Environmental dynamics and luminescence chronologyfrom the Orlovat loess–palaeosol sequence (Vojvodina,northern Serbia)

SLOBODAN B. MARKOVIC,1* ALIDA TIMAR-GABOR,2 THOMAS STEVENS,1,3 ULRICH HAMBACH,4 DRAGAN POPOV,1

NEMANJA TOMIC,1 IGOR OBREHT,1,† MLADJEN JOVANOVIC,1 FRANK LEHMKUHL,5 HOLGER KELS,5 RASTKO MARKOVIC6

and MILIVOJ B. GAVRILOV1

1Chair of Physical Geography, Faculty of Sciences, University of Novi Sad, 21000, Novi Sad, Serbia2Faculty of Environmental Science, Babes-Bolyai University, Fantanele 30, 400294 Cluj-Napoca, Romania, and InterdisciplinaryResearch Institute on Bio-Nano-Science of Babes-Bolyai University, Treboniu Laurean 42 400271, Cluj-Napoca, Romania

3Centre for Quaternary Research, Department of Geography, Royal Holloway University of London, Egham, Surrey TW20 0EX, UK4Chair of Geomorphology, University of Bayreuth, 95440, Bayreuth, Germany5Department of Geography, RWTH Aachen University, Wullnertsr. 5b D-52056, Aachen, Germany6High school “Isidora Sekulic”, Vladike Platona 2, 21000 Novi Sad, Serbia

Received 5 July 2013; Revised 13 January 2014; Accepted 18 January 2014

ABSTRACT: The Carpathian Basin contains some of the best preserved loess deposits in Europe, including someof the continent’s longest and best resolved climate records. Large areas of the basin have been intensivelyinvestigated in recent years, although deposits in the east remain largely unstudied, despite considerable regionalvariation in climate records. Here we discuss the sedimentary record exposed in the Orlovat brickyard usingdetailed litho- and pedo-stratigraphic, enviromagnetic parameters and luminescence dating. The results show anatypical Late Pleistocene succession for the Carpathian Basin. Notably, the normally widespread pedocomplexV-L1S1 is missing. This contrasts with other parts of the sequence, which appear highly resolved, such as thethicker pedocomplex V-S1 and the detailed transitions between modern pedocomplexes V-S0 and the last glacialloess unit V-L1. The luminescence chronology demonstrates a lack of intensive pedogenesis during the EarlyHolocene and raises an important general question about the beginning of Holocene soil formation in the region.The later Holocene soil formation adds to a growing body of evidence that suggests more complex terrestrialresponses of climate to global climate change. This evidence weakens the validity of previously generalized directstratigraphic correlations between regional terrestrial environmental archives, and global marine and ice corerecords. Copyright # 2014 John Wiley & Sons, Ltd.

KEYWORDS: enviromagnetism; loess; luminescence dating; Serbia; Orlovat.

Introduction

Loess deposits in the Carpathian Basin provide evidence forhighly variable climate, dust deposition and soil formationover the region during the Quaternary (Fuchs et al., 2008;Markovic et al., 2008; Schmidt et al., 2010; Stevens et al.,2011). It is not clear whether this implies strong regionalgradients in environment or local differences in loess sedi-mentation. While certain areas of the Carpathian Basin loessregion have been well studied (notably the north, central andwest of the basin), deposits in the east have received littleattention and the late Quaternary environmental and dustaccumulation record from that region is poorly known. Thisrepresents a major gap in understanding climate and dustdeposition variability over the region.The northern Serbian province of Vojvodina is a lowland

part of the southern Carpathian Basin encompassing theconfluence of the Danube, Sava, Tisa (Tisza), Drava (Drau),Morava and Tami�s (Temes, Timis) rivers (Markovic et al.,2008). These rivers separate three Vojvodinian sub-regions:Srem, Ba�cka and Banat, which partly extend to the neigh-bouring countries of Croatia, Hungary and Romania (Fig. 1).Loess sediments in the Vojvodina region are among the oldestand most complete loess–paleosol formations in Europe.These thick sequences contain a detailed palaeoclimaticrecord since the Early Pleistocene (Markovic et al., 2011).

Recently, Vojvodina loess–palaeosol sequences have beenintensively investigated, especially at the Srem, Titel andBa�cka loess plateaus (Markovic et al., 2006, 2007; Antoineet al., 2009; Bokhorst et al., 2009, 2011; Schmidt et al.,2010; Stevens et al., 2011). The continuous presence ofapparently much drier conditions in the region and persis-tence of stable ‘plateau’ accumulation (Markovic et al., 2012)has resulted in more detailed and long-term sedimentaryrecord preservation than in other European areas. However,the Tami�s loess plateau of the eastern Carpathian Basin hasnot previously been investigated.Lying on the Tami�s plateau, the Orlovat loess site is located

further to the east than similar previously investigated Serbianloess sections (Fig. 1). Its geographical position provides aunique opportunity to reconstruct climatic and environmentalevolution in the transitional area between the south-easternlimit of the Carpathian Basin and the Western Carpathianslopes and allows us to extend our understanding of regionalclimate and dust deposition into the poorly understood eastof the basin. The Carpathians are located at the boundarybetween central and eastern European lowlands, with appar-ently sharp transitions in morphology and climatic conditions.During the winter, conditions are dominated by inflow ofpolar-continental air masses arriving from the east and north-east, while during other seasons oceanic air masses from thewest predominate. The morphology of the Carpathian Moun-tains also controls the area’s precipitation distribution. Mostof the mountain chain is characterized by humid environ-mental conditions, contrasting with continental conditions inthe intermontane depressions and on the lower parts of the

�Correspondence: S. B. Markovic, as above.E-mail: slobodan.markovic@dgt.uns.ac.rs†Present address: 5Department of Geography, as above.

