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Chemistry

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Instrumentation

Chemistry Department Instrumentation

Instrumentation used to determine molecular structure of compounds:

 

Bruker 400 MHz Nuclear Magnetic Resonance (NMR) Spectrometer: The NMR facility (Science 213) contains a Bruker Avance 400-DRX spectrometer used for structure determination of small molecules. This two-channel system can observe 13C and 1H nuclei and is typically configured with a broadband observe (BBO) probe. A broadband inverse (BBI) probe is installed periodically for increased resolution of 1-D proton spectra and to observe 2-D correlations using an x, y, z–gradient amplifier. Temperature dependent studies can be conducted on either probe at temperatures ranging from -150°C to +180°C.

Bruker Alpha Fourier Transform Infrared Radiation (FT-IR): used to identify functional groups present in a molecule by measuring the transmission of IR light through solid, liquid and gas samples. Chemical bonds between various elements absorb light at differing frequencies, which allows each molecule to give IR characteristics similar to a “fingerprint” when submitted to infrared radiation. The FT-IR spectrometers can be configured with an attenuated total reflection (ATR) attachment to measure liquid or solid samples with minimal sample preparation or with a universal attachment that can measure gas, liquid, or solid samples.

 

Instrumentation used to determine components within a sample:

Agilent 6890 Gas Chromatographs (GC): used a column to separate gas-phase compounds in a sample. Samples may be dissolved in solvent and injected as a liquid to the GC, at which point the sample is vaporized to the gas phase, or injected as a gas (called headspace injection). Three GCs are used in the Chemistry department – one with a mass spectrometer detector (MSD) and the other two with thermal conductivity detectors (TCD). The type of column installed will determine what types of compounds will interact with the column and their relative retention times.

Agilent 1100 High Performance Liquid Chromatography (HPLC): used to separate components within a liquid sample by flowing the sample through a column. The HPLC is configured with a reverse-phase column, which allows compounds with more polarity to elute from the column first, and those with the least polarity to elute last. Samples are detected by UV-Vis absorbance.

Waters 2690 High Performance Liquid Chromatography (HPLC): used to separate components within a liquid sample by flowing the sample through a column. The HPLC is configured with a reverse-phase column, which allows compounds with more polarity to elute from the column first, and those with the least polarity to elute last. Samples are detected by UV-Vis absorbance.

Metrohm Professional 850 Ion Chromatography: used to determine the concentration of ions in a liquid sample. Can be configured to detect anions, cations, or organic acids via conductivity detection.

 

Instrumentation used to observe various properties of compounds:

 

Agilent 8453 Ultraviolet and Visible (UV-Vis) Spectrophotometer: used to measure the absorbance of a sample either at a single wavelength or over a range of wavelengths. Compounds with the ability to absorb light in the ultraviolet or visible wavelengths will give an absorbance. The measured absorbance can then be used to calculate the concentration of the sample.

Microplate UV-Vis: Measures the amount of light (ultraviolet and visible) transmitted through a plate of samples.

Perkin-Elmer Polarimeter: Measures the angle of rotation caused by passing polarized light through an optically active substance. Commonly used to analyze a range of compounds, including natural products, amino acids, proteins, pharmaceutical compounds, and small organic molecules.

Horiba Jobin Yvon Fluoromax-4C Fluorimeter: Measures the fluorescence given off by a sample after being brought up to an excited state. Fluorescence can be measured at room temperature or at variable temperatures, controlled by a water bath.

BAS 100 B/W Electrochemical Workstation: used to observe electroanalytical experiments in an electrochemical cell. Commonly used to produce cyclic voltammograms.

Surface Area Analyzer: used to obtain the area or pore size of surfaces on a sample.

Equipment used to prepare samples for analysis:

 

Centrifuges: used to separate liquids containing particles of different weights. Various centrifuges are located throughout the department with standard, high-speed, and refrigeration capabilities.

Lyophilizer: process in which liquid can be removed from a sample placed under high vacuum. Used most frequently on biological samples or samples that can be damaged by excessive heat. Samples are frozen, then placed on the lyophilizer and left until all liquid has sublimed.

Rotary Evaporator: used to evaporate solvent in a sample by simultaneously heating and reducing the pressure inside the sample flask. Various rotary evaporators (commonly referred to as “rota-vaps”) are used in labs located throughout the Chemistry department. Volatile organic solvents are ideal for removal by rotary evaporation. Aqueous solvents are extremely difficult to remove with this method and should be lyophilized instead.

 

This list contains the most frequently used instrumentation in Chemistry Department labs. Please contact the engineering technicians, Emil Babik and Cindy White, with any questions regarding instrumentation in the Chemistry Department.

 

Additional instrumentation at CWU is available in the Geology Department Murdock Research Laboratory.

 

 

 

 

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