Study on the chemical composition features of Longquan celadon excavated from the Chuzhou site of Huai'an City in Jiangsu Province by EDXRF

A mass of Longquan celadon shards were excavated from the Chuzhou site of Huai'an City in Jiangsu Province, China. These celadon shards were fired during the period of the Late Yuan Dynasty to the Tianshun era of the Ming Dynasty, as identified by archaeologists at Nanjing Museum. In order to research the chemical composition features of this ancient celadon porcelain, energy dispersive X-ray fluorescence (EDXRF) for non-destructive analysis was used to determine the chemical composition of the porcelain body and glaze in these shards. The results indicate that Ti and Fe in the body of Longquan celadon are characteristic elements which can distinguish porcelain produced during the Late Yuan Dynasty from those produced in the Ming Dynasties. The results of the principal component analysis (PCA) show that different body and glaze raw materials were used for the production of porcelain in different periods and the raw materials of the body and glaze are also different for various vessel shapes. The chemical compositions in the porcelain body of civilian ware are slightly different. The imperial and civilian Longquan celadon porcelains produced during the Hongwu era to the Tianshun era of the Ming Dynasty are distinguishable by the MnO, Fe₂O₃, Rb₂O and SrO content in their porcelain glaze.     

Structure Characterization of Modified Polyimide Films Irradiated by 2MeV Si Ions

Structures of polyimide （6051） films modified by irradiation of 2.0 MeV Si ions with different fluences are studied in detail. Variations of the functional groups in polyimide are investigated by attenuated total reflection Fourier transform infrared spectroscopy （ATR-FTIR） and Raman spectroscopy. The results indicate that the functional groups can be destroyed gradually with the increasing ion fluenee. The variations of structure and element contents are characterized by x-ray diffraction （XRD）, Rutherford backscattering spectrometry （RBS） and x- ray photoelectron spectroscopy （XPS）. The results indicate that the contents of N and O decrease significantly compared with the original samples, some graphite-like and carbon-rich phases are formed in the process of irradiation.     

Unique Magnetic Moment and Electronic Properties for Fe（MgO）n（n=1-8） Clusters： First-Principles Calculations

The geometries and electronic properties of Fe（MgO）n are systematically investigated by the density functional theory. The results show that the doped Fe atom is prone to bond with the O atom, and Fe almost does not disturb the frame of （MgO）n. The second-order energy difference, the fragmentation energies and the electron amnities show that Fe（MgO）4 and Fe（MgO）6 possess relatively higher stabilities. The HOMO-LUMO gaps of Fe（MgO）n decrease obviously as compared with （MgO）n. Almost equal unpaired electrons of the 3d state of the Fe atom in Fe（MgO）n result in a nearly equal magnetic moment of Fe（MgO）n.     

用主量化学组成研究汝官瓷和钧官瓷的原料来源

将84个清凉寺窑汝官瓷和钧台窑钧官瓷样品进行质子激发X射线荧光分析,得到每个样品胎和釉的7种主量化学组分。将所有样品的7种主量化学组成数据进行散布分析,以确定汝官瓷和钧官瓷原料来源是否相同。从散布分析图可以看出,汝官瓷釉和 钧官瓷釉样品的原料产地和配方明显不同,汝官瓷胎和钧官瓷胎样品的原料产地和成分接近,但有所不同。The seven main chemical components of the body and glaze samples of 84 RuGuan porcelains from Qingliangsi kiln and JunGuan porcelains from Juntai kiln are determined by the proton induced X-ray emission （ PIXE）. Then these data are analyzed by scatter analysis to confirm whether the sources of the raw materials of Ru-Guan porcelain from Qingliangsi kiln and JunGuan porcelain from Juntai kiln are the same or not. The figure of the scatter diagram shows that the sourcing area of the raw material and batch formula of RuGuan porcelain and Jun-Guan porcelain glaze are obviously different and the sources of the raw materials and components of their body samples are close but a bit different.     

用指纹元素散布分析研究古耀州瓷胎的起源

选取耀州窑瓷胎样品25个，唐三彩的胎3个，作坊匣钵料样品1个，耀州博物馆附近粘土矿样品4个．用中子活化分析测量样品中29种元素的含量，从这29种元素中挑选出8种指纹元素，将指纹元素的含量进行散布分析．结果表明，出自不同窑口的古耀州瓷的胎，有着长期稳定的、集中的原料产地．耀州窑唐三彩的胎料产地和耀州瓷胎的原料产地相同．25 samples of Yaozhou porcelain bodies, 3 samples of the tri-color pottery bodies during the Tang Dynasty, 1 samples of Saggar material during Song Dynasty and 4 samples of clay mineral taken from the place near Yaozhou Kiln Museum was selected . The technique of neutron activation analysis (NAA) has been employed to measure the content of 29 kinds of elements in the samples. 8 elements of them were selected as fingerprint elements to make scatter analysis.The conclusion is that the ancient Yaozhou por...     

