Ochre resources from the Middle Stone Age sequence of Diepkloof Rock Shelter, Western Cape, South Africa

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Journal of Archaeological Science 40 (2013) 3492e3505

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Journal of Archaeological Science

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Ochre resources from the Middle Stone Age sequence of DiepkloofRock Shelter, Western Cape, South Africa

L. Dayet a,*, P.-J. Texier b,1, F. Daniel a,2, G. Porraz c,3

aCNRS, UMR 5060-IRAMAT-CRP2A, Université Bordeaux 3, 33607 Pessac, FrancebCNRS, UMR 5199-PACEA, Université de Bordeaux 1, Talence, FrancecCNRS, UMR 7041-ArScAn-AnTET, Université de Nanterre Paris X, France

a r t i c l e i n f o

Article history:Received 29 August 2012Received in revised form17 January 2013Accepted 18 January 2013

Keywords:OchreMiddle Stone AgeSouth AfricaProvenanceProcessingPigments

* Corresponding author. Tel.: þ33 (0)557121085.E-mail addresses: [email protected] (L. Day

bordeaux1.fr (P.-J. Texier), [email protected] (F. Danparis10.fr (G. Porraz).

1 Tel.: þ33 (0)540008890.2 Tel.: þ33 (0)557124551.3 Tel.: þ33 (0)146692655.

0305-4403/$ e see front matter � 2013 Elsevier Ltd.http://dx.doi.org/10.1016/j.jas.2013.01.025

a b s t r a c t

Although no paintings are associated with archaeological contexts before the end of the Middle StoneAge, hundreds of ochre pieces were discovered on numerous southern African sites suggesting a lastingtradition of ochre use. The variability and the significance of ochre exploitation remain however poorlydocumented. The MSA site of Diepkloof Rock Shelter (Western Cape Province, South Africa) offers anideal opportunity to discuss questions of ochre procurement, processing, and use over a long sequence.This study develops an original methodology based on observations on one hand, and SEM-EDS, XRD andRaman spectrometry analyses on the other hand. By comparing raw materials with our geologicaldatabase, we show that some iron-rich raw materials were collected more than 20 km from the site. Suchlong-distance procurement combined with other elements of the overall context suggests a planning ofprocurement. One main chaîne opératoire based on grinding was identified at Diepkloof. In comparisonwith other South African sites, we observed no evidence for use as loading agent in adhesives. Weconclude that ochre use may follow regional cultural patterns.

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1. Introduction

Many discoveries have highlighted how the use of red ferrugi-nous materials is ubiquitous among Pleistocene and Holocenehunteregatherer societies. Usually referred to as ‘ochre’, in the pastdecade their use has been widely associated with questions sur-rounding the emergence of cultural modernity and complex cog-nitive capacities, especially regarding recent discoveries from theMiddle Stone Age (MSA) in Southern Africa (see e.g. McBrearty andBrooks, 2000; Henshilwood et al., 2002, 2009; Watts, 2002;Barham, 2002; Wadley et al., 2004; Marean et al., 2007). Forinstance, the engraved ochre pieces showing geometric marksfound at Blombos Cave are a convincing instance of the associationof colored material and designs which may relate to symbolicmeanings more than 75 ky ago (Henshilwood et al., 2009).

et), [email protected]), [email protected]

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Sensu stricto, ochre is colored earth, composed of a mixture ofclay, quartz, and iron oxides or oxy-hydroxides, such as hematite orgoethite. The meaning of this term has been extended in archae-ology to refer to any category of rocks containing iron oxides (oroxy-hydroxides), with a reddish or yellowish streak (Henshilwoodet al., 2009; Wadley, 2010; Hodgskiss, 2010). Probable evidence ofochre use in Africa extends back more than 280 ky on someAcheulean sites (McBrearty And Brooks, 2000). The early MSA hasyielded convincing proxies of ochre use, for instance at Twin Riversin Zambia, in layers dated tomore than 200 ky (Barham, 2002) or atSai Island in Sudan, more than 182 ky ago (Van Peer et al., 2003).Ochre occurrences and evidence of its use considerably increase inthe second part of the MSA in southern Africa from about 160 ky:hundreds and sometimes thousands of pieces were found onseveral sites, encompassing different technological cultures, forexample at Pinnacle Point (Marean et al., 2007), Sibudu Cave(Wadley et al., 2004; Hodgskiss, 2010), Blombos Cave (Henshilwoodet al., 2002; Watts, 2009) and Klasies River (Wurz, 2000) (Fig. 1). Todate such ochre quantities are not observed elsewhere in the worldbefore the Later Stone Age or the Upper Paleolithic. Worked piecesare systematically reported, indicating that this material wasintentionally collected and systematically used by MSA people(Watts, 1999, 2002; Henshilwood et al., 2002; Marean et al., 2007)(Table 1). One of the most exceptional discoveries is the complete

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Table 1Description of ochre remains (worked pieces) and artifacts covered by ochre residues cited and described in the literature. Only sites where at least two types of remains wererecovered are listed.

Site Worked pieces Grindstones Ochre on HPbacked tools

References

Ground Scraped Incisionsa Geometricengravings

South AfricaBlombos Cave Present Present Present Present (at least

2 pieces)Present (upper andlower grindstones)

No HP Henshilwood et al., 2002, 2009;Watts, 2009; Henshilwood et al., 2011

Border Cave Probable Beaumont, 1978 cited in Watts (2002)Bushman Rock Shelter Probable Possible Possible Watts, 2002; Watts, 1998 cited in

d’Errico et al., 2012Die Kelders Probable Absent Probable (upper

grindstone)No HP Avery et al., 1997; Thackeray, 2000

Diepkloof Rock Shelter Present Possible Present(1 piece)

Absent Present (lowergrindstones)

Absent This paper

Hollow Rock Shelter Probable Present Possible (2 pieces) No HP Evans, 1994; Watts, 2002Klasies River Mouth Present Present Present

(1 piece)Possible Absent (?) Singer and Wymer, 1982; Wurz, 2000;

Watts, 2002Klein Kliphuis Present Present Present

(1 pieces)Possible (1 piece) Absent (?) Mackay, 2006; Mackay and Welz, 2008

Olieboompoort Probable Possible Watts, 2002Pinnacle Point

Cave 13BPresent Present Present

(3 pieces)Possible (1 piece) No HP Marean et al., 2007; Watts, 2010

Rose Cottage Probable Present Watts, 2002; Lombard, 2007Sibudu Cave Present Present Present Wadley et al., 2004; Wadley et al., 2009;

Lombard, 2007; Hodgskiss, 2010Umhlatuzana Probable Present Watts, 2002; Lombard, 2007Ysterfontein 1 Present Possible No HP Avery et al., 2008NamibiaApollo 11 Cave Present Present Possible Wendt, 1976; Watts, 2002

Present: full descriptions and/or pictures e Probable: partial descriptions e Possible: no description or questionable cases e Absent: reported as absent e Empty spaces: noreferences (but not necessarily absent).

a Including notches and engravings without any design.

