Here is the detailed manual, written in 2007, on the method we have been employing for the H2 and O2 evolution analysis while photochemically or electrochemically driving water reduction and/or oxidation to evolve H2 and/or O2. The technique was originally developped in 1993 in order to minimize the time-consuming worku-up on the manual measurements on each study. This is to save the time for measurement and to increase the time for reading and writing while working of each research. The method use continued flow of Ar or other inert gas at a accurately fixed rate (e.g., 10 mL/min) into the reaction vessel, from which the vent gas can be connected to the sampling loop attached to the valve for injection into a gas chromatograph. Other undamentals are also described, even though the most recent version of our system has further advanced by implementing the RS-232C talking between the control PC and a commertially available integrater for further improvement in accuracy of our quantitative analysis.
Perkin Elmer 2400II CHN AnalyzerThe detailed explanation about the CHN analysis using this instrument is given in Japanese.
The principle of CHN analysis is shortly explained in Japanese.
CSD (Cambridge Structural Database�jprovides a platform enabling researchers to make access to Cambridge Crystal Data Center�iCCDC�jwhich stores all the crystal data for organic and organometallic compounds that have been reoprted to date: http://www.protein.osaka-u.ac.jp/csd/csd.html. The manual written in Japanese for the users wroking at the Kyushu University Ito Campus is provided here.
Based on the use of some free softwares supplied at CP14�iCollaborative Computational Project Number 14, determination of lattice constants using CRYSFIRE, checking the validity of the results by CHECKCELL, and the subsequent refinment of lattice constants using POUDRIX are described (in Japanese only).
In this manual, instructions are given about how to determine the unit cell constants using freely available programs supplied at the CCP14 (Collaborative Computational Project Number 14) site. First, you should obtain your own powder X-ray diffraction data in a relatively good quality. This is the first thing you have to do by yourself. After that, convert your data into a file format which can be handled in CRYSFIRE (this predicts the unit cell parameters). The problem is that this works under the MS-DOS command prompt, which sounds a little bit unfamiliar to young students. So I gave some instructions to set this program accessible in your PC. Next, the results should be analyzed in CHECKCELL, in which space group information and other things can be predicted. After that, POUDRIX will help you to refine the cell constants by lthe east-squares method. Then you should move on to the Rietveld analysis in GSAS or other available packages.
Simple instruction written for the sake of teaching students (in Japanese only).
These two files are often provided to the students and group member for letting them practice how to work along with the crsytal-structure refinment using KenX and SHELXL under the Windows platform. The data have for a long time used even at the lectures for either undergraduates or graduates.
The interactive use of these three softwares lead to rapid and rational data processing of X-ray crystal data for research, which is described for the sake of promoting research in Sakai group (in Japanese only). These are not used in our recent study, even though it is still accessible in our group.