Scientific Investigations Report 2010–5110

U.S. Department of the Interior

U.S. Geological Survey

Prepared in cooperation with the the U.S. Environmental Protection Agency and the Kickapoo 

Tribe of Oklahoma

A Reconnaissance of Selected Organic Compounds in 

Streams in Tribal Lands in Central Oklahoma, January–

February 2009
Cover: The photograph on the cover is a picture of the North Canadian River near Calumet, taken on 

December 12, 2009, by Joy Savoia, U.S. Geological Survey staff.
A Reconnaissance of Selected Organic 

Compounds in Streams in Tribal Lands in 

Central Oklahoma, January–February 2009

By Carol J. Becker

Prepared in cooperation with the U.S. Environmental Protection Agency and the 

Kickapoo Tribe of Oklahoma 

Scientific Investigations Report 2010–5110

U.S. Department of the Interior

U.S. Geological Survey
6 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

Figure 3. Hydrographs showing streamflow and precipitation during submergence of passive samplers and historical mean daily 

streamflow at U.S. Geological Survey stream-gaging stations in jurisdictional areas of several tribes in central Oklahoma, January–

February 2009. 

Precipitation, in inches

Streamflow, in cubic feet per second

Mean daily streamflow, in cubic feet per second,

for period of record (see table 2)

January 2009 Feburary 2009

Time period during which passive

samplers were submerged

Release from

Canton Lake

Release from

Lake Arcadia

7 14 21 28 7 14 21 28

Release from

upstream reservoirs

Near sample sites 

PS-1 and PS-2

S-1 Cimarron River near Ripley, Oklahoma (07161450)

 (1988-2008)

S-2 Little River near Tecumseh, Oklahoma (07230500)

 (1965-2009)

S-3 North Canadian River near Calumet, Oklahoma (07239450)

 (1988-2008)

North Canadian River near Harrah, Oklahoma (07241550)

 (1969-2008)

S-4 Deep Fork at Warwick, Oklahoma (07242380)

 (1988-2008)

S-5 Washita River near Pauls Valley, Oklahoma (07328500)

 (1962-2009)

EXPLANATION

1

No data

(1988-2009)

1,000

10

100

100

100

1,000

100

1,000

STREAMFLOW, IN CUBIC 

FEET PER SECOND

STREAMFLOW, IN CUBIC 

FEET PER SECOND

STREAMFLOW, IN CUBIC 

FEET PER SECOND

STREAMFLOW, IN CUBIC 

FEET PER SECOND

STREAMFLOW, IN CUBIC

FEET PER SECOND

STREAMFLOW, IN CUBIC 

FEET PER SECOND

200

2,000

20

400

50

2,000

30

400

6

400

3,000

300 0.0

0.5

1.0

0.0

0.5

1.0

1.0

0.0

0.5

0.0

0.5

1.0

0.0

0.5

1.0

0.0

0.5

1.0

PRECIPITATION,

 IN INCHES

PRECIPITATION,

 IN INCHES PRECIPITATION, IN INCHES PRECIPITATION, IN INCHES PRECIPITATION, IN INCHES PRECIPITATION, IN INCHES
iii

Contents

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

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

Purpose and Scope .............................................................................................................................3

Land Use/Cover and Streamflow Conditions ..................................................................................4

Acknowledgments ...............................................................................................................................7

Methods of Study ..........................................................................................................................................7

Site Selection ........................................................................................................................................7

Passive Samplers .................................................................................................................................8

Deployment and Retrieval of Passive Samplers .............................................................................8

Extraction Procedure ..........................................................................................................................8

Laboratory Analysis .............................................................................................................................9

Quality Control ......................................................................................................................................9

Data Reporting ......................................................................................................................................9

Selected Organic Compounds in Streams in Tribal Lands ...................................................................10

Pesticides and Pesticide Metabolites ............................................................................................10

Polychlorinated Biphenyl Compounds and Polycyclic Aromatic Hydrocarbons ....................10

Synthetic Organic Compounds ........................................................................................................12

Summary .......................................................................................................................................................12

References Cited .........................................................................................................................................13

Appendixes

1. Organic compounds as analyzed in extracts from Semipermeable Membrane 

Devices or Polar Organic Chemical Integrative Samplers for this study, including 

suspected endocrine disruption potential, Chemical Abstract Service number, 

possible compound uses or sources, sampler type used to sequester compound, 

and laboratory method used for analysis ..............................................................................19

2. Concentrations of pesticides and pesticide metabolites measured in extracts from 

Semipermeable Membrane Devices submerged at five U.S. Geological Survey 

stream-gaging stations in jurisdictional areas of several tribes in central Oklahoma, 

January–February 2009 ............................................................................................................29

3. Approximate concentrations of pesticides and pesticide metabolites in water 

calculated by using performance reference compounds measured in extracts from 

Semipermeable Membrane Devices submerged at five U.S. Geological Survey 

stream-gaging stations in jurisdictional areas of several tribes in central Oklahoma, 

January–February 2009 ............................................................................................................35

3. Approximate concentrations of pesticides and pesticide metabolites in water 

calculated by using performance reference compounds measured in extracts from 

Semipermeable Membrane Devices submerged at five U.S. Geological Survey 

stream-gaging stations in jurisdictional areas of several tribes in central Oklahoma, 

January–February 2009 ............................................................................................................35

4. Concentrations of pesticides, pesticide metabolites, polychlorinated biphenyl 

compounds, polycyclic aromatic hydrocarbons, and other types of synthetic 

organic compounds measured in extracts from Semipermeable Membrane Devices 

or Polar Organic Chemical Integrative Samplers submerged at two stream sites on 

the North Canadian River adjacent to the Kickapoo tribal lands in central Oklahoma, 

January–February 2009 ............................................................................................................39
The title of figure 3 should read; Streamflow and precipitation during submergence of passive samplers 

and historical mean daily streamflows at U.S. geological Survey streamflow-gaging stations in 

jurisdictional areas of several tribes in central Oklahoma, January-February 2009.
iv

Figures

1–2. Maps showing: 

1. Location of U.S. Geological Survey stream-gaging stations and stream sites 

where passive samplers where submerged in jurisdictional areas of several 

tribes in central Oklahoma, January–February 2009. ...................................................2

2. Land use/cover in central and western Oklahoma during 2001 .................................5

3. Hydrographs showing streamflow and precipitation during submergence of 

passive samplers and historical mean daily streamflow at U.S. Geological Survey 

stream-gaging stations in jurisdictional areas of several tribes in central Oklahoma, 

January–February 2009 ..............................................................................................................6

4–5. Graphs showing: 

4. The number of pesticides and pesticide metabolites detected in extracts from 

Semipermeable Membrane Devices submerged at U.S. Geological Survey 

stream-gaging stations in jurisdictional areas of several tribes in central 

Oklahoma, January–February 2009 ...............................................................................11

5. The number of detections of pesticides, pesticide metabolites, polychlorinated 

biphenyl compounds, polycyclic aromatic hydrocarbons, and other types of 

synthetic organic compounds measured in extracts from Semipermeable 

Membrane Devices or Polar Organic Integrative Samplers submerged at two 

stream sites on the North Canadian River adjacent to the Kickapoo tribal 

lands in central Oklahoma, January–February 2009 ...................................................11

Tables

1. U.S. Geological Survey stream-gaging stations, stream sites, and sample information 

for passive samplers submerged in jurisdictional areas of several tribes in central 

Oklahoma, January–February 2009 ..........................................................................................3

2. Historical streamflow statistics and upstream land use/cover for U.S. Geological 

Survey stream-gaging stations where passive samplers were submerged in 

jurisdictional areas of several tribes in central Oklahoma, January–February 2009 .......7

Conversion Factors

Multiply By To obtain

Length

inch (in) 2.54 centimeter (cm)

mile (mi) 1.61 kilometer (km)

Area

square mile (mi2

) 2.59 square kilometer (km2)

Flow rate

cubic foot per second (ft3/s) 0.028 cubic meter per second (m3/s)

Laboratory reporting level (LRL)—LRLs are the smallest measured compound concentration 

that the laboratory could accurately measure for the analytical method used. LRLs were 

calculated using the lowest equipment calibration standards with the assumption that the 
v

compound spike had a 100 percent recovery and that there were no interferences from the 

sample matrix (Duane Wydoski, U.S. Geological Survey, National Water Quality Laboratory, 

written commun., 2009). The value of the LRL was reported with a “less than” remark code for 

samples in which the analyte was not detected. 

Horizontal coordinate information is referenced to the North American Datum of 1983 (NAD 83).

Concentrations of chemical constituents in water are estimated and given in nanogram of 

compound per liter of water (ng/L). Compound concentrations measured in extracts are 

reported in nanogram per ampoule of extract from a composite of three SPMD or three POCIS 

media in each sampler. 
Heading 1 1

Abstract

The U.S. Geological Survey worked in cooperation with 

the U.S. Environmental Protection Agency and the Kickapoo 

Tribe of Oklahoma on two separate reconnaissance projects 

carried out concurrently. Both projects entailed the use of 

passive samplers as a sampling methodology to investigate 

the detection of selected organic compounds at stream sites in 

jurisdictional areas of several tribes in central Oklahoma during January–February 2009. 

The focus of the project with the U.S. Environmental 

Protection Agency was the detection of pesticides and pesticide metabolites using Semipermeable Membrane Devices at 

five stream sites in jurisdictional areas of several tribes. The 

project with the Kickapoo Tribe of Oklahoma focused on 

the detection of pesticides, pesticide metabolites, polycyclic 

aromatic hydrocarbons, polychlorinated biphenyl compounds, 

and synthetic organic compounds using Semipermeable Membrane Devices and Polar Organic Chemical Integrative Samplers at two stream sites adjacent to the Kickapoo tribal lands. 

The seven stream sites were located in central Oklahoma on 

the Cimarron River, Little River, North Canadian River, Deep 

Fork, and Washita River. 

Extracts from SPMDs submerged at five stream sites, in 

cooperation with the U.S. Environmental Protection Agency, 

were analyzed for 46 pesticides and 6 pesticide metabolites. 

Dacthal, a pre-emergent herbicide, was detected at all five 

sites. Pendimethalin, also a pre-emergent, was detected at one 

site. The insecticides chlorpyrifos and dieldrin were detected 

at three sites and p,p'-DDE, a metabolite of the insecticide 

DDT, also was detected at three sites. 

SPMDs and POCIS were submerged at the upstream edge 

and downstream edge of the Kickapoo tribal boundaries. Both 

sites are downstream from the Oklahoma City metropolitan 

area and multiple municipal wastewater treatment plants. 

Extracts from the passive samplers were analyzed for 62 pesticides, 10 pesticide metabolites, 3 polychlorinated biphenyl 

compounds, 35 polycyclic aromatic hydrocarbons, and 49 

synthetic organic compounds.

Ten pesticides and four pesticide metabolites were 

detected at the upstream site and seven pesticides and four 

pesticide metabolites were detected at the downstream site. 

Pesticides detected at both sites were atrazine, chlorpyrifos, 

dacthal, dieldrin, metolachlor, pendimethalin, and transnonachlor. Additionally at the upstream site, heptachlor, 

pentachlorophenol, and prometon were detected. The pesticide 

metabolites p,p'-DDE, cis-chlordane, and trans-chlordane also 

were detected at both sites.

Polychlorinated biphenyl compounds aroclor-1016/1242, 

aroclor-1254, and aroclor-1260 were detected at both sites. 

The upstream site had 16 polycyclic aromatic hydrocarbon detections and the downstream site had 8 detections. 

Because of chromatographic interference during analysis, 

a positive identification of 17 polycyclic aromatic hydrocarbons could not be made. Consequently, there may have 

been a greater number of these compounds detected at both 

sites. 

A total of 36 synthetic organic compounds were 

detected at the two sites adjacent to the Kickapoo tribal 

lands. The upstream site had 21 synthetic organic compound 

detections: three detergent metabolites, two fecal indicators, 

three flame retardants, seven industrial compounds, five compounds related to personal care products, and beta-sitosterol, 

a plant sterol. Fifteen synthetic organic compounds were 

detected at the downstream site and included: one fecal indicator, three flame retardants, six industrial compounds, and five 

compounds related to personal care products.

Introduction 

Sovereign tribal lands encompass a large part of central Oklahoma (fig. 1). The gathering of aquatic plants and 

animals and particularly fish for consumption from streams 

is a common cultural practice with tribal members. Pesticides 

and other types of synthetic organic compounds (SOCs) are a 

concern to tribal members and the people who use streams as a 

source of food and recreation. 

A Reconnaissance of Selected Organic Compounds in 

Streams in Tribal Lands in Central Oklahoma, January–

February 2009

By Carol J. Becker 
2 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

Figure 1. Location of U.S. Geological Survey stream-gaging stations and stream sites where passive samplers where submerged in jurisdictional areas of several tribes in central Oklahoma, January–February 2009. 

#

!(

!(

!(

!(

!(

!(

!(

!(

#V

#V

#

#

#

#

#

CADDO

GRADY

BLAINE LINCOLN

PAYNE

LOGAN

GARVIN

CANADIAN

KINGFISHER

MCCLAIN

PO

N

OKLAHOMA

POTTAWATOMIE

CLEVELAND

97°30' 98°20'

35°50' 35° Kickapoo Tribal land

Base from U.S. Geological Survey digital data, 1:100,000, 1983U.S. Census Bureau digital data; 1:5,000,000, 200

Albers Equal Area Conic projection, North American Datum 1983

^

S-3

S-1

S-4

S-2

S-5

PS-1

PS-2

Washita River

Little River

Cimarron River

Deep Fork River EXPLANATION

Tribal lands Lake 

Arcadia

LakeThunderbird

LakeCanton

0 10 20 Miles

0 10 20 Kilometers

Canadian River

North Canadian River

Study area

Oklahoma City

^

Ripley

Warwick

Shawnee

Pauls Valley

Calumet

Jones

!( Town

U.S. Geological Survey stream-gaging station (identification 

number) where Semipermeable Membrane Devices were 

deployed (in cooperation with the U.S. Environmetal Protection Agency)

#

Cimarron River near Ripley, Oklahoma (07161450)

and site identifier

Little River near Tecumseh, Oklahoma(07230500) and site identifier

North Canadian River near Calumet, Oklahoma

(07239450) and site identifier

Deep Fork at Warwick, Oklahoma (07242380)

and site identifier

Washita River near Pauls Valley, Oklahoma

(07328500) and site identifier

Stream site (identification number) where Semipermeable Membrane Devices and Polar Organic Integrative Samplers 

were deployed (in cooperation with the Kickapoo Tribe ofOklahoma)

#

V

North Canadian River at Hogback Road near Jones, Oklahoma (07241540) and site identifier

North Canadian River near Shawnee, 

Oklahoma (07241700) and site identifier

#

#

#

#

S-1

S-2

S-3

S-4

S-5

#

VPS-1

PS-2

Oklahoma

Harrah

U.S. Stream-gaging station North Canadian River 

near Harrah, Oklahoma (07241550) and site identifier

#

1

Tecumseh
Introduction 3

A wide variety of SOCs are used today in agriculture, 

pharmaceuticals, chemical manufacturing, and personal care 

products. These compounds may enter streams in surfacewater runoff from agricultural and urban land-use areas and in 

treated wastewater effluent from municipal wastewater treatment plants. The detection and types of SOCs in groundwater 

and surface water have been the focus of many studies over the 

last decade (Galloway and others, 2004; Masoner and Mashburn, 2004; Tertuliani and others, 2008). The frequency with 

which these compounds are detected in streams was shown by 

Kolpin and others (2002) in a study that found 80 percent of 

139 streams sampled across the United States had detectable 

concentrations. Many of these compounds are suspected or 

are known endocrine disruptors that can influence or interfere 

with the hormonal system of growing organisms (Rhomberg 

and Seeley, 2005; Tulane and Xavier Universities, 2009a) 

causing reproductive and developmental problems. In humans, 

the potential health effects are debatable, but research has 

shown that the consumption of low concentrations of SOCs 

or mixtures can contribute to female reproductive disorders 

(Crain and others, 2008). There also is speculation of other 

health concerns, especially to growing embryos and fetuses 

(Tulane and Xavier Universities, 2009b).

In an effort to look more closely at pesticides and other 

types of SOCs in streams in Oklahoma, the U.S. Geological Survey (USGS) Oklahoma Water Science Center worked 

in cooperation with the U.S. Environmental Protection 

Agency (US EPA) and the Kickapoo Tribe of Oklahoma on 

two separate but similar reconnaissance projects carried out 

concurrently. Both projects entailed the use of passive samplers, Semipermeable Membrane Devices (SPMD) and Polar 

Organic Chemical Integrative Sampler (POCIS) as a surfacewater sampling methodology to detect SOCs.

Purpose and Scope

The purpose of this report is to describe the results from a 

reconnaissance of selected organic compounds in streams, performed from January 15 through February 19, 2009 that used 

passive samplers at seven stream sites in jurisdictional areas of 

several tribes (fig. 1 and table 1).

