EPA/600/R-02/032
                                                            September 2001
                            Final Report
 Characterization and Eh/pH-Based Leaching Tests of Mercury-
Containing Mining Wastes from the Sulfur Bank Mercury Mine,
                      Lake County, California
                          Contract No. 68-C7-0057
                            Task Order No. 26
                              Submitted to

                 United States Environmental Protection Agency
                 National Risk Management Research Laboratory
                      26 West Martin Luther King Drive
                           Cincinnati, Ohio 45268

                              Paul de Percin
                              Project Officer

                             Paul M. Randall
                           Task Order Manager

                             Makram Suidan
                    University of Cincinnati Project Officer
                              Submitted by

                                Battelle
                             505 King Avenue
                           Columbus, Ohio 43201

                           Sandip Chattopadhyay
                              Jennifer Ickes

                            September 27, 2001

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                                        Notice
The U.S. Environmental Protection Agency through its Office of Research and Development funded
and managed the research described here under Contract No. 68-C7-0057, Task Order No. 26 to Battelle,
Columbus, Ohio. It has been subjected to the Agency's peer and administrative review and has been
approved for publication as an EPA document. Mention of trade names or commercial products does
not constitute endorsement or recommendation for use.

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                                       Foreword
The U.S. Environmental Protection Agency is charged by Congress with protecting the Nation's land,
air, and water resources.  Under a mandate of national environmental laws, the Agency strives to
formulate and implement actions leading to a compatible balance between human activities and the
ability of natural systems to support and nurture life. To meet this mandate, EPA's research program is
providing  data  and technical support for solving environmental problems  today and building a
science  knowledge  base  necessary to manage our ecological resources wisely, understand  how
pollutants affect our health, and prevent or reduce  environmental risks in the future.

The National Risk Management Research Laboratory is the Agency's center for investigation of
technological and management  approaches for preventing and reducing risks from pollution that
threatens human health and the environment.  The focus of the Laboratory's research program is on
methods and their cost-effectiveness for prevention and control of pollution to air, land, water, and
subsurface resources; protection of water quality in public water systems; remediation of contaminated
sites, sediments and ground water; prevention and control of indoor air pollution; and restoration of
ecosystems. NRMRL collaborates with both public and private sector partners to foster technologies
that reduce the cost of compliance and to anticipate emerging problems. NRMRL's research provides
solutions to environmental problems  by: developing and promoting technologies that protect and
improve the environment; advancing scientific and engineering information to support regulatory and
policy  decisions;  and  providing  the  technical support  and information transfer to ensure
implementation of environmental regulations and strategies  at the national, state, and community
levels.

This publication has been produced as part of the Laboratory's strategic long-term research plan. It is
published  and made available by EPA's  Office  of Research and Development to assist the  user
community and to link researchers with their clients.
                                        E. Timothy Oppelt, Director
                                        National Risk Management Research Laboratory
                                                 ill

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                               Acknowledgements


This technical report has been prepared by Battelle in fulfillment of Contract No. 68-C7-0057, Task
Order (TO) No. 26 under the sponsorship of the United States Environmental Protection Agency's
(USEPA's) National Risk Management Research Laboratory (NRMRL). The work was conducted at
Battelle, Columbus, Ohio during the period of September 29, 2000 to September 28, 2001.

Mr. Paul de Percin was the U. S. EPA Proj ect Officer for this contract and Mr. Paul Randall was the Task
Order Manager (TOM) for this TO. Dr. Victor Magar was the Battelle Program Manager for this contract.
Dr. Sandip Chattopadhyay was the Battelle Task Order Leader (TOL) and Project Manager. The mem-
bers of the Battelle project staff included Ms. Jennifer Ickes, Ms. KirstenHartzell, Ms. Jody Lipps, and
Mr. Daniel Janke. Editorial and graphical support was provided by Mr. Thomas Wilk, Mr. Dean Sutton,
and Ms. Loretta Bahn.
                                              IV

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                                 CONTENTS

FIGURES	vi
TABLES	vi
ACRONYMS AND ABBREVIATIONS	vii

1.0 INTRODUCTION	1
    1.1 Project Objective	2

2.0 LABORATORY EXPERIMENT AND ANALYTICAL METHODS	3
    2.1 Solid Material Preparation	3
    2.2 Variable pH Leaching Procedure	3
    2.3 Variable Eh Leaching Procedure	4
    2.4 Filtration	4
    2.5 Analytical Procedures	5

3.0 RESULTS AND DISCUSSION	7
    3.1 Characterization of Waste Materials	7
    3.2 Effect of Eh andpH Conditions	7

4.0 REFERENCES	15

APPENDIX A:  ANALYTICAL RESULTS
APPENDIX B:  LABORATORY REPORTED MERCURY DATA WITH QC SUMMARY
            FOR VARIABLE EH AND PH EXPERIMENTS
APPENDIX C:  LABORATORY REPORTED ACIDITY, ALKALINITY, AND CHLORIDE
            DATA WITH QC SUMMARY FOR VARIABLE Eh AND pH EXEPRIMENTS
APPENDIX D:  LABORATORY REPORTED DATA FOR SULFUR BANK MERCURY
            MINE WASTE ORE
APPENDIX E:  CHAIN-OF-CUSTODY FORMS

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                                          FIGURES

Figure 1-1.   Location Map of Sulfur Bank Mercury Mine	1
Figure 2-1.   Variable Eh Experimental Setup	4
Figure 2-2.   Millipore Pressure Filtration Unit Pressurized with UHP Nitrogen	5
Figure 3-1.   X-ray Diffractogram of the Waste Matrix	8
Figure 3-2a.   SEI at 1500X, and EDS Analysis of Hg-Contaminated Waste Ore	8
Figure 3-2b.   BEI at 1200X, and EDS Analysis of Hg-Contaminated Waste Ore	9
Figure 3-2c.   BEI at 500X, and EDS Analysis of Hg-Contaminated Waste Ore	9
Figure 3-3.   Leachability of Hg Conducted by TCLP Method at Different pH and Eh Conditions	10
Figure 3-4.   Concentration ofHg in the Leachate at Different pH Conditions	11
Figure 3 -5.   Eh Values at Variable pH Conditions Maintained During the Experiments	11
Figure 3-6.   Turbidity of the Leachate at Different pH Conditions	12
Figure 3-7.   Concentration ofHg in the Leachate at Different Eh Conditions	12
Figure 3-8.   Leaching Rate ofHg With Fe (Eh 0.55 V) and Without Fe (Eh 0.5 V) at pH 3.2	13
Figure 3 -9.   Concentration of Chloride in the Leachate at Different Eh Conditions	13
Figure 3-10.   Composite Leaching Profile ofHg from the Waste Material at Different Eh and
             pH Conditions	14


                                          TABLES

Table 2-1.    Critical and Noncritical Measurements and Methods	3
Table 2-2.    Fe(III) Concentrations	4
Table 3-1.    Selected Physical and Chemical Properties of SBMM Waste Ore	7
                                             VI

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                           ACRONYMS AND ABBREVIATIONS
ASTM        American Society for Testing and Materials

BDL          below detection limit
BEI           backscattered electron image

ccm           cubic centimeters per minute
CERCLA      Comprehensive Environmental Response, Compensation, and Liability Act
CVAA        cold vapor atomic absorption

EDS          energy dispersive spectrophotometer
Eh            redox equilibria (volt difference between platinum electrode and standard hydrogen
              electrode)

Fe            iron
Fe(NO3)3      ferric nitrate

Hg            mercury
HgS           cinnabar
H2O2          hydrogen peroxide
H2SO4        sulfuric acid

ICDD         International Centre for Diffraction Data

MDI          Materials Data, Inc.

NaOH        sodium hydroxide
NPL          National Priorities List
NRMRL      National Risk Management Research Laboratory
NS            not sampled
NTU          nephelometric turbidity unit(s)

ORP          oxidation-reduction potential

pH            negative logarithm of the activity of aqueous FT

QAPP        Quality Assurance Project Plan

RO           reverse osmosis

SBMM        Sulfur Bank Mercury Mine
SEI           secondary electron image
SEM          scanning electron microscope
SiO2          silicon oxide, quartz

TCLP         Toxicity Characteristic Leaching Procedure
TiO2          anatase
TO            Task Order
TOL          Task Order Leader
TOM         Task Order Manager
                                             vn

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UC            University of Cincinnati
UHP           ultrahigh purity
U.S. EPA      United States Environmental Protection Agency

XRD           x-ray diffractometer
                                              Vlll

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                                     1.0  INTRODUCTION
Clear Lake in northern California has received inputs of mercury (Hg) mining wastes from the Sulfur
Bank Mercury Mine (SBMM) (Figure 1-1). About 1.2 million tons of Hg-contaminated overburden and
mine tailings were distributed over a 50-ha surface area due to mining operations from 1865 to 1957
(Gerlach et al., 2001).  The SBMM includes an open, unlined mine pit, Herman Pit, which covers approx-
imately 23 acres and is 750 feet upgradient of Clear Lake. Reynolds et al. (1997) analyzed water samples
collected from Herman Pit and Clear Lake and reported the pH values at those locations as 3 and 8,
respectively.  The SBMM was placed on the Final National Priorities List (NPL) list in 1990.  The site
has been under investigation as a Comprehensive Environmental Response, Compensation, and Liability
Act (CERCLA) site and has experienced some minor corrective actions.  Clear Lake remains under a fish
advisory due to the mercury contamination.
                                                              Enlarged
                                                            / Area
Nevada

                      Highland Springs

                        '
                          3      9
                                          .

                     Figure 1-1. Location Map of Sulfur Bank Mercury Mine
Mercury in contaminated soils is a unique pollutant that requires innovative remediation solutions. Con-
ventional stabilization/solidification treatments cannot effectively reduce the leachability of Hg (Conner,
1990). As part of the remediation effort at the SBMM site, the U.S. EPA is assisting in the development
of treatment alternatives for waste material from the site. Waste materials consist of waste ore, waste
rock, and roaster tailings. To support this work, leaching profiles of waste  ore over a range of different
pH and oxidation-reduction (Eh) conditions were performed.  Chemical and biological processes affecting
the mobility of metals may be initiated by altering the physicochemical environment (i.e., pH and Eh con-
ditions). Important processes influencing the chemistry and availability of trace and toxic metals include
(1) precipitation as insoluble sulfides under highly reduced conditions (Morel et al., 1974); (2) formation
of discrete metal oxides and hydroxides of low solubility (Morel et al., 1974); (3) adsorption of colloidal
hydrous oxides of iron and manganese, primarily in aerobic, neutral, or alkaline environments (Windom,
1973); and (4) complex formation with soluble and insoluble organic matter (Loganathan et al., 1977).

