Driving ISM Laboratory Processing Selection with Project Goals

Transcription

1 Ask The Expert Webinar Series Driving ISM Laboratory Processing Selection with Project Goals Mark Bruce Corporate Technical Director Raymond Risden Technical Services Director Copyright 2016, TestAmerica. All rights reserved.

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

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

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

5 Better Data Drives $ O Better Decisions 5

6 Incremental Terms Multi-Incremental Sample (MIS) trademarked by Envirostat Charles Ramsey Incremental Sampling Methodology (ISM) Interstate Technology and Regulatory Council Incremental Composite Sampling (ICS) US Environmental Protection Agency More similarities than differences All are structured compositing processes

7 Incremental Sampling Systematic Random Design Random starting locations in first grid Increment collection point 7

8 Incremental Sampling 8

9 ITRC ISM Guidance Incremental Sampling Methodology Team Formed Jan TestAmerica recruited by the US Army Corps of Engineers 9

10 ITRC Guidance & Training ITRC ISM guidance publically available Feb 15, Internet based training Sept. 20 & 21,

11 ISM Guidance Introduction ISM Principles Systematic Planning Statistical ISM Design Laboratory Process Making Decisions Regulatory Concerns Case Studies 11 Field Implementation Stakeholder Input

12 Laboratory Analyses Choose the Best ISM Processes ISM Field Sampling Yes VOCs Analysis Needed? Laboratory Processing Separate Sample Container for % Moisture Determination Determine the Number & Mass of Soil Increments Collected in Methanol No Yes VOCs Analysis Needed? No % Moisture Determination Determine the Number & Mass of Soil Increments Collected % Moisture Determination % Moisture Reporting Weighing - Methanol vol/weight Determination Volatiles Analysis Bulk Sample Mass Reduction (Optional ; Not Recommended) Yes Processing in Field? Other on-site Processing Air Drying - Sieving - Subsampling On-Site No % Dry Weight Reporting Specify Air Drying on-site to facillitate sieving Sieving On-Site: Specify Mesh Size of Screen Subsampling On- Site: Determine the Number & Mass of Soil Increments Sample Containerized, Packaged and Process "As Received" Sample Conditioning ( Matrix and Analyte Specific ) Disaggregation Drying "Chopping" (May require drying) Air Oven Freeze Drying Drying Drying A Water Addition Certification Preparatory Methods GO TO Sample BOX Mixing "A" ON (Optional) NEXT PAGE Analytical Method Modifications Particle Size Selection and/or Reduction Methods/ Contamiants Method Considerations Limitations Sieving Dish and Puck Mill Mortar and Pestle Ball Mill Pulverizers Other Fundamental Error and Sample Mass Consideration/Requirements Analytical Subsampling Techniques Inorganics Organics Sectorial Splitters Riffle Splitters Rotary Splitters 1 or 2-Dimensional Japanese Slabcake Other Quality Assurance/Quality Control Sample Ready for Analytical Preparation/Extraction Blanks Laboratory Replicates Spikes (Blank or Matrix?) Reference 12 OAF

13 Sample Processing Goals Goal: Improve subsampling representativeness Represents Goal: Improve precision & minimize bias 13

14 Fundamental Decision #1 What are you looking for? Analytes Contaminants of Concern Contaminants of Potential Concern 14

15 Analyte Groups 15 Volatile organics Energetics Metals, Hg PCBs Organochlorine Pesticides Phenoxy acid herbicides Petroleum hydrocarbons Semivolatile organics Dioxins / Furans Glycols Perchlorate

16 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? 16

17 Identify the Sample Materials to remove Vegetation Oversized material Decantable water Manual removal Sieve < 2 mm (#10) 17

18 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 18

19 %RSD Using Large Subsamples Larger particles Produce larger uncertainty or require larger subsamples Nugget effect g 5 g 10 g 30 g Fundamental Error Particle size (mm) ASTM D6323 Sec. A1.1

20 Case Studies Analytes Sites PAHs, Metals, VOCs, SVOCs & PCBs urban garden, storage tank, power station, skeet shooting range, radio relay station, smelter, paper mill, golf course Surface and subsurface soils The following examples are based on real site characterization projects. 20

21 Surface Soil from Potential Urban Garden What? ~ PAHs & metals 21

22 Surface Soil from Potential Urban Garden What? ~ PAHs & metals Where? ~ < 2 mm particles ~ Particle surfaces (PAHs) ~ Particle interior & exterior (metals) 22

23 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 particulate nature of some of the analytes 23

24 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 particulate nature of some of the analytes Years of air exposure ~ Air dry at room temp. 24

25 Surface Soil from Potential Urban Garden 25 What? ~ PAHs & metals Where? ~ < 2 mm particles ~ Particle surfaces (PAHs) ~ Particle interior & exterior (metals) Nugget effect? ~ Expected to be moderate due to the particulate nature of some of the analytes Disaggregate dry soil ~ #10 & #60 sieves Split sample 1 D slabcake No milling of PAH split Ball mill for mm fraction of metals split 2 D slabcake subsampling 30 g subsample PAHs 10 g subsample metals 3 g subsample Hg

