Instrumentation – Tremaine Research Group

The Tremaine Group laboratories are located in the McNaughton Building and the Science Complex.

We have several labs with a wide variety of equipment:

Contents

1 1. Raman Spectroscopy Lab:
2 2. High Temperature & Pressure Laboratory:
3 3. Low Temperature & Pressure / Wet Chem Laboratory:
4 4. Hydrogen Laboratory:
5 5. U of G facilities:

1. Raman Spectroscopy Lab:

The LabRAM HR 800 is custom built and is a high resolution Raman spectrometer instrument with an integrated Macrochamber and Confocal Microscope for high spatial resolution imaging. The spectrograph has a focal length of 800 mm and has interchangeable gratings (1800, 1200, 600 and 300 grooves / mm) that provide different degrees of dispersion and spectral resolution. The bench top spectrometer was initially setup for the excitation wavelength 633 nm He:Ne 20 mW laser and also had two externally mounted lasers; a 785 nm (NIR) and 532nm Nd:Yag laser. This state-of-the-art instrument Macrochamber allows for polarisation experiments, 90° and 180°. Custom made cells have been built to fit to the Macrochamber and Microscope allowing measurements of aqueous complexes and electrolytes up to and including super critical water temperatures and pressures, yielding data for analysis of thermodynamic properties.

The LabRAM HR 800 Micro_and_Macrochamber — ^{The LabRAM HR 800 Raman spectrometer instrument with an integrated Macrochamber and Confocal Microscope for high spatial resolution imaging.}

Inside Raman macrochamber — _{This state-of-the-art instrument Macrochamber is setup for polarisation experiments; 90° and 180°. Custom made cells have been built to fit to the Macrochamber (and Microscope).}

2. High Temperature & Pressure Laboratory:

High Temperature/Pressure Flow-through AC electrical conductance instrumentation: This is a unique piece of equipment we received from Prof. Robert H. Wood, University of Delaware. It allows rapid and accurate electrical conductance measurements of ionic aqueous species from concentration as low as 10^-5 mol kg^-1 and up to 0.2 mol kg^-1. Experiments can be carried out from 25°C to 400°C and up to 28 MPa. Analysis of the electrical conductance measurements leads to the molar conductivity of the species in solution and to the ionization constants.

Student using conductivity apparatus — ^{High T/P flow-through AC electrical conductance}

Calorimetry and Densitometry: The Setaram C-80 uses the latest evolution of the Calvet Design calorimetric detector, in which a sample and reference cell are totally surrounded by an array of thermocouple detectors allowing for the measurement of all heat evolved (or adsorbed) including radiation, convection or conduction, thus permitting very high precision measurements.

Setaram C80 Calvet Calorimeter — *^{Setaram C-80 Calvet Calorimeter}*

Two Sodev CP-C heat capacity microcalorimeters and 03-D densimeters measure apparent molar properties of aqueous electrolytes, organic solutes and complexes from 5 to 55°C for extrapolation to infinite dilution. CSC 4400 twin cell heat-flux high pressure flow calorimeter measures heats of solution and heats of mixing to determine enthalpies of formation of solids and aqueous species near 25°C. CSC 4100 differential scanning microcalorimeter, used to determine excess molar heat capacities of mixtures from 0 to 200°C.

Prof. Tremaine with densimeter — ^{Prof. Tremaine’s high T&P Lab}

High temperature vibrating tube densitometers, one stainless steel one platinum, measure apparent molar volumes of aqueous species from 50 to 325°C and pressures up to 300 bar (Xiao et al., 1997).

Student with densimeter — ^{Vibrating tube densimeter}

UV-Vis Spectroscopy: Two Cary 50 UV-visible spectrophotometers 220-1100nm with fibre optics, used with high pressure titanium and platinum flow cells with sapphire windows to obtain spectra at temperatures up to 350°C and pressures up to 300 bar.

Student with Cary 50 Spectrophotometer with Flow Cell — *^{Cary 50 Spectrophotometer with Flow Cell}*

Parr 4561 hastelloy and zircalloy stirred pressure-vessel cells are used for pH titrations and solubility studies up to 350°C.

Student with Parr reactor — *^{Parr Pressure Vessels}*

3. Low Temperature & Pressure / Wet Chem Laboratory:

Calorimetry:

*^{Student with TA NanoDSC III Calorimeter}*

The Calorimetry Sciences Corporation (now acquired by TA) 6300 Nano differential scanning calorimeter (DSC) III with gold cylindrical cells and the TA NanoDSC 602000.901 with capillary platinum cells scan through a range of temperatures and measure the power required to maintain solutions in twin cells at the same temperature. The difference in power can be used to determine very precise heat capacities for apparent molar heat capacities at temperatures from -10°C to 130°C and pressures up to 6 atmg.

The TA Nano isothermal titration calorimeter (ITC) 601001.901 with gold cylindrical cells has a working range of 2 C to 80 C at ambient pressure. The measured rate of heat release (or absorption) can is used to calculate the enthalpy change of the titration reaction.

Densimetry:

The Anton Parr DMA 5000 can measure apparent molar properties from 5 to 90°C.

The Anton Paar DMA 4200 M, a hastelloy vibrating U-tube densimeter, can measure accurate solution densities required for apparent molar volumes at temperatures of -10°C to +200°C and up to pressures of 500 bar.

4. Hydrogen Laboratory:

We also have shared space in the hydrogen/high pressure lab together with Prof. Marcel Schlaf. This facility was specially designed for work with hydrogen and includes ‘walk in’ fumehoods and state-of-the-art safety features.

5. U of G facilities:

There additional facilities of interest on campus which are accessible to U of G researchers:

NMR Centre