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Division of Geological & Geophysical Surveys RAW-DATA FILE 2014-16 Zircon U-Pb Age Data, Alaska Highway Corridor, Tanacross and Nabesna quadrangles, Alaska by Diana N. Solie, Paul O’Sullivan, Melanie B. Werdon, Larry K. Freeman, Rainer J. Newberry, David J. Szumigala, and Trent D. Hubbard $3.00 July 2014 THIS REPORT HAS NOT BEEN REVIEWED FOR TECHNICAL CONTENT OR FOR CONFORMITY TO THE EDITORIAL STANDARDS OF DGGS Released by STATE OF ALASKA DEPARTMENT OF NATURAL RESOURCES Division of Geological & Geophysical Surveys 3354 College Road Fairbanks, Alaska 99709-3707

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Page 1: Zircon U-Pb Age Data, Alaska Highway Corridor, Tanacross ...dggs.alaska.gov/webpubs/dggs/rdf/text/rdf2014_016.pdf · Zircon U-Pb Age Data, Alaska Highway Corridor, Tanacross and Nabesna

Division of Geological & Geophysical Surveys

RAW-DATA FILE 2014-16

Zircon U-Pb Age Data, Alaska Highway Corridor,

Tanacross and Nabesna quadrangles, Alaska

by

Diana N. Solie, Paul O’Sullivan, Melanie B. Werdon, Larry K. Freeman,

Rainer J. Newberry, David J. Szumigala, and Trent D. Hubbard

$3.00

July 2014

THIS REPORT HAS NOT BEEN REVIEWED FOR

TECHNICAL CONTENT OR FOR CONFORMITY TO

THE EDITORIAL STANDARDS OF DGGS

Released by

STATE OF ALASKA

DEPARTMENT OF NATURAL RESOURCES

Division of Geological & Geophysical Surveys

3354 College Road

Fairbanks, Alaska 99709-3707

Page 2: Zircon U-Pb Age Data, Alaska Highway Corridor, Tanacross ...dggs.alaska.gov/webpubs/dggs/rdf/text/rdf2014_016.pdf · Zircon U-Pb Age Data, Alaska Highway Corridor, Tanacross and Nabesna
Page 3: Zircon U-Pb Age Data, Alaska Highway Corridor, Tanacross ...dggs.alaska.gov/webpubs/dggs/rdf/text/rdf2014_016.pdf · Zircon U-Pb Age Data, Alaska Highway Corridor, Tanacross and Nabesna

TABLE OF CONTENTS

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

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

Methodology ................................................................................................................................................................. 1

Field Methods ............................................................................................................................................................ 1

Analytical Methods .................................................................................................................................................... 2

Analytical Results ........................................................................................................................................................... 2

Igneous Rocks ............................................................................................................................................................ 2

Metamorphic Rocks ................................................................................................................................................... 2

Detrital Zircons .......................................................................................................................................................... 2

Acknowledgments ......................................................................................................................................................... 2

References Cited ............................................................................................................................................................ 3

Appendix A: Data plots for individual samples .............................................................................................................. 5

09MBW247A:......................................................................................................................................................... 5

09LF454A: .............................................................................................................................................................. 6

09TDH75A: ............................................................................................................................................................. 7

09LF279A: .............................................................................................................................................................. 8

09Z213A: ................................................................................................................................................................ 9

09LF441A: ............................................................................................................................................................ 10

09TDH74A: ........................................................................................................................................................... 11

09MBW103A:....................................................................................................................................................... 12

09LF419A: ............................................................................................................................................................ 13

09Z172B: .............................................................................................................................................................. 14

09LF254A: ............................................................................................................................................................ 15

09LF433A: ............................................................................................................................................................ 16

09LF647A: ............................................................................................................................................................ 17

09LF637A: ............................................................................................................................................................ 18

09LF644A: ............................................................................................................................................................ 19

09MBW338A:....................................................................................................................................................... 20

09LF206A: ............................................................................................................................................................ 21

09MBW400A:....................................................................................................................................................... 22

09MBW243A:....................................................................................................................................................... 23

09LF233A: ............................................................................................................................................................ 24

09LF234A: ............................................................................................................................................................ 25

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09RN242A: ........................................................................................................................................................... 26

