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On the Past Climate of the Dobrogea (Romania) During the

Late Quaternary as Reflected by Loess Geochemistry

1 2 3,4 5 6 6,7 6
L.C. Tugulan , O.G. Duliu , Ana-Voica Bojar , Delia Dumitras , Inga Zincovskaya , Otilia A. Culicov and Marina V. Frontasyeva
University of Bucharest, Doctoral School on Physics, Romania, 2University of Bucharest, Department of Structure of Matter, Earth and Atmospheric Physics and Astrophysics, Romania, 3University of Salzburg, Department of Geology and
Geodynamics, Austria, Mineralogy, Studienzentrum Naturkunde, Graz, Austria, 5National Geological Museum, Bucharest, Romania, 6Joint Institute for Nuclear Research, Frank Neutron Physics Laboratory, Dubna, Russian Federation,

National Institute for R&D in Electrical Engineering ICPE-CA, Bucharest Romania

The XRD data mentioned above documented the presence of zircon in all the Costinesti samples,
which can very well explain the higher content of both Zr and Hf. Zircon incorporates Hf during
crystallization, so that zircon contains 1-4% of Hf, in agreement with the present data showing a
Hf/Zr ratio of 3.1 ± 0.1 %, very close to those of UCC and NASC: 3.1 and 3.2 % respectively but
Loess is an aeolian type of sediments, which consists of fine grains of quartz, feldspars, clay, Mineralogy The results of XRD analysis of bulk material show that both loess and palaeosol higher than those of PAAS equal to 2.4%.
carbonates with traces of magnetite and other heavy minerals. A long term exposition of rocks to sequences consist mainly of six dominant mineral fractions: quartz, albite and K-feldspars,
atmospheric factors can be related to physical and chemical weathering, the last one progressively smectite/chlorite, mica and calcite with traces of heavy minerals, the most abundant being monazite Sc, Zr, REE, Hf and Th, due to their relative low mobility represent good indicators of the
transforms feldspars into minerals more resistant to the action of atmospheric factors like iron oxy- and zircon. Accordingly, the quartz content varies between 17 and 24 %, feldspars (albite and sedimentation processes. Indeed, both Th/Sc versus Zr/Sc (McLennan et al. 1993 ) (Fig. 5A) and
hydrates or clay minerals. microcline) between 18.2 and 40.1 %, chlorite (chamosite) between 9.6 and 16.1 %, ilite between La/Th versus Hf (Floyd and Leveridge, 1987) (Fig. 5B) biplots suggest the existence of significant
24.5 and 40.4 %, calcite between 1.1 and 9.9 %, while the content of heavy minerals varied between sediments recycling, in concordance with their continental origin.
In the case of loess deposits, which consist of loess layers separated by palaeosol strata, the former 1.1 and 3 % (Table 1). Among them, the content of calcite and albite displayed the highest variance:
formed during shorter interglacial period. In order to decipherer it, various climate-proxi such as 50 and 39 % respectively while the quartz and illite showed to be steadier with a variance of 22 %.
grain size (Marković et al. 2007), isotopic signature (Li et al. 2007, Schatz et al., 2010), magnetic
susceptibility, (Nie et al., 2013) or detailed mineralogical and geochemical investigations were The mineral composition of analyzed samples is in good agreement with the existent data regarding
carried out (Markovici et al. 2006, Schellenberger and Veit, 2006, Bokhorst et al. 2006). Among loess mineralogy, while the presence of calcium carbonate, chlorite and mica suggests a weak to
them, the chemical index of alteration (CIA) (Nesbitt and Young, 1982) provides a quantitative moderate weathering, corresponding to the so-called S1 stage (Terhorst et al. 2012). At the same
estimation of the degree of silicate hydrolysis by monitoring the content of major oxides Na2O, time, it can be noticed the absence of any significant difference between loess and palaeosols Figure 3: A biplot of the Na2O/K2O ratio versus CIA (Song et al 2014); HAL Hungarian Average
Al2O3, K2O and CaO during the chemical weathering. along the entire loess column. This is also confirmed by both Cluster and Principal Component Loess (after Újvári et al.2008) (A) and the CN-K-A ternary plot (Nesbitt and Young 1984) (B), the
Analysis. Indeed, both methods did not evidenced any correlation between soil and palaeosol last one illustrating the relative situation of Costinesti loess and palaeosol samples with respect to
Depending on the rocks type as well as on the degree of weathering, CIA can varies from 30 - 55 in samples regarding their mineralogical composition, which, in our opinion, pointed towards either to a neighboring Mircea Voda and Hungarian loess as well as some characteristics minerals and rocks
the case of fresh, basalt, granite or granodiorite, to 75 in the case of illite and muscovite rich deposits relatively weak influence of the local climate, or to a relative steady weather during the past 730 ky. presenting different degrees of weathering (some data after Buggle et al. 2011).