In cooperation with the Kickapoo Tribe of Oklahoma, 

SPMDs and POCIS were submerged at two stream sites, 

referred to as PS-1 and PS-2, on the North Canadian River 

in Oklahoma and Pottawatomie counties adjacent to the 

Table 1. U.S. Geological Survey stream-gaging stations, stream sites, and sample information for passive samplers submerged in 

jurisdictional areas of several tribes in central Oklahoma, January–February 2009.

[USGS, U.S. Geological Survey; POCIS, Polar Organic Chemical Integrative Sampler; SPMD, Semipermeable Membrane Device; PAH, polycyclic aromatic 

hydrocarbon; PCB, polychlorinated biphenyl compound; SOC, synthetic organic compound]

USGS 

station 

number

Site 

identifierUSGS stream-gaging station

Passive 

sampler 

type 

deployed

Types and number of 

organic compounds 

analyzed

Laboratory method

USGS stream-gaging stations where passive samplers were submerged in cooperation with the U.S. Environmental Protection Agency

07161450 S-1 Cimarron River near Ripley, Oklahoma SPMD 46 Pesticides, 

6 metabolites

Zaugg and others (1995)

07230500 S-2 Little River near Tecumseh, Oklahoma SPMD 46 Pesticides, 

6 metabolites

Zaugg and others (1995)

07239450 S-3 North Canadian River near Calumet, Oklahoma SPMD 46 Pesticides, 

6 metabolites

Zaugg and others (1995)

07242380 S-4 Deep Fork at Warwick, Oklahoma SPMD 46 Pesticides, 

6 metabolites

Zaugg and others (1995)

07328500 S-5 Washita River near Pauls Valley, Oklahoma SPMD 46 Pesticides, 

6 metabolites

Zaugg and others (1995)

Stream sites where passive samplers were submerged in cooperation with the Kickapoo Tribe of Oklahoma

07241540 PS-1 North Canadian River at Hogback Road near Jones, 

Oklahoma

POCIS

SPMD

62 pesticides, 

10 metabolites, 

3 PCBs, 35 PAHs,

49 SOCs 

Noriega and others (2004);

Zaugg and others (1995; 

2006; 2007) 

07241700 PS-2 North Canadian River near Shawnee, Oklahoma POCIS

SPMD

62 pesticides, 

10 metabolites, 

3 PCBs, 35 PAHs,

49 SOCs

Noriega and others (2004);

Zaugg and others (1995; 

2006; 2007)
4 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

Kickapoo tribal lands (fig. 1). Sites PS-1 and PS-2 were about 

9 miles upstream and about 24 miles downstream, respectively, from the USGS stream-gaging station North Canadian 

River near Harrah, Oklahoma (fig. 1 and table 1). Extracts 

from the POCIS and SPMDs deployed at PS-1 and PS-2, 

were analyzed for 62 pesticides, 10 pesticide metabolites, 3 

polychlorinated biphenyl compounds (PCB), 35 polycyclic 

aromatic hydrocarbons (PAH), and 49 SOCs by using the laboratory methodologies described by Noriega and others (2004) 

and Zaugg and others (1995; 2006; 2007). Nine pesticides, one 

metabolite, and eight PAHs were analyzed by using more than 

one laboratory methodology. 

In cooperation with the US EPA, SPMDs were submerged at five stream sites, referred to as S-1 through S-5, 

located at USGS stream-gaging stations; Cimarron River near 

Ripley, Oklahoma (07161450), Little River near Tecumseh, 

Oklahoma (07230500), North Canadian River near Calumet, 

Oklahoma (07239450), Deep Fork at Warwick, Oklahoma 

(07242380), and the Washita River near Pauls Valley, Oklahoma (07328500) in Payne, Pottawatomie, Canadian, Lincoln, 

and Garvin counties (respectively) in central Oklahoma (fig. 1 

and table 1). Extracts from the SPMDs were analyzed for 46 

pesticides and 6 pesticide metabolites by using the laboratory 

methodology described in Zaugg and others (1995) (appendixes 1 and 2). Approximate concentrations in water were 

calculated for the pesticides and pesticide metabolites and are 

shown in appendix 3. 

Land Use/Cover and Streamflow Conditions

Land use/cover has an effect on the types and frequencies 

of pesticides detected in surface water. USGS studies between 

1992 and 2001 showed that pesticides were most frequently 

detected in agricultural and urban areas and the types detected 

were primarily those with the greatest use (Gilliom and others, 2006). Streams in urban areas had higher detections of 

insecticides and herbicides used for nonagricultural purposes. 

Pesticides that were most frequently detected in agricultural 

and urban areas were atrazine, metolachlor, prometon, and 

simazine, and the atrazine metabolite deethylatrazine.

Land use/cover varies in Oklahoma from grassland and 

agriculture in the west to hay/pasture and forest in the east 

(fig. 2). The greatest density of urban development in the study 

area is in Oklahoma County in and surrounding Oklahoma 

City. 

In agricultural areas, cultivated crops are dominated by 

the production of wheat, with alfalfa, sorghum, and other small 

grain crops grown in smaller amounts. Pesticides are generally 

applied during the growing season from spring to autumn to 

control weeds, insects, and fungus on crops. Correspondingly, 

pesticides are a much greater concern in streams and groundwater during these times of the year. Pesticide use during winter is negligible in Oklahoma, but pre-emergent herbicides are 

used occasionally to deter the growth of winter grasses for the 

wheat spring growing season (Brad Tipton, Canadian County 

Agriculture Educator, written commun., 2008). Herbicides 

commonly applied for weed control during the winter months 

in Canadian County are sulfonylurea compounds which were 

not analyzed in this study.

Grassland covers the largest percentage of land in the 

upstream basins for five of the six gages, including the Harrah 

gage near sites PS-1 and PS-2 (table 2). Upstream from the 

Tecumseh gage, deciduous forest covers the largest percentage of land and grassland the second. Cultivated crops are the 

second largest land use in the upstream basins of the Ripley, 

Calumet, Harrah, and Pauls Valley gages. Urban development 

is the third largest land use upstream from the Tecumseh, 

Harrah, and Warwick gages making up 11, 4, and 16, percent, 

respectively.

The Ripley gage at S-1 has the largest upstream drainage 

area of 17,979 square miles (mi2

) and the largest annual mean 

streamflow of 2,236 cubic feet per second (ft3/s) during the 

period of record 1988 to 2008 (table 2). The Tecumseh gage 

at S-2 has the smallest upstream drainage area of 456 mi2 

and the smallest annual mean streamflow of 146 ft3/s (period 

of record 1965 to 2009). Streamflow data are available from 

the USGS National Water Information System website, 

http://waterdata.usgs.gov/nwis. 

The Calumet gage, at S-3 has an upstream drainage area 

of 12,962 mi2 and an annual mean streamflow of 268 ft3/s 

during the period of record 1988 to 2008 (table 2). An increase 

in streamflow, not related to precipitation, is periodically measured at the Calumet gage as a result of releases from Lake 

Canton about 60 miles upstream. The effect on streamflow 

from a release can be seen on figure 3 beginning on February 

15, as an increase from 80 ft3/s to 250 ft3/s about 4 days before 

the passive sampler was retrieved. 

The Warwick gage at S-4, has the second smallest 

drainage area of 532 mi2 and the second smallest annual 

mean streamflow of 260 ft3/s, during the period of record 

1988 to 2008 (table 2). The headwaters of the basin upstream 

from the Warwick gage begin in the northern parts of the 

Oklahoma City metropolitan area and flow into Lake Arcadia, 

which is the primary source of streamflow to the Deep Fork 

(fig. 1). Streamflow periodically increases because of releases 

from Lake Arcadia. The effects on streamflow are shown 

on figure 3, as an increase of about 60 ft3/s beginning on 

February 23, 2009 about 4 days after the passive sampler was 

retrieved.

The Harrah station, near sites PS-1 and PS-2, has an 

upstream drainage area of 13,501 mi2

 and an annual mean 

streamflow of 500 ft3/s during the period of record 1969 to 

2008 (table 2). Streamflow on the North Canadian River near 

the Harrah gage is periodically affected by water released 

from upstream reservoirs and from a series of low-water weirs 

adjacent to Oklahoma City. Streamflow also may be affected 

by periodic releases of treated effluent from multiple upstream 

municipal wastewater treatment plants, but the magnitude of 

these effects is unknown. Releases from upstream reservoirs 

are apparent on figure 3 as an increase in streamflow beginning on February 19. 
Introduction 

5Figure 2. Land use/cover in central and western Oklahoma during 2001.

#

#

# #

#

#V

#V

S-5

S-4

S-3

S-2

S-1

97° 98° 99° 100°

37°36°35°

PS-1

PS-2

0 50 25 Miles0 25 50 Kilometers

National Land Cover Data Set, 2001U.S. Geological Survey digital data, 1:100,000Albers Equal Area Conic projection, North American Datum 1983

Area shown

Oklahoma

^

S-1

Stream site where Semipermeable Membrace Devices and 

Polar Organic Integrative Samplers were deployed with site

U.S. Geological Survey streamgaging station where Semipermeable Membrance Devices weredeployed with site identifier

identifier

PS-1

Drainage basin boundary

#V

EXPLANATION

Cultivated crops

Deciduous forest

Evergreen forest

Grassland

Pasture/HayShrub/scrub

Urban development, low 

intensity and open space

Urban development, medium and high intensity

Water

Kickapoo Tribal land

^ Oklahoma City
6 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

Figure 3. Hydrographs showing streamflow and precipitation during submergence of passive samplers and historical mean daily 

streamflow at U.S. Geological Survey stream-gaging stations in jurisdictional areas of several tribes in central Oklahoma, January–

February 2009. 
Methods of Study 7

Acknowledgments

The author would like to thank Genevieve McGeisey 

and Darren Shields with the Kickapoo Tribe of Oklahoma for 

their assistance with the project. Appreciation also is given 

to Chad Ashworth, Mark Becker, Rick Hanlon, Stan Paxton, 

Ernie Smith, and Kim Winton at the USGS Oklahoma Water 

Science Center for their assistance with the project. The 

advice and guidance provided by Duane Wydoski at the USGS 

National Water Quality Laboratory in Denver, Colorado was 

invaluable. Thanks are given to Jason Masoner with the USGS 

Oklahoma Water Science Center and David Alvarez with the 

USGS Columbia Environmental Research Center for their peer 

reviews of the manuscript.

Methods of Study

SPMDs were deployed at all seven stream sites S-1 

through S-5 and PS-1 and PS-2. POCIS were deployed, in 

addition to SPMDs, at stream sites PS-1 and PS-2. Both types 

of passive samplers were submerged in streams from January 

15 through February 19 during low flow, when streamflow 

conditions generally were less than the daily mean flow for the 

period of record.

The SPMD and POCIS passive samplers have several 

advantages over surface-water grab samples. Passive samplers 

provide water-quality information during an integrated period 

of time, usually weeks, and during a range of hydrologic 

conditions. In contrast, grab samples are collected at a single 

point and only provide site-specific water-quality information for a snapshot in time. The extended exposure time of the 

passive samplers to water increases the likelihood of detecting constituents that might be in the stream only intermittently (Alvarez and others, 2004). Additionally, the SPMD 

media sequester chemicals similarly to aquatic biota and can 

provide information about the bioavailability of hydrophobic 

chemicals in streams not typically measured in water samples 

(Environmental Sampling Technologies, 2008).

Site Selection

Stream sites S-1 through S-5 were at USGS streamgaging stations; whereas, PS-1 and PS-2 were near bridges 

about 9 miles upstream and about 24 miles downstream 

(respectively) from the stream-gaging station North Canadian 

River near Harrah, Oklahoma, (07241550) (fig. 1 and table 2). 

Sample sites PS-1 and PS-2 were selected on the upstream and 

downstream boundaries of the Kickapoo tribal land. Multiple 

upstream wastewater treatment plants (2009) are permitted to 

Table 2. Historical streamflow statistics and upstream land use/cover for U.S. Geological Survey stream-gaging stations where 

passive samplers were submerged in jurisdictional areas of several tribes in central Oklahoma, January–February 2009.

[USGS, U.S. Geological Survey; ft3/s, cubic feet per second; mi2, square miles]

USGS 

station 

number

Site 

identifier

U.S. Geological 

Survey 

stream-gaging 

station 

Historical 

daily mean low 

flow/high flow

 for January 1

 to February 28

(ft3

/s)

Annual 

mean 

streamflow

(ft3

/s)

Period of 

record

(water 

year)

Upstream 

drainage area /

contributing 

drainage area

(mi2

)

Percentages of the three 

largest land use/cover 

categories in the upstream 

drainage basin

07161450 S-1 Cimarron River near 

Ripley, Oklahoma

902/

2,730

2,236 1988/

2008

17,979 /

13,053

48 percent grassland

35 percent cultivated crops

5 percent shrub/scrub

07230500 S-2 Little River near 

Tecumseh, 

Oklahoma

38/

306

146 1965/

2009

456 / 

456

44 percent deciduous forest 

35 percent grassland

11 percent urban development

07239450 S-3 North Canadian River 

near Calumet, 

Oklahoma

133/

389

268 1988/

2008

12,962 / 

8,063

65 percent grassland 

24 percent cultivated crops 

6 percent shrub/scrub

07241550 near PS-1

and PS-2

North Canadian 

River near Harrah, 

Oklahoma

267/

651

500 1969/

2008

13,501 /

8,602

63 percent grassland

25 percent cultivated crops 

4 percent urban development

07242380 S-4 Deep Fork at 

Warwick, 

Oklahoma

92/

326

260 1988/

2008

532 /

532

39 percent grassland 

37 percent deciduous forest

16 percent urban development

07328500 S-5 Washita River near 

Pauls Valley, 

Oklahoma

509/

1,070

965 1962/

2009

5,330 /

5,330

50 percent grassland 

28 percent cultivated crops 

11 percent shrub/scrub 
8 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

discharge treated wastewater effluent into the North Canadian 

River (Oklahoma Department of Environmental Quality, 2009) 

upstream from the Kickapoo tribal boundary (fig. 1). The PS-1 

sample site was at the western edge of the tribal boundary 

upstream from areas used by the tribe for ceremonies. Samplesite PS-2 was established downstream on the eastern edge 

of the tribal boundary to detect pesticides and other types of 

SOCs leaving the tribal jurisdictional area. 

Deployment sites were selected where stream depth and 

flow were adequate for the entire period of submergence. The 

sampler had to remain submerged in moving water and placed 

so it could be safely deployed and retrieved during high flow, 

if necessary. The sampler also needed to be where the chance 

of floating debris and vandalism were minimal.

Passive Samplers

Three SPMDs in a canister were deployed at each stream 

site. Each SPMD consisted of lipid-filled polyethylene tubing, 

91.4 centimeters long and 2.5 centimeters wide, wound around 

posts on a support rack to maximize surface exposure. The 

polyethylene tubing has transport properties that selectively 

allow hydrophobic compounds in water to partition into the 

SPMD and be retained by the membrane and a thin film of 

triolein (lipid). The lipid and membrane collectively sequesters 

the compounds that are later extracted and analyzed (Environmental Sampling Technologies, 2008). 

The triolein was spiked before deployment with four 

polychlorinated biphenyl compounds (PCB-4, 14, 29, and 50) 

that were used as performance reference compounds (PRC). 

As described in detail by Huckins and others (2006) and Tertuliani and others (2008) the PRCs provide an estimate of SPMD 

sampling rates at each sample site, which varies depending on 

environmental factors such as temperature, water velocity, and 

membrane biofouling. The rate of PRC loss from the SPMD 

membranes during stream submergence was compared to that 

of the PRC loss during laboratory calibration studies to derive 

an exposure adjustment factor, which was used to determine 

more accurate in situ sampling rates. This information was 

used in combination with SOC partition coefficients and 

concentrations measured in sample extracts to estimate timeweighted water concentrations by using the exposure models 

created by Huckins and others (2006) and the U.S. Geological 

Survey, Columbia Environmental Research Center (2006). 

Three POCIS in a canister were deployed only at stream 

sites PS-1 and PS-2. Each POCIS is composed of sorbent 

materials enveloped by a microporous polyethersulfone 

membrane. The membrane allows dissolved constituents to 

flow through and be sequestered while filtering out sediment 

and debris (U.S. Geological Survey, Columbia Environmental 

Research Center, 2004). The POCIS was used to sample for 

dissolved SOCs that included selected pesticides, detergent 

metabolites, fecal indicators, flame retardants, industrial 

compounds, and compounds related to personal care products 

(appendix 1). The compounds were later extracted from the 

sorbent and analyzed. 

Deployment and Retrieval of Passive Samplers

The SPMDs and POCIS were purchased from Environmental Sampling Technologies, St. Joseph, Missouri, and were 

sent to the USGS Oklahoma Water Science Center surrounded 

by argon gas in sealed metal cans. The cans containing the 

SPMDs were kept at -20° Celsius until the day of deployment 

and then chilled on ice until submergence at the deployment 

sites. 

