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Study of Colonial Manuscripts from San Nicolás

Coatepec, México, Through UV&IR Imaging and XRF

Article  in  MRS Online Proceeding Library Archive · January 2012

DOI: 10.1557/opl.2012.1375

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Mater. Res. Soc. Symp. Proc. Vol. 1618 © 2014 Materials Research Society
DOI: 10.1557/opl.2014.453

XRF Study of Mexican Iron Gall Inks: Historical and Geographical Overview of their
Chemistry

Jocelyn Alcántara García1,*, Jose Luis Ruvalcaba Sil2 and Marie Vander Meeren3
1
Andrew W. Mellon Postdoctoral Fellow. Johns Hopkins University. Sheridan Libraries and
Museums. Department of Conservation and Preservation. Brody Learning Commons 5031 C
Level. 3400 N Charles St. Baltimore, MD 21218, USA. * Research performed while affiliated
to 3. e-mail: jocelynag@gmail.com
2
Instituto de Física, Universidad Nacional Autónoma de México, Circuito de la Investigación
Científica s/n, Ciudad Universitaria, Mexico DF 04510, Mexico.
e-mail: sil@fisica.unam.mx
3
Coordinación Nacional del Patrimonio Cultural, Instituto Nacional de Antropología e Historia.
Ex Convento de Churubusco s/n esq. General Anaya. Col. San Diego Churubusco, México D.
F. 04120, Mexico.

ABSTRACT

Over 2000 micro-X-Ray Fluorescence (P-XRF) measurements of iron gall inks were
collected at the General Archive of the Nation in Mexico (Archivo General de la Nación, AGN).
The portable X-Ray system SANDRA permitted detection of common elements present in all
iron gall inks (e.g. Ca, Fe, S, etc.) as well as characteristic traces and impurities (e.g. Cu, Ni, Zn,
Pb, etc). The documents in the data set originate from all over Mexico and are dated between the
16th and 19th centuries. All manuscripts were well preserved.
Extensive statistical processing of the relative X-Ray intensities revealed common
features in groups of documents with the same provenance. Among the findings, there is a
progressive trend to complex mixtures from the beginning of the 16th century to the 17th. A
reverse trend was observed for the following century. Zinc, lead and seldom arsenic, chromium
and mercury seem characteristic for northern areas whereas manganese seems common to the
vast majority of studied inks.
As a general concern in conservation research, special attention was addressed to copper,
as it is known to have additive effects to the degradation of cellulose. This metal seems fairly
common to Mexican inks, especially during 18th century.
To the best of our knowledge, this is the first examination taken to such a large number of
inks. This study contributes to the more-focused development of suitable treatments that tailor
specific needs, since they are to be based on of ink’s composition. It sets a precedent for the
study of these inks in the Americas and allows conservators and historians to gain further insight
into the history of their usage in Mexico.

INTRODUCTION

Even when iron gall inks are perhaps the most important kind of ink in the Western
World, reports on their chemistry and degradation mechanisms remain scarce [1-7], except for
specific characterization studies on artifacts [8-13]. The earliest report on their possible
mechanism for degradation stated that “old, handwritten documents are slowly decomposing by
products of iron gall ink, containing Fe (III) compounds and by H2SO4, which has its origin in

