Toxic Hydrology Program 

Results of the Chemical and Isotopic Analyses of 

Sediment and Ground Water from Alluvium of the 

Canadian River Near a Closed Municipal Landfill, 

Norman, Oklahoma, Part 2 

By George N. Breit, Michele L.W. Tuttle, Isabelle M. Cozzarelli, Cyrus J. Berry, Scott C. Christenson, and 

Jeanne B. Jaeschke 

Open-File Report 2008–1134 

U.S. Department of the Interior 

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

DIRK KEMPTHORNE, Secretary 

U.S. Geological Survey 

Mark D. Myers, Director 

U.S. Geological Survey, Denver, Colorado 2008 

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Suggested citation: 

Breit, G.N., Tuttle, M.L.W., Cozzarelli, I.M., Berry, C.J., Christenson, S.C. and Jaeschke, J.B., 2008, Results of the chemical

and isotopic analyses of sediment and ground water from alluvium of the Canadian River near a closed municipal landfill, 

Norman, Oklahoma, Part 2: U.S. Geological Survey Open-file Report 2008-1134, 35 p. 

Open-File Reports are used for the dissemination of information that must be released immediately to fill a public need or 

for information that is not sufficiently refined to warrant formal publication. As such, Open-File Reports should not be 

viewed as final reports of major scientific investigations. Because of their preliminary nature and possibility of being 

superseded open-file reports do not introduce new or revise geologic, stratigraphic, hydrologic or taxonomic 

nomenclature. In particular, Article 4(a) of the North American Stratigraphic Code excludes, Open-file releases for the 

naming or revising of formal geologic units. Use of brand names is intended for descriptive purposes only and does not 

represent an endorsement by the U.S. Geological Survey. Any use of trade, product, or firm names is for descriptive 

purposes only and does not imply endorsement by the U.S. Government. 

ii
Contents 

Conversion Factors ............................................................................................................................................................v 

Chemical and Isotopic Symbols.....................................................................................................................................vii 

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

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

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

Sample Site Selection....................................................................................................................................................2 

Sediment Sampling.........................................................................................................................................................4 

Water Sampling and Field Analyses ...........................................................................................................................4 

Sediment Analyses.........................................................................................................................................................5 

Water Laboratory Analyses..........................................................................................................................................6 

Results ..................................................................................................................................................................................7 

Sediment Composition ...................................................................................................................................................7 

Water Composition.......................................................................................................................................................12 

References Cited ..............................................................................................................................................................17

Figures 

1. Location map of the IC sample sites ........................................................................................................................3 

2. Cumulative abundance of size fractions measured by sieve analysis of sediment samples collected 

at IC 35, IC 54, and IC South....................................................................................................................................7 

3. Depth variation in total iron concentration extracted using 0.5 N HCl and Ti3+-EDTA on sediment 

samples collected at IC 36, IC 54, and IC South..................................................................................................8 

4. Depth variation in the ratio of ferrous to total iron extracted with 0.5 N HCl from sediment samples 

collected at IC 36, IC 54, and IC South..................................................................................................................9 

5. Abundance of iron extracted from sediment samples with Ti3+-EDTA relative to the abundance of 

particles smaller than 100 μm..............................................................................................................................10 

6. Depth variation in the abundance of acid-volatile sulfide and disulfide extracted from the sediment 

samples collected at IC 36, IC 54, and IC South................................................................................................11 

7. Box plot of the sulfur isotope composition of sulfur species extracted from the sediment samples 

collected at IC 36, IC 54 and IC South.................................................................................................................12 

8. Depth variation of chloride concentration of ground water from the wells at IC 36, IC 54, and IC South 

in October 2004 and April 2005.............................................................................................................................14 

9. Depth variation of iron concentration of ground water from the wells at IC 36, IC 54, and IC South in 

October 2004 and April 2005 .................................................................................................................................14 

iii
10. Depth variation of sulfate concentration of ground water from the wells at IC 36, IC 54, and IC South 

in October 2004 and April 2005.............................................................................................................................15 

11. Piper diagram of major ion composition of ground water samples from wells at IC 36, IC 54, and IC 

South.........................................................................................................................................................................16

Tables 

1. Location of sample sites...............................................................................................................................................3 

2. Summary statistics of water composition from IC 36, IC 54, and IC South .......................................................13

Appendices 

1. Depth intervals of the wells sampled at IC 36, IC 54, and IC South ....................................................................19 

2. Elevations and descriptions of cored sediment samples.....................................................................................20 

3. Results of grain-size analysis of sediment samples .............................................................................................22 

4. Concentration of iron sequentially extracted from sediment samples using 0.5 N HCl and Ti3+-EDTA ......24 

5. Concentrations of sulfur species in sediment samples and their sulfur isotopic composition ....................26 

6. Results of chemical and isotopic analyses of ground water samples from wells at IC 36, IC 54, and IC 

South.........................................................................................................................................................................28 

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) 

mile, nautical (nmi) 1.852 kilometer (km) 

yard (yd) 0.9144 meter (m) 

Volume 

ounce, fluid (fl. oz) 0.02957 liter (L) 

pint (pt) 0.4732 liter (L) 

quart (qt) 0.9464 liter (L) 

gallon (gal) 3.785 liter (L) 

cubic inch (in3

) 0.01639 liter (L) 

Mass 

ounce, avoirdupois (oz) 28.35 gram (g) 

pound, avoirdupois (lb) 0.4536 kilogram (kg) 

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

°F=(1.8×°C)+32 

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

°C=(°F-32)/1.8 

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

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

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

v
SI to Inch/Pound 

Multiply By To obtain 

Length 

centimeter (cm) 0.3937 inch (in.) 

millimeter (mm) 0.03937 inch (in.) 

meter (m) 3.281 foot (ft) 

meter (m) 1.094 yard (yd) 

Volume 

liter (L) 33.82 ounce, fluid (fl. oz) 

liter (L) 2.113 pint (pt) 

liter (L) 1.057 quart (qt) 

liter (L) 0.2642 gallon (gal) 

cubic meter (m3

) 264.2 gallon (gal) 

cubic decimeter (dm3

) 0.2642 gallon (gal) 

liter (L) 61.02 cubic inch (in3

) 

Mass 

gram (g) 0.03527 ounce, avoirdupois (oz) 

kilogram (kg) 2.205 pound avoirdupois (lb) 

Abbreviated Units Chemical concentration and water temperature are given only in metric units. Chemical concentration 

in water is given as milligrams per liter (mg/L). Chemical concentrations in solid phase samples are given as micromoles per 

gram (μmoles g-1). Grain size abundances are listed in weight percent (wt.%). Specific conductance is given in microsiemens per 

centimeter at 25 degrees Celsius (μS/cm at 25 °C). Stable-isotope ratios are reported relative to internationally agreed-upon 

standards. Deviations from standards are expressed in per mil using the delta (δ) notation. The delta symbol in this report is 

followed by the chemical symbol for the heavier isotope measured during isotopic analysis. 

vi
vii

Chemical and Isotopic Symbols 

 

 Ag2S silver sulfide 

 AVS acid-volatile sulfide 

 BaCl2 barium chloride 

 BaSO4 barium sulfate 

 Ca calcium 

 Cl- chloride 

 DI disulfide sulfur 

 EDTA ethylenediaminetetraacetic acid 

 Fe iron 

 Fe2+ ferrous iron 

 FeS2 iron disulfide 

 Fetotal sum of ferrous and ferric iron 

 HCl hydrochloric acid 

 HCO3

-

 bicarbonate ion 

 H2S hydrogen sulfide 

 K potassium 

 Mg magnesium 

 N normal (concentration) 

 Na sodium 

 NH4

+

 ammonium 

 S sulfur 

 SO4

2- sulfate 

 Ti titanium 

 δ2HH2O hydrogen isotope composition of water 

δ

18OH2O oxygen isotope composition of water 

 δ18OSO4 oxygen isotope composition of sulfate 

δ

34SAVS sulfur isotope composition of acid-volatile sulfide 

δ

34SDI sulfur isotope composition of disulfide (reducible) sulfur 

δ

34Ssulfate-HCl sulfur isotope composition of sulfate extracted with 6N HCl 
Results of the Chemical and Isotopic Analyses of 

Sediment and Ground Water from Alluvium of the 

Canadian River Near a Closed Municipal Landfill, 

Norman, Oklahoma, Part 2 

By George N. Breit, Michele L.W. Tuttle, Isabelle M. Cozzarelli, Cyrus J. Berry, Scott C. Christenson, 

and Jeanne B. Jaeschke 

Abstract 

Analytical results on sediment and associated ground water from the Canadian River alluvium 

collected subsequent to those described in Breit and others (2005) are presented in this report. The 

data presented herein were collected primarily to evaluate the iron and sulfur species within the 

sediment at well sites IC 36, IC 54, and IC South located at the USGS Norman Landfill study site. 

Cored sediment and water samples were collected during October 2004 and April 2005. The 52 

sediment samples collected by coring were analyzed to determine grain size, the abundance of 

extractable iron species, and the abundance of sulfur forms and their isotopic compositions. 

Ground water was collected from cluster wells that sampled ground water from 11 to 15 screened 

intervals at each of the three sites. The depth range of the wells overlapped the interval of cored 

sediment. Concentrations of major ions, dissolved organic carbon (DOC), ammonium, and iron are 

reported with pH, specific conductance, and the isotopic composition of the water for the 75 water 

samples analyzed. Dissolved sulfate in selected water samples was analyzed to determine its sulfur 

and oxygen isotope composition. 

