,000 6,900 4,100

Prometon 7 39 e160 310 230

Diethylhexyl phthalate2 6 33 e150 350 230

4-Nonylphenol diethoxylate (NP2EO; sum of all 

isomers) 6 33 e670 e2,200 e1,500

4-Octylphenol monoethoxylate (OP1EO; sum of all 

isomers) 6 33 e130 e580 e260

5-Methyl-1H-benzotriazole 5 28 e22 700 e40

Benzophenone 5 28 e120 e180 e140

Cholesterol 5 28 e1,200 e2,600 e1,400

3-Methyl-1(H)-indole (Skatole) 5 28 e26 e98 e31

β-Sitosterol 4 22 e1,700 e4,600 e2,000

Indole 4 22 e38 590 e190

1,4-Dichlorobenzene 3 17 e31 e59 e32

Cotinine 3 17 e20 e56 e30

Ethylcitrate 3 17 e23 e90 e25

Triclosan 3 17 e140 600 e220

Triphenyl phosphate 3 17 e110 260 e160

Bromacil 2 11 590 2,600 1,600

Fluoranthene 2 11 250 450 350

4-Octylphenol monoethoxylate (OP1EO; sum of all 

isomers) 2 11 e370 e770 e570

Phenol 2 11 240 380 310

Pyrene 2 11 e160 350 e250

Tributyl phosphate 2 11 e100 400 e250

3-β-Coprostanol 1 6 e1,300 e1,300 e1,300

4-Cumylphenol 1 6 e130 e130 e130
50 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Table D6. Summary of results for analysis of POCIS extracts by the wastewater method for POCIS deployed in Tinkers Creek and 

its tributaries and two other tributaries to the Cuyahoga River in 2006.—Continued

[All results are considered estimates because a method validation has not been completed for POCIS extracts. e, estimated concentration less than reporting 

limit or due to laboratory quality-control factors; –, not detected]

Compound Number of 

detections

Frequency of 

detection 

(percent)

Concentrations of detections, 

in nanograms per POCIS

Minimum Maximum Median

Benzo[a]pyrene 1 6 e160 e160 e160

Diazinon 1 6 e90 e90 e90

Phenanthrene 1 6 e170 e170 e170

1-Methylnapthalene 0 0 – – –

2,6-Dimethylnapthalene 0 0 – – –

2-Methylnaphthalene 0 0 – – –

3-tert-Butyl-4-hydroxy anisole (BHA) 0 0 – – –

4-n-Octylphenol 0 0 – – –

4-tert-Octylphenol 0 0 – – –

Acetophenone 0 0 – – –

Anthracene 0 0 – – –

β-Stigmastanol 0 0 – – –

Bromoform 0 0 – – –

Camphor 0 0 – – –

Carbaryl 0 0 – – –

Carbazole 0 0 – – –

Chlorpyrifos 0 0 – – –

Cumene 0 0 – – –

d-Limonene 0 0 – – –

Isoborneol 0 0 – – –

Isophorone 0 0 – – –

Isoquinoline 0 0 – – –

Menthol 0 0 – – –

Metalaxyl 0 0 – – –

Methylsalicylate 0 0 – – –

Naphthalene 0 0 – – –

Polybrominated diphenyl ether 0 0 – – –

Tetrachlorethylene 0 0 – – –

1

Data censored for 3 environmental samples.

2

Data censored for 11 environmental samples.
Appendix E 51

Appendix E. Organic Wastewater Compounds in Semipermeable Membrane 

Device (SPMD) Extracts Table E1. Results for analysis of SPMD extracts by the hydrophobic method for SPMDs deployed in Tinkers Creek and its tributaries and two other tributaries to the Cuyahoga River in 2006.—Continued [Street, Streetsboro; Aur W, Aurora Westerly; Aur Sh, Aurora Shores; Twins, Twinsburg; Sol, Solon; Bed, Bedford; Bed Hgts, Bedford Heights; DR, Tinkers Creek at Dunham Road; FR, Furnace Run; YC, Yellow Creek; US, upstream; DS, downstream; AO, above outfall; <, less than. Data in bold print were either not detected or detected at a lower concentration in the upstream sample. Water concentration results are estimated on the basis of recovery of performance reference compounds]

Compound

Concentrations at sampling location, in nanograms per liter

Street Aur W Aur Sh Twins Sol Bed Bed Hgts DR FR YC US DS US DS US DS US DS US DS US DS AO US DS

