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Archaeological Chemistry VIII
Publication Date (Web): October 15, 2013 | doi: 10.1021/bk-2013-1147.fw001
In Archaeological Chemistry VIII; Armitage, R., et al.;

ACS Symposium Series; American Chemical Society: Washington, DC, 2013.

ACS SYMPOSIUM SERIES 1147
Archaeological Chemistry VIII
Ruth Ann Armitage, Editor

Eastern Michigan University
Ypsilanti, Michigan
James H. Burton, Editor

University of Wisconsin-Madison
Madison, Wisconsin
Sponsored by the
ACS Division of History of Chemistry
American Chemical Society, Washington, DC
Distributed in print by Oxford University Press

Library of Congress Cataloging-in-Publication Data
Archaeological Chemistry VIII / Ruth Ann Armitage, editor, Eastern Michigan University,
Ypsilanti, Michigan, James H. Burton, editor, University of Wisconsin-Madison, Madison,
Wisconsin.
pages cm. -- (ACS Symposium series ; 1147)

"Sponsored by the ACS Division of History of Chemistry."
Includes bibliographical references and index.
ISBN 978-0-8412-2924-2 (alk. paper)
1. Archaeological chemistry--Congresses. I. Armitage, Ruth Ann. II. Burton, James H.
(James Hutson), 1950- III. American Chemical Society. Division of the History of
Chemistry.
CC79.C5A734 2013
930.1--dc23
2013038018
The paper used in this publication meets the minimum requirements of American National
Standard for Information Sciences—Permanence of Paper for Printed Library Materials,
ANSI Z39.48n1984.
Copyright © 2013 American Chemical Society
Distributed in print by Oxford University Press
All Rights Reserved. Reprographic copying beyond that permitted by Sections 107 or 108
of the U.S. Copyright Act is allowed for internal use only, provided that a per-chapter fee of
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Drive, Danvers, MA 01923, USA. Republication or reproduction for sale of pages in this
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PRINTED IN THE UNITED STATES OF AMERICA

Foreword
The ACS Symposium Series was first published in 1974 to provide a
mechanism for publishing symposia quickly in book form. The purpose of
the series is to publish timely, comprehensive books developed from the ACS
sponsored symposia based on current scientific research. Occasionally, books are
developed from symposia sponsored by other organizations when the topic is of

keen interest to the chemistry audience.
Before agreeing to publish a book, the proposed table of contents is reviewed

for appropriate and comprehensive coverage and for interest to the audience. Some
papers may be excluded to better focus the book; others may be added to provide
comprehensiveness. When appropriate, overview or introductory chapters are
added. Drafts of chapters are peer-reviewed prior to final acceptance or rejection,
and manuscripts are prepared in camera-ready format.
As a rule, only original research papers and original review papers are
included in the volumes. Verbatim reproductions of previous published papers
are not accepted.
ACS Books Department

Preface
The 12th Archaeological Chemistry Symposium was held as part of the
Spring ACS National Meeting in New Orleans, Louisiana, April 7–11, 2013.
This volume is a compilation of presentations from the Symposium, the latest in
a long tradition that began at the ACS National Meeting in Philadelphia in 1950.
Publication Date (Web): October 15, 2013 | doi: 10.1021/bk-2013-1147.pr001
The numbering of the symposia is, however, somewhat in question. According

to Brill (1), “…memories of only the First and Third Symposia remained clear
[at the 4th Symposium]… We leave it (with a blush) to the historians…to decide
upon the reality of the Second Symposium…”
The symposium consisted of four half-day symposia, an evening poster
session, and a keynote address by Dr. A. Mark Pollard, Edward Hall Professor of
Archaeological Science and Director of the Research Laboratory for Archaeology
and the History of Art at the University of Oxford. We choose four broad
categories for the symposia: Pigments, Residues and Material Analysis, X-Ray
Fluorescence Spectroscopy, and Isotopes in Archaeology. These categories are
by no means comprehensive. Rather, they serve as a snapshot perspective of
archaeological chemistry today and are necessarily biased toward our areas
of expertise and those of the participants in a chemistry meeting. Notably,
studies of ancient DNA and other advances in biomolecular archaeology are
underrepresented in this volume.
The papers herein show that archaeological chemistry today is more than the
usual studies of trace elements in pottery and lithics, which continue to contribute
to our understanding of human behavior in the past. New areas of research
include more focus on portability to analyze pigments in situ and artifacts in
museums, nascent developments in non- and minimally destructive chemical
characterization, new applications of isotopic analyses, and an increasing interest
in archaeological biomolecules.
This volume is divided into sections that roughly follow those of the
Symposium. The first section, Pigments and Dyes, begins with a review of
manuscript pigments by Dr. Mary Virginia Orna, the organizer of the 9th
Archaeological Chemistry Symposium and Editor of Archaeological Chemistry:
Organic, Inorganic, and Biochemical Analysis (2). Each of the following sections
begins with a review paper from one of our invited speakers. Dr. Valerie Steele,
now at the University of Bradford in the Department of Archaeological Science,
provides an overview of the state — for better and for worse — of analyses of
archaeological residues. Portable X-ray fluorescence instruments are becoming
extremely common in archaeological chemistry investigations; Dr. Aaron
Shugar of Buffalo State University provides in his chapter some perspectives and
warnings against the indiscriminate use of this technology. Finally, Dr. Matthew
xi
Sponheimer gives an overview of the contributions of stable carbon isotope and
trace metal studies in understanding early hominin diets.
The final chapter of the book provides a perspective on the earliest work
in archaeological chemistry in the 18th century and brings us up to today’s
challenges. We find ourselves in Dr. Pollard’s text, carrying out our own
research “on a wing and a prayer, ” as both the solitary chemist supported by her
institution in part for the accessible public interest aspect of her research and a
scientist within an anthropology department, fighting for funding in this era of
sequestration and downsizing. We hope that this volume contributes toward the
“open, respectful, meaningful and iterative dialogue across the many disciplinary
boundaries” encountered in archaeological chemistry (3).
We thank all of the contributors and reviewers for their time and effort.
We especially thank technical editor Arlene Furman of ACS Books for her
Publication Date (Web): October 15, 2013 | doi: 10.1021/bk-2013-1147.pr001
patience and help in producing this volume, and Seth Rasmussen, Tom Strom,
and Vera Mainz from the Division of the History of Chemistry (HIST) for all their
help in organizing and running the Symposium. HIST and the ACS Divisional
Activities Committee provided the majority of the funding for the Symposium,
with additional support from the Society for Archaeological Sciences and Bruker
Corporation.
References
1. Brill, R. H. In Science and Archaeology; Brill, R. H., Ed.; MIT Press:
Cambridge, MA, 1968, p x−xi.
2. Archaeological Chemistry: Organic, Inorganic, and Biochemical Analysis;
Orna, M. V., Ed.; ACS Symposium Series 625; American Chemical Society:
Washington, DC, 1996.
3. Pollard, A. M. In Archaeological Chemistry VIII; Armitage, R. A., Burton
J. H., Eds.; ACS Symposium Series 1147; American Chemical Society:
Washington, DC, 2013.
Ruth Ann Armitage

Professor, Department of Chemistry, Eastern Michigan University
Ypsilanti, Michigan 48197
734-487-0290 (telephone)
rarmitage@emich.edu (e-mail)
James H. Burton
Director, Laboratory for Archaeological Chemistry, Department of Anthropology
1180 Observatory Drive, University of Wisconsin-Madison
Madison, Wisconsin 53706
608-262-4505 (telephone)
jhburton@wisc.edu (e-mail)
xii
Editors’ Biographies
Ruth Ann Armitage

Publication Date (Web): October 15, 2013 | doi: 10.1021/bk-2013-1147.ot001
Ruth Ann Armitage, Professor of Chemistry at Eastern Michigan University,

earned a B.A. in Chemistry from Thiel College in 1993. She completed a Ph.D. in
Analytical Chemistry at Texas A&M University with Dr. Marvin Rowe in 1998 on
radiocarbon dating of charcoal-pigmented rock paintings. Her research is focused
on characterizing and dating archaeological and cultural heritage materials. She
has written and presented extensively her collaborative work with archaeologists
and museum conservation scientists on analyses of rock paintings, residues, and
colorants in textiles and manuscripts. In her 12 years at EMU, she has mentored
more than 25 research students.
James H. Burton
Dr. Burton, Director of the T. Douglas Price Laboratory for Archaeological
Chemistry, received a B.S. in Chemistry from the University of Virginia in 1979
and a Ph.D. in Geology from Arizona State University in 1986. His research
interests include the development of new archaeometric methods, particularly
the use of chemical and isotopic methods for provenience studies, not only for
traditional materials but also for humans who relocated. Current projects include
exploration of alkaline-earth elements and various isotopic systems in the study of
human mobility and the development of non-destructive methods to characterize
historical materials.
© 2013 American Chemical Society

Chapter 1
Artists’ Pigments in Illuminated Medieval

Manuscripts: Tracing Artistic Influences and
Connections—A Review
Publication Date (Web): October 15, 2013 | doi: 10.1021/bk-2013-1147.ch001
Mary Virginia Orna*
Department of Chemistry, The College of New Rochelle,

