Recent advances in the analytical and experimental
study of mineralised textiles

Loïc Bertrand, Clémence Iacconi, Ineke Joosten, Caroline Tokarski, Ilaria

Degano, Jiayi Li, Laura Hendriks, Étienne Anheim, Sasja van der

Vaart-Verschoof, Karina Grömer

► To cite this version:

Loïc Bertrand, Clémence Iacconi, Ineke Joosten, Caroline Tokarski, Ilaria Degano, et al. Recent advances in the analytical and experimental study of mineralised textiles. Journal of Cultural Heritage, 2025, 75, pp.122-138. 10.1016/j.culher.2025.07.005. hal-05187910

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Review

Recent advances in the analytical and experimental study of
mineralised textiles

<figure><img src="image_3.png" /></figure>

Loïc Bertrand<sup>a,*</sup>, Clémence Iacconi<sup>a,†</sup>, Ineke Joosten<sup>b</sup>, Caroline Tokarski<sup>c</sup>, Ilaria Degano<sup>d</sup>, Jiayi Li<sup>e</sup>, Laura Hendriks<sup>f</sup>, Étienne Anheim<sup>g</sup>, Sasja van der Vaart-Verschoof<sup>h</sup>, Karina Grömer<sup>i,*</sup>

ARTICLE INFO

Article history:

Received 17 December 2024

Accepted 4 July 2025

Keywords:

Archaeological textiles

Analytical chemistry

Mineralisation

Taphonomy

Imaging

A B S T R A C T

Mineralised textiles — altered remnants of organic textiles preserved by the diffusion of metallic cations from nearby artefacts or the environment — have gradually emerged as an essential source of information on the production and use of textiles in prehistoric and antique societies, as well as on their implication on the economy, technological developments and trade. In many contexts, they are the only evidence of productions known either indirectly through tools or not at all. In this review, we highlight the contri- bution of analytical methods in recent years to their study, an evolution that began with the emerging use of optical and then electron microscopy in the 1960s and 1970s. In particular, we describe the most recent period, which has seen (i) the widespread use of digital optical microscopy in laboratories and museums, (ii) the adoption of approaches aimed at characterising molecular signatures, even for highly altered textiles, and (iii) the development of micro-imaging methods, particularly using synchrotron ra- diation or laser sources. We are finding that these methods are making an increasing contribution to the field of archaeology. We outline possible prospects for the research and documentation of mineralised textiles and the possible impact of imaging methods on museum displays.

© 2025 The Author(s). Published by Elsevier Masson SAS. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/)

1. Introduction

Textile making is one of the earliest craft technologies devel-
oped by humans in time [1]. In general, the term “textile tech-
nology” covers a range of techniques such as weaving, plaiting,
matting, twining, etc. In Europe, the development of textile tech-
nology (spinning and weaving, including patterning techniques) in
the Prehistory and Protohistory is closely linked to the “Neolithic
revolution”, which took place about 8000–7000 years ago, when
people settled down, began to cultivate plants (especially flax), do-

mesticate animals (e.g. sheep and goat) and use fibres from both
as raw material for textile production [e.g. [1–4]]. Textiles played
an essential role in ancient societies in many functions that go far
beyond clothing, soft furnishings, and domestic use, such as com-
munication, transportation, manufacturing of boats, or storage of
goods [5,6]. Their production was a much more widespread and
ubiquitous practice in most societies in the past than it is today.
Textiles played a crucial role in the development of past societies
and their economies, both in terms of production and consump-
tion [7], and as such were important for social developments. We
are even able to detect reuse and recycling, indicators of a very
careful use of resources. Textiles were very time-consuming to pro-
duce and, as such a highly valued resource, worth repairing and
reusing.

<footnote><sup>a</sup> Université Paris-Saclay, ENS Paris-Saclay, CNRS, PPSM, 91190 Gif-sur-Yvette, France</footnote>

<footnote><sup>b</sup> Cultural Heritage Agency of the Netherlands, PO Box 1600, Amersfoort, 3800 BP, Netherlands</footnote>

<footnote><sup>c</sup> Institut de Chimie et Biologie des Membranes et des Nano-objets, UMR 5248, Bordeaux Proteome, Université de Bordeaux, CNRS, Bordeaux INP, 33076 Bordeaux, France</footnote>

<footnote><sup>d</sup> Dipartimento di Chimica e Chimica Industriale, Università di Pisa, via Moruzzi 13, Pisa, 56124, Italy</footnote>

<footnote><sup>e</sup> School of Cultural Heritage, Northwest University, Xi'an, 710127, PR China</footnote>

<footnote><sup>f</sup>HEIA School of Engineering and Architecture of Fribourg, HES-SO University of Applied Sciences and Arts Western Switzerland, Pérolles 80, Fribourg, 1700, Switzerland</footnote>

<footnote><sup>g</sup> Centre de recherche en histoire, École des hautes études en sciences sociales, 54 Bd Raspail, 75006 Paris, France</footnote>

<footnote><sup>h</sup> National Museum of Antiquities Leiden, Rapenburg 28, Leiden, 2311 EW, Netherlands</footnote>

<footnote><sup>i</sup> Natural History Museum Vienna, Department of Prehistory, Burgring 7, A-1010, Vienna, Austria</footnote>

<footnote>* Corresponding authors.</footnote>

<footnote>E-mail addresses: loic.bertrand@ens-paris-saclay.fr (L. Bertrand),
karina.groemer@nhm.at (K. Grömer).</footnote>
<figure><img src="image_4.png" /><figcaption>**Fig. 1.** Three of the levels of description of archaeological textiles. (a) Weave (2/1 twill z/s) of a mineralised textile on a copper-based substrate from the Saint-Sulpice site in Barberery (5th century BCE, Aube, France). (b) Section of two threads of a textile mineralised by copper, observed under a metallographic microscope, from the La Ronce site (5th century BCE, Loiret, France). The colour green is characteristic of the formation (here negative mineralisation) of basic copper(II) carbonates close to the pure phase of malachite Cu₂CO₃(OH)₂. (c) Ancient wool fibre from the site of Lattes 1 (5th century BCE, Bouches-du-Rhône, France) observed under a scanning electron microscope. The fractured end of the fibre shows the histological macrofibrillar structure of the wool fibre, emerging from its cuticular sheath. Figure credit: Loïc Bertrand and Christophe Moulherat.</figcaption></figure>

Archaeological textile remains provide unique evidence of craftsmanship and associated practices [e.g. [1,5,8–10]]. Although textiles from archaeological contexts can be preserved in other conditions (ice, salt, waterlogged, deserts, etc.; [1]), textile traces preserved in detail in the corrosion crust of metal artefacts are an essential source of evidence in many contexts (e.g. Fig. 1). Scholars have documented since at least the early modern period the discovery of ‘mineralised’ textiles [11]. Mineralised textiles are mostly

found in funerary contexts or associated with hoards, more rarely in settlements. They have provided essential information to describe the first known attestation of cotton at the Neolithic site of Mehrgarh in current Pakistan (6th mill. BCE, Mooulherat et al. [12]). The fibre remains, identified as cotton (Gossypium sp.), were analysed using scanning electron and optical microscopy. Their characteristic morphology was observed in a microsample taken from within a heavily corroded, millimetre-sized annular copper bead. In China, archaeologists have unearthed highly mineralised silk fibres wrapped around the surface of iron artefacts at the Majiayuan cemetery (马家墩墓地), dating from the end of the Warring States period (403–221 BCE) in Gansu Province [13]. The crown of Empress Xiao of Emperor Yang of the Sui Dynasty is made of copper alloy, with several hollow hairpins attached to its sides, inside which distinct remains of mineralised cotton fibres were discovered [14]. Shamir et al. [15] discussed mineralised textile finds from a hoard at the Hellenistic Tell Iżabbā (Beth She'an, Nysa-Scythopolis) in Israel, which is dated from the time of Alexander II Zabinas (129/128–124/123 BCE). The linen cloth in which the copper-alloy coins of the hoard were wrapped was analysed in terms of material, origin and technical details [15]. Recent developments in analytical studies based on mineralised textiles have focused on four main objectives: (i) identifying the function of textiles, (ii) documenting the production techniques, (iii) understanding preservation mechanisms, and (iv) improving conservation procedures (Fig. 2).

