1. DuPont Barksdale Site Sampling and Analytical Presentation
December 12, 2001
Northern Great Lakes Visitors Center

2. Tonight’s Presentation
Residential Sampling
Why, When, Who, & How
Analytical Program
Lab Selection
Lab Methods
Reports
Independent Review
Communications
Next Meeting
Brad Nave
Harry Gearhart

3. Residential Water Sampling
Why sample the drinking water?
Chemicals from the DuPont Barksdale Site have been found in the groundwater. DuPont and the Wisconsin Department of Natural Resources want to know if the chemicals are in drinking water so that corrective action can be taken.

4. Postcard Reminder for Residential Sampling

6. Residential Water Sampling
What are you sampling for?
The primary chemicals DuPont and WDNR are looking for are called Nitroaromatic and Nitramine compounds, which were used to make explosives at the DuPont site.
DuPont and WDNR have also checked for many additional chemicals.

7. Residential Water Sampling
How is the water sampling done?
Experienced sampling personnel collect the water samples in EPA approved clean containers. Samples are collected in resident’s homes at various locations, including at the tap. Many homes now have water treatment systems, where samples are also collected.

8. Residential Water Sampling
How is the security of the samples maintained?
Special seals are placed on the cooler lid before and after sampling event.
A form called a Chain of Custody is used to track who handles the samples.

9. Chain of Custody Example

10. Residential Water Analytical Program Objectives
Obtain accurate and reliable results for low levels of explosive compounds and other test parameters.
Receive results in a timely manner.
Use a reputable laboratory.

12. Laboratory Selection
Few commercial laboratories in USA can analyze for very low levels of Nitroaromatics and Nitramines with High Performance Liquid Chromatography - Tandem Mass Spectrometry (HPLC-MS/MS), based on SW846 Method 8321A.

13. Laboratory Qualifications
Severn Trent Laboratories - Denver, CO
Wisconsin certified for explosives
US Army Corp of Engineers (USACE) approved for explosives

14. Laboratory Analysis and Reporting
Use WDNR approved analytical methods
Generate lab report

15. Analytical Method Summary
The HPLC-MS/MS analysis, based on Method 8321A, involves a multi-step analytical procedure:
Explosive compounds are extracted from a water sample by a solid phase extraction process (SPE). A solvent is used to remove the compounds from the SPE cartridge into a small final volume.

16. Analytical Methods (continued)
High performance liquid chromatography (HPLC) is used to separate the explosive compounds present in the sample extract.
The HPLC is coupled with a tandem mass spectrometer (MS/MS) for positive identification and quantitation of compounds based on the generation of mass spectra.

17. Mark Dymerski, LC/MS Group Leader
Dr. Steve Cowling, LC/MS Chemist

18. Analytical Methods (continued)
Additional Analytical Methods for other parameters.
Sulfate by EPA Method 300.0
Nitrates/Nitrites by EPA Method 353.2
VOC’s by EPA SW846 Method 8260
Metals by EPA SW846 Methods 6010, 6020, or 7470

19. Analytical Method Quality Control
Analysis sequence with quality control elements and acceptance criteria
Instrument set-up
Calibration and calibration verification
Method & procedure quality control
Sample matrix quality control

20. Field Quality Control Samples
Field sample Duplicates at a minimum of 5%
Field sample fractions for Matrix Spike & Matrix Spike Duplicate at 5% frequency or per event, whichever is greater

21. Other Quality Control Laboratory systems quality control
three separate levels of review
Agency oversight/approval
on-site audits
certification
Proficiency Test samples
DuPont audits

22. Full Laboratory Report Deliverables
Content for explosives follows EPA “National Functional Guidelines for Data Validation”
Intended to:
allow independent review of all details of qualitative and quantitative determination of analytes in samples
provide in-depth determination of data usability
summarize sample results

23. Independent Data Review
Performed as a voluntary effort as an additional quality control step
Not performed on all projects

24. Independent Data Review (continued)
Independent validation of explosives data is performed by Environmental Standards, Inc. (ESI), Valley Forge, PA
Nationally-recognized validation and quality assurance specialists
Data review protocol based on EPA “National Functional Guidelines for Data Validation”

25. Independent Data Review (continued)
Role of Independent Data Validator:
Evaluate procedures and associated data
Specify lab rework
Request additional documentation
Add data qualifiers
Flag unusable data
Provide detailed report on compliance and data usability

26. Independent Data Validation Process
Includes an in-depth examination of the following data elements:
Sample condition/security upon receipt
Sample holding times
Sample preparation
Analytical sequence
Initial and continuing calibrations
Analyte identification
Analyte quantitation

27. Independent Data Validation Process
Includes an in-depth examination of the following additional data elements:
Blank analysis results
Surrogate recoveries
MS/MSD recoveries and precision
Laboratory control spike recovery
Field duplicate precision
Field blank results

28. Reporting
Laboratory sends the completed data report to the Independent Data Validator and DuPont
Validator sends the final Quality Assurance Review to DuPont

30. Reporting and Follow-up
DuPont forwards a summary of lab results and the independent review text report to WDNR and Division of Public Health.
DuPont takes corrective action as appropriate.
Wisconsin Department of Natural Resources sends a summary letter to residents.

31. Sample Results
Who receives the analytical results and independent review report?
Wisconsin Department of Natural Resources
Wisconsin Division of Public Health
DuPont

33. Sample Results If I have questions, who do I call?
Wisconsin Department of Natural Resources
Doug Shultz at (715)
Chris Saari at (715) , extension 120
Division of Public Health
Henry Nehls-Lowe at (608)
Bayfield County Health Department
Millie Lindsey (715)
DuPont
Brad Nave at (502)
24-hour operator - toll (866)

34. Questions?

35. Next DuPont Barksdale Meeting
January 22, 2002
Washburn Museum
7:00 P.M.
Subject: Environmental Investigations
Objectives
Considerations
Techniques

36. Presentation Materials
Copies are available for:
Groundwater Primer (October 30, 2001)
Presented by Jim Richenderfer
Historical Review (November 27, 2001)
Presented by Mark Vetter