New Rochelle, New York 10805, U.S.A.
*E-mail: mvorna@cnr.edu
For the art historian, chemical analysis of pigments serves two

main purposes. It can confirm or deny the alleged attribution
or dating of a painting based on comparison with the known
painting practices of the artist or period. In addition, the
analysis of pigments can have a broader, and perhaps a more
profound, importance to the historian as a tool for understanding
more about the artistic process itself. This paper reviews the
collaborative building of a pigment database, tracing lines of
influence and interconnection between medieval centers of
manuscript production, clarifying periods of known usage of
several important artists’ pigments, the difference in pigment
usage between Armenian and Byzantine artists, the problems
involved with handling manuscripts directly, and anachronistic
pigment usage. The technical future of chemical analysis of
medieval manuscripts is also discussed.
Introduction
“Color is the most visual, pervasive example of the importance of chemistry to
our lives” (1). Though medieval artists could not have realized nor expressed this
observation since the formal discipline of chemistry would not exist for centuries
yet to come, color, for them, was the most visual and pervasive reality in their
pursuit of crafting the manuscripts they handed on to us as precious treasures of
their era. This paper will review the scientific identification of artists’ colors used
in manuscripts between the 10th and 16th centuries for the following purposes:

• To determine or confirm place of origin and date;
• To trace lines of influence between and among painting schools and
cultures;
• To recommend conservation & handling practice based on the content;
• To uncover forgeries (de-authentication);
• To specify attributions among different painters in a manuscript.
In addition to these objectives, Robert Feller (2) lists two additional ones:
objective description of method, and restoration. Although the identification
method used and described here consisted of extracting minute samples for
analysis by means of X-ray diffraction, infrared spectroscopy and measurement
of refractive index, this approach is now questionable in light of the availability
of newer, non-invasive techniques that allow the analyst access to the manuscript
in situ. The value of these methods will be discussed later in this paper.
The manuscripts described and analyzed in this work came from a variety of
Armenian and Byzantine workshops; the dates of their creation range from the
early 10th century to the late 16th century.
Pilot Project: The Gladzor (Glajor) Gospel Book of UCLA

The Gladzor Gospel Book (Armenian MS 1, UCLA) has been the subject
of very extensive study. Analysis of its palette by X-ray diffraction, Fourier
transform infrared spectroscopy and refractive index measurements yielded some
rather startling information: virtually all of the pigments used in its manufacture
were of mineral origin with the exception of red (madder) lake, which was
employed by all five of the artists who worked on the manuscript, and of gamboge,
used by the three “apprentice” artists who worked in an atelier other than that of
the two master painters (3, 4). A summary of pigment usage by atelier is given in
Table I; examples of two of the pigments is shown below in Figure 1.
Madder was derived from the roots of the Rubia tinctorum and other members
of the Rubiaceae family. It has been known from ancient times, having been
described by Strabo, Pliny the Elder, Dioscorides and the Talmud. Though most
often used as a dye, it could also be used as a pigment if precipitated on a solid
substrate such as aluminum hydroxide (5). Gamboge was another plant-derived
colorant taken from the sap or ooze of trees of the genus Garcinia. It, too, was
used extensively from ancient times (6). Since neither of these organic pigments
was used extensively in the manuscript, one could safely say that shielding the
work from light would not be a principal concern since mineral pigments are
virtually lightfast over indefinite periods of time. Such analyses are enormously
helpful to curators and conservators who must control the handling of such
precious documents.
Analysis of the Gladzor (Glajor is an alternative spelling) Gospel Book not
only yielded helpful information regarding conservation, but also was helpful in
specifying attributions among different painters in the manuscript. Differences in
the employment of the blue pigments indicated the involvement of two different
workshops: one used azurite (basic copper(II) carbonate) and high quality natural
4
ultramine, while the other used lesser quality natural ultramarine. The second
workshop also used a purple pigment that consisted of a mixture of red lake
and ultramarine; this occurred nowhere in the miniatures attributed to the first
workshop. Likewise, gamboge, used in the second workshop was not found
among the pigments of the first workshop (4).
Table I. Pigments Listed by Atelier as Used in the Gladzor Gospel Book (3, 4)
Hue “Master Painter” Atelier “Apprentice” Atelier
Black Charcoal black Charcoal black
Blue Azurite; Ultramarine Ultramarine + Ultramarine Ash
Brown Vermilion mixed with orpiment, Vermilion mixed variously with
gypsum and charcoal black orpiment, gypsum, charcoal black,
whiting and hydrated iron oxide
Flesh Orpiment mixed with realgar Orpiment mixed with realgar,
gamboge, gypsum and anhydrite
Gold Gold Gold
Green Orpiment mixed with azurite or Orpiment mixed with gamboge or
with ultramarine ultramarine plus anhydrite and a
trace of vermilion
Magenta Red lake or red lake mixed with Red lake
white lead
Olive Gamboge
Orange Minium or orpiment mixed with
minium
Purple Ultramarine mixed with red lake
Red Vermilion Vermilion
White Calcined bone mixed with quartz White lead
Yellow Orpiment Gamboge, or orpiment mixed with
massicot, or realgar mixed with
orpiment, gamboge and massicot
5
Figure 1. Two pigments found throughout the pages of the Gladzor Gospel
Book. Left: A photo-micrograph (130X magnification) of natural ultramarine.
(Photograph by M. V. Orna); Right: A broken-open sample of a madder root,
Rubia tinctorum (Photograph courtesy of Zvi C. Koren).
Additional Analyses of Armenian and Byzantine Manuscripts

Such a wealth of information was gathered from this pilot project that it was
deemed important to try to gather as much information from other Armenian
manuscripts to determine if there was indeed a traditional Armenian palette,
and also to compare this palette with manuscripts of different origins, such as
Byzantine, Persian, Iranian, etc. origins. Hence, the second phase of the study
comprised the analysis of the pigments of manuscripts in the United States and
Israel representing four distinct developments in the history of Armenian art:
A) manuscripts of Greater Armenia and Melitene in the 10th and 11th centuries;
B) manuscripts in the vicinity of Lake Sevan in the 12th to 14th centuries
(northeastern Greater Armenia); C) manuscripts in the vicinity of Lake Van in
the 14th and 15th centuries (central Armenia) (7, 8) and D) manuscripts of the
Armenian Kingdom of Cilicia in the 13th and 14th centuries (9). Table II is a
summary table of all twenty-four of the Armenian manuscripts analyzed by the
Cabelli-Orna-Mathews group (10). Figure 2 is an illustration from one of these
manuscripts, the monumental Trebizond Gospel, so-named from its find spot, but
likely to have been produced in the area of Tsamandos (11) in eastern Turkey
(12). In the pages following the summary, the results of the analyses are given
and are compared to Byzantine manuscripts at the University of Chicago (Table
III lists the ten manuscripts analyzed by Orna and Mathews (13, 14), nineteen
Iranian and eleven Indian manuscripts from the Vever Collection in the Arthur M.
Sackler Collection of the Smithsonian Institution (15), and eight Persian and three
Turkish manuscripts from the Spencer Collection of the New York City Public
Library (16).
Needless to say, it would be impossible to include the volume of data obtained
from these manuscripts in this paper, but some observations on the occurrence of
certain common pigments present in them will allow us to draw some conclusions
about pigment usage in the greater Middle East during the time period in question.
We must realize, of course, that this is a very small sampling of the entire corpus
of extant manuscripts of these genres, so any generalizations must be tentative.
With these caveats in mind, we have selected certain pigments of each observed
6
hue and listed in Table IV their occurrence on a percentage basis in each of the
types of manuscripts described above. Figure 3 is a bar graph of Table IV which
affords a basis for visual comparison.
Figure 2. Detail of the Evangelist Luke. Trebizond Gospel, San Lazzaro, Venice
1400/108 and 1925, fol. 299v. Courtesy of the Director, Mekhitarist Monastery
of San Lazzaro; photo credit: johndeanphoto.com.
Table II. Armenian Manuscripts

MS No. Name Date Origin
SL 1144/86 Queen Ml’ke Gospel 908-921 Lake Van (east)
W. 537 Gospels of the Priest 966
St. James 2555† “Second Ējmiatsin” ca. 1000
Gospels
SL 887/116 Adrianople Gospel ca. 1007 Thrace (Greece)
Continued on next page.
7
Table II. (Continued). Armenian Manuscripts
MS No. Name Date Origin
SL 1400/108 Trebizond Gospel mid-11th century Trebizond
1925
St. James 2556 Gospels of King ca. 1050
Gagik-Abas
FGA 33.5, Gospels fragment 1050 Melitene group
47.2-4
St. James 1924 Shukhr Khandara 1064-66 Melitene group
Gospels
SL 888/159 Karapet Gospel ca. 1200 Urfa, Cilicia
Chi MS 949 Red Gospels ca. 1237 Northern Armenia