During deployment the SPMDs and POCIS media, 

preloaded on support racks, were removed from the original 

metal cans and placed in a protective stainless steel canister 

as quickly as possible. The support racks were handled with 

clean gloved hands and SPMD and POCIS surfaces were not 

touched or abraded. USGS personnel refrained from the use of 

personal care products and caffeine on the day of deployment.

Canisters at six stream sites were secured to T-posts 

with a length of stainless steel chain and one canister was 

secured to the bridge. During retrieval, canisters were moved 

from the water and the passive samplers on the support 

racks were removed and returned to the original metal cans, 

sealed, and placed on ice. The sealed cans were transported 

back to USGS Oklahoma Water Science Center and were 

stored at -20° Celsius until being placed on ice and shipped 

overnight to Environmental Sampling Technologies for 

extraction. 

Extraction Procedure

The sequestered SOCs were extracted from the SPMDs 

and POCIS by Environmental Sampling Technologies. 

SOCs in the POCIS were extracted with 40 milliliters of 

methanol and concentrated under ultra high purity nitrogen. The extracts were transferred to methanol, filtered 

through a glass fiber filter (Fisher, G-6) and quantitatively 

transferred to 2-milliliter amber ampoules (Terri Spencer, 

Environmental Sampling Technologies, written commun., 

2009). 

Briefly, SOCs and performance reference compounds 

were extracted from the SPMDs by dialysis in hexane, 

concentrated by using the Kuderna-Danish method (Dean, 

2010), reduced in volume under ultra high purity nitrogen 

to about 0.5 milliliter, and then filtered through a glass fiber 

filter (Fisher, G-6) by using methylene chloride. Sample 

volumes were again reduced under ultra high purity nitrogen 

and quantitatively transferred to auto sampler vials by using 

methylene chloride as the transfer solvent. Samples underwent final clean-up by gel permeation chromatography, were 

again reduced in volume with ultra high purity nitrogen, and 

quantitatively transferred with methylene chloride to 2-milli-
Methods of Study 9

liter amber ampoules (Terri Spencer, Environmental Sampling 

Technologies, written commun., 2009).

The final SPMD and POCIS extracts for each sampling 

site were a composite of the three samplers in a canister for 

each sampler type. Similarly, the field blanks were combined 

into an extract for each sampler type. 

Laboratory Analysis

SPMD and POCIS extracts were analyzed by the USGS 

National Water Quality Laboratory (NWQL) in Lakewood, 

Colorado using custom methodologies (Duane Wydoski, 

U.S. Geological Survey, National Water Quality Laboratory, 

written commun., 2009). SPMD extracts from the sites S-1 

through S-5 and PS-1 and PS-2 were analyzed for 46 pesticides and 6 pesticide metabolites by using the technique 

described in Zaugg and others (1995). The methylene chloride 

solvent containing the extracts was replaced by a mixture of 

ethyl acetate and toluene. The solvent mixture was then analyzed by using gas chromatography/mass spectrometry by 

positive ion electron-impact ionization in the selected-ion 

mode. Each compound was identified in the extract by comparing curves to analytical standards and National Institute 

of Science and Technology reference spectra. The compound 

concentration in the extract was determined by using a 

six-point curve based on calibration that was normalized to 

internal standards.

A portion of the PS-1 and PS-2 SPMD extracts was 

replaced with hexane and analyzed for 14 pesticides, 4 pesticide metabolites and 3 PCB compounds by using the technique described in Noriega and others (2004) (appendix 4). 

The extracts were cleaned by using alumina/silica combined 

column adsorption chromatography and were split into two 

fractions. The second fraction underwent an additional adsorption chromatography step by using a Florisil column for 

cleanup. Both fractions were analyzed by dual capillarycolumn gas chromatography with electron-capture detection 

that was calibrated for both capillary columns by using multipoint calibration standards. The compound concentrations 

in the extracts were determined by using a six-point curve 

based on calibration standards that were normalized to internal 

standards. 

SPMD extracts from PS-1 and PS-2 also were analyzed 

for 2 pesticides, 32 PAHs, and 4 SOCs (appendixes 1 and 4) 

and performance reference compounds by using the instrumental conditions described in Zaugg and others (2006). 

The extracts in methylene chloride were analyzed by using 

gas chromatography/mass spectrometry by positive ion 

electron-impact ionization in the selected-ion mode. Each 

compound was identified in the extract by comparing curves 

to analytical standards and National Institute of Science and 

Technology reference spectra. Compound concentration in 

the extract was determined by using a six-point curve based 

on calibration standards that were normalized to internal 

standards. 

POCIS extracts from PS-1 and PS-2 were analyzed for 8 

pesticides, 11 PAHs, and 43 SOCs, many of which are considered indicators of wastewater effluent (appendixes 1 and 4), by 

using the technique and instrumental conditions described in 

Zaugg and others (2007). The extracts in methylene chloride, 

in addition to a set of multiple-level analytical standard solutions, were analyzed by full scan positive-ion gas chromatography/mass spectrometry in the electron-impact mode.

Quality Control

Quality control blanks were used to assess unintentional 

contamination in the field and in the laboratory. A field blank 

consisting of three SPMDs was processed with the SPMDs 

deployed at sites S-1 through S-5. A second field blank consisting of three SPMDs and three POCIS was processed with 

samplers deployed at PS-1 and PS-2. 

 Laboratory blanks and spikes were used by NWQL to 

assess the preparation, analyte recovery, and to check the 

performance of the analytical methods. Field and laboratory 

blanks and spike information are shown on appendixes 2 

and 4.

Data Reporting

The detection or nondetection of a compound is used 

for descriptive and comparative purposes in the report and 

not the laboratory or calculated water concentrations. A compound was considered detected if it was measured in 

the extract at a concentration three times, or greater, than 

the highest concentration measured in the field or laboratory 

blank. 

Compound concentrations measured in extracts are 

reported in nanogram per ampoule of extract from a composite of three SPMD or three POCIS media in each sampler. 

These extract concentrations are shown in appendixes 2 and 

4. Approximate water concentrations in nanogram per liter 

(ng/L) were calculated for selected pesticides, PCB compounds, and PAHs (appendixes 3 and 4).

Compound concentrations are reported above the laboratory reporting level which is the smallest measured compound 

concentration that the laboratory could accurately measure for 

the analytical method used. Laboratory reporting levels were 

calculated by using the lowest equipment calibration standards with the assumption that the compound spike had a 100 

percent recovery with no interferences from the sample matrix 

(Duane Wydoski, U.S. Geological Survey, National Water 

Quality Laboratory, written commun., 2009). 

The presence of many compounds could not be positively identified at less than the laboratory reporting level 

because of chromatographic interference during analysis at the 

laboratory. These concentrations are preceded by a less than 

sign (<) and are considered nondetections.
10 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

Seventeen compounds were analyzed in the SPMD and 

POCIS extracts from PS-1 and PS-2 by two different laboratory methodologies. Dieldrin and p, p ́-DDE were the only 

compounds detected in both sampler extracts; both compounds 

are counted only once as a detection in the report. 

Selected Organic Compounds in 

Streams in Tribal Lands

Extracts from the SPMDs deployed at S-1 through S-5 

were analyzed for 46 pesticides and 6 pesticide metabolites 

(appendix 2). Extracts from the POCIS and SPMDs deployed 

at PS-1 and PS-2, were analyzed for, 10 pesticide metabolites, 

3 PCBs, 35 PAHs, and 49 SOCs. Nine pesticides, one pesticide metabolite, and eight PAHs were analyzed in extracts 

from samplers deployed at the two sites by using more than 

one laboratory methodology. Approximate concentrations in 

water were calculated for selected pesticides and pesticide 

metabolites and are shown in appendixes 3 and 4.

Pesticides and Pesticide Metabolites

Sites S-1 through S-5 had one to four pesticides detected 

of the 46 analyzed in SPMD extracts (fig. 4). Sites PS-1 and 

PS-2 had 10 and seven pesticides detected, respectively, of 

the 62 pesticides analyzed in extracts from both sampler 

types (fig. 5 and appendix 4). All seven sites had detections 

of dacthal, a preemergent herbicide. Three sites, PS-1, PS-2, 

and S-4 also had detections of pendimethalin, a pre-emergent 

herbicide. Five sites (excluding S-2 and S-3) had detections 

of the insecticides dieldrin and chlorpyrifos. Chlorpyrifos, 

commonly called Dursban, was banned for domestic use in 

June 2000 but is still used for agriculture, wood treatment, 

and on golf courses (U.S. Environmental Protection Agency, 

2002b). Five sites had detections of p,p'-DDE, a metabolite 

of the insecticide DDT. Dieldrin and DDT are organochlorine 

pesticides that were banned in the U.S. more than 20 years ago 

and are referred to as legacy pesticides because of persistence 

and widespread detection in the environment (Gilliom and 

others, 2006), 

In addition to the four pesticides detected at S-1 through 

S-5, the herbicides atrazine, metolachlor, pentachlorophenol, 

and prometon and the insecticides heptachlor and transnonachlor were detected at PS-1; atrazine, metolachlor, and 

trans-nonachlor also were detected at PS-2. The pesticide 

metabolites, cis-chlordane and trans-chlordane, of the legacy 

insecticide chlordane, also were detected at sites PS-1 and 

PS-2. These pesticides and pesticide metabolites, except for 

dacthal, metolachlor, and prometon, are suspected or are 

known to have endocrine disruptor potential (Kegley and 

others, 2008). 

Concentrations of three detected pesticides and one 

metabolite are regulated in public-drinking water by the US 

EPA with maximum contaminant levels (MCLs) of atrazine 

(3,000 ng/L), heptachlor (400 ng/L), heptachlor epoxide 

(200 ng/L), and pentachlorophenol (1,000 ng/L) (U.S. Environmental Protection Agency, 2009a). All four compounds 

have potential health effects from ingestion ranging from 

reproduction problems to an increased risk of cancer (U.S. 

Environmental Protection Agency, 2009a). However, based 

on SPMD results, the approximate water concentrations 

of heptachlor and heptachlor epoxide representing stream 

samples are small, about 2,000 to 4,000 times smaller than 

the respective MCLs in drinking water. The water concentrations of atrazine and pentachlorophenol could not be estimated 

because these two compounds were sequestered by the POCIS 

sampler, which did not have PRCs needed for the calculations.

Increases in concentrations of many water-quality constituents were detected in the downstream direction of 

the North Canadian River from the Calumet station to the 

Harrah station by Brigham and others (2002). A summary 

of water-quality data from 1988 to 1999 showed that while 

specific conductance and concentrations of dissolved solids 

and sulfate decreased in the downstream direction, chloride, 

total dissolved concentrations of nitrogen and phosphorus 

compounds, and many pesticides increased in the downstream 

direction. Increases in chloride and nutrient concentrations 

may be related to effluent from wastewater treatment plants 

but also can result from urban runoff or natural sources. 

Brigham and others (2002) reported that the frequencies 

of detection for 12 of 13 pesticides increased between the 

Calumet gage and the Harrah gage. Pesticides having the 

highest frequencies of detection (in 44 to 63 samples) at the 

Harrah gage were the herbicides 2,4-D (83 percent), atrazine 

(17 percent), and simazine(67 percent), and the insecticides 

diazinon (90 percent), dieldrin (82 percent), and lindane (96 

percent). The frequencies of detection ranged from 77 percent 

for atrazine and 96 percent for lindane. 

Brigham and others (2002) reported that the herbicide 

2,4-D and the insecticide lindane were the most frequently 

detected pesticides in stream samples collected at four sites 

on the North Canadian River from 1988 to 1999. Atrazine and 

dieldrin were detected at sites PS-1 and PS-2 (near the Harrah 

gage), whereas, diazinon, lindane, and simazine were not. 

2,4-D was not analyzed in this study. 

Nationwide, Gilliom and others (2006) reported that 

USGS studies from 1992 to 2001 showed that the pesticides 

most frequently detected in streams draining agricultural and 

urban areas were the herbicides atrazine, metolachlor, prometon, and simazine, and the metabolite of atrazine, deethylatrazine. None of these compounds were detected at sites S-1 

through S-5. At sites PS-1 and PS-2, atrazine and metolachlor 

were detected in addition to prometon, a nonagricultural herbicide, at PS-1. 
Selected Organic Compounds in Streams in Tribal Lands 11

Figure 4. The number of pesticides and pesticide metabolites detected in extracts from Semipermeable Membrane Devices 

submerged at U.S. Geological Survey stream-gaging stations in jurisdictional areas of several tribes in central Oklahoma, January–

February 2009. 

Figure 5. The number of detections of pesticides, pesticide metabolites, polychlorinated biphenyl compounds, polycyclic aromatic 

hydrocarbons, and other types of synthetic organic compounds measured in extracts from Semipermeable Membrane Devices or Polar 

Organic Integrative Samplers submerged at two stream sites on the North Canadian River adjacent to the Kickapoo tribal lands 

in central Oklahoma, January–February 2009. 

0

1

2

3

4

S-1 S-2 S-3 S-4 S-5

Sample sites

NUMBER OF DETECTIONS

S-5 Washita River near Pauls 

Valley, Oklahoma (07328500)

S-1 Cimarron River near 

Ripley, Oklahoma (07161450)

S-2 Little River near Tecumseh, 

Oklahoma (07230500)

S-3 North Canadian River near

Calumet, Oklahoma (07239450)

S-4 Deep Fork at Warwick, 

Oklahoma (07242380) 

U.S. Geological Survey

stream-gaging stations

where Semipermeable

Membrane Devices were

submerged

Metabolite

Pesticide

EXPLANATION

0

2

4

6

8

10

12

14

16

NUMBER OF DETECTIONS

PS-2 North Canadian River 

near Shawnee, Oklahoma 

(07241700)

PS-1 North Canadian River

at Hogback Road near 

Jones, Oklahoma (07241540)

EXPLANATION

PCB polychlorinated biphenyl

 compound

PAH polycyclic aromatic hydrocarbon

PCP personal care product

Pesticide

Pesticide metabolite

PCB

PAH

Detergent metabolite

Fecal indicator

Flame retardent

Industrial

PCP

Plant sterol
12 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

Polychlorinated Biphenyl Compounds and 

Polycyclic Aromatic Hydrocarbons

Sites PS-1 and PS-2, had detections of the PCB compounds aroclor-1016/1242, aroclor-1254, and aroclor-1260. 

PCBs were used in many types of industrial applications, such 

as plasticizers, flame retardants, sealants, dielectric fluids, and 

adhesives (U.S. Environmental Protection Agency, 2009a). 

PCBs were banned in 1976, but are still found throughout the 

environment, as these compounds are persistent and attenuate 

slowly. The MCL for PCB compounds in drinking water is 

5,000 ng/L. The sum of those three compound concentrations 

approximated in stream water at PS-1 and PS-2 is small, less 

than 6 ng/L. 

PAHs compose a large group of organic compounds 

that are formed by the incomplete combustion of coal, oil, 

gas, wood, and other organic substances and are found in 

the environment in soil, water, or air attached to particulates. 

Selected PAHs are used in the manufacture of explosives and 

mothballs, are found in cigarette smoke, and are used in cancer 

research (U.S. Environmental Protection Agency, 1995). 

Site PS-1 had 16 PAH detections and PS-2 had 8 detections of the 35 PAHs analyzed. Because of chromatographic 

interference during analysis, a positive identification of 17 

PAHs in extracts from PS-1 and 18 in PS-2 could not be made. 

Consequently, there may have been a greater number of PAH 

compounds in extracts from these two sites. 

Five PAHs only detected at PS-1, benzo(a)anthracene, 

benzo(b)fluoranthene, benzo(ghi)perylene, benzo(k)fluoranthene, and chrysene, are considered to have endocrine 

disruption potential (Kegley and others, 2008) and except for 

benzo(ghi)perylene, are considered probable human carcinogens by the U.S. Environmental Protection Agency (2002a). 

Fluoranthene and pyrene had the largest approximate concentrations in water of the PAHs detected at PS-1 (12.6 and 12.3 

ng/L) and at PS-2 (6.12 and 5.11 ng/L), respectively. None of 

the detected PAHs have MCLs for drinking water. 

Synthetic Organic Compounds 

SOCs were grouped into five categories on the basis of 

a common use of the compound; detergent metabolite, fecal 

indicator, flame retardant, industrial compound, and PCP 

(fig. 5). Seven SOCs were categorized as industrial because 

these compounds are used in the manufacture of many types 

of products, such as pentachloroanisol, which is used in the 

manufacture of polymers, pesticides, and fire retardants and 

is also used as a wood preservative. The compound betasitosterol is a natural plant sterol and also is used as a vitamin 

supplement. This compound was detected at PS-1; however, 

because the compound is natural, it was not included in the 

five compound use groups. 

