基于极少量采样的彩绘文物颜料成分分析

随着文物保护理念的提升,越来越提倡文物样品的无损或微损分析;同时由于文物样品的复杂性,对分析技术提出了更加严苛的要求.彩绘类文物的颜料分析研究,对其文物信息的提取,以及古代人类历史、社会、文化的研究和阐述具有重要作用.结合本研究组前期的研究成果,本研究提出了一种在极少量采样的情况下,分析研究文物颜料的方法,并用于榆林卧...     

漫反射光谱结合化学计量学方法无损分析彩绘文物颜料

为了对彩绘文物颜料进行无损判别分析,该文采集了12种彩绘常用颜料参考样品的漫反射光谱,根据光谱曲线外形将参考样品分为红黄色系及蓝绿色系两类。使用主成分分析(PCA)分别对两个色系参考样品的光谱数据集进行降维,抽提出最有代表性的3个主成分,利用成分得分散点图确认了颜料间的类间差异,并通过成分矩阵探讨了对该差异贡献率最高的光谱波长区间。在此基础上,采用线性判别分析(LDA)对PCA的分析结果进行建模,拟合判别函数并将其应用于2件颐和园仁寿殿上架彩画文物样品颜料的分析。基于样品判别得分散点图与各类别参考样品间的距离,判定文物使用的颜料分别为铁红和群青。研究表明,该文构建的判别函数能够准确区分颜料的种类,可用于彩绘文物样品的无损分析鉴别。文物样品的污染或老化可能会影响分析,需事先进行表面清理。     

TiO_2-K_2SiO_3无机涂层对空间材料Ag的防护行为研究

在微波电离型原子氮（AO）源地面模拟设备中对空间材料Ag及TiO_2- K_2SiO_3无机涂层进行原子氧剥蚀效应试验。用扫描电镜（SEM）、光电子能谱（ XPS）、红外光谱（FT-IR）、X射线衍射光谱（XRD）和LAMBDA-9分光光度计，对在 模拟原子氧（AO）环境中Ag及在其表面涂覆的无机涂层，所发生的侵蚀与防护作用 进行了表征研究。AO对Ag表现了较严重的侵蚀作用，原来光亮如镜的表面形貌变得 粗糙，且失去光泽。而所施用的TiO_2-K_2SiO_3无机涂层，经AO辐照后，表面形貌 则变化甚少。实验表明，该涂层对AO辐照有较强的防护效果、较好的空间稳定性（ AO辐照前后Δα ≈ 0.024），能阻止AO对基材的侵蚀。     

Preparation of α-Fe2O3 Nanofiber via Electrospinning Process

A thin PVA/FeCl3 composite fiber was prepared by using sol-gel processing and electrospinning techniques. A nanofiber of α-Fe2O3 with the diameter of 50-150 nm was obtained via high temperature calcination of the PVA/FeCl3 composite fiber. The material was characterized by infra-red (IR) spectroscopy, X-ray diffraction(XRD), and scanning electron microscopy(SEM). The results show that the fiber after the calcination at 700℃ was a pure α-Fe2O3 nanofiber.     

X射线荧光光谱法测定平炉渣中主成分

使用3080E3型X射线荧光光谱仪,采用粉末直接压片制样,研磨克服粉末样品的粒度效应,理论d系数法校正基体效应的方法,建立了平炉渣样品中TFe、SiO2、MgO、Al2O3、CaO、MnO、TiO2、P2O5组分的快速测定方法。研究了制样条件,用内控标样作标准曲线,分析结果的相对标准偏差为0．23％～3．17％,满足日常分析的要求。     

X射线荧光光谱法测定垃圾焚烧炉渣中主要成分

使用X射线荧光光谱仪,采用粉末直接压片制样,以研磨的方式克服粉末样品的粒度效应,理论α系数法校正基体效应,建立了垃圾焚烧炉渣样品中SiO2、Fe2O3、MgO、Al2O3、CaO、K2O、TiO2、P2O5八组分的分析方法.用标准化法进行强度漂移校正,用内控标样制做校准曲线,测定结果的精密度和准确度可以满足日常分析要求.     

