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Title: Using Field Analytical Methods for Site Investigation Presented At: Pan American Studies Institute C


1
Using Field Analytical Methods for Site
Investigation Presented AtPan American Studies
Institute ConferenceJuly 23 to August 2, 2002

Presented By James Mack- New Jersey Institute of
Technology (973) 596 5857 Todd Morgan- S2C2 Inc.
(908) 542 1999
2
Objectives of Workshop
  • Become familiar with Field Analytical Methods
    information/hands-on practice
  • Understand how to use them strategically for
    faster, cheaper and more complete site
    investigations
  • Assure useable-quality data for environmental
    decision-making when using Field Analytical
    Methods

3
Presenters
  • James MackNJIT/Strategic Use of Field Analytical
    Methods
  • Todd Morgan S2C2/ Field Analytical Methods

4
History of Environmental Monitoring
  • The objectives have changed
  • Before 1950 - Basic survival
  • 1950s - Natural Environment
  • 1960s 1970s - Pollution control
  • 1970s 2000 - Remediation
  • 2000s - Sustainable development

5
Importance of the Site Investigation (SI)
  • Identifies contaminants needing clean up
  • Defines subsurface conditions (geology,
    hydrogeology, soil types)
  • Basis for remediation design
  • Targets area for remedial technology application
  • Identifies potential receptors at risk
  • Establishes level of remediation needed
  • Determines success of the remediation

6
Evolution of the Use of Field Methods in SIs
  • Initially Field Methods were crude use of gas
    sampling technology/test kits
  • Considered screening level data (i.e.first cut
    look at site)
  • Increased regulatory oversight drives need for
    standardization of SI process
  • Mid 1980s to 1990s emphasis on definitive data
    from approved lab methods
  • 1990s technology improves Field Methods gain
    acceptance (standard methods)
  • Today- Reliable Field Methods are changing how
    SIs are performed ( Triad Approach)

7
Analytical Methods
  • Traditional off-site laboratory analysis
  • Use approved standard methods (i.e. SW-846)
  • Extensive data QA/QC
  • Field Analytical Methods
  • make measurements on-site (in-situ) using
    instruments, kits or sensors
  • Portable,
    Easy use
  • Reliable
    Approved methods
  • Real time information
    Verifiable

8
Why Field Analysis?
  • Increased efficiency
  • Real-time information
  • Monitoring of remedial actions
  • Non-intrusive characterization identification
  • Reduced/focused or remedial efforts

9
Field Analytical Methods Advantages
  • Allows for quick results
  • Often less expensive
  • Reduces trips to the site
  • Reduces number of samples sent off-site for
    analysis
  • Allows for sampling flexibility and more samples
    to be taken

10
Field Analytical MethodsLimitations
  • Getting government approval
  • Requires experienced scientists in the field
  • Requires knowledge of site history
  • Knowledge of site stratigraphy and contamination
    Off-site Lab confirmation required (small portion
    of samples
  • Start-up costs sometimes higher (purchase of
    instruments)

11
Types of Field Analytical Methods Discussed
  • Gas Chromatography/Mass Spectrography
  • Immunoassay Kits
  • Ultraviolet Florescence
  • X-ray Fluorescence
  • Colorimetric Tests
  • Probes Other Devices

12
The Use of Field Methods in Site Investigations
  • Real Time Data Provided by Field Methods
    Improves the Effectiveness of Site Investigations

13
Strategic Use of Field Analytical Methods in Site
Investigations
  • Step Process to more strategic site
    investigations, using field analytical methods
  • Step 1 Systematic Planning
  • Step 2 Dynamic Work Plan Preparation
  • Step 3 Implementation using Real Time
  • Data Field Decision Making
  • Step 4 Data Evaluation QA/QC

14
Purpose of a Site Investigation
  • Identify contaminants of concern
  • Delineation of the extent of contamination
    impacts
  • Identify risk from contamination
  • Determine remedial action requirements

15
Example Case-Study
  • Site in Newark, New Jersey
  • Drum Recycling and Cleaning
  • Six Areas of Concern (AOC's)
  • Contaminants of concern (COCs) are
  • Petroleum hydrocarbons
  • Chlorinated solvents
  • Metals Lead, arsenic and cadmium

16
Example Case Study
  • Property has strong real estate value
  • Redevelop into warehouse distribution center
  • New facility need to be operational in one year
  • Clean up to industrial standards (excavate hot
    spots, cap, institutional controls)
  • SI objectives are to delineate hot spots quickly
    and in one mobilization
  • Use field analytical methods to accomplish goals

17
Step 1 Systematic Planning
  • Importance of Systematic Planning
  • - Ensures that the end goals are clearly defined
  • - Ensures that most resource effective means are
    used to achieve the goals
  • - Forces stakeholders to translate project goals
    into realistic technical objectives (creates
    communication)
  • - Identifies decisions needed to achieve project
    goals and strategies to manage decision
    uncertainty

18
Step 1 Systematic Planning
  • Components of Planning Process
  • Look at Historic Information about the site
  • Identify what contaminants may exist
  • Identify areas of concern by analysis of past use
    activities
  • Identify what measurement and sampling techniques
    you will employ
  • Develop a conceptual site model (CSM)

19
Step 1 Systematic Planning
  • Sources of site history/background information
  • Old aerial photographs
  • Compliance records
  • Interviews with employees
  • Manufacturing process/disposal records
  • Fire insurance maps

20
Step1 Systematic Planning
  • Define Possible Areas of Concern (AOC's)
  • Discharge points/chemicals discharged
  • Fuel or chemical storage tanks/spills
  • Spills/stains unknown chemicals
  • Waste disposal/mixed chemicals
  • Lagoons/chemicals embedded in sludge

21
Step 1 Systematic Planning
  • Define Possible Chemicals of Concern (COCs)
  • - Site History/Operational Records
  • - Estimate volume/amount released and time
    frame
  • - Solubility/Discharge pattern will define
    distribution
  • ( soil only or migrate to
    groundwater)
  • - What are action levels or clean up levels for
    COCs?

