CHEMICAL DATA AND LEAD ISOTOPIC COMPOSITIONS OF

GEOCHEMICAL BASELINE SAMPLES FROM STREAMBED

SEDIMENTS AND SMELTER SLAG, LEAD ISOTOPIC

COMPOSITIONS IN FLUVIAL TAILINGS, AND

DENDROCHRONOLOGY RESULTS FROM THE BOULDER

RIVER WATERSHED, JEFFERSON COUNTY, MONTANA

by Daniel M. Unruh1 David L. Fey1, and Stanley E. Church1

Open-File Report 00-038

2000

On-Line Edition

This report is preliminary and has not been reviewed for conformity with U.S. Geological Survey editorial standards

and stratigraphic nomenclature. Any use of trade, product, or firm names is for descriptive purposes only and

does not imply endorsement by the U.S. Government.

U.S. DEPARTMENT OF THE INTERIOR

U.S. GEOLOGICAL SURVEY

1 Denver, Colorado
Table of Contents

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

Methods of Study..............................................................................................4

Analytical Results...............................................................................................7

References Cited................................................................................................9

Appendix......................................................................................................11

Figures

Figure 1. Index map of Montana showing Boulder River study area and locality map for

streambed-sediment sites in the Boulder River watershed, Montana ...............................2

Figure 2. Index map of Montana showing Boulder River study area and locality map for

geochemical baseline cores, and mine waste and tailings sites, Boulder River

watershed, Montana .................................................................................3

Tables

Table 1. Sample localities of stream terrace and core samples, smelter slag, and

sampled mine wastes, Boulder River watershed, Montana.........................................15

Table 2. Site and sample descriptions of stream terrace and core samples, Boulder River

watershed, Montana..................................................................................17

Table 3. Major and trace element data from total digestions of streambed sediments from

stream terrace and core samples, Boulder River watershed, Montana............................30

Table 4. Lead isotopic data from streambed sediments from stream terrace and core samples,

Boulder River watershed, Montana..................................................................62

Table 5. Major and trace element data from total digestions of fluvial tailings deposited

on a bar in the Boulder River, Boulder River watershed, Montana................................63

Table 6. Lead isotopic data from fluvial tailings and contaminated streambed-sediment

samples, Boulder River watershed, Montana.....................................................71

Table 7. Major and trace element data from the Bullion smelter slag sample,

Jack Creek drainage, Boulder River watershed, Montana.......................................72

Table 8. Statistical summary of ore-related metal concentrations in sampled mine

wastes, Boulder River watershed, Montana.......................................................74

Table 9. Dendrochronology results from some stream terrace and core localities,

Boulder River watershed, Montana................................................................75

i
1

INTRODUCTION

As a part of the U.S. Geological Survey Abandoned Mine Lands Initiative (Buxton and others,

1997), metal-mining related wastes in the Boulder River study area in northern Jefferson County,

Montana, have been evaluated for their environmental effects. The study area includes a 24-km

segment of the Boulder River in and around Basin, Montana and three principal tributaries to the

Boulder River: Basin Creek, Cataract Creek, and High Ore Creek. Mine and prospect waste dumps

and mill wastes are located throughout the drainage basins of these tributaries and in the Boulder River.

Mine-waste material has been transported into and down streams, where it has mixed with and become

incorporated into the streambed sediments. In some localities, mine waste material was placed directly

in stream channels and was transported downstream forming fluvial tailings deposits along the stream

banks. Water quality and aquatic habitat have been affected by trace-element-contaminated sediment

that moves from mine wastes into and down streams during snowmelt and storm runoff events within the

Boulder River watershed (Buxton and others, 1997; Farag and others, 1999; Nimick and others,

1999).

Present-day trace element concentrations in the streambed sediments and fluvial tailings have

been extensively studied (Aamodt, 1978; Broxton, 1980; Campbell and others, 1982; Fey and Church,

1998; Fey and others, 1999a; 1999b, 2000). However, in order to accurately evaluate the impact of

mining on the stream environments, it is also necessary to evaluate the pre-mining trace-element

concentrations in the streambed sediments. Three types of samples have been collected for estimation

of pre-mining concentrations: 1) streambed sediment samples from the Boulder River and its tributaries

located upstream from historical mining activity, 2) stream terrace deposits located both upstream and

downstream of the major tributaries along the Boulder River, and 3) cores through sediment in

overbank deposits, in abandoned stream channels, or beneath fluvial tailings deposits. In this report, we

present geochemical data for six stream-terrace samples and twelve sediment-core samples and lead

isotopic data for six terrace and thirteen core samples. Sample localities are in table 1 and figure 1 and

figure 2, and site and sample descriptions are in table 2.

Geochemical data have been presented for cores through fluvial tailings on High Ore Creek

(Fey and Church, 1998), on upper Basin Creek (Fey and others, (1999a), and on Jack Creek and

Uncle Sam Gulch (Fey and others, (2000). Geochemical and lead isotopic data for modern streambedsediment samples have been presented by Fey and others (1999b).

Lead isotopic determinations in bed sediments have been shown to be an effective tool for

evaluating the contributions from various sources to the metals in bed sediments (Church and others,

1993, 1997). However, in order to make these calculations, the lead isotopic compositions of the

contaminant sources must also be known. Consequently, we have determined the lead isotopic

compositions of five streambed-sediment samples heavily contaminated with fluvial mine waste

immediately downstream from large mines in the Boulder River watershed in order to determine the lead

isotopic signatures of the contaminants. Summary geochemical data for the contaminants are presented

here and geochemical data for the streambed-sediment samples are given by Fey and others (1999b).