Similar to the PAHs, chromatographic interference during 

laboratory analysis affected the positive identification of SOCs 

in extracts from both sites. Consequently, the presence of 12 

SOCs from PS-1 and 4 SOCs from PS-2 could not be determined. An additional eight SOCs in extracts from PS-2 could 

not be positively identified most likely because of isopropanol 

residue from the addition of spike and surrogate solution during the analytical procedure (Duane Wydoski, U.S. Geological 

Survey, National Water Quality Laboratory, personal commun., 2009)

Sample site PS-1 had 21 SOC detections: 3 detergent 

metabolites, 2 fecal indicators, 3 flame retardants, 7 industrial 

compounds, 5 PCPs, and beta-sitosterol (fig. 5). Three detergent metabolites p-nonylphenol, 4-tert-octylphenol diethoxylate, and triclosan; two flame retardants tri(2-chloroethyl) 

phosphate, and tri(dichlorisopropyl)phosphate; the industrial 

compound pentachloroanisole, and three PCPs, benzophenone, 

galaxolide, and tonalide are suspected or are known to be 

endocrine disruptors. 

The 15 SOCs detected at PS-2, downstream from PS-1, 

were a subset of the 21 detected at PS-1 and included 1 

fecal indicator, 3 flame retardants, 6 industrial compounds, 

and 5 PCPs. Two of the flame retardants, tri(2-chloroethyl)

phosphate and tri(dichlorisopropyl)phosphate; the industrial 

compound pentachloroanisole and three PCPs, benzophenone, 

galaxolide, and tonalide are suspected or known to be endocrine disruptors. 

Three SOCs having the largest measured concentrations 

in extracts from PS-1 and PS-2 were 5-methyl-1H-benzotriazole (an antirust and corrosion inhibitor and an antioxidant 

in antifreeze and deicers), galaxolide (a musk fragrance), and 

tri(2-butoxyethyl)phosphate (a flame retardant). Galaxolide is 

the only compound of the three that is known to be an endocrine disruptor. At the time of this report (2010), none of the 

detected SOCs have MCLs in public drinking-water supplies. 

Summary

The USGS Oklahoma Water Science Center worked 

in cooperation with the US EPA and the Kickapoo Tribe of 

Oklahoma on two separate reconnaissance projects carried out 

concurrently. Both projects entailed the use of passive samplers as a sampling methodology to investigate the detection 

of selected organic compounds at stream sites in jurisdictional 

areas of several tribes in central Oklahoma during January–

February 2009. 

In cooperation with the Kickapoo Tribe of Oklahoma, 

SPMDs and POCIS were submerged at two sites; one at the 

upstream western edge (PS-1) and the other at the downstream 

eastern edge (PS-2) of the Kickapoo tribal boundaries. Both 

sites are downstream from the Oklahoma City metropolitan 

area and multiple wastewater treatment plants. Extract composites were analyzed for 62 pesticides, 10 pesticide metabolites, 3 PCBs compounds, 35 PAHs, and 49 SOCs.

Ten pesticides and four pesticide metabolites were 

detected at the upstream site (PS-1) and seven pesticides and 

four pesticide metabolites, of 62 pesticides analyzed, were 

detected at the downstream site (PS-2). Pesticides detected at 
References Cited 13

both sites were the herbicides atrazine, dacthal, metolachlor, 

pendimethalin, and the insecticides chlorpyrifos, dieldrin, 

and trans-nonachlor. Pesticide metabolites detected at both 

sites were p,p'-DDE, and cis-chlordane and trans-chlordane, 

both pesticide metabolites of the legacy insecticide chlordane. 

Additionally at the upstream site, the herbicides pentachlorophenol, prometon, and the insecticide heptachlor were 

detected. 

Concentrations of three detected pesticides and one 

metabolite are regulated in public-drinking water by the 

US EPA with maximum contaminant levels of atrazine 

(3,000 ng/L), heptachlor (400 ng/L), heptachlor epoxide (200 

ng/L), and pentachlorophenol (1,000 ng/L). However, the 

approximate water concentrations of heptachlor and heptachlor epoxide representing stream samples are small, about 

2,000 to 4,000 times smaller than the respective maximum 

contaminant levels in drinking water. The water concentrations of atrazine and pentachlorophenol could not be calculated because these compounds were measured in POCIS 

extracts. 

The PCB compounds aroclor-1016/1242, aroclor-1254, 

and aroclor-1260 were detected at both sites. The maximum 

contaminant level for PCBs in drinking water is 5,000 ng/L. 

The sum of the three compound concentrations approximated 

in stream water is small, less than 6 ng/L. 

The upstream site PS-1 had 16 PAH detections and the 

downstream site PS-2 had eight detections. Because of chromatographic interference during analysis, a positive identification of 17 PAHs could not be made. Consequently, there may 

have been a greater number of these compounds in extracts 

from the two sites. None of the detected PAHs have maximum 

contaminant levels for public drinking-water supplies. 

A total of 36 SOCs were detected at the two sites adjacent to the Kickapoo tribal lands. The upstream site PS-1 had 

21 SOC detections; three detergent metabolites, two fecal 

indicators, three flame retardants, seven industrial compounds, 

and five compounds related to personal care products. Betasitosterol also was detected. Fifteen SOCs were detected at the 

downstream site PS-2 and included; one fecal indicator, three 

flame retardants, six industrial compounds, and five compounds related to personal care products. Similar to the PAHs, 

chromatographic interference during laboratory analysis 

affected the positive identification of SOCs in extracts from 

both sites. Consequently, the presence of 12 SOCs at site PS-1 

and four at site PS-2 could not be determined. An additional 

eight SOCs in extracts from the downstream site could not be 

positively identified most likely because of isopropanol residue from the addition of spike and surrogate solution during 

the analytical procedure.

Three SOCs having the largest measured concentrations 

in extracts from PS-1 and PS-2 were 5-methyl-1H-benzotriazole (an antirust and corrosion inhibitor and an antioxidant 

in antifreeze and deicers), galaxolide a musk fragrance, and 

tri(2-butoxyethyl)phosphate a flame retardant. Galaxolide is 

the only compound of the three that is known to be an endocrine disruptor. At the time of this report, none of the detected 

SOCs have maximum contaminant levels in public drinkingwater supplies. 

In cooperation with the US EPA, SPMDs were submerged at five stream sites located at USGS stream-gaging 

stations on the Cimarron River, Little River, North Canadian 

River, Deep Fork, and the Washita River. A composite of 

extracts from three SPMDs submerged at each site was analyzed for 46 pesticides and 6 pesticide metabolites. Dacthal 

a pre-emergent herbicide was detected at all five sites. Pendimethalin also a pre-emergent was detected at one site. The 

insecticides chlorpyrifos and dieldrin were detected at three 

sites and p,p'-DDE a metabolite of the insecticide DDT also 

was detected at three sites. 

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

Development of a passive, in situ, integrative sampler for 

hydrophilic organic contaminants in aquatic environments: 

Environmental Toxicology and Chemistry, v. 23, no. 7, 

p. 1,640–1,648.

Brigham, Mark E., Payne, Gregory A., Andrews, William 

J., 2002, Statistical analysis of stream water-quality data 

and sampling network design near Oklahoma City, central 

Oklahoma, 1977–1999; U.S. Geological Survey WaterResources Investigations Report 02–4111, 24 p.

Crain, A.D., Janssen, S.J., Edwards, T.M., Heindel, Jerrold, 

Ho, Shuk-mei, Hunt, Patricia, Iguchi, Taisen, Juul, Anders, 

McLachlan, J.A., Schwartz, Jackie, Skakkebaek, Niels, 

Soto, A.M., Swan, Shanna, Walker, Cheryl, Woodruff, 

T.K., Woodruff, T.J., Giudice, L.C., and Guillette, Louis, 

Jr., 2008, Female reproductive disorders—The roles of 

endocrine-disrupting compounds and developmental timing: 

Fertility and Sterility, v. 90, no. 4, p. 911–940. 

Dean, John R., 2010, Extraction techniques in analytical sciences, Chapter 1, Pre- and post-extraction considerations: 

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37 p. [revised]. 
Blank Page
Appendix 1—Organic Compounds 

Appendix 1
Blank Page
Appendix 1 19

Appendix 1. Organic compounds as analyzed in extracts from Semipermeable Membrane Devices or Polar Organic Chemical 

Integrative Samplers for this study, including suspected endocrine disruption potential, Chemical Abstract Service number, possible 

compound uses or sources (modified from Zaugg and others [2007] and Tertuliani and others [2008]), sampler type used to sequester 

compound, and laboratory method used for analysis.—Continued

[EDC, known or suspected endocrine disruptor; -, no or status is not known; na, not available; CAS, Chemical Abstract Service; PAH, polycyclic aromatic 

hydrocarbon; US EPA, U.S. Environmental Protection Agency; SPMD, Semipermeable Membrane Device; Polar Organic Chemical Integrative Sampler, POCIS]

Compound EDC1, 2, 3 CAS 

number 6

Possible compound uses 

or sources1, 2, 3, 4, 5 

Sampler 

type

Laboratory 

method

1-Methylnaphthalene - 90-12-0 PAH, used in the manufacture of dyes, 

plastics, and resins 

POCIS Zaugg and others (2007)

1-Methyl-9H-fluorene - 1730-37-6 PAH SPMD Zaugg and others (2006)

1-Methylphenanthrene - 832-69-9 PAH SPMD Zaugg and others (2006)

1-Methylpyrene - 2381-21-7 PAH SPMD Zaugg and others (2006)

1,2,4-Trichlorobenzene - 120-82-1 PAH SPMD Zaugg and others (2006)

1,2-Dimethylnaphthalene - 573-98-8 PAH SPMD Zaugg and others (2006)

1,4-Dichlorobenzene Yes 106-46-7 Moth repellant, fumigant, deodorant POCIS Zaugg and others (2007)

1,6-Dimethylnaphthalene - 575-43-9 PAH SPMD Zaugg and others (2006)

2-Ethylnaphthalene - 939-27-5 PAH SPMD Zaugg and others (2006)

2-Methylanthracene - 613-12-7 PAH SPMD Zaugg and others (2006)

2-Methylnaphthalene - 91-57-6 PAH POCIS Zaugg and others (2007)

2,3,6-Trimethylnaphthalene - 829-26-5 PAH SPMD Zaugg and others (2006)

2,6-Diethylaniline - 579-66-8 Used in the production of triazine 

herbicides 

SPMD Zaugg and others (1995)

2,6-Dimethylnaphthalene - 581-42-0 PAH, present in diesel/kerosene (trace 

in gasoline)

SPMD, POCIS Zaugg and others (2006; 

2007)

3-beta-Coprostanol - 360-68-9 Carnivore fecal indicator POCIS Zaugg and others (2007)

3-methyl-1(H)-indole 

(Skatol)

- 83-34-1 Stench in feces, present in coal tar POCIS Zaugg and others (2007)

3-tert-Butyl-4-hydroxyanisole (BHA) Yes 25013-16-5 Antioxidant, general preservative POCIS Zaugg and others (2007)

4-Cumylphenol Yes 599-64-4 Nonionic detergent metabolite POCIS Zaugg and others (2007)

4-n-Octylphenol Yes 1806-26-4 Nonionic detergent metabolite POCIS Zaugg and others (2007)

4-Nonylphenol diethoxylate 

(NP2EO; total)

Yes na Nonionic detergent metabolite POCIS Zaugg and others (2007)

4-Nonylphenol monoethoxylate (NP1EO)

Yes 104-35-8 Nonionic detergent metabolite POCIS Zaugg and others (2007)

4-tert-Octylphenol diethoxylate (OP2EO)

Yes na Nonionic detergent metabolite POCIS Zaugg and others (2007)

4-tert-Octylphenol monoethoxylate (OP1EO; total)

Yes na Nonionic detergent metabolite POCIS Zaugg and others (2007)

4-tert-Octylphenol Yes 140-66-9 Nonionic detergent metabolite POCIS Zaugg and others (2007)

4,5-Methylenephenanthrene - 203-64-5 PAH SPMD Zaugg and others (2006)

Appendix 1. Organic compounds as analyzed in extracts from Semipermeable Membrane Devices or Polar Organic Chemical 

Integrative Samplers for this study, including suspected endocrine disruption potential, Chemical Abstract Service number, possible 

compound uses or sources (modified from Zaugg and others [2007] and Tertuliani and others [2008]), sampler type used to sequester 

compound, and laboratory method used for analysis.

[EDC, known or suspected endocrine disruptor; -, no or status is not known; na, not available; CAS, Chemical Abstract Service; PAH, polycyclic aromatic 

hydrocarbon; US EPA, U.S. Environmental Protection Agency; SPMD, Semipermeable Membrane Device; Polar Organic Chemical Integrative Sampler, 

POCIS]
20 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

Appendix 1. Organic compounds as analyzed in extracts from Semipermeable Membrane Devices or Polar Organic Chemical 

Integrative Samplers for this study, including suspected endocrine disruption potential, Chemical Abstract Service number, possible 

compound uses or sources (modified from Zaugg and others [2007] and Tertuliani and others [2008]), sampler type used to sequester 

compound, and laboratory method used for analysis.—Continued

[EDC, known or suspected endocrine disruptor; -, no or status is not known; na, not available; CAS, Chemical Abstract Service; PAH, polycyclic aromatic 

hydrocarbon; US EPA, U.S. Environmental Protection Agency; SPMD, Semipermeable Membrane Device; Polar Organic Chemical Integrative Sampler, POCIS]

Compound EDC1, 2, 3 CAS 

number 6

Possible compound uses 

or sources1, 2, 3, 4, 5 

Sampler 

type

Laboratory 

method

5-methyl-1H-benzotriazole - 136-85-6 Antirust and corrosion inhibitor, antioxidant in antifreeze and deicersPOCIS Zaugg and others (2007)

Acenaphthene - 83-32-9 PAH SPMD Zaugg and others (2006)

Acenaphthylene - 208-96-8 PAH, used in dye synthesis, insecticides, fungicides, and in the manufacture of plastics SPMD Zaugg and others (2006)

Acetochlor Yes 34256-82-1 Herbicide SPMD Zaugg and others (1995)

Alachlor Yes 15972-60-8 Herbicide, regulated in drinking water 

by the US EPA

SPMD Zaugg and others (1995)

Acetophenone - 98-86-2 Fragrance in detergent and tobacco, 

flavor in beverages

POCIS Zaugg and others (2007)

Aldrin Yes 309-00-2 Organochlorine pesticide, banned in 

1987, degrades to dieldrin

SPMD Noriega and others (2004)

alpha-Endosulfan Yes 959-98-8 Insecticide SPMD Noriega and others (2004)

alpha-Hexachlorocyclohexane (BHC)- 319-84-6 Insecticide SPMD Noriega and others (2004), 

Zaugg and others (1995)

Anthracene - 120-12-7 PAH, wood preservative SPMD Zaugg and others (2006; 

2007)

Anthraquinone - 84-65-1 PAH, dye manufacture and textiles, 

seed treatment, bird repellant

SPMD Zaugg and others (2006; 

2007)

Aroclor 1016/1242 - na A polychlorinated biphenyl compound 

used in industrial processes

SPMD Noriega and others (2004)

Aroclor 1254 Yes 11097-69-1 A polychlorinated biphenyl compound 

used in industrial processes 

SPMD Noriega and others (2004)

Aroclor 1260 - 11096-82-5 A polychlorinated biphenyl compound 

used in industrial processes

SPMD Noriega and others (2004)

Atrazine Yes 1912-24-9 Herbicide, regulated in drinking water 

by the US EPA 

SPMD Zaugg and others (1995; 

2007)

Benfluralin - 1861-40-1 Herbicide SPMD Zaugg and others (1995)

Benzo(a)anthracene Yes 56-55-3 PAH, probable human carcinogen SPMD Zaugg and others (2006)

Benzo(b)fluoranthene Yes 205-99-2 PAH, probable human carcinogen SPMD Zaugg and others (2006)

Benzo(a)pyrene Yes 50-32-8 PAH, probable human carcinogen, 

used in cancer research, combustion 

product, found in cigarette smoke, 

regulated in drinking water by the 

US EPA

SPMD Zaugg and others (2006; 

2007)

Benzo(e)pyrene - 192-97-2 PAH SPMD Zaugg and others (2006)

Benzo(ghi)perylene Yes 191-24-2 PAH SPMD Zaugg and others (2006)

Benzo(k)fluoranthene Yes 207-08-9 PAH, probable human carcinogen SPMD Zaugg and others (2006)
Appendix 1 21

Appendix 1. Organic compounds as analyzed in extracts from Semipermeable Membrane Devices or Polar Organic Chemical 

Integrative Samplers for this study, including suspected endocrine disruption potential, Chemical Abstract Service number, possible 

compound uses or sources (modified from Zaugg and others [2007] and Tertuliani and others [2008]), sampler type used to sequester 

compound, and laboratory method used for analysis.—Continued

[EDC, known or suspected endocrine disruptor; -, no or status is not known; na, not available; CAS, Chemical Abstract Service; PAH, polycyclic aromatic 

hydrocarbon; US EPA, U.S. Environmental Protection Agency; SPMD, Semipermeable Membrane Device; Polar Organic Chemical Integrative Sampler, POCIS]