1,2-Dimethylnaphthalene <0.5 <0.5 <0.5 <0.5 <0.5 <0.5 <0.5 <0.5 <0.5 <0.5 <0.5 <2.4 <0.5 <0.5 <0.5 <0.5 <0.5 <0.5

1-Ethylnaphthalene <0.4 <0.4 <0.4 <0.4 <0.4 <0.4 <0.4 <0.4 <0.4 <0.4 <0.4 <0.4 <0.4 <0.4 <0.4 <0.4 <0.4 <0.4

1-Methylfluorene <0.3 <1.5 <1.5 <0.3 <1.5 <1.5 <1.5 <1.5 0.99 <0.3 <0.3 3.9 1.3 8.2 3.5 1.7 <1.5 <1.5

1-Methylnaphthalene <0.6 <0.6 <4.8 <0.6 <0.6 <0.6 <0.6 <0.6 <0.6 <4.8 <4.8 <4.8 <0.6 <4.8 <0.6 <0.6 <0.6 <0.6

2,3,5-Trimethylnaphthalene <0.3 <0.3 <0.3 <0.3 <0.3 <0.3 <0.3 <0.3 <0.3 <0.3 2.1 2.3 <1.5 <1.5 <1.5 <1.5 <0.3 <0.3

2-Methylfluoranthene <1.4 <1.4 <1.4 <1.4 <1.4 <1.4 <1.4 <1.4 1.9 1.2 2.6 1.5 1.7 8.8 2.7 1.4 <0.02 <1.4

2-Methylnaphthalene <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <4.8 <4.8 <1.3 <4.8 <1.3 <1.3 <1.3 <1.3

2-Methylphenanthrene <1.5 <1.5 <1.5 <1.5 <1.5 <1.5 1.8 2.5 2.1 2.2 5.0 4.8 3.4 28 5.7 3.1 <1.5 1.8

3,6-Dimethylphenanthrene <1.4 <1.4 <0.03 <0.03 <1.4 <0.03 <1.4 <1.4 <1.4 <1.4 1.5 1.6 0.93 6.9 1.6 <1.4 <1.4 <1.4

4-Methylbiphenyl <2.8 <2.8 <2.8 <2.8 <2.8 <2.8 <2.8 <2.8 <2.8 <2.8 <2.8 <2.8 <2.8 <2.8 <2.8 <2.8 <2.8 <2.8

9-Methylanthracene <0.02 <0.02 <0.02 <0.02 <0.02 <0.02 <0.02 <0.02 <0.02 <0.02 <0.02 <0.02 <0.02 <0.02 <0.02 <0.02 <0.02 <0.02

Acenaphthene <2.7 <2.7 6.0 <2.7 <2.7 <2.7 <2.7 <2.7 <0.4 <2.7 2.7 <2.7 <2.7 <2.7 <2.7 <2.7 <0.4 <2.7

Acenaphthylene <0.7 <0.7 <0.7 <0.7 <0.7 <0.7 <0.7 <0.7 <0.7 <0.7 <0.7 <0.7 <0.7 <0.7 <0.7 <0.7 <0.7 <0.7

Anthracene <1.9 <1.9 <1.9 <0.3 <0.3 <0.3 <1.9 <1.9 <1.9 <1.9 2.1 1.5 1.4 6.3 3.6 <1.9 <0.3 <1.9L

Benz[a]anthracene <1.5 <1.5 <1.5 <0.02 <0.02 <1.5 1.9 1.9 4.0 2.7 5.8 2.9 4.5 27 9.1 3.2 <1.5 <1.5

Benzo[a]pyrene <1.7 <1.7 <0.01 <0.01 <1.7 <1.7 <1.7 <1.7 1.9 1.4 4.1 1.0 2.3 7.4 4.8 1.5 <1.7 <1.7

Benzo[b]fluoranthene 1.4 <1.4 <1.4 <0.02 <1.4 <1.4 2.9 3.6 8.8 4.9 13 4.1 5.8 25 11 5.1 <1.4 <1.4

Benzo[b]naphtho[2,1-d]-

thiophene <1.4 <1.4 <1.4 <0.02 <1.4 <1.4 1.8 2.0 3.8 2.6 5.0 2.4 2.4 12 4.1 2.6 <1.4 <1.4

Benzo[b]thiophene <9.3 <9.3 <9.3 <9.3 <9.3 <9.3 <9.3 <9.3 <9.3 <9.3 <9.3 <9.3 <9.3 <9.3 <9.3 <9.3 <9.3 <9.3