31
atmospheric SO2” [14]. Although this is not exactly right, this statement suggests that already in
the 1960’s there was awareness of the role of iron and acids in paper decay. Previously Waters
mentioned that “the use of correct proportions of Fe and tannin was made in 1748” and William
Lewis reported on the adverse effects excess of iron sulfate relative to tannin content (“burning-
in” of inks) [15].
The above-mentioned reports evince early observations on the deleterious effects of non-
balanced and acidic nature of iron gall inks, but it was not until 1988 that it was suggested that
“chemical and microbial factors may be the causes of ink eating” [16]. Almost a decade later the
first systematic study on the effects of deacidification started an enormous interest on iron gall
inks and their degradation mechanisms [17]. However, other than deacidification, few
alternatives have since developed to counteract “iron gall ink corrosion”. This term is used to
describe the physical effect of hydrolysis and oxidation processes in cellulose, which are
catalyzed by several metallic ions.
Nowadays, the widely accepted conservation alternative for iron gall ink corrosion is
based on the natural anti-oxidant phytate [1, 2, 14, 17-22]. However, it only decreases catalytic
properties of iron ions whereas catalytically active ions such as copper might result in
undesirable side effects when significant amounts of it are present [1-3]. This metal is known to
contribute greatly to the oxidative decay of cellulose-based artifacts. Its presence, along with that
of other metals (Mn, Zn, Al, Mg, etc.) might be due to ore-provenance or preparation, and can
potentially provide useful information attaining its origin (geography and date).
The very few studies carried out in Mexican documents showed presence of copper,
which not only makes unsuitable the “calcium-phytate”, but might even endanger collections
after treatment. Interested in knowing how frequent this transitional metal actually is, we
performed the study of a statistically significant number of inks through X-Ray Fluorescence.
The present study, of enormous importance from a historical point of view is helping to tailor
specific methodologies that take into account local and most common compositional profiles,
which thus far seem different from European. To the best of our knowledge, this is the first study
carried out into such a great number of inks. At the same time, sets an important precedent to
study iron gall ink history in the Americas.

EXPERIMENTAL DETAILS

After careful selection of the materials to be examined, the inks and paper of the
documents were analyzed using the portable XRF SANDRA device [24] with a 75W Mo X-ray
tube and a Si-PIN X123 detector from Amptek. XRF conditions for the X-ray tube were 40 kV
and 0.6 mA, 120 seconds per region. A total of 2302 measurements were carried out on inked
and 404 of non-inked areas of the documents. The beam spot was 1 mm diameter.

DISCUSSION

Iron gall ink recipes might include any imaginable component, which commonly use
local ingredients [1, 2, 25]. Although in Europe a fair number of recipes for their preparation are
known, historical preparation methodologies are currently unknown in Mexico. This arises the
question of preparation for local usage during Colonial and early Modern times in Mexico.
In our study of 2011, we found that the inks used in a 16th century “Mercedes” document
were dramatically different from that of another locally written document in close relationship

32
with the history of the town San Nicolás Coatepec [8]. One of the features we found then was
abundance of copper, which might contribute to a greater extent to the degradation processes. To
the best of our knowledge, the only systematic report on a broad number of historical iron gall
inks was conducted in Europe, at the Slovenia’s National and University Library and Regional
Archives of Maribor [2, 3]. Using non-destructive in-air PIXE, the Slovenian research group
studied 99 historical documents ranging from 14th to 20th centuries. Although they mention that
manganese, chromium, cobalt, nickel and especially copper are present, there is no reference to
the ratios and specific provenance of the documents. However, they provide the hydroxyl radical
production rate constants at different pH. Depending on the pH of the reaction medium, results
show that copper is the most effective catalyst at pH 7.7, followed in decreasing order by
mixtures, cobalt, chromium, iron, manganese, nickel and zinc [2]. The present research along
with the mentioned findings is of uttermost concern for Mexican archives, as metal contents
commonly seem to endanger collections.
In the aim of providing historical information that could help the development of tailored
and profile-focused conservation methodologies and conservation policies, we studied well
preserved documents stored at the Archivo General de la Nación (General Archive of the Nation
in Mexico) with XRF (2302 inks-on-paper and 404 paper measurements). Through the statistical
analysis of the correlations M/Fe, as this is thought to be the most abundant metal, we found a
number of coincidences and trends.
Using M/Fe intensity ratios was decided as a way to take into account the variable
thickness of the ink layers [26-30].
Due to the vast amount of information, we did the analysis by half of a century (e. g.
1600 – 1650), by state and by element. The most significant analysis was that performed by
century, which is included here.