Copyright # 2014 John Wiley & Sons, Ltd.

JOURNAL OF QUATERNARY SCIENCE (2014) 29(2) 189–199 ISSN 0267-8179. DOI: 10.1002/jqs.2693

Figure 1. The study area. (A) Map of the Vojvodina region with the geographical positions of the main loess sections (Markovic et al., 2004,modified). (B) A geomorphological map of the Tami�s loess plateau surrounded by the Tami�s and Begej river valleys (Popov et al., 2012a,modified). This figure is available in colour online at wileyonlinelibrary.com.

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190 JOURNAL OF QUATERNARY SCIENCE

southern mountain slopes leading to the Valahian plain. TheCarpathians thus represent a humid biogeographical islandand biodiversity hotspot. Considering the temporal dynamicsof Pleistocene biogeographical change, the transitional areabetween the Carpathian Basin and the south-western Carpa-thian slopes can be regarded as a zone of significantbiogeographical and biodiversity variation (e.g. Sumegi andKrolopp, 2002), potentially accounting for the variation notedfrom previous research into Quaternary loess profiles.This study presents the results of the first detailed multi-proxy

and chronometric investigation of a loess–palaeosol sequencefrom this region: the Serbian part of the Banat region in thesouth-east of the Carpathian Basin. The environmental con-ditions and dust depositional record at the site are comparedwith previously investigated loess sequences elsewhere in theVojvodina region to gauge variability in climate and loess-dustaccumulation and preservation across the Carpathian Basin.

Geomorphological setting and methods

The Tami�s loess plateau is the smallest loess plateau in theVojvodina region, extending between the settlements of E�cka,Boto�s, Orlovat and Farka�zdin, as a slightly elevated geomor-phological unit between the floodplain of the Tami�s River (onthe NE–ESE), the palaeo channel Petra (west) and the palaeochannel Sozov (north). These palaeochannels are relicts ofancient fluvial activity of, most probably, the palaeo TisaRiver (Figs 1 and 2). Hydromorphometric parameters of thePetra channel and recent Tisa meanders support this assump-tion and it is plausible that the Begej or even Tami�s riversused this riverbed after the Tisa had shifted westwards (Popovet al., 2008, 2012a, 2012b). Thus, the current distribution ofthe Tami�s loess plateau is a relic of a previously much largerloess belt reduced in extent by intensive fluvial erosion.The investigated loess–palaeosol sequence is exposed in a

brickyard at the village of Orlovat (45˚150N, 20˚350E, 88m a.s.l; 24 km SE of the city of Zrenjanin), in the central part of theTami�s loess plateau in contact with the Tami�s river valley(Fig. 1). Recent and palaeorelief conditions are very importantto consider in interpreting this site. Figure 2 shows atopographic profile from the Orlovat brickyard, over the Tami�sloess plateau to the Tami�s River alluvial plain. To illustrate thepalaeorelief conditions we used spatial data about the extentof the V-S1 palaeosol obtained at other existing exposures.

During April and May 2012, the profile near Orlovat wascarefully cleaned and sampled for rock magnetic propertiesand sediment colour proxies as well for grain size andgeochemical analyses. About 500 g sample material wascollected for magnetic analysis in plastic bags at 5-cmintervals. Additionally, eight samples were collected forluminescence dating. Here we report the field observations(litho- and pedostratigraphy), magnetic measurements and theresults from absolute luminescence chronology.

Litho- and pedostratigraphy

The profile was cleaned and described in detail on a 10-m-high vertical loess cliff. Sediment colour was determined ondried samples in the laboratory, using the Munsell Soil ColourChart. Based on investigations at various loess exposures inVojvodina, Markovic et al. (2008) developed a stratigraphiclabelling scheme following the Chinese loess stratigraphicmodel (Kukla, 1987; Kukla and An, 1989). The loess andpalaeosol stratigraphic units were designated as L and S andwere numbered in order of increasing age. The prefix ‘V’ isused to refer to the Pleistocene loess–palaeosol stratigraphy inVojvodina (Markovic et al., 2012). This scheme is applied tothe Orlovat section for ease of comparison.

Enviromagnetic properties

Environmental magnetic analyses were carried out on bulksamples. The dried sediment was packed into plastic boxes,and subsequently compressed and fixed with cotton wool toprevent movement of sediment particles during measurement.The individual density of the specimens served to normalizethe results. The initial low field susceptibility [x (10�8m3

kg�1)] was measured in an AC-field of 300 A m�1 at 920Hzusing the KLY-3-Spinner-Kappa-Bridge (AGICO, Brno, CzechRepublic). The frequency dependence of susceptibility (xfd,%) was determined with a MAGNON Susceptibility Bridge(MAGNON, Dassel, Germany) at AC-fields of 300 A m�1 at0.3 and 3 kHz at the Palaeomagnetic Laboratory of the Chairof Geomorphology, University of Bayreuth.