Benzo[e]pyrene <1.8 <1.8 <1.8 <1.8 <1.8 <1.8 2.9 3.6 6.8 4.6 11 4.0 5.0 22 8.7 5.5 <1.8 <1.8
52 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio Table E1. Results for analysis of SPMD extracts by the hydrophobic method for SPMDs deployed in Tinkers Creek and its tributaries and two other tributaries to the Cuyahoga River in 2006.—Continued Compound Concentrations at sampling location, in nanograms per liter Street Aur W Aur Sh Twins Sol Bed Bed Hgts DR FR YC US DS US DS US DS US DS US DS US DS AO US DS Benzo[g,h,i]perylene <0.04 <0.04 <0.04 <0.04 <0.04 <0.04 <2.3 <2.3 1.8 <2.3 2.8 1.1 <2.3 <2.3 2.4 <2.3 <0.04 <0.04 Benzo[k]fluoranthene <1.6 <1.6 <1.6 <0.02 <1.6 <1.6 3.0 2.3 4.9 3.7 8.8 3.2 5.4 27 6.1 3.0 <0.02 <1.6 Biphenyl <0.9 <0.9 <0.9 <0.9 <0.9 <0.9 <0.9 <0.9 <0.9 <0.9 <0.9 <0.9 <0.9 <0.9 <0.9 <0.9 <0.9 <0.9 Chrysene 3.8 5.2 8.4 <1.4 1.6 <1.4 12 14 26 17 36 15 18 87 27 19 0.90 3.1 Dibenz[a,h]anthracene <0.03 <0.03 <0.03 <0.03 <0.03 <0.03 <0.03 <0.03 <1.9 <0.03 <0.03 <1.9 <0.03 <0.03 <1.9 <0.03 <0.03 <0.03 Dibenzothiophene <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 2.3 <2.2 <2.2 5.7 2.3 <2.2 <2.2 <2.2 Fluoranthene 16 20 49 3.8 7.4 30 41 53 71 60 120 56 66 340 85 54 4.3 21 Fluorene <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 2.4 <2.2 <2.2 <2.2 <2.2 <2.2 <0.2 <2.2 Indeno[1,2,3-c,d]pyrene <2.1 <0.4 <0.4 <0.4 <0.4 <0.4 <2.1 <2.1 1.7 <2.1 2.8 <2.1 1.7 7.9 2.7 <2.1 <0.4 <0.4 Naphthalene <2.5 <2.5 <2.5 <2.5 <2.5 <2.5 <2.5 <2.5 <12.3 <12.3 <12.3 <2.5 <2.5 <2.5 <2.5 <2.5 <2.5 <2.5 Perylene 1.7 <1.5 <1.5 <1.5 <0.3 <0.3 <1.5 <0.3 <1.5 <0.3 <1.5 <0.3 <1.5 <1.5 <1.5 <0.3 <0.3 <0.3 Phenanthrene 7.4 8.4 30 3.1 4.4 15 13 15 11 13 35 18 17 100 29 17 <4.1 13 Pyrene 12 13 27 2.2 5.3 21 27 34 46 36 73 39 44 230 59 39 3.5 13
Appendix E 53

Table E2. Summary of results for analysis of SPMD extracts by the hydrophobic method for SPMDs deployed in Tinkers 

Creek and its tributaries and two other tributaries to the Cuyahoga River in 2006.

[–, not detected. Water concentration results are estimated on the basis of recovery of performance reference compounds]

Compound Number of 

detections

Frequency of 

detection 

(percent)

