United States
Environmental Protection
Agency
&EPA
Office of Research and
Development
Washington DC 20460
EPA/540/R-95/515
August 1995
HNU-Hanby PCP
Immunoassay Test Kit
Innovative
Evaluation
Technology
Report
SUPERFUND
TECHNOLOGY
INNOVATIVE
EVALUATION
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CONTACT
Jeanette Van Emon and Steve Rock are the EPA contacts for this report. Jeanette Van Emon is presently
with the new Characterization Research Division (formerly the Environmental Monitoring Systems
Laboratory) in Las Vegas, NV, which is under the direction of the National Exposure Research Laboratory
with headquarters in Research Triangle Park, NC.
Steve Rock is presently with the new Land Remediation and Pollution Control Division (formerly the Risk
Reduction Engineering Laboratory) in the newly organized National Risk Management Research Laboratory
in Cincinnati, OH.
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EPA/540/R-95/515
August 1995
HNU-HANBY PCP IMMUNOASSAY TEST KIT
INNOVATIVE TECHNOLOGY EVALUATION REPORT
NATIONAL RISK MANAGEMENT RESEARCH LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
NATIONAL EXPOSURE RESEARCH LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
LAS VEGAS, NEVADA 89193
Printed on Recycled Paper
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Notice
The information in this document has been funded wholly or in part by the U.S. Environmental Protection
Agency (EPA) in partial fulfillment of Contract No. 68-CO-0047, Work Assignment No. 0-40, to PRC
Environmental Management, me. It has been subject to the Agency's peer and administrative review, and it
has been approved for publication as an EPA document. The opinions, findings, and conclusions expressed
herein are those of the contractor and not necessarily those of the EPA or other cooperating agencies.
Mention of company or product names is not to be construed as an endorsement by the agency.
11
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Foreword
The U.S. Environmental Protection Agency is charged by Congress with protecting the Nation's land,
air, and water resources. Under a mandate of national environmental laws, the Agency strives to formulate and
implement actions leading to a compatible balance between human activities and the ability of natural systems
to support and nurture life. To meet this mandate, EPA's research program is providing data and technical
support for solving environmental problems today and building a science knowledge base necessary to manage
our ecological resources wisely, understand how pollutan s affect our health, and prevent or reduce environmental
risks in the future.
The National Risk Management Research Laboratory is the Agency's center for investigation of
technological and management approaches for reducing risks from threats to human health and the environment.
The focus of the Laboratory's research program is on methods for the prevention and control of pollution to air,
land, water and subsurface resources; protection of water quality in public water systems ; remediation of
contaminated sites and ground water; and prevention and control of indoor air pollution. The goal of this research
effort is to catalyze development and implementation of innovative, cost-effective environmental technologies;
develop scientific and engineering information needed, by EPA to support regulatory and policy decisions; and
provide technical support and information transfer
regulations and strategies.
This publication has been produced as part of the Laboratory
published and made available by EPA's Office of Research
to link researchers with their clients.
to ensure effective implementation of environmental
's strategic long-term research plan. It is
and Development to assist the user community and
E. Timothy Oppelt, Director
National Risk Management Research Laboratory
111
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Abstract
This innovative technology evaluation report describes a demonstration of the HNU-Hanby Environmental Test Kit for
determining pentachlorophenol (PCP) contamination hi soil. This kit was demonstrated in Morrisville, North Carolina,
in August 1993. The objective of this demonstration was to evaluate the technology by comparing its results to those from
a confirmatory laboratory that used standard EPA-approved analytical methods. The HNU-Hanby test kit can provide
PCP results only in samples that also contain a petroleum hydrocarbon carrier such as gasoline, kerosene, diesel fuel,
or fuel oil. The test kit uses the Friedel-Crafts alkylation reaction to detect the petroleum hydrocarbons. This reaction
is colorimetric. A reflective photometer is used to quantitatively measure the reaction color. A site-specific calibration
is needed to determine the ratio of PCP to carrier solvent. This ratio is then used to correct the results from the reflective
photometer.
Hie detection limit reported by the test kit's developer is 1.0 part per million (ppm) for soil samples. A 5.0 ppm detection
limit was used for this demonstration. The elevated detection limit was the result of reducing the sample mass used for
extraction. During the demonstration, 47 soil samples were extracted and analyzed. The precision of the test kit was
determined to be statistically the same as the precision of the confirmatory laboratory. The accuracy of the kit's data set
was evaluated as a whole and by concentrations less than and greater than 100 ppm PCP. When the entire data set was
evaluated, the test kit's results were determined to be statistically different from the confirmatory results. This was also
the case for samples in which the PCP concentrations were greater than 100 ppm. The test kit's data for samples
containing less than 100 ppm PCP was shown to be statistically similar to the corresponding confirmatory data. Based
on this evaluation, the test kit produced Level 1 data for samples containing greater than 100 ppm PCP and Level 2 data
for samples containing less than 100 ppm PCP. This indicates that there was a concentration effect oh the test kit's
accuracy. The test kit showed greater comparability to the confirmatory data when PCP concentrations in samples were
below 100 ppm.
This report was submitted hi partial fulfillment of 68-CO-0047 WA 0-40 by PRC Environmental Management, Inc.
(PRC), under sponsorship of the U.S. Environmental Protection Agency. This report covers a period from July 1, 1993,
to August 31, 1993, and work was completed as of February 1, 1994.
IV
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Table of Contents
Section
Notice
Foreword
Abstract
List of Figures
List of Tables
List of Abbreviations and Acronyms
Acknowledgments
1 Executive Summary
2 Introduction
EPA's Site Program and MMTP: An Overview
The Role of Monitoring and Measu
Defining the Process
Components of a Demonstration
Rationale for this Demonstration
Demonstration Purpose, Goals, and Objec
ives
3 Predemonstration Activities
Identifying Developers
Selecting the Sites
Selecting the Confirmatory Laboratory and
Training Technology Operators
Predemonstration Sampling and Analysis .
Analytical Methods
Demonstration Design and Description
Implementation of the Demonstration Plan
Field Modifications to the Demonstration PI
Data Collection
Statistical Analysis of Results
an
Confirmatory Analysis Results
Confirmatory Laboratory Procedures . . .
Sample Holding Times '.
Sample Extraction
Detection Limits and Initial and Continuing Calibrations
ement Technologies
..ii
. iii
. iv
. vii
. vii
viii
. ix
. 1
. 3
. 3
. 3
. 3
. 4
. 4
. 5
. 6
. 6
. .6
. 7
. 7
. 7
. 8
. 8
. 8
. 8
. 9
11
11
11
11
11
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Table of Contents (Continued)
Section
Page
Sample Analysis 12
Quality Control Procedures 12
Data Reporting 12
Data Quality Assessment ' 13
Confirmatory Laboratory Costs and Turnaround Times 14
6 HNU-Hanby Environmental Test Kit 15
Operational Characteristics 16
Performance Factors 17
Intramethod Assessment 17
Comparison of Results to Confirmatory Laboratory Results 18
7 Applications Assessment 21
8 References 22
VI
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List of
Figure
6-1 Regression of Data
List of Tables
5-1 Matrix Spike and Matrix Spike Duplicate Resu
6-1 Calibration Data
6-2 Laboratory Duplicate Results
6-3 Field Duplicate Results
6-4 Summary of Demonstration Data
6-5 Summary of Regression and Residual Results
Figures
Page
.. 20
Page
ts
13
15
18
18
19
20
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List of Abbreviations and Acronyms
DCAA 2,4-dichlorophenylacetic acid
EMSL-LV Environmental Monitoring Systems Laboratory-Las Vegas
EPA Environmental Protection Agency
ERA Environmental Research Associates
GC gas chromatograph
GC/MS gas chromatograph/mass spectrograph
IDW investigation-derived waste
ITER Innovative Technology Evaluation Report
Koppers Koppers Company
fig/kg micrograms per kilogram
mg/kg milligrams per kilogram
MMTP Monitoring and Measurement Technologies Program
NRMRL National Risk Management Research Laboratory
ORD Office of Research and Development
OSWER Office of Solid Waste and Emergency Response
PCP pentachlorophenol
PE performance evaluation
ppm part per million
PRC PRC Environmental Management, Inc.
QADE Quality Assurance and Data Evaluation
QA/QC quality assurance/quality control
QAPjP quality assurance project plan
p correlation of determination
RCRA Resource Conservation and Recovery Act
RECAP Region 7 Environmental Collection and Analysis Program
RPD relative percent difference
SARA Superfund Amendments and Reauthorization Act of 1986
SITE Superfund Innovative Technology Evaluation
SMO Sample Management Office
SVOC Semivolatile Organic Compound
VIII
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Acknowledgments
This demonstration and the subsequent preparation of this report required the services of numerous personnel from the
Environmental Protection Agency, Envkonmental Monitoring Systems Laboratory (Las Vegas, Nevada); Environmental
Protection Agency, Region 7 (Kansas City, Kansas); HNU-Hanby Systems (Houston, Texas); HNU Systems (Boston,
Massachusetts); Beazer East, Inc. (Pittsburgh, Pennsylvania); Winona Post, Inc. (Winona, Missouri); and PRO
Environmental Management, Inc. (Kansas City, Kansas; Cincinnati, Ohio; and Chicago, Illinois). The cooperation and
efforts of these organizations and personnel are gratefully acknowledged.
IX
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Section 1
Executive Summary
This innovative technology evaluation report (ITER)
presents information on the demonstration of the HNU-
Hanby Environmental Test Kit for determining penta-
chlorophenol (PCP) contamination in soil. This screen-
ing kit was demonstrated in Morrisville, North Carolina,
in August 1993. The demonstration was conducted by
PRC Environmental Management, Inc. (PRC), under
contract with the Environmental Protection Agency's
(EPA) Environmental Monitoring Systems Labora-
toryLas Vegas (EMSL-LV). The demonstration was
developed under the Monitoring and Measurement
Technologies Program (MMTP) of the Superfund
Innovative Technology Evaluation (SITE) Program.
