Study on the technique of the Roman age mural paintings by micro-XRF with Polycapillary Conic...

Study on the technique of the Roman age mural paintings by micro-XRFwith Polycapillary Conic Collimator and micro-Raman analyses

Giovanni Paternoster a,*, Raffaele Rinzivillo a, Felice Nunziata a, Emilio Mario Castellucci b,Cristiana Lofrumento b, Angela Zoppi b, Anna Candida Felici c, Gabriele Fronterotta c,

Chiara Nicolais c, Mario Piacentini c, Sebastiano Sciuti c, Margherita Vendittelli c

a Dipartimento di Scienze Fisiche dell’Università “Federico II” and INFN-Sezione di Napoli Complesso Universitario di M.S.Angelo via Cintia,80126 Napoli, Italy

b Dipartimento di Chimica, Polo Scientifico, Università di Firenze Via della Lastruccia, 350019 Sesto Fiorentino, Italyc Dipartimento di Energetica dell’Università “La Sapienza” Via A. Scarpa 14 00161 Roma, Italy

Received 24 October 2003; accepted 20 October 2004

Abstract

XRF and micro-Raman stratigraphic microanalyses of fragments of some mural paintings, belonging to the Archaeological Site of Oplonti(Napoli) and the Vigna Barberini site in the Palatino (Roma), were performed. In order to collimate the fluorescence X-rays emitted by thesamples, an X-ray polycapillary conic collimator (PCC) has been used in front of the detector. This device arrangement is compact, versatile,and portable. The nature of the pigments, the compositional elements, and the thickness of the fragment layers have been studied. Thestratigraphic analysis partially confirms the preparation techniques described by Plinius and Vitruvius; moreover it confirms the hypothesisthat the artifacts are not fresco paintings. This work has been conducted within the context of a wider research on the Roman age muralpaintings.© 2005 Elsevier SAS. All rights reserved.

Keywords: X-Ray collimator; ED-XRF; Portable Instruments; Micro-Raman; Mural paintings; Roman age

1. Aim of the research

The high quality and the good conservation status of thepaintings found at the beginnings of the Pompeii excavationsrise the problem of the techniques of their production. It hasbeen suggested that they were either encaustics, or based onfresco, tempera or even on more elaborate techniques.

For identifying such techniques with a non-destructivemethod (or better, with a quasi non-destructive method, basedon the analysis of the fragments and/or deteriorated paintingsat the archaeological sites), a very compact apparatus forstratigraphic XRF analyses, to be used also in situ, has beenset up. We tested this instrument on several fragments of muralpaintings coming from Oplonti (Napoli) and Vigna Barberini

(Palatino, Roma). Some fragments were analysed also with amicro-Raman device to determine the number and the thick-ness of the paintings layers, the nature of the used pigmentsand to check for the presence of organic compounds.

2. Introduction

In the field of Cultural Heritage, the Energy DispersiveX-Ray Fluorescence (EDXRF) technique reached a greatdevelopment thanks to its numerous advantages. It allows non-destructive, fast, versatile, sensitive, and in situ multi-elemental analyses [1–4]. In studying the techniques of ancientmural paintings and the pigments employed, these advan-tages are well suited for recognising the compounds used forthe pigments, detecting the presence of organic compounds,separating the matrix effect, and the signals coming from over-lapping layers of painting [5–7]. In order to overcome someof these difficulties, an EDXRF apparatus has been set up,

* Corresponding author.E-mail addresses: [email protected] (G. Paternoster),

[email protected] (E.M. Castellucci),[email protected] (A.C. Felici).

Journal of Cultural Heritage 6 (2005) 21–28

http://france.elsevier.com/direct/CULHER/

1296-2074/$ - see front matter © 2005 Elsevier SAS. All rights reserved.doi:10.1016/j.culher.2004.10.003

which permits to carry out stratigraphic analyses with highspatial resolution.

