14.10.2016 Views

resolver

resolver

resolver

SHOW MORE
SHOW LESS

You also want an ePaper? Increase the reach of your titles

YUMPU automatically turns print PDFs into web optimized ePapers that Google loves.

Chapter 7 155<br />

measured under Ar. Atomic absorption spectroscopic (AAS) analysis for mixed-metal<br />

materials to determine Cu, and Pd contents were performed in the Microanalytical<br />

Laboratory of the Department of Analytical Chemistry at the Ruhr‐University Bochum by<br />

K. Bartholomäus. An AAS apparatus by Vario of type 6 (1998) was employed. Data<br />

interpretation was done by W. Zhang.<br />

7.1.8 Gas Sorption<br />

Experiments on sorption of CO2 (298 K) and H2 (77 K) as well as CO (298K) was performed<br />

with assistance of D. J. Xiao and D. Reed (the group of Prof. J. R. Long) at the Department<br />

of Chemistry in the University of California, Berkeley (USA). Part of the N2 sorption data<br />

were collected and interpreted by N. Arshadi at the laboratory of Industrial Chemistry<br />

department (Prof. Dr. M. Muhler) using a Quantachrome Autosorp-1 MP instrument. Most<br />

of N2 sorption data were collected and analyzed by W. Zhang.<br />

CO adsorption (298 K) and the majority of N2 (99.999%) sorption (77 K) measurements<br />

were performed using a Micromeritics 3Flex instrument. The N2 sorption isotherms of Ru-<br />

DEMOFs with defect 5-NH2-ip linker (3a-3d) samples were collected using a<br />

Quantachrome Autosorp-1 MP instrument, optimized protocols and N2 of 99.9995 %<br />

purity. Sorption isotherms of CO2 (298 K) and H2 (77 K) were conducted on a<br />

Micromeritics ASAP 2020 gas adsorption analyzer. The sample cells were cooled with a<br />

liquid nitrogen bath (77 K) or a liquid argon bath (87 K). For room temperature<br />

measurements (298 K) the sample cells were tempered in a water bath.<br />

Calculation of specific surface area and the isosteric heat of adsorption<br />

A method generated from BET theory, which was developed by Brunauer, Emmett, and<br />

Teller in 1938 as an extension of Langmuirs monolayer adsorption to a very simple model<br />

of multilayer physisorption, is commonly employed to calculate the specific surface area<br />

of a porous solid. This area value is usually determined from the data of physisorption<br />

nitrogen isotherms recorded at 77 K.<br />

The BET theory can be derived similarly to the Langmuir theory, but with the<br />

consideration of multilayered gas molecule adsorption, where it is not required for a layer<br />

to be completed before an upper layer formation starts. For the development of the BET<br />

method five assumptions have been made: i) The sample surface is homogeneous; ii)

Hooray! Your file is uploaded and ready to be published.

Saved successfully!

Ooh no, something went wrong!