Fission-track analysis

Matthias Bernet, Ph.D.

Université Joseph Fourier
Grenoble, France
Fission-track analysis
• Formed by spontaneous
fission of 238U

• Minerals used for fission-

track analysis are apatite,
zircon and titanite
 Fission-track analysis
Frequency of spontaneous fission events
These are very rare events!

Wagner and van den Haute (1992)

Fission-track analysis
• Fission fragments formed
during spontaneous fission of
238
U
 Fission-track analysis
Energy release during
spontaneous fission

Wagner and van den Haute (1992)

 Fission-track analysis
Damage of crystal structure

Fleischer et al. (1975)

Fission-track analysis

Track formation:

Linear function of time

(t1/2 for spontaneous fission of
238
U  8.21015 y)

The age of a sample is

determined by the track density
and uranium concentration
 Fission-track analysis
• Tracks are in principal
Fission tracks in zircon randomly oriented

• But only grains mounted

parallel to the c-axis
should be dated

• Fission tracks can be

observed in a microscope
after etching
Fission-track analysis
• Transmitted and
reflected light
microscope
• Automated X-Y stage
• Digitizing tablet
• Digital camera
• PC with Windows XP
Separated apatites and zircons
Apatite Ca5(PO4)3(OH,Cl,F) Zircon Zr [SiO4 ]
Density 3.1 – 3.3 Density 4.6 – 4.7
 Sample preparation
• Rock crushing and
pulverizing
• Sieving 100-200 µm
• Separation table
Mineral separation
Fission-track analysis: external
detector method

• Zircon or apatite
with latent tracks

• Mounting of grains
in epoxy or Teflon

• Polishing to expose
an internal grain
surface
Mounting of apatite in Epoxy
• Mixture of
• resin 4 : hardener 1
• 30 ml resin and 7.5 ml
hardener for
preparing 12 samples

apatite mounting
Mounting of zircon in Teflon®

Hot plate for zircon mounting Zircon grains mounted in Teflon®

Fission-track analysis: external
detector method

• Etching for track

revelation
– HNO3 (apatite)
– NaOH-KOH (zircon)

• Etching is faster in
damaged zones of
latent tracks
 Etching of fission tracks
• Apatite etching
– 5.5 M HNO3
– 20 seconds
– 21°C
• Zircon etching
– Eutectic melt of NaOH
and KOH at 228°C
– 8 g NaOH + 11.2 g KOH
– 4 -100 hours
 Etching response

Fleischer et al. (1975)

Etching of fission tracks in apatite
Etching of fission tracks in zircon
well etched under etched

over etched
 Etching of fission tracks
Relationship between etch time and U concentration
U (ppm)

40-60h etch time 15-30h etch time 5-10h etch time

Fission-track grain age (Ma)

 Etching of fission tracks
• Etching of fission-
tracks in zircon

• Different grain
populations are well
etched depending on
U content and etch
time

Zircon
Fission-track analysis: external
detector method

• Etched fission
tracks at the grain
surface

muscovite sheet

• White mica as
external detector
Fission-track analysis: external
detector method

• Etched fission
tracks at the grain
surface

muscovite sheet

• White mica as
external detector
White mica external detector
Preparation of mica detector
Fission-track analysis: external
detector method
• Determination of U
content using 235U

• Ratio between 238U

and 235U is stable in
nature (7.2527x10-
3)

• Irradiation with
thermal neutrons
Thermal neutron irradiation

FRM II reactor
Munich, Germany
Thermal neutron irradiation
Maxwell-Boltzmann distribution

Neutron density

Neutron flux

Neutron energy

Wagner and van den Haute (1992)

 Thermal neutron irradiation
Activation cross-section

Our irradiations

Apatite
4,5 x 1015 n/cm2
6.5 – 7 min.

Zircon
0.5 x 1015 n/cm2
55 – 60 sec.

Neutron energy

Wagner and van den Haute (1992)

Fission-track analysis: external
detector method
• Induced fission of 235U
in grain

• Formation of induced
tracks in the mica

• Etching of induced
tracks in the mica after
irradiation with 48% HF
for 18 min at 20°C
 Fluence determination
• Counting of induced
tracks in mica
detectors attached to
dosimeter glasses
• Nd = number of
induced tracks

• d = t/cm2
• SE of d
Fluence determination
Fluence determination
Fission-track analysis: external
detector method

Grain image Mica image

Grain selection for counting
• Bedrock samples
– 20 best grains
• Detrital samples
– 100 grains randomly
selected
– or at least as many as
possible

Reflected light image

Counting of fission tracks

Apatite with fission-tracks

 Fission-track analysis: external
detector method
• Counting of
spontaneous tracks in
the grains
 s (spontaneous track
density)

• Counting of induced
tracks in the mica
 i (induced track
density)
Counting of fission tracks –
which are the tracks?