The Roman paintings’ stratigraphy and production tech-niques were firstly described by Vitruvio [8] and Plinius [9]the senior. A mural painting is composed of a preparatorylayer (tectorium) made of three or more (until six) layers ofplaster: starting from the raw wall, at first there is the arric-cio, constituted of three layers of lime and sea or volcanicsand (or pozzolana) and then the plaster, constituted of threelayers of lime and marble powder. When the plaster is stillwet, the pigments, mixed with suited binders and diluents,are laid over the tectorium. To preserve the paintings fromthe environmental ravages, a wax mixture is laid, heated, andsmoothed so that the painting surface appears translucent.

At the beginnings of the 50s the chemist and archaeologistSelim Augusti conducted many precise chemical analyses onlots of paintings from Ercolano and Pompeii; his results seemto prove the existence of a particular technique, already pro-posed at the beginning of the XIX century, based on the useof soaped water mixed with lime, clay (or chalk), and wax[10–12]. This particular technique has recently been foundon several paintings of the roman age [13,14]. More recently,Mora et al. [15] proposed the use of a fresco technique for thebackground, and a limed water technique for the decorativepart. However, in agreement with other recent studies, it seemsthat more then one single technique was used [16–19].

3. Experimental

3.1. Samples

The study was conducted on a total of 15 fragments withan average surface area of about 15 cm2. Eleven samples comefrom the Oplonti Archaeological Complex near Naples andbelow they will be referred to as “Oxx”, “xx” indicating areference number. These fragments had not been restored andthey had no context so we have been allowed to make somemicro-destructive analyses on them. A stratigraphic analysishas been conducted on the fragments O01 and O15. Theformer fragment has a compact and resistant blue back-ground; probably it belongs to the II Pompeian style, secondhalf of the I century BC; the latter belongs to the IV style,second half of the I century AD. It is white, smooth, and ascompact as marble. Both fragments show a shining surface,due to the presence of many crystalline inclusions.

The other four fragments come from a section of thePalatino archaeological site in Rome called Vigna BarberiniComplex. One fragment is blue and we label it the BarberiniBlue fragment (BB); a second one shows a geometric deco-ration in different colours, and we call it the Barberini Deco-rated fragment (BD). Both fragments are restored but not pre-served with any protective varnish. The third and the fourthfragment are similar to each other, probably coming from thesame painting. We will refer to them as a single sample: theBarberini Protected fragment (BP). They are black with a pink

stripe and have been restored and protected with Paraloidvarnish.

3.2. Micro-XRF

A small area of the samples is irradiated with an X-raybeam and the emitted fluorescence photons are collected andanalysed. By determining the number and the energies of thefluorescence X-ray lines, it is possible to trace up the ele-ments in the sample [20]. With our micro-XRF device wewere able to analyse areas of the sample as small as 140 µmin diameter. The stratigraphic distribution of the elements wasobtained by scanning along the lateral sections of the frag-ments [21].

The measurements have been taken with a portable devicefor EDXRF realized at the Laboratory of the University ofNaples. The X-ray generator is the E.I.S. air-cooled Pd anodegenerator with a focus of 200 × 200 µm2 and a 250 µm thickBe window; it can operate with a maximum voltage of 30 kVand a maximum current of 0.6 mA. The X-ray beam, colli-mated with tantalum diaphragms to a 1 mm diameter spotsize, is incident on the sample at 45°.

The fluorescence photons are collected along the normalto the sample surface through a Polycapillary Conic Collima-tor (PCC) mounted in front of the Si-PIN detector (Amptekmodel XR-100CR, with 165 eV resolution at 5.88 keV).

The PCC has been supplied by the Institut für GerätebauGmbH [22, 23]. Its entrance is at 11.5 mm from the samplesurface (Fig. 1) and allows a resolution of 140 µm FWHM.The X-ray tube and the detector are mounted on a three micro-metric axes stand. The positioning is obtained with two lasersand with a cross of two 20 µm golden tungsten wires on thesample. A colour micro camera was used for the positioningremote control and for the storage of the analysed point image.

