U.S. Department of the Interior

U.S. Geological Survey

Reconnaissance of Organic Wastewater Compounds at

a Concentrated Swine Feeding Operation in the

North Carolina Coastal Plain, 2008

Open-File Report 2009–1128

Prepared in cooperation with the North Carolina Department of Environment and Natural

Resources, Division of Water Quality, Aquifer Protection Section
Cover photograph. Looking upstream on Sandy Run tributary west of confluence with Plum Tree Branch, Greene County, North Carolina.
Reconnaissance of Organic Wastewater 

Compounds at a Concentrated Swine 

Feeding Operation in the North Carolina 

Coastal Plain, 2008 

By Stephen L. Harden

Prepared in cooperation with the North Carolina Department of Environment and 

Natural Resources, Division of Water Quality, Aquifer Protection Section 

Open-File Report 2009–1128

U.S. Department of the Interior

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

KEN SALAZAR, Secretary

U.S. Geological Survey

Suzette M. Kimball, Acting Director

U.S. Geological Survey, Reston, Virginia: 2009

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reproduce any copyrighted materials contained within this report.

Suggested citation:

Harden, S.L., 2009, Reconnaissance of organic wastewater compounds at a concentrated swine feeding operation in 

the North Carolina Coastal Plain, 2008: U.S. Geological Survey Open-File Report 2009–1128, 14 p.
iii

Contents

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

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

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

Description of the Study Area ............................................................................................................2

Methods...........................................................................................................................................................2

Data Results....................................................................................................................................................5

Hydrologic Conditions during Sampling............................................................................................9

Organic Wastewater Compounds......................................................................................................9

Lagoon Sample...........................................................................................................................12

Groundwater and Surface-Water Samples...........................................................................12

Summary........................................................................................................................................................13

Acknowledgments.......................................................................................................................................13

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

Figures

1–2. Maps showing—

 1. Location of study area in the Neuse River basin of North Carolina..............................3

 2. Groundwater, surface-water, and lagoon sampling locations at the 

concentrated animal feeding operation study site in Greene County, 

North Carolina........................................................................................................................4

3. Graphs showing continuous data for groundwater levels at well L2 

and stream stage at site S7 at the study site in Greene County, 

North Carolina, 2008 .....................................................................................................................9

Tables

1. Water-quality and hydrologic data network at the concentrated animal 

feeding operation study site in Greene County, North Carolina, 2008 .................................5

2. Summary of dissolved organic wastewater compounds analyzed 

in samples collected from a concentrated swine feeding 

operation study site, Greene County, North Carolina, 2008...................................................6

3. Concentrations of organic wastewater compounds detected in environmental 

and quality-control samples collected from a concentrated swine feeding 

operation study site, Greene County, North Carolina, 2008.................................................10
iv

Conversion Factors

Inch/Pound to SI

Multiply By To obtain

Length

inch (in.) 2.54 centimeter (cm)

inch (in.) 25.4 millimeter (mm)

foot (ft) 0.3048 meter (m)

mile (mi) 1.609 kilometer (km)

Area

square mile (mi2) 259.0 hectare (ha)

square mile (mi2) 2.590 square kilometer (km2) 

Vertical coordinate information is referenced to North American Vertical Datum of 1988 

(NAVD 88).

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

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

Concentrations of chemical constituents in water are given in micrograms per liter (μg/L).

Abbreviations and Acronyms

CAFO Concentrated animal feeding operation

DEET N,N-diethyl-meta-toluamide

DO Dissolved oxygen

DWQ NCDENR Division of Water Quality

GC/MS/MS Gas chromatography with tandem mass spectrometry

HIA Household, industrial, and agricultural-use compounds

HPLC/MS/MS High-performance liquid chromatography with tandem mass spectrometry

IDS Isotope-dilution standard

LC/MS Liquid chromatography with mass spectrometry

NCDENR North Carolina Department of Environment and Natural Resources

NWQL USGS National Water Quality Laboratory

OWC Organic wastewater compound

PAH Polycyclic aromatic hydrocarbon

RL Reporting level

SPE Solid-phase extraction

USGS U.S. Geological Survey

WWTP Wastewater-treatment plant
Abstract

Water-quality and hydrologic data were collected during 2008 to examine the occurrence of organic wastewater 

compounds at a concentrated swine feeding operation located 

in the North Carolina Coastal Plain. Continuous groundwater 

level and stream-stage data were collected at one monitoring 

well and one stream site, respectively, throughout 2008. One 

round of environmental and quality-control samples was collected in September 2008 following a period of below-normal 

precipitation and when swine waste was not being applied to 

the spray fields. Samples were collected at one lagoon site, 

seven shallow groundwater sites, and one surface-water site 

for analysis of 111 organic wastewater compounds, including 

household, industrial, and agricultural-use compounds, sterols, 

pharmaceutical compounds, hormones, and antibiotics.

Analytical data for environmental samples collected during the study provide preliminary information on the occurrence of organic wastewater compounds in the lagoon-waste 

source material, groundwater beneath fields that receive spray 

applications of the lagoon wastes, and surface water in the 

tributary adjacent to the site. Overall, 28 organic wastewater 

compounds were detected in the collected samples, including 11 household, industrial, and agricultural-use compounds; 

3 sterols; 2 pharmaceutical compounds; 5 hormones; and 

7 antibiotics. The lagoon sample had the greatest number 

(20) and highest concentrations of compounds compared to 

groundwater and surface-water samples. The antibiotic lincomycin had the maximum detected concentration (393 micrograms per liter) in the lagoon sample. Of the 11 compounds 

identified in the groundwater and surface-water samples, 

all with reported concentrations less than 1 microgram per 

liter, only lincomycin identified in groundwater at 1 well and 

3-methyl-1H-indole and indole identified in surface water at 

1 site also were identified in the lagoon waste material.