This technology was demonstrated in conjunction
with four other field screening technologies: (1) the
Penta RISc Test System developed by EnSys Incorpor-
ated, (2) the EnviroGard PCP Test Kit developed by the
Millipore Corporation, (3) the Penta RaPID Assay
developed by Ohmicron Corporation, and (4) the Field
Analytical Screening Program PCP Method developed
by EPA's Region 7 through its Superfund Program. The
results of the demonstrations of these other technologies
are presented in separate reports similar to this one.
The objective of this demonstration was to evaluate
the HNU-Hanby test kit for accuracy and precision at
detecting high and low levels of PCP in soil samples by
comparing its results to those from a confirmatory
laboratory that used standard EPA-approved analytical
methods. These EPA-approved methods are used to
provide legally defensible analytical data for the purpose
of monitoring or for the enforcement of environmental
regulations. Because these EPA-approved methods are
used by the regulatory community, they also were used
for this demonstration for comparison of results. While
these methods may include inherent tendencies which
may bias data or may include procedures with which
developers disagree, they are the best methods for
providing legally defensible data as defined by the
regulatory community. To remove as much of these
inherent tendencies as possible, PRC used post hoc
residual analysis to remove data outliers. The HNU-
Hanby test kit also was qualitatively evaluated for the
length of time required for analysis, ease of use, porta-
bility, and operating cost.
The site selected for demonstrating this technology
was the former Koppers Company (Koppers) site hi
Morrisville, North Carolina. This site was selected
because a Risk Reduction Engineering Laboratory
(RREL) SITE demonstration was planned for this site
allowing for a conjunction of logistical and support
efforts between RREL and EMSL-LV. However the
PCP at the former Koppers site was not introduced using
a petroleum hydrocarbon carrier. Because the HNU-
Hanby test kit provides results only for soil hi which a
petroleum hydrocarbon carrier is present, samples were
collected from the Winona Post site in Missouri and
shipped to the former Koppers site for inclusion as
demonstration samples. PCP contamination at the
Winona Post site had been introduced using a diesel fuel
carrier solvent.
The HNU-Hanby test kit is designed to provide
quick, semiquantitative and quantitative results for PCP
concentrations in soil samples. The test kit can provide
PCP results only hi samples which also contain a petro-
leum hydrocarbon carrier such as gasoline, kerosene,
diesel fuel, or fuel oil. It cannot be used to determine
PCP results for samples in which no petroleum hydro-
carbon carriers are present. The HNU-Hanby test kit
measures PCP indirectly by measuring the petroleum
hydrocarbons carrier solvent remaining hi the soil. The
ratio of PCP hi a petroleum hydrocarbon carrier may
vary due to manufacturing processes, dilution variances,
and the volatility and weathering of the petroleum
hydrocarbon carrier. Therefore, site samples must be
obtained so that site-specific calibration data can be
prepared. This can be done by analyzing the samples
both by EPA-approved methods and using the test kit.
Calibration data can then be generated by correlating the
PCP confirmatory results against the kit's corresponding
response. The test kit uses the Friedel-Crafts alkylation
reaction to detect the petroleum hydrocarbons. This
reaction is colorimetric. A reflective photometer is used
1
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to quantitatively measure the reaction color. A site-
specific calibration is needed to determine the ratio of
PCP to carrier solvent. This ratio is then used to correct
the results from the reflective photometer.
The HNU-Hanby test kit is portable and can be
operated outdoors. Temperature extremes and humidity
do not seem to affect its performance. The reagents
used with the test kit do not require refrigeration. The
reflective photometer requires electricity but can be
operated using a rechargeable battery pack. The test kit
was found to be easy to operate by individuals with no
prior environmental testing experience.
The test kit costs $1,195. This test kit provides
enough reagent and glassware to perform 30 soil sample
analyses. The reflective photometer used to provide
quantitative data costs $3,500. Other equipment, such as
extraction vials and pipettes, may need to be purchased
when using the test kit. The cost of these items will
vary depending upon the number of samples that will be
analyzed. The detection limits reported by the test kit's
developer is 1.0 part per million (ppm) for soil samples.
A 5.0 ppm detection limit was used for this demonstra-
tion. The elevated detection limit was the result of
reducing the sample mass used for extraction.
During the demonstration, 47 soil samples were
extracted and analyzed hi two 8-hour days. The average
time to analyze one soil sample was about 21 minutes.
The precision of the test kit was determined to be
statistically the same as the precision of the,confirmatory
laboratory. The kit's data set was evaluated for accur-
acy as a whole and by concentrations less than and
greater than 100 ppm PCP. When the entire data set
was evaluated, the test kit's results were determined to
be statistically different from the confirmatory results.
This was also the case for samples in which the PCP
concentrations were greater than 100 ppm. The test kit's
data for samples containing less than 100 ppm PCP was
shown to be statistically similar to the corresponding
confirmatory data. Based on this evaluation, the test kit
produced Level 1 data for samples containing greater
than 100 ppm PCP and Level 2 data for samples contain-
ing less than 100 ppm PCP. This indicates that there
was a concentration effect on the test kit's accuracy.
The test kit showed greater comparability to the confir-
matory data when PCP concentrations in samples were
below 100 ppm.
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Section 2
Introduction
This HER presents information on the demonstratio: i
of the HNU-Hanby Environmental Test Kit, a field
screening technology designed to detect PCP in soil. The
demonstration was conducted by PRC under the EPA's
SITE Program. The test kit was demonstrated
conjunction with the demonstrations of four other fieli
screening technologies: (1) the Penta PJSc Test Sys
developed by EnSys Incorporated, (2) the EnviroGa:
PCP Test Kit developed by the Millipore Corporation, (3J)
the Penta RaPID Assay developed by the Ohmicron
Corporation, and (4) the Field Analytical Screening
Program PCP Method developed by EPA's Region 7
through its Superfund Program. The results of these other
demonstrations are presented in reports similar to this one
EPA's Site Program and MMTP: an Overview
At the time of the Superfimd Amendments anc
Reauthorization Act of 1986 (SARA), it was we!
recognized that the environmental cleanup problem needec
new and better methods. The SITE Program, therefore.
was created to fulfill a requirement.of SARA that the EPA]
address the potential of alternative or innovative
technologies. The EPA made this program a joint effort
between the Office of Solid Waste and Emergency
Response (OSWER) and the Office of Research and
Development (ORD). The SITE Program includes four
parts:
The Demonstration Program
The Emerging Technology Program
The Monitoring and Measurement Technologies
Program (MMTP)
The Technology Transfer Program
The largest part of the SITE Program, the
Demonstration Program, is concerned with treatment
technologies and is administered by ORD's NRMRL in
Cincinnati, Ohio. The MMTP component, though, is
administered by EPA's EMSL-LV. The MMTP is
concerned with monitoring and measurement technologies
that identify, quantify, or monitor changes in contaminants
occurring at hazardous waste sites or that are used to
characterize a site.
The MMTP seeks to identify and demonstrate
innovative technologies that may provide less expensive,
better, faster, or safer means of completing this monitoring
or characterization. The managers of hazardous waste
sites are often reluctant to use any method, other than
conventional ones, to generate critical data on the nature
and extent of contamination. It is generally understood
that the courts recognize data generated with conventional
laboratory methods; still, there is a tremendous need to
generate data more cost effectively. Therefore, the EPA
must identify innovative approaches, and through
verifiable testing of the technologies under the SITE
Program, ensure that the innovative technologies are
equivalent to or better than traditional technologies.
The Role of Monitoring and Measurement
Technologies
Measurement and monitoring technologies are needed
to assess the degree of contamination, to determine the
effects of contamination on public health and the
environment, to supply data for selection of appropriate
remedial action, and to monitor the success or failure of
selected remedies. Thus, the MMTP is concerned with
evaluating screening technologies, including remote
sensing, monitoring, and analytical technologies.
Candidate technologies may come from within the
federal government or from the private sector. Through
the program, developers are to rigorously evaluate the
performance of their technologies. Finally, by distributing
the results and recommendations of those evaluations, the
market for the technologies is enhanced.
Defining the Process
The demonstration process begins by canvassing the
EPA's 10 regional offices (with input from OSWER .and
ORD) to determine their needs. Concurrently, classes of
technologies are identified. An ideal match is made when
there is a clear need by EPA's regions and a number of
technologies that can address that need. The
demonstrations are designed to judge each technology
against existing standards and not against each other.
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The demonstration is designed to provide for detailed
quality assurance and quality control (QA/QC) to ensure
that a potential user can evaluate the accuracy, precision,
representativeness, completeness, and compar-ability of
data derived from the innovative technology. In addition,
a description of the necessary steps and activities
associated with operating the innovative technology is
prepared. Cost data, critical to any environmental
activity, is generated during the demonstration and allows
a potential user to make economic comparisons. Finally,
information on practical matters such as operator training
requirements, detection levels, and ease of operation is
reported. Thus, the demonstration report and other
informational materials produced by the MMTP provide
a real-world comparison of that technology to conventional
technologies. With cost and performance data, as well as
"how to" information, users can determine whether a new
technology better meets their needs.
Components of a Demonstration
Once a decision has been made to demonstrate
technologies to meet a particular EPA need, the MMTP
performs a number of activities. First, the MMTP
identifies potential participants and determines whether
they are interested in participating. Each developer is
advised of the general nature of the demonstration and is
provided with information common to all MMTP
demonstrations. Information is sought from each
developer about its technology to ensure that the
technology meets the parameters of the demonstration.
