EPA/540/2-89/013
SUPERFUNDTREATABILITY
CLEARINGHOUSE
Document Reference:
Tierman, T.O., Ph.D., "Development of Treatment Data on the KPEG Process for
CERCLA/BDAT Standards." Approximately 60 pp. Prepared for U.S. EPA, HWERL.
January 1988.
EPA LIBRARY NUMBER:
Superfund Treatability Clearinghouse - EUTV
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SUPERFUND TREATABILITY CLEARINGHOUSE ABSTRACT
Treatment Process: Physical/Chemical - Dechlorination
Media: Soil/Generic
Document Reference: Tierman, T.O., Ph.D., "Development of Treatment
Data on the KPEG Process for CERCLA/BDAT
Standards." Approximately 60 pp. Prepared for
U.S. EPA, HWERL. January 1988.
Document Type: Contractor/Vendor Treatability Study
Contact: C. Rodgers
U.S. EPA, HWERL
Cincinnati, OH 45268
513-569-7757
Site Name: BOAT SARM - Manufactured Waste (Non-NPL)
Location of Test: Wright State University, Dayton, Ohio
BACKGROUND; This report describes the results of laboratory studies on
KPEG treatment of synthetic soils contaminated with a variety of compounds,
both organic and inorganic. The U.S. EPA provided soils to Wright State
University to conduct the KPEG study. Problems were encountered in
obtaining homogeneous soil samples and in the analysis of contaminants in
the soils and in the analysis for VOCs in the reaction products of the KPEG
treatment tests.
OPERATIONAL INFORMATION; EPA provided 50 pounds each of four different
standard analytical reference matrix (SARM) samples which were prepared
under a separate work assignment. Each of the soil samples were spiked
with different concentrations of known volatile organic compounds
(ethylbenzene, xylene, tetrachloroethylene, chlorobenzene, styrene,
1,2-dichloroethane and acetone), three semi-volatiles (anthracene, bis
(2-ethylhenyl) phtalate and pentachlorophenol) and seven metals (Cd, Ca,
Cr, Pb, As, Ni and Zn). The authors found the SARM soil samples to be
non-homogenous with condensation and pooling of the liquid contaminants
occurring in the soil samples. Samples could not be homogenized due to the
high moisture content of the sample. 500 gram aliquots of the SARM soils
were removed, placed in a two liter reaction vessel and reacted with KPEG
for 1 hour at 100 C to observe if the KPEG process effectively removed
certain contaminants. The KPEG reagent was provided by the U.S. EPA.
Samples before and after treatment were measured by purge/trap GC/MS. The
analytical procedures had to be extensively modified due to the high levels
of contaminants present in the reaction products. The author attributed
the substantial scatter in the results to the problem of the nonhomogenous
SARM that were used. Heavy metal analyses were performed by an EPA CLP
Laboratory.
PERFORMANCE; The metal analysis in treated and untreated samples revealed
that KPEG treatment and subsequent water washing did not reduce the metal
concentrations. Overall metal materials balance was poor. The volatile
3/89-37 Document Number: EUTV
NOTE: Quality assurnce of data may not be appropriate for all uses.
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and semi-volatile organic data also exhibited very poor mass balance and a
large scatter in results. However, the KPEG appears to have reacted with
and essentially completely destroyed dichloroethane and tetrachloro-
ethylene. The other two chlorinated organics were not' destroyed since
temperatures higher than 100 C are required to dechlorinate these
compounds. The other organic compounds, xylene, ethylbenzene and styrene
do not appear to be destroyed by this treatment. The acetone data is
suspect due to volatility problems, instrument saturation, etc. A QA
review could not be conducted due to the enormous concentrations of the
analyte present in the various samples and the inapplicability of EPA
analytical methods. The analytical data obtained are believed to be, at
best, semi-quantitative indicators of the KPEG processes ability to treat
contaminated soils.
CONTAMINANTS;
Analytical data is provided in the treatability study report.
breakdown of the contaminates by treatability group is:
The
Treatability Group
WOl-Halogenated Aromatic
Compounds
W03-Halogenated Phenols,
Cresols and Thiols
W04-Halogenated Aliphatic
Solvents
W07-Heterocyclics and
Simple Aromatics
W08-Polynuclear Aromatics
W09-0ther Polar Organic
Compounds
WlO-Non-Volatile Metals
Wll-Volatile Metals
CAS Number
108-90-7
87-86-5
107-06-2
127-18-4
100-41-4
100-42-5
1330-20-7
120-12-7
67-64-1
117-81-7
7440-47-3
7440-50-8
7440-02-0
7440-38-2
7440-43-9
7439-92-1
7440-66-6
Contaminants
Chlorobenzene
Pentachlorophenol
1,2-dichloroethane
Tetrachloroethene
Ethylbenzene
Styrene
Xylene (total)
Anthracene
Acetone
bis (2-ethyl hexyl)
phthalate
Chromium
Copper
Nickel
Arsenic
Cadmium
Lead
Zinc
3/89-37 Document Number: EUTV
NOTE: Quality assurnce of data may not be appropriate for all uses.
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WRIGHT
Wngnt State University
Dayton. Ohio 45435
January 13. 1988
Ms. Judy L. Hassling
Work Assignment Manager
PEI Associates, Inc.
11499 Chester Road
Cincinnati, OH 45246
Dear Ms. Hessling:
Enclosed are two copies of the Final Report on our work
accomplished under PEI Associates, Inc. Subcontract No. 777-87
to U.S. EPA Contract No. 68-03-3413, Work Assignment No. 0-2, PN
3741-2 with Wright State University. We have forwarded
additional copies to U.S. EPA/HWERL (Cincinnati), Mr. Charles
Rogers and to the designated EPA Washington Office.
If you have questions concerning the report, please don't
hesitate to contact us.
Sincerely,
Thomas O. Tiernan, Ph.D,
Professor of Chemistry
Enclosure
copy: C. Rogers, U.S. EPA/HWERL
J. Knapp, CDM Federal Programs Corp.
J. Cunningham, U.S. EPA/Washington
B. Thompson, U.S. EPA/HWERL
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FINAL REPORT
DEVELOPMENT OF TREATMENT DATA ON THE KPEG PROCESS FOR
CERCLA/BDAT STANDARDS
ACCOMPLISHED UNDER PEI ASSOCIATES, INC. SUBCONTRACT NO. Ill-SI
TO U.S. EPA CONTRACT NO. 68-03-3413, WORK ASSIGNMENT NO. 0-6,
PN 3741-6, WITH WRIGHT STATE UNIVERSITY
Prepared By
THOMAS 0. TIERNAN, PH.D.
WRIGHT STATE UNIVERSITY
175 BREHM LABORATORY
DAYTON, OHIO 45435, U.S.A.
Submitted To
MS. JUDY L. HESSLING
WORK ASSIGNMENT MANAGER
PEI ASSOCIATES, INC.
11499 CHESTER ROAD
CINCINNATI, OHIO 45246
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I. INTRODUCTION
Under PEI Associates, Inc. Subcontract No. 777-87 to U.S.
EPA Contract No. 68-03-3413 (Work Assignment No.-0-6, PN 3741-6),
Wright State University accomplished studies to generate bench-
scale data on KPEG treatment of soils which were representative
of those found at Superfund sites. Such soils contain a mixture
of volatile and semivolatile organic and metallic contaminants.
The data generated in this project is intended for use in setting
best demonstrated available technology (BDAT) treatment standards
for CERCLA soil and debris under the RCRA Hazardous and Solid
Waste Amendments (HSWA) of 1984. More detailed information on
the background and scope of this overall project is provided in
the "Quality Assurance Project Plan (QAPP) for Development of
Treatment Data on the KPEG Process for CERCLA/BDAT Standards"
prepared by PEI Associates, Inc. and Wright State University
(June, 1987), which was submitted to U.S. EPA. The Final Report
describing the results of Wright State's work on this program are
presented herein.
II. EXPERIMENTAL PROCEDURES
A. Soil Samples Tested In This Study
For the purposes of the study described herein, EPA provided
PEI/WSU with approximately 50 Ibs . of each of four standard
analytical reference matrix samples (SARMS) which were prepared
under a separate work assignment. Each of these soils was spiked
with known concentrations of seven volatile organic compounds
( ethylbenzene , xylene, tetrachloroethylene , chlorobenzene,
styrene, 1,2-dichloroethane, and acetone), three semivolatile
organic compounds (anthracene, bis(2-ethylhexyl) phthalate, and
pentachlorophenol), and seven metals (cadmium, copper, chromium,
lead, arsenic, nickel, and zinc). Each of the four soils were
spiked at different concentrations with these chemicals and
metals. The anticipated concentrations of these components are
listed in the PEI/WSU Quality Assurance Project Plan (QAPP)
mentioned earlier in this report.
The four SARMS just discussed were received from PEI
(delivered by PEI personnel) at Wright State on July 24, 1987,
well after the initially scheduled date. As projected in the
Anticipated Project Schedule presented in the QAPP for this
study, the KPEG treatment was originally scheduled to begin on
July 1, 1987. Therefore, a significant delay was imposed on
Wright State's work owing to this late receipt of the soil
samples. The SARM samples were at ambient temperatures when
delivered and had apparently not been refrigerated during
transport. In order to minimize possible losses of the more
volatile organic components, the sample containers were
refrigerated immediately upon receipt by Wright State.
Upon receipt of the four SARMS, each-of which was contained
in a five-gallon metal can fitted with a compression lid and
sealed with duct tape, the shipping containers were opened in
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order to inspect the soils. The following observations were made
regarding the condition of these samples. The indicated sample
designation or identifying number is that which appeared on the
sample container when it was received.
1. SARM-I-1
This sample was observed to be relatively wet and to have
rust particles on the top surface. These particles had been
dislodged from the inside of the container lid (which was
adjacent to the soil) which had rusted or corroded, presumably
after the sample had been packaged. Liquid condensate was
visible on the inside of the lid of the five-gallon can
containing the sample. Owing to the moisture content of this
soil sample, it could not be mixed effectively before removing
aliquots for treatment. Moreover, upon closer inspection, the
soil was observed to contain small stones or soil agglomerates.
These several observations clearly indicated that this soil
sample was not homogeneous and it was therefore impossible to
obtain a truly representative aliquot for use in the treatment
tests.
2. SARM-II-1
This sample appeared to be relatively dry and no rust was
observed on the inner lid of the sample container or on the top
of the soil surface. Because this sample was drier, it could at
least be stirred, in an effort to mix and homogenize it somewhat,
before subsampling. As with the other samples, small stones or
aggregates of soil particles were visible within the sample.
3. SARM-III-2
This sample was a thick mud and was virtually impossible to
manipulate. The sample could not be stirred at all prior to
subsampling. Again, liquid condensate was visible on the inside
of the lid of the five-gallon sample container, and the lid had
rusted or corroded. Rust particles had dropped from the lid onto
the surface of the soil in the container.
4. SARM-IV-1
This sample was very wet and standing pools of liquid were
visible in depressions in the soil surface. Again, liquid
condensate and rust or corrosion were observed on the inner
surface of the lid of the sample container and rust particles
were visible on the top of the soil surface. It was impossible
to effectively mix this sample, which was clearly inhomogeneous,
prior to subsampling, and a truly representative aliquot could
not be obtained for the KPEG treatment tests.
Following the initial inspection of the SARMS delivered to
Wright State by PEI, the sample containers were resealed by
replacing the lids, and information on the condition of the
samples was communicated to U.S. EPA/KWERL (C. Rogers). Since
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these SARMS were the only soils available for use in the KPEG
tests, Wright State was instructed to proceed with the tests
using these materials, and taking a sample in the best manner
possible. However, it was requested that detailed information on
the sample condition be provided in Wright State's report on the
test results.
Immediately prior to the first series of KPEG destruction
tests, which were conducted on Sept. 9-10, 1987, the SARM sample
containers were again opened and aliquots were removed for use in
the tests and for analyses. Four portions of soil were removed
from each container (after briefly stirring the samples in cases
where this was possible): a) approximately 500 grams of each
soil were transferred to separate one-liter bottles fitted with
Teflon-lined lids for use in the KPEG tests; b) approximately 40
grams of each soil were transferred to separate sample bottles
for shipment to another laboratory for metals analyses, as
instructed by EPA/PEI; c) approximately 40 grams of each soil
were transferred to separate 40 mL VOA bottles (filled to the
top) for retention as archive samples; d) additional portions,
approximately 60 grams of each soil were transferred to separate
amber bottles, again for retention as archive samples. Upon
removal of this initial set of samples, the sample cans were
again resealed by attaching the lids and resealing the lids with
duct tape. The portions of the SARMS to be used in the KPEG
destruction tests were taken immediately to the laboratory where
these tests were conducted.
B. KPEG Treatment of the Soils
The procedures utilized for the KPEG treatment of the soils
are detailed in the following. KPEG treatment was accomplished
using four sets of reaction vessels, one for each soil, the
reactions being run concurrently.
1. Apparatus
Each test apparatus consisted of a 2-liter reaction vessel
mounted within a temperature-controlled heating mantle. A
thermocouple was inserted between the reaction vessel and the
mantle in order to monitor the temperature of the mantle itself.
Each reaction flask was fitted with a cover which attached to the
flask by a ground glass joint and a Teflon gasket, the seal being
accomplished by a metal clamp. The top of each vessel
incorporated four ground glass joint openings, through which
equipment could be inserted. A motor-driven Teflon stirring
shaft having 4 blades on the end within the flask was inserted
through a water-cooled bearing into the center opening of the
vessel top. This stirrer was operated at 100 rpm during the
reaction. A thermometer with a ground glass joint was inserted
through the second opening in the vessel lid to monitor the
temperature of the reaction mixture. A ground glass joint
attached to a nitrogen purge gas tube was inserted through the
third opening in the reaction vessel. This permitted
introduction of a nitroaen blanket over the reaction mixture
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prior to heating in order to reduce the possibility of
reaction/explosion of unstable organic products which might be
evolved from the reaction mixture. Also, at the end of the
reaction, the head-space of the reaction vessel .was purged with
Nz through the condenser and solid sorbent trap in order to
collect any remaining volatile organic reactants/products .
Finally, through the last opening in the top of the reaction
vessel, a water-cooled condenser fitted with a ground glass joint
was inserted. At the top of the condenser a solid sorbent trap,
packed with 7 grams of Tenax, 20 grams of XAD-2 resin, and 10
grams of activated carbon, was attached to trap any volatiles not
condensed by the water-cooled condenser.
2. KPEG Reaction Test Procedures
The KPEG reagent used in these tests was supplied to Wright
State directly by U.S. EPA/HWERL and was transported to Wright
State by Mr. Charles Rogers of that organization. The label on
the container of KPEG supplied by EPA and used in the tests
described herein showed the following:
KPEG (400): 5 moles
KTEG (200): 5 moles
Prep. Sept. 4, 1987
The detailed procedures utilized for each of the four
destruction reaction tests with the four SARMS were as follows:
a. Transfer the soil from the 1 L bottle to the 2 L reaction
flask, and record the weight of soil transferred.
b. Add 200 mL of DMSO, and mix with a spatula until the mixture
is homogeneous.
c. Add 50 g of solid KOH pellets and mix.
d. Assemble the apparatus described above.
e. Purae the reaction vessel with nitrocren aas for 10 minutes at
a flow rate of 80 mL/min.
f. Add 400 mL of ambient temperature KPEG through an addition
funnel.
g. Adjust the Nz purge flow to 10 mL/min.
h. Stir the reaction mixture continuously for 30 min at ambient
temperature.
i. Apply heat and increase the reaction mixture temperature
(thermometer reading) to 100°C.
j. Maintain the 100°C temperature while- stirring continuously,
with continuous Nz purge gas flow for a period of 2 hours.