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Each experiment has been designed to evaluate leachability of Hg from the waste materials under con-
trolled conditions in order to assess conditions that may contribute to the destabilization of Hg in the
waste ore.

                                     1.1 Project Objective

The objective of this TO was to study a range of different pH and Eh values in order to evaluate the
potential of SBMM waste ore to leach Hg. This study was conducted in accordance with the Quality
Assurance Project Plan (QAPP) No. 63-Q1-3 (Battelle, 2001).

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             2.0 LABORATORY EXPERIMENT AND ANALYTICAL METHODS

Table 2-1 identifies both critical and noncritical measurements that were made during the course of this
study. All analytical methods are described in QAPP No. 63-Q1-3 (Battelle, 2001) except the method for
chloride analysis.  (Chloride analysis was requested by the U.S. EPA TOM via e-mail on May 22, 2001.)
                 Table 2-1. Critical and Noncritical Measurements and Methods
                     Measurement
               Method
               Mercury
               ORP
               J3H	
   Critical
U.S. EPA SW-846 Method 7470A
ORION® 96-78-00 Combination Redox Probe
U.S. EPA Method 9045C
               Turbidity
               Alkalinity/Acidity
               Chloride
 Noncritical
Hach 2100N Turbidimeter
U.S. EPA Method 310.1/305.1
U.S. EPA Method 407A
              ORP = oxidation-reduction potential.
                                2.1  Solid Material Preparation

The waste ore used in this study was obtained from the SBMM by the U.S. EPA. After receipt at
Battelle, the waste material was homogenized, and then was ground for 8 hours and passed through
American Society for Testing and Materials (ASTM)-approved No. 30 and No. 100 sieves to achieve
particle sizes between 150 (im and 600 (im. The moisture from the samples was removed according to
ASTM Method D2261-80.

                             2.2 Variable pH Leaching Procedure

The pH leaching procedure was based on University of Cincinnati's constant pH leaching procedure from
QAPP No. 63-Q1-2 (UC, 1999). All experiments were conducted in accordance with the approved QAPP
(QAPP ID No. 63-Q1-3) (Battelle, 2001).

To measure leachability at different pH values (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, and 12), 25 g of dry solid
sample were added in each 1-L bottle. Leachant at different pH values was prepared by adding nitric acid
(0.1 N) or sodium hydroxide (0.1 N) in deionized reverse osmosis (RO) water.  Duplicate samples were
prepared for pH values 2, 5, 9, and 12.  A solution to solid ratio of 20:1 was maintained in each of the
bottles containing soil waste materials. The bottles were placed on a tumbler (Model 3740-12-BRE,
Associated Design & Mfg. Co., VA) and equilibrated overnight. The pH was monitored frequently and
adjusted as needed over the 24-hour time period.  At the end of the reaction period, the pH of the leachant
and the equilibrium pH of the solid-liquid suspension were recorded.  ORPs of the leachate also were
recorded after equilibration.  Both pH and ORP were measured by a Corning pH/ion meter (Model 450).
The ORP values were converted and are reported as Eh.

The above leaching procedure was followed in presence of ferric nitrate (Fe[NO3]3 -9H2O) (J.T. Baker,
NJ) at four different pH values (3, 6, 9, and 11) to determine the effect of iron (Fe) on leaching of Hg.
The amount of Fe(NO3)3-9H2O added to each sample was based on the Hg concentration as observed
from the previous set of experiments where no  Fe was added. The amount of ferric nitrate was based on a
final Fe concentration equal to the Hg concentration from the variable pH experiments (Table 2-2).

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                               Table 2-2.  Fe(III) Concentrations
pH
o
6
6
9
11
Hg Concentration in Absence
ofFe(ni)(jig/L)
15.3
728
1,938
4,020
Fe(N03)3 9H20
0.055
2.633
7.009
14.540
(mg)

                              2.3 Variable Eh Leaching Procedure

This section describes the experimental plan to determine the effect of Eh at two different pH values, on
the mercury concentrations in the leachate. The pH of the leachant was maintained by adding suitable
amounts of sulfuric acid (H2SO4) or sodium hydroxide (NaOH).  The pH values selected by the U.S. EPA
were 3.2 and 6.0. About 500 mL of the leachant was added to 25 g of prepared waste ore material, and
the solution was readjusted to the desired pH.  The Eh of the suspension then was varied by using one of
the following three methods, without adding any chemicals: (1) purging the suspension with O2 (to make
the water aerobic); (2) purging the suspension with a mixture of H2 and O2; and (3) purging the sus-
pension with N2 or H2 (to make the water anaerobic). About 1,670 uL of 3% hydrogen peroxide (H2O2)
was added to achieve a higher Eh value of 0.63 V  during only one set of experiments.  All other exper-
iments were conducted using different proportions of gas and gas flow control to establish target Eh
values within the upper and lower Eh boundary conditions. To determine the effect of Fe(III), 0.01 g of
Fe(NO3)3-9H2O was added  in three samples during the variable Eh experiments (Table A-4).  A schematic
diagram and a photograph of the experimental setup are shown in Figure 2-1.

                                         2.4  Filtration

After leaching, the suspended samples were filtered prior to Hg analysis.  The suspension was passed
through 0.7-um Toxic Characteristic Leaching Procedure (TCLP) acid-treated low metal glass fiber filters
(Whatman, UK) using a pressure filtration unit (Millipore Corp., MA) pressurized with ultrahigh purity
                 Flowmeter
  AIR/0,
           i
          a. Schematic Diagram                             b. Photograph

                          Figure 2-1. Variable Eh Experimental Setup

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(UHP) nitrogen (see Figure 2-2). The filtrate from each sample was collected in a 500-mL bottle; a por-
tion of the sample was acidified with nitric acid to obtain a pH less than 2 and stored inside the refrigera-
tor at 4°C until analyzed for Hg.  The remainder of the sample was sent to Wilson Environmental
Laboratories (Columbus, OH) for either alkalinity/acidity analysis or chloride analysis.
          Figure 2-2.  Millipore Pressure Filtration Unit Pressurized with UHP Nitrogen
                                   2.5  Analytical Procedures

The samples were prepared and analyzed according to U.S. EPA SW-846 Method 7470A:  Mercury in
Liquid Waste and Method 7471 A: Mercury in Solid or Semisolid Waste by using a cold vapor atomic
absorption (CVAA) spectrophotometry (Perkin Elmer 51OOPC Atomic Absorption Spectrophotometer
attached with Flow Injection Automated System), in which the mercury is reduced to the elemental state
and aerated from solution in a closed system. The mercury vapor passed through a quartz cell positioned
in the light path of an atomic absorption spectrophotometer. Absorbance  (peak height) was measured at
the 253.7-nm wavelength as a function of mercury concentration. The detection limit was 0.2 ug/L.
Total elemental analysis was conducted by acid digestion as per U.S. EPA Method 3050B of 1 g of solid
sample to a final volume of 100 mL.

The turbidity of the filtrate was measured by using a Hach 2100N turbidimeter. Alkalinity and acidity
were analyzed using U.S. EPA Methods 310.1 and 305.1, respectively. Chloride was analyzed using U.S.
EPA Method 407A.

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                               3.0 RESULTS AND DISCUSSION

The results of the experiments are discussed and analyzed below; analytical results are tabulated in
Appendix A.

                            3.1 Characterization of Waste Materials

Selected physical and chemical properties of the SBMM waste ore material are given in Table 3-1. The
material has an acidic pH and was moderately oxidizing.  The homogenized and sieved solid samples
were analyzed with an x-ray diffractometer (XRD), scanning electron microscope (SEM), and energy
dispersive spectrophotometer (EDS). The XRD patterns (Figure 3-1) of the recovered crystalline phases
were compared using organic and inorganic databases from the International Centre for Diffraction Data
(ICDD) Powder Diffraction Database, and Materials Data, Inc. (MDI) Jade software for pattern treatment
and search-match. In this analysis, the crystals anatase (synthetic TiO2), cinnabar (HgS), and silicon
oxide (SiO2) were identified.  The secondary electron images (SEIs), backscattered electron images
(BEIs), and EDS elemental analyses are shown in Figures 3-2a through 3-2c.  Secondary electron imaging
shows topographic contrast, with highest resolution at low operating current.  Backscattered electron
imaging shows compositional contrasts, which are greatest at higher operating current.

                              3.2 Effect of Eh and pH Conditions

Eh and pH conditions are important influences on the mobility of Hg. Figure 3-3 illustrates different
chemical forms of Hg under specific Eh and pH conditions. The data points (  ) on the stability diagram
show the different conditions achieved during  the experiments.  In general, metallic mercury is very
insoluble in sediments over a wide pH range.  Dissolved inorganic Hg combines with chloride up to a pH
of 7. It exhibits a very high affinity for sulfide in mildly reducing environments,  such as stream and lake
sediments, forming insoluble mercuric sulfides (Wang and Driscoll, 1995). Dissolved Hg also sorbs
strongly to sediment and suspended solids, including iron oxyhydroxides (Balogh et al., 1997). Gagnon
and Fisher (1997)  demonstrated that the binding strength of mercury to sediments is high and that less
desorption occurs under acidic conditions.
            Table 3-1. Selected Physical and Chemical Properties of SBMM Waste Ore
Properties
pH
Eh
Analytical Result
3.2±0.10
0.44±0.055 V
Particle Size Distribution
Sand (>50 pm)
Silt (2-50 urn)
Clay (< 2 pm)
81%
41%
36%
Carbon Content
Organic
Total
Cation Exchange Capacity
0.44% C
0.46% C
6.5 mequiv/lOOg
Elemental Analysis
Mercury
Arsenic
Titanium
Lead
Sulfide
206 ng/g
3.9 ng/g
364.9 ng/g
36.5 p,g/g
3285.4 ng/g

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                     0.0  10.0 20.0 30.0  40.0 50.0 60.0  70.0 80.0 90.0 100.0
                                    Degrees 2-0
                 Figure 3-1. X-ray Diffractogram of the Waste Matrix
                                                    SEII at 1.500X Magnification
Spectrum
1
2
3
C
6.50
18.90
24.80
0
13.14
53.74
47.84
Al

0.31
3.43
Si
2.24
12.07
22.10
S
9.20
0.19

K


1.19
Ti

14.27
0.38
V

0.28

Fe

0.24
0.27
Cu
0.78


Hg
68.13


Total
100.00
100.00
100.00
All results in wt% and all elements are normalized.
      Figure 3-2a. SEI at 1500X, and EDS Analysis of Hg-Contaminated Waste Ore

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Spectrum
1
2
3
4
5
C
18.62
14.87
23.99
11.64
14.68
0
42.15
45.22
57.00
52.19
58.68
Al
0.37
0.30
0.54
0.26
0.00
Si
13.25
11.94
17.46
12.84
26.64
S

2.18
0.11
0.20

K

0.09
0.07


Ti
10.15
0.51
0.70
22.34

Fe
15.46

0.14
0.52

Cu

0.22
0.00


Hg

24.67



Total
100.00
100.00
100.00
100.00
100.00
     All results in wt% and all elements are normalized.