26 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 particulate nature of some of the analytes Split sample 1 D slabcake No milling of PAH split 26

27 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 particulate nature of some of the analytes No milling of PAH split Ball mill for mm fraction of metals split 27

28 28 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 particulate nature of some of the analytes ITRC ISM Prep Section 6 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 mm fraction of metals split 2 D slabcake subsampling g subsample PAHs 10 g subsample metals 3 g subsample Hg

29 Subsurface Soil Below Storage Tank What? ~ Trichloroethylene Picture from USACE-Alan Hewitt 29

30 Subsurface Soil Below Storage Tank What? ~ Trichloroethylene Where? ~ All particles ~ Particle surfaces Picture from USACE-Alan Hewitt 30

31 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 Picture from USACE-Alan Hewitt 31

32 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 Volatile analyte ~ Minimize air exposure Picture from USACE-Alan Hewitt 32

33 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 Soil plugs - coring device ~ Methanol preservation & extraction 33

34 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 Options No other processing Shipping constraint 30 ml maximum volume, ship ground or as dangerous goods 34

35 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 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 EPA SW-846 Method 5035 large scale extraction or lab composite 35

36 Electrical Power Station Hawaii New Guidance What? ~ DRO, PAHs, Hg Where? ~ All particles ~ Particle surfaces Nugget effect? ~ Expected to be small to moderate Subsurface sample ~ Minimize air exposure Disaggregate moist soil ~ No sieve No milling Accept higher variability 2 D slabcake subsampling g subsample (DRO, PAHs) 10 g subsample (Hg)

37 Surface Soil from Skeet Shooting Range What? ~ PAHs, Pb, Pellets Where? ~ < 2 mm particles ~ Particle surfaces ~ mm fraction (pellets) Nugget effect? ~ Expected to be large due to the particulate nature of the analytes Years of air exposure ~ Air dry at room temp. Disaggregate dry soil ~ #4 & #10 sieve No milling Separate pellets visually Accept high variability in PAH & Pb results 2 D slabcake subsampling g subsample (PAHs) 10 g subsample (metals) 37

38 Surface Soil from Radio Relay Station What? ~ PCBs Where? ~ < 2 mm particles ~ Particle surfaces Nugget effect? ~ Expected to be small due to the liquid nature of the analytes Low volatility analytes ~ No monochloro PCB congeners ~ Air dry at room temp. Disaggregate dry soil ~ #10 sieve No milling 2 D slabcake subsampling g subsample 38

39 Smelter Waste Piles What? ~ Metals Where? ~ All particles ~ Particle surfaces Nugget effect? ~ Expected to be large due to the particulate nature of the analytes Years of air exposure ~ Air dry at room temp. Crush waste ~ < 9.5 mm No milling Field replicates Accept moderate variability in metals results 2 D slabcake subsampling 100 g subsample (TCLP) 10 g subsample (metals) 39

40 Surface and Subsurface soil, Waste piles, Concrete, and Sediment on Paper Mill What? SVOCs, VOCs, Metals, PCBs, Pesticides Where? ~ < 2 mm particles ~ Particle surfaces Nugget effect? ~ Expected to be small due to the liquid or diffuse nature of the analytes Decades of air exposure ~ Air dry at room temp. Disaggregate dry soil ~ #10 sieve No milling ~ Little analyte expected inside crystalline particles 2 D slabcake subsampling 30 g subsample for SVOCs, OCPs and PCBs 10 gram subsample for Metals 3 gram subsample for Hg 40

41 Former Golf Course Field Demonstration Area 1 and 2 Decision Units Area 1 Green Area 2 41

42 Surface Soil from Golf Course What? ~ As Where? ~ < 2 mm particles ~ Particle surfaces Nugget effect? ~ Expected to be small Low volatility analyte ~ Air dry at room temp. Disaggregate dry soil ~ #10 sieve No milling 2 D slabcake subsampling 2 g subsample ITRC ISM Prep Section 6 / Draft 3050C 42

43 Better Precision Changes Decisions Florida Golf Course - Arsenic Data (mg/kg) Area 2 Decision Unit Discrete n = 10 (mg/kg) Incr-30 n = 3 (mg/kg) Incr-100 n = 3 (mg/kg) Mean Std Dev %UCL FDEP SCTL: 2.1 mg/kg ITRC ISM team Florida golf course case study

44 Case Studies PAHs & metals surface soil from urban garden VOCs subsurface soil from solvent release PAHs, DRO, Hg subsurface soil from power station PAHs, Pb & pellets surface soil from skeet shooting range PCB Aroclors surface soil from radio relay station Metals waste piles at smelter VOCs, SVOCs, PCBs, OCPs, Metals paper mill As surface soil from golf course 44

45 ISM Processing for Discrete & Waste Samples ISM processing can improve representativeness of the analytical subsample Better manage within sample heterogeneity Improve reproducibility of results Reduces likelihood that sample heterogeneity is the cause of variable lab results 45

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? 46

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

48 Purpose of ISM Representative samples Better data Better decisions 48

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