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k. Remove the heating mantle and allow the reaction mixture to
cool to ambient temperature, while continuing stirring and purge
flow.
1. Increase the N2 purge gas flow to 80 mL/min for a period of 15
minutes, while continuing to stir the mixture.
m. Open the vessel and transfer the total reaction mixture- to
four 500 mL amber bottles and record the weights.
n. Transfer contents of the trap (tenax, XAD, activated carbon)
to a 250 mL bottle, seal the bottle and refrigerate it.
o. Store all reaction products under refrigeration until further
workup is accomplished.
In the course of these reactions, it was observed that
condensation formed on the inside of the lid of the reaction
vessel when the temperature was elevated to 100°C, but this
disappeared when the reaction mixture was cooled to ambient
temperature. Also, during the reaction, the stones or soil
aggregates present in the SARMS were observed to settle to the
bottom of the vessel.
The measured quantities of the SARMS and the reagents used
in each of the four reactions in the first test series, as well
as the quantities of solid sorbents used with each reaction
vessel are shown in Table A.
3. Processing of KPEG Reaction Products-First Test Series
The reaction products derived from the first series of KPEG-
treatment tests were processed according to the following
procedures.
a. K?EG/Soil Separation Procedure
i) Remove the four 500 mL bottles containing each of the
treated SARM samples from the storage refrigerator.
ii) Centrifuge the four bottles at 700 rpm for 15 minutes in a
refrigerated centrifuge to separate the soil and KPEG phases.
iii) Decant the KPEG layer into a 500 mL amber glass bottle.
iv) Seal the bottle containing the KPEG phase and store it in
the refrigerator.
v) Continue processing of the residual soil left in the original
sample bottles, as described below.
b. Soil Washing Procedure
i) For each of the treated SARM samples, add 50 mL of KPLC
arade (B&J) water to each of the four bottles containing the
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residual soil (from which the KPEG has been separated).
ii) Place each bottle on a wrist action shaker and agitate for
30 minutes.
iii) Centrifuge the bottle at 700 rpm for 15 minutes in a
refrigerated centrifuge to separate the aqueous and soil phases.
iv) Determine the pH of the aqueous phases with pH paper (the
solution should be basic).
v) Transfer the aqueous liquid layer to a 500 mL amber glass
bottle by decanting.
vi) Add another 50 mL of HPLC grade water to the soil in each of
the four bottles, agitate the bottles for 30 minutes, and
centrifuge, as described above.
vii) Remove the aqueous phase and pool it with the previous
water wash in the 500 mL bottle. Seal the bottle and refrigerate
it until just prior to preparation for GC-MS analysis.
viii) Seal the bottles containing the residual treated and washed
soil and refrigerate then until just prior to preparation for GC-
MS analysis.
The quantities of the several process samples resulting from
KPEG-treatment of the four SARM samples (residual soil following
washing, spent KPEG, spent washwater and spent solid sorbents in
trap) are listed in Table B.
c. Preparation of Composite Treated Soil Sample for Analysis
Following the water washing just described, a representative
composite sample of the KPEG-treated soil was prepared for
analysis. This was accomplished by vigorously mixing the
residual soil in each of the four bottles in which each treated
soil was contained, then withdrawing equal aliquots of soil from
each of the four bottles and combining these, again with vigorous
mixing, in one new bottle, for each of the treated soils. The
new bottles were then sealed with Teflon-lined lids and stored
under refrigeration until just prior to analyses.
d. Shipment of Portions of Process Samples from KPEG Treatment
of SARM Samples to Other Laboratories for Metals Analyses and
TCL? Deliminations
As instucted by PEI in a Memorandum of Sept. 1, 1987, which
was received from Judy Hessling of PEI, portions of the various
process samples resulting from the KPEG treatment of the SARM
samples, first test series, were packaged and shipped to two
other laboratories. One of these sample sets, consisting cf
approximately 20 g. of each untreated SARM sample, 10 g. of each
residual treated soil following washing, 20 mL of the spent KPSG
reaaent from each of the four tasts, and 20 mL of the water used
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to wash each of the four created soils following treatment, was
shipped by Federal Express under Chain-of-Custody, to Analytical
Enterprises, Inc., Columbus, South Carolina, for metals analyses.
A second shipment, consisting of several portions of the residual
KPEG treated and water-washed soils only (three separate portions
of approximately 70 g., 100 g. and '25 g., respectively, for each
of the four treated SARM samples) , were shipped by Federal
Express under Chain-of Custody, to Wan Technologies, Atlanta, GA,
for TCLP testing. Both of these shipments were shipped by Wright
State University on Sept. 10, 1987.
4. KPEG Reaction Tests-Second Test Series
The second set of KPEG-treatrnent tests on the four SARM soil
samples was conducted Nov. 3 - Nov.9, 1987. Immediately prior to
this series of tests, the sample containers (5 gal. cans) were
opened and aliquots of the samples were removed for use in the
tests. The samples cans were then resealed by attaching the
lids and resealing with duct tape.
The test apparatus and the experimental procedures employed
for the second KPEG-treatment test series were quite similar to
those applied for the first test series, as already described,
with the following exceptions: a) 500 mL reaction flasks were
used in this test series; b) approximately one-fourth of the
quantities of soil and reagents used in the first test series
were employed in the second test series (see Table C for exact
quantities); c) the solid sorbent trap used in the second test
series was packed sequentially with 10 g. of Tenax, and 25 g. of
XAD-2 resin, and these sections were separated by a glass frit
from a 12 g. section of activated carbon.
Following each treatment test, the entire contents of the
reaction flask were transferred to a single 500 mL amber glass
bottle fitted with a teflon-lined lid, and the bottle was sealed
and refrigerated until just prior to phase separation. The
Tenax-XAD-2 portion of the solid sorbent was transferred to a 100
mL amber glass bottle fitted with a Teflon-lined lid and the
bottle was sealed and refrigerated until just prior to analysis.
The charcoal portion of the trap was transferred to a separate
bottle and retained.
The soil/KPEG separation and recovery procedures were
exactly as described for the first test series (except that all
of the treated sample mixture was contained in a single bottle,
as already noted). The soil washing procedure utilized for the
second test series was also just as described for the first test
series except that only 100 mL of water was used here (two 50 mL
portions for each of two wash cycles). The quantities of treated
and washed soil, spent KPEG, spent wash water and spent solid
sorbents resulting from the second test series are shown in
Table D.
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5. Materials. Chemicals and Reagents Used in Tests
The materials, chemicals and reagents used in these tests
and the sources of these are as follows:
Reaction Vessel and Components ' Ace Glass Inc.
Tenax GC, 35/60 mesh Alltech Associates
XAD-2, 16/50 mesh Supelco, Inc.
Charcoal, 6/14 mesh Fisher Scientific
DMSO Sigma Chemical Co.
KOH Pellets (A.C.S.) Fisher Scientific
KPEG reagent, labelled: C. Rogers/U.S. EPA/HWERL,
KPEG 400: 5 moles Cincinnati, Ohio
KTEG (200): 5 moles
Prep. Sept. 4, 1987
C. Analyses of Reaction Products From KPEG Treatment Tests
1. Summary of Problems Encountered in Analyses
Prior to describing the analytical methods which were
employed to characterize the reaction products resulting from
KPEG-treatment of the SARM samples, it is appropriate to discuss
the extensive problems which were encountered in attempting to
analyze the products, and the rationale for the methods which
were finally implemented. It was originally intended to apply
EPA Methods 8240 and 8270 for the Volatile Organics and
Semivolatile Organics, respectively. Owing to a variety of
complications, however, these methods proved to be largely
inapplicable for the analyses required here. The major source of
problems encountered in the analyses originated from the huge
concentrations of the analytes in the original soil samples, and
even in the samples resulting from the treatment tests.
The magnitude of these concentrations was a problem because:
a. The high concentrations required that relatively small
aliquots of both the untreated soil and the several samples
resulting from KPEG treatment be selected for analyses, in an
attempt to avoid overloading the analytical devices utilized. It
is virtually impossible to select a sample aliquot which is truly
representative of the entire bulk sample when such small samples
are taken for analysis, especially when the bulk sample is not
homogeneous and cannot be effectively mixed, as was the case
here .
b. It was impossible to predict "a priori" the concentrations of
the analytes which would be present in the various fractions from
the treatment process, and therefore selection of portions of
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these samples which would yield adequate detection limits for the
analytes of interest, but would avoid saturating or overloading
the analytical devices, was largely a matter of guess work.
Unfortunately, very high concentrations of the organics were
found to be present in many of these samples and therefore the
"guesses" as to the portion of sample selected for analysis were
frequently wrong. This led to repeated saturation of the
instrumentation and numerous repetitive analyses to get even
marginally acceptable data. The performance of the Tekmar Purge-
Trap apparatus is especially devastated by being subjected to
very high saturating concentrations of organics, and this
resulted in long "memory" or holdup of the compounds in the
Purge-Trap apparatus. The result was that carry-over of analytes
(from the previous run) occurred in many of the analyses and
eliminating this (which was never completely accomplished for
acetone) required purging the apparatus for many hours and even
days between analyses. This ultimately required literally
hundreds of analyses to obtain even passable results.
c. The extremely high concentrations present and detected in
many of the treated samples were often outside the range of
instrument calibration, again requiring many extra analyses.
d. The standard EPA procedures for analyzing compounds such as
those encountered in these studies, as documented in EPA's SW846
Manual (Methods 8240 and 8270), were not applicable for various
reasons and had to be modified extensively. For example,
pentachlorophenol (PCP) could not be detected at all in the
samples by direct injection the sample extracts into the GC-MS,
and it was necessary to acetylate or derivatize the PCP prior to
injection. This essentially doubled the time normally required
for such analyses.
e. The U.S. EPA software which is normally utilized for
processing data obtained by EPA Methods 8240 and 8270 was not
generally applicable for the analyses accomplished here because:
i) The EPA software is not desiqned to accomodate sample sizes
smaller than 0.00001 Kg (0.01 gram). In many cases, in the
present analyses, the size of the sample aliquot analyzed was
necessarily less than 0.01 gram, because of the extraordinarily
high concentrations of the analytes present in the samples.
ii) Even in cases where sample sizes were within the range of the
EPA software, the extremely high concentrations of analytes
present and detected usually exceeded the calculation capacity of
the EPA program, and therefore final analytical results could not
be automatically calculated using the EPA software. This also
made it impossible to output the data in the customary SPA
format, using the computer-generated data reporting sheets.
iii) For the reasons discussed, only the calibration curve could
be generated using EPA software control and actual data
calculations had to be accomplished almost entirely by manual
methods.
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f. As already discussed, there' was strong evidence that the
spiked soil samples provided by EPA/PSI were not homogeneous when
received. Upon initial opening of the sample containers,
condensation was observed on the can lid, and pools of liquid
were apparent on the soil surface. -The quantity of water present
in the samples prevented effective mixing and representative
subsampling. Finally, these soils were observed to contain rocks
and other foreign matter which clearly indicated non-homogeneity
and prevented accurate subsampling.
All of the above factors led to large variations in the
analytical results and were directly responsible for the delays
encountered in completing the analyses.
2. Sample Preparation - Volatiles
The procedure followed for preparation and analysis of
various samples from the KPEG-treatment experiments are generally
described in the U.S. EPA SW346 Manual, Method 8240. These
methods were applied to the treated and water washed soil, the
untreated soil, the spent KPEG, the spent wash water, and solid
sorbent trap materials. Exceptions to these procedures are
described in the following.
Initially, the assumption was made that levels of the target
analyte compounds (the compounds with which the SARM samples were
spiked) in the treated samples would be £ 1 mg/kg, due to
destruction and/or volatilization, and the "Low-Level Method" for
sediment/soil and waste samples which is described in section
7.4.3.1 of Method 8240, would therefore be applicable. Procedure
7.4.3.1 (the Low-Level Method) does not involve extraction of the
sample and consumes only 250 ng of surrogate and internal
standards for each analysis of a 1 to 5 g. portion of the sample.
Results obtained for the samples however showed much higher
levels of the target analytes than had been expected and
therefore, insufficient standards were available to accomplish
Procedure 7.4.3.1. In order to proceed with the project using
the existing calibration standard and the calibration curves
already established (in order to minimize delays) the surrogate
spike was accomplished just prior to analysis in the present
case. Therefore, less than 1 g. of high level samples were
purged in the impinaer, while samples with very high levels of
the components-were extracted with methanol (as described in
7.4.3.2), and then spiked with the surrogate/internal standard
mixture prior to analysis.
In order to analyze the Tenax/XAD-2 samples, a thermal
desorption accessory was constructed to heat the sorbent, and
introduce the desorbed components directly into the Tekmar purge
and trap apparatus for subsequent injection into the gas
chromatograph (GC). The analysis procedure involved loading
portions of the Tenax/XAD-2 sample into the thermal desorption
accessory, spiking the sample with the surrogate/internal
standards, and then heating the scrbent for 12 minutes at a
10
-------
temperature at 180°C. Surrogate/Internal Standard 109086-1,
described in the following section of this report, was used in
these determinations.
3. Sample Preparation - Semi-Volatiles
The semi-volatile extraction procedure was adapted from SW-
846, Method 3550, which is specified to be useful for "soils,
sludges and wastes". The same extraction procedure was used for
the untreated soil, treated and water-washed soil, spent wash
water and spent KPEG, because the spent wash water contained some
KPEG, and both the spent wash water and the spent KPEG contained
small amounts of soil. The standards added during sample
preparation (which are described in the following section of this
report) were:
Surrogate Standards 109084-2
Internal Standards 109084-9
The sample preparation procedure involved the following steps:
a. Weighed 0.1 g to 1 g of the sample into a 40 mL vial.
b. Acidified the sample with 50% H2SO* ( to quench the KPEG
reagent, and allow extraction of PCP).
c. Added 10 mL of methylene chloride.
d. The soil was very finely divided (except for small stones or
aggregates) and shaking completely distributed the soil into the
liquid phases. The samples were vigorously shaken for 10 minutes
on a wrist action shaker.
e. Centrifuged the sample for 10 minutes at 1500 rpm to separate
phases.
f. Collected the GHzCl2 layer.
g. The GHzCIz layer was passed through a 3 cm plug of glass wool
packed in a 10 mL pipet to remove any soil particles in the
extract. The glass wool plug was rinsed with two 3 mL methylene
chloride rinses and these were combined with the CHzClz fraction.
h. Reduced the volume to less than 10 mL using a gentle stream
of nitrogen at ambient temperature.
i. Adjusted the volume of the extract to 10.0 mL by adding
CH2C12 .
j. 5 mL to 50 uL of sample were removed for sample analysis.
(the volume withdrawn depending on the estimated level of
analytes in the sample).
k. Added standards to the sample.
