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This is to certify that the

thesis entitled

Partitioning of Trace Metals in
Glacial Till, Southern Michigan

presented by

Lynn G. Anderson

has been accepted towards fulfillment
of the requirements for

Masters Geology

degree in

 

 

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0-7639 MS U is an Affirmative Action/Equal Opportunity Institution

 

MSU

 

 

 

RETURNING MATERIALS:
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@889 1

 

 

PARTITIONING OF TRACE METALS IN GLACIAL TILL
SOUTHERN MICHIGAN

By

Lynn G. Anderson

A THESIS

Submitted to
Michigan State University
in partial fulfillment of the requirements
for the degree of

MASTER OF SCIENCE

Department of Geological Sciences

1986

J

W7. m

ABSTRACT

PARTITIONING OF TRACE METALS IN GLACIAL TILL
SOUTHERN MICHIGAN

By

Lynn G. Anderson

Tills associated with three late Wisconsinan ice lobes
(Lake Michigan, Saginaw, and .Huron/Erie) in southern
Michigan were analyzed to determine their CU, Ni, Zn, Sr,
Cr, and Pb concentrations in the bulk, residual, and
non-residual phases. The Cu, Ni, Zn, and Sr trace metal
concentrations in the residual phase were used to
differentiate tills from different ice lobes.
Specifically: I) The Lake Michigan lobe tills have
relatively low concentrations of Cu, Ni, Zn, and Sr. 2)
The Huron/Erie lobe tills have relatively high
concentrations of Cu, Ni, Zn, and Sr. 3) The Saginaw lobe
tills have Cu, Ni, Zn, and Sr concentrations intermediate
between those of the Lake Michigan and Huron/Erie lobe
tills. The most likely factor that controls the trace
metal concentrations in the residual phase of the till
sampled from each lobe is the geochemistry of the source

region.

To My Mother

ii

ACKNOWLEDGMENTS

I would like to express my thanks and appreciation to
my thesis advisor and friend, Dr. Grahame J. Larson, and to
my friend, Bill Monaghan; whose support and endeavor made
it possible for me to complete this research. I would also
like to thank my committee members, Dr. James Trow and Dr.
David Long for their help and advice. I will always
remember the support and love given to me by my father and
my wife, without which, none of this would have been

possible.

iii

TABLE OF CONTENTS

INTRODUCTION . . . . . . . . . . . . . .
SAMPLE LOCATION . . . . . . . . . . . .
PARTITIONING OF TRACE METALS . . . . . .
ANALYTICAL PROCEDURE . . . . . . . . . .
RESULTS . . . . . . . . . . . . . . . .

TRACE ELEMENT CONCENTRATIONS IN THE LAKE
SAGINAW, AND HURON/ERIE LOBES .

DISCUSSION . . . . . . . . . . . . . . .
CONCLUSIONS . . . . . . . . . . . . . .
APPENDIX A . . . . . . . . . . . . . . .
Preliminary Research . . . . . . .
APPENDIX B . . . . . . . . . . . . . . .
Experimental Procedures . . . . . .
APPENDIX C . . . . . . . . . . . . . . .
Results of Analysis . . . . . . . .
APPENDIX D . . . . . . . . . . . . . . .
Sample Averages . . . . . . . . . .
APPENDIX E . . . . . . . . . . . . . . .
Clay Analyses . . . . . . . . . . .
BIBLIOGRAPHY . . . . . . . . . . . . . .

iv

MICHIGAN

\Im-L’J‘:

12
19
19
22
23
25
25
29
29
36
36
Lu
in

43

Table 1:

Table 2:

LIST OF TABLES

Average Cu, Zn, Sr, Ni, Pb, and Cr
concentrations for the exchangeable,
carbonate, and Fe-Mn oxide; organic;
bulk; and residual phases in Michigan
tills (< 0.038 mm size fraction) . . . .

Average Cu, Zn, Sr, Ni, Pb, and Cr
concentrations for the exchangeable,
carbonate, and Fe-Mn oxide; organic;
bulk; and residual phases with respect
to individual ice lobes (< 0.038 mm size
fraction) . . . . . . . . . . . . . . .

10

'14

LIST OF FIGURES

Figure 1: Sample locations. . . . . .

. . . . . . . . 3

Figure 2: Histograms showing residual
concentrations of Cu, Ni, Zn, and Sr
with respect to individual ice lobes. . . . 16

Figure 3: Ratio of clay to medium + fine silts vs.
residual Cu, Ni, Zn, and Sr
concentrations. . . . . . . . . . . . . . . 18

vi

INTRODUCTION

In areas adjacent to southern Michigan trace-metal
content has proved useful for differentiating tills. For
example, Forslev (1957) analyzed unleached samples of late
Wisconsinan tills deposited by the Des Moines, Lake
Michigan, Saginaw, and Erie lobes in Iowa, Illinois and
Indiana and found that the Des Moines Lobe tills contain
more Zr, Ba, and Mn, and less. Sc than the others; Lake
Michigan Lobe tills contain more Ti and Al and less Sr;
Saginaw and Erie Lobe tills have more Ca and Sr; and Erie
Lobe tills contain more V. Likewise, May and Dreimanis
(1973) were able to differentiate on the basis of
trace-metal content tills from different ice lobes in
southern Onterio. Specifically, they found that the
Erie-Ontario Lobe tills are distinguished from
Huron-Georgian Bay Lobe tills by a higher content of Ni,

Cu, Zn, and Cr.

The goals of the research presented in this paper are:
l) to determine the concentration of trace metals within
till from the Huron/Erie, Saginaw, and Lake Michigan ice

lobes in southern Michigan, 2) to determine if trace—metal

Figure 1

Sample locations.

