Assessment of manufacturing processes and materials characterization on a collection of ancient Chinese Jades

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A non-invasive multi-analytic protocol (p-XRF/PCA, FTIR and µ-Raman spectroscopies, µ-X-ray diffraction) was applied to characterize materials and conservation. Eight artefacts are made of nephrite – consistently with the archaic Chinese jades composition, though insufficient to assess legitimacy. The recurrence of revealing manufacturing marks/iconographies allowed supporting these items genuineness. Six artefacts revealed different lithologies, sometimes with hardness/tenacity significantly lower than jades. For some, distinctive technological marks suggest that the choice of atypical materials was either dictated by specific necessities or consequent to the artefacts use or interment; in few cases, doubts arose about legitimacy. This study provides an archaeometric perspective for evaluating material inconsistencies between museum artefacts and archaeological specimens. Chinese jade Han dynasty non-destructive protocol nephrite legitimacy Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 Introduction The beauty and preciousness of ancient Chinese jades are renowned worldwide. Jade manufacturing in China dates back to 6000/5000 BC [ 1 , 2 ]. However, the word ‘jade’ has more recent European roots, from the Portuguese ‘ pedra de ijada ’(“kidney stone”), due to its supposed healing powers. In ancient China, jade was known as玉 ( yù in mandarin), meaning ‘gem’ or ‘treasury’ [ 3 ], referred to the material beauty and preciousness rather than to a particular stone. Under the term ‘jade’, in fact, several kinds of stones were comprised, depending on the specific context of pertinence. Scientifically, ‘jade’ includes two different rock/mineral types: ‘nephrite’ (a Ca-Mg-amphibole of the tremolite/ferro-actinolite series) and ‘jadeite’ (a sodic pyroxene with ideal formula NaAlSi 2 O 6 ) [ 4 ]. However, in the Chinese culture, other lithologies (i.e., rocks made of serpentine, sericite, quartz, talc, calcite) may also be referred to as ‘jades’ [ 5 ]. Most ancient Chinese jades are made of ‘nephrite jade’ [ 1 – 3 , 6 ], probably extracted from the alluvial deposits of the Yurungkash and Karakash rivers, in present-day Kazakhstan, until the 10th century AD. From the 12th century, nephrite was also extracted from the ancient Khotan reign [ 7 ]. Due to their exploitation, these nephrite sources became less used in the last centuries, and new materials (e.g., brucite) were also introduced on the market [ 8 ]. Another jade source was probably located in Siberia, close to the Baikal Lake, from which a dark green variety with graphite inclusions was caved (so-called ‘spinach-jade’ [ 9 , 10 ]). Regarding ‘jadeite jade’, its diffusion in ancient China is still discussed: supposed to circulate since the 10th century BC, it probably did not until the Qing Dynasty (17th century AD). Only recently (∼250 years ago) the import from Northern Myanmar (ex Birman) was legalized, from whence it is regularly caved nowadays [ 6 , 11 ]. Despite being known as “soft jade” ( 軟玉 : ruǎnyù , softer than ‘jadeite jade’), nephrite (∼6.5 on the Mohs scale) is a hard and silky rock; it is extremely difficult to work, causing the ancient Chinese artefacts to be extremely precious and expensive. However, recent archaeometric investigations proved that even in Neolithic cultures the use of nephrite must not be considered exclusive, as other "pseudo-jade materials" were used locally [ 12 ]. Research aim This study deals with the archaeometric investigation of a collection of ancient Chinese jades – consisting of 14 artefacts purchased on the legal market by the Fondazione Compagnia di San Paolo and the municipality of Turin (Italy), never exposed to the public before and held in the ‘ Museo d’Arte Orientale ’ (MAO, Museum of Oriental Art) of Turin (Italy). Their dating, based on stylistic basis, ranges from the Neolithic (2nd millennium BC) to the Han dynasty (202 BC − 220 AD). Serious uncertainties about the nature of the lithic materials and production techniques begot doubts about such attributions – questioning the legitimacy of the purchased items. Thus, the need for an in-depth archaeometric study became necessary, in order to characterize their constituent materials, state of conservation and infer information about their manufacturing processes. Materials and methods 2.1. The archaeological finds The studied archaeological record consists of fourteen artefacts (Fig. 1 ). Seven of them belong to a "flat" typology: three rings bì (Cp/7, Cp/8 and Cp/9); two zhang (墇) ritual tablets (a weapon with a fish head shape – Cp/2; an axe head – Cp/1); one ge (戈) axe (Cp/10) and a model of halberd blade jǐ (戟) (Cp/13). The ring bì (璧), marked by with a central hole, is the most classical item in Chinese glyptics, symbolizing the sun and used until the Qing dynasty [ 13 ]. Jade blades and axes were ritual items, not intended as weapons [ 14 , 15 ]. The other seven finds are more 3-dimensional. One represents a cicada (Cp/11), made of different components, probably sealed with an adhesive. Six portray fantastic animals: a feline-head buckle (Cp/19); a composite ornament with phoenix and dragon (Cp/17); a spiral-shaped creature (Cp/18); a feline-shaped plaque (Cp/16) and two dragon-shaped pendants (Cp/14 and Cp/15) [ 16 , 17 ]. Some of them (Cp/14, 15 and 18) show red surface pigmentation. For the ‘nephrite-jade’ manufacturing [ 18 ], rudimental tools – like bamboo canes and archdrills – were used. After the 4th Century BC, corundum and/or diamond could also have been employed [ 19 ] – though some authors suggest earlier use in prehistoric times [ 20 ]. In Neolithic, jade was cut and polished manually by drilling or sawing, using abrasive powders (quartz, SiO 2, or corundum, Al 2 O 3 ) with grease or shellac. Manufacturing occurred in two stages: i) shaping and ii) carving, possibly preceded by heating [ 21 – 23 ]. Techniques were mainly rotary or non-rotary. Among the former, a rudimental drill (wood or bamboo stick) was used, revolved by a rope mounted on a wooden arch, piercing the stone. Later, a disc was applied on the drill tip (‘wheel-cutting’ or ‘rotary-sawing’) to facilitate piercing. Resulting circular holes can be detected on their inner sides, with grooves parallel to their borders. In non-rotary techniques the stone was cut by saws (e.g., metal stick) or hemp/leather ropes with abrasive powders, leaving straight or slightly surface curved marks. Small cutting tools were then used to model the finer details (‘riffing’), possibly leaving linear or concave marks. Diamond could also be used to engrave the stone without abrasive powders (’point abrasion’), leaving irregular marks on the stone surface. Between the 5th and 1st Century BC, the pedal lathe was introduced improving jade manufacturing. Only after 1911, mechanical and electric grinders enables the ‘industrial’ production technology of jade artefacts. This modern manufacture causes jade artefacts to lose their original ‘oily’ aspect, simulated by artificially spreading resin on the surface [ 1 , 24 ]. Nephrite – the main material of ‘archaic Chinese jades’ [ 2 , 3 , 6 ] – is a rock made mostly of an amphibole mineral with double chain of SiO 4 tetrahedrons [T(1) and T(2), Fig. 2 ] elongating along z , with Fe/Mg in three octahedral sites [M(1), M(2) and M(3) in Fig. 2 ] plus minor ions (e.g., Mn 2+ , Al 3+ , Ti 4+ , Cr 3+ , Ni 2+ [ 2 , 22 ]). Ca 2+ mainly occupies the distorted M(4) octahedral site [ 3 , 6 , 25 ]. The variable Fe/Mg ratio defines a solid solution, whose endmembers are tremolite [Ca 2 Mg 5 Si 8 O 22 (OH) 2 ] and actinolite [Ca 2 Fe 5 Si 8 O 22 (OH) 2 ] [ 26 ]. The Fe 2+ content determines nephrite jade’s green hue [ 2 ]. The OH group stretching, shared by three octahedrons, is used to investigate the ‘fine structure’ based on the Fe/Mg ratio, which may help in discriminating tremolite from actinolite and all intermediate compositions [ 27 , 28 ]. 2.2. Experimental methods Substantiating and dating ancient jades are particularly challenging. The custom of collecting ancient jade objects – testified since 1200 BC – causes their technical/stylistic evolution to be quite complicated. Further confusion arises from the Ming dynasty (14th–17th century AD) practice of producing replicas of Han-period artefacts (2nd century BC – 2nd century AD), making authentication even more difficult [ 29 – 31 ]. Archaeometric investigations, including detailed studies of craftsmanship signs and synergic stylistic analyses, can help in pursuing such task [ 1 ]. The beauty and preciousness of this jade’s collection precluded any sampling, requiring the application of a non-invasive multi-analytical protocol. X-ray Fluorescence (XRF) data were acquired with a portable Thermo Niton Mod XL3t-900 GOLDD spectrophotometer (Ag anode, SDD detector, 3 mm spot size, He flow, acquisition time of 120 s, 4 spectra acquired with 4 operating modes: 8 kV, no filter; 20 kV, Cu filter; 40 kV, Al/Fe filter; 50 kV, Mo filter. Data were analysed using Principal Component Analysis (PCA), using a custom-made script [ 32 ], by both considering the average of all spectra for each sample and the individual ones. To increase signal-to-noise, a binning was carried out on the spectra in steps of 60 eV from 1 keV to 3 keV, from 3 keV to 7.25 keV, and from 7.25 to 17.5 keV. For some elements (Mg, Si, Ca and Fe), the peak area was calculated using the Python multichannel analyser [ 33 ] software for deconvolution. Attenuated Total Reflectance Fourier-Transform Infra-Red (ATR-FTIR) spectra were recorded on a Bruker Vertex 70 spectrophotometer, coupled with a Bruker Hyperion 3000 IR microscope and equipped with an (MCT) FPA detector, working in the 4000/900 cm − 1 spectral range. Sixty-four scans were acquired with an average resolution of 4 cm − 1 , operating with an ATR anvil diamond crystal. Raman spectra were collected with a portable BWTEK i-Raman spectrophotometer equipped with a BAC151microscope, exciting the samples with a solid-state 785 nm laser and using a 26–420 30 µm spot, in the 175 to 4200 cm − 1 range, with a 3 cm − 1 spectral resolution. Data were interpreted using the RRUFF™ Project database [ 34 ], implemented by the CrystalSleuth software; spectra were plotted with the Origin software (OriginLab Corporation). X-ray Diffraction (XRD) data were collected in the 3 to 70° 2θ angular range using a SMARTLAB XE Rigaku in micro(µ)-diffraction mode (beam width ∼ 500 µm), equipped with a vertical HyPix-3000 detector in 2D scan mode (10 mm slit, 0,02° step and 3°/min). Data were interpreted using the "DIFFRAC PLUS, EVA Application 7.0.0.1" (2001) software on suitable databases (JCPDS-ICCD; ICSD; PCPDFWIN). Optical microscopy (OM) (20x binocular, 12 mm field depth, 0.6-5.5x magnification) in incident and grazing light was used for investigating the samples surfaces and highlighting possible traces left by manufacturing signs. The protocol of studying moulds of the artefact surfaces [ 1 ] (Sax et al., 2004), obtained by coating them with Si-based resin, with scanning electron microscope (SEM) is unfit here, due to the occasional presence of pigments and/or other materials/byproducts that would risk removal – violating the modern conservation rules [ 35 , 36 ]. A Leica S9-i optical stereomicroscope was thus used directly on the artefacts surfaces, consulting all disposable datasets to identify tool marks. A Dino-Lite Pro digital microscope (AM413ZTA) was also employed, featuring 1.3-megapixel sensor, eight white LEDs, light polarizer, and 10×~50×/220× magnification). Results Based on their chemistry and mineralogy, the artefacts fall into two groups: i) eight are composed of nephrite (Cp/8–10, 14–16, 18, 19); ii) six consist of other rocks/minerals (Table 1 ), including talc, magnesite, serpentine, quartz, calcite and dickite. Calcite and dickite are the sole constituent in Cp/7 and Cp/13, respectively. Some artefacts (Cp/13–18) have engraved decorations, with traces of pigments - red (cinnabar), orange or white (talc). Table 1 Analytical results obtained on the 14 artefacts investigated by applying the non-invasive archaeometric protocol. For XRF, the elements of the main peaks are in bold . Code Artefact typology Vibrational spectroscopies (Raman; FT-IR) XRD (crystalline phases) XRF (chemical elements) Mineral or rock species Pigments Cp/1 zhang axe talc, magnesite talc + magnesite Si , Mg, Al, S, Cl, K,Ca, Cr, Mn, Fe, Ni, Zn talc + magnesite = Cp/2 axe head fish shaped talc, magnesite talc + magnesite, periclase, iron sulfide + iron oxide Si , Mg, Al, S, Cl, K,Ca, Cr, Mn, Fe, Ni talc + magnesite = Cp/7 yuan ring calcite calcite + chlorite + quartz, mica Ca Al, Si, S, Cl, K, Ca, Ti, Mn, Fe, Sr, calcite = Cp/8 bi ring tremolite tremolite + quartz, calcite + feldspar, mica Si, Ca Mg, Al, S, Cl, K, Ti, Mn, Fe, Zn, Y nephrite (tremolite) = Cp/9 bi ring tremolite/actinolite tremolite/actinolite Si, Ca Mg, Al, S, Cl, K, Ti, Mn, Fe, Zn, Sr, Y nephrite = Cp/10 ge axe tremolite/actinolite tremolite/actinolite Si, Ca Mg, Al, S, Cl, K, Ti, Mn, Fe, Sr, Y nephrite = Cp/11 cicada amulet cerussite + gypsum ankerite, cerussite + quartz, cristobalite, aluminium oxide + andalusite, anatase, feldspar Si, Ca, Pb , Al, P, S, Cl K, Mn, Fe, Sr, Zr, Ba lithic core (quartz?, cristobalite?) + external layers (ankerite, cerussite, andalusite, …) = Cp/13 reproduction of a Chinese halberd jǐ . dickite dickite + talc Al, Si P, S, Cl, K, Ca, Ti, Fe, Sr, Y dickite talc (?) Cp/14 dragonshaped pendant cinnabar tremolite + chlorite Si, Ca Mg, Al, P, S, Cl, K, Ti, Mn, Fe, Zn Hg (in all the areas) nephrite cinnabar Cp/15 dragonshaped pendant cinnabar tremolite, quartz + cinnabar + calcite, chlorite, feldspar Si, Ca Mg, Al, P, S, Cl, K, Ti, Mn, Fe, Zn