Appendix B: Zircon U-Pb Dating Methodology ............................................................................................................ 27

Sample Preparation ................................................................................................................................................. 27

LA-ICP-MS Session Details ....................................................................................................................................... 27

U-Pb Data Analysis ................................................................................................................................................... 27

Moving-Median Smoothing ..................................................................................................................................... 28

Appendix C: Zircon age standards ............................................................................................................................... 29

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RDF 2014- P a g e | 1

ZIRCON U-PB AGE DATA, ALASKA HIGHWAY CORRIDOR,

TANACROSS AND NABESNA QUADRANGLES, ALASKA

by

Diana N. Solie1, Paul O’Sullivan2, Melanie B. Werdon1, Larry K. Freeman1,

Rainer J. Newberry3, David J. Szumigala1, and Trent D. Hubbard1

ABSTRACT

Twenty-two igneous and metamorphic rock samples were collected in a 20-km-long swath centered on the Alaska

Highway between Tetlin Junction, Alaska, and the Canada border. The 15 felsic plutonic rock samples and one gabbro

sample yield Cretaceous zircon U-Pb weighted-mean ages ranging from 95.7 Ma to 106.2 Ma. Zircons from a

metadiorite yield a Triassic weighted-mean age of about 241.9 Ma. Metamorphic zircons from two samples with

felsic igneous protoliths yield Mississippian weighted-mean ages of 351.7 Ma and 354.6 Ma. Detrital zircons from

two metaconglomerates yield individual grain ages from 100 Ma to 1,811 Ma, but are predominantly between 300

Ma and 345 Ma. Detrital zircons from a quartzite yield peaks at about 2,648 Ma, 1,946 Ma, and 1,807 Ma.

INTRODUCTION

The Alaska Division of Geological & Geophysical Surveys (DGGS) conducted a multi-year project (from 2006 through

2010) studying the geology and geologic hazards along the Alaska Highway corridor (Solie and Burns, 2007). As part

of the bedrock geologic mapping, samples were collected for geochronologic analyses using 40Ar/39Ar, fission-track,

and U-Pb dating techniques. Summaries of analytical results appear on bedrock-geologic maps that are being

published in three segments. This report supplies the supporting data for the U-Pb age results from the easternmost

segment of the project, in the Tanacross and Nabesna quadrangles.

DGGS mapped the easternmost segment of the Alaska Highway corridor, from Tetlin Junction to the Canada

border, in 2009. Twenty-two igneous and metamorphic rock samples were submitted to the Apatite to Zircon, Inc.

laboratory (A2Z), where U-Pb age analysis was performed by Paul O’Sullivan in 2011. The resulting data, excerpted

from the laboratory report, are presented in this publication. All data are available from the DGGS website

(http://dggs.alaska.gov/pubs) at no charge.

METHODOLOGY

Field Methods

DGGS field geologists collected rock samples from the surface or within 0.5 m of the surface. Care was taken to

collect fresh, unweathered samples representative of rock types in the map area. Locations were recorded using

hand-held GPS units with an estimated horizontal accuracy of approximately 10 m. Location coordinates for all

dated samples are provided in an accompanying .csv file, in North American Datum of 1927 decimal degrees. This

file also contains brief descriptions of each sample based on field observations.

1 Alaska Division of Geological & Geophysical Surveys, 3354 College Road, Fairbanks AK 99709-3707 2 Apatite to Zircon, Inc., 1075 Matson Road, Viola, ID 83872-9709 3 University of Alaska Fairbanks, Department of Geology & Geophysics, P.O. Box 755780, Fairbanks AK 99775-5780

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RDF 2014- P a g e | 2

ANALYTICAL METHODS

DGGS submitted selected rock samples to Apatite to Zircon, Inc. in 2011. Paul O’Sullivan directed the processing

and analyses of the samples in the A2Z laboratory. Laser ablation–inductively coupled plasma–mass spectrometry

(LA–ICP–MS) analyses were performed at the Geoanalytical Laboratory, Washington State University, Pullman,

Washington, U.S.A. Detailed discussion of laboratory techniques is provided in appendices to this report.

ANALYTICAL RESULTS

Twenty-two rock samples were analyzed. Data plots for each sample are provided in Appendix A, from youngest to

oldest.