Introduction 

Landfills were sited adjacent to rivers prior to the passage of regulations intended to restrict the 

impact of solid wastes and leachates produced by interaction of ground and surface water with 

those wastes (Steiner and others, 1994). The U.S. Geological Survey (USGS) Toxic Hydrology 

Program is supporting the study of a closed municipal landfill located on Canadian River alluvium 

south of the city of Norman, Oklahoma, to evaluate the environmental impact of one of these waste 

repositories. The closed Norman municipal landfill operated in varying forms beginning in the 

1920s until 1985 (fig. 1) (Schlottmann, 2001). Initially the wastes were dispersed along the north 

bank of the river. Beginning in 1960, the operators excavated trenches to the water table and 

buried wastes beneath 15 cm of sand. Trenches were abandoned in 1971, and wastes were 

deposited on lifts of sand 0.6 meters above the water table. Wastes were buried daily with sand. 

The landfill was closed in 1985 and covered with a low-permeability cap, leaving two mounds 

rising about 12 meters above the surrounding land surface (Schlottmann, 2001). 

1
Movement of ground water through the waste produces a leachate distinguished by high 

concentrations of several dissolved constituents including organic carbon, iron, methane, 

ammonium, and boron (Cozzarelli and others, 2000; Schlottmann, 2001). Chemical and biological 

processes that degrade organic contaminants as the leachate moves through the Canadian River 

alluvium are the primary emphasis of the project. Collectively these attenuation processes may be 

important as a means of natural remediation. Bacterial oxidation of the contaminant organic 

compounds is supported by the presence of electron acceptors such as dissolved oxygen, nitrate, 

and sulfate, as well as solid manganese and ferric oxyhydroxides and oxides. This report presents 

data on the abundance of solid forms of iron and sulfur species in sediment within 2.8 meters of the 

ground surface as an addition to the previously published results of Breit and others (2005). In 

addition, ground water proximal to the sediment samples was chemically and isotopically analyzed. 

The depth range evaluated in this study is subject to seasonal fluctuations in water level (Becker, 

2002; Scholl and others, 2005), with the shallowest ground water originating largely from 

infiltration of precipitation into the sediment (Scholl and others, 2005; 2006). The annual changes 

in water level are anticipated to affect the redox environment of the sediment and therefore the 

abundance of electron acceptors. A greater abundance of reduced forms of iron and sulfur are 

predicted following high water levels that are characteristic of spring, and the converse behavior is 

anticipated in the fall because of low water levels in late summer (Scholl and others, 2006). Such 

an annual fluctuation may impact the availability of electron acceptors necessary for natural 

attenuation processes. To test this hypothesis, samples of sediment and ground water were 

collected in October 2004 and April 2005 to represent seasons of generally low and generally high 

water levels, respectively. Results of sediment and water analyses are presented in this report. 

Methods 

Sample Site Selection 

Previous studies by Scholl and others (2005, 2006) explored the annual variations in water 

composition at sites of three cluster wells, IC 36, IC 54, and IC South. Because of the known 

variation in water composition at these sites, they were the focus of this investigation. The IC sites 

are south of the landfill mounds (fig. 1; table 1), which is down the hydrologic gradient (Scholl and 

Christenson, 1998). The locations of the sites are: IC 36, 35 m from the toe of the landfill mound; 

IC 54, 7 m south of the slough, which is a former channel of the Canadian River; IC South, 85 m 

south of the slough and located in an area disturbed by major floods and channel avulsion during 

the 1980s (Schlottmann, 2001). 

Variations in the chemical and isotopic composition of water recovered from the IC sites reflect the 

distinct histories of water collected at the various sampled depths and locations (Scholl and others, 

2005; 2006). All sites produced water in the shallowest intervals, which is attributed to dilute 

recharge by precipitation. Deeper water at IC 36 is considered to contain a component of leachate 

from the landfill. Water in the lower wells at IC 54 is consistent with recharge from the slough and 

possibly leachate. At IC South the deepest wells sampled may produce water originally recharged 

from the slough or from the Canadian River (Scholl and others, 2005; 2006). 

2
Table 1. Location of the IC sample sites and water levels at the time of sampling. Horizontal 

coordinates relative to NAD83 datum. Elevation relative to NADV88 datum. 

Sample 

Site 

Latitude Longitude Land Surface 

Elevation 

(meters) 

Water Elevation 

October 2004 

(meters) 

Water Elevation 

April 2005 

(meters) 

IC 36 35.167496° N 97.446614° W 330.96 330.11 330.28 

IC 54 35.166582° N 97.447231° W 330.56 329.85 329.90 

IC South 35.165146° N 97.446614° W 330.31 329.62 329.59 

Figure 1. Location map of the IC sample sites (). Topographic and 

hydrologic gradients slope to the south. Outline of landfill indicates the 

extent of the two capped landfill mounds. 

3
Sediment Sampling 

Cores of the alluvium were recovered within a few meters laterally of the three IC cluster well sites 

using a Geoprobe direct-push coring device. At each of the three sites sediment was collected from 

the ground surface to a depth ranging from 2.1 to 2.8 m. Recovery of the sandy sediment was 

incomplete in the October 2004 sampling because of problems retaining the flowing sediment in 

the core barrel. The missing depth range was the focus of recovery during the April 2005 core 

collection. During coring, sediment was captured in transparent acrylic liners that were 4.1 cm in 

diameter. The recovered core was cut into 0.1 to 0.4 m lengths, frozen on site with dry ice and 

shipped with dry ice to USGS laboratories in Denver. Upon arrival in Denver, the cores were 

transferred to a freezer and stored at -10 oC to inhibit redox or microbial changes to the sediment 

until they were prepared for analysis. 

Within one month of sample collection, the frozen core was cut into lengths that approximated the 

depth range of each well in the cluster. While frozen, the core was extruded and split lengthwise 

into four approximately equivalent fractions using a hammer and chisel. One quarter of the sample 

was weighed and transferred to the glass reaction vessel for sulfur speciation as described below. 

The second quarter was transferred to a dish and allowed to air dry for the determination of 

moisture content. The third quarter of each sample collected during the October 2004 collection 

was weighed and transferred to a polyethylene bottle for extraction of water-soluble sulfate. This 

extraction was omitted during analysis of the April 2005 samples. The remaining sample was 

allowed to thaw slightly and, while still cold, was homogenized by manual mixing. Two aliquots 

of the homogenized sediment were transferred to glass vials equipped with butyl rubber septa. One 

vial was used for the iron speciation analyses, and the other was archived after freeze-drying. 

Water Sampling and Field Analyses 

Water was collected from existing wells (appendix 1) following the procedures outlined by Scholl 

and others (2005). Water was drawn slowly from each well in the cluster using a peristaltic pump. 

Specific conductance and pH were measured on site using calibrated meters. Ammonium content 

was measured spectrophotometrically on unfiltered samples that were diluted to fit the reporting 

range of the Nessler CHEMETS kit. Water samples for determination of alkalinity were filtered to 

<0.4 micrometer (μm) in the field, and transported with ice to the laboratory. An aliquot of water 

was filtered (<0.1 μm) and acidified with high-purity concentrated nitric acid to a pH less than 2 for 

analysis of cations and trace elements in the laboratory. Another aliquot was filtered in the field to 

<0.2 μm and was chilled with ice and transported to the laboratory for measurement of anions. 

Water passed through a 0.45 μm silver filter to remove bacteria and was stored in a baked glass 

bottle and acidified with phosphoric acid to a pH <2 for determination of the dissolved organic 

carbon content. Unfiltered water was also collected in a glass bottle sealed tightly with polyseal 

caps to prevent evaporation and refrigerated for later determination of the hydrogen (δ

2

H) and 

oxygen (δ

18O) isotope composition of the water. 

Sediment Analyses 

Sediment samples were analyzed to determine the grain size distribution, the abundance of 

extractable iron species, and the abundance and isotopic composition of extractable sulfur species. 

4
Stainless steel sieves were used to divide the air-dried sediment into five fractions: >500 μm, 500-

250 μm, 250-100 μm, 100-62 μm, and <62 μm. The sediment and sieves were shaken manually for 

5 minutes and the resulting sized fractions were weighed to the nearest 0.01 gram. Although large 

intraclasts of mud and silt were visually recognized, they were gently disaggregated using a mortar 

and pestle for the size analysis. Disaggregation is compatible with the emphasis of this study on 

the reactivity of the sediment, which is reasonably evaluated by the dispersed particles. 

Chemical extractions for iron speciation were modified slightly from those of Heron and others 

(1994). Approximately 5 to 10 grams of sediment was combined with 40 mL of 0.5 normal (N) 

hydrochloric acid (HCl) in an amber glass serum vial that was purged with nitrogen gas (N2(g)). 

The sediment was reacted for 24 hours with intermittent agitation to suspend the sediment. Upon 

completion of the reaction, an aliquot of the 0.5N HCl was removed using a needle and syringe. 

The withdrawn solution was immediately filtered through a 0.2-μm syringe filter and reacted with 

orthophenanthroline according to the procedure of Clesceri and others (1998) to determine ferrous 

and total dissolved iron concentrations. The remaining sediment was subsequently recovered by 

filtration, rinsed thoroughly with distilled water, and air-dried overnight. 