Hg (in all the areas) nephrite cinnabar Cp/16 imaginary feline tremolite tremolite/actinolite + talc Si, Ca Mg, Al, S, Cl, K, Ti, Mn, Fe, Zn, Rb, Sr, Y, Zr nephrite + talc = Cp/17 mobile ornament made of three different parts linked together calcite, lizardite talc, calcite + lizardite/antigorite, quartz, dolomite, ankerite, diaspore, grossular Si, Ca Mg, Al, S, Cl, K, Mn, Zn, Sr,, Ba talc + serpentine minerals + calcite (not in cylinder) = Cp/18 spiral shaped fantastic creature tremolite/actinolite tremolite/actinolite + cinnabar + iron sulfide Si, Ca Mg, Al, S, Cl, K, Ti, Mn, Fe, Zn, Sr, Zr Small Hg (only in some areas) nephrite cinnabar Cp/19 buckle surmounted by a feline head tremolite/actinolite tremolite/actinolite Si, Ca Mg, Al, S, Cl, K, Ti, Mn, Fe, Zn nephrite = 3.1 Artefacts in ‘nephrite-jade’ Cp/8, a quite circular drilled bi ring likely from North-western China, shows smoothed external borders, dotted texture and tiny surface chippings due to polishing (Fig. 3 .a), with both light greenish and blackish areas, suggesting a ‘spinach-jade’ variety. The central hole has sharp borders and a truncated-cone shape, indicating that drilling was made on one side only. µ-XRD and Raman shows amphibole as predominant phase, coupled to minor ones [K-feldspar (in whitish areas), magnesite, talc, quartz and Fe-sulphides (in darker zones)]. Raman bands at 674, 370 and 227 cm -1 , and a single IR maximum in the OH stretching region (3674 cm -1 , peak A [ 6 ]), indicate Mg 2+ abundance and tremolite-rich composition [ 3 , 21 , 37 ]. This is confirmed also by XRF, in which the Mg peak is the highest (Fig. 4 .a) among ‘nephrite-jade’ artefacts, displaying the lowest Fe/Mg peak height ratio (Fig. 4 .b). Regarding craftsmanship traces, OM in grazing/incident light shows benches of parallel tool marks inside the central hole, oriented perpendicular to the edge (Fig. 3 .b), which are not attributable to drilling (whose signs are circular). This suggests that the hole was only sketched by drilling at first (a few parallel striations to the hole border being still barely visible) and then enlarged by string sawing. Finer lapping traces are visible on the larger surfaces, mostly extending linearly between the two edges of the artefact. These likely indicate finishing touches and suggest that the tool may date to the end of the late Neolithic (Shang period, 2nd half of the 1st millennium BC). Cp/9 is another bi ring, possibly a ‘spinach-jade’, more homogeneous than the previous one, translucent and with brilliant green hue – except for diffuse alteration along one edge due to weathering [ 5 , 38 ]. Its circumference and thickness are slightly irregular. The central hole, drilled on one side only, shows a truncated-cone shape and shear angulation. µ-XRD and µ-Raman identify nephrite as the sole constituent. Raman spectra in the OH stretching region (3700 − 3600 cm -1 ) suggest an intermediate tremolite/actinolite composition, with Mg-Mg-Fe or Mg-Fe-Mg occupation in the M1 and M3 sites [ 22 , 27 , 28 ]. OM reveals circular marks within the central hole and fine linear striations on the larger surfaces, partially smoothing the hole edges (Fig. S1 ), possibly from abrasive powders moved by leather. These features support a stylistic dating following metallurgy (Shang period, 2nd half of the 1st millennium BC). Cp/10 is a tabular ge axe typical of mid-Western China, used as a weapon (if tied to a wooden rod) or having ritual purposes. Its simplified shape suggests dating between the 13 th- 8th Century BC (Western Shang-Zhou [ 24 ]). The stone visually resembles Cp/9 – with a vivid green hue (possibly a ‘spinach-jade’) and alteration near the border. Raman, FT-IR and µ-XRD confirm its nephritic nature, with an intermediate tremolite/actinolite composition [ 21 , 22 ]. XRF spectra are similar to Cp/8 and Cp/9, showing lower Al, Cl, K, Ti and higher Mn compared to other artefacts (Fig. 4 .a). PCA (PC2 vs PC1, Fig. 5 ) shows Cp/9 and Cp/10 clustering closely, while Cp/8 appears distinct. OM shows regular, parallel marks perpendicular to the artefact edges, suggesting the use of a toothed implement. Additional fine perpendicular striations (Fig. 3 .c and d) and regular circular marks inside the hole indicate a rotating drill (Fig. 3 .e). Edges are sharp, though occasional surface finishing causes them to become smoothened (Fig. 3 .f). The two main surfaces are smooth, with fine but regular and well-defined lapping marks, likely resulting from a sophisticate finishing – maybe using fine-grained corundum powder as abrasive. If confirmed, this might suggest a later dating, as Al 2 O 3 powders became widespread only from the 13th Century AD. Cp/14 and Cp/15 are nearly identical dragon-shaped pendants, though differing slightly in size and number of pierced holes (one in Cp/14; two in Cp/15), possibly sharing the same manufacture. Their shape and spiral decorations are typical of the ‘Warring States’ period (Eastern Zhou, 5th -3rd century BC). Originally coated by a red pigment, traces nowadays remain mainly in the carved areas. The slightly polished surface may result from post-depositional processes or conservation treatments. Red pigment, dirt and encrustations, hinder detection of manufacturing traces and consequent material identification. Raman detects only cinnabar (HgS, bands at 343, 286 and 254 cm -1 ; [ 39 ]; Fig. 6 .a); µ-XRD identifies tremolite as the main component, with subordinate cinnabar (Fig. 6 .b). XRF confirms Hg and S as major elements (Fig. 4 .a), along with others (Al, P, Cl, K and Ti), in higher amounts if compared to other “nephrite-jade” artefacts (Fig. 4 .a). This might indicate either use of the same raw materials or simply pigment impurities. The Fe/Mg ratio is significantly higher here (and in Cp/18), due to presence of cinnabar biasing this value and preventing information about the tremolite/actinolite content (Fig. 4 .b). As expected, in the PCA score plot Cp/14 and Cp/15 differ from the other samples – again due to high Hg and S contents (Fig. 5 ). OM reveals that the outer edge decoration was delineated first, followed by carving of central spirals, since these sometimes overlap the border (Fig. 3 .g). Circular parallel marks in the holes suggest drilling (Fig. 3 .h); irregular carvings, instead, may result from riffling. Cp/16 is a finely chiseled greenish plaque with dragon/feline motifs pierced from a unique jade block, and altered portions due to possible weathering [ 5 , 38 ]. This iconography appears in the Chinese Eastern Zhou/Western Han cultures (3rd -to-2nd century BC). Raman spectra indicate predominant tremolite [ 21 ], consistently with low Fe content and Fe/Mg ratio from XRF; µ-XRD also detects minor talc. In the PCA score plot (Fig. 5 ), Cp/16 clusters with Cp/9 and Cp/10. OM highlights manufacturing traces indicative of wheel cutting or flexible string sawing, even in openwork areas (Fig S2). Surface finishing involved fine abrasives and riffling. The precision of some details, like the feline whiskers, suggests the use of metal tools and possibly a diamond tip, placing its production after the advent of metallurgy. Cp/18 is a spiral-shaped ornament with a dragon-like head at its centre, obtained by a single jade block and coated by red pigment traces. Its stylistic features suggest Western Han attribution (3rd -1st century BC). Raman identifies nephrite as the main component on the greenish surface, with OH vibrations indicating Mg-Mg-Mg and Mg-Mg-Fe occupancies in the M1 and M3 sites [ 22 ]. The pigment is cinnabar, as confirmed by Raman (bands at 344, 284 and 254 cm -1 ), µ-XRD and XRF (Hg – although with lower intensities than in Cp/14 and Cp/15). The spiral includes openwork decoration, probably obtained by initial drilling, then enlarged and modelled by flexible string sawing. Despite surface alterations, linear marks parallel to the openwork edges are still perceivable (Fig S3.a). OM reveals slight irregularities in the carving, confirming handcrafting technique (Fig S3.b and c). Cp/19 is a finely chiseled and elongated buckle obtained by a single jade block, with a rear button and a feline head on its sharper edge, consistent with the Western Han iconography (late 3rd /1st century BC). Both Raman (bands at 674, 370, 228, 179, 161 cm - ¹ [ 21 ] and µ-XRD indicate a nephrite composition. IR spectra detect organic materials on the surface, presumably a protective agent (carbonyl group at ∼ 1750 cm -1 ). OM reveals a polished surface (Fig. 3 .j) with light manufacturing marks, indicating an elaborated technique (metal tools for the engraved decorations on the front, where minor inaccuracies are also observed: Fig. 3 .k). Rear engravings are coarser, maybe obtained with a diamond tip. Lapping is accurate. 3.2 Artefacts made of lithologies other than nephrite Regarding non-nephrite samples, Fig. 7 shows the PCA score plot of the averaged XRF spectra for all analyzed artefacts. Clear group differences are observed, in accordance with those reported in Table 1 : nephrite samples cluster together, while non-nephrite artefacts appear more scattered. Cp/1 and Cp/2 are zhang axeheads with similar stylistic and compositional features. Cp/1 is a thick trapezoidal blade with basal indentation, quite unrefined and sharpened on both edges, made of a greenish rock with evident brown-to-yellowish streaks. Cp/2, with a fish-head-alike tip and similar indentation, has decorative engravings and is apparently made of the same greenish stone, with diffuse brown-to-yellowish areas, especially at the tip. Cp/1 is a model used in Mid-to-Northern China (possibly Henan, Xia period − 2070/1600 BC); Cp/2 is typical of Southwestern China (possibly Sichuan, Shang period − 1st millennium BC). Raman and µ-XRD detect predominant talc in the greenish portions (phyllosilicate, Mg 3 Si 4 O 10 (OH) 2 : bands at 3678, 3661, 676, 361, 193 cm -1 [ 40 ]). Cp/2 also contains minor periclase, Fe-oxides and sulphides. In PCA (Fig. 7 ), Cp/1 and Cp/2 cluster closely (due to their similar XRF spectra, Fig. S4), suggesting the use of the same stone type. OM reveals for both a less accurate surface finishing, with visible crafting marks not smoothed by final lapping – especially on the lateral sides (Fig S5.a and b). Cp/7 is a bi ring stylistically attributed to the Neolithic in Northwestern China (2nd millennium BC), less refined than the other tools of the same typology (Cp/8 and Cp/9). It has an irregular roundness with several chips on the edge (Fig. S6.a), in which the raw stone has a darker tone, dissimilar to jade. Raman (bands at 1087, 714, 283, 156 cm -1 [ 41 ]) and µ-XRD show mainly a calcite composition, with minor quartz and chlorite in veins. Ca also dominates the XRF spectra, with minor Si, S, Cl, Fe and Sr amounts. The high Ca content distinguishes Cp/7 from other samples in the PCA plot (Fig. 7 ). OM reveals coarse, parallel striations with various orientations, organized into groups (Fig. S6). The central hole is significantly larger than those of other bi rings. Cp/11, the most elaborated artefact, represents a funerary amulet carved like a cicada, with a trapezoidal shape and several engravings – a typical Han dynasty iconography (1st Century BC-1st Century AD). It is made of a white translucent stone covered by an external shell – yellowish inside, brown outside. µ-XRD (Fig. 8 ) identified ankerite, cerussite, quartz and cristobalite (with andalusite, albite, anatase and Al-oxides as minor phases). Raman, though affected by strong fluorescence, showed a strong carbonate band at 1056 cm -1 (CO 3 2- stretching). FTIR detected weak bands in the 3100 − 2850 cm -1 range, suggesting an organic binder (probably tung oil [ 42 ]), together with gypsum (1095 cm -1 [ 43 ]). Consistently with µ-XRD, XRF – performed only on the external shell – detected Pb (cerussite), Ca, Fe, Mn (ankerite) and Si (quartz, cristobalite and in minor phases) – plus minor P, Ba, Ni and Sr. The high Pb content, compared to other artefacts, justifies Cp/11 separation in the PCA plot (Fig. 7 ). Based on these results, the internal core may consist of a white/blueish silicate mineral (quartz and/or cristobalite), overlaid by andalusite (a low-pressure, high-temperature silicate, often involved in ceramic processing) possibly fired at the end of the processing. The external carbonate-rich shell (cerussite and ankerite), frail and degraded, modifies the amulet original aspect. Due to conservation issues, manufacturing traces are hardly identifiable: some irregular carvings and weak linear marks may result from handcrafting and use of a straight saw, respectively. Cp/13 is a blade of a Chinese jǐ halberd. Similar bronze artefacts were used during the Zhou dynasty, in the ‘Warring States’ period (2nd half of the 5th Century BC [ 44 ]). This one, made of grey stone, is well preserved and uniform in texture, with a small hole and a slit probably for fastening to a handle. Reddish surface engravings are well visible (Fig. 9 .a). µ-Raman and µ-XRD show presence of abundant dickite (Al 2 Si 2 O 5 (OH) 4 [ 45 ]); Al and Si dominate in XRF, which also detects minor elements (P, S, Cl, K, Ca, Ti, Fe, Ni); the low Ca content justifies its isolated PCA plot position (Fig. 7 ). µXRD of the engravings also reveals talc (Fig. 9 .b), but no compound eventually responsible for the red hue. Surface handcrafting signs are irregular and well-marked, probably from point abrasion or riffing. The edges are sharp. The hole has circular marks, typical of a tubular drill, and the slit is quite sharp, possibly resulting from wheel cutting. Cp/17 is a complex artefact made of three distinct parts: a central hollow cylinder links – passing through apt slits – two tabular ornaments resembling a dragon and a phoenix, presumably dating back to the Western Han dynasty (3rd -to-1st Century BC). µ-XRD