IGNEOUS ROCKS

Sixteen of the analyzed samples were igneous rocks. Fifteen were felsic plutonic rocks, either granite, granodiorite,

or quartz monzonite; the other was gabbro. The weighted-mean age of all measurements from zircons in each

igneous sample are recorded in the accompanying .csv table. All 16 ages fall within a span of about 10.5 Ma,

between 95.7 ± 2.5 Ma (09MBW247A) and 106.2 ± 2.8 Ma (09MBW338A). There is no apparent pattern to the age

distribution across the map area, or correlation of rock type with age. The mafic igneous rock, a gabbro

(09LF647A), yields a U-Pb weighted-mean age of 103.8 ± 2.7 Ma.

METAMORPHIC ROCKS

A mafic sample from the southern map area, described in the field as diorite or possibly amphibolite with no

foliation (09LF206A), yields an age distribution between 1,372 Ma and 114 Ma. We interpret these results to

include lead loss yielding the younger measurements, and the weighted-mean age (based on 20 of 42

measurements) yields a Triassic age of 241.9 ± 13.5 Ma.

Two metamorphosed felsic igneous rocks from the northern half of the map area were dated as lower

Mississippian and upper Devonian. One, a metarhyolite (09MBW400A), yielded a weighted-mean age of 351.7 ±

9.3 Ma based on 49 tightly grouped zircon measurements. The other, a granitic orthogneiss (09MBW243A), yielded

a weighted-mean age of 354.6 ± 9.3 Ma based on 45 zircon measurements.

DETRITAL ZIRCONS

Detrital zircons from two metaconglomerate samples collected in the southern map area yield ages that are mostly

younger than 350 Ma. Sample 09LF234A yielded two measurements around 1,800 Ma, and another around 225

Ma; the other 17 measurements are Carboniferous, between ~300 Ma and 345 Ma. Sample 09LF233A yielded two

zircon measurements of ~100 Ma, and 321 Ma.

Detrital zircons from a quartzite collected about 3 km from the Canada border (09RN242A) yield a significantly

older age distribution, with measurements ranging from ~3,000 Ma to 1,030 Ma. The largest peak in the

distribution (see plots in Appendix A) is at 1,807 Ma, with two smaller but prominent peaks at 1,946 Ma and 2,648

Ma.

ACKNOWLEDGMENTS

This project was supported by Alaska State Capital Improvement Project funds. Samples used in this report were

collected by Larry Freeman, Melanie Werdon, David Szumigala, and Trent Hubbard of DGGS; and Rainer Newberry

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RDF 2014- P a g e | 3

of the University of Alaska Fairbanks Department of Geology and Geophysics. Margaret Donelick and Jim McMillan

(A2Z) provided technical assistance with sample preparation; Charles Knaack (Washington State University) provided

technical assistance with LA-ICP-MS data collection; Paul O’Sullivan and Ray Donelick (A2Z) provided valuable

assistance with LA-ICP-MS data interpretation.

REFERENCES CITED

Black, L.P., Kamo, S.L., Allen, C.M., Davis, D.W., Aleinikoff, J.N., Valley, J.W., Mundil, Roland, Campbell, I.H., Korsch,

R.J., Williams, I.S., and Foudoulis, Chris, 2004, Improved 206Pb/238U microprobe geochronology by the monitoring

of trace-element-related matrix effect—SHRIMP, ID-TIMS, ELA-ICP-MS, and oxygen isotope documentation for

a series of zircon standards: Chemical Geology, v. 205, p. 15–140.

Chang, Zhaoshan, Vervoort, J.D., McClelland, W.C., and Knaack, Charles, 2006, U-Pb dating of zircon by LA-ICP-MS:

Geochemistry, Geophysics, Geosystems, American Geophysical Union, v. 7, no. 5, 14 p.,

doi:10.1029/2005GC001100.

Chew, D.M., and Donelick, R.A., 2012, Combined apatite fission track and U-Pb dating by LA-ICP-MS and its

application in apatite provenance analysis: Mineralogical Association of Canada Short Course, v. 42, p. 219–247.

Donelick, R.A, O’Sullivan, P.B., and Ketcham, R.A., 2005, Apatite fission-track analysis: Reviews in Mineralogy and

Geochemistry, Mineralogical Society of America, v. 58, p. 49–94.