 

 

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content can be used to distinguish between tills from
different lobes, and 3) to speculate as to the sources of

the trace metals.
SAMPLE LOCATION

A total of 18 till samples, 6 associated with the Lake
Michigan Lobe, 6 associated with the Saginaw Lobe, and 6
associated with the Huron-Erie Lobe were collected from
exposures in moraines and till plains within the southern
half of the lower peninsula of Michigan. These samples of
unleached till were obtained from road cuts and natural
exposures and were taken at least 2.0 m below the ground
surface. The locations of the samples and the moraines
from which they were collected are shown in Figure 1. The
age of the moraines are believed to be between 15,000 and

13,000 y.b.p. (Farrand and Eschman, 197A).
PARTITIONING OF TRACE METALS

Although numerous investigations have focused on trace
metal content of till (Forslev 1957; May and Dreimanis,
1973; Newton 1977; Barnett 1982; Brand 1983; Shilts 1973,
1975, 1978, 1981; Pawluk and Bayrock 1969), there is no
universal agreement as to which size fraction (clay, silt,
or sand) or chemical phase (bulk, hydromorphic, or
residual) should be analysed. For example, Pilch (1970)

analysed the bulk chemistry of glacial soils in New

Brunswick and showed that the highest concentration of
anomolous Cu and Zn is generally associated with the (0.062
mm (silt and clay) fraction. Kauranne et al. (1977), on
the other hand, analyzed the bulk chemistry of three
selected size fractions in Finnish glacial soils for Co,
Cr, Cu, Ni, and Zn and showed that the highest
concentration of these metals occur in the <0.060 mm
fraction. In studies related to unweathered till from the
Northwest Territories, however, Dilabio (1979) determined
that the highest concentration of Cu, Pb, and U is
associated with the <0.002 mm (clay) fraction. Pawluk and
Bayrock (1969) likewise found that the elements Fe, E, Co,
Cu, Zn, and Mb in unweathered tills from Alberta are

principally associated with the <0.002 mm fraction.

Studies involving the geochemistry of tills have also
shown that trace metals are chemically partitioned into
different chemical phases. For example, Dilabio (1979)

showed that Cu and U in till from the Northwest Territories

are concentrated within the hydromorphic phase
(phyllosilicates, Fe and Mn oxides, and hydroxides) and
that this phase acts as a scavenger for base metals.
Partitioning of trace metals into separate chemical phases
has also been recognized by Bradshaw et al. (197A) for
soils developed on tills in the Northwest Territories.

Because a large proportion of trace metals are thought to

be associated with phases other than the residual, it is
desirable to extract these trace metals so that the
remaining lithic or residual trace metal concentrations may
be determined and information regarding the origin and mode

of occurrence may be obtained (Tessier et al, 1979).
ANALYTICAL PROCEDURE

Despite the fact that the reasons and methods of
investigation generally vary from study to study, it is
clear from the preceding investigations that maximum
trace-element concentrations tend to occur in the finer
fractions of till and associated soils and that trace
elements are partitioned into various chemical phases. In
this study the choice of (0.038 mm (med. silt-clay)
fraction was made after a preliminary semiquantitative
investigation of several till samples from southern
Michigan showed that this size fraction yielded the highest
bulk concentrations of Cu, Zn, and Sr compared to the
0.25-0.062 mm (fine and very fine sand) and 0.062-0.038 mm

(course silt) fractions (see Appendix A).

The part of the till which is of non-residual origin
includes trace metals associated with exchangeables,
carbonates, Fe-Mn oxides, and organic matter (Gupta and
Chen, 1975). The part of the till associated with the

residual phase is of lithogenous origin (lattice held) and

consists of trace metals associated with silicate minerals
and the fraction of trace metals incorporated in the clay
minerals, but excluding adsorbed species (Gupta and Chen,
1975). The chemical characteristics of each phase and the
number of fractions to be studied determines the choice of
extraction reagents to be used. Each phase may be
extracted individually or they may be grouped together,

depending on the scope of the study (Tessier et a1, 1979).

Trace metals associated with exchangeables,
carbonates, and Fe-Mn oxides were extracted by subjecting
the sample to an acid-reducing agent (Chester and Hughes,
1967). The organic fraction of the hydromorphic phase was
extracted by oxidizing the sample in an strong base (Gupta
and Chen, 1975). Lastly, the residual phase as well as the
bulk sample were prepared for analysis using a lithium
metaborate fusion procedure (Perkin-Elmer 1973). The
resultant solutions obtained from the leaches and fusions

were analyzed using atomic absorption spectrOphotometry

(see Appendix B).
RESULTS

The results of the selective chemical attacks on the
till samples collected from southern Michigan are presented
in Table 1 and Appendix C and D. Included in the table are

the average concentrations in ppm for Cu, Zn, Sr, Ni, Pb,

and Cr in the bulk, hydromorphic (exchangeable, carbonate,
Fe-MN oxide, and organic) and residual phases. In general,
the sum of trace metals extracted in the individual
successive chemical attacks plus the residual show a close
agreement with the total trace metals measured in the bulk

samples (within 10%).

COpper: The total concentration of Cu in the till
samples varies between 92 and 155 ppm and averages
about 116 ppm. Of this between 30 and 71% of the
total Cu in associated with the non-residual; The
percentage of non-residual Cu in the organic fraction

is between 3 and 15%.

