EPA/600/R-92/051
                                         March 1992
     OPERATIONS AND RESEARCH AT
THE U.S. EPA INCINERATION RESEARCH
 FACILITY:  ANNUAL REPORT FOR FY91
                        By
                    L. R. Waterland
                   Acurex Corporation
               Environmental Systems Division
               Incineration Research Facility
                Jefferson, Arkansas  72079
                 EPA Contract 68-C9-0038
             EPA Project Officer: R. C. Thurnau
   Waste Minimization, Destruction, and Disposal Research Division
            Risk Reduction Engineering Laboratory
                  Cincinnati, Ohio 45268
      RISK REDUCTION ENGINEERING LABORATORY
        OFFICE OF RESEARCH AND DEVELOPMENT
       U.S. ENVIRONMENTAL PROTECTION AGENCY
                CINCINNATI, OHIO 45268
                                           Printed on Recycled Paper

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                                      NOTICE
       The information in this document has been funded wholly or in part by the United
States Environmental Protection Agency under Contract 68-C9-0038 to Acurex Corporation. It
has been subjected to the Agency's peer and administrative review, and it has been approved for
publication as an EPA document. Mention of trade names or commercial products does not
constitute endorsement or recommendation for use.
                                         u

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                                    FOREWORD

       Today's rapidly developing and changing technologies and industrial products and
practices frequently carry with them the increased generation of materials that, if improperly
dealt with, can threaten both public health and the environment. The U.S. Environmental
Protection Agency is charged by Congress with protecting the Nation's land, air, and water
resources. Under a mandate of national environmental laws, the Agency strives to formulate
and implement actions leading to a compatible balance between human activities and the
ability of natural systems to support and nurture life. These laws direct the EPA to perform
research to define our environmental problems measure the  impacts, and search for solutions.

       The Risk Reduction Engineering Laboratory is responsible for planning, implementing,
and managing research, development, and demonstration programs to provide an authoritative,
defensible engineering basis in support of the policies, programs, and regulations of the EPA
with respect to drinking  water, wastewater, pesticides, toxic substances,  solid and hazardous
wastes, and Superfund-related activities.  This publication is one of the products of that
research and provides a vital communication link between the researcher and the user
community.

       This document reviews the accomplishments at the Incineration Research Facility
(IRF) in Jefferson, Arkansas, during Fiscal Year 1991.  In that twelve-month period,  five
major test programs were completed at the facility.  Three major EPA Program/Regional
Office programs were supported through test  activities:  the hazardous waste incinerator
regulation development program within the Office of Solid Waste (OSW); the land disposal
restriction regulation development program within OSW; and the Superfund site remediation
program within the Office of Emergency and Remedial Response (OERR) as administered by
EPA Regions 1, 2, and 3.  A sixth test program was done for Region 2, but was not  as
extensive in scope as the others.  The report outlines all efforts completed or ongoing at the
facility during FY91.

                                              E. Timothy Oppelt, Director
                                              Risk Reduction Engineering Laboratory
                                           m

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                                      ABSTRACT
        The U.S. Environmental Protection Agency's Incineration Research Facility (IRF) in
Jefferson, Arkansas, is an experimental facility that houses two pilot-scale incinerators and the
associated waste handling, emission control, process control, and safety equipment; as well as
onsite laboratory facilities.

        During fiscal year 1991, five major test programs were completed at the facility:  tests
to establish residue characteristics from the incineration of spent potliners from aluminum
production (K088) for the Office of Solid Waste (OSW); an evaluation of the incinerability of
five contaminated soils from the Drake Chemical Superfund site for Region 3; an evaluation of
the incinerability of PCB-contaminated marine sediments from the New Bedford Harbor
Superfund site for Region 1; a parametric evaluation of the fate of trace metals in a rotary kiln
incinerator equipped with a Calvert high-efficiency scrubber system; and an evaluation of the
incinerability of arsenic-contaminated soil from the Chemical Insecticide Corporation Superfund
site for Region 2.  A sixth test program consisted of an evaluation of the effectiveness of
low-temperature thermal  desorption in  decontaminating wastes  from the Caldwell Trucking
Superfund site for Region 2, but the program was not as extensive in scope as the others.  In
addition, the results of a test program completed in FY90, an evaluation of the thermal stability-
based principal organic hazardous constituent (POHC) incinerability ranking for the OSW, were
reported.  The report outlines  all efforts completed or ongoing at the  facility during FY91.
                                            IV