Gehrels, G.E., Valencia, V.A., and Ruiz, J., 2008, Enhanced precision, accuracy, efficiency, and spatial resolution of U-

Pb ages by laser ablation–multicollector–inductively coupled plasma–mass spectrometry: Geochemistry

Geophysics Geosystems, American Geophysical Union, v. 9, 13 p.

Kuiper, K.F., Deino, A., Hilgen, P.J., Krijgsman, W., Renne, P.R., and Wijbrans, J.R., 2008, Synchronizing rock clocks of

Earth history: Science, v. 320, p. 500–504.

Lanphere, M.A., and Baadsraard, H., 2001, Precise K-Ar, 40Ar/39Ar, Rb-Sr and U-Pb mineral ages from the 27.5 Ma

Fish Canyon Tuff reference standard: Chemical Geology, v. 175, p. 653–671.

Paces, J.B., and Miller, J.D., 1993, Precise U-Pb ages of Duluth Complex and related mafic intrusions, northeastern

Minnesota—Geochronological insights to physical, petrogenic, paleomagnetic, and tectonomagmatic processes

associated with the 1.1 Ga Midcontinent Rift System: Journal of Geophysical Research, v. 98, no. B8, p. 13,997–

14,013.

Paton, C., Woodhead, J.D., Hellstrom, J.C., Hergt, J.M., Greig, A., and Maas, R., 2010, Improved laser ablation U-Pb

zircon geochronology through robust downhole fractionation correction: Geochemistry, Geophysics,

Geosystems, v. 11, no. Q0AA06, doi:10.1029/2009GC002618.

Renne, P.R., Swisher, C.C., Deino, A.L., Karner, D.B., Owens, T.L., and DePaolo, D.J., 1998, Intercalibration of

standards, absolute ages and uncertainties in 40Ar/39Ar dating: Chemical Geology, v. 45, p. 117–152.

Solie, D.N., and Burns, L.E., 2007, Alaska Highway corridor geology and geophysics: Alaska GeoSurvey News, v. 10,

no. 1, p. 1–4.

Steiger, R.H., and Jäger, E., 1977, Subcommission on geochronology—Convention on the use of decay constants in

geo- and cosmochronology: Earth and Planetary Science Letters, v. 36, p. 369–371.

Zhang, M., Ewing, R.C., Boatner, L.A., Salje, E.K.H., Weber, W.J., Daniel, P., Zhang, Y., and Farnan, I., 2009, Pb*

irradiation of synthetic zircon (ZrSiO4); Infrared spectroscopic study—Reply: American Mineralogist, v. 94, p.

856–858.

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RDF 2014- P a g e | 4

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RDF 2014- P a g e | 5

APPENDIX A: DATA PLOTS FOR INDIVIDUAL SAMPLES

09MBW247A:

0

100

200

300

400

500

600

0 500 1000 1500 2000 2500 3000

Re

lati

ve A

ge F

req

uen

cy

U-Pb Age (Ma)

09MBW247Ahistogram

pdf

0

100

200

300

400

500

600

0 500 1000 1500 2000 2500 3000

Re

lati

ve A

ge F

req

uen

cy

U-Pb Age (Ma)

09MBW247A gauss pdf

0.00

0.05

0.10

0.15

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0.25

0.30

0.35

0.40

0.45

0.50

0 500 1000 1500 2000 2500 3000

Fre

qu

en

cy

U-Pb Age (Ma)

09MBW247A peak

0.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

5.0

0

100

200

300

400

500

600

0 500 1000 1500 2000 2500 3000

U/T

h (

blu

e p

oin

ts)

Re

lati

ve A

ge F

req

uen

cy (r

ed

cu

rve)

U-Pb Age (Ma)

09MBW247Apdf

U/Th

0.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

5.0

0 500 1000 1500 2000 2500 3000

U/T

h

U-Pb Age (Ma)

09MBW247A U/Th

0

1000

2000

3000

4000

5000

6000

7000

0 500 1000 1500 2000 2500 3000

U p

pm

U-Pb Age (Ma)

09MBW247A U ppm

0

200

400

600

800

1000

1200

1400

1600

1800

0 500 1000 1500 2000 2500 3000

Th p

pm

U-Pb Age (Ma)