and µ-Raman show abundant talc and serpentine (lizardite) in the central cylinder, with subordinate quartz and diaspore; calcite also appears in the tabular-shaped ornaments [ 41 , 46 ]. XRF reveals higher Ca-contents in the peripheral ornaments (indicative of calcite) and higher Fe ones in the cylinder – a compositional contrast that becomes evident in the PCA score plot (Fig. 7 ). The cylinder appears handcrafted, due to small imperfections perceivable only at higher magnifications, with no visible junctions; likely, it was first drilled and then enlarged/shaped with other techniques. The carved decorations have irregularities and variable thickness. The artefact also features an openwork decoration, in which manufacturing marks (hard to discern, due to encrustations) align with the edges. IR spectra show comparable signatures on the different parts, suggesting that they may consist of a similar lithic material. As in Cp/19, a stronger band at ∼1760 cm -1 indicates an organic material – likely an acrylic polymer, rather than wax. Discussion The performed archaeometric survey – combined with a thorough stylistic analysis – was aimed at characterizing the constituent materials and extrapolating the manufacturing procedures used on the purchased artefacts, so as to confirm the reliability about their presumed dating and provenance. Most of the studied items (i.e., all the ‘nephrite jade’ artefacts) showed compositions and crafting marks consistent with their presumed iconography and stylistic attributions, preventing any risk of non-legitimacy. However, some suspicions arose about the nature and/or production techniques for some artefacts, which are detailed hereafter. The mineral/chemistry of the rocks forming the Cp/1 and Cp/2 artefacts (talc + magnesite) is unusual. Similar rocks are known to exist in nature [ 47 , 48 ], but their use here is misleading. Talc is a very soft mineral (hardness = 1, on the Mohs scale) – and jade is supposed to be tough, first. Moreover, the distribution of the brown-to-yellowish streaks/portions on the blades/handles, in which magnesite prevails, is hardly relatable to natural causes. Archaeologists hypothesized that these brown-to-yellowish streaks/areas might represent burning marks, possibly left by combustion of cords that tied these axe-heads to wooden handles on the funeral pyre. This assumption is worth discussing. Talc – when heated at 800–1000°C (e.g., in a funeral pyre [ 49 ]) – transforms into enstatite (Mg 2 Si 2 O 6 ) and tridimite (SiO 2 ) [ 50 – 53 ]. However, if burned alongside C-based material (e.g., ancient plant-fibre cords [ 54 ]), talc may undergo carbonation forming Mg-carbonates [ 55 ]. This process is plausible here, especially since traces of periclase (MgO) – formed by magnesite decomposition at > 800°C [ 56 ] – were detected in Cp/2, specifically in the yellowish streaks/areas. Regarding possible similarities in the Cp/1 and Cp/2 rock composition, XRF spectra show that their chemistry is comparable (Fig. S4). Nonetheless, some doubts arose about their legitimacy, since manufacturing marks are not revealing and, despite their ancient appearance, deterioration signs (like possible burning marks), due to talc tenderness, could also result from recent events. Besides, no literature report exists about ancient Chinese jades made of talc. The Cp/7 bi ring is unusual due to its carbonatic composition (calcite). Similar items – with unelaborate craftsmanship and no decorations – are hard to date and authenticate, due to the lack of specific markers. The rock texture resembles white marble (although with a different grain) or alabaster, and may have been used as a jade substitute, valued more for its symbolic beauty than for its specific lithology [ 57 , 58 ]. The very few identified craftsmanship marksalign with Neolithic techniques, such as cutting, grinding, drilling, and polishing, by hand or manual rotary techniques [ 19 ]. Historical use of this material in ancient China is also documented [ 1 , 3 , 38 ]. Therefore, the ring’s authenticity appears well supported. The cicada-shaped amulet (Cp/11), made of an inner core and a superficial coating, represents the most sophisticated and puzzling item of the dataset. Affected by serious conservation problems, its material characterization also poses some troubles. Despite its traditional iconography in ancient China, doubts on its legitimacy still persist, due to its heterogeneous composition and lack of clearly identifiable manufacturing marks – likely worsened by deterioration. The Cp/13 jǐ halberd blade is the sole item made of dickite – a material softer than nephrite. Though similar halberds exist in bronze ( https://commons.wikimedia.org/wiki/File:Bronze_Halberd,_Tomb_of_Marquis_Yi_of_Zeng_(1017 0100233).jpg), the peculiar lithic composition and quite elaborate manufacturing of the one studied here suggest that it might represent a more recent copy of an ancient model, forged with a softer, less valuable material. This is further reinforced by the occurrence of possible calligraphic mistakes in the engraved characters, as hinted by archaeologists. The detection of both talc and serpentine in the Cp/17 ornament is notable. Talc may originate from Mg-minerals alteration in presence of CO 2 and H 2 O (carbonation or steatization [ 59 ]). This suggests that the artefact was originally made of serpentine (lizardite), with talc forming later as a superficial patina – possibly during burial. This patina prevents recognition of any manufacturing traces and coupled to the atypical composition and assembly of the artefact raises some doubts about its legitimacy. These concerns are emphasized by the detection of an unspecified organic material, possibly an acrylic polymer (also found on Cp/19, whose dating is uncertain). Such coatings may have been applied to mimic the glossy, ‘oily’ look of ancient jades – an effect lacking in modern ones, shaped with industrial tools – not excluding a more recent origin for Cp/17. The archaeometric investigation also highlighted other interesting aspects of nephrite artefacts. Visual and compositional lithological similarities between the Cp/9 bi ring and Cp/10 ge axe (both presumed ‘spinach jades’) suggest a common origin – i.e., from the same nephrite block. Vibrational spectroscopies and XRF display similar spectra and compositions. However, by comparing the integrated areas of the Ca/Si and Fe XRF peaks (Fig. 10 ) – markers of the nephrite composition – distinct clusters are observed, contradicting the hypothesis and indicating different sources. Identification of cinnabar in Cp/14, 15 and 18 is consistent with their stylistic dating, as this pigment was commonly used in red ancient Chinese jades [ 60 , 61 ]. Conclusions A collection of 14 presumed ancient Chinese jades, legally purchased and held by the Museum of Oriental Art of Turin (MAO, Italy), was investigated with a non-invasive archaeometric protocol to identify the constituent materials and conservation issues. OM in incident and grazing light revealed superficial manufacturing signs, linked to either traditional or modern manufacturing. The results were integrated with a stylistic analysis aimed at classifying and potentially dating the artefacts. Nephrite – the traditional lithology of ancient Chinese jades – was clearly identified in eight items. The contextual detection of traditional tool marks and/or decorating pigments – consistent with the manufacturing processes of their preumed dating and provenance, based on stylistic attributions – causes these artefacts to be reputed genuine. The remaining six objects showed an atypical lithology, with minerals softer than traditional jade (e.g., talc, calcite, dickite). Some of them also showed presence of dubious manufacturing marks (inconsistent with their presumed dating), suspicious superficial organic materials (aimed at embellishing their appearance) and/or stylistic/iconographic anomalies. The systematic recurrence of these inconsistencies might instill some doubts about the ground legitimacy of some of them. The obtained results supported a temporary exhibition at the MAO ( https://www.maotorino.it/it/evento/esposizione-giade-cinesilarte-rivelata-dalla-scienza/ ). 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Supplementary Files GiustettoetalChineseJadesSuppMat.pdf Cite Share Download PDF Status: Published Journal Publication published 27 Apr, 2026 Read the published version in npj Heritage Science → Version 1 posted Editorial decision: Revision requested 13 Oct, 2025 Reviews received at journal 27 Sep, 2025 Reviews received at journal 16 Sep, 2025 Reviewers agreed at journal 06 Sep, 2025 Reviewers agreed at journal 04 Sep, 2025 Reviewers invited by journal 01 Sep, 2025 Editor assigned by journal 29 Aug, 2025 Submission checks completed at journal 29 Aug, 2025 First submitted to journal 27 Aug, 2025 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. 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1","display":"","copyAsset":false,"role":"figure","size":1070397,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003eThe 14 artefacts constituting the ancient jades collection of the Museum of Oriental Arts (MAO) in Turin.\u003c/em\u003e\u003c/p\u003e","description":"","filename":"1.png","url":"https://assets-eu.researchsquare.com/files/rs-7472554/v1/f4a0fb39d44792d22b0bb980.png"},{"id":90886599,"identity":"56efe742-1816-488b-bba2-27eefcdfed0d","added_by":"auto","created_at":"2025-09-09 10:10:53","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":155071,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003eThe structure of the tremolite/actinolite amphibole phase, projected on the (001) crystal plane.\u003c/em\u003e\u003c/p\u003e","description":"","filename":"floatimage1.png","url":"https://assets-eu.researchsquare.com/files/rs-7472554/v1/acbd0d7ab79765aa1e161fe9.png"},{"id":90885137,"identity":"37643781-231e-4883-abe6-70c77c76c100","added_by":"auto","created_at":"2025-09-09 10:02:53","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":551165,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003ea) and (b): Micrographs of the\u003c/em\u003e\u003cstrong\u003e \u003c/strong\u003e\u003cem\u003eCp/8 bi ring. a) smoothed external edge with fine lapping traces; b) manufacturing signs inside the central hole. (c) to (f): Micrographs of the Cp/10 ge axe. c) tool marks on the artefact border, d) finished surface on the artefact border. e) detail of the hole, revealing presence of regular circular marks on the inner sides. f) sharp surface edge with fine finishing striations on the surface, occasionally smoothing the edges. (g) and (h): Micrographs of the Cp/14 and Cp/15 dragon-shaped pendants. g) on the polished surface, the spiral goes over the external frame. h) traces of red pigment in the carved areas \u003c/em\u003e232 \u003cem\u003eand on the upper portions of the decoration, partially covered by encrustations; a close-up of the opposite side of the hole also shows traces of red pigment, partially covered by encrustations, as well as circular marks. (j) and (k): Micrographs of the Cp/19 feline head. j) smooth and polished surfaces. k) detail of the decorative pattern and close-up of slight inaccuracies in the carving.\u003c/em\u003e\u003c/p\u003e","description":"","filename":"floatimage2.png","url":"https://assets-eu.researchsquare.com/files/rs-7472554/v1/ce29be9d69505954ac68416b.png"},{"id":90887069,"identity":"a0c790ad-61c6-4815-98a8-b2f583acb019","added_by":"auto","created_at":"2025-09-09 10:18:53","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":195449,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003eXRF average spectra (“light” and “low” ranges) of ‘nephrite jade’ artefacts (left) and normalized ratio of the areas of Fe and Mg XRF peaks (right). The areas of Mg peak in “light” mode and Fe peak in “low” mode were considered for the ratio. Due to the type of measurement, the peaks between light and low modes cannot be compared in absolute height.\u003c/em\u003e\u003c/p\u003e","description":"","filename":"floatimage3.png","url":"https://assets-eu.researchsquare.com/files/rs-7472554/v1/bd8474bffdd9858101333ebd.png"},{"id":90886598,"identity":"65a6aac6-ff53-479e-bf45-2179a0058eda","added_by":"auto","created_at":"2025-09-09 10:10:53","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":134816,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003ePC2 vs PC1 score plot obtained from PCA analysis on all the XRF spectra of the ‘nephrite-jade’ artefacts.\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eThe percentage explained variance for each PC is reported in brackets.\u003c/em\u003e\u003c/p\u003e","description":"","filename":"floatimage4.png","url":"https://assets-eu.researchsquare.com/files/rs-7472554/v1/0abdea9d68b74940651caec4.png"},{"id":90887070,"identity":"c8ef2bf2-26fc-42d2-9915-3204c6597be8","added_by":"auto","created_at":"2025-09-09 10:18:53","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":254690,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003ea) comparison between the Raman spectra of Cp/14 (below) and cinnabar from the RRUFF database (above); b) \u003c/em\u003eμ\u003cem\u003e-XRD pattern of the Cp/15 artefact, containing the reflections of tremolite (in red) and cinnabar (blue).\u003c/em\u003e\u003c/p\u003e","description":"","filename":"floatimage5.png","url":"https://assets-eu.researchsquare.com/files/rs-7472554/v1/073356c6aed17dfb2de49315.png"},{"id":91149031,"identity":"e6492912-2303-4fe8-86ab-a851f864b2d8","added_by":"auto","created_at":"2025-09-12 06:46:41","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":169224,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003ePC2 vs PC1 score plot obtained from PCA analysis on average XRF spectra of all the samples.