Jones, Diane - ISM Case Studies -...
Transcript of Jones, Diane - ISM Case Studies -...
2/17/2016
1
ISM Case Studies: Using Project Objectives to select Laboratory Processing Options
ISM Case Studies: Using Project Objectives to select Laboratory Processing OptionsDiane JonesMark Bruce Ph. D.
©2015, TestAmerica Laboratories, Inc. All rights rese rved.TestAmerica & Design ™ are trademarks of TestAmerica Laboratories, Inc.
2
Chasing Uncertainty Sources
• Instrumental analysis
• Sample preparation
• Laboratory sub-sampling
• Field sample collection
Does the decision unit fit in the sample jar?
3
Representative subsampling
2/17/2016
2
Why is this important?
4
Representative subsampling
X with known and less uncertainty_
Better Decisions
Better Data Drives
5
$ O
Incremental Sampling
• Systematic Random Design
6
Random starting locations in first grid
Increment collection point
2/17/2016
3
ITRC ISM Guidance
• Incremental Sampling Methodology Team~ Formed Jan. 2009
7
Disclaimer: Some of the material in this presentation has been derived from the Feb. 2012 guidance developed by the ITRC ISM team. ITRC does not endorse the use of specific vendors or technologies. This presentation is not official ITRC sanctioned training material. It has been reviewed by ITRC for compliance with the ITRC usage policy.
ITRC Guidance & Training
• ITRC ISM guidance publically available
~ Feb 15, 2012
~ www.itrcweb.org/ISM-1
• Internet based training
~ Recordings available and November 10, 2015
~ www.clu-in.org/conf/itrc/ISM/
8
ISM Guidance
Introduction
ISM Principles
Systematic Planning
Statistical ISM Design
Field Implementation9
Laboratory Process
Making Decisions
Regulatory Concerns
Case Studies
Stakeholder Input
2/17/2016
4
Choose the Best ISM Processes
10
ISM Field Sampling
VOCs Analysis Needed?
Yes
No
Determine the Number & Mass of
Soil Increments Collected
Determine the Number & Mass of Soil
Increments Collected in Methanol
Separate Sample Container for %
Moisture Determination
Processing in Field?
Yes
No
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
Other on-site Processing
Air Drying - Sieving -Subsampling
On-Site
SpecifySample
Containerized, Packaged and
Laboratory Processing
VOCs Analysis Needed?
No
Weighing - Methanol vol/weight
Determination
% Moisture Determination
% Moisture Reporting Volatiles Analysis
% Dry Weight Reporting
Yes
Bulk Sample Mass Reduction (Optional ; Not Recommended)
Sample Conditioning ( Matrix and Analyte Specific )
Water AdditionDryingDisaggregation "Chopping"
(May require drying)
Process"As Received"
Air Drying
Freeze Drying
GO TO BOX "A" ON NEXT PAGE
Oven Drying
% Moisture Determination
AF
A
Sample Mixing (Optional)
Particle Size Selection and/or Reduction
Sieving Dish and Puck Mill
Mortar and Pestle
PulverizersBall Mill Other
Analytical Subsampling Techniques
Sectorial Splitters
Riffle Splitters
Rotary Splitters
Other1 or 2-Dimensional Japanese Slabcake
Sample Ready for Analytical Preparation/Extraction
Lab
orat
ory
An
alys
es
Certification
Methods/Contamiants
Quality Assurance/Quality Control
Preparatory Methods
Analytical Method
Modifications
Method Considerations
Limitations
Fundamental Error and Sample Mass
Consideration/Requirements
OrganicsInorganics
Blanks Reference Laboratory Replicates
Spikes (Blank or Matrix?)
O
Sample Processing Goals
• Goal: Improve subsampling representativeness
• Goal: Improve precision & minimize bias
11
Fundamental Decision #1
• What are you looking for?~ Analytes
~ Contaminants of Concern
~ Contaminants of Potential Concern
12
2/17/2016
5
Analyte Groups
• Volatile organics• Energetics• Metals, Hg• PCBs• Organochlorine Pesticides• Phenoxy acid herbicides• Petroleum hydrocarbons• Semivolatile organics• Dioxins / Furans• Glycols• Perchlorate
13
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?
