Q-band esr studies of fossil teeth: Consequences for esr dating

At least 14 axial-symmetry ESR lines in Plio-Quaternary enamel fibres were observed by Q-band technique. Some lines follow a law e.g. the main anisotropic A-line whose g = 2.0018 and g = 1.9977 are close to g_eff = 2.0020 and g_eff = 1.9975 respectively of the isotropic doublets B- and E-lines. The other lines are blocked below 220K e.g. one isotropic hyperfine (g = 2.0033, a = 21.6 Gauss) M-septet and one isotropic singlet (g = 2.0007) D-line. By heating, the M-septet intensity increases up to 250°C and is lost at 280°C; B- and E-lines decrease while a new isotropic (g = 2.0056) C-line appears. At 300°C, only the two C- and A-lines usually remain and hold up to 400°C.The natural dose rate of fossil enamel is calculated from U-, Th-, K-content and disequilibrium measured both in enamel and dentine, bones and sediments in contact, by methods of low-background γ-spectrometry, isotopic dilution and fission-tracks mapping.ESR dating of quaternary Proboscidae, Bovidae, Equidae and Cervidae has been attempted by a new comparative method: the A-line intensity, normalized for the same dose rate and weight, of various fossil dental enamels varies quasi-linearly with the age of the geological sites from which they are issued.     

ESR dating and trapped electrons lifetime of quartz grains in loess of China

This paper reports the preliminary application of ESR dating to loess strata. The samples were collected from the 7th palaeosol layer (S7) of the Luochuan section, Shaanxi province in China. The ESR age of S7 is 736 ka (total dose 2945 Gy, annual dose 4 mGy/year). This age represents the original eolian accumulation age. The result is consistent with the palaeomagnetic data (730 ka). We have also carried out thermal annealing experiments on quartz grains from the S7 sample. ESR intensities (g = 2.0005) increase from 25°C to 320°C. It may be that trapped electrons transfer into the E′ centre site. ESR intensities decrease from 340°C to 460°C due to thermal annealing. We obtained a mean-life of E′ centre electrons at 20°C of 6.66 × 10⁸ years. The activation energy is 1.35 eV and frequency factor is 3.7 × 10⁸ min⁻¹.     

Interferences encountered in the determination of AD of mollusc samples

Inflexion points interfere with the radiation growth curve of the dating signal at g = 2.0014 for mollusc samples. Several experiments give evidence that the definition of the dating signal at g = 2.0014 has to be reconsidered. A reliable AD determination very often seems questionable for ESR dating of mollusc samples.     

Electron spin resonance of stabilized free radicals in sedimentary organic matter

Electron spin resonance (ESR) is evaluated as a method to study the thermal degradation of sedimentary organic matter which consists mainly of kerogen. Whole rock and separated kerogen samples were pyrolysed stepwise (ambient to 700°C at 50°C increments), extracted and analysed for elemental composition and ESR spectra at each step. Whole rock samples give rise to complex spectra which include those of paramagnetic metals and are therefore unsuitable in most cases for this purpose.The ESR parameters g value, ΔH and N_g differ for different types of immature organic matter. An increase in N_g,shift of g value to 2.0026–2.0028 and reduction in h are the main trends during pyrolysis and in natural heating of sedimentary organic matter.The peak generations of liquid and gaseous hydrocarbons coincide with maxima of free radical density. ESR spectroscopy in combination with complementary geochemical characterization of the sedimentary organic matter can serve to indicate maturity with respect to peak oil-gas generation.     