Textiles, along with wood, leather, fur, hair, and skin, are among the organic materials that can be preserved in an interpretable form through biologically controlled or induced mineralisation in archaeological contexts. Various terms, such as fossilised, petrified, pseudomorphous, or mineralised, have been used to describe these remains [11]. Here, we use the term ‘mineralisation’. Textile mineralisation involves the progressive corrosion of a metal artefact (or occasionally diffusion from an environmental source of metal cations), and the transport of these cations to the textile fibres [16,17]. Various metals, including copper, iron and silver (and their alloys), as well as silicon and calcium, can contribute to different forms of mineralisation. While most of the literature focuses on copper, iron, and silicon mineralisation, there is growing interest in textiles preserved by other cations. This includes faint textile imprints identified in soils, which have been underrepresented in past studies, such as the very interesting calcium carbonate mineralisations described in Unruh [18] and Schuurman [19]. Toxic metal cations, in particular copper or heavy metals, inhibit the short-term enzymatic lysis and oxidation of the protein or cellulosic macromolecules textiles are principally made of, even in contexts that favour degradation of tissues such as burials [20,21]. A longer-term transformation leads to the degradation of (part of) the organic content of the material, with parallel authigenic nucleation and growth of neoformed mineral phases, or to the permineralisation of the tissues (cellulose-based textiles), a mechanism similar to wood petrifaction. The mechanisms of mineralisation have not yet been fully elucidated at the micrometric to nanometric scale, although proteomics and new spectral imaging approaches have recently provided important insights [22,23].

Since the 1960s and the pioneering work of Leo Biek, micro-analytical methods have played an essential role in the description of archaeological textiles with a view to their technical analysis, understanding the small-scale mineralisation processes themselves, and/or attempting to identify the treatments the textiles have undergone, particularly mordanting and dyeing ([24–27]; see also the historical perspective in Chave et al. [11]). Over and above the different research objectives, the differences in the molecular composition of the textiles and the archaeological context, similar analytical approaches have been used to study mineralised textiles. The aim of this contribution is to review progress made in
<figure><img src="image_5.png" /><figcaption>**Fig. 2.** Main aims of published studies on mineralised archaeological textiles. Figure credit: Loïc Bertrand.</figcaption></figure>

the development of analytical approaches relevant to the study of the physico-chemistry of mineralised textiles, with an emphasis on the most promising recent approaches — from the design of analytical sequences and fieldwork to new advances in morphological, molecular and elemental analyses, as well as experimental archaeology approaches. This contribution also emphasises that, from a long-term historical perspective, recent developments in the study of mineralised textiles not only represent a quantitative increase in our knowledge of these ancient objects. They bring with them a qualitative dimension. The new analytical approaches that are emerging to study mineralised textiles are based both on technical and instrumental advances and on historical and methodological reflection, enabling a better understanding of materials that are inherently heterogeneous, altered and of uncertain representativeness. In particular, traditional divisions, such as those between spectroscopy and imaging or between organic and inorganic chemistry, which structure academic research and training, are challenged.

## 2. Design of analytical sequences

Any proper analysis of mineralised textiles starts with observation in the field (see Field work and preparatory work). The analytical procedure then follows a sequence that combines structured stages with the bricolage inherent in archaeological research and excavation at the level of the sample, as new information is observed during the course of the study. Analytical methods can be invasive or non-invasive, depending on whether a sample needs to be taken, and destructive or non-destructive, depending on whether the analyte is destroyed to an extent that prevents subsequent analysis (Fig. 3).

In most cases, non-invasive analysis should take precedence over invasive analysis, and non-destructive analysis should take precedence over destructive analysis. However, a balance has to be struck between the research objectives and the potential results, on the one hand, and the desire to preserve the discovery intact for posterity, on the other. Intermediate designations have therefore emerged (micro-destructiveness, minimal invasiveness), in which small samples are taken and/or sacrificed in order to obtain results that cannot be obtained otherwise today (molecular identification, dye analysis and dating, in particular).

For invasive analysis, on a small scale, the preparation of mineralised textile samples poses rigorous constraints because the samples contain both hard parts (e.g. metal support, carbonate minerals, sediment grains such as quartz particles) and soft parts. They

form assemblages that are therefore often brittle and prone to cracking during handling, cutting, surfacing, polishing or sample positioning during experiments. In addition, they are often 'thick' in the sense that great penetration lengths and depth of field are required to study threads that are interwoven and only partially contained within a porous and heterogeneous corrosion crust, often containing soil minerals, fractions of the metallic substrate and other materials. Samples of mineralised textiles also exhibit significant internal differences in electron density, while being for the most part non-conductive. As a consequence, non-invasive methods such as digital microscopy and X-ray microtomography are particularly well suited to their study. However, while the analysis of whole textile fragments does not require sample preparation, certain measures must be taken when the focus is on fibre identification.

Isolating the fibres and mounting them individually for analysis (e.g. for X-ray nanotomography or X-ray scattering / diffraction) presents an intermediate level of difficulty in terms of preparation, but can still be challenging when the samples are particularly brittle. They need to be mounted vertically on a metal support and held in place with glue, a step which must be carried out under a stereomicroscope because of the small size of the fibres (a few hundred microns at maximum) and the risk of contamination. On the other hand, methods requiring very clean, flat surfaces or sections, such as electron microscopy, secondary ion mass spectrometry (SIMS), X-ray fluorescence (XRF), Raman spectroscopy or mid-infrared spectroscopy (particularly in ATR mode), are difficult to apply, except on crushed fragments. In this type of situation, traditional approaches to studying heritage samples have been reported, such as embedding the sample in a block of organic resin and polishing it carefully. An additional difficulty arises when the resin is a source of excessive chemical contamination, for example when looking for specific organic molecular signatures, for specific emissions (photoluminescence), or when resins induce excessive heating during their exothermic solidification. Some authors have therefore resorted to less usual, specific methods, such as embedding samples in supercooling sulphur [17]. Another source of difficulty may lie in cutting the embedded samples to obtain cross-sections (e.g. with an ultramicrotome or a wire saw). If the focus is on studying preservation mechanism, cutting with water should be avoided, making this step much more complex. Different imaging and spectroscopy techniques can give different results depending on sample preparation and instrumental parameters. An interesting example of bias analysis was provided by Iacconi et al. [28] in comparing different means of technical analysis of highly
<figure><img src="image_6.png" /><figcaption>**Fig. 3.** Schematic representation of invasiveness versus destructiveness of analytical methods. Figure credit: Loïc Bertrand.</figcaption></figure>

mineralised textiles (see below). Addressing these variations and developing strategies for cross-validation of data would strengthen archaeological interpretation.