Then, after evaluation of the information, all respondents
are told whether they have been accepted into the
demonstration or not. While participants are being
identified, potential sites also are identified, and basic site
Information is obtained.
The next component, probably the most important, is
the development of plans that describe how the
demonstration will be conducted. A major part of the
EPA's responsibility is the development of a
demonstration plan, a quality assurance project plan
(QAPjP), and a health and safety plan. While the EPA
pays for and has the primary responsibility for these plans,
each is developed with input from all of the
demonstration's participants. The plans define how
activities will be conducted and how the technologies will
be evaluated. The MMTP also provides each developer
with site information and often predemonstration samples
so the developer can. maximize the field performance of its
innovative technology. Generally, the developers train
EPA-designated personnel to operate their technologies so
that performance is not based on the special expertise of
the developers. This also ensures that potential users have
valid information on training requirements and the types of
operators who typically use a technology successfully.
The field demonstration itself is the shortest part of
the process. During the field demonstration, data is
obtained on cost, technical effectiveness (compared to
standard methods), and limiting factors. 'In addition,
standardized field methods are developed and daily logs of
activities and observations (including photos or videotape)
are produced. The EPA is also responsible for the
comparative, conventional method analytical costs and the
disposal of any wastes generated by the field
demonstration.
The final component of an MMTP demonstration
consists of reporting the results and ensuring distribution
of demonstration information. The primary product of the
demonstration is an ITER, like this one, which is
peer-reviewed and distributed as part of the technology
transfer responsibility of the MMTP. The ITER fully
documents the procedures used during the field
demonstration, QA/QC results, the field demonstration's
results, and its conclusions. A separate QA/QC data
package also is made available for those 'interested hi
evaluating the demonstration hi greater depth. Two-page
technical briefs are prepared to summarize the
demonstration results and to ensure rapid and wide
distribution of the information.
Each developer is responsible for providing the
equipment or technology product to be demonstrated,
funding its own mobilization costs, and training of EPA-
designated operators. The MMTP does not provide any
funds to developers for costs associated with preparing
equipment for demonstration or for development, and it
does not cover the costs developers Incur to demonstrate
their products.
Rationale for this Demonstration
PCP, a regulated chemical used in the wood treatment
industry, is included on the EPA Extremely Hazardous
Substances List. Recently, PCP regulations under the
Resource Conservation and Recovery Act (RCRA) have
been created specifically for wood treatment facilities.
PCP is included as a target compound of many
EPA-approved analytical methods, including EPA 500
Series Methods 515.1 and 525, EPA 600 Series
Methods 604 and 625, and EPA SW-846 Manual
Methods 8040, 8151, 8250, and 8270. All of these
methods use solvent extraction and gas chromatograpby.
Detection and quantitation is performed with flame
ionization, electron capture, or mass spectrometer
detectors. Analyzing samples for PCP using these
methods is typically costly and time consuming.
EMSL-LV, therefore, identified the need for effective,
accurate, low-cost screening "technologies that could
provide near real-time analytical data for PCP to
Superfund and RCRA decisionmakers.
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Demonstration Purpose, Goals,
and Objectives
The HNU-Hanby test kit was qualitatively evaluated
for the length of time required for analysis, ease of use
portability, and operating cost. It also was evaluated fo
accuracy and precision at detecting high and low levels ox
PCP in soil samples. The test kit's accuracy and precision
were statistically compared to the accuracy and precision
of a conventional confirmatory laboratory that had used
EPA-approved analytical methods. These comparisons
also were used to determine the highest data quality level
that the test kit could attain in field applications. For the
purpose of this demonstration the three primary data
quality levels are defined as follows (EPA 1990):
Level 1: This data is not necessarily analyte-specific
Technologies that generate Level 1 dati.
provide only an indication of contarm-
ination. Generally, the use of these
technologies requires sample documentation
instrument calibration, and performance
checks of equipment.
Level 2: This data is analyte-specific. To provide at.
accuracy check, verification analysis for
at least 10 percent of the samples by an
EPA-approved method is necessary. The
method's analytical error is quantified. Use
of QC procedures such as sample
documentation, chain-of-custody procedures,
sample holding time criteria, initial and
continuing instrument calibration, method
blank analysis, rinsate blank analysis, and
trip blank analysis is recommended.
Level 3: This data is considered formal or
confirmatory analysis. It is analyte-specific
and generally involves second-method
confirm-ation on 100 percent of critical
samples. Analytical error is quantified
(precision, accuracy, coefficient of
variation) and monitored. The following QC
measures are used: sample documentation,
chain of custody, sample holding time
criteria, initial and continuing instrument
calibration, rinsate blank analysis, trip blank
analysis, and performance evaluation
samples. Detection limits are determined
and monitored.
Inherent in the concept of data quality levels is
accuracy. Although PRC could not find a reference that
defined the expected and quantified accuracy of each data
quality level, it imposed common accuracy criteria in
defining these data quality levels. Data quality Level 3 is
considered the most accurate of the three levels; this data
is obtained by formal analysis using approved methods.
Data quality Level 2 is less accurate but does quantify
compound concentrations. Data quality Level 1 is the
least accurate and is often considered survey data, only
identifying the presence or absence of a compound or class
of compounds.
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Section 3
Predemonstration Activities
Several activities were conducted by EMSL-LV,
PRC, and other demonstration participants before the
demonstration began. These activities included identifying
developers, selecting the demonstration sites, selecting the
confirmatory laboratory and analytical methods, and
conducting predemonstration sampling. Predemonstration
sampling and analysis are normally used to allow
developers to refine their technologies and revise their
operating instructions, if necessary, prior to the
demonstration.
Identifying Developers
EMSL-LV supplied PRC with the names of the
immunoassay developers demonstrating technologies and
asked that PRC search for other technologies that could be
demonstrated simultaneously and inexpensively. PRC
identified EPA Region 7's field gas chromatograph (GC)
method and the HNU-Hariby test kit for inclusion in the
demonstration.
Selecting the Sites
To evaluate the HNU-Hanby test kit under field
conditions, a hazardous waste site suitable for the
demonstration was needed. The following criteria were
used to select the appropriate site:
The test, kit needed to be demonstrated on samples
with a wide range of PCP contamination.
PCP concentrations at the site had to be well
characterized and documented.
The site had to be accessible for conducting
demonstration activities without interfering with any
other activities being conducted on site.
Because the test kit can only be apph'ed when a
petroleum product is the PCP carrier, the site used
had to be contaminated by PCP hi a petroleum
product carrier.
The former Koppers wood treatment site was selected
for conducting the analyses because it met the criteria for
the other demonstrations and because NRMRL was
planning a SITE demonstration of the ETG Environmental,
Inc., Base-Catalyzed Decomposition technology at the site,
allowing logistical and support efforts between NRMRL
and EMSL-LV to be combined. However, the former
Koppers site is contaminated with PCP in butane and
isopropyl ether carrier solvents. Therefore, demonstration
samples were collected from the Winona Post site in
Missouri and shipped to the former Koppers site. Soils at
the Winona Post site are contaminated with PCP in a
diesel fuel carrier solvent.
The Winona Post site is located in Winona, Missouri,
on Old Highway 60 West. It has operated as a sawmilling
and wood preserving facility since at least the early 1950s.
It currently treats pine and oak lumber with a solution of
5 percent PCP in diesel fuel. The solution is stored in a
20,000-gallon aboveground storage tank located adjacent
to the treatment building. In the past, the Winona Post
Company mixed its own solution from concentrated PCP.
Prior to the mid-1950s, the Winona Post Company treated
wood with creosol.
PCP is an organic chemical with an empirical formula
of C5C15OH and a molecular weight of 266 grams per
mole. PCP has a melting point of 191 °C and a boning
point of 310 °C. The specific gravity of PCP is
1.978 grams per cubic centimeter. PCP iSjdescribed as
almost insoluble in water, with 8 milligrams able to
dissolve into 100 milliliters of water. The octanol ratio
coefficient of PCP is 6,400, which indicates that PCP is
tightly bound to the soil matrix when it is released into the
environment.
PCP is used as a wood preservative, an insecticide, a
preharvest defoliant, a slimicide, and a defbaming agent.
The largest user of PCP is the wood treating industry.
PCP is applied to wooden utility poles, railroad ties, and
lumber to protect them from weathering and deteriorating
due to fungus and rot. About 0.23 kilogram of PCP is
required for each cubic foot of wood treated. For treating
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wood, PCP is usually diluted to a 5 percent solution with
solvents such as mineral spirits, kerosene, diesel fuel, or
fuel oil. PCP also has been applied to wood with
methylene chloride and liquified petroleum gas, such as
butane. PCP also is used in the manufacturing of learner
and tanning products, masonry products, rope and paper
products, adhesives, and paint.
Selecting the Confirmatory Laboratory
Analytical Methods
and
Before the demonstration, the EPA Region
Laboratory arranged for all samples to be analyzed undsr
the Region 7 Environmental Collection and Analysis
Program (RECAP) Contract. SW-846 protocols f>r
Level 3 data were used to analyze the samples during tt is
demonstration. All samples were extracted by EPA
Method 3540A (Soxhlet Extraction) and analyzed by EP A
Method 8270A (Semivolatile Organic Compounds by G is
Chromatograph/Mass Spectrometer [GC/MS]: capillary
column). Any samples in which PCP was not detected
using Method 8270A were reanalyzed by Method 815lk
(chlorinated herbicides by GC: capillary column)
calibrated to PCP. All of these analytical methods are
well established and approved by EPA. The QA
procedures, reporting requirements, and data quality
objectives of these methods are consistent with the goals
of the SITE Program.