1. Added 500 uL of tridecane to the sample.
11
-------
m. Concentrated the sample using a gentle stream of nitrogen at
ambient temperature to a volume of less than 1 mL.
n. Diluted the sample with isooctane to yield a 1 mL final
volume.
o. Concentration of Standards in the final solution were:
Surrogate Stds. 10 ng/mL
Internal Stds. 40 ng/mL
4. Sample Preparation - Pentachlorophenol (PCP)
Since pentachlorophenol was found to be nonchromatographable
when semi-volatile sample fractions were directly introduced into
the GC-MS, a derivatization procedure was employed to permit
analysis of PCP. The procedure utilized is outlined below.
a. A portion of the sample extract (2 mL of the 10 mL prepared
according to the semi-volatile extraction procedure reported
earlier) was reduced to near dryness at ambient temperature, in a
15 .mL vial.
b. The following were added to the sample:
2 mL of isooctane
2 mL of acetonitrile
25 mL of pyridine
10 mL of acetic anhydride
c. The mixture was agitated for 5 minutes on a wrist-action
shaker.
d. 6 mL of 10 millimolar Ha PCM were added to the sample and it
was agitated for an additional 2 minutes on a wrist-action
shaker.
e. The organic layer was removed and transferred to a vial and
the volume was reduced to near dryness at ambient temperature.
f. Rediluted the sample with 1.0 mL of isooctane, and then added
20 ML of Standard No. 109084-9 to each sample.
5. Calibration and Spiking Standards
a. Volatile Standards Preparation
The volatile standards used in these analyses and the source
of these, as well as the standards preparation procedures are
described in the following:
i) Sources of Standard Materials
a) Ethyl benzene, Supelco, Inc.
b) Xylenes, Chem Service
c) Tetrachloroethylene, Supelco, Inc.
12
-------
d) Chlorobenzene, Supelco, Inc.
e) Styrene, Chem Service
f) 1,2-dichloroethane, Supelco, Inc.
g) Acetone, Burdick and Jackson Labs Inc.
ii) Sources and Concentrations of Surrogate and Internal
Standard Materials.
a) Surrogate Standards
i) dio-ethylbenzene, 2 mg/mL, Supelco, Inc.
ii) d<-1,2-dichloroethane, 250 mg/mL, Supelco, Inc.
iii) bromofluorobenzene, 250 mg/mL, Supelco, Inc.
iv) ds-Toluene, 250 mg/mL, Supelco, Inc.
b) Internal Standards
i) bromochloromethane, 20 mg/mL, Supelco, Inc.
ii) l-chloro-2-bromopropane, 20 mg/mL, Supelco, Inc.
iii) 1,4- dichlorobutane, 20 mg/mL, Supelco, Inc.
iv) de-benzene, 2 mg/mL, Supelco, Inc.
iii) Preparation of Volatile Calibration Standards
Prepare stock solutions of the seven native components
by weighing each of the standard materials and diluting with
methanol. Combine aliquots of the seven solutions to give a
stock solution having a concentration of 100 mg/mL. Prepare
dilutions to yield the following calibration standards:
a) Standard 109085-1, 100 ng/pL
b) Standard 109085-2, 50 ng/pL
c) Standard 109085-3, 12.5 ng/pL
d) Standard 109085-4, 2.5 ng/pL
e) Standard 109085-5, 0.5 ng/pL
iv) Surrogate and Internal Standards Mixture
Prepare Standard 109086-1 by combining the 8
surrogate and internal standards described above to provide the
following concentrations in the final solution.
a) dio-ethylbenzene, 225 ng/pL
b) d<-1,2-dichloroethane, 25 ng/pL
c) bromofluorobenzene, 25 ng/pL
d) ds'-toluene, 25 ng/pL
e) bromochloromethane, 25 ng/pL
f) l-chloro-2-bromopropane, 25 ng/pL
g) 1,4-dichlorobutane, 25 ng/pL
h) ds-benzene, 25 ng/pL
b. Semi-Volatile Standards Preparation
The semi-volatile standards used in the analyses and the
source of these, as well as the standards preparation procedures
13
-------
surrogate and internal
we described in the following:
i) Sources of standard materials
a.) Anthracene, Supelco, Inc..
b) DEHP, Supelco, Inc.
c] Pentachlorophenol, Supelco, Inc.
ii) Sources and concentrations of
standard materials
a) Surrogate Standards:
i) di o -acthracene , 2 mg/mL, Supelco, Inc.
ii) x 3 C<> -pentachlorophenol , (solid - WSU prepared solution at 2
mg/mL) , Cambridge Isotope Labs
b) Internal Standards:
i) di o -acenaphthene
ii) diz-chrysene
iii) d4 -1, 4-dichlorobenzene
iv) da -naphthalene
v) di 2 -perylene
vi) di o -phenanthrene
All standards were at a concentration of 4000 pg/mL, as
received from Alltech Associates, Inc.
iii) Semi-Volatile Standards Preparation
Prepare stock solutions of the 3 native components by
weighing each of the standard materials and diluting in
isooctane. Combine aliquots of the 3 solutions to give a stock
solution with a concentration of 50 ng/mL
a) Prepared
contains :
Standard 109084-2 (surrogate standards) which
i) di o -anthracene , 1000 ng/mL
ii) x 3 Cs -pentanchlorophenol , 1000 ng/mL
b) Prepared
contains :
Standard 1090084-9 (internal standards)
which
i) di o -acenaphthene , 2000 ng/mL
ii) di 2 -chrysene, 2000 ng/mL
iii) d< -1 , 4-dichlorobenzene , 2000 ng/mL
iv) da- naphthalene, 2000 ng/mL
v) di 2 -perylene , 2000 ng/mL
vi) di o -phenanthrene , 2000 ng/mL
c) Prepared calibration standards by combining the native,
surrogate and internal standards to give the following
concentrations .
14
-------
40 ng/uL
20
10
5
1
40 ng/ML
20
10
5
1
40
40
40
40
40
ng/ML
Seal-volatile calibration standards
Native Surrogate Internal
Concentration _ Concentration Concentration
109084-4
109084-5
109084-6
109084-7
109084-8
c. Preparation of Semi-Volatile Calibration Standards for PGP
Analysis.
i) 250 pL of each of the five semi-volatile calibration
standards (109084-4 thru 109084-8) were transferred to
15 mL vials.
ii) The derivatization procedure for PCP, described above
was applied to the standard mixture.
iii) Derivatized standards were rediluted to a final volume
of 250 pL.
d. Instrumental Analyses - Apparatus and Procedures
i) Metal Analyses
As already noted, metals analyses were accomplished by a
separate EPA contract laboratory using samples received from
Wright State. Results at these analyses were provided to Wright
State (measured concentrations of the metals in the samples) and
Wright State converted the findings to total quantities of metals
in the total treated samples, using weights of the total samples
and of the aliquots which were provided to the other contract
laboratory. This permitted calculation of percent recoveries of
the several metals in the various KPEG treatment process samples.
These results are described in the following sections of the
report.
ii) GC-MS Analyses of Organics
a) Instrumentation - Volatiles Analyses
1> GC: HNU Systems model GC401
2) MS: Kratos MS-30
15
-------
3) Data System: Kratos DS-90E
4) Interface: Glass Jet Separator
5) Operating Mode: El ionization
6) GC Program: 80° C for 4 minutes 8°C/minute to 220° C and hold.
7) GC Column: 1% SP-1000 an 60/80 cardopack B. 1/8 inch x 8
feet.
8) Purge and Trap Apparatus: Tekmar Liquid Sample Concentrator
LSC-2 parameters for purging and trapping as specified in EPA
Method 8240.
b) Instrumentation - Semi-Volatiles Analyses
1) GC: Carlo Erba 5300 Mega Series
2) MS: Kratos MS-25
3) Data System: Kratos DS-90
4) Interface: Glass Jet Separator
5) Operating Mode: El ionization
6) GC Program: 180°C for 8 minutes 8°C/minute to 300°C and hold.
7) GC Column: 60 meter DB-5, 0.25 mm film thickness; 0.25 mm ID.
8) GC Carrier Gas: H2 at 2.5 kg/cm2
9) Injection Volume: 1 pL injection, in splitless mode
c) GC-MS Procedures - Semi-Volatiles
1) Tuning/Calibration: Tuning and calibration were accomplished
using high boiling PFK.
2) Calibration Standards:
Native Compounds Surrogates Internal Standards
Anthracene dio-Anthracene dio-Phenanthrene
PCP 13C12-PCP dio-Phenanthrene
DEHP di2-Chrysene
Concentration
of each
Standard Number Native is ng/ul Surrogace ng/ul Internal ng/ul
109084-4 (CM-1) 40 40 40
109084-5 (CM-2) 20 20 40
16
-------
109084-6 (CM-3) 10 10 40
109084-7 (CM-4) 55 40
109084-8 (CM-5) 11 40
3) Quantitation Ions: Ions used for quantitation varied somewhat
from EPA suggested ions. In order -to generate a standard curve
with a 40-fold concentration difference, as required here, the
sensitivity of Anthracene had to be decreased in relation to di2 -
Chrysene, so less sensitive ions were chosen for quantitating
Anthracene.
Compound Primary Ion Secondary Ion
Anthracene 176 179
PCP 266 264
DEHP 149 167
dio-Anthracene 188 186
13Ci2-PCP 272 270
dio-Phenanthrene 188 189
di2-Chrysene 240 241
4) Initial MS Calibration: Kratos MS-25 hardware tuned using
high boiling PFK; Calibrated mass range: 130-300.
5) GC Temperature Program: Initial column temperature and hold
time: 180 C for 8 minutes; Column temperature program: 8 C/min;
Final column temperature hold: 300 C
6) Other Temperatures: Injector temperature: 280 C; Transfer
temperature line: 300 C; Source temperature: 300 C.
7) Other Parameters: Column: 60M DB-5 0.25 micron film thickness
0.25 mm ID; Injector: Grob-type, splitless; Injection volume:
lul; Carrier gas: Hydrogen @50 cm/sec.
8) Operating Procedures: No background subtraction was required.
Peaks were widely separated with good response factors so DDE/DDD
degradation test was not run. Response factors were calculated
for standard runs by EPA software using automatic peak detection
and area calculations using the method listed in method 8270,
page 13. Percent relative standard deviation for Response
factors ranged from approximately 20 to 70 percent. Daily
injections of the CM-4 standard were used to verify Response
Factors.
Retention time data and correct response at the appropriate
ions monitored were used for identification. Since this was a
synthetic mixture formulated at extremely high levels, no
interferences were expected (and none were observed.)
Quantitation was accomplished using a combination of EPA
software and manual calculation. Since the EPA software was
limited to sample sizes greater than 0.01 grams, all very high
17
-------
level samples prepped with smaller sample sized were incompatable
with the existing software. In addition, many samples had
concentrations that exceeded the maximum calculation capacity of
the program in micograms per kilogram. Actual results were
calculated by forcing the EPA program to report values in ng/ul
of the actual extract and then manually converting those values
to total milligrams in the sample. Actual calculations therefore
were similiar to those shown in method 8270, page 19, but were
converted to yield total milligrams.
Quality control consisted of daily checks of the standard
injection and appropriate analysis of method blanks. Since this
was essentially a spiked sample program, no other lab spikes were
required for analysis. Quality control limits could not be
established since a minimum of 30 samples of the same matrix are
required to generate meaningful statistics.
d) GC-MS Procedures - Volatiles
The standards and samples were introduced into the gas
chromatograph by the purge-and-trap method except for the sorbent
trap materials in which, they were heated in a specially designed
apparatus and then trapped as described earlier.
The calibration procedure for the volatiles consisted of
analyzing 5 different concentration levels of native compounds
with the appropriate levels of internal and' surrogate standards
in each. Response factors were generated from these standards
using the formula given in EPA Method 8240, section 7.2.7. A
daily standard (one of the calibration standards) was checked
against this calibration to verify the response factors.
Component identification was accomplished by using the
relative retention time and characteristic ions for each
particular volatile component. The appropriate ratio criteria
were used for the characteristic ions. The samples were
quantitated using the formula in Method 8240, section 7.5.2.2.
Recoveries for the surrogate standards were calculated.
Appropriate reagent blanks were analyzed to verify the system
cleanliness for the components of interest.
These samples contained known analytes at such high
concentrations that there were no possible interferences, which
negated the need for library searches on the compounds. All
analytes were of such high levels in most samples that extremely
small sample sizes were necessary to carry out this procedure.
This prevented, the MS software from directly calculating the
final results. The MS, being a magnetic sector instrument
negated the need for use of the 4-bromofluorobenzene tuning
standard.
Mass calibration and other procedures not specifically
discussed here were the same as described above for the semi-
volatile analysis procedures.
18
-------
III. RESULTS
A. Metals
The metals concentrations measured in aliquots of the four
residual KPEG-treated and water-washed SARM soil samples, and in
the spent K?EG and wash water, by Analytical Enterprises, Inc.,
which were reported to PEI/Wright State, were used by Wright
State to calculate the total quantities of these metals in the
residual soils, spent KPEG, and wash water. From these data, the
percent recoveries of these metals in the various process
fractions and the overall recoveries were calculated by Wright
State. These results are summarized in Tables 1-4.
B. Volatile Orqanics
The measured concentrations of the target volatile organic
constituents in the various sample fractions resulting from the
first series of KPEG-treatment tests are shown in Table 5 and 6.
The designation "UN" following a sample number in these tables
(and in Tables 7-10) refers to the untreated soil. Similarly,
the designations, "SO," "KP," "WA," and "XA," in Tables 5-10
refer to the treated and water-washed soil, the spent KPEG, the
soil wash water, and the solid sorbent (used to trap evolved
volatiles), respectively. The headings in these tables,
"Acetone," "1,2-Di," "Tetrac," "Chloro," "Ethyl," "Xylene," and
"Styren" refer to acetone, 1,2-dichloroethane, tetrachloro-
ethylene, chlorobenzene, ethyl benzene and styrene, respectively.
The percent recoveries of the surrogate standards achieved
in these analyses are summarized in Table 7.
Table 8-10 present data for the second series of KPEG-
treatment tests which correspond to the data just described for
the first test series.
In Table 11 and 12, the measured concentrations of the
volatile organic constituents are converted to total quantities
present in each of the sample fractions from the KPEG tests
(residual soil, spent KPEG, wash water, solid sorbent trap), for
the first and second test series, respectively. The total
percent recoveries of these volatile organics in the entire
sample set (that is, the percent remaining after the KPEG
treatment) are also summarized in Table 11 and 12. This figure
gives an indication of the destruction efficiency of the reaction
for each analyte or alternatively, is a measure of losses by
other mechanisms such as volatilization.
C. Semi-Volatile Orqanics
The measured concentrations of the target semi-volatile
organic constituents in the various sample fractions resulting
from the first series of KPEG-traated tests are shown in Tables
13 and 14. Corresponding data for the second KPEG-treatment
tests are shown in Table 15 and 15. Tables 17 and 13 show the
19
-------
results of Method Blank analyses, while Tables 19 and 20
summarize the percent recoveries of the surrogate standards which
were achieved in these analyses. In Tables 21 and 22, the
measured concentration data have been converted to show the total
quantities of the semi-volatile constituents present in each of
the treated residual soil, spent KPSG and washwater samples, for
the first and second test series, respectively. Also shown in
Tables 21 and 22 are the total percentages of the semi-volatile
constituents recovered in the treated samples.
IV. DISCUSSION
Several general conclusions are possible from the data reported
herein with respect to the KPEG-treatment process:
a. The metals data indicate that few of the metals were
effectively removed from the soils by the KPEG treatment and,
subsequent water washing. Probably this is due to the inorganic
forms of the metals and their relatively poor aqueous
solubilities. In retrospect, extraction of these could probably
have been enhanced by using an acid water wash of the spent soil
after KPEG treatment. The overall materials balance for the
metals is quite poor, however.
b. The volatile and semi-volatile organic data also exhibit very
poor materials balances, but it seems clear that both 1,2-
dichloroethane and tetrachloroethylene have essentially been
completely destroyed by the KPEG treatment. The other
chlorinated organics, chlorobenzene and pentachlorophenol, were
apparently not significantly affected by the KPEG treatment,
which is not surprising, since it is known from other work, that
destruction of these would have required higher temperatures than
those used in the KPEG tests here. It was not practical to use
such higher temperatures in these tests because of the flash
points and volatility of the other organics (acetone,
particularly) present in these samples. The hydrocarbons
(xylene, ethylbenzene and styrene) in these samples were not
expected to be affected by the KPEG treatment, and indeed no
effects on degradation of these are discernible. The data for
acetone are so suspect in view of volatility problems and
instrument saturation, background and holdup, as to be generally
unreliable.
c. Because of the enormous concentrations of most of the analytes
present in virtually all of the samples for which analyses were
attempted in this study, the standard U.S. EPA analytical methods
(8240 and 8270) were largely inapplicable and data in the format
normally presented for a Quality Assurance review could not be
generated by the automated EPA software. Virtually all of the
results had to be manually calculated. The mass chromatograms
obtained in these analyses are available in our laboratory, and
can be supplied upon request, if dasired. These are not included
herewith, since review of these would be virtually impossible
without all of the parameters used in the manual calculations.