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                         TABLE OF CONTENTS
                                                                    Page

        FOREWORD,	   iii
        ABSTRACT	 ,	,...   jv
        FIGURES .;.''.	  viii
        TABLES				   ix

1       INTRODUCTION	  . .  .   1

2       PARAMETRIC TESTING TO EVALUATE THE PROPOSED POHC
        INCINERABILITY RANKING ....			..............   4

        2.1    TESTPROGRAM	 .r ..................   5

        2.1.1  Synthetic Waste Mixture		   5
        2.1.2  Test Conditions	   7
        2.1.3  Sampling and Analysis Procedures	   8

        2.2    TEST RESULTS		   10

        2.2.1  Test 1—Baseline Incineration Conditions  	   14
        2.2.2  Test 2—Thermal Failure (Quenching)	   14
        2.2.3  Test 3—Mixing Failure	   15
        2.2.4  Test 4—Matrix Failure	   15
        2.2.5  Test 5—Worst-Case Combination	,	   16

        2.3    CONCLUSIONS		  .   16

3       INCINERATION TESTS OF SPENT POTLINERS FROM THE PRIMARY
        REDUCTION OF ALUMINUM (K088)  	   18

        3.1    TEST PROGRAM	   18

        3.1.1  Test Conditions	   19
        3.1.2  Sampling and Analysis Procedures 	   21

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                        TABLE OF CONTENTS (continued)
Section
           3.2
                                                         Page

TEST RESULTS 	'	,	   24
           3.2.1  Proximate, Ultimate, and Silica Analysis Results	   24
           3.2.2  Cyanide and Semivolatile Organic Analysis Results 	   26
           3.2.3  Trace Metal Analysis Results 	   29
           3.2.4  Sulfide and Fluoride Analysis Results ,	   34
           3.2.5  Flue Gas Particulate and HC1 Emissions	   37
           3.3
CONCLUSIONS	   37
           INCINERATION OF CONTAMINATED SOILS FROM THE DRAKE
           CHEMICAL SUPERFUND SITE	   40
           4.1
TEST PROGRAM	   41
           4.1.1  Test Conditions	   42
           4.1.2  Sampling and Analysis Procedures	   44
           4.2
TEST RESULTS  	   46
           INCINERATION OF PCB-CONTAMINATED SEDIMENTS FROM THE
           NEW BEDFORD HARBOR SUPERFUND SITE	  	   49
           5.1
TEST PROGRAM	   50
           5.1.1  Test Conditions	   50
           5.1.2  Sampling and Analysis Procedures  	   51
           5.2
TEST RESULTS  	   54
           5.2.1   Proximate and Ultimate Analysis Results	   54
           5.2.2   PCB, Semivolatile and Volatile Organic, and Dioxin/Furan
                 Analysis Results  	   54
           5.2.3   Trace Metal Discharge Distributions	   58
           5.2.4   Particulate and HC1 Emissions Data	   63
           5.3
CONCLUSIONS	   65
                                      VI

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                     TABLE OF CONTENTS (continued)
Section

   6
   10

   11

   12
                                                        Page

FATE OF TRACE METALS IN THE ROTARY KILN SYSTEM WITH A
CALVERT FLUX/FORCE CONDENSATION SCRUBBER	  67
          6.1
      TEST PROGRAM .... . .... ...... ....	  69
          6.1.1   Synthetic Waste Mixture :...•. .'. ... ... . . . . . .rv . . :'.-v~ . .	  71
          6.1.2   Test Conditions ..;			  71
          6.1.3   Sampling and Analysis	  75

          6.2    TEST RESULTS  .			  77

          INCINERATION OF ARSENIC-CONTAMINATED SOILS FROM THE
          CHEMICAL INSECTICIDE CORPORATION SUPERFUND SITE

          7.1    TEST PROGRAM	
                                                          80

                                                          80
          7.1.1
          7.1.2
      Test Waste Description ........;. ...... ...	  81
      Test Conditions		  84
7.1.3   Sampling and Analysis			  84