Fig. 1. Locations of the main South African MSA sites were ground ochre pieces and other evidence of ochre use were found (see also Table 1).

L. Dayet et al. / Journal of Archaeological Science 40 (2013) 3492e3505 3493

L. Dayet et al. / Journal of Archaeological Science 40 (2013) 3492e35053494

tool kits from Blombos Cave, where two grinding stones, two shellfish containers and a scapula used for applying ochre have beenrecently found (Henshilwood et al., 2011). Alsoworthmentioning isthe evidence of hematite mining site from the late MSA at LionsCave (Dart and Beaumont, 1969).

Along with this increasing use of red ochre during the southernAfrican MSA, various innovations are documented. Recent sig-nificant finds reveal that MSA people produced bone tools(Henshilwoodet al., 2001; Backwell et al., 2008),manufactured shellbeads (Henshilwood et al., 2004; d’Errico et al., 2008) and engravedgeometric designs (Henshilwood et al., 2009; Texier et al., 2010).Why and how these innovations are interrelated is a central issuethat should help clarifying our understanding of the evolutionaryprocess of anatomicallymodernhumansocieties. In this context, themain issue about ochre concerns its possible uses and the role that itmight have played. Archaeological evidence in the MSA suggestspractical uses of ochre. The presence of ochre residues mixed withorganic materials on the back of Howiesons Poort segments atSibudu Cave, Umhlatuzana and Rose Cottage Cave are probably theremains of ancient adhesives for hafting tools (Wadley et al., 2004;Lombard, 2007). The same site yielded flakes with ochre residueslocated on their platforms that may be interpreted as traces left byochre lumps used as hammers (Soriano et al., 2009). On the otherhand, ochre’s use as pigment is generally assumed (see McBreartyand Brooks, 2000; Watts, 2002, 2009, 2010; Henshilwood et al.,2002, 2009; Marean et al., 2007; d’Errico et al., 2008; Rifkin, 2012).The oldest well-established traces of paintings in Africa were dis-covered at Apollo 11 Cave, Namibia, and dated at 28 000 years BP(Wendt, 1976). More recently, at the same site, red stained ostricheggshells were recovered from late MSA layers (Vogelsang et al.,2010). Before then, ochre’s use as pigment is exclusively inferredfromindirect archaeological records.Watts, for instance, argued thatbright red and deep redwere favored over other colors showing thatcolor selection was intentional (Watts, 1999, 2002, 2009; 2010).D’Errico et al. (2005) reported ochre residues on shell beads atBlombos Cave, which may be due to their rubbing against ochredskinor toadeliberate coloringof thebeads. Polishedawlswithochreresidues foundat BlombosCave couldbe interpretedasneedlesusedto pierce ochre stained skin (Henshilwood et al., 2001).

Because the frontier between ochre’s use as pigment and its usefor symbolic purposes is thin, red ochre was often assumed to havesymbolic meanings (Deacon, 1995; McBrearty and Brooks, 2000;Henshilwood et al., 2002, 2009; Marean et al., 2007; Watts, 2002,2009, 2010). Theoretical models (e.g. the female cosmetic coalitionmodel or the basic color term model) have been proposed todemonstrate the links between the color red, ochre and symbolismduring the MSA (see Knight et al., 1995; Watts, 1999, 2010). Otherauthors argued that no archaeological evidence suggests a directlink between ochre use and symbolic behaviors during the MSA(see Wadley, 2005a, 2009; Lombard, 2007). Beyond this debateabout how to interpret the occurrence of coloring materials on asite (inference from archaeological context versus predictions fromtheoretical models), there is a consensus on considering bothpractical and symbolic uses that is now well established (Wadley,2005a; Lombard, 2007; d’Errico et al., 2010; Watts, 2010;Henshilwood and Dubreuil, 2011). Indeed, the symbolic meaningspeople may attribute to ochre refer to different considerations thantechnical ones, such as aesthetic considerations. However theseconsiderations are highly dependent on the context of use, which isno longer preserved.

In this paper, we propose a detailed study of the unpublishedred ochre pieces from the MSA site of Diepkloof Rock Shelter(Western Cape Province, South Africa), focusing on the modalitiesof selection, transformation, use, and discard of ochre. The excep-tional sequence recorded at this site allows us to consider ochre

procurement and processing throughout a long period of time andacross different cultural contexts. Four main points drive this study:

1. What criteria determine the selection of ochre?2. What are the processing steps of the ochre chaîne opératoire?3. How can we interpret change versus stability in the way ochre

was processed through time?4. Are there regional differences in ochre selection, processing,

and use?

2. Methodological background

To date, studies of South African MSA ochre have been mainlybased on macroscopic examination of raw and worked pieces(Watts, 2002, 2009, 2010), observations of residues (Lombard,2007; Soriano et al., 2009), and experimentation (Wadley et al.,2004; Wadley, 2005a; Hodgskiss, 2010; Rifkin, 2012). However alack of archaeometric analyses is noticeable. Chemical analyseshave been conducted on ochre powder from Sibudu Cave (Wadley,2010; analyses done by Billing and Wilson) and Blombos Cave(Henshilwood et al., 2011), and on ochre pieces from Nelson BayCave (Bernatchez, 2008) and Klasies River (d’Errico et al., 2012).These studies are few, despite the methodological improvements oflast two decades on the chemical analyses of ochre. Numerousmethods have been successfully tested to determine the nature andthe provenance of the raw materials, such as scanning electronmicroscopy coupled with energy dispersive X-ray spectrometry(SEM-EDXS), X-ray diffraction (XRD), Raman spectrometry, X-Rayfluorescence (XRF), mass spectrometry (ICP-MS), or instrumentalneutron activation analysis (INAA) (see Hovers et al., 2003; Kiehnet al., 2007; Popelka-Filcoff et al., 2007, 2008; Salomon, 2009;d’Errico et al., 2010; Beck et al., 2011; Eiselt et al., 2011).