Downstream from the Katie mill site and Jib tailings (fig. 1, 1T), fluvial deposits of mill tailings

are present on a 10-m by 50-m bar in the Boulder River below the confluence with Basin Creek. The

source of these tailings is not known, but fluvial tailings are also present immediately downstream from

the Katie mill site, which is immediately upstream from the confluence with Basin Creek. Nine cores of

fluvial tailings from this bar were analyzed.
Missoula

Helena

Butte

Billings

M O N T A N A

Bozeman

Dillon

Study Area

2

0

0 1

1 2 MILES

2 KILOMETERS

Base from U.S. Geological Survey

Digital line graphs, 1:100,000

CONTINENTAL

DIVIDE

Basin

Weasel Gulch

Joe Bowers

Cr

Jimmys

Cr

Clear Creek

Grub

Gulch

Jack

Creek

Nellie Grant

Cr

Overland Cr

Rocker

Creek

Snow drift

Creek

Hoodoo Creek

Cataract

Creek

Uncle Sam

Gulch

Deer

Creek

Basin

Creek

Saul Haggerty Gulch Boulder River

Big

Limber

Gulch

Bishop

Creek

High

Ore

Creek

Peters Gulch

Boomerang

Gulch

Galena

Gulch

Little

Galena

Kleinsmith

Gulch

112 22'30'' o

112 15 o

46 22'30'' o

46 15' o

R.6W. R.5W.

T.8N.

T.7N.

T.6N.

P O W E L L C O

L E W I S A N D C L A R K C O

J E F F E R S O N C O 

R.4W.

BEAVERHEAD-DEERLODGE

 NATIONAL FOREST

 Three

 Brothers

 Jack 

Mountain

 

Gulch

28S

1S 2S

19S

16S

17S

18S

Bed-sediment site sampled by the U.S. Geological Survey

and site number

21S

EXPLANATION

Little Boulder R.

Boulder

River

N

40S

37S

36S

35S

34S

33S 32S

39S

38S

43S

41S

23S

22S 21S 20S

42S

26S

24S

25S

27S

29S

31S

5S 6S

3S

7S

8S 9S 10S

11S 12S

63S

13S

15S

62S

61S

60S

59S

58S

52S

51S

49S

56S

55S

54S

48S

46S

47S

45S

44S

Figure 1. Index map of Montana showing Boulder River study area and sample locality

 map for bed-sediment sampling sites in the Boulder River Watershed.

South Fork Basin Creek

Vacch iou Gulch
Missoula

Helena

Butte

Billings

M O N T A N A

Bozeman

Dillon

Study Area

3

0

0 1

1 2 MILES

2 KILOMETERS

Base from U.S. Geological Survey

Digital line graphs, 1:100,000

CONTINENTAL

DIVIDE

Basin

Weasel Gulch

Joe Bowers

Cr

Jimmys

Cr

Clear Creek

Grub

Gulch

Jack

Creek

Nellie Grant

Cr

Overland Cr

Rocker

Creek

Snow drift

Creek

Hoodoo Creek

Cataract

Creek

Uncle Sam

Gulch

Deer

Creek

Basin

Creek

Saul Haggerty Gulch Boulder River

Big

Limber

Gulch

Bishop

Creek

High

Ore

Creek

Peters Gulch

Boomerang

Gulch

Galena

Gulch

Little

Galena

Kleinsmith

Gulch

112 22'30'' o

112 15 o

46 22'30'' o

46 15' o

R.6W. R.5W.

T.8N.

T.7N.

T.6N.

P O W E L L C O

L E W I S A N D C L A R K C O

J E F F E R S O N C O 

R.4W.

BEAVERHEAD-DEERLODGE

 NATIONAL FOREST

 Three

 Brothers

 Jack 

Mountain

 

Gulch

Little Boulder

Boulder

River

N

5T

1T

4T

6T

2T

3T

2B

1B 3B

4B

19B

5B

6B

18B

17B

16B

8B

9B

10B

11B

7B

15B

14B

13B

12B

EXPLANATION

Mine waste or fluvial tailings site sampled by the U.S. Geological Survey

and site number

5T

Baseline core site sample by the U.S. Geogical Survey

and site number

16B

Figure 2. Index map of Montana showing Boulder River study area and sample locality map

 for geochemical baseline cores and mine waste and tailings sites.

S ou th Fork Basin Creek

Vacchiou Gu cl h
4

Dendrochronology samples were taken at several stream terrace localities to provide age

control on the stream terrace deposits. Trees growing on the surfaces of stream terraces provide a

minimum age for the terrace deposits, although floods subsequent to the trees’ growth could have

deposited post-mining overbank deposits around the trees. Historical data were also used to provide

estimates of minimum ages of cultural features and to bracket the age of events (Rossillon and Haynes,

1999).

METHODS OF STUDY

Sample collection

Streambed sediments and fluvial tailings samples

Elemental and lead isotopic data for the baseline streambed-sediment samples that have little, if

any, impact by historical mining have been reported by Fey and others (1999b). Their sample localities

are indicated schematically in figure 1 (samples collected at nine sites; 2S, 3S, 4S, 20S, 22S, 32S, 44S,

54S, and 58S). Samples at sites 2S, 4S, and 22S were collected in October, 1996. Samples at sites

3S, 32S, 44S, and 54S were collected in July, 1997, and the remaining samples (20S, 58S) were

collected in July, 1998. A second sample at site 3S was collected in July, 1998 in order to monitor

yearly variations in trace-element concentrations. Sites were selected to be generally upstream from

known historical mining activities. At each site, an integrated streambed-sediment sample was collected

by compositing material from the active channel alluvium from 10 to 20 individual subsites within 15 m

(50 ft) of the plotted sample locality. In the field, each composited sample was sieved through a 2-mm

(10 mesh) stainless-steel screen, and the minus-2-mm fraction retained; the larger size fraction was

discarded.

Samples of fluvial tailings collected at four sites (2T-5T, fig. 2) and the Bullion Smelter slag (6T,

fig. 2) were selected for lead isotopic analyses. Three fluvial overbank-sediment samples from the Jack

Creek drainage that were shown to contain tailings materials on the basis of their chemistry (35S, 37S,

40S) were also analyzed for lead isotopic compositions. These samples were collected in October

1996, in the same manner as the streambed-sediment samples, and were dry-sieved in the field to

preserve the water-soluble salts contained in the samples.