The electronic chain is made up of an Amptek amplifier,the Amptek multi-channel analyser MCA8000A and a por-table computer for set-up control and for storing and analys-ing the spectra [24].

Fig. 1. Lateral view of the PCC pointing to a fragment section of a muralpainting.

22 G. Paternoster et al. / Journal of Cultural Heritage 6 (2005) 21–28

Taking into account the detector efficiency, the energytransmission of the PCC and the device geometry, we candetect the K-lines from S to Zr and the L-lines from Pd to U.

The EDXRF spectra have been analysed with WinAXILsoftware [25], inserting data about the X-ray source, the detec-tor, and the device’s geometry. These parameters have beenindependently measured and fixed to reduce the error on thedetermination of the areas of the peaks from degenerate lines.

As the samples are constituted by a wide and inhomoge-neous matrix, we prefer to present the results as relative rates(i.e., percentage ratios between the single peak net rate andthe total net rate) instead of quantitative percentages.

3.3. Micro-Raman

Micro-Raman measurements were carried out at the Chem-istry Department of Florence using a Renishaw RM2000 in-strument operating with an Argon air cooled laser source anda diode laser, with excitation wavelengths at 514.5 and785.2 nm, respectively. A 50× magnification objective wasemployed to focus the laser beam onto the sample providinga spatial resolution of about 1–2 µm; a wide area could beprobed by way of consequential point-by-point analyses.Raman spectra were acquired with an irradiating laser powermeasured under the microscope of about 2 mW, while lowerpower values were required by highly light sensitive samples,for which neutral density filters were used. The spectral reso-lution was 4–6 cm–1 depending on the experimental condi-tions; the investigated spectral range spanned from about200 to 1600 cm–1 where the main diagnostic signals of inor-ganic materials (pigments and minerals) fall, while the highfrequency region between 2800 and 3100 cm–1 was mainlyinspected for the CH stretching vibrations due to organic com-ponents.

Paintings were analysed with both laser line excitations,while the presence of organic materials was mainly checkedusing the diode laser line.

All fragments were observed with a microscope, withoutany preparation. Only for the O01 sample a cross-section wasprepared.

4. Results and discussion

4.1. Pigment recognition

The painted surfaces have been analysed by XRF andmicro-Raman techniques to determine the pigments used. Inseveral samples the emitted fluorescence was so high as tohide the Raman lines.

Regarding the elemental analysis, we consider only thoseelements having a net area of the XRF peak greater then threestandard deviations and a relative rate greater then 0.1%.

Not all the elements found in a spot are characteristic ofthe pigment used because of the contribution to the XRF linescoming from the preparation layers and also because the

colours are often laid one over the other. It is possible to rec-ognise the characterising elements by correlating their peakintensities with the colours and the fragments: those ele-ments, which are present in every analysed point of one par-ticular colour with a high relative rate, are considered char-acterising the pigment (Table 1).

Some considerations on the detected elements are neces-sary:• traces of phosphorus and sulphur, spread over all the

colours, were found only in some fragments: particularlyin the O03, O05, and O17 ones. They probably arise fromashes and dust contamination that the painting samples hadbeen suffering until their recovery;

• potassium is always present, showing higher intensity(more than five times its averaged relative rate) in the greencolours, whilst lower intensities were found in the whites;

• calcium is always present, but it is dominant only in whiteand black colours;

• titanium is present in the yellow colours and in some green,brown, and red ones;

• chromium characterizes the green colours;• manganese is particularly evident in the browns, yellows,

greens, and in some reds;• iron is characteristic of all the earth colours; it is present in

traces in the other ones;• nickel characterizes the green colours and it is signifi-

cantly present in the blues;• traces of copper are present in all colours, but it is domi-

nant in the blues.• zinc is a natural impurity of the earth colours;• arsenic is present in some red colours;• strontium was detected in all colours with quite different

rates;• lead is particularly evident in some red colours and in the

Barberini fragments.As for Raman measurements, the compositional results wereobtained averaging over a wide set of data points selectedwithin the area to be characterised. The visible and near-IRlaser excitation lines were both used for pigments’ identifi-cation, according to the paint colour: in general red, brown,yellow, and white shades were investigated through the diodelaser line, while for green and blue pigments the green laserline was preferred.

