Shahdad and the bronze age in southeast Iran

A workshop commemorating Prof. A. Hakemi's work at Shahdad and 40 years of excavations in southeast Iran

Cambridge, July 15-16, 2011

A chlorite container found on the surface of Shahdad (Kerman, Iran, mid-late 4th millennium BCE)

and its cosmetic content

Massimo Vidale*, Oliver Craig**, Francois Desset***, Giuseppe Guida *, Giancarlo Sidoti*, Enrico Battistella****

* Istituto Superiore per la Conservazione e il Restauro, Rome, Italy; **Dept. of Biology, BioArch, University of York (UK); *** University Paris I Panthéon-Sorbonne, France;

****University of Bologna, Italy

Shahdad

Konar Sandal

HELMANDJAZMURIAN

Shahr-e Sukhteh

LUT

Acknowlegments

Many thanks to ICHTO and to the many Iranian colleagues who made possible and pleasant our work in their wonderful country.

This research was supported by IsIAO and the Italian Ministry for Foreign Affairs (MAE), as well as by the Istituto Superiore per la Conservazione e il Restauro (ISCR, Rome) through the access to archeometric facilities.

Arnaldo Tonelli, Franco Finotti & Fabiana Zandonai Site

 Shahdad, Iran (baricenter)

 30° 26’ 08’’N

 57° 45’ 20’’E

 5 km

Thanks to the collaboration with ASI e MCR we can use a set of high resolution radar pictures, produced by the satellites network Cosmos-Skymed. SkyMed is based upon a constellation of 4 identical satellites, endowed with synthetic-opening radars (SAR) working on a X band. The system may provide, on a planetary scale, innovative information for the interpretation and monitoring of environments. The images with topographic details of the Shahdad sites we present were taken on September 2010.

The 5th and 4th millennia BCE settlement mounds at the eastern fringe of the site complex

Arnaldo Tonelli, Franco Finotti e Fabiana Zandonai

A detail of the radar image showing the mounds of the 5th and 4th millennia BCE. The radar answers with a nominal resolution of 0.5 m. Darker areas are distiguished by a greater absorption, interpreted, in this case, by a greater retention of moisture on the topmost soil horizons.

Elaborating the previous image by comparing the maximum and minimum intensity of the radar results on a flowing matrix of 5 x 5 pixels. The result is an edge enhancement of continuity anomalies on areas of about 6 sq m. A probable buried line of qanats, invisible on surface, seems to connect the two mounds.

Arnaldo Tonelli, Franco Finotti & Fabiana Zandonai

Arnaldo Tonelli, Franco Finotti e Fabiana Zandonai

The previous image, once geo-referenced on a portion of the wider radar image of the site complex.

Shahdad, March 2009

Late 4° millennium BCE ceramics found on surface together with the chlorite flagon

Aliabad conical vases with ring foot and late Uruk/Jemdet-Nasr related ear-lugs

The flagon, made of a dark green-gray chlorite, weathered on surface, is a tall cylinder, 15.5 cm long and 3.6 cm wide at the maximum expansion. The mouth is slightly restricted (outer diameter on the lip 3.35-3,4 cm; inner mouth diameter ca. 2 cm). The lip slightly protrudes outwards, and the base is flat. The wall below the rim, where measurable, is about 0.55-0.60 cm thick. The stone’s natural veins are oriented along the vessel’s main axis.

The associated ceramics suggest that it is one of the oldest chlorite vessels so far found in Middle Asia, and this possibly explains why it finds no comparisons in the repertory of the stone vessels so far published.

The chlorite receptacle was excavated stratigraphically, carefully following variations in color and compactness of the contained substance.

layer 5 (solid substance in the bottom)

layer 4 layer 3 layer 2 layer 1

The bottom was filled, for a thickness of 2-3 cm, with a solid gray substance showing little evidence of chemical and physical alteration (layer 5). These are the samples we took

layer 5, cerussite

XRD analysis of layer 5 shows that this substance is made of cerussite (lead carbonate)

The XRD pattern of layer 5, compared to a standard cerussite XRD spectrum

almost pure lead carbonate (PbO3, cerussite)

cerussite, hydrocerussite with quartz and traces of clinochlore (aeolian activity, sedimentation and weathering of inner wall)

Kenneth Graham (in Woolley 1934: 248) originally identified lead carbonates in two cosmetic pigments - light blue and black - found in the shells of the Royal Cemetery of Ur (about 2400-2300 BCE), but stated that they had formed in the ground through the alteration of lead oxides. When Bimson (1980) analyzed some light colored pigments from the same contexts, he identified hydroxy-apatite from calcined bones, but did not rule out cerussite, perhaps added to green pigments for diluting their hue (see also Moorey 1999: 138-139).

Cerussite powders contained in semiprecious receptacles were analytically identified, among other cosmetics compounds, both at Mohenjo-daro and Harappa, ca. 2600-1800 BCE (Sana Ullah 1931, other results reviewed in Chandra 1973 and Subbarayappa 1997).

Cerussite-based pigments were recently identified in the graves of Adji Kui (Margiana, late 3rd millennium BCE)

PbSPbS

PbS

PbS

PbS

PbS

PbSLayer 5

A lead carbonate (cerussite) ground mass with calcium and aluminum and PbS (galena) tiny crystalline inclusions

Layer 5

At higher magnification, the amorphous phase shows localized tabular and complex wide crystals (ca. 5 to 50 m wide) compatible with cerussite.

