Archaeological Materials

Chapter 27 Archaeological Materials Richard I. Macphail1, Paul Goldberg2, 3 UNI VERSITY COLLEGE LONDON, LOND ON, UNITED K INGDOM; BOSTON UNIV ERSIT Y, BOS TON, M A , UNITE D STAT ES; 3 UNI VERSITY OF WOLLONGONG, WOLLONGONG, NS W, AUSTRALIA 1 2

CHAPTER OUTLINE 1. Introduction ................................................................................................................................... 779 2. Natural Soils and Sediments Employed in Construction.......................................................... 780 2.1 Turf .......................................................................................................................................... 780 2.2 Ground-Raising Constructional Materials ............................................................................ 783 2.3 Floors, Surfaces and Walls..................................................................................................... 784 2.4 Organic Floor Coverings ........................................................................................................ 790 3. Waste Materials ............................................................................................................................ 790 3.1 Inorganic Waste Materials .................................................................................................... 791 3.2 Organic Waste Materials ....................................................................................................... 794 3.2.1 Herbivore Dung ............................................................................................................... 794 3.2.2 Pig Dung.......................................................................................................................... 797 3.2.3 Dog Coprolites................................................................................................................. 799 3.2.4 Human Coprolites ............................................................................................................ 800 4. Manufactured Materials............................................................................................................... 802 4.1 Stone Tools ............................................................................................................................. 802 4.2 Plasters and Mortars .............................................................................................................. 803 4.3 Metal Working ....................................................................................................................... 805 5. Conclusions .................................................................................................................................... 807 Acknowledgements ........................................................................................................................... 807 References........................................................................................................................................... 808

1. Introduction This chapter deals with the use of soil micromorphology for examining archaeological materials, to understand their formation and the manner in which they enter the archaeological record. This knowledge can then be applied to reconstruct past human Interpretation of Micromorphological Features of Soils and Regoliths. https://doi.org/10.1016/B978-0-444-63522-8.00027-9 Copyright © 2018 Elsevier B.V. All rights reserved.

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technologies and activities, especially when combined with microfacies analysis (Courty, 2001). Included in the discussion are natural soils and sediments employed in constructions that have been little transformed. These elements should be readily recognisable to workers experienced in natural soils and sediments. In contrast, archaeological materials found in occupation areas often have origins and formation processes completely outside the experience of most micropedologists and petrologists. This article is therefore partly meant to familiarise them with these somewhat atypical objects in thin section. Lastly, manufactured materials are often familiar to material scientists, such as archaeometallurgists, but it is important that these materials, and their weathered transformations, are readily recognised more widely in thin section. The variety of archaeological materials being reported on has grown exponentially since the 1980s (Courty et al., 1989) and as a result only a restricted coverage of the subject is offered here. Soil micromorphological descriptions and supportive data are detailed in referenced articles and in the figure captions.

2. Natural Soils and Sediments Employed in Construction Natural materials, such as turf, brickearth, loess, alluvium and till, can be employed in their raw state or be mixed with various mineral and plant tempers to produce adobe materials, such as daub and mud brick (see Fig. 3C). Various raw, little-transformed and burned variants will be examined here. When encountered in their raw state, natural soils and sediments used as constructional materials may be difficult to discern. Thin sections can show the occurrence of a natural material which is not present in a local natural soil or sediment and which is thus anomalous or exotic. The archaeological context may provide key information (e.g., mound or tumulus, floor or wall within a structure), but sometimes the context is not clear, and the presence of soils and sediments as a constructional material may only be recognised on the basis of soil horizons or sediments being in anomalous positions. For example, the occurrence of Bt horizon material along with textural pedofeatures (e.g., clay coatings) that are not oriented according to the present ‘way-up’ position may indicate that a soil slab has been used for construction. When soils are employed, different horizons can be used. The use of Ah, A2, Bt and Ctk horizons of Luvisols have been reported, alongside turves from podzols (Evans, 1957; Fenton, 1968; Macphail, 1987, 2003). However, field and archaeological explanations may well be wrong, and it is the chief role of soil micromorphology to correct these interpretations (see Fig. 3A).

2.1

Turf

Turf (topsoil) has been employed ubiquitously to construct mounds and ramparts in temperate regions (Van Nest, et al., 2001; Goldberg & Macphail, 2006). It can provide important environmental information on past landscapes, especially when combined with dating, palynology and the study of land snails (Alexandrovskiy & Chichagova, 1998; also

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note pioneer studies by Dimbleby (1962), Evans (1972) and reports by I. Cornwall reviewed by Macphail (1987)) (Fig. 1). Turf has specific characteristics according to the edaphic conditions under which it formed and the types of organic forms, such as mull, moder and mor. Excrements of soil mesofauna and preservation of organic matter reflect these conditions (Babel, 1975; Bal, 1982; Nys et al., 1987; see also Gerasimova & LebedevaVerba, 2010; Stolt & Lindbo, 2010; Gerasimova & Lebedeva, 2018; Ismail-Meyer et al., 2018; Kooistra & Pulleman, 2018). For example, at some poorly drained locations, grass litter decays slowly at the soil surface as thin microlaminated layers of leaves and excrements forming a laminated mull (Barrat, 1964); the initial construction of both Hadrian’s Wall (wAD 122) near Carlisle, United Kingdom, and the Viking Age Gokstad Ship Burial Mound near Sandefjord, Vestfold, Norway, employed laminated mull turves, with sedge grassland being the turf source at Gokstad (Macphail et al., 2013). The presence of turf or buried turf (Carter, 1990) can be recognised from its humic and biological character in the form of pure organic matter, mineral soil with high organic matter content organised as organo-mineral excrements and sometimes a preponderance of organic excrements of all sizes, with structures and excrements becoming generally finer up-profile; note, however, that the broad organic excrements of comminuters may most commonly occur in surface organic horizons. Plant residues and relict roots may also be expected to be more numerous in an upward direction, thus pointing to the ‘right-way-up’ for the turf (Fig. 1).

A

B

FIGURE 1 Turf. In situ modern turf from upper part of turf roof (Bagböle, Umeå University Experimental Farm, north Sweden; see Viklund, 1998; Goldberg & Macphail, 2006). (A) Acidic grassland mull horizon with living grass roots in right-way up position, very abundant thin organic and organo-mineral excrements in the uppermost part and the presence of wood charcoal providing evidence of past land use history (conifer forest clearance or management) (NL, scale bar length 2 mm). (B) Detail of same sample showing fresh roots (FR) from grass currently growing on the turf roof, and old roots (OR) showing ‘browning’ that are probably relicts of original pasture soil used to construct the turf roof; thin and sometimes coalesced organic excrements occur between sand grains (PPL, scale bar length 1 mm).