Compound EDC1, 2, 3 CAS 

number 6

Possible compound uses 

or sources1, 2, 3, 4, 5 

Sampler 

type

Laboratory 

method

Benzophenone Yes 119-61-9 Ultra violet blocker in perfumes, 

soaps, and plastics

POCIS Zaugg and others (2007)

beta-Hexachlorobenzene Yes 319-85-7 Insecticide SPMD Noriega and others (2004)

beta-Sitosterol - 83-46-5 Plant sterol POCIS Zaugg and others (2007)

beta-Stigmastanol - 19466-47-8 Plant sterol POCIS Zaugg and others (2007)

Bisphenol A Yes 80-05-7 Plasticizer, manufacture of polycarbonate resins, antioxidant, fire 

repellant

POCIS Zaugg and others (2007)

Bromacil - 314-40-9 General use herbicide POCIS Zaugg and others (2007)

Bromoform - 75-25-2 Wastewater ozonation byproduct, 

military/explosives

POCIS Zaugg and others (2007)

Butylate - 2008-41-5 Herbicide SPMD Zaugg and others (1995)

Caffeine - 58-08-2 Beverages, diuretic, very mobile and 

biodegradable

POCIS Zaugg and others (2007)

Camphor - 76-22-2 Flavor, odorant, ointments POCIS Zaugg and others (2007)

Carbaryl Yes 63-25-2 Insecticide, crop and garden uses, low 

persistence

SPMD Zaugg and others (1995; 

2007)

Carbazole - 86-74-8 PAH, insecticide, manufacture of dyes, 

explosives, and lubricants

SPMD Zaugg and others (2006)

Carbofuran Yes 1563-66-2 Insecticide SPMD Zaugg and others (1995)

cis-Chlordane Yes 5103-71-9 Chlordane metabolite, banned, considered a legacy pesticide SPMD Noriega and others (2004)

trans-Chlordane Yes 5103-74-2 Chlordane metabolite, banned, considered a legacy pesticide SPMD Noriega and others (2004)

Chlorpyrifos Yes 2921-88-2 Insecticide, residential use restricted as 

of 2001, common name is dursban

SPMD, POCIS Zaugg and others (1995; 

2007)

Cholesterol - 57-88-5 Often a fecal indicator, also a plant 

sterol

POCIS Zaugg and others (2007)

Chrysene Yes 218-01-9 PAH, probable human carcinogen SPMD Zaugg and others (2006)

Cotinine - 486-56-6 Metabolite of nicotine POCIS Zaugg and others (2007)

Cumene (Isopropylbenzene) - 98-82-8 Manufacture phenol/acetone, fuels and 

paint thinner

POCIS Zaugg and others (2007)

Cyanazine Yes 21725-46-2 Herbicide SPMD Zaugg and others (1995)

Dacthal - 1861-32-1 Pre-emergent herbicide SPMD Zaugg and others (1995)

Deethylatrazine - 6190-65-4 Metabolite of atrazine SPMD Zaugg and others (1995)

Desulfinylfipronil - na Metabolite of fipronil SPMD Zaugg and others (1995)
22 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

Appendix 1. Organic compounds as analyzed in extracts from Semipermeable Membrane Devices or Polar Organic Chemical 

Integrative Samplers for this study, including suspected endocrine disruption potential, Chemical Abstract Service number, possible 

compound uses or sources (modified from Zaugg and others [2007] and Tertuliani and others [2008]), sampler type used to sequester 

compound, and laboratory method used for analysis.—Continued

[EDC, known or suspected endocrine disruptor; -, no or status is not known; na, not available; CAS, Chemical Abstract Service; PAH, polycyclic aromatic 

hydrocarbon; US EPA, U.S. Environmental Protection Agency; SPMD, Semipermeable Membrane Device; Polar Organic Chemical Integrative Sampler, POCIS]

Compound EDC1, 2, 3 CAS 

number 6

Possible compound uses 

or sources1, 2, 3, 4, 5 

Sampler 

type

Laboratory 

method

Desulfinylfipronil amide - na Metabolite of fipronil SPMD Zaugg and others (1995)

Diazinon Yes 333-41-5 Insecticide, residential use banned in 

2004

SPMD Zaugg and others (1995), 

Zaugg and others (2007)

Dibenz(ah)anthracene Yes 53-70-3 PAH, probable human carcinogen SPMD Zaugg and others (2006)

Dibenzothiophene - 132-65-0 PAH, present in petroleum products SPMD Zaugg and others (2006)

Dieldrin Yes 60-57-1 Insecticide, banned in 1987, considered a legacy pesticideSPMD Noriega and others (2004), 

Zaugg and others (1995)

bis(2-ethylhexyl)phthalate Yes 117-81-7 Plasticizer for polymers and resins, 

inert ingredient in pesticides

SPMD Zaugg and others (2006)

Diethylphthalate Yes 84-66-2 Plasticizer for polymers and resins SPMD Zaugg and others (2006)

Disulfoton - 298-04-4 Insecticide SPMD Zaugg and others (1995)

d-Limonene - 5989-27-5 Fragrance, cleaning products POCIS Zaugg and others (2007)

Endrin Yes 72-20-8 Insecticide, banned, considered a 

legacy pesticide, regulated in drinking water by the US EPA

SPMD Noriega and others (2004)

Eptam (EPTC) - 759-94-4 Herbicide SPMD Zaugg and others (1995)

Ethyl citrate - 77-93-0 Solvent, used in paints and perfunes, 

used to decaffeinate coffee and tea

POCIS Zaugg and others (2007)

Ethalfluralin - 55283-68-6 Herbicide SPMD Zaugg and others (1995)

Ethoprop - 13194-48-4 Insecticide SPMD Zaugg and others (1995)

Fipronil Yes 120068-37-3 Insecticide SPMD Zaugg and others (1995)

Fipronil sulfide - 120067-83-6 Metabolite of fipronil SPMD Zaugg and others (1995)

Fipronil sulfone - 120068-36-2 Metabolite of fipronil SPMD Zaugg and others (1995)

Fluoranthene - 206-44-0 PAH, component of coal tar and 

asphalt, traces in gasoline and diesel 

fuel

SPMD, POCIS Zaugg and others (2006; 

2007)

Fluorene - 86-73-7 PAH, occurs in coal tar SPMD Zaugg and others (2006)

Fonofos - 944-22-9 Insecticide SPMD Zaugg and others (1995)

Galaxolide (HHCB) Yes 1222-05-5 Musk fragrance, persistent and widespread in ground water, concern for 

bioaccumulation and toxicity

POCIS Zaugg and others (2007)

Heptachlor Yes 76-44-8 Insecticide, banned in 1974, used as a 

termaticide under certain circumstances

SPMD Noriega and others (2004)

Heptachlor epoxide Yes 1024-57-3 Metabolite of heptachlor SPMD Noriega and others (2004)
Appendix 1 23

Appendix 1. Organic compounds as analyzed in extracts from Semipermeable Membrane Devices or Polar Organic Chemical 

Integrative Samplers for this study, including suspected endocrine disruption potential, Chemical Abstract Service number, possible 

compound uses or sources (modified from Zaugg and others [2007] and Tertuliani and others [2008]), sampler type used to sequester 

compound, and laboratory method used for analysis.—Continued

[EDC, known or suspected endocrine disruptor; -, no or status is not known; na, not available; CAS, Chemical Abstract Service; PAH, polycyclic aromatic 

hydrocarbon; US EPA, U.S. Environmental Protection Agency; SPMD, Semipermeable Membrane Device; Polar Organic Chemical Integrative Sampler, POCIS]

Compound EDC1, 2, 3 CAS 

number 6

Possible compound uses 

or sources1, 2, 3, 4, 5 

Sampler 

type

Laboratory 

method

Hexachlorobenzene Yes 118-74-1 Fungicide, carcinogen, banned from 

use

SPMD Noriega and others (2004), 

Zaugg and others (2006)

Indeno(1,2,3-cd)pyrene Yes 193-39-5 PAH, probable human carcinogen SPMD Zaugg and others (2006)

Indole - 120-72-9 Pesticide inert ingredient, fragrance in 

coffee, stench in feces

POCIS Zaugg and others (2007)

Isoborneol - 124-76-5 Fragrance POCIS Zaugg and others (2007)

Isophorone - 78-59-1 Solvent for lacquer, plastic, oil, silicon, 

resin

POCIS Zaugg and others (2007)

Isoquinoline - 119-65-3 Flavors and fragrances POCIS Zaugg and others (2007)

Lindane Yes 58-89-9 Insecticide, banned in 2009 SPMD Zaugg and others (1995), 

Noriega and others (2004)

Linuron Yes 330-55-2 Herbicide SPMD Zaugg and others (1995)

Malathion Yes 121-75-5 Insecticide SPMD Zaugg and others (1995)

Menthol - 89-78-1 Liniment, cigarettes, cough drops, 

mouthwash

POCIS Zaugg and others (2007)

Metalaxyl - 57837-19-1 Fungicide POCIS Zaugg and others (2007)

Methyl azinphos - 86-50-0 Insecticide SPMD Zaugg and others (1995)

Methyl parathion Yes 298-00-0 Insecticide SPMD Zaugg and others (1995)

Methyl salicylate - 119-36-8 Liniment, food, beverage, ultra violetabsorbing lotionPOCIS Zaugg and others (2007)

Metolachlor - 51218-45-2 Herbicide, general use pesticide, indicator of agricultural drainageSPMD Zaugg and others (1995; 

2007)

Metribuzin Yes 21087-64-9 Herbicide SPMD Zaugg and others (1995)

Mirex Yes 2358-85-5 Insecticide SPMD Noriega and others (2004)

Molinate Yes 2212-67-1 Herbicide SPMD Zaugg and others (1995)

Napropamide - 15299-99-7 Herbicide SPMD Zaugg and others (1995)

N,N-diethyl-meta-toluamide 

(DEET)

- 134-62-3 Insecticide, urban uses, mosquito 

repellent

POCIS Zaugg and others (2007)

Naphthalene - 91-20-3 PAH, fumigant, moth repellent SPMD Zaugg and others (2006; 

2007)

p-Cresol - 106-44-5 Wood preservative POCIS Zaugg and others (2007)

p-Nonylphenol (total) Yes 84852-15-3 Nonionic detergent metabolite POCIS Zaugg and others (2007)

p,p'-DDD Yes 72-54-8 Metabolite of DDT SPMD Noriega and others (2004)

p,p'-DDE Yes 72-55-9 Metabolite of DDT SPMD Noriega and others (2004), 

Zaugg and others (1995)
24 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

Appendix 1. Organic compounds as analyzed in extracts from Semipermeable Membrane Devices or Polar Organic Chemical 

Integrative Samplers for this study, including suspected endocrine disruption potential, Chemical Abstract Service number, possible 

compound uses or sources (modified from Zaugg and others [2007] and Tertuliani and others [2008]), sampler type used to sequester 

compound, and laboratory method used for analysis.—Continued

[EDC, known or suspected endocrine disruptor; -, no or status is not known; na, not available; CAS, Chemical Abstract Service; PAH, polycyclic aromatic 

hydrocarbon; US EPA, U.S. Environmental Protection Agency; SPMD, Semipermeable Membrane Device; Polar Organic Chemical Integrative Sampler, POCIS]

Compound EDC1, 2, 3 CAS 

number 6

Possible compound uses 

or sources1, 2, 3, 4, 5 

Sampler 

type

Laboratory 

method

p,p'-DDT Yes 50-29-3 Insecticide, considered a legacy 

pesticide, banned in 1972

SPMD Noriega and others (2004)

p,p'-Methoxychlor Yes 72-43-5 Insecticide SPMD Noriega and others (2004)

Parathion Yes 56-38-2 Insecticide SPMD Zaugg and others (1995)

Pebulate - 1114-71-2 Herbicide SPMD Zaugg and others (1995)

Pendimethalin Yes 40487-42-1 Herbicide, preemergent SPMD Zaugg and others (1995)

Pentachloroanisole Yes 1825-21-4 Used in the production of polymers, 

pesticides, and fire retardants. Wood 

preservative, metabolite of pentachlorophenol

SPMD Zaugg and others (2006)

Pentachloronitrobenzene Yes 82-68-8 Fungicide SPMD Zaugg and others (2006)

Pentachlorophenol Yes 87-86-5 Algaecide, fungicide, herbicide, and 

wood preservative, regulated in 

drinking water by the US EPA

POCIS Zaugg and others (2007)

Permethrin Yes 61949-76-6 Insecticide SPMD Zaugg and others (1995)

Perylene - 77392-71-3 PAH SPMD Zaugg and others (2006)

Phenanthrene - 85-01-8 PAH, manufacture of explosives SPMD Zaugg and others (2006; 

2007)

Phenanthridine - 229-87-8 Dye SPMD Zaugg and others (2006)

Phenol - 108-95-2 Disinfectant, used in the manufacture 

of several products, leachate

POCIS Zaugg and others (2007)

Phorate - 298-02-2 Insecticide SPMD Zaugg and others (1995)

Prometon - 1610-18-0 Herbicide, noncrop only, applied prior 

to blacktop

SPMD, POCIS Zaugg and others (1995; 

2007)

Propachlor - 1918-16-7 Herbicide SPMD Zaugg and others (1995)

Propanil Yes 709-98-8 Herbicide SPMD Zaugg and others (1995)

Propargite - 2312-35-8 Insecticide SPMD Zaugg and others (1995)

Propyzamide Yes 23950-58-5 Herbicide SPMD Zaugg and others (1995)

Pyrene - 129-00-0 PAH SPMD, POCIS Zaugg and others (2006; 

2007)

Simazine Yes 122-34-9 Herbicide, regulated in drinking water 

by the US EPA

SPMD Zaugg and others (1995)

Tebuthiuron - 34014-18-1 Herbicide SPMD Zaugg and others (1995)

Terbacil - 5902-51-2 Herbicide SPMD Zaugg and others (1995)

Terbufos - 13071-79-9 Insecticide SPMD Zaugg and others (1995)
Appendix 1 25

Appendix 1. Organic compounds as analyzed in extracts from Semipermeable Membrane Devices or Polar Organic Chemical 

Integrative Samplers for this study, including suspected endocrine disruption potential, Chemical Abstract Service number, possible 

compound uses or sources (modified from Zaugg and others [2007] and Tertuliani and others [2008]), sampler type used to sequester 

compound, and laboratory method used for analysis.—Continued

[EDC, known or suspected endocrine disruptor; -, no or status is not known; na, not available; CAS, Chemical Abstract Service; PAH, polycyclic aromatic 

hydrocarbon; US EPA, U.S. Environmental Protection Agency; SPMD, Semipermeable Membrane Device; Polar Organic Chemical Integrative Sampler, POCIS]

Compound EDC1, 2, 3 CAS 

number 6

Possible compound uses 

or sources1, 2, 3, 4, 5 

Sampler 

type

Laboratory 

method

Tetrachloroethylene - 127-18-4 Solvent, degreaser, veterinary anthelminticPOCIS Zaugg and others (2007)

Thiobencarb - 28249-77-6 Herbicide SPMD Zaugg and others (1995)

Tonalide (AHTN) Yes 21145-77-7 Musk fragrance, persistent and widespread in water, concern for bioaccumulation and toxicityPOCIS Zaugg and others (2007)

Toxaphene Yes 8001-35-2 Insecticide, regulated in drinking water 

by the US EPA

SPMD Noriega and others (2004)

Trans-nonachlor Yes 39765-80-5 Insecticide SPMD Noriega and others (2004)

Triallate - 2303-17-5 Herbicide SPMD Zaugg and others (1995)

Trifluralin Yes 1582-09-8 Herbicide SPMD Zaugg and others (1995)

Tri(2-butoxyethyl) phosphate- 78-51-3 Flame retardant, plasticizer, solvent POCIS Zaugg and others (2007)

Tri(2-chloroethyl) phosphate Yes 115-96-8 Flame retardant POCIS Zaugg and others (2007)

Tributyl phosphate - 126-73-8 Antifoaming agent, flame retardant POCIS Zaugg and others (2007)

Triclosan Yes 3380-34-5 Disinfectant, antimicrobial (concern 

for acquired microbial resistance)

POCIS Zaugg and others (2007)

Tri(dichlorisopropyl) phosphateYes 13674-87-8 Flame retardant POCIS Zaugg and others (2007)

Triethyl citrate - 77-93-0 Cosmetics, pharmaceuticals POCIS Zaugg and others (2007)

Triphenyl phosphate - 115-86-6 Plasticizer, resin, wax, roofing paper, 

flame retardant

POCIS Zaugg and others (2007)

1

 Kegley and others (2008). 

2

 U.S. Department of Labor, Occupational Safety and Health Administration (2009).

3

 U.S. Environmental Protection Agency (1995).

