In situ high- and low-temperature unpolarized FTIR absorption spectra of hydrous components in natural Fe-rich rutile have been recorded using a FTIR600 heating and cooling stage attached to an IR microscope. Two absorption bands (3279 and 3297 cm(-1)) at room temperature are ascribed to fundamental stretching bands of OH. Both OH bands shift to lower wavenumbers at elevated temperatures, but with different amplitudes. With increasing temperature, the integral absorbance of the 3279 cm(-1) band increases while the integral absorbance of the 3297 cm(-1) band decreases. These changes are fully reversible. The different frequency shifts of the two IR absorption bands with temperature imply two different local chemical environments of H defects. Based on the chemical composition of the rutile and the electronegativity of impurity ions, the results of the in situ high- and low-temperature FTIR measurements support the band assignment of Bromiley and Hilairet (2005): the 3279 and 3297 cm(-1) bands are due to interstitial H decoupled from any substitutional defects, and H coupled to Fe(3+) on the neighboring octahedral (Ti) site (Fe(Ti)(3+) <-> Ti(Ti)(4+)), respectively. Variations in integral absorbance of the two bands suggest the transformation between decoupled H defects and coupled H defects as a function of temperature, possible due to some statistical relationship between the proportions of coupled and decoupled interstitial H dependent on the amount of heat energy applied to the system.
东汉晚期越窑青釉瓷的烧制成功,是我国陶瓷工艺技术发展过程中第三个里程碑.它的出现使中国成为世界上最早发明瓷器的国家①.越窑创建于东汉,鼎胜于唐、五代,衰落于宋代,历时千余年②.
The modern analysis technology has become an important research method in the field of the ancient jade. We carry the analysis on the 13 ancient jades in this article from the cemetery of Ying state in Pingdingshan,Henan Province. The result shows the tremolite is the main kind of jades from the cemetery of Ying state,different materials of jade are subject to a certain degree of weathering. The serpentine jade generally was weathered seriously,but deeper than the tremolite jade,and the serious weathering tremolite jade and serpentine jade are great similar in appearance. All jades'surface are attached to the cinnabar,possibly at that time people have begun to realize that the anticorrosion function of the cinnabar.
The presence of water, even in small amounts, in the continental lower crust may play a critical role in its physical and chemical properties and behavior. However, the environment and evolution of water in the deep crust remain poorly constrained. Investigation of water, dissolved as H‐related point defects in minerals of lower crustal granulites, may provide clues to clarify this issue. The analyzed and compiled water data of nominally anhydrous clinopyroxene (cpx), orthopyroxene (opx), and plagioclase (plag) in lower crustal granulites from Hannuoba, Nushan, and Daoxian in eastern China reveal significant contrast in water contents (ppm H2O by weight) between Precambrian and Phanerozoic samples, e.g., 200–2330 versus 275–720 ppm for cpx, 140–1875 versus 60–185 ppm for opx, 145–900 versus 65–345 ppm for plag, and 155–1120 versus 165–360 ppm for the bulk concentrations. Our data show consistently higher water contents in the Precambrian granulites, implying a more hydrous lower crust in the Precambrian than in the Phanerozoic. Such a difference may reflect variable water contents in the original melts, indicating higher water contents in the Precambrian upper mantle or a plume source for that part of the Precambrian lower crust.
The authors analyzed four modern turquoises from Hubei province and Anhui province by using the Raman microscopic with the samples are gathered on the spot. According to the study the authors discovered that the Raman spectra of the Hubei turquoises with different color but with the same backgrounds of mineral resource and the formation cause of mineral resource and in the same formation line of turquoise mineral resource have little difference. On the contrary, there is a strong difference in the 900-100 cm(-1) region of the Raman spectra between the turquoises from Hubei province and the turquoise from Anhui province which has remarkable different backgrounds of mineral resource and the formation cause of mineral resource. At the same time the authors studied two ancient turquoises to discuss the feasibility of using the Raman spectra of turquoises, the provenance of which is known, as the fingerprint directions to track the provenance of ancient turquoises.
Through measuring with some analytical techniques such as Raman,XRD,XRF,IR and SEM,a mosa- ic jade on the bronze ware of the pre-Qin times was studied.There are corrosion products of the bronze on the jade's surface,such as malachite,azurite and hydrocerusite etc.,it shows that the mosaic jade is not only eroded by the soil,groundwater and other environmental factors but also by corrosion products of the bronze ware.By ana- lyzing many residues on the side faces and back of the mosaic jade,the combining technics of jade and bronze in the pre-Qin times was also discussed.