Concentrations of detections, in nanograms per liter

Minimum Maximum Median

Fluoranthene 18 100 3.8 340 51

Pyrene 18 100 2.2 230 30

Phenanthrene 17 94 3.1 100 15

Chrysene 16 89 0.9 87 14

2-Methylphenanthrene 11 61 1.8 28 3.1

Benzo[b]fluoranthene 11 61 1.4 25 5.1

Benz[a]anthracene 10 56 1.9 27 3.6

Benzo[b]naphtho[2,1-d]-thiophene 10 56 1.8 12 2.6

Benzo[e]pyrene 10 56 2.9 22 5.2

Benzo[k]fluoranthene 10 56 2.3 27 4.3

2-Methylfluoranthene 8 44 1.2 8.8 1.8

Benzo[a]pyrene 8 44 1.0 7.4 2.1

1-Methylfluorene 6 33 1.0 8.2 2.6

3,6-Dimethylphenanthrene 5 28 0.9 6.9 1.6

Anthracene 5 28 1.4 6.3 2.1

Indeno[1,2,3-c,d]pyrene 5 28 1.7 7.9 2.7

Benzo[g,h,i]perylene 4 22 1.1 2.8 2.1

Dibenzothiophene 3 17 2.3 5.7 2.3

2,3,5-Trimethylnaphthalene 2 11 2.1 2.3 2.2

Acenaphthene 2 11 2.7 6. 4.4

Fluorene 1 6 2.4 2.4 2.4

Perylene 1 6 1.7 1.7 1.7

1,2-Dimethylnaphthalene 0 0 – – –

1-Ethylnaphthalene 0 0 – – –

1-Methylnaphthalene 0 0 – – –

2-Methylnaphthalene 0 0 – – –

4-Methylbiphenyl 0 0 – – –

9-Methylanthracene 0 0 – – –

Acenaphthylene 0 0 – – –

Benzo[b]thiophene 0 0 – – –

Biphenyl 0 0 – – –

Dibenz[a,h]anthracene 0 0 – – –

Naphthalene 0 0 – – –
54 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Appendix F. Organic Wastewater Compounds in Streambed Sediments Table F1. Results for analysis of streambed-sediment samples by the pharmaceutical method for samples collected in Tinkers Creek and its tributaries and two other tributaries to the Cuyahoga River in 2006. [Street, Streetsboro; Aur W, Aurora Westerly; Aur Sh, Aurora Shores; Twins, Twinsburg; Sol, Solon; Bed, Bedford, Bed Hgts, Bedford Heights, DR, Tinkers Creek at Dunham Road; FR, Furnace Run; YC, Yellow Creek; US, upstream; DS, downstream; AO, above outfall; na, not available; e, estimated concentration less than the reporting limit; <, less than. Data in bold print were either not detected or detected at a lower concentration in the upstream sample] Compound Concentrations at sampling locations, in micrograms per kilogram Street Aur W Aur Sh Twins Sol Bed Bed Hgts DR FR YC US DS US DS US DS US DS US DS US DS AO US DS 1,7- Dimethylxanthine <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 Acetaminophen <0.76 <0.76 <0.76 <0.76 <0.76 <0.76 <0.76 <0.76 <0.76 <0.76 <0.76 <0.76 <0.76 <0.76 <0.76 <0.76 <0.76 <0.76 Albuterol <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 Azithromycin na na na na na na na na na na na na na na na na na na Caffeine <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 7.7 <1.3 9.1 12 1.5 <1.3 <1.3 4.8 <1.3 <1.3 Carbamazepine <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 Cimetidine <0.88 <0.88 <0.88 <0.88 <0.88 <0.88 <0.88 <0.88 <0.88 <0.88 <0.88 <0.88 <0.88 <0.88 <0.88 <0.88 <0.88 <0.88 Codeine <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 Cotinine <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 Dehydronifedipine <1.7 12 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 Diltiazem <1.5 <1.5 <1.5 25 <1.5 <1.5 <1.5 <1.5 <1.5 <1.5 <1.5 <1.5 <1.5 <1.5 e0.79 <1.5 <1.5 <1.5 Diphenhydramine <1.4 12 3.2 75 3.4 25 <1.4 13 <1.4 15 <1.4 <1.4 e0.34 <1.4 <1.4 10 <1.4 <1.4 Erythromycin <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 <1.7 8.2 <1.7 <1.7 e0.50 Fluoxetine <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 <2.2 Miconazole <0.97 6.1 6.2 11 7.7 9.3 <0.97 <0.97 <0.97 <0.97 <0.97 <0.97 <0.97 <0.97 <0.97 <0.97 <0.97 <0.97 Ranitidine <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 <1.1 Sulfamethoxazole <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 <1.6 3.3 1.8 <1.6 2.3 1.8 Thiabendazole <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 Trimethoprim <1.5 <1.5 <1.5 7.4 <1.5 <1.5 <1.5 <1.5 <1.5 <1.5 <1.5 <1.5 <1.5 <1.5 e0.29 <1.5 <1.5 <1.5 Warfarin <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3 <1.3
Appendix F 55

Table F2. Summary of results for analysis of streambed-sediment samples by the pharmaceutical method for 

samples collected in Tinkers Creek and its tributaries and two other tributaries to the Cuyahoga River in 2006.

