Jones, Diane - ISM Case Studies - MSECAmseca.org/media/2016-02-17_-_Jones_Diane_-_ISM_Case_Studies.pdfFeb 17, 2016 · 2/17/2016 1 ISM Case Studies: Using Project Objectives to select

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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 OptionsDiane JonesMark Bruce Ph. D.

©2015, TestAmerica Laboratories, Inc. All rights rese rved.TestAmerica & Design ™ are trademarks of TestAmerica Laboratories, Inc.

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Chasing Uncertainty Sources

• Instrumental analysis

• Sample preparation

• Laboratory sub-sampling

• Field sample collection

Does the decision unit fit in the sample jar?

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Representative subsampling

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Why is this important?

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Representative subsampling

X with known and less uncertainty_

Better Decisions

Better Data Drives

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$ O

Incremental Sampling

• Systematic Random Design

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Random starting locations in first grid

Increment collection point

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ITRC ISM Guidance

• Incremental Sampling Methodology Team~ Formed Jan. 2009

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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/

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ISM Guidance

Introduction

ISM Principles

Systematic Planning

Statistical ISM Design

Field Implementation9

Laboratory Process

Making Decisions

Regulatory Concerns

Case Studies

Stakeholder Input

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Choose the Best ISM Processes

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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?)

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Sample Processing Goals

• Goal: Improve subsampling representativeness

• Goal: Improve precision & minimize bias

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Fundamental Decision #1

• What are you looking for?~ Analytes

~ Contaminants of Concern

~ Contaminants of Potential Concern

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Analyte Groups

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

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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?

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Identify the Sample

• Materials to remove

~ Vegetation

~ Oversized material

~ Decantable water

• Manual removal

• Sieve

~ < 2 mm (#10)

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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

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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.

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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

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1mm

Pictures from USACE-Alan Hewitt

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• High boiling analytes~ Air dry at room temp.







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• Disaggregate dry soil~ #10 sieve







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~ Particle size reduction to increase surface area

• Puck mill~ Smaller, better mixed

particlesPicture from USACE-Alan Hewitt

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particles

• 2 D slabcake subsampling







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particles


EPA SW-846 Method 8330B Appendix A

Subsurface Soil Below Storage Tank

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• 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

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~ Particle surfaces



• Volatile analyte~ Minimize air exposure

Picture from USACE-Alan Hewitt


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~ Particle surfaces



• Volatile analyte~ Avoid air exposure

• Soil plugs - coring device~ Methanol preservation &

extraction


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~ Particle surfaces





extraction

• Shipping constraint• 30 mL maximum volume

or ship as dangerous goods

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~ Particle surfaces





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

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• What?~ SVOCs


~ Particle surfaces


due to the liquid or diffuse nature of the analytes


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• What?~ SVOCs


~ Particle surfaces



• Decades of air exposure~ Air dry at room temp.

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• What?~ SVOCs


~ Particle surfaces






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• What?~ SVOCs


~ Particle surfaces





• No milling~ Little analyte expected

inside crystalline particles


• 30 g subsample


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• What?~ SVOCs


~ Particle surfaces





• No milling~ Little analyte expected

inside crystalline particles


• 30 g subsample

ITRC ISM Prep Section 6

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Surface Soil from Potential Urban Garden

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• What?~ PAHs & metals


~ Particle surfaces (PAHs)

~ Particle interior & exterior (metals)

• Nugget effect?~ Expected to be

moderate due to the particulate nature of some of the analytes


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• Years of air exposure~ Air dry at room temp.


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• 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


• 30 g subsample PAHs

• 10 g subsample metals

• 3 g subsample Hg

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• 3 g subsample HgITRC ISM Prep Section 6

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Surface Soil from Skeet Shooting Range

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• What?~ PAHs, Pb, Pellets


~ Particle surfaces

~ 2-4.7 mm fraction (pellets)

• Nugget effect?~ Expected to be large due

to the particulate nature of the analytes


• Disaggregate dry soil~ #4 & #10 sieve

• No milling• Count pellets visually

• Accept high variability in PAH & Pb results


• 30 g subsample (PAHs)

• 10 g subsample (metals)


Surface and Subsurface Soil from Ordnance Plant

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• What?~ As & Pb


~ Particle surfaces


moderate due to the particulate nature of the analytes

• Non volatile analytes~ Air dry at room temp.


• No milling~ Moderate variability in

results tolerable


• 10 g subsample


Surface Soil from Radio Relay Station

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• What?~ PCBs


~ Particle surfaces



• Low volatility analytes~ No monochloro PCB

congeners

~ Air dry at room temp.


• No milling• 2 D slabcake subsampling

• 30 g subsample


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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

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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?

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Two Trade-Off Decisions

• To air dry or not?

• To mill or not?

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Mechanical processing

Analyte retention

Improvedprecision

Analyte representativeness

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Purpose of ISM

Representative samples

Better data

Better decisions

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Contact Information

Mark L. Bruce Ph.D.

Corporate Technical Director

TestAmerica

4101 Shuffel St. NW

North Canton, OH 44720

Tel: 330-966-7267

[email protected]

www.testamericainc.com

Diane Jones

Subsampling Program Manager

for Canton Lab

TestAmerica

4101 Shuffel St. NW

North Canton, OH 44720

Tel: 330-497-9396

[email protected]

www.testamericainc.com

Documents

Jones, Diane - ISM Case Studies - MSECAmseca.org/media/2016-02-17_-_Jones_Diane_-_ISM_Case_Studies.pdfFeb 17, 2016 · 2/17/2016 1 ISM Case Studies: Using Project Objectives to select