The methods presented in this review all require specific expertise that must be combined with the instruments listed. Only optical microscopy and, to a lesser extent, scanning electron microscopy and FT-IR spectroscopy can be considered to be available to such an extent that they can be used at almost all levels of research. Dedicated services are available for several techniques, particularly carbon-14 dating. Micro-computed X-ray tomography, mass-spectrometry for dye analysis and proteomics are also available through services, but they require significant adaptation of the methods in order to provide relevant results for archaeological textiles, which only a handful of companies, if any, can do today.

### 3. Field and preparatory work

A systematic approach and standardised protocols are important for recording data on mineralised textiles found at archaeological sites. The context in which the textiles were found needs to be recorded, e.g. short but precise details of the grave finds, the metal artefacts to which the textiles are attached, etc. It is crucial to describe the location of the artefacts; for example, in a grave, it is essential to record the (micro)context of the textiles in relation to a body or other artefacts. As in forensics, it is essential to document the nature of the soil through appropriate observations and specific sampling in order to understand the mineralisation processes involved and their implications for any taphonomic and/or geochemical assessment. Information on the archaeological context serves as an important orientation and contextualisation of the textile finds.

On objects with mineralised textiles, sometimes multiple layers of one fabric or even different fabrics might be attached to each other. In this case, the micro-stratigraphy is of importance to describe the different textile layers. For the micro-stratigraphy and mapping of different textiles on one object, the system by Nowak-Böck and Voß [29] is useful. Important analytical steps in the examination of an archaeological textile are fibre analysis (and dye analysis, when it can be performed), determination of the thread construction, of the weaving technique and of sewing details. Techn

nical data that are recorded from a fabric are weave, thread density, thread thickness, twist of thread, S or Z twist, various seams and hems, as well as embellishments, if applicable. The condition of archaeological textiles is usually very fragmentary, so that a very careful approach is required for their conservation, treatment and museum presentation. Manuals for the excavation of archaeological textiles were published some years ago [30]. While excavating, one must always stay aware of the possible presence of textiles, as early recognition in the field is often key to their survival. When encountered, textiles — and any artefacts to which they may adher — should be recorded in detail, block-lifted when possible and transported to the laboratory for full excavation, bearing in mind that any contact or movement can be detrimental to the find. The textiles should be kept in a controlled environment.

During the conservation process, close contact between the archaeologist and conservator is crucial, so that the objectives of both can be met. For example, recording of the micro-stratigraphy by the conservator may allow the archaeologist to reconstruct the layering and possibly better inform the function of textiles. In addition, certain technical or chemical analyses that the archaeologist may wish to carry out to answer specific research questions can only be performed prior to certain conservation treatments used by the conservator to conserve the material. The application of a conservation treatment to a metal object, such as organic coatings, may complicate subsequent analysis or identification of the textile by making electron microscopy observation difficult or even impossible; it is a surface technique and the electrons cannot penetrate the organic layer covering the surface of the fibres. Dye analysis, molecular identification and dating can also be affected. Although CT scanning is still possible, it is strongly recommended that the textile be analysed prior to conservation treatment.

### 4. Morphological analysis

#### 4.1. External morphology

The technical analysis of an archaeological textile consists in the determination of its main morphometric characteristics in order to obtain information on the different stages of its production and use (Fig. 4; see also Masurel [31]). As mineralised textiles are often in-
<figure><img src="image_7.png" /><figcaption>Fig. 4. The chaîne opératoire of textile production (for woven textiles). Figure credit: K. and P. Grömer, NHM Vienna.</figcaption></figure>

separable from the remains of metal support, samples are gener-
ally first examined by observing their surface at different magni-
fications with the naked eye, under a binocular microscope or an
optical microscope, in several steps [28,32–36].

1. Overall description of the textile: this includes a brief descrip-
tion of the fabric with colour, pattern, raw material, size, shape
and number of fragments belonging to the fabric complex, as
well as the reference system (e.g. in the case of textiles cor-
roded to metal objects) and position on the object;

2. Technical information on the weaving technique: weave type, special features of the weave, fabric density, selvedges;

3. Technical information on the thread material: thread construc-
tion (spun or spliced, single or plied thread), thread thickness,
direction and angle of twist of both thread systems. The way
of identification of warp and weft is to be mentioned (e.g.
selvedges), otherwise the terms "thread system 1" and "thread
system 2" are to be used;

4. Other observation: patterns, seams and hems, details on weav-
ing faults, fulling, use-wear, marks of repair, secondary use,
knots.

The main quantitative parameters usually determined are the
weave type, the thread count (number of threads per centimetre),
the diameters of the warp and weft threads and their direction and
tightness of twist. This set of morphometric parameters is highly
revealing of cultural practices. This operation is now routinely car-
ried out in the laboratory.

From 1965 onwards, commercial scanning electron microscopes
(SEM) were introduced, which gradually came to equip physics lab-
oratories from the 1970s and 1980s, before being extended to other
disciplines. SEM made it possible to overcome the limitations of

the depth of field of optical microscopy and began to be used con-
ventionally to observe the level of morphological preservation of
mineralised fibres in the 1980s, in particular with the pioneering
work of Janaway [25] and, later, Rast-Eicher et al. [36,37]. When
a variable pressure SEM is used, whole artefacts can be examined
in the sample chamber without the need for a conductive coating.
Microscopic details were also collected for archaeological informa-
tion, in particular the search for an abundance of isolated fibres
around the edges of the threads, a clue whether the textiles had
been felted. SEM has been widely used to confirm the nature of
the fibres by observing characteristic features in addition to opti-
cal microscopy (linen kink bands, cuticle scales, size and shape of
lumens, structure of the medulla), and characterising their dimen-
sions (Fig. 5A,B).

In addition, the condition and (microbacterial) degradation of
the fibres can be indicative of the burial environment and of the
past use of the textile. Next to positive and negative imprints in
metal corrosion, Davis and Harris [38] described the presence of
ephemeral textile traces (Fig. 5C). These are comparable to cord-
impressed ceramics: when there are no textile fibre remnants, a
textile structure can still be indicated by the offset pattern of petal-
shaped rows. Remnant and ghost textile surfaces can reveal much
information, as even small traces of textiles can preserve evidence
of fibre, thread, weave structure and position in relation to metal
objects. Caricola et al. [40] identified the presence of mineralised
fur residues on a Bronze Age metal dagger and connected this in-
formation to traces of use wear on the metal surface.

Since the 2010s, digital (optical) microscopy has considerably
improved the observation of sample surfaces of mineralised tex-
tiles in laboratories, conservation studios or museums, at limited
costs. Digital reconstruction makes it possible to overcome limi-
<figure><img src="image_8.png" /><figcaption>**Fig. 5.** (A,B) Scanning electron microscope images of negative imprints of scales of mineralised sheep wool fibres (white) in a conglomerate of mineralised material, almost the entire cuticle of the fibre is lost and the scales are mineralised (Bronze Age, Chagar Bazar, Syria; A) and of negative imprints of silk fibres in chalk, the edge of the triangular fibre is clearly visible (Augustinerkirche, Konstanz, Austria; B). Figure credits: Rast-Eicher [37]. (C) SEM backscattered electron image of characteristic petal shape features preserved on the remnant textile surface of a Viking penannular brooch hoop: [1] silver metal is represented by the lightest patches, [2] copper corrosion products overlying the silver are in medium grey shades [3]. Negative casts of fibres within the corrosion lead to grey areas with a textured surface. [4] Partially preserved organic fibres in the corrosion layers appear as dark grey areas. Figure credits: Davis and Harris [38]. (D) SEM images of mineral preserved bast fibres. The surface of the fibres clearly shows the thick nodes characteristic for bast fibres (a,b). The hexagonal and oval cross-sections are visible (c,d). Figure credits: Martín Seijo et al. [39].</figcaption></figure>

tations in depth of field and to reconstruct large sample surfaces [28].

