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A Study on Chinese Ancient Jades with Mercury Alteration Unearthed from Lizhou’Ao Tomb Yi Bao1,2, Changqing Xu4, Qinwen Zhu3* & Yuesheng Li1*

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A Study on Chinese Ancient Jades with Mercury Alteration Unearthed from Lizhou’Ao Tomb Yi Bao1,2, Changqing Xu4, Qinwen Zhu3* & Yuesheng Li1* www.nature.com/scientificreports OPEN A study on Chinese ancient jades with mercury alteration unearthed from Lizhou’ao Tomb Yi Bao1,2, Changqing Xu4, Qinwen Zhu3* & Yuesheng Li1* “Alteration” geologically refers to chemical composition and/or structural changes of minerals under the infuences of hydrothermal fuids, surface water, seawater, or other environmental conditions. In this paper, we use the word “alteration” to refer to chemical component and structural changes in jade artifacts caused by human activity and natural weathering, which is diferent from the term in geology. “Mercury alteration”, a kind of black alteration related to Hg, is unique among the several types of alteration that occur in Chinese ancient jades. Mercury alteration often appears on ancient jade artifacts unearthed from high-grade tombs of the pre-Qin period (before 221 B.C.). Therefore, ancient jades with mercury alteration have attracted substantial attention from Chinese archaeologists. This paper reports the use of materials analytic techniques to study such ancient jade fragments. The studied jade samples date to the middle and late periods of the Spring and Autumn Period (~500 B.C.) and were unearthed from Lizhou’ao Tomb in Jiangxi Province, China. Structural analyses revealed the internal microstructure of the ancient jade fragments and the microdistribution of the mercury alteration. The jade fragments exhibit typical characteristics of round holes and structural hierarchy, which imply that the jades were heated before burial. The black alteration on these jade samples was found to be rich in Hg. The results of this study will be widely useful in the study of ancient jade artifacts and jade culture in Chinese archeology. As one of the most characteristic artifacts in China, ancient jade is a signifcant representative of traditional Chinese culture. Chinese jade culture has lasted more than 8000 years without interruption1. Jade not only served as a decoration in ancient Chinese life but also symbolized status and power in Chinese culture. An important typical characteristic of ancient jade artifacts from archaeological excavation is also called “alteration”2–4. Te term “alteration” here is referred to chemical component and structural changes in jade artifacts caused by human activity and natural weathering, which is diferent from the term in geology as described above5. Te alteration of ancient jades has been categorized according to 7 colors: black, white, yellow, red, blue, green and purple. Each color is produced by diferent mechanism6. A particular type of black alteration is “mercury alteration”, which is related to Hg7. Mercury alteration is typically found on ancient jades unearthed from tombs of high-class nobles. Terefore, the study of ancient jades with mercury alteration is important for Chinese archeology. Mercury alteration is recorded in ancient Chinese texts. Xu8, Chen9 and Liu10 considered that a kind of black alteration on unearthed jades was related to mercury. Tis kind of black alteration was termed “Shuiyin qin” or “Heiqigu”. Te word “Shuiyin qin” was frst used to refer to a kind of copper mirror with a white surface dating from the Eastern Han Dynasty (25 A.D.–220 A.D.), and the word “Heiqigu” was frst used in connection with a kind of copper mirror with a black surface dating from the Tang Dynasty (618 A.D.–907 A.D.)7. “Shuiyin qin” and “Heiqigu” can mean diferent things when used to refer to diferent materials (Table 1). In terms of color, “Shuiyin qin” and “Heiqigu” in jade artifacts are both black. “Shuiyin qin” on a copper mirror is white, while “Heiqigu” on a copper mirror is black. In terms of material, “Shuiyin qin” and “Heiqigu” in jades both refer to alteration relative to mercury, while “Shuiyin qin” and “Heiqigu” on copper mirrors both relate to tin. In terms of the shape of the black alteration, according to custom, “Shuiyin qin” refers to black alteration in the shape of lines or small spots, while “Heiqigu” refers to black alteration that covers all or half of a jade artifact7. 1Department of Materials Science, Fudan University, Shanghai, 200433, P.R. China. 2Institute of Archaeological Science, Fudan University, Shanghai, 200433, P.R. China. 3China University of Geosciences (Wuhan), Wuhan, 430074, P.R. China. 4Jiangxi Provincial Institute of Cultural Relics and Archaeology, Nanchang, 330008, P.R. China. *email: [email protected]; [email protected] SCIENTIFIC REPORTS | (2019) 9:19849 | https://doi.org/10.1038/s41598-019-55138-2 1 www.nature.com/scientificreports/ www.nature.com/scientificreports Name Object Color Factor Shape Start using time Ancient jades Black Hg Line or spot Shuiyin Qin Ancient copper Eastern Han White Sn On surface mirror Dynasty Ancient jades Black Hg Part or whole Heiqigu Ancient copper black Sn On surface Tang Dynasty mirror Table 1. Proper names of mercury alteration in Chinese ancient literatures. Tomb Fuhao Yejiashan Yuhe Lizhou’ao Jiuli Yangjiashan Shang Dynasty Western Zhou Spring and Autumn Spring and Autumn Warring States Warring States Time (1600 B.C.