 

The air-dried sediment residue of the 0.5N HCl was weighed and then split using a mechanical 

splitter into a fraction weighing between 1.5 to 3.0 grams. The weighed fraction was combined 

with 40 mL of 0.008 molar titanous chloride (Ti3+Cl3

) in 0.05 molar disodium 

ethylenediaminetetraacetic acid (EDTA) with pH of the combined solution adjusted to between 6 

and 6.5 using sodium hydroxide. The Ti3+-EDTA solution was prepared and introduced into an 

amber glass serum vial under N2(g). The serum vial was sealed, purged with N2(g) for 3 minutes, 

wrapped with foil, and shaken intermittently over the 24 hour reaction period. Following reaction, 

30 mL of solution was removed through the septum using a needle and syringe and then filtered 

through a 0.2-μm syringe filter. The Ti3+-EDTA solution has a medium-intensity magenta color 

prior to reaction with ferric iron. This color was apparent, although less intense, at the completion 

of the reaction indicating that the Ti3+ was not completely consumed during reaction with the 

sediment. The filtered solution was then analyzed for total iron using the orthophenanthroline 

procedure (Clesceri and others, 1998). Although the sediment was dried in air prior to evaluation 

of reducible iron, the readily reactive iron phases were removed by the 0.5 N HCl prior to air 

exposure, and any remaining reduced iron phases such as pyrite are slowly reactive and contribute 

little to the Ti3+-EDTA extraction (Heron and others, 1994). 

Water-soluble sulfate was determined by combining 40 to 80 grams of cold sediment with 200 

milliliters of deionized water. The sample and water were agitated for 1 hour. The resulting 

solution was separated from the sediment by filtration, acidified to a pH between 3 and 4 with HCl, 

heated to approximately 90 °C, and combined with 5 mL of barium chloride (BaCl2

). After several 

hours, the heating was discontinued, and the solution was allowed to cool overnight. The resulting 

barium sulfate (BaSO4

) precipitate was recovered by filtration, air-dried, and weighed. 

The abundances of acid-volatile sulfide (AVS), acid-soluble sulfate, and total reducible-disulfide 

(DI) were determined following the extraction scheme of Tuttle and others (1986). Approximately 

40 to 80 grams of frozen sediment was transferred under a nitrogen atmosphere into a glass reaction 

vessel. Under flowing N2(g) the sample was combined with 50 mL of 6 N HCl and 1 gram of 

stannous chloride and heated to evolve hydrogen sulfide (H2S) from AVS phases. The stannous 

chloride was added to reduce ferric iron present in hematite grain coatings that might oxidize 

5
evolved H2

S (Rice and others, 1993). The H2S was then carried in flowing nitrogen through a 

reservoir of pH 4 buffer to remove HCl vapor and subsequently bubbled through a trap containing 

silver nitrate, which resulted in the formation of silver sulfide (Ag2S). The Ag2S was collected by 

filtration, dried, and weighed to determine the mass of recovered sulfide. 

Following completion of release of H2S, the acid solution was separated from the remaining 

sediment by filtration. The acid solution was reacted with 10 mL of 10 weight percent BaCl2 to 

precipitate dissolved sulfate as BaSO4, following the procedure outlined for water-extracted sulfate. 

The precipitated sulfate is considered acid-soluble sulfate. 

The residual solid remaining after the 6 N HCl extraction was air-dried, weighed and placed in a 

reaction vessel under flowing nitrogen, where it was combined with 1M chromous chloride (CrCl2) 

in 4 N HCl with 10 mL of ethanol. Chromium(II) reduces sulfur in FeS2 phases, known to be 

present in the sediment (Breit and others, 2005), to produce H2S. As in the AVS analysis, evolved 

H2

S was carried through a pH 4 buffer to strip HCl vapors and then bubbled through a silver nitrate 

solution that precipitated the H2S as Ag2S. The resulting Ag2S was collected by filtration, air-dried, 

and weighed to determine the amount of contained disulfide sulfur. Replicate analyses produced 

concentrations of sulfide phases within ±10 weight percent. 

The sulfur isotope composition of Ag2S produced by the AVS and DI extractions, as well as the 

precipitated BaSO4,were measured by direct combustion (Kester and others, 2001) at the USGS 

Isotope Laboratory in Denver. Sulfur isotope data are reported relative to Vienna Canon Diablo 

Troilite (VCDT) in standard per mil values. Precision of the measurement of δ

34S values is within 

± 0.3 per mil. 

Water Laboratory Analyses 

Major ion, trace element, dissolved organic carbon, alkalinity, and isotope composition were 

determined on selected water samples in USGS laboratories in Reston, Virginia (Baedecker and 

Cozzarelli, 1992). Measurement of alkalinity was completed by tritration using a Titra Lab Tim 

900 autotitrator with 0.0254 N HCl. Alkalinity is reported as bicarbonate ion (Baedecker and 

Cozzarelli, 1992). Direct-current plasma spectrometry determined the cation and trace element 

abundances in of the water samples. Anions were measured using a Dionex 120 ion chromatograph 

equipped with an Ion Pac AS14 column. Dissolved organic carbon (DOC) was measured by the 

method of Qian and Mopper (1996). Addition of dissolved barium chloride to selected water 

samples precipitated dissolved sulfate for isotope analyses, using the same procedure for 

precipitation of sulfate that was extracted by water from the sediment samples. The pH of the 

water samples was adjusted to be between 3 and 4 with addition of HCl to remove dissolved 

carbonate species while minimizing exchange of oxygen bound to sulfate. The isotopic 

composition of recovered sulfate and water were determined at the USGS Reston Stable Isotope 

Laboratory. Sulfur isotopes and oxygen isotope composition of sulfate were determined by 

continuous flow with precisions of ± 0.2 and ±0.3 per mil respectively. Sulfate sulfur is reported 

relative to Vienna Canon Diablo Troilite (VCDT) and oxygen is reported relative to Vienna 

Standard Mean Ocean Water (VSMOW) as per mil values. The δ

2

Η composition of water was 

determined by equilibration with gaseous hydrogen; resulting precision of this analysis was ± 1 per 

mil. δ

18O of the water was determined through equilibration with CO2; resulting precision was ± 

0.1 per mil. Both hydrogen and oxygen isotope compositions are reported as per mil relative to 

6
VSMOW and normalized such that the δ

2

H and δ

18O values of Standard Light Antarctic 

Precipitation (SLAP) are -5.55 per mil and -4.28 per mil respectively. 

Results 

Sediment Composition 

The alluvium deposited by the Canadian River contains sand, silt, clay, and aggregates of finegrained sediment in intraclasts (Breit and others, 2005). Most of the samples considered in this 

study are red-brown as the result of grain-coating hematite that was eroded from Permian red beds 

within the drainage basin. Exceptions to this pervasive coloration are the samples from deeper than 

approximately 330 m elevation at the IC 36 well site, which are distinguished by their gray-brown 

color. Bedforms observed in the IC cores vary from finely laminated to massive (appendix 2). 

Sedimentary structures are readily recognized in sediment collected above the water table; watersaturated sediment was likely liquefied during the coring process, resulting in disruption of primary 

sedimentary structures to produce the massive appearance. 

-

Figure 2. Cumulative abundance of size fractions measured by sieve analysis of sediment 

samples recovered at IC 36, IC 54, and IC South. 

Results of the sieve analysis of the sediment samples are presented in figure 2 and listed in 

appendix 3. Sediment recovered from all cores is mainly medium to very fine sand. The deepest 

sediment from IC South is composed of relatively coarse-grained sediment consistent with the 

presence of pebble-sized intraclasts recovered in this interval. Sediment recovered from the upper 

7
0.5 m of IC 54 is notable for the greater abundance of particles less than 62 μm compared to other 

cored intervals. 

The amounts of iron extracted with the 0.5 N HCl and Ti3+-EDTA extractions are presented in 

figure 3 and listed in appendix 4. The amount of total iron extracted by 0.5 N HCl ranged from 1.2 

to 18.8 micromoles per gram (μmoles g-1). For all samples, Ti3+-EDTA released greater amounts of 

iron (7.9 to 48 μmoles g-1) than the 0.5 N HCl extraction. At all sites the greatest amounts of Ti3+

-

EDTA-extracted iron were from samples collected above the position of the water table at the time 

of sample collection. The abundance of ferrous iron relative to total iron extracted with 0.5 N HCl 

generally varied directly with position of the sample relative to the water table (fig. 4). Sediment 

samples collected above the water table, with the exception of one sample from IC 54, have 

Fe2+/Fetotal ratios <0.25. Below the water table there is a general increase in the ratio, with values 

approaching 1.0 near the bottom of the cored intervals. Results of the iron extractions on samples 

collected in October 2004 and April 2005 are broadly consistent with similar chemical conditions 

in the sediment during both sampling events. 

Figure 3. Depth variation in the total iron extracted using 0.5N HCl (c) and Ti3+-EDTA () on 

sediment samples collected at IC 36, IC 54, and IC South. Elevation of water table during the 

April 2005 sample collection is shown. (black, collected in October 2004; gray, collected in 

April 2005). 

8
Figure 4. Depth variation in the ratio of ferrous (Fe2+) to total iron (Fetotal) extracted with 0.5 N 

HCl from sediment samples collected at IC 36, IC 54, and IC South. Elevation of water table 

during the April 2005 sample collection is shown as a dashed line. (black, collected in 

October 2004; gray, collected in April 2005).