FGA 32.18 Baron Vasik Gospel 1250 Hromkla, Cilicia
(T’oros Roslin)
FGA 44.17 Gospel of Hohannes 1253 Hromkla; Cilicia
W. 539 Gospel on vellum 1262 Hromkla, Cilicia
(T’oros Roslin)
PML 789 Gospels fragment 1296 Eastern Armenia
PML 622 Menologium 1348 Sis, Cilicia; (Sargis
Pitsak)
St. James 365 Isaiah Commentary ca. 1305 Eastern Armenia
UCLA Arm MS Gladzor Gospel Book ca. 1305 Gladzor, eastern
1 Armenia
MMA 38.171.2 John Incipit Leaf 1300-1310 Eastern Armenia
St. James 2360 Gospels of T‘oros ca. 1321 Eastern Armenia
Tarōnets‘i
St. James 1794 Khach‘en MS by the ca. 1327 Eastern Armenia
Monk T‘uma
St. James 1941 Sultaniya Gospels by 1334-1336 Eastern Armenia
Awag
W. 543 Khizan Gospels by 1455 Lake Van, Armenia
Khach‘atur
W. 540 Gospels 1475 Lake Van, Armenia
St. James 135 Hymnal of Martiros 1575 Lake Van, Armenia
Khizants‘i
FGA = Freer Gallery of Art, Washington, D.C. MMA = Metropolitan Museum of Art,
New York, NY. St. James = Monastery of Saint James, Jerusalem. SL = Monastery of
San Lazzaro, Venice. PML = Pierpont Morgan Library, New York, NY. W = Walters
Art Gallery, Baltimore, MD. UCLA = University of California, Los Angeles: University
Research Library, Special Collections. Chi = University of Chicago, Chicago, IL.
8
Table III. University of Chicago Special Collections Byzantine Manuscripts
Analyzed by FT-IR
MS No. Name Date
46 Haskell Gospels Late 13th Century
129 Nicolaus Gospels 1133
131 Chrysanthus Gospels Late 12th Century
232 Greek (Phillipps) Gospels 12th Century
727 Georgius Gospels Late 13th Century
879 Lectionary of Constantine the Reader Late 12th Century
948 Lectionary of Saint Menas the Wonderworker Late 12th Century
965 Rockefeller – McCormick New Testament Late 12th Century

972 Archaic Mark Mid-12th Century?
1054 Elfleda Bond Goodspeed Gospels 10th Century
Figure 3. Graphical Representation of the Data in Table IV.
9
Table IV. Percent of Pigment Occurrence in Medieval Manuscripts of 6
Different Origins
Pigment Armenian Byzantine Iranian Indian Persian Turkish
(24) (9)* (19) (11) (8) (3)
Bone- 0 0 0 0 62.5 33.3
black
Carbon 12.5 33.3 73.7 81.8 0 0
Black
Charcoal 0 0 0 0 12.5 66.8
Azurite 25.0 11.1 10.5 0 12.5 33.3
Blue
Indigo 66.8 0 73.7 54.5 0 33.3

Blue
Ultrama- 75.0 66.7 89.5 63.6 62.5 100
rine Blue
Malachite 0 0 10.5 45.5 25.0 33.3
Green
Vermilion 100 55.6 89.5 72.7 75.0 100
Red
Organic 70.8 44.4 84.2 90.9 0 0
Red
White 58.3 33.3 94.7 90.9 87.5 100
Lead
Orpiment 83.3 11.1 89.5 27.3 62.5 100
Yellow
*Only nine of the ten Byzantine manuscripts list in Table III are included in this analysis.
Chicago MS 972 is discussed separately.
Results and Discussion

At first glance, there seem to be some very clear dividing lines with respect
to pigment usage for certain areas. Taking each of the pigments in Table IV, and
comparing their usage with alternatives, yields some interesting conclusions.
Carbon Black: Use of this pigment in Armenian and Byzantine manuscripts
is moderate, in Iranian and Indian manuscripts, it is the predominant black, and
it is totally absent from Persian and Turkish manuscripts. Since both boneblack
and charcoal are also entirely absent in the Armenian and Byzantine manuscripts,
we can conclude that black was not a very important pigment. Since boneblack is
present in the majority of Persian manuscripts, and both charcoal and boneblack
are present in the Turkish manuscripts, we conclude that painters in those areas
preferred the use of these blacks as opposed to carbon black, possibily because of
greater availability of wood and bone in these areas.
10
Azurite: Azurite, basic copper(II) carbonate, is a blue pigment with a greenish
tinge. Its chemical formula is 2CuCO3·Cu(OH)2. It finds its greatest usage in
Armenian and Turkish manuscripts, with moderate usage in Byzantine, Iranian,
and Persian manuscripts, whereas it is totally absent from the Indian manuscripts
in the cohort. Again, availability may be a factor since azurite deposits throughout
Europe have been known since ancient times, but would more than likely have to
be imported into the Middle East and beyond. In addition, usage of indigo as a
viable alternative blue pigment is very prevalent in almost all of the Armenian,
Iranian, and Indian manuscripts.
Ultramarine Blue: Table IV conveys the fact that this blue pigment, obtained
from the semiprecious stone lapis lazuli, was almost universally used in the
manuscripts examined. While ultramarine, a clathrate compound of polysulfide
ions in a silicate cage structure, was highly prized in Europe and cost more than
gold, its major deposit was in Afghanistan, a location on the silk road trade route.
This can possibly explain its prevalence in Middle Eastern manuscripts since it
would not have been an import subject to price hikes of middlemen along the way.
Malachite Green: Malachite, the gemstone as opposed to the organic dye of
the same name, is another basic copper(II) carbonate variant with the formula
CuCO3·2Cu(OH)2. Curiously, it is totally absent from the Armenian and Byzantine
manuscripts examined, but finds moderate usage in the other types of manuscripts.
The nearest deposits would have been the Timna Valley, Israel, and the Russian
Urals.
Vermilion Red: Evidence of this pigment’s almost universal usage is found
in Table IV. It is often the most prevalent red pigment in any ancient or medieval
sample. Known from ancient times as its natural ore, cinnabar, mercury(II)
sulfide, HgS, was also synthesized by heating elemental mercury and elemental
sufur together. Large deposits of cinnabar were, and are, found in China and in
Almaden, Spain. While it was highly prized as a pigment, its great cost led to the
use of lesser red pigments along with it: many of the manuscripts we examined
also contain organic red pigments like madder (alizarin) and cochineal (carminic
acid) (14). The latter has its origin in the “Old World” in the form of a colorant
derived from the egg sacs of scale insects of the genus Kermes, whereas its “New
World” source was the scale insect of the genus Dactylopius (18).
White Lead: Basic lead(II) carbonate, 2PbCO3·Pb(OH)2, is another highly
prized pigment used from ancient times. It was manufactured by corroding
elemental lead with vinegar in the presence of carbon dioxide (often produced
by the fermentation of hot horse dung). In the manuscripts we examined, we
see its prevalence increase the farther east we go, the Turkish manuscripts being
an exception. The Iranian, Indian, and Persian manuscripts examined used only
white lead, while silicates are present in the Armenian and Byzantine manuscripts.
Orpiment: This yellow mineral pigment, As2S3, enjoyed great usage in
Armenian, Iranian, Persian, and Turkish manuscripts, but moderate to little usage
in Indian and Byzantine manuscripts. Due to availability, the Indian manuscript
painters preferred to employ Indian Yellow, while Byzantine artists preferred to
use organic yellow pigments derived from plants. Realgar, As4S4, is a red arsenic
sulfide often found associated with orpiment in mineral deposits.
11
Gypsum is calcium sulfate dihydrate, CaSO4·2H2O. Anhydrite is its
anhydrous form.
Massicot is the yellowish to reddish-yellow orthorhombic form of lead(II)
oxide, PbO. The tetragonal form of PbO is called litharge.
Although these analyses have not yielded information enabling the
determination or confirmation of the place of origin and date of these manuscripts,
we can say at least that the pigments used correspond to the accepted known
usage periods, with one exception, as we will see in the next section. However,
the analyses have allowed us to take tentative steps toward tracing lines of
influence between and among painting schools and cultures; to recommend
conservation and handling practice based on the content, and in one instance, that
of the Gladzor Gospel Book, to specify attributions among different painters in a
manuscript. So, we have shown that virtually all the purposes associated with the
scientific identification of the colors used in manuscripts have been fulfilled with
one exception: uncovering forgeries. For this, we must return to an anomalous
manuscript grouped with the Byzantine manuscripts in Table III.
The “Archaic Mark,” Chicago MS 972 (Gregory-Aland MS

