Naturwissenschaften 76, 416- 418 (1989) 9 Springer-Verlag 1989

Thermoluminescence Dating of Archaeological Sediments

S. Chawla and A. K. Singhvi Physical Research Laboratory, Navrangpura, Ahmedabad 380 009, India

It is now being increasingly realized that an analysis of habitational deposits as archaeological analogues of geological sediments can provide useful information on the contemporary environment(s), stratigraphy and the cultural assemblages. In recent years, terms such as "anthropogenic sediments", "anthropic-soils" and "archaeo-sediments" have been coined to designate habitational deposits [ 1 - 3]. Extending the broad similarity, in respect of in situ disturbance and mixing of archaeological sediments with the soil horizons having faunal pedoturbation, it was considered that a direct dating of these deposits via recently developed thermoluminescence dating of sediments [ 4 - 7 ] should be possible. Akin to the process of pedoturbation, human activity causes a significant churning and repeated mixing up of the habitational deposit. As a result, portions of the deposits are brought to the surface and exposed to solar illumination, with a consequent resetting of the thermoluminescence clock of the constituent minerals. In this contribution, results of a successful feasibility study on thermoluminescence dating of habitational deposits from four archaeological sites in India are reported. The results unambiguously suggest that this approach can provide useful chronological data especially in situations where a radiocarbon assay and/or conventional thermoluminescence dating of burnt materials is not possible. This study, when perfected, would thus provide a new dating possibility for archaeological deposits. 416

Thermoluminescence (TL) dating of sediments is based on the notion of predepositional optical bleaching of the geologically acquired TL signal in natural minerals (e. g., quartz, feldspars) to a small residual value D(Io). Subsequent burial results in a reinitiation of TL which continues unabated till excavation. The measured signal D(Inat) comprises D(Io) and D(Id). D(Io) is the TL acquired since burial and thus reflects the age of the deposit. In the case of habitational deposits the basic premise of on-site solar illumination and consequent optical bleaching of TL appeared plausible in view of the following facts: 1) The human occupational surface was always exposed to solar illumination. 2) The human activity caused repeated mixing and churning of the deposited material. 3) The fact that an archaeological de4 posit of few meters typically spans few centuries.
.

dating were followed for the present samples [8, 9]. The samples were analyzed using the fine-grain method [10]. After a pretreatment of samples with 1N HCI (to remove carbonates if any), H202 (to remove organics) and 0.01N Na-oxalate (to deflocculate), the 4 - 11 #m size grains were separated using known Stokes settling times in acetone. Zero-glow monitoring was often used for normalization between glow curves [11]. The glow curves were recorded using a photon-counting set up coupled to an EMI 9635QA photomultiplier tube with Corning 7 - 59 and 5 - 60 blue filters along with a Chance-Pilkington HA3 filter interposed in the optical path. The laboratory irradiations were made using a 30 mCi 9~176 betaplaque and a six-seater vacuum alpha irradiation facility. The radioactivity of the samples was assayed by a thick source alpha-counting technique and gamma-ray spectrometry (for 4~ The sediment equivalent dose was estimated using the methodology used for partially bleached sediments (i.e., the Rbeta method) [12]. To optimize simulation of solar illumination duration conditions some samples were analyzed

Thus notwithstanding the episodic nature of the deposition in archaeological situationsl a small albeit finite preburial solar exposure can be reasonably assumed. As discussed below this was found true in all samples studied here. For the present study, a selection of nine samples from four spatially distal archaeological sites in central and northwestern India (Fig. 1) were analyzed. This was done in order to remove any regional or locational bias in the analysis. The standard procedures for sediment sample collection for TL

'

5 0 0 k m

Fig. 1. Location of archaeological sites

Naturwissenschaften 76 (1989) 9 Springer-Verlag 1989

w i t h several i l l u m i n a t i o n d u r a t i o n s [13]. T a b l e 1 p r o v i d e s t h e b a s i c T L d a t a , Figs. 2 a n d 3 p r o v i d e t y p i c a l glow curves a n d t h e p l a t e a u tests a l o n g w i t h T L vs. dose, g r o w t h curves. A p e r u s a l o f t h e s e d a t a sets e n a b l e s t h e f o l l o w i n g observations: 1) T h e t o t a l T L signal [i.e., D(Jnat) ] in all t h e s a m p l e s w i t h t h e e x c e p t i o n o f TL-3 is s m a l l s u g g e s t i n g a d e f i n i t i v e solar b l e a c h i n g e v e n t . I n t h e a b s e n c e o f s u c h a n e v e n t D(Ina t) w o u l d h a v e reflected geological T L w h i c h is u s u a l l y u p to t w o o r d e r s o f m a g n i t u d e h i g h e r . The data on TL-33 can be reconciled w i t h field e v i d e n c e d i s c u s s e d b e l o w . 2) M o s t s a m p l e s e x h i b i t a r e a s o n a b l e p l a t e a u in t h e 3 0 0 - 3 6 0 ~ r a n g e . T h i s is t o b e e x p e c t e d in view o f t h e f a c t t h a t