10 

Zircon with fission-tracks

 Counting of fission tracks
Apatite without fission tracks
• Counting of zero-track
grains (no
spontaneous tracks)
– Apatite YES
– Zircon NO

• If no induced tracks
are present, the grain
cannot be dated
Induced track in mica sheet
Examples of non-countable grains
Examples of countable grains
Zircon Zircon

Zircon Apatite
Counting of fission tracks
Zircon fission-track analysis
 Fission-track analysis: external
detector method

Fission-track age: 1    s c  d 
t  ln 1  
(external detector method)   i 
 I
Zeta calibration factor () : 
 f d

: decay constant of 238U (4.47 x 109 y)

 f: fission decay constant of 238U (8.2 x 1015 y)
: neutron flux
: cross section of neutron capture (580.2 x 10-24 cm2)
c: geometry factor (0.5)
I: 235
U/238U ratio (7.2527x10-3)
s, i: density of spontaneous and induced tracks
d track density of fluence monitor
 Fission-track analysis: external
detector method

Symmetrical error of a single-grain age:

1
 1 1 1   
2 2

i        
 N s ,i N i ,i N d    

Ns: spontaneous track counts

Ni : induced track count
Nd : track count of fluence monitor
: Zeta value
: error of Zeta value
Zeta factor
• Changes with
uranium content of
glass standard used
for the irradiation

• Determined by
counting fission-
tracks in age
standards
Zeta factor comparison
Zeta factor
Common glass standards
• CN1 39.80 ppm U
• CN2 36.5 ppm U
• CN5 12.7 ppm U

• IRMM 540R 15 ppm U

• SRM 612 37.4 ppm U

 Common age standards
• Apatite
– Durango (31.4 Ma)
– Fish Canyon Tuff (27.9 Ma)
– Mount Dromedary (98.8 Ma)
• Zircon
– Buluk Tuff (16.2 Ma)
– Fish Canyon Tuff (27.9 Ma)
– Tardee Rhyolite (58.7 Ma)
– Mount Dromedary (98.8 Ma)
Data presentation
 Data presentation
Radial plot Probability density plot
Horizontally confined track lengths
Horizontally confined track lengths
• Track length
measurements of
horizontally confined
tracks
 Track lengths distribution
AFT: Track Length Distribution
• Track lengths
N=100
0.30
measured from
horizontally confined
0.25
tracks on extra grain
0.20
mounts
Frequency

0.15

• Californium (Cf)
0.10
irradiation to increase
0.05
number of
measurable tracks
0.00
0 2 4 6 8 10 12 14 16 18 20
Length (µm)
Annealing of fission tracks in apatite

• Annealing as a function of
– temperature
– time
– pressure
– chemical composition
Annealing of fission tracks in zircon
• Annealing as a
function of
– temperature
– time
– radiation
damage
 Annealing of fission-tracks

Temperature and time

 Annealing of fission tracks

Temperature and time

Annealing of fission tracks

New
tracks
Old tracks

Temperature and time

Track length measurements

• Tracks disappear because of

annealing
• Non-linear process, strongly
dependant on temperature
• Numerical annealing
models for studying thermal
histories
Prediction of track lengths distributions
for different thermal histories
l/l0 = present track length/initial track length
Linear heating Linear cooling

PAZ
PAZ

Unimodal distribution Skewed distribution

Gallagher et al., 1998
Prediction of track lengths distributions
for different thermal histories
Rapid cooling Heating/cooling

PAZ PAZ

Relatively long tracks Bimodal distribution

Gallagher et al., 1998
Prediction of track lengths distributions
for different thermal histories

Gallagher et al., 1998

Prediction of track lengths distributions
for different thermal histories

Gleadow & Brown, 2000

 After
5.6 Ma

Before
5.6 Ma
Mt McKinley (Denali) 20320 feet high, from Talkeetna (south)
View from summit of Denali - looking south to Mt Foraker (16,500’)
McKinley (Denali) Apatite FT ages (Ma)
De na li

16
10 13
9 11
8
6
6
5

5
6
5

6
4
Fitzgerald et al., (1993), (1995)