Training Technology Operators
The technology was operated by a PRC operator.
Before the demonstration began, this individual was
trained on how to use the technology. This training
involved a review of operating procedures and instructions
provided by the developer, and formal training by the
developer. Training was equivalent to that recommended
by the developer for those using the test kit on actual site
characterization projects.
Predemonstration Sampling and Analysis
In August 1993, while demonstration sampling for the
other technologies was being conducted at the former
Koppers site, PRC collected five predemonstration soil
samples from areas at the Winona Post site previously
identified as containing PCP. These samples were
submitted to HNU-Hanby. These samples were not
analyzed by a confirmatory laboratory. HNU-Hanby
Systems analyzed the predemonstration samples with the
test kit and by GC/MS. The developer used this data to
calculate calibration factors for the test kit.
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Section 4
Demonstration Design and Description
The primary objective of the demonstration was to
evaluate this test kit for its effectiveness at detecting
PCP in soil when operated in field conditions. This
objective included defining the precision, accuracy, cost,
and range of usefulness for the test kit. A secondary
objective was to define the data quality objectives that
the test kit can be used to address. The evaluation was
designed so that the test kit results could be compared to
those of a confirmatory laboratory that analyzed each
sample using standard EPA-approved methods. The
design limited, as much as possible, those elements of
sample collection and analysis that would interfere with
a direct comparison of the results. These elements
included heterogeneity of the samples and interference
from other chemicals or other controllable sources.
The design also ensured that the data was collected
in a normal field environment. To do this, the test kit
was operated in a trailer located at the former Koppers
site. The operator was trained by the developer and was
able to call the developer with questions when necessary.
The operator, though, obtained all results on his own and
reported the results once he believed the results were
accurate and precise. Standard QC samples were
analyzed with each batch of environmental samples.
Numerous laboratory and field duplicate samples were
included among those analyzed to ensure a proper
measure of precision. The technology was tested for
common interferants. Qualitative measures, such as
portability and ease of operation, were also noted by the
operator. Overall, the demonstration was executed as
planned in the demonstration plan (PRC 1993), which
included the QAPjP. The final version of that plan was
approved by all participants and developers before the
demonstration began. Below is a discussion of selected
elements of that plan and a full discussion of deviations
from it.
Implementation of the Demonstration Plan
Forty soil samples and five soil field duplicates were
collected at the Winona Post site. The soil samples were
collected in areas believed to be contaminated with high
(greater than 1,000 ppm), medium (100 to 999 ppm),
and low (less than 99 ppm) concentrations of PCP. The
identification of these areas was based on past sampling
data and visual signs of waste disposal. All of the
samples were collected, packaged, and shipped to the
former Koppers site. Each soil sample was thoroughly
homogenized and then split into six replicate samples.
One replicate from each soil sample was submitted to the
confirmatory laboratory for analysis using the methods
described in Section 3. The remaining replicates were
analyzed in the trailer at the former Koppers site using
the various technologies being evaluated.
Field Modifications
to the Demonstration Plan
Two field modifications were made to the approved
demonstration plan used to demonstrate the five technol-
ogies, but neither influenced the test kit's results. First,
fluorescein was to be added to the soil samples from the
former Koppers site prior to homogenization. This test
kit, though, was used only on samples from the Winona
Post site, and the saturated silty nature of the Winona
Post soil samples allowed easy and thorough homogeni-
zation. PRC, therefore, used an EPA-approved homo-
genization method and applied it to each sample for 10
to 15 minutes.
Data Collection
The operator prepared a subjective evaluation of
how difficult the test kit was to use. Other qualitative
factors included portability, ruggedness, instrument
reliability, and health and safety considerations. Infor-
mation on these qualitative factors was collected both by
the operator of the test kit and by the project's lead
chemist.
Accuracy and precision were statistically evaluated
during this demonstration. To evaluate accuracy and
precision, all samples collected for the demonstration
were split between the test kit and the confirmatory
-------
laboratory for analysis. The results from the confirma
tory laboratory, for the purposes of this demonstration,
were considered the actual concentration of PCP in each
sample. The statistical methods used for the comparison
are detailed later hi this section. The cost of using the
test kit also was assessed. Cost, for the purposes of this
demonstration, includes expendable supplies, nonexpendj-
able equipment, labor, and investigation-derived waste
(IDW) disposal. These costs were tracked during th<
demonstration.
Statistical Analysis of Results
Besides looking at the data set as a whole, PRCJ
grouped the data into results greater than 100 ppm anc
less than 100 ppm PCP. This grouping was intended tc
assess potential concentration effects on the data analy
sis. These data sets were prepared for the statistica
analysis following the approved demonstration plan
When comparing duplicate samples or when comparing
the results of a technology to those from the confirma-
tory laboratory, sample pairs that contained a nondetec
were removed from the data sets. While other statistica
methods can be used when nondetects are encountered.
PRC felt that the variance introduced by eliminating
these data pairs would be less than, or no more thai
equal to, the variance produced by giving not detectec
results an arbitrary value.
Intramethod Comparisons
Sample results from the test kit were compared to
their duplicate sample results and to other QA/QC
sample results. These comparisons are called intra-
method comparisons. Intramethod precision was as-
sessed through the statistical analysis of relative percent
differences (RPD) between duplicates. First, the RPDs
of the results for each sample pan- hi which both the
sample and its duplicate were found to contain PCP were
determined. The RPDs then were compared to upper
and lower control limits. When using conventional
technologies, such data is often available from analysis
of samples collected during previous investigations.
Because the technology being demonstrated was itseli
being assessed, the control limits used were calculated
from data provided during this investigation. To deter-
mine these control limits, the standard deviation of the
RPDs was calculated. This standard deviation was then
multiplied by two and added to its respective mean RPD.
This established the upper control limit for the technol-
ogy. Because an RPD of zero would mean that the
duplicate samples matched their respective samples
perfectly, zero was used as the lower control limit. This
resulted in a large range of acceptable values. All
samples that fell within the control limits were consid-
ered acceptable. PRC determined that if at least
90 percent of the duplicate samples fell within these
control limits, the technology had acceptable intramethod
precision.
Intermethod Comparisons
The data sets also were statistically compared to the
results from the confirmatory laboratory, and the
precision of the technology was statistically compared to
the precision of the confirmatory laboratory. These
comparisons are called intermethod comparisons. In
both cases, the results from the confirmatory laboratory
were considered as accurate and precise as analytically
possible.
The statistical methods used to determine inter-
method accuracy were linear regression analysis and the
Wilcoxon Signed Ranks Test. PRC prepared the data
sets for the linear regression by averaging the field
duplicate results. This was done to ensure that those
samples were not unduly weighted in the regression
analysis. PRC calculated linear regression by the
method of least squares. Calculating linear regression in
this way makes it possible to determine whether two sets
of data are reasonably related, and if so, how closely.
Calculating linear regression results hi an equation that
can be visually expressed as a line. Three factors are
determined during the calculations: the y-intercept, the
slope of the line, and the coefficient of determination,
also called r2. All three of these factors had to have
acceptable values before the technology's accuracy was
considered to meet Level 3 data quality requirements.
The r2 expresses the mathematical relationship between
two data sets. If r2 is equal to one, then the two data
. sets are directly related. Lower r2 values indicate less of
a relationship. Because of the nature of environmental
samples, r2 values between 0.85 and 1 were considered
to meet data quality Level 3 accuracy requirements; r2
values between 0.75 and 0.85 were considered to meet
data quality Level 2 accuracy requirements; and r2
values below 0.75 were considered not accurate, meet-
ing, at best, Level 1 data quality objectives. The
classification of data as Level 1, 2, or 3 was implied hi
the approved demonstration plan; however, these
specific criteria were not presented.
If the regression analysis resulted hi an r2 between
0.85 and 1, then the regression line's y-intercept and
slope were examined to determine how closely the two
data sets matched. A slope of 1 and a y-intercept of zero
would mean that the results of the technology matched
those of the confirmatory laboratory perfectly. Theoreti-
cally, the farther the slope and y-intercept differ from
these expected values, the less accurate the technology.
Still, a slope or y-intercept can differ slightly from its
expected value without that difference being statistically
-------
significant. To determine whether such differences were
statistically significant, PRC used the normal deviate test
statistic. This test statistic results in a value that is
compared to a table. The value at the 90 percent
confidence level was used for the comparison. To meet
data quality Level 3 requirements, both the slope and
y-intercept had to be statistically the same as their ideal
values. If the r2 was between 0.75 and 0.85, and one or
both of the other two regression parameters was not
equal to their ideal, the test kit's results were considered
inaccurate but to be of Level 2 quality. Results in this
case could be mathematically corrected if 10 to 20
percent of the samples were sent to a confirmatory
laboratory. Analysis of a percentage of the samples by
a confirmatory laboratory would provide a basis for
determining a correction factor. Only in cases where the
r2, the y-intercept, and the slope were all found to be
acceptable did PRC determine that the test kit's results
were accurate, meeting Level 3 data quality require-
ments. Data placed hi the Level 1 category had r2 values
less than 0.75, the data was not statistically similar to the
confirmatory data, based on nonparametric testing, or
the results did not meet the manufacturer's performance
specifications.
A second statistical method used to assess inter-
method accuracy was the Wilcoxon Signed Ranks Test.