Stream terraces

Samples of stream terraces were collected at six sites along the Boulder River during July 1999

(Sites 1B-6B in fig. 2). At each site, a pit was dug by hand or backhoe. Three to five subsamples were

collected and given designations “a” through “e”, with “a” being the highest sample stratigraphically

(table 2). In general, no stratigraphy could be discerned in the gravel deposits, so each sample is really

a subsample of the gravel deposit. Each subsample was sieved through a 2 mm (10 mesh) stainlesssteel screen in the field. The minus-2-mm fraction for each subsample was retained separately and the

larger size fraction was discarded. Each sample was treated separately, and the geochemical data

evaluated to look for homogeneous distributions of ore-related trace elements throughout the terrace

deposit. Samples from terrace sediment intervals having a uniform trace elemental distribution were

used in this study to calculate the pre-mining geochemical baseline concentrations and determine the

lead isotopic composition in pre-mining streambed sediments. This goal was achieved in streambed

sediments for core 9B (table 3). Examination of the concentration data as a function of depth for
5

arsenic, copper, and lead clearly indicate the impact of historical mining whereas concentrations of zinc

show less of an impact on streambed sediments in upper Basin Creek.

Sediment cores

Twelve sediment cores were collected in acid-cleaned sections of 2 inch (5 cm) diameter PVC

pipe to determine the metal concentrations and lead isotopic compositions in streambed sediments prior

to historical mining. The objective of the sampling strategy was to sample sediments deposited through

the time period before the onset of historical mining activity. Thus, the concentrations of metals in the

cores should decrease with depth or reach a consistent concentration providing a clear indication of the

pre-mining geochemical baseline in streambed sediments. One of these samples (site 18B, fig. 2) was

collected in October 1996. Four additional cores (sites 11B, 13B, 17B, and 19B) were collected in

July 1997, and seven more were collected in July 1998 (Sites 7B, 8B, 9B, 10B, 12B, 14B, 15B).

Subsamples from ten of the sites were selected for lead isotopic analyses on the basis of their orerelated trace element concentrations and distributions within the cores.

In addition, segments of three one-inch diameter cores collected beneath the fluvial tailings were

analyzed for their lead isotopic compositions: site (3T) near the Buckeye Mine, and sites 5Ta and 5Tb

on High Ore Creek below the Comet Mine. A complete discussion of the geochemistry of the cores

from the Comet Mine on High Ore Creek is in Fey and Church (1998) and of the cores from the

Buckeye Mine on upper Basin Creek is in Fey and others (1999a).

Fluvial tailings from site T1

Nine cores were taken on the bar in the Boulder River at site 1T (fig. 2) just downstream from

the confluence with Basin Creek. Nine cores were taken at 5-m intervals along the 50 m length

beginning about 7 m from the downstream end of the bar. At sites 8 and 9, the tailings had been

removed by erosion and no core samples were taken. Cores 10 and 11 were taken at the upstream

end of the bar. The fluvial tailings deposit at site T1 is approximately 30-40 cm thick and the top of the

bar is about 1 m above the low-flow water level in the Boulder River. Core descriptions and depths of

penetration into fluvial tailings are in table 2. The cores were subdivided on the basis of discernable

stratigraphy.

Dendrochronology

Cores of live trees were taken using a standard tree corer, the core was extracted and placed in

a plastic sleeve, and most were sent to the Laboratory for Tree Ring Research, University of Arizona

for analysis. Slabs of dead trees were also sent for analysis in hopes that the time of death could be

determined to date the tree stump. The ages of the trees provides an estimate of the minimum age of the

stream terrace.

Sample Preparation

Streambed-sediment and stream-terrace samples were dried at ambient room temperature

(25oC) and sieved to minus-80-mesh (<0.18mm) prior to laboratory analyses.

Core samples were subdivided in the laboratory on the basis of mineralogy, organic content,

and apparent oxidation zones. The depth assigned to each subsample is defined as the mid point for
6

that subsample after taking compaction into account (table 2). Individual cores were generally divided

into two to ten subsamples, and ground in random order to minus-100-mesh in a vertical pulverizer.

Sample Analyses

Total digestion

The streambed-sediment, stream-terrace, and core samples were digested with a mixed-acid

solution consisting of HCl, HNO3, HClO4, and HF. This procedure is effective in dissolving most

minerals, including silicates, oxides and sulfides; resistant or refractory minerals such as zircon, chromite,

and some tin oxides are only partially dissolved. Previous investigations using a variety of materials

support the completeness of the digestion (Church and others, 1987; Wilson and others, 1994).

Results are reported for 34 elements analyzed by ICP-AES (inductively coupled plasma-atomic

emission spectroscopy; Crock and others, 1983; Briggs, 1996). Limits of determination for the total

digestion method as well as a statistical summary of mean values, standard deviations, and median

values for four National Institute of Standards and Technology (NIST) standard reference materials

(SRM-2704, SRM-2709, SRM-2710, and SRM-2711) are given by Fey and others (1999b).

Comparisons with certified values for these standards (NIST, 1993a; 1993b; 1993c; and 1993d) are

also given by Fey and others (1999b). Both analytical precision and accuracy are well within

acceptable ranges.

Warm 2M HCl-1 percent H2O2 leach extraction

The use of a partial-digestion extraction enables one to determine concentrations of trace

elements bound within different mineral phases, whereas a total-digestion extraction releases all trace

elements in a sample (Chao, 1984). All sample intervals analyzed for lead isotopic compositions were

subjected to a partial-digestion extraction consisting of warm (500 C) 2M HCl-1 percent H2O2 for three

hours with continuous agitation. The leachates were subsequently analyzed by ICP-AES for 32

elements. This partial extraction was designed to release trace elements associated with hydrous

amorphous iron- and manganese-oxide mineral coatings and colloidal particles (Appendix III of Church

and others, 1993; Church and others, 1997). Mineral coatings such as those observed in the study area

can contain a significant percentage of the trace elements in a sample (Church and others, 1993, 1997).

Because we have shown that the vast majority of the contaminant lead exists within the

amorphous iron- and manganese-oxide mineral coatings and colloidal particles (for example, Church

and others, 1993, 1997), only the leachates were analyzed for lead isotopic compositions. This

procedure presents a clearer picture of the distribution of contaminant lead and greatly reduces dilution

effects from lead bound within the major mineral phases such as potassium-feldspar.

