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ISM Case Studies: Using Project Objectives to Select Laboratory Processing Options

ISM Case Studies: Using Project Objectives to Select Laboratory Processing Options. Mark Bruce Ph. D . – Corporate Technical Director. May 6, 2014. Chasing Uncertainty Sources. Instrumental analysis Sample preparation Laboratory sub-sampling Field sample collection.

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ISM Case Studies: Using Project Objectives to Select Laboratory Processing Options

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  1. ISM Case Studies: Using Project Objectives to Select Laboratory Processing Options Mark Bruce Ph. D. – Corporate Technical Director • May 6, 2014

  2. Chasing Uncertainty Sources • Instrumental analysis • Sample preparation • Laboratory sub-sampling • Field sample collection

  3. Does the decision unit fit in the sample jar? Representative subsampling

  4. Why is this important? _ X with known and less uncertainty Representative subsampling

  5. Better Data Drives Better Decisions O $

  6. Incremental Sampling Systematic Random Design Random starting locations in first grid Increment collection point

  7. ITRC ISM Guidance Incremental Sampling Methodology Team • Formed Jan. 2009 • TestAmerica invited to participate by US Army Corps of Engineers • On-going trainer for ITRC internet based training

  8. ITRC Guidance & Training ITRC ISM guidance publically available • Feb 15, 2012 • www.itrcweb.org/ISM-1 Internet based training • Feb. 11 & 13, May 13 & 15, Sep. 9 & 16, Nov. 4 & 6, 2014 • Feb. 12 & 14, May 7 & 9, Aug. 20 & 27, Dec. 3 & 10, 2013 • www.clu-in.org/conf/itrc/ISM/

  9. ISM Guidance Introduction ISM Principles Systematic Planning Statistical ISM Design Field Implementation Laboratory Process Making Decisions Regulatory Concerns Case Studies Stakeholder Input

  10. Choose the Best ISM Processes

  11. Sample Processing Goals Goal: Improve subsampling representativeness Goal: Improve precision & minimize bias Represents

  12. Fundamental Decision #1 What are you looking for? • Analytes • Contaminants of Concern • Contaminants of Potential Concern

  13. Analyte Groups Volatile organics Energetics Metals, Hg PCBs Organochlorine Pesticides Phenoxy acid herbicides Petroleum hydrocarbons Semivolatile organics Dioxins / Furans Glycols Perchlorate

  14. Fundamental Decision #2 Where are you looking for it? • What particles in the sample container should be included in the sample? • Exposed surfaces and pores of the particles? • Interior of the particles?

  15. Identify the Sample Materials to remove • Vegetation • Oversized material • Decantable water Manual removal Sieve • < 2 mm (#10)

  16. Look On or In the Particles? Extract or leach analytes from exterior surfaces and pores Particle size reduction to make interior particle components accessible to the sample preparation process

  17. Case Studies Analytes • explosives, VOCs, SVOCs, PAHs, PCBs & metals Sites • military training range, munitions manufacturing, urban garden, skeet shooting range, radio relay station, golf course Surface and subsurface soilsThe following examples are based on real site characterization projects.

  18. Surface Soil from Military Training Range What? • Explosives Pictures from USACE-Alan Hewitt

  19. Surface Soil from Military Training Range What? • Explosives Where? • < 2 mm particles • Particle interior & exterior Pictures from USACE-Alan Hewitt

  20. Surface Soil from Military Training Range What? • Explosives Where? • < 2 mm particles • Particle interior & exterior Nugget effect? • Expected to be high due to particulate nature of the analytes Pictures from USACE-Alan Hewitt 1mm

  21. Surface Soil from Military Training Range • High boiling analytes • Air dry at room temp. What? • Explosives Where? • < 2 mm particles • Particle interior & exterior Nugget effect? • Expected to be high due to particulate nature of the analytes

  22. Surface Soil from Military Training Range • Disaggregate dry soil • #10 sieve What? • Explosives Where? • < 2 mm particles • Particle interior & exterior Nugget effect? • Expected to be high due to particulate nature of the analytes

  23. Picture from USACE-Alan Hewitt Surface Soil from Military Training Range • Particle size reduction to increase surface area • Puck mill • Smaller, better mixed particles What? • Explosives Where? • < 2 mm particles • Particle interior & exterior Nugget effect? • Expected to be high due to particulate nature of the analytes

  24. Surface Soil from Military Training Range • Particle size reduction to increase surface area • Puck mill • Smaller, better mixed particles • 2 D slabcake subsampling What? • Explosives Where? • < 2 mm particles • Particle interior & exterior Nugget effect? • Expected to be high due to particulate nature of the analytes

  25. Surface Soil from Military Training Range • High boiling analytes • Air dry at room temp. • Disaggregate dry soil • #10 sieve • Particle size reduction to increase surface area • Puck mill • Smaller, better mixed particles • 2 D slabcake subsampling What? • Explosives Where? • < 2 mm particles • Particle interior & exterior Nugget effect? • Expected to be high due to particulate nature of the analytes EPA SW-846 Method 8330B Appendix A

  26. Technical Summary Study allowed comparison of a number of factors that affected reproducibility of results. For analytes presented:

  27. Picture from USACE-Alan Hewitt Subsurface Soil Below Storage Tank • What? • Trichloroethylene

  28. Picture from USACE-Alan Hewitt Subsurface Soil Below Storage Tank • What? • Trichloroethylene • Where? • All particles • Particle surfaces

  29. Picture from USACE-Alan Hewitt Subsurface Soil Below Storage Tank • What? • Trichloroethylene • Where? • All particles • Particle surfaces • Nugget effect? • Expected to be small due to the liquid nature of the analytes

