J Forensic Sci, May 2009, Vol. 54, No.

3
doi: 10.1111/j.1556-4029.2009.01037.x
TECHNICAL NOTE Available online at: www.blackwell-synergy.com

Giampaolo Piga,1 M.Sc.; Tim J. U. Thompson,2 Ph.D.; Assumpci Malgosa,1 Ph.D.;

and Stefano Enzo,3 M.Sc.

The Potential of X-Ray Diffraction in the

Analysis of Burned Remains from Forensic
Contexts*

ABSTRACT: In view of the difficulties in extracting quantitative information from burned bone, we suggest a new and accurate method of
determining the temperature and duration of burning of human remains in forensic contexts. Application of the powder X-ray diffraction approach to
a sample of human bone and teeth allowed their microstructural behavior, as a function of temperature (200–1000C) and duration of burning (0, 18,
36, and 60 min), to be predicted. The experimental results from the 57 human bone sections and 12 molar teeth determined that the growth of
hydroxylapatite crystallites is a direct and predictable function of the applied temperature, which follows a nonlinear logistic relationship. This will
allow the forensic investigator to acquire useful information about the equilibrium temperature brought about by the burning process and to suggest a
reasonable duration of fire exposure.

KEYWORDS: forensic science, cremated remains, burned bones and teeth, hydroxylapatite, powder X-ray diffraction, forensic
anthropology

The study of burned human remains is of considerable impor- experimentally and statistically that the most important changes in
tance in forensic science, forensic anthropology, and crime scene bone that can predict burning context involve changes within the
investigation. An understanding of the changes that the body has skeletal microstructure (10). With all this in mind, it has been
undergone as a result of burning can provide significant informa- argued that a better and more reliable means of addressing these
tion regarding the context and conditions of the burning event issues is with the powder X-ray diffraction (XRD) approach, possi-
itself. Such crime scene information can include the temperature of bly combined with other types of microscopic approaches (11),
the fire, the position of the fire, and the presence of accelerants. with a particular focus on the hydroxylapatite (HA) mineral phase,
Unfortunately, the act of burning also causes a number of substan- which is the main inorganic component of bones.
tial changes to occur within the skeleton, which in turn can affect The HA phase is made of tiny micro- (or nano-) crystals with
attempts to provide an identification of the deceased. Research has average size dimension around ca. 17 nm, that are subjected to
shown that both morphological and metric methods of anthropolog- growth changes when stimulated by the temperature of a fire.
ical assessment are affected (1,2), in addition to methods of dating Broadly speaking, higher temperatures result in larger average sizes
(3) and stable isotopic analysis (4) (an analytical technique of of HA nano-crystals, more ordered crystal structures and therefore
increasing importance in the forensic field). Extracting this contex- sharper XRD peak profiles. These heat-induced crystal changes are
tual information from the remains, in addition to determining the akin to those resulting from standard bone diagenesis, and therefore
level of anthropological inaccuracy created by the burning event, is we acknowledge that in the absence of important thermal effects,
dependent upon being able to determine whether the skeletal bone material decomposing for millions of years may undergo a
remains have indeed been burned. Beyond this, one needs to be similar crystal growth mechanism—which can also be detected and
able to correlate the changes in the skeleton to this contextual accurately measured with help of the XRD patterns (12–14).
information with confidence. Traditionally, a visual inspection of The XRD technique was first applied to archaeological subjects
the remains has been used to suggest whether the bones have been in 1964 (15). Later Bonucci and Graziani (16) demonstrated that
subjected to fire (5–7), and beyond this, associations have been high temperatures of fire treatment induce a growth of the average
made between bone color and fracturing with fire temperature and crystallite size of HA, which can be appreciated relatively well
presence of soft tissues (8,9). However, this can be complicated, from the line broadening ⁄ sharpening analysis of diffraction peaks.
and the links spurious. Furthermore, it has also been shown both Since then, XRD has become a standard tool in anthropological
work, although its adoption in forensic anthropology has been
1
Unitat d’Antropologia, Department de Biologia Animal, Biologia Vegetal slow.
i Ecologia, Universitat Autnoma de Barcelona, Barcelona, Spain. In the first critical study of its kind, Shipman et al. (17) investi-
2
School of Science & Technology, University of Teesside, Borough Road, gated the microscopic morphology of various osteological materials
Middlesbrough, UK. and used XRD in order to assess whether specimens of unknown
3
Department of Chemistry, University of Sassari, Sassari, Italy.
*Financial support provided by Sardinia Autonomous Region of Master
taphonomic history were burnt and the maximum temperature
and back project TS160. reached by those specimens. Like the previously cited studies, these
Received 15 April 2008; and in revised form 4 Aug. 2008; accepted 9 investigations were based on the fact that heating of bone causes a
Aug. 2008. sharpening of diffraction patterns, attributed to increased crystallite

