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Integrating X-ray fluorescence and X-ray computed tomography for comprehensive analysis of historical ceramics from the Kraków Upland Cover

Integrating X-ray fluorescence and X-ray computed tomography for comprehensive analysis of historical ceramics from the Kraków Upland

Open Access
|Oct 2025

Figures & Tables

Fig. 1.

Location of sampling sites. 1 – Grodzisko near Skała, 2 – Jerzmanowice, 3 – Ojców, a – source clay deposits.

Table 1.

The comparison of determined and known (reference) concentrations of chemical compounds in reference samples

CompoundReference AReference C
Concentration (wt%)Concentration (wt%)
ReferenceDetermined ± St.Dev.ReferenceDetermined ± St.Dev.
Na2O1.621.740 ± 0.0131.882.440 ± 0.080
MgO0.270.150 ± 0.0400.30.337 ± 0.040
Al2O334.1635.43 ± 0.3224.827.47 ± 0.27
SiO259.9755.20 ± 0.3369.5763.66 ± 0.38
K2O3.334.41 ± 0.132.934.119 ± 0.055
CaO0.530.52 ± 0.110.520.535 ± 0.012
Fe2O3nd1.35 ± 0.410.30.3800 ± 0.0023
BaO0.120.130 ± 0.021nd0.157 ± 0.012
CompoundReference DReference G
Concentration (wt%)Concentration (wt%)
ReferenceDetermined ± St.Dev.ReferenceDetermined ± St.Dev.
Na2O1.91.77 ± 0.280.310.85 ± 0.43
MgO0.150.013 ± 0.0030.430.20 ± 0.14
Al2O322.0129 ± 340.9351 ± 14
SiO273.2363 ± 353.3344 ± 13
K2Ond3.23 ± 0.281.102.23 ± 0.43
CaOnd0.210 ± 0.0620.730.268 ± 0.021
TiO20.440.78 ± 0.521.090.55 ± 0.11
Fe2O30.771.02 ± 0.162.080.931 ± 0.085

[i] nd – no data; St.Dev. – standard deviation.

Fig. 2.

The analyzed pottery fragments. (a) Photographic image of the fragment; refer to GRO_275, refer to JER_135, refer to OJC_273, refer to OJC_965, refer to OJC_9668. (b) Frontal cross-section of the tomographic reconstruction of the sample. (c) Longitudinal cross-section of the tomographic reconstruction of the sample.

Table 2.

Elemental composition of the matrix of the ceramic body of the analyzed pottery samples and clay deposits in the Kraków Upland (in wt%, μg/g, and standard deviation) determined by XRF technique

ElementsClay depositsGRO_275JER_135OJC_273OJC_965OJC_9668
Determined concentration ± St.Dev. (%)
Na0.055 ± 0.0079<LOD0.15 ± 0.211.19 ± 0.910.198 ± 0.0730.36 ± 0.13
Mg0.320 ± 0.0720.17 ± 0.210.76 ± 0.0740.59 ± 0.251.08 ± 0.380.84 ± 0.19
Al3.9 ± 2.03.0 ± 2.211.6 ± 3.36.1 ± 2.63.9 ± 3.78.50 ± 0.98
Si11.8 ± 5.242.3 ± 3.231.2 ± 1.928.7 ± 2.928 ± 1831.2 ± 2.2
P0.039 ± 0.0240.106 ± 0.0120.091 ± 0.0990.25 ± 0.192.8 ± 2.70.18 ± 0.035
S0.016 ± 0.00790.030 ± 0.0120.097 ± 0.0340.56 ± 0.180.12 ± 0.0720.063 ± 0.015
K1.03 ± 0.250.88 ± 0.621.93 ± 0.483.2 ± 0.172.3 ± 2.23.3 ± 1.5
Ca1.42 ± 0.320.35 ± 0.311.04 ± 0.358 ± 814 ± 61.78 ± 0.32
Ti0.180 ± 0.0870.087 ± 0.0850.69 ± 0.320.57 ± 0.120.25 ± 0.230.78 ± 0.59
Fe2.23 ± 0.390.94 ± 0.783.05 ± 0.914.6 ± 1.42.5 ± 2.14.64 ± 0.59
Determined concentration ± St.Dev. (μg/g)
V39 ± 12210 ± 150236 ± 46140 ± 13035 ± 31121 ± 67
Cr48 ± 1194 ± 110148 ± 18100 ± 2662 ± 17180 ± 94
Mn180 ± 19560 ± 150360 ± 3001600 ± 3801610 ± 700820 ± 150
Ni23 ± 6208 ± 5433 ± 1351 ± 3565 ± 5668 ± 5
Cu15 ± 422 ± 955 ± 19369 ± 1858 ± 1547 ± 34
Zn82 ± 64<LOD318 ± 60229 ± 34330 ± 24 030256 ± 22
Ga12 ± 4<LOD33 ± 16147 ± 6739 ± 2934 ± 8
As17 ± 5120 ± 110<LOD<LOD115 ± 1935 ± 13
Rb64 ± 1073 ± 32126 ± 40184 ± 58143 ± 18165 ± 15
Sr42 ± 890 ± 2087 ± 49160 ± 21390 ± 120143 ± 15
Y34 ± 734 ± 4416 ± 7167 ± 7111 ± 634 ± 10
Zr84 ± 45270 ± 120235 ± 79269 ± 68104 ± 12411 ± 340
Nb22 ± 539 ± 563 ± 745 ± 1542 ± 1694 ± 40
Ba187 ± 32<LOD650 ± 480840 ± 3501580 ± 2001130 ± 530

[i] St.D. – standard deviation

Table 3.

