905R96020
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• REPORT
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PHASE I INVESTIGATION OF DIOXIN/FURAN SOIL
LEVELS IN COLUMBUS, OHIO
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• Submitted to
U.S. ENVIRONMENTAL PROTECTION AGENCY
• Office of Pollution Prevention and Toxics
and
Region V
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I EPA Contract No. 68-D2-0139
Work Assignment No. 4-2
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February 22, 1996
• Prepared by
3 BATTELLE
1505 KING AVENUE
COLUMBUS OH 43201
(614)424-4911
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TABLE OF CONTENTS
Page
SUMMARY 1
BACKGROUND INFORMATION 1
EXPERIMENTAL PROCEDURES 1
SAMPLE RESULTS 4
QUALITY CONTROL RESULTS 6
Method Blanks 6
Field Blanks 6
Surrogate Internal Standards 7
Matrix Spike/Matrix Spike Duplicate 7
Sample Duplicates 8
Standard Reference Material 8
Detection Limit (DL) Sample 8
APPENDIX A. COMPLETE ANALYSIS DATA SHEETS FOR
INITIAL ANALYSIS OF PHASE I SOILS A-l
APPENDIX B. ABBREVIATED ANALYSIS DATA SHEETS FOR
INITIAL ANALYSIS OF PHASE I SOILS B-l
APPENDIX C. ANALYSIS DATA SHEETS FOR 2,3,7,8-TCDF
SECOND COLUMN CONFIRMATION OF PHASE I SOILS . C-l
APPENDIX D. QUALITY CONTROL SAMPLE RESULTS FOR
PHASE I SOILS D-l
APPENDIX E CHROMATOGRAMS AND BENCH DATA FOR
PHASED SOILS E-l
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PHASE I INVESTIGATION OF DIOXIN/FURAN SOIL
LEVELS IN COLUMBUS, OHIO
February 22, 1996
SUMMARY
This report presents results from the analysis of polychlorinated dibenzo-p-dioxins and
polychlorinated dibenzofurans (PCDD/PCDF) in 34 soil samples from the area around a
municipal Waste-to-Energy (WTE) facility located in Columbus, OH. These samples were
analyzed according to U.S. Environmental Protection Agency (EPA) Method 8290 and the
Quality Assurance Project Plan (QAPP) established for this project.
BACKGROUND INFORMATION
The U.S. EPA Office of Pollution Prevention and Toxics conducted an initial soil
sampling study to characterize site contamination at the Columbus WTE facility. This report
provides a perspective on PCDD/PCDF contamination in the soil samples collected for Phase
I of this program. Phase II sampling will be directed according to the results from the Phase
I samples. These results, and information from previous and concurrent investigations may
indicate that more comprehensive sampling efforts are required for future site contamination
studies
EXPERIMENTAL PROCEDURES
• The 34 samples were processed in two sets of 17 with a method blank, a matrix spike,
matrix spike duplicate, and sample duplicate processed with each set. In addition to these
I four laboratory quality control (QC) samples, one of the background soils was spiked with
PCDD/PCDF at 5 times the method detection limits (MDL) to verify that detection limits
• were achieved. Method detection limits are 1, 5, and 10 pg/g for the respective tetra,
™ penta/hexa/hepta, and octa congeners. This detection limit (DL) sample was included in the
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first sample set. The soil samples and associated QC samples processed in each set, in order
of analysis, are as follows:
Set 01:
Method Blank
SOI, Field Blank
S04, Background Soil ^L
SOS, Background Soil
S06, Background Soil
S07
S17, Field Blank
S08
S09
S09, Duplicate u
SOS, Background Soil
503, Detection Limit Sample,
S02, Soil SRM
S10
Sll
S12
S13
S14
S04, Matrix Spike
S04, Matrix Spike Duplicate^
S15
Set 12:
S18
S19
S34 _^
S34, Matrix Spike
S34, Matrix Spike Duplicate
Method Blank
S20
S21
S22
S23
S24
S25
S26
S27
S28
S29
S30 -
S31 -
•7
S33, Duplicates
Approximately 10 g of each soil sample was used to determine percent solids (percent
dry weight). Another approximately 10 g of each sample was combined with sodium sulfate
for extraction. All samples were spiked with isotopically labeled analogs of fifteen of the
seventeen 2,3,7,8-substituted PCDD/PCDF prior to extraction. The samples were extracted
for approximately 18 hours with toluene in a Soxhlet apparatus. Extracts were spiked with
37Cl4-2,3,7,8-TCDD cleanup standard, partitioned against base and acid solutions, and
processed through acid/base silica, basic alumina, and carbon AX-21/Celite cleanup columns.
