Experimental Section Template and Acknowledgements
Acknowledgment of Iowa State University Support - Instrument Purchase
"Purchase of the Netzsch/Bruker TGA-DSC-MS/IR instrument used to obtain results included in this publication was supported by a coalition of ISU faculty, departments, colleges, centers, and the Office of the Vice President for Research.”
"Any opinions, findings, and conclusions or recommendations expressed in this material are those of the author(s) and do not necessarily reflect the views of the instrument purchase contributors.”
Acknowledgment of CIF Staff Assistance
"We wish to thank ISU Chemical Instrumentation Facility staff members <insert name(s) here> for training and assistance pertaining to the Netzsch TGA, DSC, and MS results and the Bruker IR results included in this publication."
Experimental Section
The Netzsch STA449 F1 Jupiter (Netzsch Instruments North America, LLC; 129 Middlesex Turnpike, Burlington, MA 01803) simultaneously provides TGA data (thermogravimetric analysis) and DSC data (differential scanning calorimetry) in one measurement. The furnace is programmable to 1500 C. In addition, the identity of gases evolved during the heating process can be determined by infrared and mass spec detection. The mass spectrometer is a Netzsch QMS 403 D Aeolos. The FTIR is a Bruker Tensor 37 (Bruker Optics Inc, 19 Fortune Drive, Billerica, MA 01821) equipped with a Bruker TGA-IR light pipe assembly. The system is fully automated and includes a 20-position sample carousel. Various purge, evacuation, and fill cycles are available to remove air and moisture from the sample area. A special oxygen-scrubbing device can also be incorporated when there is zero tolerance for O2 in the system.
The system also includes "Pulse TA" hardware to allow gases to be dosed in to calibrate the IR or MS responses, or to allow specific reactions at high temperature.
He and Ar purge gases used with the instrument are ultra-high purity UHP 300 from Airgas, Inc. Radnor Township, Pennsylvania. CO2, air, and O2 used in some measurements are regular purity, also from Airgas, Inc.
Four software packages are used with the system:
- Proteus - DSC/TGA control; acquisition and processing of DSC, TGA, and MS data
- Aeolos - MS control; triggered acquisition and limited processing of MS data
- OPUS - FTIR control; triggered acquisition and processing of IR data
- NIST - MS library and associated search software; processes MS spectra exported by Proteus
Complete measurement metadata is embedded in each file and can be viewed from within the Proteus software file browser. Similarly, metadata is embedded in each IR data file and can be viewed from within OPUS.