Prepared in cooperation with the Minnesota Pollution Control Agency

Endocrine Disrupting Chemicals in Minnesota 

Lakes—Water-Quality and Hydrological Data from 

2008 and 2010

By Larry B. Barber, Jeffrey H. Writer, Steffanie H. Keefe, Greg K. Brown, Mark L. Ferrey, Nathan D. Jahns, 

Richard L. Kiesling, James R. Lundy, Beth H. Poganski, Donald O. Rosenberry, Howard E. Taylor, 

Olivia P. Woodruff, and Heiko L. Schoenfuss

Open-File Report 2012–1124

U.S. Department of the Interior

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

KEN SALAZAR, Secretary

U.S. Geological Survey

Marcia K. McNutt, Director

U.S. Geological Survey, Reston, Virginia: 2012 

For product and ordering information:

World Wide Web: http://www.usgs.gov/pubprod

Telephone: 1-888-ASK-USGS

For more information on the USGS—the Federal source for science about the Earth, its natural and 

living resources, natural hazards, and the environment: World Wide Web: http://www.usgs.gov

Telephone: 1-888-ASK-USGS

Suggested citation: 

Barber, L.B., Writer, J.H., Keefe, S.H., Brown, G.K., Ferrey, M.L., Jahns, N.D., Kiesling, R.L., Lundy, 

J.R., Poganski, B.H., Rosenberry, D.O., Taylor, H.E., Woodruff, O.P., and Schoenfuss, H. L., 2012, 

Endocrine disrupting chemicals in Minnesota lakes—Water-quality and hydrological data from 2008 

and 2010: U.S. Geological Survey Open-File Report 2012–1124, 53 p. 

Any use of trade, product, or firm names is for descriptive purposes only and does not imply 

endorsement by the U.S. Government.

Although this report is in the public domain, permission must be secured from the individual copyright 

owners to reproduce any copyrighted material contained within this report.
iii

Contents

Abbreviations................................................................................................................................................vii

Units ............................................................................................................................................................ viii

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

Introduction.................................................................................................................................................... 1

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

Methods......................................................................................................................................................... 3

Statewide Survey ....................................................................................................................................... 3

Sullivan Lake Microhabitat Study ............................................................................................................... 3

Microhabitat Groundwater/Surface-Water Interactions........................................................................... 4

Chemical Analysis...................................................................................................................................... 4

Quality Assurance...................................................................................................................................... 6

Water-quality and Hydrological Data ............................................................................................................. 6

Statewide Lake Survey .............................................................................................................................. 6

Sullivan Lake Microhabitat Study ............................................................................................................... 7

Geohydrological Environment ................................................................................................................ 7

Microhabitat Characterization................................................................................................................. 8

Temporal Sampling ................................................................................................................................ 9

Conclusions................................................................................................................................................... 9

Acknowledgments ......................................................................................................................................... 9

References Cited......................................................................................................................................... 10

Figures

Figure 1. Site locations for the 14 Minnesota lakes sampled during 2008 and 2010 .............................. 14

Figure 2. Site locations for the four littoral-zone microhabitats investigated at Sullivan Lake, Minn........ 15

Figure 3. Site topography and preliminary hydraulic analysis of potential zones of groundwater

discharge in Sullivan Lake, Minn ................................................................................................................. 16
iv

Tables

Table 1. Site characteristics for the four Minnesota lakes that were sampled in this investigation ........ 17

Table 2. Trace elements and major elements measured by inductively coupled plasma/mass 

spectrometry (Garbarino and Taylor, 1995) and inductively coupled plasma/atomic-emission 

spectrometry (Garbarino and Taylor, 1979) at the U.S. Geological Survey National Research 

Program Laboratory, and the trace and major elements’ approximate method detection limits (MDL)........ 19

Table 3. Acidic organic compounds measured by evaporation with derivatization and gas 

chromatography/mass spectrometry (Barber and others, 2000) at the U.S. Geological Survey 

National Research Program Laboratory ...................................................................................................... 20

Table 4. Neutral organic compounds measured by continuous liquid-liquid extraction using 

methylene chloride with gas chromatography/mass spectrometry (Barber and others, 2000) at 

the U.S. Geological Survey National Research Program Laboratory........................................................... 21

Table 5. Steroid and steroidal hormone compounds measured by octadecylsilica solid-phase 

extraction with derivatization and gas chromatography/tandem mass spectrometry (Barber and 

others, 2003; Foreman and others, 2011) at the U.S. Geological Survey National Research 

Program Laboratory..................................................................................................................................... 22

Table 6. Summary of field measurements made at 11 Minnesota lakes during 2008............................ 23

Table 7. Summary of major- and trace-element data for water samples collected from 

11 Minnesota lakes during 2008.................................................................................................................. 24

Table 8. Summary of acidic organic compound data for water samples collected from 

11 Minnesota lakes during 2008.................................................................................................................. 26

Table 9. Summary of neutral organic compound data for water samples collected from 

11 Minnesota lakes during 2008.................................................................................................................. 26

Table 10. Summary of steroid and steroidal hormone compound data for water samples 

collected from 11 Minnesota lakes during 2008........................................................................................... 30

Table 11. Summary of neutral organic compound data for sediment samples collected from 

11 Minnesota lakes during 2008.................................................................................................................. 33

Table 12. Summary of steroid and steroidal hormone compound data for sediment samples 

collected from 11 Minnesota lakes during 2008........................................................................................... 36

Table 13. Summary of neutral organic compound data for polar organic compound integrative 

samplers (POCIS) deployed in 11 Minnesota lakes during 2008................................................................. 38

Table 14. Summary of steroid and steroidal hormone compound data for passive organic 

compound integrative samplers (POCIS) deployed in 11 Minnesota lakes during 2008.............................. 39

Table 15. Summary of field measurements for water samples collected from four Minnesota 

lakes during 2010 ........................................................................................................................................ 41

Table 16. Summary of acidic organic compound data for water samples collected from four 

Minnesota lakes during 2010....................................................................................................................... 41

Table 17. Summary of neutral organic compound data for water samples collected from four 

Minnesota lakes during 2010....................................................................................................................... 42

Table 18. Summary of steroid and steroidal hormone compound data for water samples 

collected from four Minnesota lakes during 2010......................................................................................... 43
v

Table 19. Summary of field data for preliminary microhabitat selection at Sullivan Lake, Minn., 

June 1, 2010................................................................................................................................................ 44

Table 20. Site characterization of Sullivan Lake microhabitat A (residential/septic influence) 

and water-quality values for pore-water samples collected July 8, 2010 ..................................................... 45

Table 21. Water column water-quality measurements for Sullivan Lake microhabitat A 

(residential/septic influence) collected from 1:30 to 3:00 PM on July 21, 2010............................................ 45

Table 22. Site characterization of Sullivan Lake microhabitat B (residential/septic influence) 

and water-quality values for pore-water samples collected July 8, 2010 ..................................................... 46

Table 23. Water column water-quality measurements for Sullivan Lake microhabitat B 

(residential/septic influence) collected 10:30 AM to 2:00 PM on July 21, 2010 ........................................... 46

Table 24. Site characterization of Sullivan Lake microhabitat C (stormwater/boat-ramp influence) 

and water-quality values for pore-water samples collected July 8, 2010 ..................................................... 47

Table 25. Water column water-quality measurements for Sullivan Lake microhabitat C 

(stormwater/boat ramp influence) collected 12:00 to 1:30 PM on July 21, 2010.......................................... 47

Table 26. Site characterization of Sullivan Lake microhabitat D (agricultural influence) 

and water-quality values for pore-water samples collected July 9, 2010 ..................................................... 48

Table 27. Water column water-quality measurements for Sullivan Lake microhabitat D 

(agricultural influence) collected 9:00 to 10:30 AM on July 21, 2010........................................................... 48

Table 28. Summary of acidic organic compound data for water samples collected from 

four microhabitat sites in Sullivan Lake, Minn., on July 8, 2010................................................................... 49

Table 29. Summary of acidic organic compound data for water samples collected from 

four microhabitat sites in Sullivan Lake, Minn., on October 12, 2010 .......................................................... 49

Table 30. Summary of neutral organic compound data for water samples collected from

four microhabitat sites in Sullivan Lake, Minnesota on July 8, 2010........................................................... 50

Table 31. Summary of neutral organic compound data for water samples collected from 

four microhabitat sites in Sullivan Lake, Minn., on October 12, 2010 .......................................................... 51

Table 32. Summary of steroid and steroidal hormone compound data for water samples 

collected from four microhabitat sites in Sullivan Lake, Minn., on July 8, 2010............................................ 52

Table 33. Summary of steroid and steroidal hormone compound data for water samples 

collected from four microhabitat sites in Sullivan Lake, Minn., on October 12, 2010 ................................... 53
vi

Conversion Factors

Inch/Pound to SI 

Multiply By To obtain

Length

centimeter (cm) 0.3937 inch (in)

meter (m) 3.281 foot (ft)

kilometer (km) 0.6214 mile (mi)

Area

square kilometer (km2) 0.3861 square mile (mi2) 

Volume

liter (L) 0.2642 gallon (gal)

Mass

gram (g) 0.03527 ounce, avoirdupois (oz)

kilogram (kg) 2.205 pound, avoirdupois (lb)

Pressure

torr 0.0193 pound per square inch (PSI)

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

°F=(1.8×°C)+32

Vertical coordinate information is referenced to the North American Vertical Datum of 1988 (NAVD 88).

Altitude, as used in this report, refers to distance above the vertical datum.

Specific conductance is given in microsiemens per centimeter at 25 degrees Celsius (μS/cm at 25°C).

Concentrations of chemical constituents in water are given either in milligrams per liter (mg/L) or 

micrograms per liter (μg/L).
vii

Abbreviations

AP, alkylphenolethoxylates

SPE, octadecylsilica solid-phase extraction

CASRN, Chemical Abstract Services Registry Number

CLLE, continuous liquid-liquid extraction

EVAP, evaporated to dryness

GC/MS, gas chromatography/mass spectrometry

GC/MS/MS, gas chromatography/tandem mass spectrometry

LAS, linear alkylbenzene sulfonate

MDL, method detection limits

NA, not available

NRPL, National Research Program Laboratory

SIM, selected ion monitoring

TM, trademarked

USGS, U.S. Geological Survey

--, not determined
viii

Units

cm, centimeter

°C, degree Celsius

hr, hour

km, kilometer

km2, square kilometer

L, liter

m, meter

mg/L, milligram per liter

mg/L C, milligram per liter carbon

mL, milliliter

mL/min/m2, milliliters per minute per square meter

mm, millimeter

ng/L, nanogram per liter

nm, nanometer

Std units, standard pH units

μg/L, microgram per liter

μm, micrometer

μS/cm, microsiemens per centimeter

v/v, volume/volume

<, less than
Endocrine Disrupting Chemicals in Minnesota 

Lakes—Water-Quality and Hydrological Data from 

2008 and 2010

By Larry B. Barber,1 Jeffrey H. Writer,

1 Steffanie H. Keefe,1 Greg K. Brown,1 Mark L. Ferrey,2 

Nathan D. Jahns,3 Richard L. Kiesling,4 James R. Lundy,5 Beth H. Poganski,

3 Donald O. Rosenberry,6

Howard E. Taylor,

1 Olivia P. Woodruff,1 and Heiko L. Schoenfuss3

Abstract

Understanding the sources, fate, and effects of endocrine disrupting chemicals in aquatic 

ecosystems is important for water-resource management. This study was conducted during 2008 

and 2010 to establish a framework for assessing endocrine disrupting chemicals, and involved a 

statewide survey of their occurrence in 14 Minnesota lakes and a targeted study of different 

microhabitats on a single lake. The lakes ranged in size from about 0.1 to 100 square kilometers, 

varied in trophic status from oligotrophic to eutrophic, and spanned a range of land-uses from 

wetlands and forest to agricultural and urban use. Water and sediment samples were collected 

from the near-shore littoral environment and analyzed for endocrine disrupting chemicals, 

including trace elements, acidic organic compounds, neutral organic compounds, and steroidal 

hormones. In addition, polar organic compound integrative samplers were deployed for 21 days 

and analyzed for the same organic compounds. One lake was selected for a detailed microhabitat 

study of multiple near-shore environments. This report compiles the results from the field 

measurements and laboratory chemical analysis of water, sediment, and polar organic compound 

integrative sampler samples collected during 2008 and 2010. Most of the organic compounds 

measured were not detected in any of the water samples, although a few compounds were 

detected in several of the lakes. 

Introduction

Most research on the occurrence and effects of endocrine disrupting chemicals (EDCs) in 

the aquatic environment has focused on effluents from wastewater treatment plants (WWTPs) 

and effluent-impacted streams (Folmar and others, 1996; Jobling and others, 1998; Tyler and 

others, 1998; Barber and others, 2007; Vajda and others, 2008; Lee and others, 2010). However, 

a variety of natural and synthetic EDCs can enter lake environments via sources such as: runoff 

 

1 U.S. Geological Survey, 3215 Marine Street, Boulder CO 80303

2 Minnesota Pollution Control Agency, 520 Lafayette Road, St. Paul, MN 55155 3 St. Cloud State University, WSB-273, 720 Fourth Avenue South, St. Cloud, MN 56301 4 U.S. Geological Survey, 2280 Woodale Drive, Mounds View, MN 55112

5 Minnesota Department of Health, St. Paul, MN 55155

6 U.S. Geological Survey, Denver Federal Center, Denver, CO 80225
2

from surrounding urban and agricultural land use, septic system discharges from residences 

along the shoreline, and recreational activity (Swartz and others, 2006; Conn and others, 2006; 

Conn and others, 2010; Writer and others, 2010; Lee and others, 2011). In general, the most 

important estrogenic chemicals in the aquatic environment include the natural and synthetic 

steroidal hormones 17β-estradiol, estrone, and 17α-ethynylestradiol, and the alkyphenol 

compounds 4-nonylphenol and 4-tert-octylphenol (Van den Belt and others, 2004; Bistodeau and 

others, 2006; Sumpter and others, 2006; Barber and others, 2007; Schoenfuss and others, 2008).

Although the occurrence of EDCs in effluents and streams (and associated endocrine 

disruption in fish) has been documented, there is less information on the occurrence and impacts 

of EDCs in lakes that do not receive WWTP effluent discharges. For example, Lake Mead 

(Arizona and Nevada), which receives the discharge from a number of upstream WWTPs, has 

been shown to have elevated concentrations of synthetic chemicals and endocrine disruption in 

common carp (Rosen and others, 2006). The potential susceptibility of lake ecosystems to 

endocrine disruption has been documented by a rapid collapse in fish populations across multiple 

species after dosing a pristine Canadian lake for several years with approximately 5 nanogram

per liter (ng/L) of the synthetic estrogen 17α-ethynylestradiol (Palace and others, 2002; Kidd and 

others, 2007). However, after the 17α-ethynylestradiol dosing was terminated, the fish 

populations recovered (Palace and others, 2009). Based partially on data presented in this report, 

Writer and others (2010) describe the low-level but widespread occurrence of EDCs and fish 

endocrine disruption in Minnesota lakes that do not have WWTP effluent inputs. Endocrine 

disruption also has been reported in fish from Lake Thun, Switzerland (Bogdal and others, 

2009). Skelly and others (2010) have described endocrine disruption in frogs from urban ponds. 

These results suggest the widespread occurrence of EDCs and fish endocrine disruption in lakes 

that do not receive WWTP effluent discharges. 

Purpose and Scope

The purpose of this cooperative study between the Minnesota Pollution Control Agency 

(MPCA) and the U.S. Geological Survey (USGS), which included collaboration with St.Cloud 

State University (SCSU), was to determine the occurrence of endocrine disrupting chemicals in 

water and sediment from lakes across the State of Minnesota. This report compiles data from a 

multi-tiered investigation into the occurrence of EDCs in Minnesota lakes conducted during 

2008 and 2010 that consisted of: (1) a statewide survey of the chemistry of 14 lakes (11 sampled 

during 2008 and three sampled during 2010; two sampled both years), and (2) a detailed 

microhabitat study to characterize the hydrology and chemistry of the littoral zone in Sullivan 

Lake. Sullivan Lake is characteristic of many Minnesota lakes influenced by the surrounding 

landscape that includes agricultural land-use and residences using septic systems for onsite 

wastewater disposal. Results from the detailed study can be used to better understand the results 

from the statewide survey.