glow c u r v e s suggest t h e T L signal t o b e q u a r t z - d o m i n a t e d a n d t h a t t h e 325 ~ glow p e a k o f q u a r t z is t h e m o s t easily photo-bleachable high-temperature glow p e a k . 3) E s t i m a t i o n o f t h e s e d i m e n t e q u i v a l e n t d o s e w i t h t w o d i f f e r e n t s o l a r illum i n a t i o n d u r a t i o n s suggests t h a t a b o u t 5 - 10 m i n s u n - l a m p e x p o s u r e ( b r o a d l y c o r r e s p o n d i n g t o a b o u t 15 - 30 m i n s u n e x p o s u r e ) is a d e q u a t e . T h i s a p p e a r s t o b e a p l a u s i b l e a s s u m p t i o n , w h i c h is also borne out by the plateau ranges. 4) T h e f a c t t h a t D(Inat) - D(Id) li.e., D(In) ] is typically 10 G y suggests t h a t t h e r e s i d u a l T L signal c o r r e s p o n d i n g t o D(Io) a b s o r b s in it t h e s u p r a l i n e a r i t y correction. Experiments on sample P R L : T L - 4 c o n f i r m e d this fact, as t h e

s u p r a l i n e a r i t y i n t e r c e p t was e s t i m a t e d t o b e 0.6 G y a t a glow c u r v e t e m p e r a t u r e o f 340 ~ F i g u r e 4, w h i c h p r o v i d e s t h e c o m p a r i s o n o f T L ages w i t h t h e a v a i l a b l e c o n trois, s h o w s t h a t a g o o d c o r r e l a t i o n f o r m o s t o f t h e s a m p l e s exists. T h e l o n e exc e p t i o n i n this is t h e s a m p l e T L - 3 3 f r o m an ochre color pottery (OCP) stratum. Sedimentological and scanning electron m i c r o s c o p e studies h a v e r e v e a l e d t h a t the OCP-bearing strata are deposited b y f l o o d [I4], a n i n f e r e n c e t h a t is c o n s i s t e n t w i t h t h e lack o f c h a r a c t e ristics o f a n o r m a l h a b i t a t i o n a l d e p o s i t . From the TL standpoint, a flood-assoc i a t e d d e p o s i t w o u l d h a v e m u c h less t i m e a v a i l a b l e f o r it t o b e solarb l e a c h e d . A s a c o n s e q u e n c e its T L

Table 1. Thermoluminescence, radioactivity data and the age estimates Site/ sample Culture Locus TL analysis Plateau region [~ Sunlamp D(Inat) D(Ia) exposure [Gy] [GYl [min] Radioactivity analysis
a

TL age Th K [ppm] [%]

Knownage

t~l/~0 U [ppm]

Dose rate* [/zGy/a] [aB.P.] 4 [aB.P.] +

Sanghol PRL:TL-4 PRL:TL-10 PRL:TL-14

LHBW

Fx-1 L-22 LHW Ex-1 L-46 PGW(?) E x - 1 L-33 SVP-1 L- 12 SVP-1 L-18

280-360 10 300-360 10 290-360 10

18 28 26

13 19 14

0.09 0.10 0.13

1.05
1.00 1.06

3.35 3.80 4.37

11.36 12.91 14.82

2.00 2.25 3.34

4550 5180 7250

2760 3660 1900

3220 3350 ll0Z(PRL-512) 4030 1760

Sringaverapura RW, PRL:TL-26 Late phase of NBPW Pre PRL : TL-34 NBPWBSW OCPW PRL : TL-33 Hulas PRL : HLS: TL-1 PRL : HLS: TL-17 Bagor PRL : TL: S-13

300- 420

27

17

0.07

n.m.

4.44

15.10

5.51

8130

2075

23003

300-400 10 5

36 105

18 81

0.13 0.09

n.m. 1.07

3.78 4.73

12.74 16.07

2.79 4.38

6210 7770

2850 10465

SVP-1 320-440 L-19E 300- 360 Xd9 Qd-1 - 2 L-7 280- 340 Xd9 Qd-1 L-7 Sand dune depth 50cm

2743 2700 1302(PRL-669) 2700 + 3003 Pre-30003 2930+_300l 2030 1501 2870 2501

Later Phase PGW LHW

5 5

28 30

14 21

0.08 0.09

1.19 1.08

3.71 5.37

12.74 18.28

2.38 3.07

4960 7110

2950 2940

Bagor ware

300- 380 Total bleach

34

24

0.12

n.m.

8.54

29.10

1,48

11720

2100

2060

PGW LHBW LHW RW

Painted grey ware Late Harappanbaraware Late Harappan ware Red ware

BSW OCPW NBPW n.m. + B.P.

Black slipped ware Ochre colour pottery ware Northern black polished ware not measured means before 1987for all the TL ages but for radiocarbon ages 1950is taken as the base year

* i 2 s 4

Water content of 20 % is assumed TL age of in situ pottery Radiocarbon age Archaeological estimate of the culture span None of the samples exhibited anomalous fading over a 2 week period 417

Naturwissenschaften 76 (1989)

9 Springer-Verlag 1989

I I I I I I Mean Acje= 2075 a "i 3 9 2 o 5L: 5 m i .