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During mound or rampart construction, any type of turf can be employed. Romans and Robertson (1983) suggested that the 5.5-m-high Neolithic mound at Strathallan, Scotland, was constructed of poorly stable agricultural topsoil; this construction led to disaggregation and the formation of very abundant textural pedofeatures (dusty clay void coatings and silty clay infillings) (Barclay, 1983; Macphail et al., 1987). Both grazed grassland and woodland turf were collected to construct the putative mound at RomanoBritish Folly Lane, St Albans, whereas a series of Bronze Age mounds at West Heath were constructed from acid heathland turf developed on podzols (Scaife & Macphail, 1983; Macphail et al., 1998; see also Macphail et al., 2003). Turf may be laid ‘right-way-up’, inverted or face to face. The experimental grassland mull turf roof at Umea˚, north Sweden, was constructed with the bottom turf facing downwards and the upper (‘living’) turf facing upwards (Cruise & Macphail, 2000; Goldberg & Macphail, 2006) (Fig. 1). Modern Icelandic turf roofs have been investigated by Milek (2006). Turf roofs cannot be made out of moder or mor horizons because these are prone to rapid oxidation and decay. The remains of (burned) grass turf wall material from the estimated 1-m-thick and 1.5-m-high walls from Iron Age Denmark were identified by a microaggregated fabric and highly humic aspect (Nørnberg & Courty, 1985). Similarly, turf fragments in a sunken building were found to contain organo-mineral and amorphous organic matter; minerogenic lenses within turf fragments are relict of rapid tephra fallout (Simpson et al., 1999). Viking house turf walls have also been studied to investigate contemporary soils (Milek, 2004). Turf in mounds and buried turf (in situ topsoil) undergo various transformations. Changes related to a decrease in pH have been reported (Macphail, 1993; Crowther et al., 1996). In field experiments, base-rich turf became compact as organo-mineral excrements became coalesced, and a more acidic mesofauna producing thin bacillocylinders became dominant (Crowther et al., 1996). At Neolithic Easton Down, Wiltshire, the baserich but decalcified turf that had formed on chalk seems to have been transformed in exactly the same way (Macphail, 1993). On loess over chalk at the turf rampart of Neolithic Belle Tout, East Sussex, no individual excrements are visible, and only the compact remains of a totally biologically reworked microfabric with relict fabric features of burrowing are present in a soil with a superimposed accommodating angular blocky microstructure. In acid sandy soils, compaction and ‘ageing’ can lead to changes in c/ f-related distribution pattern (from enaulic progressively to chitonic, gefuric and porphyric), a decrease in interference colours of the plant material and preferential preservation of poorly decomposable organic materials (lignified cells) and charcoal (Scaife & Macphail, 1983; Macphail et al., 2003). In other field experiments and at a Bronze Age site, the base of the turf core displays a predominantly porphyric c/f-related distribution pattern and well-preserved organic matter, presumably due to the maintenance of soil wetness. Organic matter and turf layers may become mineralised through postdepositional movement of sesquioxides (Runia, 1988; Macphail et al., 2003). The chemical and micromorphological transformation of barrow turf into spodic

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pyrophosphate and dithionite Fe- and Al-enriched monomorphic material was reported by Fisher and Macphail (1985) (see also Vepraskas et al., 2018). Mounds can develop iron/manganese oxide pans because of localised waterlogging, which tends to accentuate turf structures within them, as well as the contact between the mound and the underlying soil; at the Gokstad Mound mobile phosphate had formed concentrations of vivianite in litter-rich turf layers (Bouma et al.,1990; Macphail et al., 1998, 2013). Fragments of turf, which retain characteristic biological microfabrics such as thin burrows (passage features) and excrements, are sometimes common components in the fills of sunken feature houses (e.g., Grubenha¨user) because of collapsed turf walls and roofs constructed from turf (Simpson et al., 1999; Macphail et al., 2006a; Milek, 2006).

2.2

Ground-Raising Constructional Materials

Constructions often include ground-raising and surface-sealing activities (Blume, 1989). Raw materials derived from local soils and underlying bedrock are often employed (see Figs. 2 to 4). In northwest Europe, for example, this material is commonly derived from the typical Luvisols formed on loess and from aeolian silt with alluvial admixtures of sand (brickearth). In the Balkans and in the Near and Middle East, tells include mud bricks derived from local alluvial soils (Goldberg, 1979; Rosen, 1986; Stoops & Nijs, 1986; , 2003; Love, 2012; Macphail et al., 2017a). The presence of Matthews et al., 1996; Haita rounded clay clasts and allochthonous carbonate nodules can be indicative of an alluvial soil origin (Goldberg, 1979; see also Nodarou et al., 2008). From Roman, medieval to modern times, these materials were employed in urban areas for levelling ground ahead of construction (Macphail, 1994). Sometimes burned daub from razed buildings was also used. Mesopotamian tells also developed through incidental and deliberate groundraising and the accumulation of decayed mud brick (Friesem et al., 2011). This was brought about by dumps of all kinds of anthropogenic materials, such as ashes and building debris, which were also employed as ‘constructional packing’ below constructed plaster floors and matted surfaces (Matthews & Postgate, 1994; Matthews, 1995; Matthews et al., 1996) (see Fig. 8A). At Phoenician Tel Dor, Israel, however, groundraising associated with manufactured floors and animal penning episodes was achieved through refuse accumulation associated with occupation (Shahack-Gross et al., 2005). Microdebris included wood ash, bone, charcoal, ceramics, constructional materials and abundant phytoliths. There have been similar findings at other Middle Eastern sites (Stoops & Nijs, 1986; Boivin & French, 1997/1998; Matthews et al., 1998; Gur-Arieh et al., 2014). Mounds constructed of soil include medieval mottes in Europe (e.g., Gebhardt & Langohr, 1999) and Mississippian Culture mounds in the United States (Sherwood, 2006). Nevertheless, mound-raising may involve both the use of coherent soil slabs and simply dumping of soil, regolith and rock fragments in so-called basket loads. In these, the various soil materials become mixed as soil clasts and form a heterogeneous layer. In this case, the once-open voids are commonly filled with dusty to impure clay that is

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associated with textural intercalations whose texture is governed by the original grain size of the soil, all because of slaking of disturbed soil. This phenomenon was also noted by Romans and Robertson (1983) for barrow constructions and is similar to disturbed tree-throw hollow fills and to soils transported, deposited and modified under freeze-thaw conditions (Mu¨cher, 1974; Macphail & Goldberg 1990; Macphail, 1999). The presence of the aforementioned pedofeatures, which are anomalous for a natural soil profile, may help distinguish between buried natural soils and groundraising that uses soil. Lastly, construction layers employing dumped soils may develop reddish colours in the field (Sherwood, 2006), because iron-stained clay is concentrated in clay infillings and fine intercalations, but it remains conjectural whether such red layers were constructed intentionally (Courty et al., 1989).

2.3

Floors, Surfaces and Walls

Floors have been constructed from various coherent loamy and clayey deposits that are local to a site, producing so-called clay floors (Rentzel, 2011). In coastal sandy areas, estuarine silty clay (Macphail, 1990) and till (Nørnberg & Courty, 1985) have been used to produce stable living surfaces. Local wetland sediments, often rich in phytoliths and diatoms, have been imported to produce daub and clay floors, for example, in Iron Age ˚ ker ga˚rd, and Migration Period (c. AD 0 to 600) houses at Jarlsberg, Vestfold and A Hedmark, Norway (Viklund et al., 2013; McGraw, personal communication); at the ˚ ker ga˚rd, byre areas (see Section 3.2.1) had earth floors unusually well-preserved site of A strengthened by being pebbled, while relict periglacial silt loams were favoured for hearth constructions. The artificiality of such floors is inferred from the occasional inclusion of anthropogenic materials (e.g., charcoal, pottery, burned daub, bone and, even rarely, coprolites) and various iron, iron phosphate and calcium phosphate staining of their surfaces and voids (hypocoatings). The construction of clay floors was not the case, however, in most Viking and medieval sites in Iceland (e.g., 12th-century Reykholt Farm in Borgarfjo¨ro˜ur, Iceland; Sveinbjarnardo´ttir et al., 2007). In north-west Europe, brickearth and loess soils were employed to produce floor slabs of natural material (Figs. 2 and 3). This included soil from both the pale A2 horizon and the more clay-rich Bt and Ctk horizon; the latter may include relict calcitic pedofeatures. Such types of deposits are specifically built and represent truly constructed floors. They are, however, often found alternating with dark coloured, charcoal-rich occupation accumulations, which are not constructed floors per se but represent beaten or trampled material and are unlikely to have been deposited on purpose (Fig. 2). Constructed clay floors thus mark the renewal of a clean living surface (see also Matthews et al., 1996). At Reykholt Farm, this was achieved by creating thin clay plastered floors that alternate with occupation deposits (Sveinbjarnardo´ttir et al., 2007). The difference between a constructed floor and overlying beaten floor deposits can be noted in the field and in thin section as a knife-sharp,

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FIGURE 2 Earth floors. Medieval floor and beaten floor sequence (Spitalfields Hospital, London, sample M499, layer 4850 over layer 4900; Museum of London Archaeological Service; Goldberg & Macphail, 2006). The brickearth floor is a prepared mixture composed of brickearth, ‘soil’ and anthropogenic inclusions, with an apparent ‘white soil’ plastered surface employing iron-poor soil (probable A2 horizon); a beaten floor has formed over this by trampling; the brickearth floor is affected by some iron phosphate staining compared with the beaten floor which is rich in various forms of phosphate (e.g., fine bone and coprolites), organic matter and burned material (ashes, charcoal, burned soil) (NL, scale bar length 1 cm).