\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eThe percentage of explained variance for each PC is reported in brackets.\u003c/em\u003e\u003c/p\u003e","description":"","filename":"floatimage6.png","url":"https://assets-eu.researchsquare.com/files/rs-7472554/v1/a5d3ce07890b4f3eec13d984.png"},{"id":90886601,"identity":"c0f1947e-0e35-4a0b-8bff-de7c25c9dfa4","added_by":"auto","created_at":"2025-09-09 10:10:53","extension":"png","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":1165636,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003eµ-XRD analytical spots and related diffraction patterns collected on the Cp/11 artefact: 1) and 3) light- coloured underlying layer; 2) brown surface layer with a glassy appearance; 4) base material; 5) a presumably modern addition.\u003c/em\u003e\u003c/p\u003e","description":"","filename":"8.png","url":"https://assets-eu.researchsquare.com/files/rs-7472554/v1/43e2de765b3d5be77c876173.png"},{"id":90885142,"identity":"3161737f-a772-4d29-93b6-87af2eeea248","added_by":"auto","created_at":"2025-09-09 10:02:53","extension":"png","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":197470,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003eCp/13: a) magnification of an engraving; b) µ-XRD pattern of the material filling the\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eengraving (dickite and talc reflections are marked in green and blue, respectively).\u003c/em\u003e\u003c/p\u003e","description":"","filename":"floatimage7.png","url":"https://assets-eu.researchsquare.com/files/rs-7472554/v1/81b1a764b24d28fbbd69d8ec.png"},{"id":90883626,"identity":"8b81d810-f1db-4ded-9725-a0f08f2acc5b","added_by":"auto","created_at":"2025-09-09 09:54:53","extension":"png","order_by":10,"title":"Figure 10","display":"","copyAsset":false,"role":"figure","size":53136,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003eSamples Cp/9 and Cp/10: integrated areas of the Fe peaks (y-axis) vs. the ratio between the integrated areas of Ca and Si peaks (main components of nephrite; x-axis). For comparison, also Cp/8 and Cp/16 are reported.\u003c/em\u003e\u003c/p\u003e","description":"","filename":"floatimage8.png","url":"https://assets-eu.researchsquare.com/files/rs-7472554/v1/a76e68483eae6e31bd59af98.png"},{"id":108438069,"identity":"82588b8a-54d0-43b3-985c-5b3aa06ebadd","added_by":"auto","created_at":"2026-05-04 16:06:37","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":5709784,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-7472554/v1/514798ab-53b7-4238-87e3-ed676b3cb61d.pdf"},{"id":90883619,"identity":"d0fc0dee-8a48-408b-ab98-2217e3f87688","added_by":"auto","created_at":"2025-09-09 09:54:53","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"supplement","size":368876,"visible":true,"origin":"","legend":"","description":"","filename":"GiustettoetalChineseJadesSuppMat.pdf","url":"https://assets-eu.researchsquare.com/files/rs-7472554/v1/d267d24d95a03cb79d710b23.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Assessment of manufacturing processes and materials characterization on a collection of ancient Chinese Jades","fulltext":[{"header":"Introduction","content":"\u003cp\u003eThe beauty and preciousness of ancient Chinese jades are renowned worldwide. Jade manufacturing in China dates back to 6000/5000 BC [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e, \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e]. However, the word \u0026lsquo;jade\u0026rsquo; has more recent European roots, from the Portuguese \u0026lsquo;\u003cem\u003epedra de ijada\u003c/em\u003e\u0026rsquo;(\u0026ldquo;kidney stone\u0026rdquo;), due to its supposed healing powers. In ancient China, jade was known as玉 (\u003cem\u003ey\u0026ugrave;\u003c/em\u003e in mandarin), meaning \u0026lsquo;gem\u0026rsquo; or \u0026lsquo;treasury\u0026rsquo; [\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e], referred to the material beauty and preciousness rather than to a particular stone. Under the term \u0026lsquo;jade\u0026rsquo;, in fact, several kinds of stones were comprised, depending on the specific context of pertinence. Scientifically, \u0026lsquo;jade\u0026rsquo; includes two different rock/mineral types: \u0026lsquo;nephrite\u0026rsquo; (a Ca-Mg-amphibole of the tremolite/ferro-actinolite series) and \u0026lsquo;jadeite\u0026rsquo; (a sodic pyroxene with ideal formula NaAlSi\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e6\u003c/sub\u003e) [\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e]. However, in the Chinese culture, other lithologies (i.e., rocks made of serpentine, sericite, quartz, talc, calcite) may also be referred to as \u0026lsquo;jades\u0026rsquo; [\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eMost ancient Chinese jades are made of \u0026lsquo;nephrite jade\u0026rsquo; [\u003cspan additionalcitationids=\"CR2\" citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e, \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e], probably extracted from the alluvial deposits of the Yurungkash and Karakash rivers, in present-day Kazakhstan, until the 10th century AD. From the 12th century, nephrite was also extracted from the ancient Khotan reign [\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e]. Due to their exploitation, these nephrite sources became less used in the last centuries, and new materials (e.g., brucite) were also introduced on the market [\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e]. Another jade source was probably located in Siberia, close to the Baikal Lake, from which a dark green variety with graphite inclusions was caved (so-called \u0026lsquo;spinach-jade\u0026rsquo; [\u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e, \u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e]). Regarding \u0026lsquo;jadeite jade\u0026rsquo;, its diffusion in ancient China is still discussed: supposed to circulate since the 10th century BC, it probably did not until the Qing Dynasty (17th century AD). Only recently (\u0026sim;250 years ago) the import from Northern Myanmar (ex Birman) was legalized, from whence it is regularly caved nowadays [\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e, \u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eDespite being known as \u0026ldquo;soft jade\u0026rdquo; (\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e軟玉\u003c/span\u003e: \u003cem\u003eruǎny\u0026ugrave;\u003c/em\u003e, softer than \u0026lsquo;jadeite jade\u0026rsquo;), nephrite (\u0026sim;6.5 on the Mohs scale) is a hard and silky rock; it is extremely difficult to work, causing the ancient Chinese artefacts to be extremely precious and expensive. However, recent archaeometric investigations proved that even in Neolithic cultures the use of nephrite must not be considered exclusive, as other \"pseudo-jade materials\" were used locally [\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e].\u003c/p\u003e"},{"header":"Research aim","content":"\u003cp\u003eThis study deals with the archaeometric investigation of a collection of ancient Chinese jades \u0026ndash; consisting of 14 artefacts purchased on the legal market by the \u003cem\u003eFondazione Compagnia di San Paolo\u003c/em\u003e and the municipality of Turin (Italy), never exposed to the public before and held in the \u0026lsquo;\u003cem\u003eMuseo d\u0026rsquo;Arte Orientale\u003c/em\u003e\u0026rsquo; (MAO, Museum of Oriental Art) of Turin (Italy). Their dating, based on stylistic basis, ranges from the Neolithic (2nd millennium BC) to the Han dynasty (202 BC \u0026minus;\u0026thinsp;220 AD). Serious uncertainties about the nature of the lithic materials and production techniques begot doubts about such attributions \u0026ndash; questioning the legitimacy of the purchased items. Thus, the need for an in-depth archaeometric study became necessary, in order to characterize their constituent materials, state of conservation and infer information about their manufacturing processes.\u003c/p\u003e"},{"header":"Materials and methods","content":"\u003cp\u003e\u003cem\u003e\u003cem\u003e2.1.\u0026nbsp;\u003c/em\u003eThe \u003cem\u003earchaeological\u0026nbsp;\u003cem\u003efinds\u003c/em\u003e\u003c/p\u003e\u003cdiv id=\"Sec4\" class=\"Section2\"\u003e\u003ch2\u003e\u003c/h2\u003e\u003cp\u003eThe studied archaeological record consists of fourteen artefacts (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e). Seven of them belong to a \"flat\" typology: three rings \u003cem\u003eb\u0026igrave;\u003c/em\u003e (Cp/7, Cp/8 and Cp/9); two \u003cem\u003ezhang\u003c/em\u003e (墇) ritual tablets (a weapon with a fish head shape \u0026ndash; Cp/2; an axe head \u0026ndash; Cp/1); one \u003cem\u003ege\u003c/em\u003e (戈) axe (Cp/10) and a model of halberd blade \u003cem\u003ejǐ\u003c/em\u003e (戟) (Cp/13). The ring \u003cem\u003eb\u0026igrave;\u003c/em\u003e (璧), marked by with a central hole, is the most classical item in Chinese glyptics, symbolizing the sun and used until the Qing dynasty [\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e]. Jade blades and axes were ritual items, not intended as weapons [\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e, \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e]. The other seven finds are more 3-dimensional. One represents a cicada (Cp/11), made of different components, probably sealed with an adhesive. Six portray fantastic animals: a feline-head buckle (Cp/19); a composite ornament with phoenix and dragon (Cp/17); a spiral-shaped creature (Cp/18); a feline-shaped plaque (Cp/16) and two dragon-shaped pendants (Cp/14 and Cp/15) [\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e, \u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e]. Some of them (Cp/14, 15 and 18) show red surface pigmentation.\u003c/p\u003e\u003cp\u003eFor the \u0026lsquo;nephrite-jade\u0026rsquo; manufacturing [\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e], rudimental tools \u0026ndash; like bamboo canes and archdrills \u0026ndash; were used. After the 4th Century BC, corundum and/or diamond could also have been employed [\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e] \u0026ndash; though some authors suggest earlier use in prehistoric times [\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e]. In Neolithic, jade was cut and polished manually by drilling or sawing, using abrasive powders (quartz, SiO\u003csub\u003e2,\u003c/sub\u003e or corundum, Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e) with grease or shellac. Manufacturing occurred in two stages: i) shaping and ii) carving, possibly preceded by heating [\u003cspan additionalcitationids=\"CR22\" citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e]. Techniques were mainly rotary or non-rotary. Among the former, a rudimental drill (wood or bamboo stick) was used, revolved by a rope mounted on a wooden arch, piercing the stone. Later, a disc was applied on the drill tip (\u0026lsquo;wheel-cutting\u0026rsquo; or \u0026lsquo;rotary-sawing\u0026rsquo;) to facilitate piercing. Resulting circular holes can be detected on their inner sides, with grooves parallel to their borders. In non-rotary techniques the stone was cut by saws (e.g., metal stick) or hemp/leather ropes with abrasive powders, leaving straight or slightly surface curved marks. Small cutting tools were then used to model the finer details (\u0026lsquo;riffing\u0026rsquo;), possibly leaving linear or concave marks. Diamond could also be used to engrave the stone without abrasive powders (\u0026rsquo;point abrasion\u0026rsquo;), leaving irregular marks on the stone surface. Between the 5th and 1st Century BC, the pedal lathe was introduced improving jade manufacturing. Only after 1911, mechanical and electric grinders enables the \u0026lsquo;industrial\u0026rsquo; production technology of jade artefacts. This modern manufacture causes jade artefacts to lose their original \u0026lsquo;oily\u0026rsquo; aspect, simulated by artificially spreading resin on the surface [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e, \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eNephrite \u0026ndash; the main material of \u0026lsquo;archaic Chinese jades\u0026rsquo; [\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e, \u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e, \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e] \u0026ndash; is a rock made mostly of an amphibole mineral with double chain of SiO\u003csub\u003e4\u003c/sub\u003e tetrahedrons [T(1) and T(2), Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e] elongating along \u003cem\u003ez\u003c/em\u003e, with Fe/Mg in three octahedral sites [M(1), M(2) and M(3) in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e] plus minor ions (e.g., Mn\u003csup\u003e2+\u003c/sup\u003e, Al\u003csup\u003e3+\u003c/sup\u003e, Ti\u003csup\u003e4+\u003c/sup\u003e, Cr\u003csup\u003e3+\u003c/sup\u003e, Ni\u003csup\u003e2+\u003c/sup\u003e [\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e, \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e]). Ca\u003csup\u003e2+\u003c/sup\u003e mainly occupies the distorted M(4) octahedral site [\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e, \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e, \u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e]. The variable Fe/Mg ratio defines a solid solution, whose endmembers are tremolite [Ca\u003csub\u003e2\u003c/sub\u003eMg\u003csub\u003e5\u003c/sub\u003eSi\u003csub\u003e8\u003c/sub\u003eO\u003csub\u003e22\u003c/sub\u003e(OH)\u003csub\u003e2\u003c/sub\u003e] and actinolite [Ca\u003csub\u003e2\u003c/sub\u003eFe\u003csub\u003e5\u003c/sub\u003eSi\u003csub\u003e8\u003c/sub\u003eO\u003csub\u003e22\u003c/sub\u003e(OH)\u003csub\u003e2\u003c/sub\u003e] [\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e]. The Fe\u003csup\u003e2+\u003c/sup\u003e content determines nephrite jade\u0026rsquo;s green hue [\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e]. The OH group stretching, shared by three octahedrons, is used to investigate the \u0026lsquo;fine structure\u0026rsquo; based on the Fe/Mg ratio, which may help in discriminating tremolite from actinolite and all intermediate compositions [\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e, \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e].