14
Identify the Sample
• Materials to remove
~ Vegetation
~ Oversized material
~ Decantable water
• Manual removal
• Sieve
~ < 2 mm (#10)
15
2/17/2016
6
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
16
Case Studies
• Analytes~ Explosives, VOCs, SVOCs, PAHs, PCBs & metals
• Site s~ military training range, munitions manufacturing,
urban garden, skeet shooting range, radio relay station
• Surface and subsurface soils
The following examples are based on real site characterization projects.
17
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
18
1mm
Pictures from USACE-Alan Hewitt
2/17/2016
7
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
19
• High boiling analytes~ Air dry at room temp.
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
20
• High boiling analytes~ Air dry at room temp.
• Disaggregate dry soil~ #10 sieve
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
21
• 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
particlesPicture from USACE-Alan Hewitt
2/17/2016
8
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
22
• 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
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
23
• 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
EPA SW-846 Method 8330B Appendix A
Subsurface Soil Below Storage Tank
24
• 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
2/17/2016
9
Subsurface Soil Below Storage Tank
25
• 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
Subsurface Soil Below Storage Tank
26
• 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
Subsurface Soil Below Storage Tank
27
• 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
2/17/2016
10
Subsurface Soil Below Storage Tank
28
• 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 –Ground shipping only
EPA SW-846 Method 5035 – large scale extraction or lab composite
Surface Soil from Munitions Manufacturing Plant
29
• What?~ SVOCs
• Where?~ < 2 mm particles
~ Particle surfaces
• Nugget effect?~ Expected to be small
due to the liquid or diffuse nature of the analytes
Surface Soil from Munitions Manufacturing Plant
30
• What?~ SVOCs
• 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.
2/17/2016
11
Surface Soil from Munitions Manufacturing Plant
31
• What?~ SVOCs
• 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
Surface Soil from Munitions Manufacturing Plant
32
• What?~ SVOCs
• 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
Surface Soil from Munitions Manufacturing Plant
33
• What?~ SVOCs
• 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
ITRC ISM Prep Section 6
2/17/2016
12
Surface Soil from Potential Urban Garden
34
• 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
Surface Soil from Potential Urban Garden
35
• 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.
Surface Soil from Potential Urban Garden
36
• 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
• Decades 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
2/17/2016
13
Surface Soil from Potential Urban Garden
37
• 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
• Decades 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
Surface Soil from Potential Urban Garden
38
• 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
• Decades 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
Surface Soil from Potential Urban Garden
39
• 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.
• 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 HgITRC ISM Prep Section 6
2/17/2016
14
Surface Soil from Skeet Shooting Range
40
• What?~ PAHs, Pb, Pellets
• Where?~ < 2 mm particles
~ Particle surfaces
~ 2-4.7 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• Count pellets visually
• Accept high variability in PAH & Pb results
• 2 D slabcake subsampling
• 30 g subsample (PAHs)
• 10 g subsample (metals)
ITRC ISM Prep Section 6
Surface and Subsurface Soil from Ordnance Plant
41
• What?~ As & Pb
• Where?~ < 2 mm particles
~ Particle surfaces
• Nugget effect?~ Expected to be
moderate due to the particulate nature of the analytes
• Non volatile analytes~ Air dry at room temp.
• Disaggregate dry soil~ #10 sieve
• No milling~ Moderate variability in
results tolerable
• 2 D slabcake subsampling
• 10 g subsample
ITRC ISM Prep Section 6
Surface Soil from Radio Relay Station
42
• 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
• 30 g subsample
ITRC ISM Prep Section 6
2/17/2016
15
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
43
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?
44
Two Trade-Off Decisions
• To air dry or not?
• To mill or not?
45
Mechanical processing
Analyte retention
Improvedprecision
Analyte representativeness
2/17/2016
16
Purpose of ISM
Representative samples
Better data
Better decisions
46
Contact Information
Mark L. Bruce Ph.D.
Corporate Technical Director
TestAmerica
4101 Shuffel St. NW
North Canton, OH 44720
Tel: 330-966-7267
www.testamericainc.com
Diane Jones
Subsampling Program Manager
for Canton Lab
TestAmerica
4101 Shuffel St. NW
North Canton, OH 44720
Tel: 330-497-9396
www.testamericainc.com