horizontal boundary, the occupation floor deposits showing fine sorting and horizontal orientation of materials such as bone, eggshell and mollusc shell fragments. The degree of lamination reflects the degree of humidity, the level of protection from the elements and the nature of any floor coverings (Ge´ et al., 1993; Cammas, 1994; Courty et al., 1994; Cammas et al., 1996; Matthews et al., 1997; Macphail et al., 2007). It has to be kept in mind, however, that floors were often swept, and sweepings were dumped elsewhere, and that ‘occupation’ deposits in fact result from ‘disuse’, squatter occupation or building decay (Macphail, 1994; Cowan, 2003; Galinie´, personal communication; Sheldon, personal communication). Such deposits do not show the fine laminations as found in

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B

C

FIGURE 3 Floors and adobe. Middle Neolithic earth- and rock-based building material, and ground-raising and construction materials (Middle Neolithic e Yangshao, Huizui, Henan Province, China). (A) Adobe ground-raising deposits (AGR) and plant-tempered adobe preparation surface (APS), both composed of local loess, covered by a floor constructed from tufa (tufa floor layer, TFL), covered by burned daub debris (BDD) (NL, scale bar length 2 cm). (B) Plant-tempered mud-plastered loess forming a floor preparation surface (arrows indicate void pseudomorphs after plant remains); the dense character of the groundmass is due to soil slaking caused by the mud-plastering process; patches of microfabric with high interference colours result from the formation of textural intercalations caused by internal slaking creating a striated b-fabric (XPL, scale bar length 1 mm). (C) Mud brick (Iron Age, Tell Yoqneam, Israel). Earth-based, dark brown mud brick with typical large voids with elongated angular shapes that are moulds of plant remains (PPL, scale bar length 1 mm).

beaten floors and are also more likely to be markedly contaminated by latrine waste, for example. The use of brickearth slabs to form walls within timber-framed buildings in Roman London has long been documented, and one intact fallen lime plaster-coated brickearth wall at 1st to 2nd century Southwark, London, sealed a short-lived disuse occupation deposit within an abandoned building shell that included, in addition to brickearth fragments, biomixed coarse and fine charcoal, bone, eggshell, amorphous organic matter and earthworm excrements (Cowan, 2003).

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Constructed floors may show iron oxide and iron phosphate staining and associated vivianite formation (see Karkanas & Goldberg, 2018) because of contamination from liquid waste, but overall they are less phosphate-rich than the beaten occupation accumulations. In addition, the surface of soil slabs in constructed floors is sometimes ‘mud plastered’, which is recognisable because of the evidence of slaking, which concentrates infillings with clay and intercalations in the uppermost few millimetres. This plastering may have been carried out to produce a dark red colour, caused by the development of clay void coatings and intercalations where the iron content of the soil is concentrated in the clay, or simply to seal a surface. This type of surface plastering has been noted at various sites (Boivin, 1999; Matthews et al., 2000; Macphail & Crowther, 2007) (Figs. 2 to 4); it has been argued, however, that fresh plaster was not necessarily always employed and that fragmented material may have been reused (Karkanas & Van de Moortel, 2014). Sealing is also recognised for floors constructed from calcareous till (Chalky Boulder Clay) at the 12th-century wheat barn, Cressing Temple, Essex, and at Iron Age Uppa˚kra, Scania, Sweden, which has similar geology (Macphail, 1995; Macphail et al., 2017a). Roman sunken floor buildings on chalk had their subterranean floors sealed with rammed fine chalk (Bennett et al., 2008). This practice is expedient because minor recrystallisation of calcite produces a semicemented material without the use of lime. In the United Kingdom, chalky ‘clunch’ walls and a chalky daub called ‘cob’ have similar characteristics. Floors were produced from brickearth, loess or till, which was often mixed with dung and other organic matter, including a plant temper such as straw (Karkanas, 2007). Through time, this organic matter decomposed, which leaves straight-sided voids pseudomorphic after straw (see Figs. 3 to 5). In some cases, phytoliths or iron and manganese oxide stains can be observed.

FIGURE 4 Burned daub floor (Roman house, No. 1 Poultry, City of London). Cross section through charred straw, with associated blackened humic staining and shrinkage voids (PPL, scale bar length 1 mm).

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B

FIGURE 5 Clay oven. Experimental oven constructed from Cretaceous red chalk (a local material employed in both Roman and Saxon times at West Heslerton, North Yorkshire, UK) and straw. (A) Layered structure, with a lower rubefied layer which has been most affected by heating, a straw-tempered middle layer and an upper surfacesealing mud layer (NL, scale bar length 1 cm). (B) Detail of the straw-tempered layer, showing blackened and charred straw, as well as shrinkage voids (PPL, scale bar length 1 mm).

Building stone in constructions is outside the remit of this chapter, but when studying constructions, an understanding of petrographic features of rocks that were or could have been employed is obviously very useful. For example, Jurassic Oolitic limestone can be found within hydraulic mortar used in the construction of an aqueduct near Basel, Switzerland (Rentzel, 1998) (see Fig. 21), while Maya lime plaster floors were tempered with local siliceous and sponge-spicule-rich mud flat sediments at Marco Gonzalez, Belize, during the Early Classic to Late Classic (c. AD 250 to 700/760; Graham et al., 2017; Macphail et al., 2017b) (Fig. 8A). The study of Roman building materials at Pessinus, Turkey, included the characterisation of local limestone types and marble as background to the investigation of lime plasters (Stoops, 1984a). Soil micromorphology had to be employed to identify the use of quarried slabs of tufa as flooring material, which in the field had been mistakenly identified as manufactured lime plaster floors (Macphail & Crowther, 2007) (Fig. 3). In contrast to plaster, tufa is characterised by the blackened plant remains (Babel, 1975; Stoops, 2003) and by calcitic pseudomorphs after plant tissues (see Karkanas, 2007). Phytolith layers from oxidised stabling deposits, for example, have also been misidentified in the field as plaster floors because of their pale colour (Shahack-Gross et al., 2005; Albert et al., 2008). The fills of sunken feature houses (e.g., Grubenha¨user) (Simpson et al., 1999; Milek, 2006; Wegener, 2009) can be modelled as having a soil fabric dominated by mesofauna excrements. In First Nation Canadian pit houses, anthropogenic materials including burned residues and coprolites are strongly mixed with earth-based and organic roofing debris by biological activity (Goldberg, 2000). This soil material can be either natural when the locality had been little altered by human activity or strongly anthropogenic. In the latter case, when settlements are long-established, evidence includes very abundant fine charcoal and rubefied mineral grains, abundant and articulated phytoliths, rare to occasional dung fragments and residues, and coprolites (Macphail et al., 2006b;

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Macphail, 2016a). In sunken feature house fills, local silt or sandy loam hand-formed into loom weights during early medieval times can be found as anomalous fragments of clay or silt loam materials (Macphail et al., 2006b). Loom weights can be common inclusions in archaeological fills associated with textile manufacturing. Mud brick, daub and adobe are similar earth-based building materials, which can be recognised from their composition, void patterns (if plant-tempered), inclusions (charcoal, dung, soil and sediment clasts) and, in some instances, the presence of textural and fabric pedofeatures or the occurrence of slaking if material is puddled or poured as a slurry into a mould, all of which can produce fabric heterogeneity from the employment of different soil materials and clayey intercalations merging into dusty clay void coatings where the voids are closed vughs or even vesicles (Levine et al., 2004; Goldberg & Macphail, 2006; Nodarou et al., 2008). When burned, these building materials preserve well, but they can be modified by weathering and reworked by colluvial transport (Goldberg, 1979) or totally transformed into soil through pedogenic processes (Goldberg, 1979; Macphail, 1994; Friesem et al., 2014a, 2014b). Burned variants of the above-listed constructional materials often occur at archaeological sites (Kruger, 2015; Forget & Shahack-Gross, 2016). The chief characteristics caused by heating are blackening of once-humic areas (iron oxides are not strongly transformed because of localised reducing conditions or are incompletely burned) and reddening caused by the formation of hematite (oxidising conditions), best seen in OIL (Goldberg & Macphail, 2006). Another effect of heating is the formation of a crack structure, because of the loss of water by clay (Courty et al., 1989) (Figs. 4 and 5). In the case of experimental daub made from loess, a major change in macroscopic colour from hue 7.5 YR to 5 YR took place between 400 and 500 C (Dammers & Joergensen, 1996). The inclusion of organic materials produced grey, reduced areas. Examples from an experimental straw-tempered oven and a Roman straw-tempered brickearth floor demonstrate how the straw becomes charred and the surrounding matrix shrinks through desiccation (Figs. 5 and 6). Clearly, the temperature affecting the floor was not

