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ESR Dating of Optically Bleached Quartz Grains: Assessing the Impact of Different Experimental Setups on Dose Evaluations Cover

ESR Dating of Optically Bleached Quartz Grains: Assessing the Impact of Different Experimental Setups on Dose Evaluations

Open Access
|Dec 2021

Figures & Tables

Fig. 1

Vertical distribution of ESR signal intensities obtained for three different resonators. The ER4102ST (1) profile was obtained using an EMX micro 6/1 ESR spectrometer (setup #1), while the ER4102ST (2) and SHQE resonator profiles were derived from the Elexsys E500 ESR spectrometer (setups #2 and #3). To facilitate comparisons, ESR intensities were normalized according to the highest intensity value for each profile. Key: Distance = sample distance from the resonator centre. d = Distance from the centre to the top of the resonator.

Fig. 2

Evolution of the ESR intensity with time using setup #2. Different temperatures were tested. Al ESR intensities were normalized to the mean ESR intensity obtained for each aliquot. Acquisition conditions: 1 scan / 5 min for the 3−5 h tests, 1 scan / 2 min for the 2 h test and 1 scan / min for the 1 h test.

Fig. 3

Comparison of the evolution of the ESR intensities (Al centre) with the temperature (intensities normalized for T= 117 K) for setups #1 and #2.

Fig. 4

ESR spectra of sample BIZ1201 (natural aliquot) for (A): Al- and (B): Ti-centres, using both, a standard ER4102ST(2) and a HSQE resonators. ESR spectra of each centre were recorded with the same acquisition parameters. For Al centre: modulation frequency = 100 KHz, modulation amplitude = 1 G, microwave power = 10 mW, sweep time = 40.96 s, receiver gain = 60 dB and T = 94 K. For Ti centre: modulation frequency = 100 KHz, modulation amplitude = 1 G, scan = 2, microwave power = 5 mW, sweep time = 61.44 s, receiver gain = 81 dB and T= 94 K. All spectra were recorded with the Elexsys E500 ESR spectrometer.

Fig. 5

Comparison of the ESR intensities (Al centre) obtained from samples BIZ1201 and BIZ1202 with the three experimental setups. The spectra were recorded using the acquisition parameters shown in Table 3. ESR intensities were normalized according to the natural intensity of each DRC.

Fig. 6

Comparison of the ESR intensities (Ti centre) obtained from samples BIZ1201 and BIZ1202 with the three experimental setups. Spectra were recorded using the acquisition parameters shown in Table 3. ESR intensities were normalized according to the natural intensity of each DRC.

Fig. 7

DE values (Al centre) obtained from samples BIZ1201 and BIZ1202 with the three experimental setups. DE values were obtained by the fitting of an EXP+LIN function through each DRC. Final DE values are obtained by averaging the ESR intenstities derived from the 3 repeated measurements.

Fig. 8

DE values (Ti centre) obtained from samples BIZ1201 and BIZ1202 with the three experimental setups. DE values were obtained by the fitting of a Ti-2 function through each DRC. Final DE values are obtained by averaging the ESR intenstities derived from the 3 repeated measurements.

Variability of the ESR intensities of samples BIZ1201, BIZ1202 (Al and Ti centres) derived from experimental setups #1, #2 and #3_

Al CentreTi Centre

SampleExperimental setupDayNumber of aliquots per samplePrecision of each sample measurements: mean CV (%)Precision of 3 day measurements: mean CV (%)Precision of each sample measurements: mean CV (%)Precision of 3 day measurements: mean CV (%)
BIZ1201Setup #11130.821.673.802.59
2131.053.63
3131.043.62

Setup #21130.792.022.574.96
2131.253.32
3131.763.57

Setup #31131.311.283.824.15
2131.582.66
3131.544.08

BIZ1202Setup #11131.371.214.083.78
2131.473.65
3131.012.59

Setup #21131.071.842.793.06
2131.452.84
3131.192.39

Setup #31132.291.813.005.00
2131.632.54
3131.472.92

Description of Experimental Setups #1, #2 and #3_

Experimental Setup #1Experimental Setup #2Experimental Setup #3
ESR spectrometerBruker EMX 6/1 microBruker Elexsys E500Bruker Elexsys E500
Resonator modelER4102ST(1): standard cavityER4102ST(2): standard cavitySHQE: high sensitivity cavity
Low temperature systemER4141VT Digital Temperature control systemER4131VTM Digital Temperature (stabilized via PID)ER4131VTM Digital Temperature (stabilized via PID)
ChillerThermo Scientific NESLAB ThermoFlex 3500 (water-cooled)Riedel PC-100-02 (water-to-air cooled)Riedel PC-100-02 (water-to-air cooled)
Acquisition softwareBruker Win EPRBruker XeprBruker Xepr

Overview of the different groups working on ESR dating of quartz over the last decades (non-exhaustive list)_ The description of the experimental setup is based on the information provided in the respective publications cited in the last column_

Institution, city, countryESR spectrometer (temperature of ESR measurement)Reference
Museum National d’Histoire Naturelle, Paris, FranceBruker EMX (107 K)Voinchet et al., 2010
University of Cologne, Cologne, GermanyBruker ESP 300 (115 K)Beerten et al., 2006
Centro Nacional de Investigacion sobre la Evolucion Humana (CENIEH), Burgos, SpainBruker EMXmicro 6/1 (90 K)Duval et al., 2017a
McMaster University, Hamilton, CanadaJEOL FA-100 (77 K)Burdette et al., 2013
China Earthquake Administration, Beijing, ChinaBruker ER041XG (77 K)Liu et al., 2010
Okayama University of Science, Okayama, JapanJEOL PX-2300 (81–84 K)Toyoda et al., 2006

Acquisition parameters employed for the three experimental setups during the ESR measurements of Al and Ti centres_

Al centreTi centre
Experimental SetupSetup #1Setup #2Setup #3Setup #1Setup #2Setup #3
ESR spectrometerEMX 6/1 microElexsys E500EMX 6/1 microElexsys E500
Resonator modelER4102ST(1)ER4102ST(2) SHQEER4102ST(1)ER4102ST(2) SHQE
Microwave power (mW)101055
Sweep width (mT)18181818
HF modulation (kHz)100100100100
Modulation amplitude (mT)0.10.10.10.1
Number of points1024102410241024
Conversion time (ms)40406060
Sweep time (s)40.9640.9661.4461.44
Number of scans112–42–4 ST resonator 1–2 HSQE
Receiver Gain3169.860 dB25178.581 dB
Temperature (K)90949094
Language: English
Page range: 179 - 190
Submitted on: Jan 18, 2019
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Accepted on: Oct 7, 2019
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Published on: Dec 31, 2021
Published by: Sciendo
In partnership with: Paradigm Publishing Services
Publication frequency: 1 issue per year

© 2021 Verónica Guilarte, Mathieu Duval, published by Sciendo
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.