Analytical Services Laboratory

Introduction

Working in the Analytical Services Laboratory

The Analytical Services Laboratory is supported funded primarily from the faculty researchers of SAES.


Activities – 2001

The Analytical Services Laboratory (ASL) staff analyzed approximately 11,000 samples for over 22,000 analytes in this reporting year with an estimated commercial value of over $380,000 – surpassing last year’s production for dollar volume but 10% fewer samples.  The reason for this apparent discrepancy is that more organic analyses were performed in 2001 than in 2000. The inorganic and elemental analyses decreased in 2001. The laboratory manager is serving on seven theses committees – five more than the previous year. Six MSc. candidates worked in ASL for the sample preparation and chemical analysis part of their thesis this year.  ASL staff has constructed, and taught individual instrumentation-oriented classes for four graduate and undergraduate SAES laboratory classes.     

The educational impacts were the training of graduate students in instrumental analysis, the serving on thesis committees and sitting in one oral defense, and the development and teaching of experiments in teaching labs.  ASL staff analyzed samples for or collaborated with investigators in ten different ongoing research projects, and one project involving both extension and research. 

The Analytical Services Laboratory received a significant donation from Lorillard Tobacco Company with an estimated worth of $250,000.  The donations were for an upgrade of our 270 MHz NMR system – components listed below.

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General Capabilities: Analyses by AOAC, Standard Methods, EPA, FDA, and customized methodologies for organic, elemental, and inorganic analysis.

1. UV/VIS Absorption Spectrophotometry  - Ion Chromatography

Equipment: CARY 1E Double Beam UV/VIS Spectrophotometer with autosampler/sample preparation station. Perkin Elmer Lambda 3B Double Beam UV/VIS Spectrophotometer.   Lachat Flow Injection Analyzer/ Ion Chromatograph (FIA/IC).

Current Analyses: Most of the analyses are colorimetric for o-Phosphate, Nitrate/Nitrite, and Ammonium.

Capabilities: Any colorimetric analysis of any analyte with a derivative absorbing in the region of 200 to 900 nanometers. Any kinetic analysis of an analyte absorbing in the same region for an ambient-temperature reaction and a reactant half-life on the order of at least two minutes.  Both anions and cations in potable water (or low ionic strength aqueous solutions) can be measured with the ion chromatograph.  The technique is similar to HPLC, but at lower liquid pressures.


A.   Cary 1E  UV/VIS Spectrophotometer


B.  LACHAT FIA/IC

2. Gas Chromatography and Mass Spectrometry

Equipment: Two Hewlett Packard 5890 (II) gas chromatographs. One Flame Ionization (FID), two Electron Capture (ECD), two Nitrogen/Phosphorus (NPD), and one HP5971A mass spectrometer detectors. TEKMAR 7000 Static Headspace Autosampler, and model ALS2000/LCS2016 Dynamic Purge-And-Trap controller and autosampler.

Current Analyses: Most analyses are chromatographic separation and analysis of herbicides, pesticides, their metabolites, volatile chlorinated hydrocarbons, flavor chemicals in food analysis, fatty acids.

Capabilities: Volatile and Semivolatile organic molecule qualitative and quantitative analysis.

C.  SHA/GC/MS-FID-NPD
(Purge-and-Trap Unit With GC/ECD/FID in Background)

3. Nuclear Magnetic Resonance Spectroscopy

Equipment: JEOL EX-270 MHz NMR with 5 mm and 10 mm tunable broadband probes and temperature controller for sub and supra-ambient temperature sample analysis, 5 mm Carbon/Hydrogen probe, Carbon/Hydrogen solid state probe, Sun O2 workstation.  Recent upgrades (10 mm probe, solid state probe, and Sun Workstation) were donated by Lorillard Tobacco Co.

Current Analyses: Herbicides and pesticides plus metabolites, mono and diglycerides, glycoproteins and proteins with anti-microbial activity.  Upcoming projects are oriented heavily toward glycoproteins analysis and medicinal Herb/Mushroom active agents.

Capabilities: Compounds with at least parts-per-million levels (or ability to concentrate sample to this level) of compounds containing phosphorus, carbon, hydrogen, nitrogen, aluminum, and chlorine.


D.   JEOL EX-270 MHz NMR

 4.  Ion Coupled Plasma/Atomic Emission Spectroscopy (ICP/AES)

Equipment:  Perkin Elmer Optima 3300 DV with 150 place autosampler.

Current Analyses:  Phosphorus, Copper, Zinc, Sodium, Calcium, Magnesium, Manganese, Potassium, Iron, Cadmium, Selenium, Nickel. Upcoming analysis are elemental analysis of metals in medicinal mushrooms.

Capabilities: The spectrometer is a polychromator versus a monochromater meaning that more than one emission wavelength can be monitored in a parallel fashion. Six thousand emission wavelength lines that include the major emission lines for 72 of the 110 elements in the periodic chart can be monitored simultaneously. The inert gases, halogens, and certain rare earth metals cannot be detected with this instrument.


Perkin Elmer Optima 3300 DV  ICP/AES

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