Companion investigations into endocrine-disruption in wild-caught fish and controlled 

field-exposure experiments using caged fathead minnows were conducted in conjunction with 

the water sampling in the 11 lakes sampled in 2008 (Ferrey and others, 2008) and in Sullivan 

Lake during 2010 (Poganski, 2011; Schoenfuss and Poganski, 2011).
3

Methods

Statewide Survey

During 2008 and 2010, a statewide survey of 14 lakes representing a range of 

physiographic, geological, and land-use characteristics of Minnesota (fig. 1; table 1) was 

conducted to evaluate the occurrence of endocrine disrupting chemicals. The lakes covered a 

range of trophic status (oligotrophic to eutrophic) and anthropogenic inputs from agriculture and 

urban activities. Several sites were in remote locations with minimal development, including 

Northern Light Lake, Elk Lake, Beast Lake, Ryan Lake, and Bohall Lake. Between May 22 and 

August 3, 2008, water was collected during single sampling events from 11 lakes, starting in the 

southern part of the state and moving northward. Sediment samples from the same lakes were 

collected approximately one month later. Polar organic compound integrative samplers (POCIS; 

Alvarez and others, 2004) acquired from Environmental Sampling Technologies (St. Joseph, 

Missouri) were deployed during the summer of 2008 (at the time of water sampling) for 21 days 

at 11 of the lakes. During 2010, water samples were collected from three additional lakes and 

two of the lakes sampled in 2008 (Elk Lake and Sullivan Lake) were resampled. 

Grab samples from the water surface were collected using a pre-cleaned stainless steel 

bucket rinsed with lake water and processed following USGS sampling protocols (U.S. 

Geological Survey, variously dated). Samples were transported on ice to the USGS National 

Research Program Laboratory (NRPL) in Boulder, Colorado where they were stored at 4 degrees 

Celsius (°C) until analysis. Approximately 1 month after the water sampling, composite 

sediment samples were collected from the top 10 centimeters (cm) directly beneath the bed 

surface in close proximity to the sites where water and POCIS samples were collected. The 

sediment samples were stored frozen until analysis. The POCIS samplers were attached at a 

depth of 1 meter (m) to existing docks or to steel posts located approximately 5 m offshore. 

Upon retrieval, the POCIS samplers were placed in sealed cans and transported to the NRPL

where they were stored at 4°C until analysis. Water samplings and POCIS deployments were 

conducted at the same locations and during the same time periods as companion biological 

studies conducted by SCSU on endocrine disruption in wild-caught fish and caged fathead 

minnows (Ferrey and others, 2008).

Sullivan Lake Microhabitat Study

To provide a better understanding of the spatial and seasonal relationships between 

contaminant sources and processes occurring in the littoral zone, Sullivan Lake was selected for 

the detailed microhabitat study. Sullivan Lake has a relatively small watershed (3 square 

kilometers (km2)) with underlying glacial morphology that is characteristic of many Minnesota 

lakes. Sullivan Lake (fig. 2) is located near the town of St. Cloud in central Minnesota and is 

classified as meso-eutrophic (moderate biological productivity), has a surface area of 30 hectares 

(73 acres), and has a maximum depth of 16.5 m (Minnesota Department of Natural Resources, 

2010). The bottom substrate varies from sand to detritus, but primarily is muck and silt. 

Predominant land use in the Sullivan Lake watershed was 49 percent cropland, 11 percent 

deciduous forests, 8 percent developed (residential), 7 percent wetland, and other land-use 

classifications were 5 percent or less (fig. 2; Minnesota Department of Natural Resources, 2010). 

The lake may potentially be influenced by residential land use (septic systems), recreational 

activities such (boating and fishing), and agricultural runoff. 
4

The near-shore environment of Sullivan Lake was evaluated at four microhabitat sites

(fig. 2), including two residential influenced areas (sites A and B) with septic systems, a 

stormwater runoff and recreational activity influenced area (site C), and an agricultural (animal 

and crop) runoff influenced area (site D) with no residential land use. Site C contained a boat 

ramp used by lake residents and the general public. Much of the shoreline near site C was 

covered by thick emergent wetland vegetation, and the bottom sediments consisted of detritus 

and organic muck. In contrast, lawns extended to the shorelines of the residential/septic sites (A 

and B) and the near-shore bottom sediments were generally sandy with little or no emergent 

vegetation. Surface-water samples were collected at each microhabitat site in pre-cleaned and 

baked amber glass bottles in the same manner as described for the statewide lake survey and 

shipped to the NRPL, where they were stored at 4°C until analysis. Summer and fall samplings 

were conducted in order to evaluate seasonal variability. 

Microhabitat Groundwater/Surface-Water Interactions

The potential for groundwater/surface-water interactions was evaluated at the four 

microhabitat sites using near-shore transects for pore-water sampling (fig. 2) with ideal (site A) 

cross-section spacing of 1, 5, 10, and 15 m perpendicular from shore and 1, 3, and 5 m parallel to 

shore. At site B, dense emergent wetland vegetation prevented sampling at two of the sites 

closest to shore. Sites C and D had dense emergent wetland vegetation that generally limited 

sampling the near-shore environment: two locations (1 near the shore and the other 15 m 

offshore) were sampled at site C, and two transects were sampled at four locations at site D. 

Vertical hydraulic-head gradient measurements and pore-water samples were obtained 

using a hydraulic potentiomanometer (Rosenberry and LaBaugh, 2008) and a retractable well 

screen inserted to a depth of 30 cm below the sediment/water interface. A peristaltic pump was 

used to draw water from the surrounding sediments at a rate of less than 10 milliliters (mL) per 

minute (min) to minimize the hydrodynamic disturbance and avoid excessive degassing or 

inadvertent additions of lake water to the sample. A manometer was connected to the tubing 

from the well screen following collection of 60-mL pore-water samples (the pumping period 

needed to eliminate air bubbles from the system) and measurements of hydraulic-head 

differences were made at each location. Sediments at sites C were too fine for pulling water 

through the well screen and precluded measurements of hydraulic gradients. Groundwater flux 

also was determined at site A using the seepage-meter techniques described in Rosenberry and 

LaBaugh (2008). Two seepage meters were installed at different points along the shoreline and 

two measurements were made for each meter.

Field measurements (including determination of temperature and lake depth) were made 

at the time of each sample collection. Water-column, water/sediment interface, and pore-water 

temperature were determined using a rigid probe with a thermistor thermometer at the end. 

Temperature was recorded at the water/sediment interface (Twater/sediment) just above the bed 

surface and 30 cm below the water/sediment interface (T30 cm). In situ water-quality 

measurements (specific conductance, dissolved oxygen, and pH) were taken with a field probe at 

various depths in the water column along a 5-point transverse transect parallel to the shoreline 

(fig. 2) at each microhabitat site.

Chemical Analysis

Field measurements, including temperature, pH, specific conductance, and dissolved 

oxygen were made according to standard procedures (U.S. Geological Survey, variously dated). 
5

Dissolved (1-micrometer (μm) glass fiber filter) organic carbon was analyzed by platinum 

catalyzed persulfate/ultraviolet light oxidation with infrared detection (Barber and others, 2001; 

Weishaar and others, 2003). Linear alkylbenzene sulfonate (LAS) and alkylphenolethoxylates 

(AP) were analyzed in unfiltered water samples by enzyme-linked immunosorbent assay 

(ELISA) using standard methods (http://www.abraxiskits.com). Trace and major elements 

(table 2) were determined in 0.45-μm filtered water samples by inductively coupled plasma-mass 

spectrometry (Garbarino and Taylor, 1996; Taylor, 2001) and inductively coupled plasma-atomic 

emission spectrometry (Garbarino and Taylor, 1979). Because a stainless steel bucket was used 

in the collection of surface-water grab samples, there is the potential for the introduction of low 

concentrations of select trace metals and thus potential positive bias.

Unfiltered water samples were analyzed for organic constituents using three different 

analytical methods described in detail elsewhere (Barber and others, 2011). Acidic organic 

compounds (table 3) were evaporated to dryness (EVAP) and derivatized with 10 percent (v:v) 

acetyl chloride:propanol to form the propyl esters (Barber and others, 2000). Neutral organic 

compounds (table 4) were isolated using continuous liquid-liquid extraction (CLLE) with 

methylene chloride at pH 2 following ionic strength adjustment (Barber and others, 2000). 

Steroid and steroidal hormone compounds (table 5) were isolated by octadecyl silica solid-phase 

extraction (SPE) followed by elution with methanol, Florisil cleanup, and derivitization with Nmethyl-N-trimethylsilyltrifluoroacetamide (Barber and others, 2011; Foreman and others, 2012).

The CLLE and EVAP extracts were analyzed by electron impact gas 

chromatography/mass spectrometry (GC/MS) in both the full scan and selected ion monitoring 

(SIM) modes. The general chromatographic conditions were: Hewlett Packard (HP) 6890 GC; 

column - HP Ultra II (5 percent phenylmethyl silicone), 25 m × 0.2 millimeter (mm), 33-μm film 

thickness; carrier gas, ultra high purity helium with a linear-flow velocity of 27 cm per second 

(sec); injection port temperature, 300°C; initial oven temperature, 50°C; split vent open, 0.75 

min; ramp rate, 6°C/min to 300°C; hold time, 15 min at 300°C. The mass spectrometer 

conditions were: HP 5973 Mass Selective Detector; tune with perflurotributylamine; ionization 

energy, -70 eV; source pressure, 1×10-5 torr; source temperature, 250°C; interface temperature, 

280°C; full scan, 40 to 550 atomic mass units (amu) at 1 scan/sec. Concentrations were 

calculated based on SIM data using diagnostic ions for each compound, which was identified 

based on matching of retention times (plus or minus 0.05 min) and ion ratios (plus or minus 

20 percent) determined from analysis of authentic standards. External calibration curves and 

internal standard procedures were used for calculating concentrations.

Gas chromatography/tandem mass spectrometry (GC/MS/MS) analysis of the derivatized 

SPE samples was conducted using a Waters QuattroMicro QqQ GC/MS/MS with an Agilent 

6890 gas chromatograph. Chromatography was on a 30 m × 0.25 mm × 0.25 μm Restek RtxXLB capillary column at a He flow rate of 1 mL/min with the injection port maintained at 

275°C. The gas chromatograph was programmed on a variable temperature gradient from 100°C 

to 310°C. For each compound, the most abundant ion in the electron impact spectrum was 

selected as a precursor, and appropriate conditions were selected to maximize signal for three

precursor-product transitions per compound. Quantification was based on external calibration 

curves and internal standard procedure. 

Target compounds in sediment were isolated by accelerated solvent extraction (ASE) 

with isopropyl alcohol and cleaned up on a Florosil column (Burkhardt and others, 2005). The 

sediment extracts were analyzed by GC/MS as for CLLE, and then derivitized and analyzed by 

GC/MS/MS as for SPE. The OASISTM hydrophilic-lipophilic-balance SPE sequestration medium 
6

encased in the POCIS samplers was transferred into a glass column containing silanized glass 

wool and eluted with methanol. The methanol extracts were evaporated under nitrogen, 

augmented with dichloromethane:methanol (95:5 v:v), and cleaned up on Florosil column, 

followed by GC/MS analysis as for CLLE. The extract was then derivitized and analyzed by 

GC/MS/MS.

Quality Assurance

The quality-assurance program consisted of field duplicates, field samples spiked with 

target compounds, field blanks, distilled water spiked with target compounds, and distilled water 

blanks. Target compounds spiked into the distilled water and natural water matrices were

processed in the same manner as environmental samples and used to evaluate method recoveries. 

Recoveries for individual samples also were evaluated using surrogate standards spiked into each 

sample prior to isolation. No standard reference materials were available for the organic 

compounds evaluated in this study. For the EVAP and CLLE GC/MS, surrogate standards 

(tables 3 and 4) were added to the water samples prior to extraction and analysis and results are 

presented as percent recoveries. Target compound quantitation for the CLLE and EVAP GC/MS 

analysis used internal standards and multi-point calibration curves. Standards were obtained from 

Dr. Ehrenstorfer GmbH (Augsburg, Germany), Cambridge Isotope Laboratories (Cambridge, 

Massachusetts), Sigma-Aldrich (Milwaukee, Wisconsin), and Supelco (Bellefonte, 

Pennsylvania). Deuterated polynuclear aromatic hydrocarbon internal standards were added to 

the extracts prior to GC/MS analysis. The SPE GC/MS/MS analysis used 12 deuterated standards 

(table 5) added following sample collection and isotope dilution quantitation protocols (Foreman 

and others, 2012). The sediment and POCIS samples used the same surrogate standards and 

quantitation procedures as the CLLE and SPE methods. 

Method detection limits (MDLs) for water samples were defined as the concentration 

equivalent to three times the mean detection value in method blanks or five times the baseline, 

whichever was greater. For the sediments, MDLs were determined to be three times the mean 

detection value in method blanks, corrected for sediment mass extracted. For the POCIS 

samples, MDLs were set at three times the instrument detection values, corrected for number of 

POCIS extracted. Spike and recovery studies were not done for the POCIS samplers. 

Water-quality and Hydrological Data

Statewide Lake Survey

Results for the chemical analysis of water, sediment, and POCIS samples collected from 

11 lake sites during 2008 are presented in tables 6 to 14. Results for the four lake sites sampled 

during 2010 are presented in tables 15 to 18. 

The field measurement (table 6) results for the 2008 sampling indicate that the chemical 

characteristics differed broadly among the lakes, as would be expected considering they ranged 

from oligotrophic to eutrophic. For example, specific conductance ranged from 33 microsiemens 

per centimeter (μS/cm) in oligotrophic Northern Light Lake to 580 μS/cm eutrophic Cedar Lake. 

Trace element results (table 7) varied. Concentrations of boron, which typically is associated 

with WWTP effluents (Barber and others, 2011) were relatively constant and ranged from 7 μg/L 

in Kabetogama Lake (oligotrophic) to 33 μg/L in Budd Lake (eutrophic). 
7

Organic compounds commonly associated with endocrine disruption (see tables 3 to 5) 

were detected in the water, sediment, and POCIS samples collected during 2008 (tables 8 to 14).

Although only a fraction of the organic compounds measured in the water were detected and 

concentrations were typically at sub-microgram per liter (μg/L) levels, several compounds 

(including EDCs) had widespread occurrence. For example, ethylenediaminetetraacetic acid, 

4-nonylphenol, and estrone were detected in the water of multiple lakes at concentrations ranging 

from 0.05 to 0.39, 0.11 to 0.21, and 0.0006 to 0.0015 μg/L, respectively. Most of the compounds 

detected in the water also were detected in the sediments, but at much higher concentrations. 

Likewise, most compounds detected in the water also were detected in the POCIS samples.

Table 15 summarizes field measurement data for the four lakes sampled during 2010. 

Ryan Lake and Beast Lake had similar water temperature, specific conductance, dissolved 

oxygen, and pH values. Bohall Lake had lower water temperature (9.6°C) and higher dissolved 

oxygen (10.0 milligram per liter, mg/L) values. Elk Lake had the highest water temperature 

(11.8°C) and specific conductance (294 micro Siemens per centimeter, μS/cm) values, and the 

lowest dissolved oxygen (8.6 mg/L).

Table 16 summarized the acidic organic compounds detected in the lake water samples 

collected during 2010. Ethylenediaminetetraacetic acid (EDTA) was detected in Elk Lake 

(0.53 μg/L), Ryan Lake (0.40 μg/L), and Bohall Lake (0.06 μg/L), but nitrilotriacetic acid (NTA) 

and 4-nonylphenolethoxycarboxylates (4-NPEC) were not detected in any of the lakes. Surrogate 

standard recoveries ranged from 54 to 67 percent. Neutral organic compounds are summarized in 

table 17. Trace levels of 4-methylphenol; 2,6-di-tert-butyl-1,4-benzoquinone; and 2,6-di-tertbutyl-4-methylphenol were detected in several lakes. Surrogate standard recoveries ranged from 

less than 10 to 85 percent. Steroid and steroidal hormone compound data from lake samples 

collected during 2010 are summarized in table 18. Cholesterol, coprostanol, and estrone were 

detected in the lakes. Surrogate standard recoveries ranged from 37 to 115 percent. 

Sullivan Lake Microhabitat Study

Geohydrological Environment

Analyses of topographic maps, aerial photographs, and field surveys of Sullivan Lake 

were used to provide preliminary information on potential groundwater/surface-water

interactions (Winter, 1998). The landscape around Sullivan Lake is characterized by Pleistocene 

glacial deposits and appears to have been part of a larger lake (perhaps connecting to Maple 

Lake; fig. 2) that during glacial times was dammed up behind the 50-foot high, esker-like ridge 

along the eastern shoreline (fig. 3). The lake stage may have continued to rise until the lake 

eventually eroded through the ridge creating the narrow, deeply-incised canal-like outlet near the 

southeast corner of Sullivan Lake. The presence of wetlands adjacent to the north, northwest, and 

southwest shorelines indicates that hydraulically driven groundwater discharge likely is shifted

to the margins between the uplands and wetlands rather than occurring at the boundary between 

the wetlands and the open-water lake or could be controlled by lake level in topographically low 

areas. The predominant geologic feature, from the perspective of groundwater discharge into the 

lake, is the esker-like ridge along the eastern and southeastern shoreline. Higher groundwater 

head beneath the ridge creates a hydraulic gradient that increases the potential for groundwater 

discharge along the western shoreline, which coincides with the areas of maximum residential 

density and creates the greatest potential for onsite wastewater-disposal systems to discharge into 
8

the lake. Storm water and agricultural runoff along the western shoreline is potentially buffered 

by the wetlands, which may attenuate chemicals before they enter the lake.