534  2009 American Academy of Forensic Sciences

 PIGA ET AL. • XRD IN THE ANALYSIS OF BURNED REMAINS FROM FORENSIC CONTEXTS 535

size and decreased lattice strain (i.e., increased organization of the of mineralogical phases while keeping instrumental parameters into
crystal structure) of osteological phases. Rogers and Daniels (18) account. This is a necessary prerequisite in order to correctly distin-
and other recent works (10,19) have also recorded key crystalline guish the average crystallite size from the lattice disorder when
changes within the temperature range here investigated. The poten- using a peak broadening method such as this. This method may
tial for XRD to associate crystal change to burning context is there- replace previous approaches that were adopted to study the bones
fore not in doubt. based on an arbitrarily defined ‘‘index of crystallinity.’’
To further extend the validity of XRD methodologies that appear
in the literature, we present a calibration for bones and teeth as a
Results and Discussion
function of a range of temperatures of burning (200–1000C), while
simultaneously noting the effect of duration of burning (0, 18, 36, In Fig. 1, we report a pattern of XRD intensity from the
and 60 min). In practice, this would enable a more rounded untreated human femur sample, here studied as a function of the
account of the burning scenario to be realized. In fact, with this scattering angle 2h. A full curve using the Rietveld fit has been
approach it will be possible to make an accurate estimation of both calculated according to the 97 wt% contribution of the structure
temperature and likely time duration of the firing process involved. factors of HA (monoclinic, space group P21 ⁄ c, refined lattice
This is not possible with current macroscopic approaches. parameters a = 9.440, b = 18.898, c = 6.896  and b = 120.67)
We have started our analysis with dry bone. First, we acknowl- and 3.0 wt% of calcite (trigonal, R-3c, a = 4.988, c = 17.070 )
edge that this may not entirely accurately mimic real-world scenar- and has been added to the graph. As is usual in the Rietveld
ios; however, we argue that although the influence of soft tissues approach, the curve difference between calculated and experimental
may affect the temperature ⁄ duration required to alter the bone data points is shown at the bottom, while the sequence of bars indi-
microstructure to the level that we present, they would not alter the cate the expected peak positions for each phase. Examination of
ability of XRD to associate these changes to a burning context. this feature is particularly useful in determining whether skeletal
Second, it is unlikely that the presence of the organic component material has been burned or whether the changes are due to other
within the bone would alter the crystalline composition significantly taphonomic events (such as 23,24).
from that in a dry bone (data to be published in the near future, The quantitative Rietveld analysis points to the fact that HA is
but see also previous XRD studies augmented with thermo-gravim- the main phase for bones. The structure of HA is reported as hex-
etry experiments). Bonhert et al. (20) observed that for total incin- agonal with a space group of P63 ⁄ mmc, but the monoclinic struc-
eration of a body via cremation about 2 h are necessary at a ture factor (25,26) was preferred here since it gave systematically
constant temperature of 800C, while for destruction of the fleshy better agreement factors with our results. The peak profiles of HA
parts about 50 min are believed to be needed. Thus, in the follow- are very broad on account of the nanocrystalline condition of the
ing study we have selected comparable burning times. Of course, it material with very small average crystallite size and ⁄ or large lattice
is not absolutely guaranteed that the ramp heating process applied disorder. The average coherent diffraction domain calculated after
in the laboratory furnace will accurately reproduce the heating pro- separating strain from size effects according to the Rietveld
cess of a real fire. It should also be noted that a burning event may approach is in the range between 168 and 170 .
not cause complete change throughout the bone cortex; however, Note that apart from the root mean square deviation problems,
our XRD technique involves the grinding of bone samples, thereby this result may be different from the figure normally obtained by
assessing a volume-weighted average crystal size sampled over an applying the Scherrer equation (27) on the most intense peak. In
at least ‘‘bimodal’’ distribution, which would reduce the influence fact, using this equation within the Rietveld approach for a modern
of differences between the outer and inner regions of the bone. bone, Michel et al. (28) determined an average crystallite size of
138 . The value may also be distinct from the average particle
size that can be evaluated using SAXS data, as the latter may refer
Materials and Methods
to a collection of agglomerated crystallites (10,29,30). Furthermore,
We have used 57 human femoral fragments and 12 molar teeth
for this experiment. The samples used for calibration were heat-
treated with a heating rate of 20C ⁄ min at selected temperatures
(200–1000C for 0, 18, 36, and 60 minutes) in air using a NEY
muffle furnace. The specimens for X-ray investigations were
powdered by manual grinding in an agate mortar.
The XRD patterns were recorded overnight using Bruker D8
(Bruker AXS GmbH, Karlsruhe, Germany), Philips PW-1050
(PANanalytical, Almelo, The Netherlands), Siemens D-500
(Siemens AG, Munich, Germany), and Rigaku D ⁄ MAX (Rigaku
Corporation, Tokyo, Japan) diffractometers in the Bragg–Brentano
geometry with CuKa radiation (k = 1.54178 ). The goniometer
was equipped with a graphite monochromator in the diffracted
beam and the patterns were collected with 0.05 of step size. The
X-ray generator worked at a power of 40 kV and 30 mA and the
resolution of the instruments (divergent and antiscatter slits of 0.5)
was determined using a-SiO2 and a-Al2O3 standards free from the
effect of reduced crystallite size and lattice defects. The powder FIG. 1—The XRD powder pattern of untreated femour fragment used as
patterns were collected in the angular range 15–120 in 2h and sample reference coming from the Grave yard ossuary of Sassari. Experi-
ment are data points, full line is the Rietveld refinement on the basis of
were analyzed according to the Rietveld method (21), using the hydroxylapatite and calcite structure factors. The line at the bottom refers
programme maud (22). This is an efficient approach that evaluates to the residuals, i.e., the difference between calculated and experimental
quantitatively the amount, structure, and microstructural parameters square root intensities, which is indicative of the agreement obtained.
536 JOURNAL OF FORENSIC SCIENCES

