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Elemental Characterization by Edxrf of Imperial Longquan Celadon Porcelain Excavated from Fengdongyan Kiln, Dayao County*

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Elemental Characterization by Edxrf of Imperial Longquan Celadon Porcelain Excavated from Fengdongyan Kiln, Dayao County* bs_bs_banner Archaeometry 57, 6 (2015) 966–976 doi: 10.1111/arcm.12149 ELEMENTAL CHARACTERIZATION BY EDXRF OF IMPERIAL LONGQUAN CELADON PORCELAIN EXCAVATED FROM FENGDONGYAN KILN, DAYAO COUNTY* L. LI,1 L. T. YAN,1 S. L. FENG,1 Q. XU,1 L. LIU,1,2 Y. HUANG1,2 and X. Q. FENG1† 1Key Laboratory of Nuclear Radiation and Nuclear Energy Technology, Institute of High Energy Physics, Chinese Academy of Sciences, 19 Yu Quan Lu, Beijing 100049, China 2University of Chinese Academy of Sciences, Chinese Academy of Sciences, Beijing 100049, China A mass of Longquan porcelain shards carved with ‘Guan’ or the dragon patterns were unearthed in the early Ming Dynasty layer of the Fengdongyan kiln site at Dayao County. These celadon shards were fired in the Hongwu and Yongle eras of the Ming Dynasty. In order to research the raw materials and firing technology of the imperial porcelain, 85 typical shards were analysed by energy-dispersive X-ray fluorescence (EDXRF). The results indicate that the contents of TiO2 and Fe2O3 in the body vary in the Hongwu and Yongle eras. Compared with Longquan glazes in the Southern Song Dynasty, the average values of K2O, Fe2O3 and TiO2 are higher, but that of CaO is lower in early Ming imperial porcelain glazes. Principal compo- nents analysis (PCA) shows that different degrees of elutriation of the same raw materials are the main reason for this difference in the Hongwu and Yongle periods. However, the raw materials of imperial porcelain glazes show no obvious changes and have inherited the earlier tradition. The production and firing technology of imperial porcelain reached a higher level and had not declined in the Early Ming Dynasty. KEYWORDS: EDXRF, LONGQUAN KILN, IMPERIAL PORCELAIN, FENGDONGYAN KILN, PCA INTRODUCTION Longquan celadons, with higher firing technology and greater artistic merit, play a significant role in the history of ancient Chinese celadon. According to previous archaeological evidence (Li 1998), it is well known that the Longquan kilns, located in Longquan City in Zhejiang Province, began to fire celadon in the Southern and Northern Dynasties (ad 420–589), and developed in the Southern Song (ad 1127–1279) and Yuan Dynasties (ad 1271–1368). It used to be thought that the firing technology had declined in the Ming Dynasty (ad 1368–1644), as stated in several references (Chou et al. 1973; The Light Industry Hall of Zhejiang Province 1989; Li 1998). But did the firing technology of Longquan celadon really begin to decline in the Ming Dynasty? Were the Longquan kilns still the famous kilns that made porcelain for the palace? In the past, research interest was focused on the development history and the decorative arts of the civilian porcelain of Longquan celadon (Li et al. 1984; Ye et al. 1999; Jin 2007). Due to the lack of specimens, the raw materials and firing technology of the imperial porcelain of Longquan celadon has been little investigated. But the excavation of the Fengdongyan kiln provides physical evidence. From September 2006 to January 2007, the Fengdongyan kiln, located in *Received 8 January 2014; accepted 8 September 2014 †Corresponding author: email [email protected] © 2014 University of Oxford Characterization by EDXRF of imperial Longquan celadon porcelain 967 Figure 1 The location map for the Dayao County kiln, amongst the Longquan kilns. Dayao County, in Longquan City (see Fig. 1), was excavated by the Zhejiang Province Institute of Cultural Relics and Archaeology, the School of Archaeology and Museology of Peking University and the Longquan Museum. A mass of exquisite Longquan celadon shards of theYuan and Ming Dynasties were unearthed, including abundant civilian porcelain and a lot of official wares carved with ‘Guan’ or the dragon patterns in the Hongwu and Yongle eras of the Ming Dynasty (Zhejiang Institute of Cultural Relics et al. 2009). The emergence of this imperial porcelain has led to great repercussions in archaeology. Some scholars have published compari- sons between the imperial porcelain of the Ming Dynasty and the Longquan porcelain of the Southern Song Dynasty (Peng et al. 2009). However, what differences are there between the imperial porcelain of the Ming Dynasty and the civilian porcelain of the Early Ming Dynasty? At present, there is little research comparing imperial porcelain with civilian porcelain in the Ming Dynasty. In this paper, we have determined the chemical composition of imperial Longquan celadon porcelain using energy-dispersive X-ray fluorescence (EDXRF). It is well known that the con- tents of major, minor and trace elements of the porcelain body and glaze are dependent on its raw material and manufacturing technology (Li 1998; Kerr and Wood 2004; Artioli 2010), which