Introduction

During the past 10 years, the North Carolina Department of Environment and Natural Resources (NCDENR) 

and U.S. Geological Survey (USGS) have conducted studies 

to characterize the quality of groundwater and surface water 

in the Coastal Plain (Harden and Spruill, 2004; Spruill and 

others, 2005; Tesoriero and others, 2005; Harden and Spruill, 

2008), and in the Piedmont and Mountain regions (Chapman and others, 2005; McSwain and others, 2008; Pippin 

and others, 2008) of North Carolina. Characterizing waterquality conditions in different hydrogeologic settings includes 

understanding the potential effects of local land use. Some of 

the sites with different land-use conditions previously investigated by NCDENR and USGS include agricultural areas with 

concentrated animal feeding operations (CAFOs) in which 

lagoon and spray-field treatment systems are used (Harden and 

Spruill, 2004; Spruill and others, 2005; Harden and Spruill, 

2008) and a wastewater-treatment plant (WWTP) where past 

operations have included applications of municipal biosolids 

to surrounding fields (McSwain and others, 2008). A common 

objective of these studies was to document the distribution 

and amounts of nutrients in groundwater and(or) surface water 

originating from fields with different sources of applied nutrients, such as conventional fertilizers, swine lagoon effluent, or 

municipal biosolids.

Results of additional studies have shown that wastewater 

and(or) biosolids from livestock operations and municipal 

WWTPs can be contaminant sources of industrial chemicals, 

pesticides, flame retardants, pharmaceuticals and personalcare products, hormones, and antibiotics in both groundwater 

(MacKie and others, 2006; Arnon and others, 2008; Barnes 

and others, 2008) and surface water (Kolpin and others, 2002; 

Managaki and others, 2007; Focazio and others, 2008; Topp 

and others, 2008). There is growing interest in understanding 

Reconnaissance of Organic Wastewater Compounds 

at a Concentrated Swine Feeding Operation in the 

North Carolina Coastal Plain, 2008 

By Stephen L. Harden
2 Organic Wastewater Compounds at a Concentrated Swine Feeding Operation in the North Carolina Coastal Plain, 2008

the occurrence, fate, and transport of organic wastewater 

compounds (OWCs) in the environment because of concerns 

that these compounds may influence human and ecological 

health through toxicity, endocrine disruption, and promotion of antimicrobial resistance (Daughton and Ternes, 1999; 

Kolpin and others, 2002; MacKie and others, 2006; Arnon 

and others, 2008; Barnes and others, 2008). In North Carolina 

and throughout the Nation, increased knowledge is needed 

on how different waste and fertilizer management practices 

affect the occurrence of OWCs in the environment. Part of the 

mission of the NCDENR Division of Water Quality (DWQ) 

is to preserve and protect the groundwater and surface-water 

resources of North Carolina by characterizing groundwater 

flow in a variety of hydrogeologic settings and documenting the occurrence and mobility of both naturally occurring 

and land-use related contaminants. In 2008, NCDENR and 

USGS conducted a pilot study of OWCs at a swine CAFO 

in North Carolina, which is one of the top swine-producing 

states in the Nation (Center on Globalization, Governance & 

Competitiveness, 2007).

Purpose and Scope

This report summarizes a single set of water-quality and 

hydrologic data collected during 2008 at one swine CAFO 

located in the Neuse River basin, North Carolina (fig. 1). 

Water-quality data were collected during one sampling event 

in September 2008 at one lagoon site, seven groundwater 

sites, and one surface-water site. Continuous groundwater 

level and stream-stage data were collected at one monitoring 

well (L2) and one stream site (S7), respectively, throughout 

2008. Data presented in this report are intended to assist 

the DWQ in developing a broader water-quality sampling 

program to understand the presence, transport, and fate of 

OWCs in areas affected by applications of animal waste and 

municipal biosolids.

Description of the Study Area

The study was conducted at a farm located in Greene 

County in the North Carolina Coastal Plain Physiographic 

Province and south of the confluence of Sandy Run and 

Middle Swamp (figs. 1, 2). The hydrogeologic framework 

and water-quality conditions at the farm site have been well 

characterized during more than 10 years of study (Harden 

and Spruill, 2004, 2008; Spruill and others, 2005; Tesoriero 

and others, 2005; Harden, 2008). A 5,000-head swine CAFO 

in which a lagoon and spray-field treatment system are used 

has been in operation at this location since 1995. Most of 

the site is drained by a first-order stream, known locally as 

Plum Tree Branch, which is a tributary to Sandy Run and 

drains 0.59 square mile (mi2). Land use in the area is primarily agricultural, with typical row crops being corn, wheat, and 

soybeans. Agricultural fields at the site consist of somewhat 

poorly drained to well-drained soils.

Methods

The sampling network for the study (fig. 2; table 1) 

included one waste-lagoon site (LG1), seven well sites (L2M, 

L2D, L15M, L15D, L70D, L71D, and L72), and one surfacewater site (S7). Submersible pressure transducers were used 

to record stream stage at site S7 and groundwater levels at 

site L2, adjacent to groundwater sampling sites L2M and 

L2D (fig. 2). Data were recorded at these sites at 15-minute 

intervals throughout 2008. Wells at the CAFO study site are 

located in and around the spray-application fields. The wells 

were completed in the surficial aquifer at depths less than 

25 feet (table 1). Shallow groundwater at the site flows to the 

northwest and north toward the discharge areas at Plum Tree 

Branch and Sandy Run, respectively (Tesoriero and others, 

2005; Harden and Spruill, 2008). Wells L2, L2M, and L2D 

are collocated along the southern boundary of the spray fields 

(fig. 2) in an upgradient area of the groundwater-flow path. 

Well pair L15M and L15D and well L71D are located along 

the northern boundary of the spray fields in a downgradient 

area of the flow path. Well L70D is located in the middle of 

the spray fields, and well L72 is near the western boundary of 

the spray fields in the riparian buffer next to Plum Tree Branch 

(fig. 2). Surface-water site S7, located upstream of well L72, 

receives drainage from the spray fields, non-spray fields, and 

areas upstream from the study site.

Water-quality samples were collected during September 22–24, 2008, for analysis of OWCs, including household, 

industrial, and agricultural-use (HIA) compounds, sterols, 

pharmaceutical compounds, hormones, and antibiotics. 

Specific conductance, pH, water temperature, and dissolvedoxygen (DO) concentrations in samples were determined in 

the field at the time of sampling. Established, documented 

protocols for collecting and processing water samples for 

chemical analyses were followed (U.S. Geological Survey, 

variously dated). Sampling personnel also adhered to stringent 

quality-control requirements during sample collection, which 

included avoiding contact with insect repellents, antibacterial 

cleaners, caffeine, tobacco, and targeted pharmaceuticals (U.S. 

