Instrumentation

Electrochemistry

Our electrochemistry workstations allow for extraction of both kinetics and thermodynamics for reactions involving electron transfer. We have three electrochemistry setups - 

Electrochemical workstation 1: Epsiolon Bipotentiostat & Pine RRDE

Electrochemical workstation 2: CHI650D Bipotentiostat & Pine RRDE

Electrochemical workstation 3: CHI600 potentiostat for mobile electrochemistry needs, such as in a fume hood or glovebox.

Glove-Boxes

Many of our compounds are air-and moisture sensitive. Glove boxes allow for working with these compounds in an inert atmosphere. We have three double glove boxes are under a nitrogen atmosphere containing freezers, cold wells, heated antechambers, fiber optic ports for UV-Vis/IR, Electrochemical ports, and plumbed for acquiring solvent internally. Two single glove boxes are also available, and feature electrochemical and optical ports.

High Temperature/Pressure Systems

We have three different reactors that allow us to study reactions under elevated pressures and temperatures.  Our Parr batch reactor system has six parallel batch reactors that can be simultaneously charged, heated, and stirred.  These are optimized for solution and slurry reactions.  We have a quartz flow reactor, optimized for gas-solid reactions that can be loaded entirely air-free and heated up to 1000oC. Our most recent addition is a system for running NMR reactions at high-pressure, which will allow us to study our reactions in-situ under pressures up to 2500 psig.

Optical Spectroscopy

Optical spectrometers allow for quantitative information concerning electronic transitions in the UV, Visible, and Infrared region. It is a key technique to monitor reactions optically, and quantify concentrations. We have multiple UV-Vis/IR spectrometers, with some coupled through fiber optics into N2 gloveboxes for air-free measurements.

Agilent 8452 (x2) – Diode-array spectrometers capable of measuring wavelengths from 200 to 1100 nm. Equipped with an 8-cuvette sample changer with the ability to perform kinetic measurements with multiple scans per second.

Cary 5000 (Agilent) – Measures wavelengths from 175 to 3300 nm. Holders include a probe for standard 1cm cuvettes, a solid-state holder, and fiber optic coupler. Coupled into the glovebox using fiber optics.

Cary 60 (Agilent)- Measures wavelengths from 175 to 1100 nm. Holders include a probe for standard 1cm cuvettes, a solid-state holder, and fiber optic coupler. Coupled into the glovebox using fiber optics.

Olis Clarity- Spectrometer designed to measure turbid samples, equipped with an NMR-tube adapter for air-sensitive samples.

Unisoku Uv-Vis- Cryostat adapted for Agilent 8453 spectrometers. Temperature capability from -80 to 100 oC easily adjusted with LN2.

Alpha IR – Compact IR spectrometer used in the glovebox. Equipped with ATR attachment and standard IR cell holder. Currently run with a CaF2 solution cell.

Photochemistry

We have two instruments capable of initiating photochemical reactions.

Laser Flash Photolysis (LFP): This technique is used to study reactive intermediates that are generated with a short laser pulse (~5 ns). Absorbance changes associated with reactive intermediates can be followed at a single wavelength on the nano-millisecond timescale. This allows us to study the kinetics of photoinitiated chemical reactions. We have a Luzchem LFP coupled with a Continuum Minilite Nd:YAG laser.

Photolysis Lamp: We have a 100W Hg lamp (XLC, inc) with UV-filters, used to initiate photochemical reactions.

Stopped Flow Kinetics

Stopped flow kinetics allow us to optically monitor fast chemical reactions.

Our single-mixing stopped flow (Olis, Inc.) is capable of rapidly mixing two reagents in <5 milliseconds and the rapid-scanning spectrophotometer can follow the absorption spectrum of the reaction by acquiring 1000 scans/second. The instrument is equipped with a temperature bath, allowing for temperature control between 10-60°C.

The double-mixing stopped flow (TgK Scientific) is capable of rapid mixing of three reagents in two different mixing steps. The absorption spectrum of the reaction is acquired with a diode array UV/VIS spectrophometer (500 scans/second), and a temperature bath controls the reaction temperature between -80°C and 60°C.