[e, estimated concentration less than the reporting limit; –, not detected]

Compound Number of 

detections

Frequency of 

detection 

(percent)

Concentrations of detections, 

in micrograms per kilogram

Minimum Maximum Median

Diphenhydramine 9 50 e0.34 75 e12

Caffeine 5 28 1.5 12 7.7

Miconazole 5 28 6.1 11 7.7

Sulfamethoxazole 4 22 1.8 3.3 2.0

Diltiazem 2 11 e0.79 25 e13

Erythromycin 2 11 e0.50 8.2 e4.4

Trimethoprim 2 11 e0.29 7.4 e3.8

Dehydronifedipine 1 6 12 12 12

1,7-Dimethylxanthine 0 0 – – –

Acetaminophen 0 0 – – –

Albuterol 0 0 – – –

Azithromycin 0 0 – – –

Carbamazepine 0 0 – – –

Cimetidine 0 0 – – –

Codeine 0 0 – – –

Cotinine 0 0 – – –

Fluoxetine 0 0 – – –

Ranitidine 0 0 – – –

Thiabendazole 0 0 – – –

Warfarin 0 0 – – –
56 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio Table F3. Results for analysis of streambed-sediment samples by the wastewater method for samples collected in Tinkers Creek and its tributaries and two other tributaries to the Cuyahoga River in 2006.—Continued [Street, Streetsboro; Aur W, Aurora Westerly; Aur Sh, Aurora Shores; Twins, Twinsburg; Sol, Solon; Bed, Bedford; Bed Hgts, Bedford Heights; DR, Tinkers Creek at Dunham Road; FR, Furnace Run; YC, Yellow Creek; US, upstream; DS, downstream; AO, above outfall; na, not available; e, estimated concentration; m, compound presence verified through qualitative criteria, but concentration could not be quantified. Data in bold print were not detected or detected at a lower concentration in the upstream sample] Compound Concentrations at sampling locations, in micrograms per kilogram Street Aur W Aur Sh Twins Sol Bed Bed Hgts DR FR YC US DS US DS US DS US DS US DS US DS AO US DS 1,4-Dichlorobenzene <55 <40 <45

m <35 <60 <30 <30 <30 e16

m <25 <25 <30 <30 <25 <30 <25

1-Methylnaphthalene e10 e10

m e20 <40 <60

m

m e30 e40 e20 e20 e20 e20 e10 e30 e10

m

2,6-Dimethylnaphthalene e50 e40 e30 e60 e20 60 e20

m e10 e10 e10

m

m

m

m

m

m

m

2-Methylnaphthalene e20 e20 e10 e30

m e10 e10 e10 e40 e50 e30 e20 e20 e30 e20 e40 e20 e10

3-β-Coprostanol e120 e90 e80 e300 e60 e150 e80 e60 <300 e220 e60 e150 e20 <300 e30 e40 <300 e503-Methyl-1H-indole 150 100 e40 80 e20 70 e20

m

m e10

m

m e10

m e10

m

m

m

3-tert-Butyl-4-hydroxyanisole <160 <120 <140 <200 <100 <180 <90 <90 <90 <80 <80 <80 <80 <90 <90 <80 <90 <80

4-Cumylphenol <60 <40 <40 <60 <40 <60 <30 <30 <30 <20 <20 <20 <20 <30 <30 <20 <30 <20

4-n-Octylphenol <60 <40 <40 <60 <40 <60 <30 <30 <30 <20 <20 <20 <20 <30 <30 <20 <30 <20

4-Nonylphenol <820 <600 <680 e320 <520 e210 <450 <450 <450 e190 e180 e190 <380 <450 <450 <380 <450 <380

4-tert-Octylphenol <60 <40 <40 <60 <40 <60 <30 <30 <30 <20 <20 <20 e20 <30 e20 e10 <30 <20

Anthraquinone 110 71 57 e48 e38 67 98 55 240 130 190 130 68 54 88 87 e20 e22

Acetophenone e20 e20 e20 e20

m e20 e10

m e40 e90 e30 e50 <80 e40 e40 e60 e50 <80

Acetyl hexamethyl tetrahydronaphthalene 

(AHTN) <60 e20 <40 80 <40 e40

m e10 <30 e50

m e20 <20 <30 <30

m <30 <20

Anthracene 60 e30 e20 <60 e10 e10 e50 60 80 e50 110 60 50 e20 50 e40 e10 e30

Atrazine <110 <80 <90 <130 <70 <120 <60 <60 <60 <50 <50 <50 <50 <60 <60 <50 <60 <50

