SEM-EDX in Ancient Human Dental Calculus 1209
incisors of his lower jaw showed traces of the trauma of a military origin (Fig. 2c). The municipal chronicle of Majetín describes this area as a burial place of Napoleonic soldiers. No more sensitive dating material (such as parts of military equipment) was discovered there. Samples of supragingival calculus (above the gum line)
were taken manually in a flow box by germfree periodontal instruments (scaler, chisel) (Fig. 2a) into sterile plastic bags. In total, we performed EDX analysis of almost 20 sam-
ples of calculus from several individuals (different historical periods), however, there were no interesting results nor any hypothesis of their habits. Therefore they are not attached in this work. A usual spectrum (from the ancient human dental calculus), however, is shown for comparison in Figure 3.
SEM-EDX
Figure 2. Images of the samples. Bar=10mm. a: The sampling of the ancient human dental calculus from a grave in Znojmo- Hradiště No. 464 in the Czech Republic. b: Green-coloured teeth of the man No. 53 from Devín-Za kostolom in the Slovak Republic. c: Man No. 801 from the site Majetín in the Czech Republic. Incisors of his lower jaw showed traces of a trauma with a military origin.
Figure 3. The usual energy-dispersive X-ray spectrum of the ancient human dental calculus.
upper left first molar. The size of the sample was 2.5 ×1.5mm and it had light green brown color outside and light brown color inside. When the SEM was used, there were
seen crystals, bacteria (Figs. 1b, 1c), and vegetable/plant fibers. Sex and age were estimated by anthropological methods (Lovejoy et al., 1985; Bruzek, 2002). The individual was a 30–39-year-old man with no goods in the grave according to archeological records (Harmadyová, 2009). The third sample came from a 30–50-year-old man
(No. 801) from the Majetín site in the Czech Republic. The sample was taken from the buccal side of the lower right first incisor. The size of the sample was 3×2mmand it had dark brown color outside (Fig. 2c) and light brown color inside. When the SEM was used, there were seen crystals and bacteria (Fig. 1d). Sex and age were estimated by anthropo- logical methods (Lovejoy et al., 1985; Bruzek, 2002). All the
For the SEM-EDX analysis a Magellan 400 SEM (FEI) equipped with an ED APOLLO X Silicon Drift Detector (EDAX) was used. All measurements were taken at an acceleration voltage of 30 kV. The calculus samples were mounted on stubs by using double-sided carbon tape. Only one sample (from Devín-Za kostolom) was investigated both using the coating method and then also without any surface modification, in order to evaluate the pros and cons of coating and to decide which method would be better to use. This sample was at first examined without the use of surface modifications, and a 5nm chromium layer (Quorum Q150T) was sputter-coated afterwards. However, the elemental spectra were comparable with each other, so we decided to choose the less destructive method, and all samples were generally investigated without the use of surface modifications. At least five measurements were per- formed on each sample, together with measurements of the inside and the outside of calculus to eliminate burial ground contamination (to determinate for which elements from the burial environment are the calculus permeable). To evaluate our results (by the nondestructive method) we performed EDX mapping on a sample from Majetín, embedded in epoxy resin. A sample of dental calculus was embedded in epoxy block using EpoFix kit (Struers). For the vacuum impregnation (needed due to the porosity of sam- ples), an improvised apparatus was made. After that, the
epoxy blocks were carefully ground and polished down to the final stage using 1 µm diamond suspension in Struers Tegramin. The sample was at first analyzed by low-energy electron microscopy (LEEM), then it was sputter coated with a 5nm chromium layer (Quorum Q150T) for the EDX mapping.
RESULTS AND DISCUSSION
The first sample of calculus from the left second lower incisor came from a man with high degree of dental abrasion, which was probably caused by particles of grinding stones in flour. This hypothesis was verified by comparison of the elemental
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