Characterization of Organic Residues in Ceramic Potsherds

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The meals in a Tuscan building yard during the Middle Age. Characterization oforganic residues in ceramic potsherds

Gianluca Giorgi a,*, Laura Salvini b, Alessandra Pecci c

a Dipartimento di Chimica, Universitadi Siena, via Aldo Moro, 53100 Siena, Italyb Centro di Analisi e Determinazioni Strutturali, Universitadi Siena, via Aldo Moro 53100 Siena, Italyc Dipartimento di Archeologia e Storia delle Arti, Universita di Siena, via Roma n. 5653100 Siena, Italy

a r t i c l e i n f o

Article history:

Received 15 July 2009

Received in revised form

27 December 2009

Accepted 4 January 2010

Keywords:

Archaeological ceramics

Gas chromatography (GC)

Mass spectrometry (MS)

Fatty acids

a b s t r a c t

The characterization of organic residues found in ceramics objects coming from the Carmine Convent in

Siena (Central Italy), probably built in the second half of the 13th century, is described. The nine objects

analyzed in this study are pots, casseroles, and lids and they were used as filling material of the vault of

one room of the convent.

A gas chromatography-mass spectrometry approach has been used to analyze both the chloroform

methanol extracts as well as those obtained owing to alkaline hydrolysis.

On the basis of the compounds identified, the ceramic vessels were divided into three groups. One is

constituted by vessels that might have been used to cook different kinds of foodstuff (so called caul-

dron), including animals, and in particular ruminants. The second group is formed by a pot whose main

use might be as olive oil container. No traces of animal fats has been found in it. The third group is

formed by vessels mainly used for containing or boiling water or other substances not rich in fats. In

particular, one of them might have been used as a colander or to roast chestnuts, that were a common

food during the Middle Age.

These results, in conjunction with others obtained by different techniques, contribute to a better

understanding of the use of the ceramic vessels found in the Carmine Convent in Siena and on dietary,uses and customs of people living there, and more generally in Tuscany, during the Middle Age.

2010 Elsevier Ltd. All rights reserved.

1. Introduction

Ceramic objects, such as pottery vessels, are the most common

class of objects found during archaeological excavations. They

might have had different functions: containers for storing food,

such as oil, wine, water, and for cooking and serving meals.

If their conservation during the centuries was not in drastic

conditions, their organic residues contain biomarkers produced by

biochemical transformations of their original content. In particular,

the characterization of the lipid fraction in archaeological material(Rottlander, 1990) is of great importance to obtain information on

uses, custom and dietary of people who used this material ( Dudd

and Evershed, 1999; Dudd et al., 1998; Evershed et al., 1995; Mot-

tram et al., 1999; Raven et al., 1997; Evershed, 2008). In this frame,

the use of different mass spectrometry techniques and their

coupling with separation methods, play a key role in identification,

structural characterization and quantitation of molecules present

in archaeological material (Agozzino et al., 2001; Salvini et al.,

2008).

Siena is a typical Medieval town, developed on a hilly

ground, located in Central Italy, in a region called Tuscany.

Among the numerous churches and convents present in the

town, the Carmine Convent belonged to the order of the Car-

melitan monks and it was probably built in the second half of

the 13th century.The church, the courtyard, a open space, an orchard and

a rectangular building in the south-eastern part of the courtyard,

probably a store house, known by the written documents as thefondaco, formed the most ancient parts of the convent (Francovich

and Valenti, 2002). The Convent was restored and modified many

times between the 13th and 14th centuries. At the beginning of

the 14th century it overcame works to enlarge the structures of

the Convent. Among other rooms, a dormitory for the monks was

built on top of the fondaco (Francovich and Valenti, 2002). The

original first floor of this building was made bigger and a new

floor with walls of stone and bricks replaced the original one that

* Corresponding author at: Dipartimento di Chimica, Universita degli Studi di

Siena, via Aldo Moro, 53100 Siena, Italy. Tel.: 39 0577 234241; fax: 39 0577

234233.

E-mail address: [email protected](G. Giorgi).