Raman spectra were recorded irradiating directly the sur-face of the painted layers giving rise in a lot of cases to astrong fluorescence probably due to surface organic contami-nation. The fluorescence effect was that of originating a ratherstrong background signal, leading to a complication in thedetection of the weaker Raman signals, thus in the identifi-cation of the pigments employed. This was particularly evi-dent with the argon laser line, while the diode laser excitationat higher wavelength very unlikely gives rise to absorptionand then to emission of fluorescence.

Due to the lack of fluorescence, the diode source was alsopreferred for checking the presence of organic materialsthrough the detection of CH stretching vibrations modes.

23G. Paternoster et al. / Journal of Cultural Heritage 6 (2005) 21–28

Unfortunately no Raman signals were observed in that regionand no organic substances were identified.

In the O15 sample the white painting layer gave solely thespectrum of a carbonate compound that was attributed to cal-cite.

The BB and BD samples coming from “Vigna Barberini”were quite well characterised without requiring any type ofpreparation. From the BB sample, showing a light blue colour,the spectrum of Egyptian blue was obtained, while calcitewas attributed to the paint calcareous matrix. The BD sampleshowed a poli-chromatic painting for which it was possibleto investigate each region separately. Except the green andbrown drawings, which exhibited a relevant fluorescence sig-

nal, it was possible to identify the white pigment as calciumcarbonate, while hematite was identified in red and violetareas.

Most of the samples analysed showed a rather noisy lumi-nescence background, induced even by the near-infrared diodelaser line. This fluorescence emission could be at first relatedto the presence of some organic components, but this assign-ment could not be confirmed by Raman measurements sinceits intense signal in the high frequency spectral region pre-vents to reveal any Raman peak that could be undoubtedlyattributed to such chemical components.

Therefore, we can conclude that the pigments used are [15,26, 27] (Table 1):• Atramentum, amorphous C, for the black;

Table 1

Pigment analysis results


• Egyptian blue for all the analysed blue points;• ochre and red earth for the brown colours;• green earth (Creta Viridis), iron and potassium silicate, for

the green colours;• ochre for the yellow;• some variety of red earth and ochre for the red/pink/violet

colours, characterised by the ratio Mn/Fe and by smallquantity of As and Ti [27]; in four points we detected ahigher rate of lead due to the presence of minium;

• paretonium or melinum (white clays) for the white pig-ment in fragments O08 and BD; lime and calcareous pow-der for the white background in the remaining ones;

• white lead was probably used in the preparation layer ofthe Barberini paintings.

4.2. Stratigraphy

Strontium is present in all colours. It reaches a high levelin the O03, O08, and BD fragments, which have a paintedwhite background, because it is probably present in the whiteclays. This can be argued from the absence of strontium inthe analyses done on the points where the pigment is missingand on the rear side of the fragments (Table 2).

To confirm this hypothesis 0.25 cm2 of the O01 fragmenthas been milled to a depth of 600 µm by steps of 100 µm,

performing an XRF analysis at each step. In Fig. 2 theobtained relative rates are reported.

It is evident that iron and strontium decrease with depth toa small constant value, reached at –300 µm level.

Before discussing the stratigraphic microanalysis, somecomments on the visual inspection of the lateral sections ofthe fragments should be done.

At the microscope with 6× magnification, the O01 bluefragment shows a pictorial layer about 200 µm thick, welldistinguished from the preparation layers (Fig. 3). The plas-ter, about 4 mm thick, is made of at least two separated layerswith different granulation of the calcite crystals. Inside, justbelow the pictorial layer, it is possible to note a little spheri-cal black inclusion, similar to those found in the arriccio; itis probably part of the volcanic sand used in the tectorium.