          Figure 3-2b. BEI at 1200X, and EDS Analysis of Hg-Contaminated Waste Ore

                                100-pm
                                                         BEI 31SOOX Magnification
Spectrum
1
2
C

18.520
O
48.77
62.78
Al
0.55
0.38
Si
35.37
17.29
S
0.38
0.09
K
0.21
0.04
Ca
0.20

Ti
5.89
0.78
Fe
0.89
0.11
Cu
0.74
0.00
Hg
68.13

Total
100.00
100.00
All results in wt% and all elements are normalized.
           Figure 3-2c. BEI at SOOX, and EDS Analysis of Hg-Contaminated Waste Ore

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             LU
                                                     Most Surface Water
                   -1
  Figure 3-3. Leachability of Hg Conducted by TCLP Method at Different pH and Eh Conditions
  (modified after Davis et al., 1997; and surface and groundwater information obtained from Garrels and
Christ, 1965).  The data points « ) on the stability diagram show the different conditions attended during
                                        the experiments.
The effect of pH on leaching of Hg from the waste materials is plotted in Figure 3-4.  The Hg concentra-
tion increased as the equilibrium pH of the suspension increased to a pH value of 10.65.  Thereafter, the
Hg concentration decreased sharply.  Acidity and alkalinity were measured for pH experiments and
results are shown in Tables A-l and A-2.  Alkalinity concentrations were below detection level (BDL)
(<1 mg/L) at low pH and increased as the sample pH increased. Acidity was highest at low pH and
decreased BDL at pHs greater than 5. Eh of the suspension decreased as the pH increased. The Hg con-
centration, in presence of Fe(III), decreased significantly. The resulting Eh conditions, in presence and
absence of Fe(III), during the experiments at different pH values are shown in Figure 3-5. The turbidity
of the filtrate increased as the pH increased even though the same filters were used in all experiments
(Figure 3-6).

The concentration of Hg in the leachate at variable Eh conditions is shown in Figure 3-7.  During the
experiments with variable Eh, the pH values were maintained 3.2 ± 0.08 and 6.4 ±0.10 and both Eh and
pH were monitored for about 24 hours. Each data point represents individual experiment and there were
no replicates. Hg  concentration, at pH 3.2, increased with increase in oxidation potential until the Eh
value reached 0.2  V.  Further oxidizing conditions reduced the leaching of Hg from the waste matrix.
The concentration of Hg in the leachate increased sharply when H2O2 was added to attain a higher
oxidation potential (Eh = 0.63 V). At pH 3.2, Fe(III) did not show any effect on leaching of Hg. The Hg
concentration varied from 2.5 to 5.7 mg kg"1 during the experiments, when the pH was maintained at 6.4.
These experiments were conducted for about 24 hours. The rate of leaching of Hg at pH 3.2 in absence,
and in presence of Fe(III) is shown in Figure 3-8. At the beginning of the experiment, Fe(III) releases Hg
through oxidation. Burkstaller et al. (1975) reported leaching of Hg through oxidation of cinnabar in
presence of Fe(III) in acid mine waters (pH <2.0). However, presence of Fe(III) reduces the rate of Hg
leaching over a 24-hour period. The  rates of dissolution of Hg from the waste ore at pH 3.2 are calculated
as 1.02 x 10"7 s"1 and 3.32 x 10"8 s"1 in absence of Fe(III) and in presence of Fe(III), respectively. The
change in chloride concentration as the Eh values change is shown in Figure 3-9.
                                               10

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— on
j? 80
|* 70
-60
° 50
2 40
c
a) 30
o
i 20
0 10
°> „
In

[Hg] with Fe »[Hg] without Fe
-
-
-
-
-

• *

* **
123456

,
*


* *
^



i i i i i










7 8 9 10 11 12
PH
     Figure 3-4. Concentration of Hg in the Leachate at Different pH Conditions
0.3

0.2
£ °-1
0
04



* *
* •
-
.1
123456
pH


Eh with Fe * Eh without Fe

•






7 8 9 10 11 12
Figure 3-5. Eh Values at Variable pH Conditions Maintained During the Experiments
                                      11

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   70
~ 60
H 50
> 40
I 30
£2
$ 20
K 10
     0
with Fe * without Fe
4	1
       1    2    3     4    5     6    7     8    9    10   11    12
                                     PH
       Figure 3-6. Turbidity of the Leachate at Different pH Conditions

/
6
0)
M_ 5
C *f~*4
O O)
1 »3
*•• c
c S2
0) ^^
O
c 1
o
° 0

A
A
A
A
t *


•

^
	 P 	

-0.2 -0.1 0.0 0.1 0.2 0.3 0.4
Eh(V)


*pH 3.2 without Fe
OpH 3.2 with Fe
A pH 6.4 without Fe

4







* O + O



























0.5 0.6 0.7


   Figure 3-7. Concentration of Hg in the Leachate at Different Eh Conditions
                                   12

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                  10000  20000 30000 40000  50000 60000 70000  80000  90000
                                   Time (seconds)
Figure 3-8.  Leaching Rate of Hg With Fe (Eh 0.55 V) and Without Fe (Eh 0.5 V) at pH 3.2
180
TJ 160
0 140
.G
O _ 120
° S 10°
5 » so
Concentre
(i
M ^ O
,OOOO
f->


O pH 3.2 without Fe
• pH 3.2 with Fe
A pH 6.4 without Fe
A


A

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Alkaline and reduced conditions were found to enhance soluble levels of Hg. Wollast et al. (1975)
reported that although the insoluble mercuric sulfide (cinnabar) will form in reducing environments, dis-
solved levels of Hg may increase in more strongly reducing conditions by conversion of the mercuric ion
to the free metal form. Although the SBMM-water system studied for this report may differ from the
Belgium River water described by Wollast et al. (1975), it is interesting to note that this study also
detected higher levels of soluble Hg under strongly reducing conditions. The Eh-pH diagram (Figure 3-3)
showed the comparatively soluble free metallic form to be stable compared to less soluble sulfide forms.

A composite leaching profile of Hg at different Eh and pH conditions is shown in Figure 3-10.  Based on
the leaching experiments, the concentration of Hg in the leachate (mg/L) was correlated to the different
Eh (V) and pH values as follows:

      Concentration of Hg in the leachate = 6.78 - 8.16 x pH + 3.56 x pH2 - 0.7 x pH3 + 0.06 x pH4
                                            -   0.002 x PH5 + 0.0004/Eh.

The r2 of the fitted equation was 0.96. The above correlation was obtained by using TableCurve 3D™
(Jandel  Scientific) software.
 r~  4
                                                                                         0,80
                                                                                 20
                                                                                    Eh(V)
                                                                        -0.20
   Figure 3-10. Composite Leaching Profile of Hg from the Waste Material at Different Eh and
                                         pH Conditions
                                               14

-------
                                     4.0 REFERENCES

Balogh, S.J., M.L. Meyer, and D.K. Johnson.  1997.  "Mercury and Suspended Sediment Loadings in the
       Lower Minnesota River." Environmental Science and Technology, 31: 198-202.

Battelle.  2001.  Quality Assurance Project Plan for Characterization andpH-based Leaching Tests of
       Mercury Containing Mining Wastes from Sulfur Bank Mercury Mine, Lake County, California.
       QAPPIDNo. 63-Q1-3.

Burkstaller, J.E., P.L. McCarty, and G.A. Parks.  1975. "Oxidation of Cinnabar by Fe(III) in Acid Mine
       Waters." Environmental Science and Technology, 9: 676-678.

Conner, J.R. 1990. Chemical Fixation and Solidification of Hazardous Wastes. Van Nostrand-Reinhold,
       NY.

Davis, A., N.S. Bloom, and S.S. Que Hee. 1997. "The Environmental Geochemistry and Bioaccessibility
       of Mercury in Soils and Sediments: A Review." Risk Analysis, 17(5): 557-569.

Gagnon, C., and N.S. Fisher.  1997.  "Bioavailability of Sediment-Bound Methyl and Inorganic Mercury
       to a Marine Bivalve." Environmental Science and Technology, 31: 993-998.

Garrels, R.M., and C.L. Christ.  1965. Solutions, Minerals,  and Equilibria. Freeman, Cooper and
       Company, San Francisco, CA.

Gerlach, R.W., M.S. Gustin, and J.M.V. Emon. 2001.  "On-Site Mercury Analysis of Soil at Hazardous
       Waste Sites by Immunoassay and ASV." Applied Geochemistry, 16: 281-290.

Loganathan, P., R.G. Burau, and D.W. Fuerstenau.  1977. "Influence of pH on the Sorption of Co2+, Zn2+
       and Ca2+ by a Hydrous Manganese Oxide." Soil Science Society of America Journal,  41: 57-62.

Morel, F., R.E. McDuff, and J.J. Morgan.  1974.  "Interactions and Chemostasis in Aquatic Chemical
       Systems: Role of pH,  pE, Solubility, and Complexation."  In P.C. Singer (Ed.), Trace Metals and
       Metal - Organic  Interactions in Natural Waters.  Ann Arbor Science Publishers, Ann Arbor, MI.
       pp.  157-200.

Reynolds, R., R. Kauper, and H. Keller. 1997. In Vitro Production of a White Coagulant Material from
       the Mixing of Herman Pit and Clear Lake Waters Similar to that Observed in the Field, and
       Remedial Suggestion.  Clear Lake Symposium Abstracts: Sulfur Bank Mercury Mine and Related
       Processes. University of California, Davis.

University of Cincinnati (UC). 1999. Quality Assurance Project Plan: Stabilization and Testing of
       Mercury Containing Wastes.  Prepared for U.S. EPA's NRMRL, Cincinnati, OH, under Contract
       No. 68-C7-0057, QAPP ID No. 63-Q1-2.

Wang, W., and C.T. Driscoll.  1995.  "Patterns of Total Mercury Concentrations in Onondaga Lake, New
       York." Environmental Science and Technology, 29: 2261-2266.