22
Step 1 Systematic Planning
Common forms of environmental contamination
23
Step 1 Systematic Planning
  • Conceptual Site Model (CSM)
  • Blend AOC's/COCs with site conditions
  • Geology
  • Climatology
  • Hydrogeology
  • Water supply
  • Surface features
  • Defines potential migration pathways for COCs
  • Identifies potential receptors at risk from COCs

24
Step 1 Systematic Planning
  • Contents of CSM Description
  • - Brief site summary
  • - Historical information
  • - Site maps/photographs
  • - Discussion of possible source COCs
  • - Cross section of site geology/hydrology
  • - Source/pathway/receptor diagrams
  • - Description of pathway potential receptors

25
Conceptual Site Model (CSM)
26
Step 1 Systematic Planning
  • Purpose of CSM
  • - Used to test/refine hypotheses during field
    activities
  • - Field methods produce new information in real
    time to feed into CSM
  • - Expedites interpretation revision of CSM
  • - CSM matures as site investigation progresses
  • - CSM basis for determination that SI has met
    project objectives and demob from field

27
Step 1 Systematic Planning
  • Establish Data Quality Objectives (DQOs)
  • DQOs are statements that define project specific
    decision goals (qualitative or quantitative).
    These guide the development of sampling and
    analysis plans designed to produce the right
    kind of data to support project objective.

28
Step 1 Systematic Planning
  • Data Quality Objectives (DQOs)
  • - Goal oriented statements that establish
    technical requirements for the creation of
    project decision quality data
  • - Express what project decisions the data will
    support
  • - Should not specify how data will be
    generated
  • - Distinguish between DQOs and data quality

29
Step 1 Systematic Planning
Example of a DQO Statement- The measurement
method to be chosen for this project must be able
to detect compounds X,Y and Z in groundwater at a
minimum detection limit of 10 ppb with a recovery
range of 80-120 and a precision of 20 RSD
30
Step 1 Systematic Planning Seven Stages of DQO
Planning
  • Step 1 State the problem to be addressed
  • Step 2 Identify the decision(s) to be made
  • Step 3 Identify all the inputs to the
    decision(s)
  • Step 4 Narrow the boundaries of the study
  • Step 5 Develop a decision rule(s)
  • Step 6 Develop uncertainty constraints
  • Step 7 Optimize the design for obtaining data

31
Step 1 Systematic Planning
  • Data Quality
  • - Data Quality requirements are established by
    the DQOs
  • - Data Quality ability of data to provide the
    type of information that meets users needs
  • - Must distinguish analytical method from Data
    Quality (just one part)
  • - Data Quality does not simply equate to a lab
    method
  • - Data Quality is whole sampling/analysis chain

32
Step 1 Systematic Planning
  • Data Quality
  • Good Data Quality is achieved when all components
    of sampling/analysis chain are managed
  • Analytical methods are component of Data Quality,
    but not entire basis
  • Field Lab methods can work in unison to achieve
    quality data

33
Step 1 Systematic Planning
  • Data Quality- Some Terms
  • Decision Quality Data data know to be effective
    for project decision making
  • Screening Quality Data some useful information
    provided but to uncertain to support decision
    making alone
  • Collaborative Data Sets distinct data sets (of
    varying analytical quality) used in concert with
    each other to co-manage sampling and/or
    analytical uncertainties to an acceptable level

34
Step 1 Systematic PlanningSummary-DQOs vs. DQ
  • Data Quality Objectives (DQOs)
  • Broad statements about measurement requirements
    needed to achieve project objectives
  • Data Quality (DQ)
  • Information of known quality obtained from
    sampling and analysis that is representative of
    the site and sufficient to make defensible
    decisions within stated project objectives

35
Step 1 Systematic Planning
  • Define overall characterization objectives end
    goals
  • Identify the data need to support decisions
  • Define the spatial and temporal boundaries to
    study area
  • Identify specific receptors at risk
  • Determine limits on sample collection
  • Identify clean up action levels

36
Step 2 Dynamic Work Plan
  • A guidance document that provides a framework for
    implementing an adaptive or flexible SI based
    upon field decision making

37
Step 2 Dynamic Work Plan
  • What is a Dynamic Work Plan?
  • - Guidance document for making in the field
    decisions on subsequent site activities
  • - Provides regulator approved decision trees
    that define rules for adaptive or flexible
    sampling
  • - Supported by real time data collected,
    analyzed and interpreted in the field
  • - Implemented by experienced personnel empowered
    to make decisions based upon decision logic in WP

38
Step 2 Dynamic Work Plan
  • Elements of a Dynamic Work Plan
  • Identification of field team
  • Sampling Strategies
  • Decision Rules
  • Communication Plan
  • Sample Collection Technologies
  • Quality Assurance Plan (QAP)
  • SOPs
  • Health and Safety Plan
  • Data management plan

39
Step 2Dyanamic Work Plan Technical Team
  • Assemble the project team by getting the right
    people involved
  • May include statistician, chemist, hydrologist,
  • biologist, etc.

