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Article

Combined Zircon/Apatite U-Pb and Fission-Track Dating by LA-ICP-MS and Its Geological Applications: An Example from the Egyptian Younger Granites

by
Sherif Mansour
1,*,
Noriko Hasebe
2,
Ehab Azab
3,
Ashraf Y. Elnaggar
3 and
Akihiro Tamura
4
1
Geology Department, Faculty of Science, Port Said University, Port Said 42522, Egypt
2
Institute of Nature and Environmental Technology, Kanazawa University, Kanazawa 920-1192, Japan
3
Department of Food Science and Nutrition, College of Sciences, Taif University, P.O. Box 11099, Taif 21944, Saudi Arabia
4
Department of Earth Sciences, Kanazawa University, Kanazawa 920-1192, Japan
*
Author to whom correspondence should be addressed.
Minerals 2021, 11(12), 1341; https://doi.org/10.3390/min11121341
Submission received: 3 October 2021 / Revised: 23 November 2021 / Accepted: 25 November 2021 / Published: 29 November 2021
(This article belongs to the Section Mineral Deposits)
Browse Figures
Versions Notes

Abstract

:
Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS) is classically used in U-Pb dating to measure U and Pb isotopic concentrations. Recently, it has become frequently used in fission-track (FT) chronometry too. As an advantage, the U-Pb and FT double dating will enable efficiently determining the crystallization ages and the thermo-tectonic history concurrently as samples volume, analytical time, efforts, and cost will be greatly reduced. To demonstrate the validity of this approach, a Younger granite (Ediacaran age) sample from North Eastern Desert (NED), Egypt was analyzed for U-Pb and FT double dating. The integration of multiple geochronologic data yielded a zircon U-Pb crystallization age of 599 ± 30 Ma, after emplacement, the rock cooled /uplifted rapidly to depths of 9–14 km as response to the post-Pan African Orogeny erosional event as indicated by apatite U-Pb age of 474 ± 9 Ma. Afterwards, the area experienced a slow cooling/exhumation for a short period, most-likely as response to denudation effect. During the Devonian, the area was rapidly exhumed to reach depths of 1.5–3 km as response to the Hercynian tectonic event, as indicated by a zircon FT age of 347 ± 16 Ma. Then the studied sample has experienced a relatively long period of thermal stability between the Carboniferous and the Eocene. During the Oligocene-Miocene, the Gulf of Suez opening event affected the area by crustal uplift to its current elevation. This integration of Orogenic and thermo-tectonic information reveals the validity, efficiency, and importance of double dating of U-Pb and FT techniques using LA-ICP-MS methodology.

1. Introduction

The integration of different geochronological (e.g., U-Pb, K-Ar, Helium and FT dating) techniques provide useful information on the formation and development of the upper crust through geological time [1,2,3]. FTs are approximately linear damages, formed in the lattices of certain minerals and glasses by natural fission of heavy isotopes like U-238, U-235, Th-232 [4]. The preservation of FTs in minerals mainly depends on the temperature and cooling rate. For FTs in typical F-apatite, such as, for instance, Durango apatite, the temperature interval between 110 °C and 60 °C [5,6] is often referred to as the partial annealing zone (PAZ). So far, however, little is known about the mechanism and kinetics of FT annealing in Cl-rich apatite specimens. FTs in Cl-apatite are seemingly more resistant to thermal annealing if compared with tracks in F-apatite [7,8]. This feature can be especially observed during the dating of clastic samples which commonly contain partially reset to set apatite grains, factually Cl-rich ones, which may yield older FT ages as compared with F-apatite grains [9]. For example, for apatite with Cl of 3 wt.%, Donelick et al. [6] postulated that FTs begin to anneal at ca. 90 °C and experience total annealing at temperatures higher than 160 °C. This implies that the PAZ in Cl-rich apatite is wider and hotter if compared with the PAZ in F-apatite. For FTs in zircon, the effective closure temperature ranging 240 °C and 200 °C depending on cooling rates [10].
Partial annealing will reduce the apparent FT age and shorten the lengths of tracks, whereas total annealing will reset the FT age to zero removing all the spontaneous fission tracks. Therefore, FT lengths, combined with FT ages, can be used to reconstruct detailed thermal histories of rock samples [5,11].
The FT thermochronology is a powerful tool that may be applied to resolve several geological problems in a variety of geological settings [12,13,14,15]. The FT age is calculated by determining the number of spontaneous fission tracks (i.e., formed by daughter nuclides) and the number of U-238 atoms (i.e., parent nuclides) per weight of sample. In the conventional FT dating, the concentrations of U-238 are measured indirectly by irradiating of samples with thermal neutrons at a nuclear power reactor [3,16,17]. Currently, the FT ages may be determined rapidly and safely employing laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) technique for in-situ quantification of U-238 (ICP-MS: Yokogawa Analytical Systems, Japan; MicroLas: GeoLas Q-plus by MicroLas, Germany) [6,18]. The ability of LA-ICP-MS to measure rare earth elements simultaneously with U, Th, Sr, Y, Mn, Mg, Cl, and isotopic ratios—as done in many modern studies including this work—gives complementary chemical composition of apatite (or zircon, titanite) which may be used for simultaneous double dating of individual crystals by U–Pb and FT techniques as well as for petrogenetic, metallogenetic and provenance studies [19,20].
The U-Pb dating is based on decay of U and Th-232 isotopes to Pb isotopes. It is one of the most commonly used geochronological tools to obtain the protolith and magmatic ages of rocks [21]. The U-Pb system is extremely resistant to thermal overprinting (>900 °C; [22]) and is, therefore, unaffected by thermal events when the most suitable mineral, zircon, is analyzed. These advantages and improvements in the technology of LA-ICP-MS made it a rapid, precise and accurate method for U-Pb geochronology which has recently been extended [23,24,25,26,27,28,29,30,31,32]. The combination of U-Pb and FT methods could provide insights on history of the provenance that has undergone metamorphism. In this study, a Younger granite (Ediacaran age) sample from the North Eastern Desert (NED) of Egypt was analyzed to examine the possibility of achieving a simultaneous double dating of both U-Pb and FT by coeval measuring of all required isotopes using LA-ICP-MS with the final purpose of integrating the obtained results to investigate a comprehensive thermo-tectonic history of the studied sample since its crystallization. This sample is part of the Arabian-Nubian Shield (ANS) which represents the crust beneath north-eastern Africa, Arabia and SW Asia (Figure 1).

