Palaeogeography, Palaeoclimatology, Palaeoecology 438 (2015) 239–244

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Palaeogeography, Palaeoclimatology, Palaeoecology

journal homepage: www.elsevier.com/locate/palaeo

Thermogravimetric analysis of property changes and weight loss in

incinerated bone☆
S.T.D. Ellingham ⁎, T.J.U. Thompson, M. Islam
School of Science and Engineering, Teesside University, TS5 5QG, Middlesbrough, United Kingdom

a r t i c l e i n f o a b s t r a c t

Article history: Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) are thermal analyses techniques,
Received 16 April 2015 which can give vital information about a material's properties and phase transitions when exposed to heating.
Received in revised form 8 August 2015 This study utilised a combined TGA-DSC approach to determine how exposure to varying temperatures and dif-
Accepted 10 August 2015
ferent heating regimes affect the decomposition of skeletal hard tissue. It was found that an accelerated heating
Available online 18 August 2015
rate causes the onset of phase changes in the bone matrix to be delayed to higher temperatures. The progression
Keywords:
of matrix changes within a certain phase is also highly dependent on the rate of heating. Longer exposure times or
Thermogravimetric analysis slower heating rates increase progression of decomposition within a certain phase, progression to a different ma-
Differential scanning calorimetry terial phase however will only occur after a key “activation temperature” is reached. These findings have impor-
Burnt bone tant implications for the subsequent analytical investigations of burnt bone.
Forensic anthropology © 2015 Published by Elsevier B.V.
Cremation

1. Introduction and geometrical spatial arrangement of bone vary between different

Burnt bones are a frequent occurrence in forensic contexts, be it in
the aftermath of a mass disaster, intentional immolation or to hide a
homicide, as well as in archaeological contexts. Heat is an extremely de-
structive force, which changes not only the morphology and architec-
ture but also the elemental and isotopic compositions of bone. The
extracellular matrix of bone is composed of a mineral phase (65 wt.%),
an organic phase (25 wt.%) and water (10 wt.%) (Chen et al., 2011).
The mineral phase consists of a poorly crystalline, non-stoichiometric
form of hydroxyapatite (Ca10(PO4)6(OH)2), also known as dahllite,
which incorporates several elemental substitutions, such as Mg and
other ions, however the most abundant substitution is carbonate
(3–8 wt.%) (Figueiredo et al., 2010). Depending on its crystal position,
carbonate apatite is classified either as a “Type A” (OH−) or “Type B”
(PO34 −) substitution, with the latter being more commonly found in
human bone. Despite the low percentage of lattice substitutions they
play a vital role in the bone's metabolism, and it has been found that car-
bonate not only decreases bone's crystallinity, but also accelerates its
biodegradation rate (Figueiredo et al., 2010). The main component of
the organic matrix is type I collagen, secondary components are non-
collagenous organic proteins including phosphoproteins, which may
play a role in the regulation of crystal size, orientation and habit of the
mineral matrix (Rho et al., 1998; Olszta et al., 2007). The composition
☆ The results of this study have been presented at the 67th Annual Meeting of the
American Academy of Forensic Sciences, Orlando, FL, February 2015.
⁎ Corresponding author.
E-mail address: ellingham.sarah@gmail.com (S.T.D. Ellingham).
skeletal elements, or depending on factors such as age, pathology,
disease or species (Aerssens et al., 1998; Quelch et al., 1983).
Thermogravimetric analysis (TGA) and differential scanning calo-
rimetry (DSC) are techniques very well established in materials sciences
and frequently applied to determine the properties of natural and syn-
thetic hydroxyapatites (Stanczyk and Van Rietbergen, 2004; Raynaud
et al., 2002; Figueiredo et al., 2010; Bertoni et al., 1998; Bahrololoom
et al., 2009; Gelinsky et al., 2008) for tissue engineering. Both tech-
niques measure the heat effects accompanying chemical reactions and
phase transitions as a function of temperature.
Their potential for the advancement of knowledge in the archaeo-
logical sciences is yet to be fully utilised.
The literature is in congruence in finding the weight loss of heated
bone to occur in three successive stages, the first below 200 °C, the
second between 200 °C and 600 °C and a third step between 700 °C
and 900 °C. At temperatures beyond 900 °C weight loss has been de-
termined to not be of significance (Figueiredo et al., 2010; Mkukuma
et al., 2004; Peters et al., 2000; Mayne Correia, 1997; Pramanik et al.,
2013). The first weight loss phase corresponds to an evaporation of
water bound to the bone matrix, the so-called “dehydration” phase
(Thompson, 2004) whereas the second, the so-called “decomposition”
phase is attributed to the combustion of the organic bone components,
particularly collagen. The last weight loss phase is mainly due to the re-
lease of CO2 produced though the decomposition of carbonate. This is
accompanied by an appearance of hydroxide ions (Mkukuma et al.,
2004) and a re-crystallisation of the mineral apatite in the “inversion”
phase. The final phase of bone transition occurring at temperatures be-
yond 900 °C, the “fusion” phase, does not exhibit a large weight loss, but