XVI century. Period 1500 – 1599

Table I summarizes the results from hierarchical cluster analysis. From the corresponding
tree diagrams, as the one in Figure 1, the different groups were chosen. Depending on the
century, linkage distance within each group spans from 0.1 to approximately 5, whereas linkage
distance between each of the groups is approximately 6. Taking into account that the greater the
differences between the groups (i. e. linkage distance) the greater the differences between the
compositional profile, it is feasible to differentiate between ink profiles by groups [31].
Inks used during the early years of Spanish occupancy display similar profiles. Still, it is
possible to clearly differentiate two and four main groups during the first and second halves of
the 16th century (1500-1599). Before 1551 the two main groups are related with a linkage
distance of approximately 6 (see Figure 1). Both include Guerrero and Mexico City but only the
first one includes Veracruz, whereas only the latter includes Michoacán. This could be a result of
local materials or perhaps imported goods delivered to one coastal zone or the other.
Analysis of the first half of the 16th c. shows that only Group 2 coincides with the
absence of Nickel and presence of copper, although the latter in small concentrations (average
Cu/Fe 0.2).

33
 Figure 1. Tree diagram for studied inks dated between 1500 and 1550 (XVI-1).

Results from the second half of the 16th century show similar compositional profiles
except for those from Oaxaca, which constitute a cluster related to the rest of the inks by a
linkage distance of 9. Such a comparatively large number may be interpreted as a local
production of inks in this state.
The second group contains three subsets, all of which include inks from Mexico City,
Mexico State and Jalisco, important regions for economy and demography. As stated above,
Group 4 is linked to Groups 2 and 3 by a distance of approximately 7, while the first two groups,
that also include San Luis Potosí, relate with each other by a distance of 6, meaning profile
differences are small (see Table 1).

Table 1. Groups of states as clustered in tree diagrams obtained by hierarchical cluster analysis
for XVI century inks. CAM-Campeche; CAL-Californias (Baja California, Baja California Sur
and California); CHIS-Chiapas; CHIH-Chihuahua; COL-Colima; DUR-Durango; GRO-
Guerrero; GTO-Guanajuato; HDGO-Hidalgo; JAL-Jalisco; MXC-Mexico City; MXS-Mexico
State; MICH-Michoacán; NLEON-Nuevo Leon; OAX-Oaxaca; PUE-Puebla; QRO-Queretaro;
SLPS-San Luis Potosí; VER-Veracruz; YUC-Yucatan; ZAC-Zacatecas.

1500-1550
Group1 Group2
GRO GRO
MXC MICH
VER MXC
1551-1599
Group1 Group2 Group3 Group4
OAX JAL JAL CHIS
MXC MICH JAL
MXS MXC MXC
SLPS MXS MXS
SLPS

34
XVII century. Period 1600 – 1699

In contrast to the previous century, in which there was a strong connection between
elemental profiles and geography, during the first part of the 17th century similarities are less
evident. In fact, the tree diagram does not show clusters. However, the largest linkage distance is
again 7, which suggests homogeneity.
All inks include manganese and in 40% of them there is also copper, which ranges from
2 up to 50% Cu to Fe ratio. Histograms in Figure 2 show manganese and copper abundance by
centuries.
We had observed extended presence of manganese previously [8], and the present study
may indicate that this metal is characteristic of Mexican inks. Its presence in studied documents
spans from 0.01 manganese to iron ratio up to Mn/Fe = 20 (Figure 2).

Figure 2. Manganese (left) and copper (right) presence in Mexican iron gall inks (1521 – 1899).