it should be kept in mind that average values from transmission temperature range corresponds with the temperature of the average
electron microscopy observations refer to a surface weighted mean house fire (32). For specimens treated at temperatures higher than
(31), and thus may also differ from this work. 850C and for long burning times, the determination of the average
In Fig. 2, the XRD pattern and Rietveld fit of an untreated human crystallite size may be difficult to reproduce because of the upper
tooth is reported. In comparison to Fig. 1, it can be seen that the resolution of instrument broadening. In fact, an upper limit of
peaks for calcite are absent. Moreover, the peaks for apatite appear 1500  for crystal size determination is generally associated with
sharper (on account of a larger average crystallite size of ca. 224 ). this technique. This upper limit is a problem also experienced by
Differences in microstructure are likely related to the different other techniques (30).
mechanical properties of apatite in teeth and bones, respectively. The simplistic association between bony changes and tempera-
The results of our investigation into the average crystallite size ture alone has been criticized previously, whereby it was argued
of the sample of femoral bone as a function of applied temperature that high temperature and low duration events may result in similar
(which is an equilibrium temperature of the furnace) and duration heat-induced changes to low temperature and high duration events
of burning are reported in Table 1 and given in ngstrom () (10). Our data confirms this assertion, as here a burning time of
units. For temperatures of 200C to around 650C (0 min) no sig- 60 min evidences an effect of crystallite growth that would be
nificant growth of HA appears to be induced. Also, the burning obtained at temperatures c. 100C higher without any burning time.
times of 18, 36, and 60 min at these temperatures are not dramati- The markedly different behavior for the specimens treated above
cally changing the microstructure, with only slight effects of grain 650C is clearly seen in Fig. 3a, b, where symbols refer to the
growth, on account of a relative stability of the system. This is not measured crystallite size values as a function of temperature treat-
so from 700C (36, 60 min) to higher temperatures, where an effect ment. For the sake of clarity, the results concerning the curve with
of sudden growth appears evident and further distinguishable in the 36 min of burning time are reported separately since they closely
temperature range 750–850C, where three separate trends for the overlap the data of curve from 18 min exposure. Restricting our
growth processes can be evaluated. This is significant since this