The amount of iron extracted was also evaluated relative to the grain size of the samples. No 

systematic distribution of 0.5 N HCl-extractable iron with grain size distribution of the sediment 

was recognized. In contrast, the amount of Ti3+-EDTA-extractable iron did increase as the fraction 

of sediment smaller than 100 μm increased (figure 5). For samples with similar contents of 

particles smaller than 100 μm, those collected above the water table generally contain markedly 

greater amounts of Ti3+-EDTA-extractable iron than samples from the saturated zone. 

The abundances of water-soluble sulfate, acid-soluble sulfate, acid-volatile sulfide, and disulfide 

sulfur recovered from the sediment are listed in appendix 5 along with the δ

34S values of these 

phases. Results of the water-soluble sulfate extraction on sediment collected in October 2004 

yielded only small amounts of sulfate (less than 0.5 μmoles g-1 sulfate sulfur); therefore, the 

extraction was not applied to the April 2005 sample set. The amounts of acid-soluble sulfate 

recovered vary from less than 0.1 to 2.4 μmoles g-1. Acid-volatile sulfide concentrations range 

from less than 0.1 to 3.8 μmoles g-1, and disulfide sulfur varies from less than 0.1 to 15 μmoles g-1

. 

Most samples contain greater amounts of acid-volatile sulfide than disulfide sulfur. 

Depth variations in the abundance of acid-volatile sulfide and disulfide sulfur are plotted on figure 

6. The vertical variations in the concentrations of acid-volatile sulfide and disulfide sulfur are 

similar at each site, but the profiles are distinct among the IC sites. Sediment above the water table 

at IC 36 lacks detectable sulfide, whereas large amounts were recovered from the same depth range 

9
at IC 54 and minor amounts at IC South. Sediment a few tens of centimeters below the water table 

at all sites has lower sulfide concentrations than deeper sediment. Sulfide concentrations at IC 36 

and IC 54 increase sharply in samples below the water table, while the profile for IC South portrays 

a more gradual increase with depth. 

The range of sulfur isotope compositions of acid-soluble sulfate (4 to 20 per mil) is distinct from 

the values measured for acid-volatile sulfide (-0.5 to -21.5 per mil) and disulfide sulfur (-4 to -25.1 

per mil) (fig. 7). The δ

34S values of acid-soluble sulfate collected at IC South are consistently 

smaller than those measured at IC 36 and IC 54 (fig. 7). Sulfur isotope values of acid-volatile 

sulfide among the three cores are generally similar, while the δ

34S of disulfide sulfur measured in 

IC 54 core is greater than at the other sites. The typically negative values for δ

34S of the sulfide 

phases relative to the values of sulfate are consistent with formation of sulfide by bacterial sulfate 

reduction (Breit and others, 2007). 

Figure 5. Abundance of iron extracted from sediment samples with Ti3+-EDTA relative to 

the abundance of particles smaller than 100 μm. (‘above’, samples collected above the 

saturated zone; ‘below’, samples collected within the saturated zone). 

10
Figure 6. Depth variation in the abundance of acid-volatile sulfide (c) and disulfide () extracted 

from sediment collected at IC 36, IC 54, and IC South. Elevation of water table during the April 2005 

sample collection is shown by the dashed line. (Black indicates samples collected in October 

2004; gray indicates samples collected in April 2005). 

11
Figure 7. Box plot of the sulfur isotope composition of sulfur species extracted from 

the sediment samples collected at IC 36, IC 54 and IC South. 

Water Composition 

The composition of water samples is presented in appendix 6 and summarized in table 2. In 

general, the concentration of dissolved constituents at the IC site follows the vertical trends 

described by Scholl and others (2005, 2006). Low concentrations of most measured constituents 

were detected at shallow depths at all three sites. This tendency is indicated in the profiles of 

chloride concentration at IC 36 and IC South (fig. 8). 

 

Dissolved iron concentrations generally increase with depth, but the trends vary at each IC site (fig. 

9). Sample preservation problems limited the iron analyses of water samples from IC 36 that were 

collected in October, but the April samples suggest two maxima in iron content. 

Samples from IC 54 have low dissolved iron contents without a clear maximum for samples 

gathered in October, whereas the April samples define a maximum 1.0 m below the ground surface 

and an increase in iron concentration in the two deepest wells. The profile for IC South is similar 

for both the October and April sampling, with maxima at approximately 1.5 m depth. 

The concentration of dissolved sulfate increases with depth to a maximum value and then declines 

to concentrations near the limit of detection at all sites (fig. 10). The depth of the maxima is similar 

in both the October and April sampling, although the concentrations that define the maxima are 

greater in October. 

12
Table 2. Statistical summary of parameters measured on ground water samples collected from IC wells in Octobe

[Sp. Cond. – specific conductance; μS/cm, microSiemens per centimeter; DOC, dissolved organic carbon; mg/L, milligrams per liter ]

IC 36 IC 54 IC South IC 36 IC 54 

pH Iron (mg/L)

Median 7.07 7.24 7.10 Median 7.8 1.9 

Minimum 6.78 6.75 6.07 Minimum 0.1 0.3 

Maximum 7.49 7.70 7.80 Maximum 14 7.8 

Sp. Cond. (μS/cm) Ammonium (mg/L) 

Median 3600 1400 920 Median 65 2.8 

Minimum 600 1100 620 Minimum <0.7 <0.7 

Maximum 4800 2400 1500 Maximum 430 8.6 

Calcium (mg/L) DOC (mg/L) 

Median 99 96 160 Median 57 20 

Minimum 67 50 100 Minimum 6.0 2.1 

Maximum 240 170 200 Maximum 92 32 

Magnesium (mg/L) Bicarbonate (mg/L) 

Median 55 35 19 Median 1850 864 

Minimum 7.5 22 8.0 Minimum 337 765 

Maximum 95 59 45 Maximum 2330 1150 

Potassium (mg/L) Chloride (mg/L) 

Median 150 6.4 4.2 Median 255 81 

Minimum 0.6 4.5 1.3 Minimum 8.9 41 

Maximum 230 9.1 5.2 Maximum 396 256 

Sodium (mg/L) Sulfate (mg/L) 

Median 350 190 14 Median 18 21 

Minimum 0.6 77 5.4 Minimum 0.2 0.2 

Maximum 530 310 110 Maximum 78 120 

13
The major ion characteristics of water samples are depicted on a Piper plot (fig. 11) in 

which the bicarbonate concentration is multiplied by 0.1 to enhance contrast in anion 

composition among the water samples. Water samples from IC 36 and IC 54 tend to have 

consistently greater proportions of chloride than most samples from IC South. Similarly, 

IC 36 and IC 54 have a greater relative content of sodium than ground water sampled from 

IC South. 

Figure 8. Depth variation of chloride concentration of ground water sampled from 

the wells at IC 36, IC 54, and IC South in October 2004 ({) and April 2005 (T). 

14
Figure 9. Depth variation in iron concentration of ground water from the wells at IC 

36, IC 54, and IC South in October 2004 ({) and April 2005 (T). 

Figure 10. Depth variation of sulfate concentration of ground water sampled from the wells 

at IC 36, IC 54, and IC South in October 2004 ({) and April 2005 (T). Elevation of water table 

during the April 2005 sample collection is shown by the dashed line.

15
Figure 11. Piper diagram of major ion composition water samples collected from the wells at 

IC 36 (Å), IC 54 (μ), and IC South ({). Note that the bicarbonate concentration is multiplied 

by 0.1. 

16
References Cited 

Baedecker, M.J., and Cozzarelli, I.M., 1992, The determination and fate of unstable 

constituents of contaminated groundwater, in Lesage, Suzanne and Jackson, R.E., 

Groundwater contamination and analysis at hazardous waste sites: Environmental 

Science and Pollution Control Series, 4, New York, Marcel Dekker, p. 425-461. 

Becker, C.J., 2002, Hydrology and leachate plume delineation at a closed municpal 

landfill, Norman, Oklahoma: U.S. Geological Survey, Water-Resources Investigations 

Report 01-4168, 36 p. 

Breit, G.N., Tuttle, M.L.W., and Cozzarelli, I.M., 2007. Using δ

34S and δ18O of sulfate to 

resolve processes affecting sulfur in alluvium beneath a riparian area, Oklahoma: 

Geological Society of America Abstracts with Program, v. 39, no. 6, p. 481. 

Breit, G.N., Tuttle, M.L.W., Cozzarelli, I.M., Christenson, S.C., Jaeschke, J.B., Fey, D.L., 

and Berry, C.J., 2005, Results of the chemical and isotopic analyses of sediment and 

water from alluvium of the Canadian River near a closed municipal landfill, Norman, 

Oklahoma: U.S. Geological Survey Open-File Report 2005-1091, 37 p. 

Clesceri, L.S., Freenber, A.E., and Eaton, A.D., eds., 1998, 3500-Iron B. Phenanthroline 

method in Standard Methods for the Examination of Water and Wastewater 20th ed.: 

Washington, D.C., American Public Health Association, p. 3-76 to 3-78. 

Cozzarelli, I.M., Suflita, J.M., Ulrich, G.A., Harris, S.H., Scholl, M.A., Schlottmann, J.L., 

and Christenson, Scott, 2000, Geochemical and microbiological methods for evaluating 

anaerobic processes in an aquifer contaminated by landfill leachate: Environmental 

Science and Technology, v. 34, p. 4025-4033. 