Geological Survey, variously dated). Samples from the wells 

and the lagoon were collected by using Teflon® tubing and a 

peristaltic pump. At stream site S7, a grab sample was collected directly into a sample bottle. Quality-control samples, 

including a source-solution blank, field-equipment blank, and 

a replicate sample, were collected during the sampling event 

to ensure that sampling procedures did not introduce contamination during the collection of the environmental samples. All 

samples were collected into pre-cleaned amber glass bottles 

or Teflon® bottles (depending on analytical requirements), 

chilled, and shipped by overnight delivery to the USGS 

analyzing laboratories. 

Three laboratory analytical methods were used in this 

study to test for as many as 111 compounds in each sample, 

including 55 HIAs, 4 sterols, 4 pharmaceutical compounds, 
Methods 3

WILSON

NASH

MARTIN

BERTIE

GREENE

EDGECOMBE

SAMPSON JONES

WAYNE

JOHNSTON

WAKE

FRANKLIN

LENOIR

PITT

CRAVEN

BEAUFORT

78 77

Generalized physiographic province line

Basin boundary

EXPLANATION

Greenville

Neuse

River

Basin

Washington

New Bern

BLUE RIDGE

PIEDMONT COASTAL PLAIN

LOCATION OF STUDY AREA, PHYSIOGRAPHIC PROVINCES, AND THE NEUSE RIVER BASIN IN NORTH CAROLINA

0 25 MILES

0 25 KILOMETERS

36

35

Figure 1. Location of study area in the Neuse River basin, North Carolina. 

Kinston

Bear

Little Contentnea

Contentnea

Cr.

Cr.

Creek

Neuse

Neuse R.

River

Area enlarged

in figure 2

Figure 1. Location of study area in the Neuse River basin of North Carolina.
4 Organic Wastewater Compounds at a Concentrated Swine Feeding Operation in the North Carolina Coastal Plain, 2008

S7

S7 L2, L2M and

L2D

L70D

L2

Sandy

Run

Plum Tree

Branch

Spray

fields

Non-spray

field

Waste

lagoon

Middle

Swamp

Non-spray

field

L71D

L15M

L15D

L72

3531’

3531’30”

3532’

77 77 33’30” 34’ 77

33’

EXPLANATION

Base from digital files of

U.S. Geological Survey

Digital Raster Graph, Farmville Quad

1:24,000

Figure 2. Groundwater, surface water, and lagoon sample locations at the CAFO study site, Greene County,

 North Carolina.

0 2,000 4,000 FEET

0 500 1,000 METERS

Riparian

buffer

HALF MOON POCOSIN

Surface-water sampling site and number

Groundwater sampling site and number

Lagoon grab sampling site and number

Field ditch

Hog houses

LG1

LG1

Figure 2. Groundwater, surface-water, and lagoon sampling locations at the concentrated animal feeding operation 

study site in Greene County, North Carolina.
Data Results 5

17 hormones, and 31 antibiotics (table 2). All analyses were 

performed on filtered samples and, therefore, the results 

represent compounds present in the dissolved phase. Analytical method 1 is a USGS-approved production method (Zaugg 

and others, 2006) that was used to analyze for 60 organic 

compounds spanning several classes of chemicals, including 

54 HIAs (such as fire retardants, non-ionic surfactants, plasticizers, solvents, disinfectants, polycyclic aromatic hydrocarbons (PAHs), and high-use domestic pesticides), 4 sterols, 

and 2 pharmaceutical compounds (caffeine and cotinine). 

Analytical method 2 is a research method that was used to 

analyze for 17 hormones, 1 HIA, and 2 sterols. This method 

employs isotope-dilution quantitation to improve quantitative 

accuracy by accounting for sample-specific procedural losses 

in the determined analyte concentrations (William Foreman, 

U.S. Geological Survey, written commun., 2009). Deuteriumlabeled isotope-dilution standards (IDSs) were added to 

all environmental and quality-assurance samples prior to 

extraction. The method analytes and IDSs in samples were 

extracted by using solid-phase extraction (SPE). Analysis was 

peformed by using capillary-column gas chromatography with 

tandem mass spectrometry (GC/MS/MS). Analyte concentrations were quantified relative to specific IDS concentrations 

in the sample, which directly compensates for procedural 

losses (or recovery) in the determined and reported analyte 

concentrations. The two sterols analyzed by using method 2 

(3-beta-coprostanol and cholesterol) also were analyzed by 

using method 1 (table 2). Analyses for methods 1 and 2 were 

conducted at the USGS National Water Quality Laboratory 

(NWQL) in Lakewood, Colorado.

Analytical method 3 is a research method that was used 

to analyze for 2 pharmaceutical compounds (carbamazepine 

and ibuprofen) and 31 human and veterinary antibiotics and 

selected degradation products. Target analytes were extracted 

by using online SPE and analyzed by high-performance liquid 

chromatography with tandem mass spectrometry (HPLC/MS/

MS) using positive and negative electrospray-ionization with 

multiple reaction monitoring modified from the online SPE 

LC/MS method of Meyer and others (2007). Target compounds were identified by using relative retention time and the 

ratio of the quantitation-to-confirming daughter-ion ratio and 

were quantified by using a multilevel extracted standard curve. 

Method 3 was performed by the USGS Organic Geochemistry 

Research Laboratory in Lawrence, Kansas. The laboratory 

reporting levels (RLs) for the OWCs analyzed in the groundwater and surface-water samples collected during the study 

are provided in table 2. Analytical RLs for the lagoon sample 

generally are 2 to 100 times higher than those listed in table 2 

because the concentrated waste material required dilutions 

prior to laboratory analysis.

Data Results

Upon initiation of this project, scheduling constraints 

required the water-quality sampling to be conducted in late 

summer 2008. One round of water-quality sampling was performed during September 22–24, 2008, to test for the presence 

of OWCs in groundwater, surface water, and lagoon waste 

Table 1. Water-quality and hydrologic data network at the concentrated animal feeding operation study site in Greene County, 

North Carolina, 2008.