Microhabitat Characterization

A preliminary shoreline site investigation was conducted during the microhabitat siteselection process and the results are presented in table 19. Based on these results and 

hydrological considerations, four sampling sites were selected. Microhabitat A (residential/septic

influence) had several hydraulic head values that were higher than the lake surface (positive 

values, table 20) and that ranged up to 15 mm. The hydraulic-head values were generally low 

near the shore and greatest at sample location (point 1, 3). The near-shore seepage-meter 

measurements indicated groundwater influx of -0.94 to 4.3 milliliters per minute per square 

meter (mL/min/m2). Dissolved organic carbon values in the pore water samples ranged from 2.1 

to 7.4 mg/L. Linear alkylbenzene sulfonate values in pore water samples ranged from less than 

0.02 to 0.92 mg/L. There was only a single AP detection (0.14 mg/L). T30 cm measurements were 

generally lower than Twater/sediment values. Water-quality measurements were taken within the 

water column in microhabitat A (table 21). Water temperature, specific conductance, and pH 

were generally constant with depth with the exception of the 15, 5 point. Dissolved oxygen 

values were either constant within the water column or decreased with depth. 

Microhabitat B (residential/septic influence) had several hydraulic-head values that were 

slightly lower than the lake surface (negative values, table 22), suggesting the potential for flow 

from the lake to groundwater at this location. Dissolved organic carbon values in the pore-water 

samples from microhabitat B (7.6 to 11.4 mg/L) were greater than microhabitat A. The LAS

values ranged from less than 0.02 to 0.12 mg/L, and there were sporadic detections of AP (up to 

0.11 mg/L). No T30 cm or Twater/sediment measurements were recorded in microhabitat B. The watercolumn temperature, specific conductance, dissolved oxygen, and pH were relatively constant at 

microhabitat B (table 23).

Dense emergent vegetation limited access to sampling locations in microhabitat C 

(stormwater/boat ramp influence). Dissolved organic carbon values of pore-water samples 

ranged from 7.3 to 11.2 mg/L (table 24). Low levels of LAS (0.03 mg/L) and AP (0.11 mg/L) 

were detected in pore-water samples. The T30 cm temperatures (17.7 to 19.4°C) were lower than 

the Twater/sediment temperatures (23.7 to 28.6°C). A thick layer of organic muck at the 

water/sediment interface prevented hydraulic head measurements. Measurements taken within 

the water column in microhabitat C indicated that water temperature and specific conductance 

were relatively constant (table 25). Dissolved oxygen concentrations decreased with depth in the 

water column and near-bottom values were as much as 43 percent lower than near-surface 

values. The 3, 5 point was an exception where dissolved oxygen and pH were fairly constant 

with depth. 

Dense emergent vegetation and deep water limited sampling in microhabitat D 

(agricultural influence). A thick layer of organic muck near the water/sediment interface limited 

hydraulic head measurements (table 26). Linear alkylbenzene sulfonates were detected at 

concentrations ranging from 0.02 to 0.11 mg/L, and no AP were detected. Values for T30 cm 

(16.7 to 18.8°C) were lower than Twater/sediment (19.9 to 23.8°C). Measurements taken within the 

water column at microhabitat D (table 27) indicated that temperature was relatively constant and

dissolved oxygen and pH decreased with depth (with the exception of 0, 5 where they remained 

relatively constant). Specific conductance values did not follow the same trends. 
9

Temporal Sampling

Acidic organic compounds detected in the summer 2010 Sullivan Lake microhabitat 

sampling are listed in table 28. Ethylenediaminetetraacetic acid, nitrilotriacetic acid, and 

4-nonylphenolmonoethoxycarboxylic acid were detected at all of the microhabitat sites. 

Surrogate standard recoveries ranged from 66 to 98 percent. Acidic organic compounds detected 

in the fall 2010 sampling are listed in table 29. Ethylenediaminetetraacetic acid was present in all 

microhabitats, and microhabitat A (residential/septic influence) had the only detection of 

nitrilotriacetic acid and 4-nonylphenoldiethoxycarboxylic acid. Surrogate standard recoveries 

ranged from 46 to 70 percent.

Neutral organic compounds detected in the summer 2010 Sullivan Lake microhabitat 

sampling are listed in table 30. Several compounds were detected at multiple sites, including 

bisphenol A; 2,6-di-tert-butyl-1,4-benzoquinone; 2,6-di-tert-butyl-4-methylphenol; N,N-diethylmeta-toluamide; 4-methylphenol; and 4-nonylphenol. Microhabitat A had the highest levels of 

N,N-diethyl-m-toluamide and 4-nonylphenol, and had the only caffeine detection among the four 

sites. Surrogate standard recoveries ranged from 29 to 99 percent, and matrix spike recoveries 

ranged from less than 10 to 163 percent. Neutral organic compounds detected in the fall 2010 

sampling are listed in table 31. Sites A and B had detections of bisphenol A; 2,6-di-tert-butyl1,4-benzoquinone; 2,6-di-tert-butyl-4-methylphenol; N,N-diethyl-meta-toluamide; and 

4-nonylphenol. 4-tert-Octylphenol and caffeine also were detected at sites A and B. Surrogate 

recoveries ranged from 19 to 57 percent. 

Steroid and steroidal hormone analysis for the summer 2010 Sullivan Lake microhabitat 

sampling are listed in table 32. Cholesterol, coprostanol, and estrone were detected at all 

microhabitat sites and 4-androstene-3,17-dione was detected at all sites except microhabitat A. 

Surrogate standard recoveries ranged from less than 10 to 183 percent, and matrix spike 

recoveries (excluding cholesterol, which had such high background concentrations it was 

difficult to calculate recoveries) ranged from 15 to 235 percent. Table 33 lists steroid and 

steroidal hormone analysis of surface-water samples from each microhabitat site collected in the 

fall of 2010. Cholesterol and coprostanol were detected at all sites, and a single detection of 

estrone occurred in microhabitat D. Surrogate standard recoveries ranged from 15 to 121 percent.

Conclusions

This report presents the results from field measurements and laboratory analysis for 

water, sediment, and POCIS samples collected from 14 Minnesota lakes during 2008 and 2010. 

These data provide a snapshot of the occurrence of a variety of potential endocrine-disrupting 

compounds in the near shore environment of 14 geographically distributed Minnesota lakes 

covering a range of land use and trophic status. One of the lakes, Sullivan Lake, was studied in 

detail to assess potential contaminant sources and evaluate the spatial and seasonal relationships.

Acknowledgments

The field assistance of Harold Wiegner (Minnesota Pollution Control Agency) is greatly 

appreciated. We also thank the homeowners on Sullivan Lake for access to their properties. This 

study was supported by the U.S. Geological Survey’s National Research Program and Toxics 

Substances Hydrology Program. 
10

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14

Figure 1. Site locations for the 14 Minnesota lakes sampled during 2008 and 2010 (after Writer and 

others, 2010).
15

Figure 2. Site locations for the four littoral-zone microhabitats investigated at Sullivan Lake, Minn.

Numbers in parentheses (indicate microhabitat groundwater/surface water sampling locations in meters 

parallel (x) and perpendicular (y) to the shoreline.
16

Figure 3. Site topography and preliminary hydraulic analysis of potential zones of groundwater discharge 

in Sullivan Lake, Minn.
Table 1. Site characteristics for the 14 Minnesota lakes that were sampled in this investigation.—Continued

[DOW, Division of Wildlife; km2, square kilometer; m, meter; m3, cubic meter; μg/L, microgram per liter; km, kilometer; n/a, not applicable; Eu; eutrophic; Meso, mesotrophic; polar organic compound integrated samplers; --, not available; Date format: M/DD/YY ]

Unit Owasso Cedar Budd Red Sand Sullivan White Sand Kabetogama Shingobee Stewart Northern Light Elk Bea

Latitude 45.0313 44.9562 43.6397 46.3810 45.2200 46.3599 48.4442 46.9994 47.1825 47.9081 47.1965 4Longitude -93.1300 -93.3254 -94.4744 -94.2861 -93.9423 -94.2874 -93.0284 -94.6874 -91.7547 -90.2521 -95.2216 -9Lake DOW 

number 62005600 27003900 46003000 18038600 86011900 18037900 69084500 29004300 38074400 16008900 15001000 690837

County Ramsey Hennepin Martin Crow Wing Wright Crow Wing St. Louis Hubbard Lake Cook Clearwater St. L

Hydrologic 

class Headwater Drainage Drainage Drainage Headwater Headwater Riverine Drainage Drainage Riverine Drainage n/

Watershed

area

km2 12 10 107 18 3 5 717 42 5 478 35 n/

Lake surface 

area

km2 1.64 .72 .94 2.17 .31 1.81 104 .75 1.03 1.97 1.33 

Maximum 

depth m 11.3 15.5 5.18 7 16.5 7.9 23.8 11 6.1 2.3 28.4 2

Lake volume m3 5.0E+06 4.0E+06 3.1E+06 2.3E+06 1.3E+06 5.0E+06 7.3E+08 4.0E+06 1.9E+06 2.3E+06 1.3E+07 n/

Volume/

watershed area

 .410 .395 .029 .125 .420 .983 1.023 .096 .388 .005 .364 n/

Shoreline m 9.1E+03 4.9E+03 3.6E+03 6.1E+03 2.7E+03 5.4E+03 1.8E+05 4.9E+03 5.1E+03 -- -- n/

Trophic index Eu Eu Eu Eu Eu Meso Meso Meso Meso Oligo Oligo OliTotal

phosphorous μg/L 39 24 89 26 48 21 15 31 14 13 11 2

Septic

systems number 0 0 0 68 42 138 100 3 3 0 0 

Docks and 

marinas number 164 5 80 32 6 85 242 1 13 0 1 

Shoreline

septicdensity 

per/km .0 .0 .0 11.2 15.4 25.6 .6 .6 .6 .0 .0 

Shoreline 

dock density per/km 18.1 1.0 22.3 5.2 2.2 15.8 1.4 .2 2.6 .0 .2 

Total length 

of streams km 2,508.9 112.2 48,797.0 1,953.3 15.3 .0 391,614.1 6,907.3 24.2 227,398.2 5,010.6 n/

Total length 

of roads km 94,722.2 95,536.9 163,712.4 54,841.7 6,841.4 23,179.0 97,550.2 48,231.9 400.4 92,969.5 6,283.6 n/

Total

population persons 13,227.0 13,329.7 5,805.3 2,162.2 168.9 1,345.3 264.3 391.4 1.5 51.5 2.0 n/

Population 

density person/km2 1,078.2 1,327.9 54.3 117.4 55.1 264.6 .4 9.3 .3 .1 .1 n/

Road density km/km2 7.7 9.5 1.5 3.0 2.2 4.6 .1 1.1 .1 .2 .2 Stream 

density km/km2 .205 .011 .457 .106 .005 .000 .546 .164 .005 .476 .141 n/

Developed 

cover percent 73 80 10 10 8 19 0 4 0 0 1 n/

Deciduous 

cover percent 9 8 0 45 11 24 54 45 38 24 60 n/

Evergreen/

mixed cover percent 2 1 n/a 1 1 0 16 21 38 57 26 n/

17
Table 1. Site characteristics for the 14 Minnesota lakes that were sampled in this investigation.—Continued

[DOW, Division of Wildlife; km2, square kilometer; m, meter; m3, cubic meter; μg/L, microgram per liter; km, kilometer; n/a, not applicable; Eu; eutrophic; Meso, mesotrophic; polar organic compound integrated samplers; --, not available; Date format: M/DD/YY ]

Unit Owasso Cedar Budd Red Sand Sullivan White Sand Kabetogama Shingobee Stewart Northern Light Elk Bea

Grassland 

cover percent 0 0 4 4 11 2 2 18 0 0 0 n/

Cropland 

cover percent n/a n/a 76 2 49 2 0 2 n/a n/a 0 n/

Wetland cover percent 3 2 2 14 7 18 10 2 1 4 1 n/Open water 

cover percent 14 7 6 22 8 34 14 6 21 12 12 n/

Barren cover percent n/a n/a 0 n/a n/a n/a 0 n/a n/a 0 n/a n/

Shrubland 

cover percent n/a 0 n/a 1 5 n/a 3 2 1 3 0 n/

POCIS

deployment date 5/23/08 5/23/08 5/27/08 6/18/08 6/19/08 6/18/08 8/21/08 7/15/08 7/14/08 8/4/08 6/18/08 n/

Water

sampling date 6/2/08 6/2/08 6/3/08 6/27/08 6/29/08 6/27/08 7/3/08 7/15/08 7/14/08 8/4/08 6/27/08 10/19

18
Table 2. Trace elements and major elements measured by inductively coupled plasma/mass spectrometry 

(Garbarino and Taylor, 1996; Taylor, 2001) and inductively coupled plasma/atomic-emission spectrometry 

(Garbarino and Taylor, 1979) at the U.S. Geological Survey National Research Program Laboratory, and the 

trace and major elements’ approximate method detection limits (MDL).

[atomic symbols shown in parenthesis; μg/L, microgram per liter; mg/L, milligram per liter]

Element MDL (μg/L) Element MDL (μg/L)

Aluminum (Al) 0.05 Manganese (Mn) 0.02

Antimony (Sb) .02 Molybdenum (Mo) .03

Arsenic (As) .04 Neodymium (Nd) .003

Barium (Ba) .01 Nickel (Ni) .02

Beryllium (Be) .02 Potassium (K) .02 mg/L

Bismuth (Bi) .01 Praseodymium (Pr) .005

Boron (B) 4 Rhenium (Re) .001

Cadmium (Cd) .006 Rubidium (Rb) .002

Calcium (Ca) .02 mg/L Samarium (Sm) .003

Cerium (Ce) .001 Selenium (Se) .2

Cesium (Cs) .06 Silica (SiO2) .1 mg/L

Chromium (Cr) .2 Sodium (Na) .02 mg/L

Cobalt (Co) .01 Strontium (Sr) .02

Copper (Cu) .02 Sulfur (S) .002 mg/L

Dysprosium (Dy) .002 Tellurium (Te) .01

Erbium (Er) .002 Terbium (Tb) .0003

Europium (Eu) .001 Thallium (Tl) .005

Gadolinium (Gd) .003 Thorium (Th) .004

Holmium (Ho) .0005 Thulium (Tm) .0005

Iron (Fe) .7 Tungsten (W) .004

Lanthanum (La) .0005 Uranium (U) .002

Lead (Pb) .006 Vanadium (V) .05

Lithium (Li) .1 Ytterbium (Yb) .0014

Lutetium (Lu) .0005 Yttrium (Y) .0004

Magnesium (Mg) .002 mg/L Zinc (Zn) .08

Zirconium (Zr) .01

19
Table 3. Acidic organic compounds measured by evaporation with derivatization and gas 

chromatography/mass spectrometry (Barber and others, 2000) at the U.S. Geological Survey National 

Research Program Laboratory.

[This report contains CAS Registry Numbers® (CASRN), which is a Registered Trademark of the American Chemical 

Society. CAS recommends the verification of the CASRNs through CAS Client ServicesSM; MDL, method detection 

limit; μg/L, microgram per liter; NA, not available; *, potential endocrine-disrupting compound]

Compound CASRN MDL (μg/L)

Ethylenediaminetetraacetic acid 60-00-4 0.05

Nitrilotriacetic acid 139-13-9 .05

4-Nonylphenolmonoethoxycarboxylic acid* NA .1

4-Nonylphenoldiethoxycarboxylic acid* 106807-78-7 .1

4-Nonylphenoltriethoxycarboxylic acid* NA .1

4-Nonylphenoltetraethoxycarboxylic acid* NA .1

Surrogate Standard

4-normal-Nonylphenoldiethoxycarboxylate NA NA

20
Table 4. Neutral organic compounds measured by continuous liquid-liquid extraction using methylene 

chloride with gas chromatography/mass spectrometry (Barber and others, 2000) at the U.S. Geological 

Survey National Research Program Laboratory.

