Modern Analytical Instrumentation

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Transcription:

Modern Analytical Instrumentation Atomic Absorption and Emission Spectroscopy (AAS and AES) High Performance Liquid Chromatography (HPLC) Mass Spectrometry (MS) Also: Molecular UV-Vis Spectroscopy Fluorescence Spectroscopy NMR FTIR Raman Scattering Chem M3LC R. Corn

Absorption, Emission and Fluorescence Spectroscopies Chem M3LC. R. Corn

Inductively Coupled Plasma - Atomic Emission Spectrometer Liquid samples are nebulized into an argon plasma (10000 K) that breaks the sample into atoms and ions. Narrow band atomic emission is measured and the elemental composition is obtained. Pictures from Concordia College (MN) http://sites.cord.edu/chem-330-lab-manual/experiments/icp-aes

Spectroscopic Methods for Trace Metals in Seawater Atomic Emission Spectroscopy Each element has a unique emission spectrum

High Performance Liquid Chromatography (HPLC) Partition chromatography Normal phase chromatography Reversed-phase chromatography Size-exclusion chromatography Ion-exchange chromatography Bioaffinity chromatography Samples are passed over a packed column (stationary phase) and separated. Many types of chromatography based on different physical separation principles - the simplest is just partitioning (phase equilibria). Picture from Waters Company http://www.waters.com/

High Performance Liquid Chromatography (HPLC) Partition chromatography Normal phase chromatography Reversed-phase chromatography Size-exclusion chromatography Ion-exchange chromatography Bioaffinity chromatography Samples are passed over a packed column (stationary phase) and separated. Many types of chromatography based on different physical separation principles - the simplest is just partitioning (phase equilibria). IEC data from Universidad de Antioquia - Instituto de Química (Columbia) http://quimica.udea.edu.co/~carlopez/cromatoion/ion2.html

Mass Spectrometry

Mass Spectrometry

Mass Spectrometry Mass Analyzers: 5. Orbitrap. See Q. Hu et al., J. Mass Spectrom. 2005; 40: 430 443

Mass Spectrometry

Bromine 50/50 mix MW 79 and 81 Mass Spectrometry

Mass Spectrometry Ultra-high resolution MS can resolve different species with the same molecular weight! For example: Hydrogen-1: 1.007825 amu Nitrogen-14: 14.003074 amu Carbon-12: 12.0000 amu NH2 16.0187 amu CH4 16.0313 amu

Presolar Stardust Embedded in the fine-grained dust of chondrites are presolar grains, which predate the formation of our solar system and originated elsewhere in the galaxy. Larry R. Nittler, Earth and Planetary Science Letters, 209 259-273 (2003). Presolar stardust in meteorites: recent advances and scientific frontiers.

C12/C13 Ratios in Presolar Grains Carbon isotopic ratios measured in presolar grains from meteorites. Carbon on the Sun, Earth, Moon, Mars, and the other planets has about 89 12C atoms for every 13C atom. Presolar grains, on the other hand, contain the original atoms from their parent stars with different isotopic ratios. Presolar silicon carbide and graphite grains have carbon isotopic ratios that range from about 3 to 10,000!

Nanodiamonds (ca. 2.5 nm diameter) are the most abundant, but least understood type of pre-solar grains. Scientists believe that only supernovae can form the nanodiamond or SiC grains found in presolar stardust. Isotope Ratio Measurements Nanodiamonds - Key to the Universe? Nanodiamonds are identified as presolar on the basis of containing highly unusual Xe isotopic ratios (from Xe trapped in the nanodiamond), which seem to reflect nucleosynthetic processes in supernovae (SN). However, their small size precludes isotopic measurement of individual grains. Making matters worse is the fact that the Xe abundance is such that only about one in a million diamond grains contains a single Xe atom! Raman Spectrum of Diamond One sharp band at 1332 cm -1 Raman Imaging is used to map nanodiamonds in meteorites