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Received: May 4, 2016; Revised: July 21, 2016; Accepted: October 21, 2016
ABSTRACT
The ability of baked clay-elaborated objects to record the temporal variations of both
direction and intensity of the geomagnetic field at the time of their elaboration or last use
has been widely used during the last decades to fill the gaps left by available time-discrete
volcanic-rock logs for a better knowledge of the evolution of the geomagnetic field.
Further refinement of the secular variation curves has motivated the search for
alternative non-conventional materials as attractive targets for archeomagnetic studies.
Both clay and copper have been used since pre-Hispanic times for the elaboration of
a wide variety of ornamental and utilitarian objects in Mesoamerica. Previous studies
carried out in Europe and Israel have shown the usefulness of copper slags as one of
these non-conventional materials. We present the results of an integrated study carried
out on ten copper slags from seven ancient metallurgical sites of Michoacán. The analysis
included a series of rock magnetism experiments, scanning electron microscope analysis,
archeointensity determinations following the Thellier-Coe method and their
corresponding dating. Based on the results obtained the slag-set analyzed can be divided
in two main groups: low Fe concentrations (associated with high Cu concentrations) for
slags comprising the first group, and high Fe concentrations (associated with low Cu
concentrations) for slags from second group. Slags from the first group are characterized
by almost reversible thermomagnetic curves, while those corresponding to the second
group show a quite irreversible behavior. A crystalline (vitreous) structure within the
massive surface of the slags is observed for those coming from the second (first) group.
These striking features could reflect significant differences in the metallurgical process
followed at these sites, which according to archeological and historical evidences
correspond to Colonial and pre-Hispanic usage metallurgical sites; first and second
group, respectively. The good experimental behavior exhibited by these materials
demonstrates the suitability of copper slag to obtaining absolute archeointensity data
which can be used to improve the existing Mesoamerican archeomagnetic record. This in
turn, can be used both for geomagnetic field modelling purposes and archeomagnetic
dating.
1. INTRODUCTION
Knowledge the evolution of the past Earth’s magnetic field beyond instrumental direct
measurements, and even more before human existence, is only possible by means of the
analysis of the magnetic record contained in rocks, which are widely distributed
worldwide and cover a wide range of ages. Among the different types of rock, those with
an igneous origin (volcanic rocks) are considered to be the most reliable Earth’s magnetic
field recorders. However, the limited spatial distribution of volcanic rocks offers only
a semi-continuous record of the variations of the field strength at geological timescale.
Moreover, not all volcanic rocks are suitable for retaining unaltered their paleomagnetic
record because of internal and/or external factors, which can degrade their capabilities as
reliable recorders. This potentially continuous knowledge is hindered additionally by the
paused emanation of magnetically-recordable material of volcanic activity.
The ability of baked clay-elaborated objects, such as pottery and bricks, to record the
characteristics - direction and intensity - of the Earth’s magnetic field at the time of their
elaboration or last use, archeomagnetism, recognized long ago by Thellier (1936), has
been widely used in Europe to fill the gaps left by available time-discrete volcanic-rock
logs for a better knowledge of the evolution of the geomagnetic field for the last millennia
(e.g., Gallet et al., 2002; Schnepp and Lanos, 2005; Spassov et al., 2008). Although at
a lower rate, however, many important archeomagnetic studies have been carried out in
North America during the last decade (for review see Carrancho et al., 2015).
It is worth mentioning that most archeomagnetic studies carried out were mainly
dedicated to retrieve the ancient direction (archeodirection). This requires the objects to be
in situ, a condition difficult to meet when dealing with ceramic pieces. Archeointensity
studies, on the contrary, offers the possibility to use also displaced objects, which
represents a very significant improvement for the knowledge of the past Earth’s magnetic
field.
Further refinement of the secular variation curves has led to the search for alternative
materials, which has identified non-conventional materials like lithic clasts, lime plasters,
mural paintings and wattle and daub building (Goguitchaichvili et al., 2004; Carrancho et
al., 2014; Terán-Guerrero et al., 2016) as attractive targets for archeomagnetic studies.