Zinc: The total Zn content in the till samples ranges
from 111 to 193 ppm and averages 1A8 ppm. Between 10
and 54% of the total Zn is non-residual in nature and
from 14 to 52% of the non-residual Zn is associated

with the ogranic fraction.

Strontium: The total Sr concentration in the till
varies between 24 and 57 ppm and averages about 43
ppm. Of this between 7 and 37% of the total Sr is
non-residual in nature. Between 0 and 70% of the
non-residual Sr is associated with the organic

fraction.

Table 1

Average Cu, Zn, Sr, Ni, Pb, and Cr concentrations for

the exchangeable, carbonate,

bulk;

and Fe-Mn oxide; organic;

and residual phases in Michigan tills (< 0.038

mm size fraction).

 

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10

Nickel: The total Ni content in the till samples
varies from 89 to 133 ppm and averages about 108 ppm.
Approximately 6 to 21% of the total N1 is non residual
and between 17 to 6A% of this fraction is incorporated

into the organic fraction.

Lead: The total Pb content in the till samples varies
from 323 to 390 ppm and averages about 350 ppm.
Between 5 to 15% of the total Pb is of non-residual
origin, and between 22 and A1% of the non-residual Pb

is associated with the organic fraction.

Chromium: The total Cr concentration in the till
varies between 53 and 65 ppm and averages 58 ppm. Of
this between 3 and 13% of the total Cr is non-residual
in nature. Between AA and 97% of the non-residual Cr

is associated with the organic fraction.

Generally, the order of abundance of trace metals in

the till samples is: Pb>Zn>Cu>Ni>Cr>Sr. With the exception

of Cu, most of the trace metals appear to be associated
with the residual phase; The order of abundance in this

phase tends to be: Pb>Zn>Ni>Cu>Cr>Sr.

In the hydromorphic phase, on the other hand, the bulk
of the trace metals appear to be tied up with the
exchangeable, carbonate, and Fe-Mn oxide fraction.

However, Cr seems to be an exception. In general, the

11

order of abundance of trace metal in the exchangeable,
carbonate, and Fe-Mn oxide fraction is: Cu>Zn>Pb>Ni>Sr>Cr.
In the organic fraction of the hydromorphic phase the order

of abundance is: Zn>Cu>Pb>Ni>Cr>Sr.

TRACE ELEMENT CONCENTRATIONS IN THE LAKE

MICHIGAN,SAGINAW, AND HURON/ERIE LOBES

The trace metal content in the bulk, hydromorphic, and
residual phases of till samples collected from the Lake
Michigan, Saginaw, and Huron/Erie ice lobes are shown in
Table 2. ' From this data it is apparent that trace metal
concentrations within the hydromorphic and bulk fractions
cannot be used to differentiate tills of different lobes.
However, tills can be differentiated on the basis of their
trace metal concentrations within the residual phase. For
example, the Lake Michigan lobe is characterized by
relatively low concentrations of Cu, Ni, Zn, and Sr whereas
the Huron/Erie lobe is characterized by rather high
concentrations of Cu, Ni, Zn, and Sr. The Saginaw lobe
generally has Cu, Ni, Zn, and Sr concentrations
intermediate between those of the Lake Michigan and
Huron/Erie lobes. These differences in the geochemistry of
the lobes are graphically represented in Figure 2. Pb and
Cr show little variation between the lobes and are

therefore not included in Figure 2.

12

 

Inn

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an

0.I

Table 2
Average Cu, Zn, Sr, Ni, Pb, and Cr concentrations for the
exchangeable, carbonate, and Fe-Mn oxide; organic; bulk;

and residual phases with respect to individual ice lobes (<
0.038 mm size fraction).

13

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Fraction Cu Zn Sr Ni Pb Cr
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RP .
g on Organic x 11.0 18.9 1.2 5.0 8.7 2.6
1
lo c Sx 8.5 15.8 1.8 3.6 4.1 1.2
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o
B Total x 107.7 151.9 35.3 109.7 326.0 53.9
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o Sx 14.0 28.7 7.7 11.2 11.3 3.4
B
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(”m") 3x 19.1 20.9 7.7 12.8 13.1 2.3
an Exchang x 44.8 19.0 2.2 7.7 17.9 1.6
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(15 x 68.4 133.4 45.9 106.1 329.0 54.4
B Residual
E 3,, 6.6 14.9 6.7 7.0 13.4 3.9
’ x 111.4 152.0 47.5 120.6 338.0 53.3
Total
(Bulk) 3,, 12.4 11.3 9.9 4.0 12.9 3.4

 

l4

 

Figure 2
Histograms showing residual concentrations of Cu, Ni, Zn,

and Sr with respect to individual ice lobes.

15

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Zn, and Sr concentrations.

17

 

 

 

 

 

 

 

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18

DISCUSSION

There are two possible explanations that might account
for the observed differences in trace metal concentrations
within the residual phase of till samples collected from
the Lake Michigan, Saginaw, and Huron/Erie lobe. The first
is that trace metals concentration within the (0.038 mm
size fraction is controlled by the ratio of clay to medium
and fine silt in each lobe (Shilts 1971, 1975). The second
is that the source region or provenance of each lobe has a
distinct trace metal geochemistry and that this

geochemistry is reflected in the till derived from these

regions.