7.2    TEST RESULTS  .. ^.. ^ ..:....:.......: i I/. .'....•	  86
                : ,    •            -       'w   '     ' '
FACILITY PHYSICAL PLANT IMPROVEMENTS	  87

8.1    OFFICE SPACE	 .  87
8.2    INCINERATION SYSTEM IMPROVEMENTS  	'.	  87
8.3    FLAMMABLE CHEMICAL STORAGE BUILDING	  88
8.4    BENCH-SCALE THERMAL TREATABILITY TEST UNIT	  88

HEALTH AND SAFETY, ENVIRONMENTAL COMPLIANCE, AND
PERMIT ADMINISTRATION	'.	 . . .	.	  92

9.1    TOXIC SUBSTANCE CONTROL ACT RESEARCH AND
      DEVELOPMENT PERMIT . .	 . . .		  92
9.2    RCRA FACILITY INVESTIGATION .........	.	  93

THIRD-PARTY TESTING		. .  		  94

EXTERNAL COMMUNICATIONS  	  95

PLANNED EFFORTS FOR FY92 .	   101

REFERENCES	   103
                                  Vll

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                                     FIGURES
Number




  1      Schematic of the IRF rotary kiln incineration system.



  2      Sampling matrix	




  3      Kiln exit POHC DREs for Test 1	




  4      Kiln exit POHC DREs for Test 2. ...	




  5      Kiln exit POHC DREs for Test 3	




  6      Kiln exit POHC DREs for Test 4.	




  7      Kiln exit POHC DREs for Test 5	




  8      Sampling matrix	




  9      Test sampling locations.	



  10      Sampling matrix.	




  11      Afterburner exit particle size distributions	




  12      Schematic of the Calvert Scrubber System	



  13      Test sampling locations	




  14      Sampling matrix	




  15      TTU: external configuration	




  16      TTU: internal configuration	
Page




.   6




.   9




  11



  11




  12




  12




  13




  22




  47



  53




  65




  70




  76




  85




  90



  91
                                       vui

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                                       TABLES






Number



  1       Synthetic waste mixture composition .....'	•	   7




  2       Target test conditions	•	   8




  3       Target test conditions	,	,	   20



  4       Actual versus target operating conditions for the K088 Tests  . . .	   20




  5       Waste feed and ash collected  	• • •  •	> •.	•	   21



  6       Trace metals determined	24




  7       Proximate and silica analysis results	   25



  8       Test program composite proximate component distributions	   25




  9       Cyanide analysis results	   27




  10      Test program composite cyanide distributions	   28




  11      Cyanide DREs  		.	. .. . :	• •	• • •	   28



  12      BDAT trace metal analysis results	   30



  13      Nonhazardous constituent metal analysis results	   32




  14      Test program composite BDAT trace metal distributions	   35




  15      Test program composite nonhazardous constituent metal distributions	   35




  16      Sulfide and fluoride analysis results for waste feed and kiln ash samples	   36




  17      Test program sulfide and fluoride distributions	   38




  18      Flue gas particulate levels	   38




  19      Stack gas HC1 emissions	   38




  20      Target test conditions	   43



  21      Target versus actual operating  conditions for the Drake chemical soil tests  . .   45
                                           IX

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                                 TABLES (continued)


Number                                                                          page

  22     Soil feed and ash collected  	.......=..	   45

  23     Incinerator system operating conditions held constant......;	;.   50

  24     Actual versus target operating conditions for the New Bedford Harbor tests  .   52

  25     Proximate and ultimate analysis results for the composite sediment feed
         sample	   55

  26     Sediment feed and ash collected	         55

  27     PCB analysis results  	   56

  28     PCB decontamination effectiveness	   57

  29     PCB DREs	    58

  30     Flue gas PCDD/PCDF analysis results	    59

  31     Trace metals analysis results	    60

  32     Normalized trace metal distributions	    62

  33     Apparent scrubber collection efficiencies	    64

  34     Flue gas particulate levels	    64

  35     Flue gas HC1 levels	    64

  36     Test organic liquid mixture compositions  	   72

  37     Metal spike concentrations	   73

  38     Target test conditions	   74

 39      Test conditions held constant 	   75

 40      Actual versus target operating conditions for the calvert scrubber trace
         metal tests	   73

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                                 TABLES (continued)






Number                                                                         Page