  30. Picture from USACE-Alan Hewitt Subsurface Soil Below Storage Tank • Volatile analyte • Minimize air exposure • What? • Trichloroethylene • Where? • All particles • Particle surfaces • Nugget effect? • Expected to be small due to the liquid nature of the analytes

  31. Subsurface Soil Below Storage Tank • Soil plugs - coring device • Methanol preservation & extraction • What? • Trichloroethylene • Where? • All particles • Particle surfaces • Nugget effect? • Expected to be small due to the liquid nature of the analytes

  32. Subsurface Soil Below Storage Tank • No other processing • Shipping constraint • 30 mL maximumvolume or ship as dangerous goods • What? • Trichloroethylene • Where? • All particles • Particle surfaces • Nugget effect? • Expected to be small due to the liquid nature of the analytes

  33. Subsurface Soil Below Storage Tank • Volatile analyte • Avoid air exposure • Soil plugs - coring device • Methanol preservation & extraction • Shipping constraint • 30 mL maximum volume or ship as dangerous goods or ground transport • What? • Trichloroethylene • Where? • All particles • Particle surfaces • Nugget effect? • Expected to be small due to the liquid nature of the analytes EPA SW-846 Method 5035 – large scale extraction or lab composite

  34. Surface Soil from Potential Urban Garden • What? • PAHs & metals

  35. Surface Soil from Potential Urban Garden • What? • PAHs & metals • Where? • < 2 mm particles • Particle surfaces (PAHs) • Particle interior & exterior (metals)

  36. Surface Soil from Potential Urban Garden • What? • PAHs & metals • Where? • < 2 mm particles • Particle surfaces (PAHs) • Particle interior & exterior (metals) • Nugget effect? • Expected to be moderate due to the particulatenature of some of the analytes

  37. Surface Soil from Potential Urban Garden • Years of air exposure • Air dry at room temp. • What? • PAHs & metals • Where? • < 2 mm particles • Particle surfaces (PAHs) • Particle interior & exterior (metals) • Nugget effect? • Expected to be moderate due to the particulatenature of some of the analytes

  38. Surface Soil from Potential Urban Garden • Disaggregate dry soil • #10 & #60 sieves • Split sample 1 D slabcake • No milling of PAH split • Ball mill for 0.25-2 mm fraction of metals split • 2 D slabcake subsampling • 30 g subsample PAHs • 10 g subsample metals • 3 g subsample Hg • What? • PAHs & metals • Where? • < 2 mm particles • Particle surfaces (PAHs) • Particle interior & exterior (metals) • Nugget effect? • Expected to be moderate due to the particulatenature of some of the analytes

  39. Surface Soil from Potential Urban Garden • Split sample 1 D slabcake • No milling of PAH split • What? • PAHs & metals • Where? • < 2 mm particles • Particle surfaces (PAHs) • Particle interior & exterior (metals) • Nugget effect? • Expected to be moderate due to the particulatenature of some of the analytes

  40. Surface Soil from Potential Urban Garden • No milling of PAH split • Ball mill for 0.25-2 mm fraction of metals split • What? • PAHs & metals • Where? • < 2 mm particles • Particle surfaces (PAHs) • Particle interior & exterior (metals) • Nugget effect? • Expected to be moderate due to the particulatenature of some of the analytes

  41. Surface Soil from Potential Urban Garden • Years of air exposure • Air dry at room temp. • Disaggregate dry soil • #10 & #60 sieves • Split sample 1 D slabcake • No milling of PAH split • Ball mill for 0.25-2 mm fraction of metals split • 2 D slabcake subsampling • 30 g subsample PAHs • 10 g subsample metals • 3 g subsample Hg • What? • PAHs & metals • Where? • < 2 mm particles • Particle surfaces (PAHs) • Particle interior & exterior (metals) • Nugget effect? • Expected to be moderate due to the particulatenature of some of the analytes ITRC ISM Prep Section 6

  42. Former Golf Course Field Demonstration Area 1 and 2 Decision Units Area 1 Green Area 2

  43. Surface Soil from Golf Course • Low volatility analyte • Air dry at room temp. • Disaggregate dry soil • #10 sieve • No milling • 2 D slabcake subsampling • 2 g subsample • What? • As • Where? • < 2 mm particles • Particle surfaces • Nugget effect? • Expected to be small ITRC ISM Prep Section 6 / Draft 3050C

  44. Better Precision Changes Decisions Florida Golf Course - Arsenic Data (mg/kg) FDEP SCTL: 2.1 mg/kg ITRC ISM team Florida golf course case study

  45. Case Studies Explosives – surface soil from military training range VOCs – subsurface soil from solvent release SVOCs – surface soil from munitions manufacturing PAHs & metals – surface soil from urban garden PAHs, Pb & pellets – surface soil from skeet shooting range As & Pb - surface and subsurface soil from ordnance plant PCB Aroclors – surface soil from radio relay station As – surface soil from golf course

  46. Two Fundamental Decisions What are you looking for? • Complete list of individual analytes Where are you looking for it? • What particles in the sample container should be included in the sample? • Exposed surfaces and pores of the particles? • Interior of the particles?

  47. Two Trade-Off Decisions To air dry or not? To mill or not? Mechanical processing Analyte retention Improved precision Analyte representativeness

  48. Purpose of ISM Representative samples Better data Better decisions

  49. Contact Information Mark L. Bruce Ph.D. Corporate Technical Director Mark.Bruce@TestAmericaInc.com 330.966.7267 Patricia McIsaac Product Manager Patricia.McIsaac@TestAmericaInc.com 703.758.8381

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