Ion exchange and mass spectrometry for lead isotope analyses

The lead separation procedure used on the 2M HCl-1 percent H2O2 extraction leachates to

obtain the lead isotopic data is similar to those reported by Tatsumoto and others (1976) and by Unruh

and others (1979). ICP-AES analyses of the selected samples provided an in-solution concentration

for lead (Church and others, 1993). This concentration value is then used to calculate the volume of

leachate needed to contain approximately 0.5 μg of lead; this aliquot is then evaporated to dryness in a
7

teflon beaker. Then 0.5 to 1.0 mL of 1.0 N hydrobromic acid (HBr) is added to the sample and

warmed gently for 5 to 10 minutes. The sample is allowed to cool, is centrifuged, and the supernatant

loaded onto an anion-exchange column (0.8-1.0 mL resin volume) using Dowex AG1-X8 anionexchange resin. The column is washed with 1.2 N HBr and water, and then the lead is eluted with

either 8N hydrochloric acid (HCl) or 0.5-1.0 N nitric acid (HNO3). The sample is again evaporated to

dryness and then loaded onto a second anion-exchange column with a resin volume of 0.1-0.2 mL. The

column is washed with 1.2 N HBr and water, and the lead is eluted with 0.5 N nitric acid. Two or

three drops of dilute (0.25-0.5 percent) phosphoric acid (H3PO4) are added to the sample, and it is

then evaporated again to dryness.

Approximately one-half of the sample is taken up in approximately 10 μL of dilute colloidal

silica gel, loaded onto a rhenium-ribbon filament, and evaporated to dryness. The filament is then

loaded into a solid-source thermal ionization mass spectrometer and heated to 1150-1350oC for data

acquisition. Most analyses were made using a VG Sector 54, 7-collector mass spectrometer run in

“static” mode. A few samples were run on a Micro Mass 54R, single-collector mass spectrometer.

No systematic biases have been observed between the two mass spectrometers (Taylor and others,

1999). Analyses of NIST SRM 981 were used to monitor mass fractionation during mass

spectrometry (Cantanzaro and others, 1968; Todt and others, 1993). Methods of calculation of the

analytical uncertainty are presented in the Appendix. The lead isotopic data for replicate analyses of

SRM-981 are in table A1.

As demonstrated by Fey and others (1999b), data from analyses of the leachates are inherently

less reproducible than those from total digestion analyses. As a test of the leaching procedure for lead

isotopic analyses, leachates of four NIST standards SRM 2704, 2709, 2710, and 2711 were analyzed

for lead isotopic ratios. The lead isotopic analyses of replicate solutions of the four NIST standards are

in Table A2.

ANALYTICAL RESULTS

Geochemical Baseline Samples

Geochemical data for total-digestion analyses of the baseline stream-terrace and core samples

are given in table 3. Toxic ore-related trace element concentrations (for example, Pb, As, Cu) are

generally similar to those found in streambed sediments upstream from known mineralization (Pb, near

60 ppm; As, about 45 ppm; Cu, about 50 ppm; Fey and others, 1999b). However, elevated

concentrations of these three ore-related trace elements are found in pre-mining streambed sediments in

Uncle Sam Gulch (site 17B), above the Bullion Mine (site 14B), and in High Ore Creek (site 19B).

Elevated copper concentrations are found at several other sites (table 3). Zinc concentrations are quite

variable throughout the study area as evidenced by the wide range in zinc concentrations among baseline

streambed-sediment samples (Zn, ranges from 40 to 600 ppm; Fey and others, 1999b).

Lead isotopic data (206Pb/204Pb; table 4) show an inverse relationship with lead concentrations

as is observed throughout the study area (Fey and others, 1999b). The highest 206Pb/204Pb values

(approximately 18.1) found among the baseline samples are similar to those found in the streambed

sediments from sites upstream from known historical mining activities. A major exception to the overall

trend is the stream terrace sample collected at the confluence of Basin Creek with the Boulder River

(site 2B). The 206Pb/204Pb of this sample is the lowest in the entire study area, and although it shows
8

low lead and arsenic concentrations (26 ppm and 35 ppm, respectively; table 3), its copper value is the

highest of any of the baseline samples.

Fluvial tailings deposits from site T1

Geochemical data for core-samples of the fluvial tailings collected from site T1, the bar in the

Boulder River below Basin Creek, are in table 5. Ore-related trace element concentrations are

generally more uniform in this fluvial tailings deposit than in those from the other mine-waste sites within

the study area.

Contaminant Source samples

Lead isotopic compositions in samples of fluvial tailings and in streambed sediments collected

from just below major mines are shown in table 6. The overall inverse correlation between 206Pb/204Pb

and lead concentrations observed among other samples from the district (table 4; Fey and others,

1999b) is also observed among the samples in table 6. The most contaminated samples from the Basin

Creek and Cataract Creek drainages (Pb concentrations greater than 1,000 ppm) show a very narrow

range of 206Pb/204Pb, ranging from 17.90 to 17.93. The sample collected below the Comet Mine on

High Ore Creek (site 59S, fig. 1) has 206Pb/204Pb of 18.07, a value found consistently in the High Ore

Creek drainage below the Comet Mine (Fey and others, 1999b). The lead isotopic results indicate that

the mineralization at the Comet Mine is from a different source and/or of a different age than the other

mines in the area.

Geochemical data from the smelter slag sample from the Bullion Smelter are in table 7.

Geochemical data from the mine wastes collected at sites 1T-5T are summarized for the ore-related

trace elements arsenic, cadmium, copper, lead, silver, and zinc in table 8. Statistical summaries and

ranges of compositions are given for all mine waste samples above the concentration ranges given in

table 8. Since the geochemical data for these elements from these sites are highly skewed distributions,

the best estimate of the composition of the deposit would be represented by the median or the

geometric mean concentrations. Complete published geochemical data are in the references given for

each data set in table 8.