To determine if the amount of clay in each sample
significantly affects the trace metal concentration within
the residual phase, the < 0.038 mm size fraction of each
till sample was analyzed for clay and silt using a pipet
technique (Guy, 1969). The ratio of clay to medium and
fine silt within each sample (Appendix E) was then compared
to the measured trace metal concentration recorded in each
sample. These analyses are presented in Figure 3 and
clearly shows that there is no obvious relationship between
the sample texture and trace metal content. It also
suggests that the difference in trace metal content within
the residual phase of till must be a function of the lithic

composition of the till; in other words, it must be a

19

function of the geochemistry of the source area.
CONCLUSIONS

A total of 18 till samples, 6 from the Lake Michigan
lobe, 6 from the Saginaw lobe, and 6 from the Huron/Erie
lobe were collected from eXposures in moraines and till
plains within the southern half of the lower peninsula of
Michigan. The samples were dry sieved using a 0.038 mm
wire mesh screen and the < 0.038 mm (medium and fine silts
plus clays) size fraction was subjected to a series of
chemical attacks. These attacks were used to extract the
trace metals associated with the exchangeable, carbonate,

Fe-Mn oxide, and organic fractions of the till samples.

The results of the analyses show that:

1) The highest bulk concentrations of trace metals in till
occur within the (0.038 mm size fraction.

2) With the exception of Cu, most of the trace metals in
the < 0.038 mm size fraction are associated with the
residual phase. Copper is associated with the
exchangeable, Fe-Mn oxide , and carbonate fraction of
the non-residual phase.

3) T1115 from the Lake Michigan, Saginaw, and Huron/Erie
ice lobes can be differentiated on the basis of their
Cu, Ni, Zn, and Sr concentrations within the residual

phase.

20

Q) There is no relationship between trace metal content and

clay content in each sample.

21

APPENDIX A

22

Preliminary Research

Three till samples, one from each lobe, were collected
and stored in plastic zip-loo bags. After being allowed to
dry, the till was passed through a series of nested sieves
measuring 0.25 mm, 0.062 mm, and 0.038 mm. Two grams of
the 0.25 mm—0.062 mm, 0.062 mm-0.038 mm, and (0.038 mm size
fractions were sieved for analysis. Each sample was then
placed in a ball mill and crushed for five minutes to

eliminate all grain size differences.

To prepare the samples for analysis, 0.2 grams of each
size fraction was mixed with 1.0 gram of lithium metaborate
and fused in an oven at 1000 C for 15 minutes. The fused
sample was immediately poured into a glass beaker
containing 5.0 ml hydrochloric acid, 50.0 ml double
distilled water, and a magnetic stirring rod. Upon
dissolution, the sample was volumetrically diluted to 100.0
ml and stored in polyethylene bottles for analysis.
Triplicate fusions were prepared for each sample and
analysis was performed on a model 560 Perkin-Elmer atomic

absorption spectrophotometer.

23

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mmc.ov
wmo.O1EE
N0O.O1EE

mmo.ov
wmo.onaa
Neo.01EE

muum

mmuwm awwuw pouooaom How AEQQ GHV mommamcm uamfiwpmm stm

«no.0
mN.o

Noo.o
mN.o

Noo.o
m~.o

ma

onEmm

24

APPENDIX B

25

Experimental Procedures

Samples were air dried and dry sieved using a 0.038 mm
sieve to obtain approximately 20.0 grams of each sample. A
combination of two fusions and two selective chemical
extractions were used to prepare four fractions for

analysis.

1) Bulk: 0.2 grams of dry sediment were mixed with 1.0 gram
of lithium metaborate and fused at 1000 C for 15
minutes. The fused sample was immediately poured into a
glass beaker containing 5.0 m1 hydrochloric acid, 50.0
ml double distilled water, and a magnetic stirring rod.
Upon dissolution, the sample was volumetrically diluted
to 100.0 ml with double distilled water (Perkin-Elmer
1973).

2) Exchangeable, Carbonate, and Fe-Mn Oxides: 5.0 grams of
dry sediment was leached with 50.0 ml of 1.0 M
hydroxylamine hydrochloride and 25% (V/V) acetic acid at
room temperature with continuous agitation for 4 hours
(Chester and Hughes, 1967). Upon completion the sample
was centrifuged and the supernate volumetrically diluted

to 100.0 ml with double distilled water.

26

3) Organic: The residue from 2) was leached with 15.0 ml of
0.02 M nitric acid and 25.0 ml of 30% hydrogen peroxide
(pH=2 with nitric acid). The mixture was heated to 85 C
for 5 hours with occasional agitation. After the first
2 hours an additional 15.0 ml of 30% hydrogen peroxide
(pH=2) was added to each sample. After cooling, 25.0 ml
of 3.2 M ammonium acetate in 20% (V/V) nitric acid was
added and the sample was diluted to 100.0 m1 and
agitated continuously for 30 minutes. The addition of
the ammonium acetate is designed to prevent absorption
of the extracted metals onto the oxidized sediment

(Gupta and Chen, 1975).

A) Residual: The residue from 3) was dried at room
temperature and 0.2 grams of the dried sediment were

fused using the same procedure as in l).

The chemical extractions were performed in 250.0 ml
polyethylene bottles. After each extraction, the sample
was centrifuged at 1200 rpm for 15 minutes. The supernate
was removed and stored in 125.0 ml polyethylene bottles for
analysis. Next, each sample was washed by adding 25.0 ml
double distilled water and then agitating continuously for
15 minutes. The sample was again centrifuged at 1200 rpm
for 15 minutes, after which the water was decanted. Rinse
water volumes were kept minimal to avoid excessive

solubilization of solid material. All fusions and

27

extractions were performed in triplicate for each sample
and double distilled water was used in the preparation of
all stock solutions. All glassware was soaked for at least
2A hours in 15% hydrochloric acid (V/V) and rinsed with
double distilled water prior to use. All reagents were of
analytical grade or better. All analyses were performed on

a Perkin-Elmer model 560 atomic absorption

spectrophotometer.