[This report contains CAS Registry Numbers® (CASRN), which is a Registered Trademark of the American Chemical 

Society. CAS recommends the verification of the CASRNs through CAS Client ServicesSM; MDL, method detection 

limit; μg/L, microgram per liter; NA, not available; *, potential endocrine-disrupting compound]

Compound CASRN MDL (μg/L)

Bisphenol A* 80-05-7 0.01

2[3]-tert-Butyl-4-methylphenol 25013-16-5 .01

4-tert-Butylphenol 98-54-4 .01

Caffeine 58-08-2 .01

2,6-Di-tert-butyl-1,4-benzoquinone 719-22-2 .01

2,6-Di-tert-butyl-4-methylphenol 128-37-0 .01

2,6-Di-tert-butylphenol 128-39-2 .01

1,2-Dichlorobenzene 95-50-1 .01

1,3-Dichlorobenzene 541-73-1 .01

1,4-Dichlorobenzene* 106-46-7 .01

N,N-Diethyl-meta-toluamide 134-62-3 .01

4-Ethylphenol 123-07-9 .01

5-Methyl-1H-benzotriazole 136-85-6 .01

4-Methylphenol 106-44-5 .01

4-Nonylphenol * 25154-52-3 .05

4-Nonylphenolmonoethoxylate* 9016-45-9 .05

4-Nonylphenoldiethoxylate* NA .05

4-Nonylphenoltriethoxylate* NA .05

4-Nonylphenoltetraethoxylate* NA .05

4-normal-Octylphenol* 1806-26-4 .01

4-tert-Octylphenol* 140-66-9 .01

4-tert-Octylphenolmonoethoxylate* 9036-19-5 .01

4-tert-Octylphenoldiethoxylate* NA .01

4-tert-Octylphenoltriethoxylate* NA .01

4-tert-Octylphenoltetraethoxylate* NA .01

4-tert-Octylphenolpentaethoxylate* NA .01

4-tert-Pentylphenol* 80-46-6 .01

4-Propylphenol 645-56-7 .01

Triclosan 3380-34-5 .01

Surrogate Standards

d6 Bisphenol A 86588-58-1 NA

d21 2,6-Di-tert-butyl-4-methylphenol 64502-99-4 NA

4-normal-Nonylphenol 104-40-5 NA

4-normal-Nonylphenolmonoethoxylate NA NA

4-normal-Nonylphenoldiethoxylate NA NA

21
Figure 5. Steroid and steroidal hormone compounds measured by octadecylsilica solid-phase 

extraction with derivatization and gas chromatography/tandem mass spectrometry (Barber and others, 

2003; Foreman and others, 2012) at the U.S. Geological Survey National Research Program Laboratory.

[This report contains CAS Registry Numbers® (CASRN), which is a Registered Trademark of the American Chemical 

Society. CAS recommends the verification of the CASRNs through CAS Client ServicesSM; MDL, method detection 

limit; μg/L, microgram per liter; *, potential endocrine-disrupting compound; NA, not available; --, not applicable]

Compound CASRN MDL (μg/L)

4-Androstene-3,17-dione 63-05-8 0.0001

cis-Androsterone 53-41-8 .0001

Cholesterol 57-88-5 .005

Coprostanol 360-68-9 .005

Diethylstilbesterol* 56-53-1 .0001

Equilenin* 517-09-9 .0001

Equilin* 474-86-2 .0001

17α-Estradiol* 57-91-0 .0001

17β-Estradiol* 50-28-2 .0001

Estriol* 50-27-1 .0001

Estrone* 53-16-7 .0001

17α-Ethinylestradiol* 57-63-6 .0001

Mestranol* 72-33-3 .0001

19-Norethisterone* 68-22-4 .0001

Progesterone 57-83-0 .0001

Testosterone 58-22-0 .0001

dihydro-Testosterone 521-18-6 .0001

epi-Testosterone 481-30-1 .0001

11-keto-Testosterone 53187-98-7 .0001

Surrogate Standards

d7-Androstenedione 67034-85-9 --

d7-Cholesterol 83199-47-7 --

d12-Chrysene 1719-03-5 --

d4-Dihydrotestosterone NA --

d4-17α-Ethinylestradiol NA --

d4-17β-Estradiol 66789-03-5 --

d3-Estriol 79037-36-8 --

d4-Estrone 53866-34-5 --

d4-Mestranol NA --

d6-Norethindrone NA --

d9-Progesterone 15775-74-3 --

d5-Testosterone 21002-80-2 --

22
Table 6. Summary of field measurements made at 11 Minnesota lakes during 2008.

[Date format: M/DD. μS/cm, microsiemen per centimeter, mg/L, milligram per liter; mg/L, std Unit, standard unit, mV, millivolts; NM, not measured]

Waterbody Date Water temp

°C

Specific

conductivity

μS/cm

Total

dissolved

solids

mg/L

Salinity

per

thousands

Dissolved

oxygen

percent

Dissolved

oxygen

mg/L

pH

std unit

Oxidation

reduction

potential

mV

Cedar 5/23 18.1 580 430 0.33 120 11 8.2 140

Cedar 6/2 19.9 550 400 .3 140 13 8.5 150

Cedar 6/13 20.1 490 350 .26 100 9.5 7.5 140

Cedar 7/10 25.4 540 350 .26 83 6.6 8.8 130

Owasso Lake 5/23 16.6 330 260 .19 NM 10 7.6 150

Owasso Lake 6/2 20.0 330 280 .18 140 12 8.2 150

Owasso Lake 6/13 19.9 300 220 .16 89 8.1 7.3 140

Budd Lake 5/22 16.2 430 340 .25 96 9.4 10 120

Budd Lake 6/3 18.8 490 360 .27 NM 9.0 8.3 160

Budd Lake 6/12 20.5 420 300 .22 94 8.4 9.3 140

White Sand 7/9 26.2 140 86 .06 95 7.6 7.9 110

Red Sand Lake 6/18 24.1 53 37 .03 120 10 2.5 240

Red Sand Lake 7/9 26.9 170 100 .07 100 8.3 8.1 120

Sullivan Lake 6/18 21.8 89 60 .05 92 7.9 2.2 260

Elk Lake 6/18 18.2 220 160 .12 120 11 7.8 120

Elk Lake 7/9 21.8 250 180 .13 93 8.1 7.7 130

Stewart Lake 7/14 20.3 48 35 .02 96 8.5 7.8 68

Shingobee Lake 7/14 21.1 280 200 .14 85 7.6 7.6 140

Lake Kabetogama 7/2 18.6 67 50 .03 97 9.1 1.2 280

Northern Light Lake 8/3 21.8 33 25 .02 91 8.0 NM 110

23
Table 7. Summary of major- and trace-element data for water samples collected from 11 Minnesota lakes during 2008.

[mg/L, milligram per liter; μg/L, microgram per liter; <, less than]

Constituent Unit Owasso Cedar Budd Sullivan Red Sand Shingobee White Sand Stewart Kabetogam

Aluminum μg/L 16 7.7 8.2 2.3 3.3 0.3 1.0 7.0 10 

Antimony μg/L .39 .23 .22 .074 .033 .015 .042 .039 .048 

Arsenic μg/L 11 1.9 1.2 1.3 .93 .71 .63 .45 .38 

Barium μg/L 38 38 55 34 28 59 36 10 12 

Beryllium μg/L .008 .006 <.005 <.005 .006 <.005 <.005 .005 .008 Bismuth μg/L <.006 <.006 <.006 <.006 <.006 <.006 <.006 <.006 <.006 

Boron μg/L 22 20 33 26 16 26 16 14 7 

Cadmium μg/L .055 .038 .015 <.002 .007 .009 .004 .011 .010 

Cesium μg/L .05 .04 .03 .03 .03 .02 .04 .01 .04 

Calcium mg/L 25 36 57 38 15 46 25 14 11 

Cerium μg/L .021 .011 .015 .0036 .0091 .0039 .0098 .018 .055 

Chromium μg/L <1 <1 <1 <1 <1 <1 <1 <1 <1 

Cobalt μg/L .036 .051 .050 .032 .029 .0031 .016 .014 .048 

Copper μg/L 2.4 .81 2.5 .25 .37 .50 1.5 .93 .90 

Dysprosium μg/L .0024 .0017 .0025 .0007 .0014 .0003 .0008 .0037 .0057 

Erbium μg/L .0016 .0006 .0021 .0003 .0007 <.0001 .0007 .0019 .0037 

Europium μg/L .0013 .0009 <.0001 .0008 .0008 .0004 .0011 .0007 .0022 

Gadolinium μg/L .0024 .0011 .0029 .0012 .0009 .0006 .0012 .0034 .0084 

Holmium μg/L .0004 .0003 .0004 .0002 .0003 .0001 .0002 .0006 .0014 

Iron μg/L 30 7 11 9 204 <2 112 33 23 

Lanthanum μg/L .018 .0083 .0097 .0037 .0071 .0030 .0069 .014 .056 

Lead μg/L .60 .33 .20 .17 .12 .05 .07 .06 .12 

Lithium μg/L 2.3 12 18 13 1.1 4.0 .85 1.0 1.1 

Lutetium μg/L .0002 .0002 .0004 .0001 .0004 .0000 .0003 .0003 .0004 

Magnesium mg/L 6.0 9.6 28 19 5.4 16 6.1 4.5 3.9 

Manganese μg/L 2.8 5.3 7.0 1.1 4.8 .26 1.0 1.1 2.1 

Molybdenum μg/L 0.63 0.91 2.6 0.43 0.04 0.38 0.08 0.20 0.18 

Neodymium μg/L .018 .0069 .0097 .0020 .0051 .0021 .0050 .014 .045 

Nickel μg/L 1.1 1.0 1.5 1.1 .37 .90 .60 .48 .70 

Potassium mg/L 3.6 2.9 2.3 4.0 .51 1.5 .40 .52 .89 

Praseodymium μg/L .0039 .0027 .0021 .0005 .0012 .0008 .0014 .0036 .011 

24
Beryllium μg/L .008 .006 <.005 <.005 .006 <.005 <.005 .005 .008 

Rhenium μg/L .002 .003 .040 .012 .001 .001 .001 .002 .001 

Rubidium μg/L 2.0 2.2 .89 2.4 .98 .98 .53 .55 1.2 

Samarium μg/L .0039 .0021 .0025 .0005 .0014 .0006 .0012 .0033 .0085 

Selenium μg/L .4 .2 1.4 .2 .2 <.1 .1 .1 <.1 

Silica dioxide mg/L .10 .22 6.2 4.4 2.9 13 1.8 3.9 4.1 

Sodium mg/L 30 64 6.5 7.9 8.0 4.9 7.5 1.8 1.6 

Strontium μg/L 42 59 202 106 37 82 46 35 24 

Sulfur mg/L 1.7 4.3 14 2.5 .46 1.6 .48 1.1 1.4 

Tellerium μg/L <.007 <.007 .009 <.007 .007 <.007 <.007 <.007 <.007 Terbium μg/L .0005 .0003 .0003 .0001 .0002 .0001 .0001 .0004 .0011 

Thallium μg/L .0044 .0038 .0066 .0031 .0031 .0010 .0040 .0023 .012 

Thorium μg/L <.02 <.02 <.02 <.02 <.02 <.02 <.02 <.02 <.02 

Thulium μg/L .0002 .0001 .0003 .0001 .0001 .0001 .0001 .0005 .0004 

Tin μg/L .046 .013 .009 <.008 <.008 <.008 <.008 <.008 <.008 

Tungsten μg/L .0061 .047 .012 .0023 .0047 .0021 <.001 .0018 .0093 

Uranium μg/L .091 .34 8.9 .56 .011 .13 .018 .037 .060 

Vanadium μg/L .47 .4 1.6 .16 .13 <.1 <.1 .19 .30 

Ytterbium μg/L .0011 .0009 .0018 .0006 .0008 <.0003 .0011 .0018 .0043 

Yttrium μg/L .015 .0091 .020 .0048 .0072 .0031 .0066 .026 .041 

Zinc μg/L 5.9 11 3.4 1.7 1.7 .92 1.3 7.9 11 

Zirconium μg/L .05 .03 .13 .04 .02 .06 .04 .03 .06 

Table 7. Summary of major- and trace-element data for water samples collected from 11 Minnesota lakes during 2008.—Continued[mg/L, milligram per liter; μg/L, microgram per liter; <, less than]

Constituent Unit Owasso Cedar Budd Sullivan Red Sand Shingobee White Sand Stewart Kabetogam

25
Table 8. Summary of acidic organic compound data for water samples collected from 11 Minnesota lakes during 2008. 

[μg/L, microgram per liter; <, less than; Dup, duplicate sample]

Compound Owasso μg/L Cedar μg/L Budd μg/L Budd Dup μg/L Sullivan μg/L Red Sand μg/L Shingobee μg/L White Sand μg/L Stewart μg/L Kabeto

μg/

Ethylenediaminetetraacetic acid 0.35 0.19 0.12 0.14 0.39 0.21 0.11 0.11 0.05 0.06 

Nitrilotriacetic acid <.05 .07 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 

4-Nonylphenolmonoethoxycarboxylic acid <.1 .27 <.1 <.1 <.1 <.1 .18 <.1 <.1 <.1 

4-Nonylphenoldiethoxycarboxylic acid <.1 .14 <.1 <.1 <.1 <.1 <.1 <.1 <.1 <.1 

4-Nonylphenoltriethoxycarboxylic acid <.1 <.1 <.1 <.1 <.1 <.1 <.1 <.1 <.1 <.1 

4-Nonylphenoltetraethoxycarboxylic acid <.1 <.1 <.1 <.1 <.1 <.1 <.1 <.1 <.1 <.1 

Surrogate Recovery (percent)

4-normal-Nonylphenoldiethoxycarboxylic acid 44 49 36 30 32 39 39 38 40 38 

Table 9. Summary of neutral organic compound data for water samples collected from 11 Minnesota lakes during 2008.—Continued[avg, average; μg/L, microgram per liter; <, less than; Dup, duplicate sample; MS, matrix spike recovery in percent]

Compound Owasso μg/L Cedar μg/L Budd μg/L Sullivan μg/L Red Sand (avg) μg/L Shingobee μg/L White Sand μg/L Stewart μg/L Kabetogam

(avg) μg/L 

Bisphenol A 0.03 <0.01 0.04 <0.01 <0.01 0.02 <0.01 0.02 <0.01 

2[3]-tert-Butyl-4-methylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 4-tert-Butylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 Caffeine .13 .09 .02 <.01 <.01 .01 <.01 .01 <.01 1,2-Dichlorobenzene <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 1,3-Dichlorobenzene <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 1,4-Dichlorobenzene <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 2,6-Di-tert-butyl-1,4-benzoquinone <.01 .14 <.01 .08 .08 <.01 .09 <.01 <.01 2,6-Di-tert-butyl-4-methylphenol .07 .07 .07 <.01 .02 <.01 .02 <.01 <.01 2,6-Di-tert-butylphenol <.01 <.01 .18 <.01 <.01 <.01 <.01 <.01 <.01 

N,N-Diethyl-meta-toluamide .09 .05 .03 .03 .01 .58 .03 .05 .02 

4-Ethylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

5-Methyl-1H-benzotriazole <.01 .04 .01 <.01 <.01 <.01 <.01 <.01 <.01 

4-Methylphenol .03 .02 <.01 .02 .02 .01 .02 .02 .02 

26
Table 9. Summary of neutral organic compound data for water samples collected from 11 Minnesota lakes during 2008.—Continued

[avg, average; μg/L, microgram per liter; <, less than; Dup, duplicate sample; MS, matrix spike recovery in percent]

Compound Owasso μg/L Cedar μg/L Budd μg/L Sullivan μg/L Red Sand (avg) μg/L Shingobee μg/L White Sand μg/L Stewart μg/L Kabetogam

(avg) μg/L 

4-Nonylphenol <.05 <.05 <.05 <.05 <.05 .11 <.05 <.05 <.05 

4-Nonylphenolmonoethoxylate <.05 <.05 .06 <.05 <.05 .09 <.05 <.05 <.05 

4-Nonylphenoldiethoxylate <.05 <.05 <.05 <.05 <.05 .17 <.05 <.05 <.05 

4-Nonylphenoltriethoxylate <.05 <.05 <.05 <.05 <.05 .12 <.05 <.05 <.05 4-Nonylphenoltetraethoxylate <.05 <.05 <.05 <.05 <.05 .03 <.05 <.05 <.05 4-normal-Octylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 4-tert-Octylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

4-tert-Octylphenolmonoethoxylate <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 4-tert-Octylphenoldiethoxylate <.01 <.01 .03 <.01 <.01 .03 <.01 <.01 <.01 

4-tert-Octylphenoltriethoxylate <.01 <.01 <.01 <.01 <.01 .01 <.01 <.01 <.01 4-tert-Octylphenoltetraethoxylate <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

4-tert-Octylphenolpentaethoxylate <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