At the centre of image on top, the crystal of about 5μm, at the top right, shows a trigonal symmetry marked by the basal face (rectangular shape, (001) form), with the emergence of a singular crystallographic axe; the adjacent face, in contrast, has the shape of an irregular hexagon, and belongs to the romboedron, (112) form. While these crystals are near to a prismatic habit, there are other crystalline formations, almost thick tabular, growing from the matrix with irregular hexagonal outlines.

Above 900 °C lead compounds start to volatilize (Hatakeyama & Zhenhai Liu 1998). In our sample the weight loss was about 10.5 % meaning that our sample made of lead carbonates for a value included between 63 and 76%. TheTGA curve shows that the sample is made for ca. 4% of calcium carbonate, confirming the presence of a certain amount of calcium also detected by SEM-EDXRF analysis

Layer 4, TGA analysis

Layer 5

Traces of copper probably left by the use of a copper pin-applicator

TO SUM UP

We could be dealing with an artificial cerussite.

Ancient sources (Ist century BCE-Ist century AD) state that white lead was made by hanging lead sheets over terracotta jars full of vinegar, surrounded by dung. Vinegar vapours reacted with the lead surfaces, creating a lead acetate. The carbon dioxide from the fermenting dung reacted with acetate creating white, shiny lead carbonate.

This or other processes would represent the earliest known example of «wet chemical processes».

In this cerussite mass are evenly scattered minute compact crystalline formations, with a marked and intense cubic cleavage, resulting from metallogenetic processes, of galena (PbS), ca. 50 to 200 m in length. They are surrounded by a layer of molten metal

These tiny galena particles are surrounded by a homogeneous film of molten lead, about 10-20 m thick. Galena crystals contain (on surface) a certain amount of sulphur, but that the same element is absent in the molten outer film, chemically identical to the groundmass, thus confirming their pyro-technological origin (because sulphur was gradually removed by heating).

SEM elements mapping: lead vs. sulphur

Layer 5.

Vegetal particles included in the carbonate groundmass and imprints of tiny vegetal inclusions.

FTIR (Fourier Transform Infrared Spectroscopy), layer 4

Even though the spectrum could not interpreted univocally due to the low amount of organic matter, the signals at 2853, 2923, 2954 cm-1 (C_H stretching) and at 1737 cm-1 (C==O stretching) suggest the presence of traces of oils or wax.

possible traces of oils or wax added to the cosmetic substance as binding agents

layer 1

layer 4

layer 5

GC-MS analysisThe organic content of layer 5 is low, however this does not rule out the presence of the additional compounds more recalcitrant or not amenable by gas chromatography. Traces of 8-methylcoumarin were noted in layer 5 (m/z 160, 132, 104, 51). This is an aromatic compound derived from a range of plant species. To note, 8-methylcoumarin was not found in the sample from the upper part of the vessel so may be endogenous to the sample. However, we cannot rule out an exogenous source.

Some genuses and several species of plants available to the 4th-3rd millennium

craftspersons of Shahdad naturally contain coumarins, among others

Verbascum

Lavandula (lavander)

Cyminum comynum (cumin: seeds used as a spice at Shahr-e Sukhteh)

Galium odoratum

Anthoxantum odoratum (vanilla-scented)

IN CONCLUSION

The inorganic components of the Shahdad cosmetic, possibly the earliest product of this type ever found in the Near East and Middle Asia, was a cerussite-based face-paint or white foundation.

As far as the organic content is concerned, contamination in principle cannot be excluded, but the substance does include a few tiny vegetal particles. It might retain minimal traces of organic materials like binders (oils or wax) and perhaps some aromatic ingredients are endogenous.

The traces of copper we found by SEM-EDXRF in the lowermost layer reveal the use of a copper applicator, as those found in later Bronze-age burials at Shahdad and in Margiana.

White lead (cerussite) pigments and foundations

Among cross-cultural factors of facial attractiveness range youthfulness, skin homogeneity and luminance, conformity or similarity of the face to the population average, bilateral symmetry, sexual dimorphism (masculinity vs. femininity). Female skin is universally lighter than male skin, with a greater luminance contrast between eyes and lips.

Besides concealing perspiration and skin defects, a white face might be universally perceived as a super-feminine feature.

Cosmetics are a complex technology that provided females with the unnatural complexion required by new virtual identities and official roles. Cosmetics, like writing, organized and managed social interaction.

faces of power

A couple of bone cosmetic flagons from Bactria (in a private collection) made out of camel’s phalanges (thanks to Tonino Tagliacozzo & Jacopo de Grossi Mazzorin)

Courtesy of Edoardo Lolliva (ISCR)

Courtesy of Gianfranco Priori (ISCR)

Courtesy of Gianfranco Priori (ISCR)

A receptacle for an applicator rather than a cosmetic container

Traces of white lead and copper powder were found by SEM on the bone applicator

CuPb

Courtesy of Sergio Dipilato (Ospedale Regina Margherita, Rome) and Giuseppe Guida (ISCR), research by Martina Masin (University of Padua)