In Mesoamerica clay has been used since pre-Hispanic times for the elaboration of a
wide variety of baked ornamental and utilitarian objects (e.g., pottery, tiles,) as well as for
constructive techniques (wattle and daub buildings, bricks, etc.). These items are
extensively employed for archeomagnetic studies due to the iron oxides contents in clays,
which are able to maintain a reliable record of the direction and/or intensity of Earth’s
magnetic field at the time of its elaboration or last use (Morales et al., 2011, 2015).
Also copper has been used in the production of a plenty variety of objects, usually
valuable non-utilitarian belongings. As a result of the pyro-metallurgical process of Cu-
sulfide ores to obtain this metal, copper slags are generated. Depending on the nature of
the ores, and other factors, the main oxides present in the slags are those of Fe (i.e.
hematite and magnetite), Si, Al, Ca and Cu. Similarly to the case of iron-oxides content in
clays, its presence within the matrix of copper slags would record the conditions of
geomagnetic field during its last cooling. This fact was verified by Ben-Yosef et al.
(2008), who showed empirically the usefulness of this material for the research of the
ancient geomagnetic field from a study conducted on hundreds of samples of copper slag
from Southern Levant. Shaar et al. (2010) studied the suitability of copper slag for
absolute paleointensity (Thellier type) experiments using electron microscopy and rock
magnetic experiments.
In this investigation we analyzed different fragments of copper slags (querendas in
Purépecha language) coming from seven pre-Hispanic and Colonial metallurgical sites of
Michoacán in order to (i) magnetically and chemically characterize this abundant waste
material, and (ii) assess their suitability to obtain absolute archeointensity determinations.
We report the results of rock magnetism experiments, scanning electron microscopy
(SEM) analysis and archeointensity determinations carried out on ten copper slag
fragments of archeological sites of Michoacán, western México. The results obtained from
most of the slags evidence the excellent behavior of these materials and confirm its
usefulness as a dating mean of ancient metallurgical centers of pre-Hispanic and Colonial
activity areas.
has been suggested the existence of smelting places during the pre-Hispanic and Colonial
stages; this is the case of Santa Clara del Cobre area (Fig. 1).
The listed archeological sites are concentrated in two main groups. The first group
encompasses sites where archeological elements of pre-Hispanic manufacture, associated
with the period of the Señorío Tarasco, possibly from the XVXVI century are found; i.e.
sites that were inhabited since pre-Hispanic times and continued to be occupied during the
Colonial era. Itziparátzico, very close to the present town of Santa Clara del Cobre, stands
out among these sites. Another site in the same category is Tiripatillo, where very few
examples of slag have been found. Finally, the site of Cuitzitan is a small settlement on
the shores of the town of the same name, which was located in a concentration of pre-
Hispanic and Viceroyalty archeological materials, including some samples of slag.
The second group of archeological sites comprises the settlements of Iramuco, Paso
del Muerto, Querendal, and Tepetate (Fig. 1). Here vast quantities of slag, product of
smelting processes at a larger scale than in the previous sites, can be found and only
viceroyalty-archeological vestiges and much recent historical material were found,
without any evidence of pre-Hispanic occupation on these sites. Through historical
sources it is known that from 1533 Santa Clara was added the nickname “de los cobres”;
which indicates an early vocation of the town for the metallurgical work during the
Viceroyalty. Yet in 1606, the ‘Fundición Real’ was settled at Santa Clara under the direct
administration of the Spanish Crown, becoming since then one of the most important
places of metallurgic work in Mexico.
Ten copper slag fragments, of varying thickness and textures, coming from pre-
Hispanic - Colonial (Itziparátzico, Cuitzitan and Tipitarillo) and Colonial (Iramuco, Paso
del Muerto, El Querendal and Tepetate) metallurgical sites, were analyzed.
3. METHODOLOGY
Archeointensity experiments
All prepared specimens were submitted to the Thellier-Coe method of archeointensity
determinations (Thellier and Thellier, 1959; Coe, 1967) at LIMNA facilities. The
experiments were carried out using a ASC Scientific TD48-SC furnace; all
heating/cooling runs were performed in air. Ten temperature steps were distributed
through the entire temperature range (from room temperature to 540C) with
reproducibility better than 2C between two heating runs to the temperature in turn. The
laboratory field strength was set to 45.0 ± 0.5 T along the cylindrical axis of the pellets.