A

B

FIGURE 6 Hearth ash (Brean Down, Somerset, UK). In situ Bronze Age hearth within a round house. (A) Charcoal (c), ash (a) and burned bone (b) layers (PPL, scale bar length 0.5 mm). (B) Same field in XPL, illustrating high interference colours of calcite ash and modified birefringence of charred bone.

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excessive, as the major loss of organic matter in daub tempered by barley straw occurs between 200 and 300 C, with most organic material lost at 400 C (Dammers & Joergensen, 1996; see also Berna et al., 2007) (see Fig. 8B). At an early Neolithic site in Hungary, burned daub and burned plant-tempered daub constitute the most abundant evidence of constructions (Crowther, 2003, 2007; Macphail, 2003; Carneiro & Mateiciucova´, 2007). Soil micromorphological and mineralogical analyses at Tel Dor reveal that surfaces constructed from local calcareous sandstone were heated to produce a plaster floor (Shahack-Gross et al., 2005); heated plaster floors also characterised salt working levels at Late Classic Marco Gonzalez, Belize (Graham et al., 2017) (Fig. 8A).

2.4

Organic Floor Coverings

Floors and surfaces were sometimes covered with organic materials, which include turfs (Milek, 2006), mats and, more conjecturally, skins (Courty, 2001; Courty et al., 1994; Macphail et al., 1997). These organic floor coverings occur in Palaeolithic to medieval sediments, where ‘mats’ are characterised by thin, millimetre-thick layers of articulated phytoliths of Poaceae (grasses, reeds, straw) or they consist of identifiable plant remains, as at the Middle Stone Age of Sibudu Cave, KwaZulu-Natal, South Africa (Goldberg et al., 2009b). As found in Viking Age Trondheim and Oslo, Norway, under waterlogged conditions, centimetre-thick accumulations of organic coverings can be preserved on wooden floors, which under more strongly oxidising conditions may be in part preserved by iron phosphate impregnation (Macphail & Goldberg, 2017, pp. 377-379). In certain cases, these surfaces are associated with horizontal planar voids and iron and phosphate staining of the associated fine sediments as a result of trampling and of the mat acting as a hydraulic barrier, a phenomenon that also affects many clay floors and other floor make-ups (Matthews et al., 1996; Macphail et al., 1997; Macphail, 2005; Milek, 2006). Voids between the woven mat fibres can be partially filled with thin organo-mineral excrements from both the buried soil and overlying trampled soil (Macphail & Cruise, 2001). Beaten floor deposits (Ge´ et al., 1993; Cammas, 1994; Cammas et al., 1996; Milek, 1997; Macphail et al., 2004, 2006b, 2007; Sveinbjarnardo´ttir et al., 2007) (see Fig. 2) that can form on floors and matted surfaces have been already briefly mentioned in Section 2.3. Some of the anthropogenic materials within them, and which help characterise both in situ use of space and local activities, will be dealt with in the following text (e.g., domestic/hearth, stabling and industrial waste origins) (Cammas, 1994; Matthews et al., 1997; Banerjea et al., 2015).

3. Waste Materials Human occupation produces concentrations of all kinds of organic and inorganic waste (Courty et al., 1989, 1994; Goldberg & Macphail, 2006). These are found in middens, structures, or pits or simply concentrated around hunter-gatherer campsites. Additionally, these occurrences are the focus of scavenging by animals that leave their own waste.

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Inorganic Waste Materials

In addition to fuel residues (charcoal, clinker from coal, and charred peat, turf and dung) that generally can be found in and around occupation areas (Carter, 1998; Milek, 2005; Milek & French, 2007), inorganic waste materials were commonly employed in northern regions for soil amelioration, as for example the manured soils at Papa Stour, Shetland (Adderley et al., 2006). Hearths normally produce calcitic ash (Wattez & Courty, 1987; Courty et al., 1989; Shahack-Gross et al., 2004a, 2014), often in layers alternating with wood charcoal beds, the latter recording incomplete combustion, whereby the layered structure can be preserved in conditions of rapid burial (Fig. 7) (Macphail, 1990). In the last case, ethnoarchaeological observations of different Hadza hearth types in Tanzania revealed that differently functioning hearths were both disturbed and weathered by natural agencies, with people reusing hearths and scooping out ashes, for example; there have also been experiments to replicate Middle Palaeolithic hearth fires (Mallol et al., 2007, 2013). The presence of vesicular porous char in hearths indicates the burning of flesh or animal fat (Goldberg et al., 2009b; Villagran et al., 2013; Mentzer, 2014). Although often converted by weathering into general poorly diagnostic micritic calcite masses (Courty et al., 1989; Gur-Arieh et al., 2014; Shahack-Gross et al., 2014), some wood ash can, on occasion, be preserved as coarse lozenge-shaped crystals, which are pseudomorphs after calcium oxalate crystals that formed inside the wood cells (Franceschi & Horner, 1980; Brochier, 1983; Wattez & Courty, 1987; Karkanas et al., 2007; Mentzer, 2014; PoloDı´az et al., 2016), and termed POCC, an acronym of ‘pseudomorphose d’oxalate de calcium en calcite’ (Brochier & Thinon, 2003). If temperatures exceed 600 C, these pseudomorphs are converted into lime (CaO), which in turn is transformed to undiagnostic micritic calcite by hydration and carbonation (Brochier & Thinon, 2003). Bark and leaves produce greater amounts of calcium oxalates than wood (Franceschi & Horner, 1980; Brochier & Thinon, 2003), and calcium oxalates are abundant where ashes are

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FIGURE 7 Grass ash (Early Iron Age site, Maiden Castle ditch, Dorchester, UK). (A) Burned Poaceae remains from cereal processing and dung, rich in phytoliths, including articulated phytolith sheets; note humic staining which may indicate the presence of burned dung (PPL, scale bar length 100 mm). (B) Same field in XPL, showing scattered and clustered fine calcite ash, small calcite spherulites suggesting dung may be a component, and cereal material (charred seeds).