40
Step 2 Dynamic Work PlanSampling Strategies
  • Factors that need to be considered when doing an
    assessment
  • What kind of sample?
  • Grab samples
  • Composite samples
  • Representative samples
  • Sampling methods
  • Sampling frequency
  • Sampling location
  • Sampling pattern

41
Step 2 Dynamic Work PlanSampling Strategies
Cont
  • Develop a sampling plan
  • Identify locations for sampling
  • Identify decision logic used to select sample
    locations
  • Sample splits
  • Field methods can screen sites rapidly and focus
    sampling efforts
  • Data quality needs to be considered with samples
    collected and analyzed either in the field or at
    a laboratory MUST BE A PART of your SAMPLING
    STRATEGY

42
Step 2 Dynamic Work PlanDecision Rules
  • If-then type statements
  • Define an action and alternative
  • Used to guide the investigation and anticipate
    questions that arise
  • Based on field measurement value as compared to
    an action level
  • Analytical instruments detection levels must
    meet action levels required

43
Step 2 Dynamic Work PlanDecision Rules Cont
  • Field sampling analysis technologies generate
    real time data which is the basis for the
    decision process
  • Example
  • If XRF sampling data from a 50 x 100 foot area
    indicates that the mean level of lead in soil is
    gt250 ppm (lead action level 250 ppm), then an
    additional 6 inches of soil will be excavated.

44
Step 2 Dynamic Work Plan
  • Additional Examples of Decision Rules
  • If real time conductivity probe information
    indicates a sharp contact between historic fill
    and native soil then collect soil samples
    immediately above and below the contact depth
  • If hot spot delineation samples are above project
    specific action levels then step out 10 feet in
    appropriate directions and resample

45
Step 2 Dynamic Work PlanReal Time Data
  • The basis of a Dynamic Work Plan is real time
    decision making
  • Real time decisions need real time data
  • Real time decision allows for a seamless flow of
    information during investigation
  • Results fewer mobs, less cost, more efficient

46
Step 2 Dynamic Work PlanSample Collection and
Analytical Technologies
  • Wide variety of field tools and methods
    available
  • Sampling tools must be chose to match the site
    conditions
  • Field analytical methods compatible with COCs
  • Real time analysis critical to successful
    dynamic work plan
  • In all cases, the tools chosen must generate data
    of KNOWN quality

47
Step 2 Dynamic Work Plan
  • Sample Collection Technologies and In Field
    Sensors

48
Step 2 Dynamic Work PlanSampling Collection
Technologies
  • Conventional Drilling Techniques
  • Auger
  • Rotary
  • Sonic
  • Direct-push (hydraulic) Techniques
  • Cone penetrometer
  • Hammer/push

49
Step 2 Work PlanSample Collection Technologies
  • Auger drilling
  • Most common drilling method
  • Useful for subsurface soil description and
  • sampling of soil groundwater
  • Sensors or samples are advanced ahead of the
    cutting bit
  • Cannot be used in consolidated bedrock

50
Geoprobe
6600 flatbed
model
51
Step 2 Work PlanSample Collection Technologies
  • Rotary drilling
  • Generally applied to soils that contain boulders
    or in bedrock conditions
  • Uses drilling fluids to maintain hole integrity
  • Produces drilling mud wastes that will need
    handling
  • Sonic drilling
  • Uses vibration to drive sampling tool
  • More expensive than other methods
  • Produces less waste

52
Step 2 Work PlanSample Collection Technologies
  • Cone penetrometer method
  • Can use physical and chemical sensors
  • Static reaction force/pressed into ground
  • real-time analysis with sensors
  • Direct Push/Hammer method
  • Uses static force and dynamic loading
  • Smaller more portable
  • Collect groundwater and soil samples

53
Step 2 Work PlanCone Penetrometer Truck
54
Geoprobe
6600/PC111
model
55
Geoprobe
5410
model
56
Geoprobe
540B
model
57
Dual Tube 21 Soil Sampling System
58
Collecting Soil Samples from Push Technology Soil
Cores
59
Dual Tube Profiler
60
Step 2 Dynamic Work PlanIn Field Sensors
  • Sensors can be attached to push units to collect
    real time data on subsurface conditions
  • Examples of sensors are
  • soil conductivity
  • laser induce florescence (LIF)
  • MIPS, etc

61
Step 2 Dynamic Work PlanIn Field Sensors
  • Soil Conductivity Sensor
  • Used to determine soil lithology
  • Driven into soil by push unit rig
  • Measures soil electrical conductance
  • Real time readout allows identification of soil
    strata changes in the field
  • Also will identify unusual zones in soil or fill
  • Field decision to focus sampling at strata
    interfaces or at soil anomalies