2,2 ́,4,4 ́-tetrabromodiphenyl 

ether <55 <40 <45 <65 <35 <60 <30 <30 <30 <25 <25 <25 <25 <30 <30 <25 <30 <25

Benzo[a]pyrene 150 80 80 e30 e50 80 160 170 290 230 390 260 200 60 220 130 e30 50

Benzophenone <60 <40 <40 <60 <40 <60 <30 <30 <30 <20 <20 <20 <20 <30 <30 <20 <30 <20β-Sitosterol e2,500 e1,400 e2,100 e2,300 e1,100 e2,100 e890 e640 310 e600 e300 e210 e370 e480 e310 e250 e490 e790β-Stigmastanol e590 e380 e290 e1,100 e280 e640 e190 e30 <300 e100 e60 e50 e60 <300 e60 <250 e70 e140bis(2-Ethylhexyl) phthalate e80 e50 e60 e60 e40 e110 e50 e50 e80 e120 e90 e120 e60 e50 e50 e50 <150 e30Bisphenol A na na na na na na e60 na na e20 na na na na na na na na

Bromacil <550 <400 <450 <650 <350 <600 <300 <300 <300 <250 <250 <250 <250 <300 <300 <250 <300 <250Camphor <60 <40 <40 <60 <40 <60 <30 <30 <30 <20 <20 <20 <20 <30 <30 <20 <30 <20Carbazole 60 e40 e30 e30 e20 e30 60 50 130 70 110 60 60 e20 e50 50

m e20

Chlorpyrifos <60 <40 <40 <60 <40 <60 <30 <30 <30 <20 <20 <20 <20 <30 <30 <20 <30 <20
Appendix F 57

Table F3. Results for analysis of streambed-sediment samples by the wastewater method for samples collected in Tinkers Creek and its tributaries and two other tributaries to the Cuyahoga River in 2006.—Continued[Street, Streetsboro; Aur W, Aurora Westerly; Aur Sh, Aurora Shores; Twins, Twinsburg; Sol, Solon; Bed, Bedford; Bed Hgts, Bedford Heights; DR, Tinkers Creek at Dunham Road; FR, Furnace Run; YC, Yellow Creek; US, upstream; DS, downstream; AO, above outfall; na, not available; e, estimated concentration; m, compound presence verified through qualitative criteria, but concentration could not be quantified. Data in bold print were not detected or detected at a lower concentration in the upstream sample]

Compound

Concentrations at sampling locations, in micrograms per kilogram

Street Aur W Aur Sh Twins Sol Bed Bed Hgts DR FR YC US DS US DS US DS US DS US DS US DS AO US DS

Cholesterol e1,400 e870 e2,800 e2,400 e520 e1,300 e690 e600 e320 e1,000 e400 e410 e340 e480 e310 e260 e410 e810

N,N-diethyl-meta-toluamide 

(DEET) <110 <80 <90 <130 <70 <120 <60 <60 <60 <50 <50 <50 <50 <60 <60 <50 <60 <50

Diazinon <60 <40 <40 <60 <40 <60 <30 <30 <30 <20 <20 <20 <20 <30 <30 <20 <30 <204-Nonylphenol diethoxylate

(NP2EO; sum of all isomers) e330 e250 <900 e450 e200 e900 <600 <600 <600 e390 e320 e910 <500 <600 <600 <500 <600 <500

4-Octylphenol diethoxylate 

(OP2EO; sum of all isomers) <60 <40 <40 <60 <40 <60 <30 <30 <30 e20 <20 e20 e10 <30 e20 e10 <30 <20

Diethyl phthalate e10 <80 e30 <130 <70 <120 <60 <60 <60 <50 <50 <50 <50 <60 <60 m e10 <50

d-Limonene <60 <40 m <60 <40 e10 <30 <30 <30 <20 <20 <20 <20 <30 <30 <20 <30 <204-Octylphenol monoethoxylate

 (OP1EO; sum of all isomers) <280 <200 <220 <320 <180 <300 <150 <150 <150 <120 <120 <120 <120 <150 <150 e20 <150 <120

Fluoranthene 670 310 270 80 180 280 680 600 990 820 1,400 1,400 580 280 680 490 80 210