2. The Studied Sample

The ANS crops out in Egypt along the Red Sea coastline and in south Sinai (Figure 1). It was formed through multiple tectonic activities ended by accretion of island arcs during the Late Neoproterozoic [35,36,37,38]. Typical island-arc related granitoid rocks are common in the ANS [33,39,40,41,42,43]. Some previous studies proposed that these granitoids can be divided into two main groups; the older (Tonian-Cryogenian) calc-alkaline granitites and the younger (Ediacaran) alkaline granitoids [44,45,46,47]. However, more recent studies indicate that there is sometimes a coeval occurrence of the calc-alkaline and the alkalinegranitoids [48,49]. After the formation of the ANS, the Egyptian Nubian Shield (ENS) was eroded before the end of Cambrian-Silurian time and buried beneath fluvial and near shore marine sedimentary successions with Lower Cambrian-aged fossils [50,51,52]. After the Cambrian, a period of tectonic stability with the deposition of platform sediments was established [53]. This period of stability was interrupted by number of vertical movements and unconformities [54]. During the Devonian-Carboniferous, the Hercynian (Variscan) tectonic event occurred by the collision of Gondwana and Laurasia, causing significant uplift and erosion of the Lower Palaeozoic sedimentary successions by Late Carboniferous time [55,56,57,58]. During the Jurassic-Cretaceous, Gondwana began to break apart forming extensional basins with volcanism in the ENS [59,60]. Simultaneously, during the Mid-Jurassic time, the mid-Atlantic opening caused an eastward movement of Africa with respect to Eurasia producing a large sinistral shear, extensive alkaline magmatism, normal NW-SE and N-S trending faults, as well as the formation of the broad northeast trending folds of the Syrian Arc domal system [61,62,63,64]. During Oligocene to Miocene period, a significant period of uplift and erosion started along the flanks of the Red Sea-Gulf of Suez rift system, exposing the ANS terrane, active fault systems and basaltic dykes have emerged in the course of crustal uplift.
Numerous schemes classified the Egyptian granites; one of the simpler schemes divided the granites into two groups. This approach includes; the Grey and Gattarian granites [44]; the Older Grey and Younger Red granites [46]; or the syn-orogenic and Younger granites [65]. In Sabet, [65] schema, the granitic rocks became more silicic and potash rich throughout the East African Orogeny. The Older Grey granites include the assemblage of felsic plutonic rocks of essentially intermediate composition [66,67]. While, the Younger Red granite shows a pronounced shift from the dominantly trondhjemitic, tonalitic, granodioritic, and calc-alkalic plutonism to one characterized by predominance of more felsic, more alkalic, granodioritic and granitic rock types [50].
Formation of Younger granites could be resolved into two major events; the first magmatic event (630 Ma to 570 Ma) is called the Dokhan event, during which most the Younger granites of the Eastern Desert were emplaced. The second magmatic event (570 Ma to 530 Ma) is called the Katherina event which is restricted to northern ANS [68]. The studied sample was collected from the Younger granite of the Dokhan event at Gebel Somr El-Qaa area, western the Gulf of Suez, in the NED, Egypt (Figure 2). In this region, the outcrops of the ENS Precambrian rocks non-conformably overlain by the sandstone of the Araba and Naqus formations with Cambrian-Ordovician age and the consequent Cretaceous to Eocene marine carbonate rocks [69,70].
The Younger Granites are muscovite biotite granitoids, however, hornblende may occur in association with biotite in the less evolved varieties. Almandine-rich garnet is common in per-aluminous granites, while, arvedsonite and riebeckite are more common in peralkaline grantoids [71,72,73]. The Younger granites are characterized by SiO2 ranging between 70 wt.% and 80 wt.%, K2O > 3.8 wt.%, the K2O/Na2O ratios > 1, the FeO*/MgO ratios > 4, and the CaO ranges between 0.1 wt.% and 1.6 wt.%. They are enriched in the high field strength elements and total REEs and relatively depleted in Ba, Sr, and have high Rb/Sr and conversely low K/Rb ratios [74,75].