[USGS, U.S. Geological Survey; ft bls, feet below land surface; —, not applicable]

USGS station name

Map 

number

(see fig. 2)

Well depth

(ft bls) USGS site number Sample/data type Sample date/time

SR5-LG1 LG1 — 353126077334201 Lagoon grab sample 09/24/08 1240

GR-082 L2 N26q2 nr Lizzie, NC (surficial) L2 16 353103077333401 Groundwater levels 2008

GR-088 LWQ2M L2M 11.4 353103077333407 Groundwater sample 09/23/08 1720

GR-088 L2D L2D 20 353103077333402 Groundwater sample 09/24/08 0855

GR-167 LWQ15M L15M 11.6 353127077333705 Groundwater sample 09/22/08 1415

GR-109 L15D L15D 23 353127077333704 Source solution blank 09/22/08 1000

Groundwater sample 09/22/08 1650

GR-169 LWQ70D L70D 14.6 353114077333102 Field equipment blank 09/23/08 1325

Groundwater sample 09/23/08 1500

Replicate sample 09/23/08 1505

GR-171 LWQ71D L71D 14.2 353126077332102 Groundwater sample 09/24/08 1035

GR-203 LWQ72 L72 10 353114077334905 Groundwater sample 09/24/08 1310

Unnamed trib to Sandy Run at SR1335 near 

Lizzie, NC

S7 — 0209173150 Surface-water sample 09/23/08 1150

Stream stage 2008
6 Organic Wastewater Compounds at a Concentrated Swine Feeding Operation in the North Carolina Coastal Plain, 2008

 

Table 2. Summary of dissolved organic wastewater compounds analyzed in samples collected from a concentrated swine feeding 

operation study site, Greene County, North Carolina, 2008.—Continued

[Analytical method 1 is an approved U.S. Geological Survey production method; methods 2 and 3 are U.S. Geological Survey research methods. Cholesterol and 

3-beta-coprostanol were analyzed by more than one method. μg/L, micrograms per liter; —, not detected; E, estimated concentration]

Analytical 

method 

(see text)

Organic wastewater compound

Reporting 

level 

(μg/L)

Minimum 

concentration 

detected (μg/L)

Maximum 

concentration 

detected (μg/L)

Number 

of 

detections

Total 

number of 

samples

Household, industrial, and agricultural-use compounds

1 1,4-dichlorobenzene 0.1 — — 0 12

1 1-methylnaphthalene 0.1 — — 0 12

1 2,6-dimethylnaphthalene 0.1 — — 0 12

1 2-methylnaphthalene 0.1 — — 0 12

1 3-methyl-1H-indole (skatol) 0.08 E0.014 38 2 12

1 3-tert-butyl-4-hydroxyanisole (BHA) 0.6 — — 0 12

1 4-cumylphenol 0.1 — — 0 12

1 4-nonylphenol 1.0 E0.7 E0.7 1 12

1 4-nonylphenol diethoxylate (NP2EO) 5.0 — — 0 12

1 4-normal-octylphenol 0.16 — — 0 12

1 4-tert-octylphenol 1.0 — — 0 12

1 4-tert-octylphenol diethoxylate (OP2EO) 1.0 — — 0 12

1 4-octylphenol monoethoxylate (OP1EO) 1.0 — — 0 12

1 5-methyl-1H-benzotriazole 0.08 — — 0 12

1 9,10-anthraquinone 0.2 — — 0 12

1 Acetophenone 0.4 — — 0 12

1 Acetyl-hexamethyl tetrahydronaphthalene (AHTN) 0.5 — — 0 12

1 Anthracene 0.1 — — 0 12

1 Benzo[a]pyrene 0.1 — — 0 12

1 Benzophenone 0.1 E0.03 E0.1 2 12

2 Bisphenol-A 0.100 0.139 0.139 1 12

1 Bromacil 0.4 — — 0 12

1 Camphor 0.1 E0.1 E0.1 1 12

1 Carbaryl 1.0 — — 0 12

1 Carbazole 0.1 — — 0 12

1 Chlorpyrifos 0.1 — — 0 12

1 Diazinon 0.1 — — 0 12

1 d-Limonene 0.4 — — 0 12

1 Fluoranthene 0.1 — — 0 12

1 Hexahydro-hexamethyl cyclopentabenzopyran (HHCB) 0.5 — — 0 12

1 Indole 0.1 E0.01 E4.5 2 12

1 Isoborneol 0.1 — — 0 12

1 Isophorone 0.1 — — 0 12

1 Isopropylbenzene (cumene) 0.1 — — 0 12

1 Isoquinoline 0.2 — — 0 12

1 Menthol 0.2 — — 0 12

1 Metalaxyl 0.1 — — 0 12

1 Methyl salicylate 0.1 — — 0 12

1 Metolachlor 0.1 — — 0 12

1 Naphthalene 0.1 — — 0 12

1 N,N-diethyl-meta-toluamide (DEET) 0.1 0.8 1.4 2 12

1 para-Cresol 0.18 — — 0 12
Methods 7

Table 2. Summary of dissolved organic wastewater compounds analyzed in samples collected from a concentrated swine feeding 

operation study site, Greene County, North Carolina, 2008.—Continued

[Analytical method 1 is an approved U.S. Geological Survey production method; methods 2 and 3 are U.S. Geological Survey research methods. Cholesterol and 

3-beta-coprostanol were analyzed by more than one method. μg/L, micrograms per liter; —, not detected; E, estimated concentration]

Analytical 

method 

(see text)

Organic wastewater compound

Reporting 

level 

(μg/L)

Minimum 

concentration 

detected (μg/L)

Maximum 

concentration 

detected (μg/L)