and reaches a maximum value of 100 in the case of kaolinite or gibbsite (Nesbitt and Young, 1982;
Fedo et al., 1995, Bahlburg and Dobrzinski, 2011). CIA values ranging between 50 and 70 indicate a Table 1 X ray diffraction data concerning the mineral composition of Costinesti loess and palaeosol samples The content of major elements from the acid leached samples allowedto calculate both CIA (Nesbitt
weak weathering, which is characteristic for a cold and arid climate. CIA values between 70 and 85 and Young, 1982) and CIW Harnois (1988). CIA values varied between 54.6 and 64 with an average
show a moderate degree of weathering specific to a warm and humid climate while CIA values over Sample value of 59.2 ± 3.3, lower than the neighboring Hungarian loess, but very close to the average loess
85 characterize a high degree of chemical weathering (Nesbitt and Young 1982, Taylor and Mineral as defined by Ujvari et al (2008) (Table 2). With respect to UCC (Taylor and McLennan, 1991) whose
PS I LI L II L III PS II L IV PS II LV L VI PS IV Figure 5: The Th/Sc versus Zr/Sc plot (McLennan et al. 1983) of both Costinesti loess and palaeosol ilustrating Zr
McLennan 1991). CIA is of 48.6, Costinesti loess presented slightly higher values, but significantly lower than those of enrichment (high Zr/Sc ratio) due to sediment recycling. For comparison, the similar data for UCC, NASC and PAAS
Calcite 5.7 2.1 3.3 1.6 7.8 3.5 7.9 8.9 8.6 7.5 NASC (CIA equal to 67.8) (Gormet et al. 1984) and PAAS (CIA equal to 70.5) (Taylor and McLennan, are illustrated too (A) as well as the The La/Th versus Hf plot (Floyd and Leveridge, 1987) of the same samples which,
Due to the relative higher mobility of Sr with respect to Rb, the Rb/Sr ratio (Dypvik and Harris, 2001), Quartz 27.4 23.1 17.2 27.0 20.0 19.1 23.2 21.7 21.9 19.8 1991). by a relative high content of Hf and low La/Th ratio suggests the presence of recycled components. For comparison,
can be used as well in order to evaluate the degree of post-depositional weathering of loess Smectite/Chamosite 9.9 8.2 9.0 6.8 10.0 8.9 6.10 9.5 5.2 6.2 the similar data for UCC, NASC and PAAS are illustrated too.
sequences (Zhang et al. 2013). K-feldspar 9.7 10.5 12.6 11.0 9.5 13.7 16.1 13.7 13.1 16.1 A linear fit of the CIA values versus depth showed, within experimental uncertainties, an almost
constant value suggesting a steady and relative moderate chemical weathering, which, at its turn,
Albite 8.4 17.5 30.5 17.2 20.9 23.2 13.2 15.0 8.9 16.8
In Romania, loess occupies about one third of territory (Fig. 1), the most important deposits being indicate a moderate arid and cold climate during the past four glacial cycles. This finding is The REE contents offer information concerning origin and evolution of rocks (McLennan, 1989).
Ilite 36.9 33.5 24.5 34.8 28.3 28.7 31.1 27.5 40.4 30.4 The distribution on a chondrite normalized diagram (Fig. 6) shows a typical pattern for the
localized in Dobrogea and in the Romanian Plain where, at Hagieni, loess deposits reaches a sustained also by the biplot of Na2O/K2O molar ratio versus CIA (Song et al 2014) (Fig. 3A) where all
maximum thickens of 55 m (Jipa, 2013). Previous investigations of the loess deposits from Romania Heavy minerals 1.9 2.0 2.8 1.9 2.8 2.9 2.5 3.7 3.0 3.1 points corresponding to Costinesti loess show a rather cold and arid climate. continental crust , very similar to those of UCC, NASC as well as PAAS. According to the data
were summarized by Radan (2012). In this study we are performing for a loess sequence from reproduced in Table 4, all of them present almost the same La/Yb ratio of 17.3 ± 1.1, slightly higher
Costinesti, Dobrogea, a detailed geochemical and mineralogical analysis applying different The Rb/Sr ratios equal to 0.35 ± 0.09, showed a value lower than Hungarian average loess but than those of UCC and PAAS but significantly higher than NASC. A possible explanation is related
climate-related proxies as well as by multi-variate statistical analysis, which bring new comparable with those of the average loess (Ujvari et al (2008) and slightly higher than UCC (Table to a relatively high content of monazite, as indicated by XRD data.
palaeoclimatic insights. 2). A correlation coefficient of 0.6772 at p < 0.05 between SiO2 and Rb/Sr indicates a terigenous
origin of loess (Xu et al, 2010). Also the absence of a notable difference between loess and Another parameter which characterize the REE distribution consists of the EuN/Eu* ratio (EuN
palaeosol values of the Rb/Sr ratio is consistent rather constant weathering processes. stands for chondrite normalized content while Eu* is equal to the geometric mean of the product of
Sm and Gd contents normalized to chondrite, i.e. Eu*= (SmN*GdN)½ which define the Eu