3. Materials and Methods

Apatite and zircon grains were concentrated using conventional mineral separation techniques such as rock crushing, sieving, Frantz separator (S. G. Frantz Co., Inc., City, PA, USA), and heavy liquids. Approximately 200 apatite grains extracted from the studied sample under a stereoscopic microscope (Nikon Solutions Co., Ltd., Tokyo, Japan) were mounted with EpoFix resin in a 2.5-cm-diameter plastic ring (most grains were mounted with their surfaces parallel to the crystallographic c-axis). Approximately 100 zircon crystals were mounted in a Teflon. Mounted crystals were polished to expose their internal surfaces (i.e., to 4π geometry). Polished apatite crystals were etched in 5.5 M HNO3 at 21 ± 1 °C for 20 s to reveal spontaneous fission tracks [6]. Zircon grains were etched in in a NaOH-KOH eutectic melt at 220 ± 5 °C [76] for 60–210 min.
FTs counting and horizontally confined tracks (CTs) length measurements were performed using a Nikon Eclipse 80i (Nikon Solutions Co., Ltd., Tokyo, Japan) upgraded with a digital camera, an image processing software, and dry objectives. For each apatite grain dated and CT measured, the etch pit values was determined as a kinetic parameter (Dpar; [5,6])
The U isotopic concentrations for both FT and U-Pb dating as well as the Pb isotopes for U-Pb dating were measured by the LA-ICP-MS at Kanazawa University, Kanazawa, Japan. Detailed operating conditions were reported by Morishita et al. [75] and are summarized in Table 1. For each single-spot analysis, time-resolved signals were monitored to ensure stable signal intervals; free from detectable inclusions, core–rim features, zones of high common Pb or strong evidence of fractionations. The isotopic concentrations were then calculated from background corrected intensities. In order to avoid mass bias and reduce elemental fractionation decoupling of U-Th from Pb during micro-sampling by laser ablation; (1) short wavelength of 193 nm was used [77,78], (2) stream of Ar and He mixture was used as a carrier gas to transport the ablated material, (3) short ablation time of 30 s was applied to avoid extreme heating of the ablation site and losing focusing state on the ablated surface [26,78,79], and (4) we measured repeatedly an external reference material (e.g., NIST glass) to correct the residual laser induced fractionation and instrument mass bias [26,79]. Thus, the U, Th and Pb signal intensities were calibrated against silicate glass reference SRM 610 [80]; the U-238 concentration of 456 ppm is based on the total amount of uranium and isotope ratio [81,82]; the total Pb concentration is 431 ± 15 ppm [82] and the concentration of each Pb isotope is estimated based on their isotopic ratios [83,84]. The results for measured isotopes using standard glasses were normalized using Ca-43 as an internal standard in apatite grains and taking the chemical data reported previously [8]. For zircon crystals, the results for measured masses were normalized using Si-29 as an internal standard and tacking the chemical composition from [85,86]. Zircon grains were imaged using cathodoluminescence (CL) probe facility of Kanazawa University.

4. Results and Discussion

U-Pb and FT (ZFT) dating was performed simultaneously in twelve zircon grains. Similarly, 49 apatite grains were analyzed synchronously for apatite U-Pb and apatite FT (AFT) dating. Concurrently, 28 measurements were done on the analytical standard NIST SRM 612 glass to monitor the precision of our measurement protocol.

4.1. Zircon (U-Th)/Pb

The separated zircon crystals are mostly transparent and euhedral. Grains with either visible inclusions or cracks were excluded from the U–Pb dating. Therefore, only twelve zircon grains were analyzed from the Younger granite sample (Figure 3). All the dated zircon grains have common Pb occurrence under our system detection limit with low average intensity of 7.6 cps, while the average detection limit is 72 cps. Thus, no common lead correction was performed. The U-238 content varies between 10.6 ppm and 269.8 ppm. The Th/U ratio ranges from 0.04 to 1.11 (Table 2), indicating the igneous origin for all the analyzed grains [87,88]. Zircon U-Pb ages were calculated and a Concordia diagram was plotted using the IsoplotR code [86]. Grain C7 was not used for calculations because of discordant percentage higher than 10%. This grain shows abnormal isotopic concentrations (207Pb/235U = 14.55 ppm) which recommend possible inclusions or distorted fractures (Table 2). All the other treated zircon grains are well clustered on the Concordia (Figure 3B).
Zircon grains A1 and A8 yielded concordant pre-Pan-African 206Pb/238U ages of 1730 ± 76 Ma and 1723 ± 68 Ma, respectively (Table 2 and Figure 3). Both grains are inherited from older crust, and therefore, they were not included in the weighted mean age calculations. Several previous studies already demonstrated that inherited zircon crystals are very common in the ENS [48,49,89,90,91,92,93]. Grain D3 has an age of 770 ± 36 Ma which is apparently derived from reworked Pan-African crust. Most grains dated define a uniform Pan-African U-Pb weighted mean age of 599 ± 30 Ma which can be interpreted as the crystallization age of the granitic sample studied. Cathodoluminescence (CL) imagery shows a variety of internal structures (Figure 4).

4.2. Apatite U-Pb

The apatite U-Pb ages were calculated for the same 49 grains of the FT method, where ages were calculated and isochrone diagram was plotted using the IsoplotR code [86]. These yielded apatite U-Pb weighted mean ages ranges between ca. 592 Ma and ca. 368 Ma with a weighted mean average age of ca. 440 ± 17 Ma (Table 3 and Figure 5). The effective closure temperature of apatite U-Pb varies from ca. 550 °C to ca. 450 °C [22,91,94]. The U-238 concentration ranges between ca. 22 ppm and ca. 129 ppm. Apatite grains B2, D6, H4, and I10 will not be used in age calculations because they have discordant percentage higher than 10% (Table 3). Grain B2 has a relatively higher common Pb concentration of 0.51 ppm and higher Th/U concentration of 0.84 which recommend unrecognizable inclusions. Grains D6, H4, and I10 show low 207Pb/235U concentration of ca. 0.18, 0.44, and 0.48, respectively (Table 3), which recommend a Pb-206 enrichment. All the other apatite grains define a post-Pan-African apatite U-Pb weighted mean age of 474 ± 9 Ma which is considered as a cooling age with tectonic significance. Although, this is the first apatite U-Pb study on the ENS, few studies presented high-temperature thermochronological data [54,95]. These, study produced Ar-Ar and Sphene FT ages which are comparative to our apatite U-Pb ages.