Partial thermoremanent magnetization (pTRM) checks, carried out every third temperature
step, as well as pTRM tail checks determinations (Riisager and Riisager, 2001) at 350C
were also added to the protocol. Both natural and laboratory induced remanent
magnetizations were measured by using a AGICO JR6 dual speed spinner magnetometer.
Archeomagnetic dating
Attempts to obtain the most probable age interval for some slags were carried out by
assessment of the corresponding probability density function (PDF) obtained by the of use
the Matlab tool developed by Pavón-Carrasco et al. (2011), along with the global model
SHA.DIF.14k of Pavón-Carrasco et al. (2014) (calculated for the geographical position of
the site). This model is the latest developed using all the available paleomagnetic data for
their corresponding time intervals and applying the classical modeling approach, i.e. the
spherical harmonic analysis in space and the penalized cubic B-splines in time.
4. RESULTS
IRM acquisition curves for most samples look very similar in shape (Fig. 2), although
corresponding saturation remanence (SIRM) values are highly variable; while saturation is
reached in general between 300 and 400 mT, SIRM varies between 4 106 and
2.6 104 Am2/kg (see inset in Fig. 2). Low SIRM values correspond to Colonial
samples. Most samples show a pot-bellied shape (Fig. 3ac), while the Querendal-14 one
is of the wasp-waisted type (Fig. 3d). Similarly, all samples except Querendal-14 fall into
the pseudo-single-domain (PSD) region within the Day diagram (Fig. 3e); the outlier
sample locates in between the single-domain (SD) and PSD regions.
The homogeneity among magnetic properties above described also holds for the
heating branch of thermomagnetic curves; monotonically decrease up to 600C showing
the presence of at least two ferrimagnetic phases with Curie temperatures (TC) around 550
and 300C (Fig. 4); almost pure magnetite and substituted magnetite magnetic phases.
Likely candidates (at different proportions in each slag) could be (1) maghemite, as
a result of the transformation of iron-containing phases during the laboratory experiment,
(2) goethite, common in lacustrine areas of central Mexico, where wet and relatively cool
conditions are found (Morales et al., 2012), and which dehydrate to hematite between 200
and 400C, and (3) greigite, which breaks down to magnetite at ~270350C. The
singularities of Querendal-14 are also highlighted by thermomagnetic experiments, by
Fig. 3. a), b) and c) Representative hysteresis loops of copper slags. d) Hysteresis loops of the
Querendal-14 sample (M: magnetization). e) Corresponding Day plot (Mrs: saturation remanence;
Ms: saturation magnetization; Hcr: remanence of ceorcivity; Hc: coercive force). See Fig. 1 for site
codes.
Fig. 4. Thermomagnetic curves of representative samples. See Fig. 1 for site codes.
noting the remaining magnetization at high temperature. This remanence could be due to
the presence of hematite (Neél temperature TN 680C), in addition to other magnetic
components. In some cases, however, the cooling branch departs significantly from the
heating one (cooling curve above the heating curve). This may result from the presence of
a reducing atmosphere during the original smelting process (smelting at a covered
furnace), in which the reduced iron oxides (e.g., hematite) contained transform to new
magnetite during the laboratory experiment (Rada et al., 2008).
SEM observations reveal the presence of a crystalline structure (Fe and Cu sulfides
intergrowths) within the massive surface of some slags (Fig. 5), while a vitreous structure
is observed in some of them (Fig. 6). The presence of Cu and S were detected by spectral
X-ray mapping analysis (Figs 7a1a3 and 8a18a3), as well as lower contents of Ca and
Mg, and in very low proportions K, P and Ti. Most of the slags are shaped by Fe and O,
and in minor proportions by Al, Si and C (Figs 7b and 8b and Table 1). In general, the
massive surface of the iron mass, with lithic fragments (Si-Al), is observed.
So as to be considered as reliable estimations of the ancient geomagnetic field
strength, archeointensity determinations must satisfy the following conditions:
1. Directions of NRM end-points at each step obtained from archeointensity
experiments must align reasonably along a straight line directed to the origin in the
interval selected for archeointensity determination.
Fig. 5. High vacuum (20 kV) back-scattered-electron images of the pre-Hispanic ITZI-14
(SUP-65) sample. Note the growth of Fe and Cu sulfides crystals at higher magnification.