Heron, Gorm, Crouzet, Catherine, Bourg, A.C.M., and Christensen, T.H., 1994, Speciation 

of Fe(II) and Fe(III) in contaminated aquifer sediments using chemical extraction 

techniques: Environmental Science and Technology, v. 28, p. 1698-1705. 

Kester, C.L., Rye, R.O., Johnson, C.A., Schwartz, Ch., and Homes, Ch., 2001, On-line 

sulfur isotope analysis of organic material by direct combustion: preliminary results and 

potential applications: Isotopes in Environmental Health Studies, v. 37, p. 53-65. 

Qian, Jianguo, and Mopper, Kenneth, 1996, Automated high performance, high 

temperature combustion total organic carbon analyzer: Analytical Chemistry, v. 68, p. 

3090-3097. 

Rice, C.A., Tuttle, M.L., and Reynolds, R.L., 1993, The analysis of forms of sulfur in 

ancient sediments and sedimentary rocks: comments and cautions: Chemical Geology, 

v. 107, p. 83-95. 

17
Schlottmann, J.L, 2001, Water chemistry near the closed Norman Landfill, Cleveland 

County, Oklahoma: U.S. Geological Survey Water-Resources Investigations Report 00-

4238, 44 p. 

Scholl, M.A., and Christenson, S.C., 1998, Spatial variation in hydraulic conductivity 

determined by slug tests in the Canadian River alluvium near the Norman Landfill, 

Norman, Oklahoma: U.S. Geological Survey Water-Resources Investigations Report 

97-4292, 28 p. 

Scholl, M.A., Christenson, S.C., Cozzarelli, I.M., Ferree, D.M., and Jaeschke, J., 2005, 

Recharge processes in an alluvial aquifer riparian zone, Norman Landfill, Norman, 

Oklahoma, 1998-2000: U.S. Geological Survey Scientific Investigations Report 2004-

5238, 27 p. 

Scholl, M.A., Cozzarelli, I.M., and Christenson, S.C., 2006, Recharge processes drive 

sulfate reduction in an alluvial aquifer contaminated with landfill leachate: Journal of 

Contaminant Hydrology, v. 86, p. 239-261. 

Steiner, Frederick, Pieart, Scott, Cook, Edward, Rich, Jacqueline, and Coltman, Virginia, 

1994, State wetlands and riparian area protection programs: Environmental 

Management, v. 18, p. 183-201. 

Tuttle, M.L., Goldhaber, M.B., and Williamson, D.L., 1986, An analytical scheme for 

determining forms of sulfur in oil shales and associated rocks: Talanta, v. 33, p. 953-

961. 

18
19

Appendix 1. Depth intervals of the wells sampled at IC 36, IC 54 and IC South. Elevations 

are in meters and are relative to the North American Vertical Datum of 1988.

Well Site Well 

Number 

Top 

Elevation 

Bottom Elevation 

IC 36 3 330.33 330.19 

IC 36 4 330.20 330.06 

IC 36 5 330.06 329.93 

IC 36 6 330.94 329.80 

IC 36 7 329.80 329.66 

IC 36 8 329.67 329.54 

IC 36 9 329.52 329.38 

IC 36 10 329.39 329.25 

IC 36 11 329.27 329.13 

IC 36 12 329.13 328.99 

IC 36 13 328.99 328.85 

IC 36 14 328.85 328.72 

IC 36 15 328.72 328.59 

IC 36 16 328.59 328.45 

IC 36 17 328.45 328.32 

IC 54 3 329.99 329.84 

IC 54 4 329.84 329.69 

IC 54 5 329.69 329.54 

IC 54 6 329.54 329.38 

IC 54 7 329.38 329.23 

IC 54 8 329.23 329.07 

IC 54 9 329.10 328.95 

IC 54 10 328.95 328.80 

IC 54 11 328.80 328.64 

IC 54 12 328.64 328.49 

IC 54 13 328.49 328.34 

IC 54 14 328.34 328.19 

IC South 3 329.73 329.58 

IC South 4 329.58 329.43 

IC South 5 329.43 329.28 

IC South 6 329.27 329.12 

IC South 7 329.11 328.96 

IC South 8 328.97 328.82 

IC South 9 328.84 328.69 

IC South 10 328.67 328.52 

IC South 11 328.52 328.37 

IC South 12 328.37 328.22 

IC South 13 328.22 328.07 

IC South 14 328.07 327.92 
Appendix 2. Elevation and description of cored sediment samples. Elevations are reported relative to North Ame

of 1988. 

Sample Number Sampled Interval Sediment Description 

Upper Elevation (m) Lower Elevation (m) 

IC 36-04-A 330.80 330.69 red-brown, laminated, clayey, fine sand; overl

with landfill trash fragments 

IC 36-04-B 330.69 330.55 red, laminated, fine sand IC 36-04-C 330.55 330.41 red-brown, laminated, clayey, fine-medium sa

IC 36-04-D 330.41 330.28 red-brown, laminated, medium sand 

IC 36-04-E 330.28 330.14 brown, laminated, clayey, medium sand 

IC 36-04-F 330.14 329.97 gray-brown, massive, medium sand 

IC 36-04-G 329.56 329.33 gray-brown, massive, medium sand IC 36-04-H 329.33 329.11 gray-brown, massive, medium sand 

IC 36-04-I 329.11 328.93 gray-brown, massive, medium sand 

IC 36-04-J 328.93 328.66 red-gray-brown, massive, medium sand 

IC 36-05-A 330.4 330.32 red-brown, fine sand 

IC 36-05-B 330.32 330.19 red brown, bedded, medium sand IC 36-05-C 330.19 330.04 red-brown, bedded, fine-medium sand 

IC 36-05-D 330.04 329.94 red-brown, massive, medium to coarse sand 

IC 36-05-E 329.94 329.82 gray-brown, medium sand with sparse clay pa

IC 36-05-F 329.82 329.68 gray-brown, medium sand with laminae of dar

fragments of carbonized plant fragments 

IC 36-05-G 329.68 329.53 gray-brown, massive, medium sand IC 36-05-H 329.53 329.41 gray-brown, massive, medium sand IC 54-04-A 330.56 330.38 Brown, fine sand overlying brown silt 

IC 54-04-B 330.38 330.16 red-brown, fine sand with interbedded brown IC 54-04-C 330.16 329.96 red-brown, laminated, silt and fine sand 

IC 54-04-D 329.96 329.75 red, laminated, medium sand 

IC 54-04-E 329.16 328.97 gray-brown, massive, medium sand 

IC 54-04-F 328.97 328.82 gray-brown, medium sand 

IC 54-04-G 328.82 328.66 brown, massive, medium sand IC 54-04-H 328.66 328.51 gray-brown, medium sand 

IC 54-04-I 328.40 328.30 intraclast conglomerate of red-brown, clayey, 

red-brown coarse-medium sand with carboniz

IC 54-05-A 330.12 330.01 red-brown, fine sand 

IC 54-05-B 330.01 329.89 red-brown, silt 

20
21

Appendix 2. Elevation and description of cored sediment samples —Continued.

Sample Number Sampled Interval Sediment Description 

Upper Elevation (m) Lower Elevation (m) 

IC 54-05-C 329.89 329.77 red-brown, laminated, fine sand 

IC 54-05-D 329.77 329.69 red, medium sand 

IC 54-05-E 329.69 329.54 red, faintly bedded, medium sand 

IC 54-05-F 329.54 329.40 light red-brown, medium sand 

IC 54-05-G 329.40 329.23 gray-brown, medium-fine sand with distorted IC 54-05-H 329.23 329.05 gray-brown, massive, medium sand with a few 

IC South-04-A 330.01 329.71 red, laminated, fine sand 

IC South-04-B 329.71 329.47 red, laminated, fine-medium sand intebedded IC South-04-C 329.47 329.31 red-brown, laminated, clayey, fine sand with d

granules and small carbonized wood fragment

IC South-04-D 329.31 329.15 red-brown, clayey, fine sand 

IC South-04-E 329.15 329.00 red-brown, fine sand with silty laminae 

IC South-04-F 328.61 328.40 red, massive, fine sand 

IC South-04-G 328.40 328.26 red, massive, fine sand IC South-04-H 328.26 328.18 red-brown, fine-medium sand 

IC South-04-I 328.18 327.92 upper 8 cm is red-brown, medium sand; lowe

upper medium sand with minor mud-clast frag

IC South-04-J 327.92 327.78 red-brown, upper medium sand, with deforme

IC South-04-K 327.78 327.63 red-brown, upper medium sand with mud clas

IC South-04-L 327.63 327.51 red-brown, upper medium sand with mud clas

IC South-05-A 329.69 329.58 red-brown, laminated, fine sand with carboniz

IC South-05-B 329.58 329.43 red, faintly laminated, fine sand IC South-05-C 329.43 329.33 red-brown, laminated, fine sand 

IC South-05-D 329.33 329.12 red, with faintly visible distorted bedding, fine 

IC South-05-E 329.12 328.93 brown, medium-fine sand 
Appendix 3. Results of the grain-size analysis of sediment samples. 