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rather is characterised by the sintering and melting of the crystallites
and the formation of an additional mineral phase, the β-tricalcium
phosphate (Thompson, 2004; Ellingham et al., 2015).
In a study designed to determine the effects the proportions of or-
ganic content in bone have on the thermal decomposition of the mineral
phase, Mkukuma et al. (Mkukuma et al., 2004) found that the two factors
are indeed closely related. Whilst all bones lose carbon dioxide when
heated between 200 °C and 600 °C, they found this loss to continue
more predominantly in bones with a low organic content up to temper-
atures of 1500 °C, accompanying an adsorption of water. They also found
bone of lower organic content to exhibit a greater carbonate content
than ones with a higher percentage of organic material, which in turn
have a larger content of HPO2− 4 ions in their mineral than the former.
Figueiredo et al. (Figueiredo et al., 2010) investigated the differential
behaviour of bovine, porcine and human bone (sections from a femoral
diaphysis) upon heating, thus drawing inferences on their property
variations. Through thermogravimetric analysis (TGA) at a temperature
increase of 10 °C/min, they discovered that whilst human and bovine
bone exhibit similar water contents, the H2O content of porcine bone
was markedly higher. Collagen content differed no more than 4% be-
tween species, with porcine bone also showing the highest weight
percentage. The carbonate content of all three tested species is also
very similar, with the bovine bone showing slightly higher amounts
than the other two.
Peters et al. (Peters et al., 2000) compared the different properties of
human healthy spongy bone, callus bone and tumour bone, and found
a substantially higher mineral content in tumour bone and the least
mineralisation in spongy bone, with the values for callus bone lying
in-between. Their study showed tumour bone to exhibit a carbonate
content over twice as high as spongiosa, the amount of carbonate in cal-
lus bone ranging somewhere in-between. These studies give an insight
into the various factors influencing bone composition.
Raynaud et al. (Raynaud et al., 2002) investigated the thermal prop-
erties of isolated hydroxyapatite powder. They found the first weight
loss to occur at between 1000 °C and 1450 °C, caused by the dehydrox-
ylation of the hydroxyapatite, which accompanies the formation of
tricalcium phosphate and tetracalcium phosphate monoxide in a highly
endothermic reaction.
Several studies have monitored the thermal behaviour of both, colla-
gen and hydroxyapatite, separately (Lozano et al., 2003; Trȩbacz and
Wójtowicz, 2005). A study comparing the thermal behaviour of intact
Fig. 1. Average TGA curves of bones subjected to differing heating regimes.
bone samples and isolated collagen (Lozano et al., 2003) found extracted
collagen to be more thermally stable than collagen in bone. They attri-
bute the lack of stability of collagen in bone to the fact that hydroxyap-
atite crystals in the fibril intraspaces act as fracture centres, decreasing
the number of collagenous cross linkage (Lozano et al., 2003; Miles
et al., 2005). Trȩbacz and Wójtowicz (Trȩbacz and Wójtowicz, 2005)
who compared the thermal behaviour of intact bone, demineralised
bone and tendon collagen up to 300 °C found the first endothermic
peak, which is associated with the loss of water, to occur at temperatures
around 100 °C lower in collagen and demineralised bone than in intact
bone.
It is the aim of this study to investigate the influence that different
heating regimes and varying exposure times have on the rate of proper-
ty changes of heated bone, and thus the exposure temperature ranges
after which successful further analyses can be carried out.
2. Materials and methods
Fresh domestic sheep (Ovis aries) rib bones, acquired from a local
butcher, containing both compact and cancellous bone, were cut into
cross sections weighing approximately 20 mg and analysed on an
Evisa® STA 1500 Simultaneous Thermal Analyzer (Bähr-Thermoanalyse
GmbH, Hüllhorst, Germany). Samples were enclosed in aluminium oxide
crucibles and heated from 20 °C to 1100 °C in a stream of air delivered
from a cylinder. Samples were heated in triplicates at heating rates of
6 °C/min, 12 °C/min and 24 °C min. Additionally two sets of samples
were heated at a rate of 12 °C/min up to a maximum of 300 °C and
400 °C, at which temperature they were held for 45 min. An empty cru-
cible was heated simultaneously under the same conditions as the sam-
ples and the resulting thermogram was subtracted from that of the
samples, enabling the correction of buoyancy effects.
3. Results
The thermograms of the samples subjected to the three different
heating regimes exhibited comparable patterns showing three distinct
stages of weight loss, however occurring at slightly different rates
(Fig. 1).
Similarly, the DCS heat flow curves indicated an approximately 25 °C
delay in the temperature onset of the matrix phase changes, with every
doubling of the heating rate (Fig. 2).
 S.T.D. Ellingham et al. / Palaeogeography, Palaeoclimatology, Palaeoecology 438 (2015) 239–244 241