4.3. Zircon Fission Track

The ZFT ages (closure temperature of ca. 240–200 °C; [12,96]) were obtained for the same grains analyzed by the zircon U-Pb technique (Table 2), using the IsoplotR code [86]. The ZFT weighted mean ages from twelve grains range between 372 ± 69 Ma and 319 ± 39 Ma with a weighted mean age of 347 ± 16 Ma (Figure 6). The U-238 concentrations vary from ca. 93 ppm and ca. 372 ppm (Table 4). The analyzed grains pass the chi-square probability test, indicating that these zircon grains belong to a single cooling event. The lack of any discernible correlation between ZFT grains ages and uranium concentrations medicate that metamictisation effect is neglectable.
The weighted mean ZFT age of 347 ± 16 Ma is concordant with previously reported ZFT data from other parts of the ANS [54,97], indicating a tectonically driven uplift. These thermochronological results are consistent with the sedimentary hiatus in the region between the Cambrian and the Carboniferous [98,99].

4.4. Apatite Fission Track

The AFT ages (closure temperature ca. 110 °C; [100]) were calculated for the same 49 grains analyzed by the apatite U-Pb method (Table 3), using the IsoplotR code [86]. The AFT ages range between 331 ± 70 Ma and 235 ± 36 Ma with a weighted mean age of 283 ± 7 Ma (Figure 7). The U-238 concentrations vary from ca. 11 ppm to ca. 95 ppm (Table 5).
The Dpars (total 201), parallel to the c-axis of each measured grain were measured showing values range between 1.22 µm and 1.71 µm (Table 5). These Dpar values indicate a uniform typical near-end-member calcium-fluorapatites [7]. Concurrently, 185 CTs were measured.
These lengths show a wide distribution, tall of short tracks, a positive skewness, and mean track length of 10.33 µm (Table 5). Therefore, the AFT weighted mean age here indicates no special event as it represents a mixed (partially reset) age.

4.5. Time-Temperature Modelling

For a better evaluation of the sample’s thermal history and representation of the event-corresponding age, the AFT data (ages, CTs and Dpars) were modelled with the “HeFTy” program (V. 1.8.3) [101]. Additionally, we used time-temperature constraints based on the obtained zircon U-Pb, apatite U-Pb, ZFT, and AFT ages. The fourth constraint represents the mixed AFT age; therefore, it is widened to represent wider age possibilities, the fifth represents the Oligocene-Miocene thermal event accompanied the Gulf of Suez formation (Figure 8). Thus, these boxes limiting possible solution to t-T model were added based on known and reasonable constraints.
The model paths (Figure 8) indicate a slow cooling after formation, flowed by a rapid cooling by the end of the Cambrian through the Devonian-Carboniferous until the block reaches the AFT PAZ equivalent depths during the Carboniferous. The ANS was affected by intense post-accretion erosional event before the Cambrian [50,102,103], which must have triggered isostatic rebound by rock exhumation. While, the Hercynian tectonic event affected the ENS by uplifting and erosion during the Devonian-Carboniferous [56,57,58,104]. Afterwards, the area experienced a relatively long period of thermal stability since the Carboniferous till the Eocene. This stability is not consistent with the tectonic active Cretaceous period [60,61,63,105], however, previous thermochronological studies on the ENS reported differential blocks movement [16,94,95,105,106,107]. Therefore, our sample might has been located within un-uplifted block during the Cretaceous. Finally, a rapid cooling event occurred as response to the Gulf of Suez initiation during the Oligocene-Miocene. The t-T model shows no thermal overprinting accompanying the Gulf event (Figure 8), that is supported by synchronous un-resetting of the AFT age.

5. Geological Interpretation

The obtained thermochronological data are consistent with the previously reported data; however, our data provides more robust and detailed information due to the simultaneous measurement of isotopic concentrations in zircon and apatite crystals. This double dating of U-Pb and FT techniques applied in this study enabled examination of the thermal history of the studies area through four different paleo-isotherms; zircon U-Pb (ca. 900 °C), apatite U-Pb (ca. 550 °C to 450 °C), ZFT (ca. 240 °C to 200 °C), and AFT (ca. 110 °C to 60 °C). We have integrated these thermochronological information and reconstructed the t-T history (Figure 8A). The zircon U–Pb results indicate that the Younger granite was formed during the Neoproterozoic (i.e., at 599 ± 30 Ma; Ediacaran). The magma source contained zircon grains with old ages of ca. 1.7 Ga which were inherited from a Pre-Pan-African crust. Another old grain yielded a Pan-African zircon U-Pb age of 770 ± 36 Ma. These older age grains indicate a local magmatic source. After the emplacement in the lower crust 599 ± 30 Ma, the granite cooled through the apatite U-Pb isotherm (ca. 550 °C to 450 °C) to reach depths of 22 ± 3 km at 474 ± 9 Ma (geothermal gradients of 21 °C/km; [109]). Assuming a homogeneous uplifting rate and starting at ca. 550 Ma, this event of uplifting was accompanied by ca. 0.3 km/Ma exhumation rate with a moderate cooling rate of ca. 6 °C/Ma. This exhumation event was initiated as response to the intensive erosional event inferred from the ANS being eroded before the end of the Cambrian followed by deposition of cycles of fluvial to near shore marine Lower Cambrian sediments [49,50,51]. Afterwards, a second exhumation event (or the first event was continued) at ca. 425 Ma (Figure 8A) was responsible for uplifting rocks from depths equivalent to the apatite U-Pb closure temperature (ca. 550 °C to 450 °C; ~22 ± 3 km) to those of the AFT (110°C to 60 °C; ca. 3 ± 2 km) through the ZFT (ca. 240 °C to 200 °C; ~10 ± 1 km) in ca. 100 Ma. This tectonic event occurred with an exhumation rate of ca. 0.2 km/Ma (i.e., assuming a homogeneous uplifting rate), and a cooling rate of ca. 3.4 °C/Ma. This exhumation event is previously reported in the region [53], which may indicate the continuity of the post-accretion erosional event till the Silurian. That was followed by a period of thermal stability and slow erosional uplifting within the apatite PAZ. This period of tectonic stability indicates the absence of any tectonic effect for the Cretaceous breaking apart of Gondwana on the studied block. The last uplifting stage accompanied by the Gulf of Suez formation which exhumed the rocks from depths equivalent to ca. 80 °C (ca. 2 km for geothermal gradient of 42 °C/km; [110]) to elevations close to the present (281 m.a.s.l.). This event accompanied by ca. 0.4 km/Ma exhumation rate and with an elevated cooling rate of ca. 12 °C/Ma, and a corresponding total rock uplift of ca. 2 km. The surprisingly small amount of uplift and the low thermal regime (ca. 80 °C) accompanied the Gulf of Suez formation may be explained by the development of the rift/basement bounding the listric normal faults at the first stage of rift formation. These listric faults kept the rift flanks unaffected by any of the rift development features. Otherwise, the later tectonic affects as well as the thermal overprinting were restricted to the main rift axis.