The extensive problems encountered in this study with the
-------
inadequate analytical procedures resulted in analytical data
which are, at best, semi-quantitative indicators of the
efficiency of the KPEG process.
21
-------
TABLE A
QUANTITIES OF SOIL AND REAGENTS IN REACTION MIXTURES AND QUANTITY
OF SOLID SORBENTS IN VAPOR TRAP FOR KPEG REACTION TESTS-FIRST
SERIES
EPA/PEI
SAMPLE NO.
SOIL
DMSO
KOH
KPEG
SOLID
SORBENTS
IN TRAP3 •
SARM-I-1 505.6 g 217.2 g 50.0 g 491.6 g 28.8 g
SARM-II-1 506.0 219.9 50.0 482.5 27.4
SARM-III-2 504.5 220.8 50.0 486.3 27.9
SARM-IV-1 502.9 217.9 50.0 483.5 30.5
a. XAD-2 and tenax only, the activated carbon portion of the
vapor trap was not used for VOA analysis, since previous
experience demonstrated it could not be effectively desorbed.
-------
TABLE B
QUANTITIES OF VARIOUS SAMPLE FRACTIONS RESULTING FROM KPEG
TREATMENT OF SARM SAMPLES FOLLOWING SEPARATION AND WASHING OF
RESIDUAL SOIL
EPA/PEI
SAMPLE NO.
SARM-I-1
SARM-II-1
SARM-III-2
SARM-IV-1
TREATED AND
WATER-WASHED SPENT
SOIL KPEG
572
529
552
462
.7 g
.2
.2
.7
594
625
612
662
.1 g
.0
.6
.9
SPENT
WASH
WATER
466.
477.
471.
500.
4 g
5
6
0
SPENT
SOLID
SORBENTS
IN TRAP3 •
28
27
27
30
.8 g
.4
.9
.5
a. XAD-2 and Tenax only; the activated carbon portion of the
vapor trap was not used for VGA analysis, since previous
experience demonstrated that it could not be effectively
desorbed.
-------
TABLE C
QUANTITIES OF SOIL AND REAGENTS IN REACTION MIXTURES AND
QUANTITIES OF SOLID SORBERTS IN VAPOR TRAP FOR KPEG REACTION
TESTS - SECOND SERIES
EPA/PEI
SAMPLE NO.
PEI7-1-1A/
SARM-I-1
PEI7-2-1A/
SARM-II-1
PEI7-3-1A/
SARM-III-2
PEI7-4-1A/
SOLID
SORBENTS
SOIL DMSO KOH KPEG IN TRAP3 •
105.3 g 53.3 g 12.6 g 145.9 g 34.7 g
106.9 55.1 12.6 155.6 35.3
116.7 54.0 12.5 157.0 36.6
97.9 53.9 11.5 142.4 35.7
SARM-IV-1
a. XAD-2 and Tenax only; the activated carbon portion of the
vapor trap was not used for VOA analysis, since previous
experience demonstrated that it could not be effectively
desorbed.
-------
TABLE D
QUANTITIES OF VARIOUS SAMPLE FRACTIONS RESULTING FROM KPEG
TREATMENT OF SARM SAMPLES FOLLOWING SEPARATION AND WASHING OF
RESIDUAL SOILS
EPA/PEI
SAMPLE NO.
PEI7-1-1A/
SARM-1-1
PEI7-2-1A/
TREATED AND
WATER-WASHED
SOIL
89.0 g
130.7
SPENT
KPEG
210.0 g
179.9
SPENT
WASH
WATER
113.1 g
122.2
SPENT
SOLID
SORBENTS
IN TRAP3 •
34.7 g
35.3
SARM-II-1
PEI7-3-1A/
SARM-III-2
PEI7-4-1A/
SARM-IV-1
130.4
115.7
190.3
178.9
116.5
120.8
36.6
35.7
a. XAD-2 and Tenax only; the activated carbon portion of the
vapor trap was not used for VOA analysis, since previous
experience demonstrated that it could not be effectively
desorbed.
-------
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-------
Tablt
RECOVERY OF METALS IN STANDARD ANALYTICAL, REFERENCES MATRIX
SAMPL E CHROM1 UN CHRONI UN
WEIGHT FOUND ug/g TOTAL
UNTREATED SOIL I-I 5O5.6O g 3O.OO 15168.OO ug
TREATED SOIL I-I
MASH MATER I-I
SPENT REAGENT I-I
-/. PEC IN SOIL
O"EPALL REC
UNTREATED SOIL I I I -2
TREATED SOIL I I 1-2
MASH MATER I I 1-2
SPENT REAGENT 1 I I -2
% PEC IN SOIL
IJUERALL REC
UNTREATED SOIL IU-1
TREATED SOIL IU-1
MASH MATER IU-1
SPENT REAGENT IU-1
;: PEC IN SOIL
OVERALL REC
UNTREATED SOIL I I-I
TREATED SOIL I I-I
MASH MATER I I-I
SPENT REAGENT 1 I-I
'•'- PEC IN SOIL
OVERALL REC
572.
466.
594.
5O4.
552.
471 .
612.
5O2.
462.
50O.
662.
5O6.
529.
477.
625.
7O
4O
10
SO
2O
6O
6O
90
7O
OO
9O
OO
2O
5O
OO
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
21 .
0.
O.
TOTAL
1 163.
826.
168.
2.
TOTAL
14O7.
918.
174.
13.
TOTAL
33.
23.
8.
0.
TOTAL
00
97
O2
OO
OO
00
2O
OO
00
OO
OO
OO
00
20
02
12026.
452.
1 1 .
1249O.
79.
82.
586733.
4561 17.
79228.
1347.
536693.
77.
91 .
7O7580 .
424758.
87OOO.
8617.
520376.
60.
73.
15698.
12171 .
3915.
12.
16099.
72.
96.
7O
41
88
99
29
35
50
2O
80
72
72
74
47
30
6O
OO
70
3O
O3
54
OO
6O
SO
50
6O
89
42
ug
ug
ug
ug
ug
ug
ug
ug
ug
ug
ug
ug
ug
ug
ug
COPPER COPPER
FOUND ug/g TOTAL
349.OO 176454.4O ug
251.00
1 3 . OO
7.9O
TOTAL
% REC IN SOIL
OUERALL REC
143747.7O ug
6O63.2O ug
4693.39 ug
154504.29
81.46
87.56
1167S.OO 5891551.OO ug
6736.OO 3719619.20 uq
281.OO 132519.6O ug
38.OO 23278.80 ug
TOTAL
% REC IN SOIL
OUERALL REC
:;875417.6O
63. 13
65. 78
1O928.OO 5495691.2O ug
9381.00 434O538.70 ug
454.OO 22700O.OO ug
31O.OO 2O5499.OO ug
TOTAL
% REC IN SOIL
OUERALL REC
4773087.70
78.98
86.85
376.OO 19O256.0O ug
33O.00
2O. OO
1 7 . OO
TOTAL
% REC IN SOIL
OUERALL REC
174636.00 ug
955O.OO ug
10625.00 ug
194811.OO
91 . 79
102.39
-------
Tah 3
ni'ERN ,r METALS IN STANDARD ANALYTICAL REFERENCt MATRIX
SAMPLE ARSENIC ARSENIC
HEIGHT FOUND ug/g TOTAL
UNTREATED SOIL I-I 505.6O g 2O.OO IO112.OO ug
TREATED SOIL I-I
MFiSH HATER I-I
5PEMT REAGENT I-I
TREATED SOIL I I I-2
HASH HATER I I 1-2
SPENT REAGENT I I I-2
572.7O g
466.AO g
594.1O g
•-x PEC IN SOIL
0"ERALL REC
UNTREATED SOIL I I 1-2 5O4.5O
8.10 4638.87 ug
8.2O 3824.48 ug
O.O4 23.76 ug
TOTAL 8487.11
45.87
83.93
) 359.OO 181115.50 ug
552.2O g
471.60 g
612.6O g
184.OO
O.OO
1 .20
TOTAL
1O16O4.8O ug
O.OO ug
735.12 ug
102339.92
CADMIUM CADMIUM
FOUND ug-'g TOTAL
45.0O
2 1 . OO
1 .SO
2. 40
TOTAL
% REC IN SOIL
OVERALL REC
861.OO
1 . 80
4.50
22752.OO
ug
1 2O,d6 . 7O ug
699.6O ug
1425.84 ug
14152.14
52.86
62. 2O
3488.OO 1759696.00 ug
TOTAL
475444.20 ug
848.88 ug
2756.7O ug
479O49.78
•< PEC IN SOIL
O"EPALL REC
56. 10
56.51
% REC IN SOIL
OVERALL REC
27. O2
27.22
UinPEATED SOIL IU-1 5O2.9O g 338.OO 16998O.2O ug
TREATED SOIL IU-1
HASH HATER IU-1
SPENT REAGENT IU-1
462.7O g
5OO.OO g
662.9O g
168.OO
458.OO
96. OO
TOTAL
77733.60 ug
229OOO.OO uq
63638.4O ug
370372.00
6148.00 3O91829.20 ug
4855. OO 224-64O8.5O ug
4.SO 225O.OO ug
7. It) 47O6.59 ug
TOTAL
2253365.O9
: PEC IN SOIL
0"EPALL REC
45.73
217.89
% REC IN SOIL
OUERALL REC
72.66
72. 88
UNTREATED SOIL I I-I 5O6.OO g 2O.OO
TREATED SOIL I I-I 529.2O g 8.7O
HASH HATER II-I 477.50 g 8.6O
SPENT REAGENT I I-I 625.OO g O.O4
TOTAL
1O12O.OO ug
46O4.O4 ug
41O6.5O ug
25.OO ug
8735.54
59 . OO
34.OO
1 . 8O
6 . 3O
TOTAL
29854.OO ug
17992.8O ug
859.50 ug
3937.SO ug
22789.8O
* PEC IN SOIL
n"ERALL PEC
45. 49
86. 32
;; REC IN SOIL
OVERALL PEC
60. 27
76. 34
-------
TabK
PECCi"ERY OF NETALS I N
UNTREATED SOIL I-1
TPEriTED 5O I L I-I
MfiSH HATER I-I
SPEHT REAGENT I-I
STANDARD ANALYTICAL REFERENCES MATRIX
SAMPLE zinc ZINC
WEIGHT FOUND ug/g TOTAL
5O5.6O g 1O28.OO 519756.8O ug
572.7O g
466.4O g
594.10 g
492.OO
3.70
3.3O
TOTAL
281768.40 ug
1725.68 ug
I960.53 ug
285454.61
PEC IN SOIL
REC
54.21
54.92
UNTREATED SOIL I I I-2 5O4.5O g 24262.OO 1224O179.OO ug
TREATED SOIL I I I-2
HASH HATER I I I-2
SPENT REAGENT I I I-2
552.2O g
471.60 g
612.6O g
973.OO
1966.OO
566.OO
TOTAL
53729O.6O ug
927165.6O ug
346731.6O ug
1811187.80
•> PEC IN SOIL
O1 'ERALL REC
4. 39
1 4 . 80
UNTREATED SOIL IU-1 5O2.9O g 23414.OO 117749OO.6O ug
TREATED SOIL K1-1
UASH UATER IU-1
SPENT REAGENT IU-1
462.7O g 14736.OO 6818347.2O ug
5OO.OO g 2576.OO 1288OOO.OO ug
662.9O g 933.OO 618485.7O ug
TOTAL
8724832.9O
*; PEC IN SOIL
ru'ERALL REC
57. 91
74. 1O
UNTREATED SOIL I I-I 5O6.OO g 1725.OO 87285O.OO ug
TREATED SOIL I I-I 529.2O g 1269.OO
HASH I.IATER ii-i 477.50 g 10.00
SPENT REAGENT II-I 625.OO g 1 1 . OO
TOTAL
671554.80 ug
4775.00 ug
6875.OO ug
6832O4.SO
•i PEC IN SOIL
G' IERALL REC
76. 94
78. 27
-------
Table 5
Wright State University, Dayton, Ohio 45435
Analysis for Destruction of Volatiles with KPEG-First Test Series
Concentrations Found (micrograms per gram of sample or parts-per-mi11ion)
PEI
Sample Aceton 1,2-Di Tetrac Chloro Ethyl Xylene Styren
Number
SAHM-1-1 UN 7885 584 585 345 3917 10063 827
SAJRM-1 SO 3.46 ND 0.140 0.106 1.05 3.67 0.367
0.0018
SARM-1 KP 1815 ND 6.11 265 1852 5355 596
1.80
SARM-1 WA 1179 ND ND 55.0 220 650 92.3
0.0840 0.118
SARM-1 XA 625 0.434 29.9 25.0 343 711 19.3
-2-1 UN 212 0.193 23.5 4.26 28.4 101 123
SARM-2 SOIL 7.59 0.0160 0.0129 0.0161 0.0718 0.247 0.0568
SARM-2 KP 89.3 ND 2.30 5.71 47.8 146 15.5
0.133
SARM-2 WA 3.28 0.0966 0.0376 1.82 9.86 35.3 5.16
SARM-2 XA 4.47 ND 0.0900 0.240 3.48 11.5 8.07
0.0141
a. The designation ND indicates "None Detected" in excess of the minimum detectable
concentration which is listed directly below the ND designation.
-------
Table 6
Wright State University, Dayton, Ohio 45435
Analysis for Destruction of Volatiles with KPEG-First Test Series
Concentrations Found (micrograms per gram of sample or parts-per-mi11ion)
PEI
Sample
Number
Aceton 1,2-Di Tetrac Chloro Ethyl Xylene Styren
SARM-3-2 UN 496 6.63 27.2 13.1 188 500 40.5
SARM-3 SO 4.86 0.130 0.0068 0.0306 0.0918 0.280 0.0547
SARM-3
SARM-3
SARM-3
-4-1
SARM-4
SARM-4
SARM-4
SARM-4
KP
WA
XA
UN
SO
KP
WA
XA
59.4
17.8
3.34
3059
3.35
1633
269
11.6
ND
0.114
ND
0.0205
ND
0.0034
151
ND
0.0030
ND
1.79
ND
0.128
0.149
1.87
ND
0.0420
0.668
1265
0.156
4.89
ND
0.322
1.90
9.49
2.18
1.00
387
0.0102
246
38.5
1.75
85.1
13.6
10.5
2916
0.0623
1801
206
38.1
246
31.8
51.6
7451
0.216
4950
593
75.5
16.7
1.80
5.39
721
0.0349
496
54.3
5.49
a. The designation ND indicates "None Detected" in excess of the minimum detectable
concentration which is listed directly below the ND designation.