Fig. 2. Average DSC curves of bones subjected to different heating regimes.

In order to determine the exact temperature ranges of increased
weight changes the first derivative of the TGA curve (Δmass/Δtemp)
was calculated. Distinct peaks were noted at around 100/125/150 °C,
350/375/400 °C, 475/500 °C/NA and 750/775/800 °C at the heating
rates of 6, 12 and 24 °C/min respectively (Fig. 3).
These observed weight changes correspond with the matrix phase
alterations shown by the DSC, which show an endothermic process
taking place until heating of around 350 °C, peaking between 100 °C
and 150 °C, which is superseded by an exothermic reaction up to around
450 °C, which is followed by another brief endothermic phase, imme-
diately trailed by a strong exothermic reaction with a peak at 500 °C
and continuing until 750–800 °C at which point a slight endothermic
phase remains.
The three different heating regimes also resulted in different weight
losses at the maximum temperature of 1100 °C. The largest weight loss
occurred in the samples heated at a rate of 6 °C/min, which retained
an average of merely 40.4% of their original mass. Samples heated at
12 °C/min retained 42.3% and samples heated at 24 °C/min retained
45.9% of their mass.
Exposure time also appeared to have an influence on the samples
which were held at fixed temperatures. The samples which were held
at 300 °C retained an average of 83.46% of their original weight, which
however was reduced to a mere 66.68% after being held at this constant
temperature for 45 min (Fig. 4).
Samples held at a constant when reaching 400 °C started out with
64.8% of their original weight, which was reduced to 50.6% after 45 min.
4. Discussion
The overall thermal behaviour of the experimentally heated sheep
ribs was in concordance with the findings of previous studies, albeit
temperature ranges for the onset of mass loss varied slightly. Previous
studies have reported weight changes to occur between 300 °C and
1000 °C (Thompson, 2005), the weight loss observed in this study