>500 μm 

(wt.%) 

500 to 250 μm 

(wt.%) 

250 to100 μm 

(wt.%) 

100 to 62 μm 

(wt.%) 

<62 μm 

Sample Number (wt.%) 

IC 36-04-A <1 1 10 79 10 

IC 36-04-B <1 6 18 64 12 

IC 36-04-C <1 13 65 19 2 

IC 36-04-D 1 19 50 26 4 

IC 36-04-E 1 33 57 8 <1 

IC 36-04-F <1 20 50 27 2 

IC 36-04-G 1 15 54 28 2 

IC 36-04-H 4 19 45 29 3 

IC 36-04-I <1 32 55 11 1 

IC 36-04-J <1 44 43 11 2 

IC 36-05-A <1 13 46 34 7 

IC 36-05-B <1 14 56 27 3 

IC 36-05-C <1 11 54 33 3 

IC 36-05-D 1 41 44 12 1 

IC 36-05-E 1 23 58 17 1 

IC 36-05-F <1 7 54 36 3 

IC 36-05-G 2 34 55 7 2 

IC 36-05-H 1 38 48 12 2 

IC 54-04-A 12 4 24 29 31 

IC 54-04-B <1 <1 33 27 40 

IC 54-04-C <1 <1 9 42 49 

IC 54-04-D <1 20 50 27 2 

IC 54-04-E 1 23 73 2 1 

IC 54-04-F <1 26 71 3 1 

IC 54-04-G <1 19 74 6 1 

IC 54-04-H <1 21 66 13 1 

IC 54-04-I 4 35 47 7 8 

22
Appendix 3. Results of the grain-size analysis of sediment samples—Continued. 

>500 μm 

(wt.%) 

500 to 250 μm 

(wt.%) 

250 to100 μm 

(wt.%) 

100 to 62 μm 

(wt.%) 

<62 μm 

Sample Number (wt.%) 

IC 54-05-A <1 1 21 27 51 

IC 54-05-B <1 <1 26 29 44 

IC 54-05-C <1 2 37 55 6 

IC 54-05-D <1 32 65 3 1 

IC 54-05-E <1 46 46 7 <1 

IC 54-05-F 5 60 32 4 <1 

IC 54-05-G <1 24 61 13 1 

IC 54-05-H 1 37 57 4 1 

IC South-04-A <1 4 26 64 6 

IC South-04-B 1 7 45 39 8 

IC South-04-C <1 1 34 60 4 

IC South-04-D <1 <1 21 79 1 

IC South-04-E <1 <1 15 79 6 

IC South-04-F <1 <1 21 71 8 

IC South-04-G <1 <1 34 62 4 

IC South-04-H <1 2 55 41 2 

IC South-04-I 3 21 46 28 2 

IC South-04-J 10 59 26 4 1 

IC South-04-K 7 60 28 3 1 

IC South-04-L 10 66 21 2 1 

IC South-05-A <1 <1 27 69 4 

IC South-05-B <1 <1 23 72 4 

IC South-05-C <1 <1 14 80 5 

IC South-05-D <1 <1 23 70 7 

IC South-05-E <1 1 35 59 5 

23
Appendix 4. Concentration of iron sequentially extracted from the sediment samples using 0.5 N 

HCl and Ti3+-EDTA. Concentrations were calculated on an air-dried sediment basis. 

[ppm, parts per million; Fe2+, ferrous iron; Fetotal, sum of ferrous and ferric iron] 

 

Sample Number 

Fe2+ 

 0.5 N HCl 

(μmole g-1) 

Fetotal 

0.5N HCl 

(μmole g-1) 

Fe2+/Fetotal 

0.5N HCl 

Fe 

Ti3+-EDTA 

(μmole g-1) 

IC 36-04-A 0.3 6.3 0.05 21.1 

IC 36-04-B 0.5 5.4 0.10 27.4 

IC 36-04-C 0.5 6.1 0.09 33.7 

IC 36-04-D 0.6 2.3 0.26 21.8 

IC 36-04-E 0.4 1.2 0.32 12.2 

IC 36-04-F 0.5 1.3 0.42 7.9 

IC 36-04-G 4.7 4.7 1.00 15.2 

IC 36-04-H 4.8 4.8 1.00 14.7 

IC 36-04-I 4.8 4.8 1.00 8.2 

IC 36-04-J 3.9 3.9 1.00 11.1 

IC 36-05-A 0.7 3.4 0.20 24.5 

IC 36-05-B 0.5 3.4 0.14 19.9 

IC 36-05-C 0.6 2.3 0.28 15.9 

IC 36-05-D 0.8 2.0 0.42 7.5 

IC 36-05-E 2.1 2.7 0.80 11.8 

IC 36-05-F 3.0 3.0 1.00 17.4 

IC 36-05-G 6.1 6.1 1.00 8.1 

IC 36-05-H 4.5 4.5 1.00 10.9 

IC 54-04-A 1.6 7.9 0.20 37.6 

IC 54-04-B 6.8 12.5 0.54 43.3 

IC 54-04-C 0.5 7.0 0.07 49.6 

IC 54-04-D 0.6 1.4 0.42 26.0 

IC 54-04-E 1.8 2.1 0.83 8.4 

IC 54-04-F 2.1 2.3 0.92 8.4 

IC 54-04-G 2.3 2.5 0.93 8.4 

IC 54-04-H 3.0 3.2 0.94 11.5 

IC 54-04-I 19.0 18.8 1.01 20.6 

24
Appendix 4. Concentration of iron sequentially extracted from the sediment samples—Continued. 

Sample Number 

Fe2+ 

 0.5 N HCl 

(μmole g-1) 

Fetotal 

0.5N HCl 

(μmole g-1) 

Fe2+/Fetotal 

0.5N HCl 

Fe 

Ti3+-EDTA 

(μmole g-1) 

IC 54-05-A 1.2 6.1 0.20 34.0 

IC 54-05-B 9.8 15.0 0.66 45.7 

IC 54-05-C 1.3 4.5 0.28 33.3 

IC 54-05-D 0.7 2.7 0.28 6.8 

IC 54-05-E 0.5 1.7 0.28 6.4 

IC 54-05-F 1.0 2.1 0.45 6.1 

IC 54-05-G 2.9 3.0 0.94 5.7 

IC 54-05-H 3.0 3.0 1.00 10.2 

IC South-04-A 0.6 3.4 0.19 29.2 

IC South-04-B 0.4 7.2 0.06 27.4 

IC South-04-C 6.4 9.8 0.65 29.2 

IC South-04-D 1.0 3.6 0.29 22.9 

IC South-04-E 4.5 4.7 0.96 22.7 

IC South-04-F 3.8 3.9 0.95 21.1 

IC South-04-G 2.9 3.2 0.89 20.2 

IC South-04-H 3.0 3.4 0.89 17.5 

IC South-04-I 3.0 3.2 0.94 12.5 

IC South-04-J 3.0 3.0 1.00 9.0 

IC South-04-K 2.3 2.3 1.00 7.9 

IC South-04-L 7.7 7.7 1.00 22.6 

IC South-05-A 2.0 4.5 0.44 20.8 

IC South-05-B 1.6 3.4 0.47 24.7 

IC South-05-C 4.7 5.0 0.93 23.3 

IC South-05-D 4.7 4.8 0.96 23.3 

IC South-05-E 4.8 5.2 0.93 19.3 

25
Appendix 5. Concentrations of water-soluble sulfate sulfur, acid-soluble sulfate sulfur, acid-volatile 

sulfide and disulfide sulfur extracted from the sediment samples and their sulfur isotope composition 

(δ34S). Recovered water-soluble sulfate was insufficient for isotope analyses. Acid-soluble sulfate 

extracted with hot 6 N HCl. Concentrations were calculated on an air-dried sediment basis. 

[nd, not determined; sulfate-HCl, acid-soluble sulfate; AVS, acid-volatile sulfide; DI, disulfide sulfur] 

Sample Number SulfateSulfur H O 2

(μmole g-1) 

SulfateSulfur 

6N HCl 

(μmole g-1) 

AVS 

(μmole g-1) 

DI 

(μmole g-1) 

δ

34Ssulfate-HCl 

(per mil) 

δ

34SAVS 

(per mil) 

δ

34SDI 

(per mil) 

IC 36-04-A 0.2 1.0 0.1 <0.1 10 nd nd 

IC 36-04-B <0.2 0.5 0.1 <0.1 9.6 nd nd 

IC 36-04-C <0.2 0.8 <0.1 <0.1 10.2 nd nd 

IC 36-04-D <0.2 0.7 <0.1 <0.1 11.4 nd nd 

IC 36-04-E 0.2 0.8 <0.1 <0.1 11.6 nd nd 

IC 36-04-F <0.2 0.7 <0.1 0.1 12.7 nd nd 

IC 36-04-G <0.2 0.7 1.7 2.2 13.3 -16.8 -24.0 

IC 36-04-H <0.2 0.6 2.8 1.2 15 -8.8 -19.3 

IC 36-04-I <0.2 0.7 1.7 0.6 13.7 -3.9 -19.1 

IC 36-04-J <0.2 0.6 0.6 0.5 11 -13.6 -17.7 

IC 36-05-A nd 0.2 <0.1 <0.1 7.6 nd nd 

IC 36-05-B nd 0.5 <0.1 <0.1 10.6 nd nd 

IC 36-05-C nd 0.4 <0.1 <0.1 12.1 nd nd 

IC 36-05-D nd 0.8 <0.1 0.2 15.2 nd nd 

IC 36-05-E nd 0.7 0.7 1.2 14.9 -16.3 -16 

IC 36-05-F nd 1.0 2.3 5.5 14.7 -18.5 -25.1 

IC 36-05-G nd 0.6 2.8 1.1 15.1 -7.6 -21.5 

IC 36-05-H nd 0.2 1.3 0.7 nd -4.9 -13.3 

IC 54-04-A 0.2 1.6 0.2 1.2 4 nd -9.1 

IC 54-04-B 70.2 2.4 0.2 <0.1 7.3 nd nd 

IC 54-04-C 70.2 1.7 0.1 <0.1 6.5 nd nd 

IC 54-04-D 0.3 0.7 <0.1 0.1 14.8 nd nd 

IC 54-04-E <0.2 0.4 0.6 0.2 14.1 -15.0 nd 

IC 54-04-F <0.2 0.4 0.8 0.2 15.8 -13.1 -18.8 

IC 54-04-G <0.2 0.7 0.4 0.3 20.1 -12.0 nd 

26
27

Appendix 5. Concentrations and isotopic composition of sulfur species—Continued. 