Fig. 6. Low vacuum (20 kV) back-scattered-electron images of the Colonial IRA-14 (SUP-313)
sample. Here a vitreous structure is observed instead.
7. Successful pTRM checks, i.e., pTRM check deviation is lower than 10%.
8. Residual pTRM tail is ≤ 10% (Riisager and Riisager, 2001).
Based on the above described criteria, seven out of the ten analyzed fragments yield
successful archeointensity determinations (Table 2), which corresponds to a 70% success
rate. These fragments showed an unusual experimental behavior, even better than ceramic.
It is clearly seen from Fig. 9a,b that conditions 1 and 2 are fulfilled, although small
viscous remanent magnetizations are observed. These magnetizations are, however,
eliminated at the very first temperature steps. The number of aligned point lies between 7
and 10, respectively. The f and q factors for the slag from the second group (CUITZI 14
SUP-315) vary from 0.917 to 0.951 and from 25.2 to 120.9, respectively, while for the
slag from the first group (PAMU 14 SUP-263) from 0.828 to 0.920 and from 30.1 to 45.1,
respectively. There are no concave-up shapes visible in these figures. pTRM check
deviation and residual pTRM tail are lower than 10% and 20%, respectively. It is worth
noting the high stability of the magnetic mineralogy, which is evidenced from the
successful pTRM check carried out from a high temperature step (450C) to a very low
temperature step (150C).
Fig. 7. a1)a3) Elementary spectral mapping of the pre-Hispanic ITZI-14 (SUP-65) sample,
showing the distribution of Fe, Cu and S, respectively, within the matrix of the slag.
b) Corresponding semi-quantitative geochemical results.
Fig. 8. The same as in Fig. 7, but for the Colonial IRA-14 (SUP-313) sample. Note the Fe and Cu
as sulphides segregation (darker areas in the center-bottom part).
pre-Hispanic
ITZI CUITZI
During the last decade some alternative material came into focus of archeomagnetic
research due to their thermally stable magnetic properties (Carrancho et al., 2015). Ben-
Yosef et al. (2008) showed that copper slag is usually produced during the heating of
copper ore up to 1200C. Gram-Jensen et al. (2000) carried out archeointensity
experiments on iron slags from Denmark. Ben-Yosef et al. (2009) reported systematic
investigations of copper smelting deposits. These slags are formed by fast cooling of the
melt and are derived from silicate and carbonate copper ores (see also Carrancho et al.,
2015). From these studies, a reasonably good agreement between archeointsities retrieved
Table 1. Continuation.
Colonial
PAMU IRA
from both copper slags and contemporaneous pottery samples is observed. This means
that, in terms of reliability, slags under study and pottery samples are reliable geomagnetic
field recorders. Similar material from Syria also exhibited very high thermal stability and
suitability to obtaining absolute archeointensity. Shaar et al. (2010) also considered the
suitability of copper slag for Thellier-type experiments using electron microscopy and
rock magnetic experiments. Their results, obtained by reproducing the intensity in
controlled experiments, showed a high accuracy of this approach using copper slags.
In the case of the Mesoamerican copper slags examined in this study, contrasting
differences can be identified from the different analysis carried out. Based on the obtained
values of Ms retrieved from IRM curves, which is a parameter mainly dependent to the
concentration of iron oxides, two main groups may be identified (see inset in Fig. 2). The
first group, shaped by those fragments gathered at four Colonial (Iramuco, Paso del
Muerto, Querendal and Tepetate) and two pre-Hispanic (Itziparátzico SUP 44,
Itziparátzico SUP 199) metallurgical sites, is characterized by low Ms values in the
interval (from 4 106 to 1.0 104 Am2/kg). The second group, composed exclusively
by the slags coming from two pre-Hispanic archeological sites (Itziparátzico SUP 25 and
Cuitzitán), corresponds high Ms values in the interval from 2.0 to 2.5 104 Am2/kg. At
this point it is worth remembering that pre-Hispanic archeological sites continued to be
occupied during the Colonial era.