Dendrochronology

The age data from tree samples collected at selected stream terrace sites are reported in table

9. Unfortunately, no local dendrochronological record could be constructed from the ring structure of

living trees that would allow dating of the older dead trees. The tree ring structure in living trees is

complacent, that is the variation in the width of the tree rings was consistent from year to year and

provided no markers in the tree ring structure that would allow ages to be assigned (written commun.,

Dec., 1999, Jeff Dean, Laboratory of Tree-Ring Research, Univ. of Arizona, Tucson, Ariz.). Ages

from living trees therefore provide minimum ages of the terraces. These data, along with relevant

historical data (Rossillon and Haynes, 1999), provide minimum ages for some of the stream terrace and

core samples collected for determination of the pre-mining geochemical baseline.
9

REFERENCES CITED

Aamodt, P.L., 1978, Uranium hydrogeochemical and stream sediment pilot study of the Boulder

batholith, Montana: GJBX-56(78), U.S. Dept. of Energy, Grand Junction, Colo., 118 p.

Briggs, P.H., 1996, Forty elements by inductively coupled-plasma atomic emission spectrometry, in

Arbogast, B.F., ed., Analytical methods manual for the Mineral Resources Program: U.S.

Geological Survey Open-File Report 96-525, p. 77-94.

Broxton, W.W., 1980, Uranium hydrogeochemical and stream sediment reconnaissance data release

for the Butte NTMS quadrangle, Montana, including concentrations of forty-two additional

elements: GJBX-129(80), U.S. Dept. of Energy, Grand Junction, Colo., 207 p.

Buxton, H.T., Nimick, D.A., von Guerard, P., Church, S.E., Frazier, A., Gray, J.R., Lipin, B.R.,

Marsh, S.P. Woodward, D., Kimball, B., Finger, S., Ischinger, L., Fordham, J.C., Power,

M.S., Bunck, C., and Jones, J.W., 1997, A science-based Watershed strategy to support

effective remediation of abandoned mine lands: in Fourth International Conference on Acid

Rock Drainage Proceedings, v. IV, Vancouver, B.C. Canada, May 31-June 5, 1997, p. 1869-

1880.

Campbell, W.L., Mcdanal, S.K., and Hopkins, R.T., Jr., 1982, Sample location and analytical data for

samples collected and analyzed as of June 1, 1982, in eight 30-minute divisions of the Butte 1

degree x 2 degree CUSAMAP quadrangle, Montana: U.S. Geological Survey Open-File

Report 82-617-A, 8 p.

Cantanzaro, E.J., Murphy, T.J., Shields, W.R., and Garner, E.L., 1968, Absolute isotopic abundance

ratios of common, equal atom, and radiogenic lead isotopic standards: Journal of Research of

the National Bureau of Standards, v. 72A, p. 261-267.

Chao, T.T., 1984, Use of partial dissolution techniques in geochemical exploration: Journal of

Geochemical Exploration, v. 20, p. 101-135.

Church, S.E., Mosier, E.L., and Motooka, J.M., 1987, Mineralogical basis for the interpretation of

multielement (ICP-AES), oxalic acid, and aqua-regia partial digestions of stream sediments for

reconnaissance exploration geochemistry: Journal of Geochemical Exploration, v. 29, p.

207-233.

Church, S.E., Holmes, C.E., Briggs, P.H., Vaughn, R.B., Cathcart, James, and Marot, Margaret,

1993, Geochemical and lead-isotope data from stream and lake sediments, and cores from the

upper Arkansas River drainage: Effects of mining at Leadville Colorado on heavy-metal

concentrations in the Arkansas River: U.S. Geological Survey Open-File Report 93-534, 61 p.

Church, S.E., Kimball, B.A., Fey, D.L., Ferderer, D.A., Yager, T.J., and Vaughn, R.B., 1997, Source,

transport, and partitioning of metals between water, colloids, and bed sediments of the Animas

River, Colorado: U.S. Geological Survey Open-File Report 97-151, 135 p.

Crock, J.G., Lichte, F.E., and Briggs, 1983, Determination of elements in National Bureau of Standards

geologic reference materials SRM 278 obsidian and SRM 688 basalt by inductively coupled

plasma-atomic emission spectroscopy: Geostandards Newsletter, v. 7, p. 335-340.

Farag, A.M., Woodward, D.F., Skaar, D., and Brumbaugh, W.G., 1999, Characterizing the aquatic

health in the Boulder River watershed, Montana, in Morganwalp, D.W., and Buxton, H.T.,

eds., U.S. Geological Survey Toxic Substances Hydrology Program—Proceedings of the

Technical Meeting, Charleston, South Carolina, March 8-12, 1999—Volume 1 of 3—

Contamination from Hardrock Mining: U.S. Geological Survey Water-Resources Investigations

Report 99-4018A, p. 55-58.

Fey, D.L., and Church, S.E., 1998, Analytical results for 42 fluvial tailings cores and 7 stream sediment

samples from High Ore Creek, northern Jefferson County, Montana: U. S. Geological Survey

Open-File Report 98-215, 49 p.

Fey, D.L., Church, S.E., and Finney, C.J., 1999a, Analytical results for 35 mine-waste tailings cores

and six bed-sediment samples, and an estimate of the volume of contaminated material at

Buckeye Meadow on upper Basin Creek, northern Jefferson County, Montana: U.S.

Geological Survey Open-File Report 99-537, 59 p.

Fey, D.L., Unruh, D.M., and Church, S.E., 1999b, Chemical data and lead isotopic compositions in

stream-sediment samples from the Boulder River watershed, Jefferson County, Montana: U. S.

Geological Survey Open-File Report 99-575, 147 p.
10

Fey, D.L., Church, S.E., and Finney, C.J., 2000, Analytical results for Bullion Mine and Crystal Mine

waste samples and bed sediments from a small tributary to Jack Creek and from Uncle Sam

Gulch, Boulder River watershed, Montana U.S. Geological Survey Open-File Report 00-031,

63 p.

Ludwig, K.R., 1980, Calculation of uncertainties of U-Pb isotope data: Earth and Planetary Science

Letters, v. 46, p. 212-220.

