1. MINORITY/LOW INCOME STUDENTS SCIENCE RESEARCH MENTORING PROGRAM Asopuru Okemgbo a Washington State University Tri- Cities 2710 University Drive Richland, WA 99354 a CH2M Hill Hanford, Inc. Richland, WA 99352 Whitney Harris 1 Guadalupe Contreras 2 ACS Project SEED Interns 1 Kennewick High School 2 Pasco High School

2. Research Report Evaluation of Solid Phase Extraction/GC-FID of Phenols in Synthetic Hanford Waste Guadalupe Contreras (Presenter) Pasco High School, Pasco

3. Analytical Chemistry Lab

4. Objectives n To investigate the extraction of phenols in high alkaline synthetic Hanford waste (SHW) using various commercially available solid phase extraction sorbent. n To evaluate the effects of ion-pairing reagent in the isolation of phenols from high basic synthetic Hanford waste.

5. Hanford Tank Waste –Nuclear waste accumulated between1944 and 1987 was one of the aftermaths of World War II and Cold War nuclear bomb production. –It is the biggest US environmental restoration, waste management, and waste treatment project. –A $5.8 billion DOE Waste Treatment Project under construction. Hanford Site Background

6. Hanford Underground Tanks 149 Single Shell Tanks (SST’s) - Built 1943-1964. - Capacity of 55,000 to 1 million gal. 28 Double Shell Tanks (DST’s) - Built 1966-1986. - Capacity of 1.25 million gal. each. Contains about 54 million gal. Waste.

7. n At the Hanford Site, tank waste clean-up, waste treatment, tank closure, and environmental restoration are the highest priorities of the Department of Energy. n Characterization of the waste is a very important step towards meeting these goals. n EPA methods have not been amenable to the measurement of phenols in basic aqueous sample. n There is, therefore, no suitable method to measure them. n This method development project will be a major contribution to the waste characterization of the Hanford nuclear waste. Background and Significance

8. Sample Prep for Synthetic Hanford Waste n To 5mL of synthetic Hanford waste add 100μg/L of phenols n Add 2mL of PIC-A reagent n Extract with SPE sorbent (Strata-X from Phenomenex, Nexus from Varians, Oasis from Waters) n Elute with 2mL of methanol n Inject 2μL into GC

9. GC Conditions n Initial Oven Temperature n Ramp Rate: n Final Temperature n Injection Temperature Detector Temperature n Run Time n Carrier gas n Carrier Flow n 70°C n 10°C/min n 280°C n 300°C n 350°C n 21 min. n He n 1.9mL/min

10. Chromatogram of Phenols Standard phenol 1, 2-chlorophenol 2, 2-nitrophenol 3, 2,4-dimethylphenol 4, 2,4-dichlorophenol 5, 4-chloro-3-methylphenol 6, 3-nitro-o-xylene 7, 2,4,6-trichlorophenol 8, 2,4-dintrophenol 9, 2,3,4,5-tetrachlorophenol 10, 2,4,6-tribromophenol 11 1 2 9 6 8 11 5 7 10 4 3

11. Chromatogram of PIC-A Reagent Blank

12. Chromatogram of phenols in SHW treated with PIC-A Strata-X sorbent 9 6 811 4 2

13. Chromatogram of phenols in SHW not treated with PIC-A Strata-X sorbent 6 9 5

14. Chromatogram of phenols in SHW treated with PIC-A Nexus sorbent 9 10 6

15. Chromatogram of phenols in SHW treated with PIC-A Oasis sorbent 11 9 61 2 4 8 10

16. Conclusion n Solid phase extraction of phenols in highly basic synthetic Hanford waste afforded analyte isolation with small sample size, minimum sample prep, and elimination of large volumes of hazardous organic solvents commonly used in liquid-liquid extraction methods. n Preliminary data from using PIC-A reagent suggest improved recovery of phenols from high alkaline synthetic Hanford waste. n Additional work required to optimize the method.

17. Acknowledgements n ACS Project SEED Interns –Whitney Harris, Kennewick High School –Guadalupe Contreras, Pasco High School n ACS Project SEED Program n MSRM Matching Fund Donors –Dr. Andy Ward –Dr. Feyi Ward –Dr. P.S. Sundar –Riverside Rotary Club –Northwest Agricultural Products –MESA WSU Tri-Cities –WSU Tri-Cities n CH2M Hill Hanford, Incorporated