Proterozoic–Paleozoic development of the basement of the Central Andes (18–26°S) — a mobile belt of the South American craton

The Late Precambrian–Early Paleozoic metamorphic basement forms a volumetrically important part of the Andean crust. We investigated its evolution in order to subdivide the area between 18 and 26°S into crustal domains by means of petrological and age data (Sm–Nd isochrons, K–Ar). The metamorphic crystallization ages and t_DM ages are not consistent with growth of the Pacific margin north of the Argentine Precordillera by accretion of exotic terranes, but favor a model of a mobile belt of the Pampean Cycle. Peak metamorphic conditions in all scattered outcrop areas between 18 and 26°S are similar and reached the upper amphibolite facies conditions indicated by mineral paragensis and the occurrence of migmatite. Sm–Nd mineral isochrons yielded 525±10, 505±6 and 509±1 Ma for the Chilean Coast Range, the Chilean Precordillera and the Argentine Puna, and 442±9 and 412±18 Ma for the Sierras Pampeanas. Conventional K–Ar cooling age data of amphibole and mica cluster around 400 Ma, but are frequently reset by Late Paleozoic and Jurassic magmatism. Final exhumation of the Early Paleozoic orogen is confirmed by Devonian erosional unconformities. Sm–Nd depleted mantle model ages of felsic rocks from the metamorphic basement range from 1.4 to 2.2 Ga, in northern Chile the average is 1.65±0.16 Ga (1σ; n=12), average t_DM of both gneiss and metabasite in NW Argentina is 1.76±0.4 Ga (1σ; n=22), and the isotopic composition excludes major addition of juvenile mantle derived material during the Early Paleozoic metamorphic and magmatic cycle. These new data indicate a largely similar development of the metamorphic basement south of the Arequipa Massif at 18°S and north of the Argentine Precordillera at 28°S. Variations of metamorphic grade and of ages of peak metamorphism are of local importance. The protolith was derived from Early to Middle Proterozoic cratonic areas, similar to the Proterozoic rocks from the Arequipa Massif, which had undergone Grenvillian metamorphism at ca. 1.0 Ga.     

ESR dating of saline sediments using NaHCO3 and NaCl

Age estimates of NaCl and NaHCO₃ in the sediments at Searles Lake, California have been obtained using electron spin resonance (ESR). ESR signals are identified as H⁺Ca²⁺---CO₃³⁻ or H⁺---CO₂⁻ electron type and hole CO₃⁻ type centres, stabilized by impurities in NaHCO₃ and in NaCl. The total dose of natural radiation (TD) and the tentative ESR ages were determined using these signals based on U, Th and K analyses assuming uranium series disequilibrium for a simple infinite medium. Although ESR ages are concordant with the stratigraphy, radiation assessment considering the loss and incorporation of radioactive elements must be made to get reliable absolute ages.     

Precambrian palaeomagnetism in Australia I: Basic dykes and volcanics from the Yilgarn Block

The palaeomagnetism of 54 dykes sampled from the many swarms that intrude the Yilgarn Block of Western Australia shows that their directions of magnetization fall into five distinct groups.Preliminary Rb-Sr age determinations made on samples used in the study however, indicate that for one, and possibly two of those groups, the dykes belong to two widely different ages suggesting that the palaeomagnetic field has been sampled at two widely separated points in time but when its direction was essentially the same. The seven groups of directions thus obtained imply that the dykes belong to at least six, possibly seven periods of intrusion. Relative-age information relating to four of those periods, determined from cross-cutting and baked contact studies, agrees with that obtained radiometrically.The poles and ages of the groups are as follows: Group YA dykes (c. 2500 or c. 1700 m.y.) 21.7S 133.7E (A₉₅ = 17.9°) Group YB dykes (750—700 m.y.) 19.9S 282.0E (A₉₅ = 28.1°) Group YC dykes (1500 m.y., Group YB) 79.7N 2.7E (A₉₅ = 13.0°) Group YD dykes (1700 m.y.) 23.5S 46.1E (A₉₅ = 9.9°) Group YE dykes (c. 2500 m.y.) 28.3S 0.4E (A₉₅ = 31.0°) Group YF dykes (c. 1700 m.y.) 24.7N 101.8E (A₉₅ = 14.0°) Ravensthorpe dykes (2500 ± 100 m.y.) 38.3S 136.2E (A₉₅ = 25.5°)Results from eight samples of the 1390 ± 140 m.y. Morawa Lavas of the Billeranga Hills yield a pole at 42.8N 22.4E (A₉₅ = 14.7°).     