Luminescence dating

Sampling and sample preparation

The eight samples for luminescence dating were collected byhammering opaque PVC or stainless steel tubes into the

Figure 2. Topographic profile A–A0 (Fig. 1) from the investigated Orlovat section to the Tami�s river. This figure is available in colour online atwileyonlinelibrary.com.

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THE ORLOVAT LOESS–PALAEOSOL SEQUENCE, NORTHERN SERBIA 191

freshly cleaned loess profiles. Sample preparation wasperformed under low-intensity red light conditions in theluminescence laboratory of Babes-Bolyai University, ClujNa-poca, Romania. Three days of HCl (concentration 10%)treatment was employed for removal of carbonated materialfollowed by another 3 days of H2O2 (30%) treatment fororganic matter removal. The 63–90-mm fraction was separat-ed through wet sieving. A two-step density separation usingheavy liquids and centrifuging was performed to isolatequartz from other minerals. The heavy liquid solutioncontained sodium metatungstate, Na6[H2W12O40].xH2O, anddistilled water. First, the quartz (density 2.65–2.66–g cm�3)and plagioclase grains were separated in a –2.63 g cm�3

heavy liquid solution from the lighter minerals, such aspotassium and sodium feldspars. The second step employed a–2.75-g cm�3 heavy liquid solution, in which the quartz andplagioclase feldspars were isolated from the heavy minerals,such as zircons and apatite. Quartz grains were isolated fromthis fraction through an HF acid (40% concentration) treat-ment for 40min. The etching also removed the outer surfaceof the quartz grains, reducing to negligible the internalionizing alpha radiation contribution to the grains. Precipitat-ed fluorides after the HF treatment were removed via a 60-min HCl (10%) immersion.

Instrumentation

Quartz grains were mounted as large (8mm) aliquots in amonolayer using silicone oil on a 10-mm-diameter stainlesssteel disc. Luminescence investigations were carried out usingan automated TL/OSL-DA-20 Risø reader equipped with blue(470� 30nm) light-emitting diodes. Stimulation with infrared(IR) light was through IR light-emitting diodes (875� 80nm).All luminescence emissions were detected through a 7.5-mm-thick Hoya U-340 UV filter. Further details regarding theequipment can be found in Thomsen et al. (2008). Theradioactive 90Sr-Y beta source was calibrated using gamma-irradiated calibration quartz supplied by Risø NationalLaboratory and had a dose rate to sandy grains (63–90mm)on stainless steel discs of 0.15 Gy s�1. The heating rate was5 ˚C s�1. All thermal treatments and stimulations at temper-atures higher than 200 ˚C were carried out in a nitrogenatmosphere.The specific activities of radionuclides of interest for dose

rate determination were obtained through high-resolutiongamma spectrometry using an ORTEC hyperpure germaniumdetector having the following characteristics: active volumeof 181 cm3, 0.878 keV FWHM at 5.9 keV, 1.92 keV FWHMand 34.2% relative efficiency at 1332.5 keV, calibrated inefficiency using International Atomic Energy Agencystandards.

Measurement protocol

The luminescence characteristics of the samples were investi-gated using a single-aliquot regenerative-dose (SAR) protocol(Murray and Wintle, 2000). Stimulation with the blue light-emitting diodes was for 40 s at 125˚C. The initial 0.30 s of thedecay curve was used, less a background evaluated from theinterval 2.31–3.08 s. A constant test dose of 15 Gy was usedin all experiments. Unless stated otherwise, a preheat of 10 sat 220 ˚C preceded the measurement of natural and regenera-tive signals. A cutheat to 180 ˚C (ramp heating held for 0 s atmaximum temperature) preceded the stimulation of each testdose signal. Following measurement of each test dose signal,a high-temperature bleach was performed by stimulating withthe blue light-emitting diodes for 40 s at 280 ˚C (Murray andWintle, 2003). To define the sensitivity to infrared stimulation

and possible feldspar contamination, the IR depletion ratiowas employed. This represents the ratio of two repeated dosemeasurements, the second one having an IR stimulationbefore the (blue) optically stimulated luminescence (OSL).The sensitivity to IR stimulation was defined as significant ifthe IR depletion ratio deviated by more than 10% from unity,with aliquots not satisfying this criterion being rejected(Duller, 2003).

Results

Litho- and pedo-stratigraphy

The stratigraphic framework of loess in the Vojvodina regionis generally relatively simple (Markovic et al., 2008) becausethe sequences were formed from relatively continuous depo-sition of aeolian dust on near-horizontal platforms similar tothe Chinese loess plateau (e.g. Liu, 1985; Kukla, 1987; Kuklaand An, 1989). Here we test whether this is also the case atthe Orlovat site in the south-east of the basin and present thefirst chronostratigraphic model for loess in this area.The profile has a total thickness of approximately 10m.