Sample Number SulfateSulfur H O 2

(μmole g-1) 

SulfateSulfur 

6N HCl 

(μmole g-1) 

AVS 

(μmole g-1) 

DI 

(μmole g-1) 

δ

34Ssulfate-HCl 

(per mil) 

δ

34SAVS 

(per mil) 

δ

34SDI 

(per mil) 

IC 54-04-H <0.2 0.7 0.9 0.4 19.0 -11.2 -15.9 

IC 54-04-I 0.5 1.9 3.8 15.0 10.8 4.3 3.6 

IC 54-05-A nd 1.4 0.1 0.1 nd nd nd 

IC 54-05-B nd 0.5 <0.1 0.1 nd nd nd 

IC 54-05-C nd 0.3 <0.1 0.1 nd nd nd 

IC 54-05-D nd 0.4 0.1 <0.1 12.8 nd nd 

IC 54-05-E nd 0.5 <0.1 <0.1 13.7 nd nd 

IC 54-05-F nd 0.8 0.1 <0.1 13.6 nd nd 

IC 54-05-G nd 0.5 0.5 0.3 18.1 -12.4 -16.4 

IC 54-05-H nd 0.6 1.1 1.1 11.3 -2 2.7 

IC South-04-A <0.2 0.8 <0.1 0.2 7.0 nd -16 

IC South-04-B <0.2 1.1 <0.1 0.1 6.2 nd nd 

IC South-04-C 0.2 1.3 0.4 0.5 5.5 -18.5 -19.7 

IC South-04-D <0.2 0.8 0.1 0.1 6.8 nd nd 

IC South-04-E 0.2 0.8 0.5 0.3 5.7 -14.4 -18.8 

IC South-04-F 0.2 0.9 0.4 0.6 5.5 -15.4 -22.4 

IC South-04-G <0.2 0.6 0.6 0.4 7.3 -17.8 -17.4 

IC South-04-H <0.2 0.7 0.6 0.4 9.7 -21.5 -15.4 

IC South-04-I <0.2 0.8 0.7 0.5 10.2 -17.8 -20.3 

IC South-04-J <0.2 1.4 2.4 1.4 9.5 -7.1 -16 

IC South-04-K <0.2 0.9 1.5 0.3 12.4 -7.8 -12 

IC South-04-L <0.2 1.2 2.1 2.0 11.4 -7.1 -13.3 

IC South-05-A nd 0.8 0.1 0.2 7.3 nd -17 

IC South-05-B nd 0.7 0.2 0.3 7.2 nd -19.7 

IC South-05-C nd 0.8 0.8 0.6 7.1 -13.3 -22.1 

IC South-05-D nd 0.8 0.5 0.3 6.6 -18.4 -23.5 

IC South-05-E nd 0.6 0.6 0.5 6.8 -17.4 -19.9 
Appendix 6. Results of chemical and isotopic analyses of ground water samples from wells at IC 36, IC 54, and IC 

[nd, not determined; S.Cond., specific conductance; μS/cm, microSiemens per centimeter; DOC, dissolved organic carbon; mg/L, milli

Well Sample 

Date 

Elevation of Well 

Screen Center pH 

S. Cond. 

(μS/cm) 

Ca 

(mg/L) 

Mg 

(mg/L) 

K 

(mg/L) 

Na 

(mg/L) 

IC 36-5 13-Oct-04 329.995 7.40 760 91.8 12 47 29 

IC 36-6 13-Oct-04 329.870 7.27 1040 67.2 18 0.6 0.60 

IC 36-7 13-Oct-04 329.730 7.33 1410 81.8 30 87 92 

IC 36-8 13-Oct-04 329.605 7.34 2330 238 89 108 245 

IC 36-9 13-Oct-04 329.450 7.22 2330 134 66 151 292 

IC 36-10 13-Oct-04 329.320 7.20 3350 90.2 48 188 303 

IC 36-11 13-Oct-04 329.200 7.01 3350 84.2 54 213 354 

IC 36-12 13-Oct-04 329.060 7.02 4340 87.8 63 228 395 

IC 36-13 13-Oct-04 328.920 7.06 4660 90.0 66 189 371 

IC 36-14 13-Oct-04 328.785 6.98 4800 130 86 208 473 

IC 36-15 13-Oct-04 328.655 7.02 4653 133 78 153 437 

IC 36-16 13-Oct-04 328.520 7.03 4630 164 95 172 531 

IC 36-17 13-Oct-04 328.385 7.02 4570 nd nd nd nd 

IC 36-3 19-Apr-05 330.260 7.28 584 86.6 7.4 13 19 IC 36-4 19-Apr-05 330.130 7.28 584 106 14.1 21 22 

IC 36-5 19-Apr-05 329.995 7.07 928 125 23 28 38 

IC 36-6 19-Apr-05 329.995 7.07 928 176 48 51 99 

IC 36-7 19-Apr-05 329.730 7.07 928 219 70 82 170 

IC 36-8 19-Apr-05 329.605 7.07 3104 238 89 108 245 IC 36-9 19-Apr-05 329.450 7.08 2826 202 83 142 273 

IC 36-10 19-Apr-05 329.320 6.78 3691 171 73 182 352 IC 36-11 19-Apr-05 329.200 7.23 4068 120 54 200 379 IC 36-12 19-Apr-05 329.060 7.49 4424 108 59 229 466 IC 36-13 19-Apr-05 328.920 7.10 4313 82.0 57 198 472 

28
Appendix 6. Results of chemical and isotopic analyses of ground water samples from wells—Continued. 

Well 

Sampled 

DOC 

(mg/L) 

HCO3-

mg/L 

Cl-

(mg/L) 

SO42-

(mg/L) 

δ18OSO4 

(per mil) 

δ34SSO4 

(per mil) 

δ18OH2O 

(per mil) 

IC 36-5 nd nd 21 50 6.6 10.7 -5.66 IC 36-6 9.4 nd 43 25 13.6 36.0 -5.83 

IC 36-7 16 nd 90 42 15.0 43.0 -5.94 

IC 36-8 29 nd 130 67 16.6 38.9 -6.04 IC 36-9 49 nd 210 78 16.5 36.5 -5.98 

IC 36-10 57 nd 230 24 17.6 41.3 -5.89 

IC 36-11 69 nd 270 7.9 nd nd -5.84 

IC 36-12 80 nd 340 1.4 nd nd -5.71 

IC 36-13 86 nd 360 0.5 nd nd -5.74 

IC 36-14 92 nd 390 0.6 nd nd -5.62 

IC 36-15 88 nd 400 0.6 nd nd -5.66 

IC 36-16 85 nd 400 0.8 nd nd -5.63 

IC 36-17 82 nd 400 0.5 nd nd -5.57 

IC 36-3 6.0 336.9 8.9 18.9 nd 14.7 -6.96 

IC 36-4 16 442.9 18.4 16.9 nd 20.6 -6.68 IC 36-5 20 533.7 35.8 21 nd 27.4 -6.84 IC 36-6 11 1008 91.2 47 nd 29.8 -7.12 IC 36-7 19 1417 143 60 15.2 30.1 -6.96 

IC 36-8 18 1768 185 51 20.0 46.2 -6.82 

IC 36-9 30 1897 203 38 18.5 50.4 nd 

IC 36-10 50 2071 244 46 17.6 49.3 -6.31 

IC 36-11 55 2180 274 39 16.9 48.0 -6.06 

IC 36-12 70 2332 329 15.2 nd nd -5.81 

IC 36-13 80 2224 348 1.0 nd nd -5.48 

29
Appendix 6. Results of chemical and isotopic analyses of ground water samples from wells—Continued. 

Well Sample 

Date 

Elevation of Well 

Screen Center pH 

S. Cond. 

(μS/cm) 

Ca 

(mg/L) 

Mg 

(mg/L) 

K 

(mg/L) 

Na 

(mg/L) 

IC 36-14 19-Apr-05 328.785 6.95 4030 82.7 56 166 447 

IC 36-15 19-Apr-05 328.655 7.10 3694 84.8 53 146 440 

IC 36-16 19-Apr-05 328.520 7.02 3639 87.4 51 135 425 

IC 36-17 19-Apr-05 328.385 6.97 3592 86.4 50 119 414 

IC 54-4 14-Oct-04 329.765 7.10 1580 150 51 7.5 125 

IC 54-5 14-Oct-04 329.615 7.15 1580 118 44 7.6 187 

IC 54-6 14-Oct-04 329.460 7.24 1470 96 35 7.8 191 

IC 54-7 14-Oct-04 329.305 7.28 1160 76 28 7.2 130 

IC 54-8 14-Oct-04 329.150 7.42 nd 67 28 7.2 138 IC 54-9 14-Oct-04 329.025 7.42 1120 54 24 6.7 181 