Dating of a volcanic rock by electron spin resonance

The age of a volcanic rock has been determined by ESR dating using the Ge center in quartz. The total dose of natural radiation and the age obtained from the Ge center are 460 krad and 2.07 ± 0.50 Ma, respectively, and those from the unidentified defect at g = 2.011 are 484 krad and 2.16 ± 0.21 Ma, respectively. These dates agree well with the age of 2.0 ± 0.5 Ma determined by the fission-track method. High stress or temperature destroy these accumulated defects but, in the same time, produce a lot of new diamagnetic precursors which enable us to observe the clear ESR signal.     

ESR dating of palaeolithic calcite: A comparison between powder and monocrystal spectra with thermal annealing

Evolution of ESR spectra with thermal annealing at different temperatures is studied for a monocrystal calcite taken in the Orgnac III site. Up to 20 ESR lines are recognized from the angular dependence of these lines. These lines are compared with the ESR lines observed for powder and rotating monocrystal calcites.The h1 line (g = 2.0057) and h3 line (g = 2.0007) are isotropic or nearly isotropic and are due to the electrons trapped in the amorphous region formed by fission tracks or alpha-ray recoil nuclei. The h2 line (g = 2.0021) is a composite of several different lines.     

Travels of the Cache Creek Terrane: a paleomagnetic, geobarometric and Ar/Ar study of the Jurassic Fourth of July Batholith, Canadian Cordillera

The Middle Jurassic Fourth of July Batholith and cross-cutting mafic dikes have been studied geochronologically, geobarometrically and paleomagnetically to estimate subsequent tectonic motion of the Cache Creek Terrane (CCT) in the northern Canadian Cordillera. ⁴⁰Ar/³⁹Ar hornblende ages from a granodiorite phase are similar to U–Pb zircon ages and indicate rapid cooling of the batholith upon intrusion, suggesting that the magnetization age is coincident with the 173-Ma crystallization age. Argon ages of biotite from the granodiorite and two mafic dikes have similar ages of 165 Ma, which dates cooling through 280 °C.Aluminum-in-hornblende geobarometry indicates differential uplift of the batholith across a north–south fault zone along Atlin Lake with >6 km more uplift on its eastern side. Also, the eastern side has been tilted downward to the south–southwest by 9°.Combined paleomagnetic data from 20 granitoid and 11 mafic dike sites yield an in situ paleopole at 55°W, 63°N (d_p=5°, d_m=5°) and a tilt-corrected paleopole at 81°W, 55°N (d_p=5°, d_m=6°). Compared to the 173-Ma reference pole for the North American craton, the tilt-corrected pole suggests a significant southward translation of 16.1±3.7° and a significant clockwise rotation of 107±7°. The translation estimate is similar to the Jurassic Teslin Crossing pluton in the Stikine Terrane, however, the rotation estimate is very different. This could indicate that the Cache Creek Terrane was at a similar latitude of the Stikine Terrane, but the two were not yet amalgamated.     

He diffusion and (U–Th)/He thermochronometry of zircon: initial results from Fish Canyon Tuff and Gold Butte