Compositional profile differences are usually caused by transition metal-content, such as

lead, chromium, zinc, mercury and nickel. States in which the mining was common, such as
Guanajuato, San Luis Potosí and Hidalgo tend to present more frequently these metals. One
particular case is that of Chiapas and to a smaller extent, Jalisco, which exhibit contents of nickel
(up to a 0.2 Ni/Fe ratio). This could be due to soil and/or water, which might have contained
metal traces from mining.
To prepare inks three basic ingredients are needed according to European historical
records: water, gum Arabic and “vitriol”. Vitriol is the term historically associated with zinc,
copper and iron sulfate for white, blue and green vitriol, respectively [1, 2]. In Europe, until late
18th century, when iron sulfate was synthesized in factories, production of vitriol was by mining
the crystals or by freezing or evaporating iron and sulfur-rich waters. If similar methodologies
were used in Mexico, it is expected to find inks containing metal-traces commonly found in
mines, hence suggesting local production.
The above-mentioned assumption is further supported by characteristic compositional
profiles of many inks, for example lead and chromium contents in Zacatecas, San Luis Potosí
and to a lesser extent Guanajuato. Furthermore, manganese and copper are the second and third
most common transition metals during the 17th century, respectively. Average Mn/Fe ratio is 0.3
whereas Cu/Fe ratio is 0.2. There are few examples of inks from Michoacan, Chihuahua and
Chiapas in which the content is about 50% and there is one ink from Guanajuato and one from
Puebla in which Cu-content is higher than that of Fe.

35
 Analysis of the late 17th century showed that inks from northern states as Chihuahua and
Durango share a similar compositional profile. They cluster with a linkage distance of
approximately 1, which evince a close chemical profile, even when they are part of a larger
cluster.

Table 2. Groups of states as clustered in tree diagrams obtained by hierarchical cluster analysis
for XVII century inks. CAM-Campeche; CAL-Californias (Baja California, Baja California Sur
and California); CHIS-Chiapas; CHIH-Chihuahua; COL-Colima; DUR-Durango; GRO-
Guerrero; GTO-Guanajuato; HDGO-Hidalgo; JAL-Jalisco; MXC-Mexico City; MXS-Mexico
State; MICH-Michoacán; NLEON-Nuevo Leon; OAX-Oaxaca; PUE-Puebla; QRO-Queretaro;
SLPS-San Luis Potosí; VER-Veracruz; YUC-Yucatan; ZAC-Zacatecas.

1600-1650
Group1 Group2 Group3 Group4 Group5 Group6 Group7 Group8
CHIS MXC CHIS CHIH CHIH CAM CAM NMEX CHIS
MICH JAL MXC CHIS DUR SLPS JAL
YUC MXC MXS DUR GTO ZAC MXC
OAX OAX MICH JAL OAX
SLPS QRO MXC MICH PUE
VER PUE MXC
ZAC
1651-1699
Group1 Group2 Group3 Group4
PUE CHIS JAL SLPS CAM CAM QRO
CAM MICH VER GTO GTO
CHIH MXC YUC JAL JAL
DUR PUE ZAC MXC MXC
GTO QRO PUE PUE

XVIII century. Period 1700 – 1799

The majority of the 1700’s inks show compositional profiles more homogeneous than in
the late 1600’s. Maximum linkage distance in both early and late 18th centuries is between 6 and
7, and only a reduced number of clusters are distinguishable. Although there is not a strict
“regionalization” for most of the inks, those produced in northern states and the Bajío Region
(“the Californias”, Sonora and Jalisco) group separately (see Group 1 of late 1700’s in Table 3
and Figure 3). Furthermore, as in previous centuries there is a cluster only for inks from Oaxaca,
in addition to the inks with shared compositional profile.
In this century about 50% of the inks analyzed contain both copper and zinc, 50% at
least traces of lead and 10% at least traces of mercury. It is outstanding that only one of the two
main groups between 1700 and 1750 contain examples from Mexico City while only the second
has inks from Mexico State. Being in such geographical proximity, these differences might be
explained by trade (see figure 4).