Contents lists available atScienceDirect

Journal of Archaeological Science

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0305-4403/$ see front matter 2010 Elsevier Ltd. All rights reserved.

doi:10.1016/j.jas.2010.01.005

Journal of Archaeological Science xxx (2010) 15

Please cite this article in press as: Giorgi, G., et al., The meals in a Tuscan building yard during the Middle Age. Characterization of organicresidues in ceramic potsherds, J. Archaeol. Sci. (2010), doi:10.1016/j.jas.2010.01.005
mailto:[email protected]://www.sciencedirect.com/science/journal/03054403http://www.elsevier.com/locate/jashttp://www.elsevier.com/locate/jashttp://www.sciencedirect.com/science/journal/03054403mailto:[email protected]


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had earthen walls. It is supposed that this was done in order to

build a sleeping area for the monks, as some documents report

that in 1301 the town of Siena paid for this a large amount offiorini, the currency used at that time (Francovich and Valenti,

2002).

In order to build the upper floor, the ceiling of the first floor

was provided with a vault, and the empty space between the

vault and the new floor was filled with ceramics by using

a technique that goes back to the Roman times and was used in

other buildings of that period, like in Assisi and Prato, two towns

in Central Italy. In fact, the filling between the vault and the floor

needed not to be too heavy, in order not to break down the

ceiling and walls of the lower floor: the ceramic materials ful-

filled at all this aim, allowing to fill space without adding too

much weight (Fig. 1).

During the restoration works of the Convent started in 2001, the

vault wasdiscovered, with the great numberof ceramic objects that

were used as filling material of the vault. The portion of the vault

that has been investigated has dimensions 12 4 m.More than360

intact ceramic vessels have been recovered. It has been estimated

that about 868 ceramics objects were present with 20002500

pieces of ceramics. Most of the ceramic objects are discarded

material obtained from the ceramic manufacturing in thenumerous workshops present in the town. Only a few of them are

characterized by a coarse mixture and show burnt traces. This

suggests that they were fragments of pots and pans probably used

by the workers in the building yard, or in the convent, for cooking

the meals of the monks.

The characterization of the organic residues therein contained

should allow to obtain information on the original content of the

vessels and on life and dietary in the Medieval Age. With this aim,

we wish to report here on a gas chromatography-mass spectrom-

etry investigation of the organic residues absorbed in nine

potsherds taken from the ceramics recovered in the Carmine

Convent in Siena (Fig. 1,Table 1).

2. Experimental

2.1. Materials and sampling

All solvents used were pesticides analysis grade and purchased

from Merck (Milan, Italy).n-Octacosane, used as internal standard,

N,O-bis(trimethylsilyl)trifluoro-acetamide (BSTFA) and trimethyl-

chlorosilane were purchased from Sigma Aldrich (Milan, Italy).

Nine ceramic vessels were sampled and analyzed. Samples were

obtained by drilling small holes in the ceramic body after havingcleaned smoothly the surface. About 2 g of powder were recovered

from each sample. In order to make comparative and differential

analyses, when possible, more than one sample for each manufact

was taken.

A weighted amount of fine powder of each potsherd sample was

transferred in a vial and it was extracted by chloroform/methanol

(2:1 v/v, 10 mL, 2 15 min ultrasonication). An aliquot of the total

extract was derivatized using BSTFA containing 1% v/v trimethyl-

chlorosilane and maintained at 70 C for 40 min.

After solvent extraction, the residue was treated with 0.5 M

NaOH in MeOH/H2O (9:1 v/v, 10 mL). The mixture was heated at

70 C for 90 min in ultrasonic bath. After cooling, the saponified

mixture was centrifuged (2000 r.p.m., 20 min). 3 mL of the liquid

phase were acidified with 1 M HCl (20 drops) and extracted withchloroform (2 3 mL). The solvent was evaporated under

a nitrogen gas stream. The residues were left overnight in a vacuum

desiccator. Trimethylsilylation was then performed as described

above.

2.2. Gas chromatography-mass spectrometry

Gas chromatography-mass spectrometry (GCMS) analyses

were performed using a gas chromatograph Varian 3800 (Varian,

Walnut Crick, CA) equipped with a 30 m 0.25 mm (i.d.) fused

silica capillary column coated with a DB5 stationary phase (film

thickness 0.25mm). Ultra pure helium was the carrier gas. The gas

chromatograph is coupled with a Saturn 2000 ion trap mass

spectrometer (Varian, Walnut Crick, CA).

The column temperature was held at 50 C for 1 min immedi-

ately after injection, then the temperature was increased to 300 C

at 5 C/min and held for 10 min.

The mass spectrometer operated in the electron ionization

mode (70 eV) in the 40650m/zrange with source temperature of

150 C. The injector and the transfer line temperatures were

maintained at 280 and 170 C, respectively.