Number 

of 

detections

Total 

number of 

samples

Household, industrial, and agricultural-use compounds—Continued

1 Phenanthrene 0.1 — — 0 12

1 Phenol 0.2 100 100 1 12

1 Prometon 0.2 — — 0 12

1 Pyrene 0.1 — — 0 12

1 Tetrachloroethylene 0.1 — — 0 12

1 Tris(2-butoxyethyl) phosphate 0.4 — — 0 12

1 Tris(2-chloroethyl) phosphate (FYROL CEF) 0.1 E5.3 E5.3 1 12

1 Tris(dichloroisopropyl) phosphate (FYROL FR2) 0.1 E0.1 E0.1 1 12

1 Tributyl phosphate 0.2 — — 0 12

1 Tribromomethane 0.1 — — 0 12

1 Triclosan 0.2 — — 0 12

1 Triethyl citrate (ethyl citrate) 0.2 — — 0 12

1 Triphenyl phosphate 0.1 E0.1 E0.1 1 12

Sterols

1 3-beta-coprostanol 1.0 E170 E170 1 12

2 3-beta-coprostanol 2 E174 E174 1 12

1 beta-sitosterol 2.0 — — 0 12

1 beta-stigmastanol 1.0 E78 E78 1 12

1 Cholesterol 1.0 — — 0 12

2 Cholesterol 2 26 26 1 12

Pharmaceuticals

1 Caffeine 0.1 E4.2 E4.2 1 12

3 Carbamazepine 0.005 — — 0 12

1 Cotinine 0.4 — — 0 12

3 Ibuprofen 0.05 0.477 0.477 1 12

Hormones

2 11-ketotestosterone 0.002 0.186 0.186 1 12

2 17-alpha-estradiol 0.008 — — 0 12

2 17-beta-estradiol 0.0008 — — 0 12

2 17-alpha-ethynylestradiol 0.0008 — — 0 12

2 Norethindrone 0.0008 — — 0 12

2 4-androstene-3,17-dione 0.0008 E0.00042 E0.00051 2 12

2 Cis-androsterone 0.0008 E0.00025 0.165 2 12

2 Dihydrotestosterone 0.004 — — 0 12

2 Epitestosterone 0.004 — — 0 12

2 Equilenin 0.002 — — 0 12

2 Equilin 0.004 — — 0 12

2 Estriol 0.002 0.0877 0.0877 1 12

2 Estrone 0.0008 0.804 0.804 1 12

2 Mestranol 0.0008 — — 0 12

2 Progesterone 0.008 — — 0 12

2 Trans-diethylstilbestrol 0.0008 — — 0 12

2 Testosterone 0.0008 — — 0 12
8 Organic Wastewater Compounds at a Concentrated Swine Feeding Operation in the North Carolina Coastal Plain, 2008

Table 2. Summary of dissolved organic wastewater compounds analyzed in samples collected from a concentrated swine feeding 

operation study site, Greene County, North Carolina, 2008.—Continued

[Analytical method 1 is an approved U.S. Geological Survey production method; methods 2 and 3 are U.S. Geological Survey research methods. Cholesterol and 

3-beta-coprostanol were analyzed by more than one method. μg/L, micrograms per liter; —, not detected; E, estimated concentration]

Analytical 

method 

(see text)

Organic wastewater compound

Reporting 

level 

(μg/L)

Minimum 

concentration 

detected (μg/L)

Maximum 

concentration 

detected (μg/L)

Number 

of 

detections

Total 

number of 

samples

Antibiotics (*degradation product)

3 Azithromycin 0.005 — — 0 12

3 Chloramphenicol 0.10 — — 0 12

3 Chlorotetracycline 0.01 — — 0 12

3 Ciprofloxacin 0.005 — — 0 12

3 Doxycycline 0.01 — — 0 12

3 Enrofloxacin 0.005 — — 0 12

3 Epi-iso-chlorotetracycline* 0.01 36 36 1 12

3 Epi-chlorotetracycline* 0.01 — — 0 12

3 Epi-oxytetracycline* 0.01 — — 0 12

3 Epi-tetracycline* 0.01 0.02 0.02 1 12

3 Erythromycin 0.008 — — 0 12

3 Erythromycin-H20* 0.008 — — 0 12

3 Iso-chlorotetracycline* 0.01 52 52 1 12

3 Lincomycin 0.005 0.018 393 2 12

3 Lomefloxacin 0.005 — — 0 12

3 Norfloxacin 0.005 — — 0 12

3 Ofloxacin 0.005 — — 0 12

3 Ormetoprim 0.005 — — 0 12

3 Oxytetracycline 0.01 55 55 1 12

3 Roxithromycin 0.005 — — 0 12

3 Sarafloxacin 0.005 — — 0 12

3 Sulfachloropyridazine 0.005 — — 0 12

3 Sulfadiazine 0.01 — — 0 12

3 Sulfadimethoxine 0.005 — — 0 12

3 Sulfamethazine 0.005 1.15 1.15 1 12

3 Sulfamethoxazole 0.005 — — 0 12

3 Sulfathiazole 0.05 — — 0 12

3 Tetracycline 0.010 0.572 0.572 1 12

3 Trimethoprim 0.005 — — 0 12

3 Tylosin 0.008 — — 0 12

3 Virginiamycin 0.005 — — 0 12

 

 
Data Results 9

at the CAFO study site. Groundwater-level and streamflow 

data were collected throughout 2008 as part of other work at 

the study site. The hydrologic conditions during the sampling 

event and the analytical results of water-quality samples collected at the CAFO are summarized below. Analytical data 

for environmental samples collected during the study provide 

preliminary results on the occurrence of OWCs, hormones, 

and antibiotics in the lagoon-waste source material, the 

groundwater beneath the fields that receive spray applications 

of the lagoon wastes, and in the surface water in the tributary 

adjacent to the site. 

Hydrologic Conditions during Sampling

The September 22–24, 2008, sampling was preceded 

by a period of below-average precipitation, as noted in 

data recorded from a raingage (USGS Station number 

353137077332801) at the site. The total monthly precipitation (in inches) for May (2.19), June (1.21), July (2.43), and 

August (2.44) in 2008 was considerably less than the median 

monthly totals recorded for May (4.39), June (4.41), July 

(4.63), and August (5.67) during the 7-year period from 2001 

through 2007. The relatively dry conditions from May to 

August 2008 are reflected in the groundwater hydrograph at 

site L2 and the stream hydrograph at site S7 (fig. 3). During 

sampling, the groundwater level at site L2 and stream stage 

at site S7 were near the annual low for the 2008 period of 

data collection (fig. 3). Gaps in the stream hydrograph at site 

S7 from late May through early July indicate missing data 

because of equipment failure, and data gaps from mid-July 

to early September indicate dry periods when no streamflow 

occurred. No recent applications of lagoon-waste material 

in the spray fields were noted immediately before or during sample collection. Based on the available data, it is not 

known whether the constituent concentrations observed during 

September 2008 are representative of those that would be 

observed during periods of normal amounts of rainfall, higher 

groundwater levels, higher streamflows, or more recent applications of lagoon waste.

Organic Wastewater Compounds

A total of 9 environmental samples (1 lagoon sample, 

7 groundwater samples, and 1 stream sample) and 3 qualitycontrol samples, including a source-solution blank, fieldequipment blank, and replicate sample, were collected for 

analyses of 111 OWCs. The analytes listed in table 2 include 

the RLs, minimum and maximum observed concentrations, 

and number of detections for both the regular environmental 

samples and the quality-control samples.