The loess unit V-L2 is exposed for only about 100 cm at thebase of profile. The lower part of this loess unit has not beenexcavated during previous raw material exploitation. The unitdisplays light yellowish brown (10YR 6/4) sediment scatteredwith many root channels and carbonate concretions. Thethickness of the overlying strongly developed soil complex V-S1 is approximately 400 cm. A major change in sedimentolo-gy occurs at the pedocomplex V-S1 boundaries, with loesslayers V-L1 above and V-L2 below it. The basal part ofpedocomplex V-S1 is a strongly developed olive brown (2.5Y4/3) blocky AB horizon that gradually transforms from lightolive brown (2.5Y 5/4 and 5/6) to three Ah granular horizons.The uppermost part of the pedocomplex includes a lightyellowish brown loessic layer, a granular Ah3 horizon and aweakly developed initial A horizon at the top (Fig. 3).In contrast to other loess sections in the Vojvodina region,

a weakly developed palaeosol complex V-L1S1 is notdetected at Orlovat. V-L1S1 normally corresponds to MarineIsotope Stage (MIS) 3 (Stevens et al., 2011). At Orlovat, onlyan undifferentiated V-L1 is represented, reaching 405 cmthickness. It is a typical porous loess (10YR 6/3) with oneinitial pedogenetic horizon in the middle and two similarweakly developed palaeosols below the modern soil V-S0.The Holocene soil S0 spans the upper 75 cm of the sectionwith an upper steppic Ah horizon and a lower transitional AChorizon with small soft spherical carbonate concretions (from1 to 2 cm in diameter). The whole of the uppermost part ofthe section is scattered with krotovinas (Fig. 3).

Enviromagnetic record

Mass-specific magnetic susceptibility (x) variations are gener-ally similar to those seen in previously investigated loess–palaeosol sequences along the Danube River, at the easternand northern shores of the Black Sea, and in Central Asia andChina (e.g. Heller and Evans, 1995; Evans and Heller, 2001;Buggle et al., 2009; Markovic et al., 2009). The absolute xvalues vary between 19 and 96� 10�8 m3 kg�1. These valuesare similar to previously measured low field magneticsusceptibility records from other loess sites in the Vojvodinaregion (Fuchs et al., 2008; Markovic et al., 2008, 2011, 2012;Bokhorst et al., 2009; Stevens et al., 2011). The two majorsoil complexes V-S1 and V-S0 have significantly higher xvalues (from 35 to 60� 10�8 m3 kg�1, and from 55 to96�10�8 m3 kg�1, respectively) than the loess unit V-L1(small amplitude of variations around 20–�10�8 m3 kg�1).

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192 JOURNAL OF QUATERNARY SCIENCE

However, contrary to the typical pattern of the magneticsignal recorded at other previously investigated sections inVojvodina, the typically gentle increase of x values related tothe pedocomplex V-L1S1 is not observed at Orlovat (Fig. 3).The frequency-dependent susceptibility (xfd) varies from

approximately 0.2 to 10% with significantly higher values inpedocomplex V-S1 and peaks in the recent soil V-S0, ascompared with loess unit V-L1. Values of xfd graduallydecrease upwards in pedocomplex V-S1 from almost 9 to2%. In loess unit V-L1, xfd values range from 0.23 to 8.86%with a clearly gradually increasing trend. Modern soil V-S0has high values of xfd from 8.73 to 9.71% (Fig. 3) and, again,there is no sign of V-L1S1 in the xfd record.

Luminescence dating

Luminescence characteristics

Figure 4(a) presents a typical dose–response curve for thesample. The growth of the signal with dose passes very closeto the origin (i.e. recuperation is negligible) and the correc-tion for sensitivity change is apparently properly performed(recycling ratio is close to unity). The OSL signals exhibit arapid decay during optical stimulation and the natural andregenerated signals have the same shape and appear indistin-guishable (Fig. 4a, inset). The parameters indicating thesuitability of the measurement protocol for all the samplesanalysed are also presented in Table 1.For high doses (Fig. 4b), the growth of the signal with dose

is best represented by the sum of two single saturatingexponential functions of the form:

IðDÞ ¼ I0 þ Að1� expð�D=D01ÞÞ þ Bð1� expð�D=D02ÞÞ

This has been as reported by other recent studies on quartz(Lowick et al., 2010; Chapot et al., 2012; Timar-Gabor et al.,2012). It can also be seen that the artificial dose–response isnot dependent on sample age (Fig. 4b) and there is very littlescatter between aliquots and samples. The average character-istic doses (D01 and D02) of 33 and 300 Gy have beenobtained on 20 aliquots of samples ORL1, ORL2, ORL3 andORL4, for which dose–response curves have been con-structed for doses up to 1000 Gy.Contamination with a thermally less stable slow compo-

nent is unlikely to be significant considering the backgroundsubtraction and the shape of the decay curves. However, wehave performed a preheat plateau test to test this further. Thepreheat plateau is specifically intended to isolate a thermallystable signal; we observed a lack of dependence of theequivalent dose on preheat temperature (Fig. 5). Thus, it canbe concluded that: (i) the dosimetric signal investigatedcomes from traps that are thermally stable; (ii) any unwantedthermal transfer is not significant; and (iii) sensitivity changesare properly corrected for (as different thermal treatmentsmay lead to a different degree of sensitivity change).The applicability of the SAR protocol to date the fine sand-

sized (63–90mm) quartz grains was also tested through adose–recovery test. Natural aliquots were bleached twice for250 s at room temperature using blue light-emitting diodes;the two bleaching treatments were separated by a 10-kspause. Aliquots were then given a known dose chosen to beapproximately equal to the estimated equivalent dose, andmeasured using the SAR protocol. The results are shown inFig. 6. The given dose can be recovered reasonably accurate-ly over the entire dose range (i.e. from �30 to �350 Gy). Theresults from the dose–recovery test indicate that the SAR

Figure 3. Sediment colour, x and xfd records related to pedostratigraphy of the Orovat loess–palaeosol sequence. Ages shown next to the sequencerepresent the results of luminescence dating. This figure is available in colour online at wileyonlinelibrary.com.