2427)
We have deliberately omitted this manuscript from the above analysis because
of the occurrence of an anachronistic pigment on many pages of this manuscript.
Figure 4 shows two infrared spectra. The bottom spectrum was obtained from
a blue pigment from MS 972 (2427); the top spectrum is a reference spectrum
of Prussian blue. The band corresponding to the C≡N of ferric ferrocyanide
is common to both spectra. Replicate spectra of blue pigments removed from
different locations in MS 972 (2427) indicate that the average frequency of this
band is 2083 ± 6 cm-1. The ubiquitousness of an iron blue in this manuscript raises
doubts about its authenticity. Figure 5 is a detail from folio 34v, the location of
the Prussian blue sample from which the spectrum in Figure 4 was derived.
The iron blues are the first of the artificial pigments with a known history
and an established date of first preparation. The color was made by the Berlin
color makers Johann Jacob Diesbach and Johann Konrad Dippel (1673-1734)
in or around 1706 (17). Moreover, the material is so complex in composition
and method of manufacture that there is practically no possibility that it was
invented independently in other times and places (18, 19). This fact, in addition
to the evidence indicating that both MS 972 (2427) and a Gospel fragment from
the Hermitage Museum, St. Petersburg (20), were copies of a late 12th century
gospel book in the National Library of Greece, codex 93 (21), suggests that these
manuscripts originated some time much later than their purported 12th century
fabrication. Furthermore, neither of these manuscripts has a geneaology that can
be traced prior to 1930, a fact suggesting that their origin very well may be during
the flurry of Athenian forgeries that came to the market in the 1920s (13).
12
Figure 4. Fourier-Transform Infrared Spectrum of folio 34v, Ms. 972 (2427),

the “Archaic Mark.”, and Archaeological Chemistry, IV. Reproduced with
permission from reference Orna, M. V.; Lang, P. L.; Katon, J. F.; Mathews, T.
F.; Nelson, R. S. Applications of infrared microspectroscopy to art historical
questions about medieval manuscripts. In Allen, R.O., Ed. Archaeological
Chemistry, IV (Advances in Chemistry Series, 220). American Chemical Society:
Washington, D.C., 1989; pp. 265-288. Copyright 1989, American Chemical
Society (13).
In 2006, the University of Chicago Library and the University of Chicago

Divinity School moved to lay to rest once and for all the questions that arose from
our study and from some later studies done by Abigail B. Quandt of the Walters
Art Gallery by calling for further research (22). Thanks to funding provided by an
anonymous donor, McCrone Associates, Inc. of Westmont, Illinois, was charged
with taking samples of the manuscript, specifically from the parchment, the ink,
and a range of paints in the manuscript illuminations, and for all the spectrographic
analysis carried out on them. The determined goal was, for the first time, to make a
comprehensive chemical examination of all components of the codex (parchment,
ink, paints and coatings), utilizing the most current technologies available (23).
The McCrone report (24) unambiguously reconfirmed our initial finding
of Prussian blue, an invention of the early 18th century, in the manuscript.
Furthermore, the report documented the presence of additional materials that were
incongruent with a 12th date, namely, zinc white (ZnO), not used as a pigment
until about 1780, and blanc fixe, a synthetic form of barium sulfate introduced
in the 1820s. The report also said that the combination of zinc white and blanc
fixe suggested the presence of lithopone, or Orr’s white, which was not invented
until 1874. These findings alone placed the manuscript, at its earliest, at the latter
13
part of the 19th century. Furthermore, infrared spectroscopy also indicated the
presence of cellulose nitrate most likely used as a binding medium; it was only
in 1920 that this material became widely available. Finally, almost three months
later, the report on the radiocarbon dating of the manuscript parchment gave a
calibrated (95% confidence) date range of 1461-1640 (25), indicating that the
forger(s) used old parchment, but apparently, not old enough!
Figure 5. Folio 34v, Chicago Ms 972 (2427), the “Archaic Mark.” The blue
pigment in this miniature was analyzed by FT-IR (spectrum above) and found to
be Prussian blue. Courtesy Special Collections Research Center, University of
Chicago Library.
In a video produced by the University of Chicago and broadcast on 26 October

2009 (26), Dr. Margaret M. Mitchell, one of the principal investigators on the
Archaic Mark project, announced the results of the investigation. She first stated
the importance of the discovery because of all the New Testament manuscripts
extant, the Archaic Mark had the highest degree of correspondence with Codex
Vaticanus, the oldest complete text of the Gospel of Mark (4th century). She then
announced that the manuscript, purchased by the university in 1941, is a modern
production that was fabricated between 1874 and the first decades of the 20th
century, and would no longer be included in critical editions of the Greek New
Testament. However, she also pointed out the value of the data collected insofar
as it will help ongoing scholarly investigations into and detection of manuscripts
forged in the modern period.
14
The Future of Illuminated Manuscript Analysis
All of the examples cited above, including the very recent re-analysis
of the “Archaic Mark,” were done by extraction of minute particles from the
manuscripts, and then subsequent small particle analysis by a variety of means,
including X-ray crystallography, Fourier transform infrared microspectroscopy,
polarized light microscopy, chemical microscopy, scanning electron microscopy
with X-ray fluorescence analyzer and X-ray fluorescence. These methods, though
highly sophisticated, are almost universally available to the analytical chemist.
A very promising method that until about a decade or so ago has not been
universally available is micro Raman spectroscopy, or Raman microscopy (RM),
a method capable of delivering unambiguous results without the necessity of
removing small particles from the manuscript, and therefore a method most dear
to the heart of any curator of precious manuscripts. Furthermore, according

to the doyen of RM, Robin J. H. Clark (27), the method can identify mixtures
of pigments at high spatial (≤ 1 μm) resolution and down to even picogram
quantities, is non-destructive, largely immune to interference, and able to be
applied to manuscripts in situ, and even to identifying the reaction products of
inorganic pigments that have degraded on the manuscript page (28). Difficulties
arise when organic pigments are present as they are both prone to photochemical
degradation and to fluorescence. A typical RM instrument is shown in Figure 6.
Figure 6. A typical RM Spectrometer (Horiba LabRAM) equipped with EDGE

filters, 10, 50 and 100X objectives and telecamera. Courtesy of the University of
Modena and Reggio Emilia, Italy. Photograph: M. V. Orna.
15
Another difficulty to overcome initially was the lack of a comprehensive guide
to the pigments used in antiquity and a library of their Raman spectra for the sake
of comparison. By dint of hard work over a period spanning more than six years,
Clark and his co-workers succeeded in assembling pigment databases (29, 30)
that have become among the most cited papers in art conservation science. From
their first major success in identifying the pigments in a 13th century Paris bible
(31), the Clark team has gone on to identify and characterize yellow pigments in
manuscripts (32), examine spectroscopically almost 200 manuscript cuttings and
miniatures from a variety of Italian schools (33), and establish the palette of 16th
and 17th century Persian manuscripts (34), among many other projects summarized
in a Chemistry in New Zealand review article (35). Using RM, another team based
at Trinity College, Dublin, succeeded in confirming the pigment analysis work
done on the famed Book of Kells over the course of the past 60 years (36). New
data on RM analysis of Armenian manuscripts from Yerevan, Armenia, is being

developed by an Italian team headed by Pietro Baraldi anYeghis Keheyan (37). It
is to be hoped that their data can be profitably added to the database discussed in
this paper.
In addition to the spectral databases cited above, a cooperative database of
IR (in the mid-infrared range) and Raman spectra pertinent to cultural heritage
materials has been developed by the Infrared and Raman Users’ Group (IRUG)
and is available online at www.irug.org. Its most recent peer-reviewed edition
contains over 2000 peer-reviewed spectra.
Another analytical tool, terahertz time-domain spectroscopic imaging
(THz-TDSI), is becoming quite popular in the area of evaluation and conservation
of works of art. The availability of the technique is growing rapidly, as is
evidenced by the recent multi-session symposium held on the topic at the
245th American Chemical Society National Meeting at New Orleans, Louisiana
during the week of April 7-11, 2013. And this one technique seems to be able
to fulfill all of the requirements for examination of historical artifacts – to be
non-destructive, non-invasive, spatially precise, and applicable in situ (38). While
these are attributes of RM as well, THz-TDSI has another that is fast making
it indispensable, i.e., imaging that includes THz tomography which can give
non-invasive cross section images of works of art (39). Furthermore, as in the
mid-infrared region, THz frequency spectra exhibit fingerprint-like absorption
bands of substances of cultural heritage interest.
The frequency of the THz range is from 0.1 to 10 THz (3 – 300 cm-1, i.e.,
between the far infrared and radar regions of the spectrum). Its use as an analytical
tool was limited in the past by the lack of stable THz sources as well as by the
necessity of custom building the necessary apparatus. Although these technical
difficulties have largely been solved and there are several commercial instruments
now on the market, an ongoing problem for THz users in art conservation was the
lack of a suitable database comparable to the IRUG database. This problem is also
in the process of being solved by the establishment of an online spectral database of
artists’ materials (www.thzdb.org) which, as of the writing of this paper, contained
over 1500 spectra obtained by FT-THz in transmission and reflection modes, and
by THz-TDSI in transmission mode (40). It seems that THz-TDSI is rapidly
16
catching up with RM and that the two together will form a formidable partnership
in the future analysis of cultural heritage artifacts.
References
1. Freemantle, M. C&EN, February 26, 2001, p 50.
2. Feller, R. L., Ed.; Artists’ Pigments: A Handbook of their History and
Characteristics; National Gallery of Art: Washington, DC, 1986; Vol. I.
3. Orna, M. V.; Mathews, T. F. Stud. Conserv. 1981, 26, 57–72.
4. Mathews, T. F.; Sanjian, A. K. Armenian Gospel Iconography: The tradition
of the Glajor Gospel, with contributions by Mary Virginia Orna, OSU,
and James R. Russell; Dumbarton Oaks Research Library and Collection:
Washington, DC, 1991; pp 48−51 and 227−230.