6. Conclusions

The use of LA-ICP-MS in U-Pb and FT chronometry has advantages for the measurement of a wide variety of elements and isotopes concurrently without any special preparation. Simultaneous calculation of U-Pb and FT ages for both zircon and apatite grains may, therefore, be provided. Based on this double dating approach, detailed insights on the thermo-tectonic history of a granitic sample from the ENS could be revealed. The granitic sample was crystallized at 599 ± 30 Ma (zircon U-Pb age). After emplacement, it was affected by three major exhumation events represent the influence of three tectonic events on the region: (1) Before 474 ± 9 Ma (apatite U-Pb age), the rock was uplifted as response to the ANS post-accretion erosional event. This event might have extended through the Silurian. (2) During the Devonian-Carboniferous, the granitic rock was exhumed to the AFT PAZ as response to the Hercynian tectonic event. (3) The Gulf of Suez opening caused exhumation of the sample to its current elevation during the Oligocene-Miocene.

Author Contributions

Conceptualization, S.M. and N.H.; methodology, N.H. and S.M.; validation, N.H. and S.M.; formal analysis, A.T. and S.M.; investigation, S.M.; resources, N.H., E.A., A.Y.E. and S.M.; data curation, S.M., E.A. and A.Y.E.; writing—original draft preparation, S.M.; writing—review and editing, N.H., E.A., A.Y.E. and S.M.; visualization, S.M.; supervision, N.H.; project administration, A.T.; funding acquisition, E.A., A.Y.E., S.M. and N.H. All authors have read and agreed to the published version of the manuscript.

Funding

This research received no external funding.

Data Availability Statement

Data is contained within the article.

Acknowledgments

We thank Taif University Researchers Supporting Project Number (TURSP-2020/32), Taif University, Taif, Saudi Arabia; Efforts of Mohamed Ahmed, Faculty of science, Suez Canal University, Egypt are greatly appreciated for their help during the field work.

Conflicts of Interest

The authors declare no conflict of interest.