北京颐和园古建筑上红色颜料的分析研究

本文利用X射线荧光(XRF)、X射线衍射(XRD)、光学显微镜、扫描电镜能谱(SEM-EDX)等多种仪器组合技术,对取自北京颐和园古建筑上的13个样品的23个红色颜料点进行了分析测试。研究结果表明:红色颜料大多为赤铁矿,有少量是铅丹,朱砂仅见于一个文物样品上,另有一部分是有机染料。赤铁矿和有机染料多存在于表层颜料中,而铅丹都作打底之用。该工作提供了古代建筑油饰彩画颜料分析的技术方法,对了解中国古代建筑彩画特别是官式彩画的材料组成、制作工艺和修复保护具有重要意义。     

三门峡虢季墓遗址盐害分析与调查

针对三门峡虢季墓遗址部分区域存在起甲、泛白、疱疹等由可溶盐引起的病害,在其遗址不同部位取样进行土遗址本体含盐分析.取样区域包括虢季墓、梁姬墓和近代墓遗址.采用X射线荧光光谱(XRF)和离子色谱(IC)分析所取样品的可溶盐成分、含量及可溶盐成盐元素在土遗址中的成盐规律.采用电子能谱(XPS)和X射线衍射(XRD)分析样品的物相组成及盐分状态,扫描电子显微镜/能谱(SEM/EDS)进一步考察含盐土质的颗粒组成、微观形貌等.结果表明:虢季墓取样区域所含盐分主要为Na_2SO_4、CaCO_3和少量的其他盐分如CaCl_2、KNO_3和NaCl等.靠近地面部位所取样品盐分含量高于其他部位,盐害表现更为明显.梁姬墓取样区域总盐分含量略高于虢季墓与近代墓,硝酸盐含量较高.而近代墓遗址可溶盐盐分含量略低,盐害不明显.在不同取样点可溶盐含量有所差异,但在邻近区域,其成盐具有一定规律性,这一点对于遗址基体中盐害的深入研究与防治具有重要意义.     

新型中微孔复合分子筛的研究

报道一种中微孔复合分子筛Y/MCM-41的研究，通过XRD，SEM，IR，BET，水热 老化等手段对复合材料进行了表征。研究结果表明，复合分子筛与机械混合物存在 明显差别，复合分子筛中孔结构的水热稳定性优于普通合成的纯中孔分子筛。     

应用先进光谱技术研究无机离子的环境界面化学

发生在环境界面的吸附-解吸和氧化-还原等反应对于污染物在环境介质间传输、转化以及归趋起着重要的调控作用。传统的研究方法虽然可以在实验室模拟并进而描述污染物环境界面过程,但是不能揭示界面反应机制,限制了对污染物环境界面行为的认识。近二十年来,各种谱学技术(例如X射线吸收精细结构和傅里叶红外光谱等)应用于环境界面反应的研究,推动了这一领域研究的发展,特别是在分子水平研究污染物的环境界面过程。通过现代光/波谱技术原位分析,可以实时获取界面反应的定量与结构信息,从而更准确地判断反应机制,极大促进了对污染物在多介质环境界面迁移转化规律的认识。本文将在概述环境界面化学反应的基础上,针对无机离子在环境界面的反应过程,重点介绍几种关键光/波谱技术(X射线吸收精细结构光谱、傅里叶红外光谱、拉曼光谱、核磁共振谱和穆斯堡尔谱等)在环境界面化学研究中的应用,并展望其在环境界面过程研究中的应用前景。     

Spectrum Analysis of the Colored Pottery Figurines from Yangling Tombs of the Han Dynasty

ABSTRACT

The analysis of the colored pottery figurines from Yangling Tombs of the Han Dynasty was realized by X-ray diffraction, emission spectroscopy, infrared spectroscopy, X-ray fluorescence and fiber optics reflectance spectroscopy (FORS). Consequent results showed that the colored components were respectively mercuric(II) sulphide, ferric (III) oxide, and carbon, among which mercuric(II) sulphide was an artificial pigment.     