4

 U.S. Environmental Protection Agency (2002b).

5

 U.S. Environmental Protection Agency (2009b).

6

 This report contains CAS Registry Numbers®, which is a Registered Trademark of the American Chemical Society. CAS recommends the verification of the 

CASRNs through CAS Client ServicesSM. 
Blank Page
Appendix 2—Concentrations of Pesticides and Pesticide 

Metabolites
Blank Page
Appendix 2 29

Appendix 2. Concentrations of pesticides and pesticide metabolites measured in extracts from Semipermeable Membrane Devices submerged at five U.S. Geological Survey stream-gaging stations in jurisdictional areas of several tribes in central Oklahoma, January–February 2009.—Continued [Extracts were a composite of the three passive sampler media deployed at each sampling site. Compounds were analyzed by using laboratory methodologies described in Zaugg and others (1995). Laboratory reporting level is less than 5 nanograms per ampoule of extract. Approximate concentrations in water are shown in appendix 3. Compounds bolded were considered detected because concentration was three times, or greater, than the highest concentration measured in the field or laboratory blank; Site identifier, stream-gaging station and (number); <, less than; N., North; ng/ampoule, nanogram of compound per ampoule of extract; --, not applicable; UD, matrix interference prevented the detection of the compound if present in the sample]

Compound

S-1

Cimarron 

River near 

Ripley, 

Oklahoma

(07161450)

(ng/ampoule)

S-2

Little 

River near 

Tecumseh, 

Oklahoma 

(07230500)

(ng/ampoule)

S-3

N. Canadian 

River near 

Calumet, 

Oklahoma

(07239450)

(ng/ampoule)

S-4

Deep Fork 

at Warwick, 

Oklahoma

(07242380)

(ng/ampoule)

S-5

Washita 

River near 

Pauls Valley, 

Oklahoma

(07328500)

(ng/ampoule)

Field blank

(ng/ampoule)

Laboratory 

blank

(ng/ampoule)

Laboratory 

reporting level

(ng/ampoule)

Laboratory 

spike

(percent 

recovery)

Pesticides

2,6-Diethylaniline <5 <5 <5 <5 <5 <5 <5 <5 92Acetochlor <5 <5 <5 <5 <5 <5 <5 <5 70Alachlor <5 <5 <5 <5 <5 <5 <5 <5 72alpha-Hexachlorocyclohexane (BHC) <5 <5 <5 <5 <5 <5 <5 <5 103Atrazine <5 <5 <5 <5 <5 <5 <5 <5 83Benfluralin <5 <5 <5 <5 <5 <5 <5 <5 67Butylate <5 <5 <5 <5 <5 <5 <5 <5 77Carbaryl <5 <5 <5 <5 <5 <5 <5 <5 110

Carbofuran <5 <5 <5 <5 <5 <5 <5 <5 82

Chlorpyrifos 49.4 <5 <5 49.6 530 <5 <5 <5 54Cyanazine <5 <5 <5 <5 <5 <5 <5 <5 82Dacthal 1.94 3.55 1.91 2.96 3.86 <5 <5 <5 110Diazinon <5 <5 <5 <5 <5 <5 <5 <5 88Dieldrin 27 <5 <5 30.2 16.6 <5 <5 <5 110Disulfoton <5 <5 <5 <5 <5 <5 <5 <5 90Eptam (EPTC) <5 <5 <5 <5 <5 <5 <5 <5 96Ethalfluralin <5 <5 <5 <5 <5 <5 <5 <5 87Ethoprop <5 <5 <5 <5 <5 <5 <5 <5 69Fipronil <5 <5 <5 <5 <5 <5 <5 <5 80Fonofos <5 <5 <5 <5 <5 <5 <5 <5 40Lindane <5 <5 <5 <5 <5 <5 <5 <5 92Linuron <5 <5 <5 <5 <5 <5 <5 <5 93

Malathion <25 <5 <25 <5 <5 <5 <5 <5 78

Appendix 2. Concentrations of pesticides and pesticide metabolites measured in extracts from Semipermeable Membrane Devices submerged at five U.S. Geological Survey stream-gaging stations in jurisdictional areas of several tribes in central Oklahoma, January–February 2009. [Extracts were a composite of the three passive sampler media deployed at each sampling site. Compounds were analyzed by using laboratory methodologies described in Zaugg and others (1995). Laboratory reporting level is less than 5 nanograms per ampoule of extract. Approximate concentrations in water are shown in appendix 3. Compounds bolded were considered detected because concentration was three times, or greater, than the highest concentration measured in the field or laboratory blank; Site identifier, stream-gaging station and (number); <, less than; N., North; ng/ampoule, nanogram of compound per ampoule of extract; --, not applicable; UD, matrix interference prevented the detection of the compound if present in the sample]

Appendix 2
30 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma Appendix 2. Concentrations of pesticides and pesticide metabolites measured in extracts from Semipermeable Membrane Devices submerged at five U.S. Geological Survey stream-gaging stations in jurisdictional areas of several tribes in central Oklahoma, January–February 2009.—Continued [Extracts were a composite of the three passive sampler media deployed at each sampling site. Compounds were analyzed by using laboratory methodologies described in Zaugg and others (1995). Laboratory reporting level is less than 5 nanograms per ampoule of extract. Approximate concentrations in water are shown in appendix 3. Compounds bolded were considered detected because concentration was three times, or greater, than the highest concentration measured in the field or laboratory blank; Site identifier, stream-gaging station and (number); <, less than; N., North; ng/ampoule, nanogram of compound per ampoule of extract; --, not applicable; UD, matrix interference prevented the detection of the compound if present in the sample] Compound S-1 Cimarron River near Ripley, Oklahoma (07161450) (ng/ampoule) S-2 Little River near Tecumseh, Oklahoma (07230500) (ng/ampoule) S-3 N. Canadian River near Calumet, Oklahoma (07239450) (ng/ampoule) S-4 Deep Fork at Warwick, Oklahoma (07242380) (ng/ampoule) S-5 Washita River near Pauls Valley, Oklahoma (07328500) (ng/ampoule) Field blank (ng/ampoule) Laboratory blank (ng/ampoule) Laboratory reporting level (ng/ampoule) Laboratory spike (percent recovery) Methyl azinphos <5 <5 <5 <5 <5 <5 <5 <5 73 Methyl parathion <5 <5 <5 <5 <5 <5 <5 <5 37 Metolachlor <5 <5 <5 <5 <5 <5 <5 <5 65 Metribuzin <5 <5 <5 <5 <5 <5 <5 <5 67 Molinate <5 <5 <5 <5 <5 <5 <5 <5 76 Napropamide <25 <25 <25 <25 <25 <5 <5 <5 77 Parathion <5 <5 <5 <5 <5 <5 <5 <5 58 Pebulate <5 <5 <5 <5 <5 <5 <5 <5 80 Pendimethilan <5 <5 <5 78 <5 <5 <5 <5 81 Permethrin <5 <5 <5 <5 <5 <5 <5 <5 80 Phorate <5 <5 <5 <5 <5 <5 <5 <5 102 Prometon <5 <5 <5 <5 <5 <5 <5 <5 71 Propachlor <5 <5 <5 <5 <5 <5 <5 <5 76 Propanil <5 <5 <5 <5 <5 <5 <5 <5 71 Propargite <5 <5 <5 <5 <5 <5 <5 <5 66 Propyzamide <5 <5 <5 <5 <5 <5 <5 <5 66 Simazine <5 <5 <5 <5 <5 <5 <5 <5 76 Tebuthiuron <5 <5 <5 <5 <5 <5 <5 <5 61

Terbacil <5 <5 <5 <5 <5 <5 <5 <5 74Terbufos <5 <5 <5 <5 <5 <5 <5 <5 82Thiobencarb UD <25 <25 <25 <25 <5 <5 <5 75

Triallate <5 <5 <5 <5 <5 <5 <5 <5 86

Trifluralin <5 <5 <5 <5 <5 <5 <5 <5 65Number of detections 3 1 1 4 3 -- -- -- --
Appendix 2 31

Appendix 2. Concentrations of pesticides and pesticide metabolites measured in extracts from Semipermeable Membrane Devices submerged at five U.S. Geological Survey stream-gaging stations in jurisdictional areas of several tribes in central Oklahoma, January–February 2009.—Continued [Extracts were a composite of the three passive sampler media deployed at each sampling site. Compounds were analyzed by using laboratory methodologies described in Zaugg and others (1995). Laboratory reporting level is less than 5 nanograms per ampoule of extract. Approximate concentrations in water are shown in appendix 3. Compounds bolded were considered detected because concentration was three times, or greater, than the highest concentration measured in the field or laboratory blank; Site identifier, stream-gaging station and (number); <, less than; N., North; ng/ampoule, nanogram of compound per ampoule of extract; --, not applicable; UD, matrix interference prevented the detection of the compound if present in the sample]

Compound

S-1

Cimarron 

River near 

Ripley, 

Oklahoma

(07161450)

(ng/ampoule)

S-2

Little 

River near 

Tecumseh, 

Oklahoma 

(07230500)

(ng/ampoule)

S-3

N. Canadian 

River near 

Calumet, 

Oklahoma

(07239450)

(ng/ampoule)

S-4

Deep Fork 

at Warwick, 

Oklahoma

(07242380)

(ng/ampoule)

S-5

Washita 

River near 

Pauls Valley, 

Oklahoma

(07328500)

(ng/ampoule)

Field blank

(ng/ampoule)

Laboratory 

blank

(ng/ampoule)

Laboratory 

reporting level

(ng/ampoule)

Laboratory 

spike

(percent 

recovery)

Pesticide metabolites

p,p'-DDE <5 <5 5.88 3.68 15.3 <5 <5 <5 63Deethylatrazine <5 <5 <5 <5 <5 <5 <5 <5 80Desulfinylfipronil <5 <5 <5 <5 <5 <5 <5 <5 59Desulfinylfipronil amide <5 <5 <5 <5 <5 <5 <5 <5 61Fipronil sulfide <5 <5 <5 <5 <5 <5 <5 <5 42Fipronil sulfone <5 <5 <5 <5 <5 <5 <5 <5 33Number of detections 0 0 1 1 1 -- -- -- --

Percent recovery

Surrogate compoundsD6-alpha-Hexachlorocyclohexane (BHC) 109 109 106 106 10 94 99 -- 91

D10-Diazinon 121 136 132 132 131 103 67 -- 74
Blank Page
Appendix 3—Approximate Concentrations of Pesticides and 

Pesticide Metabolites
Blank Page
Appendix 3 35

Appendix 3. Approximate concentrations of pesticides and pesticide metabolites in water calculated using performance reference 

compounds measured in extracts from Semipermeable Membrane Devices submerged at five U.S. Geological Survey stream-gaging 

stations in jurisdictional areas of several tribes in central Oklahoma, January–February 2009.—Continued 

[Extracts were a composite of three Semipermeable Membrane Device media deployed at each sampling site. Compounds were analyzed by using laboratory 

methodologies described in Zaugg and others (1995). Compounds that are bolded were considered detected because concentration of the compound measured in 

the extract was three times, or greater, than the highest concentration measured in the field or laboratory blank. Concentrations measured in extracts are shown in 

appendix 2. All concentrations are in nanogram of compound per liter of water; N, North; site identifier, stream-gaging station and (number); Nc, not calculated 

because the concentration measured in the extract was below the laboratory reporting level]

Compound

S-1

Cimarron River 

near Ripley, 

Oklahoma

(07161450)

S-2

Little River near 

Tecumseh, 

Oklahoma 

(07230500)

S-3

N. Canadian River 

near Calumet, 

Oklahoma

(07239450)

S-4

Deep Fork at 

Warwick, 

Oklahoma

(07242380)

S-5

Washita River 

near Pauls Valley, 

Oklahoma

(07328500)

2,6-Diethylanaline Nc Nc Nc Nc Nc

Acetochlor Nc Nc Nc Nc Nc

Alachlor Nc Nc Nc Nc Nc

alpha-Hexachlorocyclohexane Nc Nc Nc Nc Nc

Atrazine Nc Nc Nc Nc Nc

Benfluralin Nc Nc Nc Nc Nc

Butylate Nc Nc Nc Nc Nc

Carbaryl Nc Nc Nc Nc Nc

Carbofuran Nc Nc Nc Nc Nc

Chlorpyrifos 1.41 Nc 1.64 .18 2.74

Cyanazine Nc Nc Nc Nc Nc

Dacthal .07 .01 .01 .01 .02

Diazinon Nc Nc Nc Nc Nc

Dieldrin .72 Nc .07 .04 .06

Disulfoton Nc Nc Nc Nc Nc

Eptam (EPTC) Nc Nc Nc Nc Nc

Ethalfluralin Nc Nc Nc Nc Nc

Ethoprop Nc Nc Nc Nc Nc

Fipronil Nc Nc Nc Nc Nc

Fonofos Nc Nc Nc Nc Nc

Lindane Nc Nc Nc Nc Nc

Linuron Nc Nc Nc Nc Nc

Malathion Nc Nc Nc Nc Nc

Methyl azinphos Nc Nc Nc Nc Nc

Methyl parathion Nc Nc Nc Nc Nc

Metolachlor Nc Nc Nc Nc Nc

Metribuzin Nc Nc Nc Nc Nc

Molinate Nc Nc Nc Nc Nc

Napropamide Nc Nc Nc Nc Nc

Parathion Nc Nc Nc Nc Nc

Pebulate Nc Nc Nc Nc Nc

Pendimethilan Nc Nc Nc .15 Nc

Permethrin Nc Nc Nc Nc Nc

Phorate Nc Nc Nc Nc Nc

Appendix 3. Approximate concentrations of pesticides and pesticide metabolites in water calculated using performance reference 

compounds measured in extracts from Semipermeable Membrane Devices submerged at five U.S. Geological Survey stream-gaging 

stations in jurisdictional areas of several tribes in central Oklahoma, January–February 2009. 

[Extracts were a composite of three Semipermeable Membrane Device media deployed at each sampling site. Compounds were analyzed by using laboratory 

methodologies described in Zaugg and others (1995). Compounds that are bolded were considered detected because concentration of the compound measured in 

the extract was three times, or greater, than the highest concentration measured in the field or laboratory blank. Concentrations measured in extracts are shown in 

appendix 2. All concentrations are in nanogram of compound per liter of water; N, North; site identifier, stream-gaging station and (number); Nc, not calculated 

because the concentration measured in the extract was below the laboratory reporting level]

Appendix 3
36 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

Appendix 3. Approximate concentrations of pesticides and pesticide metabolites in water calculated using performance reference 

compounds measured in extracts from Semipermeable Membrane Devices submerged at five U.S. Geological Survey stream-gaging 

stations in jurisdictional areas of several tribes in central Oklahoma, January–February 2009.—Continued 

[Extracts were a composite of three Semipermeable Membrane Device media deployed at each sampling site. Compounds were analyzed by using laboratory 

methodologies described in Zaugg and others (1995). Compounds that are bolded were considered detected because concentration of the compound measured in 

the extract was three times, or greater, than the highest concentration measured in the field or laboratory blank. Concentrations measured in extracts are shown in 

appendix 2. All concentrations are in nanogram of compound per liter of water; N, North; site identifier, stream-gaging station and (number); Nc, not calculated 

because the concentration measured in the extract was below the laboratory reporting level]

Compound

S-1

Cimarron River 

near Ripley, 

Oklahoma

(07161450)

S-2

Little River near 

Tecumseh, 

Oklahoma 

(07230500)

S-3

N. Canadian River 

near Calumet, 

Oklahoma

(07239450)

S-4

Deep Fork at 

Warwick, 

Oklahoma

(07242380)

S-5

Washita River 

near Pauls Valley, 

Oklahoma

(07328500)

Prometon Nc Nc Nc Nc Nc

Propachlor Nc Nc Nc Nc Nc

Propanil Nc Nc Nc Nc Nc

Propargite Nc Nc Nc Nc Nc

Propyzamide Nc Nc Nc Nc Nc

Simazine Nc Nc Nc Nc Nc

Tebuthiuron Nc Nc Nc Nc Nc

Terbacil Nc Nc Nc Nc Nc

Terbufos Nc Nc Nc Nc Nc

Thiobencarb Nc Nc Nc Nc Nc

Triallate Nc Nc Nc Nc Nc

Trifluralin Nc Nc Nc Nc Nc

Pesticide metabolites

p,p'-DDE Nc Nc .03 .01 .06

Deethylatrazine Nc Nc Nc Nc Nc

Desulfinyl fipronil Nc Nc Nc Nc Nc

Desulfinyl fipronil amide Nc Nc Nc Nc Nc

Fipronil sulfide Nc Nc Nc Nc Nc

Fipronil sulfone Nc Nc Nc Nc Nc
Appendix 4—Concentrations of Pesticides, Pesticide 