In Fig. 3B, the points corresponding to Costinesti samples on the a CN-K-A (Nesbitt and Young, anomaly). In the case of Costinesti samples, the EuN/Eu* ratio has an average value of 0.63 ± 0.06
1984, 1989) ternary diagram show on one hand that between loess and palaeosols there are no close to those of UCC and PAAS (Taylor and McLennan 1991). Moreover, the average La/Th ratio,
significant differences, and that, despite different CIA values, Costinesti loess shows the same has for loess/ palaeosol samples an average value of 2.78 ± 0.06, very close too to all three average
Costinesti loess The aeolian deposits of south Dobrogea (Fig. 1) presents some features origin as Micea Voda (Central Dobrogra) and Hungarian loess. sedimentary rocks: UCC, NASC and PAAS.
which could be considered typical for loess such as the absence of bedding or a high porosity
estimated to 45-50%. Located in the immediate vicinity of the Black Sea as one of the most On this diagram, all points corresponding to both loess and palaeosol from Costinesti, are on the
representative for this region. Moreover, the Costinesti cliff loess, with a thickness of 19-20 m, same weathering sequence as UCC. This suggest that, the original material of Costinesti samples
displays a relatively well expressed alternation of loess and palaeosols a characteristic feature of had initially a mineral composition very close to the UCC, but that during weathering, although
the most loess deposits (Haase and Richter, 1957, Conea, 1970, Constantin et al. 2014) (Fig. 1). relatively weak, K2O and CaO from the silicates was partially leached.
Here six loess horizons (LI LVI) were put in evidence, interbedded with six palaeosol levels (PSI
PSVI) and overlying the Lower Pleistocene reddish clay deposited above the Sarmatian limestones The content of major elements of the Costinesti loess deposit shows that the original material had a The Costinesti loess deposit developed during the last four glacial cycles consists mainly of quartz,
(Conea, 1970). Palaeosol layers, PSI and PSII, contain chernozem while the other ones, i.e. PSIII Figure 2: Spider diagram representing the content ± 1 s of major elements normalized to UCC(Taylor and albite and K-feldspars and smectite/chlorite with minor calcite and chamosite as well as with traces
chemical composition very close to the UCC, and that during the past four glacial cycles, the loess
to PS VI are rich in forest soil. Paleomagnetic data estimated the age of the lowermost palaeosol McLennan, 1991) (A) and the tree diagram illustrating the correlation between the major elements of loess and of heavy minerals, which monazite and zircon show a higher content. The geochemistry of major,
was deposited in a relatively cold and arid climate which subsequently determined a reduced
layer to 650 ± 90 ky, which corresponds to the Güntz-Mindel interglacial (Conea, 1970, Ghenea and palaeosol samples from Costinesti (B). rock forming elements, show that Al, Si and Ca as oxides, account for 85 to 88 of all major elements,
degree of weathering. At the same time, the absence of a sizable difference between loess and
Radan, 1993). The upper layers of loess, i.e. L I, LII and LIII were attributed to Würm glacial period, palaeosol showed that in interglacial periods, the weathering process did not significantly close to existing data regarding average rocks UCC, NASC and PAAS. At the same time, the
the intermediary one, i.e. L IV to Riss glacial period while the basal horizons consisting of altered Major elements The content of all nine major elements, as oxides, illustrated by means of the developed. average contents of 26 trace elements was, with the exception of Cr, Ni, Zr and Hf , very close to
Loess correspond to Mindel glacial period (Conea, 1970). More recent spider diagram reproduced in Fig. 2 A show, that SiO2, Al2O3 and, at a lesser extent CaO, represents those of the average rocks UCC, NASC and PAAS.
paleomagnetic and optical stimulated luminescence data attributed the the dominant component of both loess and palaeosols with a total content between 85 and 88 Trace Elements The content of 26 trace elements, including 10 REE as determined by INAA
L I loess layer cover to Marine Isotopic Stage (MIS) 2 to 4, paleosol PS I %.The data are very close to both Hungarian and average loess as well as to UCC, but exceeding were determined in the same samples of loess and palaeosol. The resulted data are illustrated, by a The distribution of low mobility elements as Sc, Zr, REE, Hf and Th proved not only the continental
layer to MIS 5, while L II and L II strata correspond to MIS 6 and MIS 7 with few percent both NASC and PASS contents. Regardless the local variation, the total content of spider diagram in Fig. 4A. For a better comparison with respect with continental average origin of loess material, but also the existence of significant recycling process of the loess material.