National Institute of Standards and Technology (NIST), 1993a, Certificate of Analysis Standard

Reference Material 2704, Buffalo River Sediment.

______, 1993b, Certificate of Analysis Standard Reference Material 2709, San Joaquin Soil.

______, 1993c, Certificate of Analysis Standard Reference Material 2710 Montana Soil.

______, 1993d Certificate of Analysis Standard Reference Material 2711 Contaminated Montana Soil.

Nimick, D.A., Church, S.E., Cleasby, T.E., Fey, D.L., Kimball, B.A., Leib, K.J., Mast, A.M., and

Wright, W.G., 1999, Characterization of metals in water and bed sediment in two watersheds

affected by historical mining in Montana and Colorado, in Morganwalp, D.W., and Buxton,

H.T., eds., U.S. Geological Survey Toxic Substances Hydrology Program—Proceedings of the

Technical Meeting, Charleston, South Carolina, March 8-12, 1999—Volume 1 of 3—

Contamination from Hardrock Mining: U.S. Geological Survey Water-Resources Investigations

Report 99-4018A, p. 11-18.

Rossillon, M., and Haynes, T., 1999, Basin Creek Mine reclamation heritage resource inventory

1998, [Report for the Beaverhead-Deerlodge National Forest, U.S. Forest Service, Dillon,

Montana]: Renewable Technologies, Inc., Butte, Montana, v. 1, 126 p., v.2, Appendices.

Tatsumoto, M., and Unruh, D.M., 1976, KREEP basalt age: Grain by grain U-Th-Pb systematics study

of the quartz monzodiorite clast 15405,88: Proceedings of the 7th Lunar Science Conference, p.

2107-2129.

Taylor, H.E., Antweiler, R.C., Alpers, C.N., Roth, D.A., Brinton, T.I., Cain, D.J., Ball, J.W., Unruh,

D.M., and Dileanis, P.D., 1999, Quality assurance and control, In: (Alpers, C.N., Taylor,

H.E., and Domagalski, J.L., eds.) Metals transport in the Sacramento River, California, 1996-

1997, Volume 1: Methods and data: Water Resources Investigations Report 99-4286, p. 38-

59.

Todt, W., Cliff, R.A., Hanser, A., and Hofmann, A.W., 1993, Re-calibration of NBS lead standards

using a 202Pb-205Pb double spike: Abstracts presented to the 7th meeting of the European Union

of Geosciences, p. 396.

Unruh, D.M., Hutchison, R., and Tatsumoto, M., 1979, U-Th-Pb age of the Barwell chondrite:

Anatomy of a discordant meteorite: Proceedings of the 10th Lunar and Planetary Science

Conference, p. 1011-1030.

Wilson, S. A., Briggs, P.H., Mee, J.S., and Siems, D.F., 1994, Determinations of thirty-two major and

trace elements in three NIST soil SRMs using ICP-AES and WDXRF: Geostandards

Newsletter, v. 18, p. 85-89.
11

Appendix

The largest contributor to the analytical uncertainty of the lead isotopic analyses of common lead

is the mass fractionation induced during mass spectrometry (Ludwig, 1980). The effects of the mass

fractionation are monitored by lead isotopic analyses of NIST standard SRM-981 (Cantanzaro and others,

1968; Todt and others, 1993). Results of replicate analyses of the SRM lead standards are shown in Table

A1. A mass-fractionation factor, δ, is calculated from the standard runs from each of the three isotopic

ratios 206Pb/204Pb, 207Pb/206Pb, and 208Pb/206Pb in the following manner (Ludwig, 1980):

δ = {(206Pb/204Pbt /206Pb/204Pbm)-1}/2

δ = (207Pb/206Pbt /207Pb/206Pbm)-1

δ = {(208Pb/206Pbt /208Pb/206Pbm)-1}/2

where the subscripts “t” and “m” refer to the true (certified) and measured values, respectively. The

average of the three values is used to correct sample data for mass fractionation. Corrections to the raw

sample data are applied using a linear fractionation correction in the following manner (Ludwig, 1980):

206Pb/204Pbc = 206Pb/204Pbm * (1+ 2 * δ)

207Pb/206Pbc = 207Pb/206Pbm * (1+ δ)

208Pb/206Pbc = 208Pb/206Pbm * (1+ 2 * δ)

where the subscripts “c” and “m” denote corrected and raw measured data, respectively. Many of the

standards were run at different temperatures to assess the effects of running temperature on mass

fractionation. Standards run at higher temperatures (>1250°C) show a mean δ-value of 0.12 percent/amu

(atomic mass unit) whereas standards run at lower temperatures indicate a larger correction of 0.14

percent/amu is required.

 An uncertainty in the mass fractionation correction of ± 0.03 percent/amu is applied to the

corrected sample data and represents the 2-sigma external variation of the entire data set. Overall

uncertainties in the lead isotopic data reported in table 4 and 6 are calculated in the manner given by

Ludwig (1980) and represent the uncertainties at the 95% confidence interval (approximately 2σm).

Because the analytical blank does not significantly affect the measured isotopic compositions, the

analytical uncertainty in an individual corrected ratio, Rc, is calculated in the following manner (Ludwig,

1980):

ΣRc

2

 = ΣRm

2

 + (Δm * σδ)2

where 100 * Σ is the percent uncertainty, ΣRm is the uncertainty in the measured ratio from mass

spectrometry, Δm is the nominal mass difference between the isotopes in the numerator and denominator

(i.e. for 206Pb/204Pb, Δm = 2) and σδ = 0.0003 (0.03 percent/100 from above).