Metabolites, Polychlorinated Biphenyl Compounds, Polycyclic 

Aromatic Hydrocarbons, and Other Types of Synthetic Organic 

Compounds
Blank Page
Appendix 4 39

Appendix 4. Concentrations of pesticides, pesticide metabolites, polychlorinated biphenyl compounds, polycyclic aromatic 

hydrocarbons, and other types of synthetic organic compounds measured in extracts from Semipermeable Membrane Devices or Polar 

Organic Chemical Integrative Samplers submerged at two stream sites on the North Canadian River adjacent to the Kickapoo tribal 

lands in central Oklahoma, January–February 2009.—Continued 

[Compound concentrations measured in extracts are reported in nanogram per ampoule of extract from a composite of three SPMD or three POCIS media in 

each sampler. Compounds that are bolded were considered detected because concentration was three times, or greater, than the highest concentration measured 

in the field or laboratory blank. A compound measured by more than one laboratory method was counted only once as a detection; site identifier, stream-gaging 

station and (number); N., north; ng/L, nanogram of compound per liter of water; ng/ampoule, nanogram of compound per ampoule of extract; <, less than; E, 

concentration is approximate because trace levels of contamination were found in the blanks at levels below the reporting level; R-Delete, spike fraction was lost 

during sample preparation at laboratory; --, not applicable; *, indicates compound could not be positively identified in the extract below the reported concentration because of chromatographic interference; Nc, not calculated because presence of the compound could not be positively identified in the extract or concentration was below the laboratory reporting level; UD, compound was not recovered most likely because of residual isopropanol from the addition of spike and 

surrogate solution; Np, water concentration could not be calculated because compound was measured in extract from Polar Organic Integrative Sampler which 

did not have performance reference compounds needed for calculation]

Compound

PS-1

N. Canadian River at 

Hogback Road near 

Jones, Oklahoma

(07241540)

PS-2

N. Canadian River 

near Shawnee, 

Oklahoma 

(07241700)

Field blank

(ng/ampoule)

Laboratory 

blank

(ng/ampoule)

Laboratory 

reporting 

level

(ng/ampoule)

Laboratory 

spike

(percent 

recovery)

(ng/ampoule) (ng/L) (ng/ampoule) (ng/L)

Pesticides

2,6-Diethylaniline <5 Nc <5 Nc <5 <5 <5 92

Acetochlor <5 Nc <5 Nc <5 <5 <5 70

Alachlor <5 Nc <5 Nc <5 <5 <5 72

Aldrin <2.0 Nc <2.0 Nc <2.0 <2.0 <2.0 92

alpha-Endosulfan <.5 Nc <.5 Nc <.5 <.5 <.5 R-Delete

alpha-Hexachlorocyclohexane (BHC)<1.5 Nc <1.5 Nc <1.5 <1.5 <1.5 R-Delete

alpha-Hexachlorocyclohexane (BHC)<5 Nc <5 Nc <5 <5 <5 103

Atrazine <5 Nc <5 Nc <5 <5 <5 83

Atrazine 200 Np 200 Np <.04 <.04 <.04 100

Benfluralin <5 Nc <5 Nc <5 <5 <5 67

beta-Hexachlorobenzene <.5 Nc <.5 Nc <.5 <.5 <.5 R-Delete

Bromacil <680* Np <640* Np <.08 <.08 <.08 101

Butylate <5 Nc <5 Nc <5 <5 <5 77

Carbaryl <180* Np <250* Np <44* <.03 <.03 97

Carbaryl <5 Nc <5 Nc <5 <5 <5 110

Carbofuran <5 Nc <5 Nc <5 <5 <5 82

Chlorpyrifos 340 1.88 370 1.85 <5 <5 <5 54

Chlorpyrifos <.16 Np <.16 Np <.16 <.16 <.16 91

Cyanazine <5 Nc <5 Nc <5 <5 <5 82

Dacthal 9.02 .05 8.91 .05 <5 <5 <5 110

Diazinon <5 Nc <5 Nc <5 <5 <5 88

Diazinon <.16 Np <.16 Np <.16 <.16 <.16 95

Dieldrin 180 .84 120 .50 <.5 <.5 <.5 R-Delete

Dieldrin 300 1.09 160 .52 <5 <5 <5 110

Disulfoton <5 Nc <5 Nc <5 <5 <5 90

Endrin <1.0 Nc <1.0 Nc <1.0 <1.0 <1.0 R-Delete

Eptam (EPTC) <5 Nc <5 Nc <5 <5 <5 96

Appendix 4

Appendix 4. Concentrations of pesticides, pesticide metabolites, polychlorinated biphenyl compounds, polycyclic aromatic 

hydrocarbons, and other types of synthetic organic compounds measured in extracts from Semipermeable Membrane Devices or Polar 

Organic Chemical Integrative Samplers submerged at two stream sites on the North Canadian River adjacent to the Kickapoo tribal lands 

in central Oklahoma, January–February 2009. 

[Compound concentrations measured in extracts are reported in nanogram per ampoule of extract from a composite of three SPMD or three POCIS media in each 

sampler. Compounds that are bolded were considered detected because concentration was three times, or greater, than the highest concentration measured in the 

field or laboratory blank. A compound measured by more than one laboratory method was counted only once as a detection; site identifier, stream-gaging station 

and (number); N., north; ng/L, nanogram of compound per liter of water; ng/ampoule, nanogram of compound per ampoule of extract; <, less than; E, concentration is approximate because trace levels of contamination were found in the blanks at levels below the reporting level; R-Delete, spike fraction was lost during 

sample preparation at laboratory; --, not applicable; *, indicates compound could not be positively identified in the extract below the reported concentration 

because of chromatographic interference; Nc, not calculated because presence of the compound could not be positively identified in the extract or concentration 

was below the laboratory reporting level; UD, compound was not recovered most likely because of residual isopropanol from the addition of spike and surrogate 

solution; Np, water concentration could not be calculated because compound was measured in extract from Polar Organic Integrative Sampler which did not have 

performance reference compounds needed for calculation]
40 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

Appendix 4. Concentrations of pesticides, pesticide metabolites, polychlorinated biphenyl compounds, polycyclic aromatic 

hydrocarbons, and other types of synthetic organic compounds measured in extracts from Semipermeable Membrane Devices or Polar 

Organic Chemical Integrative Samplers submerged at two stream sites on the North Canadian River adjacent to the Kickapoo tribal 

lands in central Oklahoma, January–February 2009.—Continued 

[Compound concentrations measured in extracts are reported in nanogram per ampoule of extract from a composite of three SPMD or three POCIS media in 

each sampler. Compounds that are bolded were considered detected because concentration was three times, or greater, than the highest concentration measured 

in the field or laboratory blank. A compound measured by more than one laboratory method was counted only once as a detection; site identifier, stream-gaging 

station and (number); N., north; ng/L, nanogram of compound per liter of water; ng/ampoule, nanogram of compound per ampoule of extract; <, less than; E, 

concentration is approximate because trace levels of contamination were found in the blanks at levels below the reporting level; R-Delete, spike fraction was lost 

during sample preparation at laboratory; --, not applicable; *, indicates compound could not be positively identified in the extract below the reported concentration because of chromatographic interference; Nc, not calculated because presence of the compound could not be positively identified in the extract or concentration was below the laboratory reporting level; UD, compound was not recovered most likely because of residual isopropanol from the addition of spike and 

surrogate solution; Np, water concentration could not be calculated because compound was measured in extract from Polar Organic Integrative Sampler which 

did not have performance reference compounds needed for calculation]

Compound

PS-1

N. Canadian River at 

Hogback Road near 

Jones, Oklahoma

(07241540)

PS-2

N. Canadian River 

near Shawnee, 

Oklahoma 

(07241700)

Field blank

(ng/ampoule)

Laboratory 

blank

(ng/ampoule)

Laboratory 

reporting 

level

(ng/ampoule)

Laboratory 

spike

(percent 

recovery)

(ng/ampoule) (ng/L) (ng/ampoule) (ng/L)

Ethalfluralin <5 Nc <5 Nc <5 <5 <5 87

Ethoprop <5 Nc <5 Nc <5 <5 <5 69

Fipronil <5 Nc <5 Nc <5 <5 <5 80

Fonofos <5 Nc <5 Nc <5 <5 <5 40

Heptachlor 27.5 .10 <1.0 Nc <1.0 <1.0 <1.0 86

Hexachlorobenzene <3.0 Nc <3.0 Nc <3.0 <3.0 <3.0 84

Hexachlorobenzene <75* Nc <70* Nc <25 <25 <25 110

Lindane <5 Nc <5 Nc <5 <5 <5 92

Lindane <.5 Nc <.5 Nc <.5 <.5 <.5 R-Delete

Linuron <5 Nc <5 Nc <5 <5 <5 93

Malathion <5 Nc <5 Nc <5 <5 <5 78

Metalaxyl <.08 Np <.08 Np <.08 <.08 <.08 103

Methyl azinphos <5 Nc <5 Nc <5 <5 <5 73

Methyl parathion <5 Nc <5 Nc <5 <5 <5 37

Metolachlor <5 Nc <5 Nc <5 <5 <5 65

Metolachlor 48 Np 64 Np <.02 <.02 <.02 92

Metribuzin <5 Nc <5 Nc <5 <5 <5 67

Molinate <5 Nc <5 Nc <5 <5 <5 76

Napropamide <5 Nc <5 Nc <5 <5 <5 77

Parathion <5 Nc <5 Nc <5 <5 <5 58

Pebulate <5 Nc <5 Nc <5 <5 <5 80

Pendimethilan 240 .97 270 .97 <5 <5 <5 81

Pentachloronitrobenzene <25 Nc <25 Nc <25 <25 <25 114

Pentachlorophenol 330 Np <.16 Np <.16 <.16 <.16 104

Permethrin <5 Nc <5 Nc <5 <5 <5 80

Phorate <5 Nc <5 Nc <5 <5 <5 102

Prometon <5 Nc <5 Nc <5 <5 <5 71

Prometon 110 Np <.08 Np <.08 <.08 <.08 97

Mirex <1.5 Nc <1.5 Nc <1.5 <1.5 <1.5 93
Appendix 4 41

Appendix 4. Concentrations of pesticides, pesticide metabolites, polychlorinated biphenyl compounds, polycyclic aromatic 

hydrocarbons, and other types of synthetic organic compounds measured in extracts from Semipermeable Membrane Devices or Polar 

Organic Chemical Integrative Samplers submerged at two stream sites on the North Canadian River adjacent to the Kickapoo tribal 

lands in central Oklahoma, January–February 2009.—Continued 

[Compound concentrations measured in extracts are reported in nanogram per ampoule of extract from a composite of three SPMD or three POCIS media in 

each sampler. Compounds that are bolded were considered detected because concentration was three times, or greater, than the highest concentration measured 

in the field or laboratory blank. A compound measured by more than one laboratory method was counted only once as a detection; site identifier, stream-gaging 

station and (number); N., north; ng/L, nanogram of compound per liter of water; ng/ampoule, nanogram of compound per ampoule of extract; <, less than; E, 

concentration is approximate because trace levels of contamination were found in the blanks at levels below the reporting level; R-Delete, spike fraction was lost 

during sample preparation at laboratory; --, not applicable; *, indicates compound could not be positively identified in the extract below the reported concentration because of chromatographic interference; Nc, not calculated because presence of the compound could not be positively identified in the extract or concentration was below the laboratory reporting level; UD, compound was not recovered most likely because of residual isopropanol from the addition of spike and 

surrogate solution; Np, water concentration could not be calculated because compound was measured in extract from Polar Organic Integrative Sampler which 

did not have performance reference compounds needed for calculation]

Compound

PS-1

N. Canadian River at 

Hogback Road near 

Jones, Oklahoma

(07241540)

PS-2

N. Canadian River 

near Shawnee, 

Oklahoma 

(07241700)

Field blank

(ng/ampoule)

Laboratory 

blank

(ng/ampoule)

Laboratory 

reporting 

level

(ng/ampoule)

Laboratory 

spike

(percent 

recovery)

(ng/ampoule) (ng/L) (ng/ampoule) (ng/L)

p,p'-DDT <1.0 Nc <1.0 Nc <1.0 <1.0 <1.0 R-Delete

p,p'-Methoxychlor <3.5 Nc <3.5 Nc <3.5 <3.5 <3.5 R-Delete

Toxaphene <200 Nc <200 Nc <200 <200 <200 <200

Propachlor <5 Nc <5 Nc <5 <5 <5 76

Propanil <5 Nc <5 Nc <5 <5 <5 71

Propargite <5 Nc <5 Nc <5 <5 <5 66

Propyzamide <5 Nc <5 Nc <5 <5 <5 66

Simazine <5 Nc <5 Nc <5 <5 <5 76

Tebuthiuron <5 Nc <5 Nc <5 <5 <5 61

Terbacil <5 Nc <5 Nc <5 <5 <5 74

Terbufos <5 Nc <5 Nc <5 <5 <5 82

Thiobencarb <5 Nc <5 Nc <5 <5 <5 75

trans-Nonachlor E32 E.15 E18 E.07 <1.0 <1.0 <1.0 R-Delete

Triallate <5 Nc <5 Nc <5 <5 <5 86

Trifluralin <5 Nc <5 Nc <5 <5 <5 65

Number of detections 10 7 -- -- -- --

Pesticide metabolites

cis-Chlordane E100 E.47 E66 E.26 <1.0 <1.0 <1.0 R-Delete

trans-Chlordane E98.0 E.44 E42.0 E.16 <.5 <.5 <.5 R-Delete

p,p'-DDD <2.5 Nc <2.5 Nc <2.5 <2.5 <2.5 R-Delete

p,p'-DDE E14 E.02 <1.5 Nc <1.5 <1.5 <1.5 100

p,p'-DDE 22.9 .09 16.9 .06 <5 <5 <5 63

Deethylatrazine <5 Nc <5 Nc <5 <5 <5 80

Desulfinylfipronil <5 Nc <5 Nc <5 <5 <5 59

Desulfinylfipronil amide <5 Nc <5 Nc <5 <5 <5 61

Fipronil sulfide <5 Nc <5 Nc <5 <5 <5 42

Fipronil sulfone <5 Nc <5 Nc <5 <5 <5 33

Heptachlor epoxide 5.5 .03 35.5 .15 <1.5 <1.5 <1.5 R-Delete 

Number of detections 4 4 -- -- -- --
42 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

Appendix 4. Concentrations of pesticides, pesticide metabolites, polychlorinated biphenyl compounds, polycyclic aromatic 

hydrocarbons, and other types of synthetic organic compounds measured in extracts from Semipermeable Membrane Devices or Polar 

Organic Chemical Integrative Samplers submerged at two stream sites on the North Canadian River adjacent to the Kickapoo tribal 

lands in central Oklahoma, January–February 2009.—Continued 

[Compound concentrations measured in extracts are reported in nanogram per ampoule of extract from a composite of three SPMD or three POCIS media in 

each sampler. Compounds that are bolded were considered detected because concentration was three times, or greater, than the highest concentration measured 

in the field or laboratory blank. A compound measured by more than one laboratory method was counted only once as a detection; site identifier, stream-gaging 

station and (number); N., north; ng/L, nanogram of compound per liter of water; ng/ampoule, nanogram of compound per ampoule of extract; <, less than; E, 

concentration is approximate because trace levels of contamination were found in the blanks at levels below the reporting level; R-Delete, spike fraction was lost 

during sample preparation at laboratory; --, not applicable; *, indicates compound could not be positively identified in the extract below the reported concentration because of chromatographic interference; Nc, not calculated because presence of the compound could not be positively identified in the extract or concentration was below the laboratory reporting level; UD, compound was not recovered most likely because of residual isopropanol from the addition of spike and 

surrogate solution; Np, water concentration could not be calculated because compound was measured in extract from Polar Organic Integrative Sampler which 

did not have performance reference compounds needed for calculation]

Compound

PS-1

N. Canadian River at 

Hogback Road near 

Jones, Oklahoma

(07241540)

PS-2

N. Canadian River 

near Shawnee, 

Oklahoma 

(07241700)

Field blank

(ng/ampoule)

Laboratory 

blank

(ng/ampoule)

Laboratory 

reporting 

level

(ng/ampoule)

Laboratory 

spike

(percent 

recovery)

(ng/ampoule) (ng/L) (ng/ampoule) (ng/L)