5. Schweppe, H.; Winter, J. Madder and Alizarin. In Artists’ Pigments: A
Handbook of their History and Characteristics; FitzHugh, E. W., Ed.; Oxford
University Press: New York; Vol. 3, pp 47−79.
6. Hanelt, P., Ed.; Mansfield’s Encyclopedia of Agricultural and Horticultural
Crops (except Ornamentals); Springer: Heidelberg, Germany, 2011; pp 1352
ff.
7. Cabelli, D. E.; Mathews, T. F. J. Walters Art Gallery 1982, XL, 37–40.
8. Cabelli, D. E.; Mathews, T. F. Revue des études arméniennes, n.s. 1984,
XVIII, 33–47.
9. Cabelli, D. E.; Orna, M. V.; Mathews, T. F. Analysis of Medieval Pigments
from Cilician Armenia. In Archaeological Chemistry, III; Lambert, J.
B., Ed.; Advances in Chemistry Series 205; American Chemical Society:
Washington, DC, 1984; pp 243−254.
10. Mathews, T. F.; Wieck, R. S. Treasures in Heaven: Armenian Illuminated
Manuscripts; The Pierpont Morgan Library: New York and The Princeton
University Press: Princeton, NJ, 1994; p 136.
11. Bell, G. Amurath to Amurath: A Journey along the Banks of the Euphrates,
1st ed.; W. Heinemann: London, 1911; p 345.
12. Mathews, T. F. The Kars-Tsamandos Group of Armenian Illuminated
Manuscripts of the Eleventh Century. Philopation: Studies in Honor of Arne
Effenberger; Romisch-Germanisches Zentralmuseum: Mainz, Germany,
2013.
13. Orna, M. V.; Lang, P. L.; Katon, J. F.; Mathews, T. F.; Nelson, R. S.
Applications of Infrared Microspectroscopy to Art Historical Questions
about Medieval Manuscripts. In Archaeological Chemistry, IV; Allen, R.
O., Ed.; Advances in Chemistry Series 220; American Chemical Society:
Washington, DC, 1989; pp 265−288.
14. Lang, P. L.; Orna, M. V.; Richwine, L. J.; Mathews, T. F.; Nelson, R. S.
Microchem. J. 1992, 46, 234–248.
15. FitzHugh, E. W. Study of Pigments on Selected Paintings from the Vever
Collection. In An Annotated and Illustrated Checklist of the Vever Collection;
Lowry, G. D., Beach, M. C., Eds.; Arthur M. Sackler Gallery, Smithsonian
Institution: Washington, DC, 1988; p 426.
17
16. Data supplied by Barbara Schmitz.
17. Kraft, A. Bull. Hist. Chem. 2008, 33 (2), 61–67.
18. Orna, M. V. The Chemical History of Color; Springer: Heidelberg, Germany,
2013; p 57.
19. Gettens, R. J.; Stout, G. L. Painting Materials: A Short Encyclopedia; Dover
Publications: Garden City, NY, 1966; pp 20−21.
20. Treu, K. Die grieschischen Handschriften des neuen Testaments in der USSR;
Akademie-Verlag: Berlin, Germany, 1966; pp 229−230.
21. Marava-Chatzinicolaou, A.; Toufexi-Paschou, C. Catalogue of the
Illuminated Byzantine Manuscripts of the National Library of Greece;
Publications Bureau of the Academy of Athens: Athens, 1978; Vol. 1, pp
224−243.
22. Mitchell, M. M.; Duncan, P. A. Novum Testamentum 2006, 48, 1–35.
23. Mitchell, M. M.; Barabe, J. G.; Quandt, A. B. Novum Testamentum 2010, 52,
101–33.
24. Private communication to Patricia A. Gibbons (University of Chicago) from
Joseph G. Barabe (McCrone Associates), dated July 21, 2008; 61 pp.
25. Private communication to Joseph G. Barabe (McCrone Associates) from A.
J. T. Jull (NSF Arizona AMS Laboratory), dated October 9,2008.
26. Mitchell, M. M. University of Chicago Video broadcast on October
26, 2009. http://mindonline.uchicago.edu/media/communications/news/
archaic_mark_10262009_512k.mov (accessed on February 5, 2013).
27. Everts, S. C&EN, December 17, 2012, p 36.
28. Clark, R. J. H. Chem. Soc. Rev. 1995, 187–196, DOI: 10.1039/
cs9952400187.
29. Bell, I. M.; Clark, R. J. H.; Gibbs, P. J. Spectrochim. Acta, Part A 1997, 53,
2159.
30. Burgio, L.; Clark, R. J. H. Spectrochim. Acta, Part A 2001, 57, 1491.
31. Best, S.; Clark, R.; Daniels, M.; Withnall, R. Chem. Br. 1993 February,
118–122.
32. Clark, R. J. H.; Cridland, L.; Kariuki, B. M.; Harris, K. D. M.; Withnall, R.
J. Chem. Soc. Dalton Trans. 1995, 2577–82.
33. Burgio, L.; Clark, R. J. H.; Hark, R. R. Proc. Nat. Acad. Sci. U.S.A. 2010,
107 (13), 5726−5731. www.pnas.org/cgi/doi/10.1073/pnas.0914797107.
34. Muralha, V. S. F.; Burgio, L.; Clark, R. J. H. Spectrochim. Acta, Part A 2012,
92, 21–28.
35. Clark, R. J. H.Chem. N. Z., January 2011, pp 13−21.
36. Bioletti, S.; Leahy, R.; Fields, J.; Meehan, B.; Blau, W. J. Raman Spectrosc.
2009, 40, 1043–1049.
37. Baraldi, P.; Eliazian, G.; Keheyan, Y. A Study on the Polychromy
and Technique ofSome Armenian Illuminated Manuscripts by Raman
Microscopy, 2013, in press and private communication.
38. Jackson, J. B.; Mourou, M.; Whitaker, J. F.; Duling, I. N., III; Williamson, S.
L.; Menu, M.; Mourou, G. M. Opt. Commun. 2008, 281, 527–532.
39. See for example, Adam, A. J. L.; Planken, P. C. M.; Meloni, S.; Dik, J. Opt.
Express 2009, 17, 3407.
40. Fukunaga, K.; Picollo, M. Appl. Phys. A 2010, 100, 591–597.
18
Chapter 2
Investigation of Ancient Roman Pigments by

Portable X-ray Fluorescence Spectroscopy and
Polarized Light Microscopy
Ruth F. Beeston*,1 and Hilary Becker2

1Department of Chemistry, Davidson College,
Davidson, North Carolina 28035
2Department of Classics, University of Mississippi,
University, Mississippi 38677

*E-mail: rubeeston@davidson.edu
The subject of this study is a collection of raw pigments from

a second to early fourth century C.E. pigment shop located
in the Area Sacra di S. Omobono, in the Forum Boarium in
Rome. The shop was excavated in 1974, yielding a total of
more than two kilograms of blue, light blue, green, yellow,
orange, red, pink, and white pigments. An ongoing project
to re-examine materials from this excavation resulted in an
opportunity to study this remarkable pigment collection. A
Bruker Tracer III-SD portable X-ray fluorescence spectro-meter
was used to determine major, minor and trace elements present
in representative samples of each pigment. On this basis, the
types of pigments available for trade in this ancient marketplace
were identified as Egyptian blue (two prep-arations), green
earth, at least five distinct iron earth pigments (red, yellow, and
orange ochres) and lime white (calcium carbonate). Additional
characterization of select pigment samples was conducted
using polarized light microscopy. Particle characteristics
observed under transmitted and reflected light and between
crossed-polars were compared to those observed for reference
samples of historical pigments.

Background
The scientific examination of colorants used in antiquity has a long history,
beginning with the characterization of pigment samples from Rome and Pompeii
by Jean-Antoine Chaptal and Sir Humphry Davy in the early 19th century (1).
Pigment studies have been motivated by the desire to understand more fully the
materials and methods of ancient artists, to attribute objects to particular time
periods more accurately, to re-imagine the original appearance of painted objects,
and to determine appropriate treatments for the conservation of painted surfaces. A
great deal is now known about the availability and origins of natural and synthetic
pigments in antiquity and the techniques used to apply them to wall paintings,
sculpture, architecture, and pottery.
Much of what we know about pigment use by the Greeks and Romans
comes from ancient literary sources, including De Lapidibus by Theophrastus,