36
 During XVIII century, copper content in studied inks from San Luis Potosí and Mexico
State is higher than in previous centuries. At least 30% of the inks contain this metal in a 1:1
Cu/Fe ratio, but we found examples in which the ratio could be as high as 4:1. Such findings are
of great importance because this metal displays higher hydroxyl radical production than Fe (III)-
containing systems [2, 3]. In turn, high contents such as these can further accelerate autoxidation
of cellulose.

Figure 3. Map of Mexico that shows similar ink profiles during early 18th century (1700 – 1750).

Figure 4. Tree diagram for inks dated between 1700 and 1750 (XVIII-I).

37
Table 3. Groups of states as clustered in tree diagrams obtained by hierarchical cluster analysis
for XVIII century inks. CAM-Campeche; CAL-Californias (Baja California, Baja California Sur
and California); CHIS-Chiapas; CHIH-Chihuahua; COL-Colima; DUR-Durango; GRO-
Guerrero; GTO-Guanajuato; HDGO-Hidalgo; JAL-Jalisco; MXC-Mexico City; MXS-Mexico
State; MICH-Michoacán; NLEON-Nuevo Leon; OAX-Oaxaca; PUE-Puebla; QRO-Queretaro;
SLPS-San Luis Potosí; VER-Veracruz; YUC-Yucatan; ZAC-Zacatecas.

1700-1750
Group1 Group2
GTO CAM PUE SLPS
MXS MICH MXC
OAX VER
YUC YUC
ZAC ZAC
1751-1799
Group1 Group2 Group3 Group4
CAL MICH CAL HDGO PUE OAX
JAL OAX CHIS JAL QRO
SLPS SLPS COL MICH SIN
SON VER GTO MXC SON
YUC GRO OAX VER
ZAC

XIX century. Period 1800 – 1899

Inks from San Luis Potosí dated between 1800 and 1850 are distinguishably different
from those of other states during this period. With a linkage distance to the other major group of
17, this cluster contains a variety of inks with very high contents of copper and/or zinc (up to 2:1
copper and/or zinc to iron ratio). Despite that most of the San Luis Potosí inks are included in
this first major cluster, the group is not of homogeneous compositions (linkage distances span
from 0.1 to 11). Approximately 55% of these have high contents of sulfur as well calcium. Sulfur
to iron ratio higher than 1 is associated with sulfuric acid-induced hydrolysis, whereas S/Fe<1
suggests that iron Redox-processes might occur. However, excess of sulfur can too be related to
fillers such as calcium sulfate, as it is likely in this group. In addition to the fact that all
documents were well preserved, high contents of calcium were found both for inked and non-
inked areas [18].
Besides this first large group that only contains San Luis Potosí inks, we observed two
other inks from the same state. Both linked to the rest of the inks by a linkage distance of 27,
contain high lead to iron ratios: Pb/Fe ≥10. It is worth pointing out that these inks contain no
significant amounts of other metals and seem no different to the majority on a naked eye.
The second major group is roughly divided in three subgroups that do not have apparent
connection to any specific region nor are of homogeneous profile. The tree diagram for late 19th

38
century shows a similar tendency except that this group is more homogeneous and is
interconnected with smaller linkage distances than the previous half (17 vs. 5).
Although we did not find any characteristic ink profile from a specific century or state,
we found that metal contents are of a wider variety than those previously reported. Presence of
Zn, Ni, Mn, Co, Cr, Pb, As and Cu spans from traces up to 10 M/Fe ratio. This yields to a
particularly complex chemistry for inks in Mexico. Of concern are the frequent high amounts of
copper, because above pH 8 its rate of hydroxyl radical production, one of the main mechanisms
for cellulose degradation, is about 300 times higher than Fe (III)-containing systems [2].
Furthermore, the current best alternative for treatment of ink-corroded manuscripts, that chelates
catalytically active Fe (II) is not advised when copper is present. The “calcium phytate”
treatment can chelate copper as well and the corresponding phytate complex increases its
catalytic activity [2, 3, 15].
Of particular importance is the presence of high contents of arsenic and lead. Both users
and conservators frequently manipulate documents without gloves. As no visual, geographical or
temporal feature can be provided at this point, it is valuable to acknowledge the potential danger
of the sole contact. Michoacán, Jalisco, Sinaloa, Zacatecas, Guerrero and Mexico City are the
states in which we found higher contents of this element.

