1. 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

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

3. 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.

4. Atomic Spectrometry at RTI International Essential Trace Metals: Cr, Mn, Fe, Co, Ni, Cu, Zn, Mo, Se…?

5. 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

6. 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 73.9216 Mass Resolution 75.9605 74.9150 Mass Resolution 74.9670

7. Isobaric Interference on 75 As

8. Chemical Form: Arsenic

9. 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).

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

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

12. L-ephedrine  Mol wt.: 165.23  Mol formula: C10H15NO Analytical work:  Identification/Confirmation  Impurity determination

13. 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.

14. NMR spectrum

15. Identity - NMR Chemical Shift (ppm) Multiplicity Integral Ratio Assignment 0.85-0.89d3.0a 2.52-2.54s3.1b 2.69Exchange peak2.5* 2.82-2.90m1.4c 4.84-4.86s1.0d 7.28-7.36s5.0e 7.25-7.27-solvent

16. Peak No. Ret. Time (min) Rel. Ret. Time % of Total Area 1 15.19 1 100 Identity/Purity - HPLC LC analysis: compare with standards.