Table 2. Individual intensity results of the different specimens per site: Tmin and Tmax: minimum
and maximum temperature step of the interval used for the intensity determination; N: number of
heating steps used for the intensity determination; m: slope of the best fit line; m: standard
deviation of m; f: fraction of extrapolated NRM used for intensity determination; g: gap factor;
q: quality factor as defined by Coe et al. (1978); H: archeointensity value; H: standard deviation
of H; pTRM Tail: remaining tail of partial thermoremanent magnetization at 350C. See Fig. 1 for
site codes.
No significantly differences in the grain size, as evidenced at the Day plot (Fig. 3e),
seem to be induced as a result of the particular pyro-metallurgical process of the Cu-
sulfide ores followed at both stages (pre-Hispanic and Colonial). The wasp-waisted
behavior shown by the Querendal 14 sample seems to be a characteristic of the used ore,
as well as of oxidizing smelting conditions.
In regard to thermomagnetic plots information, some other significant differences can
be observed. (1) Curves corresponding to samples from second group (pre-Hispanic) are
quite irreversible, while those from first group (Colonial) are mainly reversible (upper and
lower part of Fig. 4, respectively). This could be explained, again, in terms of significant
differences in the smelting prevailing conditions; smelting at a covered furnace (reducing
atmosphere) in the second group, while open air (oxidizing atmosphere) in the first one, as
Table 2. Continuation.
Table 2. Continuation.
Tmin Tmax H H pTRM Tail
[°C] N m m f g q [%]
[°C] [T] [T]
TIRI 14 (SUP-316), uncertain
20 515 12 0.972 0.018 0.967 0.870 45.43 43.74 0.81 1.1
20 465 10 0.889 0.038 0.890 0.833 17.34 40.01 1.71 1.7
100 515 11 0.982 0.017 0.926 0.862 46.11 44.19 0.77 0.2
100 500 10 0.899 0.012 0.920 0.851 58.65 40.46 0.54 0.5
150 500 9 1.019 0.013 0.878 0.835 57.47 45.86 0.59 4.0
100 500 10 0.983 0.012 0.924 0.844 63.88 44.24 0.54 5.7
Mean 43.1
St. Dev. 2.3
shown by Costanzo-Álvarez et al. (2006). (2) Initial magnetization values for slags of the
first group (in the order of 105106 Am2/kg) are one to two orders of magnitude lower
than those of the second group (104 Am2/kg). These differences can be explained, again,
in terms of differences in concentration and composition of iron oxides.
Fig. 10. Archeomagnetic dating of a) Cuitzitan and b) Tiripatillo sites. Upper panels: Intensity
reference curves (thick solid curves) with the 95% error envelope (dashed curves) calculated from
the SHA.DIF.14k global geomagnetic field model (Pavón-Carrasco et al., 2014) and the undated
archeointensity data (thick straight lines) with the 95% error envelope (dashed straight lines). Lower
panels: probability density function (PDF), calculated at 95% probability level, after comparison of
the site mean archeointensity value with the SHA.DIF.14k reference curve (Pavón-Carrasco et al.,
2014).
Fig. 11. The same as in Fig. 10, but for a) Itziparátzico and b) Paso del Muerto sites.
Datings shown in Fig. 10 are consistent with their pre-Hispanic and Colonial context,
respectively. The inconsistent results shown in Fig. 11 could be attributed to the
continuous pre-Hispanic - Colonial usage of the Itziparátzico site on the one hand. Partial
re-heating during Colonial period could have caused a decrease of the original
archeointensity value. On the other hand, the probably existence of a local (positive)
magnetic anomaly, due to the huge amount of superficial magnetic material, at Paso del
Muerto site - a locality where smelting processes at a larger scale were carried out - could
have generated an enhancement of the original archeointensity value. This is something
common in ore deposits, specially of iron.
In any case, the inherent interdisciplinary nature of the archeomagnetism must be
taking into account before any attempt of dating.
Acknowledgments: The exhaustive and constructive revisions of Bernard Henry and Ángel
Carrancho are greatly acknowledged. The authors are grateful to María de la Luz Gómez-Rivera and
Orlando Hernandez-Cristóbal (ENES, Unidad Morelia) for their participation in the archeointensity
and SEM determinations, respectively. AG is grateful for financial support of CONACyT 252149
and UNAM-PAPIIT projects IN105214 and 101717.
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