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Applications of Analytical Chemistry at RTI International. Argon plasma instruments Atomic Emission (ICP-AES) – 3 Quadrupole Mass Spectrometers (ICP-MS) - 2 Sector Field Mass Spectrometer (SFICP-MS) -1 Fluorescence Cold Vapor (for Hg) Hydride Generation (for As, Se, etc.) Absorption.
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Applications of Analytical Chemistryat RTI International • Argon plasma instruments Atomic Emission (ICP-AES) – 3 Quadrupole Mass Spectrometers (ICP-MS) - 2 Sector Field Mass Spectrometer (SFICP-MS) -1 • Fluorescence Cold Vapor (for Hg) Hydride Generation (for As, Se, etc.) • Absorption
Contamination Control • Class 10, 100 hoods • Class 100 cleanrooms • Class 10,000 cleanroom
Analytical Support RTI has performed major component, trace and ultra-trace level organic & inorganic analyses in support of variety of studies… • Animal toxicology/ADME studies - Bulk chemical characterization, impurity analysis, tissue burden analysis. • Human exposure studies - (Hg in hair; Pb in blood; As, Cd, Se, Cu, etc. in blood and plasma, etc.) • Environmental studies – drinking water, food, air samples, sediments, etc.
Atomic Spectrometry at RTI International Essential Trace Metals: Cr, Mn, Fe, Co, Ni, Cu, Zn, Mo, Se…?
Assessment of Human Exposure to Arsenic • Exposure: • Ingestion - Drinking water and food. • Inhalation – negligible • Internal dose: • Urine analysis • Hair analysis • Toxicity of Species: • As(III), As(V), AsB, AsC, MMA, and DMA
Interferences – Atomic Masses • High-Resolution ICP-MS solves many problems… • …but is not a magic bullet As=74.921594 ArCl=39.962384+34.965903=74.928287 As As 74.9150 Mass Resolution 74.9670 73.9216 Mass Resolution 75.9605
Calibration Standard – Urine matrix • Chromatogram 10ppb calibration standard (urine). • Key: • 1- AsB, 2 - As3+ • 3-DMA, 4-AsC • 5-MMA, 6-As5+ • IS - Internal standard (Potassium Hexahydroxy Antimonate V).
North Carolina Stream Data Data from North Carolina Geological Survey – ca. 1993
L-ephedrine • Mol wt.: 165.23 • Mol formula: C10H15NO Analytical work: • Identification/Confirmation • Impurity determination
Identity - FTIR Assignments: 3470-N-H Stretch; 3298-N-H Stretch; 3085-O-H Stretch; 2979- Aromatic C‑H Stretch; 1491-N‑CH3 Bend; 1450-N‑CH3 Bend; 1373-N‑CH3 Bend; 1353-C‑O Stretch; 1136-C‑N Stretch; 1089-O‑H Stretch; 983-C‑H Bend; 750-Aromatic C‑H Bend; 702-Aromatic C‑H Bend.
Identity/Purity - HPLC LC analysis: compare with standards. Peak No. Ret. Time (min) Rel. Ret. Time % of Total Area 1 15.19 1 100