Windom, H.L.  1973. Investigations of Changes in Heavy Metals Concentrations Resulting from
       Maintenance Dredging of Mobile Bay Ship Channel, Mobile Bay, Alabama.  Report for Contract
       No. DACW01-73-C-0136. U.S. Army Corps of Engineers, Mobile District.

Wollast, R., G. Billen, and F.F. Mackenzie. 1975. "Behavior of Mercury in Natural Systems and Its
       Global Cycle." In: A.R. Mclntyre, C.F. Mills (Eds.), Ecological Toxicology Research. Plenum
       Publishing Co., NY. pp. 145-166.
                                              15

-------
    APPENDIX A




ANALYTICAL RESULTS

-------
                      Table A-l.  Analytical Results for pH Experiments
Sample ID
pH=2
pH=2 DUP
pH=3
pH=4
pH=5
pH=5 DUP
pH=6
pH=7
pH=8
pH=9
pH=9 DUP
pH=10
pH=ll
pH=12
pH=12 DUP
Blank
Hg
(ng/L)
4
17.5
15.3
248
373
385
728
835
1,431
1,938
1,790
3,691
4,020
2,236
1,976
<2.5
Hg
(mg/kg)
0.08
0.35
0.31
4.96
7.46
7.70
14.56
16.70
28.62
38.76
35.80
73.82
80.40
44.72
39.52
BDL
Final pH
2.06
2.02
3.04
3.91
4.72
4.49
5.62
6.10
7.33
8.75
8.72
9.96
10.65
11.69
11.59
5.58
Final Eh
(V)
0.22
0.21
0.20
0.16
0.20
0.15
0.10
0.10
0.09
0.05
0.06
0.05
0.02
-0.02
-0.01
0.17
Turbidity
(NTU)
0.28
3.85
4.05
33.5
42.1
27.8
25.5
32.0
33.2
29.3
30.7
29.3
40.2
52.6
59.9
0.179
Acidity
(mg/L)
1,050
1,275
110
3
8
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
17
Alkalinity
(mg/L)
<1
<1
<1
32
44
38
38
36
55
72
75
310
1,020
4,150
4,000
19
BDL = below detection limit.
             Table A-2.  Analytical Results for pH Experiments with Iron Addition
Sample ID
pH3-WithFe
pH6-WithFe
pH9-WithFe
pHll-WithFe
Blank- With Fe
Hg
(ng/L)
0.9
2.6
164
296
<2.5
Hg
(mg/kg)
0.018
0.052
3.28
5.92
BDL
Final pH
2.94
5.28
8.45
10.38
7.06
Final Eh
(V)
0.24
0.13
0.06
0.09
0.09
Turbidity
(NTU)
1.42
0.946
19.2
16.3
0.479
Acidity
(mg/L)
59
6
10
<1
2
Alkalinity
(mg/L)
<1
29
69
750
30
             Table A-3. Analytical Results for Eh Experiments at Target pH = 3.2
Gas
(Flow rate, ccm)
H2 (150)
H2(110)/02(85)
O2 (94)/H2 (70)
02(110)/H2(38)
N2 (65)
02 (75)
O2 (150)
O2( 150)+ peroxide
Hg
(Hg/L)
26.7
137
133
71.1
97.6
15.5
9.1
195
Hg
(mg/kg)
0.53
2.74
2.66
1.42
1.95
0.31
0.18
3.90
Average pH
3.10
3.25
3.30
3.20
3.24
3.18
3.05
3.18
Average Eh
(V)
-0.01
0.11
0.19
0.30
0.37
0.49
0.56
0.63
Chloride
(mg/L)
1
<1
<1
<1
<1
6
7
1
     ccm = cubic centimeters per minute.

-------
    Table A-4. Analytical Results for Eh Experiments at Target pH = 3.2 with Iron Addition
Gas (Flow
rate, ccm)
H2 (150)
02 (75)
O2 (150)
Hg
(ng/L)
12.8
16.1
15.2
Hg
(mg/kg)
0.26
0.32
0.30
Average pH
3.18
3.12
2.99
Average Eh
(V)
0.00
0.54
0.59
Chloride
(mg/L)
1
<1
8
             Table A-5. Analytical Results for Eh Experiments at Target pH = 6.4
Gas (Flow
rate, ccm)
H2 (150)
H2 (55)
H2 (30)/O2 (122)
N2 (150)
02(150)
Hg
(Hg/L)
174
287
124
197
253
Hg
(mg/kg)
3.48
5.74
2.48
3.94
5.06
Average pH
6.42
6.31
6.47
6.26
6.48
Average Eh
(V)
-0.13
-0.01
0.11
0.21
0.26
Chloride
(mg/L)
6
2
NS
5
6
       NS = not sampled.
Table A-6. Analytical Results for Eh Kinetics Experiments at Target pH = 3.2 Without Iron (Flow
                                      rate = 50 ccm)
Time
(seconds)
120
420
1320
2220
3120
4020
11220
14820
75720
82920
Hg
(Ug/L)
202.29
155.88
164.24
91.43
60.26
114.24
152.39
27.89
1,238.05
623.51
Hg
(mg/kg)
4.05
3.12
3.28
1.83
1.21
2.28
3.05
0.56
24.76
12.47
Hg
(jimol/L)
1.01
0.78
0.82
0.46
0.30
0.57
0.76
0.14
6.17
3.11
PH
3.36
3.18
3.19
3.20
3.32
3.20
3.21
3.14
3.36
3.40
Eh
(V)
0.48
0.48
0.49
0.48
0.49
0.49
0.49
0.56
0.53
0.49
 Table A-7. Analytical Results for Eh Kinetics Experiments at Target pH = 3.2 With Iron (Flow
                                      rate = 50 ccm)
Time
(seconds)
120
420
1320
2220
3120
4020
11220
14820
75720
82920
Hg
(Ug/L)
98.31
136.06
117.63
187.55
65.64
85.86
252.59
25.50
360.56
275.90
Hg
(mg/kg)
1.97
2.72
2.35
3.75
1.31
1.72
5.05
0.51
7.21
5.52
Hg
(jimol/L)
0.49
0.68
0.59
0.93
0.33
0.43
1.26
0.13
1.80
1.38
pH
3.27
3.08
3.31
3.33
3.21
3.25
3.21
3.33
3.13
3.18
Eh
(V)
0.52
0.58
0.57
0.53
0.52
0.52
0.52
0.58
0.55
0.55

-------
                         APPENDIX B




LABORATORY REPORTED MERCURY DATA WITH QC SUMMARY FOR VARIABLE




                    Eh AND pH EXPERIMENTS

-------
G466507-UC41
   TO 26 MERCURY LEACHING
           Variable pH Experiments

           Project #
           Samples Received
           Samples Analyzed
           Method Used
   G466507-UC41
          3/29/01
            4/3/01
EPA SW-846-7470
SAMPLE I.D.

pH=2
pH=2 DUP
pH=3
pH=4
pH=5(a)
pH=5 DUP(a)
pH=6
pH=7
pH=8
pH=9
pH=9 DUP
pH=10
pH=11
pH=12
pH=12DUP
Hg CONCENTRATION
(ng/L)
4
17.5
15.3
248
8713
<500*
728
835
1431
1938
1790
3691
4020
2236
1976
          * Sample "pH=5 DUP" was diluted 1 TO 1000. This dilution was beyond the range of the calibration curve.
          This sample will be properly re-analyzed with the subsequent sample set.
          (a) Samples pH=5 and pH=5 Dup were rerun because of problems filtering the samples.
QC SUMMARY
Calibration Curve 1
Calibration Curve 2
Continuing Calibration Verification (CCV) 1
CCV2
Corr. Coefficient | Recovery
0.9995
0.9974




108%
110%
                                           9/18/01 11:35 AM

-------
                                          RESULTS
                                                      9/18/01 11:34 AM
Variable pH Experiments

Project #
Samples Received
Samples Analyzed
Method Used
    G466507-UC41
           4/17/01
           4/18/01
  EPA SW-846-7470
Sample ID

pH5-rerun
pH5-rerun DUP
pH3-With Fe
pJH6-With Fe
pH9-With Fe
pH11-WithFe
Blank-With Fe
Hg Concentration
(ng/ L)
373
385
0.9
2.6
164
296
<2.5
Quality Control
Date: 4/18/01

Sample ID

Blank
CCV 5 ppb
Percent Recovery
pH11 wFe
pH11 wFeDup
Relative Percent Difference
CCV 5 ppb
Percent Recovery '
CCV 5 ppb
Percent Recovery ;; ;;.
Mercury
(WJ/L)

0
4.9
' ,!98%
373
385
3%
4.9
-i , „ 98%
5.2
;; 	 ;..';. 104%
                                      HG_041801_FINAL

-------
RESULTS MERCURY
Variable Eh Experiments

Project #
Title
Samples Received
Samples Analyzed
Results Reported
Method Used
   G466507-UC41
 Mercury Leaching
         6/29/01
          7/3/01
          7/5/01
EPA SW-846 7470
SAMPLE I.D.