At the same magnification the O15 white fragment showsa very similar stratigraphy, except for the absence of the pic-

Table 2

Elements relative rate measured on points of missing colour and in the rearparts (plaster) of the Vigna Barberini fragments

Fig. 2. Relative rate of the elements vs. depth for the Oplonti 01 blue fragment, measured on successive milled layers. The “X” stays for elements heavier thanCu, apart the Sr.

Fig. 3. Transversal section of the Oplonti O01 blue fragment seen with astereo-microscope (6×).


torial layer and for the calcite crystals, that can reach a size ofabout 2 mm in the innermost plaster layer (Fig. 4).

The dimension and the structure of the calcite crystals con-firm theAugusti’s hypothesis that crushed limestone was usedinstead of marble powder.

The two plaster layers have a thickness of 1–2 and 2–4 mm,respectively, depending on the wall and the arriccio rough-ness. This stratigraphy does not agree with that described inthe introduction, but it is coherent with that found by Augusti[10].

4.3. Micro-XRF stratigraphy

Few millimetres on the lateral side of two fragments fromOplonti, the O01 (blue) and the O15 (white), were gently

smoothed and polished. On that region a series of micro-XRF analyses has been conducted.

The O15 white fragment shows a very high content of cal-cium with traces of lighter elements until a depth of about5 mm; from there on, iron and strontium are also present. Inthe O01 blue fragment section, four regions, of differentelemental content, can be distinguished (Figs. 5 and 6):• the pictorial layer, about 200 µm thick, containing Ca and

Cu as major elements due to the Egyptian blue pigment. Itcontains also Fe and K, but no lighter elements. Theseresults agree with those found in previous analysis;

• an intermediate region, less then 150 µm thick, where onlyCu disappears while the other elements remain constant intheir relative rate;

• a third region, 4 mm thick, similar to the one found in theO15 white fragment. The elements identified are: calcium(major element) with traces of potassium and iron, but noevidence of strontium. This region corresponds to the plas-ter made with milled limestone, as recognised at the opti-cal microscope;

• the arriccio layer containing iron, potassium, strontiumand traces of Zn, Zr, and Pb, in addition to the calcium.

4.4. Micro-Raman stratigraphy

A cross-section embedded in a resin matrix was preparedto investigate better the nature of the blue painting layer. Thislayer was about 80–100 µm deep, made of minute blue grainsthat were identified to be Egyptian blue, a copper silicate(CaCuSi4O10) widely used since antiquity [28, 29]. The under-neath layer, about 170 µm thick, appeared with a light tonedue to carbonate crystals of calcite (CaCO3), wherein spo-radic small orange grains (<2 µm) could be observed but were

Fig. 4. Transversal section of the Oplonti O15 white fragment seen with astereo-microscope (6×).

Fig. 5. The relative rate of the majority and minority elements vs depth measured in a lateral section of the Oplonti O01 blue fragment. The “X” stays forelements heavier than Cu, apart the Sr. On the upper line are indicated the layers boundaries.


not analysed. Going down, also the plaster was investigatedwhere calcite was mainly identified, with traces of silicatecomponents (such as diopside CaMgSi2O6), while no ironminerals were detected. The inferior part of the section, thearriccio, was black brown in colour. Here, Raman spectrarevealed the presence of hematite (a-Fe2O3) [28] and somefeldspars; a high signal at 667 cm–1 in the hematite spectrumcould be related to magnetite content.