## 4.2. Cross-sectional morphology

Cross-sections of mineralised fibres may be visible in the form of holes whose shape is characteristic of the type of fibre, i.e. silk

has a triangular shape, while wool fibres are round and the shape of the cuticle scales might have left negative imprints in the imprint formed by corrosion products. Distinguishing between flax and hemp is difficult when they have been replaced by minerals, even under SEM [1]. Martín Seijo et al. [39] identified mineralised fibres from a medieval castle in Galicia as flax according to their diameter (10–20 µm), their hexagonal and oval cross-sections (Fig. 5D).

## 4.3. Virtual internal morphology

Of recent development in the field, synchrotron micro-computed X-ray tomography (SR-μCT) can lead to virtual 3D reconstructions (the electron density) of textile fragments as small as millimetres in size [28]. The method allows for the technical characterisation of features hidden deep within samples, for example when their surface is soiled or abraded, or when samples are multilayered [10,28,41]. Iacconi et al. [28] reported a segmentation approach based on the local orientation of textile fibres to aid determining standard technical parameters in 3D, from the scale of the fibres to the thread and weave types. This was reported on superimposed Iron Age mineralised textiles from the Creney-le-Paradis site (late 6th–5th c. BCE, Aube, France; Fig. 6). This approach made it possible to identify at least 16 different fabrics, including three solely with μCT, which would otherwise have remained undetected, helping to confirm the site's elite status [10].

Laboratory μCT instruments have also been successfully used to examine mineralised textiles, such as in the study carried out by Suomela et al. [42] on two mineralised textiles from inhumation graves at Ravattula Ristimäk (1150s–1220s, Kaarina, Finland), which enabled the identification of their materials, i.e. flax and nettle, as well as their weave and thread structure, including their direction of twist. Karjalainen et al. [43] used laboratory μCT to study two tablet-woven textiles pieces and a tabby from a late medieval inhumation burial at Valmarinniemi (late 13th–early 14th centuries, Keminmaa, Finland), preserved thanks to the spiral metal tubes to which they were attached. This has enabled the structural components of the thread and the original weaving pattern to be segmented. In addition, the authors used nanoscale CT imaging (also denominated nano-CT or nCT) for the identification of the fibres making up the tabby found on a bronze ring. They were able to determine that it was cotton.

Another advantage of μCT is the ability to retrieve simultaneously morphological and chemical information. For example, semi-quantitative SR-μCT studies of mineralised textiles associated with copper-based artefacts from the Nausharo site (3rd–2nd millennium BCE, southern Mesopotamia, present-day Iraq) has enabled a precise, non-invasive 3D mapping of internal and external mineral phases providing essential clues to the long-term preservation process [44]. μCT and nano-CT can be used at sub-micrometre resolutions to determine the morphological characteristics of individual mineralised fibres. A quantitative estimate of in situ local attenuation coefficients can be obtained at this length scale to help disambiguate compound identification and describe the taphonomic process [17,44].

The advantages of CT imaging have been highlighted by other authors, including Lipkin et al. [45], who mentioned certain limitations of the technique when studying archaeological mineralised textiles. In particular, attempts to visualise the finest details of samples with the highest resolution require higher doses and longer exposure time, which can have impact [46–48]. This highlights the need to take into account the entire analytical process when examining mineralised textiles, for example by carrying out infrared analyses before X-ray and electron irradiation of samples. In addition, Iacconi et al. [28] pointed out biases that need to be taken into account in order to make the results obtained more
<figure><img src="image_9.png" /><figcaption>**Fig. 6.** X-ray microtomographic reconstructions of a mineralised textile fragment on a bronze-based substrate from the Creney-le-Paradis Early Iron Age site (6th–5th century BCE, Aube, France). The grey level intensity is represented from white to black, corresponding to high and low X-ray attenuation respectively, which is indicative of the electron density of the compounds present. (a) 3D reconstruction of the textile fragment and its virtual section (b). (c) Virtual section of the whole sample in the XZ plane. The different layers of textiles, three in total, are observed on one side of the remains of the copper-based substrate. (d) Virtual sections in the XY plane of layers: L1 (d); L2 (e) and L3 (f). The latter two are inaccessible by non-invasive examination. All scale bars: 1 mm, except in (c), 0.5 mm. Figure credit: Clémence Iacconi.</figcaption></figure>

robust and intercomparable. These biases include the effect of an abraded surface of the fabric on the determination of the thickness of textile layers, the effect of mineralisation which artefactually increases fibre diameter, and perception biases that tend to lead analysts to define morphometric parameters on the basis of the most compact threads.

# 5. Molecular analysis

## 5.1. Dye identification

The assessment of the colour of archaeological textiles is paramount in understanding their original aspect, function, and to evaluate the technological skills of the culture that produced them. This task is far from easy, as organic dyes are minor components of archaeological textiles samples, and consist of complex mixtures of naturally occurring organic molecules extracted from plants, insects or shellfish [49].

The nature and characteristics of natural dyes have been widely reviewed in the literature, as the main strategies applied for their identification in archaeological and historical textiles [50]. Indeed, the visual assessment of the colour of an archaeological textile is often impaired by contamination from the soil. In addition, when studying wool textiles, it can be difficult to determine whether the fibres are coloured because of the natural pigmentation or if the colour is caused by a natural dyestuff, since naturally coloured wool fibres contain both (brown) eumelanin and (red and yellow) pheomelanin [51].

All these aspects make the commonly used non-destructive spectroscopic techniques (hyperspectral imaging, FORS, MRI, Fourier-transform infrared spectroscopy and Raman spectroscopy) only partially informative, but very useful to guide selective sampling for further analysis [52,53], which entail micro-destructive techniques based on the chromatographic separation of the single analytes. The quantification and identification can then be performed via spectrophotometric or mass spectrometric detection.

Even when chromatographic techniques are applied, analysis can be complicated by the presence of high amounts of inorganic salts, as in the case of mineralised textiles, that might alter the extraction yields of sample treatments, increase background noise in the separation and detection especially by mass spectrometric techniques. This adds to the difficulties arising from the possible degradation of the dye species in time, which may have undergone photochemical and biological alteration leading to changes in the molecular profiles of the original chromophore-containing species, not to mention the contribution of the environment and the textile matrix [54]. Most of these issues can be overcome by applying suitable sample treatments, which aim at maximising the information achieved while minimising sample size and matrix effects.

When interpreting the results obtained, the contribution of the environment can be particularly difficult to assess when the burial conditions are rich in plant residues and humic acids, which can produce tannin-like species leading to incorrect attributions. Additionally, the assessment of the mordant used (if any) can be hindered by external factors, first and foremost because these elements can also originate from the archaeological environment, through diagenesis or contamination, while loss of soluble cations
can also occur [55]. Taking into account all the aspects mentioned above (including the possible degradation of the dye markers) and the range of different sensitivities of the detectors available, the size of the sample required can now be reduced to less than 1 mg of material or to fragments 0.5 mm wide.