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THE ORLOVAT LOESS–PALAEOSOL SEQUENCE, NORTHERN SERBIA 193

protocol is able to measure laboratory doses given before anyheat treatment both accurately and reasonably precisely.

Luminescence ages

Table 1 summarizes the information relevant to the agecalculation. Dose rates were calculated from radionuclideactivities using the conversion factors tabulated by Adamiecand Aitken (1998). A factor of 0.94 (� 5% relative uncertain-ty) was adopted to correct the external beta dose rates for theeffects of attenuation and etching (Mejdahl, 1979) and aninternal dose rate of 0.010� 0.002 Gy ka�1 was assumed forthe coarser fraction, based on the recommendation ofVandenberghe et al. (2008). The dose rate contribution fromcosmic rays was calculated based on the formula given byPrescott and Hutton (1994). The as-found moisture contentwas used for samples collected from and beneath the palae-osol horizon. For samples collected from L1, the measuredmoisture content ranged between 6 and 12%, and an averagemoisture content of 10% with an assumed relative error of25% was used in calculations. Uncertainties on the ageswere calculated following the error assessment system formal-ized by Aitken and Alldred (1972) and Aitken (1976). It can T

able

1.

Summaryofeq

uivalen

tdoses(D

e),recyclingratios,recu

perationvalues,IR

dep

letionratios,calculateddose

rates,opticalages,an

drandom

(sr)an

dsystem

atic

(ss)uncertainties.Theuncertainties

inthe

luminescence

anddosimetry

dataarerandom;theuncertainties

quotedwiththeopticalages

aretheoveralluncertainty.Alluncertainties

represent1s.Thenumber

ofreplicate

Demeasuremen

tsis

givenin

paren

theses.Thetotaldose

rate

includes

theco

ntributionfrom

cosm

icrays,an

dallowan

cewas

mad

efortheeffect

ofmoisture.

Lab.

code

Dep

th(cm)

De(G

y)Recycling

ratio

IRdep

letion

ratio

Recuperation

(%)

226Ra

(Bqkg

�1)

232Th

(Bqkg

�1)

40K

(Bqkg

�1)

Water

content

(%)

Dose

rate

(Gyka

�1)

Age

(ka)

Relative

random

errorsr(%

)

Relative

system

atic

errorss(%

)

ORL1

965

347�38

(8/12)

0.91�0.01

0.93�0.01

0.19�0.03

32.4�0.9

35.6�0.3

406�4

20

2.18�0.02

159�23

11

9.2

ORL2

700

229�24

(5/8)

0.90�0.01

0.91�0.01

0.20�0.08

31.9�0.6

38.6�0.4

456�7

15

2.49�0.02

92�12

10.5

7.9

ORL3

600

225�13

(10/16)

0.94�0.01

0.94�0.01

0.09�0.02

37.0�0.6

38.2�0.3

471�7

10

2.76�0.02

81�8

5.8

7.9

ORL4

500

181�10

(11/16)

0.94�0.01

0.94�0.01

0.15�0.06

32.1�0.4

36.0�0.4

444�7

10

2.57�0.02

70�6

5.6

6.7

ORL5

400

180�10

(10/14)

0.96�0.01

0.96�0.01

0.05�0.02

34.4�0.4

37.1�0.3

462�6

10

2.70�0.02

67�6

5.6

6.7

ORL6

300

133�7

(13/13)

0.96�0.01

0.95�0.01

0.07�0.01

37.4�0.5

42.6�0.3

546�7

10

3.10�0.02

43�4

5.3

6.7

ORL7

180

36.3�1.8

(13/13)

0.96�0.01

0.97�0.01

0.09�0.01

35.7�0.6

34.9�0.4

481�7

10

2.78�0.02

13�1

5.0

6.6

ORL8

150

28.8�1.1

(13/13)

0.95�0.01

0.97�0.01

0.11�0.01

34.8�0.7

35.7�0.2

476�6

10

2.77�0.02

10�1

3.9

6.6

Figure 4. (A) Representative SAR growth curve for a single,representative aliquot of quartz extracted from sample ORL6.Recycling and IR depletion ratio points are shown as open triangles.The recuperation point is represented as an open square, and thenatural signal is depicted as a star. The inset shows the natural and aregenerated OSL decay curve. (B) Comparison of average SAR–OSLgrowth curves for four samples of different ages; the number ofaliquots (n) used to obtain the average is specified in the legend. Theaverage dose response fitting function for all aliquots is given. Thisfigure is available in colour online at wileyonlinelibrary.com.