This test is a nonparametric method for comparing
matched pairs of data. It can be used to evaluate
whether two sets of data are significantly different. The
test requires no assumption regarding the population
distribution of the two sets of data being evaluated other
than that the distributions will occur identically. In other
words, when one data point deviates, its respective point
in the other set of data will deviate similarly. Because
the only deviation expected during the demonstration was
a difference in the concentrations reported by each
technology, the two sets of data were expected to deviate
in the same way. The calculation performed in the Wil-
coxon Signed Ranks Test uses the number of samples
analyzed and a ranking of the difference between the
result obtained from a technology and the corresponding
result from the confirmatory laboratory. The rankings
can be compared to predetermined values on a standard
Wilcoxon distribution table, which indicates whether,
overall, the two methods have produced similar results.
In cases where the linear regression produced an r2 less
than 0.75 and the Wilcoxon Signed Ranks Test indicated
that the data sets were statistically similar, the regression
data was not considered correct. Such occurrences were
due to one or both data sets not meeting the fundamental
assumption for regression analysis, normally distributed
data sets.
Finally, the test kit's precision was statistically
compared to the precision of the confirmatory laboratory
using Dunnett's Test. This test was used to assess
whether the precision of the test kit and that of the
confirmatory laboratory were statistically equivalent.
First, the mean RPD for all samples and their respective
duplicates analyzed by the confirmatory laboratory was
determined. The RPDs of each duplicate pair analyzed
by the test kit was then statistically compared to this
mean. It should be noted that a Dunnett's Test result
showing the precisions are not similar does not mean that
the precision of the technology was not acceptable, only
that it was different from the precision of the confirma-
tory laboratory. In particular, Dunnett's Test has no
way of determining whether or not any difference
between the two data sets actually resulted because a
technology's data was more precise than the confirma-
tory laboratory's. Verification of the Dunnett's Test
results was provided by the Wilcoxon Signed Ranks
Test.
Overall, for this demonstration, the determination of
significance for inferential statistics was set at
90 percent. However, regression analysis was consid-
ered to show a significant relationship if the coefficient
of determination (r2) was greater than 0.85 for Level 3
data and between 0.75 and 0.85 for Level 2 data.
10
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Section 5
Confirmatory
Analysis Results
All samples collected during this demonstration
were submitted to the EPA Region 7 Laboratory for
confirmatory analysis under the RECAP Contract. The
result for each sample is presented in a table near the
end of Section 6.
Confirmatory Laboratory Procedures
EPA Region 7 Laboratory Quality Assurance am.
Data Evaluation (QADE) Branch personnel conducted a
Level II data review on the results provided by the
confirmatory laboratory. A Level II data review does
not include an evaluation of the raw data or a check of
calculated sample values. A review of the raw data and
a check of the calculations was performed by QG
personnel from the confirmatory laboratory before
submitting the data package to EPA Region 7 Laboratory
QADE Branch. PRC was not able to review all of the
raw data generated from the analysis of samples.
However, PRC did review the laboratory case narrative!
and the EPA Region 7 Laboratory QADE Branch
comments generated by the Level II data review. The
following paragraphs discuss specific procedures used to
identify and quantitate semivolatile organic compounds
(SVOC), specifically PCP, using the following methods:;
EPA Method 8270A and EPA Method 8151A.
Sample Holding Times
All of the analytical methods used for confirmatory
analysis require that all sample extractions be completed
within 7 days from the time a sample was collected.
Due to the stability of PCP, ORD's Methods Validation
Section extended these holding tune requirements by 4
days for this demonstration. The analysis of the sample
extracts must be completed within 40 days of validated
sample receipt. The holding tune requirements for the
samples collected during this demonstration were met.
Sample Extraction
The method used for the extraction of soil samples
prior to analysis by EPA Method 8270A was EPA
Method 3550. EPA Method 3550 involves sonication
extraction of the soil using methylene chloride. The
confirmatory laboratory used both the low concentration
extraction method and the high concentration extraction
method discussed in EPA Method 3550. To determine
the appropriate extraction method to use for the analysis
of individual soil samples, the confirmatory laboratory
screened each sample using the screening techniques
recommended in EPA Method 8270A. Soil samples
with concentrations at or near the detection limits of
Method 8270A were reanalyzed using Method 8151A.
EPA Method 8151A includes an acidification of the soil
sample followed by an ultrasonic extraction with methy-
lene chloride. This extraction is similar to EPA Method
3550's sonication extraction. The soil sample extract
was then taken through an acid-base partition. The
acid-base partition was used to remove potentially
interfering compounds from the sample extract. The
sample extract was then concentrated and taken through
a diazomethane derivatization. This procedure replaces
the hydrogen atom of the alcohol group with a methyl
anion. This derivatization removes the polarity associ-
ated with PCP and enables improved chromatographic
behavior. PCP standards used for sample identification
and quantitation were taken through the same deriv-
atization steps to allow a direct comparison of concentra-
tion. That is, no correction factor needs to be used for
the molecular weight of the derivatization product.
Detection Limits and Initial
and Continuing Calibrations
The detection limit for samples analyzed by EPA
Method 8270A was reported as 0.330 ppm. The detec-
11
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tion limit for soil samples analyzed by EPA Method
8151A was reported as 0.076 parts per billion. Meth-
od-required initial and continuing calibration procedures
were appropriately conducted, and all method-required
criteria for these calibrations were met.
Sample Analysis
The confirmatory laboratory performed sample
analysis by first screening samples using EPA
Method 8270A. Based upon the screening results, the
samples were extracted with either the low concentration
method or the high concentration method discussed in
EPA Method 3550. Samples that did not provide a
positive response for PCP with EPA Method 8270A
were analyzed by EPA Method 8151 A.
For EPA Method 8270A, compound identification
was required to meet two criteria: (1) the sample
component relative retention time was to fall within ±
0.06 relative retention time units of the standard compo-
nent, and (2) the mass spectrum of the sample compound
was to correspond with the standard compound mass
spectrum. If compound identification was not made,
samples were analyzed by EPA Method 8151A. For
EPA Method 8151A, compound identification was made
if a sample peak eluted within the retention tune window
established during the initial calibration.
Quality Control Procedures
Method blanks are used to monitor the presence of
laboratory-induced contamination. The EPA Region 7
Sample Management Office (SMO) provided blank soil
for use as method blank samples. An acceptable method
blank must not provide a positive response for the target
compounds above the reported detection limit. Method
blank samples were stored, extracted, and analyzed in
exactly the same manner as the demonstration samples.
Results for all method blank samples extracted and
analyzed were found to be acceptable.
Internal standards were used for the analysis of
demonstration samples by EPA Method 8270A. Internal
standards were added to all standards, blanks, samples,
and QC samples prior to injection into the GC/MS
system. The internal standards were used to provide
response factors for each of the target compounds. Six
samples exhibited internal standard responses which
were outside of the QC limits of 50 to 150 percent
recovery. All of the affected samples provided internal
standard responses which were less than 50 percent.
The soil samples affected were samples 060, 062, 068,
090, 091, 095. Of these samples, three - 090, 091, and
095 were found to contain no detectable levels of
PCP, and no corrective action was taken. Instead, they
were reanalyzed using EPA Method 8151 A. The
remaining samples were reanalyzed to verify that the
internal standard response was below 50 percent recov-
ery. The reanalysis showed that internal standard
response was below 50 percent recovery. No corrective
action was taken by the laboratory, which attributed the
low recovery to matrix effects inherent to the samples.
The Region 7 Laboratory QADE Branch reached the
same conclusion during its review of the data.
Surrogate standards were used to evaluate the
efficiency of the extraction and analysis processes and to
evaluate matrix effects. Surrogate standards used for
EPA Method 8270A include deuterated standards which
provide a different mass spectrum when compared to the
nondeuterated compound. The surrogate standard used
for EPA Method 8151A was 2,4-dichlorophenylacetic
acid (DC A A). The DCAA acceptance range was
determined by the RECAP and Region 7 Laboratory
through a statistical analysis of 30 or more standard
surrogate recoveries. The mean and standard deviation
were then calculated, and the acceptance range was
determined by applying a ± 3 standard deviation around
the mean. All samples analyzed with EPA Method
8151A provided surrogate recoveries that fell within the
laboratory-generated control limits. ;
Matrix spike samples are aliquots of original sample
into which a known concentration of the target com-
pounds were added. The EPA Region 7 Laboratory
SMO designated the samples which were to be used as
matrix spike samples. The designated soil samples were
samples 073, 087, and 098, all analyzed using EPA
Method 8270A, and sample 089, analyzed using EPA
Method 8151A. The soil matrix spike samples were
spiked with all of the target compounds reported by the
method. Soil matrix spike data for PCP is shown in
Table 5-1. The recoveries of these samples were greatly
influenced by the high concentrations of PCP present in
the original sample relative to the amount spiked. Only
one sample, 098, resulted in recoveries for both the
matrix spike and matrix spike duplicate sample which
could be considered acceptable. A clear evaluation of
the effects of matrix on PCP recovery is not possible due
to the high concentrations of PCP in the sample and the
comparatively low levels of PCP added to the matrix
spike samples.
Data Reporting
The data report PRC received from the EPA Region
7 Laboratory included a standard EPA Region 7 Analysis
Request Report. Results were reported on a dry weight
basis, as required in the methods. PRC obtained data on
12
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TABLE 5-1. MATRIX SPIKE AND. MATRIX SPIKE DUPLICATE RESULTS.
Sample No.
Amount Found
In Original Sample
Amount Added
To Matrix Spike
Sample
Amount Found In
Matrix Spike
Sample
Percent Recovery
073
087
089
098
86.0
46.0
0.247
0.70
11.0
1.40
0.098
0.41
130
57.0
0.315
0.82
400
786
69
29
Sample No.
073
087
089
098
Amount Added Amo
To Matrix Spike M;
Duplicate Sample Dupl
(ppm)
11.0
1.40
0.098
0.41
jnt Found In
itrix Spike
icate Sample
(ppm)
93.0
64.0
0.241
0.98
Percent Recovery
(%)
64
1,285
0
68
Relative Percent
Difference
(%)
145
48
200
80
the loss-on-drying determination for each of the samples.