Extracts were spiked with l,2,3,4-TCDD-13C12/l,2,3,7,8,9-HxCDD-13C12 recovery standard
and concentrated to a final volume of 20
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During the final sample preparation steps for the second set of samples, a stop work
order was received from EPA. Sample extracts were processed through the carbon column
cleanup procedure and were ready for final sample concentration. The extracts, in 100-mL
round bottom flasks, were sealed with teflon tape and stored in a refrigerator for 3 weeks
until authorization to proceed was received. During this storage period, four sample extracts,
S19, S20, S21, and S22, went dry in the round bottom flasks. After reconstituting these four
samples with 1 mL of hexane, all of the Set #2 samples were concentrated to a final volume
of 20 /iL as with Set #1.
Sample extracts were analyzed on a VG AutoSpec high resolution gas
chromatography/high resolution mass spectrometer (HRGC/HRMS) (Serial #X088, System
#6744) in the selected ion monitoring mode on a J&W DB-5 capillary column (Serial
#4499117) at an instrument resolution of approximately 10,000 (10 percent valley). A
Hewlett Packard 5890 Series II Gas Chromatograph (C128/83) served as the inlet. Data
reduction was performed on a VAX station 3100, M38, Model WS42A-BC (Serial
#AB11300V6D) using OpusQuan software. The criteria used to identify chromatographic
peaks were: (1) >2.5 signal-to-noise ratio; (2) ion abundance ratios within 15% of theoretical
values; (3) retention times of native analytes within ±2 seconds of 13C12-labelled internal
standards; and (4) no diphenyl ether interferences. Some samples were diluted to reduce
chromatographic interference problems. The dilution factor is noted on individual analysis
data sheets. Because 2,3,7,8-TCDF is not completely resolved from all other tetra-
chlorinated isomers on the DB-5 column, second column confirmation of 2,3,7,8-TCDF
levels above 1 pg/g dry weight in the initial analysis was performed on a J&W DB-Dioxin
column (Serial #2743516) for 14 samples.
Per the QAPP for this project, the following deviations to Method 8290, which are
part of routine sample preparation/analysis in Battelle's Dioxin Laboratory, were employed:
Sample Preparation
1. The following additional internal standards were added to the samples prior to extraction
to improve analytical accuracy:
i3
I3Cr-2,3,4,7,8-PeCDF I3C12-l,2,3,4,7,8-HxCDD
13Cp-1.2,3,6,7,8-HxCDF 13C12-l,2,3,7,8,9-HxCDF
13CP-2,3,4,6,7,8-HxCDF 13C12-l,2,3,4,7,8,9-HpCDF
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2. A cleanup standard, 37Cl4-2,3,7,8-TCDD, was added to the samples prior to processing
through cleanup columns to evaluate analyte recovery through cleanup.
3. A 30-mL volume of acid was used for the first acid wash of the sample extract, rather
than 40-mL; 20 mL of acid was used for each successive acid wash instead of 40 mL; 15
mL of base was used for the base wash; and 20 mL of distilled water was used instead of
the 40 mL of 5% sodium chloride washes.
