Method for Qualitative and Quantitative Analysis of Ancient Lead Enamel Using Laser Inducted Breakdown Spectroscopy
Лазерлік ұшқын эмиссиялық спектроскопия көмегімен құрамында қорғасыны бар археологиялық қорғасын эмалын сапалық және сандық талдау әдісі
Метод качественного и количественного анализа свинцовой археологической эмали с использованием лазерной искровой эмиссионной спектроскопии
Fomin V.N. Gyul E.F. Usmanova E.R. Kelesbek N.K. Turovets M.A. Zemskij O.I. Saulebekov D.M. Aldabergenova S.K.
2022E.A.Buketov Karaganda State University Publish House
Bulletin of the Karaganda University Chemistry Series
2022#108Issue 4107 - 117 pp.
The method of laser induced breakdown spectroscopy (LIBS) was used in analysis of the archaeological enamel samples from the ancient settlement of Jochi Khan (XIV century). During the qualitative analysis, it was found that the elements of the enamel matrix are Si, Pb, K, Na, Mg, Ca, Al. The glaze color is due to the presence of copper and iron. Clustering by the k-means method revealed two groups of samples similar in composition of enamel, but differing in place of origin within the settlement. For the studied samples the semi-quantitative composition of glazes was established from the spectra of LIBS using a method based on the hypothesis of local thermodynamic equilibrium (LTE) and a chemometric approach (Projection to Latent Structures, PLS). Probabilistic deterministic design of experiment was used to search for pairs of element lines that are not subject to changes when the conditions for spectra registration vary, and to determine the coefficients in the equations based on LTR. Calculations using the PLC method were carried out in the “R” programming environment. The following content of the matrix elements was obtained in terms of the most stable oxides, %: SiO2 — 49–61, PbO — 23–31, MgO — 1.7–2.3, CaO — 4.6–6.9, Na2O — 4.1–5.3, K2O — 5.1–6.4, Al2O3 — 0.8–1.7, CuO — 0.32–0.4, Fe2O3 — 0.09–0.16. The results of both methods are generally consistent with each other. The inaccuracy between 4 parallel determinations were 15-24 % for LTE, and 9–14 % for PLS. Taking into account the data of semi-quantitative analysis, it was concluded that the division into two groups is based on a different ratio of copper and iron in enamel.
archeology , chemometrics , cluster analysis , LIBS , low-melting lead enamels , PLS , probabilistic deterministic design of experiment , settlement of Jochi Khan
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Karagandy University of the Name of Academician E.A. Buketov, Universitetskaya Street, 28, Karaganda, 100024, Kazakhstan
Institute of Art History of the Academy of Sciences of the Republic of Uzbekistan, Mustakillik, 2, Tashkent, Uzbekistan
South Ural State University, Lenina, Chelyabinsk, 76, Russian Federation
Department of Inorganic and Technical Chemistry, Karagandy University of the Name of Academician E.A. Buketov, Universitetskaya Street, 28, Karaganda, 100024, Kazakhstan
Department of Physical and Analytical Chemistry, Karagandy University of the Name of Academician E.A. Buketov, Universitetskaya Street, 28, Karaganda, 100024, Kazakhstan
Karagandy University of the Name of Academician E.A. Buketov
Institute of Art History of the Academy of Sciences of the Republic of Uzbekistan
South Ural State University
Department of Inorganic and Technical Chemistry
Department of Physical and Analytical Chemistry
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