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Minerals 11 01341 g001 550
Figure 1. Location map for the ANS (the ENS; the Egyptian part of the Nubian Shield) in the frame of the African continent, and the studied sample (modified after [33,34]).
Figure 1. Location map for the ANS (the ENS; the Egyptian part of the Nubian Shield) in the frame of the African continent, and the studied sample (modified after [33,34]).
Minerals 11 01341 g001
Minerals 11 01341 g002 550
Figure 2. Simplified Geologic Map for Gebel Somr El-Qaa area, NED, Egypt (modified after [70]) representing the studied sample location and the main lithology of the region; the ANS granite (750–530 Ma), Dokhan volcanics (630–570 Ma), Araba and Naqus Formations (Lower Palaeozoic age).
Figure 2. Simplified Geologic Map for Gebel Somr El-Qaa area, NED, Egypt (modified after [70]) representing the studied sample location and the main lithology of the region; the ANS granite (750–530 Ma), Dokhan volcanics (630–570 Ma), Araba and Naqus Formations (Lower Palaeozoic age).
Minerals 11 01341 g002
Minerals 11 01341 g003 550
Figure 3. Concordia diagram [86]. (A) for all dated zircon U-Pb ages representing the two pre-Pan-African grains, (B) for all grains with Pan-African ages which gives weighted mean age of 599 ± 30 Ma (7 grains) if the older D3 grain was excluded.
Figure 3. Concordia diagram [86]. (A) for all dated zircon U-Pb ages representing the two pre-Pan-African grains, (B) for all grains with Pan-African ages which gives weighted mean age of 599 ± 30 Ma (7 grains) if the older D3 grain was excluded.
Minerals 11 01341 g003
Minerals 11 01341 g004 550
Figure 4. Cathodoluminescence (CL) images showing the location of analysis spots and their 206Pb/238U weighted mean ages for some of the analyzed zircon grains.
Figure 4. Cathodoluminescence (CL) images showing the location of analysis spots and their 206Pb/238U weighted mean ages for some of the analyzed zircon grains.
Minerals 11 01341 g004
Minerals 11 01341 g005 550
Figure 5. Tera–Wasserburg plots [86], displaying apatite U–Pb results obtained from the studied samples with excluding the discordant grains in Table 3.
Figure 5. Tera–Wasserburg plots [86], displaying apatite U–Pb results obtained from the studied samples with excluding the discordant grains in Table 3.
Minerals 11 01341 g005
Minerals 11 01341 g006 550
Figure 6. Radial plot diagram [86] for all dated ZFT grains.
Figure 6. Radial plot diagram [86] for all dated ZFT grains.
Minerals 11 01341 g006
Minerals 11 01341 g007 550
Figure 7. Radial plot diagram [89] for all dated AFT grains.
Figure 7. Radial plot diagram [89] for all dated AFT grains.
Minerals 11 01341 g007
Minerals 11 01341 g008 550
Figure 8. (A): Thermal history model for the studied sample obtained using HeFTy [103]. Resulting t–T curves show four different reliability levels; green paths: acceptable fit (all t–T paths with a merit function value of at least 0.05), purple paths: good fit (all t–T paths with a merit function value of at least 0.5), black line: best fit and dashed blue line: the weighted mean path [101,108]. Four constrain boxes, based on zircon U-Pb, apatite U-Pb, ZFT, and AFT ages, and the Gulf of Suez initiation age were chosen to guide the randomness. P: number if inverse models’ iterations, A: acceptable fit models, G: good fit models, D: determined FT age ± 1-σ error, M: modelled FT age, G.O.F.: goodness of fit between the measured and the model age, N: number of single grains. (B): Confined track lengths (CTs) distribution for the c-axis projected tracks. D: determined CTs ± 1-σ error, M: modelled CTs ± 1-σ error, G.O.F.: goodness of fit between the measured and the model CTs, N: number of CTs. (C): comparison between the corresponding AFT details of AFT age, CTs lengths, and Dpar values.
Figure 8. (A): Thermal history model for the studied sample obtained using HeFTy [103]. Resulting t–T curves show four different reliability levels; green paths: acceptable fit (all t–T paths with a merit function value of at least 0.05), purple paths: good fit (all t–T paths with a merit function value of at least 0.5), black line: best fit and dashed blue line: the weighted mean path [101,108]. Four constrain boxes, based on zircon U-Pb, apatite U-Pb, ZFT, and AFT ages, and the Gulf of Suez initiation age were chosen to guide the randomness. P: number if inverse models’ iterations, A: acceptable fit models, G: good fit models, D: determined FT age ± 1-σ error, M: modelled FT age, G.O.F.: goodness of fit between the measured and the model age, N: number of single grains. (B): Confined track lengths (CTs) distribution for the c-axis projected tracks. D: determined CTs ± 1-σ error, M: modelled CTs ± 1-σ error, G.O.F.: goodness of fit between the measured and the model CTs, N: number of CTs. (C): comparison between the corresponding AFT details of AFT age, CTs lengths, and Dpar values.
Minerals 11 01341 g008
Table
Table 1. Operating conditions for the LA-ICP-MS.
Table 1. Operating conditions for the LA-ICP-MS.
ICP-MSDetalis
ModelAgilent 7500 s
Forward power1200 W
Reflected power1 W
Carrier gas flow 1. 31/min−1 (Ar)
0.31/min−1 (He)
Auxiliary gas flow1.01/min−1