4. In the acid/base silica column cleanup, a 1-g plug of silica gel was placed between the
basic silica and the acid silica layers. In addition, sodium sulfate was added to the top of
the column. The column is rinsed with 30 mL of hexane instead of 10 mL. The sample
was usually applied in 5 mL of hexane instead of the 2 mL of hexane specified in Method
8290. The column was eluted with 75 mL of hexane instead of 90 mL.
5. In the alumina column cleanup, Sigma basic alumina, WB-2, activity grade I, was used
instead of acidic or neutral alumina. For the first elution, the alumina column was rinsed
with 15 mL of 3% methylene chloride/hexane instead of 20 mL of hexane. The second
elution, containing the PCDD/PCDF, consisted of 40 mL of 50% methylene
chloride/hexane instead of 15 mL of 60% methylene chloride/hexane specified in Method
8290.
6. For the carbon column cleanup, the columns did not include plugs of celite at the top and
bottom of the carbon/celite packed bed. The carbon column was eluted with 30 mL of
toluene instead of 20 mL as specified in Method 8290.
Sample Analysis
1. Commercially-prepared calibration standards at concentrations specified in Method 1613
were used instead of calibration concentrations specified in Method 8290. The Method
1613 calibration concentrations cover a wider range and lower limits for some compounds
than the Method 8290 calibration concentrations.
2. Typical injection volume was 0.5 fiL or 1 fj.L instead of 2 pL specified in Method 8290.
Acceptable sensitivity (i.e., 1 pg/g detection limit for soil samples) has been demonstrated
by Battelle using the smaller injection volume.
SAMPLE RESULTS
Appendix A includes data sheets with analytical results from the initial analysis and
associated quality control results. Abbreviated analysis data sheets presenting only sample
results are provided in Appendix B. Data sheets in Appendix C present 2,3,7,8-TCDF
concentrations from second column confirmation analysis of 14 samples. Where applicable,
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results from the 2,3,7,8-TCDF second column confirmation analysis have been inserted into
the initial analysis data sheets in Appendices A and B. Please note the following when
reviewing these results:
(1) The "*" on the data sheets indicates that the analyte was not detected at a
concentration above the sample limit of detection.
(2) The HRGC/HRMS instrumentation was calibrated in the ranges corresponding
to analyte levels in the samples of 1.3 to 520 pg/g dry weight for tetra
compounds, 6.4 to 2560 pg/g dry weight for penta through hepta compounds,
and 13 to 5120 pg/g dry weight for octa compounds. These calibration ranges
are based on an average sample dry weight of 7.8 g and a 1-^L injection
volume. Concentrations below these calibration ranges have been reported;
however, accuracy of concentrations outside the calibration range cannot be
guaranteed.
(3) Of the 34 samples, 29 had 2,3,7,8-TCDF concentrations above 1 pg/g dry
weight and required second column confirmation analysis. Only 14 of these 29
samples received a second column confirmation analysis due to budget
constraints. For those samples which received a second column confirmation
run, the 2,3,7,8-TCDF value from the second run has been inserted into the
initial data sheet. The 2,3,7,8-TCDF values for the 14 extracts which were
processed through the second column confirmation run showed a 25% - 50%
decrease from 2,3,7,8-TCDF values obtained in the initial analysis.
(4) Some samples had polychlorinated diphenyl ether (PCDPE) responses at the
same retention time as 1,2,3,4,7,8-HxCDF and 1,2,3,6,7,8-HxCDF. Per
Method 8290, Section 7.8.4.4, 1,2,3,4,7,8-HxCDF and 1,2,3,6,7,8-HxCDF
peaks could not be identified definitively as PCDF and were therefore not
quantified as PCDF.
(5) The matrix spike recoveries for S34 MS and S34 MSD were calculated using
the equation:
% REC = 100 (MS cone. found)/(Spike cone. -I- Background cone.)