62
Conductivity Probe for Real Time Soil Stratigraphy
63
Field Computer Used to Perform Real Time
Interpretation of
Conductivity Probe Data
64
Electrical Conductivity Log
65
Step 2 Dynamic Work Plan In Field Sensors
  • Fuel Florescence Sensor
  • Rapid delineation of aromatic hydrocarbons
  • Map a fuel spill plume
  • Detects florescence produced by fuels when
    excited by UV light
  • Probe pushed by CPT or push unit rig
  • Continuous real time measurement over entire
    depth
  • Data viewed graphically in real time on computer
    screen

66
Step 2 Dynamic Work Plan In Field Sensors
  • Permeable Membrane Interface Probe
  • Determine position and approx. concentration of
    VOCs in soil
  • Tool is driven into soil with push unit
  • Membrane window on probe
  • VOCs in soil/liquid adsorb on to membrane
  • Diffuse across membrane into probe
  • Carried to surface by gas sweep
  • Detector at surface used to measure VOC
    concentration

67
Membrane Interface Probe and Log
68
Membrane Interface Probe (MIP)
69
Step 2 Dynamic Work Plan
  • Direct Push Installed Microwells
  • Small diameter prepacked wells that can be
    installed with push unit
  • Rapid, inexpensive method for groundwater
    sampling
  • Studies by US Navy has shown sampling results to
    be comparable to conventional wells

70
Prepacked Screen
Monitoring Wells
71
Step 2 Dynamic Work Plan
  • Field Analytic Methods (FAMs)

72
Step 2 Dynamic Work Plan
  • Common accepted FAMs will be discussed
  • Some have formal USEPA SW-846 acceptance
  • Many are modifications of standard methods
  • Available from range of vendors

73
Field Gas ChromatographyLevels of Sophistication
  • Field screening i.e. OVM,OVA,Hnu
  • Field GC i.e. Photovac
  • Field portable i.e. Tri-Corder, Viking
  • Field Transportable i.e. laboratory grade GC
    GC/MS

74
Field Gas Chromatography Methods
  • Miniaturized, rugged version of a laboratory GC
  • Consists of injection port, isothermal column,
    carrier-gas, column, data system and detector
  • A mixture of analytes are moved through the
    column and separated, then detected by a detector
    system (ECD Electron Capture Detector, ELCD
    Electrolytic Conductivity Detector, TCD Thermal
    Conductivity Detector, NPD Nitrogen-Phosphorus
    Detector, Mass Spectrometer)

75
Field portable Photovac GC operated out of the
back of a van
76
Field prepared sample extracts for injection into
field GC
77
Field portable GC/MS System
78
Direct Sampling Ion Mass Spectrometry (DSITMS)
  • Newly approved method for measuring VOCs in soil,
    water, soil gas gas (method 8265)
  • Rapid quantitative measurement, continuous real
    time monitoring
  • Sample materials are introduced directly into ion
    trap MS
  • Little sample preparation no chromatographic
    separation
  • Response of instrument is nearly instantaneous
  • Instrument is rugged relatively easy to operate
    maintain

79
Tri-Corders Environmental, Inc.
Direct Sampling Ion Trap Mass Spectrometry
(DSITMS)
Instrument
80
Tri-Corders DSITMS Rig
81
Field Mobile Laboratories
  • Transport laboratory grade instruments to field
  • Run standard method or modified methods
  • Full range of analytical parameters
  • Integrates with FAMs to provided QA/QC backup
    low detection limits

82
Field Transportable GCs GC/MS
Interior of Mobile Laboratory Showing GC and
GC/MS
Equipment
83
Field Gas Chromatography Applications
  • Compounds Identified
  • VOCs
  • SVOCs
  • PAHs, PCBs, pesticides, herbicides, dioxin,
    phenols phthalates, amines, amides
  • Extraction Methods
  • Soxhlet, liquid-liquid, or sonication
  • Abbreviated field methods
  • Accelerated solvent extraction (ASE)
  • Microwave-assisted extraction (MAE)

84
Field Gas ChromatographyApplications
  • Media Analyzed
  • Ambient Air Gases
  • Soil Gas
  • Liquids
  • Soil by extraction

85
Field Gas ChromatographyAdvantages
  • Rapid turnaround of results
  • Cost effective
  • Provides real-time information
  • Flexible
  • Provide compound specific identification of COCs

86
Field Gas ChromatographyLimitations
  • Requires higher level of operator sophistication
  • Data comparability i.e. Head space vs. purge
    trap
  • Collaborative data may be required
  • Performance may be impacted by sample preparation

87
Field Gas ChromatographyData Quality
  • Operator experience fundamentally impacts data
    quality
  • Requires calibration curve
  • Blanks mid-level cal checks as needed
  • Sample preparation techniques will greatly impact
    performance
  • Soil head space data considered order of
    magnitude level

88
Field Gas ChromatographyExamples of Vendors
  • Perkin Elmer formerly Photovac
  • Inficon
  • Viglent formerly MIT Analytical Instruments
  • SRI Instruments
  • Sensidyne, Inc.