Hexahydrohexamethylcyclopentabenzopyran 

(HHCB) <60 70 <40 230 <40 220 e20 e20 <30 390 m 50 <20 <30 <30 e30 <30 <20

Indole 1,100 780 380 760 300 670 250 100 e30 e50 e40 e40 e30 e40 e50 e40 e60 e50Isoborneol <60 <40 <40 <60 <40 <60 <30 <30 <30 <20 <20 <20 <20 <30 <30 <20 <30 <20

Isophorone <60 <40 <40 <60 <40 <60 <30 <30 <30 <20 <20 <20 <20 <30 <30 <20 <30 <20Isopropylbenzene (cumene) <110 <80 <90 <130 <70 <120 <60 <60 <60 <50 <50 <50 <50 <60 <60 m <60 <50Isoquinoline <110 <80 <90 <130 <70 <120 <60 <60 <60 <50 <50 <50 <50 <60 <60 <50 <60 <50Menthol <60 <40 <40 <60 <40 <60 <30 <30 <30 <20 <20 <20 <20 <30 <30 <20 <30 <20Metolachlor <60 <40 <40 <60 <40 <60 <30 <30 <30 <20 <20 <20 <20 <30 <30 <20 <30 <204-Nonylphenol monoethoxylate (NP1EO; sum of all 

isomers)

<550 e190 e150 e500 <350 e370 <300 <300 <300 e260 e200 e290 <250 <300 <300 <250 <300 <250

Naphthalene e30 e20 e10 e30 m e20 e20 e10 e30 e40 e20 e20 e20 e20 e20 e30 e10 e10

p-Cresol e140 e120 e60 e260 e30 e100 e50 e10 e30 e50 e40 e30 <120 e30 e30 e30 e30 <120Phenanthrene 210 110 110 <60 80 120 300 290 560 310 720 340 290 140 290 250 60 120

Phenol e80 e150 e70 e100 e80 e200 e60 <30 e40 220 e20 e30 <20 e30 e70 e50 e70 <20
58 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio Table F3. Results for analysis of streambed-sediment samples by the wastewater method for samples collected in Tinkers Creek and its tributaries and two other tributaries to the Cuyahoga River in 2006.—Continued [Street, Streetsboro; Aur W, Aurora Westerly; Aur Sh, Aurora Shores; Twins, Twinsburg; Sol, Solon; Bed, Bedford; Bed Hgts, Bedford Heights; DR, Tinkers Creek at Dunham Road; FR, Furnace Run; YC, Yellow Creek; US, upstream; DS, downstream; AO, above outfall; na, not available; e, estimated concentration; m, compound presence verified through qualitative criteria, but concentration could not be quantified. Data in bold print were not detected or detected at a lower concentration in the upstream sample] Compound Concentrations at sampling locations, in micrograms per kilogram Street Aur W Aur Sh Twins Sol Bed Bed Hgts DR FR YC US DS US DS US DS US DS US DS US DS AO US DS Prometon <60 <40 <40 <60 <40 <60 <30 <30 <30 <20 <20 <20 <20 <30 <30 <20 <30 <20 Pyrene 510 240 200 70 140 210 490 440 720 590 1,000 1,100 450 210 520 370 60 150 Tributyl phosphate <60 <40 <40 <60 <40 <60 <30 <30 <30 <20 <20 <20 <20 <30 <30 <20 <30 <20 Triclosan <55 <40 <45 e56 <35 <60 <30 <30 <30 e36 <25 e30 <25 <30 <30 <25 <30 <25 Triphenyl phosphate <60 <40 <40 <60 <40 <60 <30 <30 <30 <20 <20

m <20 <30 <30 <20 <30 <20

Tris(2-butoxyethyl) phosphate <160 <120 <140 <200 <100 <180 <30 e30 e30 e50 e70 e70 <80 e30 <90 e20 <90 <80

Tris(2-chloroethyl) phosphate <110 <80 <90 <130 <70 <120 <90 <60 <60 <50 <50 <50 <50 <60 <60 <50 <60 <50

Tris(dichloroisopropyl) 

phosphate <110 <80 <90 <130 <70 <120 <90 <60 <60 <50 <50 <50 <50 <60 <60 <50 <60 <50
Appendix F 59

Table F4. Summary of results for analysis of streambed-sediment samples by the wastewater method for samples collected in 

Tinkers Creek and its tributaries and two other tributaries to the Cuyahoga River in 2006.—Continued

[e, estimated concentration; –, not detected; nqd, no quantified detections]