(L. P. Provost and R. S. Elder, "Interpretation of Percent Recovery Data,"
Amer. Lab., 15(12), pg. 57, 1983). The above equation was employed since
the background level of analytes was much higher than the spike level. In this
method of calculating percent recovery, the small spike levels are not "lost in
the noise" of laige background levels.
(6) Sample S27 had very poor chromatography in the 2,3,7,8-TCDD window
which may have affected its detection.
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(7) In some instances an analyte concentration which is slightly below the
instrument limit of quantitation (LOQ) has been reported. In these cases, the
analyst judged the analyte met Method 8290 identification criteria and so the
concentration determined has been reported along with the sample limit of
detection (LOD) and the instrument limit of quantitation (LOQ).
(8) The sample limits of detection shown on the data sheets were calculated
according to Method 8290, Section 7.9.5.1.1. For all but two analyses, the
LODs achieved were well below the method detection limits outlined in
Method 8290 of 1, 5, and 10 pg/g for tetra, penta/hexa/hepta, and octa
congeners. The SOS and SOS DL spike samples had to be diluted 1:2 due to
chromatographic interferences. As a result, the LODs shown on the data
sheets in Appendix A are above the method detection limits for these two
samples. The LOD achieved for OCDD in two samples was higher than the
method detection limit of 10 pg/g, however, since OCDD was found at much
higher levels in background soil samples, this high LOD does not adversely
impact the sample results.
QUALITY CONTROL RESULTS
Appendix C contains summary tables of quality control results for matrix spike, matrix
spike duplicate, sample duplicate, standard reference material, and detection limit (DL)
samples. In addition, prior method detection limit study results and prior soil SRM results
have been provided.
Method Blanks: A method blank was processed with each of the two sample sets to
demonstrate freedom from contamination in the laboratory processing and analysis
procedures. A 10-g aliquot of sodium sulfate was processed through all extraction, cleanup,
and analysis procedures as if it were an actual sample. PCDD/PCDF were not detected or
were detected at levels below the sample limits of detection achieved for the background soil
samples S03 and S04.
Field Blanks: In order to verify that the reference matrix (playsand) used for field blanks
was PCDD/PCDF-free prior to^use, a 10-g aliquot of the playsand was spiked with internal
standards, extracted, and processed through all cleanup procedures as described for field
samples. In addition, an aliquot of methylene chloride was used to rinse the jars in which the
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field blanks would be shipped. Both play sand extract and the jar rinsate samples were
analyzed and found to be free of PCDD/PCDF. Field blank samples were thus prepared by
rinsing new 500-mL jars with methylene chloride, filling about 1/2 full with playsand, and
sealing jars with lids and teflon tape.
The field blanks for Phase I sampling effort were samples SOI, S17, and S32. In each
case, PCDD/PCDF were not detected or were detected at levels well below both the LOQ
and below the sample limit of detection achieved for the background soil samples S03 and
S04.
Surrogate Internal Standards: Each sample was spiked with 13C12-labeled analogs of
fifteen of the seventeen 2,3,7,8-PCDD/PCDF prior to extraction. Recovery of these internal
standards gives an indication of method performance. All internal standard recoveries were
within the 40-135 percent limit stated in Method 8290 except for OCDD-13C12 in sample S18
and several internal standards in samples S20 and S23. For sample S23, chromatographic
interferences may have caused the low internal standard recoveries. The low recoveries for
sample S20 may have resulted from the sample going dry during the storage period required
by the stop work order.
Matrix Spike/Matrix Spike Duplicate: A matrix spike (MS) and matrix spike duplicate
(MSD) were processed with each sample batch by spiking both samples with a low level of
the seventeen 2.3,7,8-PCDD/PCDF and processing through all extraction, cleanup, and
analysis procedures.
Spike recoveries for these four quality control samples were 81 to 139 percent with one
exception. Recovery of the 1,2,3,7,8,9-HxCDD in the S34 matrix spike and S34 matrix
spike duplicate was high and is attributed to polychlorinated diphenyl ether interference.
