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
    INTTTAL ANALYSIS OF PHASE I SOILS

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