The analysis of dyes in mineralised textiles employing non-destructive techniques as Fourier-transform infrared (FT-IR) microscopy was first presented by Gillard and co-authors, who purposely built a suitable reference database [56]. In their following paper on the investigation of fibre mineralisation by FT-IR, the spectrum obtained from a thread collected from a man's tunic dated 16th century AD clearly showed the bands associated with dyeing with indigo [57].

The first successful attempts to analyse dyes at the molecular level in Bronze Age textiles were reported in research carried out on textile fragments recovered from the Hallstatt mines, which had been in use since at least the 14th century BCE. More than 200 textile fragments have been discovered, most of which date from between 1400 and 400 BCE, and are in an excellent state of preservation [60-62]. The fragments were preserved as embedded in the "heathen's rock" (Heidengebirge), which is a layer consisting of salt, clay, gypsum, broken shafts, fragments of spruce and fir used as torches, food residues and broken bronze tools. Several investigations were conducted on the dyes employed in the textiles, starting the year 2000, led by Regina Hofmann-de Keijzer (University of Applied Arts Vienna), Maarten van Bommel (Instituut Collectie Nederland) and Ineke Joosten (Instituut Collectie Nederland). Textiles from the Hallstatt period found in salt mines display a wide variety of patterns and techniques and are mainly made of wool, with the exception of two single threads spun from flax or hemp, and three textiles made of horsehair. White and naturally pigmented brown, grey or black wool was used, and red, blue or yellow dyes were detected. In particular, the analysis by HPLC-DAD of the blue textiles highlighted the presence of indigotine, indirubin and isatin, pointing at the use of woad, of quercetin, occurring in most plants and not indicative of a specific dye and finally elagic acid, typical of tannins. For the black textiles, an elagic acid equivalent was detected suggesting the use of tannins, along with woad. For yellow textiles, luteolin and apigenin were found, likely pointing to the use of weld, or other luteolin-containing species. Rhamnetin and quercetin were also detected. The latter dyestuff was also hypothesised together with woad to achieve the green colours, and together with woad and orchil (orcein was identified) for the browns. Purpurin was detected in the red threads, in some cases together with rubiadin and alizarin, pointing at the use of a madder-type dye; in some samples carminic acid (hence an insect dye) and orcein (marker of orchil) were also tentatively identified. Since most of the detected species are mordant dyes, elemental analysis was performed. Nonetheless, it was not possible to distinguish between a deliberately added mordant and contamination possibly caused by the diffusion of aluminium, copper and iron salts from the mine minerals into the wool threads [63].

Particular attention has been paid in the literature to the possible detection of shellfish purple, the most precious and expensive dye used in the Mediterranean region since the Bronze Age. Especially during Roman time, purple dye was the colour of seniorial rank and later on became specific for the Emperor's family. Ciccola et al. [59] investigated the pink colour found in a mineralised textile fragment belonging to the MANN (Museo Archeologico Nazionale di Napoli) collection. As part of the excavations at Pompeii, several textiles were discovered which, although preserved, rarely show traces of their original colour, as they are often charred or mineralised. Conversely, this study focused on one fragment consisting of a mineralised fabric decorated with gold, still showing traces of a purple dye (Fig. 7C). Indeed, the analyses performed by Raman spectroscopy, Raman-SERS (after extraction

in dimethylformamide) and finally HPLC with high resolution mass spectrometry all concurred in the detection of a profile consistent with purple. Chromatographic analyses performed on the sample treated with dimethylformamide, dimethylsulfoxide and eventually resuspended in methanol clearly confirmed the presence of indigotine, monobromoindigotine and dibromoindigotine (Fig. 7D).

Very recently, mineralised textile fragments were found in the inhumation grave excavated from the Uden-Slabroek cemetery, which is one of the richest Early Iron Age burials (ca. 8th BCE) found in the Netherlands. HPLC-high-resolution mass spectrometry allowed the detection of indigotine and carminic acid in two samples collected from one textile fragment, pointing at the use of woad and a scale insect for the production of a shepherd's check pattern [41].

Finally, Ballard et al. [58] have shown the successful application of direct analysis in real time mass spectrometry (DART-MS) to dye detection in extremely degraded textiles. In particular, they addressed the characterisation of textiles retrieved from the burnt level of the City Mound, Gordon (capital of the Phrygian kingdom, ca. 800 BCE) and in particular from tumulus MM (Fig. 7A). Inside the tomb chamber, deterioration of the textiles had occurred, and while some of the textiles were intact, most of them resulted as amalgamated, dense, powdery solids. Some samples are now entirely devoid of fibre and present "yarns" composed of goethite, whose origin is still debated; a few also were proven by DART-MS analysis to contain traces of indigo dye markers, whereas other textile fragments featured the molecular markers of a madder-type dye (Fig. 7B). These results were obtained by applying DART-MS to solid fragments 0.5-3 mm wide, directly held by forceps in the 7 mm gap between the DART probe and transfer tube. The presence of a dye was assessed when the signal in the mass spectrum appeared consistently during the analysis time; the high resolution of the mass measurement was paramount to discriminate the signal due to the molecular markers from the background.

In conclusion, few examples of dyes analysis in mineralised textiles have been attempted and provided positive results. In several cases, the identification of the procedure used to produce colour was not possible, due to the limited number of molecular markers detected, which did not allow for the final and positive assignment of a specific plant or insect as source of the dyeing material. Even more inconclusive results were obtained by elemental analysis aimed at identifying the use of possible mordants. Nonetheless, the availability of high resolution mass spectrometry, allowing for unprecedented selectivity and sensitivity, and the widening of databases of possible dye sources will allow in the future more detailed and conclusive determination to be conducted, as shown by the more recent studies presented here.

## 5.2. Molecular composition

FT-IR has been used in a number of studies to characterise the chemical nature of the organic remains present in archaeological fibres and textiles [17,27,64]. The use of the method has been reviewed by Margariti [65] towards aiding fibre identification in difficult cases and studying biodeterioration mechanisms. Similar trends have been observed in the related field of the study of human hair in archaeology and forensic medicine [66-69]. The controlled experimental reproduction of mineralisation mechanisms was tested under conditions imitating burial while monitoring the oxidation of disulphide bonds in the mid-infrared [57,70], as has also been done in studies on wool composting [71], showing the value of the methodology used in these mechanistic studies. FT-IR in attenuated total reflectance (ATR) mode coupled with chromatometric analysis has recently been used to study wild silk species and has shown promise that this technique could be used to differentiate and group them according to their species [72].
<figure><img src="image_10.png" /><figcaption>**Fig. 7.** (A) Textile sample 2003-Tx-9 retrieved from the MM Tumulus, burnt level of the City Mound, Gordion (capital of the Phrygian kingdom, ca. 800 BCE) and corresponding DART mass spectrum (B). (C) Mineralised textile fragment excavated at Pompeii, belonging to the MANN (Naples, Italy) and corresponding HPLC-HRMS chromatograms (D) relating to non-brominated (top), monobrominated (middle), and dibrominated (bottom) indigoids in the DMSO extract of the sample. Reprinted from Ballard et al. [58] (Figures 12 & 28) and Ciccola et al. [59] (Figures 1 & 4), under CC-BY licence.</figcaption></figure>

