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

Contamination Control  Class 10, 100 hoods  Class 100 cleanrooms  Class 10,000 cleanroom

Analytical Support RTI has perform ed 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= ArCl= = As Mass Resolution Mass Resolution

Isobaric Interference on 75 As

Chemical Form: Arsenic

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).

Urine sample. 1-AsB, 2-DMA, and 3-MMA.

North Carolina Stream Data Data from North Carolina Geological Survey – ca. 1993

L-ephedrine  Mol wt.:  Mol formula: C10H15NO Analytical work:  Identification/Confirmation  Impurity determination

Identity - FTIR Assignments: 3470-N-H Stretch; 3298-N-H Stretch; 3085-O-H Stretch; 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.

NMR spectrum

Identity - NMR Chemical Shift (ppm) Multiplicity Integral Ratio Assignment d3.0a s3.1b 2.69Exchange peak2.5* m1.4c s1.0d s5.0e solvent

Peak No. Ret. Time (min) Rel. Ret. Time % of Total Area Identity/Purity - HPLC LC analysis: compare with standards.