89
Immunoassay
  • Takes advantage of the ability of antibodies to
    selectively bind to the target analytes in a
    sample matrix, such as soil and water.
  • Very selective and compound specific is capable
    of giving very low detection limits for a variety
    of compound classes

90
Immunoassay
Schematic of Antibody - Antigen Interaction  
                                                  
         
91
Immunoassay Operation
  • Antibody-coating
  • Sample and enzyme conjugate addition
  • Competitive binding reaction
  • Color formation
  • Measurement of color

92
Immunoassay Analytes and DLs
93
ImmunoassayAdvantages
  • Field Portable
  • Little training time
  • Rapid
  • Inexpensive
  • Wide range of analytes
  • Low detection limits

94
ImmunoassayLimitations
  • Prior knowledge of analytes present at site
  • Reagents may need to be refrigerated
  • Cross reactivity to similar compounds (false
    positives)
  • Semi quantitative analysis in some cases
  • Under certain circumstances not compound specific

95
ImmunoassayExamples of Vendors
  • Strategic Diagnostics a wide assortment of
    tests
  • BioNebraska Inc. mercury test
  • New Horizons Diagnostics SMART Test

96
Ultraviolet (UV) Florescence
  • Used to measure variety of petroleum hydrocarbons
    in soil and water
  • Compounds include TPH fuel oils, PAHs, BTEX, PCBs
    and diesel fuel
  • Samples are first extracted in solvent and the
    analyzed on a portable ultraviolet fluorometer
  • High sample throughput, low measurement cost

97
Ultraviolet (UV) Fluorescence
  • Theory of operation
  • Relies on the electronic configuration of the
    molecular structure of COC
  • Aromatic hydrocarbons excite and emit energy at
    specific wavelengths
  • Fluorescence response of sample is quantified by
    UVF instrument
  • Instrument is calibrated using certified
    standards sensitive to the wavelengths of
    interest

98
Ultraviolet (UV) Fluorescence
Ultraviolet fluorescence equipment in field
laboratory
99
Ultraviolet (UV) Fluorescence
  • Advantages
  • High sample throughput (5 min per sample)
  • Ease to use
  • Low measurement cost (less than 20/sample)
  • Detection limits as low as 50 to 100 ppb
  • Compares well to conventional methods

100
Ultraviolet (UV) Fluorescence
  • Disadvantages
  • Not compound specific (measures groups of
    compounds)
  • Subject to matrix interference due to spectral
    overlap of different luminescent compounds
  • Difficulty in distinguishing individual compound
    groups in samples with a broad range of
    hydrocarbons

101
Ultraviolet (UV) Fluorescence
  • QA/QC
  • Chose a UVF calibration to best match the most
    dominant source of contamination
  • Periodically analyze 1 or 2 calibration standards
    as if they were samples to test for instrument
    drift
  • Periodically check Methanol by running a solvent
    blank
  • Keep glass cuvette clean of excess liquid or
    fingerprints
  • Before running samples perform 5 point
    calibration using supplied standards

102
Energy Dispersive X-ray Fluorescence
NHSRC
  • Scope and application
  • Metals in soil and sediment
  • Lead in paint and house dust
  • Metals in air filters
  • Metals in water

103
X-Ray Fluorescence
  • Theory of Operation
  • Sealed radioisotope source used to irradiate
    sample with x-rays
  • Electrons in atomic structure adsorb x-rays
  • Electron is ejected from atom
  • Vacancy created from electron being ejected is
    filled by a more outer shell electron
  • In dropping to lower energy level, electron gives
    off energy in form of x-rays
  • Energy is characteristic to a particular metal,
    which is identified by detector
  • Number of x-rays detected is concentration

104
X-Ray Fluorescence
  • Three modes of Sample Analysis
  • Point and Shoot mode is when instrument is
    placed directly on soil and reading taken
  • Plastic bag mode is when sample is place in
    plastic bag and reading is taken through bag
  • Prepared bulk sample is when sample is dried,
    ground and sieved before analysis.
  • Sample preparation minimizes effects of moisture,
    large partial size and partial size variation

105
X-Ray Fluorescence
Instrument being used in point and shoot mode
106
X-Ray Fluorescence
Soil sample being analyzed using plastic bag
method
107
X-Ray Fluorescence Interferences
NHSRC
  • Physical matrix effects
  • Moisture content
  • Inconsistent positioning of samples
  • Chemical matrix effects (absorption and
    enhancement phenomena)
  • Spectral interferences (peak overlaps)

108
X-Ray FluorescenceGeneral Detection Limits
  • Detection Limits- 60 sec test
  • sand matrix SRM matrix
  • Cr 220 ppm 420 ppm
  • Zn 40 ppm 70 ppm
  • Ni 100 ppm 210 ppm
  • As 20 ppm 25 ppm
  • Pb 20 ppm 30 ppm
  • Hg 25 ppm 40 ppm
  • Cd 35 ppm 50 ppm
  • Cu 70 ppm 100 ppm
  • Co 120 ppm 380 ppm
  • Detection Limits- 120 sec test
  • sand matrix SRM matrix
  • Cr 150 ppm 300 ppm
  • Zn 25 ppm 50 ppm
  • Ni 70 ppm 150 ppm
  • As 10 ppm 15 ppm
  • Pb 10 ppm 20 ppm
  • Hg 15 ppm 25 ppm
  • Cd 25 ppm 35 ppm
  • Cu 50 ppm 60 ppm
  • Co 80 ppm 270 ppm

109
X-Ray Fluorescence QA/QC
NHSRC
  • Energy calibration checks
  • Blanks
  • Instrument
  • Method
  • Calibration verification checks
  • Precision
  • Detection limits dependent upon sample
    preparation
  • Reporting results i.e. sample preparation
    analysis time