Fig. 3. Average TGA 1st derivative curves from bones subjected to different heating regimes.
242 S.T.D. Ellingham et al. / Palaeogeography, Palaeoclimatology, Palaeoecology 438 (2015) 239–244
Fig. 4. Average TGA curves of bones heated to 300 °C and 400 °C respectively and held at these temperatures for 45 min.
commenced at temperatures as low as 50 °C in samples heated at
6 °C/min and ceased to lose any further mass at 700 °C in the 6°/min
heated samples and at 900 °C in the 24 °C/min samples.
The first phase of weight loss, peaking in the temperature range
of 100–150 °C is mainly attributed to the evaporation of water which
can be detected as the large endothermic event on the DSC graph
(Fig. 2). The second weight loss phase, which is also the most severe,
is attributed to the combustion of the organic components which intro-
duces the exothermic process of the hydroxyapatite re-crystallising.
A brief endothermic event attends the decomposition of the carbonate
at around 450 °C, which is followed by a strong exothermic phase as
the bone's collagen continues to combust, spiking at around 500 °C,
and the re-crystallisation of mineral proceeds. The process remains exo-
thermic up to 750–800 °C, at which point the minerals begin to sinter
and melt in a slightly endothermic event. From 400 °C onwards the
1st derivative of the TGA curve clearly shows a different weight loss
pattern between the samples subjected to the differing heating regimes.
The 6 °C/min exhibits a sharp weight loss peak at 460 °C, associated with
the decomposition of carbonate, and some less prominent smaller peaks
at 550 °C and 660 °C, before ceasing to lose any more mass from 700 °C
onwards. The carbonate loss peak is less pronounced in the samples
heated at 12 °C/min, peaking between 450 °C and 500 °C. The last organic
components are lost at around 800 °C, seen as a spike on the derivative
plot, after which no more mass loss is recorded. Samples heated at a
rate of 24 °C/min do not show any weight loss peak associated with
carbonate loss in the TGA derivative curve, but rather a regular
decrease, indicating a prolonged loss of carbonate over progressive
heating, rather than the almost instant loss which can be seen in the
6 °C/min curve. At temperatures exceeding 900 °C the 24 °C/min
samples do not exhibit any further weight loss.
The increase in heating rate did not only delay the onset of the bone's
phase transition and the temperature at which all organic components
were completely combusted and no more weight loss occurred, but
also demonstrated an influence on the total weight loss, the samples
heated at 6 °C/min having lost 5% more mass when heated to 1100 °C
than the samples heated at 24 °C/min. The observation that exposure
time has an influence on the loss of mass was confirmed by the sam-
ples which were held at fixed temperatures of 300 °C and 400 °C re-
spectively for 45 min. The samples which were held at a constant of
300 °C reached this temperature after 22 min retaining 83.46% of their
starting mass, and continued to lose another 16.78% in the remainder
of the holding time due to the complete evaporation of water and com-
mencing combustion of the organic compounds. As can be extracted
from the 1st derivative curve of the TGA measurements, a prominent
loss of 8.2% mass occurs within 7 min of first reaching the target temper-
ature of 300 °C, after which it continues at a less dramatic rate losing an
additional 8.6% in the following 40 min. The samples which were con-
tinuously heated to 400 °C and subsequently held at this temperature,
demonstrated a pattern identical to the one described for the samples
continuously heated at 12 °C/min, exhibiting a prominent weight loss
peak due to the combustion of organic compounds between 300 °C
and 400 °C (Fig. 5).
However, instead of experiencing another spike in weight loss
for the decomposition of carbonate, as has been observed in samples
heated to temperatures of up to 500 °C, the samples held at a constant
of 400 °C only continued to lose 14.2% mass associated with retained
organic components over the following 45 min. This can be extracted
from the corresponding DSC curve showing no phase changes after
the one introducing the collagen combustion at around 300 °C (Fig. 6).
These observations show, that whilst an increase in exposure time
may increase overall bone weight loss as the processes started at a spe-
cific activation temperature continue to proceed, however, from what
can be seen in the framework of this experimental work, the bone will
not enter transition to a different material phase by mere duration in-
crease, if the appropriate phase activation temperature is not reached.
These findings are in concordance with the findings of Ellingham et al.
(Ellingham et al., 2015) who found that a variation in exposure time
did not have a significant influence on the Fourier transform infra-red
(FTIR) spectra of burnt bone and therefore retrospective temperature
prediction. Once a certain phase change has commenced, its progress
can, however, be altered by the exposure time; in this study the weight
loss peaks for samples heated at 6 °C, 12 °C and 24 °C exhibited a ca 25 °C
shift with every doubling of temperature. This can be explained by the
fact that the activation energy in bones heated at a slower rate is signif-
icantly higher than at faster rates, a phenomenon which has also been
measured by Yang et al. (Yang et al., 1997).
Gaining a more comprehensive understanding of the factors
influencing the onset of property changes and phase transitions in
heated bone can be crucial to determine whether a sample will yield
results from further analyses, such as carbon dating, stable isotope
analyses or even DNA analyses, which can be quite cost- and time con-
suming. Studies have showed DNA to be successfully amplifiable in
 S.T.D. Ellingham et al. / Palaeogeography, Palaeoclimatology, Palaeoecology 438 (2015) 239–244 243

Fig. 5. Average TGA 1st derivative curves of bones heated to 300 °C and 400 °C respectively and held at these temperatures for 45 min.

