&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-
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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

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