4-tert-Pentylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

4-Propylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

Triclosan <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

Surrogate Recovery (percent)d6-Bisphenol A 67 60 63 43 44 65 63 77 63 d21-2,6-Di-tert-butyl-4-

methylphenol 27 24 7 10 26 36 25 42 40 

4-normal-Nonylphenol 43 30 38 32 34 42 32 49 50 4-normalNonylphenolmonoethoxylate 22 17 24 28 21 36 20 31 34 4-normal-Nonylphenoldiethoxylate 17 13 22 21 17 24 14 14 22 

27
Duplicates, Blanks, and Matrix Spikes

Table 9. Summary of neutral organic compound data for water samples collected from 11 Minnesota lakes during 2008.—Continued[avg, average; μg/L, microgram per liter; <, less than; Dup, duplicate sample; MS, matrix spike recovery in percent]

Compound

Red

Sand

μg/L

Red

Sand

Dup

μg/L

Elk

μg/L

Elk Dup

μg/L

Kabetogama

μg/L

Kabetogama

Dup

μg/L

Northern 

Light

μg/L

Northern 

Light

Dup

μg/L

Distilled 

Water 

Blank

μg/L

Distilled 

Water 

Blank

μg/L

Bisphenol A <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 0.01 0.01 <0.01 <0.01 2[3]-tert-Butyl-4-methylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 4-tert-Butylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 Caffeine <.01 <.01 .01 <.01 <.01 <.01 .03 .01 <.01 .02 1,2-Dichlorobenzene <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 1,3-Dichlorobenzene <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 1,4-Dichlorobenzene <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 2,6-Di-tert-butyl-1,4-benzoquinone .08 <.01 .15 <.01 <.01 <.01 <.01 <.01 .07 <.01 2,6-Di-tert-butyl-4-methylphenol .01 .02 .02 .01 <.01 <.01 .02 <.01 .01 <.01 

2,6-Di-tert-butylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

N,N-Diethyl-meta-toluamide .01 .01 .27 .17 .02 .02 .07 .03 <.01 .08 

4-Ethylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

5-Methyl-1H-benzotriazole <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

4-Methylphenol .01 .02 .01 .02 .01 .03 .05 .03 <.01 <.01 4-Nonylphenol <.05 <.05 <.05 <.05 <.05 <.05 .28 .15 <.05 <.05 4-Nonylphenolmonoethoxylate <.05 <.05 <.05 <.05 <.05 <.05 .17 <.05 <.05 <.05 

4-Nonylphenoldiethoxylate <.05 <.05 <.05 <.05 <.05 <.05 <.05 .13 <.05 <.05 4-Nonylphenoltriethoxylate <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 

4-Nonylphenoltetraethoxylate <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 

4-normal-Octylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

4-tert-Octylphenol <.01 <.01 <.01 <.01 <.01 <.01 .01 <.01 <.01 <.01 4-tert-Octylphenolmonoethoxylate <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

4-tert-Octylphenoldiethoxylate <.01 <.01 <.01 <.01 <.01 <.01 .04 .04 <.01 <.01 4-tert-Octylphenoltriethoxylate <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

4-tert-Octylphenoltetraethoxylate <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

4-tert-Octylphenolpentaethoxylate <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

4-tert-Pentylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 

28
Table 9. Summary of neutral organic compound data for water samples collected from 11 Minnesota lakes during 2008.—Continued

[avg, average; μg/L, microgram per liter; <, less than; Dup, duplicate sample; MS, matrix spike recovery in percent]

Compound

Red

Sand

μg/L

Red

Sand

Dup

μg/L

Elk

μg/L

Elk Dup

μg/L

Kabetogama

μg/L

Kabetogama

Dup

μg/L

Northern 

Light

μg/L

Northern 

Light

Dup

μg/L

Distilled 

Water 

Blank

μg/L

Distilled 

Water 

Blank

μg/L

4-Propylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 Triclosan <.01 <.01 <.01 <.01 <.01 <.01 <.01 .01 <.01 <.01 Surrogate Recoveryd6-Bisphenol A 37 51 41 50 47 79 112 87 13 61 d21-2,6-Di-tert-butyl-4-methylphenol 24 28 18 19 30 50 62 48 32 28 4-normal-Nonylphenol 31 36 34 40 38 61 79 63 48 91 4-normal-Nonylphenolmonoethoxylate 20 23 24 30 27 41 57 34 33 102 4-normal-Nonylphenoldiethoxylate 16 17 17 23 18 26 28 17 14 57 

29
Table 10. Summary of steroid and steroidal hormone compound data for water samples collected from 11 Minnesota lakes during 2008.—Continued

[avg, average; μg/L, microgram per liter; <, less than; Dup, duplicate sample; MS, matrix spike recovery in percent]

Compound Owasso μg/L Cedar μg/L Budd μg/L Sullivan μg/L Red Sand (avg) μg/L Shingobee μg/L White Sand (avg) μg/L Stewart μg/L Kabetogam

(avg) μg/L 

4-Androstene-3,17-dione <0.0001 <0.0001 <0.0001 0.0007 0.0004 0.0005 0.0010 0.0003 0.0005 

cis-Androsterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 

Cholesterol 9.0 7.8 2.5 7.1 5.7 <.005 7.5 <.005 2.0 

Coprostanol NM <.005 <.005 <.005 <.005 <.005 <.005 <.005 <.005 

Diethylstilbesterol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 

Equilenin <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 

Equilin <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 .0003 <.0001 <.0001 

17α-Ethinylestradiol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 

17α-Estradiol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 

17β-Estradiol .0001 .0004 <.0001 .0001 <.0001 <.0001 .0001 <.0001 <.0001 

Estriol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 

Estrone <.0001 <.0001 <.0001 .0007 .0006 .0011 .0006 .0015 <.0001 

Mestranol .0002 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 

Norethindrone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 

Progesterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 

Testosterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 .0005 <.0001 <.0001 

dihydro-Testosterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 

epi-Testosterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 

11-keto-Testosterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 

Surrogate Recovery (percent)d7-Androstenedione 0 0 0 45 62 64 45 68 51 

d7-Cholesterol 14 33 23 56 51 27 52 30 62 

d12-Chrysene 79 92 82 88 84 76 86 84 98 

d4-Dihydrotestosterone 0 0 0 62 86 79 28 81 31 

d4-Ethinyl estradiol 49 60 57 82 81 53 84 74 91 

d4-Estradiol 50 65 55 80 74 52 61 81 71 

d3-Estriol 41 53 36 60 50 19 56 40 70 

d4-Estrone 0 0 0 85 75 59 98 88 103 

d4-Mestranol 56 63 59 89 93 64 89 79 90 

30
Table 10. Summary of steroid and steroidal hormone compound data for water samples collected from 11 Minnesota lakes during 2008.—Continued

[avg, average; μg/L, microgram per liter; <, less than; Dup, duplicate sample; MS, matrix spike recovery in percent]

Compound Owasso μg/L Cedar μg/L Budd μg/L Sullivan μg/L Red Sand (avg) μg/L Shingobee μg/L White Sand (avg) μg/L Stewart μg/L Kabetogam

(avg) μg/L 

d6-Norethindrone 0 0 0 35 57 58 57 79 80 

d9-Progesterone 0 0 0 0 2 19 0 19 1 

d5-Testosterone 0 0 0 47 69 67 43 66 39 

Duplicates, Blanks, and Matrix Spikes

Compound

Red

Sand

μg/L

Red 

Sand 

Dup

μg/L

White 

Sand

μg/L

White 

Sand 

Dup

μg/L

Kabetogama

μg/L

Kabetogama 

Dup

μg/L

Northern 

Light

μg/L

Northern 

Light 

Dup

μg/L

Elk

μg/L

Elk Dup

μg/L

Field 

blank

μg/L

Di

W

B

4-Androstene-3,17-dione <.0001 .0004 .0010 .0010 .0006 .0004 <.0001 <.0001 .0008 .0009 <.0001 <

cis-Androsterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Cholesterol 6.5 4.8 7.5 7.5 2.0 2.0 <.005 <.005 8.5 8.1 <.005 <

Coprostanol <.005 <.005 <.005 <.005 <.005 <.005 <.005 <.005 <.005 <.005 <.005 <

Diethylstilbesterol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Equilenin <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Equilin <.0001 <.0001 <.0001 .0003 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

17α-Ethinylestradiol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

17α-Estradiol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

17β-Estradiol <.0001 <.0001 .0001 .0001 <.0001 <.0001 .0008 .0001 .0004 .0004 <.0001 <

Estriol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Estrone <.0001 .0007 .0006 .0007 <.0001 <.0001 <.0001 <.0001 .0011 .0011 <.0001 <

Mestranol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Norethindrone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

31
Table 10. Summary of steroid and steroidal hormone compound data for water samples collected from 11 Minnesota lakes during 2008.—Continued

[avg, average; μg/L, microgram per liter; <, less than; Dup, duplicate sample; MS, matrix spike recovery in percent]

Compound

Red

Sand

μg/L

Red 

Sand 

Dup

μg/L

White 

Sand

μg/L

White 

Sand 

Dup

μg/L

Kabetogama

μg/L

Kabetogama 

Dup

μg/L

Northern 

Light

μg/L

Northern 

Light 

Dup

μg/L

Elk

μg/L

Elk Dup

μg/L

Field 

blank

μg/L

Di

W

B

Progesterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Testosterone <.0001 <.0001 <.0001 .0005 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

dihydro-Testosterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

epi-Testosterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

11-keto-Testosterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Surrogate Recovery (percent)d7-Androstenedione 66 58 46 43 51 51 28 28 38 79 112 123 

d7-Cholesterol 56 46 62 43 58 67 96 22 13 45 12 19 

d12-Chrysene 88 79 92 80 99 97 94 85 74 92 95 99 

d4-Dihydrotestosterone 77 94 31 25 31 31 29 25 36 73 85 80 

d4-Ethinyl estradiol 85 77 91 77 91 91 104 68 29 54 82 74 

d4-Estradiol 76 72 65 57 71 72 94 66 32 55 88 65 

d3-Estriol 53 48 66 47 69 70 74 40 36 52 50 50 

d4-Estrone 83 68 104 93 103 102 117 87 33 52 98 81 

d4-Mestranol 99 87 93 84 90 91 102 69 29 51 89 88 

d6-Norethindrone 53 61 62 53 78 82 82 71 23 62 91 108 

d9-Progesterone 1 3 0 1 1 2 1 8 0 2 28 100 

d5-Testosterone 63 75 47 39 37 41 31 29 36 72 97 103 

32
Table 11. Summary of neutral organic compound data for sediment samples collected from 11 Minnesota lakes during 2008.—Continued

[avg, average; μg/kg, microgram per kilogram; <, less than; MS, matrix spike recovery in percent; Dup, duplicate sample; Trip, triplicate sample]

Compound Owasso μg/kg Cedar (avg) μg/kg Budd μg/kg Sullivan μg/kg Red Sand (avg) μg/kg Shingobee (avg) μg/kg White Sand μg/kg Stewart μg/kg Kabe

togam

μg/k

Bisphenol A 20 6.3 17 6.7 17 19 35 <1 16 

2[3]-tert-Butyl-4-methylphenol <1 <1 <1 <1 <1 <1 <1 <1 <1 

4-tert-Butylphenol <1 <1 <1 6 <1 <1 <1 <1 <1 

Caffeine <1 110 <1 <1 <1 <1 <1 <1 <1 

1,2-Dichlorobenzene <1 <1 <1 <1 <1 <1 <1 <1 <1 

1,3-Dichlorobenzene <1 <1 <1 <1 <1 <1 <1 <1 <1 

1,4-Dichlorobenzene <1 <1 <1 <1 1.1 0 <1 <1 <1 

2,6-Di-tert-butyl-1,4-benzoquinone <200 <200 <200 <200 <200 <200 <200 <200 <200 

2,6-Di-tert-butyl-4-methylphenol <3 <3 <3 <3 <3 <3 <3 <3 <3 

2,6-Di-tert-butylphenol <1 <1 <1 <1 <1 <1 <1 <1 <1 

N,N-Diethyl-meta-toluamide <1 <1 <1 <1 <1 <1 <1 <1 <1 

4-Ethylphenol 59 8.2 <3 21 <3 96 23 <3 607 

5-methyl-1H-Benzotriazole <1 <1 <1 <1 <1 <1 <1 <1 <1 

4-Methylphenol 595 12 <3 131 355 160 186 <3 1,100 

4-Nonylphenol <100 <100 <100 <100 100 350 <100 <100 <100 

4-Nonylphenolmonoethoxylate <20 <20 <20 <20 <20 30 <20 <20 <20 

4-Nonylphenoldiethoxylate <1 <1 <1 <1 <1 59 <1 <1 <1 

4-Nonylphenoltriethoxylate <1 <1 <1 62 <1 <1 <1 <1 <1 

4-Nonylphenoltetraethoxylate <1 <1 <1 <1 <1 <1 <1 <1 <1 

4-normal-Octylphenol <1 <1 <1 <1 <1 <1 <1 <1 <1 

4-tert-Octylphenol 98 4.4 <3 8 <3 22 33 <3 <3 

4-tert-Octylphenolmonoethoxylate <1 <1 <1 <1 1.3 6 <1 <1 <1 

4-tert-Octylphenoldiethoxylate <1 <1 <1 <1 21 <1 74 3 45 

4-tert-Octylphenoltriethoxylate <1 <1 <1 <1 <1 <1 <1 <1 <1 

4-tert-Octylphenoltetraethoxylate <1 <1 <1 <1 <1 <1 <1 <1 <1 

4-tert-Octylphenolpentaethoxylate <1 <1 <1 <1 <1 <1 <1 <1 <1 

4-tert-Pentylphenol 88 <1 <1 23 <1 <1 74 <1 <1 

4-Propylphenol <1 <1 <1 <1 <1 <1 <1 <1 <1 

Triclosan 33 44 <1 <1 <1 <1 <1 <1 <1 

Surrogate Recovery (percent)

33
Table 11. Summary of neutral organic compound data for sediment samples collected from 11 Minnesota lakes during 2008.—Continued

[avg, average; μg/kg, microgram per kilogram; <, less than; MS, matrix spike recovery in percent; Dup, duplicate sample; Trip, triplicate sample]

Compound Owasso μg/kg Cedar (avg) μg/kg Budd μg/kg Sullivan μg/kg Red Sand (avg) μg/kg Shingobee (avg) μg/kg White Sand μg/kg Stewart μg/kg Kabe

togam

μg/kg 

d6-Bisphenol A 59 51 54 48 75 61 87 25 54 

d21-2,6-Di-tert-butyl-4-methylphenol 19 26 4 5 48 24 95 3 17 

4-normal-Nonylphenol 114 108 140 97 133 105 144 45 92 

4-normal-Nonylphenolmonoethoxylate 216 73 229 138 163 137 193 66 183 

4-normal-Nonylphenoldiethoxylate 106 66 214 90 101 109 122 43 139 

Replicates, Blanks, and Matrix Spikes

Compound Cedar μg/kg Cedar Dup μg/kg Cedar Trip μg/kg Red Sand μg/kg Red Sand Dup μg/kg Shin- gobee μg/kg Shingobee Dup μg/kg Sand Blank μg/kg Sand Blank μg/kg Sa

Bla

μg/

Bisphenol A <1 <1 6 5 28 14 24 <1 <1 <

2[3]-tert-Butyl-4-methylphenol <1 <1 <1 <1 <1 <1 <1 <1 <1 <

4-tert-Butylphenol <1 <1 <1 <1 <1 <1 <1 <1 <1 <

Caffeine <1 53 161 <1 <1 <1 <1 <1 <1 <

1,2-Dichlorobenzene <1 <1 <1 <1 <1 <1 <1 <1 <1 <

1,3-Dichlorobenzene <1 <1 <1 <1 <1 <1 <1 <1 <1 <

1,4-Dichlorobenzene <1 <1 <1 1 <1 2 <1 1 <1 <

2,6-Di-tert-butyl-1,4-benzoquinone <200 <200 <200 <200 <200 <200 <200 <200 <200 <20

2,6-Di-tert-butyl-4-methylphenol <3 <3 <3 <3 <3 <3 <3 <3 <3 <

2,6-Di-tert-butylphenol <1 <1 <1 <1 <1 <1 <1 <1 <1 <

N,N-Diethyl-meta-toluamide <1 <1 <1 <1 <1 <1 <1 <1 <1 <

4-Ethylphenol 10 <3 7 <3 <3 70 122 <3 <3 <

5-methyl-1H-Benzotriazole <1 <1 <1 <1 <1 <1 <1 <1 <1 <

34
Table 11. Summary of neutral organic compound data for sediment samples collected from 11 Minnesota lakes during 2008.—Continued

