Sample Collection and Management for Environmental

Forensics Investigations
Environmental Forensic Investigation

‘Forensics’ - the application of scientific knowledge and

analysis to for public discussion/debate OR potential
litigious (concerned with lawsuits) issues

“The application of
scientific methods used to
identify the origin and
timing of a contaminant
release” How???
Two Categories of EFIs
1. Academic & Research
- Develop the techniques
2. Liability Driven
Remediation planning
• The focus of the investigation
is driven by a need to
understand the nature and
scale of potentially hazardous
impacts
Liability assignment
• the need to compensate for the
costs associated with removing
an environmental hazard, often
cited as “The Polluter Pays
Principle.”
 Litigation and Liability Driven EFIs

• Adversarial process (involving a conflict)

• Goal – make you look bad or incompetent while making
themselves look good/sympathetic
• They are trying to tell if you are telling the truth or not
• Good science does not necessarily prevail

Need to prove it beyond a reasonable doubt

Easiest to Attack ‘Data Quality’
 Science Experiment

All environmental investigations should be

treated as a science experiment:
• Design (hypothesis, to answer a question)
• Data (correct, enough)
• Controls (to know validity of data and
uncertainty)
Investigation Road Map
Reporting

Laboratory Analysis

Data Review
Sampling Design

DQOs

Field Event

QAPP
Planning and Preparation

• Data Quality Objectives (DQOs),

• Data Quality Indicators (DQIs),
• Data Quality Assurances (DQAs), and
• Quality Assurance Project Plan (QAPP)
DQOs, DQIs, DQAs, and QAPP

• The US EPA formulations to site investigations

• Data quality objectives (DQOs)
• used to establish performance and acceptance
criteria, which serve as the basis for designing a plan
for collecting data of sufficient quality and quantity
to support the goals of the study
• Seven step process
DQOs, DQIs, DQAs, and QAPP
Seven step process:
1. State the problem
• e.g., assess the current groundwater monitoring approach and redesign the well-field network
2. Identify goal of the study
• e.g., Determine if the current monitoring well networks for Operable Units delineate plume
extent and, therefore, require no action; if the networks need to be redesigned using existing
wells; or if new monitoring wells should be installed.
3. Identify information inputs
• e.g., The data may already exist or may be derived from computational or surveying/sampling
and analysis methods.
4. Define boundaries of the study
• e.g., identify the population of interest, define the spatial and temporal boundaries that apply
to each decision statement.
5. Develop the analytical approach
• e.g., develop a decision rule (DR) for each decision statement in the form of an “IF…THEN…”
6. Specify performance criteria
• Because sample analytical data and field measurements are made based on measurement data
could potentially be in error (i.e., decision error).
7. Develop plan for obtaining data
• present alternative data collection designs that meet the minimum data quality requirements
specified in DQO Steps 1 through 6. A selection process is then used to identify the most
resource-effective data collection design that satisfies all of the data quality requirements.
DQOs, DQIs, DQAs, and QAPP
Quality Assurance Project Plan (QAPP)
• Describes the activities of an environmental data
operations project involved with the acquisition of
environmental information
• purpose to document the results of a project’s technical
planning process
• a clear, concise, and complete plan
• Reviewed and accepted by all stakeholders (regulators,
public (if necessary)) prior to beginning investigation
 DQOs, DQIs, DQAs, and QAPP

• Data quality indicators (DQIs)

• The principal DQIs are precision, bias, representativeness, completeness,
comparability, and sensitivity
• Reviewed as part of the data validation (discussed later)
 DQOs, DQIs, DQAs, and QAPP
• Data quality assessment (DQAs)
• Last thing to be completed
• data quality is meaningful only when it relates to the intended
use of the data
• Follows a stepwise approach:
• Review the objectives and sampling design
• Conduct preliminary data review
• Select the statistical method
• Verify the assumptions of the statistical method
• Draw conclusions from the data
 Data Flow for Environmental Investigations