The lack of such studies on MSA ochre remains might be partlyexplained by the destructiveness of many of them. In this paper, wepropose to combine different approaches, based on both archaeo-logical and geologicalmaterial, onmacroscopic and non-destructivechemical analyses, in order to enhance our understanding of howochre materials were selected and processed by MSA inhabitants.

3. Material and methodology

3.1. Archaeological material

Diepkloof Rock Shelter is a large quartzitic sandstone shelteroverlooking the Verlorenvlei River about 14 km from the presentAtlantic shoreline. Ochre pieces are present throughout thesequence, from the deepest MSA stratigraphic units (SUs) to theLater Stone Age (not studied here).

The main sequence of Diepkloof Rock Shelter e about 3.10 mdepth e has been excavated over a 3 m2 restricted area. Severaltechno-complexes were identified from the base to the top of theMSA sequence: lower MSA (type Mike), pre-SB (type Lynn), Stillbay(type Larry), Howiesons Poort (subdivided into an Early, an Inter-mediate and a Late phase), a technologically distinct MSA industryinter-fingeredbetween theEarlyand the IntermediateHP (MSAtypeJack) and post-Howiesons Poort (type Claude) (Porraz et al., 2013).The ages obtained bydifferent authors are in good agreement for theupper part of the sequence but there are some discrepancies for thelower part, especially for the Late HP and SB (Jacobs et al., 2008;Tribolo et al., 2009; 2013). The SB at Diepkloof has been previouslydated by Jacobs et al. (2008) at 70.9 � 2.3 ky but the correspondingSUshave since been reassigned to theHP (EarlyHP). Older ageswereestablished by Tribolo et al. (2013) for this complex (105�10 ky and109� 10 ky) and for the SB complex just below (109� 10 ky). Theseages suggest that there is no gap between the two phases. According


to the same author, the Intermediate and Late HP were depositedbetween 85 � 9 ky and 52 � 5 ky. Ochre pieces from this area (twosquares: M6, N6), were retained to be examined, from the SU Mike(MSA typeMike) to the SU Claude (post-Howiesons Poort). A total of558 pieces were identified as ferruginousmaterial (545) or possibleferruginous material (13 pieces) (Fig. 2). Among them, 58 wereindividually plotted while the others were collected from the sieves(using a 5mmmesh) by SUs and sub-squaremeters (see Parkingtonet al., 2013). A weight of 1.9 kg is estimated for the totality of theochre pieces. Ochre residues were also observed on several lithicartifacts, mostly on quartzite slabs (Fig. 3) and on some silcreteflakes.

3.2. Geological material

Geological surveys were carried out around Diepkloof. Sources ofshale and ferricrete were identified. Our initial surveys focuseddirectly around the shelter (100 m from the shelter) and along thevalley of the Verlorenvlei River. Samples from the closest outcrops

Fig. 2. Photos of some ochre pieces. A: Nodule of ferricrete with a matte cortex, showing coxide crystals. C: Pieces of ferricrete with fibrous iron oxide crystals, entirely ground and pyconvex ground face. F: Fragment of shale showing two small ground facets cut by fractures

were analyzed (six shale beds and four ferricrete outcrops) (Fig. 4).Raw materials coming from more than 20 km from the shelter aredefinedasnon-local rawmaterials according toprocurement systemsdefined elsewhere (Geneste, 1988; Porraz et al., 2008, 2013).

Shale outcrops occur throughout the three main geologicalformations present around Diepkloof:

a) The closest outcrop is located inside the rock shelter: it occursas a long thin dusky red bed of shale in the back of the shelterwithin quartzitic sandstones of the Table Mountain group(Paleozoic);

b) Klipheuwel beds (proto-Paleozoic) are located along the riverwhich runs below the Diepkloof hill, the nearest being 10 kmsouth of the site (sub-local). They are more than 10 m thick andextend more than 100 m;

c) Thicker Malmesbury’s red beds of shale (proto-Paleozoic) wereobserved at more than 20 km southewest of the site (non-local). They are finely laminated micaceous shale or phyllite(see Saggerson and Turner, 1995).

racks due to the action of soluble salts. B: Fragment of ferricrete showing fibrous ironramidal-shaped. D and E: nodules of ferricrete with a lustrous cortex, showing a large.

Fig. 3. Quartzite slab covered by a red-pinkish stain (possibly shale powder) showing smoothed, abraded and striated grains. It was probably used as a grindstone.

Fig. 4. Geological map with the closest sources from the site studied by the analytical methods reported here. Stars represent shale beds and squares represent ferricrete outcrops.


Fig. 5. The key used to assign the different kind of raw materials. Sandstone andquartzite were first separated to fine grained materials. Massive and globular forms ofrocks were assigned to ferricrete e no mudstones were identified at Diepkloof. Layeredmicaceous rock samples were assigned to shale. Layered pieces with no or few micaswere assigned either to the shale, ferricrete, or intermediate shale/ferricrete categorydepending on their density.


Ferricretes occur within tertiary to quaternary soils. Most of thereported ferricrete outcrops are located near Malmesbury for-mations, southewest of the site, and some of them are clearlyassociated with shale beds (localized lateritic weathering profilecould explain such association). The nearest ferricrete source cur-rently recorded is located 20 km from the site. However, some smalltabular nodules of unclear origin were also found next to theshelter, on the side of a second hill.