REPORTING LIMIT
1 Hg
2 Hg w/ Fe
3Hg
4 Hg w/ Fe
5Hg
6 Hg w/ Fe
7Hg
8Hg
9Hg
10 Hg
11 Hg
T = 0m
T = 0 m Fe
T = 5m
T = 5 m Fe
T=15m
T = 15mFe
T = 30m
T = 30 m Fe
T = 45m
T = 45 m Fe
T = 1 hr
T = 1 hr Fe
T = 3hr
T = 3 hr Fe
T = 5hr
T = 5 hr Fe
T = 21 hr
T = 21 hr Fe
T = 23 hr
T = 23 hr Fe
Concentration of mercury
(ug/L)
0.2 |jg/ L
9.0637
15.2390
26.6932
12.8486
15.5378
16.1355
137.0518
133.1673
97.6096
71.1155
194.9203
202.2908
98.3068
155.8765
136.0558
164.2430
117.6295
91 .4343
187.5498
60.2590
65.6375
114.2430
85.8566
152.3904
252.5896
27.8884
25.4980
1238.0478
360.5578
623.5060
275.8964
HG 7-3-01 TO26 RESULTS
   9/18/01 11:20 AM

-------
MERCURY QC
Variable Eh Experiments

Project #
Title
Samples Received
Samples Analyzed
Results Reported
Method Used
        G466507-UC41
TO26 - Mercury Leaching
               6/29/01
                7/4/01
                7/5/01
     EPA SW-846 7470
SAMPLE I.D.
CCB
CCV 5 ppb

METHOD BLANK 7-4-01

1 Hg
1 Hg Method Duplicate

CCB
CCV 5 ppb

lOJHg DILUTED 1 TO 10
10 Hg OIL 1 TO 10 Method Spike

Vl Hg DILUTED 1 TO 10
11 Hg OIL 1 TO 10 Method Duplicate
ilpII^iiHliW'BiHSlSllillPWHfiti 	 i
T = 45 m DILUTED 1 TO 10
T = 45 m OIL 1 TO 1 0 Method Spike
^j^ffSiii^j^li^r^^m^^Sjiiiji 	 ;fe,w,;,;,
CCB
CCV 5 ppb
	 !i!!l
T = 24 hr Fe DILUTED 1 TO 100
T = 24 hr Fe OIL 1 TO 1 00 Method Spike

CCB
CCV 5 ppb

1 Hg
1 Hg Method Duplicate

CCB
CCV 5 ppb
	
Hg
0.1
5.0

0.0

9.1
9.0
	
0.19
5.07
	
7.1
11.6

19.5
19.6
	
6.0
11.0

OJ
5.0

2.8
7.0

0.1
5.1
Sim^mK^LmgKi^
9.0
9.2

OO
4.6

HG 7-3-01 TO26 RESULTS
    9/14/01 2:24 PM
1 OF1

-------
Variable Eh Experiments
Project #
Title
Samples Received
Samples Analyzed
Method Used
   G466507-UC41
 Mercury Leaching
         7/26/01
         8/10/01
EPA SW-846 7470
SAMPLE I.D.

Reporting Limit
14 Hg
15 Hg
16 Hg
17 Hg
18 Hg
Concentration of mercury
(ng/L)
0.2 ng/ L
253
197
174
124
287
Analyte
Mass
Sample Unit
Blank
Standard 1
Standard 2
Standard 3
Standard 4
Standard 5
Standard 6
Standard 7
Standard 8
Standard 9
CCV-25

14 Hg 1-10
14 Hg 1 -1 0 Analytical Duplicate

18 Hg 1-10
1 8 Hg 1 -1 0 Analytcial Spike

CCV-25
,/.::.::.:: ..:. .-,.:'. .:.."..: :«, . . -. '.. '" :"'
Hg
199
ng/L

1.00
0.15
3.30
5.22
10.69
25.41
50.08
100.65
249.64
25.52
102%
26.15
25.16
, ',',',;• * •.. r - , 4%
28.38
56.67
' '"' '" ' WA
23.31
<: ••;:•• 93%
Hg
200
ng/L

1.07
0.17
3.31
5.32
10.75
25.66
50.53
100.92
249.42
25.60
102%
25.34
25.83
' • •* -s2%
28.67
57.52
,?..s415%
23.88
96%
Hg
202
MS/L

1.01
0.15
3.30
5.34
10.92
25.44
49.97
100.68
249.64
25.54
102%
26.20
26.02
1%
28.63
58.70
M.:"«2'0%
23.73
95%

-------
                          APPENDIX C




LABORTORY REPORTED ACIDITY, ALKALINITY, AND CHLORIDE DATA WITH QC




          SUMMARY FOR VARIABLE Eh AND pH EXPERIMENTS

-------
       WILSON
       ENVIRONMENTAL LABORATORIES, INC.
                                                                                   MEMBER
                                                                                   AOL
MS.  JENNIFER ICKES
BATTELLE MEMORIAL  INSTITUTE
505  KING AVENUE
COLUMBUS,OHIO 43201-2693
            407 Venture Drive • Suite C • Westerville, Ohio 43081 • (614) 431-0010 • Fax: (614) 431-1650
                                              Page 1 of 15
                                     Lab Number:  WE10685-1

                                     PROJECT:  G466507-UC41
SAMPLE DESCRIPTION

PH2

CONSTITUENT
    REPORT OF ANALYTICAL RESULTS

     MATRIX    SAMPLED BY     SAMPLED DATE/TIME   RECEIVED

     Aqueous    K. HARTZELL            27 MAR 01  30 MAR 01

RESULT      *D.L.   UNITS     METHOD   ANALYZED   BY NOTES
ACIDITY
Alkalinity
1050            1   mg/L     305.1     04-10-01  WTW
       <1       1   mg/L     310.1     04-10-01  WTW
     *  Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T.  Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                                                     Page 2 of 15
                                                             Lab Number: WE10685-2

                                                             PROJECT: 6466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

PH2 DUP                        Aqueous   K. HARTZELL           27 MAR 01 30 MAR 01
CONSTITUENT
                          RESULT

                          1275
                                      *D.L.   UNITS
                                                       METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
                                 <1
1   mg/L     305.1     04-10-01 WTW
1   mg/L     310.1     04-10-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KINO AVENUE
COLUMBUS,OHIO 43201-2693
                                           Page 3 of 15
                                   Lab Number: WE10685-3

                                   PROJECT: G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

PH3                            Aqueous   K. HARTZELL           27 MAR 01 30 MAR 01
CONSTITUENT
RESULT

 110
                                      *D.L.
     UNITS
METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
       <1
1   mg/L     305.1     04-10-01
1   mg/L     310.1     04-10-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                           Page 4 of 15
                                   Lab Number: WE10685-4

                                   PROJECT: 0466507-UC41
SAMPLE DESCRIPTION

PH4

CONSTITUENT
    REPORT OF ANALYTICAL RESULTS

     MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

     Aqueous   K. HARTZELL           27 MAR 01 30 MAR 01

RESULT      *D.L.   UNITS    METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
   3
  32
1   mg/L     305.1     04-10-01 WTW
1   mg/L     310.1     04-10-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc,
Wilson T. Walker

-------
This page intentionally left blank (i.e., no page 5 of 15).

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                         Page 6 of 15
                                 Lab Number: WE10685-6

                                 PROJECT: 6466507-UC41
SAMPLE DESCRIPTION

PH5 DUP

CONSTITUENT
  REPORT OF ANALYTICAL RESULTS

   MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

   Aqueous   K. HARTZELL           27 MAR 01 30 MAR 01
                          RESULT
          *D.L.
                                              UNITS
                           METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
38
<1      1   mg/L     305.1     04-10-01 WTW
        1   mg/L     310.1     04-10-01 WTW
    * Detection Limit.
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KINO AVENUE
COLUMBUS,OHIO 43201-2693
                                         Page 7 of 15
                                 Lab Number: WE10685-7

                                 PROJECT: G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

PH6                            Aqueous   K. HARTZELL           29 MAR 01 30 MAR 01
CONSTITUENT
                          RESULT
          *D.L.
                                              UNITS
                                                       METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
38
<1      1   mg/L     305.1     04-10-01 WTW
        1   mg/L     310.1     04-10-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                         Page 8 of 15
                                 Lab Number: WE10685-8

                                 PROJECT: G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

PH7                            Aqueous   K. HARTZELL           29 MAR 01 30 MAR 01
CONSTITUENT
                          RESULT
                                      *D.L.
                                              UNITS
                                                       METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
36
<1      1   mg/L     305.1     04-10-01 WTW
        1   mg/L     310.1     04-10-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                         Page 9 of 15
                                 Lab Number: WE10685-9

                                 PROJECT: G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

PH8                            Aqueous   K. HARTZELL           29 MAR 01 30 MAR 01
CONSTITUENT
                          RESULT
                                      *D.L.
                                              UNITS
                                                       METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
55
<1      1   mg/L     305.1     04-10-01 WTW
        1   mg/L     310.1     04-10-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                           Page 10 of 15
                                  Lab Number: WE10685-10

                                   PROJECT: G466507-UC41
SAMPLE DESCRIPTION

PH9

CONSTITUENT
    REPORT OF ANALYTICAL RESULTS

     MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

     Aqueous   K. HARTZELL           29 MAR 01 30 MAR 01

RESULT      *D.L.   UNITS    METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
  72
<1      1   mg/L     305.1     04-10-01 WTW
        1   mg/L     310.1     04-10-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                                                     Page 11 of 15
                                                            Lab Number: WE10685-11

                                                             PROJECT: G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

                               Aqueous   K. HARTZELL           29 MAR 01 30 MAR 01
PH9 DUP

CONSTITUENT
                          RESULT
                                      *D.L.   UNITS    METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
                            75
<1      1   mg/L     305.1     04-10-01 WTW
        1   mg/L     310.1     04-10-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                          Page 12 of 15
                                 Lab Number: WE10685-12

                                  PROJECT: G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

PH10                           Aqueous   K. HARTZELL           29 MAR 01 30 MAR 01
CONSTITUENT
                          RESULT
                                      *D.L.
                   UNITS
                                                       METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
310
<1      1   mg/L     305.1     04-10-01 WTW
        1   mg/L     310.1     04-10-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KINO AVENUE
COLUMBUS,OHIO 43201-2693
                                                                     Page 13 of 15
                                                            Lab Number: WE10685-13

                                                             PROJECT: 6466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

                               Aqueous   K. HARTZELL           29 MAR 01 30 MAR 01
PH11

CONSTITUENT
                          RESULT
                                      *D.L.
                                              UNITS
                                                       METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
                          1020
<1      1   mg/L     305.1     04-10-01 WTW
        1   mg/L     310.1     04-10-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                                                     Page 14 of 15
                                                            Lab Number: WE10685-14

                                                             PROJECT: G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

                               Aqueous   K. HARTZELL           29 MAR 01 30 MAR 01
PH12

CONSTITUENT
                          RESULT
                                       D.L.
                                              UNITS
                                                       METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
                          4150
<1      1   mg/L     305.1     04-10-01 WTW
        1   mg/L     310.1     04-10-01 WTW
      Detection Limit
Wilson Environmental Laboratories, Inc,
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                           Page 15 of 15
                                  Lab Number: WE10685-15

                                   PROJECT: 0466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

PH12 DUP                       Aqueous   K. HARTZELL           29 MAR 01 30 MAR 01

CONSTITUENT               RESULT      *D.L.   UNITS    METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
4000
<1      1   mg/L     305.1     04-10-01 WTW
        1   mg/L     310.1     04-10-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
       WILSON
       ENVIRONMENTAL LABORATORIES, INC.
                                                                                  ACIL
MS. JENNIFER ICKES
BATTELLE  MEMORIAL INSTITUTE
505 KING  AVENUE
COLUMBUS,OHIO 43201-2693
            407 Venture Drive • Suite C • Westerville, Ohio 43081 • (614) 431-0010 • Fax: (614) 431-1650
                                             Page  1 of 7
                                     Lab Number: WE10711-1

