TA4.2

SINTEF ChLab - In situ characterization of sold materials for CCS

Facility Location
City & country
Trondheim (Norway)
Description & contacts of the access provider
Legal name of organisation
SINTEF - Stiftelsen SINTEF
Infrastructure contact - Primary contact
Richard Blom
RICC contact - Secondary contact
Rune Bredesen
Facility Availability
Unit of access
Days
Availability per year
100 days
Expected duration of single experiment:
1-10 days

Solid and liquid state Nuclear Magnetic Resonance Spectroscopy (NMR).

For solid state NMR analyses a Bruker Avance III 500 MHz wide bore spectrometer equipped with four probes for different applications is available: Two MAS probes for solid samples, 3.2 and 4 mm. The 4 mm probe is useable up to about 300ºC and has a wide tuning range covering NMR frequencies for all elements. One high resolution probe for tissue samples, gels, and other liquid-solid dual phase samples. One flow probe for NMR studies of gases reacting with solids (in-situ). Useable up to 350ºC at atmospheric pressure. In addition a Bruker Avance III 400 MHz spectrometer is available for liquid samples.

In-situ powder X-ray diffraction (XRD)

A PANalytical Empyrean X-ray powder diffractometer equipped with an Anton Paar XRK 900 in situ cell can be used to get mechanistic information on sorbent function and possible degradation during operation. Using the in situ cell, measurements can be performed up to 900°C and 10 bars. A variety of gas compositions can be mixed by an automated gas feeding and mixing system (H2, CO2, CO, CH4, N2, H2O, and misc.). Additionally, the in situ cell can also be connected to a vacuum pump for measurements under vacuum. For experiments under gas flow, the gas will pass through the sample and the effluent gas can be analysed by IR or MS.

In-situ Diffuse Reflectance Infrared Spectroscopy (DRIFTS):

DRIFTS characterization can be carried out in various pre-mixed gas streams at temperatures from -80°C to 800°C. Such data typically gives information about chemical reactions taking place and the formation of surface groups within the pores of a solid. Information obtained from such experiments is often complementary to the information obtained from solid state NMR and powder XRD, but together the three methods may give a complete picture of the sample studied.

State of the art, uniqueness, & specific advantages

The major part of the infrastructure contains various experimental techniques used to investigate mechanistic aspects of liquid and solid sorbents and membranes. All techniques offered are modern and the results obtained are expected to be of high scientific quality. The experiments can be conducted at relevant conditions and the equipment is run and monitored by skilled technicians/scientists. The choice of the right experiment/experimental conditions for a specific test should be established through discussion with our experts. The main aim of such studies is to examine why materials work as they do which again will form the basis for the development of improved materials for a certain application. Typical studies might include: • Mechanistic investigation of solvent based sorption by NMR in the presence of CO2/ 13CO2 Solid State analysis of porous adsorbent during adsorption/desorption of CO2/ 13CO2 • Degrading studies of high temperature sorbents by powder XRD during multicycle testing at realistic conditions – chemical looping, carbonate looping • Etc.

Scientific Environment

We offer the above mentioned experiments to be carried out in one infrastructure. Skilled scientists and technicians are available to assist visiting partners. Also, a desk with internet access will be available during the stay. Beside the infrastructure itself are more standard laboratories where sample preparation can be performed are available. SINTEF Materials and Chemistry has implemented and maintains a quality management system which fulfils the requirements of the standard NS-EN ISO 9001:2008 within research and development within material technology, advanced materials and nanotechnology, applied chemistry and bio technology, oil and gas, and green energy and process industry.

selected publications

Cristina Perinu, Bjørnar Arstad, Aud. M. Bouzga, and Klaus-J. Jens (2014)
13C and 15N NMR Characterization of Amine Reactivity and Solvent Effects in CO2 Capture
J. Phys. Chem. B, 118, 10167−10174
Cristina Perinu, Bjørnar Arstad, Aud M. Bouzga, John A. Svendsen, and Klaus J. Jens (2014)
NMR-Based Carbamate Decomposition Constants of Linear Primary Alkanolamines for CO2 Capture
Ind. Eng. Chem. Res., 53, 14571−14578
Carlos A. Grande, Anna Lind, Ørnulv Vistad, and Duncan Akporiaye (2014)
Olefin–Paraffin Separation Using Calcium-ETS-4
Ind. Eng. Chem. Res., 53 (40), 15522–15530
Bjørnar Arstad, Anna Lind, Kari Anne Andreassen, Joanna Pierchala, Knut Thorshaug, Richard Blom (2014)
In-situ XRD studies of dolomite based CO2 sorbents
Energy Procedia, 63, 2082–2091
Carlos A. Grande, Vicente I. Águeda, Aud I. Spjelkavik, Richard Blom (2015)
An efficient recipe for formulation of metal-organic frameworks
Chem. Eng. Sci., 124, 154-158. DOI: 10.1016/j.ces.2014.06.048
Jennifer E. Readman, Anja Olafsen, Jens B. Smith, Richard Blom (2006)
Chemical looping combustion using NiO/NiAl2O4: Mechanisms and kinetics of redox reactions from insitu powder X-ray diffraction and TG experiments
Energy & Fuel, 20(4); 1382-1387
P. D. C. Dietzel, R. E. Johnsen, R. Blom, H. Fjellvåg (2008)
Structural changes and coordinatively unsaturated metal atoms on dehydration of honeycomb analogous microporous metal-organic frameworks
Chem. Eur. J, 14, 2389-2397