Of the 111 analytes examined, 28 were detected in 

samples collected at the study site, including 11 HIAs, 3 sterols, 2 pharmaceutical compounds, 5 hormones, and 7 antibiotics (table 2). Of the 28 analytes detected, 21 were detected 

only once; 7 analytes each were detected twice (table 2). 

Concentrations of the 28 detected analytes, including estimated values, are summarized for each sample in table 3. Concentrations of 3-beta-coprostanol, determined by using both 

methods 1 and 2, are included in table 3. Approximately half 

of the analyte detections were reported as qualified “E” values, 

indicating that the compounds were identified (based on 

stringent laboratory analyte confirmational criteria) in samples 

at estimated concentrations less than the analytical RLs. In 

these cases, the analyzing laboratory confirmed the presence 

of the analytes in the samples but with less confidence (greater 

uncertainty) in the reported concentrations.

Data for the quality-control samples were examined to 

determine if any of the analytes detected in the environmental samples potentially were influenced by sampling and(or) 

analytical methodologies. Results of the source-solution blank 

indicate that the water used to prepare the field-equipment 

blank contained none of the analytes detected in the environmental samples (table 3). The field-equipment blank was used 

to determine if the sampling equipment (tubing and bottles) 

and processing or laboratory handling were potential sources 

of contaminants identified in the environmental water samples. 

Sept. 22–24

Sept. 22–24

1/1 2/1

77

75

73

71

69

67

3/1 4/1 5/1 6/1 7/1

2008

8/1 9/1 10/1 11/1 12/1

A

WATER LEVEL IN FEET ABOVE NAVD 88

4.70

4.50

4.30

4.10

3.90

3.70

3.50

B

STREAM STAGE IN FEET

Figure 3. Continuous data for (A) groundwater levels at 

well L2 and (B) stream stage at site S7 at the study site in 

Greene County, North Carolina, 2008.
10 Organic Wastewater Compounds at a Concentrated Swine Feeding Operation in the North Carolina Coastal Plain, 2008

Table 3. Concentrations of organic wastewater compounds detected in environmental and quality-control samples collected from a concentrated swine feeding operation study site, Greene County, North Carolina, 2008.[HIAs, household, industrial, and agricultrual-use compounds; μg/L, micrograms per liter; Numbers in parentheses are U.S. Geological Survey parameter codes; <, less than; E, estimated concentration; italics indicate quality-control samples]

Map 

number

(fig. 2, 

table 1)

Sample

date/time Sample type

HIAs

3-Methyl-1Hindole, filtered, 

μg/L

(62058)

4-Nonylphenol 

(all isomers), 

filtered, μg/L 

(62085)

Benzophenone, 

filtered, μg/L

(62067)

Bisphenol-A, 

filtered, μg/L

(67304)

Camphor, 

filtered, 

μg/L

(62070)

Indole, 

filtered, 

μg/L

(62076)

DEET, 

filtered, 

μg/L

(62082)

Phenol, 

filtered, 

μg/L

(34466)

Tris(2-chloroethyl)

phosphate, 

filtered, μg/L

(62087)

LG1 09/24/08 1240 Lagoon 38 < 100 < 12 0.139 < 10 E4.5 < 10 100 E5.3L2M 09/23/08 1720 Groundwater < 0.08 < 1 < 0.1 < 0.100 < 0.1 < 0.1 < 0.1 < 0.2 < 0.1L2D 09/24/08 0855 Groundwater < 0.08 < 1 E0.1 < 0.100 < 0.1 < 0.1 1.4 < 0.2 < 0.1L15M 09/22/08 1415 Groundwater < 0.08 < 1 < 0.1 < 0.100 < 0.1 < 0.1 < 0.1 < 0.2 < 0.1L15D 09/22/08 1000 Source solution blank < 0.08 < 1 < 0.1 < 0.100 < 0.1 < 0.1 < 0.1 < 0.2 < 0.1L15D 09/22/08 1650 Groundwater < 0.08 < 1 < 0.1 < 0.100 < 0.1 < 0.1 < 0.1 < 0.2 < 0.1L70D 09/23/08 1325 Field equipment blank < 0.08 < 1 < 0.1 < 0.100 < 0.1 < 0.1 < 0.1 < 0.2 < 0.1L70D 09/23/08 1500 Groundwater < 0.08 < 1 < 0.1 < 0.100 < 0.1 < 0.1 < 0.1 < 0.2 < 0.1L70D 09/23/08 1505 Replicate < 0.08 < 1 < 0.1 < 0.100 < 0.1 < 0.1 < 0.1 < 0.2 < 0.1L71D 09/24/08 1035 Groundwater < 0.08 E0.7 < 0.1 < 0.100 < 0.1 < 0.1 < 0.1 < 0.2 < 0.1L72 09/24/08 1310 Groundwater < 0.08 < 1 E0.03 < 0.100 < 0.1 < 0.1 0.8 < 0.2 < 0.1S7 09/23/08 1150 Surface water E0.014 < 1 < 0.1 < 0.100 E0.1 E0.01 < 0.1 < 0.2 < 0.1

Map 

number

(fig. 2, 

table 1)

Sample

date/time Sample type

HIAs Sterols Pharamaceuticals Hormones

Tris(dichloroisopropyl) 

phosphate, 

filtered, μg/L 

(62088)

Triphenyl 

phosphate, 

filtered, 

μg/L

(62092)

3-betaCoprostanol, 

filtered,

μg/L

(62057 – 

method 1)

3-betaCoprostanol, 

filtered,

μg/L

(64512 – 

method 2)

beta-Stigmastanol, 

filtered, 

μg/L

(62086)

Cholesterol, 

filtered, 

μg/L

(64514)

Caffeine, 

filtered, 

μg/L

(50305)

Ibuprofen, 

filtered, 

μg/L

(62014)

11-Ketotestosterone, 

filtered,

μg/L

(64507)