                                PROJECT:  T026 G466507-UC41
SAMPLE DESCRIPTION

PH=5 RERUN

CONSTITUENT
    REPORT  OF ANALYTICAL RESULTS

     MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

     Aqueous    J.  ICKES               10 APR 01  11  APR 01

RESULT      *D.L.    UNITS    METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
   8
  44
1   mg/L      305.1     04-19-01 WTW
1   mg/L      310.1     04-19-01 WTW
    * Detection Limit
Wilson  Environmental Laboratories, Inc,
Wilson  T.  Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KINO AVENUE
COLUMBUS,OHIO 43201-2693
                                           Page 2 of 7
                                   Lab Number: WE10711-2

                              PROJECT: T026 G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED
============================== ========= ============= ================= _===_____
PH=3 U>/ Ft                     Aqueous   J. ICKES              10 APR 01 11 APR 01
CONSTITUENT
RESULT

  59
                                      *D.L.
                                              UNITS
                                                       METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
       <1
1   mg/L     305.1     04-19-01 WTW
1   mg/L     310.1     04-19-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KINO AVENUE
COLUMBUS,OHIO 43201-2693
                                         Page 3 of 7
                                 Lab Number: WE10711-3

                            PROJECT: T026 G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

PH=6  tO/ Fe.                     Aqueous   J. ICKES              10 APR 01  11 APR 01

CONSTITUENT               RESULT      *D.L.   UNITS    METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
 6
29
1   mg/L     305.1     04-19-01 WTW
1   mg/L     310.1     04-19-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KINO AVENUE
COLUMBUS,OHIO 43201-2693
                                         Page 4 of 7
                                 Lab Number: WE10711-4

                            PROJECT: T026 G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

PH=9  W/ft.                      Aqueous   J. ICKES              10 APR 01 11 APR 01
CONSTITUENT
                          RESULT
                                      *D.L.
                                              UNITS
                                                       METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
10
69
1   mg/L     305.1     04-19-01 WTW
1   mg/L     310.1     04-19-01 WTW
      Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                          Page 5 of 7
                                  Lab Number: WE10711-5

                             PROJECT: T026 O466507-UC41
                              REPORT OF ANALYTICAL RESULTS
SAMPLE DESCRIPTION
                               MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

PH=11  U>/ Fc                    Aqueous   J. ICKES              10 APR 01  11 APR 01

CONSTITUENT               RESULT      *D.L.   UNITS    METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
750
<1      1   mg/L     305.1     04-19-01 WTW
        1   mg/L     310.1     04-19-01 WTW
      Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                           Page 6 of 7
                                   Lab Number: WE10711-6

                              PROJECT: T026 G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

BLANK  U>/ R                    Aqueous   J. ICKES              10 APR 01  11 APR 01
CONSTITUENT
RESULT
                                      *D.L.
     UNITS
                                                       METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
   2
  30
1   mg/L     305.1     04-19-01 WTW
1   mg/L     310.1     04-19-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc.
Wilson T. Walker

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                         Page 7 of 7
                                 Lab Number: WE10711-7

                            PROJECT: T026 G466507-UC41
SAMPLE DESCRIPTION
  REPORT OF ANALYTICAL RESULTS

   MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED
BLANK WITHOUT FE               Aqueous   J. ICKES              10 APR 01  11 APR 01

CONSTITUENT               RESULT      *D.L.   UNITS    METHOD   ANALYZED  BY NOTES
ACIDITY
Alkalinity
17
19
1   mg/L     305.1     04-19-01 WTW
1   mg/L     310.1     04-19-01 WTW
    * Detection Limit
Wilson Environmental Laboratories, Inc<
Wilson T. Walker

-------
         WILSON
         ENVIRONMENTAL LABORATORIES, INC.
MS. JENNIFER ICKES
BATTELLE  MEMORIAL INSTITUTE
505 KING  AVENUE
COLUMBUS,OHIO 43201-2693
               401 Venture Drive • Suite C • Westenille, Ohio 43081 • (614) 431-0010 • fax; (614) 431-1650
                                              Page 1 of  11
                                     Lab Number:  WE10865-1

                                PROJECT: TO26 G466507-UC41
SAMPLE  DESCRIPTION

1 Hg

CONSTITUENT
    REPORT  OF ANALYTICAL RESULTS

     MATRIX    SAMPLED BY     SAMPLED DATE/TIME  RECEIVED
     Aqueous   J. ICKES               19  JUN 01 02 JUL  01

RESULT       *D.L.   UNITS     METHOD   ANALYZED  BY NOTES

   7            1   mg/L      407A      07-10-01 WMB
Chloride

     *  Detection Limit
Wilson Environmental Laboratories,  Inc.
 W.  Martin Bell

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                           Page 2 of 11
                                   Lab Number: WE10865-2

                              PROJECT: TO26 G466507-UC41
SAMPLE DESCRIPTION

2 Hg w/Fe

CONSTITUENT

Chloride
    REPORT OF ANALYTICAL RESULTS

     MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

     Aqueous   J. ICKES              19 JUN 01 02 JUL 01

RESULT      *D.L.   UNITS    METHOD   ANALYZED  BY NOTES

   8           1   mg/L     407A      07-10-01 WMB
    * Detection Limit
Wilson Environmental Laboratories, Inc.
W. Martin Bell

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                           Page 3 of 11
                                   Lab Number: WE10865-3

                              PROJECT: TO26 G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

3 Hg                           Aqueous   J. ICKES              20 JUN 01 02 JUL 01
CONSTITUENT

Chloride

    * Detection Limit
RESULT

   1
*D.L.   UNITS    METHOD   ANALYZED  BY NOTES

   1   mg/L     407A      07-10-01 WMB
Wilson Environmental Laboratories, Inc.
W. Martin Bell

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KINO AVENUE
COLUMBUS,OHIO 43201-2693
                                       Page 4 of 11
                               Lab Number: WE10865-4

                          PROJECT: TO26 G466507-UC41
SAMPLE DESCRIPTION
REPORT OF ANALYTICAL RESULTS

 MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED
4 Hg w/Fe                      Aqueous   J. ICKES              20 JUN 01 02 JUL 01

CONSTITUENT               RESULT      *D.L.   UNITS    METHOD   ANALYZED  BY NOTES
Chloride

    * Detection Limit
               mg/L
407A
07-10-01 WMB
Wilson Environmental Laboratories, Inc.
W. Martin Bell

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                           Page 5 of 11
                                   Lab Number: WE10865-5

                              PROJECT: TO26 G466507-UC41
SAMPLE DESCRIPTION

5 Hg

CONSTITUENT

Chloride
    REPORT OF ANALYTICAL RESULTS

     MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

     Aqueous   J. ICKES              21 JUN 01 02 JUL 01

RESULT      *D.L.   UNITS    METHOD   ANALYZED  BY NOTES

   6           1   mg/L     407A      07-10-01 WMB
    * Detection Limit
Wilson Environmental Laboratories, Inc.
W. Martin Bell

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KINO AVENUE
COLUMBUS,OHIO 43201-2693
                                           Page 6 of 11
                                   Lab Number: WE10865-6

                              PROJECT: TO26 G466507-UC41
SAMPLE DESCRIPTION

6 Hg w/Fe

CONSTITUENT

Chloride
    REPORT OF ANALYTICAL RESULTS

     MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

     Aqueous   J. ICKES              21 JUN 01 02 JUL 01

RESULT      *D.L.   UNITS    METHOD   ANALYZED  BY NOTES

       <1      1   mg/L     407A      07-10-01 WMB
    * Detection Limit
Wilson Environmental Laboratories, Inc.
W. Martin Bell

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                                                     Page 7 of 11
                                                             Lab Number: WE10865-7

                                                        PROJECT: TO26 G466507-UC41
SAMPLE DESCRIPTION

7 Hg
                              REPORT OF ANALYTICAL RESULTS

                               MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED
                               Aqueous   J. ICKES              22 JUN 01 02 JUL 01

CONSTITUENT               RESULT      *D.L.   UNITS    METHOD   ANALYZED  BY NOTES
Chloride

    * Detection Limit
                                 <1
mg/L
                                                      407A
07-10-01 WMB
Wilson Environmental Laboratories, Inc.
W. Martin Bell

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                           Page 8 of 11
                                   Lab Number: WE10865-8

                              PROJECT: TO26 G466507-UC41
SAMPLE DESCRIPTION

8 Hg

CONSTITUENT

Chloride
    REPORT OF ANALYTICAL RESULTS

     MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

     Aqueous   J. ICKES              26 JUN 01 02 JUL 01

RESULT      *D.L.   UNITS    METHOD   ANALYZED  BY NOTES

       <1      1   mg/L     407A      07-10-01 WMB
    * Detection Limit
Wilson Environmental Laboratories, Inc.
W. Martin Bell

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                           Page 9 of 11
                                   Lab Number: WE10865-9

                              PROJECT: TO26 G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

9 Hg                           Aqueous   J. ICKES              26 JUN 01 02 JUL 01
CONSTITUENT

Chloride

    * Detection Limit
RESULT
            *D.L.   UNITS    METHOD   ANALYZED  BY NOTES

               1   mg/L     407A      07-10-01 WMB
Wilson Environmental Laboratories, Inc.
W. Martin Bell

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OHIO 43201-2693
                                           Page 10 of 11
                                  Lab Number: WE10865-10

                              PROJECT: T026 G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

10 Hg                          Aqueous   J. ICKES              27 JUN 01 02 JUL 01
CONSTITUENT

Chloride

    * Detection Limit
RESULT
            *D.L.   UNITS    METHOD   ANALYZED  BY NOTES

               1   mg/L     407A      07-10-01 WMB
Wilson Environmental Laboratories, Inc.
W. Martin Bell

-------
MS. JENNIFER ICKES
BATTELLE MEMORIAL INSTITUTE
505 KING AVENUE
COLUMBUS,OH10 43201-2693
                                                                     Page 11 of 11
                                                            Lab Number: WE10865-11

                                                        PROJECT: TO26 G466507-UC41
                              REPORT OF ANALYTICAL RESULTS

SAMPLE DESCRIPTION             MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

                               Aqueous   J. ICKES              28 JUN 01 02 JUL 01
11 Hg

CONSTITUENT

Chloride

    * Detection Limit
                          RESULT      *D.L.   UNITS    METHOD   ANALYZED  BY NOTES

                             1           1   mg/L     407A      07-10-01 WMB
Wilson Environmental Laboratories, Inc.
W. Martin Bell