Non-invasive surface analysis of ancient bronze arrowheads with scanning electron microscopy and X-ray powder diffractometry

In this research, surfaces of eight ancient metal arrowheads were investigated regarding chemical composition, homogeneity, and products of corrosion. To perform that, two nondestructive techniques were applied: Scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS), and X-ray powder diffractometry (XRPD). Importantly, both methods did not require sampling, cutting, nor significant cleaning of the historical artifacts, which made the measurements not only nondestructive but noninvasive too. SEM-EDS measurements provided information on the morphology and elemental composition of the surfaces of the studied objects as well as the distribution of chemical elements on the surfaces and supported crystalline phase analysis. It was revealed that the arrowheads were cast of tin bronze, but some of them contained high amounts of lead and admixtures of antimony and arsenic while copper and tin oxides and lead carbonates were found as the major corrosion products. In some cases, distribution of elements in the surface exhibited serious nonhomogeneity, probably resulting from limited solubility of the casting metals and degradation processes. Based on the obtained results, authenticity and declared provenience of the arrowheads were assessed in reference to the characteristics of similar objects described in literature.     

Analysis of the Chemical Composition of Red Pigments and Inks for the Characterization and Differentiation of Contemporary Prints

Prints are one of the most popular artistic forms. They consist of an original matrix that is printed on a paper support. The stamps are part of a series, and each series is composed of a particular number of prints. Many contemporary prints are made using oil inks and synthetic pigments (reds and yellows). Inks are mainly composed of pigments (organic or inorganic) and a binding medium. The analysis of inks has the potential to facilitate and complement the identification of stamps of different origins.

Fourier transform infrared spectroscopy (FTIR) and Scanning Electron Microscopy-Energy Dispersive X-ray (SEM-EDX) are techniques that are typically available in museums and centers related to the study of works of art. Both can be classified as micro-destructive and provide complementary information about the organic and some inorganic compounds (FTIR), and the elemental composition (SEM-EDX). In this article, the two techniques were used to analyze the composition of red ink in prints. As a result of these analyses, it was possible to distinguish among nearly all of the pigments and inks, indicating that the composition of the red ink can be reliably used to differentiate between stamps of different origins in a series of prints.     

Chromatographic,Microscopic, and Spectroscopic Characterization of a Wooden Architectural Painting from the Summer Palace,Beijing, China

The wooden construction painting is a type of an ancient decorative art on Chinese ancient structures. Comprehensive reports concerning the composition of these materials are rather limited. Here multiple analytical methods were applied to systematically explore the morphology and materials. Several paintings were characterized using a morphological microscope. Scanning electron microscopy–energy dispersive spectrometry (SEM-EDS), X-ray fluorescence (XRF), and X-ray diffraction (XRD) detected emerald green and ultramarine in the paint layers. Gas chromatography–mass spectrometry (GC-MS) indicated that the binding medium in the first layer was composed of blood. Our study helps to comprehensively understand the preparation of the wooden construction paintings in the renowned Summer Palace and provide a scientific basis for its restoration and related archeology work.     

铜铝合金中γ_2相沉淀的分析电镜研究

Cu-12.7(wt)%Al合金从900℃高温淬至365℃～500℃温度范围等温不同时间(30秒至15分钟)的试样中形成了大量树枝状的γ_2相沉淀粒子。应用配有X线能谱仪(XEDS)和电子能量损失谱仪(EELS)的分析电子显微镜(JEOL JEM-2000FX型)对上还试样研究,结果表明:这些γ_2相粒子具有富铝的“核心”,长大到粒子线度大于约800nm后以不稳定方式生长成“花朵”状。生长过程中伴随着溶质元素Al由基体向γ_2相内的富集。而且在γ_2相粒子内部呈现出Spinodal分解组织的形貌特征,表明γ_2粒子内形成了化学成分调幅。EELS分析表明试样含氧。     

Investigation of roman age pigments found on pottery fragments

This work deals with the study of the physico-chemical characteristics of pigments found on pottery fragments from an excavation in Vicenza (Contrà Pedemuro S. Biagio). The examined pigments were: a blue colour on a terracotta fragment; an olive green on a black pot bottom; yellow traces on a red depurated terracotta; an olive green plate bottom with an amaranth “a fresco” test; a deep red on a depurated terracotta; a white trace, again on a depurated terracotta. The techniques used were optical microscopy, scanning electron microscopy (SEM), equipped with an energy dispresive (EDS) microanalysis detector, X-ray powder diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. Most of those techniques were non-destructive and able to provide the required results. All the pigments belonged to the group of basic colours, we did not find “precious” pigments. They have many similarities to those discovered in other European sites in France and Switzerland, witnessing the active trading exchange in which X^a Regio, Venetia et Histria played an important role.     