De Architectura by Vitruvius, and Historia Naturalis by Pliny the Elder.
Other information relating to the procurement of colorants has been gathered
through experimental archaeology, including efforts to recreate processes for
the production of manufactured pigments such as Egyptian blue (2, 3) and the
extraction of Tyrian purple from murex snails (4).
Most studies involving the scientific analysis of ancient pigments require the
examination of samples removed from painted surfaces or in situ analysis using
non-destructive techniques. Because painting methods involve incorporating
the pigments into the surface layer of lime mortar applied to a wall or other
support (fresco technique), or mixing powdered pigments with an organic binder
such as wax, egg, gum, or oil (secco techniques), pigment analyses are usually
complicated by the presence of mixtures of materials. The application of pigment
to a surface typically results in a complex, multi-layered structure that requires
careful sampling and interpretation. Further complications can be introduced by
surface weathering, deterioration due to the burial environment, discoloration
reactions, improper cleaning of painted objects, and modern restorations. Despite
these complications, many successful studies involving the analysis of pigments
found in Roman wall paintings have been conducted (e.g. (5–8)).
In more unusual instances, deposits of raw, unadulterated pigments ready
for use by ancient artists have been uncovered and studied. These finds present
archaeologists with unique glimpses into the practice of painting through the
observation of the pure raw materials available to artists. Commercial spaces,
such as workshops and shops for production and sale of colorants, a number of
which were uncovered in Pompeii, offer the opportunity to study not just pigment
composition but also the economics of the pigment industry in antiquity (9, 10).
There is even a house that was in the process of being painted on the day of the
eruption of Mt. Vesuvius, the “House of the Painters at Work” (Casa dei pittori
al lavoro (IX, 12, 9)) in Pompeii. The excavation of this house revealed pigments
in their pure form (contained in roughly 50 ceramic vessels), containers of lime
plaster, artists’ tools, along with frescoes that were only partially finished at the
time of the fateful eruption (10, 11).
Pigments were an important commodity for the production of frescoes and the
decoration of architectural elements as well as for use in cosmetics and medicinal
20
preparations. The economic values of pigments varied based on availability, the
intensity of the hue, the distance from the source to the place of sale, and the
difficulty in manufacturing or processing the colorant. Pliny (HN 35.30) describes
a distinction between “florid” pigments (floridi colores), those that are rare and
highly valuable, such as cinnabar and purple, and “austere” pigments (austeri),
those that are common, abundant, and less brilliant, including the earth pigments.
One of the motivations for this study was to understand better the trade in colorants
in the Roman world during the first through fourth centuries C.E.: What pigments
could one easily purchase in a marketplace? Were they mined or manufactured
locally? How do they compare to the colorants described in literary sources?
The Pigment Shop at Area Sacra di S. Omobono

The pigment samples that are the subject of this study originate from a pigment
shop dating to the second to early fourth centuries C.E. located in the Forum
Boarium in Rome. The pigment shop was excavated in 1974, and the function of
the shop was immediately apparent to those excavating (12). It was one of several
shops built on the podium of twin temples dedicated to Fortuna and Mater Matuta
in the Forum Boarium, located adjacent to the Tiber River. The pigment shop
consisted of two rooms, but pigments were found only in the front room that faced
a street. The pigments were found along with occasional sherds of commonware
pottery mixed in with earth of the two occupation layers of this store. Significantly,
this pigment shop is, to date, the only extant pigment shop from ancient Rome
and so provides a fascinating opportunity to see the supply-side of an important
commodity in ancient Rome.
An initial report of chemical analysis of some of the pigments was published
by Maria M. Capasso in the contemporary excavation report in 1978. Selected
pigment samples were examined by Marisa Laurenzi Tabasso at the Istituto
Centrale del Restauro in Rome using microchemical testing and non-dispersive
x-ray fluorescence; a limited number of elements (Ca, Cu, Fe, Sn, and Pb) were
detected and reported (13). The pigments were rediscovered in 2009 as part of
a systematic effort to re-examine the stratigraphy and material remains revealed
by past excavations of the site. The scientific examination of the pigments was
initiated in 2011.
Techniques for Pigment Characterization

Numerous analytical techniques have been applied to the identification and
characterization of ancient pigments. Noninvasive methods applied to painted
surfaces include infrared and ultraviolet photography, portable x-ray fluorescence
spectrometry, and, more recently, Raman scattering. Where sampling is an option,
the examination of pigment particles via polarized light microscopy, scanning
electron microscopy with energy dispersive x-ray analysis, and microchemical
testing can give valuable information about particle properties and elements
present in the sample. X-ray diffraction and IR and Raman spectroscopy provide
more detailed information about the specific compounds and polymorphs present
in a pigment sample.
21
For this study, portable x-ray fluorescence spectroscopy (pXRF) was
conducted on-site, allowing the determination of characteristic elements present
in each sample. In this method, the sample (lump of raw pigment or powdered
material) is excited by a beam of x-rays from an x-ray tube, causing the ejection
of core electrons from the atoms at the surface of the sample. As higher energy
electrons fall to fill these vacancies, characteristic x-rays are emitted by the
atoms. The x-rays are detected and a plot of intensity (number of photons)
versus energy of the transition (keV) is displayed. The elements present give
rise to characteristic peaks in the spectrum, enabling the user to identify major,
minor, and trace elements in the sample. Disadvantages of the method include
the fact that elements lighter than magnesium are not detected, and the spectrum
cannot be relied upon for quantitative information without very careful analysis
of standards that are closely related to the samples under study. An excellent
source of information about applications and limitations of pXRF as a tool for

examination of archaeological samples can be found in a recent book edited by
Shugar and Moss (14).
In addition to characterization by pXRF, the technique of polarized light
microscopy (PLM) was utilized to examine selected pigment samples from S.
Omobono. This technique allows the determination (and comparison to reference
samples) of particle properties such as color, transparency, size distribution,
refractive index, behavior under crossed polars, and purity. The presence of
combinations of particles can provide evidence for particular types of pigments
or for the mixing of pigments to produce various hues.
Materials and Methods

Samples for analysis were selected from over 15 containers each holding up
to 450 g of raw pigments in lump or pellet form, sorted by color and kept in
storage since their discovery during the 1974 excavation season. Sample labels
used here include the pigment color and sacchetta number previously assigned to
each container.
Most samples were analyzed without disturbing the surface, but in some cases
the surface was scraped with a porcelain spatula to reveal a fresh layer, and in other
cases powdered samples were produced by crushing a portion of a lump or pellet
in a porcelain crucible. Historical pigment samples used for comparison purposes
were obtained from Kremer Pigments, Inc. (New York) and Zecchi (Florence).
XRF spectra were collected using a Bruker Corporation Tracer III-SD portable
XRF spectrometer. Samples were placed on a 2.5 inch diameter disc of 40μm
gauge polypropylene film (Premier Lab Supply) placed directly over the x-ray
window on the stage. The instrument was operated with S1PXRF software with a
timed run time of 240 seconds. Two sets of conditions were used for each sample.
For detection of low mass elements (Al, Si, P, Cl, S, K, Ca, C, Cr, and Fe), the
“Blue” filter (0.001" Ti) was installed and the portable vacuum pump was turned
on. Voltage was set to 15 keV with a current setting of 22.8 μA. To optimize
detection of higher mass elements, the “Green” filter (0.003" Cu, 0.001" Ti, 0.012"
Al) was installed, as recommended by the manufacturer for analysis of silicate and
22
ceramic materials as well as colorants. No vacuum was applied, and the instrument
was set to 40 keV and 14 μA.
pXRF spectra were processed and analyzed using ARTAX software. The
broad signal centered at 19 keV (Compton backscatter peak) and peaks for Rh
(Kα, 20.22 keV; Kβ, 22.72) and Pd (Kα, 21.18 keV; Kβ, 23.82 keV) arise from
the x-ray target and detector collimator, and are ignored in the spectra, since these
are unrelated to the sample. Most spectra revealed a small peak at 25.27 keV,
characteristic of Sn. However this peak may also be attributable to a Pb sum peak
(14). The presence of Sn is only noted in the results presented here when both Kα
and Kβ peaks can be discerned. It should also be pointed out that trace signals
for other elements (Fe, Ni, Cu, Zn) may also arise from the instrument rather than
the sample, depending on instrument parameters and sample density. Finally, large
peaks for certain elements may mask the presence of trace peaks for other element.
Selected pigment pieces were packaged into vials, and with appropriate
permission, delivered to our laboratory at Davidson College for further analysis
by polarized light microcopy. An Olympus BX-40 Polarizing Microscope was
utilized at 400X magnification. Slides were prepared as dispersion samples
using Meltmount from Cargille Labs (refractive index 1.662). Refractive index
determinations were made using the Becke line method. Photographic images
were obtained with an Infinity 1-2c Camera and Infinity Analyzer software. A
reference set of paint pigment slides was obtained from McCrone Microscopes
and Accessories.
Results and Discussion