The loss-on-drying values were used to convert the
confirmatory laboratory data from a dry weight basis to
a wet weight basis.
Results were reported by the confirmatory labora-
tory in micrograms per kilogram Otg/kg) for soil sam-
ples. Soil sample results were converted to milligrams
per kilogram (mg/kg) so they could be compared to the
results from the technologies, all of which reported
results for soil samples in mg/kg.
Data Quality Assessment
Accuracy refers to the difference between the
sample result and the true concentration of analyte in the
sample. Bias, a measure of the departure from complete
accuracy, can be caused by such processes as loss of
analyte during the extraction process, interferences, and
systematic contamination or carryover of an analyte from
one sample to the next. Accuracy for the confirmatory
laboratory was assessed through the use of two perform-
ance evaluation (PE) samples purchased from Environ-
mental Research Associates (ERA). These samples
contained a known quantity of PCP. ERA supplied data
sheets for each PE sample which included the true
concentration and an acceptance range for the sample
based on the 95 percent confidence interval taken from
data generated by ERA and EPA interlaboratory studies.
The true value concentration of soil PE sample 099 (the
low-level sample) was 7.44 ppm with an acceptance
range of 1.1 to 13 ppm. The result reported by the
confirmatory laboratory for this sample was 4.02 ppm,
which was within the acceptance range. The percent
recovery of this sample by the confirmatory laboratory
was 54 percent. The true concentration of soil PE
sample 100 (the high-level sample) was 101 ppm with an
acceptance range of 15 to 177 ppm. The result reported
for this sample by the confirmatory laboratory was 52.4
ppm, which was within the acceptance range. The
percent recovery of this sample by the confirmatory
laboratory was 52 percent.
Precision refers to the degree of mutual agreement
among individual measurements and provides an estimate
of random error. Precision for the confirmatory labora-
tory results was determined through the use of field
duplicate samples. Normally laboratory duplicates are
used for this. However, no laboratory duplicates were
analyzed by the confirmatory laboratory. Field dupli-
cates are two samples collected together but delivered to
the laboratory with separate sample numbers. Typically,
field duplicate samples are used to measure both sam-
pling and analysis error. PRC established control limits
for field duplicate RPDs. These control limits are
similar to those used to determine matrix spike recovery
acceptance control limits. To establish the control
limits, all sample pairs that did not produce two positive
results were removed from the data set. Then the RPD
for each pair was calculated, and the mean RPD and
standard deviation were determined. The lower control
limit was set at zero because this would mean that the
13
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results from a duplicate and its sample matched per-
fectly. The upper control limit was set by multiplying
the standard deviation by two and adding it to the mean
RPD. The RPD of each sample pair was then compared
to these control limits. Each sample pair RPD was
expected to fall within the control limits.
Five field duplicate samples were collected and
analyzed by the confirmatory laboratory during this
demonstration. RPD values for the duplicate pairs
ranged from 4 to 58. The mean RPD value of the soil
field duplicate pairs was 23 percent, with a standard
deviation of 25 percent. For the soil field duplicate pairs
the control limits were found to be 0 to 73 RPD. All of
the five field duplicate sample pairs fell within this
range. Overall, this data shows excellent agreement
between the samples and their respective field duplicates,
indicating a high degree of precision by the confirmatory
laboratory. The mean RPD also indicated that the
method used to homogenize the samples before splitting
them for analysis was highly effective.
Completeness refers to the amount of data collected
from a measurement process compared to the amount
that was expected to be obtained (Stanley and Verner
1983). For this demonstration, completeness referred to
the proportion of valid, acceptable data generated by the
confirmatory laboratory. The completeness objective
for this project was 95 percent. Completeness for the
confirmatory laboratory was 100 percent.
Confirmatory Laboratory Costs
and Turnaround Times
The cost for performing PCP analysis by EPA-
approved analytical methods varies from laboratory to
laboratory. The cost of analysis depends upon the
number of samples submitted for analysis, the matrix,
and the level of QC performed. The following costs are
given as general guidelines. EPA Method 8270A
analysis costs range from $250 to $400 per sample.
EPA Method 8151A analysis costs range from $150 to
$250 per sample. Turnaround tunes for samples submit-
ted for analysis with EPA-approved analytical methods
range from 14 to 30 days. The turnaround time also
depends upon the number of samples submitted for
analysis, the matrix, and the level of QC performed.
Faster turnaround times may be available for an addi-
tional cost.
14
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Section 6
HNU-Hanby Environmental Test Kit
The HNU-Hanby test kit is designed to provid;
quick, quantitative results for aromatic and petroleum
compounds hi soil samples. This test kit determines
PCP concentrations in soil samples indirectly by measurl
ing the carrier solvents used in wood treating that
contain PCP. This application assumes that the ratio of
carrier solvent concentration to PCP concentration is
constant. HNU-Hanby Systems claims that the test *'"
can detect petroleum carrier solvents containing PCP ;
concentrations as low as 1 to 5 ppm in soil. The test:
uses the Friedel-Crafts alkylation reaction to detect
aromatic and petroleum hydrocarbon compounds in soil
In the Friedel-Crafts alkylation reaction, an aromatic
substitution occurs where the aromatic ring attacks a
carbocation electrophile. The electrophile is formed by
the reaction of a Lewis acid catalyst, such as aluminum
chloride, with an alkyl halide. An excess amount of this
catalyst is added to act as a dehydrant to enable, the
Friedel-Crafts reaction to proceed. Electrophile aro
matic substitution products are generally very larg
molecules with a high degree of electron dislocation tha
cause intense coloring. When using the test kit, th
sample's color is then compared to site-specific colo
standards for a semiquantitative assessment of PCI
concentrations.
The standards are produced by analyzing severa
samples from the site. These samples should contain
PCP concentrations representative of contamination al
the site. The analysis is conducted using a GC/MS tc
determine the PCP-to-carrier solvent ratio. Alterna-
tively, the change hi the color can be read in millivolt:
using a reflective photometer. In this method, a PCF
calibration chart is developed between millivolt readings
and the concentration of PCP based on the GC/MS
analysis. The sample reading as obtained from the
reflective photometer is then cross-referenced with thi
calibration charts to obtain a quantitative sample resul
for PCP. HNU-Hanby Systems has said that the test kii
is extremely sensitive due to the intense coloring thai
develops during the Friedel-Crafts reaction.
Because the Friedel-Crafts reaction involves only
aromatic compounds, this test kit does not work on all
PCP carriers. Only those carriers that have aromatic
compounds, such as gasoline, diesel fuel, and kerosene,
can be detected.
Generally, PCP is added in a certain percentage to
the carrier solvent for application onto wood. This
percentage may differ from site to site. To assess the
ratio between the carrier solvent and PCP hi the Winona
Post samples, HNU-Hanby Systems obtained contami-
nated soil samples collected from Winona Post site,
diluted these samples when required, and analyzed these
samples for PCP. Later, the same samples were ana-
lyzed using the test kit, and the corresponding reflective
photometer readings in millivolts were obtained. A
regression line was then calculated to allow the kit's
operator to predict PCP concentrations when millivolt
readings were known. This type of site-specific calibra-
tion should minimize the effect of the weathering of the
carrier solvent that could affect the ratio. Following the
completion of the demonstration, HNU-Hanby Systems
sent the PCP calibration data to PRC. This data is
presented in Table 6-1.
TABLE 6-1. CALIBRATION DATA.
Reflective
Photometer Reading
(millivolts)
890
826
738
670
556
434
223
111
89
79
PCP
Concentration
(ppm)
0.00 (Blank)
0.20
0.50
1.00
2.00
5.00
25.0
100
200
1,000
15
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Operational Characteristics
The HNU-Hanby test kit weighs about 17 pounds
and comes in a ragged, plastic carrying case. The
carrying case is 15 inches high by 19 inches wide by 8
inches deep. Overall, the test kit was found to be
portable. Each test kit contains the following materials:
(1) a 10-milliliter graduated cylinder, (2) a 50-milliliter
beaker, (3) 36 screw-top test tubes, (4) 30 ampules of
extraction solvent consisting of 20 percent carbon
tetrachloride and 80 percent heptane, (5) 30 vials of
color development reagent such as aluminum chloride,
(6) a 500-milliliter separatory funnel, (7) a tripod ring
stand, (8) one pair of safety glasses, (9) six pairs of
plastic gloves, (10) an instructional video, (11) a color
chart depicting test results, and (12) a reflective photo-
meter.
Other materials used by the operator during the
demonstration besides those mentioned above included:
(1) a scale capable of measuring ± 0.05 grams, (2) a
stainless-steel spatula, (3) laboratory wipes, (4) a stop
watch, (5) pipette bulb, and (6) marking pens.
The test kit's logistical requirements include elec-
tricity or battery replacements. For this demonstration,
a fume hood also was used because the extraction solvent
contains carbon tetrachloride. All extraction and analy-
sis can be carried out hi a small open area or within a
small fume hood. The test kit requires approximately 2
square feet of work surface. The reflective photometer
can be operated using a 110-volt or 220-volt electrical
supply. This instrument also is equipped with a re-
chargeable battery. This battery requires 8 to 24 hours
of charging, and when fully charged, the battery can last
up to 8 hours.
The operator chosen to analyze samples using the
technology was Mr. Dan Fenton, an employee of PRC.
Mr. Fenton has worked for PRC for 2 years. He has
been primarily involved in environmental potentially
responsible party searches and the writing of Superfund
enforcement memorandums. He has had 6 credit hours
of college inorganic chemistry and 4 credit hours of
inorganic laboratory. Training was conducted by the
technology developer. Mr. Fenton received training
from HNU-Hanby Systems and reviewed a training
videotape that explained the operation of the technology.