To evaluate the potential of (U–Th)/He geochronometry and thermochronometry of zircon, we measured He diffusion characteristics in zircons from a range of quickly and slowly cooled samples, (U–Th)/He ages of zircons from the quickly cooled Fish Canyon Tuff, and age-paleodepth relationships for samples from 15 to 18 km thick crustal section of the Gold Butte block, Nevada. (U–Th)/He ages of zircons from the Fish Canyon Tuff are consistent with accepted ages for this tuff, indicating that the method can provide accurate ages for quickly cooled samples. Temperature-dependent He release from zircon is not consistent with thermally activated volume diffusion from a single domain. Instead, in most samples apparent He diffusivity decreases and activation energy (E_a) increases as cycled step-heating experiments proceed. This pattern may indicate a range of diffusion domains with distinct sizes and possibly other characteristics. Alternatively, it may be the result of ongoing annealing of radiation damage during the experiment. From these data, we tentatively suggest that the minimum E_a for He diffusion in zircon is about 44 kcal/mol, and the minimum closure temperature (T_c, for a cooling rate of 10 °C/myr) is about 190 °C. Age–paleodepth relationships from the Gold Butte block suggest that the base of the zircon He partial retention zone is at pre-exhumation depths of about 9.5–11 km. Together with constraints from other thermochronometers and a geothermal gradient derived from them in this location, the age–depth profile suggests a He T_c of about 200 °C for zircon, in reasonable agreement with our interpretation of the laboratory measurements. A major unresolved question is how and when radiation damage effects become significant for He loss from this mineral.     

An explosion seismology investigation of the continental margin west of the Hebrides, Scotland, at 58°N

During summer 1975, a line of large shots was fired across the continental margin between the Rockall Trough and the Hebridean shelf along 58°N. Arrivals were observed at temporary seismic stations set up across Scotland and in northwestern Ireland. A clear P₂ phase was observed to cross the margin and a converted phase P₁ also seen on the records is interpreted as travelling in the sub-sedimentary oceanic crust of Rockall Trough and in the upper continental crust beneath the shelf.The continental crust beneath the Hebridean shelf is estimated to be 27 ± 2 km thick, with P_g = 6.22 ± 0.03 km/s and P_n = 8.01 ± 0.04 km/s as determined by time-term analysis. P_g delays on the outer shelf are interpreted in terms of a seaward thickening wedge of Mesozoic sediments which pre-date the split. P_n beneath the Rockall Trough was poorly determined at 8.20 ± 0.17 km/s and the Moho is estimated to be 18 ± 2 km deep at 58°N. This and other seismic and gravity work indicates a northward thickening of the crust along the Rockall Trough, accounting for the northward decrease in the height of the slope.Our results, and those of gravity interpretations, indicate a relatively abrupt transition between continental and oceanic crust, possibly correlating with the lack of major shelf subsidence. This is attributed to a relatively cool origin for this margin. The main thinning of the continental crust beneath the slope is attributed to outslip of continental crustal material into and beneath the newly forming oceanic crust during the first few million years after the split, possibly enhanced by pre-split stretching.     

Age of the metamorphic sole of the Papuan Ultramafic Belt ophiolite, Papua New Guinea

The Papuan Ultramafic Belt (PUB) ophiolite is former oceanic crust and upper mantle emplaced onto continental crust in Papua New Guinea (PNG) in a zone of general convergence between the Pacific and Australian plates. The metamorphic sole beneath the ophiolite is best exposed in the Musa–Kumusi divide and comprises a 40- to 300-m-thick body of granulite and amphibolite facies rocks. Geochronological studies on the metamorphic sole, using amphiboles from the granulites and amphibolites, yield measured K–Ar ages ranging from 65.0±0.7 to 57.2±0.6 Ma and average ⁴⁰Ar–³⁹Ar direct total fusion ages ranging from 67.0±0.7 to 59.5±0.2 Ma. Five of the six ⁴⁰Ar–³⁹Ar plateau ages, derived from age spectra, lie between 58.6±0.2 and 57.8±0.2 Ma, with an overall mean age of 58.3±0.4 Ma. The large spread in measured K–Ar and ⁴⁰Ar–³⁹Ar total fusion ages is thought to be caused by the presence of variable amounts of excess argon. The mean plateau age for five samples of 58.3±0.4 Ma is interpreted to mark the time of cooling of the metamorphic sole following peak metamorphism. We suggest that the development of the metamorphic sole and emplacement of the PUB ophiolite onto the PNG crust occurred in a relatively short time interval in the Paleocene.     