09MBW247A Th ppm

0

500

1000

1500

2000

2500

3000

3500

4000

4500

5000

0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000

Low

er-

Age

Inte

rcep

t (M

a)

Upper-Age Intercept (Ma)

09MBW247A

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RDF 2014- P a g e | 6

09LF454A:

0

50

100

150

200

250

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350

400

450

500

0 500 1000 1500 2000 2500 3000

Re

lati

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ge F

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uen

cy

U-Pb Age (Ma)

09LF454Ahistogram

pdf

0

50

100

150

200

250

300

350

400

450

500

0 500 1000 1500 2000 2500 3000

Re

lati

ve A

ge F

req

uen

cy

U-Pb Age (Ma)

09LF454A gauss pdf

0.00

0.10

0.20

0.30

0.40

0.50

0.60

0 500 1000 1500 2000 2500 3000

Fre

qu

en

cy

U-Pb Age (Ma)

09LF454A peak

0.0

1.0

2.0

3.0

4.0

5.0

6.0

0

50

100

150

200

250

300

350

400

450

500

0 500 1000 1500 2000 2500 3000

U/T

h (

blu

e p

oin

ts)

Re

lati

ve A

ge F

req

uen

cy (r

ed

cu

rve)

U-Pb Age (Ma)

09LF454Apdf

U/Th

0.0

1.0

2.0

3.0

4.0

5.0

6.0

0 500 1000 1500 2000 2500 3000

U/T

h

U-Pb Age (Ma)

09LF454A U/Th

0

2000

4000

6000

8000

10000

12000

0 500 1000 1500 2000 2500 3000

U p

pm

U-Pb Age (Ma)

09LF454A U ppm

0

500

1000

1500

2000

2500

3000

3500

4000

4500

0 500 1000 1500 2000 2500 3000

Th p

pm

U-Pb Age (Ma)

09LF454A Th ppm

0

500

1000

1500

2000

2500

3000

3500

4000

4500

5000

0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000

Low

er-

Age

Inte

rcep

t (M

a)

Upper-Age Intercept (Ma)

09LF454A

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RDF 2014- P a g e | 7

09TDH75A:

0

50

100

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450

0 500 1000 1500 2000 2500 3000

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U-Pb Age (Ma)

09TDH075histogram

pdf

0

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250

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450

0 500 1000 1500 2000 2500 3000

Re

lati

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uen

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U-Pb Age (Ma)

09TDH075 gauss pdf

0.00

0.10

0.20

0.30

0.40

0.50

0.60

0 500 1000 1500 2000 2500 3000

Fre

qu

en

cy

U-Pb Age (Ma)

09TDH075 peak

0.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

0

50

100

150

200

250

300

350

400

450

0 500 1000 1500 2000 2500 3000

U/T

h (

blu

e p

oin

ts)

Re

lati

ve A

ge F

req

uen

cy (r

ed

cu

rve)

U-Pb Age (Ma)

09TDH075pdf

U/Th

0.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

0 500 1000 1500 2000 2500 3000

U/T

h

U-Pb Age (Ma)

09TDH075 U/Th

0

100

200

300

400

500

600

700

800

900

1000

0 500 1000 1500 2000 2500 3000

U p

pm

U-Pb Age (Ma)

09TDH075 U ppm

0

100

200

300

400

500

600

0 500 1000 1500 2000 2500 3000

Th p

pm

U-Pb Age (Ma)

09TDH075 Th ppm

0

500

1000

1500

2000

2500

3000

3500

4000

4500

5000

0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000

Low

er-

Age

Inte

rcep

t (M

a)

Upper-Age Intercept (Ma)

09TDH075

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RDF 2014- P a g e | 8

09LF279A:

0

50

100

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400

0 500 1000 1500 2000 2500 3000

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U-Pb Age (Ma)

09LF279Ahistogram

pdf

0

50

100

150

200

250

300

350

400

0 500 1000 1500 2000 2500 3000

Re

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U-Pb Age (Ma)

09LF279A gauss pdf

0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.40

0.45

0.50

0 500 1000 1500 2000 2500 3000

Fre

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en

cy

U-Pb Age (Ma)