LG1 09/24/08 1240 Lagoon < 12 < 10 E170 E174 E78 26 E4.2 < 0.05 0.186L2M 09/23/08 1720 Groundwater < 0.1 E0.1 < 1 < 2 < 1 < 2 < 0.1 < 0.05 < 0.002L2D 09/24/08 0855 Groundwater E0.1 < 0.1 < 1 < 2 < 1 < 2 < 0.1 0.477 < 0.002L15M 09/22/08 1415 Groundwater < 0.1 < 0.1 < 1 < 2 < 1 < 2 < 0.1 < 0.05 < 0.002L15D 09/22/08 1000 Source solution blank < 0.1 < 0.1 < 1 < 2 < 1 < 2 < 0.1 < 0.05 < 0.002L15D 09/22/08 1650 Groundwater < 0.1 < 0.1 < 1 < 2 < 1 < 2 < 0.1 < 0.05 < 0.002L70D 09/23/08 1325 Field equipment blank < 0.1 < 0.1 < 1 < 2 < 1 < 2 < 0.1 < 0.05 < 0.002L70D 09/23/08 1500 Groundwater < 0.1 < 0.1 < 1 < 2 < 1 < 2 < 0.1 < 0.05 < 0.002L70D 09/23/08 1505 Replicate < 0.1 < 0.1 < 1 < 2 < 1 < 2 < 0.1 < 0.05 < 0.002L71D 09/24/08 1035 Groundwater < 0.1 < 0.1 < 1 < 2 < 1 < 2 < 0.1 < 0.05 < 0.002L72 09/24/08 1310 Groundwater < 0.1 < 0.1 < 1 < 2 < 1 < 2 < 0.1 < 0.05 < 0.002S7 09/23/08 1150 Surface water < 0.1 < 0.1 < 1 < 2 < 1 < 2 < 0.1 < 0.05 < 0.002
Data Results 11

Map 

number

(fig. 2, 

table 1)

Sample

date/time Sample type

Hormones Antibiotics

4-Androstene3,17-dione, 

filtered, μg/L

(64513)

Cis-androsterone, filtered, 

μg/L

(64515)

Estriol, 

filtered, 

μg/L

(64515)

Estrone, 

filtered, 

μg/L

(64521)

Epi-isochlorotetracycline, 

filtered, 

μg/L

(64047)

Epi-tetracycline, 

filtered, 

μg/L

(63727)

Isochlorotetracycline, 

filtered, 

μg/L

(64175)

Lincomycin, 

filtered, 

μg/L

(62894)

Oxytetracycline, 

filtered, 

μg/L

(61759)

LG1 09/24/08 1240 Lagoon < 0.490 0.165 0.0877 0.804 36 0.02 52 393 55L2M 09/23/08 1720 Groundwater < 0.0008 < 0.0008 < 0.002 < 0.0008 < 0.01 < 0.01 < 0.01 < 0.005 < 0.01L2D 09/24/08 0855 Groundwater < 0.0008 < 0.0008 < 0.002 < 0.0008 < 0.01 < 0.01 < 0.01 < 0.005 < 0.01L15M 09/22/08 1415 Groundwater < 0.0008 < 0.0008 < 0.002 < 0.0008 < 0.01 < 0.01 < 0.01 < 0.005 < 0.01L15D 09/22/08 1000 Source solution blank < 0.0008 < 0.0008 < 0.002 < 0.0008 < 0.01 < 0.01 < 0.01 < 0.005 < 0.01L15D 09/22/08 1650 Groundwater E0.00042 < 0.0008 < 0.002 < 0.0008 < 0.01 < 0.01 < 0.01 < 0.005 < 0.01L70D 09/23/08 1325 Field equipment blank < 0.0008 E0.00025 < 0.002 < 0.0008 < 0.01 < 0.01 < 0.01 < 0.005 < 0.01L70D 09/23/08 1500 Groundwater < 0.0008 < 0.0008 < 0.002 < 0.0008 < 0.01 < 0.01 < 0.01 < 0.005 < 0.01L70D 09/23/08 1505 Replicate < 0.0008 < 0.0008 < 0.002 < 0.0008 < 0.01 < 0.01 < 0.01 < 0.005 < 0.01L71D 09/24/08 1035 Groundwater < 0.0008 < 0.0008 < 0.002 < 0.0008 < 0.01 < 0.01 < 0.01 0.018 < 0.01L72 09/24/08 1310 Groundwater < 0.0008 < 0.0008 < 0.002 < 0.0008 < 0.01 < 0.01 < 0.01 < 0.005 < 0.01S7 09/23/08 1150 Surface water E0.00051 < 0.0008 < 0.002 < 0.0008 < 0.01 < 0.01 < 0.01 < 0.005 < 0.01

Map 

number

(fig. 2, 

table 1)

Sample

date/time Sample type

Antibiotics Total 

number of 

analytes 

detected

Sulfamethazine, filtered, 

μg/L

(61762)

Tetracycline, 

filtered, μg/L

(62781)

LG1 09/24/08 1240 Lagoon 1.15 0.572 20L2M 09/23/08 1720 Groundwater < 0.005 < 0.010 1L2D 09/24/08 0855 Groundwater < 0.005 < 0.010 4L15M 09/22/08 1415 Groundwater < 0.005 < 0.010 0L15D 09/22/08 1000 Source solution blank < 0.005 < 0.010 0L15D 09/22/08 1650 Groundwater < 0.005 < 0.010 1L70D 09/23/08 1325 Field equipment blank < 0.005 < 0.010 1L70D 09/23/08 1500 Groundwater < 0.005 < 0.010 0L70D 09/23/08 1505 Replicate < 0.005 < 0.010 0L71D 09/24/08 1035 Groundwater < 0.005 < 0.010 2L72 09/24/08 1310 Groundwater < 0.005 < 0.010 2S7 09/23/08 1150 Surface water < 0.005 < 0.010 4

Table 3. Concentrations of organic wastewater compounds detected in environmental and quality-control samples collected from a concentrated swine feeding operation study site, Greene County, North Carolina, 2008.—Continued[HIAs, household, industrial, and agricultrual-use compounds; μg/L, micrograms per liter; Numbers in parentheses are U.S. Geological Survey parameter codes; <, less than; E, estimated concentration; italics indicate quality-control samples]
12 Organic Wastewater Compounds at a Concentrated Swine Feeding Operation in the North Carolina Coastal Plain, 2008

The occurrence of cis-androsterone in the equipment blank 

at an estimated concentration (0.00025 microgram per liter 

(μg/L)) less than the RL of 0.0008 μg/L (table 3) was not 

considered to be a source of contamination to the environmental samples. The lagoon sample was the only environmental 

sample with a detection of cis-androsterone, and the reported 

concentration of 0.165 μg/L was approximately three orders of 

magnitude higher than the estimated result for the equipment 

blank. The replicate sample, obtained from monitoring well 

site L70D (fig. 2), was used to examine potential variability 

introduced during sample collection, processing, and laboratory handling. No analytes were detected above laboratory 

RLs for either the groundwater sample or the replicate sample 

collected at site L70D (table 3), which indicates that the samples were collected, processed, and analyzed under consistent 

conditions. Based on the results of the quality-control samples, 

no quality-assurance issues were apparent during the collection and processing of the environmental samples.