Towards single grain ESR dating of sedimentary quartz: first results

In optically stimulated luminescence dating, apparent ages of individual grains are thought to reflect a wide distribution of initial bleaching levels in hard to bleach sediments. Although having a larger age range (up to 1 Ma and beyond), this approach has not been used yet in electron spin resonance (ESR) dating. Here we report on the first results of ESR measurements on single sedimentary quartz grains. Initial bleaching levels are evaluated for two different River Meuse deposits in Limburg, NE Belgium. Measurements were done with a Q-band ESR spectrometer on transparent quartz grains of sufficiently large diameter (0.5–0.7 mm). Single crystal ESR properties were used to identify different ESR active centres. In about 50% of the selected grains an Al and/or Ti–Li signal was detected and the latter has been selected for further measurements. Artificial bleaching experiments show a strong signal decrease with UV light exposure. After gamma-ray irradiation, a number of different signal intensity vs. artificial dose curves could be observed: exponential growth, exponential saturation, linear, with inflexion points, and unclear ones. Many grains show increasing ESR signals with doses up to 1000 Gy, suggesting that the age range could be extended over 1 Ma, covering the Middle Pleistocene and part of the Early Pleistocene. Accumulated doses of individual grains were calculated using the additive dose method. The results show a large dose distribution of individual grains for both deposits. It is concluded that insufficiently bleached grains can be detected using single grain ESR measurements of sedimentary quartz in a fluvial environment.     

Paleomagnetism in Greece: Indications for relative block movement

There is a difference of 120° between the strike of the Pindos mountain chain and that of the Argolis peninsula. Both consist of rocks of the same age (Triassic Jurassic).Samples were collected to see if paleomagnetic data also exhibited this difference in angle. 23 samples from two sites and four lava strata of the Pindos resulted in normal and reversed directions with a mean direction D = 334°, I = 22° with α_95° = 9°, and 24 samples from four sites of the Argolis peninsula in a mean direction of D = 82°, I = 19° with α_95° = 17°. This is a declination difference of D = 108°. Therefore, a relative rotational block movement with an angle of about 110° could be assumed. The result depends to a great extent on the dip correction of the lava flows.     

Cosmogenic Be dating of the Salpausselkä I Moraine in southwestern Finland

We determined in situ cosmogenic ¹⁰Be ages for nine boulders sampled on the Salpausselkä I (Ss I) Moraine. Previous dating of this moraine indicated that it formed during the Younger Dryas Stadial along the southern margin of the Scandinavian Ice Sheet in southern Finland. Our new exposure ages range from 10.9±1.0 to 13.5±1.2 ¹⁰Be ka, with an error-weighted mean age of 12.4±0.7 ¹⁰Be ka. Our results confirm four previous ¹⁰Be ages obtained 40 km northeast of our sample location. The combined data (n=13) indicate that retreat from the Ss I Moraine occurred at 12.5±0.7 ¹⁰Be ka, in excellent agreement with an age of 12.1 ka for retreat from the Ss I Moraine based on varve chronologies. These results identify the Ss I Moraine as among the best-dated margins associated with Late Quaternary ice sheets.     

Dating the Lower Paleolithic Open-Air Site of Holon, Israel by Luminescence and ESR Techniques

The open-air Acheulian site in Holon, Israel, was dated by the luminescence methods and by electron spin resonance (ESR). Situated in the coastal plain Quaternary Kurkar Group, the Holon site was first excavated in the late 1960s, when typical lower Paleolithic lithics and middle Pleistocene fauna were found. In order to date the site, new test pits were dug adjacent to the earlier excavations and the archaeological bed was exposed in a section comprising a series of paleosols and aeolianites. Alkali feldspars separated from the sediments were dated using the infrared stimulated luminescence and thermoluminescence signals, and quartz was dated using the optically stimulated luminescence signal. The age of the archaeological bed is constrained by two samples to 198,000 ± 22,000–201,000 ± 17,000 yr. The age of the base of the section is 240,000 ± 29,000 yr, and the age of the top is 81,000 ± 8000 yr. Two teeth from the archaeological bed, recovered from the original excavation collection, yielded an average ESR age of 204,000 ± 16,000 yr, calculated using the linear uptake model, which is in a very good agreement with the luminescence ages. These dates place Holon within the range of other late Acheulian and Acheulo-Yabrudian sites in this region such as Tabun E (younger chronology), Yabrud I (archaeological level 18), and Berekhat Ram.     