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194 JOURNAL OF QUATERNARY SCIENCE

be seen that the systematic uncertainties are usually largerthan the random uncertainties. Random uncertainties increasewith the age of the sample (from �4% for ORL8 to �11%relative error for samples ORL1 and ORL2) and mainly reflectthe scatter in the obtained equivalent doses. This scatter canbe attributed to the shape of the growth curve in the regionwhere the natural signals are interpolated. Nevertheless, thisis not unusual, as other recent studies also report significantscatter for equivalent doses obtained using coarse quartzextracted from loess (Lomax et al., 2013).

Discussion

Figure 7 compares the stratigraphy and luminescence chro-nology of four loess sections in the Vojvodina region:Crvenka (Stevens et al., 2011), Surduk (Fuchs et al., 2008),Stari Slankamen (Schmidt et al., 2010) and Orlovat. Accord-ing to proposed multi-millennial chronostratigraphy for Serbi-an loess sections (Martinson et al., 1987; vanKreveld et al.,

2000; Thompson and Goldstein, 2006; Markovic et al., 2008,2012) the V-S0 unit should correspond with MIS 1 (approxi-mately 0–12 ka), V-L1L1 covers MIS 2 (12–25 ka), V-L1S1 isrelated to MIS 3 (25–56 ka), V-L1L2 is an equivalent of MIS 4(56–80 ka), V-S1 covers MIS 5 (80–130 ka) and V-L2 shouldrepresent MIS 6 (>130 ka). However, the results presentedindicate only very general agreement between the lumines-cence dating and the expected ages based on a correlation tothe MIS stratigraphy-based age model (Martinson et al., 1987;Markovic et al., 2008). While the models broadly match toabout 40 ka, below this (i.e. lower part of V-L1S1, V-L1L2, V-S1 and V-L2) all the luminescence ages are younger thanthose expected from MIS stratigraphy.However, some sedimentological properties of the Orlovat

loess–palaeosol sequence demonstrate several important dif-ferences when compared with other previously investigatedloess sites in the Vojvodina region (e.g. Markovic et al., 2008,2009, 2011; Antoine et al., 2009; Bokhorst et al., 2009;

Figure 6. Summary of dose recovery data for all samples using apreheat of 10 s at 220 ˚C. The given dose was chosen to approximatethe equivalent dose. The solid line (eye guide) represents the 1: 1relation; the dotted lines (eye guide) bracket a 10% deviation fromunity.

Figure 7. Comparison between luminescence chronologies ofCrvenka (Stevens et al., 2011), Surduk (Fuchs et al., 2008), StariSlankamen (Schmidt et al., 2010) and Orlovat loess sections and MISchronostratigraphy (Martinson et al., 1987; vanKreveld et al., 2000;Thompson and Goldstein, 2006). This figure is available in colouronline at wileyonlinelibrary.com.

Figure 5. Preheat plateau test for sample ORL6. For all investigatedpreheat treatments the cutheat was fixed to 180 ˚C. With theexception of the 220 ˚C treatment (13 aliquots), for each temperaturefour aliquots were used and the data plotted present the averagevalue.

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Stevens et al., 2011). The most important include the lack ofthe Middle Pleniglacial pedocomplex V-L1S1, and the unusu-ally thick pedocomplex V-S1 (405 cm), apparently character-ized by higher accumulation rates during the final part of MIS5 and MIS 4 based on luminescence dates, magneticproperties, and litho- and pedo-stratigraphic features. There isalso evidence of at least two phases of initial pedogenesisduring the Early Holocene and for a relatively late start of theformation of the strongly developed chernozem V-S0, asindicated by the luminescence dating. We suggest that thereason for this is related to the site’s palaeogeomorphologicalconditions. Almost all previously investigated loess sectionsin the region are associated with plateau-like dust deposition,characterized by stable and quasi-continuous accumulationand sediment preservation, at least over multi-millennialtimescales (e.g. Markovic et al., 2012). The lower part of theOrlovat loess–palaeosol sequence indicates sedimentary con-ditions characterized by the influence of occasional slopeprocesses at the southern limit of the Tami�s loess plateau.Figure 2 shows that reconstruction of the palaeotopographicsurface at the base of pedocomplex V-S1 at Orlovat wasabout 4m lower than at approximately 1-km distant expo-sures on the Tami�s River bank. However, at the end offormation of V-S1 this difference in relative altitude wasreduced to 2.5m, indicating a significantly thicker lastinterglacial–early glacial palaeosol at Orlovat, probably dueto basin infilling and slope deposition. This observation isclearly supported by luminescence ages of samples ORL2(92.0�12.0 ka) and ORL3 (81.0� 8.0 ka), confirming highdeposition rates during the latest part of MIS 5 (0.09mm a�1)despite intense soil formation.The middle Pleniglacial interval is represented in the

Vojvodina region by a weakly developed soil complex L1S1,which appears either as a single, complete pedohorizon(Ruma site), or as double (Batajnica, Irig, Mi�seluk, Susek and