单一颗粒物扫描电镜能谱定量分析方法研究

采用实测标准样品、实际样品与模拟样品相结合的方法,对文献中报导的用于定量分析单一颗粒物化学组成的Casino和Quanta计算程序进行了考察和比较。计算结果表明,在校正颗粒物粒径效应时,Casino程序显示了良好效果。Quanta程序在计算沙尘颗粒物中常见的Na、Mg、A l、S i、P、S、K、Ca、Ti、Fe等元素含量时,取得和Casino程序基本一致结果。     

X射线晶体学结合电子晶体学在复杂无机晶体结构解析中的应用

自然界中的材料,比如无机材料,有机材料,生物材料等等,均有其独特的物理和化学性质。而材料的性能又与材料的结构息息相关,只有充分了解了材料的结构,才能更加深入的研究材料性质。因此,材料结构的确定在化学、物理、生物等学科中的显得尤为重要。X射线晶体学作为传统的结构解析技术仍然是目前最重要的结构解析手段,但是对于复杂结构,X射线衍射晶体学解析结构也存在一些不足,往往需要其他技术手段相补充才能完成复杂结构的结构解析。电子晶体学虽然起步比X射线晶体学晚,但是,经过近几十年的发展,已经是结构解析领域一个非常重要的手段。本文将主要介绍X射线晶体学结合电子晶体学在复杂无机晶体结构解析中的应用。     

Chemical Liquid Phase Deposition of Thin Aluminum Oxide Films

Introduction Inorganic oxide films have attracted a lot of interest in the last several decades. Among them, silicon dioxide films are widely used in modern microelectronics, optics and mechanics. This material has been grown by various methods including thermal oxidation, chemical vapor phase deposition, plasma-enhanced chemical vapor phase deposition, and so on.1,2 Recently, Nagayama et al.3 have reported that SiO2 thin films could be produced by a new chemical method of liquid phase depos…     

Chemical Composition and Thermogravimetric Behaviors of Glanded and Glandless Cottonseed Kernels

Common “glanded” (Gd) cottonseeds contain the toxic compound gossypol that restricts human consumption of the derived products. The “glandless” (Gl) cottonseeds of a new cotton variety, in contrast, show a trace gossypol content, indicating the great potential of cottonseed for agro-food applications. This work comparatively evaluated the chemical composition and thermogravimetric behaviors of the two types of cottonseed kernels. In contrast to the high gossypol content (3.75 g kg⁻¹) observed in Gd kernels, the gossypol level detected in Gl kernels was only 0.06 g kg⁻¹, meeting the FDA’s criteria as human food. While the gossypol gland dots in Gd kernels were visually observed, scanning electron microcopy was not able to distinguish the microstructural difference between ground Gd and Gl samples. Chemical analysis and Fourier transform infrared (FTIR) spectroscopy showed that Gl kernels and Gd kernels had similar chemical components and mineral contents, but the former was slightly higher in protein, starch, and phosphorus contents. Thermogravimetric (TG) processes of both kernels and their residues after hexane and ethanol extraction were based on three stages of drying, de-volatilization, and char formation. TG-FTIR analysis revealed apparent spectral differences between Gd and Gl samples, as well as between raw and extracted cottonseed kernel samples, indicating that some components in Gd kernels were more susceptible to thermal decomposition than Gl kernels. The TG and TG-FTIR observations suggested that the Gl kernels could be heat treated (e.g., frying and roasting) at an optimal temperature of 140–150 °C for food applications. On the other hand, optimal pyrolysis temperatures would be much higher (350–500 °C) for Gd cottonseed and its defatted residues for non-food bio-oil and biochar production. The findings from this research enhance the potential utilization of Gd and Gl cottonseed kernels for food applications.