Environmental Security Technology Certification Program Field Demonstration Report Applied Innovative Technologies for Characterization of Nitrocellulose- and Nitroglycerine Contaminated Buildings and Soils Badger Army Ammunition Plant Baraboo, Wisconsin January 5, 2007 Revision 1 Distribution Statement A: Approved for Public Release, Distribution is Unlimited Report Documentation Page Form Approved OMB No. 0704-0188 Public reporting burden for the collection of information is estimated to average 1 hour per response, including the time for reviewing instructions, searching existing data sources, gathering and maintaining the data needed, and completing and reviewing the collection of information. Send comments regarding this burden estimate or any other aspect of this collection of information, including suggestions for reducing this burden, to Washington Headquarters Services, Directorate for Information Operations and Reports, 1215 Jefferson Davis Highway, Suite 1204, Arlington VA 22202-4302. Respondents should be aware that notwithstanding any other provision of law, no person shall be subject to a penalty for failing to comply with a collection of information if it does not display a currently valid OMB control number. 1. REPORT DATE 3. DATES COVERED 05 JAN 2007 2. REPORT TYPE 00-00-2007 to 00-00-2007 4. TITLE AND SUBTITLE 5a. CONTRACT NUMBER Field Demonstration Report Applied Innovative Technologies for 5b. GRANT NUMBER Characterization of Nitrocellulose- and Nitroglycerine Contaminated Buildings and Soils 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR(S) 5d. PROJECT NUMBER 5e. TASK NUMBER 5f. WORK UNIT NUMBER 7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES) 8. PERFORMING ORGANIZATION Badger Army Ammunition Plant,Baraboo,WI,53913 REPORT NUMBER 9. SPONSORING/MONITORING AGENCY NAME(S) AND ADDRESS(ES) 10. SPONSOR/MONITOR’S ACRONYM(S) 11. SPONSOR/MONITOR’S REPORT NUMBER(S) 12. DISTRIBUTION/AVAILABILITY STATEMENT Approved for public release; distribution unlimited 13. SUPPLEMENTARY NOTES 14. ABSTRACT A field demonstration was conducted to assess the performance of three field analytical methodologies for the presence and/or concentration of nitrocellulose (NC) and nitroglycerine (NG) in soils as well as wood and concrete building materials collected at Badger Army Ammunition Plant (BAAAP) in Baraboo, WI. Acetone extracts of soils, concrete material, and wood samples were analyzed by each of the on-site methods and results compared to off-site laboratory analysis using high performance liquid chromatography (HPLC) with EPA SW-846 Method 8330 for NG and MCWAA Method 353.2 for NC, an automated colorimetric method. The field methods evaluated included EXPRAY? and DROPEXPlus colorimetric test kits (total NC/NG), CRREL RDX colorimetric test (proposed EPA SW-846 8510) (total NC/NG) and GC/TID field gas chromatograph (NG only). Accuracy of the qualitative methods was evaluated based on percent false positive / false negatives. The quantitative on-site methods were evaluated using linear regression analysis and relative percent difference (RPD) comparison criteria. The primary use of these analytical methods would be for characterization of explosive? contaminated buildings. Adequate characterization could allow many buildings to be left in place resulting in substantial cost avoidance and expedited transfer of properties out of Department of Defense (DOD) control. Findings from the field demonstration are presented. 15. SUBJECT TERMS 16. SECURITY CLASSIFICATION OF: 17. LIMITATION OF 18. NUMBER 19a. NAME OF ABSTRACT OF PAGES RESPONSIBLE PERSON a. REPORT b. ABSTRACT c. THIS PAGE Same as 130 unclassified unclassified unclassified Report (SAR) Standard Form 298 (Rev. 8-98) Prescribed by ANSI Std Z39-18 TABLE OF CONTENTS Page List of Tables ....................................................................................................................iii List of Figures ....................................................................................................................iv List of Acronyms ....................................................................................................................vi Acknowledgements ...................................................................................................................vii Abstract ...................................................................................................................vii 