The current shoreline is located 14 km from Diepkloof but wasfarther away during some parts of the MSA. We estimate that theshorewas ca. 25 km from the sitewith a sea level regression of 50mand at ca. 50 km with a regression of 100 m. The sea regressionwould have exposed raw material sources that are currently notaccessible. The offshore geology at Elandsbaai suggests that mostlyTable Mountain formation should occur in this area. For theframework of this study, we assume that these sub-local and non-local (currently) under-water resources do not differ from thosethat we sampled in the area of Diepkloof. Some raw material couldhave been available in the past within the Verlorenvlei terraces.However, to date no ochre pieces have been discovered in old ter-races, especially those identified below Diepkloof. Archaeologicalpieces are assumed to show a secondary cortex (indicating rollednodules) if they come from such terraces.

3.3. Examination

For both archaeological and geological samples, macroscopicfeatures were recorded: texture (sand, silt and/or clay texture);macroscopic fabric (laminated, massive, globular, porous, etc.);presence of coarse particles (quartz, micas); magnetism (with amagnet); and presence of a weathering cortex. Each samplewas kept intact during analysis. We did not consider hardnessand coloring power because they cannot be estimated withoutscratching the surface of the sample. Likewise, we did not considerthe color of the streak for this reason and because the ochre piecesprobably changed color due to the burning of materials and sedi-ments in several units (Miller et al., 2013).

For each piece, the nature of the rock can be determined basedon the texture, the fabric and the silt to coarse particles identified(quartz or micas). The results of both the chemical analysis (seebelow) and the observations were compared. Macroscopic fea-tures and the chemical compositions of the rocks do not strictlymatch. For instance, fine grained and laminated rocks show var-iable iron content, which may be similar to the one of massiveferricrete samples. The more representative macroscopic featureswere recognized after having analyzed all kind of rock types(Fig. 5).

Techno-typological features were noticed:marks of processingand use-wear traces (striations, incisions, shaping marks); num-ber and shape of worked faces; and shape of the worked pieces.Use-wear traces were identified based onmacroscopic observation.The conclusions of the experimental work of Salomon (2009),Hodgskiss (2010), and partly from Rifkin (2012) were used to assignthemechanical action to the observed use-wear traces and marks,which are mainly grinding or scraping (sometimes called scoring).We carried out preliminary experiments to confirm these obser-vations (SOM Table 1).

3.4. Bulk and structural analyses

A selection of 98 archaeological samples was analyzed as well as83 geological samples (SOM Table 2). Archaeological pieces char-acteristic of the raw material diversity as well as pieces of a moredoubtful attribution were analyzed. Shale and ferricrete sources ofeach kind of geological formation were selected and samples from

the closest outcrops to the site were analyzed. In total, two to 15samples of each source were analyzed, depending on their distancefrom the site (10e15 samples for the closest, only two to five for thefarthest). A JEOL 6460 LV SEM instrument equipped of a lowvacuumsystemwas used allowing the imagery and analysiswithout specificpreparation (coating) of the sample. The distribution, the size andthe shape of minerals measuring more than 1 mm were taken intoaccount. Semi-quantitative analyses were carried out using EDXSOxford XMax 20 spectrometer coupled to the SEM instrument,directly on the surface of complete archaeological pieces and geo-logical fragments of rocks (98 archaeological and 30 geologicalsamples).

Structural phases were determined by X-ray diffraction. Datawere collected with a Bruker D8 Advance diffractometer, equippedwith a PSD Lynxeye detector and operating with a Cu Ka radiation(l ¼ 1.5405 �A). Parallel beam geometry (obtained with a Göbelmirror) was used to carry out surface analyses on complete pieces(83 archaeological and 30 geological samples). Bragg-Brentanogeometry was used to analyze geological powder samples (83geological samples). Raman spectrometry measurements weredone in some cases in complement to XRD analyses. The Ramanspectrometer (Renishaw RM 2000) was coupled with a confocalmicroscope (Leica DMLM) and a CCD detector. A 632.8 nm and a532 nm laser were used (5 archaeological samples). The calibrationof the spectrometer was done with a Si standard (main band:520.5 cm�1).

4. Results of the examination and analysis

4.1. Ochre raw materials

4.1.1. Raw material identificationThree main categories of rocks were identified at Diepkloof:

shale, ferricrete and shale/ferricrete (or intermediate) (Fig. 5and Table 2). Some pieces of ferruginous sandstone and ferru-ginous quartzite were grouped into a fourth category under thedenomination ‘others’. Pieces that have not yet been identifiedand still remain to be analyzed were grouped into a fifth cat-egory named ‘undetermined’. Most of the assemblage (morethan 95% of the pieces) is composed of fine-grained material(predominately clay to silt particles); sandstone and quartzitewere in very low frequencies. No mudstones were identifiedaccording to both examination and analytical results and

Table 2Number and percentages of ochre pieces modified, possibly modified or unmodified by mechanical processes per category of rock.

Raw material Worked Questionable Not worked Total

Nb % Per category % Total worked Nb % Per category Nb % Per category Nb %

Shale 19 4.8 20.0 8 2.0 365 93.1 392 71.4Intermediate 24 57.1 26.7 0 0.0 18 42.9 42 7.7Ferricrete 42 48.3 47.8 4 4.6 41 47.1 87 15.8Fibrous ferricrete 2 11.8 2.2 0.0 0.0 15.0 88.2 17 3.1Quartzite/sandstone 3 27.3 3.3 1 9.1 7 63.6 11 2.0Total 90 16.4 100.0 13 2.4 446 81.2 549 100.0


possible siltstones were classified with shales because of theirlaminated fabric.

Shale dominates the assemblage and accounts for more than71% of the 549 ochre pieces (so, not including the non-ochrepieces). Shale pieces are mainly characterized by a clayesilt tex-ture, laminated fabric, and silt-coarse mica particles. Shale piecesare composed of more than 50% of clay minerals (estimation, 33pieces analyzed) and contain illite-type clay minerals (Fig. 6; seeSOM Table 2). Platy particles of micas are present, which may bemuscovite (composition Si, Al, K). Quartz grains (clay- to sand-sized) are also observed within most of the shale samples, as wellas clays of the kaolinite group.