Petrovaradin) or multiple (Stari Slankamen, Titel and Crvenka)palaeosols (Markovic et al., 2008). Loess sub-layers intercalat-ed into V-L1S1 have preserved evidence of sudden changesin climatic and environmental conditions. In contrast to otherEuropean Late Pleistocene loess records (Vandenberghe et al.,1998; Antoine et al., 2001; Rousseau et al., 2001; Schatzet al., 2011), the middle Pleniglacial palaeosol V-L1S1 isweakly developed in the Vojvodina region.At the Orlovat loess section, evidence for this middle

Pleniglacial pedogenesis is not observed at all. In contrast toother sections in the Vojvodina region (Markovic et al., 2005,2006, 2007, 2009, 2011; Fuchs et al., 2008; Bokhorst et al.,2009; Stevens et al., 2011), the Orlovat sequence does notindicate a typical pattern of gently increased x valuesassociated with the appearance of the V-L1S1 pedocomplex.xfd, which is an even more sensitive indicator of pedogeneticintensity, also indicates just two main periods of pedogenesisin the sequence, related to interglacial pedocomplexes V-S1and V-S0, without any significant pedogenetic overprint onthe loess V-L1 unit. Figure 8 shows a comparison between xfdrecords of the Orlovat, Ruma and Mo�sorin sections in theVojvodina region (Fig. 1). Arrows represent the generalizedxfd trends. Dashed arrows indicate intervals of more highlyresolved deposition at the Orlovat section. A missing sedi-mentary interval at Orlovat is indicated by a lack of a typicalpattern of xfd records seen in Carpathian Basin loess that isrelated to slightly higher values associated with the appear-ance of the V-L1S1 complex, as observed in both the Rumaand the Batajnica sites further west. This interval is indicatedwith a ‘?’ in Fig. 8. This anomaly in the Orlovat environmen-tal magnetic record indicates a potential depositional hiatusbetween approximately 2.5 and 2m depth in the Orlovatprofile. It is partly supported by the luminescence dates. Aftera relatively smooth decrease in luminescence age from thetop of palaeosol V-S1 (ORL2, 92� 12 ka) to the middle part

Figure 8. Correlations between Mo�sorin,Orlovat and Ruma xfd records. Potentialdepositional hiatuses are indicated with a ‘?’.This figure is available in colour online atwileyonlinelibrary.com.

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of the last glacial loess unit V-L1 (ORL5, 67� 6 ka) achronological shift occurs below and above sample ORL6(43� 4 ka) over the interval between 4 and 3m depth,indicating a significant reduction in accumulation rates, orthe likely occurrence of a hiatus in sedimentation. To identifymore precisely these depositional gaps we plan to applymore detailed sampling for luminescence dating, similar tothat presented in the recent studies of Stevens et al. (2006,2007, 2008) on the Chinese Loess Plateau. Thus, twoindependent lines of evidence, the magnetic record andluminescence chronology, confirm a discontinuity in deposi-tion as suggested by an incomplete stratigraphy whencompared with sections further west. However, on the basisof the existing results it is very difficult to indicate preciselythe age of the hiatuses in the Orlovat loess–palaeosolsequence, especially given the large variability in the sedi-mentological and pedological characteristics of pedocomplexV-L1S1 in the region.These sedimentary gaps can also be linked to a reduction

in the Tami�s loess plateau surface area by intensive fluvialerosion. Dry valleys on the Tami�s loess plateau, and formerriver beds and large palaeomeanders indicated from thefluvial terraces near the investigated section at Orlovat arerelicts of ancient fluvial activity (Fig. 1). For example, Popovet al. (2012b) reported quite intensive fluvial activity at thenearby sequence at Mu�zlja sand pit (Tisa River valley) duringthe final period of terrace formation between 15 and 18 ka.Finally, the two uppermost luminescence dates clearly

demonstrate an Early Holocene age almost 0.7m below theHolocene soil V-S0. This raises important questions regardingthe onset of soil formation and the cessation of loessdeposition in the region: When do soil-forming conditionsregain dominance in the region during the Holocene? Whatdoes this imply for the timing of glacial–interglacial transi-tions in the region? According to the results presented here,the beginning of chernozem formation should be youngerthan the most recent estimated age (ORL8, 10.1� 0.8 ka),implying that loess deposition continued well into theHolocene and that chernozem soil-forming conditions didnot fully take hold until later in the Early Holocene. Thisinterpretation is supported by very young IRSL ages (7.6� 0.5ka) from the lower part of modern soil V-S0 at Stari Slanka-men (Schmidt et al., 2010) and ages of 10.0�1.1 ka from thelast glacial loess V-L1 at 1.6m below the lower boundary ofthe modern soil in the Rogulic gully on the Titel loess plateau(Bokhorst et al., 2011). It is also supported by a very young14C age (7.3� 0.38 cal ka BP) for the uppermost part of thelast glacial loess V-L1 at Surduk (Hatte et al., 2013).However, at Crvenka, quartz OSL dates from the Holocenesoil and the boundary with last glacial loess unit V-L1 suggestthat soil formation began at the onset of the Holocene(Stevens et al., 2011). It may be likely that many terrestrialrecords are characterized by a similar lag between Holoceneglobal climate shifts and local or even regional environmentalresponses. For example, Lehmkuhl et al. (2103) have alsoreported an absence of soil formation during the EarlyHolocene at the Suohuduo loess–palaeosol located on theeastern margin of the Tibetan Plateau.Although variable between sites, based on the dates