respectively (Constantin et al. 2014).

Actual soil
these three components remains almost constant. Moreover, the cluster analysis showed that all composition, in Fig. 4A, all contents were normalized to UCC (Taylor and McLennan, 1991). The REE distribution showed a typical upper continental pattern with a well evidenced Eu negative
Loess I
nine major elements form two clusters (Fig. 2B), one of them consisting only of calcium oxide while anomaly.

Analitical methods Energy Dispersive X Ray Fluorescence Paleosoil I the other one contains all other elements grouped in three sub-clusters. By taking into account the Excepting Cr and Ni as well as Zr and Hf, the average content of all other elements is close to UCC
mineral composition of both loess and palaeosol samples as determined by XRD, the first cluster and PAAS (Taylor and McLennan, 1991) as well as NASC (Gormet et al. 1984), this fact indicating as Three different climatic proxies: CIA, CIW and Rb/Sr ratios pointed towards a rather arid and cold
(EDXRF) and Epithermal Neutron Activation Analysis (ENAA) were 4
climate during loess deposit development, confirmed by the mineralogical data regarding the
used to determine the content of nine major and 28 trace elements PS I
Loess II
could be mainly attributed to calcium carbonate, while the other one, by taking into account the well the continental origin of the loess material. It is difficult to evidence any significant difference,
presence of silicon and aluminum oxides could be attributed to feldspars and clay minerals. within the experimental uncertainties, between loess and palaeosol trace elements distribution. This presence of both calcite and clay minerals.
respectively. While the X Ray Diffraction (XRD) were used to 6