As a test of the reproducibility of the leaching procedure, separate leachates of 4 NIST standards

have been analyzed. Results are shown in table A2. Uncertainties have been calculated based on the

procedure outlined above. The data are reproducible to within a total range of 0.2 percent in 206Pb/204Pb

for each standard. Also shown are the lead isotopic data for leachates of three of the samples reported by

Church and others (1997).
12

Table A1. Lead isotopic compositions in replicate analyses of NIST Standard SRM-981

[Uncertainties are in percent and represent 2 sigma-mean for the individual runs and 2 sigma for the mean values of each group]

Run T

206Pb Uncertainty 207Pb Uncertainty 208Pb Uncertainty

No. (°C) 204Pb 2s mean

(percent)

206Pb 2s mean

(percent)

206Pb 2s mean

(percent)

Certified value116.9322 0.0047 0.914561 0.0044 2.16662 0.0060

VG Sector 54 Mass Spectrometer

981-1 1196 16.8811 0.0117 0.913193 0.0030 2.16088 0.0030

981-2 1160 16.8871 0.0099 0.913319 0.0036 2.16088 0.0030

981-2 1236 16.8918 0.0087 0.913358 0.0027 2.16129 0.0039

981-4 1203 16.8950 0.0540 0.913293 0.0087 2.16105 0.0075

981-5 1185 16.8806 0.0184 0.913163 0.0054 2.15990 0.0036

981-6 1191 16.8837 0.0099 0.913184 0.0030 2.16029 0.0030

981-7 1194 16.8852 0.0093 0.913227 0.0033 2.16036 0.0033

981-7 1237 16.8883 0.0123 0.913303 0.0033 2.16094 0.0033

981-9 1191 16.8852 0.0150 0.913168 0.0045 2.16020 0.0039

981-9 1235 16.8850 0.0120 0.913200 0.0030 2.16040 0.0036

981-10 1195 16.8854 0.0100 0.913262 0.0036 2.16041 0.0048

981-11 1203 16.8836 0.0150 0.913190 0.0039 2.15991 0.0036

981-14 1189 16.8899 0.0054 0.913313 0.0018 2.16110 0.0039

981-14 1230 16.9070 0.0060 0.913615 0.0027 2.16334 0.0027

981-15 1186 16.8844 0.0120 0.913168 0.0045 2.16012 0.0039

981-16 1200 16.8840 0.0190 0.913079 0.0036 2.16006 0.0036

981-17 1201 16.8943 0.0230 0.913288 0.0045 2.16109 0.0048

981-17 1196 16.8870 0.0210 0.913331 0.0066 2.16076 0.0114

981-18 1203 16.8821 0.0132 0.913175 0.0036 2.16031 0.0030

981-19 1176 16.8905 0.0072 0.913243 0.0021 2.16082 0.0033

981-19 1219 16.8956 0.0084 0.913376 0.0024 2.16159 0.0039

981-20 1196 16.8886 0.0150 0.913188 0.0027 2.16074 0.0054

981-22 1204 16.8950 0.0130 0.913284 0.0039 2.16141 0.0063

981-23 1203 16.8847 0.0090 0.913188 0.0039 2.16034 0.0048

981-24 1193 16.8823 0.0120 0.913137 0.0027 2.16013 0.0033

981-25 1188 16.8870 0.0220 0.913291 0.0060 2.16082 0.0042

981-26 1188 16.8943 0.0240 0.913271 0.0051 2.16110 0.0033

981-28 1193 16.8957 0.0150 0.913357 0.0036 2.16166 0.0036

981 99-1 1201 16.8885 0.0150 0.913261 0.0042 2.16082 0.0048

981 99-2 1193 16.8903 0.0096 0.913280 0.0027 2.16091 0.0027

981 99-3 1197 16.8910 0.0150 0.913323 0.0039 2.16118 0.0036

981 99-4 1199 16.8846 0.0150 0.913221 0.0027 2.16056 0.0033

981 99-5 1194 16.8889 0.0300 0.913156 0.0051 2.16031 0.0045

981 99-6 1189 16.8848 0.0168 0.913175 0.0036 2.16036 0.0039

981 99-7 1223 16.8878 0.0190 0.913237 0.0036 2.16071 0.0033

981 99-9 1189 16.8848 0.0168 0.913175 0.0036 2.16036 0.0039

981 99-10 1175 16.8860 0.0240 0.913218 0.0060 2.16023 0.0051

981 99-11 1200 16.8855 0.0190 0.913141 0.0039 2.16048 0.0042

981 99-12 1194 16.8856 0.0110 0.913192 0.0039 2.16031 0.0030

981 99-13 1189 16.8818 0.0120 0.913137 0.0039 2.16015 0.0042

981 99-14 1195 16.8808 0.0330 0.913092 0.0630 2.16017 0.0057

981 99-15 1192 16.8872 0.0150 0.913205 0.0039 2.16063 0.0039

981 99-16 1188 16.8881 0.0102 0.913236 0.0033 2.16092 0.0048

981 99-17 1197 16.8901 0.0246 0.913382 0.0045 2.16122 0.0048

981 99-18 1200 16.8926 0.0220 0.913290 0.0039 2.16109 0.0045

Mean216.8873 0.0460 0.913236 0.0160 2.16066 0.0410
13

Table A1. Lead isotopic compositions in replicate analyses of NIST Standard SRM-981—continued

Run T

206Pb Uncertainty 207Pb Uncertainty 208Pb Uncertainty

No. (°C) 204Pb 2s mean

(percent)

206Pb 2s mean

(percent)

206Pb 2s mean

(percent)