3. Results and discussion

The gas chromatograms obtained from the lipid extraction and

the alkaline treatment of the insoluble residues of the samples 19

show the presence of different classes of compounds, most of them

Fig.1. View of the ceramics characterized in this study. Ceramic objects used as filling

material (top); particular of the pan with holes 8 (bottom).

Table 1

Ceramic samples characterized in this study.

# Object description Part of the object analyzed

1 Pot Base

2 Pot Body

3 Pot Rim

4 Pan Body

5 Lid Body

6 Pot Base with calcareous deposits7 Pan Base

8 Pan with holes Base

9 Lid Base

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being fatty acids. On the basis of their content, the samples have

been divided into three main groups.

3.1. Group 1. Samples 1,3,4,5,7

Samples 1,3,4,5,7 are characterized by high amounts of fatty

acids of different nature. The most abundant species are palmitic

(C16:0), stearic (C18:0) and C18:1fatty acids (Fig. 2). While palmiticacid is abundant in nature and it can be found in almost all

animal and vegetable species, stearic acid can be related to

degraded animal fats (Mottram et al., 1999). The presence of its

unsaturated derivative C18:1can be related to the original content

of vegetable oils in the ceramic material (Evershed et al., 2002;

Mottram et al., 1999). Going deeply insights into the character-

ization of these samples, clear differences can be observed in the

relative amounts of the C16:0/C18:0 fatty acids. The inspection of

objects 1, 3 (pots), 4 (a pan) and 5 (a lid) suggests that they are

general purpose cooking vessels. In their extracts the C16:0/C18:0ratio is close to 1.

Furthermore, the presence of odd number fatty acids, such as

C15:0 and C17:0 and their branched forms,that might be produced by

ruminant animals due to the activities of gut bacteria, suggests thatthese vessels contained ruminant fats (Mottram et al., 1999).

Although GC-C-IRMS was not performed to verify this hypothesis,

these data are in agreement with archaeozoological studies that

have identified rests of ruminants, mainly sheeps and goats in the

vault (Francovich and Valenti, 2002).

Thus we propose that ceramics 1,35 can be considered as

cauldron potsherds (Mottram et al., 1999) and general purpose

cooking vessels, as their content is constituted by lipid residues of

different animal origin.

In contrast, in sample 7 (a pan), the C16:0 component is more

abundant than its higher homologue C18:0, and there are no odd

number fatty acids and their branched forms. All this suggests that

cooking of ruminant animals can be reasonably excluded for

sample 7. These results are similar tothose of the so called drippingdishes used to collect the fat from animal carcasses during spit

roasting (Mottram et al., 1999; Evershed et al., 2002), a typical

cooking procedurein Tuscany during the MiddleAge. The discovery

of some pig bones in the vault supports the idea that the pan was

used to cook pig meat, or that lard was used in the food processing.

The presence of an animal content in samples 1,35,7 is also

confirmed by the identification of cholesterol in their alkaline

extracts.

In samples3and4, methyl esters of C16:0, C18:0and of C18:1were

also found. These molecules are uncommon in archaeological

material. In fact it is known that they may undergo partial

decomposition in open air, likely by autoxidation (Rottlander,

1990). In the present case, the close dried space between the vault

and the upper floor has allowed a good preservation not only of the

ceramic material, as it is suggested by the presence of fatty acid

methyl esters, but also of paper and leather found in the filling

material of the vault.

Not only the pots and pans show the presence of some absorbed

organic residues, but also the lid (sample5). This is probably due to

an evaporation process and it allows to take into account also these

materials for the study of the ancient dietary habits.

3.2. Group 2. Sample 2

Sample2 has been obtained from the body of a pot. Its GCMS

trace and the list of compoundsidentified are reported in Fig. 3, top,

and inTable 2, respectively.

The results are almost different from those of the other samples:

in fact in this case the main component is the C18:1acid followed by

C16:0, and a minor amount of C18:0 with a ratio of 100:40:17. The

predominance of a monounsaturated derivatives suggests a vege-

table origin of thefatty acids,probably oliveoil. This is supported by

considering that laboratory degradation experiments performed on

olive oil absorbed in ceramic potsherds showed a lipid profile

similar to that obtained for sample 2 (Dudd et al., 1998). Further, the

alkaline treatment of the insoluble residue of sample 2 shows the

distinctive predominance of the azelaic acid, a bicarboxylic C9:0

acid, and high amounts of 9,10-dihydroxyoctadecanoic acid (Fig. 3,top,Table 2). These acids are related with the decomposition of the

oleic acid, that is particularly abundant in this sample (see above).