Several clayish weathered or clayish burnt materials do notshow micaceous particles on a macroscopic scale (while platyparticles are clearly observed by SEM-EDS). Theymight be confusedwith ferricrete formed after the ferruginization of shale or otherlaminated rocks during weathering. Indeed, some iron rich piecesare laminated and may present residual micas (see Fig. 5).A subjective estimation of density was used to differentiate lami-nated clay-rich shale from laminated ferruginized materials. Anintermediate category shale/ferricrete was created to classifydoubtful pieces (Fig. 5). This artificial category does not reflect thereal complexity of the weathered materials encountered from theshale to the ferricrete forms but reflects the limits of the exami-nation method. This intermediate shale/ferricrete category repre-sents about 8% of the assemblage. The majority of the shale/ferricrete pieces analyzed show more than 50% of Fe2O3 and noillite-type clayminerals (see SOM Table 2). They show similar rangeof Fe content than ferricrete pieces. The other pieces of shale/fer-ricrete contain either more than 50% of Fe2O3 and illite-type clayminerals or less than 50% of Fe2O3 and no well-crystallized clayminerals (none was detected by XRD). They probably come fromferruginized shale outcrops where well crystallized clay and/ormica minerals still remain or from weathered clay formations.

Ferricretes account for more than 19% of the pieces. They areidentified by their clay texture and their fabric, either foliated,massive (most of the cases), globular or laminated (rare). Ferrugi-nized materials are often porous. Ferricrete pieces show no illite-type clay minerals and more than 50% of Fe2O3 (Fig. 6). Within fer-ricretes, the iron oxide components are mixed up with differentmineral inclusions, such as quartz grains and micas (platy particlescomposed of Si, Al and K). Prismatic elongated crystals of varioussizes (fromabout5 to100mm)wereobservedwithin several globularferricretes (Fig. 6). Theyaccount forabout3%of the total of thepieces.

The average length of shale, ferricrete, and shale/ferricretepieces ranges between 2 and 2.5 cm. Pieces are small whatever thetype of rawmaterial (sandstone and quartzite not included). All thepieces examined show red to brown hues. No yellowmaterials havebeen discovered yet. Hematite is identified in almost all the pieces,while goethite is detected in only one shale piece as a minorcomponent. Several pieces (about 20%) are magnetic. A magneticiron oxide (maghemite or magnetite) is identified in several ferri-crete and shale/ferricrete pieces either mixed with hematite or

alone, as well as in two shale pieces (see SOM Table 2). Maghemitewas clearly identified instead of magnetite in seven samples(according to XRD and Raman spectrometry results) (Fig. 6 andSOM). The presence of magnetic iron oxides may be explained bythe heating or the burning of pieces (Pomiès et al., 1999; Cornelland Schwertmann, 2003).

4.1.2. Raw materials origin: comparison with geological sourcesMost of the archaeological shale pieces encountered present

characteristics similar to the shale samples collected from theoutcrop of the back of the shelter (Table Mountain Formation): theyshow laminated structure; white potassium-rich micas; and illiteand kaolinite type clay minerals (see SOM Table 3). These piecesmay have entered the deposits from natural erosion of the shaleoutcrop located in the shelter. More relevant information can beobtained by considering possible exogenous materials. Four ana-lyzed shale and one shale/ferricrete pieces show a finely laminatedfabric well-crystallized illite type micas (potassic ones). Malmes-bury shale formations respond to such description. A non-localorigin for these pieces is suspected.

The low iron content of the shale bed located in the back of theshelter indicates an exogenous procurement for all the iron-richshale pieces. Moreover, about 70% of the ferricretes and 55% of theintermediates show a primary cortex that is absent from geologicalsamples recovered near the Diepkloof hill. Ferricretes with differentfabrics were collected within tertiary to quaternary formationsmostly associated with Malmesbury formation during our survey.These formations have undergone more intense weathering pro-cesses than the Table Mountain and Klipheuwel ones, explainingwhy ferricretes are easier found in this context (Roberts, 2003;Porraz et al., 2008). Among the globular geological nodules fibrousiron oxideswere observedon somepieces (three on the sixobservedby SEM-EDS). Well-crystallized iron-oxide formation requiresintense weathering conditions that are typical of the Malmesburyformations’ secondary alteration. The 17 archaeological piecesshowing such crystals’ arrangement are therefore probably fromthis formation and non-local. Massive ferricretes may either comefrom the ferruginization of massive rocks or from the precipitationof iron oxides such as those encountered near Malmesbury for-mations. As the surrounding rocks are mainly laminated ones, thesecond hypothesis seems more probable. Petrographic and geo-chemical analyses would be required to confirm an associationwithMalmesbury’s ferricretes. Nothing can be said about the origin oflaminated ferricretes and shale/ferricretes which may have beenformed after any of the laminated sedimentary formations sur-rounding the site.

Interestingly the majority of the geological ferricretes analyzedcontain either goethite or hematite but none of them containmaghemite. This confirms that maghemite detected in thearchaeological pieces was probably produced by heating andtherefore may be of anthropogenic origin (either intentional oraccidental). It could indicate that some goethite-bearing materialswere initially collected by MSA people. However, goethite is still

Fig. 6. XRD spectra and SEM images of some ochre pieces. A and B: Backscattered electron SEM image of an archaeological ferricrete piece, radial arrangement of elongated ironoxide crystals; XRD spectrum of the same piece. C and D: Backscattered electron SEM image of a geological ferricrete nodule (Ferr 2), radial arrangement of iron oxide crystals; XRDspectrum of a powder sample of the same piece. E and F: Backscattered electron SEM image of an archaeological shale piece, clay particles in gray, mica-like platy particles of Si, Aland K in gray, iron-rich particles in white; XRD spectrum of the same piece. G and H: Backscattered electron SEM image of a geological shale fragment from the local source (shale1); XRD spectrum of a powder sample of the same piece. Mineral phases: illite/muscovite (I), quartz (Q), kaolinite (K), hematite (H), maghemite (M), goethite (G).


present in only two analyzed pieces and as a minor component.Mostly hematite, namely red materials, may have been favoredalthough it is not possible to exclude that yellow materials mayhave been collected.