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derived mainly from stabling of animals foddered on woodland ‘leaf hay’. Ash from grass, as well as from cereal processing and dung, produces finer crystals and an abundance of associated phytoliths, some of which may have melted to produce vesicular slags (Macphail & Cruise, 2001; Milek, 2005; Weiner, 2010) that can be enriched in phosphate (Fig. 7). These slags are autofluorescent in blue light, possibly because of a carbonatesubstituted hydroxylapatite component (Weiner, 2010; Karkanas, personal communication). Burned phytoliths have a refractive index greater than 1.440 (Albert et al., 2008). Some siliceous burned monocotyledonous plant pseudomorphs are spherical in shape, or oblate when more strongly heated; these partially melted siliceous plant remains have seemingly vesicular voids which are simply relicts of natural vessels within stems (Macphail et al., 2012). Ash from cereal processing is often mixed with charred chaff (Macphail, 1991, 2000). Weathering, reuse of hearths and disturbance by digging scavengers can produce isolated and granular aggregates of ash. Some hearths produce burned bone (Karkanas et al., 2007), which appears to be more resistant to acid soil weathering than unburned bone, possibly because of alteration of the phosphate into a more stable, but unknown form than apatite (Berna, personal communication). Burned stones from hearths or burned rock mounds sometimes have residual ash cemented to their surfaces as a testimony to their hearth origin. Clearly, the accurate micromorphological and mineralogical identification of burned bone and hearth deposits in early human sites is crucial (Goldberg et al., 2001; Karkanas et al., 2007; Mentzer, 2014). Burned food waste typically includes charred bone (rubefied, with lowered interference colours and lowered autofluorescence), calcined bone (whitish, optically isotropic and non-autofluorescent under blue light), burned eggshell (Fig. 9), large burned mollusc shells and charred cereal grains or seeds. Burned soil and constructional materials that only show reddening may be of domestic hearth origin. Strongly burned soil showing a loss of birefringence of the aluminium-silicate minerals (as in some potsherds) and quartz (and melted ‘dewdrop’shaped and bubbled vesicular quartz, with a loss of birefringence mirroring loss of crystalline structure) is more typical of industrial hearths when very high temperatures are reached (>850 C, up to 1713 C) (Courty et al., 1989; Gue´lat et al., 1998; Berna et al., 2007; see also Mathieu & Stoops, 1972; Angelucci, 2008) (Fig. 8B). Experiments employing a combination of open fires and furnaces with bellows showed kaolinite was lost and smectite suffered dehydroxylation and partial vitrification at 500-700 C, quartz was transformed at 1000-1200 C to a glaze-like (glassy) phase and to cristobalite at 1300 C (Berna et al., 2007). Salt working typically employs low-temperature fires to boil brine, sometimes using salt-rich coastal sediments. Hearth surfaces (Fig. 8A) and briquetage become rubefied because of this processing, but development of a hightemperature glazed surface has also been observed for briquetage used as bellows plates (Macphail et al., 2012). The ‘redhills’ of Essex, United Kingdom, and salt working levels at Marco Gonzalez have developed from the rapid accumulation of burned tidal flat sediments used to extract brine (Graham et al., 2017; Macphail et al., 2017b) (Fig. 8A).

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FIGURE 8 Industrial activities (salt-working hearth floor at Marco Gonzalez, Belize, and furnace waste from Åmot øvre, Stokke, Vestfold, Norway). (A) Flatbed scan of Late Classic Maya lime plaster floor (PF). This shows a sequence of a lime floor constructed over debris which includes pottery fragments (P; probable Coconut Walk ware used in salt working). The lime floor surface is weakly rubefied from the use of small fires to heat brine; ash and other fuel waste (charcoal) occurs above, where there is a dump of limestone (L) and burned sediments (BS) used in brine extraction (Graham et al., 2017; Macphail et al., 2017b) (NL, scale bar length is 1 cm). (B) Vesicular, fused fine sands and partially melted sands (quartz and feldspars which have lost or partially lost their birefringence), with small area of silicate glass formation (G) as identified by micro-FTIR. Iron staining suggests an association with iron-working (Viklund et al., 2013; F. Berna, personal communication) (PPL, scale bar length 1 mm).

FIGURE 9 Burned eggshell (early medieval London Guildhall, City of London, UK), showing horizontal alignment, typical edge crystals and blackening produced by burning (PPL, scale bar length 0.5 mm).

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Different activities can be implied from inclusions of leather and non-ferrous metal materials (craftwork), bark and wood (wood working or construction), exotic igneous rock fragments (grindstones) and exotic limestone and sandstone associated with lime plasters and mortar (construction). Thus, predominantly domestic and industrial spaces and areas within structures that are employed to house domesticated animals can be differentiated on the basis of the associated archaeological materials (Cammas et al., 1996; Macphail et al., 1997, 2004, 2007; Shahack-Gross et al., 2004a, 2005; Milek, 2006; Banerjea et al., 2015).

3.2

Organic Waste Materials

Animal and human faecal waste is a source of phosphate and organic matter. Although bat guano (Shahack-Gross et al., 2004b) and bone-rich bird guano remains are typical of some natural cave sediments (Macphail & Goldberg, 1999; Goldberg & Macphail, 2012), scavenging by birds can be similarly recorded from occupation areas and cremationand excarnation-associated deposits where bodies were exposed (Macphail & Crowther, 2008; Macphail & Goldberg, 2017, pp. 487-489; see also Angelucci 2008). Dung of herbivores (cattle, sheep, goats, horses) can be ubiquitous: in structures, fields and trackways where finely fragmented residues can occur alongside phosphateenriched inwashed clays and neoformed iron, calcium or phosphate nodules (Engelmark & Linderholm, 2008; Macphail, 2011; Macphail et al., 2017a); manured fields may include articulated phytoliths that can be identified and counted in thin section (Devos et al., 2013). Herbivore dung can normally be differentiated from that of omnivores (pigs, humans) and carnivores (dogs, hyenas) (Courty et al., 1989, 1994; Horwitz & Goldberg, 1989; Macphail, 2000; Goldberg et al., 2009a). Oxidised dung remains, especially from ovicaprids, may be rich in ‘faecal spherulites’, formed of calcite or monohydrocalcite (Brochier, 1983; Brochier et al., 1992; Canti, 1999; Shahack-Gross et al., 2004a, 2004b; Shahack-Gross, 2011). However, not all calcite spherulites (<20 mm) found in archaeological sediments are necessarily of faecal origin. Calcite spherulites have been experimentally obtained from recrystallisation of Tamarix aphylla wood ash (Shahack-Gross & Finkelstein, 2008). Clearly, the simple presence of calcite spherulites is inconclusive evidence for stabling or animal stocking. In tell sites, individual spherulite occurrences can be ubiquitous, and only where they are concentrated in high numbers do they have significance. Even in this case, it is their organisation within the soil microfabric and relationship with other constituents that allow any proper interpretation of their occurrence (in situ and microstratified stabling layers with identifiable dung remains, dumps, background herbivore presence, trampled concentrations) (Binder et al., 1993; Macphail et al., 1997, 2017a; Matthews et al., 1997; Sordoillet, 1997, 2009; Boschian & Montagnari-Kokelji, 2000; Shahack-Gross et al., 2003, 2004a, 2004b; Angelucci et al., 2009).

3.2.1 Herbivore Dung Herbivore dung dominated by Poaceae remains (grasses and cereals) is not universal, and both ovicaprids and cattle were stalled or overwintered on a diet of woodland ‘leaf hay’

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during prehistory in Swiss lake village sites (e.g., fir) and in Mediterranean rock shelters (e.g., oak). In the latter case, ashed stabling deposits record layered deposits of dark brown twig wood ‘stable floor’ layers and grey layers of ashed dung and fodder that were first fully identified at the Arene Candide (Italy) and Pendimoun (France) caves (Courty et al., 1991; Binder et al., 1993; Macphail & Goldberg, 1995). Subsequent investigations of numerous Neolithic animal management sites (e.g., France, Italy, Spain and Switzerland) have confirmed these findings (Brochier, 1996; Macphail et al., 1997; Sordoillet, 1997; Boschian & Montagnari-Kokelji, 2000; Akeret & Rentzel, 2001; Angelucci et al., 2009; PoloDı´az et al., 2016). Calcium oxalates, their pseudomorphs and burned (blackened) residues are abundant, while phytoliths are rare. Charred twig wood, leaves and bark, and calcite ash pseudomorphic after the original wood cell structure are also visible, alongside ashed herbivore coprolites. It can also be noted that dung residues can contribute to grass ash (see Fig. 7); in some cases, recognisable fragments of ashed dung pellets can be preserved. Herbivore dung is dominated by poorly digested plant tissues and small amounts of amorphous organic matter and organic phosphate staining that is normally pale to dark brown under PPL and blackish brown under OIL. Cattle often produce dung with microlayered ‘long’ plant fragments, whereas sheep/goats produce rounded pellets with stained margins and a convoluted structure formed from ‘short’ plant fragments reflecting how these animals differently process a grass and cereal diet; herbivores are efficient at digesting cellulose and hence this material suffers a loss of birefringence as part of the humification process (Courty et al., 1994; Akeret & Rentzell, 2001; Macphail et al., 2004). Experimental and ethnoarchaeological stabling and animal compounds from the United Kingdom and Africa have demonstrated these differences (Macphail & Goldberg, 1995; Shahack-Gross et al., 2003, 2008; Shahack-Gross, 2011). Stabling features include thin layers of phytolith-dominated dung residues resulting from stabling within buildings, which had at first been misidentified as plaster layers before a thin section study was carried out (Shahack-Gross et al., 2005). Compacted dung enriched in liquid animal waste can form phosphate-enriched layers and even cemented crusts (Heathcote, 2002), and in this process carbonates are partially transformed to Ca-phosphates (Shahack-Gross et al., 2003) on the floors of stables (e.g., as carbonatesubstituted hydroxylapatite; Macphail et al., 2004, 2006b). These crusts have a finely laminated character because of the horizontal compaction of grass stems (and cereal remains) and the long, articulated phytoliths that characterise these plant remains; as humification continues, these phytoliths become more visible but in such crusts remain articulated as >1-mm-size lengths (Macphail & Cruise, 2001). In some cases, they occur within a finely dotted yellowish brown cement that is autofluorescent under blue light when hydroxylapatite is present. How these stabling features preserve relates to the type of dung, whether it was burned or not, and overall environmental conditions and ageing (Figs. 10 and 11). At Atzmaut rock shelter in the Negev Desert (Rosen et al., 2005; Macphail & Crowther, 2008), recent goat dung is dominated by fragmented pellets and plant fragments, with organic material being more dominant than phosphate, whereas compressed, aged and