Second harmonic generation (SHG) microscopy was used by Reynaud et al. [17] to map specifically (organic) fibrillar cellulose fragments in ancient textile fibres from the ancient Near East, revealing highly heterogeneous states of preservation at the microscopic level (Fig. 8). A titanium-sapphire laser source was used ($\lambda$ = 860 nm), collecting the SHG signal emitted anisotropically at $\lambda/2$ = 430 nm, both in the “forward” and “backward” directions (see also Melelli et al. [73] and references therein). The authors observed that, inside the cell walls, cellulosic macromolecular chains are packed into microfibrils (10–30 nm in diameter), which themselves aggregated into macrofibrils (typically 1 $\mu$m in diameter). The $I\beta$ form of the crystalline domains of cellulose, mainly present in plant fibres, crystallises in a monoclinic system and a $P2_1$ space group [74]. These domains are therefore non-centrosymmetric and exhibit a non-zero second-order non-linear susceptibility, $\chi^{(2)}$, leading to SHG emission under appropriate excitation. The authors observed that microscopic domains consisting of exceptionally well-preserved assemblies of cellulose macromolecules were adjacent to much less well-preserved domains in these highly mineralised textiles.

Proteomics has been another area of recent development targeting mainly taxon identification from textile proteins such as keratins from hair, wool or fur, collagens from skin and leather or fibroins from silk [22,75–78]. The end of the 2000s showed some of the first taxonomic studies of the clothing and fur of a 5300-

year-old Tyrolean mummy called Ötzi, based on both keratin peptide mass fingerprint (PMF) and sequencing using MALDI-TOF/TOF mass spectrometry [79,80]. The PMF technique was later applied to other textile materials, such as pelt and textile samples found in association with copper-alloy objects (3rd c. BCE–10th c. AD) with different degrees of mineralisation (Fig. 9), resulting in a successful taxon identification of both keratin- and collagen-based materials ([81]; Fig. 9).

Taxonomic identification using PMF or peptide sequencing methods (LC ESI-MS/MS) opened new insights in the study of textile materials. The following section describes mineralised cases, but also non-mineralised cases relevant to the (future) analysis of mineralised materials. Proteomics proved to provide new insights in the study of cultural habits from the past and cultural practices, (i) confirming for example the choice of raw material used – e.g. dog and goat fibres in Coast Salish weave materials [82], (ii) linking raw material to the function of textiles – e.g. Bronze Age and Iron Age sites in China with most woven textiles made from sheep wool and pelts from goat [83], or (iii) revealing techniques of production – e.g. cattle gut membrane-based or goat/sheep skin-based metal threads in medieval textiles and additional (egg/glue) binders depending on the metal coating [84].

Proteomics-based taxonomic studies can also provide key information for classifying materials by location and date, as in the study of membrane metal threads used to identify bovine
<figure><img src="image_11.png" /><figcaption>**Fig. 8.** Backward SHG microscopy reconstructed in-focus image of a bundle of fibres collected directly on a fragment of mineralised braided fabric (copper-based), woven in tabby with S-twist threads, from Tello (present-day Iraq) and dated to the second millennium BCE. The fluorescence and SHG signals are shown in red and green, respectively. The SHG signal is indicative of the presence of preserved cellulosic fibres. Figure credit: Reynaud et al. [17].</figcaption></figure>

<figure><img src="image_12.png" /><figcaption>**Fig. 9.** Peptide mass fingerprint spectra of mineralised fibres from Gol Mod 2 cemetery in Mongolia (3rd c. BCE - 2nd c. AD). Textile remains were found associated with copper-alloy artefacts. **Top:** pseudomorph-type fibres. **Bottom:** fibres in an early stage of mineralisation ("physically robust", as identified by Solazzo et al. [81]). Keratin peptide markers allowed the identification of the Ovis genus. Figure adapted from Solazzo et al. [81].</figcaption></figure>
intestine or stomach membranes from 14th c. Italian textiles [85], or in the medieval textiles mentioned above, which allow correlations to be established between Eurasian manufacturing centres [84].

The study of proteins from mineralised textiles remains challenging in several aspects. Access to proteins is a major challenge, given the source materials and/or heterogeneous matrices. The limited organic matter content also represents a constraint (e.g. in pseudomorphs, [70]). This requires appropriate sample preparation and analysis methods, developed from modern and ancient samples, e.g. flax [86]; silk [87]; hair, wool and skin [88–91], but also from soil [92,93]. In sedimentary environments, silk fibroin peptide sequences have been reported, some of which have been found in tombs dating back 8500 years [92]. Methodological approaches targeting both proteins and other components such as dyes from keratin-based textiles were also proposed [94].

Another challenge arises from the protein identification / characterisation by itself considering the large number of protein polymorphic variants; e.g. keratins and keratin associated proteins (KAPs) [95]; collagen family and proteoforms [96]. Several works have shown how the expression levels of several KAPs can be correlated to the between-breed difference (white and black merino wools, [97]) or to the breed discrimination (e.g. mouflon, merino and Soay sheep, Solazzo [22]; Churros, Bordaleiros and Merinos ovine breeds, Plowman et al. [98]). Aspects related to protein quantification have also been useful in distinguishing between wild and domesticated plant species, such as cotton in the study of modern fibres [99] or in identifying sheep versus yak cashmere [100,101]. Considering the lack of referenced genome sequences for under-represented species (or partial sequences available in protein databases), both targeted and untargeted analyses are proposed nowadays to overcome these limitations and identify key taxonomic peptides in archaeological textiles and fibres. In particular, multivariate MS studies with molecular networking and database-assisted de novo sequencing were proposed to identify diagnostic peptides, such as in South American Camelidae [102].

The protein degradation / chemical modification that may arise from different sources, such as fibre processing (e.g. effect of treatments) or the mineralising environment (e.g. effects of burial conditions). Protein modifications such as deamidation (amide functional group converted into carbonic acid) and oxidation (covalent modification of amino acids induced by (in)direct reactions with reactive oxygen species) are of major importance in textile proteomics studies. The deamidation rate of wool α-keratin was shown to be time-dependent in a controlled environment, and influenced by primary and higher-order structures [103]. In archaeological samples, it was shown to be influenced by the local environment (e.g. acidic soil facilitate glutamine hydrolytic deamidation, [103]) or the presence of inhibitors such as copper corrosion products [81]. With regard to damage caused by UVs, photo-oxidation products of aromatic amino acids have been identified, influenced by dyes and mordants [104]. Insights into structural degradation were also shown through studies targeting surface morphology and secondary structure of silk [105]. Microbial activity is another factor contributing to the physical deterioration of textile materials, as shown by studies on the biodegradation of wool [106] and silk fabrics [107].

Studies also provide a better understanding of animal domestication and breeding, as well as the trade in raw materials. A range of new instrumentation, analytical workflows and data processing methods, also involving genomic data on fibres [108–111], is improving the level and quality of the information collected (sensitivity, identification of chemical structures, etc.) and opens up new perspectives in the proteomic study of textiles and mineralised textiles.