Lagoon Sample

The lagoon sample (site LG1) contained the highest 

number and concentrations of OWCs among the environmental samples (fig. 2; table 3). The 20 analytes identified 

in the lagoon sample represent a range of general uses and 

sources. The 5 detected HIA compounds include 2 fragrances 

(3-methyl-1H-indole and indole), 1 plasticizer (bisphenol-A), 

1 disinfectant (phenol), and 1 fire retardant (tris(2-chloroethyl) 

phosphate). Three sterols (3-beta-coprostanol, beta-stigmastanol, and cholesterol) derived from animals or plants were 

detected in the lagoon sample. Caffeine, a nonprescription 

stimulant, was the only detected pharmaceutical compound. 

Four hormones were identified in the lagoon sample that were 

indicative of either male characteristics (11-ketotestosterone 

and cis-androsterone) or female characteristics (estriol and 

estrone). Seven common veterinary antibiotics or their degradates were detected in the lagoon sample, including epi-chlorotetracycline, epi-tetracycline, iso-chlorotetracycline, lincomycin, oxytetracycline, sulfamethazine, and tetracycline (table 3).

Groundwater and Surface-Water Samples

Of the 20 analytes indentified in the lagoon sample, only 

3 of the same analytes also were identifed in the groundwater 

or surface-water samples. The antibiotic lincomycin was 

detected at a concentration of 0.018 μg/L in water from well 

L71D (fig. 2; table 3). The concentration of lincomycin in the 

lagoon sample was 393 μg/L, which represents the highest concentration of any OWC detected during this study. At 

surface-water site S7, the HIA compounds 3-methyl-1H-indole 

(estimated concentration of 0.014 μg/L) and indole (estimated 

concentration of 0.01 μg/L) were detected below the analytical RLs (table 3). The lagoon sample had a concentration 

of 38 μg/L for 3-methyl-1H-indole and an estimated concentration of 4.5 μg/L for indole. The compounds 3-methyl1H-indole and indole commonly are used as fragrances or 

fragrance fixatives; however, these compounds also occur 

naturally in feces. None of the sterols or hormones detected in 

the lagoon sample was detected in the groundwater or surfacewater samples (table 3).

Eight analytes that were detected at low levels in the 

groundwater and surface-water samples were not identified 

in the waste-lagoon sample (table 3), which possibly reflects 

the higher analytical RLs associated with the lagoon sample 

or sources other than swine waste. The following groundwater sites had estimated concentrations of HIA compounds at 

or below the RLs, including well L2M (0.1 μg/L for triphenyl phosphate), well L2D (0.1 μg/L for benzophenone and 

0.1 μg/L for tris(dichloroisopropyl) phosphate), well L71D 

(0.7 μg/L for 4-nonylphenol), and well L72 (0.03 μg/L for 

benzophenone). At surface-water site S7, the HIA compound 

camphor had an estimated concentration of 0.1 μg/L. The HIA 

compound DEET (N,N-diethyl-meta-toluamide) had the highest detected concentrations above the analytical RL in water 

samples from wells L2D (1.4 μg/L) and L72 (0.8 μg/L). DEET 

was reported as less than the RL of 10 μg/L in the lagoon 

sample (table 3).

Analysis of the pharamaceutical compounds indicated 

that ibuprofen, a nonprescription anti-inflammatory drug, 

was detected in water from well L2D at a concentration of 

0.477 μg/L. Ibuprofen was reported as less than the RL of 

0.05 μg/L in the lagoon sample and at all other sites. The 

occurrence of both ibuprofen and DEET in the sample from 

well L2D is interesting in that this well is located at the 

hydraulically upgradient edge of the spray fields near local 

residences. It is unclear whether the presence of these compounds in water from well L2D reflects local agricultural 

and(or) domestic sources.

The occurrence of hormones in groundwater and surfacewater samples was limited to 4-androstene-3,17-dione, which 

was detected at estimated concentrations of 0.00042 μg/L 

in groundwater from well L15D and 0.00051 μg/L at 

surface-water site S7. The hormone 4-androstene-3,17-

dione was reported as less than the RL of 0.490 μg/L for the 

lagoon sample.
References Cited 13

Summary

The analytical results for the OWCs, hormones, and 

antibiotics obtained in this study are based on one round of 

sampling that occurred following a period of below-normal 

precipitation and when swine waste was not being applied 

to the fields. Future studies designed to examine the occurrence of OWCs, hormones, and antibiotics in groundwater and 

surface water associated with animal-waste application fields 

could enhance the body of information by including sampling strategies that represent seasonal differences in rainfall, 

groundwater levels, streamflow, and waste applications.

Acknowledgments

Funding for this study was provided by the North Carolina Department of Environment and Natural Resources, Division of Water Quality, Aquifer Protection Section. In addition, 

the author acknowledges the U.S. Environmental Protection 

Agency’s National Risk Management Research Laboratory in 

Cincinnati, Ohio, for their support of research activities conducted at the study site. Much appreciation is extended to the 

private landowner who graciously allowed access and collection of samples at the study site. The author thanks Ryan Rasmussen of the U.S. Geological Survey North Carolina Water 

Science Center for his help in collecting and processing waterquality samples for the study. 

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Prepared by:

USGS Publishing Network

Raleigh Publishing Service Center

3916 Sunset Ridge Road

Raleigh, NC 27607

For additional information regarding this publication, contact:

Stephen L. Harden, Hydrologist

USGS North Carolina Water Science Center

3916 Sunset Ridge Road

Raleigh, NC 27607

email: slharden@usgs.gov

Or visit the USGS North Carolina Water Science Center Web site at:

http://nc.water.usgs.gov/

Harden—Reconnaissance of Organic Wastewater Compounds at a Concentrated Swine Feeding Operation in the North Carolina Coastal Plain—Open-File Report 2009–1128