-------
Table 7
Wright State University, Dayton, Ohio 45435
Surrogate Standards Recoveries-First Test Series
PEI
Sample %Rec %Rec %Rec %Rec
Number d4-DiChlo d8-Toluen dlO-Ethyl BromoFlor
SARM-1-1
SARM-1
SARM-1
SARM-1
SARM-1
SARM-2-1
UN
SO
KP
WA
XA
UN
SARM-2 SOIL
"•"M-2
oAhM-2
SARM-2
SARM-3-2
SARM-3
SARM-3
SARM-3
SARM-3
SARM-4-1
SARM-4
SARM-4
SARM-4
SARM-4
KP
WA
XA
UN
SO
KP
WA
XA
UN
SO
KP
WA
XA
152
103
112
60
63
72
66
94
106
86
100
100
94
52
85
57
86
102
86
78
204
80
118
97
38
96
121
104
102
83
249
89
78
66
59
100
102
133
75
76
223
62
209
105
64
71
70
113
111
129
387
93
77
67
86
153
104
192
64
172
94
131
155
162
175
224
101
143
146
116
118
152
144
163
98
286
135
143
127
91
-------
Table 8
Wright State University, Dayton, Ohio 45435
Analysis for Destruction .of Volatiles with KPEG-Second Test Series
Concentrations Found (micrograms per gram of sample or parts-per-million)
PEI
Sample
Number
SARM-1-1 UN
SARM-1-1 SO
SAHM-1-1 KP
SARM-1-1 WA
SARM-1-1 XA
Aceton
7885
75.8
1392
230
406
1,2-Di
584
ND
0.0845
ND
0.807
ND
0.0370
1.79
Tetrac
585
0.684
ND
1.91
ND
0.0548
10.8
Chloro
345
8.00
254
35.2
12.7
Ethyl
3917
95.2
1894
163
164
Xylene
10063
265
5586
413
409
Styren
827
27.0
554
79.0
31.1
-2-1 UN 212 0.193 23.5 4.26 28.4 101 123
SARM-2-1 SO 14.7 ND 2.21 0.146 0.882 2.92 0.488
0.0262
SARM-2-1 KP 284 ND 1.48 4.40 47.6 155 17.4
0.912
SARM-2-1 WA 12.2 ND ND 1.59 8.84 31.1 4.88
0.0174 0.0142
SARM-2-1 XA 28.3 ND 0.854 ND 2.17 5.38 20.1
0.0698 0.0552
a. The designation ND indicates "None Detected" in excess of the minimum detectable
concentration which is listed directly below the ND designation.
-------
Table 9
Wright State University, Dayton, Ohio 45435
Analysis for Destruction of Volatiles with KPEG-Second Test Series
Concentrations Found (micrograms per gram of sample or parts-per-mi11ion)
PEI
Sample Aceton 1,2-Di Tetrac Chloro Ethyl Xylene Styren
Number
SARM-3-2 UN 496 6.63 27.2 13.1 188 500 40.5
SARM-3-2 SO 15.6 ND 1.27 0.457 3.05 9.76 0.766
0.0200
SARM-3-2 KP
SARM-3-2 WA
SARM-3-1 XA
-4-1 UN
SARM-4-1 SO
SARM-4-1 KP
SARM-4-1 WA
169
13.7
42.3
3059
250
1208
13.2
ND
0.384
ND
0.0239
0.0784
151
ND
0.395
ND
1.07
ND
0.0571
2.29
ND
0.0214
1.18
1265
1.85
ND
3.65
0.503
8.05
2.13
0.431
387
3.69
242
25.7
76.5
13.7
10.0
2916
38.0
1769
82.1
244
47.3
26.3
7451
88.6
5501
265
16.1
721
569
SARM-4-1 XA 487 4.95 26.9 17.8 172 461 45.5
a. The designation ND indicates "None Detected" in excess of the minimum detectable
concentration which is listed directly below the ND designation.
-------
Table 10
Wright State University, Dayton, Ohio 45435
Surrogate Standards Recoveries-Second Test Series
PEI
Sample %Rec %Rec %Rec %Rec
Number d4-DiChlo d8-Toluen dlO-Ethyl BromoFlor
SARM-1-1 UN
SARM-1-1 SO
SARM-1-1 KP
SARM-1-1 WA
SARM-1-1 XA
SARM-2-1 UN
SARM-2-1 SO
"<°M-2-l KP
SArtM-2-1 WA
SARM-2-1 XA
SARM-3-2 UN
SARM-3-2 SO
SARM-3-2 KP
SARM-3-2 WA
SARM-3-1 XA
SARM-4-1 UN
SARM-4-1 SO
SARM-4-1 KP
SARM-4-1 WA
SARM-4-1 XA
152
80
93
110
89
72
91
282
105
94
100
86
102
143
61
57
129
76
103
119
204
164
184
130
71
96
85
113
109
167
249
69
107
120
124
100
185
175
146
81
223
204
183
113
66
71
80
144
98
257
387
82
109
143
100
153
226
193
169
75
94
132
119
90
121
224
86
84
125
101
118
91
96
98
180
286
87
144
80
122
-------
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ii't-n) :;m)j yf.ii'i't- KIT' miHj.ii HI ly.ioi
K"1 J'n n'll 0 n .;'•;!. '-''I b'!.- XHH'JI1' i]HX
ii'n ii'u n'ti n ii 'i't-i.'"8 8'Jl 'Vt^t- .ij.lHH
,'K •!".»•[] i,'I n'n Tin I 'S-.-I-HC h't'.'j 'V.J-i ')-)j;t
r II'M ii'it ::')J I n J'i::'i. f.'h o'~Vj IIn1-- OJlUiJI
i'M t-' .".'•:[ .".'."• ::'H":': H"< H'.'."lTj. IV%t- S'Hii II'T- U.1JM3.J.IUM
I IU" MH,'. C 1 HUH; (HJ. I',: 3 ' IHi'1.. l.'.H' I J MUH'r. CMnlH1 -I H14H: ilHIJI Jl.JUH- [il T'l 3 HUH-;. 1HHI3JH -)Zll.
!'•!"! ';( 'tin ' 'Hint M) itjiii (Him HI .iNfi i lyiiu tl[ lUni T-UnI HI ' iHn I 1U1HI Mt IMO i IHJnt H) ' INM I ) |.-)Ud\ X U IHU
'illtlHnn '.JllNMII'i '.Jlltltiiin iMUMHiiii .', UlllHriM .', I [ ItlHl'm .UllNHllo
111 -U.-lH'.. UN ) HUH-;
'i)3,J,iiih. ',i\ liiN ii.i
K '"' l"i' '-'., n" •'_•', n' 5':. rr S"iilMt- 'V,' .r'S:'j I |H':. UllM'fol
"' •' M'1, .' MI , M |.'i l'M'.;tt f:'_ i'j,[." '"t- I'ltOli 'i''_r ±'<_i. .-'ii M'..'^"jiii O'-n." I.I'HIIIJ HO'. UJ'ii JJIHII
•HUM ,M H,', I I • IUi" 1NH,"' ;iHH>'_ I.'.Hl.l H l.tUH M in |H H.|UH': jH.iOI J UUH1: M r'l 3 HUH';. 3HMI3JH J7]i.
IHI''I ''! I!|M ;H'"! 'Jl '4''i IHl'i; Hi INi"1 i Ib'Ji'l i; 1 iHn IMlni ,j I ' ilinj IHInl HI ' JHO I IHInl HI ' i«U I JIJUH'". X UJHU
11-UdHl. 'ilH IHUM'.
1 il3,',Mir.", Bil |ii|j 41.1
J.I INl'liiUH. 'MINIMUM ':
HIT; inim.li MI IHJ.II
n'n- ii' j" ] ' I •)!:. i 'i.." II'M n'n n'ljiiiiftl ir .," i :?.'.-;,." '.HH.ll''' ilUX
'•' 'i^'j i.''ji Vt[ I'M II'M iV M •-(* •-,::: t" t- ^ M'. ftt f'l'it1 H |!'H
' •" .'-,'Hi '• '• i . ' "M. ; M' ' , :l .,'".l.'"l n''i i. M'"' 'i' I'l II'M MM -,'[i.'f'.'Ml iv-,!::( I'H.j Old')
'' '"' ' ' ''"''' ' '! ' Vj I'M ."n. I'M n'n M n ',"1">I :,'': .'',.['; i [n1-. UllHJdl
'•'•"•• '' ' '"' " ' >. »"n .I'.'tf ii' ••"(-(• > n' ,|- M't'iji;.' n",. , KM'"jt". ' i"i t".vi n 1-.'nt::f. ri'-.1::1,1 '.-i'iii'j liu. lUIMj.UHll
:tH- ' i i IH"' IN:).', 1 • IUH I'M!) -i|UH: >'1HiM HUM; mil.) I •) 1 lilH [il."'l 1": IUI" 3lln I I iH -)Z I ".
11111 ' .'-H"! '<' ' '>!' ' !M|li: H! 'H>' ' 1N|n| HI II'M |Ml"i rii ' nln i I'ihil i'[ "iHn i |M1M| H) ' iHni 3'HUH1.. X UJfU
i'. IHN'."1 UHI''JI|.- .'.illHHhH ,,l(lMHi'i ,', lUIIUlin .'alJNUll'.'
i. j., HIMH M '.>!>. in-.im i -M i u f,u ji-iuw
atqei J'-31 J
-------
OND TEST
SIMPLE mi. f:ti~i
MUFF ix SADPLE core.
SIZt ACETONE
nilFFtHFED SOIL 105.3 7U8S.O
FFtflFEFj SMIL 89.0 75.8
CFE'. 210.0 1392.0
HRTFP 113.1 230.0
Xliri-,.7TEMHX 34.7 406.0
Furfll IH TPERTED SOIL
;; FEdHlHIHb '-AMOUNT PECOl-EREO
OR NOT HESTRfiVED)
SfiriPLE HO. SRPd-II
HHTPIX SflflPLE COHC.
SIZE ACEIOHE
HtlTFTHirO SOIL 106.9 212.0
TREATED SiiH 130.7 14.7
CFtO 179.9 284.0
UllFEP 122.2 12.2
XRIi-j.'TEHflX 35.3 28.3
TOTAL IH TREATED SOIL
:; PtrifllMlHfi •'AnnUMT RECOUPED
OR HOT DESTROVED)
SAMPLE MO. SAP.d-III
MATP1 X SfldPLE CONC.
SIZE flCETOHE
HMTFFHFED SOIL 116.7 496.0
TPCRTED SOIL 130.4 15.6
CFEi. 191.3 169.0
UHFEF: 116.5 13.7
XHU-2/TENHX 36.6 42.3
FnrfiL IH TREHTED SOIL
'; PEHfllHINb >'AnoUHF PECOI'ERED
OR HOT DESTRuVEFC'
sfinrtE HO. sflpn-iu
tlflTPIX SAMP1E COHC.
SIZE flCETuHE
IINTPEAFEO SOIL 97.9 3059.0
TPERTEFi SiiIL 115.7 250.0
HFEO 178.9 12U3.0
HHFER 120.8 13.2
KiTfll IH TREATED SOIL
T; FtnAINlHi) (flhuUHT F'ECOUEPED
1 CtU 1 C
MiHi.ENTPflllON OT AHflLVI |/g>
PUAHTITV
IH TuFRL
SHWIE
83M2-J0.5
b746.2
292320.0
26013.0
140S8.2
339167.4
4U.B
CUHHTITV
IN TOTRL
SHdPI E
2261.2.8
1921.3
51091.6
1490.8
999.0
55502.7
244.9
PUflHTITV
IH TOTAL
SfldFlE
578K3.2
2034.2
32329.7
1596.1
37508.2
64. a
CURHTITV
IN TuTRL
SAWI E
299476. 1
28925.0
216111.2
1594.6
17385.9
264016.7
;-.«.2
OUAMTITV
fOHC. IH TnTAL
1,^-W SHIIPIE
584.0 61495.2
0.0 0.0
u.O 0.0
U.O 0.0
1.8 62.1
(2.1
0.1
euflriTiTV
COHC. IH TuTflL
1,2-Di SHHPLE
0.2 20.6
0.0 0.0
0.0 0.0
0.0 0.0
0.0 0.0
0.0
0.0
KUrtHTITV
CONC. IN TuTflL
i,2-ni SHtiFiE
6.6 773.7
0.0 0.0
U.O 0.0
0.0 0.0
0.1 3.7
3.7
0.5
CUHNTITV
COHC. IH T'lTfll.
1,2-HI SflhPLE
151.0 147U2.9
U.O ii. 0
0.0 U.O
0.0 0.0
5.0 176.7
176.7
1.2
UUHHTITV
com. IH TOTAL
TEIFRC SHdPLE
St.S.U 616MU.5
0.7 60.9
1.9 401.1
0.0 0.0
10.8 374.3
836.7
1.4
QUAHTIIV
CONC. IH luTfll.
IETRHC SHHPLE
23.5 2512.2
2.2 288.8
1.5 266.3
U.O 0.0
0.9 31.8
5:.:6.9
23.4
CUflHTITV
COHC. IH TUTRL
TETPflC SAdPLE
27.2 3174.2
1.3 165.6
2.3 438.1
0.0 0.0
1.2 43.2
646.9
20.4
fiuHHTl TV
com. IH TOTAL
lETFflC SrtrtF'LE
11-1.5.0 123843.5
1.9 214.0
0.0 U.I)
0.5 6U.4
26.9 960.3
1234.>;
1.0
com .
CIILfiFO
345.0
8.0
254.0
35.2
12.7
COHC .
CHIURO
4.3
0.1
4.4
1.6
0.0
COHC.
CMLORO
13.1
0.5
8.1
2.1
0.4
CONC .
CHI Ofru
3K7.0
3.7
242. 0
25.7
17. a
OURNTITV
IN TOFFlL
SHdFlE
36328.5
712.0
53340.0
3981.1
440.7
58473.8
161.0
CURHTI TV
IH TuTflL
SfldltE
455.4
19.1
791.6
194.3
0.0
1004.9
220.7
KURHT1 TV
IH TOTflL
SAdFLE
1528.8
59.6
1540.0
248.1
15.8
1863.5
Ul.9
OUflHTI TV
IN TUFHL
SrtdF'LE
378
-------
Table 13
HSU KPEG
First Test
Concentration (ug/kg)
Total Quantit/ ing)
PEI Soil
Saaple No.
SARH-I-1
SARH-I-1
SARH-I-1
SARH-I-1
SARH-I-1
SARH-I-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-III-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-IV-1
SARH-IV-1
SARH-IV-1
SARH-IV-1
SARH-IV-1
Treatment
Hunter
SARH-I-1
SARH-I-1
SARH-I-l
SARH-I-1
SARH-II-2
SARH-II-2
SARH-II-2
SARH-II-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-IV-1
SARH-IV-1
SARH-IV-1
HSU Run
Nuiber
PEISV0058
PEISV0070
PEISV0072
PEISV0073
— - Destruc
PEISV0064
PEISV0038
PEISV0074
PEISV0075
— Destruc
PEISV0063
PEISV0062
PEISV0077
PEISV0078
— Destrui
PEISV0059
PEISV0071
PEISV0079
PEISV0080
Saiple Type
Listed Levels
Untreated soil
Treated soil
KPEG
Hater
.
tion Totals - —
Listed Levels
Untreated soil
Treated soil
KPEG
Hater
;tion Totals
Listed Levels
Untreated soil
Treated soil
KPEG
Water
:tion Totals
Listed Levels
Untreated soil
Treated soil
KPEG
Water
Anthracene
6,600,000
4,554,420
395,500
667,480
270
660
,536
,000
227,540
55
105
11
660
13
81
186
22
6,600
4,210
167
66
821
,533
,870
,102
,000
,740
,127
,847
,980
,000
,040
,380
,960
,481
DEHP
2,500,000
539,680
33,380
24,280
3
250
40
1
2
1
250
62
4
7
1
2,500
936
27
37
11
,916
,000
,200
,773
,990
,612
,000
,240
,436
,529
,507
,000
,560
,420
,140
,592
' Fraction
Height (g)
505.