It is not known if the various pigment colors were found completely
intermingled within the shop or were discovered in concentrated clusters of
particular colors. Also unclear is the method by which the pigments were sorted
by the original excavation team prior to storage. When rediscovered in 2009, the
pigments were organized by color in numbered plastic containers. Figure 1 shows
photos of the individual pigments in their storage containers.
In the following sections, we discuss the pigments known to be available
to ancient Roman painters, and we present our findings regarding the elemental
composition and particle properties of each type of pigment represented at S.
Omobono.
Blue and Light Blue
It is the vivid blue pigments that are the most noticeable during a first glance at
the array of Roman pigments from S. Omobono. These are also the most abundant
of the samples, with a total mass of 1100 g and colors ranging from deep blue to
sky blue.
Blue pigments known to be used during this time period include azurite, a
ground copper mineral (2CuCO3·Cu(OH)2); indigo, an organic colorant from plant
leaves that was used as both a dye and a pigment (C16H10N2O2); and Egyptian blue,
the first manufactured pigment, dating to the third millenium B.C.E. The chemical
23
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Title: The Cornhill Magazine (vol. XLII, no. 251 new series, May
1917)
Author: Various
Release date: November 25, 2023 [eBook #72225]
Language: English
Original publication: London: Smith, Elder and Co, 1860
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MAY 1917.
BRING UP THE GUNS.
by boyd cable.
When Jack Duncan and Hugh Morrison suddenly had it brought
home to them that they ought to join the New Armies, they lost little
time in doing so. Since they were chums of long standing in a City
office, it went without saying that they decided to join and ‘go through
it’ together, but it was much more open to argument what branch of
the Service or regiment they should join.
They discussed the question in all its bearings, but being as
ignorant of the Army and its ways as the average young Englishman
was in the early days of the war, they had little evidence except
varied and contradictory hearsay to act upon. Both being about
twenty-five they were old enough and business-like enough to
consider the matter in a business-like way, and yet both were young
enough to be influenced by the flavour of romance they found in a
picture they came across at the time. It was entitled ‘Bring up the
Guns,’ and it showed a horsed battery in the wild whirl of advancing
into action, the horses straining and stretching in front of the
bounding guns, the drivers crouched forward or sitting up plying whip
and spur, the officers galloping and waving the men on, dust swirling
from leaping hoofs and wheels, whip-thongs streaming, heads
tossing, reins flying loose, altogether a blood-stirring picture of
energy and action, speed and power.
‘I’ve always had a notion,’ said Duncan reflectively, ‘that I’d like to
have a good whack at riding. One doesn’t get much chance of it in
city life, and this looks like a good chance.’
‘And I’ve heard it said,’ agreed Morrison, ‘that a fellow with any
education stands about the best chance in artillery work. We’d might
as well plump for something where we can use the bit of brains
we’ve got.’
‘That applies to the Engineers too, doesn’t it?’ said Duncan. ‘And
the pottering about we did for a time with electricity might help there.’
‘Um-m,’ Morrison agreed doubtfully, still with an appreciative eye
on the picture of the flying guns. ‘Rather slow work though—digging
and telegraph and pontoon and that sort of thing.’
‘Right-oh,’ said Duncan with sudden decision. ‘Let’s try for the
Artillery.’
‘Yes. We’ll call that settled,’ said Morrison; and both stood a few
minutes looking with a new interest at the picture, already with a
dawning sense that they ‘belonged,’ that these gallant gunners and
leaping teams were ‘Ours,’ looking forward with a little quickening of
the pulse to the day when they, too, would go whirling into action in
like desperate and heart-stirring fashion.
‘Come on,’ said Morrison. ‘Let’s get it over. To the recruiting-office
—quick march.’
And so came two more gunners into the Royal Regiment.
When the long, the heart-breakingly long period of training and

waiting for their guns, and more training and slow collecting of their
horses, and more training was at last over, and the battery sailed for
France, Morrison and Duncan were both sergeants and ‘Numbers
One’ in charge of their respective guns; and before the battery had
been in France three months Morrison had been promoted to Battery
Sergeant-Major.
The battery went through the routine of trench warfare and dug its
guns into deep pits, and sent its horses miles away back, and sat in
the same position for months at a time, had slack spells and busy
spells, shelled and was shelled, and at last moved up to play its part
in The Push.
Of that part I don’t propose to tell more than the one incident—an
incident of machine-pattern sameness to the lot of many batteries.
The infantry had gone forward again and the ebb-tide of battle was
leaving the battery with many others almost beyond the water-mark
of effective range. Preparations were made for an advance. The
Battery Commander went forward and reconnoitred the new position
the battery was to move into, everything was packed up and made
ready, while the guns still continued to pump out long range fire. The
Battery Commander came in again and explained everything to his
officers and gave the necessary detailed orders to the Sergeant-
Major, and presently received orders of date and hour to move.
This was in the stages of The Push when rain was the most
prominent and uncomfortable feature of the weather. The guns were
in pits built over with strong walls and roofing of sand-bags and
beams which were weather-tight enough, but because the floors of
the pits were lower than the surface of the ground, it was only by a
constant struggle that the water was held back from draining in and
forming a miniature lake in each pit. Round and between the guns
was a mere churned-up sea of sticky mud. As soon as the new
battery position was selected a party went forward to it to dig and
prepare places for the guns. The Battery Commander went off to
select a suitable point for observation of his fire, and in the battery
the remaining gunners busied themselves in preparation for the
move. The digging party were away all the afternoon, all night, and
on through the next day. Their troubles and tribulations don’t come
into this story, but from all they had to say afterwards they were real
and plentiful enough.
Towards dusk a scribbled note came back from the Battery
Commander at the new position to the officer left in charge with the
guns, and the officer sent the orderly straight on down with it to the
Sergeant-Major with a message to send word back for the teams to
move up.
‘All ready here,’ said the Battery Commander’s note. ‘Bring up the
guns and firing battery waggons as soon as you can. I’ll meet you on
the way.’
The Sergeant-Major glanced through the note and shouted for the
Numbers One, the sergeants in charge of each gun. He had already
arranged with the officer exactly what was to be done when the order
came, and now he merely repeated his orders rapidly to the
sergeants and told them to ‘get on with it.’ When the Lieutenant
came along five minutes after, muffled to the ears in a wet
mackintosh, he found the gunners hard at work.
‘I started in to pull the sand-bags clear, sir,’ reported the Sergeant-
Major. ‘Right you are,’ said the Lieutenant. ‘Then you’d better put the
double detachments on to pull one gun out and then the other. We
must man-handle ’em back clear of the trench ready for the teams to
hook in when they come along.’
For the next hour every man, from the Lieutenant and Sergeant-
Major down, sweated and hauled and slid and floundered in slippery
mud and water, dragging gun after gun out of its pit and back a half
dozen yards clear. It was quite dark when they were ready, and the
teams splashed up and swung round their guns. A fairly heavy
bombardment was carrying steadily on along the line, the sky winked
and blinked and flamed in distant and near flashes of gun fire, and
the air trembled to the vibrating roar and sudden thunder-claps of
their discharge, the whine and moan and shriek of the flying shells.
No shells had fallen near the battery position for some little time, but,
unfortunately, just after the teams had arrived, a German battery
chose to put over a series of five-point-nines unpleasantly close. The
drivers sat, motionless blotches of shadow against the flickering sky,
while the gunners strained and heaved on wheels and drag-ropes to
bring the trails close enough to drop on the hooks. A shell dropped
with a crash about fifty yards short of the battery and the pieces flew
whining and whistling over the heads of the men and horses. Two
more swooped down out of the sky with a rising wail-rush-roar of
sound that appeared to be bringing the shells straight down on top of
the workers’ heads. Some ducked and crouched close to earth, and
both shells passed just over and fell in leaping gusts of flame and
ground-shaking crashes beyond the teams. Again the fragments
hissed and whistled past and lumps of earth and mud fell spattering
and splashing and thumping over men and guns and teams. A driver
yelped suddenly, the horses in another team snorted and plunged,
and then out of the thick darkness that seemed to shut down after
the searing light of the shell-burst flames came sounds of more
plunging hoofs, a driver’s voice cursing angrily, threshings and
splashings and stamping. ‘Horse down here ... bring a light ... whoa,
steady, boy ... where’s that light?’
Three minutes later: ‘Horse killed, driver wounded in the arm, sir,’
reported the Sergeant-Major. ‘Riding leader Number Two gun, and
centre driver of its waggon.’
‘Those spare horses near?’ said the Lieutenant quickly. ‘Right. Call
up a pair; put ’em in lead; put the odd driver waggon centre.’
Before the change was completed and the dead horse dragged
clear, the first gun was reported hooked on and ready to move, and
was given the order to ‘Walk march’ and pull out on the wrecked
remnant of a road that ran behind the position. Another group of five-
nines came over before the others were ready, and still the drivers
and teams waited motionless for the clash that told of the trail-eye
dropping on the hook.
‘Get to it, gunners,’ urged the Sergeant-Major, as he saw some of
the men instinctively stop and crouch to the yell of the approaching
shell. ‘Time we were out of this.’
‘Hear, bloomin’ hear,’ drawled one of the shadowy drivers. ‘An’ if
you wants to go to bed, Lanky’—to one of the crouching gunners
—‘just lemme get this gun away fust, an’ then you can curl up in that
blanky shell-’ole.’
There were no more casualties getting out, but one gun stuck in a
shell-hole and took the united efforts of the team and as many
gunners as could crowd on to the wheels and drag-ropes to get it
moving and out on to the road. Then slowly, one by one, with a
gunner walking and swinging a lighted lamp at the head of each
team, the guns moved off along the pitted road. It was no road really,
merely a wheel-rutted track that wound in and out the biggest shell-
holes. The smaller ones were ignored, simply because there were
too many of them to steer clear of, and into them the limber and gun
wheels dropped bumping, and were hauled out by sheer team and
man power. It took four solid hours to cover less than half a mile of
sodden, spongy, pulpy, wet ground, riddled with shell-holes,
swimming in greasy mud and water. The ground they covered was
peopled thick with all sorts of men who passed or crossed their way
singly, in little groups, in large parties—wounded, hobbling wearily or
being carried back, parties stumbling and fumbling a way up to some
vague point ahead with rations and ammunition on pack animals and
pack-men, the remnants of a battalion coming out crusted from head
to foot in slimy wet mud, bowed under the weight of their packs and
kits and arms; empty ammunition waggons and limbers lurching and
bumping back from the gun line, the horses staggering and slipping,
the drivers struggling to hold them on their feet, to guide the wheels
clear of the worst holes; a string of pack-mules filing past, their
drivers dismounted and leading, and men and mules ploughing
anything up to knee depth in the mud, flat pannier-pouches swinging
and jerking on the animals’ sides, the brass tops of the 18-pounder
shell-cases winking and gleaming faintly in the flickering lights of the
gun flashes. But of all these fellow wayfarers over the battlefield the
battery drivers and gunners were hardly conscious. Their whole
minds were so concentrated on the effort of holding and guiding and
urging on their horses round or over the obstacle of the moment, a
deeper and more sticky patch than usual, an extra large hole, a
shattered tree stump, a dead horse, the wreck of a broken-down
waggon, that they had no thought for anything outside these. The
gunners were constantly employed manning the wheels and heaving
on them with cracking muscles, hooking on drag-ropes to one gun
and dragging it clear of a hole, unhooking and going floundering
back to hook on to another and drag it in turn out of its difficulty.
The Battery Commander met them at a bad dip where the track
degenerated frankly into a mud bath—and how he found or kept the
track or ever discovered them in that aching wilderness is one of the
mysteries of war and the ways of Battery Commanders. It took
another two hours, two mud-soaked nightmare hours, to come
through that next hundred yards. It was not only that the mud was
deep and holding, but the slough was so soft at bottom that the
horses had no foothold, could get no grip to haul on, could little more
than drag their own weight through, much less pull the guns. The
teams were doubled, the double team taking one gun or waggon
through, and then going back for the other. The waggons were
emptied of their shell and filled again on the other side of the slough;
and this you will remember meant the gunners carrying the rounds
across a couple at a time, wading and floundering through mud over
their knee-boot tops, replacing the shells in the vehicle, and wading
back for another couple. In addition to this they had to haul guns and
waggons through practically speaking by man-power, because the
teams, almost exhausted by the work and with little more than
strength to get themselves through, gave bare assistance to the pull.
The wheels, axle deep in the soft mud, were hauled round spoke by
spoke, heaved and yo-hoed forward inches at a time.
When at last all were over, the teams had to be allowed a brief rest
—brief because the guns must be in position and under cover before
daylight came—and stood dejectedly with hanging ears, heaving
flanks, and trembling legs. The gunners dropped prone or squatted
almost at the point of exhaustion in the mud. But they struggled up,
and the teams strained forward into the breast collars again when
the word was given, and the weary procession trailed on at a jerky
snail’s pace once more.
As they at last approached the new position the gun flashes on the
horizon were turning from orange to primrose, and although there
was no visible lightening of the Eastern sky, the drivers were
sensible of a faintly recovering use of their eyes, could see the dim
shapes of the riders just ahead of them, the black shadows of the
holes, and the wet shine of the mud under their horses’ feet.
The hint of dawn set the guns on both sides to work with trebled
energy. The new position was one of many others so closely set that
the blazing flames from the gun muzzles seemed to run out to right
and left in a spouting wall of fire that leaped and vanished, leaped
and vanished without ceasing, while the loud ear-splitting claps from
the nearer guns merged and ran out to the flanks in a deep drum roll
of echoing thunder. The noise was so great and continuous that it
drowned even the roar of the German shells passing overhead, the
smash and crump of their fall and burst.
But the line of flashes sparkling up and down across the front
beyond the line of our own guns told a plain enough tale of the
German guns’ work. The Sergeant-Major, plodding along beside the
Battery Commander, grunted an exclamation.
‘Boche is getting busy,’ said the Battery Commander.
‘Putting a pretty solid barrage down, isn’t he, sir?’ said the
Sergeant-Major. ‘Can we get the teams through that?’
‘Not much hope,’ said the Battery Commander, ‘but, thank
Heaven, we don’t have to try, if he keeps barraging there. It is
beyond our position. There are the gun-pits just off to the left.’
But, although the barrage was out in front of the position, there
were a good many long-ranged shells coming beyond it to fall
spouting fire and smoke and earth-clods on and behind the line of
guns. The teams were flogged and lifted and spurred into a last
desperate effort, wrenched the guns forward the last hundred yards
and halted. Instantly they were unhooked, turned round, and started
stumbling wearily back towards the rear; the gunners, reinforced by
others scarcely less dead-beat than themselves by their night of
digging in heavy wet soil, seized the guns and waggons, flung their
last ounce of strength and energy into man-handling them up and
into the pits. Two unlucky shells at that moment added heavily to the
night’s casualty list, one falling beside the retiring teams and
knocking out half a dozen horses and two men, another dropping
within a score of yards of the gun-pits, killing three and wounding
four gunners. Later, at intervals, two more gunners were wounded by
flying splinters from chance shells that continued to drop near the
pits as the guns were laboriously dragged through the quagmire into
their positions. But none of the casualties, none of the falls and
screamings of the high-explosive shells, interrupted or delayed the
work, and without rest or pause the men struggled and toiled on until
the last gun was safely housed in its pit.
Then the battery cooks served out warm tea, and the men drank
greedily, and then, too worn out to be hungry or to eat the biscuit and
cheese ration issued, flung themselves down in the pits under and
round their guns and slept there in the trampled mud.
The Sergeant-Major was the last to lie down. Only after everyone
else had ceased work, and he had visited each gun in turn and
satisfied himself that all was correct, and made his report to the
Battery Commander, did he seek his own rest. Then he crawled into
one of the pits, and before he slept had a few words with the
‘Number One’ there, his old friend Duncan. The Sergeant-Major,
feeling in his pockets for a match to light a cigarette, found the note
which the Battery Commander had sent back and which had been
passed on to him. He turned his torch light on it and read it through
to Duncan—‘Bring up the guns and firing battery waggons ...’ and
then chuckled a little. ‘Bring up the guns.... Remember that picture
we saw before we joined, Duncan! And we fancied then we’d be
bringing ’em up same fashion. And, good Lord, think of to-night.’
‘Yes,’ grunted Duncan, ‘sad slump from our anticipations. There
was some fun in that picture style of doing the job—some sort of
dash and honour and glory. No honour and glory about “Bring up the
guns” these days. Na poo to-night anyway.’
The Sergeant-Major, sleepily sucking his damp cigarette, wrapped
in his sopping British Warm, curling up in a corner on the wet cold
earth, utterly spent with the night’s work, cordially agreed.
Perhaps, and anyhow one hopes, some people will think they
were wrong.
FRANCE AND BRITAIN: THEIR
COMMON MEMORIES.
‘France and England, whose very shores look pale
With envy of each other’s happiness.’
Shakespeare, Henry V., Act v. sc. ii.
‘Each the other’s mystery, terror, need and love.’
Rudyard Kipling.
Our common memories? Well, are they so many of this nature