HNU-Hanby Systems prepared the calibration factors for
the final data evaluation.
Mr. Fenton found the test kit easy to operate. Prior
experience in analytical chemistry is useful, but not
required. Operation of the test kit involves weighing
samples, carefully breaking open glass ampules, shaking
vials, adding catalyst to vials and measuring readings on
the reflective photometer. The test kit is designed for
use either hi the field or hi a laboratory. . Some of its
instrumentation and equipment require special handling.
This instrumentation includes the reflective photometer,
the portable balance, and the pipettor. This equipment
must be handled carefully to avoid damage. The proto-
type reflective photometer failed to give consistent
results because the batteries were weak. The reflective
photometer had no low battery indicator to warn the
operator. When the weak battery was noted, the pho-
tometer was plugged into an available electricity outlet.
Also, highly contaminated samples turned black and
developed gas pockets. These samples seemed to
interfere with the precision of the reflective photometer
readings.
The photometer's reliability was monitored daily by
checking a white calibration standard. The reflective
photometer should read 1,020 millivolts when analyzing
the white calibration standard. As the intensity of the
color increases, the corresponding millivolt reading
decreases. The calibration check should give the highest
reading. During the two calibration checks conducted
during the sample analysis, the reflective photometer
read 812 and 866 millivolts. HNU-Hanby Systems said
that these readings were within the acceptable range of
a calibration check.
The test kit uses a proprietary solvent to extract
organic compounds from different sample matrices.
This solvent contains heptane an.d carbon tetrachloride.
The test kit also uses aluminum chloride in large
amounts as a Lewis acid catalyst. Care should be taken
when using these chemicals. Heptane is a highly flam-
mable solvent that tends to explode in the presence of an
ignition source. Carbon tetrachloride is a probable
human carcinogen. Aluminum chloride is a probable
teratogen that reacts violently with alkenes. It is recom-
mended that proper personal protective wear, such as
gloves and safety glasses, be worn when handling these
chemicals.
The HNU-Hanby test kit is priced at $1,195. This
test kit contains color charts for color interpretation; it
does not include a reflective photometer. Each test kit
contains enough reagents and other supplies to analyze
30 samples. The cost of HNU-Hanby Systems' reflec-
tive photometer is $3,500. Other costs associated with
the analysis were the cost of 40-milliliter vials, the cost
of pipettes and a pipette bulb, and the operator cost.
The operator cost depends on the operator's qualifica-
tions and experience. The total cost for quantitative
application of this test kit , excluding operator's costs,
was about $6,000 for the 52 samples analyzed, which is
about $112 per sample. However, as more samples are
analyzed, the cost of the reflective photometer will be
16
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distributed among more samples, reducing the pe:
sample cost. When used semiquantitatively, the cost off
the reflective photometer can be deducted from the total
cost. In the semiquantitative analysis, the color develr
oped by each sample is compared to the standard color
chart, which is included in the test kit for the determinaL
tion of the concentration. In this case, the cost per
sample for this demonstration would be about $48i.
Waste disposal cost is not included in the cost per sample
described above. The waste generated during this
demonstration filled approximately one-half of a
55-gallon drum. The disposal cost for this quantity of
PCP-contaminated laboratory waste is approximated
$1,000.
Performance Factors
The sensitivity of the method depends on the sensi
tivity of the reflective photometer. The literature on thi >
method claims that aromatic compounds as low as
1.0 ppm can be detected in soils. In fact, the calibration
chart prepared for the test kit shows a range from 0.2
ppm to 1,000 ppm. During this demonstration, all
sample extracts that developed moderate to dark color
were diluted with the proprietary solvent. This dilution
was performed by taking 0.3 milliliter of sample extract
and adding 10 milliliters of solvent. This produced a
172-fold dilution for a 1.0 gram soil sample. These
dilutions increased the detection limits for the samples
involved. The modified detection limit was 5 ppm.
HNU-Hanby Systems has stated that 50 samples can
be analyzed in an 8-hour work day. During this demonl
stration, the average time taken to extract each sample
and prepare it for analysis was 21 minutes. The analysis
of the prepared sample in the reflective photometer
required less than 1 minute. Based on the average time
of 21 minutes per sample, approximately 22 samples
were analyzed in an 8-hour day. This number was
influenced by factors such as the number of samples thaf:
required dilution, and the analysis of QC samples.
The linear range of the test kit is dependent on
linear range of the reflective photometer. The line,
range of the reflective photometer was not evaluate^
during the demonstration. However, HNU-Hanb;
Systems sent the calibration data which included a PCIj
concentration range of 0.2 ppm to 1,000 ppm. When
this data between the millivolt readings and PCP conceni
trations was plotted on a normal-scale plot, the coeffij-
cient of determination (r) indicated that the response
between the reflective photometer readings and corre
spending PCP concentrations was not linear. A natura.
logarithm transformation of the data gave a linea'
response with an r of 0.96.
Drift in this method was considered the instability
associated with reflective photometer readings. As noted
by the operator, whenever the battery was either fully
charged or weak, sample readings fluctuated more. This
problem was later solved by connecting the instrument
to an outlet.
Intramethod Assessment
Reagent blank samples were prepared by talcing
reagents through all extraction and reaction steps of the
analysis. Reagent blanks were prepared with each batch
of 20 samples. Two reagent blanks were prepared, and
analyzed during the demonstration. The reagent blank
samples did show some readings on the reflective
photometer. When these millivolt readings were con-
verted to PCP concentrations, they gave values of
2.19 ppm and 1.8 ppm. Both of these values are below
the technology's detection limit of 5 ppm used during
this demonstration. Therefore, none of the data was
rejected because of reagent blank contamination.
Completeness refers to the amount of data collected
from a measurement process compared to the amount
that was expected to be obtained (Stanley and Verner
1983). For this demonstration, completeness refers to
the proportion of valid, acceptable data generated using
the technology. The completeness objective for this
project was 90 percent. Forty-five soil samples includ-
ing field duplicates were analyzed during the demonstra-
tion. Two reagent blanks and five laboratory duplicates
were analyzed along with the 45 samples. Results were
obtained from all samples. Completeness for the
samples analyzed by the kit was 100 percent.
Intramethod precision was assessed by determining
the method's ability to reproduce its results on duplicate
samples. These duplicate samples included five labora-
tory duplicates and five field duplicates. Usually these
duplicate samples are used to determine matrix variabil-
ity and the effects of using several operators. To use the
duplicates to measure the method's precision, PRC both
controlled for matrix variability by thoroughly homogen-
izing the samples and controlled for operator effects by
using only one operator for the entire demonstration.
Laboratory duplicate samples are two analyses per-
formed on a single sample delivered to a laboratory.
Five laboratory duplicates were analyzed by this technol-
ogy. The results of laboratory duplicate analyses are
presented in Table 6-2. The initial analysis of the
duplicate samples ranged from 158 to 4,590 ppm. When
the analysis was duplicated, the results ranged from 130
17
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TABLE 6-2. LABORATORY DUPLICATE RESULTS.
Sample
No.
059D
062
064
066
067
Original
Sample
Result
(ppm)
4,590
748
354
213
158
Laboratory
Duplicate
Sample
Result
(ppm)
4,320
775
395
440
130
Relative
Percent
Difference
(%)
6
4
11
70
19
TABLE 6-3. FIELD DUPLICATE RESULTS.
Sample
No.
059
073
074
086
087
Original
Sample
Result
(ppm)
3,130
8.60
40
7.54
4.94
Field
Duplicate
Sample
Result
(ppm)
4,590
7.42
32.5
5.86
4.17
Relative
Percent
Difference
(%)
38
15
21
25
17
to 4,320 ppm. Field duplicate samples also were
analyzed during the demonstration. Field duplicates are
two samples collected together but brought to the
laboratory with separate sample numbers. Five field
duplicate samples were collected and analyzed by this
technology during the demonstration. The results for the
field duplicate samples are included in Table 6-3. The
RPDs between original samples and their duplicates were
calculated. The RPDs for all duplicate samples ranged
from 4 to 70 percent. Even the best technology that
determines results quantitatively cannot reproduce its
results every time. Therefore, PRC established control
limits like those sometimes used to evaluate laboratory
duplicates. These control limits were then used to
determine whether the difference between a result from
a duplicate and the result from its respective sample was
reasonable. The RPD for each sample pair was calcu-
lated, and the mean RPD and population standard
deviation were determined. The lower control limit was
set at zero because this would mean that the results from
a duplicate and its sample matched perfectly. The upper
control limit was set by multiplying the standard devia-
tion by two and adding it to the mean RPD. The RPD
of each sample pak was then compared to these control
limits. Each was expected to fall within them. If
greater than 90 percent fell within this range, the
technology's precision was considered adequate. If
fewer than 90 percent of them fell within this range, the
data was reviewed, and if no explanation could be found,
the technology's precision was considered inadequate.
The control limits established using the procedure
delineated above were from 0 to 61 percent. Comparing
the RPDs to these control limits showed that only one
sample's RPD was outside the control limit. As a result,
90 percent of RPDs fell within the control limits making
the technology's precision acceptable.
Comparison of Results to Confirmatory
Laboratory Results
The quantitative results of the test kit were analyzed
by using the linear regression techniques and the inferen-
tial statistics detailed in Section 5. All of the data used
for the analyses is presented in Table 6-4. The initial
linear regression analysis was based on results from 32
samples. The concentrations found in eight of the
samples were below the test kit's detection limit and,
therefore, were not used hi the comparative analysis.