Plasma gas flow151/min−1
InterfaceNi sample cone
Ni skimmer cone
LaserDetails
ModelMicroLas GeoLas Q plus
Wavelength193 nm (Excimer ArF)
Repetition rate5 Hz
Pulse energy8 J/cm2
Pit diameter20 µm
Table
Table 2. Zircon U-Th-Pb Data for the studied sample.
Table 2. Zircon U-Th-Pb Data for the studied sample.
Grain No.Intensities (cps)Conc. (ppm)Isotopic Ratios and 1σ ErrorsAge (Ma) and 1σ Errors% dis-c.
204Pb3σ238U1σTh/U±1σ206Pb/238U±1σ207Pb/235U±1σ208Pb/232Th±1σ206Pb/238U±1σ207Pb/235U±1σ208Pb/232Th±1σ238U/235U
A1 *−17953.54.51.030.0390.3080.0054.9020.1570.0930.0021730761810601440394.0
A8 *−1513690.89.81.110.0060.3060.0014.9260.0100.1000.001172376183660608244.6
B19.1119135.312.40.840.0020.1030.0010.9750.0100.0360.0016303068835791258.8
B6 *53.560266.110.10.290.0020.0960.0030.8680.4330.0346.586591286343338532366.8
C7 *−37310.68.70.040.0020.2200.00114.5500.0088.1400.0011283582851686981954.0
D3 *0.36456.216.10.430.0020.1270.0011.1790.0140.0460.001770368023950642.6
D82.096269.815.20.730.0060.0910.0020.7750.0230.0320.0015602760332425153.9
E713.276101.211.30.370.0090.0980.0010.8200.0060.0330.0016012962633796131.1
F16.9132141.76.70.390.0160.0980.0010.8490.0060.0330.0016022963533596153.6
G418.4122102.86.81.080.0060.0920.0010.7640.0080.0310.0015672759632489221.7
G51.17170.98.51.100.0080.0990.0010.7900.0220.0340.00161029617334226−3.2
H75.570144.59.90.260.0050.1030.0010.8520.0210.0330.00163430643345409−1.3
A1 is symbol of analyzed grain, grains with * was not used in the weighted mean age, Intensities represent background corrected signal intensities, 3σ calculated for signal background to representing the detection limit of our system, Conc. = Isotopic concentrations, and isotopic ratios area background corrected values, 204Pb negative concentrations indicate being the 204Pb concentration in the mineral grain is lower than that in the background of gas flow, ±1σ error was calculated for both the isotopic ratios and ages.
Table
Table 3. Apatite U-Th-Pb Data for the studied sample.
Table 3. Apatite U-Th-Pb Data for the studied sample.
Gr.Intensities (cps)Conc. (ppm)Isotopic Ratios and 1σ ErrorsAge (Ma) and 1σ Errors% dis-c.
204Pb3σ238U1σTh/U±1σ206Pb/238U±1σ207Pb/235U±1σ208Pb/232Th±1σ206Pb/238U±1σ207Pb/235U±1σ207Pb/206Pb±1σ238U/235U
A20.0917.933.53.30.320.020.070.0090.4880.0080.0210.009407164031242611−1.0
A30.1145.927.62.80.100.010.080.0100.6020.0100.0250.010489234791850613−2.2
A60.0312.419.62.00.200.010.1030.0120.7030.0120.0270.011570315402353213−5.6
A70.0971.234.23.30.060.010.070.0090.5980.0100.0230.0094391847617469127.7
B10.107.019.72.00.160.010.090.0120.7630.0130.0270.0115442857627533135.4
B2 *0.5112.321.40.80.840.040.080.0101.3010.0210.0240.01046821846674801244.7
B30.1015.437.71.40.080.010.060.0080.4070.0070.0200.00836813346939610−6.1
B40.089.064.46.30.040.010.060.0080.4140.0070.0190.00837013352938810−5.1
B50.088.611.50.40.220.010.090.0120.6730.0110.0290.012558305222157614−6.9
B60.0821.318.10.50.160.010.090.0120.7690.0130.0290.0125763257927581150.5
B80.084.031.53.10.080.010.070.0090.5530.0090.0210.009452194471542611−1.0
B90.081.830.63.10.090.010.080.0100.5530.0090.0260.010465204471550913−4.0
C60.097.618.21.90.150.010.0840.0110.7010.0120.0260.0105182654023518133.9
C90.0833.729.92.90.110.010.060.0080.4710.0080.0210.008401153921142311−2.3
D10.084.926.72.80.110.010.080.0100.6340.0100.0240.0104812249919489123.4
D6 *0.0617.994.82.40.010.010.080.0110.1900.0030.0760.030498231772147637−181.9
E30.0845.927.61.00.180.010.080.0100.6350.0110.0220.0094862249919444112.7
E60.5112.446.03.10.560.030.090.0110.7840.0130.0260.0105372758828519138.7
E80.0971.249.81.10.060.010.090.0110.8040.0130.0290.0125402859929576149.8
E100.097.017.00.50.660.030.100.0130.7210.0120.0300.012592335512459415−7.3
F50.1212.325.91.00.300.010.070.0090.5880.0100.0210.0084331847017421117.8
F70.1015.411.12.10.110.010.070.0090.4970.0080.0220.0094081641012445110.5
F90.109.025.30.80.490.020.070.0100.5560.0090.0240.010453194491547812−0.9
F100.088.624.30.70.080.010.080.0110.6640.0110.0280.0114992451721551143.6
G20.1021.313.92.00.130.010.080.0100.6020.0100.0240.0104632047918479123.2
G30.124.037.13.70.120.010.070.0090.4830.0080.0240.009438184001247212−9.4
G40.081.845.33.70.350.020.080.0100.6260.0100.0230.0094672149319466125.4
G50.117.648.11.80.230.010.070.0090.5220.0090.0200.0084191742614390101.6
G60.4133.728.93.00.490.020.070.0090.5790.0100.0230.0094301746416454117.3
G70.084.930.11.10.070.010.070.0090.5450.0090.0240.0104401844215484120.5
G80.1217.949.71.50.630.030.080.0100.5550.0090.0250.010485224481550313−8.2
G90.0845.931.03.00.080.010.070.0100.5320.0090.0250.010452194331449412−4.4
G100.1012.456.84.60.070.010.070.0100.6100.0100.0240.0104511948318482126.7
H20.0871.228.82.90.080.010.080.0100.5880.0100.0250.010476214691750713−1.3
H30.077.013.81.50.150.010.100.0130.8790.0150.0300.0125893364034590158.0
H4 *0.0912.346.43.30.090.010.090.0110.4470.0070.0240.009540283751047412−43.9
H60.0815.424.62.60.200.010.080.0100.5670.0090.0230.009488234561645812−6.9
H90.109.035.51.30.120.010.070.0090.5250.0090.0220.0094151642914435113.2
I10.098.669.31.90.070.010.070.0100.6260.0100.0230.0094622049419456116.5
I20.0821.310.91.10.200.010.090.0120.7890.0130.0290.0115673159128572144.0