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FIGURE 10 Recent goat dung stabling level (Atzmaut rock shelter, Mizpe Ramon, Negev Desert, Israel), showing plant tissue remains from fragmented goat pellets and dark brown humified amorphous organic matter (PPL, scale bar length 1 mm).

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FIGURE 11 Bronze Age stabling accumulation of compacted goat pellets, from the same locality as the material in Figure 10. (A) Layered deposit mainly composed of humified amorphous organic matter, phytoliths and humified monocotyledonous plant fragments (optically isotropic or very low birefringence), and with some scattered silt and fine sand mineral grains (PPL, scale bar length 1 mm). (B) Detail showing a concentration of small calcitic faecal spherulites that are only partially masked by amorphous organic matter and are responsible for the overall optical anisotropy of the layer (XPL, scale bar length 100 mm).

oxidised Bronze Age stable floor layers are phosphate enriched, and interference colours are moderately high because faecal spherulites are no longer obscured by organic matter. Matthews et al. (1997) report interbedded lenses of dung pellet fragments and digested plant remains from stables. At 1st millennium BC Lattes, southern France, pure, bedded dung of horses or cattle is believed to have accumulated under humid exterior conditions, whereas dung bedded with quartz grains accumulated in dry conditions (Cammas, 1994).

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Both layered dung from cattle and fragments of ovicaprid dung are reported from a Swiss Gallo-Roman stable at Brig Gliss VS, but here the stabling deposits were accidentally burned in situ (Gue´lat et al., 1998). This is not an uncommon occurrence where dung layers become generally strongly ‘blackened’ and ‘browned’ (see also Macphail et al., 2004). A burning temperature of c. 900 C was estimated from the presence of vitrified phytoliths at Brig Gliss VS (Gue´lat et al., 1998). Dung fragments can also be preserved by iron, and iron and manganese mineralisation in which poor but still recognisable pseudomorphs are formed in intermittently waterlogged conditions (Macphail et al., 1998) or they can be completely preserved by anaerobic conditions (e.g., Akeret & Rentzel, 2001; Ismail-Meyer & Rentzel, 2004). Phosphate-cemented dung or stable floor fragments preserve well and occur in middens and manured soils; dung itself has been employed as constructional material, for example, to line wattle walls. In an experimental manured plot in northern Sweden, characterised by a high proportion of organic phosphate, recognisable herbivore manure occurs as fragments (4 mm) of compact humified layered plant fragments within an amorphous organic matter matrix that resembles stable floor crust material (Macphail et al., 2004, 2006b; Goldberg & Macphail, 2006). Similar fragments occur in experimentally manured fields at Butser Ancient Farm and in Iron Age to Viking Period cultivated soils in Denmark, Norway and Sweden, and these still retain high proportions of their phosphate as organic phosphate from these dung inputs; dung fragments also occur in a well fill associated with one a mixed farming system (Engelmark & Linderholm, 1996; Goldberg & Macphail, 2006; Viklund et al., 2013). Such manuring raised the level of biological activity compared with the natural soil, usually manifesting itself as an increase in the amount and size of organic and organo-mineral excrements compared with a previous dominance of extremely thin organic excrements. In present-day northern Norway, when virgin and cultivated soils were treated with cattle slurry, the cultivated sandy soil developed an increase in fine material content (Sveistrup et al., 1995). The surface of the virgin soil became compacted, however, and examples of slurry coatings and panning were observed for all soils. In archaeological soils, such modern slurry coatings need to be identified as contamination (Viklund et al., 2013). On the other hand, phosphatic void coatings due to seepage from cess pits can be penecontemporaneous (Macphail, 2016b; Macphail & Goldberg, 2017, pp. 458-461).

3.2.2 Pig Dung Pig dung may contain both large amounts of plant tissues and amorphous organic matter and organic phosphate, along with calcium oxalates from partially digested plant material and ingested silt (Courty et al., 1989, 1994). The latter is sometimes also present in herbivore dung and found intercalated in laminated stabling crusts. Pigs fed on a husk-rich cereal feed at ‘West Stow Anglo-Saxon Village’, Suffolk, United Kingdom,

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produced a moderately phosphate-enriched trampled surface soil in their enclosure where cereal husks occur as horizontally oriented inclusions; the immediately underlying soil contains neoformed amorphous Fe-P-Ca nodules (Macphail & Crowther, 2011). The pig pasture at West Stow was churned by pigs forming heterogeneous soils; such mixing and microcolluviation was also reported from the ‘medieval’ farm at Lann-Gouh, Brittany, France (Gebhardt, 1995). Faecal spherulites have also been found in fresh wild boar and pig excrements (Brochier, 1996; Canti, 1999) (Figs. 12 and 13).

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FIGURE 12 Fresh pig dung (wild boar) (Northern Apennines, Italy). (A) Excrement likely containing root fragments and biogenic mineral material (PPL, scale bar length 100 mm). (B) Same field in XPL, showing relict food material, such as root fragments, as birefringent cellulose; biogenic crystals occur as single calcitic faecal spherulites and as aggregates of probable calcium oxalates.

FIGURE 13 Pig dung (coprolite) (Late Bronze Age/Early Iron Age Potterne, Wiltshire, UK) essentially composed of amorphous organic matter and organic phosphate and containing soil diatoms (arrow) such as reasonably wellpreserved Hantzschia amphioxys and Navicula mutica (aquatic species indicating drinking from ponds; Nigel Cameron, University College London, personal communication) (PPL, scale bar length 50 mm).

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3.2.3 Dog Coprolites Dogs and other canids scavenge and produce coprolites that can contain coarse bone fragments, including fish bone and fins (Matsui et al., 1996), as well as quartz silt that becomes embedded in a presumed hydroxylapatite cement (Fig. 14). This cement is commonly a fine dotted blackish grey (PPL) material, with undifferentiated b-fabric, white in OIL and strongly autofluorescent under blue light (Courty et al., 1989; Macphail, 2000). As reported for Ca-phosphate-cemented hyena coprolites, it is believed that trapped intestinal gas in dog coprolites can produce vesicles and that ingested fur or wool leaves narrow curved voids (Horwitz & Goldberg, 1989; Lewis, 1997; Larkin et al., 2000; Macphail & Goldberg, 2012). Where dogs scavenged sheep carcasses as evidenced by bone gnawing, there are wool-size curved voids in the coprolites; pollen analysis on both thin sections and prepared pollen samples shows that much cereal material was eaten, possibly from scavenged human faeces (Scaife, 2000; Cruise, personal communication). It can be noted here that when bone is digested by dogs (and by humans and birds, for example) it can become leached, losing birefringence and autofluorescence; when embedded in guano and/or cess, however, the edges of bone fragments may become phosphatised and display high autofluorescence (Courty et al., 1989; Macphail & Goldberg, 1999; Macphail & Crowther, 2008).