4.2. Processing of ochre

4.2.1. General features of the processed piecesTaphonomic issues have to be considered before going farther.

Indeed, friable and fragmented shale pieces were observed

throughout the sequence. Trampling, salt growth or burning mayhave eroded their surfaces. These taphonomic phenomena mayhave erased use-wear traces and therefore the number of modifiedpieces observed may have been higher in the past, especially thenumber of modified shale pieces.

Use-wear traces left by past mechanical actions have beensecurely recognized in 16% of the whole assemblage (Table 3). Morequestionable traces were observed on 2.5% of the pieces. Someregular smoothed faces may be due to abrasion although only fewsmoothed grooves are observed on them. Natural lustrous

Table 3Number and percentages of worked faces observed on the ochre pieces as a function of their shape.

1 Face 2 Faces 3 Faces 4 Faces >4 faces Entirelyfaceted

Total % Total

Irregular 14 9 4 0 2 0 29 32.2Irregular, large base 6 3 2 0 0 0 11 12.2Tabular 3 5 2 1 0 1 12 13.3Tabular, triangular base 4 2 2 0 0 0 8 8.9Prismatic 2 2 1 0 1 0 6 6.7Parallelepipedic 4 3 2 0 0 0 9 10.0‘Crayon’ 0 0 8 2 3 2 15 16.7Total 33 24 21 3 6 3 90 100.0% Total 36.7 26.7 23.3 3.3 6.7 3.3 100.0


striations were also observed on geological shale sampled duringthe surveys. These kinds of striations are often recognized becausethe surface of the piece is irregular and the striations are rounded(Fig. 8D and F).

Ferricrete and shale/ferricretes are the two main worked rawmaterials (Table 2 and Fig. 7). Modified ferricrete pieces account forabout 44% of the overall modified pieces. If globular ferricretes areconsidered separately, only two of them are modified among the 15pieces counted. However, they both are intensively ground (one isentirely ground while the other is ground on one large face). Thecontradiction highlighted here could indicate a different control ofthis kind of raw material during the use-life.

Worked shale/ferricrete pieces account for 28% of workedpieces. The difference of proportion of modified pieces betweenferricretes and shale/ferricretes is not significant (probability of thechi2 ¼ 0.1, calculated considering modified, questionable and notmodified pieces). Shale/ferricretes and ferricretes can be seen as aunique group of raw materials. If considered together, shale/ferri-cretes and ferricretes account for about 74% of the modified pieces.

There is a significant difference between the proportion ofmodified shale and ferricrete pieces. Indeed, less than 5% of theshale pieces are modified, probably because at least some of themrepresent natural falls of small shale fragments from the back of theshelter. However, shale pieces account for 21% of the modifiedpieces (Table 2) showing that shale was also used by MSA people.

4.2.2. Knapping marks, wear traces and processingKnapping marks were recognized on five pieces of various raw

materials and may occur on five others. Only two pieces werepossibly knapped before being ground. By contrast, several pieceswere clearly broken e no knapping marks e after being ground orduring grinding (35%), and a weathering cortex is visible undersome striated facets. Regarding this evidence, knapping wasprobably not part of the chaînes opératoires of ochre processing.

Fig. 7. Distribution of the number of worked and unworked pieces as a function of rawmaterial.

Only pieces showing wear traces were included in processed piecesfor this reason.

All of the worked pieces show signs of grinding (N ¼ 90).Abrasion facets showing groups of parallel or more seldom sub-parallel striations are observed (Fig. 8). Ground facets are planar toconvex, except for two pieces with subparallel striations on aconcave face adjacent to planar faces. Both pieces are too small toreach firm conclusions on the process used, either grinding orscraping. No incisions or engraving were identified within thestudied samples.

The number of ground facets ranges from one to seven per piecewith a majority of them showing one or two facets (63%). But thenumber of facets is not necessarily related to the intensity of theprocess. The creation of large convex faces requires numerous backand forth grinding movements to totally erase the natural shape ofa piece, especially for hard ferricrete pieces. Pieces with a singlelarge face and with three ground faces or more constitute about45% of the total worked pieces.

The shape of the ground pieces is more or less linked to thenumber of ground facets (Table 3). Tabular shapes are commonlyobserved among laminated rock fragments or laminated nodules,and most of them show one or two ground faces. However severalof them show a triangular base. The ground facets are located onthe thinner faces of the tabular piece and the triangle base wasformed after abrasion. This shape is likely the results of their havingbeen held by their larger natural faces. ‘Crayon’-shaped pieces,referring to pieces with faces forming an apex compounded of atleast three ground faces, describes 15 pieces that account for about17% of the ground pieces. They have been also shown to come fromholding and from changes of the piece’s orientation during theprocess (see Wadley, 2005b). On the softer ‘crayon’-shaped pieces,use-wear traces appear more smoothed on some facets. They mayhave been smoothed by fingers rubbing on the piece, according toboth our experiments and previous research (Soressi and D’Errico,2007; Rifkin, 2012). In contrast with what Watts (2010) proposed,our experiments show that no breakage is required to form a‘crayon’-shape, only a change of orientation. The apex of the‘crayons’ do not show smaller facets on the tip as previouslydescribed for pieces which were used to draw on hard materials.They are more likely waste products than intentionally shapedartifacts.

Among the artifacts covered by ochre residues found during theexcavations, three are large tabular fragments of quartzite. Theochre residues are not distributed across the piece but extend as athin layer. Smoothed areas are observed on two of them (fromHowiesons Poort units). This is consistent with a use as a lowgrindstone (Hamon, 2008). In sum, all the observations indicateochre transformation by grinding in order to produce powder. Thevariability of shape observed in the assemblage is not related todifferent purposes but more likely to various intensities of use(stage of discard) and to various raw shapes.

Fig. 8. Microscopic images of archaeological and geological pieces. A and C: groups of parallel striations on a ferricrete pieces. B: groups of parallel striations on a shale piece. D:taphonomic irregular grooves on a shale piece. E: groups of parallel striations on a ground fragment of geological shale from the back of the shelter. F: irregular surface andsmoothed grooves on a geological piece of shale from the back of the shelter.


4.3. Stratigraphic repartition and diachronic changes

All the stratigraphic units studied yielded ochre pieces exceptfor SU Eve. Some of them do not contain worked pieces (absent infive among the 36 reported). However, ground ochre pieces areencountered in these units in other sections of the site (squares L6,M7-9, N7-9). Therefore ochre procurement, processing, and useappear to be consistently performed through time.