Data Generation and Review

QAPP Analytical requirements sent to lab
1 2
3 4
Quality Assurance
Project Scope Project Plan (QAPP) Samples + Laboratory
Defined Requirements Field Activities COC info Analysis
Identified
Analytical
Field Logs Data on
Data
Information Sample
Location Package
8 7
Project External Parties
Data Repository e.g., Decision(s) + Validated Validation of the
Data Quality
Database (General or Data Usability Analytical Laboratory Analytical
Supporting Data Assessment
Project) Data Data (Not the Lab)
6 5

Data may
support future
Project needs Each investigation is a scientific experiment…
EPA Documents

http://www.epa.gov/QUALITY/qs-docs/g4-final.pdf
http://www.epa.gov/QUALITY/qs-docs/g5-final.pdf
http://www.epa.gov/QUALITY/qs-docs/g8-final.pdf
Summary of Planning and Preparation

• Set up investigation like an experiment

• Proper controls, appropriate sampling matrix, number of
samples chosen wisely
• Know what you are doing
• Method used to collect sample has been used before and
practiced
• Procedures in place to collect and document
• Roles and responsibilities of the team members have
been organized
• All equipment is ready to go, supplies are in stock
• Field work can now begin… but where to sample?
 Sampling
Plan

• Who will collect the samples? Do you have sufficient resources to

conduct sampling?
• What are the analytes in question and the matrices involved (air, soil,
water)? What sampling equipment and other resources will be
required?
• What are the data quality requirements? What equipment, containers,
and shipping materials will you need?
• Where will samples be collected? This may be governed by such factors
as regulatory requirements, the physical setup of the site or facility to
be sampled, ease of access to sampling sites, water depth, and other
factors.
 Sampling
Plan

• When will your sampling be carried out? This will depend on the nature
of the investigation. Is the season a factor? Is the lab available to
analyze the samples? In the case of time-sensitive analytes, will you be
able to get the sample to the lab for analysis quickly enough?
• How will samples be collected? How will you get to the site? How many
samples will be taken and shipped to the lab? How are the samples
being transported to the laboratory? Courier involved?
Sampling Statistics • How do I collect a
representative sample?
• How many samples do I
have to collect to prove
non-compliance?
• How much do I have to
exceed the regulatory limit
by in order to assure myself
that a non-compliance
situation exists?
Sampling Strategies
Systematic (stratified sampling)
• Involves taking samples over
regular distances or intervals -
horizontal (systematic) or vertical
(stratified).
• Two examples are:
1) shellfish samples taken at 1-km
intervals along a shore
2) water samples taken from
varying depths in the water
column.
Sampling Strategies
• Judgmental sampling (often the
method of choice for regulatory
and emergency response)
• relies on experience and the
available information to
determine locations that will
provide the most representative
samples.
• requires knowledge of the
distribution of the parameter(s)
in question; the sample validity
will depend on the accuracy of
this knowledge.
 Sampling Strategy
• Composite or discrete

Systematic grid Systematic grid Random

Sampling Strategy

• Must have a strategy before heading to site

• Non-biased, statistical sampling is best
• If judgmental sampling
• Is the person qualified to make the judgments?
• Are the judgments being documented – reasons why?
• Used years later
• Remember that one person s judgment may be
different than another
• Must be able to defend choices
Sampling

• Use approved procedures for sampling

• If no approved procedure is available, it should be
validated prior to conducting the field work
• How to sample is up to the investigator and the
science/techniques that are available
• Use approved or appropriate sampling containers
Carpet Dust Sampling

• Must follow
standardized
procedures where
available
• Difficult to change
approaches
• Validation required if
methodology changes

HVS-3 Vacuum Cleaner

Dust sampling

www.chemistry-matters.com
Wipe sampling
Soil sampling

Project
Water sampling

www.chemistry-matters.com
Gas Sampling

www.chemistry-matters.com
Standard Operating Procedures
• Standardized procedures to be used to execute
the project
• Use best practices for sample collection for the
investigation
• International Organization for Standardization (ISO)
guidance
• American Standards for Testing and Materials
(ASTM)
• Sometimes it needs to be new for the sample type
or matrix
• Must be documented and validated prior to using in
the field
Differences Between Legal and Research
• Documentation
• Documentation Date
Project id. Date Project id.