1.0 Introduction ..................................................................................................................1-1 1.1 Background..........................................................................................................1-1 1.2 Study Objectives..................................................................................................1-1 1.3 Regulatory Issues.................................................................................................1-1 1.4 Stakeholder/End-User Issues...............................................................................1-3 1.5 Previous Testing..................................................................................................1-3 2.0 Demonstration Approach.................................................................................................2-1 2.1 Demonstration Site / Facility Description...........................................................2-1 2.2 Demonstration Objectives....................................................................................2-3 2.3 Testing Design and Description...........................................................................2-4 2.4 Sampling Plan......................................................................................................2-4 2.4.1 Sample Locations....................................................................................2-4 2.4.2 Sample Collection..................................................................................2-10 2.4.3 Test Sample Preparation........................................................................2-12 2.5 Sample Analysis Scheme...................................................................................2-15 2.6 Reference Test Methods....................................................................................2-16 2.6.1 Reference Method MCAWW 353.2 Methodology..............................2-16 2.6.2 Reference Method EPA SW-846 8330/8332 Methodology................2-17 3.0 Field Test Methods and Results.......................................................................................3-1 3.1 Qualitative Sample Screening Using DROPEXPlus and EXPRAY™..................3-1 3.1.1 Introduction/Narrative.............................................................................3-1 3.1.2 Materials..................................................................................................3-1 3.1.3 Method.....................................................................................................3-2 3.1.4 Data Assessment......................................................................................3-2 3.1.5 Data Assessment Summary.....................................................................3-9 3.1.6 Conclusion...............................................................................................3-9 3.2 Quantitative Analysis Using CRREL RDX Method.........................................3-11 3.2.1 Introduction/Narrative...........................................................................3-11 3.2.2 Instrumentation and Materials...............................................................3-11 3.2.3 CRREL Methodology............................................................................3-11 3.2.4 Data Assessment....................................................................................3-12 3.2.5 Wood......................................................................................................3-14 3.2.6 Soil.........................................................................................................3-20 3.2.7 Concrete Material..................................................................................3-26 3.2.8 Data Assessment Summary....................................................................3-35 3.2.9 CRREL Method Conclusions................................................................3-37 3.3 Quantitative Analysis for NG by GC/TID.........................................................3-38 3.3.1 Introduction............................................................................................3-38 3.3.2 Instrumentation......................................................................................3-39 1/5/2007 ESTCP/BAAAP Field Demonstration Rev 1 C14811.doc i 3.3.3 