determine the minerals presented in loess and paleosol samples. Cc

Paleosoil II
Regarding the calcium oxide, it should be remarked that its average content is about the same that is in agreement with previous observations regarding the weak influence of paleoclimactic
of Hungarian loess, but significant higher than those of average loess, as well as of the other conditions on both loess and palaeosol deposits. Moreover, a ternary diagram of insoluble elements Neither mineralogical or geochemical composition evidenced, within experimental uncertainties,
L II Loess III average sedimentary rocks. Moreover, the CaO content presented the higher variance of about 40 Sc-La-Th (Fig. 4B) shows that all Costinesti samples form a single cluster together with any difference between loess and palaeosol samples, this peculiarity suggesting the presence of a
Depth (m)

%, most probable due to the irregular distribution of calcium carbonate concretions whose presence corresponding points of UCC, NASC and PASS, in perfect agreement with the above mentioned semi-arid and rather cool climate during the past 780 ky.
Ucraina L III
Paleosoil III
48o 10 L IV Loess IV was observed along entire loess/palaeosol column (For XRF analysis calcium carbonate was remarks regarding the continental origin of loess palaeosol deposits.
Paleosoil IV
Satu Mare LV
removed with HCl.
Baia Mare Suceava L IV Loess V
Hungary Bi
12 References: Bland, W., and Rolls, D. (1998) Weathering. An introduction to the scientific principles. Arnold Publishers, London, 271 Bahlburg, H., and Dobrzinski, N. (2011) A
iver st review of the Chemical Index of Alteration (CIA) and its application to the study of Neoproterozoic glacial deposits and climate transitions, in: E. Arnaud, G.P. Halverson and G. Shields-
es R rit Moldova Paleosoil V
Som a Zhou (eds), The Geological Record of Neoproterozoic Glaciations, Geological Society, London, Memoirs, 36, 81-92, doi: 10.1144/M36.6. Bjørlykke, K. (2010) Sedimentary
Oradea Bistrita Riv
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Table 2 The content of major elements oxides (wt %) as well as of the Rb and Sr (ppm) of the Costinesti loess and Geochemistry: How Sediments are Produced , in: Petroleum Geoscience: From Sedimentary Environments to Rock Physics, (K. Bjørlykke , ed.), Springer-Verlag Berlin, pp. 87-110;
Paleosoil V
Neamt palaeosol sample. For comparison the content of the same elements in average Hungarian loess (AH) , average loess Bokhorst, M.P., et al. (2009) Quaternary International 198, 113-123; Buggle, B., et al (2011). Quaternary International 240, 12-21; Catt, J.A. (1986) Soils and Quaternary geology. A
Cluj-Napoca Loess VI Handbook for Field Scientist, Oxford Sciences Publications, Clarendon Press, Oxford; Conea, A. (1970) Quaternary Deposits of Dobrudja, Academia Publishin House, Bucharest (in
, UCC, NASC, and PAAS are given as well.

Targu Bacau 16 Romanian); Constantin, D., et al. (2014) Quaternary International 334-335, 20-29; Crystallography Open Database (2014) http://www.crystallography.net/ (last accessed 01.06.2014);
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t Riv

Ele- Sample
Paleosoil VI study of the Black Sea Holocene depositional cycles: paleoenvironmental reconstructions, Ph.D. Thesis, University of Bucharest (in Romanian) Floyd, P. A., and Leveridge, B. E.
Prut River