All this strongly suggests that this vessel has contained olive oil

(Regert et al., 1998).

On the other hand, the presence of cholesterol and of linear and

branched C15:0 e C17:0fatty acids, also found in sample 2, suggests

that this vessel might have been also used to cook animal meet. In

fact sample 2 is a pot and it might have been used in different times

to store the oil and eventually to cook meat broths.

The identification of olive oil markers in sample 2 is very

interesting. And indeed olive oil is supposed to be a very common

food in Tuscany and in the other Southern regions in Italy in the

Middle Age, and also nowadays, while in North Italy, where the

climate was too rigid for olive tree cultivation, lard was the mostcommon condiment used (Montanari, 2008; Cortonesi et al.,

2002). Nevertheless, some archaeological data contradict such

a concept, showing that the consumption of olive oil was limited

to some parts of the population, while lard and other animal fats

were more common, even in the Southern part of the Italian

Peninsula. Among other data, it is of some interest that the anal-

yses of more than 150 samples from medieval ceramic vessels, all

coming from Tuscany, carried out by us, show the presence of

olive oil only in a few of them. These results, together with

archaeobotanic data coming from different archaeological exca-

vations state that olive oil was less distributed than that we are

used to think.

It is noteworthy the presence of sample 2 in a convent: in fact

institutions, such as hospitals and convents, had better access to

10 20 30 40 50

60

C16:0C18:0

C18:1

C16:0 C18:0

C18:1

C16:0 C18:0

C18:1

C16:0 C18:0

C18:1R

elative

intens

ity

(arb.

units)

min

Fig. 2. Partial GCMS traces of the total lipid extract of samples 1, 3, 4, 5 (top to

bottom) showing the presence of fatty acids.

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foodstuffs than others, and they were provided with food in

general, and olive oil in particular, from the lands of which they

were owners (Belli et al., 2004).

3.3. Group 3. Samples 6, 8, 9

The content of the extracts obtained by samples6,8,9 is quite

poor and, differently from the other objects, the presence of fatty

acids was undetectable. This is an interesting result for twodifferent reasons: a) the very scarce presence of organic molecules

in these samples, that were collected in the same area of the others,

suggests that all the ceramic objects have not received environ-

mental contamination; b) from an archaeological point of view, it

shows that vessels6,8 and9were not used to contain vegetable or

animal oils, broth or any other food rich in fats. It is likely that

sample6 (base of a pot) was probably used to contain or to boil

water, and possibly vegetables and cereals, while sample9 (base of

a lid) might have been used to strain water, although the burnt

traceson the external part suggest that it wasexposedto the fire. Its

shape and the burnt traces in the outside and inside of the vessel

point to the possibility that it was used for roasting chestnuts,

a very common food during the Middle Age. In fact the form of the

pan is very similar to that of modern metal casseroles still used inTuscany for the same aim. To support this hypothesis, we per-

formed an experiment burning one hundred chestnuts in a ceramic

pan with holes, similar to that reported in Fig. 1, bottom. The

analyses of the samples recovered from the pan before and after the

experiment show that no organic residues are produced by this

activity, and that burnt traces are present in the inside of the vessel

due to the burning of the peel and in the outside due to the fire of

the stove. These results are compatible with those obtained for

sample9. Furthermore, we know that chestnuts were consumed in

the Carmine Convent, because chestnut peels were found in the

filling material of the vault, together with animal bones, fruit seeds

and other food waste.

It is noteworthy that, with the exception of sample 2, in all the

samples traces of dehydroabietic acid have been found. This is

10

12

3 4 5

6

7

8

9

11 1213

14

15

16

17

1819

2021

22

23

24

25

26

27

28

1

2

4

56

7

8

9

10 11

1213

14

15

16

17

19

20

21

22

23

2425

26

27 28

20 30 40 50 60 70

100

50

0

100

50

0

R

elativ

e

in

te

n

s

ity

(%)

min

Fig. 3. GCMS traces of the alkaline treatment of the insoluble residue of samples 2 (top) and 4 (bottom). The numbering corresponds to the compounds names as reported in

Table 2.

Table 2

Compounds found in the GCMS trace of pot 2 after hydrolysis. Their chemical

names, (common names in parentheses) and retention times (min) are also repor-

ted. TMS trimethylsilyl residue.