Method...................................................................................................3-39 3.3.4 Data Assessment....................................................................................3-40 3.3.5 Summary of GC/TID Performance Metrics...........................................3-49 3.3.6 GC/TID Method Conclusions................................................................3-49 4.0 Summary of Method Conclusions...................................................................................4-1 5.0 Cost Assessment..............................................................................................................5-1 5.1 Cost Reporting.....................................................................................................5-1 5.2 Cost Analysis.......................................................................................................5-1 5.2.1 Cost Basis................................................................................................5-1 5.2.2 Cost Comparison......................................................................................5-2 6.0 Implementation Issues.....................................................................................................6-1 6.1 Environmental Checklist......................................................................................6-1 6.2 Other Regulatory Issues.......................................................................................6-1 6.3 End-User Issues...................................................................................................6-1 6.3.1 EXPRAYTM / DROPEXPlus Test Kits for NC and NG.............................6-1 6.3.2 CRREL Methodology for NC/NG...........................................................6-1 6.3.3 GC/TID Method for NHG.......................................................................6-2 7.0 References ..................................................................................................................7-1 Appendix B.1 Sampling Building Maps B.2 Lab Data Summary Tables B.3 STL Validation Reports 1/5/2007 ESTCP/BAAAP Field Demonstration Rev 1 C14811.doc ii LIST OF TABLES Number Title 2-1 Sample Summary 2-2 Sampling Log Summary Table 3-1 Bench Test Detectable Limits DROPEXPlus/EXPRAY™ 3-2 DROPEXPlus/EXPRAY™ Wood Results 3-3 DROPEXPlus/EXPRAY™ Soil Results 3-4 DROPEXPlus/EXPRAY™ Concrete Material Results 3-5 DROPEXPlus/EXPRAY™ Summary of Performance Measures 3-6 Comparison of CRREL Method Calibration Results for Wood 3-7 Modified CRREL Results for Wood samples 3-8 Comparison of CRREL Method Calibration Results for Soil 3-9 CRREL Results for Soil Samples 3-10 CRREL Results for Concrete Material Samples 3-11 NC/NG Results for Concrete Expansion Joint Material 3-12 CRREL RDX Method Performance Metrics for NC/NG Analysis 3-13 Modified CRREL Method Performance Metrics for NC/NG Analysis 3-14 GC/TID Results for Wood Samples 3-15 GC/TID Results for Soil Samples 3-16 GC/TID Results for Concrete Material Samples 3-17 GC/TID Performance Metrics for NG Analysis 4-1 Wood Samples Performance Evaluation Against Primary and Secondary Criteria 4-2 Soil Samples Performance Evaluation Against Primary and Secondary Criteria 4-3 Concrete Material Performance Evaluation Against Primary and Secondary Criteria 5-1 Demonstration Costs 1/5/2007 ESTCP/BAAAP Field Demonstration Rev 1 C14811.doc iii LIST OF FIGURES Number Title 1-1 BAAAP Building with XXX (3X) Classification 2-1 BAAAP Shaw Lab Trailer Location on Site 2-2 Shaw Lab Trailer and Generator on Site 2-3 Testing Inside Lab Trailer 2-4 BAAAP Storage Bunker 2-5 Wood Samples Inside Bunker 2-6a Typical Structure Found at BAAAP 2-6b Typical Structure Found at BAAAP 2-7 Concrete Core Sampling Team 2-8 Core Taken at Expansion Joint 2-9 Surface Soil Sample 1885-02-SS-0-72- Tunnel Location Beside Bldg 1885-02 Box Storage House 2-10 Sub-Surface Soil-Bore Hole 2-11 Nitrate House Wood Shavings from Transfer Trough Cover 2-12 Blender Homogenized Wood Less Than 1/4 inch 2-13 Crushing Concrete 2-14 Removal of Expansion Joint Material (EJM) 2-15 Sieving Soil Samples 2-16 Propellant Recovered From Soil Sample 1885-02-SS-073 2-17 Propellant Recovered From Soil Sample 1885-02-SS-072 2-18 Acetone Extracts of Soil Samples 3-1 Shaw Lab Trailer DROPEXPlus and EXPRAY™ Testing on Sample Extracts 3-2 Comparison of DROPEXPlus and EXPRAY™ on BAAAP Wood Extracts 3-3 CRREL Method Color Development 