Based on powder simulation experiments, the authors preliminarily simulated the acid and alkaline environments in which the ancient jades are buried. In the soaking experiment, the different massive shapes of jade materials were dipped in acid and alkaline buffer solutions, and the contrast analysis with the result of the powder simulation experiment was carried out, with the purpose of deepening the understanding of the weathering mechanism of the ancient jade.
Mineral dissolution is an important process in mineral weathering, and therefore the research on the mineral dissolution process helps to reveal the mineral weathering mechanism. The ancient jade has been in a dissolution reaction system of soil and soil-water in its long burial process. Generally speaking, the soils of southern China are somewhat acid, whereas soils in northern China tend to be alkaline. The authors preliminarily simulated the acid and alkaline environments that buried ancient jades experienced. Based on the soaking experiment in which the powder shapes of different jade materials were dipped in acid and alkaline buffer solutions, this paper preliminarily discusses the weathering mechanism of different jade materials.
Five painted pottery shards and two pieces of red mineral aggregate were analyzed, which were excavated from the Shuangdun site of Bengbu city, by Raman spectrometry, X-ray diffraction (XRD) and wavelength dispersive X-ray fluorescence spectrometry (WDXRF). The results show that the main phases of red pigment of the painted pottery are hematite, α-quartz, dolomite and calcite. Meanwhile, it also clarifies that the black paint is infiltrating charcoal instead of mineral pigment. And furthermore the results verify the feasibility of those three analytical methods for phase identification and component analysis in archaeology study.
本文采用ICP-MS技术测试了三个现代矿产地和贾湖遗址出土的绿松石样品的微量元素.结果表明:通过多元统计方法遴选出的微量元素组合以及稀土元素配分模式可以很好地区分不同产地的绿松石样品,并且进一步验证了"贾湖遗址绿松石不是来源于陕西、湖北、安徽".
This paper discusses the relationship between the volume loss, fluid flow and component variations in the ductile shear zone of the southern Tan-Lu fault belt. The results show that there is a large amount of fluids flowing through the shear zone during mylonitization, accompanied with the loss of volume of rocks and variations of elements and oxygen isotopes. The calculated temperature for mylonitization in different mylonites ranges from 446 to 484 degrees C, corresponding to that of 475 to 500 degrees C for the wall rocks. The condition of differential stress during mylonization has been obtained between 99 and 210 MPa, whereas the differential stress in the wall rock gneiss is 70-78 MPa. The mylonites are enriched by factors of 1.32-1.87 in elements such as Ti02, P205, MnO, Y, Zr and V and depleted in SiO2, Na2O, K2O, Al2O3, Sr, Rb and light REEs compared to their protolith gneiss. The immobile element enrichments are attributed to enrichments in residual phases such as ilmentite, zircon, apatite and epidote in mylonites and are interpreted as due to volume losses from 15% to 60% in the ductile shear zone. The largest amount of SiO2 loss is 35.76 g/100 g in the ductile shear zone, which shows the fluid infiltration. Modeling calculated results of the fluid/rock ratio for the ductile shear zone range from 196 to 1192 by assuming different degrees of fluid saturation. Oxygen isotope changes of quartz and feldspar and the calculated fluid are corresponding to the variations of differential flow stress in the ductile shear zone. With increasing differential flow stress, the mylonites show a slight decrease of delta O-18 in quartz, K-feldspar and fluid.
Through observing with naked eyes and microscope,measuring with some analytical techniques such as gravimetry,hardness test,X-ray diffraction analysis,Fourier transform-infrared spectrometry and laser Raman spectrometry,122 pieces of ancient jade samples excavated from Xuejiagang site were identified.The physical features and structural characteristics of jades were also discussed.Furthermore,the proposals on protection of excavated jades were put forward.The analytical results indicate that the probability of misjudgemment for the ancient jades under serious weathering with naked eye testing is much higher than with other methods.If the influence from air within the samples could be thoroughly eliminated,the components of the ancient jades can be precisely distinguished by gravity test.Although there are differences in color,density and etc.in inner and outer surface of the ancient jades,principal phase compositions are identical.
Energy Dispersive X-ray fluorescence Spectrometric(EDXRFS) probe was applied to the analysis for the major,minor and trace-elements in samples of ancient white glaze made in kilns of Xing,Gong,Ding and Yiyang in northern China.Through the analysis of chemical composition and the multivariable statistical analysis,regional characteristics of products from different kilns were revealed.It was found that there was close relationship between the white porcelain produced by Yiyang kiln and the white porcelain produced by Gong kiln.