A final consideration should be made with respect to thehypothesis that the strontium element detected by XRF couldbe an evidence of its presence as a carbonate. Actually, stron-tium carbonate, namely strontianite mineral, shows a promi-nent signal, due to the CO3

– anion symmetric stretching vibra-tion, that falls about 12 cm–1 below the calcite one. Ifstrontium had been present as SrCO3, according to the minorcontent with respect to calcium element, a medium bandshould have been detected in the calcite spectrum, while ithas been observed a signal around 1083 cm–1 free from neigh-bouring features; in many other cases the calcite spectrumappeared of such poor intensity that even the detection of theweaker SrCO3 spectrum was complicated, leaving the ques-tion unresolved.

5. Conclusion

A portable apparatus with a PCC for micro-XRF analyseshas been set up for studying some fragments of mural paint-ings of Roman age. After having identified the elementspresent in the pictorial layer, we did a stratigraphic analysis,determining the number and the thickness of the preparationlayers. The Raman analyses on the samples confirmed theXRF results, giving clear indication on the pigments used.

The preparation of the mural paintings follows the schemedescribed by Augusti [11]. On the rough wall there is a layerof lime and (volcanic) sand, named Arriccio, followed by twolayers of lime and crushed limestone, made of particles ofdifferent grain size, and a preparation layer of lime and whiteclay. More recent study on Roman mural paintings seems toconfirm the presence of a thin calcite layer under the pictorialone [30].

Strontium is present only in the pictorial and preparationlayers, thus coming from the compounds used to lay them.Its presence is also compatible with the use of gypsum, whichcan explain the poor firmness of the colours on some frag-ments. It must be noticed that gypsum has never been used inthe fresco technique; however it has been found in the plasterof Egyptian and Middle Eastern ruins [10]. Moreover theanalyses do not reveal the presence of sulphates both in thepictorial layers and in the tectorium.

We could not identify any particular organic compound toconfirm the use of soaped water, suggested by Augusti [11],because of the high fluorescence background. However, thegreasiness of the pictorial and preparation surfaces could bedue to the presence of wax that, according to Vitruvio [8],was used to polish the painting.

In any case, we think that the analysed fragments were notmade using a real fresco technique for several reasons. Firstly,the painting was made with a superposition of the differentcolour pigments over a uniform preparatory layer. Secondly,even in the fragments with a white background, which seemsto correspond to the topmost layer of the plaster, the colourpulverises and has a poor endurance, leaving only light tracesonce taken away from the surface. This is not consistent witha fresco technique or with the mere use of limewater. Thepresence in the pictorial layer of a certain percentage of stron-

Fig. 6. The relative rate of the majority and minority elements vs. depth measured from 1 to 8 mm in a lateral section of the Oplonti O01 blue fragment. The “X”stays for elements heavier than Cu, apart the Sr. On the upper line are indicated the layers boundaries.


tium leads to guess the use of a calcium compound for thedilution and the drawing up of the pigments, namely whiteclay [15].

There appears no great technical difference between thetwo groups of fragments from Oplonti and from Rome. Somedifferences have been highlighted in the pigments and com-pounds used in the preparation layers: this is the case, forinstance, of the preparation layer of the Barberini fragmentsin which evident traces of lead and stronger strontium peakshave been found, while the Oplonti fragments contain agreater amount of pure lime and calcareous compounds.

Acknowledgments

We wish to thank Prof. Piero Guzzo, Superintendent ofPompei and Ercolano, for the authorisation and the collabo-ration given. A particular acknowledgement to Dr. LorenzoFergola, Director of the archaeological site of Oplonti, forhaving kindly given us the fragments we studied. We have tothank also the Archaeological Superintendence of Rome (andin particular Dr. Maria Antonietta Tomei), which gave us theopportunity to study the fragments from Vigna Barberini inPalatino, property of the Ècole Française de Rome but keptin Museo Nazionale Romano. They were kindly placed atour disposal by the Director of the “Laboratori del Restauro”of Museo Nazionale Romano, Dr. Giovanna Bandini.

This research has been partially supported by the “Con-siglio Nazionale delle Ricerche”.

For the Raman measurements, the financial support of theEU, contract No. G6RDCT2001-00602, is kindly acknowl-edged.

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