\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec5\" class=\"Section2\"\u003e\u003ch2\u003e2.2. Experimental methods\u003c/h2\u003e\u003cp\u003eSubstantiating and dating ancient jades are particularly challenging. The custom of collecting ancient jade objects \u0026ndash; testified since 1200 BC \u0026ndash; causes their technical/stylistic evolution to be quite complicated. Further confusion arises from the Ming dynasty (14th\u0026ndash;17th century AD) practice of producing replicas of Han-period artefacts (2nd century BC \u0026ndash; 2nd century AD), making authentication even more difficult [\u003cspan additionalcitationids=\"CR30\" citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e]. Archaeometric investigations, including detailed studies of craftsmanship signs and synergic stylistic analyses, can help in pursuing such task [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eThe beauty and preciousness of this jade\u0026rsquo;s collection precluded any sampling, requiring the application of a non-invasive multi-analytical protocol.\u003c/p\u003e\u003cp\u003eX-ray Fluorescence (XRF) data were acquired with a portable Thermo Niton Mod XL3t-900 GOLDD spectrophotometer (Ag anode, SDD detector, 3 mm spot size, He flow, acquisition time of 120 s, 4 spectra acquired with 4 operating modes: 8 kV, no filter; 20 kV, Cu filter; 40 kV, Al/Fe filter; 50 kV, Mo filter. Data were analysed using Principal Component Analysis (PCA), using a custom-made script [\u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e32\u003c/span\u003e], by both considering the average of all spectra for each sample and the individual ones. To increase signal-to-noise, a binning was carried out on the spectra in steps of 60 eV from 1 keV to 3 keV, from 3 keV to 7.25 keV, and from 7.25 to 17.5 keV. For some elements (Mg, Si, Ca and Fe), the peak area was calculated using the Python multichannel analyser [\u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e] software for deconvolution.\u003c/p\u003e\u003cp\u003eAttenuated Total Reflectance Fourier-Transform Infra-Red (ATR-FTIR) spectra were recorded on a Bruker Vertex 70 spectrophotometer, coupled with a Bruker Hyperion 3000 IR microscope and equipped with an (MCT) FPA detector, working in the 4000/900 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e spectral range. Sixty-four scans were acquired with an average resolution of 4 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, operating with an ATR anvil diamond crystal.\u003c/p\u003e\u003cp\u003eRaman spectra were collected with a portable BWTEK i-Raman spectrophotometer equipped with a BAC151microscope, exciting the samples with a solid-state 785 nm laser and using a 26\u0026ndash;420 30 \u0026micro;m spot, in the 175 to 4200 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e range, with a 3 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e spectral resolution. Data were interpreted using the RRUFF\u0026trade; Project database [\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e], implemented by the CrystalSleuth software; spectra were plotted with the Origin software (OriginLab Corporation).\u003c/p\u003e\u003cp\u003eX-ray Diffraction (XRD) data were collected in the 3 to 70\u0026deg; 2θ angular range using a SMARTLAB XE Rigaku in micro(\u0026micro;)-diffraction mode (beam width \u0026sim; 500 \u0026micro;m), equipped with a vertical HyPix-3000 detector in 2D scan mode (10 mm slit, 0,02\u0026deg; step and 3\u0026deg;/min). Data were interpreted using the \"DIFFRAC PLUS, EVA Application 7.0.0.1\" (2001) software on suitable databases (JCPDS-ICCD; ICSD; PCPDFWIN).\u003c/p\u003e\u003cp\u003eOptical microscopy (OM) (20x binocular, 12 mm field depth, 0.6-5.5x magnification) in incident and grazing light was used for investigating the samples surfaces and highlighting possible traces left by manufacturing signs. The protocol of studying moulds of the artefact surfaces [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e] (Sax et al., 2004), obtained by coating them with Si-based resin, with scanning electron microscope (SEM) is unfit here, due to the occasional presence of pigments and/or other materials/byproducts that would risk removal \u0026ndash; violating the modern conservation rules [\u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e, \u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e]. A Leica S9-i optical stereomicroscope was thus used \u003cem\u003edirectly\u003c/em\u003e on the artefacts surfaces, consulting all disposable datasets to identify tool marks. A Dino-Lite Pro digital microscope (AM413ZTA) was also employed, featuring 1.3-megapixel sensor, eight white LEDs, light polarizer, and 10\u0026times;~50\u0026times;/220\u0026times; magnification).\u003c/p\u003e\u003c/div\u003e"},{"header":"Results","content":"\u003cp\u003eBased on their chemistry and mineralogy, the artefacts fall into two groups: i) eight are composed of nephrite (Cp/8\u0026ndash;10, 14\u0026ndash;16, 18, 19); ii) six consist of other rocks/minerals (Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e), including talc, magnesite, serpentine, quartz, calcite and dickite. Calcite and dickite are the sole constituent in Cp/7 and Cp/13, respectively. Some artefacts (Cp/13\u0026ndash;18) have engraved decorations, with traces of pigments - red (cinnabar), orange or white (talc).\u003c/p\u003e\u003cp\u003e\u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e\u003ccaption language=\"En\"\u003e\u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e\u003cdiv class=\"CaptionContent\"\u003e\u003cp\u003eAnalytical results obtained on the 14 artefacts investigated by applying the non-invasive archaeometric protocol. For XRF, the elements of the main peaks are in \u003cb\u003ebold\u003c/b\u003e.\u003c/p\u003e\u003c/div\u003e\u003c/caption\u003e\u003ccolgroup cols=\"7\"\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c6\" colnum=\"6\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c7\" colnum=\"7\"\u003e\u003c/div\u003e\u003cthead\u003e\u003ctr\u003e\u003cth align=\"left\" colname=\"c1\"\u003e\u003cp\u003eCode\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c2\"\u003e\u003cp\u003eArtefact typology\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c3\"\u003e\u003cp\u003eVibrational spectroscopies\u003c/p\u003e\u003cp\u003e(Raman; FT-IR)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c4\"\u003e\u003cp\u003eXRD\u003c/p\u003e\u003cp\u003e(crystalline phases)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c5\"\u003e\u003cp\u003eXRF\u003c/p\u003e\u003cp\u003e(chemical elements)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c6\"\u003e\u003cp\u003eMineral or rock species\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c7\"\u003e\u003cp\u003ePigments\u003c/p\u003e\u003c/th\u003e\u003c/tr\u003e\u003c/thead\u003e\u003ctbody\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e\u003cb\u003eCp/1\u003c/b\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c2\"\u003e\u003cp\u003e\u003cem\u003ezhang\u003c/em\u003e axe\u003c/p\u003e \u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003etalc, magnesite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003etalc\u0026thinsp;+\u0026thinsp;magnesite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e\u003cb\u003eSi\u003c/b\u003e,\u003c/p\u003e\u003cp\u003eMg, Al, S, Cl, K,Ca,\u003c/p\u003e\u003cp\u003eCr, Mn, Fe, Ni, Zn\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003etalc\u0026thinsp;+\u0026thinsp;magnesite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003e=\u003c/p\u003e \u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e\u003cb\u003eCp/2\u003c/b\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c2\"\u003e\u003cp\u003eaxe head fish shaped\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003etalc, magnesite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003etalc\u0026thinsp;+\u0026thinsp;magnesite, periclase, iron sulfide\u0026thinsp;+\u0026thinsp;iron oxide\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e\u003cb\u003eSi\u003c/b\u003e,\u003c/p\u003e\u003cp\u003eMg, Al, S, Cl, K,Ca, Cr, Mn, Fe, Ni\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003etalc\u0026thinsp;+\u0026thinsp;magnesite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003e=\u003c/p\u003e \u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e\u003cb\u003eCp/7\u003c/b\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c2\"\u003e\u003cp\u003e\u003cem\u003eyuan\u003c/em\u003e ring\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003ecalcite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003ecalcite\u0026thinsp;+\u0026thinsp;chlorite\u0026thinsp;+\u0026thinsp;quartz, mica\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e\u003cb\u003eCa\u003c/b\u003e\u003c/p\u003e\u003cp\u003eAl, Si, S, Cl, K, Ca, Ti, Mn, Fe, Sr,\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003ecalcite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003e=\u003c/p\u003e \u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e\u003cb\u003eCp/8\u003c/b\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c2\"\u003e\u003cp\u003e\u003cem\u003ebi\u003c/em\u003e ring\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003etremolite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003etremolite\u0026thinsp;+\u0026thinsp;quartz, calcite\u0026thinsp;+\u0026thinsp;feldspar, mica\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e\u003cb\u003eSi, Ca\u003c/b\u003e\u003c/p\u003e\u003cp\u003eMg, Al, S, Cl, K, Ti, Mn, Fe, Zn, Y\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003enephrite (tremolite)\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003e=\u003c/p\u003e \u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e\u003cb\u003eCp/9\u003c/b\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c2\"\u003e\u003cp\u003e\u003cem\u003ebi\u003c/em\u003e ring\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003etremolite/actinolite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003etremolite/actinolite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e\u003cb\u003eSi, Ca\u003c/b\u003e\u003c/p\u003e\u003cp\u003eMg, Al, S, Cl, K, Ti,\u003c/p\u003e\u003cp\u003eMn, Fe, Zn, Sr, Y\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003enephrite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003e=\u003c/p\u003e \u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e\u003cb\u003eCp/10\u003c/b\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c2\"\u003e\u003cp\u003e\u003cem\u003ege\u003c/em\u003e axe\u003c/p\u003e \u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003etremolite/actinolite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003etremolite/actinolite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e\u003cb\u003eSi, Ca\u003c/b\u003e\u003c/p\u003e\u003cp\u003eMg, Al, S, Cl, K, Ti, Mn, Fe, Sr, Y\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003enephrite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003e=\u003c/p\u003e \u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e\u003cb\u003eCp/11\u003c/b\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c2\"\u003e\u003cp\u003ecicada amulet\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003ecerussite\u0026thinsp;+\u0026thinsp;gypsum\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003eankerite, cerussite\u0026thinsp;+\u0026thinsp;quartz, cristobalite, aluminium oxide\u0026thinsp;+\u0026thinsp;andalusite, anatase, feldspar\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e\u003cb\u003eSi, Ca, Pb\u003c/b\u003e,\u003c/p\u003e\u003cp\u003eAl, P, S, Cl K, Mn,\u003c/p\u003e\u003cp\u003eFe, Sr, Zr, Ba\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003elithic core (quartz?, cristobalite?)\u0026thinsp;+\u0026thinsp;external layers (ankerite, cerussite, andalusite, \u0026hellip;)\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003e=\u003c/p\u003e \u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e\u003cb\u003eCp/13\u003c/b\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c2\"\u003e\u003cp\u003ereproduction of a Chinese halberd \u003cem\u003ejǐ\u003c/em\u003e.\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003edickite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003edickite\u0026thinsp;+\u0026thinsp;talc\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e\u003cb\u003eAl, Si\u003c/b\u003e\u003c/p\u003e\u003cp\u003eP, S, Cl, K, Ca, Ti, Fe, Sr, Y\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003edickite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003etalc (?)