Table 4. Groups of states as clustered in tree diagrams obtained by hierarchical cluster analysis
for XIX century inks. CAM-Campeche; CAL-Californias (Baja California, Baja California Sur
and California); CHIS-Chiapas; CHIH-Chihuahua; COL-Colima; DUR-Durango; GRO-
Guerrero; GTO-Guanajuato; HDGO-Hidalgo; JAL-Jalisco; MXC-Mexico City; MXS-Mexico
State; MICH-Michoacán; NLEON-Nuevo Leon; OAX-Oaxaca; PUE-Puebla; QRO-Queretaro;
SLPS-San Luis Potosí; VER-Veracruz; YUC-Yucatan; ZAC-Zacatecas.

1800-1850
Group1 Group 2 Group3 Group4
SLPS CHIH MXS CAM MXC VER CHIH
GTO PUE GTO MXS YUC JAL
JAL SLPS GRO NLEON ZAC MICH
MICH YUC JAL OAX PUE
MXC ZAC MICH PUE VER
1851-1899
Group1 Group2 Group3
ZAC CAM PUE MXC
GTO VER QRO
GRO YUC SLPS
MICH VER
MXC YUC

39
CONCLUSIONS

This study sets a precedent for studying iron gall inks. A deeper understanding on their
chemistry is important for the development of problem-specific conservation.
Early Colonial inks are of much simpler composition and profiles tend to get more
complex with time. Usage of local materials seems probable, especially in regions where there
was mining. This is more pronounced in states as San Luis Potosí, Zacatecas and Guerrero, with
a rich Colonial mining industry.
On the other hand, northern states as Sonora, Chihuahua, Durango and the Californias
(Baja California, Baja California Sur and California) usually cluster together. A similar feature
was often found in San Luis Potosí, Mexico State and especially in inks from Oaxaca.
Composition heterogeneity is commonly associated with presence of transition metals,
although arsenic is frequently present as well, with no evident geographical or temporal
relationship.
High abundance of manganese is thought to be one feature of Mexican iron gall inks.
Almost as common as Mn, copper is the third most abundant element in this study. Both
elements are of particular conservation concern. Magnesium can promote dismutation of
superoxide to H2O2, hence accelerating autoxidation processes and it is catalytically active
towards hydroxyl radical production at neutral pH. Copper, on the other hand, can be up to 300
times more catalytically active than Fe (II).
Toxic elements such as lead and arsenic can be found on several inks and so far we have
not found any specifics on its provenance. This finding should be used to promote safer
manipulation practices through Mexican archives.
Finally, this study was conducted in well preserved documents at the Archivo General de
la Nación in Mexico. Storage conditions at this facility usually meet good conservation
standards. Our future work will focus on comparison of these results with corroded materials to
gain insight on compositional profiles that are more prone to degradation.

ACKNOWLEDGMENTS

Examination of a large number of inks was only possible thanks to very close
collaboration between Mexican scientists, conservators and historians, especially for the
documents from the XVI century. Authors wish to thank the people from the paper labs at the
Archivo General de la Nación as well as the Coordinación Nacional del Patrimonio Cultural,
Instituto Nacional de Antropología e Historia (INAH) for the support in photographic records
and selection of the materials. Many special thanks to Paola D’Rugama, Alejandra Odor, Tania
Estrada and Patricia de la Garza. This research has been carried out with support of UNAM
PAPIIT IN403210 and IN402813 ANDREAH projects as well as the CONACYT Mexico grant
MOVIL II 131944. This study has been performed in the frame of the Non Destructive Study of
the Mexican Cultural Heritage ANDREAH network (www.fisica.unam.mx/andreah).

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