O-Dose [ G y ]
0.4

Temperature [~
Meon Age:2760a

o
_

d--

o
20 I0 I0 20
i

,
I 50 l I I
I / II

1 , 500
[ L

'

I l 400 I I

~-Dose [Gy]
I i i i I i i i PRL:TL- Z6 SRINGAVERAPURA Soil associated with Late NBP Ware

Temperature (~
I I

'ti "~
~, ~ 0.3
ca. 0"2 0-1 <

= o

ii::
30 20 I0 0 I0

/
20 30 40

"R

/
I 250 I 300 PRL:TL-4 SANGHOL Soil associated with Late HB Ware

e ,<

0-0

1 350

/ ",k

1.5

\\
k

1.5

/
/ // /

\
\ \\ \ \ \ \ \
\\\

%,

,%
.o i . 0 o [a.

N+.B ( 2 0 G y )

s i.o

[
,n
~ o.5 I

/ t I ZGM Peak /

o
~0.5

A;'
9 I00

/
~ 0.0 0

I
I00
200

...... ; i
t

300

400

500

Temperature [aC]
400

200

300

Temperature [%]

Fig. 2. Thermoluminescence glow curves for natural sample (N), natural sample bleached by sun-lamp (N+ SL) and natural sample with additional laboratory beta exposure (N+/3). Also shown are R-/~ plot (top left) and age plateau (top right) for PRL : TL-26, the mean age in the 300-420 ~ region is plotted as the plateau. This is considered as reasonable in view of the experimental error which is also indicated Fig. 3. Glow curves for natural (N), sun lamp-bleached (N+ SL) and beta-exposed (N+/~) sample. Note that TL intensity for N + SL exceeds N at glow curve temperatures beyond 380 ~ suggesting a phototransfer from deeper traps. R-/~ plots and age plateau are also shown for PRL : TL-4

thanks C S I R - l n d i a for financial assistance by way of pool officership. Received February 27 and June 8, 1989 1. Stein, J. K., Rapp, Jr., R., in: Contributions to Agean Archaeology, p. 143 (E. Wilkie, W. D. E. Coulson, eds.). Minneapolis: Kendall and Hunt 1985 2. Rapp, Jr., G.: Ann. Rev. Earth Planet. Sci. 15, 97 (1987) 3. Courty, M. A., Fedoroff, N." PACT J. 7, 257 (1982) 4. Singhvi, A. K., Wagner, G. A., in: Dating Young Sediments, p. 19 (A. J. Hurford, E. Jiger, I. A. M. Tencate, eds.). Bangkok: CCOP, UN Press 1986 5. Singhvi, A. K., Mejdahl, V.: Nucl. Tracks 10, 137 (1985) 6. Wintle, A. G., Catt, J. A.: J. Soil Sci. 36, 293 (1985) 7. Huntley, D. J., et al.: PACT J. 9, 607 (1983) 8. Aitken, M. J.: Thermoluminescence Dating. New Y o r k : Academic Press 1985 9. Singhvi, A. K., Chawla, S.: J. Arch. Chem. 4, 59 (1986) 10. Zimmerman, D. W.: Archaeometry 13, 29 (1971) 11. Aitken, M. J., Bussell, G. D.: Ancient TL 6, 13 (1979) 12. Wintle, A. G., Huntley, D. J.: Can. J. Earth Sci. 17, 348 (1980) 13. Huntley, D. J.: Phys. Chem. Miner. 12, 122 (1985) 14. Agrawal, D. P., Deshpande, M. N., Rajaguru, S. N., Roy, B.: Proc. Ind. Acad. Sci. 87, 23 (1978) 15. Huntley, D. J., et al.: Nature 313, 105 (1985) 9 Springer-Verlag 1989

clock was not reset and thus a higher

D(I d) is observed.
The foregoing discussion clearly demonstrates that a potentially new dating
5 l L I
I l I i I

9 Bagor
4 9 HuLas 9 Sanghot

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9 Sringaverapura

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+_10 % boun(~

method for archaeological chronology can be developed 9 It may be prudent here to point out that in any future application o f this approach, the behavior o f D(Id) with the duration of solar illumination should be carefully monitored to assess the correct preburial solar bleaching and consequently to avoid age overestimation linked with overbleaching. Also, pits should not be sampled. It m a y also be worth examining these samples by the optical dating method [15], which by definition probes only the optically sensitive charge traps and to a large extent obviates the risk o f overbleaching. We gratefully acknowledge the help from Prof. K. T. M. Hegde, Dr. K. N. Dikshit, Prof. V. N. Mishra, and Dr. G. B. Sharma in respect o f the sampling of the sites. W e thank Dr. B. P. Agrawal for providing us the pottery TL dates on the Hulas sequence. SC

I
3

i
4

Known age [ks]

Fig. 4. Comparison of TL ages with "known ages" 418

Naturwissenschaften 76 (1989)