Polychlorinated biphenyls 

Aroclor 1016/1242 E96 E0.39 E113 E0.40 <0.5 <5.0 <5.0 79

Aroclor 1254 130 2.3 120 .69 <.5 <5.0 <5.0 96

Aroclor 1260 170 3.0 150 2.20 <.5 <5.0 <5.0 99

Number of detections 3 3 -- -- -- --

Polyaromatic hydrocarbons

1-Methylnaphthalene <9.6* Np <.02 Np 7.2 <.02 <.02 97

1,2,4-Trichlorobenzene <25 Nc <25 Nc <25 <25 <25 127

1,2-Dimethylnaphthalene <130* Nc <110* Nc <110* <25 <25 111

1,6-Dimethylnaphthalene E180 E1.06 E110 E.62 E110 <25 <25 105

1-Methyl-9H-fluorene <180* Nc <150* Nc <120* <25 <25 106

1-Methylphenanthrene E200 E.75 E79 E.26 <25 <25 <25 118

1-Methylpyrene E230 E.83 E130 E.41 <25 <25 <25 118

2,3,6-Trimethylnaphthalene E188 E.76 E150 E.53 E130 <25 <25 111

2,6-Dimethylnaphthalene E210 E1.13 E150 E.74 E150 <25 <25 118

2,6-Dimethylnaphthalene <18.4* Np <.02 Np 5.2 <.02 <.02 99

2-Ethylnaphthalene E130 E.81 E110 E.62 E110 <25 <25 116

2-Methylanthracene <150* Nc <25 Nc <25 <25 <25 110

2-Methylnaphthalene 9.2 Np <.02 Np 15.2 <.02 <.02 98

4,5-Methylenephenanthrene E610 E3.56 E390 E2.06 <25 <25 <25 114

Carbazol <120* Nc <25 Nc <25 <25 <25 115

Fluorene E290 E2.34 E180 E1.39 <100* <25 <25 114

Acenaphthene E250 E1.57 E160 E.93 <50* <25 <25 103

Acenaphthylene E150 E1.11 <140* Nc <140* <25 <25 105

Anthracene <160* Nc <120* Nc <25 <25 <25 121

Anthracene <28.4* Np <34* Np <.01 <.01 <.01 96

Anthraquinone <890* Nc <440* Nc <25 <25 <25 111

Anthraquinone <56* Np <.02 Np <.02 <.02 <.02 92

Benz(a)anthracene E310 E1.24 <1,700* Nc <25 <25 <25 115
Appendix 4 43

Appendix 4. Concentrations of pesticides, pesticide metabolites, polychlorinated biphenyl compounds, polycyclic aromatic 

hydrocarbons, and other types of synthetic organic compounds measured in extracts from Semipermeable Membrane Devices or Polar 

Organic Chemical Integrative Samplers submerged at two stream sites on the North Canadian River adjacent to the Kickapoo tribal 

lands in central Oklahoma, January–February 2009.—Continued 

[Compound concentrations measured in extracts are reported in nanogram per ampoule of extract from a composite of three SPMD or three POCIS media in 

each sampler. Compounds that are bolded were considered detected because concentration was three times, or greater, than the highest concentration measured 

in the field or laboratory blank. A compound measured by more than one laboratory method was counted only once as a detection; site identifier, stream-gaging 

station and (number); N., north; ng/L, nanogram of compound per liter of water; ng/ampoule, nanogram of compound per ampoule of extract; <, less than; E, 

concentration is approximate because trace levels of contamination were found in the blanks at levels below the reporting level; R-Delete, spike fraction was lost 

during sample preparation at laboratory; --, not applicable; *, indicates compound could not be positively identified in the extract below the reported concentration because of chromatographic interference; Nc, not calculated because presence of the compound could not be positively identified in the extract or concentration was below the laboratory reporting level; UD, compound was not recovered most likely because of residual isopropanol from the addition of spike and 

surrogate solution; Np, water concentration could not be calculated because compound was measured in extract from Polar Organic Integrative Sampler which 

did not have performance reference compounds needed for calculation]

Compound

PS-1

N. Canadian River at 

Hogback Road near 

Jones, Oklahoma

(07241540)

PS-2

N. Canadian River 

near Shawnee, 

Oklahoma 

(07241700)

Field blank

(ng/ampoule)

Laboratory 

blank

(ng/ampoule)

Laboratory 

reporting 

level

(ng/ampoule)

Laboratory 

spike

(percent 

recovery)

(ng/ampoule) (ng/L) (ng/ampoule) (ng/L)

Benzo(a)pyrene <170* Nc <250* Nc <25 <25 <25 112

Benzo(a)pyrene <.01 Np <.01 Np <.01 <.01 <.01 95

Benzo(b)fluoranthene E320 E1.23 <900* Nc <25 <25 <25 118

Benzo(e)pyrene E270 E1.31 <1,100* Nc <25 <25 <25 102

Benzo(ghi)perylene E210 E1.33 <250* Nc <25 <25 <25 102

Benzo(k)fluoranthene E190 E.82 <250* Nc <25 <25 <25 119

Carbazole <22.8* Np <22* Np <.01 <.01 <.01 101

Chrysene 1,090 4.03 <1,900* Nc <25 <25 <25 115

Dibenz(ah)anthracene <250* Nc <250* Nc <25 <25 <25 105

Dibenzothiophene E170 E.90 <110* Nc <70 <25 <25 116

Fluoranthene 3,440 12.6 1,900 6.12 E84 <25 <25 127

Fluoranthene <8* Np <.01 Np <8* .64 <.01 96

Indeno(1,2,3-cd)pyrene <220* Nc <250* Nc <25 <25 <25 107

Naphthalene E190 E4.70 E140 E3.43 E230 <25 <25 109

Naphthalene 14 Np <.01 Np 21.2 <.01 <.01 97

Perylene <25 Nc <250* Nc <25 <25 <25 112

Phenanthrene 1,530 7.71 E610 E2.78 E110 <25 <25 116

Phenanthrene <13.6* Np <.01 Np 13.6 <.01 <.01 94

Pyrene 3,380 12.3 1,600 5.11 E86 <25 <25 116

Pyrene <8.4* Np <.01 Np 4.8 <.01 <.01 97

Number of detections 16 8 -- -- -- --

Synthetic organic compounds

1,4-Dichlorobenzene <.04 Np <.04 Np <.04 <.04 <.04 93

3-beta-Coprostanol2 440 Np <.16 Np <400* <.16 <.16 61

3-Methyl-1H-indole2

 (skatol) 21.2 Np 21.2 Np <.02 <.02 <.02 102

3-tert-Butyl-4-hydroxyanisole 

(BHA) 

<.08 Np <.08 Np <.08 <.08 <.08 91

4-Cumylphenol <40* Np UD Np UD UD <.02 UD

4-n-Octylphenol <64* Np UD Np UD UD <.01 UD
44 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

Appendix 4. Concentrations of pesticides, pesticide metabolites, polychlorinated biphenyl compounds, polycyclic aromatic 

hydrocarbons, and other types of synthetic organic compounds measured in extracts from Semipermeable Membrane Devices or Polar 

Organic Chemical Integrative Samplers submerged at two stream sites on the North Canadian River adjacent to the Kickapoo tribal 

lands in central Oklahoma, January–February 2009.—Continued 

[Compound concentrations measured in extracts are reported in nanogram per ampoule of extract from a composite of three SPMD or three POCIS media in 

each sampler. Compounds that are bolded were considered detected because concentration was three times, or greater, than the highest concentration measured 

in the field or laboratory blank. A compound measured by more than one laboratory method was counted only once as a detection; site identifier, stream-gaging 

station and (number); N., north; ng/L, nanogram of compound per liter of water; ng/ampoule, nanogram of compound per ampoule of extract; <, less than; E, 

concentration is approximate because trace levels of contamination were found in the blanks at levels below the reporting level; R-Delete, spike fraction was lost 

during sample preparation at laboratory; --, not applicable; *, indicates compound could not be positively identified in the extract below the reported concentration because of chromatographic interference; Nc, not calculated because presence of the compound could not be positively identified in the extract or concentration was below the laboratory reporting level; UD, compound was not recovered most likely because of residual isopropanol from the addition of spike and 

surrogate solution; Np, water concentration could not be calculated because compound was measured in extract from Polar Organic Integrative Sampler which 

did not have performance reference compounds needed for calculation]

Compound

PS-1

N. Canadian River at 

Hogback Road near 

Jones, Oklahoma

(07241540)

PS-2

N. Canadian River 

near Shawnee, 

Oklahoma 

(07241700)

Field blank

(ng/ampoule)

Laboratory 

blank

(ng/ampoule)

Laboratory 

reporting 

level

(ng/ampoule)

Laboratory 

spike

(percent 

recovery)

(ng/ampoule) (ng/L) (ng/ampoule) (ng/L)

4-Nonylphenol diethoxylate 

(NP2EO; total)

<4,000* Np UD Np 720 UD <0.32 UD

4-Nonylphenol monoethoxylate 

(NP1EO; total) 

<1,520* Np UD Np UD UD <.06 UD

4-tert-Octylphenol diethoxylate1, 7 (OP2EO; total) 

1,440 Np UD Np <640* UD <.02 UD

4-tert-Octylphenol monoethoxylate (OP1EO; total) <1,160* Np <.06 Np <120* <.06 <.06 76

4-tert-Octylphenol E44 Np <.01 Np E2.8 <.01 <.01 89

5-methyl-1H-benzotriazole4 2,200 Np 1,320 Np <.16 <.16 <.16 101

Acetophenone5 160 Np 180 Np 40 <.04 <.04 93

Benzophenone5, 7 210 Np 180 Np 44 <.04 <.04 100

beta-Sitosterol6 1,360 Np UD Np UD UD <.39 UD

beta-Stigmastanol <6,400* Np <.10 Np <3,960* <.10 <.10 143

Bisphenol A <840* Np <400* Np 26.4 UD <.02 UD

Bromoform <.08 Np <.08 Np <.08 <.08 <.08 92

Caffeine <150* Np <.04 Np <10.4* <.04 <.04 98

Camphor <.04 Np <.04 Np 4.4 <.04 <.04 96

Cholesterol E3,640 Np <.16 Np E3,040 <.16 <.16 51

Cotinine <100* Np <.04 Np 27.2 <.04 <.04 93

Cumene (Isopropylbenzene) .02 Np .02 Np 2.24 .02 .02 95

Bis(2-ethylhexyl)phthalate E450 E8.63 <800* Nc E430 <90* <90* 112

d-Limonene 19.2 Np <.08 Np 10.4 <.08 <.08 91

Diethylphthalate E273 E72.5 E250 E65.3 E260 <45* <45* 105

Ethyl citrate <.02 <.02 <.02 <.02 <.02 <.02 <.02 85

Galaxolide5, 7 (HHCB) 3,200 Np 1,240 Np 26.4 <.02 <.02 94

Indole4 200 Np 320 Np <.02 <.02 <.02 101

Isoborneol <29.6* Np UD Np UD UD <.04 UD

Isophorone4 92 Np 160 Np 2.64 <.02 <.02 87

Isoquinoline <18.4* Np <.02 Np <4.4* <.02 <.02 92

Menthol <64* Np UD Np UD UD <.16 UD
Appendix 4 45

Appendix 4. Concentrations of pesticides, pesticide metabolites, polychlorinated biphenyl compounds, polycyclic aromatic 

hydrocarbons, and other types of synthetic organic compounds measured in extracts from Semipermeable Membrane Devices or Polar 

Organic Chemical Integrative Samplers submerged at two stream sites on the North Canadian River adjacent to the Kickapoo tribal 

lands in central Oklahoma, January–February 2009.—Continued 

[Compound concentrations measured in extracts are reported in nanogram per ampoule of extract from a composite of three SPMD or three POCIS media in 

each sampler. Compounds that are bolded were considered detected because concentration was three times, or greater, than the highest concentration measured 

in the field or laboratory blank. A compound measured by more than one laboratory method was counted only once as a detection; site identifier, stream-gaging 

station and (number); N., north; ng/L, nanogram of compound per liter of water; ng/ampoule, nanogram of compound per ampoule of extract; <, less than; E, 

concentration is approximate because trace levels of contamination were found in the blanks at levels below the reporting level; R-Delete, spike fraction was lost 

during sample preparation at laboratory; --, not applicable; *, indicates compound could not be positively identified in the extract below the reported concentration because of chromatographic interference; Nc, not calculated because presence of the compound could not be positively identified in the extract or concentration was below the laboratory reporting level; UD, compound was not recovered most likely because of residual isopropanol from the addition of spike and 

surrogate solution; Np, water concentration could not be calculated because compound was measured in extract from Polar Organic Integrative Sampler which 

did not have performance reference compounds needed for calculation]

Compound

PS-1

N. Canadian River at 

Hogback Road near 

Jones, Oklahoma

(07241540)

PS-2

N. Canadian River 

near Shawnee, 

Oklahoma 

(07241700)

Field blank

(ng/ampoule)

Laboratory 

blank

(ng/ampoule)

Laboratory 

reporting 

level

(ng/ampoule)

Laboratory 

spike

(percent 

recovery)

(ng/ampoule) (ng/L) (ng/ampoule) (ng/L)

Methyl salicylate 76 Np <0.04 Np 38.8 <0.04 <0.04 96

N,N-diethyl-meta-toluamide5

(DEET)

E160 Np E130 Np E4 <.02 <.02 104

p-Cresol4 252 Np <108* Np 38 <.04 <.04 80

Pentachloroanisol4, 7 E270 E.98 E88 E.28 <25 <25 <25 110

Phenanthridine <25 Nc <25 Nc <25 <25 <25 115

p-Nonylphenol1, 7 (total) 1,600 Np <1,120* Np 384 <.16 <.16 88

Phenol4 800 Np 760 Np 268 <.04 <.04 74

Tetrachloroethylene <.08 Np <.08 Np <.08 <.08 <.08 84

Tonalide (AHTN)5, 7 376 Np 116 Np 5.6 <.02 <.02 102

Tri(2-butoxyethyl) phosphate3 E3,480 Np E2,040 Np <.08 <.08 <.08 91

Tri(2-chloroethyl) phosphate3, 7 560 Np 480 Np <.08 <.08 <.08 97

Tributyl phosphate4 E560 Np E290 Np E13.6 <.02 <.02 82

Triclosan1 E760 Np <.02 Np <.02 <.02 <.02 88

Tri(dichlorisopropyl) phosphate3, 7

480 Np 480 Np <.16 <.16 <.16 89

Triethyl citrate <.02 Np <.02 Np <.02 <.02 <.02 85

Triphenyl phosphate <.04 Np <.04 Np <.04 <.04 <.04 98

Number of detections 21 15 -- -- -- --

Surrogate compound

D6-alpha-Hexachlorocyclohexane (BHC)104 108 94 99 -- 91 

D10-Diazinon 132 132 103 67 -- 74

Isodrin 87 82 85 84 -- 82

Nonachlor 92 89 88 90 -- 84

alpha-Hexachlorocyclohexane 74 66 79 89 -- R-Delete

Nitrobenzene-d5 89 92 90 95 -- 133

2-Fluorobiphenyl 92 97 83 95 -- 110

Terphenyl-d14 96 97 102 95 -- 96

Decafluorobiphenyl 93 96 84 95 -- 92

d8-Caffeine 107 92 96 82 -- 91
46 A Reconnaissance of Selected Organic Compounds in Streams in Tribal Lands in Central Oklahoma

Appendix 4. Concentrations of pesticides, pesticide metabolites, polychlorinated biphenyl compounds, polycyclic aromatic 

hydrocarbons, and other types of synthetic organic compounds measured in extracts from Semipermeable Membrane Devices or Polar 

Organic Chemical Integrative Samplers submerged at two stream sites on the North Canadian River adjacent to the Kickapoo tribal 

lands in central Oklahoma, January–February 2009.—Continued 

[Compound concentrations measured in extracts are reported in nanogram per ampoule of extract from a composite of three SPMD or three POCIS media in 

each sampler. Compounds that are bolded were considered detected because concentration was three times, or greater, than the highest concentration measured 

in the field or laboratory blank. A compound measured by more than one laboratory method was counted only once as a detection; site identifier, stream-gaging 

station and (number); N., north; ng/L, nanogram of compound per liter of water; ng/ampoule, nanogram of compound per ampoule of extract; <, less than; E, 

concentration is approximate because trace levels of contamination were found in the blanks at levels below the reporting level; R-Delete, spike fraction was lost 

during sample preparation at laboratory; --, not applicable; *, indicates compound could not be positively identified in the extract below the reported concentration because of chromatographic interference; Nc, not calculated because presence of the compound could not be positively identified in the extract or concentration was below the laboratory reporting level; UD, compound was not recovered most likely because of residual isopropanol from the addition of spike and 

surrogate solution; Np, water concentration could not be calculated because compound was measured in extract from Polar Organic Integrative Sampler which 

did not have performance reference compounds needed for calculation]

Compound

PS-1

N. Canadian River at 

Hogback Road near 

Jones, Oklahoma

(07241540)

PS-2

N. Canadian River 

near Shawnee, 

Oklahoma 

(07241700)

Field blank

(ng/ampoule)

Laboratory 

blank

(ng/ampoule)

Laboratory 

reporting 

level

(ng/ampoule)

Laboratory 

spike

(percent 

recovery)

(ng/ampoule) (ng/L) (ng/ampoule) (ng/L)

d10-Fluoranthene 97 94 94 90 -- 88

d8-Bisphenol A 57 0 59 0 -- 0

1

 Detergent.

2

 Fecal indicator.

3

 Flame retardant.

4

 Industrial compound.

5

 Personal care product.

6

 Plant sterol.

7

 Suspected or known endocrine disruptor. 

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