• Documentation Address

Write down everything done on

site and sign!!!
No correction after that

Date

Notes and pictures/videos

Flow of the investigation
• Documentation
• Sample Handling
• Chain of Custody
• Laboratory Competence
• Standard Procedures
• Communicating Results
 Documentation
Name

COCs

Field Notes Sampling Maps

Forms

• Done in real time to actual sampling (not at hotel later that evening)
Legally Defensible Notes

• Waterproof notebooks and pens

• Only use legally defensible notebooks
–

www.riteintherain.com/
Legally Defensible Notes

• Permanent ink (not pencil)

• Water proof Project

• Single spaced
• Errors crossed out with single line
• No pages removed
• Page numbered
• Cross out unused areas, with initials
• Each page dated
• Systematically written
• Third person, no feelings/assumptions – only
facts/observations
• Dedicated notebook is a good idea for each
project (in case notebook subpoenaed)

www.riteintherain.com/
Documentation
• Pictures, Pictures, Pictures
– Document like “CSI”
• Video standard procedures as needed
– Sometimes video every sample collected
• GPS – use best technique available
– Many people associate precision = accuracy
• Handheld GPS +/- 3-5 m vs sub-cm
 Completeness

• No empty fields
• Completeness/thoroughness is key
• Data blanks make it look incomplete or careless
• Questioning whether procedures were followed

Data used months to years after the fact for

litigation
You may not remember the field event
Sometimes new consultant needs to use the data
Field Notes & Documentation
• Good notes caught observation that well pump
had duct tape on it
• Positive hit for toluene in water – potential
blame on the client for impacting well
• Electricians tape had a concentration of toluene
that was calculated to be 290 mg/kg
• Could show that electrical tape caused positive
hit for toluene

•Field notes
•Observations
from experiment
Maintaining Custody

From a legal perspective, a

sample is under custody if:
• the sample is in a person’s
possession
• the sample was in the
person’s possession and
then was locked up to
prevent tampering
• the sample is in a
designated secure area
 Chain of Custody

• Should be filled out

in completion
• All samples
accounted for
– Lab issues
– Loss of custody
• COC used for
future reference

www.chemistry-matters.com
 Sample Packaging: Cooler
Check List
Item Yes If no....
Are samples properly contained and chemically Correct
preserved?
Are samples properly labeled? Correct
Initials of collector, time, date of collection? Correct
Are samples properly sealed? Correct
Is necessary preservative present, i.e. ice? Correct
Has chain of custody form been completed? Correct
Does chain of custody information match sample labels? Correct
Copy of chain of custody form taped to cooler lid and Correct
maintained inside cooler in whirlpack bag?
Samples properly packaged to withstand breakage? Correct
Are coolers custody sealed? Correct
Was storage temperature maintained between sample May require
collection and lab receipt resampling

www.chemistry-matters.com
Thermochron
40

30
Samples
collected
20
Temperature (° C)

Samples Samples
moved to received
10
freezer

-10

-20
Samples moved to
shipping cooler
-30
8 8 08 8 08 08 08 08 08 08
-0 -0 v- -0 v- v- v- c- c- c-
ov ov o ov o o No De De De
-N -N -N - N -N -N 0- 1- 2- 3-
24 25 26 27 28 29 3

Date

f04-07-9780444594242
Sample Stability

• Regulated time between collection of sample

and analysis of sample to ensure the sample
is representative of the place and time it
was collected.
• Termed “Hold Time”

• EPA has a list of hold times for many different

analytes.
• List not always scientific but must be met if
data is to be considered valid.
Sample Stability