# Compound Retention time (min)

1 2-Hydroxypropanoic acid (Lactic acid) 2TMS 15:77

2 2-Hydroxyacetic acid 2TMS 16:44

3 Oxalic acid 2TMS 19:30

4 b-Hydroxybutyric acid 2TMS 20:41

5 Benzoic acid TMS 23:92

6 Octanoic acid (Caprylic acid) TMS 24:87

7 Glycerol 3TMS 25:92

8 a,u-Butanedioic acid (Succinic acid) 2TMS 27:30

9 N on an oic a ci d (Pela rgoni c a ci d) T MS 2 9:07

10 2 -Hydroxyheptanoic acid 2TMS 29:63

11 a,u-Pentandioic acid (Glutaric acid) 2TMS 31:17

12 Decanoic acid (Vapric acid) TMS 33:08

13 a,u-Hexanedioic acid (Adipic acid) 2TMS 35:30

14 a,u-Heptanedioic acid (Pimelic acid) 2TMS 39:02

15 a,u-Octanedioic acid (Suberic acid) 2TMS 42:47

16 a,u-Nonanedioic acid (Azelaic acid) 2TMS 45:92

17 Tetradecanoic acid (Myristic acid) 2TMS 47:40

18 a,u-Decanedioic acid (Sebacic acid) 2TMS 49:11

19 Hexadecanoic acid (Palmitic acid) methyl ester 49:82

20 Pentadecanoic acid TMS 50:59

21 a,u-Undecanedioic acid 2TMS 52:18

22 Hexadecanoic acid (Palmitic acid) TMS 53:76

23 Heptadecanoic acid (Margaric acid) TMS 56:57

24 11-trans-Octadecenoic acid TMS 58:64

25 11-cis-Octadecenoic acid TMS 58:84

26 Octadecanoic acid TMS 59:41

27 E icosanoic acid ( Arachic acid) TMS 64:70

28 2-Hydroxy-a,u-d ec anedioic a ci d 3 TM S 6 8:04

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a marker of resinous material fromPinaceaetrees, probably used as

covering material of ceramic manufacts. This shows that the habit

of a coarse coating in vessels was more common than that is usually

thought (Salvini et al., 2008).

4. Conclusions

This study was aimed at the characterization of the organic

residues in ceramic vessels found in a vault of the convent of

Carmine (Siena, Italy). These rests are probably waste of the meals

of the laborers of the yard or the monks that lived in the convent.

A GCMS approach, both on chloroform/methanol extracts

and owing to alkaline hydrolysis, has shown the presence of

different fatty acids, with well defined ratios, in the samples

analyzed. The differentiation of the extracts depends upon the

nature of the ceramic samples and suggests a different use of

these objects.

On the basis of the total lipid profiles, the nine objects can be

grouped into three main groups. The results obtained by samples1,

3, 4, 5, and 7, that constitute the first group, suggest that these

vessels might have been used to cook different kinds of foodstuffs,

including animals. This is in agreement with the identification of

bones of domestic animals, mainly ruminant, such as goats andsheep, in the convent. These animals were consumed mostly when

they were adults, after they had finished their working life. It was

common to boil their meat and the broth might be eaten with other

food, such as cereals, legumes, vegetables.

The olive oil traces in sample 2 seem to point out that this vessel

was surely used in the convent, while the animal origin of the

residues is in agreement with the so called practice of the

monopoly of the broths, a common practice in the Middle Age

(Giovannini, 1994).

Due to the absence of high amounts of animal fatty acids in pot

2, it is supposable that it was not used for extensive cooking of

animal meat, but mainly as olive oil container. In this sample

neither traces of dehydroabietic acid nor related acids were iden-

tified, excluding the presence of a waterproofing of the vessel.The absence of fatty acids in samples 6 and9 suggests that they

were used for containing or boiling water or other substances not

rich in fats.In particular, sample 8 mighthavebeenused asa colander

or to roast chestnuts, a common food during the Middle Age.

These results, together with others obtained by archae-

ozoological and archaeobotanical analyses, have yielded important

information on the use of the ceramic potsherds found in the

Carmine Convent in Siena and, as more generally, on the dietary

habits in a Tuscan building yard during the Middle Age.

Acknowledgements

The Archaeological project was carried out under the direction

of late Prof. Riccardo Francovich and Prof. Marco Valenti of the

University of Siena. The archaeobotanical data were analyzed under

the direction of Prof. Gaetano di Pasquale (University of Naples) and

the archaeozoological analyses have been carried out by Dr Franco

Salvadori (University of Siena).

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