presented here, previous statements that the boundary be-tween the Holocene soil and last glacial loess below itrepresents the exact time of the boundary between theHolocene and Late Pleistocene in globally integrated recordssuch as global ice volume (e.g. Antoine et al., 2001;Rousseau et al., 2001; Markovic et al., 2005) may beproblematic. The precise timing of Termination 1 does notnecessarily occur coevally between loess and palaeosol units

as compared with marine oxygen-isotope stratigraphic tran-sitions. This has major implications for understanding theterrestrial response to global climate changes. It implies asignificant lag between ice volume or insolation forcing andenvironmental response on land, perhaps via delayed land-scape stabilization or onset of more humid conditions.Potentially, sediment availability remained high during theearliest Holocene, leading to high dust accumulation ratesand retarded soil formation. This may have been accentuatedthrough Alpine glacial meltwater transport of material.Alternatively, atmospheric circulation did not change suffi-ciently to allow more humid conditions to prevail over thebasin until later in the Holocene. Such delayed onset of fullHolocene humid westerly flow is seen in arid zone recordsfurther east in Central Asia (Chen et al., 2008). High sample-resolution OSL dating has also shown this kind of asynchro-nous regional response on the Chinese Loess Plateau and itmay be a feature of a large number of continental settingswhere the interaction of multiple atmospheric systems pre-cludes linear responses to global climate forcing (Stevenset al., 2008). Regardless, these results call into question manybasic assumptions underpinning the correlation of recordsworldwide and imply that the terrestrial environment in thelarge Eurasian loess belt shows complex responses to chang-ing boundary conditions. More focused studies on theHolocene–Pleistocene boundary are needed to fully considerthe timing of the transition to full interglacial conditions inthis region as most of the studies showing this discrepancyhave not dated the boundary at sufficiently high resolution.This is especially important because the dominant modes ofair circulation are associated with different geographicallatitudes which do not experience completely synchronousinsolation forcing during the summer (e.g. Ruddiman, 2008).If a major global climatic shift such as Termination 1 does

not dictate a uniform response of the terrestrial ecosystem, itis hard to imagine that climatic fluctuations of smallermagnitude would be characterized by worldwide synchronic-ity in environmental change. This situation may be typical forthe investigated region, which was drier than ‘classical’European loess provinces (Markovic et al., 2007, 2008;Bokhorst et al., 2009, 2011; Stevens et al., 2011; Hatte et al.,2013; Zech et al., 2013) where environmental responses tothe last glacial climate variations have been close to thethreshold between loess deposition and the initiation ofpedogenesis. This explains why it is hard to distinguishdifferences between loess and initial pedogenetic layers inthese sections and why over short distances the samestratigraphic subunits have quite different expressions.

Conclusions

Multi-proxy investigations of the loess–palaeosol sequence atOrlovat demonstrate the importance of this site as a record ofLate Pleistocene palaeoclimate and palaeoenvironment inSerbia. The Orlovat section provides an opportunity toreconstruct local and regional environmental and climaticconditions during the Late Pleistocene in a poorly studiedregion of the Carpathian Basin.Due to the slope depositional conditions at Orlovat, the

preserved loess–palaeosol sequence also reveals a pattern ofsedimentation that contrasts with other previously investigat-ed northern Serbian loess sections, characterized by plateau-like deposition. Correlation with environmental magneticrecords from other key loess sites in the Vojvodina regionconfirms the absence of at least parts of pedocomplex V-L1S1. This is also supported by independent evidence fromthe luminescence chronology. Contrary to many previous

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interpretations, the presented chronological results indicatethe absence of significant pedogenesis during the earliest partof the Holocene in the Vojvodina region. Thus, the formationof the modern soil (V-S0) started with a delay of severalthousands of years in comparison with previous expectationsderived from analysis of globally integrated records. Thisinterpretation raises an important question mark over thevalidity of generalized direct stratigraphic correlations be-tween European loess records and global marine records andsuggests a more complex response of loess terrestrial systemsto global forcing. Finally, this study again confirms theimportance of the simultaneous application of detailed expo-sure description, multi-proxy approaches and a detailedindependently derived chronology for accurate temporal andspatial reconstruction of the evolution of environmental anddepositional changes in complex terrestrial environments(2007, 2008; Vandenberghe, 2012; Vandenberghe et al.,2014) and that inadequate one-dimensional investigationscan suggest misleading associations between global andregional processes.

Acknowledgements. This research was financially supported byProject 176020 of the Serbian Ministry of Education and Science, aswell as a grant (114-451-2262/2011) of the Provincial Secretariat forscience and technological development of the Vojvodina Govern-ment, A.T-G. acknowledges the financial support from a grant of theRomanian National Authority for Scientific Research (CNCS-UEFISC-DI, PN-II-RU-TE-2011-3-0062, no. 73/05.10.2011). F.L. wishes tothank the German Research Foundation (Deutsche Forschungsge-meinschaft, DFG) for funding in the frame of the CollaborativeResearch Center ‘Our way to Europe’ (CRC 806).

Abbreviations. SAR, single-aliquot regenerative-dose; IR, infrared;OSL, optically stimulated luminescence; MIS, Marine Isotope Stage.

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