09LF279A peak

0.0

1.0

2.0

3.0

4.0

5.0

6.0

0

50

100

150

200

250

300

350

400

0 500 1000 1500 2000 2500 3000

U/T

h (

blu

e p

oin

ts)

Re

lati

ve A

ge F

req

uen

cy (r

ed

cu

rve)

U-Pb Age (Ma)

09LF279Apdf

U/Th

0.0

1.0

2.0

3.0

4.0

5.0

6.0

0 500 1000 1500 2000 2500 3000

U/T

h

U-Pb Age (Ma)

09LF279A U/Th

0

1000

2000

3000

4000

5000

6000

7000

8000

0 500 1000 1500 2000 2500 3000

U p

pm

U-Pb Age (Ma)

09LF279A U ppm

0

500

1000

1500

2000

2500

3000

3500

4000

4500

0 500 1000 1500 2000 2500 3000

Th p

pm

U-Pb Age (Ma)

09LF279A Th ppm

0

500

1000

1500

2000

2500

3000

3500

4000

4500

5000

0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000

Low

er-

Age

Inte

rcep

t (M

a)

Upper-Age Intercept (Ma)

09LF279A

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RDF 2014- P a g e | 9

09Z213A:

0

50

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150

200

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350

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450

500

0 500 1000 1500 2000 2500 3000

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U-Pb Age (Ma)

09Z213Ahistogram

pdf

0

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100

150

200

250

300

350

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450

500

0 500 1000 1500 2000 2500 3000

Re

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U-Pb Age (Ma)

09Z213A gauss pdf

0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.40

0 500 1000 1500 2000 2500 3000

Fre

qu

en

cy

U-Pb Age (Ma)

09Z213A peak

0.0

2.0

4.0

6.0

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h (

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Re

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ed

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U-Pb Age (Ma)

09Z213Apdf

U/Th

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09Z213A U/Th

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09Z213A U ppm

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U-Pb Age (Ma)

09Z213A Th ppm

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Inte

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Upper-Age Intercept (Ma)

09Z213A

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RDF 2014- P a g e | 10

09LF441A:

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09LF441Ahistogram

pdf

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09LF441A gauss pdf

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09LF441A peak

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U-Pb Age (Ma)

09LF441Apdf

U/Th

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09LF441A U/Th

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09LF441A U ppm

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09LF441A Th ppm

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Inte

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a)

Upper-Age Intercept (Ma)

09LF441A

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RDF 2014- P a g e | 11

09TDH74A:

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09TDH074histogram

pdf

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09TDH074 gauss pdf

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09TDH074 peak

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U-Pb Age (Ma)

09TDH074pdf

U/Th

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09TDH074 U/Th

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09TDH074 U ppm

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09TDH074 Th ppm

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Inte

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a)

Upper-Age Intercept (Ma)

09TDH074

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RDF 2014- P a g e | 12

09MBW103A:

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U-Pb Age (Ma)

09MBW103Ahistogram

pdf

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09MBW103A gauss pdf

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09MBW103A peak

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U/T

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U-Pb Age (Ma)

09MBW103Apdf

U/Th

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09MBW103A U/Th

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09MBW103A U ppm

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09MBW103A Th ppm

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Inte

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Upper-Age Intercept (Ma)

09MBW103A

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RDF 2014- P a g e | 13

09LF419A:

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U-Pb Age (Ma)

09LF419Ahistogram

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09LF419A gauss pdf

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09LF419A peak

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09LF419Apdf

U/Th

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09LF419A U/Th

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09LF419A U ppm

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09LF419A Th ppm

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09LF419A

Page 18: Zircon U-Pb Age Data, Alaska Highway Corridor, Tanacross ...dggs.alaska.gov/webpubs/dggs/rdf/text/rdf2014_016.pdf · Zircon U-Pb Age Data, Alaska Highway Corridor, Tanacross and Nabesna

RDF 2014- P a g e | 14

09Z172B:

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09Z172Bhistogram

pdf

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09Z172B gauss pdf

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09Z172B peak

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09Z172Bpdf

U/Th

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09Z172B U ppm

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09Z172B Th ppm

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09Z172B

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RDF 2014- P a g e | 15

09LF254A:

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U-Pb Age (Ma)