IC 54-10 14-Oct-04 328.875 7.70 1160 50 22 5.8 183 IC 54-11 14-Oct-04 328.720 7.70 1250 52 24 5.1 180 

IC 54-12 14-Oct-04 328.565 7.50 nd 65 29 5.9 214 IC 54-13 14-Oct-04 328.415 7.60 1290 58 26 4.8 194 

IC 54-14 14-Oct-04 328.265 7.50 1360 61 28 4.5 211 

IC 54-3 19-Apr-05 329.915 7.07 1580 168 44 9.1 77 

IC 54-4 19-Apr-05 329.765 6.75 1322 159 48 5.8 77 IC 54-5 19-Apr-05 329.615 6.84 1471 159 55 6.4 113 IC 54-6 19-Apr-05 329.460 6.84 1539 146 51 8.0 160 IC 54-7 20-Apr-05 329.305 6.83 1426 96 35 6.3 168 

IC 54-8 20-Apr-05 329.150 7.10 1410 87 34 6.8 197 

IC 54-9 20-Apr-05 329.025 7.10 1442 83 33 6.7 207 

IC 54-10 20-Apr-05 328.875 7.30 1586 91 37 6.3 238 

IC 54-11 20-Apr-05 328.720 7.25 1696 103 42 6.0 262 

30
Appendix 6. Results of chemical and isotopic analyses of ground water samples from wells—Continued. 

Well 

Sampled 

DOC 

(mg/L) 

HCO3-

mg/L 

Cl-

(mg/L) 

SO42-

(mg/L) 

δ18OSO4 

(per mil) 

δ34SSO4 

(per mil) 

δ18OH2O 

(per mil) 

IC 36-14 90 2037 328 0.2 nd nd -5.31 IC 36-15 88 1886 314 0.5 nd nd -5.17 IC 36-16 82 1851 300 0.5 nd nd -5.02 IC 36-17 81 1840 306 0.5 nd nd -5.09 

IC 54-4 6.6 nd 84 98 13.9 15.6 -3.80 

IC 54-5 9.8 nd 94 117 nd nd -3.43 IC 54-6 15 nd 89 87 16.0 26.4 -3.24 

IC 54-7 19 nd 68 25 nd nd -3.05 

IC 54-8 32 nd 64 8.6 18.6 42.9 -2.78 IC 54-9 21 nd 63 7.7 nd nd -4.04 

IC 54-10 22 nd 64 10.6 21.4 61.5 -3.02 

IC 54-11 25 nd 73 21 nd nd -2.56 

IC 54-12 25 nd 75 15.1 22.0 65.7 -2.49 

IC 54-13 25 nd 73 1.6 nd nd -2.62 

IC 54-14 24 nd 82 1.0 nd nd -2.89 

IC 54-3 2.1 813 41 27 nd 49.4 -5.36 IC 54-4 5.4 820 43 33 nd 14.2 -5.21 IC 54-5 20 870 65 57 nd 18.4 -4.62 IC 54-6 13 858 74 61 nd 24.8 -3.91 IC 54-7 16 766 81 40 nd nd -3.26 IC 54-8 27 765 86 26 nd nd -2.90 IC 54-9 14 812 87 16.5 nd nd -2.44 

IC 54-10 17 883 110 21 nd 74.1 -1.70 

IC 54-11 17 807 130 27 nd nd -1.27 

31
Appendix 6. Results of chemical and isotopic analyses of ground water samples from wells—Continued.

Well Sample 

Date 

Elevation of Well 

Screen Center pH 

S. Cond. 

(μS/cm) 

Ca 

(mg/L) 

Mg 

(mg/L) K (mg/L) 

Na 

(mg/L) 

IC 54-12 20-Apr-05 328.565 7.23 1822 105 43 5.8 272 

IC 54-13 20-Apr-05 328.415 7.28 2032 118 49 5.3 280 IC 54-14 20-Apr-05 328.265 6.87 2368 144 59 5.6 309 

IC South-3 14-Oct-04 329.655 7.80 797 144 11 2.1 5.6 

IC South-4 14-Oct-04 329.505 7.20 928 200 13 2.4 6.4 

IC South-5 14-Oct-04 329.355 7.20 907 182 13 3.1 8.1 IC South-6 14-Oct-04 329.195 7.20 913 183 16 4.2 11 

IC South-7 14-Oct-04 329.035 7.10 979 201 20 5.1 13 

IC South-8 14-Oct-04 328.895 7.21 1010 170 19 4.9 12 

IC South-9 14-Oct-04 328.765 7.20 993 161 19 4.8 14 

IC South-10 14-Oct-04 328.595 7.20 930 141 20 4.9 23 

IC South-11 14-Oct-04 328.445 7.30 972 141 23 5.2 42 

IC South-12 14-Oct-04 328.295 7.35 1140 142 32 5.2 66 

IC South-13 14-Oct-04 328.145 7.40 1210 128 35 4.8 74 

IC South-14 14-Oct-04 327.995 7.40 1320 142 40 4.9 99 

IC South-3 20-Apr-05 329.655 7.50 800 104 12 2.1 17.2 IC South-4 20-Apr-05 329.655 6.63 628 123 8.1 1.3 5.4 IC South-5 20-Apr-05 329.355 6.63 676 138 11 1.7 6.7 

IC South-6 20-Apr-05 329.195 6.71 781 154 14 2.7 8.4 

IC South-7 20-Apr-05 329.035 6.58 888 178 17 3.7 11 

IC South-8 20-Apr-05 328.895 6.75 922 185 19 4.0 13 

IC South-9 20-Apr-05 328.765 6.78 918 181 19 4.1 14 

IC South-10 20-Apr-05 328.595 6.81 934 153 19 4.0 25 

IC South-11 20-Apr-05 328.445 6.61 1082 158 24 4.5 52 

32
Appendix 6. Results of chemical and isotopic analyses of ground water samples from wells—Continued. 

Well 

Sampled 

DOC 

(mg/L) 

HCO3-

mg/L 

Cl-

(mg/L) 

SO42-

(mg/L) 

δ18OSO4 

(per mil) 

δ34SSO4 

(per mil) 

δ18OH2O 

(per mil) 

IC 54-12 26 969 160 7.9 20.2 62.1 -1.09 

IC 54-13 20 1030 210 1.1 nd nd -1.60 

IC 54-14 24 1160 260 0.2 n d nd -2.14 

IC South-3 7.3 nd 1.3 27 nd nd -5.19 IC South-4 7.2 nd 0.3 22 12.0 -6.88 -5.18 IC South-5 10 nd 0.3 48 nd nd -5.30 IC South-6 nd nd 0.7 96 14.0 -5.9 -5.36 IC South-7 7.3 nd 0.9 130 nd nd -5.41 IC South-8 5.9 nd 1.4 127 13.5 -4.8 -5.38 

IC South-9 6.5 nd 2.3 99 nd nd -5.20 

IC South-10 6.8 nd 12.6 42 18.0 11.1 -5.07 

IC South-11 7.0 nd 22 22 nd nd -4.88 

IC South-12 4.6 nd 53 9.7 18.1 31.3 -4.55 

IC South-13 11 nd 65 23 nd nd -4.28 

IC South-14 9.2 nd 78 23 20.5 40.1 -4.01 

IC South-3 4.9 278 8.5 14.8 nd 14.7 -6.09 IC South-4 2.8 414 2.4 14.5 nd nd -5.59 

IC South-5 7.6 432 2.1 36 nd nd -5.28 

IC South-6 3.4 482 2.3 60 nd nd -5.37 

IC South-7 1.3 550 3.5 80 14.5 -1.3 -5.41 

IC South-8 3.7 586 6.0 68 15.3 31.8 -5.42 

IC South-9 1.1 581 8.7 54 nd nd -5.33 

IC South-10 1.6 575 31 23 nd nd -5.12 IC South-11 4.9 638 60 9.3 nd nd -4.54 

33
Appendix 6. Results of chemical and isotopic analyses of ground water samples from wells—Continued. 

Well Sample 

Date 

Elevation of Well 

Screen Center pH 

S. Cond. 

(μS/cm) 

Ca 

(mg/L) 

Mg 

(mg/L) K (mg/L) 

Na 

(mg/L) 

IC South-12 20-Apr-05 328.295 6.07 1343 169 31 4.6 67 

IC South-13 20-Apr-05 328.145 6.62 1412 173 44 4.5 102 

IC South-14 20-Apr-05 327.995 6.97 1507 167 45 4.1 110 

34
35

Appendix 6. Results of chemical and isotopic analyses of ground water samples from wells—Continued. 

Well 

Sampled 

DOC 

(mg/L) 

HCO3-

mg/L 

Cl-

(mg/L) 

SO42-

(mg/L) 

δ18OSO4 

(per mil) 

δ34SSO4 

(per mil) 

δ18OH2O 

(per mil) 

IC South-12 5.5 756 104 4.7 nd nd -4.65 IC South-13 3.8 786 116 6.0 21.5 69.5 -3.96 

IC South-14 5.8 829 134 6.5 nd 69.5 -3.68