\u003c/p\u003e\u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e\u003cb\u003eCp/14\u003c/b\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c2\"\u003e\u003cp\u003edragonshaped pendant\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003ecinnabar\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003etremolite\u0026thinsp;+\u0026thinsp;chlorite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e\u003cb\u003eSi, Ca\u003c/b\u003e\u003c/p\u003e\u003cp\u003eMg, Al, P, S, Cl, K, Ti, Mn, Fe, Zn\u003c/p\u003e\u003cp\u003eHg (in all the areas)\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003enephrite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003ecinnabar\u003c/p\u003e\u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e\u003cb\u003eCp/15\u003c/b\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c2\"\u003e\u003cp\u003edragonshaped pendant\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003ecinnabar\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003etremolite, quartz\u0026thinsp;+\u0026thinsp;cinnabar\u0026thinsp;+\u0026thinsp;calcite, chlorite, feldspar\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e\u003cb\u003eSi, Ca\u003c/b\u003e\u003c/p\u003e\u003cp\u003eMg, Al, P, S, Cl, K, Ti, Mn, Fe, Zn\u003c/p\u003e\u003cp\u003eHg (in all the areas)\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003enephrite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003ecinnabar\u003c/p\u003e\u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e\u003cb\u003eCp/16\u003c/b\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c2\"\u003e\u003cp\u003eimaginary feline\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003etremolite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003etremolite/actinolite\u0026thinsp;+\u0026thinsp;talc\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e\u003cb\u003eSi, Ca\u003c/b\u003e\u003c/p\u003e\u003cp\u003eMg, Al, S, Cl, K, Ti,\u003c/p\u003e\u003cp\u003eMn, Fe, Zn, Rb, Sr,\u003c/p\u003e\u003cp\u003eY, Zr\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003enephrite\u0026thinsp;+\u0026thinsp;talc\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003e=\u003c/p\u003e \u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e\u003cb\u003eCp/17\u003c/b\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c2\"\u003e\u003cp\u003emobile ornament made of three different parts linked together\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003ecalcite, lizardite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003etalc, calcite\u0026thinsp;+\u0026thinsp;lizardite/antigorite, quartz, dolomite, ankerite, diaspore, grossular\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e\u003cb\u003eSi, Ca\u003c/b\u003e\u003c/p\u003e\u003cp\u003eMg, Al, S, Cl, K,\u003c/p\u003e\u003cp\u003eMn, Zn, Sr,, Ba\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003etalc\u0026thinsp;+\u0026thinsp;serpentine minerals\u0026thinsp;+\u0026thinsp;calcite (not in cylinder)\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003e=\u003c/p\u003e \u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e\u003cb\u003eCp/18\u003c/b\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c2\"\u003e\u003cp\u003espiral shaped fantastic creature\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003etremolite/actinolite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003etremolite/actinolite\u0026thinsp;+\u0026thinsp;cinnabar\u0026thinsp;+\u0026thinsp;iron sulfide\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e\u003cb\u003eSi, Ca\u003c/b\u003e\u003c/p\u003e\u003cp\u003eMg, Al, S, Cl, K, Ti,\u003c/p\u003e\u003cp\u003eMn, Fe, Zn, Sr, Zr\u003c/p\u003e\u003cp\u003eSmall Hg (only in some areas)\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003enephrite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003ecinnabar\u003c/p\u003e\u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e\u003cb\u003eCp/19\u003c/b\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c2\"\u003e\u003cp\u003ebuckle surmounted by a feline head\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003etremolite/actinolite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003etremolite/actinolite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e\u003cb\u003eSi, Ca\u003c/b\u003e\u003c/p\u003e\u003cp\u003eMg, Al, S, Cl, K, Ti,\u003c/p\u003e\u003cp\u003eMn, Fe, Zn\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003enephrite\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003e=\u003c/p\u003e \u003c/td\u003e\u003c/tr\u003e\u003c/tbody\u003e\u003c/colgroup\u003e\u003c/table\u003e\u003c/div\u003e\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cdiv id=\"Sec7\" class=\"Section2\"\u003e\u003ch2\u003e3.1 Artefacts in \u0026lsquo;nephrite-jade\u0026rsquo;\u003c/h2\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003e\u003cul\u003e\u003cli\u003e\u003cp\u003eCp/8, a quite circular drilled \u003cem\u003ebi\u003c/em\u003e ring likely from North-western China, shows smoothed external borders, dotted texture and tiny surface chippings due to polishing (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e.a), with both light greenish and blackish areas, suggesting a \u0026lsquo;spinach-jade\u0026rsquo; variety. The central hole has sharp borders and a truncated-cone shape, indicating that drilling was made on one side only.\u003c/p\u003e\u003c/li\u003e\u003c/ul\u003e\u003c/p\u003e\u003cp\u003e\u0026micro;-XRD and Raman shows amphibole as predominant phase, coupled to minor ones [K-feldspar (in whitish areas), magnesite, talc, quartz and Fe-sulphides (in darker zones)]. Raman bands at 674, 370 and 227 cm\u003csup\u003e-1\u003c/sup\u003e, and a single IR maximum in the OH stretching region (3674 cm\u003csup\u003e-1\u003c/sup\u003e, peak A [\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e]), indicate Mg\u003csup\u003e2+\u003c/sup\u003e abundance and tremolite-rich composition [\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e, \u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e, \u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e37\u003c/span\u003e]. This is confirmed also by XRF, in which the Mg peak is the highest (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e.a) among \u0026lsquo;nephrite-jade\u0026rsquo; artefacts, displaying the lowest Fe/Mg peak height ratio (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e.b).\u003c/p\u003e\u003cp\u003eRegarding craftsmanship traces, OM in grazing/incident light shows benches of parallel tool marks inside the central hole, oriented perpendicular to the edge (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e.b), which are not attributable to drilling (whose signs are circular). This suggests that the hole was only sketched by drilling at first (a few parallel striations to the hole border being still barely visible) and then enlarged by string sawing. Finer lapping traces are visible on the larger surfaces, mostly extending linearly between the two edges of the artefact. These likely indicate finishing touches and suggest that the tool may date to the end of the late Neolithic (Shang period, 2nd half of the 1st millennium BC).\u003c/p\u003e\u003cp\u003e\u003cul\u003e\u003cli\u003e\u003cp\u003eCp/9 is another \u003cem\u003ebi\u003c/em\u003e ring, possibly a \u0026lsquo;spinach-jade\u0026rsquo;, more homogeneous than the previous one, translucent and with brilliant green hue \u0026ndash; except for diffuse alteration along one edge due to weathering [\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e, \u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e38\u003c/span\u003e]. Its circumference and thickness are slightly irregular. The central hole, drilled on one side only, shows a truncated-cone shape and shear angulation. \u0026micro;-XRD and \u0026micro;-Raman identify nephrite as the sole constituent. Raman spectra in the OH stretching region (3700\u0026thinsp;\u0026minus;\u0026thinsp;3600 cm\u003csup\u003e-1\u003c/sup\u003e) suggest an intermediate tremolite/actinolite composition, with Mg-Mg-Fe or Mg-Fe-Mg occupation in the M1 and M3 sites [\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e, \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e, \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e]. OM reveals circular marks within the central hole and fine linear striations on the larger surfaces, partially smoothing the hole edges (Fig. \u003cspan refid=\"MOESM1\" class=\"InternalRef\"\u003eS1\u003c/span\u003e), possibly from abrasive powders moved by leather. These features support a stylistic dating following metallurgy (Shang period, 2nd half of the 1st millennium BC).\u003c/p\u003e\u003c/li\u003e\u003cli\u003e\u003cp\u003eCp/10 is a tabular \u003cem\u003ege\u003c/em\u003e axe typical of mid-Western China, used as a weapon (if tied to a wooden rod) or having ritual purposes. Its simplified shape suggests dating between the 13\u003csup\u003eth-\u003c/sup\u003e8th Century BC (Western Shang-Zhou [\u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e]). The stone visually resembles Cp/9 \u0026ndash; with a vivid green hue (possibly a \u0026lsquo;spinach-jade\u0026rsquo;) and alteration near the border. Raman, FT-IR and \u0026micro;-XRD confirm its nephritic nature, with an intermediate tremolite/actinolite composition [\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e, \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e]. XRF spectra are similar to Cp/8 and Cp/9, showing lower Al, Cl, K, Ti and higher Mn compared to other artefacts (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e.a). PCA (PC2 \u003cem\u003evs\u003c/em\u003e PC1, Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e) shows Cp/9 and Cp/10 clustering closely, while Cp/8 appears distinct.\u003c/p\u003e\u003c/li\u003e\u003c/ul\u003e\u003c/p\u003e\u003cp\u003eOM shows regular, parallel marks perpendicular to the artefact edges, suggesting the use of a toothed implement. Additional fine perpendicular striations (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e.c and d) and regular circular marks inside the hole indicate a rotating drill (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e.e). Edges are sharp, though occasional surface finishing causes them to become smoothened (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e.f). The two main surfaces are smooth, with fine but regular and well-defined lapping marks, likely resulting from a sophisticate finishing \u0026ndash; maybe using fine-grained corundum powder as abrasive. If confirmed, this might suggest a later dating, as Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e powders became widespread only from the 13th Century AD.\u003c/p\u003e\u003cp\u003e\u003cul\u003e\u003cli\u003e\u003cp\u003eCp/14 and Cp/15 are nearly identical dragon-shaped pendants, though differing slightly in size and number of pierced holes (one in Cp/14; two in Cp/15), possibly sharing the same manufacture. Their shape and spiral decorations are typical of the \u0026lsquo;Warring States\u0026rsquo; period (Eastern Zhou, 5th -3rd century BC). Originally coated by a red pigment, traces nowadays remain mainly in the carved areas. The slightly polished surface may result from post-depositional processes or conservation treatments. Red pigment, dirt and encrustations, hinder detection of manufacturing traces and consequent material identification. Raman detects only cinnabar (HgS, bands at 343, 286 and 254 cm\u003csup\u003e-1\u003c/sup\u003e; [\u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e39\u003c/span\u003e]; Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e.a); \u0026micro;-XRD identifies tremolite as the main component, with subordinate cinnabar (Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e.b). XRF confirms Hg and S as major elements (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e.a), along with others (Al, P, Cl, K and Ti), in higher amounts if compared to other \u0026ldquo;nephrite-jade\u0026rdquo; artefacts (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e.a). This might indicate either use of the same raw materials or simply pigment impurities. The Fe/Mg ratio is significantly higher here (and in Cp/18), due to presence of cinnabar biasing this value and preventing information about the tremolite/actinolite content (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e.b). As expected, in the PCA score plot Cp/14 and Cp/15 differ from the other samples \u0026ndash; again due to high Hg and S contents (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e).\u003c/p\u003e\u003c/li\u003e\u003c/ul\u003e\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eOM reveals that the outer edge decoration was delineated first, followed by carving of central spirals, since these sometimes overlap the border (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e.g). Circular parallel marks in the holes suggest drilling (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e.h); irregular carvings, instead, may result from riffling.\u003c/p\u003e\u003cp\u003e\u003cul\u003e\u003cli\u003e\u003cp\u003eCp/16 is a finely chiseled greenish plaque with dragon/feline motifs pierced from a unique jade block, and altered portions due to possible weathering [\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e, \u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e38\u003c/span\u003e]. This iconography appears in the Chinese Eastern Zhou/Western Han cultures (3rd -to-2nd century BC). Raman spectra indicate predominant tremolite [\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e], consistently with low Fe content and Fe/Mg ratio from XRF; \u0026micro;-XRD also detects minor talc. In the PCA score plot (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e), Cp/16 clusters with Cp/9 and Cp/10. OM highlights manufacturing traces indicative of wheel cutting or flexible string sawing, even in openwork areas (Fig S2). Surface finishing involved fine abrasives and riffling. The precision of some details, like the feline whiskers, suggests the use of metal tools and possibly a diamond tip, placing its production after the advent of metallurgy.\u003c/p\u003e\u003c/li\u003e\u003cli\u003e\u003cp\u003eCp/18 is a spiral-shaped ornament with a dragon-like head at its centre, obtained by a single jade block and coated by red pigment traces. Its stylistic features suggest Western Han attribution (3rd -1st century BC). Raman identifies nephrite as the main component on the greenish surface, with OH vibrations indicating Mg-Mg-Mg and Mg-Mg-Fe occupancies in the M1 and M3 sites [\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e]. The pigment is cinnabar, as confirmed by Raman (bands at 344, 284 and 254 cm\u003csup\u003e-1\u003c/sup\u003e), \u0026micro;-XRD and XRF (Hg \u0026ndash; although with lower intensities than in Cp/14 and Cp/15). The spiral includes openwork decoration, probably obtained by initial drilling, then enlarged and modelled by flexible string sawing. Despite surface alterations, linear marks parallel to the openwork edges are still perceivable (Fig S3.a). OM reveals slight irregularities in the carving, confirming handcrafting technique (Fig S3.b and c).