28

 

APPENDIX C

29

Smpl.

10

11

12

13

14

15

OUQOO’DOUNOU’DOUQOU’QOU‘DOU‘DOO‘DOUQOUQOUQOU‘DOUWOU’N

105.0
95.0
90.0

110.0

110.0

115.0

170.0

175.0

180.0

115.0

110.0

110.0
80.0
80.0
85.0
70.0
70.0
70.0

105.0

105.0

105.0

115.0

120.0

125.0
95.0
95.0

100.0
95.0
95.0

100.0

155.0

145.0

140.0

120.0

105.0

135.0

105.0

100.0

130.0

110.0

125.0

135.0

140.0

105.0

100.0

Bulk Fraction Analysis (in ppm)

100.0
95.0
85.0

100.0

105.0

105.0

105.0

110.0

100.0

130.0

130.0

130.0

100.0

105.0

105.0

125.0

125.0

130.0

125.0

120.0

120.0

100.0

105.0

100.0

120.0

105.0

115.0

130.0

125.0

135.0

100.0

105.0

100.0

105.0
95.0
95.0

125.0

120.0

125.0

115.0

125.0

120.0

115.0

110.0

115.0

160.0
160.0
145.0
185.0
180.0
180.0
155.0
155.0
165.0
180.0
180.0
180.0
120.0
125.0
120.0
115.0
115.0
115.0
145.0
145.0
140.0
125.0
125.0
125.0
120.0
125.0
125.0
125.0
130.0
125.0
160.0
155.0
140.0
175.0
175.0
180.0
145.0
140.0
140.0
145.0
170.0
165.0
170.0
165.0
165.0

30

35.
35.
40.
35.
30.
25.
40.
40.
40.
25.
25.
35.
40.
40.
30.
40.
40.
40.
40.
40.
35.
35.
35.
40.
50.
50.
55.
55.
55.
60.
45.
50.
40.
40.
45.
45.
45.
45.
50.
35.
30.
35.
40.
40.
35.

OOOOOOOGOOOOCOOOCOOOOCOOCDOOOCOOOOOOCOOCOOOCO

60.
55.
50.
60.
60.
65.
55.
55.
60.
50.
50.
45.
50.
45.
50.
60.
55.
45.
55.
55.
55.
50.
55.
55.
55.
50.
55.
50.
50.
55.
60.
60.
55.
50.
50.
55.
50.
50.
50.
50.
50.
60.
55.
50.
45.

OOOOOOCOCDDOOOOOOOCOOOOOOOCOOCOOOOQOOOOOOOOOO

320.0
320.0
315.0
320.0
330.0
340.0
325.0
330.0
320.0
330.0
350.0
350.0
335.0
335.0
330.0
305.0
305.0
310.0
325.0
330.0
315.0
325.0
335.0
335.0
355.0
340.0
355.0
335.0
315.0
330.0
355.0
350.0
355.0
345.0
345.0
355.0
360.0
375.0
355.0
340.0
340.0
335.0
325.0
325.0
325.0

U)

3
'U

p—n

1...;
a:

H
.q
OUNOU’SDOC'Q

18

Smpl.

OUNOUNOUQOO’QOO’WOUDOUNOU’Q

IS

95.
90.
105.
125.
120.
130.
100.
100.
90.

COOOOCOOO

125.0
120.0
120.0
125.0
125.0
125.0
120.0
120.0
120.0

IE

HH
ON
0 O

O O O O O O O O O C C O C O O
OOCCOCOOOOOOOCDOOQOOOOOO

HHH r—I
mmmwwwNHwoooooommmNNm-q-q-QH
O O O O O O 0

(cont)

150.0
140.0
150.0
165.0
155.0
155.0
140.0
140.0
135.0

52.0
48.0
46.0
23.0
21.0
22.0
33.0
33.0
31.0
21.0
16.0
21.0
19.0
19.0
20.0
16.0
16.0
17.0
19.0
18.0
19.0
30.0
30.0
30.0

31

55.0
55.0
60.
55.
50.
55.
55.
55.
60.

OCOOOCO

U)
a

H

l-|
kmwmmmwwmowo-thbwwwhwooooq
O O. O. O. .0. O. O O O O. O O

O O O O O
OOOOCOOOOOQOOOCOOOOCCOOO

IQ

OOOOQOOO

l9

OOHWWNOOCHHHCCONHNHHHHHH
o 00 ea c as use. a oo o oo o a. a o o

oocowhomoooocooccHr-owoon-ar-‘mwmmhw

In:
a-

315.
330.
330.
345.
345.
330.
335.
340.0
345.0

COOCOOO

Exchangable, Carbonate, Fe-Mn Oxide Fraction Analysis (in ppm)

' (cont)

Smpl 9.1. .111. E 2‘. 9!. 1’2
9 a 53.0 5.0 23.0 2.0 1.9 29.0
b 54.0 5.0 20.0 1.0 1.6 25.0

