improving tims monazite geochronology (?). why tims? high-precision – typically better than 0.2%...
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![Page 1: Improving TIMS monazite geochronology (?). Why TIMS? High-precision – typically better than 0.2% Benchmark ages of reference materials – LA-ICPMS – SIMS](https://reader036.vdocument.in/reader036/viewer/2022070306/5518b823550346991f8b5210/html5/thumbnails/1.jpg)
Improving TIMS monazite geochronology (?)
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Why TIMS?
• High-precision – typically better than 0.2%
• Benchmark ages of reference materials – LA-ICPMS– SIMS– EPMA
• No matrix correction / background calibration• No need to assume concordance
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Challenges with TIMS
• Minimal spatial resolution – However, studies have successfully:• Broken off tips (Schärer & Allègre, 1982)• Used X-ray maps to guide micro-drilling of
compositional domains (Corrie & Kohn, 2007)
• Weeks of analysis time• Currently, no widely available Th–Pb spike*– Therefore only U–Pb (and Pb–Pb) ages
*Cottle and Peterman are currently preparing a calibrated U–Th–Pb spike specifically for monazite
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6 samples analyzed in study
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Broad range in age and composition
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Method development
• Iterative process– Typical single step dissolution accomplished at
180°C in 12M HCl for 24 hours
• Our variables:– Acid strength (HCl) 12M, 6M and 3.1M– Initial T at 120, 100 and 80°C– Dissolution times of 12 and 6 hours
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Jefferson County
Jefferson County
Annealed;Pre-etch
Annealed;Post-etch
Amelia
Not-annealed;etched
Amelia
Annealed;etched
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Conditions used for analysis
• Parallel digestion of annealed (1000°C, 48 hours in air) with not-annealed grains (or fragments)
• Starting T: 80°C• Acid: 3.1M HCl• Duration of step: initially 12 hours– After 5 steps, reduced time to 6 hours and started
increased T by 10°C (to ensure sufficient dissolution to measure precisely via TIMS)
– Geochemist rule of thumb—increase of 10°C nearly equivalent to doubling the step time
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Why 1000°C, 48 hours in air?Experiments demonstrate structural recovery if annealed in air. Recrystallization occurs if annealing is fluid-mediated.
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Structural recovery of monazite accomplished by simple heating; “defects completely disappear”
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Conditions used for analysis
• Parallel digestion of annealed (1000°C, 48 hours in air) with not-annealed grains (or fragments)
• Starting T: 80°C• Acid: 3.1M HCl• Duration of step: initially 12 hours– After 5 steps, reduced time to 6 hours and started
increased T by 10°C (to ensure sufficient dissolution to measure precisely via TIMS)
– Geochemist rule of thumb—increase of 10°C nearly equivalent to doubling the step time
![Page 13: Improving TIMS monazite geochronology (?). Why TIMS? High-precision – typically better than 0.2% Benchmark ages of reference materials – LA-ICPMS – SIMS](https://reader036.vdocument.in/reader036/viewer/2022070306/5518b823550346991f8b5210/html5/thumbnails/13.jpg)
a b c d e f g h i j k l m n0
10
20
30
40
50
60
70
80
90
100
Dissolution Rates
Jeff N
SmithN
Burke N
JeffA
SmithA
BurkeA
Dissolution steps
Am
ou
nt
dis
solv
ed
(%
)
Amelia N
Amelia A
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Age data presented
• 238U–206Pb age spectra– 235U–207Pb, where appropriate
• Plotted following 40Ar/39Ar convention– X-axis = percent of sample – Y-axis = age– Height of box = uncertainty
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Example age diagramImprecise; ~10% of mnz
Shaded = included
in calc’ed age
Not shaded = not included
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Compositional data presented
• Data collected from column elutions via ICPMS with internal and external standards
• Also follows 40Ar/39Ar convention– X-axis = percent of sample – Y-axis = compositional ratio– Used blank-corrected ratios (normalized to 31P)
because each step dissolved different amounts of monazite (concentration therefore not useful)
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4 selected ratios
Reflect changes in compositional domains (as per EPMA data)
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Amelia – ages
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Annealed vs. not-annealed
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Burke – ages
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Annealed vs. not-annealed
*note change in scale on axes
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Jefferson County – ages
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Annealed vs. not-annealed
*note change in scale on axes
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Major findings
(and how it may apply to your research)
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Annealing repairs dislocations and lattice damage induced by alpha-recoil and fission.
Results in slower dissolution rate
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Not-annealed samples ( n = 3):heterogeneity in first step,
largely homogeneous chemical spectraAmelia Burke Jefferson County
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Annealed samples (n = 6): complicated compositional spectra
These are the pairs to the not-annealed aliquots
Amelia Burke Jefferson County
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3 additional samples
These samples do not have not-annealed aliquots
Elk Mountain Madagascar 554
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Annealing affects chemistry… and age?
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Suggestions for your research, should you choose to use TIMS
• Don’t anneal– Apparently induces recrystallization
• Use multi-step TIMS or use x-ray maps to guide microdrilling – Single step TIMS will yield a precise age that may
be quite inaccurate