[avg, average; μg/kg, microgram per kilogram; <, less than; MS, matrix spike recovery in percent; Dup, duplicate sample; Trip, triplicate sample]

Compound Cedar μg/kg Cedar Dup μg/kg Cedar Trip μg/kg Red Sand μg/kg Red Sand Dup μg/kg Shin- gobee μg/kg Shingobee Dup μg/kg Sand Blank μg/kg Sand Blank μg/kg Sa

Bla

μg/

4-Methylphenol <3 6 18 31 680 108 213 <3 <3 <

4-Nonylphenol <100 <100 <100 103 <100 <100 349 <100 <100 <10

4-Nonylphenolmonoethoxylate <20 <20 <20 <20 <20 30 <20 <20 <20 <2

4-Nonylphenoldiethoxylate <1 <1 <1 <1 <1 59 <1 <1 <1 <

4-Nonylphenoltriethoxylate <1 <1 <1 <1 <1 <1 <1 <1 <1 <

4-Nonylphenoltetraethoxylate <1 <1 <1 <1 <1 <1 <1 <1 <1 <

4-normal-Octylphenol <1 <1 <1 <1 <1 <1 <1 <1 <1 <

4-tert-Octylphenol <3 <3 4 <3 <3 22 <3 <3 <3 <

4-tert-Octylphenolmonoethoxylate <1 <1 <1 <1 1 <1 6 <1 <1 <

4-tert-Octylphenoldiethoxylate <1 <1 <1 21 <1 <1 <1 <1 <1 <

4-tert-Octylphenoltriethoxylate <1 <1 <1 <1 <1 <1 <1 <1 <1 <

4-tert-Octylphenoltetraethoxylate <1 <1 <1 <1 <1 <1 <1 <1 <1 <

4-tert-Octylphenolpentathoxylate <1 <1 <1 <1 <1 <1 <1 <1 <1 <

4-tert-Pentylphenol <1 <1 <1 <1 <1 <1 <1 <1 <1 <

4-Propylphenol <1 <1 <1 <1 <1 <1 <1 <1 <1 <

Triclosan <1 <1 44 <1 <1 <1 <1 <1 <1 <

Surrogate Recovery (percent)d6-Bisphenol A 44 44 65 91 59 58 63 68 46 5

d21-2,6-Di-tert-butyl-4-methylphenol 29 22 29 39 56 29 19 64 33 6

4-normal-Nonylphenol 85 121 117 136 129 99 110 105 117 14

4-normal-Nonylphenolmonoethoxylate 0 111 106 173 152 117 156 70 120 4

4-normal-Nonylphenoldiethoxylate 49 80 68 123 80 91 127 52 72 3

35
Table 12. Summary of steroid and steroidal hormone compound data for sediment samples collected from 11 Minnesota lakes during 2008.—Continu

[avg, average; μg/kg, microgram per kilogram; <, less than; Dup, duplicate sample; Trip, triplicate sample; MS, matrix spike recovery in percent]

Compound Owasso μg/kg Cedar (avg) μg/kg Budd μg/kg Sullivan μg/kg Red Sand (avg) μg/kg Shingobee (avg) μg/kg White Sand μg/kg Stewart μg/kg Kabetogam

μg/kg 

4-Androstene-3,17-dione 2.3 <0.05 0.22 0.39 0.55 0.94 0.59 0.33 <0.05 

cis-Androsterone <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 

Cholesterol 4,200 330 530 1,400 1,200 1,600 770 1,200 3,600 

Coprostanol 790 47 32 360 320 340 35 130 380 

Diethylstilbesterol <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 3.8 

Equilenin <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 

Equilin <5 <5 <5 <5 <5 <5 <5 <5 <5 

17α-Estradiol <.05 <.05 .08 .06 .10 .17 .46 .08 <.05 

17β-Estradiol 1.3 <.05 .05 .15 .35 1.3 .58 .12 .85 

Estriol <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 

Estrone 2.9 <.05 .27 .82 .69 2.4 .99 .59 5.6 

17α-Ethinylestradiol <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 

Mestranol <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 

Norethindrone <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 

Progesterone <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 

Testosterone 1.4 <.05 <.05 <.05 .26 <.05 .23 <.05 2.7 

dihydro-Testosterone <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 

epi-Testosterone <.05 <.05 <.05 <.05 .14 <.05 <.05 <.05 .89 

11-keto-Testosterone <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 

Surrogate Recovery (percent)d7-Androstenedione 19 0 33 13 15 28 26 10 51 

d7-Cholesterol 7 1 9 11 20 12 13 4 39 

d8-Diethylstilbesterol 25 0 25 64 54 43 50 22 24 

d4-Dihydrotestosterone 24 2 53 16 26 43 46 15 56 

d4-Ethinylestradiol 41 3 40 37 62 63 68 33 92 

d4-Estradiol 25 2 34 47 53 54 58 22 33 

d4-Mestranol 47 3 75 39 63 83 2 38 94 

d6-Norethindrone 11 0 21 8 17 16 18 5 27 

d5-Testosterone 23 1 33 15 21 32 32 10 51 

36
Replicates, Blanks, and Matrix Spikes

Table 12. Summary of steroid and steroidal hormone compound data for sediment samples collected from 11 Minnesota lakes during 2008.—Continu[avg, average; μg/kg, microgram per kilogram; <, less than; Dup, duplicate sample; Trip, triplicate sample; MS, matrix spike recovery in percent]

Compound Cedar μg/kg Cedar Dup μg/kg Cedar Trip μg/kg Red Sand μg/kg Red Sand Dup μg/kg Shingobee μg/kg Shingobee Dup μg/kg Sand Blank μg/kg Sand Blank μg/kg San

Blan

μg/k

4-Androstene-3,17-dione <.05 <.05 <.05 <.05 .55 .97 .92 <.05 .11 cis-Androsterone <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <Cholesterol 420 320 260 870 1400 910 2400 41 72 12 Coprostanol 50 51 41 270 370 220 460 <5 <5 <5 Diethylstilbesterol <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <Equilenin <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <Equilin <5 <5 <5 <5 <5 <5 <5 <5 <5 <5 17α-Estradiol <.05 <.05 <.05 .07 .13 .16 .17 <.05 <.05 <17β-Estradiol <.05 <.05 <.05 .20 .49 1.00 1.58 <.05 <.05 <Estriol <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <Estrone <.05 <.05 <.05 .30 1.08 1.98 2.78 <.05 <.05 <

17α-Ethinylestradiol <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <Mestranol <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <Norethindrone <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <Progesterone <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <Testosterone <.05 <.05 <.05 <.05 .26 <.05 <.05 <.05 <.05 <

dihydro-Testosterone <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <

epi-Testosterone <.05 <.05 <.05 <.05 .14 <.05 <.05 <.05 <.05 <11-keto-Testosterone <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <.05 <Surrogate Recovery (percent)d7-Androstenedione 1 0 0 6 25 32 24 19 12 18 

d7-Cholesterol 1 0 1 29 12 12 11 10 14 33 

d8-Diethylstilbesterol 0 0 0 56 52 39 46 32 0 65 

d4-Dihydrotestosterone 2 0 2 14 38 52 34 63 50 69 

d4-Ethinyl estradiol 3 1 4 65 60 64 62 54 20 67 

d4-Estradiol 3 1 3 55 52 49 60 60 29 126 

d4-Mestranol 4 1 5 57 69 95 72 64 51 72 

d6-Norethindrone 0 0 0 2 32 19 13 15 10 18 

d5-Testosterone 1 0 1 6 35 36 28 31 22 33 

37
Table 13. Summary of neutral organic compound data for polar organic compound integrative samplers (POCIS) deployed in 11 Minnesota lakes du

[μg/POCIS, microgram per POCIS; <, less than]

Compound

Owasso

μg/

POCIS

Cedar

μg/

POCIS

Budd

μg/

POCIS

Sullivan

μg/

POCIS

Sullivan

Day 7 

μg/

POCIS

Sullivan

Day 14

μg/

POCIS

Sullivan

Day 21

μg/

POCIS

Red

Sand

μg/

POCIS

Shingobee

μg/

POCIS

White 

Sand

μg/

POCIS

Stewart

μg/

POCIS

Kab

Bisphenol A <0.01 <0.01 <0.01 0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0

2[3]-tert-Butyl-4-methylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

4-tert-Butylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

Caffeine .02 .11 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

1,2-Dichlorobenzene <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

1,3-Dichlorobenzene <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

1,4-Dichlorobenzene <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

2,6-Di-tert-butyl-1,4-benzoquinone <.01 <.01 <.01 .05 .07 .08 .05 .04 .29 .02 .21 

2,6-Di-tert-butyl-4-methylphenol .35 <.01 <.01 .22 .22 .24 <.01 .17 .02 .06 .01 

2,6-Di-tert-butylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

N,N-Diethyl-meta-toluamide .12 .09 <.01 .08 .02 .02 .04 .03 .01 .09 .06 

4-Ethylphenol .02 .04 <.01 <.01 <.01 <.01 .01 <.01 .01 <.01 .01 

5-methyl-1H-Benzotriazole <.01 .06 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

4-Methylphenol .06 .03 .02 .06 .01 .01 .02 .04 .06 .01 .06 

4-Nonylphenol .09 .06 .03 .09 .05 .04 .06 .12 .06 .08 .09 

4-Nonylphenolmonoethoxylate <.01 <.01 <.01 .04 <.01 <.01 .03 .03 <.01 .02 <.01 <

4-Nonylphenoldiethoxylate <.01 <.01 <.01 <.01 <.01 <.01 <.01 .12 <.01 <.01 <.01 <

4-Nonylphenoltriethoxylate <.01 <.01 <.01 .06 <.01 <.01 <.01 <.01 <.01 .09 <.01 <

4-Nonylphenoltetraethoxylate <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

4-normal-Octylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

4-tert-Octylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

4-tert-Octylphenolmonoethoxylate <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

4-tert-Octylphenoldiethoxylate <.01 <.01 <.01 <.01 .02 <.01 <.01 <.01 <.01 <.01 <.01 <

4-tert-Octylphenoltriethoxylate <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

4-tert-Octylphenoltetraethoxylate <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

4-tert-Octylphenolpentaethoxylate <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

4-tert-Pentylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

4-Propylphenol <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

Triclosan <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <.01 <

Surrogate Recovery (percent)d6-Bisphenol A 22 20 9 147 167 92 107 123 161 131 144 99 

d21-2,6-Di-tert-butyl-4-methylphenol 13 3 6 23 36 36 8 8 73 3 40 4

4-normal-Nonylphenol 23 17 8 144 146 50 106 116 143 116 133 10

4-normal-Nonylphenolmonoethoxylate 18 13 6 197 187 53 130 155 189 158 170 13

4-normal-Nonylphenoldiethoxylate 96 0 24 685 1250 261 863 95 1276 74 92 857 

38
Table 14. Summary of steroid and steroidal hormone compound data for passive organic compound integrative samplers (POCIS) deployed in 11 Min

Continued[avg, average; μg/POCIS, microgram per POCIS; <, less than; Dup, duplicate sample; Trip, triplicate sample; --, not quantified]

Compound

Owasso 

(avg)

μg/

POCIS

Cedar 

(avg)

μg/

POCIS

Budd 

(avg)

μg/

POCIS

Sullivan

μg/

POCIS

Sullivan 

Day 7 

μg/

POCIS

Sullivan 

Day 14

μg/

POCIS

Sullivan 

Day 21

μg/

POCIS

Red Sand

μg/

POCIS

Shingobee

μg/

POCIS

White 

Sand

μg/

POCIS

Stewart

μg/

POCIS

Ka

POCIS extracted 1 1 1 3 3 3 3 3 3 3 3 3 

4-Androstene-3,17-dione <.0001 <.0001 .0023 .0005 <.0001 <.0001 <.0001 .0007 <.0001 .0009 .0007 <

cis-Androsterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Cholesterol <.5 <.5 4.6 .5 <.5 <.5 <.5 .5 <.5 <.5 <.5 <

Coprostanol <.5 <.5 <.5 <.5 <.5 <.5 <.5 <.5 <.5 <.5 <.5 <

Diethylstilbesterol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Equilenin <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Equilin <.5 <.5 <.5 <.5 <.5 <.5 <.5 <.5 <.5 <.5 <.5 <

17α-Estradiol <.0001 <.0001 <.0001 .0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

17β-Estradiol .0005 .0006 .0003 .0003 <.0001 .0001 <.0001 <.0001 .0001 .0001 .0002 

Estriol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Estrone .0012 .0012 .0010 .0013 <.0001 <.0001 .0004 .0012 .0008 .0011 .0022 <

17α-Ethinylestradiol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Mestranol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Norethindrone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Progesterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Testosterone .0004 <.0001 .0004 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

dihydro-Testosterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

epi-Testosterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

11-keto-Testosterone <.0001 <.0001 .0017 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Surrogate Recovery (percent)d7-Androstenedione 136 132 143 149 109 75 81 93 91 54 107 79 

d7-Cholesterol 59 63 83 45 81 23 35 68 28 23 65 30 

d8-Diethylstilbestrol 94 84 91 101 60 37 38 55 68 55 69 45 

d4-Ethinyl estradiol 109 106 124 143 100 65 65 88 68 59 98 57 

d4-Estradiol 95 88 104 1 139 88 74 111 93 74 108 78 

d3-Estriol -- -- -- -- -- -- -- -- -- -- -- 

d4-Estrone 124 118 138 140 106 69 76 89 82 54 95 67 

d4-Mestranol 89 90 100 118 90 41 59 70 64 49 78 55 

d6-Norethindrone 128 124 138 160 110 86 75 94 78 58 104 74 

d9-Progesterone 170 166 194 200 139 75 81 135 75 81 144 92 

d5-Testosterone 109 109 125 140 92 63 59 78 67 56 89 62 

39
Replicates

Table 14. Summary of steroid and steroidal hormone compound data for passive organic compound integrative samplers (POCIS) deployed in 11 Min2008.—Continued[avg, average; μg/POCIS, microgram per POCIS; <, less than; Dup, duplicate sample; Trip, triplicate sample; --, not quantified]

Compound

Owasso

μg/

POCIS

Owasso Dup

μg/

POCIS

Owasso Trip

μg/

POCIS

Cedar

μg/

POCIS

Cedar Dup

μg/

POCIS

Cedar Trip

μg/

POCIS

Budd

μg/

POCIS

Bu

P

POCIS extracted 1 1 1 1 1 1 1 1 4-Androstene-3,17-dione <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 .0020 

cis-Androsterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <Cholesterol <.5 <.5 <.5 <.5 <.5 <.5 3.4 5

Coprostanol <.5 <.5 <.5 <.5 <.5 <.5 <.5 <Diethylstilbesterol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <Equilenin <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <Equilin <.5 <.5 <.5 <.5 <.5 <.5 <.5 <17α-Estradiol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <17β-Estradiol .0004 .0002 .0007 .0010 .0004 .0005 .0002 <Estriol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <Estrone .0014 .0010 .0014 .0011 .0014 .0011 .0010 <17α-Ethinylestradiol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <Mestranol <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <

Norethindrone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <Progesterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <Testosterone <.0001 <.0001 .0004 <.0001 <.0001 <.0001 <.0001 

dihydro-Testosterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <epi-Testosterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 <11-keto-Testosterone <.0001 <.0001 <.0001 <.0001 <.0001 <.0001 .0017 <

Surrogate Recovery (percent)d7-Androstenedione 87 160 160 85 139 173 107 153 

d7-Cholesterol 49 56 73 16 90 83 67 94 

d8-Diethylstilbestrol 46 119 118 62 82 108 62 100 d4-Ethinyl estradiol 78 120 129 54 121 144 97 137 

d4-Estradiol 64 109 112 52 99 112 89 103 d3-Estriol 0 0 0 0 0 0 0 0 

d4-Estrone 75 151 147 70 126 159 103 153 

d4-Mestranol 62 100 106 54 98 118 77 112 

d6-Norethindrone 88 143 153 69 137 166 107 151 d9-Progesterone 114 189 206 66 205 228 139 226 d5-Testosterone 72 122 133 66 115 145 93 134 

40
Table 15. Summary of field measurements for water samples collected from four Minnesota lakes during 2010.

[°C, degrees Celsius; μS/cm, microsiemens per centimeter; mg/L, milligrams per liter; std unit, standard unit]

Temperature

°C

Specific

conductance

μS/cm

Dissolved

oxygen

mg/L

pH

std unit

Elk 11.8 294 8.6 8.4

Beast 10.7 23 9.5 6.9

Bohall 9.6 182 10.0 8.0

Ryan 10.7 23 9.8 6.8

Table 16. Summary of acidic organic compound data for water samples collected from four Minnesota 

lakes during 2010.