09LF254Ahistogram

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09LF254A gauss pdf

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09LF254A peak

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09LF254Apdf

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09LF254A Th ppm

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09LF254A

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RDF 2014- P a g e | 16

09LF433A:

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09LF433Ahistogram

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09LF433A gauss pdf

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09LF433A peak

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09LF433Apdf

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09LF433A U/Th

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09LF433A Th ppm

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09LF433A

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RDF 2014- P a g e | 17

09LF647A:

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09LF647Ahistogram

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09LF647A gauss pdf

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09LF647Apdf

U/Th

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09LF647A

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RDF 2014- P a g e | 18

09LF637A:

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09LF637Ahistogram

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U-Pb Age (Ma)

09LF637A gauss pdf

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09LF637A peak

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U-Pb Age (Ma)

09LF637Apdf

U/Th

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09LF637A U ppm

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09LF637A Th ppm

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09LF637A

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RDF 2014- P a g e | 19

09LF644A:

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U-Pb Age (Ma)

09LF644Ahistogram

pdf

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09LF644A gauss pdf

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09LF644A peak

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U-Pb Age (Ma)

09LF644Apdf

U/Th

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09LF644A U/Th

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RDF 2014- P a g e | 27

APPENDIX B: ZIRCON U-PB DATING METHODOLOGY

Sample Preparation

Zircon grains were isolated and prepared for Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-

MS) analysis using standard procedures combined with specific customized procedures described by Donelick et al.

(2005). Whole rock samples were crushed using a jaw crusher with the minimum jaw separation set to 2-3 mm,

sieved through 300 µm nylon mesh, and the <300 µm size fraction washed with tap water and allowed to dry at

room temperature. Zircon was separated from other mineral species using a combination of lithium metatungstate

(density ~2.9 g/cm3), Frantz magnetic separator, diiodomethane (density ~3.3 g/cm3), and hand-panning separation

procedures. Epoxy wafers (~1 cm x 1 cm) containing zircon grains for LA-ICP-MS were polished manually using 3.0

µm and 0.3 µm Al2O3 slurries to expose internal zircon grain surfaces. The polished zircon grain surfaces were washed

in 5.5 M HNO3 for 20 s at 21⁰ C prior to introduction into the laser system sample cell.

LA-ICP-MS Session Details

LA-ICP-MS data collection was performed at the Geoanalytical Laboratory, Washington State University, Pullman,

Washington, U.S.A. Individual zircon grains were targeted for data collection using a New Wave YP213 213 nm solid

state laser ablation system using a 20 µm diameter laser spot size, 5 Hz laser firing rate, and ultra-high purity He as

the carrier gas. Isotopic analyses of the ablated zircon material were performed using a ThermoScientific Element2

magnetic sector mass spectrometer using high purity Ar as the plasma gas. The following masses (in amu) were

monitored for 0.005 s each in pulse detection mode: 202, 204, 206, 207, 208, 232, 235, and 238. At time = 0.0 s, the

mass spectrometer began monitoring signal intensities; at time = 6.0 s, the laser began ablating zircon material; at

time = 30.0 s, the laser was turned off and the mass spectrometer stopped monitoring signal intensities. A total of

250 data scans were collected for each zircon spot analyzed comprising: approximately 55 background scans;

approximately 20 transitions scans between background and background+signal, approximately 175

background+signal scans. A scheme was developed to check whether mass 238 experienced a switch from pulse to

analog mode during data collection and a correction procedure was employed to ensure the use of good quality

intensity data for masses 235 and 238 when such a switch was observed.

U-Pb Data Analysis

Previous LA-ICP-MS studies of U-Pb zircon dating used the so-called intercept method which assumes that isotopic

ratio varies linearly with scan number due solely to linearly varying isotopic fractionation (Chang et al., 2006; Gehrels

et al., 2008). The data modeling approach favored here was the modeling of background-corrected signal intensities

for each isotope at each scan. Background intensity for each isotope was calculated using a fitted line (for decreasing

background intensity) or using the arithmetic mean (for non-decreasing background intensity) at the global

minimum of selected isotopes (206Pb, 232Th, and 238U) for the spot. Background+signal intensity for each isotope at

each scan was calculated using the median of fitted (2nd-order polynomial) intensity values for a moving window (7

scans wide here) that includes the scan. The precision of each background-corrected signal intensity value was

calculated from the precision of background intensity value and the precision of the background+signal intensity

value.