The correlation data of the ceramic sample according to the data from XRF analysis

Na2OMgOAl2O3SiO2P2O5SO3K2OCaOTiO2Fe2O3VCr2O3MnONiOCuZnOGaAsRbSrOY2O3ZrNbBaOPb
Na2O1
MgO−0.031
Al2O300.321
SiO2−0.45−0.87−0.381
P2O5−0.20.67−0.45−0.451
SO30.97−0.04−0.04−0.46−0.121
K2O0.670.560.36−0.770.010.541
CaO0.260.63−0.43−0.650.90.350.281
TiO20.330.410.88−0.56−0.420.220.75−0.281
Fe2O30.690.440.53−0.71−0.220.560.970.080.871
V0.18−0.720.360.44−0.840.24−0.31−0.710.15−0.081
Cr2O3−0.060.060.79−0.03−0.66−0.230.4−0.70.830.550.271
MnO0.620.43−0.48−0.620.630.650.510.9−0.160.33−0.57−0.591
NiO−0.39−0.78−0.680.94−0.18−0.39−0.73−0.35−0.76−0.750.17−0.3−0.311
Cu0.98−0.08−0.04−0.43−0.1610.550.310.230.570.26−0.20.63−0.371
ZnO0.120.940.57−0.930.450.150.60.50.60.56−0.420.170.33−0.950.111
Ga0.980.110.06−0.59−0.070.990.660.390.340.680.14−0.150.68−0.520.990.291
As−0.58−0.15−0.820.490.56−0.54−0.610.28−0.88−0.79−0.49−0.610.10.72−0.55−0.45−0.61
Rb0.750.590.32−0.870.110.670.980.430.680.94−0.290.230.63−0.80.670.670.79−0.631
SrO−0.030.71−0.44−0.560.980.040.20.95−0.32−0.04−0.88−0.620.76−0.26−0.010.490.10.460.291
Y2O30.98−0.21−0.07−0.3−0.290.970.540.170.230.580.31−0.110.55−0.250.99−0.040.95−0.530.62−0.131
Zr0.18−0.320.360.25−0.78−0.040.38−0.720.560.490.30.83−0.420.090.03−0.280.01−0.420.19−0.680.191
Nb−0.210.660.52−0.440.08−0.380.59−0.060.670.55−0.510.69−0.12−0.48−0.370.57−0.22−0.230.430.14−0.360.441
BaO0.140.960.09−0.870.730.110.650.760.30.49−0.83−0.080.65−0.690.090.830.25−0.050.690.82−0.03−0.30.61
Pb−0.290.120.8−0.11−0.28−0.2−0.22−0.380.42−0.030.520.37−0.6−0.42−0.220.39−0.18−0.51−0.17−0.4−0.3−0.120.06−0.181
Fig. 3.

(a) SiO2-Al2O3-CaO and (b) SiO2-Al2O3-Na2O+K2O ternary plots showing the matrix composition of the ceramic body of the analyzed sample measured by XRF technique.

Fig. 4.

Segmented image emphasizing the inclusions of sample GRO_275 (in mm).

Fig. 5.

Segmented image emphasizing the inclusions of sample JER_135 (in mm).

Fig. 6.

Segmented image emphasizing the inclusions of sample OJC_965 (in mm).

Fig. 7.

Segmented image emphasizing the inclusions of sample OJC_9668 (in mm).

Fig. 8.

Segmented image emphasizing the voids of sample GRO_275 (in mm).

Fig. 9.

Segmented image emphasizing the voids of sample JER_135 (in mm).

Fig. 10.

Segmented image emphasizing the voids of sample OJC_965 (in mm).

Fig. 11.

Segmented image emphasizing the voids of sample OJC_9668 (in mm).

Fig. 12.

Segmented image emphasizing the voids of sample OJC_273 (in mm).

DOI: https://doi.org/10.2478/nuka-2025-0010 | Journal eISSN: 1508-5791 (formerly 0029-5922) | Journal ISSN: 0029-5922
Language: English
Page range: 97 - 109
Submitted on: Apr 14, 2025
Accepted on: Jun 16, 2025
Published on: Oct 21, 2025
Published by: Institute of Nuclear Chemistry and Technology
In partnership with: Paradigm Publishing Services
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© 2025 Romisaa Abdelrahman, Sebastian Wroński, Michał Wojenka, Jacek Tarasiuk, Lucyna Samek, published by Institute of Nuclear Chemistry and Technology
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.