I30.584.022.02.20.870.040.070.0090.4720.0080.0220.009425173931143011−8.3
I40.081.832.23.00.110.010.070.0090.5920.0100.0230.0094381847217449117.2
I90.087.612.41.50.280.010.090.0120.7620.0130.0300.012576325752759515−0.2
I10 *0.09337.037.33.30.150.010.080.0100.4830.0080.0160.00647021400123148−17.7
J20.104.919.72.00.140.010.080.0110.6310.0100.0290.012497234971958215−0.2
J50.127.068.82.10.060.010.070.0090.5910.0100.0240.0104311747117477128.6
J60.0812.316.00.70.210.010.090.0110.6840.0110.0230.009534275292245211−0.9
J90.0915.441.64.40.180.010.060.0080.4300.0070.0190.008374133631038010−3.0
A20.089.022.60.80.230.010.070.0090.5990.0100.0220.0094421847717442117.3
Gr = Grains, A1 grain symbol, and B2 * refers to grains with %Discordance ˃10 which were excluded from age calculations, Intensities represent background corrected signal intensities, 3σ calculated for signal background to representing the detection limit of our system, Conc. = concentration by µg/g, ±1σ error for 238U was estimated as 5%, ±1σ error was calculated for both the isotopic ratios and ages, % dis-cord. = % discordance between 206Pb/238U and 207Pb/235U ages.
Table
Table 4. Zircon fission-track ages.
Table 4. Zircon fission-track ages.
Gr.238U1σNsAρsAge1σ
[ppm](×103 Track/cm2)[Ma]
A192.74.5113814.631939
A8209.49.8105618.136964
B1266.112.4117430.233042
B6217.410.1118524.434640
C7187.58.7132622.737269
D3345.516.1139720.535063
D8326.415.297425.133469
E7243.211.391331.334947
F1144.56.777326.535421
G4144.96.8193449.835115
G5182.28.571418.335154
H7212.59.9124816.033526
Weighted Mean ZFT Age34716
Gr = Grains, A1 grain symbol, U; Uranium concentration in ppm, 1σ = uncertainty of 1-sigma, Ns; number of spontaneous tracks, A; Area in square microns, ρs; density of spontaneous tracks (103 tr/cm2), W.M. age; weighted mean age in million years calculated using IsoplotR [86].
Table
Table 5. Apatite fission-track ages.
Table 5. Apatite fission-track ages.
Gr.238U1σNsAρsCTLSDθDparSDAge1σ
[µg/g](×103 Track/cm2)[µm][µm]°[µm][Ma]
A233.53.359125.1 10.20.6481.50.0229048
A327.62.83184.0 9.12.1631.50.2027757
A619.62.01863.1 10.31.4401.50.1630277
A734.23.33584.5 10.81.9401.50.1125350
B119.72.01562.6 10.72.8601.60.0825169
B221.40.81243.1 9.80.4601.70.1927785
B337.71.43065.2 10.43.2471.50.0426255
B464.46.3111129.6 7.31.5651.60.0628339
B511.50.41061.7 8.60.5631.60.1928795
B618.10.51142.8 9.40.4451.60.1829995
B831.53.1322655.4 9.63.2751.50.0929263
B930.63.1102205.3 10.30.4541.60.1432737
C618.21.928122.4 10.80.7501.50.1225454
C929.92.93293.7 9.21.5671.50.1723648
D126.72.82364.0 9.50.3551.60.1028466
D694.82.42221812.7 10.10.5661.50.0725720
E327.61.03894.4 9.30.9571.40.0630258
E646.03.12646.7 10.44.2751.50.1027961
E849.81.16288.0 8.92.5521.40.0530750
E1017.00.51882.3 10.00.3411.70.1326167
F525.91.02893.2 9.71.5231.50.0723851
F711.12.1741.8 12.12.5501.50.05310121
F925.30.83493.9 10.90.7441.50.0229458
F1024.30.71243.1 9.11.2671.60.1424475
G213.92.01362.2 9.40.2631.50.0730790
G337.13.744104.5 9.61.5741.40.1523536
G445.33.798166.3 9.41.3551.60.1526730
G548.11.86597.5 9.93.1751.50.1429638
G628.93.051124.4 9.72.6781.50.1729050
G730.11.150124.3 9.90.8471.40.0427347
G849.71.5165208.5 11.62.6501.70.0732731
G931.03.04194.7 11.41.8571.50.0829054
G1056.84.6116158.0 10.41.1561.30.0526933
H228.82.92965.0 9.92.1491.40.0433070
H313.81.532122.2 9.81.2681.50.1230454
H446.43.35386.1 10.00.8541.60.0725143
H624.62.63763.8 10.72.6731.20.2729657
H935.51.331155.3 10.22.1561.30.0928759
I169.31.95599.5 11.02.4611.70.3626144
I210.91.114101.6 9.80.5541.60.1628180
I322.02.21162.8 11.81.2471.50.2924779
I432.23.04865.5 10.72.3471.60.0932657
I912.41.51792.0 10.12.5731.50.1830179
I1037.33.32045.2 12.62.6551.40.0526565
J219.72.02493.1 9.60.7631.40.2230164
J568.82.17199.2 10.71.1671.40.0725540
J616.00.73742.5 10.41.7471.40.1230350
J941.64.45785.9 12.01.7631.50.0927139
Weighted Mean AFT Age2837
Gr = Grains, A1 grain symbol, U; Uranium concentration in ppm, 1σ = uncertainty of 1-sigma, Ns; number of spontaneous tracks, A; Area in square microns, ρs; density of spontaneous tracks (103 tr/cm2), CTL; confined track lengths, SD; Standard deviation of CTLs, θ; Angle from the c-axis in degrees, W.M. age; weighted mean age in million years calculated according to the equation in [18].
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Mansour, S.; Hasebe, N.; Azab, E.; Elnaggar, A.Y.; Tamura, A. Combined Zircon/Apatite U-Pb and Fission-Track Dating by LA-ICP-MS and Its Geological Applications: An Example from the Egyptian Younger Granites. Minerals 2021, 11, 1341. https://doi.org/10.3390/min11121341

AMA Style

Mansour S, Hasebe N, Azab E, Elnaggar AY, Tamura A. Combined Zircon/Apatite U-Pb and Fission-Track Dating by LA-ICP-MS and Its Geological Applications: An Example from the Egyptian Younger Granites. Minerals. 2021; 11(12):1341. https://doi.org/10.3390/min11121341

Chicago/Turabian Style

Mansour, Sherif, Noriko Hasebe, Ehab Azab, Ashraf Y. Elnaggar, and Akihiro Tamura. 2021. "Combined Zircon/Apatite U-Pb and Fission-Track Dating by LA-ICP-MS and Its Geological Applications: An Example from the Egyptian Younger Granites" Minerals 11, no. 12: 1341. https://doi.org/10.3390/min11121341

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