which brings closer those who recollect them together? They are
indeed! Let this article be a friendly protest, a grounded protest
against the idea which is no doubt, still, the prevalent popular idea
on both sides of the Channel, I mean this one: ‘The Entente Cordiale
is something splendid, but when one comes to think about it, how
wonderful, how new!’ Yes, when we think about it superficially, how
wonderful, how new, but when we think somewhat more deeply and
with a little more knowledge of the past, how natural! Not a miracle:
the logical result, only too long deferred, of the long centuries of our
common history. It is not mere pastime to show it. How important on
the contrary, how practically important for the present and for the
future of our alliance, to make conscious again the old moral ties and
to reawaken the sleeping sense of historical fellowship!
II.
To make that fellowship apparent, at a glance, at least from certain
points of view, I have devised the appended diagram. There you see
represented, as it were, the streams of the history of our two nations
from their farthest origins down to our own times. Please note the
scale of centuries. See both streams rising about eight or six
centuries before Christ in the same mountain—if I may say so
figuratively—in the same mountain of the Celtic race. They spring, as
you see, from the same source, and, though geographically divided,
their waters remain a long time of the same colour—green in my
draught.
SYMBOLIC DRAUGHT ILLUSTRATING THE HISTORY OF FRANCO-BRITISH

RELATIONS.
We have, on that point of their origins, very interesting and very

numerous testimonies, chiefly in the contemporary Greek and
Roman writers. Very striking in particular was the fellowship of
ancient Britons and Gauls with regard to religion. If you open one—I
may say any one—of our French history text-books, you will see that
it begins exactly as one of yours, with the same story, and pictures,
of Druids, priests, teachers, and judges—some of them bards; the
same story of the solemn gathering of the mistletoe verdant in winter
on the bare branches of oaks, symbol of the cardinal creed of the
race: the immortality of the soul. Caesar, who had a Druid among his
best friends, observes that the young Gauls who wanted to go
deeper into the study of their religion generally used to go over to
Britain in order to graduate, if I may say so, in this mysterious and

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In Archaeological Chemistry VIII; Armitage, R., et al.;

In Archaeological Chemistry VIII; Armitage, R., et al.;

Archaeological Chemistry VIII

Ruth Ann Armitage, Editor

James H. Burton, Editor

American Chemical Society, Washington, DC

Distributed in print by Oxford University Press

In Archaeological Chemistry VIII; Armitage, R., et al.;

pages cm. -- (ACS Symposium series ; 1147)

Copyright © 2013 American Chemical Society

Distributed in print by Oxford University Press

PRINTED IN THE UNITED STATES OF AMERICA

In Archaeological Chemistry VIII; Armitage, R., et al.;

developed from symposia sponsored by other organizations when the topic is of

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ACS Books Department

In Archaeological Chemistry VIII; Armitage, R., et al.;

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