Published: June 8th, 2016
Modern high resolution X-ray powder diffraction (XRPD) in the laboratory is used as an efficient tool to determine crystal structures of long-known corrosion products on historic objects.
The crystal structure determination and refinement process of corrosion products on historic art objects using laboratory high-resolution X-ray powder diffraction (XRPD) is presented in detail via two case studies.
The first material under investigation was sodium copper formate hydroxide oxide hydrate, Cu4Na4O(HCOO)8(OH)2∙4H2O (sample 1) which forms on soda glass/copper alloy composite historic objects (e.g., enamels) in museum collections, exposed to formaldehyde and formic acid emitted from wooden storage cabinets, adhesives, etc. This degradation phenomenon has recently been characterized as "glass induced metal corrosion".
For the second case study, thecotrichite, Ca3(CH3COO)3Cl(NO3)2∙6H2O (sample 2), was chosen, which is an efflorescent salt forming needlelike crystallites on tiles and limestone objects which are stored in wooden cabinets and display cases. In this case, the wood acts as source for acetic acid which reacts with soluble chloride and nitrate salts from the artifact or its environment.
The knowledge of the geometrical structure helps conservation science to better understand production and decay reactions and to allow for full quantitative analysis in the frequent case of mixtures.
Conservation science applies scientific (often chemical) methods in the conservation of artifacts. This includes investigations of the production of artifacts ('technical art history': How was it made at that time?) and their decay pathways as a prerequisite to develop proper conservation treatments. Oftentimes these studies deal with metal organic salts like carbonates, formates and acetates. Some of them have been deliberately manufactured using suitable compounds (e.g., vinegar), others derive from deterioration reactions with the atmosphere (carbon dioxide or carbonyl compounds from indoor air pollution)1. As a matter of fact, the cryst....
1. Sample Preparation
High resolution XRPD was used to determine the previously unknown crystal structures of two long-known corrosion products on historic objects. The samples were taken from two museum objects and carefully grinded before they were sealed in transmission and capillary sample holders (Figures 6, 7). Standard measurements using a state of the art laboratory high resolution powder diffractometer in transmission and Debye-Scherrer geometry using monochromatic X-rays were perform.......
XRPD is a suitable technique for conservation research as it is non-destructive, fast and easy-to-use. XRPD data can be used in routine qualitative analysis, owing to the fact that the powder pattern is a fingerprint signature to the corresponding crystal structure. The biggest advantage of XRPD over other analytic techniques is the ability of performing simultaneous qualitative and quantitative analysis of crystalline constituents in mixtures by using the Rietveld refinement method5. Moreover, the presence of.......
The authors gratefully acknowledge Ms. Christine Stefani for performing the XRPD measurements. Marian Schüch and Rebekka Kuiter (State Academy of Art and Design Stuttgart) are acknowledged for the pictures of the tile (Fig. 7).....
|Stoe & Cie GmbH
|Mythen 1-K (450 μm)
|Position Sensitive Detector
|Mark tube borosilicate glass No. 50, 0.5 mm diameter
|Low absorbing capillaries
|Bruker AXS Advanced X-ray Solutions GmbH
|Powder Diffraction Evaluation Software
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