505.
572.
594.
466.
506.
6
6
7
1
4
0
506.0
529.2
625.
477,
504
504.
552
612,
471
502
502
462
0
.5
.5
,5
.2
.6
.6
.9
.9
.7
662.9
500
.0
Anthracene
3337.0
2302.7
226.5
396.5
126.2
[749.2]
334.0
115.1
29.4
66.2
5.3
[100.^3
333.0
6.9
44.8
114.5
10.8
[170.1]
3319.1
2117.2
77.4
44.4
410.7
DEHP
1264.0
272.9
19.4
14.4
1.3
[35.6]
126.5
20.3
0.9
1.4
0.8
[3.6]
126.1
31.4
2.4
4.6
0.7
[7.7]
1257.3
470.7
12.7
24.6
5.8
fln^f ,,,,,f , nr. Tn*olr T^IO ^ 1 [ A~S ll
-------
PEI Soil
SaBpie No.
SARH-I-1
SARH-I-1
SARH-I-1
SARH-I-1
SARH-I-1
SARH-I-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-III-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-IV-1
SARH-IV-1
SARH-IV-1
SARH-IV-1
SARH-IV-1
o i nu r 1 1 i
WSU KPEG
Treatient
Nuiber
SARH-I-1
SARH-1-1
SARH-1-1
SARH-1-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-III-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-IV-1
SARH-IV-1
SARH-IV-1
f i nu _ Til _ i
WSU Run
Number
PEIPCP0011
PEIPCP0030
PEIPCP0031
PEIPCP0032
— Destruc
PEIPCP0025
PEIPCP0033
PEIPCP0034
PEIPCP0035
— Destruc
PEIPCP0019
PEIPCP0037
PEIPCP0038
PEIPCP0039
--- Destruc
PEIPCP0018
PEIPCP0040
PEIPCP0041
Table 14
First Test
Concentration (ug/kg)
Sample Type PentaChloroPhenol
Listed Levels
Untreated soil
Treated soil
KPEG
Hater
tion Totals
Listed Levels
Untreated soil
Treated soil
KPEG
Hater
tion Totals —
Listed Levels
Untreated soil
Treated soil
KPEG
Hater
tion Totals --•
Listed Levels
Untreated soil
Treated soil
KPEG
PEIPCP0043 Hater
1,000,
242,
4,
212,
15,
100,
3,
11,
1,
100,
61,
000
670
732
255
461
000
970
324
133
199
000
,590
225
17,511
1,142
1,000
85
3
53
3
,000
,009
,640
,575
,532
- Fraction
Height (g)
505.6
505. b
572.7
594.
46b.
1
4
506.0
506.0
529.2
625
.0
477.5
504
504
552
612
.5
.5
.2
.6
471. b
502
502
462
662
500
.9
.9
.7
.9
.0
Total Quantity (ig)
PentaChloroPhenol
505.
122.
2
126.
[13b.
50.
2.
0.
7.
0.
[ 7
50.
31
0,
10
b
1
2
0]
b
,0
.2
.0
,6
.8]
.4
.1
.1
7
0.5
C 11.3]
502.9
42.8
1.7
35
1
r -?o
.5
.8
nl
-------
Table 15
WSU XPEG
Second Test
Concentration (ug/kg)
Total Quantity (ig)
PEI Soil
Sample No.
SARH-I-1
SARH-I-1
SARH-I-1
SARH-I-1
SARH-I-1
SARH-I-1
SARM-II-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-III-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-IV-1
SARH-IV-1
SARH-IV-1
SARH-IV-1
SARH-IV-1
SARH-IV-1
Treataent
Nusiber
PEI7-1-1A
PEI7-1-1A
PEI7-1-1A
PEI7-1-1A
PEI7-2-1A
PEI7-2-1A
PEI7-2-1A
PEI7-2-1A
PEI7-3-1A
PEI7-3-1A
PEI7-3-1A
PEI7-3-1A
PEI7-4-1A
PEI7-4-1A
PEI7-4-1A
PEI7-4-1A
WSU Run
Number
PEISV0058
PEISV0047
PEISV0040
PEISV0041
— Destrui
PEISV0064
PEISV0037
PEISV0051
PEISV0054
— Destrui
PEISV0063
PEISV0050
PEISV0052
PEISV0056
— Destrui
PEISV0059
PEISV0048
PEISV0053
PEISV0057
-— Destrut
Saaple Type
Listed Levels
Untreated soil
Treated soil
KPEG
Water
:tion Totals
Listed Levels
Untreated soil
Treated soil
KPEG
Water
,tion Totals
Listed Levels
Untreated soil
Treated soil
KPEG
Hater
,tion Totals
Listed Levels
Untreated soil
Treated soil
KPEG
Water
,tion Totals
Anthracene
6,bOO,000
4,554,420
lt,7,100
57^,360
212,716
660,000
227,540
251,050
161,962
3,650
660,000
13,740
185,186
172,883
2,442
6,600,000
4,210,040
124,960
126,730
44,573
DEHP
2,500
539
13
115
35
250
40
3
2
1
250
62
3
1
1
2,500
936
23
1
,000
,680
,200
,820
,144
,000
,200
,696
,018
,017
,000
,240
,322
,983
,884
,000
,560
,180
,880
144
" Fraction
Weight (g)
105.3
105.3
89.0
210.
0
113.1
106.
106.
130.
179.
122.
116.
116.
130.
190.
116.
97.
97.
115.
9
9
7
9
2
7
7
4
3
5
9
9
7
178.9
120.
8
Anthracene
695.
479.
14.
121.
24.
[IbO.
70.
24.
32.
29.
0.
[62.
77.
1
24.
32.
0
6
8
7
1
7]
6
3
8
1
4
3]
0
6
1
9
0.3
[ 57.3]
646.1
412.2
14.5
22.
5.
[ 42.
7
4
6]
" / i ™y /
DEHP
2b3.3
56.8
1.8
24.3
4.0
[2'.5]
26.7
4.3
0.5
0.4
0.1
[ 1-0]
29.2
7.3
0.4
0.4
0.2
[ i.o]
244.8
91.7
2.7
0.3
0.0
[3.0]
-------
PEI Soil
Sa«ple No.
SARH-I-1
SARH-I-i
SARH-I-1
SARH-I-1
SARH-I-1
SARH-I-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-II-1
SARH-III-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-III-2
SARH-IV-1
SARH-IV-1
SARH-IV-l
SARH-IV-1
SARH-IV-1
HSU KPEG
Treatient
Nusber
PEI7-1-1A
PEI7-1-1A
PEI7-1-1A
PEI7-1-1A
PEI7-2-1A
PEI7-2-1A
PEI7-2-1A
PEI7-2-1A
PEI7-3-1A
PEI7-3-1A
PEI7-3-1A
PEI7-3-1A
PEI7-4-1A
PEI7-4-1A
PEI7-4-1A
WSU Run
NuBber
PEIPCP0011
PEIPCP0008
PEIPCP0009
PEIPCP0010
— Destruc
PEIPCP0025
PEIPCP0026
PEIPCP0027
PEIPCP0028
— - Destruc
PEIPCP0019
PEIPCP0022
PEIPCP0023
PEIPCP0024
-— Destruc
PEIPCP0018
PEIPCP0013
PEIPCPOOU
Table 16
Second Test
Concentration (ug/kg)
Saiple Type PentaChloroPhenol
Listed Levels
Untreated soil
Treated soil
KPEG
Hater
tion Totals —
Listed Levels
Untreated soil
Treated soil
KPEG
Hater
tion Totals
Listed Levels
Untreated soil
Treated soil
KPEG
Hater
tion Totals
Listed Levels
Untreated soil
Treated soil
KPEG
PEIPCP0017 Hater
1,000,000
242,670
5,bfa5
636,320
204,
,865
100,000
3,970
217
1
100
61
2
1,000
85
3
,593
523
,000
,590
594
,696
736
,000
,009
,895
320,590
82
,096
• Fraction
Height (g)
105.
105.
89.
210.
113.
3
3
0
0
1
106.9
106.9
130.7
179.
122.
116,
116
130,
.9
,2
.7
.7
.4
190.3
116
.5
97.9
97.9
115.7
178
120
.9
.8
Total Quantity («g)
PentaChloroPhenol
105.3
25.6
0.5
144.
1
23.2
[167.8]
10.7
0.4
0.0
0
0,
[ o
11
7
0
0
0
[ o
97
8
0
57
9
r ^7
•7
. o
.1
.4]
.7
.2
.1
.5
.1
-7]
.9
.3
.4
.4
.9
71
-------
Table 17
Blank Analysis
PEI Soil
Sample No.
WSU KPEG
Treataent
Nuiber
Total Quantity (ug)
WSU Run
Nuiber
in Extract
Saiiple Type
Anthracene
DEHP
Assueed
• Saiple
Weight (g)
Effective Quantity (sg)
Anthracene
DEHP
PEISV0081 Hethod Blank 0.0115 0.1296 0.20 0.06 O.b5
-------
Table 18
Blank Analysis
PEI Soil
Sasple No.
HSU KPE6
TreaUent
Nuaber
WSU Run
Nuiber Saiple Type
DtTTDPDnn/1,1 Unihn/4 Dl->nL
Total Quantity (ug)
in Extract
Pentachlorophenol
n fu/ i
Assuied
' Saiple
Height (g)
n on
Effective Quantity (ig!
PentaChloroPhenol
n n"?
-------
Table 19
Percent Recovery of Surrogate Standard
HSU Run Nmber I Rec dlO - Anthracene
PEISV0037
PEISV0038
PEISV0040
PEISV0041
PEISV0047
PEISV0048
PEISV0050
PEISV0051
PEI5V0052
PEISV0053
PEISV0054
PEISV0056
PEISV0057
PEISV0058
PEISV0059
PEISV0062
PEISV0063
PEISV0064
PEISV0070
PEISV0071
PEISV0072
PEISV0073
PEISV0074
PEISV0075
PEISV0077
PEISV0078
PEISV0079
PEISV0080
PEISV0081
51.4
36.3
41.2
111
51.9
152
94.3
71.1
80.2
61.2
44.0
96.6
98.4
132
86.9
72.8
90.4
41.5
84.6
58.2
26.6
51.8
153
21.4
82.5
48.6
67.0
76.2
58.9
-------
Table 20
Percent Recovery of Surrogate Standard
WSU Run Number I Rec c!3 - PentaChloroPhenol
PEIPCP0008
PEIPCP0009
PEIPCP0010
PEIPCPOOil
PEIPCP0013
PEIPCP0014
PEIPCP0017
PEIPCP0013
PEIPCP0019
PEIPCP0022
PEIPCP0023
PEIPCP0024
PEIPCP0025
PEIPCP0026
PEIPCP0027
PEIPCP0028
PEIPCP0030
PEIPCP0031
PEIPCP0032
PEIPCP0033
PEIPCP0034
PEIPCP003S
PEIPCP0037
PEIPCP0038
PEIPCP0039
PEIPCP0040
PEIPCP0041
PEIPCP0043
PEIPCP0044
23.0
227
148
34.0
12.0
116
77.5
15.8
85.3
10.4
6.3
5.0
15.4
8.1
4.9
3.7
13.6
65.3
9.8
15.7
26.1
6.0
8.3
31.0
7.0
16.6
22.4
4.3
22.2
-------
Tabli
FIRST TEST
CO'
RflTIOH OF RllflLYTES
SFJIFLE HO. SflRM-I
SflMPLE
SIZE
MATRIX
UHTRERTED SO 505.6
TRERTED SOIL
kFEG
HATER
572.7
594.1
466.4
QUflHTITY
COMC. IH TOTAL
RIITHRflCEUE SflMPLE
(ug/kg> (019)
45-54420 2302.7
395500
667480
270536
226.5
396.5
126.2
COt 1C.
DEHP
(ug/kg)
539680
33880
24280
3916
QUflHTITY
IH TOTRL
SfiMPLE
<.nig>
242670 122.7
4732
212255
15461
2.7
126. 1
7.2
TOTfiL IH TRERTED SOIL
•/. P.EMRIHIHG (AMOUNT RECOVERED
OR HOT DESTROYED)
749.2
32.5
35.7
13.1
136.0
110.9
SflHPLE HO. SRRM-II
MHTRIX SfiMPLE
SIZE
UHTRERTED SO 506
TFERTED SOIL 529.2
KFEG 625
HATER 477.5
QUflHTITY
COHC. IH TOTRL
RHTHRRCEHE SflMPLE
(ug/kg) «fig>
227540 115.1
55583
105370
11102
29.4
66.2
5.3
COHC.
DEHP
(ug/kg)
40200
1773
2990
1612
QUflHTITY
IH TOTflL
SRMPLE
20.3
0.9
1.9
0.8
QUflHTITY
COHC. IH TOTflL
PEHTflCHLOROPHEHOL SflMPLE
(ug/kg) (dig)
3970 2.0
324
11133
1199
0.2
7.0
0.6
TOTflL IN TREflTED SOIL
','. REMAININS (AMOUNT RECOVERED
OR HOT DESTROYED)
100.9
87.6
3.6
17.6
7.7
383.4
SFIMPLE HO. SARM-III
MATRIX SRMPLE
SIZE
UHTREflTED SO 504.5
TFERTED SOIL
KPE6
UftTER
;:FO-2/TENAX
552.2
612.6
471.6
27.9
QUflHTITY
COHC. IH TOTflL
RHTHRflCEHE Sfit-IPLE
(ug/kg) <«ig)
13740 6.9
81127
186847
22980
TOTflL IH TPERTED SOIL
•/. REMAIN IMG (AMOUNT RECOVERED
OR MOT DESTROYED)
44.8
114.5
10.8
170.1
2453.9
QUflHTITY QUANTITY
COHC. IN TOTflL COHC. IN TOTflL
DEHP SflMPLE PEHTflCHLOROFHEHOL SflMPLE
(ug/kg) (mg) (ug/kg) (mg)
62240 31.4 61590 31.1
4436 2.4 225 0.1
7529 4.6 17511 10.7
1507 0.7 1142 0.5
7.8
24.8
11.4
36.7
SAMPLE MO. 3ARM-IV
MATRIX SflMPLE
SIZE
UMTPEflTED SO 502.9
TPEflTED SOIL
KPE6
UHTER
XflD-2/TEHRX
462.7
662.9
500
30.5
QUflHTITY
COHC. IH TOTflL
ANTHRACENE SflMPLE
(ug/ky)
-------
Tab!
SECOND TEST
HTRRTIOH OF RNRLYTES
SflHPLE HO. SRRM-I
HRTRIX
SFIMPLE
SIZE
UHTRERTED SO
105.3
PURHTITY
COHC. IH TOTRL
RHTHRRCEHE SRMPLE
4554420 479.6
TF-ERTED SOIL 89 167100 14.9
kPEG 210 579360 121.7
HRTER 113.1 212716 24.1
TOTRL IH TRERTED SOIL 160.6
'.'. PEMRIMIHG CRMOUHT RECOVERED 33.5
OR HOT DESTROYED)
cone.