Palaeomagnetism of Upper Bhander Sandstones from Central India and implications for a tentative Cambrian Gondwanaland reconstruction

A virtual geomagnetic pole position for the uppermost Vindhyan sediments in Central India, probably correlative with the Cambrian of the Salt Range (W. Pakistan), was obtained from 43 oriented cores (7 sites) drilled from the Upper Bhander sandstones in the Great Vindhyan basin.Alternating field and thermal demagnetization resulted in a mean direction: D = 207.5°, I = +9.5° (k = 137.5, α₉₅ = 5.5°) and a virtual geomagnetic northpole position: 146.5° W48.5°N (dp = 3°, dm = 5.5°).This pole position disagrees with the Cambrian palaeomagnetic results from the Salt Range. Implications of this disagreement for the pre-drift configuration of Gondwanaland, based on palaeomagnetc results, are discussed.     

Marine C reservoir ages for 19th century whales and molluscs from the North Atlantic

In order to compare radiocarbon dates on marine and terrestrial samples the former have to be corrected for a reservoir age. We present reservoir ages from dating 21 whales collected 1860–1901 and recalculating dates of 23 molluscs collected 1857–1926. Most of the whales were caught along the coast of Norway, but one is from France and one from Iceland. We assume the former mainly lived in the North and equatorial Atlantic and in the Norwegian Sea. Whales feed only on pelagic organisms and will provide the reservoir age for the open ocean surface water. However, they travel long distances and will integrate the reservoir ages of the different water masses along their way. Molluscs (dated from Norway, Spitsbergen and Arctic Canada) are stationary and monitor the sea water passing their dwelling site, but some also take up carbon from particulate food or sediment pore water. Coastal water also often contains some continental carbon. We present two different views on how to analyze and interpret the data. Mangerud recommends to use reservoir ages based on a combination of the whale and mollusc dates, i.e. 380±30 and 360±30 yr relative to Intcal04 and British oak, respectively, and a ΔR value of 20±30 for the surface water in the N-Atlantic and Norwegian Sea. Bondevik and Gulliksen maintain that the reservoir age—and ΔR—along the Norwegian coast is latitude dependant, with ΔR-values increasing from −3±22 in the South to 105±24 at Spitsbergen. Whales, reflecting North Atlantic open ocean surface water have lower ΔR (7±11) than most molluscs.     

Compressional and shear wave velocities of igneous rocks and volcanic glasses to 900° C and 20 kbar

Simultaneous measurements of compressional and shear wave velocities, V_p and V_s, in acidic and basic igneous rocks and volcanic glasses, were made up to 900°C and at 10–20 kbar.The effects of pressure and temperature on V_p and V_s in glasses and glassy rocks change at about 600°C, presumably the glass transition temperature. These effects are directly related to the silica content in the samples. and for obsidian are negative at room temperature and 245°C, but are positive at 655°C. The velocity—pressure relations for obsidian display an obvious hysteresis phenomena. for basalt glass is slightly negative, but is positive for usual substances at room temperature, and for obsidian and glassy andesite are positive up to about 600°C but are negative above that temperature. However, for basalt glass as well as other crystalline rocks, and are negative at all temperatures. Glass once heated above the glass transition temperature T_g under pressure P₁ retains the memory of pressure P₁ after it is cooled down below T_g and while subjected to another pressure P₂. An abrupt shift of the velocities correlating to pressure P₂ occurs when the glass is again heated to T_g. V_p−T and V_s−T relations for obsidian, glassy andesite, and basalt glass clearly exhibit this pressure memory.