Regulations also require specific preservation

activities. Examples include…

Store samples between 2 and 8oC

- Inhibits bacterial degradation

Store samples in correct sample vessel material

- Should be inert – glass or stainless steel, not
plastic

Store in dark
- Photolysis – breakdown chemicals
 Tamper proof seals
• Samples used in litigation
matters should have
tamper proof seals
• Demonstrates sample
integrity
• Can also tape around
cooler once packed and
use tamper proof seals
Examples of tamper proof seals

f04-05-9780444594242

f04-03-9780444594242

f04-04-9780444594242
 Cease to claim COC

• Each person that handles samples until

(including) receipt at lab must sign/date
COC
• Best to have samples sorted for
laboratory receipt
• Good practice – samples grouped by
analysis requested
• Don’t need sorting issue to be a problem
after all the effort put into collecting f04-02-9780444594242

samples
 Collecting sediment samples

Grab sampler

Core sampler
Collecting sediment samples

Long sediment core sampler

Ice core samples
Case Background
• Residents of town in Texas claimed
exposure to contaminants from
local wood treatment facility
• Initiated a class action lawsuit
• PAHs, Dioxins/Furans, metals
• Each side collects their own data
Choice of Sampling Locations

Residents’ representative
• Sampled oldest houses
in the town
• Only sampled homes
closest to plant
Sampling Strategy
• Best to have strategy before heading to site
• Non-biased, statistical sampling is best
• If judgmental sampling
– Is the person qualified to make the judgments
– Are the judgments being documented – reasons
why?
• Used years later
– Remember that one person’s judgment may be
different than another
• Must be able to defend choices
Choice of Sampling Locations

Residents’ representative
• Sampled oldest houses
in the town
• Only sampled homes
closest to plant

Defendants
• Sampled homes of all
ages and areas of town,
including “background”
Choice of Sampling Technique

Residents’ representative
- Vacuum bought at local store
then to collect samples
 Sampling Procedures

• Always use standardized or validated

sampling (operating) procedures
• Always have an SOP written and at
the site
• Have staff read and sign they have
read and understood the SOP
• Check to make sure staff are following
the SOPs
• Video the sampling of contentious
sites

www.chemistry-matters.com
Choice of Sampling Technique

Residents’ representative
- Vacuum bought at local store
then to collect samples

Defendants
- Used US-EPA developed
vacuum design
- Followed ASTM Method D5438–
05 protocol for sampling
Sample Containers

Residents’ representative
• Water bottles, cut in half and
taped together with duct tape
 Sample Containers
• Never use water bottles to
collect a sample
• Use appropriate
containers
– Careful of contaminant
• Is preservative necessary?
• How full does container
need to be?
– Headspace, no
headspace
– Will sample be frozen
• Tamper proof seal
 Sample Containers

Residents’ representative
• Water bottles, cut in half and
taped together with duct tape

Defendants
• EPA approved
glass, certified
clean sample jars
Sampling Locations

Residents’ representative
• Collected dust from normally
inaccessible attics spaces

www.chemistry-matters.com
Sampling
• Why are you taking the
sample?
• What are the CoCs?
• What is your conceptual site
model?
– What exposure are you
worried about or trying to
represent?
• Is the sampling technique
appropriate for the
model/guideline?
www.chemistry-matters.com
Figure downloaded from http://www.itrcweb.org/risk-3/Content/3.%20Planning.htm
Sampling Locations

Residents’ representative
• Collected dust from normally
inaccessible attics spaces

Defendants
• Sampled carpet in living
areas of the homes

www.chemistry-matters.com
Sample Pre/Post-Treatment

Residents’ representative
• Sample was submitted as is…

www.chemistry-matters.com
Sample Pre/Post-Treatment

Residents’ representative
• Sample was submitted as is…

Defendants
• Need to represent human
exposure which is <120 μm
particles
• Sieved to <120 μm following
ASTM standard 422-63

www.chemistry-matters.com
 % Recoveries Told the Story

Minimum and Maximum PAH Standard Recoveries

965%

900

PLAINTIFF DATA
Recovery (%)

700

500

300
138%
146%
EPA Maximum Recovery 150%
100 0%
EPA Minimum Recovery 25%
65% 44%
Soil House Attic
Dust Dust