FIGURE 14 Dog coprolite (Middle Saxon West Heslerton, North Yorkshire) showing typical dark greyish groundmass, with numerous curved voids pseudomorphic after fur or wool (dogs gnawed sheep carcasses at this site) (PPL, scale bar length 1 mm).

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3.2.4 Human Coprolites Human coprolites, as identified through nematode egg analysis (Kenward & Hall, 1995), may have a presumed hydroxylapatite matrix similar to that of dog coprolites but differ by normally being a yellowish colour (Courty et al., 1989; Goldberg et al., 2009a; Macphail, 2016b). They also often have a different content reflecting their omnivorous diet (both bone and plant remains occur), and they do not typically contain much clastic mineral material or coarse bone. As such, they are far more likely to include plant food fragments, such as legume testa and cereal material, including articulated phytolith-rich bran; thin sections of mummified intestinal contents found solely leguminous seed cases in some Chilean mummies (Macphail, 2016b) (Figs. 15 and 16). Here the cellulose of the seed cases is still birefringent, unlike the humified cellulose found in herbivore dung e herbivores being better adapted to digest cellulose compared with humans. Body stains and probable intestinal remains that autofluoresce in blue light have been found in an Iron Age grave in Norway where bands of vivianite can also mirror wooden coffin remains; both amorphous yellow (Ca-P) and reddish brown (Fe-Ca-P) body stains occur in the pelvic area of a warrior found in a boat grave near the Gokstad Mound (Macphail et al., 2013; Viklund et al., 2013). Latrines contain mineralised cess, again with a probable carbonate hydroxylapatite composition (Fig. 17). Such waste can contain embedded cereal material of dietary origin, as well as sphagnum moss that was most likely used as toilet paper. Fine fragments of this type of latrine waste often occur as a regular component of Roman and Medieval beaten floors in the United Kingdom. Dumped toilet waste and seepage from

FIGURE 15 Human coprolite (Viking Age Coppergate site, York), identification confirmed by nematode egg studies (Andrew Jones, York Trust). Detail of legume testa as a food remain within the apatite groundmass; the hook-like tissue cells making up the testa are diagnostic (Ann Butler, Institute of Archaeology, University College London, personal communication) (PPL, scale bar length 25 mm).

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FIGURE 16 Human coprolite (Middle Saxon settlement site Maiden Lane, London, UK), identification confirmed by parasite egg study (Claire de Rouffignac, Museum of London Archaeological Service, personal communication). The sample exhibits voids from trapped gas; dark black and reddish brown colours relate to iron and manganese oxide staining associated with unidentifiable but likely food plant traces embedded within the coprolite (PPL, scale bar length 1 mm).

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FIGURE 17 Lower fill of a cess pit (Norman cess pit, Monkton, Kent, UK). (A) Cess preserved as amorphous yellow material (probably calcium phosphate); mineralised cess (formed in aerobic conditions) is yellow, mainly optically isotropic although some birefringent materials can also be present in addition to probable hydroxylapatite (PPL, scale bar length 1 mm). (B) Same field in BLF, showing strong autofluorescence of the material.

cess pits, like modern day sewage sludge, produces yellow amorphous infillings and nodules of Fe-Ca-phosphates, sometimes with neoformation of vivianite (Macphail, 2016b; see Karkanas & Goldberg, 2018). It is common to find phosphate-embedded charcoal, both in latrine waste and in fields, implying that such material e which may also include embedded ash e was used as a ‘night soil’ fertiliser worldwide (Henning & Macphail, 2004; Goldberg & Macphail, 2006).

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4. Manufactured Materials The study of manufactured materials in archaeology is commonly thought of as being a specialist field. However, archaeological sites often include fragments of pottery and other ceramic materials (e.g., roof tiles, pipes, kilns). These materials need to be distinguished routinely from natural rocks or debris, which provides clues to local industries (see Berna et al., 2007). In complex societies, the types of materials (e.g., lime and gypsum plasters), and how they have been applied (e.g., single coat vs several layers), can be indicative of the status of buildings or rooms and the associated social standing of the former occupants. The petrology of pottery has been well studied (Rice, 1987), and handmade pottery can be distinguished from wheel-made ceramics by, at low magnification comparing air-void patterns, general coarse particle distribution and general aspects of the groundmass, and at high magnification examining the morphology and arrangement of clay domains formed by the packing of clay- and siltsize particles and overall birefringence fabrics (Courty et al., 1989; Roux & Courty, 1998; Quinn, 2013). Neolithic pottery has commonly been manufactured using organic tempers and local soils and sediments (Spataro, 2002).

4.1

Stone Tools

Stone tools are probably the earliest worked material to be found in archaeological sites. Flint or chert is composed of microcrystalline quartz or chalcedony and is a common example of a natural rock material that flakes well to produce sharp-edged tools (Angelucci, 2010). Flint, which can occur in a variety of colours and lustres in the field, is normally colourless in thin section (Fig. 18), unless stained by iron oxides. It may occur as an exotic rock because of human importation. Other silicate-dominated rocks used for tools are quartzite and various volcanic rocks, such as rhyolites, basalts, or obsidian.

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FIGURE 18 Manufactured stone tools (Lower Palaeolithic Boxgrove, West Sussex, UK). (A) Edge of colourless flint flake of anthropogenic origin, present in once-humic (now replaced by iron oxides) silty colluvium (PPL, scale bar length 1 mm). (B) Same field in XPL, showing low-order interference colours of microcrystalline quartz.

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When burned, colourless flint can become greyish brown (PPL) (white in OIL), and cracks appear along with so-called pot-lidding of small hemispherical spalls that lack striking platforms (Andrefsky, 1998). Heating can also cause a change in texture resulting in a reduction in crystal size. Fire-altered cherts can be found with other heat-altered rocks in middens and burned rock mounds (e.g., Goldberg & Guy, 1996).

4.2

Plasters and Mortars

Lime- and gypsum-based plasters and mortar have been studied worldwide. Plaster floors are formed from layers of grey to greyish brown (PPL) micritic lime plaster that often includes unburned limestone components (Goren & Goldberg, 1991) and fine organic fragments, sometimes along with fine burned mineral material and charcoal (Matthews et al., 1996) (Fig. 19). Plaster is normally whitish in OIL. A comparison between experimental lime plaster and natural calcareous sediments (Karkanas, 2007) indicates that the most promising features for identifying lime are transitional textures of partially carbonised slaked lime (composed of poorly crystallised portlandite and mixtures of cryptocrystalline calcite) that can be observed in the lime lumps and the binding matrix cement. Well-formed calcitic groundmass and shrinkage cracks are also possible indicators of lime plasters (Karkanas, 2007). Fine charcoal and reddened burned mineral inclusions may also suggest the presence of burned lime. Chalk, limestone and, in coastal areas where limestone is unavailable, shells have been burned to produce lime. For example, burned conch shell, of presumed limemaking origin, occurs in some New World Maya lime plasters on the island site of

FIGURE 19 Manufactured lime plaster (Pre-Pottery Neolithic Yiftah El, Israel). Layers of very fine and sometime pure lime plaster, applied as cover of a floor; note very thin layers of finer plaster that cover a coarser layer in the middle and traces of fine organic matter from the manufacturing and mixing process (PPL, scale bar length 0.5 mm).