The two main types of raw materials (shale, iron-rich pieces)are present throughout the sequence (Fig. 9 and SOM Table 2). Atthe bottom the base of the sequence to the Still Bay unitsunmodified shale fragments are abundant. Taphonomic biasesprevent us from reaching conclusions on whether this accumu-lation is of anthropogenic origin. Iron-rich pieces are observed ineach unit except for a Still Bay one. There is a similar distributionbetween modified and iron-rich pieces of ochre from the base of

the sequence to the SU Ester (Late Howiesons Poort). Theexploitation of iron-enriched materials was consistent throughtime until this period. Also noticeable is the distribution of theiron-rich materials identified as non-local (pieces associated toMalmesbury formations). They appear from SU John (one groundpiece) and are mostly encountered in the Late Howiesons Poortwhere 15 of them were recovered in three different units (SUFrans, Eric and Debbie).

5. Discussion

5.1. Ochre processing and use at Diepkloof Rock Shelter

Our analysis allows us to describe the basic steps of ochre col-lection and processing at Diepkloof (Fig. 10). Whereas shale piecesmay have been mainly collected at the site, iron-rich pieces are

Fig. 9. Distribution of ochre pieces, worked ochre pieces, and iron-rich piecesthroughout the MSA sequence of Diepkloof Rock Shelter (archaeological sequence afterPorraz et al., 2013).

Fig. 10. Summary of the main ‘chaîne opératoire’ axes identified, from the raw material pronodules were selected. Grinding is the only mechanical process identified, probably with thepieces were probably burnt after being discarded.


undoubtedly exogenous. A non-local type of ferricrete (ferricretewith well-crystallized iron oxide) was recognized. This type offerricrete appears from the SU John (Intermediate HowiesonsPoort). This could reflect either a change in supply strategies overthe sequence or the depletion of some ochre sources. Other ferri-crete types were collected along with the non-local type in eachstratigraphic unit where they were found. This suggests that morediverse sources were exploited from the Intermediate HP and moreprobably implies a change in supply strategies. This procurementpattern fits well with the increase of raw materials diversityobserved in parallel for the HP lithic industries at Diepkloof (Porrazet al., 2013).

Fragments of shale and ferricrete nodules were probablydirectly ground on a passive quartzite slabs at the site. The Die-pkloof inhabitants did not commonly use percussion to fractureochre, probably because of the small size of the collected nodules.Scraping, although doubtful on two pieces, is unlikely to have beensubstituted for grinding at any time considering the presence ofground pieces throughout the sequence. However grinding withtwo grinding stones (or pounding) can not be excluded. Indeed, theevidence left by such process is minimal: they may be recognizedby the presence of ochre staining within the archaeological layers(Salomon, 2009). However no accumulation of ochre powder hasbeen observed during excavation, neither at a macroscopic nor at amicroscopic scale (Miller et al., 2013). Finally, several samples mayhave been heated according to the presence of maghemite. Noevidence that heating may have occurred before grinding havebeen discovered. Accidental burning of the pieces would be con-sistent with the abundant evidence of fire action within thearchaeological deposits, such as ashes or charcoal lenses or burntbones (Miller et al., 2013, Steele and Klein, 2013). However, anintentional heating of some pieces can’t be excluded.

With regards to investigating the technical skill and the socio-economical organization of early modern human hunteregatherersocieties, the processing of non-local materials at Diepkloof isclearly significant: it implies planning tasks related to specific needs.

curement to the discard of the remains. Either small shale fragment or small iron-richgoal of producing powder. Heat treatment before grinding is possible although several


Moreover, the grayish or blackish appearance of the non-local fer-ricretesmakes them less recognizable as potential hematite-bearingmaterials than reddish forms. A clear distinction was then madebetween the appearance of a massive material and the powderextracted from it.

In contrast with the technological changes recorded in the lithicindustries (Porraz et al., 2013), the exploitation of the ochreresource remains quite constant. However it is worth mentioningthat the production of powder does not imply a complex man-agement of the block of raw material: the whole piece can beconverted into powder whatever the technique used. The grindingtechnique is more likely to have been chosen according to thehardness of the raw materials or other criteria which would haveremaindered consistent through time, such as the quality of thepowder produced. For instance, powder tends to be finer whenusing direct grinding than when using two grindstones (Salomon,2009; Rifkin, 2012).

It is important to note that although red materials were alreadyavailable in the shelter, iron-enrichedmaterials were brought to thesite and processed from the beginning of the MSA occupation atDRS. This means that MSA people deliberately selected ochredepending to its properties and not only to its availabilities. Thecoloring power of iron oxides, higher in iron-rich materials, mayhave been one of these properties. The drying property of hematite,demonstrated by different experiments, and the abrasive propertyof hematite powder may be other desired qualities (Audouin andPlisson, 1982; White, 1996; Wadley, 2005a).

From an overall point of view, the site of Diepkloof has notyielded direct evidence of any purpose of the use of ochre. How-ever, several hypotheses are improbable when other archaeologicaldata are considered. For instance, no polished or pointed pieceshave been found at Diepkloof (no bone industry), whichmight haveindicated ochre’s use as an abrasive. There were no ochre residueson lithic tools used to work hide, according to preliminary exami-nation of use-wear traces (Igreja and Porraz, 2013). Ochre’s use as aloading agent, in adhesives for instance, is even more doubtfulbecause none of the studied lithic tools show ochre residues onareas where they were held or hafted (Charrié-Duhaut et al., 2013).With regard to ochre’s possible use as pigment, no paintings werefound in the MSA units at Diepkloof. The production of engravedgeometric signs by MSA people at Diepkloof is however wellestablished (Texier et al., 2010; 2013). The question arises ofwhether ochre powder may also have been used as pigment toproduce designs, although to date only indirect evidence supportssuch use, such as the potential for the ground ochre pieces toproduce pigment powder.