Compound Number of

 detections

Frequency of

 detection 

(percent)

 Concentrations of detections, 

in micrograms per kilogram

Minimum Maximum Median

2,6-Dimethylnaphthalene1 18 100 e10 60 e25

2-Methylnaphthalene1 18 100 e10 e50 e20

3-Methyl-1H-indole1 18 100 e10 150 e30

Anthraquinone 18 100 e20 240 e70

Benzo[a]pyrene 18 100 e30 390 e140

β-Sitosterol 18 100 e210 e2,500 e620

Carbazole1 18 100 e20 130 e50

Cholesterol 18 100 e260 e2,800 e560

Fluoranthene 18 100 80 1,400 540

Indole 18 100 e30 1,100 e55

Naphthalene1 18 100 e10 e40 e20

Pyrene 18 100 60 1,100 400

Anthracene 17 94 e10 110 e50

bis(2-Ethylhexyl) phthalate 17 94 e30 e120 e60

Phenanthrene 17 94 60 720 250

1-Methylnaphthalene1 16 89 e10 e40 e20

Acetophenone1 16 89 e10 e90 e35

p-Cresol 16 89 e10 e260 e35

3-β-Coprostanol 15 83 e20 e300 e80

β-Stigmastanol 15 83 e30 e1,100 e140

Phenol 15 83 e20 220 e70

Acetyl hexamethyl tetrahydronaphthalene 

(AHTN) 1 10 56 e10 80 e30

Hexahydrohexamethylcyclopentabenzopyran 

(HHCB) 1 9 50 e20 390 e60

4-Nonylphenol diethoxylate (NP2EO; sum of all 

isomers) 8 44 e200 e910 e360

4-Nonylphenol monoethoxylate (NP1EO; sum of 

all isomers) 7 39 e150 e500 e260

Tris(2-butoxyethyl) phosphate 7 39 e20 e70 e30

4-Nonylphenol 5 28 e180 e320 e190

4-Octylphenol diethoxylate (OP2EO; sum of all 

isomers) 5 28 e10 e20 e20

Diethyl phthalate1 4 22 e10 e30 e10

1,4-Dichlorobenzene1 3 17 e16 e16 e16

4-tert-Octylphenol 3 17 e10 e20 e20

Triclosan 3 17 e30 e56 e36

Bisphenol A 2 11 e20 e60 e40

d-Limonene1 2 11 e10 e10 e10

4-Octylphenol monoethoxylate (OP1EO; sum of 

all isomers) 1 6 e20 e20 e20

3-tert-Butyl-4-hydroxy anisole1 1 6 nqd nqd nqd

Isopropylbenzene1 1 6 nqd nqd nqd

Triphenyl phosphate 0 0 – – –

4-Cumylphenol 0 0 – – –
60 Occurrence of Organic Wastewater Compounds in the Tinkers Creek Watershed, Northeast Ohio

Table F4. Summary of results for analysis of streambed-sediment samples by the wastewater method for samples collected in 

Tinkers Creek and its tributaries and two other tributaries to the Cuyahoga River in 2006.—Continued

[e, estimated concentration; –, not detected; nqd, no quantified detections]

Compound Number of

 detections

Frequency of

 detection 

(percent)

 Concentrations of detections, 

in micrograms per kilogram

Minimum Maximum Median

4-n-Octylphenol 0 0 – – –

Atrazine 0 0 – – –

2,2 ́,4,4 ́-Tetrabromodiphenyl ether 0 0 – – –

Benzophenone 0 0 – – –

Bromacil 0 0 – – –

Camphor 0 0 – – –

Chlorpyrifos 0 0 – – –

N,N-Diethyl-meta-toluamide (DEET) 0 0 – – –

Diazinon 0 0 – – –

Isoborneol 0 0 – – –

Isophorone 0 0 – – –

Isoquinoline 0 0 – – –

Menthol 0 0 – – –

Metolachlor 0 0 – – –

Prometon 0 0 – – –

Tributylphosphate 0 0 – – –

Tris(2-chloroethyl) phosphate 0 0 – – –

Tris(dichloroisopropyl) phosphate 0 0 – – –

1

 Compound was detected in one or more samples but not quantified. Statistics of concentrations reported for this compound are based only on quantified 

concentrations.
Tertuliani and others—Organic Wastewater Compounds in Tinkers Creek Watershed, Northeast Ohio—Scientific Investigations Report 2008–5173

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