Experimental evaluation of rate coefficients for Rb（5Dj）＋H2→ RbH＋H reaction

The Rb（5Dj）＋H2→RbH＋H photochemical reaction has been studied. Rb vapor mixed with H2 is irradiated in a glass cell with 778-nm pulses which populate one of the 52D states by two-photon absorption. Measurements for the relative intensities of the atomic fluorescence and the absorption of the RbH product near the axis of the cell yield the rate coefficients for the Rb（5D3/2）＋H2 and Rb（5D5/2）＋H2 reactions, which are （3.6±1.3） ×10^-11 and （1.7±0.6）×10^-11 cm^3/s, respectively. The relative reactivity with H2 for Rb（5D3/2） is higher than that for Rb（5D5/2）.     

不同窑口古代青瓷的产地特征的中子活化分析

产地属性是科学鉴别遗址和墓葬中出土的古陶瓷烧制产地的重要依据.用仪器中子活化（INAA）有损分析了浙江寺龙口越窑、江西洪州窑和陕西耀州窑出土的古瓷碎片样品,通过实验数据的统计分析,结果表明3个窑口古瓷的元素组成具有各自的特征,它们之间具有可以区分的依据,寺龙口越窑与南方江西洪州窑的制胎原料关系较近,与北方陕西耀州窑的关系较远.这些试验结果将为古陶瓷地研究提供重要参数.Provenance characteristic is an important scientific parameter to identify ancient porcelain wares unearthed from sites and graves.The porcelain samples of Si Long Kou kiln of Zhejiang Province,Hong Zhou kiln of Jiangxi Province and Yao Zhou kiln of Shanxi Province have been analyzed with neutron activation analysis(NAA) in this paper.The experimental data were studied with statistic methods.The results show that the chemical compositions of porcelain body samples for three kilns were different. The difference was been able identified. The body materials of both Si Long Kou Yue kiln and Hong Zhou kiln of Jiangxi were similar. The samples of Yao Zhou kiln in north of China existed obvious difference.     

Effect of Gd doping on the magnetism and work function of Fe1-xGdx/Fe（001）

The magnetism and work function Ф of Fe1-xGdx/Fe （001） films have been investigated using first-principles methods based on the density functional theory. The calculated results reveal that Gd doping on the Fe （001） surface would greatly affect the geometrical structure of the system. The restruction of the surface atoms leads to the transition of magnetic coupling between Gd and Fe atoms from ferromagnetic （FM） for 0.5 ≤x ≤ 0.75 to antiferromagnetic （AFM） for x = 1.0. For Fe1-xGdx/Fe （001） （x = 0.25, 0.5, 0.75, 1.0）, the charge transfer from Gd to Fe leads to a positive dipole formed on the surface, which is responsible for the decrease of the work function. Moreover, it is found that the magnetic moments of Fe and Gd on the surface layer can be strongly influenced by Gd doping. The changes of the work function and magnetism for Fe1-xGdx/Fe （001） can be explained by the electron transfer, the magnetic coupling interaction between Gd and Fe atoms, and the complex surface restruction. Our work strongly suggests that the doping of the metal with a low work function is a promising way for modulating the work function of the magnetic metal gate.     

Preparation of enamel coating by laser irradiation

Enamel coatings is produced on steel substrates using CW CO_2 laser irradiation from the same raw material as used for industrial enamel coating. The formed coating fairly well join to the substrate and has a bumpy glossy surface. Its microstructure is uniform and glassy with a liitle of small pores. It contains less Na and K than the initial composition. Fe element has been transfered into the coating, the content is high in the interface zone and low in the main body. This distribution may be at a time establish the good chemical stability of coating and its strong adhension to substrate. The present investigation also makes comparison of the laser irradiated coating with the ordinarily enamelled one.     