C 56.0 5.0 23.0 2.0 1.6 27.0

10 a 43.0 6.0 24.0 6.0 2.7 18.0
b 42.0 5.0 22.0 5.0 2.6 15.0

C 46.0 5.0 26.0 5.0 2.7 17.0

11 a 73.0 8.0 37.0 2.0 2.3 24.0
b 71.0 7.0 32.0 3.0 1.9 18.0

c 75.0 7.0 37.0 2.0 2.3 24.0

12 a 41.0 8.0 23.0 1.0 1.2 44.0
b 44.0 8.0 23.0 2.0 1.2 38.0

C 43.0 8.0 24.0 1.0 1.3 52.0

13 a 35.0 7.0 16.0 2.0 1.4 16.0
b 34.0 6.0 14.0 3.0 1.1 16.0

C 35.0 6.0 15.0 2.0 1.4 17.0

14 a 50.0 10.0 22.0 1.0 2.0 18.0
b 47.0 9.0 19.0 2.0 1.6 16.0

c 50.0 9.0 21.0 1.0 2.0 17.0

15 a 28.0 7.0 12.0 2.0 1.3 14.0
b 27.0 7.0 11.0 2.0 1.6 12.0

C 29.0 6.0 12.0 2.0 1.5 12.0

16 a 40.0 5.0 21.0 2.0 1.6 19.0
b 40.0 4.0 19.0 1.0 1.6 17.0

C 40.0 4.0 20.0 2.0 1.3 18.0

17 a 67.0 15.0 28.0 2.0 1.7 24.0
b 66.0 14.0 25.0 2.0 1.6 24.0

C 68.0 15.0 28.0 3.0 1.9 24.0

18 a 47.0 5.0 19.0 3.0 1.5 19.0
b 49.0 5.0 19.0 3.0 2.0 19.0

C 54.0 5.0 21.0 3.0 1.9 19.0

Organic Fraction Analysis (in ppm)

Smpl _C_u iii .23 .SL' .91 El).
1 a 14.0 12.0 48.1 0.0 1.9 6.7
b 14.0 12.2 46.4 0.0 3.2 6.1

C 14.6 11.0 48.3 0.0 3.2 5.9

2 a 4.0 4.8 11.2 0.0 3.4 5.9
b 8.0 5.1 15.0 0.0 4.2 7.0

c 11.2 7.4 25.1 0.0 5.9 8.2

32

(cont)

Smpl

804044633424892027298308736874741862694482299962

576677698687446787233818699943709587587798798688
111 111 1 11

262266839693686841666949425169996968339699847292
O O

o o o a o a o co 0 o e c o a

000000957985000728955930928859562991452955608481

00000024002900.00002432442541311311354122232243131232

143673235588459580973060542525785402500973909529

ooooooooooooooo
327742354355128355579809471481344795478579686482
121113 111 1

04554449666926939867006895065074.7525676670050274

I O O O O O O O
334436111122446111234565248234233347234234338236

149036745925782593143015976233024386237143608862

O O O O
872793253243119365678797500488565578243678692501
132 111 1 11...

abcabcabcabcabcabcabcabcabcabcabcabcabcabcabcabC

0 1.. 2 3 4 5 6 7. oo
3 4 5 6 7. oo 9 1 1.. 1 1 1 1.. 1 1 1

33

Residual Fraction Analysis (in ppm)

34

Smpl 9.9 111 a a .91: 22
1 a 35.0 85.0 90.0 25.0 60.0 340.0
b 30.0 85.0 85.0 25.0 60.0 325.0

c 25.0 90.0 70.0 30.0 50.0 325.0

2 a 50.0 80.0 125.0 20.0 50.0 330.0
b 45.0 70.0 115.0 20.0 45.0 325.0

c 45.0 80.0 115.0 25.0 45.0 310.0

3 a 45.0 95.0 80.0 35.0 55.0 305.0
b 45.0 95.0 85.0 30.0 50.0 305.0

c 35.0 85.0 80.0 30.0 50.0 305.0

4 a 45.0 90.0 115.0 20.0 50.0 325.0
b 65.0 105.0 110.0 15.0 50.0 320.0

C 40.0 100.0 100.0 20.0 55.0 325.0

5 a 60.0 95.0 100.0 25.0 55.0 335.0
b 55.0 90.0 100.0 25.0 50.0 330.0

C 50.0 90.0 95.0 20.0 50.0 330.0

6 a 50.0 85.0 90.0 40.0 50.0 305.0
b 55.0 80.0 90.0 35.0 60.0 305.0

C 55.0 80.0 90.0 25.0 65.0 320.0

7 a 50.0 105.0 70.0 30.0 50.0 325.0
b 50.0 90.0 90.0 35.0 55.0 320.0

c 35.0 90.0 75.0 40.0 50.0 305.0

8 a 55.0 85.0 90.0 30.0 60.0 320.0
b 50.0 85.0 85.0 30.0 55.0 250.0

c 55.0 90.0 100.0 30.0 55.0 335.0

9 a 45.0 115.0 95.0 50.0 55.0 340.0
b 50.0 95.0 95.0 50.0 50.0 325.0

C 50.0 95.0 105.0 50.0 50.0 300.0

10 a 40.0 100.0 105.0 40.0 60.0 325.0
b 40.0 95.0 110.0 50.0 60.0 315.0

C 40.0 90.0 105.0 55.0 60.0 290.0

11 a 75.0 115.0 115.0 45.0 60.0 330.0
b 70.0 120.0 105.0 40.0 60.0 315.0

C 75.0 115.0 105.0 40.0 55.0 335.0

12 a 65.0 85.0 155.0 40.0 55.0 295.0
b 75.0 85.0 160.0 40.0 55.0 325.0

C 75.0 90.0 170.0 40.0 50.0 380.0

13 a 60.0 105.0 110.0 40.0 50.0 340.0
b 65.0 100.0 130.0 35.0 55.0 350.0

c 55.0 100.0 125.0 50.0 50.0 325.0

14 a 75.0 110.0 135.0 50.0 50.0 315.0
b 80.0 140.0 135.0 45.0 50.0 330.0

C 75.0 105.0 120.0 40.0 55.0 300.0

15 a 70.0 105.0 150.0 35.0 50.0 315.0
b 70.0 100.0 175.0 35.0 50.0 310.0

c 75.0 110.0 160.0 35.0 50.0 315.0

(cont)