5.2. Diepkloof in the southern African context

The regular presence of ochre pieces throughout the MSAsequence of Diepkloof is in agreement with previous descriptionsof ochre use within South African sites from the end of the MiddlePleistocene (Watts, 1999, 2002, 2009; 2010; McBrearty and Brooks,2000; Henshilwood et al., 2011). Considering the absence of anysignificant gaps within the deposits (Miller et al., 2013), the Die-pkloof sequence highlights the lasting tradition of ochre exploita-tion from about 110 ky to 50 ky ago.

The relative abundance of raw materials varies greatly from onesite to another, and Diepkloof shows higher proportions of iron-richpieces compared to Blombos Cave for instance (Watts, 2009).Geological context is probably the main variable affecting differ-ences in raw material selection. Indeed, the geological contexts arequite similar at Blombos Cave and Pinnacle Point (Table Mountainand Bokkeveld formations) while the geological context near Die-pkloof is different (Malmesbury and Table Mountain formations).

Regional influences on procurement patterns were previouslyhighlighted by Watts (1999, 2002) within 11 MSA ochre assemb-lages from southern Africa, including both Klasies River and BorderCave. By contrast, fine-grained materials and iron-enriched mate-rials were preferentially selected at both Pinnacle Point (Watts,2010) and Diepkloof. Such properties probably reflect intendedneeds and maybe similar needs in both sites.

With regard to the processing of ochre, the proportion ofmodified pieces (16%) is within the range of other MSA sites (Watts,2002, 2009, 2010). Like at Diepkloof, grinding is the major processidentified at Pinnacle Point (Watts, 2010) and Sibudu Cave(Hodgskiss, 2010) (see Table 1). The absence of scraping is a tech-nical difference with the other sites. At Blombos Cave, scrapedpieces were shown to be softer than ground pieces, and softermaterials appear to be iron-poor materials such as siltstone orsandstone (Watts, 2009; Henshilwood et al., 2009; Rifkin, 2012).These raw materials are rare at Diepkloof compared to BlombosCave. MSA people probably adapted the powder extraction techni-que to the nature of the raw materials. However there are otherdifferences between Diepkloof and Blombos Cave. Crayon-shapedpieces do not show use-wear traces of a secondary use at Die-pkloof unlike those from Blombos Cave. Possible engravings wereobserved on some pieces from Klasies River (Singer and Wymer,1982), Klein Kliphuis (Mackay and Welz, 2008) and Pinnacle Point(Watts, 2010) but only those from Blombos Cave show clear geo-metric patterns. Although no incisionswere reported on the studiedassemblage, one incised piece was reported within the SU Jude inthe adjacent square L6 (MacKay, personal communication). Nogeometric designs can be recognized on the piece. These differencescould be related to rawmaterials differences, but theyare difficult tolink to any technical issue. They rather suggest that ochre may havebeen regarded differently by the inhabitants of these sites. They areinsufficient data to make a conclusion but the role of ochre mustcontinue to be questioned through its processing.

With regard to potential use, the use of ochre in hafting isunlikely at Diepkloof during the Howiesons Poort (Charrié-Duhautet al., 2013). On the contrary, ochre is clearly observed on the backof segments at Sibudu Cave, Rose Cottage Cave and Umhlatuzana inHowiesons Poort units making it highly probable that ochre wasused in hafting adhesives (Wadley, 2005a; Lombard, 2007; Wadleyet al., 2009). This confirms the hypothesis put forward by severalauthors that ochre was used in various ways during the MSA(Wadley, 2005a; Lombard, 2007; d’Errico et al., 2010; Watts, 2010;Henshilwood and Dubreuil, 2011). The use of ochre as a loadingagent is persistent through time at Sibudu Cave, but it remainsconfined to sites located in the Eastern part of South Africa (Wadleyet al., 2004, 2005a; Lombard, 2007). Regional cultural traits mayexplain this difference in use at contemporaneous sites from dif-ferent areas.

6. Conclusion

Examination and analytical methods provide a powerful com-bination to study ochre pieces. We showed how ochre may havebeen a wide-spread resource at Diepkloof throughout the secondpart of the MSA and how it constitutes a clearly separate technicalsub-system from other lithic resources. While several changes areobserved regarding the lithic industries sub-system, the mainprocessing step of ochre’s mechanical transformation and themineralogical composition of the selected rawmaterials remain thesame. The main change observed is linked to a change in theexploited sources. This emphases how ochre exploitation was wellestablished from at least the lower MSA. Comparing Diepkloof’sdata with the data from other regional sites brought us new insighton the cultural patterns of ochre exploitation. Behind an extended


exploitation through time and space during the MSA, different usewas shown to occur at a regional scale, adding new lines of evi-dence for the delimitation of regional cultural influences. Never-theless, we must emphasize how incomplete the data are aboutochre processing and its use during the Middle Stone Age.Increasing the number of studies of large and coherent assemblagesof ochre would be of great help for increasing comparisonsbetween sites.

Acknowledgements

The scientific project and excavation at Diepkloof have beenfunded by the French Ministry of Foreign Affairs (MAE), theAquitaine region, the Provence-Alpes-Côte-d’Azur region and bythe Centre National de la Recherche Scientifique (CNRS). We arethankful to the Paleontological Scientific Trust (PAST) and theNational Research Foundation (NRF) of South Africa for funding,and to D. & M. van Wyk and J. Pollet for permission to work ontheir land, as well as the Heritage Western Cape (HWC) for per-mits to excavate at DRS. The University of Cape Town has been ofgreat support in providing space, facilities and other logisticalhelp.

This study has been funded by the University of Bordeaux 3, theCentre National de la Recherche Scientifique and the RégionAquitaine. We sincerely thank John Parkington and Judith Sealy fortheir personal help. Thank you to the South African HeritageResources Agency (SAHRA) for granting us permission to exportochre pieces in France. We are grateful to Sarah Wurz who helpedus obtaining the permits. Thank you to Nadia Cantin, StéphaneDubernet and Yannick Lefrais for their advice concerning thearchaeometric part. We also thank Cuan Hahndiek and AlexMacKay for our discussions and Teresa Steele for the reading of theEnglish and her comments.

Appendix A. Supplementary data

Supplementary data related to this article can be found at http://dx.doi.org/10.1016/j.jas.2013.01.025.

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