The r2 for this regression was 0.19, indicating that little
or no relationship exists between the data sets. A
residual analysis of the data, though, identified samples
59 to 62, 65, 72, 75 and 76 as outliers. PRC removed
these points, recalculated the regression, and defined an
r2 of 0.31, still indicating that little or no relationship
exists between the two data sets. The parameters of this
regression line are shown on Table 6-5. Figure 6-1
shows the regression graphically. The Wilcoxon Signed
Ranks Test was used to verify these results. It indicated
at a 90 percent confidence level that the data was
significantly different from that of the confirmatory
laboratory. These results indicate that this test kit is not
accurate and that it cannot be mathematically corrected
to estimate corresponding confirmatory data. This
places test kit results for the combined soil data set into
the Level 1 data quality category.
The confirmatory laboratory found that 16 of the 32
samples had concentrations less than 100 ppitn. Of these
the test kit detected contamination above the detection
limit hi only 10 samples. The initial linear regression on
these 10 samples defined an r2 of 0.23, indicating that
little or no relationship exists between the two data sets.
A residual analysis of the data identified no samples as
outliers. However, the Wilcoxon Signed Ranks Test
indicated at a 90 percent confidence level that the
method's data was not significantly different from that of
the confirmatory laboratory. This contradicts the
regression analysis and indicates that one or both of the
data sets do not meet the condition of normality required
for regression analysis. Therefore, the regression data
18
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TABLE 6-4. SUMMARY OF DEMONSTRATION DATA.
Sample
No.a
059
059D
060
061
062
063
064
065
066
067
068
069
070
071
072
073
073D
074
074D
075
076
077
078
HNU-Hanby
Environmental Test
Kit
(5 ppm)b
3,130
4,590
1,030
1,400
748
445
354
1,200
213
158
218
540
435
181
5,570
8.60
7.42
40.0
32.5
303
751
508
252
Confirmatory
Laboratory
(ppm)
9,600
10,260
1,008
2,744
138.0
1,610
1,978
1,577
57.80
110.0
47.70
798.0
2,888
289.0
336.0
74.80
78.20
836.0
1,520
3,692
4,590
2,040
1,720
Sample
No.a
079
080
081
082
083
084
085
086
086D
087
087D
088
089
090
091
092
093
094
095
096
097
098
HNU-Hanby
Environmental Test
Kit
(5 ppm)b
562
263
8.16
127
9.46
83.4
5.27
7.54
5.86
5.94
5.17
2.72d
2.14d
2.65d
2.55d
2.43d
2.36d
4.47d
89.4
108
7.63
2.78d
Confirmatory
Laboratory
(ppm)
792.0
2,550
125.0
2,400
270.0
1,140
57.70
6.59
6.88
34.00
51.80
2.58
0.21°
0.55C
0.28°
0.57C
0.1 9C
1.02C
0.088°
59.80
14.60
0.57
All samples numbered before 059 were collected at
the operator of this technology.
Detection limit. When below the detection limit
analysis..
Sample analyzed by Method 8151 A; all other sampl
Result is below detection limit.
thfe
he former Koppers site and, therefore, were not analyzed by
sample's result was not considered during the regression
js were analyzed by Method 8270A.
19
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TABLE 6-5. SUMMARY OF REGRESSION AND RESIDUAL STATISTICS
N
Y-int
Wilcoxon Probability
All Data 37 0.27 126
<100ppm 16 0.16 14
>100ppm 20 0.04 308
0.16
1.2
0.22
Significant difference
No significant difference
Significant difference
Notes:
N Number of data points
r2 Coefficient of determination adjusted for variance
Y-int Y-axis intercept of the regression line
FIGURE 6-1. REGRESSION OF DATA.
t OKtflViwn tpfMnf
i 1
»
i
I
| '
M.PMIV.
" -
. .
TnxtNogoUws
«
Tnw Positives
*
*
FofceNegffltoj
Confkmttoty Lctxxitoty Cone«nti«ion (ppm)
was considered suspect. These results indicate that this
technology produces data statistically similar to the
confirmatory laboratory. This factor places this technol-
ogy into the level 2 data quality category for the samples
with PCP concentrations less than 100 ppm; however,
the data cannot be mathematically corrected.
The confirmatory laboratory found that 23 of the 32
samples contained PCP concentrations of more than 100
ppm. The initial linear regression on these samples
defined an r2 of 0.09, indicating that no relationship
exists between the two data sets. A residual analysis of
the data identified samples 59, 72, and 79 as outliers.
PRC removed these three points, recalculated the
regression, and defined an r2 of 0.04, still indicating that
no relationship exists between the two data sets. The
Wilcoxon Signed Ranks Test verified these results.
These results indicate that this test kit is not accurate and
that it cannot be mathematically corrected to estimate
corresponding confirmatory data. This factor places this
technology for the samples with PCP concentrations
above 100 ppm into the Level 1 data quality category.
To compare the precision of the test kit's results to
the precision of the confirmatory laboratory's results, a
Dunnett's Test was performed on the RPDs determined
from the field duplicate samples and their respective
samples. The Dunnett's Test determines the probability
that the data sets on which it is based are the same. If
the RPDs from the confirmatory laboratory and those
from the technology are the same, then it can be as-
sumed that the precisions are also similar. A Wilcoxon
Signed Ranks Test was used to supplement the Dunnett's
test results. The Wilcoxon Signed Ranks Test was used
to test the hypothesis that no significant difference exists
between the technology's RPDs and the:confirmatory
laboratory's RPDs. When the Dunnett's Test compared
the RPDs between the method's data set and the confir-
matory laboratory data set, it indicated the precisions
were statistically similar. The Wilcoxon Signed Ranks
Test confirmed this data.
20
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Section 7
Applications Assessment
The principal advantage of the test kit is that it can
analyze a large number of samples in a short period oi
time. Other advantages include the following: (1) the
test kit is inexpensive when compared to formal labora-
tory analysis using EPA-approved methods for PCP,
(2) it is simple to operate even for individuals with no
prior experience using the test kit, (3) it is portable and
can be operated outdoors, (4) it requires electricity, but
a rechargeable battery can be used without the need for
an electrical hookup at the site, and (5) its reagents do
not require refrigeration.
The principal limitations of the test kit are (1) that
it can only be used on sites where petroleum products
are the carrier solvent for PCP, and (2) that it provides
only an indirect measurement of PCP concentration.
The test kit requires detailed site-specific calibration
prior to use. This indirect measurement is performed
through a measurement of petroleum hydrocarbons in a
sample. An estimated ratio of PCP versus the petroleum
hydrocarbon carrier is calculated and used to correct the
sample results. The test kit, therefore, can only be used
at sites where the PCP to petroleum carrier solvent ratio
is stable, and it cannot be used to determine PCP results
in samples where no petroleum hydrocarbon carriers are
present. The ratio of PCP hi a petroleum hydrocarbon
carrier may vary due to manufacturing processes,
dilution variances, and the volatility and weathering of
petroleum hydrocarbon carriers. This volatility and
weathering may change with depth, and thus, the
ratio-based calibration may vary with depth. All of
these variances can lead to errors when interpreting PCP
results. It is essential that samples from the site be
investigated and analyzed for the purpose of preparing
site-specific calibration data.
The test kit's estimation of PCP concentrations in
samples was generally found not to agree with results
from the confirmatory laboratory. However, for
samples contaminated with less than 100 ppm of PCP,
the technology's data was statistically similar to the
confirmatory data. The test kit contains the hazardous
chemicals heptane, carbon tetrachloride, and aluminum
chloride. Proper safety and disposal practices need to be
employed when using the technology.
The test kit can be used to provide screening results
for PCP soil samples. HNU-Hanby Systems also
markets it for use on water samples. The demonstration
results indicate that the test kit is most accurate with
samples containing less than 100 ppm PCP. Therefore,
it should only be used to produce Level 2 data at sites
where the PCP action level is below 100 ppm.
Generally, the larger the site or the larger the
number of samples which will be collected, the greater
the advantage of using the test kit. The use of the test
kit at these types of sites will decrease the cost of the
investigation by enabling more work to be completed
during a single sampling visit. The use of the test kit
can allow work to continue without having to wait for
confirmatory laboratory results. The results of the
demonstration indicate that the test kit can be used as an
EPA Level 1 screening tool over a wide concentration
range. However, the kit will not detect PCP if the
carrier solvent is heavily weathered and is no longer
present in the sample. This could lead to a false deter-
mination of no PCP present in the sample. This failure
to detect the presence of a contaminant does not meet
Level 1 criteria. For PCP concentrations of less than
100 ppm at a site where the PCP-to-carrier ratio appears
stable, this demonstration indicates that the test kit can
produce Level 2 data. The determination of data quality
levels will be site-specific and dependent on the stability
of the PCP-to-carrier ratio. Field investigators should
confirm that results obtained from the test kit correlate
with confirmatory laboratory results. Field investigators
must realize that the test kit is designed only as a
screening tool to assist hi evaluating petroleum contam-
ination and its use as a PCP screening tool is very
site-specific.
21
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Section 8
References
PRC Environmental Management, Inc. (PRC). 1993. "Final Demonstration Plan for the Evaluation of
Pentachlorophenol Field Screening Technologies." EPA Contract No. 68-CO-0047.
Stanley, T. W. and S. S. Verner. 1983. "Interim Guidelines and Specifications for Preparing Quality Assurance
Project Plans." U.S. Environmental Protection Agency, Washington D.C. EPA/600/4-83/004.
U.S. Environmental Protection Agency (EPA). 1990. "Quality Assurance/Quality Control Guidance for Removal
Activities." EPA/540/G-90/004. April.
22
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Environmental Protection Agency
National Risk Management
Research Laboratory (G-72)
Cincinnati, OH 45268
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