(a)

(b)
FIG. 2—The XRD pattern (data points) and relevant Rietveld fit (full line)
of an untreated tooth. From the quality of fit it is concluded that the tooth
is made of pure apatite single-phase with average crystallite size of 224 ,
larger than the correspondent figure observed for human bones.

TABLE 1—Average crystallite size of the hydroxylapatite mineral phase

(1  = 10)10 m).

Temperature (C) 0 min 18 min 36 min 60 min

Not burned 170
200 175 175 175 175
300 180 184 186 188
400 195 203 204 205
500 202 202 205 210
600 204 226 230 256
650 213 240 250 258
700 229 294 463 486
750 268 611 712 800 FIG. 3—(a & b) The average crystallite size evolution for hydroxylapatite
775 350 836 880 920 as a function of temperature treatment and residence times indicated. The
800 432 1030 1160 1200 experimental data from the Rietveld analysis have been fitted with sigmoid
825 732 1120 1140 1254 curves of logistic type which are typical of physico-chemical growth pro-
850 923 1380 1450 1500 cesses. The scatter of data and curves gives an idea of the uncertainty
900 1351 >1500 (1616) >1500 (1680) >1500 (2621) related to the determination of the temperature treatment for a bone of
1000 >1500 (1569) >1500 (2195) >1500 (2600) >1500 (2950) unknown provenance.
 PIGA ET AL. • XRD IN THE ANALYSIS OF BURNED REMAINS FROM FORENSIC CONTEXTS 537

attention to the specimens heated without any burning time, we can

appreciate even with the logarithmic scale the rather sudden
increase of the average crystallite size for temperatures around
750C, in agreement with previous XRD observations.
The growth process seems to proceed up to 1000C following a
sigmoidal growth-type law typical of most reactions in a solid state.
The following equation (full lines) was fit to the experimental data:
y ¼ A2 þ ðA1  A2 Þ=ð1 þ ðx=x0 Þp Þ