can be used to indicate the age of the porcelain and its provenance. From a statistical analysis of the elemental data, the raw material and the development of porcelain firing technology are dis- cussed. The information is used to display the inheritance relationship of the raw materials used for the body and glaze in different periods. © 2014 University of Oxford, Archaeometry 57, 6 (2015) 966–976 968 L. Li et al. Figure 2 Photographs of imperial porcelain samples from the HWM and YLM periods. Table 1 Detailed information on the celadon shards from the Fengdongyan kiln site Group Date Number of shards Exterior characteristics HWM Hongwu era of the Ming Dynasty 32 Celadon glaze, grey body YLM Yongle era of the Ming Dynasty 53 Celadon glaze, grey body EM Early Ming Dynasty 48 Celadon glaze, grey body SAMPLES In this work, 85 typical shards of imperial porcelain from the Fengdongyan kiln were provided by Zhejiang Province Institute of Cultural Relics and Archaeology. These imperial porcelain samples can be grouped into two cultural periods: the Hongwu (HWM group) and the Yongle (YLM group) eras of the Ming Dynasty. Since Hongwu and Yongle are Early Ming, 48 shards of civilian porcelain excavated at Fengdongyan dated to the Early Ming Dynasty (EM group) were selected for comparison with the imperial porcelain. Some photographs of imperial por- celain shards are shown in Figure 2 and detailed information about the samples is listed in Table 1. THE EDXRF EXPERIMENT A sample measuring 30 mm × 10 mm was cut from the shard, and the cross-section was polished, and then washed three times in an ultrasonic cleaner with deionized water and dried at 105°C. The EDXRF experiments were performed on an EDAX Eagle III spectrometer at the Institute of High Energy Physics, CAS, Beijing, China. The spectrometer has a Mo tube and a 125 μmBe window with an incident beam angle of 65° and an emergence angle of 60°. The detector is a liquid-nitrogen-cooled Si(Li) crystal with a resolution of 160.3 eV at Mn–Kα. There is a vacuum chamber and the diameter of the X-ray beam spot is selected to be 1 mm. The voltage and current of the X-ray tube are 40 kV and 250 μA, respectively. The software employed for spectrum deconvolution and analysis is VISION32, which is associated with the instrument. A set of standard reference samples with known chemical compositions, which were developed by the © 2014 University of Oxford, Archaeometry 57, 6 (2015) 966–976 Characterization by EDXRF of imperial Longquan celadon porcelain 969 Table 2 The quantitative results for the ancient ceramic samples Na2O MgO Al2O3 SiO2 K2O CaO TiO2 MnO Fe2O3 Cu Zn Rb Sr (%) (%) (%) (%) (%) (%) (%) (%) (%) (ppm) (ppm) (ppm) (ppm) Experimental 0.65 0.62 24.34 67.54 2.27 0.54 0.88 0.022 2.77 46 54 119 109 value Certified 0.44 0.70 23.90 67.50 2.30 0.62 0.95 0.026 2.70 27 59 113 103 value Institute of High Energy Physics, are used to calibrate the ceramic matrix in order to obtain reliable experimental data. The homogeneity of elements in these ceramic reference samples met the requirements for non-destructive quantitative analysis (Li et al. 2010). The elemental abundances of Na2O, MgO, Al2O3, SiO2,K2O, CaO, TiO2, MnO, Fe2O3, CuO, ZnO, Rb2O and SrO are quantified by the fundamental parameter (FP) method (He and Espen 1991; Sitko 2008). This method assumes that the unknown samples have approximate compo- sitions, and then calculates the fluorescence intensities based on the Sherman equation (Sherman 1955) and compared to the measured intensities (Lachance and Claisse 1994). Successive adjustments of the composition are carried out until the theoretical and measured intensities are consistent. The final concentrations are assumed to represent the actual compositions. In order to get a better measure of the precision and accuracy of the data in this work, ancient ceramic samples of known composition are selected to compare the expected and observed elemental concentrations measured on the ceramic reference samples used in the analysis. The results show that the experimental values are well in agreement with the certified ones (see Table 2). The average values of each elemental composition in the porcelain body and glaze are displayed below, in Tables 3 and 5, respectively. In this paper, the data for Na2O and MgO are provided as references because of the poor fluorescent yields and low counts obtained for the characteristic X-ray radiation. DISCUSSION The elemental characteristics of imperial porcelain with a Longquan celadon body There are no evident differences between the average concentrations of SiO2,Al2O3 and MnO in the imperial porcelain body for the HWM and YLM groups, as shown in Table 3. It can be seen that the K2O contents in the Hongwu era of the Ming Dynasty are a little higher than those of the Yongle era of the Ming Dynasty, while the CaO contents are lower, as can be seen in Figure 3. ± ± The average TiO2 content in the HWM group is 0.21 0.03 % higher than that (0.14 0.02 %) in the YLM group.
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