[μg/L, microgram per liter; <, less than]

Compound Elk

μg/L

Beast

μg/L

Bohall

μg/L

Ryan

μg/L

Ethylenediaminetetraacetic acid 0.53 <0.05 0.06 0.40

Nitrilotriacetic acid < .05 < .05 < .05 < .05

4-Nonylphenolmonoethoxycarboxylic acid < .1 < .1 < .1 < .1

4-Nonylphenoldiethoxycarboxylic acid < .1 < .1 < .1 < .1

4-Nonylphenoltriethoxycarboxylic acid < .1 < .1 < .1 < .1

4-Nonylphenoltetraethoxycarboxylic acid < .1 < .1 < .1 < .1

Surrogate Recovery (percent)

4-normal-Nonylphenoldiethoxycarboxylic acid 61 59 67 54

41
Table 17. Summary of neutral organic compound data for water samples collected from four Minnesota lakes during 2010.

[μg/L, microgram per liter; <, less than; --, not quantifiable]

Compound Elk

μg/L

Beast

μg/L

Bohall

μg/L

Ryan

μg/L

Acetylhexamethyltetrahydronaphthalene <0.01 <0.01 <0.01 <0.01

Bisphenol A < .01 < .01 < .01 < .01

2[3]-tert-Butyl-4-methylphenol < .01 < .01 < .01 < .01

4-tert-Butylphenol < .01 < .01 < .01 < .01

Caffeine < .01 < .01 < .01 < .01

2,6-Di-tert-butyl-1,4-benzoquinone .05 .04 .02 < .01

2,6-Di-tert-butyl-4-methylphenol .01 < .01 < .01 < .01

2,6-Di-tert-butylphenol < .01 < .01 < .01 < .01

1,2-Dichlorobenzene < .01 < .01 < .01 < .01

1,3-Dichlorobenzene < .01 < .01 < .01 < .01

1,4-Dichlorobenzene < .01 < .01 < .01 < .01

N,N-Diethyl-meta-toluamide < .01 < .01 < .01 < .01

4-Ethylphenol < .01 < .01 < .01 < .01

Hexahydrohexamethylcyclopentabenzopyran < .01 < .01 < .01 < .01

5-Methyl-1H-benzotriazole < .01 < .01 < .01 < .01

4-Methylphenol < .01 .01 < .01 .01

4-Nonylphenol < .05 < .05 < .05 < .05

4-Nonylphenolmonoethoxylate < .05 < .05 < .05 < .05

4-Nonylphenoldiethoxylate < .05 < .05 < .05 < .05

4-normal-Octylphenol < .01 < .01 < .01 < .01

4-tert-Octylphenol < .01 < .01 < .01 < .01

4-tert-Octylphenolmonoethoxylate < .01 < .01 < .01 < .01

4-tert-Octylphenoldiethoxylate < .01 < .01 < .01 < .01

4-tert-Octylphenoltriethoxylate < .01 < .01 < .01 < .01

4-tert-Octylphenoltetraethoxylate < .01 < .01 < .01 < .01

4-tert-Octylphenolpentaethoxylate < .01 < .01 < .01 < .01

4-tert-Pentylphenol < .01 < .01 < .01 < .01

4-Propylphenol < .01 < .01 < .01 < .01

Triclosan < .01 < .01 < .01 < .01

Surrogate Recovery (percent)

d6-Bisphenol A 27 49 52 32

d21-2,6-Di-tert-butyl-4-methylphenol 53 85 21 63

4-normal-Nonylphenol 38 56 10 37

4-normal-Nonylphenolmonoethoxylate 38 51 47 37

4-normal-Nonylphenoldiethoxylate 46 63 -- 34

42
Table 18. Summary of steroid and steroidal hormone compound data for water samples collected from four Minnesota lakes during 

2010.

[μg/L, microgram per liter; <, less than]

Compound Elk

μg/L

Beast

μg/L

Bohall

μg/L

Ryan

μg/L

4-Androstene-3,17-dione <0.0001 <0.0001 <0.0001 < .0001

cis-Androsterone < .0001 < .0001 < .0001 < .0001

Cholesterol 1.4 1.2 1.2 2.4

Coprostanol .06 .08 .01 < .005

Diethylstilbestrol < .0001 < .0001 < .0001 < .0001

Equilenin < .0001 < .0001 < .0001 < .0001

Equilin < .0001 < .0001 < .0001 < .0001

17α-Estradiol < .0001 < .0001 < .0001 < .0001

17β-Estradiol < .0001 < .0001 < .0001 < .0001

Estriol < .0001 < .0001 < .0001 < .0001

Estrone .0001 .0001 .0001 .0008

17α-Ethynylestradiol < .0001 < .0001 < .0001 < .0001

Mestranol < .0001 < .0001 < .0001 < .0001

Norethindrone < .0001 < .0001 < .0001 < .0001

Progesterone < .0001 < .0001 < .0001 < .0001

Testosterone < .0001 < .0001 < .0001 < .0001

dihydro-Testosterone < .0001 < .0001 < .0001 < .0001

epi-Testosterone .0001 < .0001 < .0001 < .0001

11-keto-Testosterone < .0001 < .0001 < .0001 < .0001

Surrogate Recovery (percent)

d7-Cholesterol 64 40 48 54

d12-Chrysene 101 100 99 98

d8-Diethylstibestrol 75 78 83 90

13C6

-Estradiol 57 60 76 82

d2-epi-Estriol 96 90 66 94

13C6

-Estrone 115 109 95 105

d4-Ethynylestradiol 94 90 83 91

d3-Medroxyprogesterone 76 67 56 37

d4-Mestranol 95 90 82 90

d3-Nandrolone 102 93 86 83

43
Table 19. Summary of field data for preliminary microhabitat selection at Sullivan Lake, Minn., June 1, 2010.

[Std unit, standard unit; μS/cm, microsiemens per centimeter; Temp, temperature; °C, degrees Celsius; mg/L, milligrams per liter; NM, not measured; Temp residual = Temp lakresidual less than 2°C indicates lake water loss downward to groundwater; Temp residual from 2°C to 5°C indicates mixing of groundwater and surface water; Temp residual gregroundwater discharge to lake]

Location Study site Matrix Lakebed pH std unit Specific conductance

μS/cm

Nitrate mg/L Temp °C 

r

Surface water 

and pore water 

physio-chemical

characteristics of the 

eastern shoreline

of Sullivan Lake 

(from southwest

to northeast)

Southwest

of site B

Pore Silt/clay NM 1,395 0.2 18.6–19.1 3

Lake Silt/clay 7.16 416 .2 22.5

Pore Silt/clay NM 548 .2 16.0–16.9 5

Lake Silt/clay 7.89 379 .2 22.5

Site B

Pore Sandy NM 590 NM 16.6 

Lake Sandy 7.87 403 NM 23.7

Pore Sandy NM 610 .1 21.4 

Lake Sandy 8.19 402 NM 23.7

Pore Sandy NM 754 NM NM 

Lake Sandy 7.85 424 NM 23.7

Pore Sandy NM 721 NM NM 

Pore Sandy NM 871 NM NM 

Pore Sandy NM 916 NM NM 

Lake Sandy 7.75 400 .2 24.39

Pore Sandy NM 1,229 NM NM 

Site A

Pore Sandy NM 876 .3 NM 

Pore Sandy NM 692 .3 NM 

Pore Sandy NM 678 .3 NM 

Pore Sandy NM 2,053 .2 NM 

NM Silt/clay NM NM NM NM 

Between sites

A and C

Pore Silt/clay NM 1,868 4.6 NM 

Pore Silt/clay NM 1,454 NM NM 

Site C Lake Silt/clay 8.4 389 NM 24.3

44
Table 20. Site characterization of Sullivan Lake microhabitat A (residential/septic influence) and water-quality values for pore-water 

samples collected July 8, 2010.

[x, distance parallel to shore; y, distance perpendicular to shore; see fig. 2 for specific sampling-grid orientation; m, meters; mg/L, milligrams per liter; mm, 

millimeters; °C, degrees Celsius; <, less than; NM, no field measurement; cm, centimeters]

Constituent

Location (x, y) in m

(0, 1)

(0, 3)

(0, 5)

(5, 1)

(5, 3)

(5, 5)

(10, 1)

(10, 3)

(10, 5)

(15, 1)

(15, 3)

(15, 5)

Dissolved organic carbon mg/L 3.0 2.6 2.1 2.1

5.9 4.0 2.1 3.4

3.2 7.4 3.6 3.7

Linear alkylbenzene sulfonates mg/L < .02 .29 .04 .16

< .02 .92 .13 .13

 .38 .15 .04 .10

Alkylphenolethoxylates mg/L .14 < .02 < .02 < .02

< .02 < .02 < .02 < .02

< .02 < .02 < .02 < .02

Hydraulic head mm 0 NM .8 .1

15 2.1 .1 .3

3.1 1.4 .7 2.8

Temperaturewater/sediment °C 24.3 25.4 24.6 23.8

25.1 25.6 25.0 23.0

25.6 25.5 25.9 23.1

Temperature30 cm °C 22.9 21.7 21.2 16.5

24.0 23.7 22.4 19.2

23.4 23.6 23.4 20.5

Table 21. Water column water-quality measurements for Sullivan Lake microhabitat A (residential/septic influence) collected from 

1:30 to 3:00 PM on July 21, 2010.

[x, distance parallel to shore; y, distance perpendicular to shore; see fig. 2 for specific sampling-grid orientation; m, meters; total depth, distance from water 

surface to bed sediments; cm, centimeters; °C, degrees Celsius; mS/cm, microsiemens per centimeter; mg/L, milligrams per liter; std unit, standard unit]

Location (x, y) in m

Total

depth

cm

Depth from

water surface

cm

Temperature

°C

Specific

conductance

μS/cm

Dissolved

oxygen

mg/L

pH

std unit

(0, 5) 42 10 29.1 390 8.9 8.5

32 28.9 392 7.7 8.3

(3, 5) 39 10 29.1 388 7.9 8.6

29 28.7 390 7.9 8.5

(5, 5) 42 10 29.1 384 9.1 8.7

32 30.0 385 8.8 8.6

(10, 5) 44 10 29.1 386 7.8 8.6

34 28.9 386 7.8 8.5

(15, 5) 48 10 29.0 385 8.4 8.5

38 27.4 414 5.8 7.9

45
Table 22. Site characterization of Sullivan Lake microhabitat B (residential/septic influence) and water-quality values for pore-water 

samples collected July 8, 2010.

[x, distance parallel to shore; y, distance perpendicular to shore; see figure 2 for specific sampling-grid orientation; m, meters; mg/L, milligrams per liter; mm, 

millimeters; °C, degrees Celsius; <, less than; NM, no field measurement; cm, centimeters]

Constituent

Location (x, y) in m

NM

(0, 3)

(0, 5)

NM

(5, 3)

(5, 5)

(10, 1)

(10, 3)

(10, 5)

(15, 1)

(15, 3)

(15, 5)

Dissolved organic carbon mg/L NM NM 7.6 9.4

7.8 7.6 8.7 10.4

10.3 10.0 11.4 10.1

Linear alkylbenzene sulfonates mg/L NM NM < .02 < .02

 .02 .04 < .02 < .02

 .12 .02 < .02 .03

Alkylphenolethoxylates mg/L NM NM < .02 < .02

< .02 .10 < .02 .04

 .11 < .02 < .02 < .02

Hydraulic head mm NM NM –1 –3

–2 0 –3 1

3 –1 –1 0

Temperaturewater/sediment °C NM NM NM NM

NM NM NM NM

NM NM NM NM

Temperature30 cm °C NM NM NM NM

NM NM NM NM

NM NM NM NM

Table 23. Water column water-quality measurements for Sullivan Lake microhabitat B (residential/septic influence) collected 10:30 

AM to 2:00 PM on July 21, 2010.

[x, distance parallel to shore; y, distance perpendicular to shore; see fig. 2 for specific sampling-grid orientation; m, meters; total depth, distance from water 

surface to bed sediments; cm, centimeters; °C, degrees Celsius; mS/cm, microsiemens per centimeter; mg/L, milligrams per liter; std unit, standard unit]

Location (x, y) in m Total depth 

cm

Depth from water 

surface

cm

Temperature

°C

Specific conductance 

μS/cm

Dissolved oxygen 

mg/L pH std unit

(0, 5) 52 10 27.0 378 7.2 8.7

26 26.8 378 8.0 8.7

42 26.6 379 7.7 8.6

(3, 5) 54 10 27.1 377 7.8 8.7

27 26.9 379 8.1 8.7

44 26.8 378 8.7 8.7

(5, 5) 55 10 27.0 379 8.4 8.7

28 26.8 378 8.7 8.8

45 26.8 378 8.4 8.8

(10, 5) 60 10 27.2 378 8.8 8.7

30 27.0 378 9.5 8.8

50 26.9 378 8.9 8.7

(15, 5) 65 10 27.2 378 9.2 8.7

22 27.0 378 9.3 8.8

55 26.7 378 9.6 8.8

46
Table 24. Site characterization of Sullivan Lake microhabitat C (stormwater/boat-ramp 

influence) and water-quality values for pore-water samples collected July 8, 2010.

[x, distance parallel to shore; y, distance perpendicular to shore; see fig. 2 for specific sampling-grid orientation; 

m, meters; mg/L, milligrams per liter; °C, degrees Celsius; <, less than; NM, not measured; cm, centimeters]

Constituent

Location (x, y) in m

(0, 1)

NM

NM

(15, 5)

Dissolved organic carbon mg/L 11.2 NM

NM 7.3

Linear alkylbenzene sulfonates mg/L < .02 NM

NM .03

Alkylphenolethoxylates mg/L .11 NM

NM < .02

Temperaturewater/sediment °C 23.7 NM

NM 28.6

Temperature30 cm °C 19.4 NM

NM 17.7

Table 25. Water column water-quality measurements for Sullivan Lake microhabitat C (stormwater/boat ramp influence) collected 

12:00 to 1:30 PM on July 21, 2010.

[x, distance parallel to shore; y, distance perpendicular to shore; see fig. 2 for specific sampling-grid orientation; m, meters; total depth, distance from water 

surface to bed sediments; cm, centimeters; °C, degrees Celsius; mS/cm, microsiemens per centimeter; mg/L, milligrams per liter; std unit, standard unit]

Location (x, y) in m Total depth

cm

Depth from water 

surface cm Temperature °C Specific conductance 

μS/cm

Dissolved oxygen 

mg/L

pH std 

unit

(0, 5) 82 10 27.1 384 9.2 8.4

41 26.3 387 7.8 8.1

72 26.2 392 5.2 7.8

(3, 5) 69 10 27.4 383 7.7 8.4

35 26.8 385 7.8 8.3

59 26.3 384 7.5 8.3

(5, 5) 68 10 27.4 381 8.4 8.4

34 26.6 384 7.8 8.2

58 26.2 389 6.9 7.7

(10, 5) 73 10 27.5 379 9.6 8.5

37 26.5 384 9.1 8.1

63 26.3 388 7.3 7.8

(15, 5) 71 10 26.9 379 10.1 8.5

36 26.5 384 8.0 8.1

61 26.1 394 5.9 7.5

47
Table 26. Site characterization of Sullivan Lake microhabitat D (agricultural influence) and water-quality values for pore-water 

samples collected July 9, 2010.

[x, distance parallel to shore; y, distance perpendicular to shore; see fig. 2 for specific sampling-grid orientation; m, meters; mg/L, milligrams per liter; mm, 

millimeters; °C, degrees Celsius; <, less than; NM, no measurement; * positive bias due to high inorganic carbon content; cm, centimeters]

Constituent

Location (x, y) in m

(0, 1)

(0, 3)

(0, 5)

NM

NM

(5, 5)

Dissolved organic carbon mg/L 31.8* NM

12.6* NM

32.3* 5.0

Linear alkylbenzene sulfonates mg/L .02 NM

 .11 NM

 .02 .11

Alkylphenolethoxylates mg/L < .02 NM

< .02 NM

< .02 < .02

Hydraulic head mm 1.2 NM

NM NM

NM NM

Temperaturewater/sediment °C 22.9 NM

23.8 NM

21.7 19.9

Temperature30 cm °C 18.5 NM

18.8 NM

17.4 16.7

Table 27. Water column water-quality measurements for Sullivan Lake microhabitat D (agricultural influence) collected 9:00 to 10:30 

AM on July 21, 2010.