Smpl 93 11. 22 .8: 2r. 82
16 a 65.0 100.0 125.0 50.0 55.0 365.0
b 65.0 110.0 140.0 50.0 55.0 335.0

C 50.0 95.0 110.0 55.0 50.0 345.0

17 a 70.0 120.0 150.0 50.0 60.0 330.0
b 75.0 105.0 140.0 50.0 55.0 330.0

C 70.0 105.0 120.0 50.0 60.0 330.0

18 a 70.0 100.0 130.0 50.0 60.0 325.0
b 75.0 100.0 125.0 50.0 60.0 320.0

c 65.0 100.0 120.0 55.0 60.0 345.0

35

APPENDIX D

36

Sample Averages for Bulk Fraction (in ppm)

+|

5.0
2.9
2.9
2.9
2.9
7.6
0.0

55.0

2.9
10.0

7.6 318.0

93.3
101.7

2.9
5.0
0.0
5.6
5.8
0.0

36.7

8.7
2.9
5.8

155.0
0.0

181.7

7.6
2.9

96.7
111.7

62.0

330.0

2.9
5.0
0.0

30.0

2.

5.0 57.0

11.5

325.0

105.0

40.0

5.0

175.0
111.7

3.

158.0
180.0
121.7

48.3

130.0 343.0

101.7

28.3

2.9

4.

48.3

2.9
2.9
7.6
5.8
8.7

10.4

333.0

2.9

36.7

2.9
0.0

2.9
0.0
0.0

81.7

53.0

307.0

2.9

115.0 40.0 126.7

143.3
125.0

70.0
105.0

55.0

323.0

2.9
2.9

38.3 2.9 121.7
2.9
7.6

2.9
0.0

7.

37

2.9
2.9
2.9

332.0

101.7

36.7

5.0

120.0

8.

.53.3

53.0

350.0

113.3

2.9
2.9
5.0

51.7

2.9
2.9

10.4

123.3
126.7
151.7
176.7

2.9
2.9
7.6
15.0
16.0
12.6

21.8

96.7

52.0

5.0 326.7

130.0

56.7

96.7
146.7

10.
11.
12.
13.
14.
15.
16.
l7.
18.

2.9
2.9
0.0
5.8
5.0
2.9
2.9

58.0

2.9
5.8
5.0

2.9

353.0
348.0
360.0

2.9

101.7

45.0

52.0

5.8
2.9
5.0

98.3
123.3
120.0

2.9
2.9
2.9
2.9
2.0
2.9

2.9 43.3

2.9
13.2

120.0
111.7

50.0

46.7

141.7

53.0

33.3 338.0
325.0
325.0

160.0

123.3

50.0

0.0
8.7
8.7
5.0

38.3 113.3 2.9
121.7

2.9
5.8

5.8

166.7

115.0

52.0

2.9

56.7

7.6 146.7

5.0

96.7
125.0

57.0

340.0

125.0 0.0
120.0

53.3

158.3

2.9

58.0

340.0

0.0

5.8 138.3 2.9 56.7 2.9

96.7

Sample Averages for Exchangable, Carbonate, and Fe-Mn Oxide Fraction (in ppm)

+|

+|

+|

0.1

1.4
1.5
2.0
0.1

0.0
1.0
1.2
2.3
0.0
0.6
0.0
1.0
2.0

15.0

1.0
0.0
0.0
0.0
0.0

0.6 11.0
0.6
0.6
1.5
0.6

0.6
2.1

2.1 48.7 3.1 7.7

53.3

0.2
0.9
0.0
0.0

0.1

16.0

7.0
2.0
6.0
8.0

12.0

3.3

1.0
1.2
2.9
0.6
0.6
0.6
0.0

2.0 22.0

11.6

51.0

12.0

3.3
5.3
9.7

32.2

78.3

24.0

19.3

5.5
1.2

0.6

42.3

1.0
0.8

16.0

19.3

43.3

16.8

1.0
0.0
0.0
0.0
0.6

2.3
4.3

16.3

46.3

0.5
0.2
0.2

0.1

3.0
0.9
1.7

2.7

11.0

3.0
6.0
5.0
5.3
7.3
8.0
6.3
9.3
6.7
4.3

14.7

1.5 18.7

1.2

52.3

14.0

1.0
0.6
0.6
0.6
0.6
0.6
0.6
0.0
0.6
0.6
0.6

3.0
1.7

30.0

68.3

27.0

1.7
2.0

22.0

1.5
2.1

54.3

1.0
3.5
7.0
0.6

17.0

5.3
2.3

24.0

43.7

10.
11.
12.
13.
14.
15.
16.
17.
18.