110
X-Ray Fluorescence Advantages
  • Portable
  • Fast analysis
  • Multi-element analysis technique
  • No waste generated
  • Easy to operate
  • Little sample preparation
  • Nondestructive technique
  • Low cost of operation

111
X-Ray FluorescenceLimitations
  • Relatively high detection limits
  • Sample preparation dependent
  • Matrix-variable results (interferences)
  • Mostly applicable to soil rather than water
  • Radioactive sources requires special permits

112
X-Ray Fluorescence Examples of Vendors
  • Advanced Analytical Products Services
  • NITON Corporation
  • Assoma Instruments Inc.
  • Metorex Inc.
  • Rigaku/USA, Inc.
  • Spectrace

113
Colorimetric Indicator Tubes
  • Primarily used for Health and Safety these kits
    provide on-site rapid detection of a wide range
    of contaminants in soil, air and water. They
    have relatively low costs too.

114
Colorimetric Indicator Tubes
115
Colorimetric Indicator TubesOperation
  • Theory of operation varies for each kit but most
    use a color change when the substance is present
    or not. The degree of color is typically
    proportional in some way to the concentration

116
Colorimetric Indicator TubesApplications
  • Used for Health and Safety
  • Monitors Air contaminants
  • Measures VOCs and other gases

117
Colorimetric Indicator TubesAdvantages
  • Quick
  • Inexpensive
  • Does not require a trained operator
  • Wide range of contaminants
  • Wide range of matrices

118
Colorimetric Indicator TubesLimitations
  • Typically qualitative
  • Does require some training
  • Potential interference
  • Non specific
  • Color-blind - impossible

119
Colorimetric Indicator Tubes Examples of Vendors
  • Hanby Field Test Kits
  • Dexsil Co.
  • Chlor-N-Oil
  • Chlor-N-Soil
  • PetroFLAG
  • AccuSensor
  • Envirol Quick Test
  • Hanna Instruments
  • Neogen Corp.
  • CHEMetrics

120
Laser induced Fluorescence
  • LIF provides a real-time, in situ, field
    screening of petroleum hydrocarbons in subsurface
    soil and groundwater. This method can guide an
    investigation or removal or delineate boundaries
    of subsurface contamination prior to installing
    monitoring wells or taking soil samples

121
Laser induced Fluorescence
122
Laser induced FluorescenceOperation
  • Laser excitation
  • Transmission of signal back to the truck
  • Analysis of data
  • Static mode
  • On the fly
  • Geophysical information combined with analytical
    data

123
Laser induced FluorescenceApplication
  • Measures TPH, PAHs and other organics that
    fluoresce
  • SCAPS (Site Characterization and Analysis
    Penetrometer System)
  • ROST (Rapid Optical Screening Tool)
  • Uses Lasers down hole device on the fly
    measurement

124
Fluorescence Fiber Optic AnalyzersApplication
  • Measures TPH, BTEX and PAHs to the ppb level
    on-site
  • Simple to use
  • Need to perform instrument calibration
  • Need preliminary GC/MS data to develop
    correlation
  • Can look at various groups of PAHs if combined
    with chromatography

125
Laser induced Fluorescence
  • Advantages
  • Rapid Real-time data
  • Spatial resolution
  • No drill cuttings
  • Limitations
  • Poor quantitative correlation
  • Cost on small projects
  • Stratigraphy constraints
  • Depth
  • Potential interferences

126
Laser induced Fluorescence Examples of Vendors
  • FCI Environmental Inc.
  • Geotech Environmental Equipment Inc.
  • Gregg Drilling and Testing Inc.
  • Noverflo Inc.
  • O.K. Optik Keramik Technologies
  • Osmonics
  • Savannah River Technology Center
  • Applied Research Associates

127
Analyze Immediately Parameters
  • Probed sensors designed to give immediate
    information
  • Now available with multiple sensors on one probe
  • Example In Situ Troll 9000 Low Flow Sampling
    System
  • One probe DO, conductivity, temp, pH, ORP,
    salinity, depth, turbidity, TDS
  • Field download to data logger or computer for
    instant readouts or trend analysis
  • Used for water quality profiling/surveys, GW
    sampling long term monitoring

128
Water Quality Parameters
  • Simple field based water quality tests for up to
    50 parameters
  • Test for dissolved metals, pH, sulfides,
    hardness, nitrate, COD and many more
  • Colorimetric or photometric analysis using
    pre-measured reagents
  • Need to know expected range of target parameter
    concentration to select correct kit
  • Parameter specific kits available if testing for
    limited number of analytes

129
Emerging Field Analytical Technologies
  • Primarily originate from USDOD USDOE research
    activities
  • Development of sensors for in-situ analysis of
    specific analytes such as Cr6 BTEX
  • Development of field deployable methods for to
    locate DNAPL in subsurface
  • Development of improved computer visualization of
    field generated data

130
Dynamic Work Plan
  • Selecting the Appropriate Field Analytical
    Methods (FAMs)

131
Step 2 Dynamic Work PlanFAM Selection
  • Important Selection Considerations
  • Method detection limits vs. action levels
  • Compound specific vs. groups of compounds
  • Training requirements
  • Performance history
  • 3rd party verification
  • Ease of use