[x, distance parallel to shore; y, distance perpendicular to shore; see fig. 2 for specific sampling-grid orientation; m, meters; cm, centimeters; °C, degrees Celsius; mS/cm, microsiemens per centimeter; mg/L, milligrams per liter; std unit, standard unit; NM, no measurement]

Location (x, y) in m Total depth 

cm

Depth from water 

surface cm Temperature °C Specific

conductance μS/cm

Dissolved 

oxygen mg/L pH std unit

(0, 5) 70 10 25.1 388 4.1 7.4

35 25.2 388 3.7 7.5

50 25.1 389 3.6 7.5

(3, 5) 72 10 25.5 880 4.3 7.6

36 25.1 406 3.2 6.9

52 25.0 443 2.9 6.7

(5, 5) 76 10 25.4 389 4.4 7.5

38 25.2 450 2.9 6.7

56 25.0 540 1.9 6.7

(10, 5) 71 10 25.8 385 5.1 7.9

36 25.4 472 2.5 6.7

51 NM 252 1.9 6.6

(15, 5) 78 10 26.1 384 5.6 7.9

39 25.6 387 4.8 7.7

58 25.2 451 3.0 6.8

48
Table 28. Summary of acidic organic compound data for water samples collected from four microhabitat sites in Sullivan Lake, Minn., on July 8, 201

[Microhabitats A and B, residential/septic influenced; microhabitat C, stormwater/boat-ramp influenced; microhabitat D, agriculture influenced; μg/L, microgram per liter; <, lesMS, matrix spike recovery in percent; NM, no measurement]

Compound

Site

A

μg/L

Site

A-Dup

μg/L

Site

A-MS

Percent

Site

B

μg/L

Site

B-Dup

μg/L

Site

C

μg/L

Site

C-Dup

μg/L

Site

C-MS

percent

Site

D

μg/L

Site

D-Dup

μg/L

Ethylenediaminetetraacetic acid 0.2 0.2 63 0.2 0.2 0.2 0.2 68.6 0.6 0.6 

Nitrilotriacetic acid .1 .1 101 .1 .1 .1 .1 98.4 .1 .1 

4-Nonylphenolmonoethoxycarboxylic acid .6 .4 90 .4 .4 .4 .5 90.9 .4 .4 

4-Nonylphenoldiethoxycarboxylic acid .5 .1 95 < .1 < .1 < .1 < .1 90.0 < .1 < .1 

4-Nonylphenoltriethoxycarboxylic acid < .1 < .1 80 < .1 < .1 < .1 < .1 78.1 < .1 < .1 

4-Nonylphenoltetraethoxycarboxylic acid < .1 < .1 84 < .1 < .1 < .1 < .1 80.0 < .1 < .1 

Surrogate Recovery (percent)4-normal-Nonylphenoldiethoxycarboxylic acid 69 66 95 68 72 68 87 85 79 75 

Table 29. Summary of acidic organic compound data for water samples collected from four microhabitat sites in Sullivan Lake, Minn., on October 12[Microhabitats A and B, residential/septic influenced; microhabitat C, stormwater/boat-ramp influenced; microhabitat D, agriculture influenced; μg/L, microgram per liter; <, les

Compound

Site

A

μg/L

Site

A Dup

μg/L

Site

B

μg/L

Site

C

μg/L

Ethylenediaminetetraacetic acid 0.3 0.3 0.2 0.2 

Nitrilotriacetic acid .1 .1 < .05 < .05 

4-Nonylphenolmonoethoxycarboxylic acid < .1 < .1 < .1 < .1 

4-Nonylphenoldiethoxycarboxylic acid .2 .1 < .1 < .1 

4-Nonylphenoltriethoxycarboxylic acid < .1 < .1 < .1 < .1 

4-Nonylphenoltetraethoxycarboxylic acid < .1 < .1 < .1 < .1 

Surrogate Recovery (percent)4-normal-Nonylphenoldiethoxycarboxylic acid 64 46 55 70 

49
Table 30. Summary of neutral organic compound data for water samples collected from four microhabitat sites in Sullivan Lake, Minn. on July 8, 201

[Microhabitats A and B, residential/septic influenced; microhabitat C, stormwater/boat-ramp influenced; microhabitat D, agriculture influenced; μg/L, microgram per liter; <, lesMS, matrix spike recovery in percent; NM, not measured]

Compound

Site

A

μg/L

Site

A-Dup

μg/L

Site

A-MS

percent

Site

B

μg/L

Site

B-Dup

μg/L

Site

B-MS

percent

Site

C

μg/L

Site

C-Dup

μg/L

Site

C-MS

percent

Sit

D

μg/

Acetylhexamethyltetrahydronaphthalene <0.01 <0.01 111 <0.01 <0.01 114 <0.01 <0.01 131 <0.0

Bisphenol A .03 .02 67 .05 .01 68 < .01 < .01 85 < .02[3]-tert-Butyl-4-methylphenol < .01 < .01 118 < .01 < .01 92 < .01 < .01 131 < .0

4-tert-butylphenol < .01 < .01 111 < .01 < .01 116 < .01 < .01 129 < .0

Caffeine .01 .02 31 < .01 < .01 31 < .01 < .01 30 < .02,6-Di-tert-butyl-1,4-benzoquinone .03 .03 NM .04 .03 NM .04 .03 NM .02,6-Di-tert-butyl-4-methylphenol .04 .02 NM .02 .01 NM .03 .04 NM .02,6-Di-tert-butylphenol < .01 < .01 136 < .01 < .01 98 < .01 < .01 146 < .01,2-Dichlorobenzene < .01 < .01 99 < .01 < .01 98 < .01 < .01 88 < .01,3-Dichlorobenzene < .01 < .01 98 < .01 < .01 96 < .01 < .01 88 < .0

1,4-Dichlorobenzene < .01 < .01 98 < .01 < .01 96 < .01 < .01 87 < .0

N,N-Diethyl-meta-toluamide .15 .14 107 .13 .13 118 .07 .08 117 .0

4-Ethylphenol < .01 < .01 73 < .01 < .01 69 .01 < .01 68 < .0Hexahydrohexamethylcyclopentabenzopyran < .01 < .01 107 < .01 < .01 107 < .01 < .01 124 < .0

5-Methyl-1H-Benzotriazole < .01 < .01 <10 < .01 < .01 <10 < .01 < .01 <10 < .0

4-Methylphenol .02 .03 43 .03 .03 39 .03 .04 41 .04-Nonylphenol .09 .09 122 .05 .05 131 < .05 < .05 163 < .04-Nonylphenolmonoethoxylate .28 .09 134 .09 .08 137 < .05 < .05 161 < .04-Nonylphenoldiethoxylate < .05 < .05 110 < .05 < .05 117 < .05 < .05 137 < .04-normal-Octylphenol < .01 < .01 12 < .01 < .01 12 < .01 < .01 15 < .0

4-tert-Octylphenol .04 .02 137 .02 .01 138 .02 .01 162 < .04-tert-Octylphenolmonoethoxylate .02 < .01 113 < .01 < .01 115 < .01 < .01 133 < .0

4-tert-Octylphenoldiethoxylate < .01 < .01 109 < .01 < .01 108 < .01 < .01 122 < .0

4-tert-Octylphenoltriethoxylate < .01 < .01 95 < .01 < .01 83 < .01 < .01 91 < .04-tert-Octylphenoltetraethoxylate < .01 < .01 70 < .01 < .01 72 < .01 < .01 73 < .04-tert-Octylphenolpentaethoxylate < .01 < .01 47 < .01 < .01 34 < .01 < .01 45 < .04-tert-Pentylphenol < .01 < .01 122 < .01 < .01 128 < .01 < .01 147 < .04-Propylphenol < .01 < .01 115 < .01 < .01 114 < .01 < .01 122 < .0Triclosan < .01 < .01 100 < .01 < .01 87 < .01 < .01 100 < .0

Surrogate Recovery (percent)d6-Bisphenol A 72 78 78 77 96 99 85 d21-2,6-Di-tert-butyl-4-methylphenol 49 71 59 61 60 89 65 4-normal-Nonylphenol 52 57 53 52 69 76 55 4-normal-Nonylphenolmonoethoxylate 47 52 52 51 74 77 56 4-normal-Nonylphenoldiethoxylate 29 39 41 40 59 63 45 

50
Table 31. Summary of neutral organic compound data for water samples collected from four microhabitat sites in Sullivan Lake, Minn., on October 1

[Microhabitats A and B, residential/septic influenced; microhabitat C, stormwater/boat ramp influenced; microhabitat D, agriculture influenced; μg/L, microgram per liter; <, les

Compound Site A μg/L Site A-Dup μg/L Site B μg/L Site B-Dup μg/L Site C μg/L Site 

μg/

Acetylhexamethyltetrahydronaphthalene 0.02 0.01 0.01 0.02 <0.01 <0.0

Bisphenol A .01 .01 .15 .02 < .01 < .0

2[3]-tert-Butyl-4-methylphenol < .01 < .01 < .01 < .01 < .01 < .0

4-tert-Butylphenol < .01 < .01 < .01 < .01 < .01 < .0

Caffeine .02 .05 .04 .01 < .01 < .0

2,6-Di-tert-butyl-1,4-benzoquinone .06 .09 .04 .06 .04 < .0

2,6-Di-tert-butyl-4-methylphenol .01 .01 < .01 .01 .01 .0

2,6-Di-tert-butylphenol < .01 < .01 < .01 < .01 < .01 < .0

1,2-Dichlorobenzene < .01 < .01 < .01 < .01 < .01 < .0

1,3-Dichlorobenzene < .01 < .01 < .01 < .01 < .01 < .0

1,4-Dichlorobenzene < .01 < .01 < .01 < .01 < .01 < .0

N,N-Diethyl-meta-toluamide .09 .08 .09 .07 < .01 < .0

4-Ethylphenol < .01 < .01 < .01 < .01 < .01 < .0

Hexahydrohexamethylcyclopentabenzopyran .01 .02 < .01 .02 < .01 < .0

5-Methyl-1H-benzotriazole < .01 < .01 < .01 < .01 < .01 < .0

4-Methylphenol < .01 < .01 .02 .01 < .01 < .0

4-Nonylphenol .06 .05 < .05 < .05 < .05 < .0

4-Nonylphenolmonoethoxylate .11 .08 < .05 < .05 < .05 < .0

4-Nonylphenoldiethoxylate < .05 < .05 < .05 < .05 < .05 < .0

4-normal-Octylphenol < .01 < .01 < .01 < .01 < .01 < .0

4-tert-Octylphenol .09 .06 .05 .03 < .01 < .0

4-tert-Octylphenolmonoethoxylate < .01 < .01 < .01 < .01 < .01 < .0

4-tert-Octylphenoldiethoxylate < .01 < .01 < .01 < .01 < .01 < .0

4-tert-Octylphenoltriethoxylate < .01 < .01 < .01 < .01 < .01 < .0

4-tert-Octylphenoltetraethoxylate < .01 < .01 < .01 < .01 < .01 < .0

4-tert-Octylphenolpentaethoxylate < .01 < .01 < .01 < .01 < .01 < .0

4-tert-Pentylphenol < .01 < .01 < .01 < .01 < .01 < .0

4-Propylphenol < .01 < .01 < .01 < .01 < .01 < .0

Triclosan < .01 < .01 < .01 < .01 < .01 < .0

Surrogate Recovery (percent)d6-Bisphenol A 19 40 44 40 39 40 

d21-2,6-Di-tert-butyl-4-methylphenol 20 31 21 38 57 56 

4-normal-Nonylphenol 26 47 37 45 36 43 

4-normal-Nonylphenolmonoethoxylate 52 53 38 43 35 39 

4-normal-Nonylphenoldiethoxylate 44 53 47 53 43 49 

51
Table 32. Summary of steroid and steroidal hormone compound data for water samples collected from four microhabitat sites in Sullivan Lake, Minn

[Microhabitats A and B, residential/septic influenced; microhabitat C, stormwater/boat-ramp influenced; microhabitat D, agriculture influenced; μg/L, microgram per liter; <, lesMS, matrix spike recovery in percent; NQ, not quantifiable]

Compound

Site

A

μg/L

Site

A-Dup

μg/L

Site

A-MS

percent

Site

B

μg/L

Site

B-Dup

μg/L

Site

B-MS

percent

Site

C

μg/L

Site

C-Dup

μg/L

Site

C-MS

percent

Site

D

μg/L

4-Androstene-3,17-dione <0.0001 <0.0001 138 0.0009 0.0005 118 0.0005 0.0005 134 0.001

cis-Androsterone < .0001 < .0001 150 < .0001 < .0001 139 < .0001 < .0001 130 < .000

Cholesterol 5.7 NQ 348 7.6 4.4 266 30 11 -664 23 

Coprostanol .029 .065 104 .042 .025 103 .053 .090 86 .20 

Diethylstilbestrol < .0001 < .0001 97 < .0001 < .0001 66 < .0001 < .0001 97 < .000

Equilenin < .0001 < .0001 105 < .0001 < .0001 86 < .0001 < .0001 101 < .000

Equilin < .0001 < .0001 98 < .0001 < .0001 78 < .0001 < .0001 97 < .000

17α-Estradiol < .0001 < .0001 117 < .0001 < .0001 132 < .0001 < .0001 112 < .000

17β-Estradiol < .0001 < .0001 107 < .0001 < .0001 106 < .0001 < .0001 108 < .000

Estriol < .0001 < .0001 115 < .0001 < .0001 73 < .0001 < .0001 62 < .000

Estrone .0007 .0008 120 .0010 .0009 111 .0011 .0009 110 .000

17α-Ethynylestradiol < .0001 < .0001 110 < .0001 < .0001 100 < .0001 < .0001 103 < .000

Mestranol < .0001 < .0001 107 < .0001 < .0001 99 < .0001 < .0001 106 < .000

Norethindrone < .0001 < .0001 106 < .0001 < .0001 99 < .0001 < .0001 104 < .000

Progesterone < .0001 < .0001 15 < .0001 < .0001 26 < .0001 < .0001 27 < .000

Testosterone < .0001 < .0001 124 < .0001 < .0001 114 < .0001 < .0001 121 < .000

dihydro-Testosterone < .0001 < .0001 130 < .0001 < .0001 109 < .0001 < .0001 123 < .000

epi-Testosterone < .0001 < .0001 128 < .0001 < .0001 121 < .0001 < .0001 120 < .000

11-keto-Testosterone < .0001 < .0001 81 < .0001 < .0001 69 < .0001 < .0001 95 < .000

Surrogate Recovery (percent)d7-Cholesterol 47 <10 37 41 19 10 40 d12-Chrysene 105 106 183 115 115 119 105 

d8-Diethylstibestrol 59 <10 47 18 42 18 34 

13C6-Estradiol 80 18 56 33 36 28 28 

d2-epi-Estriol 42 18 46 49 39 19 16 

13C6-Estrone 96 30 75 97 71 65 97 

d4-Ethynylestradiol 82 26 62 71 47 49 70 d3-Medroxyprogesterone 19 12 45 33 44 35 28 d4-Mestranol 83 30 63 70 48 48 71 d3-Nandrolone 63 24 54 61 54 45 30 

52
Table 33. Summary of steroid and steroidal hormone compound data for water samples collected from four microhabitat sites in Sullivan Lake, Minn

[Microhabitats A and B, residential/septic influenced; microhabitat C, stormwater/boat-ramp influenced; microhabitat D, agriculture influenced; μg/L, microgram per liter; <, les

Compound

Site

A

μg/L

Site

B

μg/L

Site

C

μg/L

4-Androstene-3,17-dione <0.0001 <0.0001 <0.0001 

cis-Androsterone < .0001 < .0001 < .0001 

Cholesterol 3.3 3.4 2.8 

Coprostanol .042 .017 .017 

Diethylstilbestrol < .0001 < .0001 < .0001 

Equilenin < .0001 < .0001 < .0001 

Equilin < .0001 < .0001 < .0001 

17α-Estradiol < .0001 < .0001 < .0001 

17β-Estradiol < .0001 < .0001 < .0001 

Estriol < .0001 < .0001 < .0001 

Estrone < .0001 < .0001 < .0001 

17α-Ethynylestradiol < .0001 < .0001 < .0001 

Mestranol < .0001 < .0001 < .0001 

Norethindrone < .0001 < .0001 < .0001 

Progesterone < .0001 < .0001 < .0001 

Testosterone < .0001 < .0001 < .0001 

dihydro-Testosterone < .0001 < .0001 < .0001 

epi-Testosterone < .0001 < .0001 < .0001 

11-keto-Testosterone < .0001 < .0001 < .0001 

Surrogate Recovery (percent)d7-Cholesterol 39 46 53 

d12-Chrysene 82 94 94 

d8-Diethylstibestrol 80 69 83 

13C6-Estradiol 63 65 58 

d2-epi-Estriol 85 98 97 

13C6-Estrone 118 116 106 

d4-Ethynylestradiol 91 99 92 

d3-Medroxyprogesterone 55 43 47 

d4-Mestranol 103 101 94 

d3-Nandrolone 121 96 98 

53