981-1 1272 16.8876 0.0093 0.913253 0.0033 2.16092 0.0063

981-3 1252 16.8835 0.0087 0.913136 0.0030 2.16014 0.0042

981-3 1288 16.8900 0.0084 0.913271 0.0021 2.16102 0.0054

981-4 1316 16.8960 0.0175 0.913488 0.0057 2.16225 0.0036

981-5 1319 16.8838 0.0075 0.913174 0.0027 2.16032 0.0057

981-8 1260 16.8900 0.0084 0.913296 0.0030 2.16096 0.0057

981-10 1271 16.8988 0.0069 0.913495 0.0024 2.16210 0.0063

981-11 1271 16.8934 0.0150 0.913343 0.0048 2.16117 0.0120

981-15 1290 16.8903 0.0100 0.913265 0.0039 2.16075 0.0054

981-16 1250 16.9000 0.0078 0.913453 0.0027 2.16219 0.0051

981-17 1299 16.8936 0.0130 0.913376 0.0036 2.16136 0.0069

981-18 1288 16.8887 0.0081 0.913323 0.0030 2.16124 0.0054

981-20 1310 16.9045 0.0084 0.913578 0.0039 2.16309 0.0045

981-21 1292 16.8868 0.0300 0.913372 0.0078 2.16148 0.0118

981-22 1301 16.9021 0.0099 0.913365 0.0033 2.16210 0.0066

981-24 1288 16.8933 0.0120 0.913320 0.0036 2.16141 0.0090

981-26 1301 16.8910 0.0081 0.913213 0.0036 2.16098 0.0036

981-27 1279 16.8824 0.0190 0.913069 0.0036 2.16018 0.0036

981 99-1 1318 16.9031 0.0180 0.913515 0.0057 2.16269 0.0150

981 99-2 1299 16.8995 0.0057 0.913485 0.0024 2.16222 0.0039

981 99-3 1286 16.8986 0.0072 0.913463 0.0021 2.16214 0.0042

981 99-5 1288 16.8829 0.0150 0.913153 0.0033 2.16017 0.0039

981 99-6 1289 16.8950 0.0090 0.913382 0.0027 2.16158 0.0042

981 99-7 1302 16.8913 0.0110 0.913325 0.0024 2.16134 0.0045

981 99-8 1292 16.9085 0.0420 0.913741 0.0075 2.16411 0.0052

981 99-9 1289 16.8950 0.0090 0.913382 0.0027 2.16158 0.0042

981 99-10 1313 16.8860 0.0075 0.913244 0.0033 2.16049 0.0048

981 99-11 1302 16.9011 0.0420 0.913406 0.0072 2.16236 0.0069

981 99-13 1292 16.8938 0.0090 0.913345 0.0033 2.16160 0.0066

981 99-17 1301 16.9020 0.0051 0.913574 0.0021 2.16277 0.0021

981 99-18 1301 16.8989 0.0099 0.913442 0.0030 2.16208 0.0036

Mean316.8938 0.0690 0.913360 0.0230 2.16149 0.0590

Micro Mass 54R Mass spectrometer

981-54R-1 1245 16.8991 0.0190 0.913400 0.0120 2.16084 0.0160

981-54R-1 1310 16.9038 0.0420 0.913643 0.0120 2.16249 0.0370

981-54R-2 1235 16.8834 0.0240 0.913313 0.0090 2.16071 0.0060

981-54R-2 1335 16.8927 0.0130 0.913408 0.0060 2.16113 0.0910

Mean ± 2σ 16.8950 0.0980 0.913440 0.0260 2.16116 0.0410

1Certified value from Todt and others (1993)

2Mean value for mass spectrometer runs at low temperature ± 2σ (percent); average temperature was 1198 ± 15°C

3Mean value for mass spectrometer runs at high temperature ± 2σ (percent); average temperature 1291 ± 18°C
14

Table A2. Lead isotopic compositions in NIST standards SRM 2704, SRM 2709, SRM 2710, and SRM 2711

[Data are corrected for mass fractionation; uncertainties are absolute and are calculated in the manner of Ludwig, (1980)]

Sample1 206Pb/204Pb 207Pb/204Pb 208Pb/204Pb 207Pb/206Pb 208Pb/206Pb

SRM-2704-1 18.777 ± 0.011 15.634 ± 0.014 38.433 ± 0.046 0.83172 ± 0.00025 2.0469 ± 0.0012

SRM-2704-2 18.819 ± 0.011 15.665 ± 0.014 38.544 ± 0.046 0.83148 ± 0.00025 2.0482 ± 0.0012

SRM-2704-3 18.799 ± 0.012 15.641 ± 0.014 38.466 ± 0.046 0.83112 ± 0.00025 2.0462 ± 0.0012

SRM-2704-4 18.788 ± 0.012 15.631 ± 0.016 38.438 ± 0.047 0.83103 ± 0.00041 2.0458 ± 0.0012

SRM-2709-1 19.087 ± 0.013 15.674 ± 0.015 38.964 ± 0.048 0.82028 ± 0.00026 2.0413 ± 0.0012

SRM-2709-2 19.077 ± 0.012 15.668 ± 0.014 38.939 ± 0.047 0.82042 ± 0.00025 2.0412 ± 0.0012

SRM-2709-3 19.060 ± 0.012 15.652 ± 0.014 38.862 ± 0.047 0.82029 ± 0.00025 2.0390 ± 0.0012

SRM-2709-4a 19.059 ± 0.012 15.652 ± 0.015 38.879 ± 0.048 0.82049 ± 0.00026 2.0399 ± 0.0013

SRM-2709-4b 19.050 ± 0.013 15.646 ± 0.016 38.864 ± 0.049 0.82057 ± 0.00029 2.0401 ± 0.0012

Church and others (1997) 19.065 15.646 38.864

SRM-2710-1 17.818 ± 0.011 15.533 ± 0.014 38.126 ± 0.046 0.87095 ± 0.00026 2.1397 ± 0.0013

SRM-2710-2 17.806 ± 0.011 15.518 ± 0.014 38.078 ± 0.046 0.87056 ± 0.00026 2.1385 ± 0.0013

SRM-2710-3 17.800 ± 0.011 15.509 ± 0.014 38.047 ± 0.046 0.87053 ± 0.00026 2.1375 ± 0.0013

Church and others (1997) 17.819 15.537 38.141

SRM-2711-1 17.102 ± 0.010 15.437 ± 0.014 36.947 ± 0.044 0.90165 ± 0.00027 2.1604 ± 0.0013

SRM-2711-2 17.105 ± 0.010 15.438 ± 0.014 36.956 ± 0.045 0.90176 ± 0.00027 2.1606 ± 0.0013

SRM-2711-3 17.118 ± 0.010 15.460 ± 0.014 37.021 ± 0.045 0.90233 ± 0.00027 2.1628 ± 0.0013

Church and others (1997) 17.086 15.419 36.888

Church and others (1997) 17.097 15.430 36.936

1Subsample numbers 1-4 denote separate leaches. Samples SRM-2709- 4a and -4b are separate chemical separations of the same leach.