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Overview
The Peter A. Rock Thermochemistry Laboratory, supervised by A. Navrotsky, is a unique laboratory
for the determination of thermodynamic properties by calorimetric
techniques. It occupies over 5000 square feet of space on the fourth
floor of the Chemistry Annex building. Though used primarily by
Navrotsky's group, it is open to collaborative research and is
a major resource for NEAT (Nanomaterials in the Environment, Agriculture,
and Technology).
Click here to open a copy of the laboratory brochure in a new window.
The Laboratory Detailed
Calorimeters:
The
heart of the Peter A. Rock Thermochemistry Laboratory is the collection of both custom
built Calvet micro-calorimeters for solution calorimetry using molten
oxide solvents and commercial calorimeters. The following is available:
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4
Calvet-type, high temperature, custom-built, calorimeters for
solution and reaction calorimetry at 700° to 800° C.
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1
Setaram HT-1500 calorimeter for transposed-temperature-drop,
direct melting, and scanning experiments at 600° to1500° C.
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1
Setaram 9600 calorimeter system for heat capacities, heats of
reaction, and large mass thermogravimetry (TGA) at 700° to 1500° C.
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1
Setaram Setsys 2400 calorimeter system for heats of reaction,
thermogravimetry (TGA), and thermal mechanical analysis (TMA)
at 25° to 2400° C.
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1
C-80 and 1 Setaram BT2.15 Calvet-type calorimeter for analysis between –150° to 300° C and 2 CSC 4400 Isothermal Microcalorimeters for
analysis between –40° to 100° C. These very sensitive instruments
are used for heat of solution experiments in aqueous and organic
solvents, for gas adsorption studies, and for in situ synthesis
calorimetry.
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3
Setaram DSC 111 TG systems for differential scanning calorimetry
and thermogravimetry (TGA) at 50° to 700° C. Two of the
DSC 111s can be combined with the Micromeritics
ASAP2020 gas sorption analyzers so that heat of gas absorption
and surface area can be determined simultaneously.
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1
Netzsch 404 System with a low temperature cell (-50° to 250°
C) and a high temperature cell (40° - 1500° C) for differential
scanning calorimetry (DSC).
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1
Netzsch 409 DSC/DTA and 1 Netzsch 449 DSC/DTA thermal analysis
systems for thermogravimetry (TGA), differential scanning calorimetry
(DSC), and evolved gas analysis (EGA) from 40° and 1500° C . Qualitative gas analysis
is done by mass spectrometry (MS) and quantitative gas analysis by Fourier transform infrared (FTIR) spectroscopy.
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comprehensive collection of thermodynamic data compilations and
software (Phase Equilibria Database, FACTSage, and HSC Chemistry) for calculating
thermodynamic parameters.
Sample
Synthesis and Preparation:
When high quality samples are not available through collaboration with
other research groups, the following equipment is available for synthesis
by group members.
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High
temperature furnaces, a hydrothermal synthesis bench, balances,
gas flow systems, and other ancillary equipment.
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2
glove boxes for air and moisture sensitive samples.
- We are currently constructing a laser ablation synthesis system for nanoparticle synthesis under conditions that exclude water, wiht sample handling capabilities to maintain such dry samples all the way into the drop solution calorimetric experiments.
Characterization:
For thermodynamic data to be of use, the samples used to generate
the data must be well characterized both compositionally and structurally.
These instruments are used primarily by members of the Thermochemistry
Group for specialized studies and are not available routine sample
characterization that can be done elsewhere on campus.
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An
INEL x-ray diffractometer, operated jointly with S.M. Kauzlarich (Professor
of Chemistry), has a position-sensitive detector (PSD) covering
120°. A variety of sample holders (flat plate, capillary,
rotating for both reflective and transmission modes, and a holder
for air sensitive samples) are available. A heating stage (30° to 1200° C) is also available. Complete diffraction patterns
can be obtained in 1 to 10 minutes.
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A Bruker D8 Advance x-ray diffractometer with a variety of interchangable components. The instrument;s capabilities include rapid analysis for qualitative phase identification includeing samples that fluoresce in copper radiation, high resolution data for lattice parameter and Riedtveld analysis and small angle scattering data for particle size analysis. The parallel geometry configuration allows irregular sample surfaces to be analyzed.
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wide range of software for processing and analyzing diffraction
data, (JADE, TOPAS3, EVA, WINDIF, GSAS, and others), and major crystallographic
databases (PDF, ICSD, and CCDC) are available. There is also
software to simulate diffraction patterns and to visualize crystal
models (jPWD and CrystalMaker) and to optimize crystal structures
(Material Studio and Cerius 2 molecular modeling packages).
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John
Neil, a staff member in Navrotsky's group, has extensive diffraction
experience and is in charge of these instruments.
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Bruker Equinox 55 FTIR spectrometer for mid- and near-IR range
analysis. Transmission and reflective sample holders are available
as well as a gas cell.
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Belzers MSC 200 quadrapole mass spectrometer for identifying
gaseous decomposition products.
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Two
Micromeritics ASAP2020 gas sorption analyzers for determining
surface area, porosity, pore size and pore distributions of zeolites
and nanomaterials.
Other
Facilities:
Because of the complexities of modern instrumentation and the details
needed to describe a sample, it is not feasible for one group to have
and maintain all the instruments needed. The following lists the outside
facilities routinely used to further our studies.
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Access
to low-temperature, adiabatic, calorimeters is available through
our collaboration with Brian Woodfield’s group at Brigham
Young University.
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Access
to 2 piston-cylinder high-pressure apparatus for synthesis between
25° and 1400° C and between 5 and 25 kbars at the UC Davis
Geology Department.
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Access
to synchrotron and neutron diffractometers can be arranged at
several national facilities.
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The
FEI XL30-SFEG, high resolution, Scanning Electron Microscope
(SEM) at the Materials Science Central Facilities, UC Davis.
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JEOL JEM-2500SE, High Resolution Transmission Electron Microscope
(HRTEM), a Philips CM-12 Trans-mission Electron Microscope (TEM)
and the Electron Microscopy Specimen Prep Lab at the Materials
Science Central Facilities, UC Davis.
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Access
to the National Center for Electron Microscopy (NCM) at the Lawerence
Berkeley National Laboratory.
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400
and 500 MHz solid state Nuclear Magnetic Resonance (NMR) spectrometers
at UC Davis.
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Cameca
SXC-100 electron microprobe with staff support at the UC Davis
Geology Department’s Electron
Microprobe Lab.
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