132
Step 2Dynamic Work Plan FAM Selection
  • Additional Consideration Items
  • -Availability/vendor support
  • -Cost/time advantage
  • -Maximum sample through-put rate
  • -Regulatory acceptability
  • -Matrix compatibility
  • -Approved SOPs

133
Step 2 Dynamic Work PlanFAM Selection Process
  • Identify the compounds requiring analysis
  • Identify matrix (soil, water, air, sediments)
  • Identify regulatory action levels needed to be
    achieved
  • Identify appropriate FAMs
  • Evaluate FAMs based upon selection criteria
  • If necessary, perform site specific pilot test

134
Step 2 Dynamic Work PlanFAM Selection Process
  • Pilot Test to Demonstrate FAM Performance
  • Collect several representative site samples
  • Collect from various matrix and range of
    anticipate COC concentrations
  • Prepare samples as per FAM field procedures
  • Analyze samples using FAM along with appropriate
    QA/QC samples
  • Confirm results with standard fixed baser methods
  • Evaluate results using statistical comparison

135
Step 2Dynamic Work planQuality Assurance Plan
(QAP)
  • Elements of a QAP
  • Define project objective
  • Establish data requirements (I.e. action level
  • Discuss sampling rational and approach
  • Define sampling methods
  • Define analytical methods
  • Identify quality control procedures
  • Standard operating procedures (SOPs)
  • Data management procedures
  • Data validation methods

136
Step 2 Dynamic Work plan QAP FAM data quality
concerns
  • Sample representativeness
  • Matrix interferences
  • Method calibrations
  • Instrument stability
  • Ability of operator
  • Adherence to Method/SOPs
  • Documentation defensibility/record keeping
  • Defined accuracy precision

137
Step 2 Work plan Standard Operating Procedures
(SOPs)
  • Used to establish protocols and procedures for
    sampling and analysis
  • Why are SOPs important?
  • Provides necessary control of data quality
  • Uniform methods for instrument operation
  • Identify QA/QC steps
  • Identification of method modifications

138
Step 2 Work planExamples of SOPs
  • Sample chain of custody procedures
  • Field log book documentation
  • Sample storage, preservation and handling
  • Soil sampling using direct push methods
  • Groundwater sampling from monitoring wells
  • Use of XRF for the determination of metal
    concentrations in soil and sediment
  • Soil screening for PAHs by immunoassay
  • VOCs in soil using equilibrium headspace analysis

139
Step 2 Work plan SOPs Cont..
  • Include copies of the SOPs in the work plan for
    reference by field team

140
Step 2 Work plan Health and Safety Plan (HSP)
  • Defines protective clothing/gear
  • Identifies emergency procedures
  • Establishes site safety officer and decision
    making responsibility
  • Discusses hazards of potential contaminants of
    concern
  • Identifies safety monitoring equipment and
    procedures

141
Step 3 Field Implementation
  • Taking the Dynamic Work Plan to the Field and
    Performing a FAM Based Program

142
STEP 3 Field Implementation
  • YOUR IN THE FIELD!
  • Mobilization
  • Field communication
  • Field quality control
  • Field data management
  • Data feedback loop

143
STEP 3 Field ImplementationMobilization
  • Organization of field team
  • Acquire field methods/instruments
  • Subcontractors (drilling, soil sampling,
    instrumentation, surveying)
  • Access/utility mark out
  • Field laboratory setup

144
STEP 3 Field ImplementationField Communication
  • Identify all parties who contribute to decisions
    (stakeholders)
  • Establish chain of decision command
  • Identify key decision maker (field team leader)
  • Arrange for regular communication times (i.e. at
    end of each day)
  • Establish mode of communication (i.e. radio, cell
    phone, internet)

145
STEP 3 Field Implementation Field Data
Management
  • Proper data handling
  • Recording information
  • Ensuring proper sample transfer
  • Comparing field results to the laboratory
  • Confirmation
  • How much do you need?
  • Data storage/display

146
Step 3 Field ImplementationConceptual Site Model
  • Daily Cycle to Refine CSM
  • Step 1- Collect samples at location identified
    during previous day planning
  • Step 2- Analyze sample with appropriate FAMs
  • Step 3- Evaluate results within the context of
    the site CSM
  • Step 4 IF results complete CSM picture then
    move to next study location
  • IF results do not complete CSM picture plan
    next days sampling program
  • Step 5- Continue until site wide CSM is
    complete enough to meet project objectives

147
Data Quality vs. Information
148
Improve Decision Quality--Manage Uncertainties
From This
To This
149
Marrying Analytical Methods to Make Sound
Decisions Involving Heterogeneous Matrices
Costly definitive analytical methods
Cheaper/screening analytical methods
Collaborative Data
150
Step 3 Field ImplementationUse of Collaborative
Data
  • Blended data sets that compliment each other
  • Sample representativeness is managed by high
    density sampling using cheaper methods
  • Analytical uncertainty is managed by using more
    rigorous methods
  • Together these data sets remove uncertainty,
    providing decision quality data
  • Usually more cost effective than using a single
    technique to manage sampling analytical
    uncertainty