Microstructure evolution of zircaloy-4 during Ne ion irradiation and annealing: An in situ TEM investigation

The microstructural evolution of zircaloy-4 was studied, including the amorphization and recrystallization of Zr（Fe, Cr）2 precipitates, and the density of dislocations under in situ Ne ion irradiation and post annealing. The results show that irradiation at a relatively high temperature and dose induces the formation of nanocrystals in pre-amorphized Zr（Fe, Cr）2 precipitates. The recrystallized nanocrystals also have the structure of hcp-Zr（Fe, Cr）2. The formation of the nanocrystals is thought to be the consequence of competition between atomistic disordering and the recrystallization of precipitates under ion irradiation. The free energy of the nanocrystal is lower than that of the amorphous state, which is another reason for the recrystallization of the precipitates. With increased annealing temperature, the density of the nanocrystals is increased. The dislocation density sharply decreases with the increase in the annealing temperature, and its size increases.     

历代定窑白瓷的EDXRF和XAFS分析

定窑是我国宋代五大名窑中唯一以生产白瓷而闻名于世的窑厂,其高超的刻印花纹技术及首创的支圈覆烧工艺,对国内外许多窑场产生了深远的影响。采用(energy dispersive X-ray fluorescence, EDXRF)探索了历代定窑白瓷的组成配方,并采用X射线吸收精细结构(XAFS)法分析了瓷釉中Fe元素的价态,以探讨定窑白瓷的相关烧制工艺。研究发现,定窑白瓷瓷胎具有典型北方瓷器“高铝低硅”的特征,并在瓷胎中特意添加了富含CaO的矿物原料,对瓷胎的烧结有一定的促进作用。瓷胎中的TiO₂应主要是高岭土原料中的杂质。定窑白瓷瓷釉具有“高钙高镁”特征,基本属于钙镁釉或钙镁碱釉。其瓷釉配方中应含有一定量的白云石或滑石。瓷釉中K₂O的含量逐步增加,反映了定窑瓷釉由钙镁釉向钙碱釉发展演变的过程。此外,根据瓷釉中的Al₂O₃,MnO和P₂O₅等含量的特征,可以推测釉料配方中应添加了草木灰和高岭土。由XAFS分析结果可知,晚唐五代时期定窑白瓷釉中Fe3+比例最高,金代次之,宋代最低,不同时期定窑白瓷皆是在还原气氛中烧成。宋金时期定窑白瓷白中泛黄可能由于燃料煤中富含的硫在燃烧过程中与瓷釉反应,生成Fe-S化合物所致。     

后司岙匣钵工艺特征及其对青瓷釉面呈色的影响

越窑青瓷是我国最早烧制成熟的青瓷器,其中使用瓷质匣钵烧造秘色青瓷是越窑独特的烧造技术,为揭示越窑上林湖后司岙窑址出土的唐五代时期匣钵的工艺特征及其对装烧青瓷的影响,采用能量色散X荧光光谱仪（ED-XRF）、超景深显微镜、扫描电子显微镜（SEM）等现代测试分析手段,对后司岙窑址出土的唐五代时期瓷质匣钵、普通匣钵、普通青瓷、秘色青瓷进行了元素组成、显微结构、吸水率等测试分析。同时采用分光光度计,对该遗址出土的唐五代普通青瓷和秘色青瓷表面色度进行了测试分析。分析结果表明：唐五代普通匣钵的基体部分和瓷质匣钵组成相似,采用了SiO₂含量约为75%、Al₂O₃含量约为16%,且与青瓷胎体类似的当地冲积粘土类原料;而唐五代瓷质匣钵中TiO₂和Fe₂O₃的含量高于青瓷胎体且差异略大,说明青瓷胎体淘洗工艺更加严格。其中普通匣钵内存在大量平均尺寸在530 μm左右,且具有颗粒级配呈现一定规律的夹杂粗颗粒,是一类为增加普通匣钵使用寿命特意拣选添加的高硅质原料,增加了匣钵的透气性、机械强度和热稳定性从而延长匣钵的使用寿命;唐五代瓷质匣钵的气孔率为1.61%、吸水率为0.73%,低于普通匣钵8.18%和4.28%,而体积密度为2.22 g·cm-3高于普通匣钵的1.99 g·cm-3,且导热性能高于普通匣钵,有利于减少匣钵内外温差、缓解温度滞后现象。另外,上林湖后司岙窑址出土的秘色青瓷使用气孔率较低的瓷质匣钵,并进行口沿封釉,有效降低了装烧青瓷釉在冷却过程中被二次氧化的程度,提高了匣钵内气氛的稳定性和青瓷釉层中Fe2+的含量,改善了其呈色稳定性和外观效果。同时秘色青瓷釉层略厚,减少了胎体对产品外观的影响,增大了釉面折射率和明亮度,使其在CIE色度空间中相比普通青瓷处在更偏蓝绿色区域。     

