&EPA
United States
Environmental Protection
Agency
EPA/540/MR-95/528
August 1995
SUPERFUND INNOVATIVE
TECHNOLOGY EVALUATION
Demonstration Bulletin
Field Analytical Screening Program: POP Method
U.S. Environmental Protection Agenctf
Technological Description: The Superfund Innovative Technol-
ogy Evaluation (SITE) Program evaluates new technologies to
assess their effectiveness. This bulletin summarizes results from
the 1993 SITE demonstration of the Field Analytical Screening
Program (FASP) Pentachlorophenol (PCP) Method to determine
PCP in soil and water. The demonstration was conducted by the
National Exposure Research Laboratory, Las Vegas, Nevada.
The U.S. Environmental Protection Agency (EPA) Superfund
Section developed the FASP PCP Method.
The FASP PCP Method uses a gas chromatograph (GC) equipped
with a megabore capillary column and a flame ionization detector
(FID) and an electron capture detector (ECD) to identify and
quantify PCP. Gas chromatography is an EPA-approved method
for determining PCP concentrations in soil, water, and waste
samples. The FASP PCP Method is an abbreviated, modified
version of these EPA-approved methods.
Soil and water samples are extracted with methyl tert-butyl ether
before GC analysis. To remove interferences caused by petro-
leum hydrocarbons, which are common PCP carriers, an acid-
base partition cleanup step is used. In this step, the petroleum
hydrocarbons are removed from the reagent water, while the
potassium phenates remain in the reagent water. Then the solu-
tion is acidified and the pentachlorophenates are transformed
back into PCP. The acidified solution is then solvent extracted.
The sample extracts are concentrated and used for GC analysis.
Instrumentation and equipment required for the FASP PCP Method
are not highly portable. However, when mounted in a mobile
laboratory trailer, the method can be operated on or near most
sites relatively easily. Use of this method requires electricity, and
PCP standards require refrigeration. An exhaust hood and GC
carrier gases also are needed. For the method to produce reli-
able results, it must be operated by a trained and experienced
operator. A minimum of 6 mo experience in using a GC and a
minimum of 1 mo experience in analyzing phenols is suggested
for the operator. The total cost of the analytical equipment is
$23,214. The costs of renting comparable equipment should
range from $1,500 to 2,500 per month. The reagents and equip-
ment needed to perform the extraction, preparation, and analysis
of soil and water samples was estimated to be $5,000.
Waste Applicability: The FASP PCP Method is designed to
provide quick, accurate results for PCP concentrations in soil and
water in the field. This method also can detect and quantify other
phenols. The detection limit for the method for soil samples is 0.8
mg/kg; for water samples it is 200 |ig/L using the FID and 0.5 jig/
L using the ECD. The average number of samples analyzed in a
10-hr day during the demonstration was 14.
The FASP PCP Method can provide quantitative results with
relatively low detection limits at sites where PCP contamination is
suspected or known. This method is specific to PCP; however, it
is susceptible to interferences such as PCP carrier solvents
(diesel fuel). Where high levels of diesel fuel are suspected, a
rigorous cleanup step is needed to minimize the effects of inter-
ferences. The FID detector will provide only high parts per billion
detection levels of PCP. To achieve a lower detection limit, the
sample extracts must be [analyzed using an ECD.
Advantages
• Inexpensive when compared to formal laboratory analysis
• High sample throughput
• Quick quantitative results
• Detection limit for water less than maximum contaminant level
of 1.0 ng/L i
• Specific to PCP; can identify other phenols as well
• Gas chromatography is an EPA-approved method for determin-
ing PCP in soil and water
Limitations
• Not very portable; requires a trailer, electricity, and refrigeration
• Relative high initial equipment cost
• Requires experienced GC operator
• Susceptible to interferences, especially from carrier solvents
such as diesel fuel ;
• Uses hazardous chemicals for extraction and analysis
Demonstration Results: This demonstration consisted of ana-
lyzing 112 soil samples, 16 water samples, 14 soil field dupli-
cates, 10 water field duplicates, two soil performance evaluation
(PE) samples, and three; water PE samples. Samples were col-
Printed on Recycled Paper
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looted and analyzed from two sites to evaluate the effects of
different sample matrices and different PCP carriers, diesel fuel
and isopropyl ether-butane. Each sample was evaluated by both
the FASP PCP Method and by confirmatory laboratory analysis
according to EPA SW-846 methods or by EPA 500 Series Meth-
ods for Organics In Drinking Water.
In a comparison of the FASP PCP Method's results to those of a
confirmatory laboratory, it was found that the method produced
Level 2 data for soil and water samples in which the PCP carrier
was isopropyl ether. Level 1 data was produced for soil and water
samples in which diesel fuel was the PCP carrier.
The accuracy of the FASP PCP Method was assessed by analyz-
ing PE, matrix spike (MS), and matrix spike duplicate (MSD)
samples, and by direct comparison to data from the confirmatory
laboratory. Precision for this technology was assessed by analyz-
ing laboratory duplicate, field duplicate, and MS/MSD samples.
Operational characteristics, performance factors, and specificity
of the FASP PCP Method also were evaluated.
Tho GC must undergo an Inltialcalibration (ICAL), which involves
analyzing standards containing three different concentrations of
PCP. When an acceptable ICAL has been completed, sample
analysis can begin. Microliter amounts of the extracts are injected
into a GC, which is equipped with a megabore capillary column.
Sample peak retention times and peak responses are then com-
pared to the PCP standards to identify and quantitate the con-
centrations of PCP in the sample. Samples with concentrations
outside the calibration range must be diluted and rerun. Daily
continuing calibrations are used to monitor the performance of
the GC.
An Innovative Technology Evaluation Report (ITER) describing
the complete demonstration will be available in late 1995.
Acknowledgment: This Bulletin was prepared by the U.S. Envi-
ronmental Protection Agency, Office of Research and Develop-
ment, National Risk Management Research Laboratory, Cincinnati,
OH 45268.
For Further Information
EPA Project Manager:
Mr. Lary Jack
U.S. Environmental Protection Agency
944 EasfHarmbri
Las Vegas, NV 89193-3478
(702) 798-2373
Fax (702) 798-2692
United States
Environmental Protection Agency
National Risk Management Research Laboratory (G-72)
Cincinnati, OH 45268
Official Business
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EPA/540/MR-95/528
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