### 5.3. Molecular organisation

As early as in the 1970s, Diane Lee Carroll tested an innovative protocol combining X-ray diffraction (XRD) together with optical microscopy, SEM, and XRF [112]. Carroll was actively looking for traces of organic matter in mineralised textiles adhering to an Etruscan bronze bowl from the Newark Museum. She used a Guinier-De Wolff focusing camera, but was unable to detect any organic signatures, as she had hoped. Carroll concluded that the sample did not contain any residual organic phases. However, even if it were still present, the small-angle scattering signal from the cellulose would probably have been of very limited intensity compared to the dominant central scattering from copper in the organic material and from the basic copper carbonates she identified.

Two decades later, synchrotron-based small-angle X-ray scattering (SAXS) was successfully used to characterise the organisation of fibrillar keratins in archaeological fibres. In wools and hairs, fibrillar keratins are involved in a complex architecture made up of mesoscale coilings at several molecular levels, in particular with a coiled-coil structure involving individual α-keratin molecules. The associated periodicities can be characterised by SAXS to help identify the nature of the fibres and study the modification of the molecular structure of wools during long-term alteration. The method showed the preservation of archaeological fibre supramolecular packing — from the ordering of microfibrils down to interatomic levels, and characterised their swelling behaviour in ancient and model fibres [66,113]. Similar approaches were used by Müller et al. [[114,115]] to study single 2000-year-old archaeological fibres from textile fragments excavated in the Cave of Letters in the Dead Sea region, identifying most of them as wool, some as plant bast fibres (flax), in comparison with modern reference samples. The molecular and supramolecular structure of both were found intact. Hermes et al. [116] studied the degradation of silk fabrics from the Famen temple (法门寺; T'ang dynasty, 618–907 AD) using synchrotron µXRD scanning with a beam of ca. 1 µm × 1 µm. The azimuthal width of the 210 reflection, linked to the distribution of the macroscopic orientation of the fibres and the orientation of the crystalline domains within the nanofibrils, was found to be sensitive to the degree of decay of the fabric. The authors observed an initial alteration of the proteinaceous random chain network, followed by alteration at the level of the nanofibrils, with the silk fibres breaking up into even smaller fractions. Bertrand et al. [69] observed the perfect conservation of the supramolecular organisation of α-keratins in mineralised hair strands from Abbess Marie de Bretagne, whose entire locks of hair were found preserved, still very supple, thanks to the presence of copper-based hairpins in her hair. The use of SAXS and WAXS for the positive identification of the nature of fibres, although very diagnostic, has become somewhat depreciated and has been replaced by direct microcopy techniques (SEM, optical microscopy, and to a far lesser extent µCT). The main reason for this is that the observation in the reciprocal space requires dedicated expertise, provides an average observation and does not account for the observation of variations within a corpus of fibres, except if fibres are mounted individually (see Design of analytical sequences). However, the method remains particularly suitable for the average analysis of the molecular behaviour of the mesostructure of textile fibres during their very long-term alteration.

XRD is also the standard technique, with (polarised) optical microscopy and SEM, for identifying inorganic crystals and has been used to characterise the mineral products involved in fibre mineralisation [23]. It can be used for point analysis, or in mapping mode, the latter particularly at synchrotron facilities to collect large maps at high angular resolution [117]. Micro-XRD could be used to better describe the stratigraphy observed in mineralised textiles at microscale.
# 6. Elemental and isotopic analysis

## 6.1. Elemental analysis

Scanning electron microscopy can be coupled with energy-dispersive X-ray spectroscopy (EDX) to establish the local elemental composition of textile samples. The resolution obtained can typically be a few micrometres. EDX profiles can be used to characterise exogenous inorganic materials, and have been used, for example, to characterise micrometric gold particles found in Iron Age mineralised textiles [41,118], or to search for traces of aluminium that might indicate the use of a mordant before dyeing. SEM-EDX can be used to better understand the mechanisms of mineralisation, as can the physically closely related technique, XRF spectroscopy. XRF spectroscopy has been used to study the composition of samples at a resolution that makes it possible to obtain the profile of the elemental distribution across the diameter of isolated fibres. For example, it was used to study individual hair fibres collected from the burial of the Abbess Marie de Bretagne in Orléans, France. The elemental concentration profiles of copper and lead have made it possible to propose a multiscale taphonomic mechanism to explain the exceptional preservation of human tissues and textiles in this specific context, consistent with the archaeological information about the burial context [69].

## 6.2. Stable isotopes

The provenance of wool or textile materials remains one of the main interests of archaeologists. The isotopic composition of archaeological textiles is thought to reflect the bioavailable content of grazing land and henceforth can be used to infer a geographical setting of the raw material i.e. provenance thereof. Both the light isotope system (H, C, N, O, S) and the heavy isotope system (Sr, Pb) are relevant for attribution of origin, allowing the distinction between local and non-local material [1,119-127]. Although it is not always clear in what form (raw fibres, spun threads or woven textiles) they circulated, isotopic analysis allows rethinking wool production and trade routes. The above examples refer to archaeological textiles that are not mineralised. Early attempts to isotopically trace textiles attached to metal objects were successful, but only when the textile material was in a minimally altered state of preservation [128]. To the best of the authors' knowledge, no attempts have been made on mineralised textiles. The question of the source of the material must be raised concerning the availability of the original organic material. In the case of partial mineralisation, some original material remains, whereas in the case of complete mineralisation, the original material is lost. To what event does the isotopic analysis refer to when the original textile organic material is replaced by metallic corrosion products?

## 6.3. Radioactive isotopes ($^{14}$C dating)

The dating of archaeological textiles goes back to 1949 as part of the first published radiocarbon studies [129]. This type of analysis requires the presence of carbon in the sample and can be generalised to any organic compound or carbonate-bearing material. The question is how to deal with mineralised textiles where the organic material has partially or completely disappeared. The state of preservation of the investigated textiles is of relevance, as highlighted in the study of Margariti et al. [130] on charred and mineralised textiles. The latter were found preserved in copper alloy urns, used to wrap the remaining bones of the deceased. As such, the formation of copper carbonate corrosion products may be hypothesised. In general, the obtained dates were earlier than the relative dates and the authors noted that "the degree of mineralisation is crucial to the $^{14}$C dating results, the higher the degree

of mineralisation, the lower the reliability of the results" [130]. A statement which is most certainly true for the majority of samples submitted to radiocarbon laboratories for dating under the label textiles, as they will endure the classical acid-base-acid (ABA) pretreatment, a procedure ill-suited for metal carbonates forms of mineralisation which are sensitive to acid and readily dissolve. Generally, the quality of the produced $^{14}$C dates correlate with the amount of recovered carbon. The most important factor when conducting traditional $^{14}$C dating approaches is the state of preservation / mineralisation, presence / absence of organic matter.

# 7. Experimental approaches

Experimental approaches are an integral part of the analytical procedure developed to study textiles, in order to link microscopic and macroscopic observations. Only a limited number of works have dealt with experimental archaeology and experimental taphonomy in the context of mineralised textiles.

## 7.1. Experimental archaeology

Experimental archaeology is a link between an analytical approach and the practical understanding of human behaviour [131]. Experimental archaeology in terms of archaeological textiles is usually carried out with a technological and craft-centred approach, using this method to understand both how ancient techniques work, details of the chaîne opératoire, and also about time consumption and cross-craft interaction. The latter points to the handicraft experience of different craftspeople such as woodworkers, potters or metal smiths, who are linked to each other by the design and production of tools used in textile production. Experiments have concentrated on investigating the functionality of certain types of tools or textile techniques, for example concerning spinning techniques [132,133], and expenditure of time required by spinning, as well as performance of spindle whorls or the reconstruction of specific tablet woven bands [134-136]. This kind of experiments is also an interesting contact-point between academic research and the interests of today's society (Fig. 10). Experimental archaeology also helps to visualise techniques and can be used to disseminate the work, as well as experiments concerning the use of textiles for garments in combination with accessories. This has been done e.g. on the case study of an Early Bronze Age grave find from Franzhausen in Austria [137], also examining influences of garments on body language and the potential of clothing as medium of non-verbal communication.