experimentally burnt sections up to temperatures of 200 °C at 2-hour
exposure duration (Imaizumi et al., 2014; Fredericks et al., 2012), tem-
peratures that coincide with the onset of collagen degradation as ob-
served by the thermogravimetric studies.
For the dating of skeletal remains the collagen making up the organic
portion of the bone is routinely used. This is the case for two reasons:
collagen includes 95% of the bone's carbon and therefore allows smaller
sample sizes to still yield results, and secondly, the carbon which is
found in the mineral fraction of the bone, the carbonate apatite, has
been found to be thermodynamically unstable and prone to diagenetic
changes (Zazzo et al., 2009). When heated, the bone organic matter is
completely degraded at temperatures between 500 °C and 600 °C;
nonetheless carbon dating has successfully been performed on cremat-
ed bone which has been subjected to temperatures of 700 °C and above,
in fact, the success rate has been found to increase from temperatures of
600 °C onwards (van Strydonck et al., 2005, 2010; Zazzo et al., 2012;
Hüls et al., 2010). These findings indicate that an intercalation of “for-
eign” carbon from the atmosphere or the fuel source into the bone apa-
tite takes place whilst the bone is undergoing the phase changes caused
by heating. These physico-chemical changes during calcination, such as
the re-crystallisation, increase the bone's resistance to diagenetic factors,
which in turn has a direct positive impact on its reliability for 14C dating
(Zazzo et al., 2012). The apatite carbonate decomposes, thus causing
a decrease in the stress on the crystal structure, and the subsequent re-
crystallisation functions as a protective barrier, rendering the calcined
bone a closed system trapping in the deposited carbon. Several authors,
however, cautioned that the external carbon uptake might pose a source
for error, should “old” fuel, such as ancient wood, coal or peat, be used
(van Strydonck et al., 2005; Snoeck et al., 2014a). In some instances
they reported this effect to cause a dating offset of decades and centuries.
Similar trends to those observed for the success rate of carbon
dating, have been found to apply to the analyses of stable isotopes,

Fig. 6. Average DSC curves of bones heated to 300 °C and 400 °C respectively and held at these temperatures for 45 min.
244 S.T.D. Ellingham et al. / Palaeogeography, Palaeoclimatology, Palaeoecology 438 (2015) 239–244
such as 86Sr and 87Sr, the two isotopes of strontium, which are widely
used to reconstruct faunal geographical origin or mobility in archaeo-
logical settings as well as in forensic investigations (Bentley, 2006;
Price et al., 2000; Beard and Johnson, 2000; Snoeck et al., 2014b).
Calcined bone, meaning bones which have already undergone re-
crystallisation and therefore have been exposed to temperatures of
700 °C and above, have been found to produce the most reliable
87
Sr/86Sr isotope ratios (Snoeck et al., 2014b). The protective shield
formed by the re-crystallised hydroxyapatite locks in in vivo isotope ra-
tios and is extremely resistant to the intercalation of exogenous stron-
tium from the burial or depositional environment.
5. Conclusion
Thermogravimetric analyses are a valuable tool for gaining a more
comprehensive understanding of the thermal behaviour of bone. This
study has shown, that the progression of the matrix changes within a
certain phase (dehydration, decomposition, inversion and fusion) is
highly dependent on the rate of heating, with an accelerated heating
rate causing a delayed onset of phase changes to higher temperatures.
It has, however, been shown that in order for this accelerated progres-
sion to occur, a certain “activation temperature” to enter a certain
phase has to be reached first. Prolonged exposure to a certain tempera-
ture will progress the characteristics of this phase, but will not cause
entry into the next phase change, at least not for the time spans observed
within this experimental setup. An extended exposure to “decomposi-
tion” temperatures of 300 °C for example, will entail a progress in the de-
composition of organic bone components and an increased weight loss,
however the “inversion” stage of mineral re-crystallisation will not be
entered at these temperatures. These are crucial insights into the ther-
mal behaviour of bone, with important implications for an improved
estimation of the success rate of subsequent analytical investigations.
Acknowledgments
The authors would like to express their gratitude to Dr. Yongxin
Pang (Teesside University) for his assistance with the operation of the
thermogravimetric analyser, as well as Reem Abdulhadi (CChem, Uni-
versity of Edinburgh) for her invaluable help with formatting the
figures.
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