Recoveries of all of the analytes in the S34 MS and S34 MSD were calculated using the
equation listed on the data table in Appendix D. The equation was employed since the
background level of analytes was much higher than the spike level. In this method of
calculating percent recovery, me small spike levels are not "lost in the noise" of large
background levels.
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Required control limits for matrix spike/matrix spike duplicate agreement were ±20%
relative percent difference (RPD). This control limit was met for both sets of matrix
spike/matrix spike duplicates.
Sample Duplicates: One sediment sample was processed in duplicate for both extraction
sets. Required control limits for duplicates were less than 25% RPD for analytes at levels
greater than ten times the method detection limit. The control limit was met for all analytes
in both samples. In S09, RPD greater than 25 percent were obtained for some analytes but
in these cases analyte concentrations were less than ten times the method detection limit and
in most cases below the instrument limit of quantitation.
Standard Reference Material: One soil standard reference material (Cambridge Isotope
Laboratories #EDF-2513) was received with the soil samples, designated S02. This soil
SRM was extracted with the first set of samples. Recoveries of the analytes ranged from
86.4% for 1,2,3,6,7,8-HxCDD to 123.5% for OCDD. A table of previous results obtained
for this soil SRM can be found in Appendix D.
Detection Limit (PL) Sample: One of the background soils (S03) was used to verify that
method detection limits were achieved. Two aliquots of S03, one spiked with PCDD/PCDF
at about 5 times the method detection limit (MDL) and one unspiked to serve as its
background, were extracted with the first set of samples. The recoveries of the analytes
ranged from 75.0% to 117.0%. Recoveries were calculated using the same equation as for
the S34 MS/S34 MSD:
% REC = 100 (Cone. found)/(Spike cone. + Background cone.)
(L. P. Provost and R. S. Elder, "Interpretation of Percent Recovery Data," Amer. Lab.,
15(12), pg. 57, 1983). The above equation was employed due to the high OCDD
a
background concentration measured in unspiked sample S03. In this method of calculating
percent recovery, the small spike levels are not "lost in the noise" of large background levels.
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The acceptable recoveries obtained for the DL sample demonstrate that PCDD/PCDF
concentrations near the method detection limit can be accurately quantified.
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• APPENDIX A
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COMPLETE ANALYSIS DATA SHEETS FOR
INITIAL ANALYSIS OF PHASE I SOILS
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Phase I Sample Analyses
Set#l:
47482-6-22
47482-6-16
47482-6-2
47482-6-3
47482-6-4
47482-6-5
47482-6-15
47482-6-6
47482-6-7
47482-6-20
47482-6-18
47482-6-19
47482-6-17
47482-6-8
47482-6-9
47482-6-10
47482-6-11
47482-6-12
47482-6-21
47482-6-23
47482-6-13
47482-6-14
FMethod Blank
LS01, Field Blank
\_S04, Background Soil
S05, Background Soil
S06, Background Soil
S07
CS17, Field Blank
SOS
S09
[JS09, Duplicate -- ^
S03, Background Soil
Detection Limit Sample
Soil SRM
S10
Sll
S12
S13
^S04, Matrix Spike
CS04, Matrix Spike Duplicate
S15
Set #2:
47482-
47482-
47482-
47482-
47482-
47482-
47482-
47482-
47482-
47482-
47482-
47482-
47482-
47482-
47482-
47482-
47482-
47482-
47482-
47482-
47482
10-2
10-3
10-19
10-20
10-21
10-22
10-4
10-5
10-6
10-7
10-8
10-9
10-10
10-11
•1GH2
10-13
•10-14
10-15
10-16
10-17
-10-18
34, Matrix Spike Duplicate
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SET#1
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APPENDIX B
ABBREVIATED ANALYSIS DATA SHEETS FOR
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PCDD/PCDF ANALYSIS DATA SHEET
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12-06-95
C-95 Time 1858 11
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