安徽繁昌柯家冲窑青白瓷釉化学组成及其制釉工艺来源研究

为了解繁昌柯家冲窑青白瓷釉化学组成特征及其演变过程,并探索我国南方早期青白釉的工艺技术来源,本文运用能量色散X射线荧光光谱法(EDXRF)分析了柯家冲窑五代至北宋中期不同阶段青白瓷釉的化学组成,并将分析结果与同时期北方定窑白瓷釉及南方越窑青瓷釉化学组成进行了综合对比研究。结果显示,繁昌柯家冲窑青白釉化学组成在北宋中期时发生了明显变化,其中尤以SiO₂含量的下降和CaO含量的上升最为明显,着色元素Fe,Mn,Ti的氧化物含量自五代时期至北宋中期变化幅度很小,繁昌柯家冲窑青白釉釉色由偏白向偏青转变的原因可能与该窑瓷器胎色的不断加深有关。此外,主成分分析及具有相似功能特性的元素组合对比分析结果显示,繁昌柯家冲窑青白瓷釉的化学组成与北方定窑白瓷釉较为接近,其釉料配方工艺可能来源于同时期我国北方地区以定窑为代表的白瓷窑场。本文研究结果对了解我国早期青白瓷釉的化学组成特征及晚唐五代时期南、北方制瓷工艺技术交流问题等有重要学术价值。     

耀州古瓷釉层呈色机理的质谱研究方法

采用实验室自制飞秒激光电离飞行时间质谱(fs-LI-TOFMS)对唐代、五代、宋代、金代以及明代等五个朝代的耀州窑古瓷片釉层进行多元素同时分析,研究其呈色机理,以过渡元素为重点考察陶瓷釉层中所有可能着色元素的着色效果。推测耀州黑瓷烧制采用的很可能是Co-Cr-Fe-Mn系黑色釉料;明代白釉形成的主要原因是Fe元素含量低,还有可能与Ni元素有关;釉层中P 元素含量增多会导致釉色偏黄。毫无疑问,这一系列发现是对整个耀州瓷体系釉层呈色机理的重要补充。     

Mass Spectrometric Methods for Colorative Mechanism Analysis of Yaozhou Porcelain GlazeSCIEI北大核心CSCD

An in-house-built femtosecond laser ionization time-of-flight mass spectrometry (fs-LI-TOFMS) has been applied to the multi-elemental analysis of porcelain glaze from Yaozhou kiln. The samples are selected representing products of different dynasties, including Tang, Five, Song, Jin, and Ming Dynasty. For exploring the colorative mechanism of Yaozhou porcelain through the elemental analysis of the glaze, the effects of all potential coloring elements, especially transition elements, were considered. There was a speculation that the typical Co-Cr-Fe-Mn recipe was used in the fabrication of Yaozhou black glaze; the low content of Fe and high content of Ni resulted in the porcelain of white glaze; an increase content of P could lead the porcelain to be yellow-glazed. Undoubtedly, this research is an important supplement to the study of the colorative mechanism of the Yaozhou porcelain system.     

金诃脑血康胶囊中微量、宏量元素的测定分析

文章采用火焰原子吸收分光光度法测定了5批藏成药金诃脑血康胶囊中镉、铬、钴、铜、铁、镁、锰、镍、铅、锌等10种微量、宏量金属元素的含量,并对其结果进行了分析。结果表明,金诃脑血康胶囊中含有丰富的宏量元素Mg和有益的微量元素Cu,Zn,Fe,Mn,Ni等,有毒元素Pb,Cd含量较低,金属元素的含量高低顺序为：Fe＞Mg＞Zn＞Mn＞Cu＞Ni＞Cr＞Pb＞Co＞Cd。测定结果为探讨藏成药中微量、宏量元素与治疗心脑血管疾病功效的关系提供了有用的数据。     