The optimized parameters (presented in Table 2) have a precise

physical meaning: A1 value was actually fixed to the size dimen-
sion of HA for samples before any heat-induced growth; A2 is the
size limit reached at the end of the growth process; x0 is the tem-
perature relevant to the flex point of the logistic curves and p is a
parameter for the growth rate, likely dependent on scanning rate,
temperature, and duration of burning. Note that for the series with FIG. 4—The comparison of the growth kinetics of hydroxylapatite crystal-
duration of 0 min the growth phenomenon is particularly sharp in lites as a function of temperature for teeth and bones at 0 min of residence
the range 750–900 C since p = 24, while for the other two curves time. Full lines are fit of experimental data according to the logistic
function reported in the text. The characteristic temperature of the process
the growth kinetics appears to occur in a more extended range from (i.e. the inflection point of curves) is the same in the two cases while the
600C to 1000C where the relevant p-values are quite close to 12. sharpness and amplitude is larger for bones.
It can be seen from Table 3 that the behavior and growth mech-
anism of teeth as a function of firing temperature (with 0 min of
burning time) is similar to that observed in bones. This is a useful 224 , the A2 figure was 994 , while the inflection point for the
observation as it suggests that data collected from one hard tissue growth process Xo is located at 841 , with the p parameter of 17.
are applicable to the other. However, the final average values of These numerical parameters emphasize the similarities and differ-
HA microcrystallites at high temperature appear slightly reduced. ences between the behavior of teeth and bones as a function of
This is of limited surprise since the enamel tooth crowns are temperature, which is reported for the sake of comparison in
known to fragment under firing in the temperature range between Fig. 4. As can be seen, the average size increases for the crystal-
700 and 750C—presumably due to the high pressure exerted by lites of HA are lower when compared to those observed for the
water molecules trapped inside by the tooth enamel, which is of HA of femoral bone, but the inflection point of the two sigmoidal
course made by highly compacted HA. Nonetheless, the data plot- curves appears to be practically the same.
ted confirm a logistic trend which was fitted again with the sigmoi- We report in Fig. 5 a selected portion of the patterns from
dal equation used previously. Of course, the A1 parameter turns out between 30 to 39 in 2h from the burning of the femoral speci-
to be close to the initial value for the average crystallite size of mens at temperatures of 700, 775, 800, 825, 850, 900, and 1000C,
respectively. Figure 5 shows the disappearance of the calcite and
TABLE 2—The best-fit parameters of the four logistic curves represented
in Fig. 3a and 3b.

Parameters 0 min 18 min 36 min 60 min

A1 (fixed) 180 180 180 180
A2 1597 2420 2832 3528
X0 845 844 855 860
p 24 12 12 12.46
At variance with duration of exposure, the three sigmoidal curves are all
located around 850C. The p parameter is related to the sharp behavior of
the function.

TABLE 3—The average crystallite size of HA phase of teeth as a function

of temperature. Also, in this case the growth mechanism can be located at
c. 850C.

Average
Temperature ⁄ C Cystallite Size
Not burned 224
200 227
300 228
400 230
500 233
600 245
700 293
750 345 FIG. 5—A selected range of the XRD patterns of sample bone treated at
800 400 the indicated temperatures. It is evident the progressive peak sharpening of
850 659 hydroxylapatite as a function of the indicated temperatures, simultaneous to
900 827 the appearance of CaO phase following the decarbonization reaction which
1000 947 starts at 775C.
538 JOURNAL OF FORENSIC SCIENCES

that burning event. In the thermal treatment of 0 min, the growth

rate parameter p seems to be higher than in the results from
increased periods of burning. Thermal treatments at a given temper-
ature for 60 min demonstrate the equivalent growth effects for
0 min of burning but at 100C higher.
In the case of teeth, the growth phenomena induced by firing are
again described with a logistic type function with a characteristic
temperature of 841C, very close to that of bones, in spite of typi-
cal fragmentation induced in the temperature range 700–750C.
However, the average crystallite size of HA in untreated teeth
(224 ) is significantly larger than in untreated skeletal bones
(c. 170 ), respectively. Alternatively, the average size of HA crys-
tallites from burning above 900C is larger in bones than teeth.
This suggests that the two types of natural bioapatite need to be
compared to their specific calibration curves when the precise esti-
mation of the temperature of a fire is desired, and that one curve
for all hard tissues is not advised.

Acknowledgments
The authors thank Prof. Vittorio Mazzarello (University of
Sassari) for supplying the osseous materials employed in this
FIG. 6—A selected portion of the XRD patterns of teeth treated at the study. Thanks are also due to: Dr. Ignasi Galts (Universitat
quoted temperatures (data points) with the correspondent Rietveld fit (full
lines). The appearance of the CaO cubic phase is perceived after treatment
Autnoma de Barcelona) for helpful discussions concerning the
at 850C. The fraction of CaO with respect to hydroxylapatite is lower than forensic applications.
for the case of bones.
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