The structures and compositions of theBaihuimianfrom Taosi and Yucisi sits were analyzed by XRD,XRF,ICP-AES,ICP-MS and Raman spectroscopy methods,respectively.It was shown that theBaihuimianwere calcite,which proved that the ancient Chinese had known the technology of making lime about4000years ago.Moreover,it indicated that one sample ofBaihuimianfrom Taosi sit was gypsum,which also suggested that the technology of exploiting and using gypsum had been mastered by ancient Chinese in architecture about4000years ago.
The physical characteristics of the ancient jades in Lingjiatan site, such as color, transparence, hardness and absorbingwater capability etc. had changed much after their being entombed for a long time. Some of ancient jades even show special phenomenon, which is denser outside, looser inside. Through working on microstructure and microanalysis of the ancient jade, the conclusion was got that after being entombed, the ancient jade in Lingjiatan site has gone through two stages. One is weathering and eluviating stage, another is penetrating and cementing stage.
采用X-射线荧光光谱分析法对贾湖遗址出土的绿松石饰物进行了成分的定性和定量分析,得到了它们的主要成分的含量.除个别样品外,大多绿松石的成分较纯,材质较好.这部分样品的含铁量较低,Fe2O3含量都在5%以下,有的仅千分之几.将这批样品和选自陕西安康、湖北郧县和安徽马鞍山的绿松石矿石样品中的P2O5、As2O5、Fe2O3、CuO和ZnO含量作聚类分析,发现贾湖出土的绿松石不太可能来自陕西安康、湖北郧县和安徽马鞍山等地的绿松石矿区,但应来自同一个未知地区.
Non-destructive analysis is always the aim in jades' research. The present article applied the Raman spectroscopy to the research on jades excavated from the Xue Jiagang site and achieved good result in the main mineral, inclusion and phenocryst. The study shows that as a non-destructive technique Raman spectroscopy can be applied to ancient jades conveniently and practically, and it can detect not only the surface information of ancient jades, but also the interior information. The technique is important to the verification and provenance of ancient jades.
Gong kiln, for its long porcelain-firing history, was one of three representative white porcelain kilns in northern China. In order to improve the quality and whiteness of white porcelain, a decorating layer or cosmetic earth was laid on the body surface in Gong kiln during early Tang dynasty, which was able to blot out rough surface and weaken the influence of fuscous body upon surface color. In this paper the main chemical composition of the white porcelain's profile was analyzed by using energy disperse X-Ray fluorescence. The result showed that different materials were used as cosmetic earth during early Tang dynasty, in accordance with the phenomenon under optical microscope. In addition, the glaze belongs to calcium glaze in which plant ash was added.
Archaeological studies have indicated that the “red burnt clay”excavated from Lingjiatan site,about 5500 BP,might be the earliest ceramic material for building in China.Some tests on“red burnt clay”,such as the structure,firing temperature,water absorptivity and strength of pressure resistance were dose. Furthermore,some comparative tests on bricks from Han,Ming Dynasties and modern age were introduced,it was found that“red burned clay”was fired from clay material over 950℃.and there were certain variational gradations from outside to inside of “red burnt clay”.The conclusion could be reached that strength of pressure resistance and water absorptivity for “red burnt clay”was similar to those of bricks of Han Dynasty and modern age,and better than those of Ming Dynasty.All of these results support strongly the archaeologist' conjecture that the “red burnt clay”from Lingjiatan site might be the rudiment of brick.
This paper is focused on the microstructure and microanalysis of the ancient Chinese Ru imperial ware and its imitations, the ancient Jun ware and Yue celadon ware. Samples were measured by stereomicroscope, polarized-microscope, XRD, SRXRF, HR-TEM and F-SEM, both equipped with EDX. We concluded that there are three phases in the glaze of the Ru imperial ware, a crystalline plus two amorphous phases, while only two amorphous phases were found in the glaze of the Ru's imitation and Jun wares, and only one amorphous phase in the glaze of the Yue celadon. Great differences were observed between the Ru ware and its imitations. Ru's imitations had more similarities with the ancient Jun blue-glazed ware. The unique crystalline phase found in the Ru imperial ware glaze was identified as anorthite. Mechanism of forming blue color in the glaze of Ru imperial ware is related to the Rayleigh scattering. The interlayer found between the glaze and the body had the same mineral paragenesis as the body itself. This and the distribution of the bubbles in the glaze, led us to conclude that the Ru ware was fired before it was glazed and the glassy appearance of its glaze was due to the sudden drop of temperature not because of the high firing temperature as believed in other researches.