0.3
0.1

2.2

22.0

0.6
0.0
0.6
0.6
0.6

2.9
0.6

35.3

2.0
1.5

0.6
1.7

73.0

1.2
1.3
1.9
1.5
1.5
1.7

44.0

1.3

2.3
1.3

2.9
1.7

23.3

42.7

0.2

16.3

1.0
1.5
0.6

15.0

34.7

0.2
0.2
0.2
0.2
0.3

1.0

17.0

20.7

49.0

1.2
1.0
0.0
0.0

13.0

1.0 11.7

0.0

28.0

18.0

0.6
0.6

1.6
1.7

20.0

40.0

24.0

2.3
2.7

1.0 27.0
3.6

67.0

1.8

19.0

0.0

5.0

1.2

19.7

50.0

Sample Averages for Organic Fraction (in ppm)

2.6
4.5
3.0
2.8

0.4

6.4
7.0
6.4

11.7 0.6
16.9

0.0
0.0
0.0
0.0
0.8
0.5
0.0
0.8
0.9

0.0
0.0
0.0
0.0
3.7

1.0
7.2
4.7

47.6

0.3
3.6

10.0

14.6

1.3
1.1
1.6
0.4
0.3
1.1

1.2
0.6
0.8

1.4
0.8
1.5
0.2
0.7

5.8
3.6
4.8

17.1

7.7
26.1

17.6

21.5 9.4
1.1

3.4

10.0

1.0
1.6
5.3
1.1
1.6
2.1
3.0
1.5
1.8
2.8
1.7
1.8
2.6
2.8

1.4
0.9
0.8
0.6

8.1

1.6
2.4

5.2
1.7

4.3

1.4
0.7
4.3
1.7

3.9
3.5

14.2

7.3

3.4
0.0
3.6
4.0

4.1

1.3
4.1

5.0
14.3

5.3
7.6
13.3

1.5
0.3

0.3
0.0
0.3

1.1

4.8

5.2

1.0
1.4
1.6

2.5
1.4

9.4
8.5
12.6

0.7
0.8

3.4
5.8

1.2
0.8

1.7
1.3
3.4
3.5
0.6
4.1

7.6
9.2
7.7

1.1
1.1
8.1

7.3
7.9
9.1

39

0.6
0.5
0.2

2.6
0.7
0.5
2.1

5.1

2.3
2.4
4.4
2.3
2.7
3.6

2.1

2.8
2.4
0.6
1.7
1.1
1.1
3.1

11.
12.
13.
14.
15.
16.
17.
18.

3.4
3.3
5.1

1.0
1.1
0.5
0.7
0.8
0.8
0.9

6.9
5.5
7.2

9.1

4.3
10.5

1.0
0.4
0.1

1.4
1.7

7.2

7.3
8.5
8.7
7.9

1.0
0.7

3.6
3.4
4.8

1.8
1.7
0.6
4.2

6.5
7.6
7.3
8.5

3.4
7.3
9.5

1.2
1.4
0.9

1.0
0.5

2.8
2.1

4.1

2.8

3.0

9.2

Sample Averages for Residual Fraction (in ppm)

co
m
€—
01 +I
O
>4 .
L‘
In
D-
Q
“I
a. +|
G
>< .
C
M
3:.
”<3
(D o
N
2: +|
L‘-
>< .
(D
oo
65
en” -
N
£—
00 +1
L~
>4 .
to
N
fl'
to” .
O
c H
N +|
L‘
¥:.q
co
O
mx -
In
h
L) +|
O
>< .
O
6°
'—
{g .4

2.9
2.9
2.9
2.9
5.0

47.3

.4

10

322.0

—.——o.’-

5.8
5.8
7.6

76.7

2.9
2.9

21.7

5.8
2.9
7.6
2.9
0.0

118.3
10.4

2.9
5.8

13.2

46.7

52.3

0.0

81.7 31.7 91.7 305.0

108.3

41.7

52.3

2.9
2.9
8.7

10.4

323.3

98.3

2.9
2.9
7.6

18.3

50.0

52.3

332.3

2.9
2.9
8.7

91.7

23.3

98.3

5.0
2.9
8.7

55.5

55.0

310.0

81.7

33.3

90.0

53.3

2.9
2.9
2.9

52.3

317.0

95.0

5.0
0.0
0.0

35.0

78.3

45.0

45.0 57.3
20. 52.3

302.0
322.0

2.9

11.5

86.7
101.7

7.6 30.0
98.3 5.8 50.0

91.7
106.7

2.9
2.9

0.0

53.3
48.3

40

7.6 95.0 5.0 310.0 18.0 60.0 0.0
116.7

48.3

2.9

40.0

10.
11.
12.
13.
14.
15.
.16.

2.9
2.9
2.9
2.9
0.0

327.0 10.4 58.3

2.9

2.9
0.0
7.6

108.3 5.8 41.7

161.7

2.9
5.8
5.0
2.9

73.3

333.0 43.0 53.3

2.9

2.9
18.9

40.0 86.7
101.7

7.6
10.4

71.7

338.0 12.6 52.3
315.0

313.0
348.0

41.7

121.7

60.0

52.3

15.0

118.3
105.0

8.7 45.0 5.0
0.0

12.6

130.0

76.7

50.0

2.9
15.3

5.0
7.6

35.0

2.9 161.7

8.7

71.7

2.9
2.9
0.0

53.3

125.0 15.0 51.7 2.9 101.6
0.0

136.7

60.0

0.0 58.3
13.2

330.0

8.7
0.0

110.0

50.0

71.7 2.9 15.3
5.0

17.
18.

60.0

330.0

5.0 51.7 2.9 100.0

125.0

70.0

APPENDIX E

41

Clay analyses

(1)
Clay

Wt. (g)

12.74

9.64
14.61
11.41
.12
.23
.84
.76
.20
.51
.14
.24
.54
.55
.74
.54
.43
.54

H
mVNChwUIU'IO‘OOU'I

thhJ
Lead»

42

(2)

Med + Fine

Silt Wt.

12.
16.
33.
24.
12.
14.
12.
15.
13.

7.
17.
17.
18.
14.
13.
13.
17.
14.

74
92
43
51
8O
97
36
24
O4
97
82
88
55
37
94
82
25
14

(g)

A
H
V

__?77_

OOOOOOOOOOOOOOOOOH

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44

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