DEHP
539680
13200
115820
35144
PURHTITY
IH TOTRL
SRMPLE
f,mg>
56.8
1.2
24.3
4.0
29.5
51.9
PURHTITY
COHC. IH TOTRL
PEHTRCHLOPCIFHEHOL SRMFLE
Ojq.'Vg) 'rug)
242670 25.6
5665 0.5
686320 144.1
204365 23.2
167.8
656.7
SRIIFLE HO. SRRM-II
MATRIX SRMFLE
SIZE
UHTRERTED SO 106.9
TPERTED SOIL 130.7
KFEG 179.9
MATER 122.2
OURIITITY
COHC. IH TOTHL
RHTHRRCEHE SRMPLE
(uq/kg)
227540 24.3
251050
161962
3650
32.8
29.1
0.4
OUANTITY
COHC. IH TOTRL
DEHF SRMPLE
3970 0.4
0.5
0.4
0.1
217
1593
523
.0
0.3
0.1
TOIRL IH TREHTED SOIL
;: REMRINIH6 (AMOUNT RECOVERED
OR NOT DESTROYED)
62.4
256.5
1.0
22.6
0.4
89.3
SRtlFLE HO. SRRM-III
MRTRIX SRMFLE
SIZE
UHTRERTED SO 116.7
TPERTED SOIL 130.4
KPEG 190.3
HRTER 116.5
OURHTITY
COHC. IH TOTRL
RHTHRRCEHE SRMPLE
(ug^'kg) <.mg)
13740 1.6
185186
172:383
2442
24.1
32.9
0.3
COHC.
DEMP
< ug/kg >
62240
3322
1933
1884
niJRHTITY
IH TOTRL
SRMFLE
7.3
0.4
0.4
0.2
PURHTITY
COHC. IN TOTRL
PEHTRCHLOPOPHEHOL SRMPLE
(mq)
"61590 "7.2
594
2696
736
0. 1
0.5
0.1
TOTRL IH TRERTED SOIL
•/. REMfUHINU (RMOUHT RECOV/ERED
OR HOT DESTROYED)
57.3
3575.5
1.0
14.2
0.7
9.4
SflHPLE NO. SRRM-IV
MRTPIX SRMPLE
SIZE
UHTPERTED SO 97.9
TFERTED SOIL
h'FEG
UOTER
115.7
178.9
120.8
COHC.
RHTHRRCEHE
(ug/l:g)
4210040
124960
126730
44573
QURNTITY
IH TOTRL
SflMPLE
412.2
14.5
22.7
5.4
COHC.
DEHF
(uq/kg)
936560
23180
1880
144
OIJHHTITY
IH TOTRL
SRMPLE
'nig"1
91.7
2.7
0.3
.0
PURNTITY
COHC. IH TOTRL
FEHTRCHLOROFHEHOL SRMPLE
(uq/kg)
-------
WRIGHT
SIATC
Wright State University
Dayton. Ohio 45435
December 4, 1987
Mr. Bart Thompson
U.S. Environmental Protection Agency
Mail Code WH-548E
401 M Street, S.W.
Washington, D.C.20460
Dear Mr. Thompson:
The purpose of this letter is to provide you with a status report
on our investigations relating to the Development of Treatment
Data on the KPEG Process for SARA/BDAT Standards for the U.S.
EPA, and to apprise you of the major problems and difficulties
which we have encountered in the analytical portions of this
work, which have resulted directly in the lengthy delays
experienced in Wright State's completion of the project. Wright
State's work on this project is being accomplished under
Subcontract No. 777-87 to prime Contract No. 68-03-3413 between
PEI Associates, Inc. and the U.S. Environmental Protection
Agency. The brief report presented here is intended primarily to
indicate to you the trends and overall conclusions which can be
derived from the data obtained thus far (and the limitations of
the data) in the hope that this will permit some useful
comparisons with other destruction and/or removal technology
which EPA is attempting to evaluate in this program. A more
comprehensive report will be presented upon completion of the
project, probably within the next week.
The procedures and techniques developed and implemented in this
program by Wright State in evaluating the KPEG Process have been
described in detail in documentation which Wright State has
submitted to PEI Associates, Inc. and in the Quality Assurance
Plan for the project which was jointly prepared by PEI and Wright
State. Briefly, Wright State received from PEI four (4) soil
samples prepared by that organization to contain known amounts of
the volatile organic compounds, acetone, 1,2-dichloroethane,
tetrachloroethylene, chlorobenzene, ethyl benzene, xylene and
styrene, as well as the semivolatile organics, anthracene, bis-
(2-ethylhexyl)phthalate and pentochlorophenol. These soils also
contain the metals, cadmium, copper, chromium, lead, arsenic,
nickel and zinc. The concentrations of these components were
different in the four samples provided, but in all cases were
quite large, being several orders of magnitude higher than the
concentrations usually encountered in the environment. Wright
State initially treated these soils by reacting portions or
aliquots of each soil (in duplicate) with KOH and KPEG in closed
laboratory reactors at a controlled temperature (100°C) for a
-------
Mr. Bart Thompson
Page 2
December 4, 1987
period of 2 hours. The treated samples were separated by phase,
the spent KPEG in each reactor was removed from the residual soil
and retained for analysis, the residual soils were washed with
water, and the wash water and spent soil were separated and
retained for analyses. A solid sorbent, used to trap volatile
emissions from the reactor during treatment was also analyzed. A
total of eight KPEG treatment tests were therefore accomplished
(4 soils treated in duplicate) and four samples resulted from
each test (spent soil, spent KPEG, soil wash water, volatile
sorbent trap). Thus, 32 samples derived from the tests, and 8
samples of the original soils, or a total of 40 samples were to
be analyzed by Wright State for all of the organic compounds
known to be present in the spiked soils.
Metals analyses for the treated soils and starting materials were
to be accomplished by Analytical Enterprises, Inc. of Columbus,
SC, another U.S. EPA contractor. In addition, TCLP tests were to
be conducted on these treated samples and the original soils by
Wan Technologies of Atlanta, GA, also a U.S. EPA contractor.
Immediately upon completion of the treatment experiments, on
September 10, 1987, Wright State shipped portions of each of the
several samples from the treatment process to these two
laboratories by Federal Express. In addition, at that point,
Wright State initiated attempts to analyze potions of these
samples for the volatile and semi-volatile organic components of
the soil. From the outset, these attempts were impeded by severe
problems. Some of the problems encountered are outlined below:
1. The major source of problems encountered in the analyses
originated from the huge concentrations of the analytes in
the soil samples, and even in the samples resulting from the
treatment tests. The magnitude of these concentrations was
a problem because:
a. The high concentrations required that relatively small
aliquots of both the untreated soil and the several
samples resulting from KPEG treatment be selected for
analyses, in an attempt to avoid overloading the
analytical devices utilized. It is virtually
impossible to select a sample aliquot which is truly
representative of the entire bulk sample when such
small samples are taken for analysis.
b. It was impossible to predict "a priori" the
concentrations of the analytes which would be present
in the various fractions from the treatment process,
and therefore selection of portions of these samples
which would yield adequate detection limits for the
analytes of interest, but would avoid saturating or
overloading the analytical devices, was largely a
-------
Mr. Bart Thompson
Page 3
December 4, 1987
matter of guess work.- Unfortunately, very high
concentrations of the organics were found to be present
in many of these samples and therefore the "guesses" as
to the portion of sample selected for analysis were
frequently wrong. This lead to repeated saturation of
the instrumentation and numerous repetitive analyses to
get even marginally acceptable data. The performance
of the Tekmar Purge-Trap apparatus is especially
devastated by being subjected to very high saturating
concentrations of organics, and this resulted in long
"memory" or holdup of the compounds in the Purge-Trap
apparatus. The result was that carry-over of analytes
(from the previous run) occurred in many of the
analyses and eliminating this (which was never
completely accomplished for acetone) required purging
the apparatus for many hours and even days between
analyses. This ultimately required literally hundreds
of analyses to obtain even passable results.
c. The extremely high concentrations present and detected
in many of the treated samples were often outside the
range of instrument calibration, again requiring many
extra analyses.
d. The standard EPA procedures for analyzing compounds
such as those encountered in these studies, as
documented in EPA's SW846 Manual, were not applicable
for various reasons and had to be modified extensively.
For example, pentachlorophenol (PCP) could not be
detected at all in the samples by direct injection of
the sample extracts into the GC-MS, and it was
necessary to acetylate or derivatize the PCP prior to
injection. This essentially doubled the time normally
required for such analyses.
e. There was strong evidence that the spiked soil samples
provided by PEI were not homogeneous were received.
Upon initial opening of the sample containers,
condensation was observed on the can lid, and pools of
liquid were apparent on the soil surface. The quantity
of water present in the samples prevented effective
mixing and representative subsampling. Finally, these
soils were observed to contain rocks and other foreign
matter which clearly indicated non-homogeneity and
prevented accurate subsampling.
All of the above factors led to large variations in the
analytical results and were directly responsible for the delays
encountered in completing the analyses. Nevertheless, by major
efforts, well in excess of those anticipated, our Laboratory has
-------
Mr. Bart Thompson
Page 4
December 4, 1987
completed a substantial portion of the required analyses. The
data presented here include the following:
1) Metals Data: The measured concentrations of metals in all of
the treated and untreated soil samples as reported by Analytical
Enterprises have been converted to the total quantities of the
untreated and treated samples, from our knowledge of total sample
weights for each fraction analyzed. These results are shown in
Tables 1-4, attached herewith.
2) Volatile Organics Data: Volatile organics data available at
present are summarized in Tables 5-9 attached herewith. The
designation "UN" following a sample number refers to the
untreated soil. Similarly, the designations, "SO," "KP," "WA,"
and "XA," in Tables 5-9 refer to spent soil, spent KPEG, soil
wash water, and XAD solid sorbent (used to trap evolved
volatiles), respectively. The headings in these tables,
"Acetone," "1,2-Di," "Tetra," "Chloro," "Ethyl," "Xylene," and
"Styren" refer to acetone, 1,2-dichloroethane,
tetrachloroethylene, chlorobenzene, ethyl benzene and styrene,
respectively.
3) Semi-Volatile Organics Data: The data for semi-volatile
organic compounds obtained thus far are summarized in Tables 10-
13.
Several general conclusions are possible from these data, which
are likely to remain valid even after all the analyses have been
completed. These are:
a. The metals data indicate that few of the metals were
effectively removed from the soils by the KPEG treatment
and, subsequent water washing. Probably this is due to the
inorganic forms of the metals and their relatively poor
aqueous solubilities. In retrospect, extraction of these
could probably have been enhanced by using an acid water
wash of the spent soil after KPEG treatment. The overall
materials balance for the metals is quite poor, however.
b. The volatile and semi-volatile organic data also exhibit
very poor materials balances, but it seems clear that both
1,2- dichloroethane and tetrachloroethylene have essentially
been completely destroyed by the KPEG treatment. The other
chlorinated organics, chlorobenzene and pentachlorophenol,
were not significantly affected by the KPEG treatment, which
is not surprising, since it is known from other work, that
destruction of these would have required higher temperatures
than those used in the KPEG tests here. It was not
practical to use such higher temperatures in these tests
because of the flash points and volatility of the other
-------
Mr. Bart Thompson
Page 5
December 4, 1987
organics (acetone, particularly) present in these samples.
The hydrocarbons (xylene, ethyl benzene and styrene) in
these samples were not expected to be affected by the KPEG
treatment, and indeed no effects on degradation of these are
discernible. The data for acetone are so suspect in view of
volatility problems and instrument saturation, background
and holdup, as to be totally unreliable.
We hope that these results are useful in comparing the several
technologies evaluated on this project and we are working
vigorously to complete the full final report in the coming week.
The delays in completing the analyses which we have encountered
were beyond our control, but we regret that this has impeded the
overall technology assessment.
Sincerely, ,
'
Thomas O. Tiernan, Ph.D.
Professor of Chemistry
pat
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-------
Table 3
uw i r •*-••*
b/.-:. /*
•n~ i-i. M*<
b'i"*. 1 «i
1 1 IHuMIl 'fl
f ( lUNl) M U / D
n 3*. V"/i
n i"; 1 . vn9
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u iS. '/'._'
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1 UT«L
1S1 (.O. i?^ uu
1 J't?"ii!G. 7 tf* MII
•i5.= . 'ii MCI
1 1. on MD
LtJlT'CR CI-'I'-PER
FOUI-ih "u/n TOlfiL
j 'i'j. li'M' 1 /L-'itJ'i. -Hi'
•/ nr f. 11
OVFRfil i.
ro r
15 •('£»(?. 33
•<• RLC IN blitL
(jVt.f
lt.ll. '/'k-l
5Bf>7 j.j. ^i
't'-'.'f: 1 1 /. ,:.vi >.ia
f3i.fl). (lO Mil
1 11// (3. V"
t. /.','_•. «"
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l.lVt.Hill.l HI I-
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•'- i* n
SC-EM i inliiOflt.tl ] I -I t-a'5. vi-3 u
£>.._•'?'
TOT fil,
1£ 1 7 1 . £1? uii
3315. :.tf no
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I 7-'«636. V"/<
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1'JMBI I . i-^
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9G.
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uvt urn i. m c
-------
Table 4
[IL 1-1 5 •?:.,. em u
IN ^iniiDMhi) nnni.vi IC:»IL I IPII 'L fc i I MC i l NC
iii". it, in fruiiMi> MP/O IOIOL
i.iij.vn!' si9/:5r... 0*. no
n Kim 1-
Wn'.M lui II N 1 • I
bl-LNI ULMtft. HI I
i":OI7f.a. MI?I 1.1 u
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liVl Id II l (»
t / \ . t.fi a
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UNTHLOILI) SIIIL IV-l
1 1 77 V3««l. OS MD
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fi I tiHfatfj. V«i i.i a
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D 17£5.
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t.7 1 55'». B'i'i LIU
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fcfi7ti. Cut* uu
7fi. £7
-------
Table 5
•fright State University, Dayton. Ohio 45435
Analysis for Destruction of Volatiles with KPE3
Concentrations Found (Microorans oer orau of saaole or oarts-oer-aillion)
>EI 1-1
Saaole
iuaoer
SRM-l-i UN
IARJI-1-1 SO
'ARM-1-1 KP
aw-i-i m
3WH-1 Xfl
flceton
7885
75.8
1392
230
376
1,2-Di
584
ND
0.0845
ND
0.807
ND
8.0370
3.06
Tetrac
585
0.684
ND
1.91
ND
0.0548
5.66
Chloro
345
8.N
254
35.2
12.4
Ethyl
3917
95.2
1894
163
108
Xylene
10063
265
5586
413
177
Styren
827
27.0
554
79.0
29.8
a. The designation ND indicates 'None Detected* in excess of the uniiua detectable
corcentratlon which is listed directly below the ND designation.
-------
TAble 6
Wright State University, Dayton, Ohio 45435
Analysis for Destruction of Volatiles with KPES
Concentrations Found (aicrograas oer graa of saiole or oarts-oer-nillion)
1-2
Aceton 1,2-Di Tetrac Chloro Ethyl Xylene Styren
SRM-2-1 UN 212 0.133 23.5 4.26 28.4 181 123
BftRM-2-1 SO 14.7 ND 2.21 8.146 8.8fl2 2.92 8.488
0.8262
47.6 155 17.4
8.84 31.1 4.88
2.17 5.38 29.1
a. The desionation ND indicates 'None Detected1 in excess of the Binimu detectable
concentration which is listed directly below the ND designation.
$91-2-1
£91-2-1
£R?r2-l
KP
«
Xfl
284
12.2
23.3
ND
8.312
ND
8.0174
ND
8.8638
1.48
ND
8.8142
8.854
4.41
1.5!
ND
8.0552
-------
Table 7
Wright State University, Dayton, Ohio 45435
flnalysis for Destruction of Volatiles with KPEB
Concentrations Found (iticrooraus oer graa of saaole or oarts-oer-million)
PEI 1-3
Sasole flceton 1,2-Di Tetrac Chloro Ethyl Xylene Styren
Nuaber
SflRM-3-2 UN 496 6.53 27.3 13.1 188 588 48.5
SARM-3-2 SO 15.6 ND 1.27 8.457 3.85 9.76 8.766
SARM-3-2 KP 169 MD 2.29 8.85 76.5 244 18.1
8.384
SARM-3-2 UA 13.7 ND ND 2.13 13.7 47.3 5.22
8.8239 8.8214
a. Tlie designation ND indicates 'None Detected" in excess of the ainimn detectable
concentration which is listed directly below the ND designation.
