Volume 31(2) - Summer 2015

I would like to take this opportunity to address the recent acquisition of Agilent’s XRD business by Rigaku Corporation and the subsequent creation of a new combined Rigaku Oxford Diffraction single crystal group.

Our decision to make this acquisition was based on a number of things, but key among those reasons was the synergy that we recognized between the two groups. Rigaku’s strength in the structural biology market and Oxford Diffraction’s strength in the field of chemical crystallography will be combined to create a stronger overall single crystal organization. As the boundaries between chemical crystallography and macromolecular crystallography continue to be reduced, synergistic use of our combined technologies will lead to better products for both sets of customers.

We felt it was particularly important to bring back the name of “Oxford Diffraction” as it is synonymous with innovative, leading edge hardware and software that has greatly expanded the capabilities of chemical crystallography over the last 15 years. During the same period, Rigaku was advancing the development of X-ray source technology and multilayer optics as applied to the expanded number of life science and structural genomics projects around the world. Thus our new name of “Rigaku Oxford Diffraction” symbolizes our continued commitment to further advance instrumentation technologies for all fields of single crystal analysis.

We now have factories in Japan and Poland that are involved in Rigaku Oxford Diffraction instrument production and single crystal products from these factories will be branded in the same way. Our R&D groups have already started working together and the overall integration process is progressing faster than we expected.

SmartLab Studio II is an integrated X-ray diffraction software package for SmartLab 3, an automated multipurpose X-ray diffractometer. The package covers the full spectrum of operations required for X-ray diffraction analysis, including measurement, analysis, data display and reporting on a single platform. SmartLab Studio II is designed from the ground up with ease-of-use in mind, so that even novice users are able to quickly master their X-ray diffraction

Thermo Mass Photo is a thermogravimetry-differential thermal analysis-mass spectrometry (TG-DTA-MS) instrument and a main product in the lineup of Rigaku’s evolved gas analytical systems. It consists of thermogravimetry-differential thermal analysis (TG-DTA) and photoionization mass spectrometry (PIMS) equipped with a skimmer-type interface. Weight change, endothermic or exothermic phenomena, and evolved gases can be analyzed simultaneously. Therefore, Thermo Mass Photo is considered a promising analytical tool for fundamental research, qualification control, and development of new materials.

Thermo Mass Photo has been optimized as the “all-in-one” package consisting of TG-DTA and MS providing a small footprint, safety and easymaintenance. The software supports an easy operation with a guidance function. A complicated multi-steps reaction accompanied with various evolved gases can be investigated by the combination of controlled-rate TG (CRTG) and PIMS. In addition, the compact automatic sample changer called Smart Loader can contribute to the throughput enhancement.

Hyphenated methodology combined with thermal analysis and other analysis methods has been widely applied to the investigation of complex phenomena. Thermo Mass Photo is a thermogravimetry-differential thermal analysis-mass spectrometry (TG-DTA-MS) instrument, which is one of the most widespread hyphenated systems, and a main product in the lineup of Rigaku’s evolved gas analytical systems. It consists of thermogravimetry-differential thermal analysis (TG-DTA) and photoionization mass spectrometry (PIMS) equipped with a unique skimmer-type interface. The simultaneous analysis of weight changes, endothermic or exothermic phenomena, and evolved gases can be applied to fundamental research, quality control, and development of new materials, etc. In this article, we have introduced several applications of the thermal decompositions of the polymers, minerals, and pharmaceuticals by Thermo Mass Photo.

For the analysis of powders by XRF, sample inhomogeneity due to segregation, grain size and mineralogical effects influence X-ray intensity and can cause analysis errors. It is therefore recommended to analyze powder samples after fine pulverizing as described in “Sample Preparation for X-ray Fluorescence Analysis II. Pulverizing methods of powder sample.” However, when inhomogeneity can not be sufficiently removed by pulverization and more accurate analysis is required, fusion bead method is advisable.

The fusion bead method first established in the 1950s, has since progressed such that it is not only applicable to powders as oxides but also to non-oxides such as metals, carbides, sulfides which had previously been considered to be difficult. Characteristics of the fusion bead method are that (a) analysis error due to grain size and mineralogical effects can be removed, (b) matrix effect is reduced due to dilution, (c) standard samples can be prepared by mixing of reagents. Characteristics of fusion bead and pressed powder methods are compared.

In this article, general preparation methods, equipment, reagents and other important considerations for powders with typical grain size and drying conditions are described. If analysis must be performed in accordance to a specific standard test method, adhere to its prescribed conditions. In a following issue on fusion beads, various applications such as for ferroalloy, silicon carbide and copper concentrate samples will be reported.

Among the various analysis techniques, single crystal X-ray structure analysis can be regarded as the most effective analysis technique for acquiring knowledge about the 3-dimensional configuration of molecules. However, in single crystal X-ray structure analysis, there is also a major problem in that measurement cannot be done if the target sample will not form a single crystal. In addition, even if a crystal is obtained, it is often a twin.

Previously, if the crystal was a twin, the usual approach was to examine the crystallization conditions again, and repeat the process a number of times until a single crystal was obtained. However, due to the development of equipment and software in recent years, it has become possible to carry out a certain amount of analysis even if the crystal is twinning. Therefore, this paper discusses the steps for this procedure, from the method of determining twinning to the method of refinement.

There are two basic objectives in scientific analysis of tangible cultural properties: appraisal of authenticity, and investigation of materials for purposes of preservation or restoration. Targets of these analyses are buildings, sculptures, paintings, craft objects, old documents and so on.

Many art and craft items have become the objects of speculation by collectors throughout the world. As a result, the field has an aspect that drives incidents of theft and forgery of and damage to works by improper restoration. In the case of paintings, it is not unusual even with famous works for the artist himself to make changes in the underlying sketch or picture composition prior to completion, or for a third party to work on the picture after the artist has died. One such example is the “Madonna del Granduca”(1505) by Raphael. This image of the Madonna and Child, which was publicly exhibited in Japan for the first time in March 2013, is known for having a jet-black background—a feature not seen in other works by Raphael. During the exhibition of this masterpiece of the Madonna and Child painting genre, the results of scientific analysis of the jet-black area were also presented. An X-ray image taken in 1984 showed that Raphael had originally painted a different scene in the background, but that scene had been covered with jet-black paint by someone in a later generation.

To determine authenticity by analyzing the painting process and the time and place where the materials were produced, it is essential not only to carry out verification by humanities or social sciences, but also to analyze based on the knowledge of natural science using the results available from X-ray equipment.