-------
FROM :  UILSON ENUIRONMENTAL LABS
                                    PHONE NO.
                                                                         flug.  09 2001  12:00PM P2
           WILSON
           ENVIRONMENTAL LABORATORIES. IMC.
   MS.  JENNIFER  ICKES
   BATXBLLE MEMORIAL INSTITUTE
   505  KING AVENUE
   COLUMBUS,OHIO 43201-2693
                                          40; Ventun Drive • Suite C • Westervie, Ohio 43091 • (614) 431-0010 • Fax: (614) 431-16SO
                                                                         Page 1  of  4
                                                                Lab Number: WE10902-1

                                                                        PROJECT:  TO 26
                                  REPORT OF ANALYTICAL RESULTS

   SAMPLE DESCRIPTION              MATRIX    SAMPLED  BY    SAMPLED DATE/TIME  RECEIVED
   =======================:;=====  ========= =========3==== sssssaasaasassssssss aassasssa
   14.Hg                            Aqueous   J.  ICKES              30  JUL 01 31 JUL 01
                          ========  ========= ============= ===========:==:===:= =========
                              RESULT      *D.L.   UNITS    METHOD    ANALYZED  BY NOTES
===================;
CONSTITUENT
   Chloride

       * Detection  Limit
                                                rog/L
407A
08-17-01  MWB
   Wilson Environmental Laboratories, Inc.
   W. Martin  Bell

-------
                                   rnunc rsu.
                                                                   Hug.
MS. JENNIFER ICKBS
BATTELLE MEMORIAL INSTITUTE
505 KINO AVBNXIB
COLUMBUS,OHIO 43201-2693
                                                                      Page 2 of 4
                                                              Lab Number: WE10902-2

                                                                     PROJECT: 10 26
                              REPORT OF ANALYTICAL  RESULTS

                               MATRIX     SAMPLED  BY    SAMPLED DATE/TIME  RECEIVED
                             = ======:=:=:=  asssesaaassssa ================= ========
                               Aqueous    J.  ICKES              30 JUL 01 31 JUL 01
           ====»==:====!======== =========  ============= ================= =========
CONSTITUENT               RESULT      *D.L.    UNITS    METHOD   ANALYZED  BY NOTES
SAMPLE DESCRIPTION
======
15. Hg
Chloride

    * Detection Limit
                                             mg/L
407A
08-17-01 MWB
Wilson Environmental Laboratories, Inc.
W. Martin Bell

-------
FROM :  UIILSON ENUIRONMENTPL LflBS
        PHONE NO.
flug.  09 2001  12:01PM P4
  MS. JENNIFER  ICKES
  BATTELLE  MEMORIAL INSTITUTE
  505 XING  AVENUE
  COLUMBUS,OHIO 43201-2693
                                           Page  3 of  4
                                   Lab Number: WB10902-3

                                          PROJECT: TO 26
   SAMPLE DESCRIPTION

   16.Hg
   ===================:===:=
   CONSTITUENT
    REPORT OF ANALYTICAL RESULTS

     MATRIX    SAMPLED BY    SAMPLED DATE/TIME   RECEIVED

     Aqueous   J. ICKES              30 JUL  01  31 JUL 01

RESULT      *D.L.   UNITS    METHOD   ANALYZED   BY NOTES

   6           1   mg/L     407A      08-17-01  MWB
   Chloride

       * Detection Limit
   Wilson Environmental Laboratories,  Inc.
   W. Martin Bell

-------
rrsun .  wii_=>un enviMjlNnsm HL LHSb
                                     PHONE NO.  :
                    flug.  09 2001  12:01PM P5
   MS.  JENNIFER ICKES
   BATTELLE MEMORIAL INSTITUTE
   SOS  KING AVENUE
   COLUMBUS,OHIO 43201-2693
                       Page  4  of  4
               Lab Number; WE10902-4

                      PROJECT: TO 26
   SAMPLE DESCRIPTION
   ==================:
   18. Hg
   CONSTITUENT

   Chloride

       * Detection Limit
    REPORT OP ANALYTICAL RESULTS

     MATRIX    SAMPLED BY    SAMPLED DATE/TIME  RECEIVED

     Aqueous   J. ICKES

RESULT      *D.L.

   2           1   mg/L     407A       08-17-01 MWB
                 30 JUL 01  31  JUL 01
======== =================  =========
UNITS    METHOD   ANALYZED   BY NOTES
   Wilson Environmental Laboratories,  Inc.
   V). Martin Bell

-------
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-------
     WILSON
     ENVIRONMENTAL LABORATORIES, INC.
                                                                            AOL
                                    __ _  _

                                    401 Venture Drive • Suite C • Westervil/e, Ohio 43081 • (614) 431-0010 • Fax: (614) 431- 1650
  August 24, 2001


  Ms. Jennifer Ickes
  Battelle Memorial Institute
  505 King Avenue
  Columbus, Ohio 43201


  RE: QC Report - Project T026 G466507-UCC41

  Dear Ms. Ickes,
WE10685


WE10711


WE10865


WE10902
                   Alkalinity and Acidity


                   Alkalinity and Acidity

                   Total Chloride


                   Total Chloride
 Alkaline Inn A^Jf P°rt ^flects' standard Quality control procedures for the
 Akahmty and Acidity analyses included  a laboratory  control  sample  method
 blank and duplicate analysis.   Matrix spike and  matrix spike dupLTe QC
 samples were not included.  The Total Chloride runs included the ma n? spikes

                            addition <
    s
assistance pertaining to this QC report.

Sincerely,
WILSON ENVIRONMENTAL LABORATORIES, INC.
encl

-------
                             WILSON ENVIRONMENTAL LABORATORIES, INC.
                               401 Venture Drive, Suite C • Westerville, Ohio 43081
                                   Phone: (614) 431-0010 • FAX: (614) 431-1650
 Battelle Memorial Institute
 505 King Avenue
 Columbus, Ohio 43201

 Project: TO26 G466507-UC41
                                  Order No.: WE10685
                                          WE10711
                                   QC Report

                         Laboratory Control Sample (LCS)
Alkalinity, Total
Acidity, Total
4/19/01
4/19/01
39
37.69
                    mg/L
103
                                 Pagel

-------
Battelle Memorial Institute
505 King Avenue
Columbus, Ohio 43201
                       WILSON ENVIRONMENTAL LABORATORIES, INC.
                        401 Venture Drive, Suite C • Westerville, Ohio 43081
                             Phone: (614) 431-0010 • FAX:  (614) 431-1650
       Order No. ;WE10685
               WE10711
Project: TO26 G466507-UC41
                          Method Blank Report
                  Parameter    Analysis Date    Result
                  Alkalinity, Total
                  Acidity, Total

                  Alkalinity, Total
                  Acidity, Total
4/10/01
4/10/01

4/19/01
4/19/01
mg/L
mg/L

mg/L
mg/L
                          Page 2

-------
 Battelle Memorial Institute
 505 King Avenue
 Columbus, Ohio 43201

 Project: TO26 G466507-UC41
                                   WILSON ENVIRONMENTAL LABORATORIES, INC.
                                    401 Venture Drive, Suite C •  Westerville, Ohio 43081
                                         Phone:  (614) 431-0010-FAX:  (614)  431-1650
                                                 Order No.: WE10685
                                                          WE10711
                                                QC Report
Parameter
Alkalinity, Total
Acidity, Total

Alkalinity, Total
Acidity, Total
                                         Sample Duplicate Report
 Analysis Date   Duplicate Result
ss&E&ssssxssssttssttasssattssssssa&ssai^sssassssssttStt
        4/10/01         205
        4/10/01        1050
        4/19/01
        4/19/01
18
17
19
17
5
0
                                       Pages

-------
Battelle Memorial Institute
505 King Avenue
Columbus, Ohio 43201

Project: TO26 G466507-UC41
                            WILSON ENVIRONMENTAL LABORATORIES, INC.
                             401 Venture Drive, Suite C •  Westerville, Ohio 43081
                                 Phone: (614) 431-0010 • FAX:  (614) 431-1650
Order No: WE10865
       WE10902
                                QC Report

                       Laboratory Control Sample (LCS)
                               Page 1

-------
Battelle Memorial Institute
505 King Avenue
Columbus, Ohio 43201

Project: TO26 G466507-UC41
                               WILSON ENVIRONMENTAL LABORATORIES, INC.
                                401 Venture Drive, Suite C • Westerville, Ohio 43081
                                     Phone: (614) 431-0010 • FAX: (614) 431-1650
                      Order No: WE10865
                              WE10902
                                   Matrix Spike Report
Parameter
Chloride, Total
Sample Amount
     is
     32
Analysis Date
   7/10/01
   8/17/01
                                  Page 2

-------
                          WILSON ENVIRONMENTAL LABORATORIES, INC.
                            401 Venture Drive, Suite C • Westerville, Ohio 43081
                                Phone: (614) 431-0010 • FAX:  (614) 431-1650
Battelle Memorial Institute
505 King Avenue
Columbus, Ohio 43201

Project: TO26 G466507-UC41
Order No: WE10865
       WE10902
                       Matrix Spike Duplicate Report
                              PageS

-------
                          WILSON ENVIRONMENTAL LABORATORIES, INC.
                            401 Venture Drive, Suite C • Westerville, Ohio 43081
                                Phone: (614) 431-0010 - FAX:  (614) 431-1650
Battofle Memonal Instrtute                                Order No: WE10865
505 King Avenue                                              WE10902
Columbus, Ohio 43201                                          vvciuyu^

Project: TO26 G466507-UC41

                          Method Blank Report


                 Parameter    Analysis Date   Result
                 Chloride, Total      7/10/01     <1 mg/L
                                 8/17/01     <1 mg/L
                             Page 4

-------
                             WILSON ENVIRONMENTAL LABORATORIES, INC.
                              401 Venture Drive, Suite C • Westerville, Ohio 43081
                                   Phone: (614) 431-0010 • FAX: (614) 431-1650
Battelle Memorial Institute
505 King Avenue
Columbus, Ohio 43201

Project: TO26 G466507-UC41
                                          Order No: WE10865
                                                 WE10902
                                      QC Report
                               Sample Duplicate Report
Parameter    Analysis Date
Chloride, Total
7/10/01
8/17/01
Duplicate Result
      15
      32
                                             Sample Result
                                                  15
                                                  32
                                Pages

-------
                          APPENDIX D




LABORATORY REPORTED DATA FOR SULFUR BANK MERCURY MINE WASTE ORE

-------
Solid Mercury Ore
              Project ID: G466507-UC61
                   Date: 8/29/01
Analyst: c. BURTON
Sample ID
Mercury Waste Rock TOC