\u003c/p\u003e\u003c/li\u003e\u003cli\u003e\u003cp\u003eCp/19 is a finely chiseled and elongated buckle obtained by a single jade block, with a rear button and a feline head on its sharper edge, consistent with the Western Han iconography (late 3rd /1st century BC). Both Raman (bands at 674, 370, 228, 179, 161 cm\u003csup\u003e-\u003c/sup\u003e\u0026sup1; [\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e] and \u0026micro;-XRD indicate a nephrite composition. IR spectra detect organic materials on the surface, presumably a protective agent (carbonyl group at \u0026sim; 1750 cm\u003csup\u003e-1\u003c/sup\u003e). OM reveals a polished surface (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e.j) with light manufacturing marks, indicating an elaborated technique (metal tools for the engraved decorations on the front, where minor inaccuracies are also observed: Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e.k). Rear engravings are coarser, maybe obtained with a diamond tip. Lapping is accurate.\u003c/p\u003e\u003c/li\u003e\u003c/ul\u003e\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec8\" class=\"Section2\"\u003e\u003ch2\u003e3.2 Artefacts made of lithologies other than nephrite\u003c/h2\u003e\u003cp\u003eRegarding non-nephrite samples, Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e shows the PCA score plot of the averaged XRF spectra for all analyzed artefacts. Clear group differences are observed, in accordance with those reported in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e: nephrite samples cluster together, while non-nephrite artefacts appear more scattered.\u003c/p\u003e\u003cp\u003e\u003cul\u003e\u003cli\u003e\u003cp\u003eCp/1 and Cp/2 are \u003cem\u003ezhang\u003c/em\u003e axeheads with similar stylistic and compositional features. Cp/1 is a thick trapezoidal blade with basal indentation, quite unrefined and sharpened on both edges, made of a greenish rock with evident brown-to-yellowish streaks. Cp/2, with a fish-head-alike tip and similar indentation, has decorative engravings and is apparently made of the same greenish stone, with diffuse brown-to-yellowish areas, especially at the tip. Cp/1 is a model used in Mid-to-Northern China (possibly Henan, Xia period \u0026minus;\u0026thinsp;2070/1600 BC); Cp/2 is typical of Southwestern China (possibly Sichuan, Shang period \u0026minus;\u0026thinsp;1st millennium BC).\u003c/p\u003e\u003c/li\u003e\u003c/ul\u003e\u003c/p\u003e\u003cp\u003eRaman and \u0026micro;-XRD detect predominant talc in the greenish portions (phyllosilicate, Mg\u003csub\u003e3\u003c/sub\u003eSi\u003csub\u003e4\u003c/sub\u003eO\u003csub\u003e10\u003c/sub\u003e(OH)\u003csub\u003e2\u003c/sub\u003e: bands at 3678, 3661, 676, 361, 193 cm\u003csup\u003e-1\u003c/sup\u003e [\u003cspan citationid=\"CR40\" class=\"CitationRef\"\u003e40\u003c/span\u003e]). Cp/2 also contains minor periclase, Fe-oxides and sulphides. In PCA (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e), Cp/1 and Cp/2 cluster closely (due to their similar XRF spectra, Fig. S4), suggesting the use of the same stone type. OM reveals for both a less accurate surface finishing, with visible crafting marks not smoothed by final lapping \u0026ndash; especially on the lateral sides (Fig S5.a and b).\u003c/p\u003e\u003cp\u003e\u003cul\u003e\u003cli\u003e\u003cp\u003eCp/7 is a \u003cem\u003ebi\u003c/em\u003e ring stylistically attributed to the Neolithic in Northwestern China (2nd millennium BC), less refined than the other tools of the same typology (Cp/8 and Cp/9). It has an irregular roundness with several chips on the edge (Fig. S6.a), in which the raw stone has a darker tone, dissimilar to jade. Raman (bands at 1087, 714, 283, 156 cm\u003csup\u003e-1\u003c/sup\u003e [\u003cspan citationid=\"CR41\" class=\"CitationRef\"\u003e41\u003c/span\u003e]) and \u0026micro;-XRD show mainly a calcite composition, with minor quartz and chlorite in veins. Ca also dominates the XRF spectra, with minor Si, S, Cl, Fe and Sr amounts. The high Ca content distinguishes Cp/7 from other samples in the PCA plot (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e). OM reveals coarse, parallel striations with various orientations, organized into groups (Fig. S6). The central hole is significantly larger than those of other \u003cem\u003ebi\u003c/em\u003e rings.\u003c/p\u003e\u003c/li\u003e\u003c/ul\u003e\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003e\u003cul\u003e\u003cli\u003e\u003cp\u003eCp/11, the most elaborated artefact, represents a funerary amulet carved like a cicada, with a trapezoidal shape and several engravings \u0026ndash; a typical Han dynasty iconography (1st Century BC-1st Century AD). It is made of a white translucent stone covered by an external shell \u0026ndash; yellowish inside, brown outside. \u0026micro;-XRD (Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003e) identified ankerite, cerussite, quartz and cristobalite (with andalusite, albite, anatase and Al-oxides as minor phases). Raman, though affected by strong fluorescence, showed a strong carbonate band at 1056 cm\u003csup\u003e-1\u003c/sup\u003e (CO\u003csub\u003e3\u003c/sub\u003e\u003csup\u003e2-\u003c/sup\u003e stretching). FTIR detected weak bands in the 3100\u0026thinsp;\u0026minus;\u0026thinsp;2850 cm\u003csup\u003e-1\u003c/sup\u003e range, suggesting an organic binder (probably tung oil [\u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e42\u003c/span\u003e]), together with gypsum (1095 cm\u003csup\u003e-1\u003c/sup\u003e [\u003cspan citationid=\"CR43\" class=\"CitationRef\"\u003e43\u003c/span\u003e]). Consistently with \u0026micro;-XRD, XRF \u0026ndash; performed only on the external shell \u0026ndash; detected Pb (cerussite), Ca, Fe, Mn (ankerite) and Si (quartz, cristobalite and in minor phases) \u0026ndash; plus minor P, Ba, Ni and Sr. The high Pb content, compared to other artefacts, justifies Cp/11 separation in the PCA plot (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e). Based on these results, the internal core may consist of a white/blueish silicate mineral (quartz and/or cristobalite), overlaid by andalusite (a low-pressure, high-temperature silicate, often involved in ceramic processing) possibly fired at the end of the processing. The external carbonate-rich shell (cerussite and ankerite), frail and degraded, modifies the amulet original aspect. Due to conservation issues, manufacturing traces are hardly identifiable: some irregular carvings and weak linear marks may result from handcrafting and use of a straight saw, respectively.\u003c/p\u003e\u003c/li\u003e\u003c/ul\u003e\u003c/p\u003e\u003cp\u003e\u003cul\u003e\u003cli\u003e\u003cp\u003eCp/13 is a blade of a Chinese \u003cem\u003ejǐ\u003c/em\u003e halberd. Similar bronze artefacts were used during the Zhou dynasty, in the \u0026lsquo;Warring States\u0026rsquo; period (2nd half of the 5th Century BC [\u003cspan citationid=\"CR44\" class=\"CitationRef\"\u003e44\u003c/span\u003e]). This one, made of grey stone, is well preserved and uniform in texture, with a small hole and a slit probably for fastening to a handle. Reddish surface engravings are well visible (Fig.\u0026nbsp;\u003cspan refid=\"Fig9\" class=\"InternalRef\"\u003e9\u003c/span\u003e.a). \u0026micro;-Raman and \u0026micro;-XRD show presence of abundant dickite (Al\u003csub\u003e2\u003c/sub\u003eSi\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e5\u003c/sub\u003e(OH)\u003csub\u003e4\u003c/sub\u003e [\u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e45\u003c/span\u003e]); Al and Si dominate in XRF, which also detects minor elements (P, S, Cl, K, Ca, Ti, Fe, Ni); the low Ca content justifies its isolated PCA plot position (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e). \u0026micro;XRD of the engravings also reveals talc (Fig.\u0026nbsp;\u003cspan refid=\"Fig9\" class=\"InternalRef\"\u003e9\u003c/span\u003e.b), but no compound eventually responsible for the red hue. Surface handcrafting signs are irregular and well-marked, probably from point abrasion or riffing. The edges are sharp. The hole has circular marks, typical of a tubular drill, and the slit is quite sharp, possibly resulting from wheel cutting.\u003c/p\u003e\u003c/li\u003e\u003cli\u003e\u003cp\u003eCp/17 is a complex artefact made of three distinct parts: a central hollow cylinder links \u0026ndash; passing through apt slits \u0026ndash; two tabular ornaments resembling a dragon and a phoenix, presumably dating back to the Western Han dynasty (3rd -to-1st Century BC). \u0026micro;-XRD and \u0026micro;-Raman show abundant talc and serpentine (lizardite) in the central cylinder, with subordinate quartz and diaspore; calcite also appears in the tabular-shaped ornaments [\u003cspan citationid=\"CR41\" class=\"CitationRef\"\u003e41\u003c/span\u003e, \u003cspan citationid=\"CR46\" class=\"CitationRef\"\u003e46\u003c/span\u003e]. XRF reveals higher Ca-contents in the peripheral ornaments (indicative of calcite) and higher Fe ones in the cylinder \u0026ndash; a compositional contrast that becomes evident in the PCA score plot (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e). The cylinder appears handcrafted, due to small imperfections perceivable only at higher magnifications, with no visible junctions; likely, it was first drilled and then enlarged/shaped with other techniques. The carved decorations have irregularities and variable thickness. The artefact also features an openwork decoration, in which manufacturing marks (hard to discern, due to encrustations) align with the edges. IR spectra show comparable signatures on the different parts, suggesting that they may consist of a similar lithic material. As in Cp/19, a stronger band at \u0026sim;1760 cm\u003csup\u003e-1\u003c/sup\u003e indicates an organic material \u0026ndash; likely an acrylic polymer, rather than wax.\u003c/p\u003e\u003c/li\u003e\u003c/ul\u003e\u003c/p\u003e\u003c/div\u003e"},{"header":"Discussion","content":"\u003cp\u003eThe performed archaeometric survey \u0026ndash; combined with a thorough stylistic analysis \u0026ndash; was aimed at characterizing the constituent materials and extrapolating the manufacturing procedures used on the purchased artefacts, so as to confirm the reliability about their presumed dating and provenance. Most of the studied items (i.e., all the \u0026lsquo;nephrite jade\u0026rsquo; artefacts) showed compositions and crafting marks consistent with their presumed iconography and stylistic attributions, preventing any risk of non-legitimacy. However, some suspicions arose about the nature and/or production techniques for some artefacts, which are detailed hereafter.\u003c/p\u003e\u003cp\u003eThe mineral/chemistry of the rocks forming the Cp/1 and Cp/2 artefacts (talc\u0026thinsp;+\u0026thinsp;magnesite) is unusual. Similar rocks are known to exist in nature [\u003cspan citationid=\"CR47\" class=\"CitationRef\"\u003e47\u003c/span\u003e, \u003cspan citationid=\"CR48\" class=\"CitationRef\"\u003e48\u003c/span\u003e], but their use here is misleading. Talc is a very soft mineral (hardness\u0026thinsp;=\u0026thinsp;1, on the Mohs scale) \u0026ndash; and jade is supposed to be tough, first. Moreover, the distribution of the brown-to-yellowish streaks/portions on the blades/handles, in which magnesite prevails, is hardly relatable to natural causes. Archaeologists hypothesized that these brown-to-yellowish streaks/areas might represent burning marks, possibly left by combustion of cords that tied these axe-heads to wooden handles on the funeral pyre. This assumption is worth discussing. Talc \u0026ndash; when heated at 800\u0026ndash;1000\u0026deg;C (e.g., in a funeral pyre [\u003cspan citationid=\"CR49\" class=\"CitationRef\"\u003e49\u003c/span\u003e]) \u0026ndash; transforms into enstatite (Mg\u003csub\u003e2\u003c/sub\u003eSi\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e6\u003c/sub\u003e) and tridimite (SiO\u003csub\u003e2\u003c/sub\u003e) [\u003cspan additionalcitationids=\"CR51 CR52\" citationid=\"CR50\" class=\"CitationRef\"\u003e50\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR53\" class=\"CitationRef\"\u003e53\u003c/span\u003e]. However, if burned alongside C-based material (e.g., ancient plant-fibre cords [\u003cspan citationid=\"CR54\" class=\"CitationRef\"\u003e54\u003c/span\u003e]), talc may undergo carbonation forming Mg-carbonates [\u003cspan citationid=\"CR55\" class=\"CitationRef\"\u003e55\u003c/span\u003e]. This process is plausible here, especially since traces of periclase (MgO) \u0026ndash; formed by magnesite decomposition at \u0026gt;\u0026thinsp;800\u0026deg;C [\u003cspan citationid=\"CR56\" class=\"CitationRef\"\u003e56\u003c/span\u003e] \u0026ndash; were detected in Cp/2, specifically in the yellowish streaks/areas. Regarding possible similarities in the Cp/1 and Cp/2 rock composition, XRF spectra show that their chemistry is comparable (Fig. S4). Nonetheless, some doubts arose about their legitimacy, since manufacturing marks are not revealing and, despite their ancient appearance, deterioration signs (like possible burning marks), due to talc tenderness, could also result from recent events. Besides, no literature report exists about ancient Chinese jades made of talc.