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Ucraina Al2O3 14.62 14.37 11.64 16.17 13.43 15.26 14.61 12.60 15.52 17.08 14.53 ± 1.63 13.45 11.74 15.2 16.90 18.9 Geology, 55, 319322; Johnsson, M.J. (1993) The system controlling the composition of clastic sediments. in: M.J. Johnsson and A. Basu (eds) Processes controlling the composition of
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SiO2 61.96 65.00 64.83 67.37 59.40 61.89 65.88 60.22 61.37 60.33 62.83 ± 2.73 63.48 70.71 66.9 64.08 62.8
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ge Ialomita loess deposits. The TIO2 0.71 0.71 0.71 0.80 0.61 0.67 0.71 0.59 0.74 0.74 0.7 ± 0.06 0.91 0.71 0.5 0.70 1.0
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Pitesti sR R iver MnO 0.10 0.09 0.09 0.11 0.08 0.09 0.10 0.08 0.11 0.12 0.1 ± 0.01 0.09 0.07 0.08 0.06 0.11
inset illustrates the (2001) Geochemistry, Geophysics, Geosystems 2, 24, 2000GC000109; Nesbitt, H.W. (1979) Nature 279, 206-210, Nesbitt, H.W., and Young, G.M. (1982) Nature 299, 715 - 717;

ive FeO 5.08 4.94 5.44 6.11 4.91 5.01 5.36 4.31 5.46 6.82 5.34 ± 0.7 4.67 3.75 4.5 5.09 6.5
r Bucharest Black loess column stra- Nesbitt, H.W., and Young, G.M., (1984) Geochimica et Cosmochimica Acta 48, 1523-1534; Nesbitt, H.W., and Young, G.M. (1989) Journal of Geology 97, 129147; Nie, J., et al. (2013)
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Constanta Sea tigraphy. Collecting Sr 234 275 307 220 261 263 193 250 305 251 256 ± 35 183 210 350 142 200
Figure 4: Spider diagram illustrating the content ± 1  of trace elements normalized to UCC (Taylor and McLennan, al. (2010) Quaternary International 240; Schnetger, B., 1992. Neues Jahrbuch für Mineralogie Monatshefte 1, 2947; Song, Y., et al. (2014) Quaternary International, doi:
100 km 24o Giurgiu Costinesti points are marked CIA 61.5 54.6 57.8 59.2 60.8 55.2 56.0 59.4 64.0 63.5 59.2 ± 3.3 64.6 59.8 48.6 67.8 70.5 10.1016/j.quaint.2013.12.053; Taylor, S,. McLennan, S. (1991) The continental crust: its composition and evolution. Blackwell, Oxford, ISBN 978-0632011483; Terhorst, B., et al.
Danube River
Bulgaria CIW 70.1 58.3 65.7 68.1 68.9 62.9 65.2 67.8 71.7 71.2 67.0 ± 4.1 73.6 68.0 54.2 81.8 82.7 1991)(A) an Figure 8 the Sc-La-Th ternary diagram for Costinesti samples (B). Together with UCC, NASC and PAAS, (2012) Quaternary International 265, 142154; Tugulan, L.C, and Duliu, O.G. (2014) Romanian Reports in Physics, 66, 862876, Újvári, G., et al. (2008) Quaternary Research, 69, 421
by red dots. Rb/Sr 0.35 0.34 0.28 0.47 0.26 0.32 0.55 0.28 0.29 0.38 0.35 ± 0.09 0.56 0.37 0.32 0.88 0.80 the Costinesti samples form the same cluster proving the continental origin of loess and palaeosol material. 437; Xie, Y. et al. (2014) Catena, 123, 70-78; Xu, H., et al. F.(2010) Geochemical Transactions 2010, 11:3, Wang, W., et al. (2012) International Journal of Earth Science, 101, 1723-
1744, Zhang, W., et al. (2013) Environmental Earth Science, 70, 2191-2202

Acknowledgment This work was partially done within the Protocol No. 4322-4-14/16 between the Joint Institute of Nuclear Research and the University of Bucharest. BY