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Marco Gonzalez, Belize (Macphail et al., 2017a; Graham et al., 2017); tempering material included high proportions of unburned shell, pottery fragments and siliceous marine tidal flat sediments, which had sometimes been burned. In Roman structures, a typical coarse/fine ratio for a plaster, or matrix within a coarse tempered mortar, is 60/40 (Stoops, 1984b; Macphail, 2003). Plaster often shows very thin layers associated with the plastering process, carried out, for example, on brickearth walls or over mortared wall surfaces, ahead of painting (Pye, 2000/2001) (Fig. 20). Babylonian red floors had, in some cases, a 20-mm-thick supporting ‘white’ layer composed of a microcrystalline calcite cement and a temper of well-sorted (1-3 mm) coarse sand to fine gravel, composed of quartz and feldspar, below a c. 6-mm-thick red surface layer. The latter is characterised by a similar temper, but the matrix is formed from microcrystalline calcite and hematite dust (Stoops & Stoops, 1994). Multiple plaster floors are considered as evidence of both ritual activity and level of social status, but contemporary floors in different domestic structures may show a varying composition, which was probably determined by the individual households (Karkanas & Efstratiou, 2009).

B

A

C

FIGURE 20 Roman wall lime plaster (The House of Amaranthus, Pompeii). (A) Reference section through fine wall plaster layers, including an inner fine plaster (a, with sand-size temper derived from volcanic material) and an outer pure lime wall surface plaster (b, with unburned calcite inclusions from the manufacturing process) (XPL, scale bar length 1 mm). (B) Opaque painted surface (p), covering the pure lime wall plaster surface, with inclusions of coarse-grained calcite (c) and micritic carbonate aggregates (mc) (PPL, scale bar length 0.5 mm). (C) Detail of paint layer, which from SEM-EDS seems to be iron-oxide based (OIL, scale bar length 100 mm).

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Fragments of plaster and mortar are common in the Roman to early Medieval dark earth of European cities and as weathering features in Maya sites of the New World (Macphail, 1994; Cammas, 2004; Straulino et al., 2013; Borderie et al., 2014; Graham et al., 2017) and within fills of tells (Matthews et al., 1996; Boivin & French, 1997/1998). In Europe, mortar may contain brick fragments and volcanic rock clasts, which may imply that they are hydraulic mortars because these are a source of neoformed aluminium silicates that cement this mortar type rather than simply being cemented by neoformed calcite. Similarly, it has been suggested that the Maya may also have used volcanic materials to produce pozzolanic plasters in mainland Belize (Villasen˜or & Graham, 2010). However, the identification of neoformed aluminium silicates in hydraulic mortar requires X-ray diffraction analyses (e.g., Rentzel, 1998). In addition, relicts of calcium of aluminium hydrates are amorphous, featureless and optically isotropic in thin section (St John et al., 1998).

4.3

Metal Working

Hammerscale, iron slag and silt to coarse sand-size vesicular iron spheroids are evidence of industrial activities and may occur alongside fuel ash waste and high-temperature melted and fused soil; in the last, minerals may be altered, with quartz and feldspar, for example, losing their birefringence (Viklund et al., 2013, see Section 3.1) (see Fig. 8B). Opaque in transmitted light, hammerscale has a layered metallic edge, visible in OIL and SEM-BSE images, comprising an outer hematite layer and inner magnetite and wu¨stite (FeO) layers in some examples (Kresten & Hja¨rthner-Holdar, 2001). Iron slag is very dark (PPL) and has a typical vesicular void pattern. It includes optically isotropic areas, dark materials showing dendritic patterns (e.g., wu¨stite) and iron silicates such as fayalite
2þ Fe 2 ðSiO4 Þ ; such patterns are strongly visible in SEM-BSE images (Kresten & Hja¨rthner-Holdar, 2001; Macphail, 2003). Iron slag and hammerscale also often occur as poorly preserved nodular material because of postdepositional gleying. Thin, angular iron flakes also occur in kitchen debris from the use of iron pots, and these can also be differentiated from iron-pan fragments by a metallic lustre under OIL, as confirmed by EDS testing (Macphail et al., 2016). Non-ferrous metal and glass working also produce metal droplets (‘prills’) and ‘glassy’ furnace slags (Merkel, personal communication). Quantitative SEM-EDS and microprobe analyses are often necessary alongside optical microscopy. For example, petrographic analysis of a Bronze Age pit fill showed colourless to grey cassiterite aggregates (SnO2), with characteristic high relief, high birefringence and extinction parallel to cleavage (Macphail & Crowther, 2008); blue-green aggregates in Roman London were identified as copper and tin working waste and associated corrosion products. Presumed bell-making activities in medieval Magdeburg also produced blue-green stained bronze droplets (Goldberg & Macphail, 2006). A Cu-Pb alloy was found in trampled floor spreads at a medieval hospital, alongside strongly burned sediments (Fig. 21). In thin section, it was found to be a mainly opaque

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A

B

C

FIGURE 21 Metal droplet from non-ferrous metal working, within ash-rich deposits (medieval Spitalfields Hospital, sample M605B, London; Museum of London Archaeological Service). (A) Metal droplet including some crystals of unknown composition; note high-order interference colours of the ash (XPL, scale bar length 1 mm). (B) Backscattered electron image of same field; the corrosion rim is less bright than the unaltered interior because it still includes heavier elements (Pb). (C) Element map for the same field (rotated), showing that the metal droplet is composed of a Pb-Cu alloy (centre) with areas of pure Cu and Pb, and the corrosion rim consists of Cu- and Caphases, indicating that corrosion products are mixed into the Ca-dominated ash occupation deposit.

material (PPL), with elsewhere generally very low interference colours, but with bright yellow and reddish colours in OIL. On the other hand, it was possible with the help of specialist archaeometallurgists to identify probable corroding lead fragments in Roman ashy dumps where pure lead is opaque, with a blackish lustre under OIL (Borderie et al., 2014). A coating of ‘red’ lead oxide is also opaque but reddish under OIL, while corrosion staining of the surrounding calcitic ashes also produced grey (PPL), high-order interference colours and white (OIL) lead carbonate.

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5. Conclusions An archaeological material is any matter that has been utilised or produced by humans or that formed as a by-product of their activities. Soil micromorphology, using optical microscopy and associated techniques, is one of the best methods for characterising and identifying archaeological materials, especially when they occur as microscopic fragments at archaeological sites. In fact, although bulk and microfossil studies can provide useful supporting information, often the data from these techniques can only really be properly understood when soil micromorphology is available. For example, some phytoliths can be understood better when unfragmented in thin section, while the exact nature of phosphate-enrichment in archaeological contexts can often be identified, as produced by in situ bone, ash or dung concentrations, or which only result from secondary phosphate accumulations. In addition, the identification of such microartefacts is an essential new tool for characterising archaeological contexts. Archaeological materials include natural mineral and organic materials that have been used in their raw state (dung, flint, turf, tufa, wood) or as little-transformed material (earth-floors and walls, adobe and mud brick, leather), as well as fully manufactured products (iron, lime plaster, metal alloys). Other archaeological matter include waste from occupation, such as dung and mineralised coprolites from domestic animals, human waste (coprolites, cess), food (bone, cereal grains, eggshell, mollusc shell) and hearth remains (ash, charcoal, briquetage). Sites also produce strongly burned residual remains, fused ash, slag, vitrified ceramics, burned bone and flint, for example. As research continues, the number of identified archaeological materials continues to increase and permits an ever deeper understanding of different cultures and human activities through time. Clearly, it is also required to comprehend the nature of the archaeological context and type of deposit in which these materials occur. Such strategies can provide a fuller understanding of past human activities operating at the site.

Acknowledgements The authors thank the anonymous referees, Panagiotis Karkanas and the editors for their comments and gratefully acknowledge the specialists who supplied data supporting and complementing soil micromorphological identifications and interpretations, namely Francesco Berna, Jan Bill, Marie-Agne`s Courty, John Crowther, Gill Cruise, Tom Gregory, Takis Karkanas, Johan Linderholm, John Merkel, Kevin Reeves, Thilo Rehren, Ruth Shahack-Gross, Karin Viklund, Luc Vrydaghs, and the many members of the Archaeological Soil Micromorphology Working Group who have contributed so much to this discipline over the last 25 years. Because of a lack of space most of the supporting chemical and microfossil data for this chapter have had to be omitted. The authors also gratefully acknowledge longterm funding by various North American, British and European government agencies, funding bodies and archaeological companies. R.I. Macphail specifically thanks The Leverhulme Trust for support with this project.

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