151
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152
Step 3 Field Implementation Field Decision
Assist Software
  • Spatial Analysis and Decision Assistance (SADA)
  • Downloadable modules to assist data
    visualization, statistical analysis, sampling
    design decision analysis
  • http//www.sis.utk.edu/cis/sada
  • Field Integrated Environmental Location Decision
    Support (FIELDS) software
  • Integrates various information systems (GIS,
    GPS, imaging, etc) to facilitate site
    characterization decision making
  • http//www.epa.gov/region5filds

153
STEP 3 Field ImplementationConfirmation/Verific
ation Samples
  • Delineate extent of impacted area
  • Establish clean zone
  • Used to obtain regulatory approval
  • Define end points of investigation
  • Usually require standard methods analysis with
    full QA/QC documentation
  • Number will depend upon the information value of
    the collaborative data set

154
Step 4 Data Evaluation Reporting
  • Telling the World What You Just Found Out About
    the Site

155
Step 4 Data Evaluation Reporting
  • Data validation/usability verification
  • Compiling Assembling Data
  • Integrate data into the CSM
  • Verify assumptions
  • Generate findings/conclusions
  • Reporting results

156
Step 4 Data Evaluation ReportingData
Validation
  • Review data vs. study objectives DQOs
  • Review implemented sampling vs. DWP decision
    rules
  • Do decision rules support sampling sequence
    patterns
  • Review field documentation for completeness
  • Evaluate sample blanks for field contamination
  • Review FAM applications with regard to SOP
    specified QA/QC procedures

157
Step 4 Data Evaluation ReportingData
Validation
  • Evaluate data against instrument performance
    criteria
  • Review confirmation/verification sample results
    relative to FAM performance
  • Review confirmation/verification sample results
    relative to site specified action levels
  • This is an analysis of data usability

158
Step 4 Data Evaluation ReportingData
Compiling Assembly
  • Organize data
  • Tables, databases, boring logs, etc
  • Display data
  • Maps, GIS, cross sections
  • visualization/imaging
  • Reduce data
  • Identify important data
  • Calculations to support data (i.e. GW flow rates)

159
Step 4 Data Evaluation ReportingData
Interpretation
  • Statistical tests
  • Comparison against action levels
  • Verify CSM assumptions
  • Refine CSM based upon delineations
  • Compare findings to original objectives
  • Evaluate receptor exposure
  • Develop conclusions

160
Step 4 Data Evaluation Reporting Data
Interpretation
  • Statistical test
  • Select the statistical hypothesis test
  • Identify key assumptions that underlie the test
  • One sample tests are used when comparing sample
    results from a single data set against a fixed
    threshold value such as an action limit
  • Two sample test are used when comparing sample
    results from two data sets such as comparing
    concentrations of samples at a site with off site
    background concentrations of contaminants

161
Step 4 Data Evaluation ReportingData
Interpretation
  • Verifying the Assumptions
  • Determine if statistical test can be used for the
    data set
  • Identify an approach to verifying the key
    assumptions
  • Perform the tests necessary to verify assumptions
  • Identify corrective actions if necessary

162
Step 4 Data Evaluation Reporting Data
Interpretation
  • Drawing Conclusions based on the data
  • Perform the appropriate statistical tests
  • Evaluate information completeness with regard to
    original project objectives
  • Evaluate the performance of the sampling design
    to achieve project objectives
  • Evaluate exposure scenarios
  • Evaluate delineation vs. action levels

163
Step 4 Data Evaluation ReportingConclusions
  • Did original AOC's create impacts above action
    levels?
  • If impacts have occurred, have they been
    delineated to action levels?
  • What is the appropriate remedial approach?
  • Is there enough data to design cost remedial
    approach?
  • Are receptors at risk and level of risk?

164
Step 4 Data Evaluation ReportingReporting
  • Organize data into tables, graphs, figures
  • Refine conceptual model
  • Discuss usability of data
  • Develop text to describe the data and finding
  • Prepare draft for review

165
Summary
  • The performance of Field Analytical Methods
    (FAMs) have significantly improved over the last
    five years
  • FAMs, combined with field decision making
    (dynamic work plans) greatly improve the
    efficiency of site investigations (SIs)
  • Conceptual site model is constantly upgraded as
    new site data is developed

166
Summary
  • SIs that rely on dynamic work plans must be
    designed to produce decision quality data in
    the field
  • Collaborative data sets are the basis for
    creating decision quality data
  • Regulatory acceptance for this type of an
    approach to implementing SIs is growing

167
Exercise- Case Study
  • Remember the Case Study?
  • Will use it to do the exercise
  • Focus on the Underground (USTs) Tank Area
  • Four USTs excavated removed- known to have
    leaked
  • Delineate BTEX impacts in soil GW

168
Field Analytical Method
  • Will use the DTECH BTEX Test Kit (SDI)
  • Designed to provide quick, reliable semi
    quantitative test results
  • Based upon immunoassay technology
  • Develops a color that is inversely proportional
    to concentration of BTEX in sample
  • Measures soil in PPM and water in PPB
  • One kit contains does four tests

169
DTECH Test ProcedureSoils
  • Break up soil so it is fairly uniform
  • Perform extraction using DTECH BTEX Soil
    Extraction Pac procedures
  • Transfer extract to DTECH BTEX Test Kit
    workstation
  • Mix extract with various reagents as per test kit
    instructions
  • Interpret results using kit supplied color card
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