–1046 Dynasty (1046 Period (770 Period (770 Period (475 Period (475 B.C.) B.C.–771 B.C.) B.C.–476 B.C.) B.C.–476 B.C.) B.C.–221 B.C.) B.C.–221 B.C.) Hunan Province Henan Province Hubei Province Henan Province Jiangxi Province Hunan Province Province Middle of the Middle of the Middle of the Middle of the Middle of the Middle of the Location Yellow River Yangtze River Yellow River Yangtze River Yangtze River Yangtze River Status of Queen Vassal King Vassal King Noble Vassal King Noble Owner Tomb Grade High High High High/Middle High Low References In press Luo et al. 2018 Xu and Wang12 Tis paper Zhao et al.13 Zhao et al.13 Table 2. Te unearthed ancient jade artifacts identifed with mercury alteration. Ancient jade artifacts with mercury alteration from 5 tombs of the pre-Qin period (before 221 B.C.) have been examined using X-ray fuorescence (XRF): Fuhao Tomb (in press), Yejiashan Tomb, Yuehe Tomb11,12, Jiuli Tomb12 and Yangjiashan Tomb7,13 (Table 2). Te ancient jades with mercury alteration unearthed from these tombs have some common characteristics. In terms of time period, most date to the period between the Shang Dynasty and the Warring States Period (1600 B.C.–221 B.C.). Tis period was important to the formation of the Chinese nation. Geographically, such jade artifacts are mainly distributed along the middle reaches of the Yangtze River and the middle reaches of the Yellow River, which together represent the core area of the Chinese nation during that period. According to the tomb degree system used in archeology, these jades were mainly unearthed from high-grade tombs, particularly tombs from the Shang Dynasty and the Western Zhou Dynasty. Te research sam- ples described in this study are ancient jade artifacts with mercury alteration unearthed from Lizhou’ao Tomb. Te results of this paper indicate a widening of the distribution of ancient jades with mercury alteration to Jiangxi Province and a richer variety of samples than previously assumed (Table 2). Owing to the age and degree of these tombs, the study of the ancient jade artifacts with mercury alteration found in them has attracted considerable archaeological research attention. A small number of ancient jades with mercury alteration were previously examined by XRF12–14. Te results agreed with the fndings of ancient Chinese texts. Xu8, Chen9 and Liu10 considered that a kind of black alteration appearing on unearthed jades was related to mercury and referred to it as “Shuiyin qin” and “Heiqigu” in Chinese. Wen studied Chinese ancient jade materials using a geological method systematically combined with the fndings of the ancient Chinese literature15–17. Gaines conducted the frst study on mineralogical alteration in Chinese ancient jades using X-ray difraction (XRD) and scanning electron microscopy (SEM)18. Douglas and Wen proposed that certain Chinese ancient jades might have been heated during processing and during cremation in the historical period mainly using XRD and Fourier transform infrared spectroscopy (FTIR)19. Preliminary heating experiments by Bao using several advanced characterization methods, including XRD, a thermogravimetric analyzer (TGA), an ultraviolet-visible spec- trophotometer (UV-Vis), FTIR and SEM equipped with energy-dispersive spectroscopy (SEM-EDS), revealed appearance changes in nephrite jade that occurred during the heating process20. Te ancient jade fragment samples studied in this paper were unearthed from Lizhou’ao Tomb and date to the middle and late period of the Spring and Autumn Period (~500 B.C.). Lizhou’ao Tomb was excavated in Jing’an, Jiangxi Province, in 2007. Tis tomb is famous for its extraordinary structure, which is a single-pit multicofn grave (Fig. 1A). Tis grave is widely known as the earliest tomb found in China and the one with the greatest number of cofns21,22. Jiangxi Province was the transition zone of the Han nation and the Yue nation during the middle and late period of the Spring and Autumn Period. Certain researchers believe that Lizhou’ao Tomb refects the fusion of the two nations23. Tis special tomb refects both the diversity and the unity of Chinese culture. A total of 11 pieces of ancient jade have been unearthed from the tomb, 9 of which belong to G21 (Fig. 1B). Materials and Methods Description of ancient jade samples. Ancient jade fragments unearthed from G21 of Lizhou’ao Tomb were studied in this paper (Fig. 1B). Te jade samples were provided by Jiangxi Provincial Institute of Cultural Relics and Archaeology24. All 9 pieces of ancient jade unearthed from G21 have similar characteristics. G21:2-1 and G21:2-2, which exhibit the best phenomenological features, were chosen as representative study samples. Details of the two samples are listed in a table that presents the ancient jade analysis system (Table 3).
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