The SFU Chemistry Dept. is exceptionally well equipped with larger shared equipment, including multiple NMR spectrometers, a myriad of Mass Spectrometers (including MALDI, which we use very regularly), on-site CHNS combustion elemental analysis, TGA and DSC thermal properties characterization, and a huge suite of other materials characterization equipment (including many microscopy/imaging tools and Powder X-ray diffractometers) and a Class 100 Clean Room in the 4D Labs facilities on campus.
In addition, the Leznoff group houses an unusually wide and often unique array of characterization equipment, which Leznoff group students manage and use on a very regular basis. Details of some the key equipment in our group (and accessible by other researchers at and beyond SFU) are described below...
In addition, the Leznoff group houses an unusually wide and often unique array of characterization equipment, which Leznoff group students manage and use on a very regular basis. Details of some the key equipment in our group (and accessible by other researchers at and beyond SFU) are described below...
SINGLE-CRYSTAL X-RAY DIFFRACTOMETER
In the Leznoff lab, we maintain and operate a single-crystal X-ray diffractometer (SC-XRD). It is a dual source instrument with both copper and molybdenum X-ray sources. available. The system has mobility along the θ (detector) axis, ω (crystal mount lateral motion) and φ (crystal mount rotation) axies. The detector for this system is the new Photon II (replacing the APEX II shown in the above photo). Within this set-up is also an Oxford Cryosystems Cryostream, capable of achieving sample temperatures from 100-300 K, all while under a stream of inert N2(g). This instrument is ideal for running crystals of both inorganic materials (such as coordination polymers and MOFs), as well as organic and inorganic molecular samples. The copper source is capable of assigning absolute configuration, and the Cryostream both increases resolution of poorly diffracting samples and protects air sensitive samples. Students will get experience running their own crystals, as well as processing, solving, and interpreting their crystallographic data.
UV-VIS-NIR FLUOROMETERThe group's Edinburgh Photonics FS5 fluorometer can measure emission spectra from 400 nm well into the NIR - up to 1650 nm. It includes an integration sphere to obtain quantum yields, and can also measure phosphorescence lifetimes. Set up for both solid and liquid samples, it also has a liquid nitrogen cryostat (for variable temperature fluorescence measurements down to 78 K).
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X-RAY FLUORESCENCEThe Panalytical Epsilon 3XLE X-ray Fluorometer in the Leznoff lab is useful for determining the relative amount of elements in a sample. This particular instrument is capable of measuring for any element above carbon in weight, making it an excellent complement to elemental analysis for inorganic chemistry.
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GLOVEBOXThe Leznoff group has a MBraun dual station nitrogen-glovebox for air-sensitive chemistry (primarily organometallic and redox-active species). It has both a small and large port entrance chambers which can be placed under vacuum, as well as a nitrogen atmosphere for transfer of samples, equipment and waste in and out of the enclosure. There is a stirplate/hotplate and three other stirplates, a Coldwell depression for conducting reactions in the box down to -78 °C, a valve connected to an exterior coldtrap to remove solvents via reduced pressure, a -35C freezer, an analytical balance and a UV-vis-NIR (max wavelength of 1080 nm) absorption detector able to analyze samples within the enclosure via fibreoptic cables. A solvent-purification system for oxygen/moisture-free solvents is attached to the glovebox.
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RAMAN SPECTROMETERThe Renishaw inVia Raman microscope is designed for analysis of materials through an upright optical microscope (5X, 20X and 50X). The system uses a 514 nm laser or a 785 nm laser for obtaining the Raman spectra. The laser is focused onto the sample through the optical microscope. The spectral signatures are collected through the microscope objectives and analyzed using an in-line spectrometer. It has a motorized stage allowing for surface scanning of solid samples, and a temperature control apparatus. We particularly use it to monitor the vCN stretches in cyanometallate coordination polymers.
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POROSIMETERUsing gas adsorption methodology, our Micromeritics ASAP 2020 porosimeter can measure the pore size/volume and surface area of many porous materials, including our coordination polymers when appropriate, and using a wide range of different gases and vapours. Both chemisorbed and physisorbed analytes can be examined.
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MÖSSBAUER SPECTROMETEROne of the very few such instruments in Canadian Chemistry Departments, Mössbauer spectrometry is excellent for determining the oxidation state and spin-state of iron in iron-containing materials such as our metallophthalocyanines and diamido complexes, as well as following spin-transitions and magnetic ordering or freezing transitions in our coordination polymers. The spectrometer can acquire data from 4-600 K. If equipped with an appropriate gamma-ray source, Sn and several other elements can also be probed.
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INFRARED SPECTROMETEROur Nicolet FT-IR spectrometer (with an ATR sample plate, rather than KBr pellets) has a greatly expanded range compared to typical systems, allowing measurements from 50 - 11000 wavenumbers, allowing access to both the near-IR and far-IR. Additionally it has a temperature control add-on allowing for measurements down to 77K and up to 500K. Our cyanometallate and related coordination polymers nearly all see time on this instrument.
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REFRACTIVE INDEX MEASUREMENT SYSTEMRarely available in a Chemistry Department, this optical instrument can measure the refractive index of a crystalline solid or thin film. The Leznoff group has pioneered the rational design and synthesis of birefringent (the difference between refractive indices in two crystallographic directions) coordination polymer materials, reflecting our interest in the basic property of refraction in materials.
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OTHER EQUIPMENT
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