-------
Table 8
Urignt State University, Dayton, Ohio 45435
flnalysis for Destruction of Volatiles with KPE5
Concentrations Found (uicrograas per graa of saaole or oarts-oer-Million)
•El 1-4
kaole Aceton 1,2-Di Tetrac Chloro Ethyl Xylene Styren
Junber
aflt-4-1 UN 3859 151 1265 387 2916 7451 721
•>flRfl-4-! SO 250 ND 1.85 3.69 38.0 88.6 13.0
0.395
3RM-4-1 KP 1208 ND ND 242 1769 5501 569
1.07 3.65
•flRM-4-1 M 13.2 ND 0.503 25.7 82.1 265 66.6
0.8571
a. The designation ND indicates 'None Detected* in excess of the niniiui detectable
concentration which is listed directly below the ND designation.
-------
Table 9
Wriont State University, Davton, Ohio 45435
flnalysis for Destruction of Volatiles with KPEG
Concentrations Found (aicrograss per oraa of sanole or parts-oer-aillion)
•El SET 1
knole Aceton 1,2-Di Tetrac Chloro Ethyl Xylene Styren
iuaoer
-l UN
7885
584
585
345
3917 18063
827
SfiWH SOIL 3.46 NO 8.148 8.1% 1.85 3.67 8.367
8.9018
SRM-2-1 tM
212 8.133 23.5 4.26 28.4
181
123
3B-2 SOIL 7.59 8.91S0 8.8129 8.81S1 8.3713 8.247 8.9553
496 6.63 27.2 13.1
188
583 48.5
3ARM-3 SOIL 4.86 0.138 0.9068 0.0386 8.8918 8.288 8.0547
TM-1 UN 3859
151 1265
387 2916 7451
721
3flR«-4 SOIL 3.35 NO 8.156 8.0182 8.8623 8.216 8.8343
0.8838
a. The designation ND indicates 'None Detected* in excess of the iiiniiiui detectable
concentration which is listed directly below the ND designation.
-------
Table 10
«S'J K?Z5 Concentration (ug/kgi Total Quantity .jg)
PEI Soil Treaties: SSu Run Fraction
* **« • » •• w •
SARK-I-1
SARK-I-1
SARK-I-1
SARK-I-1
SARK-I-1
SARK-I-1
SARK-II-1
SAHK-II-1
SARK-II-1
SAM-II-1
SARK-II-1
SARK-II-1
SARK-III-2
SARK-III-2
SARK-III-2
3ARM-III-2
SARK-III-2
SARK-III-2
SARK-IV-1
SARK-I7-1
^a-.;-.
PZISV0353
PEI7-1-1A PEIS70047
PSI7-1-1A PEIS70040
PEI7-1-1A PEIS70041
PEI7-1-1A — Destr
... .... STTCVPfJJ
riiivuuci
PSI7-2-1A PSISV0037
PEI7-2-1A PEIS70051
PBI7-2-1A PEISV0054
PEI7-2-1A — Destr
......... offTcvnfiCT
PEI7-3-1A PSIS70350
PEI7-3-1A PEISV0052
PEI7-3-1A PEIS70056
PEI7-3-1A — Destr
...... 5TT?t'Pr.!G
riliVuUiJ
r:I.-J-4i
* " i ~ "t ~ 1 "" * Y - "
* +m v • » 4 ^ w w
Listed levels
Untreated soil
Treated soil
KPEC
later
j.-IwU iOCalS
Listed Levels
Untreated soil
Treated soil
JPEG
later
uction Totals ------
Listed Levels
Untreated soil
Treated soil
KPEG
Water
uction Totals
Listed Levels
Untreated soil
. „ ; 1 1. c '* a ^ * _
6,530
4,554
157
579
212
660
^*1
44 I
251
151
3
660
13
185
172
2
6,600
4,210
1.4
, 3
,000
,420
,100
,360
,715
,000
,540
,050
,362
,550
,000
,740
,186
,833
,442
,000
,040
.«.
i . -
2,500,
539,
13,
115,
35,
250,
40,
3,
2,
1,
250,
62,
3,
1,
1,
2,500,
936,
*«! i
300
680
200
820
144
000
200
696
018
017
000
240
322
983
884
000
560
t 1 ft
13G
• = 1 3 u
105
105
89
210
113
106
106
130
179
122
116
116
130
190
116
97
97
_ . a
W \y !
.3
.3
.0
.0
.1
.9
_9
T
. I
.9
.2
.7
.7
.4
.3
.5
.9
.9
. /
. 3
n-ivJl3
635
479
14
121
24
[160
70
24
32
29
0
[ 62
77
1
24
32
0
I 57
546
412
it
L L
IEUC
.0
.6
.8
.7
.1
.7]
.6
.3
.8
.1
.4
.3]
.0
.6
.1
.9
.3
.3]
.1
.2
.5
1
~ •**•
263.3
55. d
1.3
24.3
4.3
[29.5]
26.7
4.3
0.5
0.4
0.1
[ i.o]
29.2
7.3
0.4
0.4
0.2
; i.o]
244.3
91.7
6 . I
SARK-I7-1 PEI7-4-1A PEIS70C57 i'ater 44,573 144 120.8 5.4
SARK-IV-1 PEI7-4-1A — Destruction Totals [ 42.6]
-------
Tahle 11
?il Soil
Saicle No.
?S3Y-"-i
3.1ilZ . i
? \ nu.T. '
iAK3 i 1
SARK-I-1
SAXK-I-1
SARK-I-1
SlPX-I-1
CSPV.7T.1
JAKfl i- i
ClDlf-TT-'
iAKfl ii i
SARK-II-1
SARK-II-1
SARK-II-1
eiBU.TT.I
O8M-TTT-1
5AKH ill 4
ClDY.TTT-^
5AK.*. Ill i
5ARK-III-2
SARK-III-2
SARK-III-2
CJDB.TTT-l
C13¥-TV-1
iAKn ii 1
C S DM.TU- 1
;A.,H-iV-l
SARK-I7-1
^lRH-TV-1
Treatie:t ifSU Rua
Nuiier Suaier Saiple Tj;a
--------- Listed Bevels
rSIS«0053 Untreated soil
SARK-I-1 PEISV0070 Treated soil
SARK-I-1 PEIS70072 KPEG
SARK-I-1 PEIS70073 later
PE»S70u64 Untreated soil
SARK-II-2 PEIS70033 Treated soil
SARK-II-2 PEIS70074 JPEG
SARK-II-2 PEISV0075 Kater
PEISV0063 Untreated soil
SARK-III-2 PEISV0062 Treated soil
SARK-III-2 PEISV0077 IPEG
SARK-III-2 PEIS70078 later
Listed Levels
PEISVOO'8 Untreated soil
SlOif.TY-1 3?'"'!Qfl "*33-;j 5;-'
»T^rS
SARM7-1 PEIS70030 iater
o,ouu,OCi
,::4,420
395,500
657,480
270,536
£ i ,1 "1 0 fl
gOO , JuU
^0* .40
L!( , 3*u
55.583
105,870
11.102
fen rtrtrt
oou,yuu
11 T Af\
IJ, /4U
31,127
186,847
22,980
6; n rt n rt fl
, QUO, 000
4.^x0,040
5; '*'
821,431
DSH?
,500,000
539, o30
33,880
24,230
3,916
1Cfl rtrtft
-------
Table 12
?SD KFZG T:tal Quaa:::? lu?) Tc:ai ;ui::i:j is;)
:I S:il Treaties: ISU Xun in Sz:ract Praccioa
asie Xo. Huiier S'iacar Saipie lyce A:;irace:e 3ZE- . Keigat ig) ls:arj:s:e DSH?
- - ....... DPTCVfrflO VarHfl'f 5T*n'» rt 11X5 5 11Q
— --------- rSlJiUUl* 38C.18U JiaflX U.1J43 J.AUJ
-------- ......... OrT?"JfinJ1 Marring SlanV fl rt11? ft 119J
Cflrt rt
"OU.U
100.3
?m A
Jl)U . J
100.0
Ol'l
.Jo/
0.013
Oftftfl
.UU9
0.002
i 'i
2.ou
0.52
Of C
.03
0.13
-------
Table 13
PEI Soil
SdMle No.
SWH-1
SWH-1
SUH-I-1
SWH-1
SftfflH-1
SfWH-1
SWHI-1
SWHI-1
SWHI-1
SWHI-1
SWHI-1
SWHI-1
SWHII-2
SflRM-III-2
SflRM-III-2
SWHII-2
SWHII-2
SWHV-1
SWHV-1
SWHV-1
SWHV-1
SWHV-1
SflRM-!V-l
USU KPE5
Treatment
Nuiber
PEI7-1-W
PE17-l-lfl
PEI7-1-W
PEI7-1-W
PEI7-2-1B
PEI7-2-W
PEI7-2-W
PEI7-2-lfl
PEI7-3-1B
PEI7-3-1B
PEI7-3-1S
PEI7-3-1A
PEI7-4-1A
PEI7-4-W
PEI7-4-1P
PEI7-4-10
USU Run
Number
PEIPCP0311
PEIPCP0009
Concentration (uD/kg)
Saiole Tyoe PentaChloroPhenol
Listed Levels
Untreated soil
Treated soil
KPES
PEIPCP0010 Water
PEIPCP0025
PEIPCP8026
PEIPCP0027
Listed Levels
Untreated soil
Treated soil
KPES
PEIPCP0028 Water
PEIPCP0019
PEIPCP0022
PEIPCP0023
Listed Levels
Untreated soil
Treated soil
KPE6
PEIPCP0024 Water
Uebvruk
PE1PCP0018
PEIPCPW13
PEIPCP0014
Listed Levels
Untreated soil
Treated soil
KPEB
PEIPCPM17 Water
242.678
5.665
686,320
204,865
100,000
3,970
217
1,533
523
100,000
61,590
594
2,696
736
1 MA flfllflt
lj VWVf vtfC
85,009
3,895
320,590
82,096
Fraction
Weight (g)
105.3
105.3
89.0
210.0
113.1
106.9
106.9
139.7
179.3
122.2
116.7
116.7
130.4
190.3
116.5
97.9
97.9
115.7
178.9
120.8
Total Quantity (E
PentaChloroPheno
185.3
25.6
9.5
144.1
23.2
C167.M
10.7
0.4
0.9
0.3
0.1
[ 8.4]
11.7
7.2
0.1
8.5
9.1
[ 8.7]
37.9
8.3
8.4
57.4
9.9
r C7 71
-------
I -
REPORT ON METAL ANALYSES TO DEVELOPMENT OF TREATMENT DATA
ON THE KPEG PROCESS FOR SARA/BDAT STANDARDS
Prime Contract No. 7C3072 YAWE
Subcontract No. 4-87-1-0275
Submitted To
Mr. Charles Rogers
U. S. Environmental Protection Agency
Mr. T. D. Ferguson
U. S. Environmental Protection Agency
Ms. J. L. Hessling
.PEI
Prepared By
James T. Kinard
Analytical Enterprises, Incorporated.
-------
SAMPLE INVENTORY
A total of sixteen (16) samples were received from Wright State University, 175
Brehm Research Laboratory, Dayton, Ohio 45435, on September 19, 1987. Samples
were delivered by Federal Express. The contents of the package were examined
for possible breakage and each sample was logged in AEI's Sample Log Book. All
containers were intact and their was no damage to packed samples.
The Sample Inventory is given below:
SARM - EPA/PEI SAMPLE INVENTORY
1. SARM-I-I
2. SARM - II - I
3. SARM-III-2
4. SARM - IV - 1
5. SARM - I - I
6. SARM-II-I
7. SARM - III - 2
8. SARM - IV - 1
9. SARM - I - I
10. SARM - II-1
11. SARM-III-2
12. SARM - IV-1
13. SARM-I-I
14. SARM - II-1
15. SARM-HI-2
16. SARM - IV - 1
Untreated Soil
Untreated Soil
Untreated Soil
Untreated Soil
Treated Soil
Treated Soil
Treated Soil
Treated Soil
Spent Reagent
Spent Reagent
Spent Reagent
Spent Reagent
Wash Water
Wash Water
Wash Water
Wash Water
-------
SAMPLE PREPARATION AND ANALYSES
Based on the "Statement of Work" in Prime Contract No. 7C3072YAWE/Subcontract
No. 4-87-1-0275, AEI was to analyze samples for the eight metals: Arsenic (As);
Beryllium (Be); Cadmium (Cd); Chromium (Cr); Copper (Cu); Lead (Pb); Nickel (Ni)
and Zinc (Zn).
The soil samples were sludges with considerable amounts of water present. An aliquot
of each soil sample was weighed out and digested according to SWA-846, Method
3050 for all metals, except arsenic, with the final digestate taken up in a hydrochloric
(HC1) acid matrix. A separate aliquot was digested for arsenic, with the final
digestate existing in a nitric (HNOs) acid medium. Aliquots of spent reagents and
wash waters were digested according to Methods 3010 and 3005, respectively for
arsenic. The remaining amounts of wash waters and spent reagents were digested
for all the other metals.
Samples were analyzed for arsenic using a Perkin Elmer 5000 Atomic Absorption
Spectrophotometer with Zeeman Background Correction, an HGA - 500, and an AS-40
Autosampler.
The other metals were determined in the prepared samples by use of Flame Atomic
Absorption Spectrophotometry. Each sample was analyzed by using the method
of standard additions. Blanks and spiked samples were also run.
The results of the sample analyses are reported in the attached table. All sample
results are based on wet weight.
-------
Concentration of Metals in Standard Analytical References Matrix - Potassium Polyethylene Glycol Treatment Samples
Arsenic
METALS
(ug metal/g sample)
Beryllium
Cadmium
Chromium
Copper
Lead
Nickel
Zinc
Treated
Soil I-I
Untreated
Soil I-I
Treated
Soil 11-1
Untreated
SoU II-l
Treated
Soil III-2
Untreated
Soil III-2
Treated
Soil 1V-1
Untreated
SoU IV-1
Wash Water
I-I
Wash Water
II-I
Wash Water
III-2
Wash Water
IV-1
Spent
Reagent I-I
Spent
Reagent II-I
Spent
Reagent III- 2
Spent
Reagent IV-1
8.1
20
8.7
20
184
359
168
338
8.2
8.6
—
458
Undetected
(DL = .04 ng)
Undetected
(DL = 0.04ng)
1.2
96
•Undetected
Undetected
Undetected
Undetected
Undetected
Undetected
Undetected
Undetected
Undetected
Undetected
Undetected
Undetected
Undetected
Undetected
Undetected
21
45
34
59
861
3,488
4,855
6,148
1.5
1.8
1.8
4.5
2.4
6.3
4.5
7.1
21
30
23
33
826
1,163
918
1,407
0.97
8.2
168
174
Undetected
(DL = 0.02)
Undetected
(DL = .02)
2.2
13
251
349
330
376
6,736
11,678
9,381
10,928
13
20
281
454
7.9
17
38
310
195
304
169
379
11,350
14,451
9,827
17,175
6.8
18.2
1,970
1,836
18
29
1,435
977
32
68
33
70
1,615
2,409
2,332
2,448
2.0
2.2
4.4
2.6
8.4
13
3.0
8.7
492
1,028
1,269
1,725
973
24,262
14,736
23,414
3.7
10
1,966
2,576
r, . 'j
11
566
933
•Detection Limit for beryllium is 0.01 ug/g.
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