\u003c/p\u003e\u003cp\u003eThe Cp/7 \u003cem\u003ebi\u003c/em\u003e ring is unusual due to its carbonatic composition (calcite). Similar items \u0026ndash; with unelaborate craftsmanship and no decorations \u0026ndash; are hard to date and authenticate, due to the lack of specific markers. The rock texture resembles white marble (although with a different grain) or alabaster, and may have been used as a jade substitute, valued more for its symbolic beauty than for its specific lithology [\u003cspan citationid=\"CR57\" class=\"CitationRef\"\u003e57\u003c/span\u003e, \u003cspan citationid=\"CR58\" class=\"CitationRef\"\u003e58\u003c/span\u003e]. The very few identified craftsmanship marksalign with Neolithic techniques, such as cutting, grinding, drilling, and polishing, by hand or manual rotary techniques [\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e]. Historical use of this material in ancient China is also documented [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e, \u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e, \u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e38\u003c/span\u003e]. Therefore, the ring\u0026rsquo;s authenticity appears well supported.\u003c/p\u003e\u003cp\u003eThe cicada-shaped amulet (Cp/11), made of an inner core and a superficial coating, represents the most sophisticated and puzzling item of the dataset. Affected by serious conservation problems, its material characterization also poses some troubles. Despite its traditional iconography in ancient China, doubts on its legitimacy still persist, due to its heterogeneous composition and lack of clearly identifiable manufacturing marks \u0026ndash; likely worsened by deterioration.\u003c/p\u003e\u003cp\u003eThe Cp/13 \u003cem\u003ejǐ\u003c/em\u003e halberd blade is the sole item made of dickite \u0026ndash; a material softer than nephrite. Though similar halberds exist in bronze (\u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://commons.wikimedia.org/wiki/File:Bronze_Halberd,_Tomb_of_Marquis_Yi_of_Zeng_(1017\u003c/span\u003e\u003cspan address=\"https://commons.wikimedia.org/wiki/File:Bronze_Halberd,_Tomb_of_Marquis_Yi_of_Zeng_(1017\" targettype=\"URL\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e 0100233).jpg), the peculiar lithic composition and quite elaborate manufacturing of the one studied here suggest that it might represent a more recent copy of an ancient model, forged with a softer, less valuable material. This is further reinforced by the occurrence of possible calligraphic mistakes in the engraved characters, as hinted by archaeologists.\u003c/p\u003e\u003cp\u003eThe detection of both talc and serpentine in the Cp/17 ornament is notable. Talc may originate from Mg-minerals alteration in presence of CO\u003csub\u003e2\u003c/sub\u003e and H\u003csub\u003e2\u003c/sub\u003eO (carbonation or steatization [\u003cspan citationid=\"CR59\" class=\"CitationRef\"\u003e59\u003c/span\u003e]). This suggests that the artefact was originally made of serpentine (lizardite), with talc forming later as a superficial patina \u0026ndash; possibly during burial. This patina prevents recognition of any manufacturing traces and coupled to the atypical composition and assembly of the artefact raises some doubts about its legitimacy. These concerns are emphasized by the detection of an unspecified organic material, possibly an acrylic polymer (also found on Cp/19, whose dating is uncertain). Such coatings may have been applied to mimic the glossy, \u0026lsquo;oily\u0026rsquo; look of ancient jades \u0026ndash; an effect lacking in modern ones, shaped with industrial tools \u0026ndash; not excluding a more recent origin for Cp/17.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eThe archaeometric investigation also highlighted other interesting aspects of nephrite artefacts.\u003c/p\u003e\u003cp\u003eVisual and compositional lithological similarities between the Cp/9 \u003cem\u003ebi\u003c/em\u003e ring and Cp/10 \u003cem\u003ege\u003c/em\u003e axe (both presumed \u0026lsquo;spinach jades\u0026rsquo;) suggest a common origin \u0026ndash; i.e., from the same nephrite block. Vibrational spectroscopies and XRF display similar spectra and compositions. However, by comparing the integrated areas of the Ca/Si and Fe XRF peaks (Fig.\u0026nbsp;\u003cspan refid=\"Fig10\" class=\"InternalRef\"\u003e10\u003c/span\u003e) \u0026ndash; markers of the nephrite composition \u0026ndash; distinct clusters are observed, contradicting the hypothesis and indicating different sources.\u003c/p\u003e\u003cp\u003eIdentification of cinnabar in Cp/14, 15 and 18 is consistent with their stylistic dating, as this pigment was commonly used in red ancient Chinese jades [\u003cspan citationid=\"CR60\" class=\"CitationRef\"\u003e60\u003c/span\u003e, \u003cspan citationid=\"CR61\" class=\"CitationRef\"\u003e61\u003c/span\u003e].\u003c/p\u003e"},{"header":"Conclusions","content":"\u003cp\u003eA collection of 14 presumed ancient Chinese jades, legally purchased and held by the Museum of Oriental Art of Turin (MAO, Italy), was investigated with a non-invasive archaeometric protocol to identify the constituent materials and conservation issues. OM in incident and grazing light revealed superficial manufacturing signs, linked to either traditional or modern manufacturing. The results were integrated with a stylistic analysis aimed at classifying and potentially dating the artefacts.\u003c/p\u003e\u003cp\u003eNephrite \u0026ndash; the traditional lithology of ancient Chinese jades \u0026ndash; was clearly identified in eight items. The contextual detection of traditional tool marks and/or decorating pigments \u0026ndash; consistent with the manufacturing processes of their preumed dating and provenance, based on stylistic attributions \u0026ndash; causes these artefacts to be reputed genuine.\u003c/p\u003e\u003cp\u003eThe remaining six objects showed an atypical lithology, with minerals softer than traditional jade (e.g., talc, calcite, dickite). Some of them also showed presence of dubious manufacturing marks (inconsistent with their presumed dating), suspicious superficial organic materials (aimed at embellishing their appearance) and/or stylistic/iconographic anomalies. The systematic recurrence of these inconsistencies might instill some doubts about the ground legitimacy of some of them.\u003c/p\u003e\u003cp\u003eThe obtained results supported a temporary exhibition at the MAO (\u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://www.maotorino.it/it/evento/esposizione-giade-cinesilarte-rivelata-dalla-scienza/\u003c/span\u003e\u003cspan address=\"https://www.maotorino.it/it/evento/esposizione-giade-cinesilarte-rivelata-dalla-scienza/\" targettype=\"URL\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e).\u003c/p\u003e"},{"header":"Declarations","content":"\u003ch3\u003eAcknowledgements\u0026nbsp;\u003c/h3\u003e\n\u003cp\u003e\u003cstrong\u003e\u0026nbsp;\u003c/strong\u003eThe authors would like to thank Marco Guglielminotti \u0026ndash; former curator of East Asian section and director of the \u0026lsquo;\u003cem\u003eMuseo d\u0026rsquo;Arte Orientale\u003c/em\u003e\u0026rsquo; (MAO \u0026ndash; Museum of Oriental Art) of Turin \u0026ndash; for his invaluable hints.\u0026nbsp;\u003c/p\u003e\n"},{"header":"References","content":"\u003col\u003e\n\u003cli\u003eSax, M., Meeks, N.D., Michaelson, C., Middleton, A.P. (2004). The identification of carving techniques on Chinese jade. Journal of Archaeological Science, 31(10), 1413-1428.\u003c/li\u003e\n\u003cli\u003eChen, T.H., Calligaro, T., Pages, S., Menu, M. (2004). Investigation of Chinese archaic jade by PIXE and μRaman spectrometry, Appl. Phys. A 79, 177\u0026ndash;180.\u003c/li\u003e\n\u003cli\u003eXu, J.A.; Huang, E.; Chen, C-H.; Tan, L.P.; Yu, B.S. (1996). A Raman spectroscopic study of archaic jades. Acta Geologica Taiwanica. 32, 11-42.\u003c/li\u003e\n\u003cli\u003eDamour, M.A. (1846). Analyse du jade oriental: r\u0026eacute;union de cette substance \u0026agrave; la tremolite. \u003cem\u003eAnn.Chim. Phys., 3\u003csup\u003erd\u003c/sup\u003e ser\u003c/em\u003e., 17, 469-474.\u003c/li\u003e\n\u003cli\u003eWang, R. (2011). Progress review of the scientific study of chinese ancient jade. Archaeometry, 53, 4, 674-692. doi: 10.1111/j.1475-4754.2010.00564.x\u003c/li\u003e\n\u003cli\u003eMiddleton A., Ambers J. (2005). 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Materials and technology of Chinese jades dating to the Western Zhou period (1050771 BCE). Science in China Series E: Technological Sciences. 51, 4, 467-480.\u003c/li\u003e\n\u003cli\u003eScheuermann, W., Ritter, G. J. (1969). Raman Spectra of Cinnabar (HgS), Realgar (As\u003csub\u003e4\u003c/sub\u003eS\u003csub\u003e4\u003c/sub\u003e) and Orpiment (As\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e3\u003c/sub\u003e). Zeitschrift f\u0026uuml;r Naturforschung A, 24, 3, 408-411.doi: doi.org/10.1515/zna-1969-0317.\u003c/li\u003e\n\u003cli\u003eBlaha, J.J., Rosasco, G.J. (1978). Raman Microprobe Spectra of Individual Microcrystals and Fibers of Talc, Tremolite, and Related Silicate Minerals. Analytical Chemistry. 50, 7, 892-896.\u003c/li\u003e\n\u003cli\u003eRutt, H.N., Nicola, J.H. (1974). Raman spectra of carbonates of calcite structure. Journal of Physics C: Solid State Physics. 7, 4522-4528.\u003c/li\u003e\n\u003cli\u003eSch\u0026ouml;nemann, A., Edwards, H.G.M. (2011). 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PMID: 31882588; PMCID: PMC6934827.\u003c/li\u003e\n\u003cli\u003eMai, Y., Wang, R., Cui, H. (2021). Study on the blackening mechanism of buried cinnabar within ancient Chinese jades. Journal of Cultural Heritage, 49, 164-173.\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"npj-heritage-science","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"hsci","sideBox":"Learn more about [Heritage Science](http://heritagesciencejournal.springeropen.com)","snPcode":"40494","submissionUrl":"https://submission.nature.com/new-submission/40494/3","title":"npj Heritage Science","twitterHandle":"@SpringerOpen","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"BMC/SO AJ","inReviewEnabled":true,"inReviewRevisionsEnabled":true},"keywords":"Chinese jade, Han dynasty, non-destructive protocol, nephrite, legitimacy","lastPublishedDoi":"10.21203/rs.3.rs-7472554/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-7472554/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eA collection of 14 Chinese jades of the Museum of Oriental Art, Turin (Italy), was stylistically described and studied at the optical microscope in incident/grazing light, to detect manufacturing marks and reconstruct production techniques (handcrafted or mechanical) without risking removal of materials. A non-invasive multi-analytic protocol (p-XRF/PCA, FTIR and \u0026micro;-Raman spectroscopies, \u0026micro;-X-ray diffraction) was applied to characterize materials and conservation. Eight artefacts are made of nephrite \u0026ndash; consistently with the archaic Chinese jades composition, though insufficient to assess legitimacy. The recurrence of revealing manufacturing marks/iconographies allowed supporting these items genuineness. Six artefacts revealed different lithologies, sometimes with hardness/tenacity significantly lower than jades. For some, distinctive technological marks suggest that the choice of atypical materials was either dictated by specific necessities or consequent to the artefacts use or interment; in few cases, doubts arose about legitimacy. This study provides an archaeometric perspective for evaluating material inconsistencies between museum artefacts and archaeological specimens.\u003c/p\u003e","manuscriptTitle":"Assessment of manufacturing processes and materials characterization on a collection of ancient Chinese Jades","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-09-09 09:54:48","doi":"10.21203/rs.3.rs-7472554/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2025-10-14T02:51:16+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-09-27T15:52:05+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-09-16T06:12:23+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"338328922660116000741897351376492278835","date":"2025-09-06T08:06:49+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"257704870459645301411088016522978493003","date":"2025-09-04T06:16:33+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2025-09-01T06:03:09+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2025-08-29T05:08:14+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2025-08-29T05:06:29+00:00","index":"","fulltext":""},{"type":"submitted","content":"npj heritage science","date":"2025-08-27T14:19:10+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"npj-heritage-science","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"hsci","sideBox":"Learn more about [Heritage Science](http://heritagesciencejournal.springeropen.com)","snPcode":"40494","submissionUrl":"https://submission.nature.com/new-submission/40494/3","title":"npj Heritage Science","twitterHandle":"@SpringerOpen","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"BMC/SO AJ","inReviewEnabled":true,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"d2e9c2eb-97dc-43e6-86b7-0ea71fb9d6b6","owner":[],"postedDate":"September 9th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[],"tags":[],"updatedAt":"2026-05-04T16:06:24+00:00","versionOfRecord":{"articleIdentity":"rs-7472554","link":"https://doi.org/10.1038/s40494-026-02497-5","journal":{"identity":"npj-heritage-science","isVorOnly":false,"title":"npj Heritage Science"},"publishedOn":"2026-04-27 15:57:23","publishedOnDateReadable":"April 27th, 2026"},"versionCreatedAt":"2025-09-09 09:54:48","video":"","vorDoi":"10.1038/s40494-026-02497-5","vorDoiUrl":"https://doi.org/10.1038/s40494-026-02497-5","workflowStages":[]},"version":"v1","identity":"rs-7472554","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-7472554","identity":"rs-7472554","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}