漫反射光谱在“老挝石”颜色成因上的应用

近来,一种产自老挝的新型印章石(俗称“老挝石”)涌进国内市场,对我国印章石市场造成一定影响,“老挝石”的研究尚处于起步阶段,对其颜色成因的研究更为缺乏。采用漫反射光谱(DRS)结合X射线粉晶衍射(XRD)、红外光谱(FTIR)、X射线荧光光谱(EDXRF)等测试对红色“老挝石”的矿物成分和致色机理进行深入研究。结果显示,“老挝石”的主要矿物成分为地开石,并含有少量高岭石,化学成分中的Fe含量和“老挝石”红色色调呈正相关关系,即颜色越深Fe的含量越高。铁质矿物呈微晶集合体浸染分布于地开石的颗粒间,由于其含量低、粒度细小,常规的微区测试方法无法确认其种属。相比之下,漫反射光谱对微晶铁矿物的鉴定十分有效,对可见光波段漫反射光谱处理得到导数等,在土壤沉积物中已经被用来定量测定针铁矿和赤铁矿。该研究中“老挝石”基体与土壤沉积物均为粘土矿物,可以用漫反射光谱来判定“老挝石”中铁矿物种属。漫反射光谱一阶导数法显示,其谱峰位于565～570 nm,由此确认铁矿物的种属为赤铁矿。微晶赤铁矿分布于“老挝石”矿物颗粒间,使样品产生红色,赤铁矿含量越高,红色调越深。     

X‐ray compositional microanalysis and diffraction studies of Haltern 70 amphorae sherds

Haltern 70 amphorae sherds from excavations at Castro do Vieito, north of Portugal, and amphora sherds found inside kilns from Baetican and Lusitanian provinces of the Roman Empire are studied by X‐ray diffraction and X‐ray fluorescence (scanning electron microscopy/energy‐dispersive X‐ray spectroscopy). The comparison of these results is also made. The chosen methods give the possibility to determine element composition of the pottery, which is already fired, and thus try to single out the match of the two series of amphorae sherds. From the chemical analysis, the Castro do Vieito sherds are very homogeneous, but this is not the case of the sherds collected in the overall kilns. Vieito sherds have nearly no Na content, and Al content is about 9 wt% as well as samples from kilns from Medium Guadalquivir, Cadiz Bay and Guadiana estuary. Ca content in Vieito sherds are about 1 wt% and in amphorae kilns sherds except in the case of samples from Puerto Real and Arva, where Ca concentration is about 5 wt% and Lebrija and Pinguele where Ca concentration is about 10 wt%. The main conclusion drawn is that the provenance of Castro do Vieito sherds seems to be confirmed as being from Baetica (actual Andaluzia) because of the aforementioned reasons together with the fact that the elements found in the sherds are the same as the ones known to belong to raw materials from Baetica. Copyright © 2011 John Wiley & Sons, Ltd.     

原子吸收光谱法测定膜荚黄芪不同器官矿质元素含量

应用混合酸HNO₃-HClO₄ (4∶1) 在常压微沸条件下对膜荚黄芪根系及茎叶样品进行消解,采用原子吸收光谱法测定了膜荚黄芪不同器官即根及茎叶中五种人体必需矿质元素K,Fe,Zn,Mn和Cu含量,并对结果进行了统计分析与比较。该方法标准曲线相关系数为0.997 3～0.999 9, 加标回收率为92.88%～109.25%, 相对标准偏差(RSD,n=5) 为0.393 5%～3.175 2%。方法简单,结果可靠。结果显示,膜荚黄芪根及茎叶中5种矿质元素含量顺序均为K>Fe>Zn>Mn>Cu。膜荚黄芪不同器官矿质元素含量不同,根中富含Fe,Zn,Cu元素,根内Fe含量是茎叶的1.54倍。茎叶中也含有丰富的矿质元素,特别是K和Mn元素。茎叶中K含量是根的1.63倍,这与黄芪的药效相符合。试验结果将为研究矿质元素在黄芪植株中的分布以及矿质元素含量与黄芪药效相关性提供理论依据。     

荆芥不同器官在不同采收时间的ICP-AES矿质元素分析

各种矿质元素在荆芥各器官间贮藏差异。从矿质元素角度了解荆芥合理的药用部位组成以及收时间。应用ICP-AES技术,测定并分析了在不同采收时间,荆芥的不同器官矿质元素含量、累积量和比例。结果显示, 在不同采收时间,(1)荆芥穗中常量矿质元素K, P和微量矿质元素Cu含量最高,荆芥叶中常量元素Mg, Ca, Na和微量元素Fe, Mn, Zn含量最高。(2)荆芥不同器官所含常量元素中Ca和K含量最高,Na含量最低;所含微量元素中Fe含量最高,Mo含量最低。(3)在荆芥茎中,K∶P最高,而Zn∶Cu则为最低;Ca∶Mg和Fe∶Mn在荆芥穗中最低。(4)随着采收时间的推移,各元素在荆芥不同器官中的含量变化并不显著。荆芥茎中各矿质元素含量均较低; 从矿质元素含量的角度看,在合理的采收时间范围内,荆芥的质量受时间影响不显著。