## 7.2. Experimental taphonomy

Experimental taphonomy, defined as the "documentation of the stages through which an organism decays" [138] can extend to the non-living tissue that make up textiles. Chave et al. [11] have shown that reproduction experiments of wood petrifaction were developed as early as in the 16th century [139]. A limited number of experiments are reported that simulated degradation under conditions relevant to archaeological objects (non-synthetic textiles, materials produced using traditional means, imitation of burial or funerary environments, etc.). The literature prior to 2000 has been summarised by Janaway [140], mainly concerning death scenes from a forensic perspective, but mentioning a number of studies conducted by archaeologists, as well as interesting standards aimed at testing the resistance of textiles to biodegradation. Janaway [140] mentioned the 'Bradford experiments' which studied textile degradation by tracking molecular changes using FT-IR microscopy. The author notes that "perhaps the most relevant is the amount of the original material that is recoverable in a morphologically identifiable state", highlighting the central use of vi-
<figure><img src="image_13.png" /><figcaption>**Fig. 10.** Tablet weaving by Dr. Kayleigh Saunderson (University of Vienna) using means available during the Hallstatt period. Photo credit: Armin Öller.</figcaption></figure>

sual observation (using scores to designate the general condition of textiles on recovery, based on five classes qualifying the loss of surface area of the fabric).

In the last few years, experimental archaeology has also focused on the understanding of mineralised textiles as found in cremation graves. Recent experiments on cremation burials had the aim of understanding the dynamics of incineration of textiles on a pyre [141]. Important for textile research are the circumstances of how and for how long textiles could last during a cremation pyre (e.g. did they fall down from the pyre before being completely destroyed) and how they might have been collected and deposited together with metal artefacts in urns.

Wilson et al. [142] reported the examination of human hairs inoculated with soil microorganisms through soil burial in the field and under laboratory conditions to produce experimentally degraded samples. The degraded hair fibres were subjected to detailed histological examination using a combination of high-resolution optical microscopy, transmission electron microscopy and SEM to investigate the nature and sequence of degradative change to hair structural components.

In a temperate climate, in the absence of metals or toxic or 'rapidly encapsulating' elements (e.g. iron), textile decomposition takes place over a period ranging from a week to a month. This is corroborated by studies using standard test soil on various cellulosic and non-cellulosic materials such as cotton, jute, linen, flax, wool used for the reinforcement of soil [143]. The latter used a combination of microscopy (optical, SEM), FT-IR spectroscopy in ATR mode and thermogravimetric analysis (TGA). Only the past works of Gillard et al. [70] and Gillard and Hardman [57] directly dealt with the mechanisms of mineralisation of textiles. They developed a method specifically designed to reproduce the formation of mineralised fibres, analysing the results using SEM, SEM-EDX, UV reflectance spectroscopy, (C, H, N) elemental analysis and FT-IR microscopy, and examining the effects of mordanting, dyeing and different environmental conditions.

Forensic scientists have developed atlases to help identify altered textile fibres [144]. Beyond forensics, recent work of interest includes studies on waste management and biodegradability of textiles (e.g. Park et al. [145]), in particular with composting stud-

ies of waste wool [146] and 30 % linen / 70 % cotton textiles [71]. Both studies used controlled compost mixtures (according to existing standards or described protocols), and monitoring of the compost pile. Hustvedt et al. [146] reported hand screening and analysis of the elemental composition of the mix. Esmaeilzadeh and Rashidi [71] reported the characterisation of textile particles and analytical characterisations based on FT-IR spectroscopy (analysing the evolution of characteristic peaks), SEM for monitoring the disintegration of fibres during decomposition, as well as monitoring the morphology, colour, odour and other biochemical properties of the microbial consortium.

## 8. Conclusions and perspectives

Mineralised textiles are located at an interesting cross-road in terms of methodology because they involve a diversity of challenges. They are mineralised, but they have been shown to retain organic molecular remains and organic molecular assemblies even long after they have been deposited, even in cases of heavy mineralised textiles [17,81]. They therefore require the combined use of methods derived from organic chemistry, mineral chemistry and mineralogy, geochemistry and biochemistry. They are recrystallised, but often show an astounding preservation of their mesostructural organisation, which is why some were shown to diffract from low to high angles [69]. They therefore require a combination of local microscopy methods and approaches capable of gathering information on the mesoscopic organisation of organic molecules. They are very complex when observed using 3D imaging techniques, but their measurable complexity can be addressed with the development of characterisation methods at multiple scales, giving hope to better understand their history and the history of their chemical formation. In particular, the 10 nm – 10 µm length scale range, which was difficult to characterise in the past, is now covered by direct imaging methods.

Beyond a technical catalogue, we therefore believe that the series of methods detailed here offers an interesting perspective on future developments in analytical chemistry for complex archaeological samples. The reconsideration of the scales of documentation available on a given artefact is striking: the documentary
context moves from a broad macroscale (the context of the find, taphonomic proxies, the site, archaeological experimentation) to a deeper microscale (facilitated by advances in instrumentation, from a purely quantitative point of view). Innovative couplings of dye analysis and 3D imaging [41], optical microscopy and proteomics [22], SEM and radiocarbon dating [23], or SHG microscopy and FT-IR spectroscopy [17] are therefore not coincidental: all these examples show novel combinations of spectroscopy and imaging. They allow associating data on the composition of the sample (matter) with data on the morphology of the sample (shape). Together with the advent of spectral imaging, the resulting spatialisation of information opens the way to a better (more detailed, more statistically robust) understanding of the heterogeneity of mineralised textiles. The current difficulty may be less to join contrasting quantitative and qualitative data, or destructive and non-destructive analyses, than to collect and confront these two very different aspects of knowledge of the material object. This evolution in the spatial perception of the object at all scales (from geographical location and the archaeological site to spatialisation at the micro or even nano scale) allowed by new approaches are also paving the way to a new historical perception of the artefact. The combination of analyses, in particular spectral imaging, reinforces a processual perception of the object, which refers to the operating chain and the long history of the object.

### CRediT authorship contribution statement

**Loïc Bertrand:** Conceptualization, Methodology, Writing – original draft, Writing – review & editing. **Clémence Iacconi:** Formal analysis, Writing – review & editing. **Ineke Joosten:** Formal analysis, Writing – review & editing. **Caroline Tokarski:** Writing – review & editing. **Ilaria Degano:** Writing – review & editing. **Jiayi Li:** Methodology, Writing – review & editing. **Laura Hendriks:** Formal analysis, Writing – review & editing. **Étienne Anheim:** Methodology. **Sasja van der Vaart-Verschoof:** Writing – review & editing. **Karina Grömer:** Writing – review & editing.

### Acknowledgements

CI's PhD was funded by the Île-de-France Region as part of the Paris Region doctoral scholarship programme ParisRegionPhD (MUSETEX3D project), co-funded by Novitom. CI acknowledges the support of the SNSF through grant no. 229047.

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