Mercury Waste Rock TC


Date
8/29/01



8/29/01


Weight mg
42.86
32.22
33.76

24.42
30.97
42.83
ugof C
193.59
140.39
143.18

120.69
141.01
183.14
%c
0.452
0.436
0.424

0.494
0.455
0.428
Average


0.437



0.459
%RSD


3.17



729
                           Project ID: G466507-UC61
                                Date:    8/29/01
        Analyst: C. BURTON
                           Calibration Check Standards
Time
13:30
14:45
Calcium
Carbonate (mg)
16.69
17.12
12.89
18.23
15.13
14.27
Theoretical fig
of C
2002.83
2054.43
1546.83
2187.64
1815.63
1712.43
Actual u,g
ofC
1972.37
1956.75
1544.02
2144.55
1693.42
1707.30
% Error
1.521
4.755
0.181
1.970
6.731
0.299
Average %
Error
2.152
3.000

-------
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-------
RESULTS MERCURY
Solid Mercury Ore Analysis

Project #
Title
Samples Received
Samples Analyzed
Results Reported
Method Used
                            G466507-UC41
                            Mercury Leaching
                                        8/24/01
                                        9/6/01
                                        9/7/01
                            EPA Method 7471A
SAMPLE I.D.
1 HG
1 HG-DUP
Concentration of mercury
(ug/ g)
3125
3125
 * results based on sample weight of 0.32g into volume of 5 mL
Project #
Title
Samples Received
Samples Analyzed
Results Reported
Method Used
                            G466507-UC41
                            Mercury Leaching
                                       8/24/01
                                        9/6/01
                                        9/7/01
                            EPA Method 7471A
                  SAMPLE I.D.
                                                    Hq
CCVIOppb
                                                         10.0
G6V Percemiiigavery
                                                        100%
1 HG
                                                         20.0
1 HG-DUPLICATE
                                                         20.0
 CCVIOpb
                                                         10.0
                                                        100%
                                                          8.0
CCVIOppb
                                                          8.0
ER Hg 9-6-01
                                       9/14/01 2:17PM

-------
Project #
Title
Samples Received
Samples Analyzed
Results Reported
Method Used
G466507-UC41
Mercury Leaching
               8/24/01
                9/6/01
                9/7/01
U.S. EPA Method 3050
METHOD BLANK

Friday                              September 07
Sample
c:\elandata\dataset\er 9-6-01 totalquant\Blank.012
                                1
Average
Average
Dual
                               35
                               35
                                1
C:\elandata\Sample\CDC SOILS 9-07-01 .sam
C:\elandata\Method\TotalQuant.mth
c:\elandata\dataset\er9-6-01 totalquant\METHOD BLANK.014
default.tun
default.dac
c:\elandata\System\current.rsp
                       2001 11:22:35
Analyte
H
He
Li
Be
B
C
N
O
F
Ne
Na
Mg
Al
Si
P
S
Cl
Ar
K
Ca
Sc
Ti
V
Cr
Mn
Fe
Co
Concentration (mg/L)


0.00002
0.0001
0.00318
0
129744.8458



0.03186
0.009
0.01076
0.0197
0.02919
42.31853
0

0.0027
0
0.0004
0.0008
0.00016
0.00031
0.00058
0.08423
0.00005
Intensity


29
51
5815
0
13496167

0
0
470522
40856
92221
246760
38264
17936083
0
0
28122
0
5528
9051
1698
3473
8374
1092652
587
Intensity Units
Not Measured
Not Measured





Not Measured




















-------
Analyte
Ni
Cu
Zn
Ga
Ge
As
Se
Br
Kr
Rb
Sr
y
Zr
Nb
Mo
Ru
Rh
Pd
Ag
Cd
In
Sn
Sb
Te
1
Xe
Cs
Ba
La
Ce
Pr
Nd
Sm
Eu
Gd
Tb
Dy
Ho
Er
Tm
Yb
_u
Hf
Ta
W
Re
Os
Ir
Pt
Au
Hq
Tl
Pb
Bi
Th
U
Concentration (mg/L) (Intensity | Intensity Units
0.00039
0.0005
0.00338
0.00001
0.00001
0.0003
0
0.00264

0.00001
0.00069
0.00002
0.00635
0.00001
0.00136
0
0
0
0.00013
0
0.01222
0.01524
0.00022
0
0.00001

0
0.00094
0.00001
0.00004
0
0.00001
0
0
0
0.00139
0
0
0
0
0
0.00002
0.00002
0
0.00035
0
0
0
0
0.00005
0.00015
0
0.00417
0.00002
0.00004
0.00009
2898
3373
12498
93
64
314
0
607
0
167
8114
211
82096
61
12879
0
0
0
990
0
76180
98882
874
0
121
0
7
8731
94
573
27
111
50
0
14
30082
27
7
0
0
19
428
388
24
8335
0
0
0
0
333
984
10
94139
424
471
1231

























































-------
1 HG
Friday                              September 07
Sample
c:\elandata\dataset\er 9-6-01 totalquant\Blank.012
                                 1
Average
Average
Dual
                                35
                                35
                                 1
C:\elandata\Sample\CDC SOILS 9-07-01 .sam
C:\elandata\Method\TotalQuant.mth
c:\elandata\dataset\er9-6-01 totalquantM HG.015
default.tun
default.dac
c:\elandata\System\current.rsp
2001 11:27:24
Analyte
H
He
Li
Be
B
C
N
O
F
Ne
Na
Mg
Al
Si
P
S
Cl
Ar
K
Ca
Sc
Ti
V
Cr
Mn
Fe
Co
Ni
Cu
Zn
Ga
Ge
As
Se
Br
Kr
Rb
Concentration (mg/L) | Intensity


0.00105
0.00012
0.0051
0.41934
118864.4815



0.48039
0.71365
3.908
3.18869
0.10623
28.33976
0

2.22665
0
0.01179
5.02087
0.04579
0.02517
0.03387
12.04184
0.00534
0.00349
0.0451
0.03495
0.0152
0.00069
0.05787
0
0.02607

0.02257


1462
57
9337
398082
12364382

0
0
7094953
324071 1
33493416
39934174
139261
12011390
0
0
23222299
0
163474
56619073
499690
279546
486015
156214499
59250
25880
307205
129386
124086
4598
60977
0
5997
0
268635
Intensity Units
Not Measured
Not Measured





Not Measured






























-------
Analyte
Sr
V
Zr
Nb
Mo
Ru
Rh
Pd
Ag
Cd
In
Sn
Sb
Fe

Xe
Cs
Ba
La
Ce
Pr
Nd
Sm
Eu
Gd
Tb
Dy
Ho
Er
Tm
Yb
Lu
Hf
Ta
W
Re
Os
Ir
Pt
Au
Hg
Tl
Pb
Bi
Th
U
Concentration (mg/L) | Intensity | Intensity Units
0.52803
0.00631
0.31658
0.00127
0.00187
0
0.00004
0.00085
0.00107
0.00026
0.00077
0.03348
0.04187
0.00009
0.00091

0.00378
24.94128
0.02789
0.02821
0.00317
0.00931
0.00156
0.00297
0.00148
0.00023
0.00118
0.0002
0.00062
0.00009
0.00062
0.00009
0.00808
0.00004
0.00031
0
0
0
0.00007
0.00008
0.1133
0.00299
0.54435
0.00155
0.01245
0.00737
6231008
82408
4093259
13987
17632
27
287
6104
8221
1311
4783
217291
162883
137
8406
0
36634
231541784
336200
382986
40705
143771
28773
53031
29830
4928
24486
4801
14635
2077
13951
2242
206540
864
7423
6
0
54
1075
579
749351
72162
12292449
27387
162372
102838















































-------
1 HG-DUP
Friday                             September 07
Sample
c:\elandata\dataset\er 9-6-01 totalquant\Blank.012
                                 1
Average
Average
Dual
                                35
                                35
                                 1
C:\elandata\Sample\CDC SOILS 9-07-01 .sam
C:\elandata\Method\TotalQuant.mth
c:\elandata\dataset\er9-6-01 totalquantM HG-DUP.016
default.tun
default.dac
c:\elandata\System\current.rsp
2001 11:33:22
Analyte
H
He
Li
Be
B
C
N
O
F
Ne
Na
Mg
Al
Si
P
S
Cl
Ar
K
Ca
Sc
Ti
V
Cr
Mn
Fe
Co
Ni
Cu
Zn
Ga
Ge
As
Se
Br
Kr
Concentration (mg/L)


0.00119
0.00019
0.00611
0.42052
114931.4738



0.45353
0.79725
3.91865
3.4684
0.10196
22.22825
0

2.55835
0
0.01219
5.33539
0.04971
0.02641
0.04026
11.7318
0.00531
0.00358
0.04284
0.03755
0.01609
0.00082
0.05886
0
0

Intensity | Intensity Units


1653
91
11191
399202
11955267

0
0
6698295
3620344
33584654
43437118
133675
9421117
0
0
26681734
0
169072
60165841
542560
293287
577690
152192522
58878
26503
291772
139024
131393
5465
62022
0
0
0
Not Measured
Not Measured





Not Measured





























-------
Anaiyte Concentration (mg/L)
Rb
Sr
Y
Zr
Nb
Mo
Ru
Rh
Pd
Ag
Cd
In
Sn
Sb
fe
1
Xe
Cs
Ba
La
Ce
Pr
Nd
Sm
Eu
Gd
Tb
Dy
Ho
Er
Tm
Yb
Lu
Hf
Ta
W
Re
Os
Ir
Pt
Au
Hg
Tl
Pb
Bi
Th
U
0.02109
0.53985
0.00694
0.34172
0.00114
0
0
0.00003
0.00078
0.00063
0.00046
0.00037
0.03321
0.03829
0.00002
0.00105

0.00383
25.97077
0.02884
0.03048
0.00351
0.01005
0.0017
0.00286
0.00159
0.00023
0.00139
0.00025
0.00066
0.0001
0.00067
0.00009
0.00847
0.00005
0.00026
0
0
0
0.00009
0.00007
0.14052
0.0031
0.49236
0.00149
0.01295
0.0082
Intensity | Intensity Units
251052
6370492
90617
4418355
12556
0
0
234
5564
4802
2339
2336
215531
148933
36
9677
0
37152
241099021
347696
413828
45092
155266
31335
51139
31987
4958
28908
6038
15578
2481
15111
2389
216664
1044
6085
16
0
9
1292
492
929416
74734
11118357
26375
168890
114419
















































-------
      APPENDIX E




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