Zircon U-Pb age standards used during analysis are summarized in Appendix C, including the 1099±0.6 Ma FC zircon

(FC-1 of Paces and Miller, 1993) used here as the primary age standard. Isotopic data for FC were used to calculate

Pb/U fractionation factors and their absolute errors for each FC data scan at each FC spot; these fractionation factors

were smoothed session-wide for each data scan using the median of fitted (1st-order polynomial) fractionation factor

values for a moving window (11 FC spots wide here) that includes the current FC spot and scan. Under the operating

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RDF 2014- P a g e | 28

conditions of the LA-ICP-MS sessions in this study, fractionation factors were found to vary strongly with scan

number, decreasing with increasing scan number (presumably due to increasing ablation pit depth and the effect

this had on fractionation, (e.g., Paton et al., 2010). The zircon crystal lattice is widely known to accumulate α-

radiation damage (e.g., Zhang et al., 2009 and references therein). It was assumed here that increased α-damage in

a zircon leads to a decrease in the hardness of the zircon; this in turn leads to a faster rate of laser penetration into

the zircon during ablation leading to dependence of isotopic fractionation on the degree of zircon lattice radiation

damage. Ages calculated for all zircon age standards, when those standards were treated as unknowns, were used

to construct a fractionation factor correction curve (exponential form) in terms of accumulated radiation damage.

The notion of matrix-matched zircon standard and zircon unknown has been proposed largely on the basis of trace

element chemistry (e.g., Black et al., 2004). In this study, time and lattice damage, parameters invisible to

instruments used to characterize trace element chemistry, were introduced and applied based on measured U and

Th chemistries to effectively matrix-match standard and unknown zircons.

Uranium decay constants and the 238U/235U isotopic ratio reported in Steiger and Jäger (1977) were used in this

study. Errors for the isotopic ratios 207Pb/235Uc (235Uc = 137.88238U), 206Pb/238U, and 207Pb/206Pb at each scan included

errors from the background-corrected signal values for each isotope, the fractionation factor error, and an additional

relative error term required to force 95% of the FC ages to be concordant. Ages for the ratios 207Pb/235Uc, 206Pb/238U,

and 207Pb/206Pb were calculated for each data scan and checked for concordance; concordance here was defined as

overlap of all three ages at the 1 level (the use of 2 level was found to skew the results to include scans with any

significant common Pb). If the number of concordant data scans for a spot was greater than zero, the more precise

age from the concordant-scan-weighted ratio 207Pb/235Uc, 206Pb/238U or 207Pb/206Pb was chosen as the preferred age.

Asymmetrical negative-direction and positive-direction age errors were calculated by subtracting and adding,

respectively, the isotopic ratio errors in the appropriate age equation (Chew and Donelick, 2012).

Moving-Median Smoothing

Moving-median smoothing (MMS) is applied here to a subset (window) of N data points x,y of width m values of x

to which a polynomial of order n is fitted. For each value of x at each position of the data window, a value of y is

calculated for the fitted polynomial. The window is positioned with the right-hand boundary at the left-hand x value

and then shifted N-1 times until the left-hand boundary of the window is positioned at the right-hand x value. At

each x position, m fitted values of y are calculated and the median of these fitted values is taken.

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APPENDIX C: ZIRCON AGE STANDARDS

Standard Standard U-Pb age (2) Reference

FC Duluth complex

1099.0 0.6 Ma Paces and Miller, 1993

F5 Duluth complex

1099.0 0.6 Ma (assumed equal to FC-1)

Paces and Miller, 1993

IF Fish Canyon Tuff

28.201 0.012 Ma Lanphere et al., 2001; Kuiper et al., 2008

MD Mount Dromedary

99.12 0.14 Ma Renne et al., 1998

PX Peixe 563.5 1.6 Ma Gehrels et al., 2008

R3 Braintree complex

418.9 0.4 Ma Black et al., 2004

T2 Temora 2, Middledale gabbroic diorite

416.78 0.33 Ma Black et al., 2004

TR Tardree Rhyolite

61.23 0.11 Ma Dave Chew, pers. commun.