3-4 Wood NC/NG Calibration Curves for the Modified CRREL Method 3-5 Modified CRREL Results for NC/NG on Wood vs. STL Reference Method Results 3-6a Soil NC/NG Calibration Curves for the CRREL RDX Method 3-6b Soil NC/NG Calibration Curves for the Modified CRREL Method 3-7 CRREL RDX Results for NC/NG on Soil vs STL Reference Method Results 3-8 Modified CRREL Results for NC/NG on Soil vs. STL Reference Method Results 3-9 Concrete NC/NG Calibration Curves for the CRREL RDX Method 3-10 Standard Response for NC Spiked on Concrete vs. Time on Matrix 3-11 Calibration Curve for Fibrous NC on Concrete for the CRREL RDX Method 1/5/2007 ESTCP/BAAAP Field Demonstration Rev 1 C14811.doc iv 3-12 Calibration Curve for NC on Concrete for the Modified CRREL Method - NC in Acetone Spike 3-13 Calibration Curve for Fibrous NC on Concrete for the Modified CRREL Method 3-14 Effect of Resin Column Cleanup on CRREL Method Response for NC -Concrete Matrix 3-15 CRREL Method Results for NC/NG on Concrete vs. STL Reference Method Results 3-16 SRI GC/TID 3-17 GC/TID Results for NG on Wood vs. STL Method 8330 Results 3-18 Bench Test NG Results on Wood vs. STL Method 8330 Results 3-19 GC/TID Results for NG on Soil vs. STL Reference Method 8330 Results 1/5/2007 ESTCP/BAAAP Field Demonstration Rev 1 C14811.doc v LIST OF ACRONYMS BAAAP Badger Army Ammunition Plant °C degrees Celsius cm centimeter CRREL Cold Regions Research and Engineering Laboratory EPA U.S. Environmental Protection Agency ESTCP Environmental Security Technology Certification Program EJM Expansion Joint Material F Fahrenheit g gram GC gas chromatograph(y) GC/TID gas chromatograph(y) with thermionic ionization detection HPLC high-performance liquid chromatography LCS laboratory control sample MCAWW Methods for the Chemical Analysis of Wastewater MS matrix spike sample MSD matrix spike duplicate sample mg/kg milligrams per kilogram mg/L milligrams per liter µL microliter mL milliliter mm millimeter NC nitrocellulose NG nitroglycerine nm nanometer psi pounds per square inch RDX Royal Demolition Explosive, cyclotrimethylenetrinitramine SRI SRI Instruments, Inc. SS stainless steel STL Severn Trent Laboratories, Inc. TDL Technology Development Laboratory TID thermionic ionization detector UXO unexploded ordinance SUXOSO Shaw UXO Safety Officer 1/5/2007 ESTCP/BAAAP Field Demonstration Rev 1 C14811.doc vi Acknowledgements We gratefully acknowledge the hosting of this demonstration at the Badger Army Ammunition Plant. In particular we would like to thank the Installation Director Joan Kenney for her support. We would like to thank ESTCP for their guidance and support. We would also like to acknowledge the US Army Corps of Engineers personnel that assisted in the performance of the project, including Jay Hodges. Numerous Shaw employees contributed to this project including Dan Mckellin, Mike Clemens, Bill Eilbeck, Duane Root, Ellen Lay, Ed Morren and Steve Crouch. Abstract A field demonstration was conducted to assess the performance of three field analytical methodologies for the presence and/or concentration of nitrocellulose (NC) and nitroglycerine (NG) in soils as well as wood and concrete building materials collected at Badger Army Ammunition Plant (BAAAP) in Baraboo, WI. Acetone extracts of soils, concrete material, and wood samples were analyzed by each of the on-site methods and results compared to off-site laboratory analysis using high performance liquid chromatography (HPLC) with EPA SW-846 Method 8330 for NG and MCWAA Method 353.2 for NC, an automated colorimetric method. The field methods evaluated included EXPRAY™ and DROPEXPlus colorimetric test kits (total NC/NG), CRREL RDX colorimetric test (proposed EPA SW-846 8510) (total NC/NG) and GC/TID field gas chromatograph (NG only). Accuracy of the qualitative methods was evaluated based on percent false positive / false negatives. The quantitative on-site methods were evaluated using linear regression analysis and relative percent difference (RPD) comparison criteria. The primary use of these analytical methods would be for characterization of explosive– contaminated buildings. Adequate characterization could allow many buildings to be left in place resulting in substantial cost avoidance and expedited transfer of properties out of Department of Defense (DOD) control. Findings from the field demonstration are presented. 1/5/2007 ESTCP/BAAAP Field Demonstration Rev 1 C14811.doc vii