  41     Synthetic waste fed and ash collected  	   79




  42     Soil characterization sample analysis results  	   82




  43     Soil characterization sample TCLP leachate analysis results	   83




  44     IRF program reports and presentations in FY91 .  .	 . . . .	   96




  45     Visitors to the IRF	   98
                                          XI

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                                      SECTION 1

                                   INTRODUCTION
        The U.S. Environmental Protection Agency's (EPA) Incineration  Research Facility
(IRF) in Jefferson, Arkansas, is an experimental facility that currently houses two pilot-scale
incinerators (a rotary kiln incineration system and a k'quid injection incineration system) and
their associated waste handling, emission control, process control, and safety equipment. The
IRF also has onsite laboratory facilities for waste characterization  and analysis of process
performance samples.

        The objectives of research projects conducted at the IRF have been and continue to be
as follows:

        •    To develop technical information on the performance capability of the hazardous
             waste incineration process to assist EPA Regional Offices and state environmental
             agencies in the review,  assessment,  and issuance of reasonable and responsible
             permits for regulated hazardous waste incineration facilities, and to assist waste
             generators and incinerator operators in the preparation  of permit applications

        •    To develop incinerator system performance data for regulated hazardous wastes
             to support current Resource Conservation and Recovery Act (RCRA) incinerator
             regulations and performance standards, and to provide a sound technical basis for
             any necessary future standards

        •    To promote an understanding of the hazardous waste incineration process and
             develop methods to predict the performance of incinerators of varying scale and
             design for the major classes of incinerable hazardous wastes as a function of key
             process operating variables

         •    To develop  methods of improving reliability and  control of  the incineration
             process, including the use of destruction and removal efficiency (DRE) surrogates

         •    To provide a means of conducting specialized test burns (particularly for high
             hazard or special waste materials such as Superfund site  wastes)  iri support of
             specific Regional Office permitting or enforcement actions and Regional Office
             or private party Superfund site remediation efforts

         •    To test the performance of new  and advanced  incinerator components and
             subsystems, and emission control devices

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         Fiscal year 1991 (FY91, October 1,  1990 through September 30, 1991) saw the return
 of production-paced incineration testing to the IRF after the final completion of a major facility
 ejqpansion and reconfiguration construction effort begun in FY89. Beginning in December 1990
 and continuing through August 1991, incineration testing proceeded virtually uninterrupted.
 Over this time period, five test programs were completed. These test programs focused on the
 objectives above.

         Three major EPA Program/Regional Office programs were supported  through test
 activities in FY91.

         •    The hazardous waste incinerator regulation  development program within  the
              Office of Solid Waste (OSW), via testing to evaluate the fate of trace metals fed.
              to a rotary kiln incinerator  equipped with a Calvert Flux Force/Condensation
              Scrubber system

         •    The land disposal restriction regulation development program within OSW, via
              incineration testing  of  spent  potliner waste  from the primary reduction  of
              aluminum (listed waste K088) to develop treatment residuals characteristics

         •    The Superfund site remediation program within the Office  of Emergency and
              Remedial Response (OERR) as administered by

              —    EPA Region 3, via incineration treatability testing of contaminated soil from
                   the Drake Chemical Superfund site in Lock Haven, Pennsylvania

              —    EPA Region 1, via incineration  treatability  testing of PCB-contaminated
                   sediments from the New Bedford Harbor Superfund site in New Bedford,
                   Massachusetts

              —    EPA Region 2, via incineration treatability testing of arsenic-contaminated
                   soil from the Chemical Insecticide Corporation Superfund site in Edison,
                   New Jersey

In addition, the results of a series of tests to evaluate the principal organic hazardous constituent
(POHC) thermal-stability-based incinerability ranking, completed in support of OSW in FY90,
were assembled and reported in FY91.  Also, the test planning documents (test plan and quality
assurance project plan [QAPjP]) for two additional Superfund site contaminated soil treatability
tests in support of Regions 2 and 5 were completed.

        Activities completed during FY91 are discussed in more detail in the following sections.
Section 2 presents the results of the POHC incinerability ranking evaluation tests. Section 3
presents results of the K088 incineration residuals characterization tests. Section 4 discusses
results of the Drake Chemical Superfund site treatability tests. Section 5 presents results of the
New Bedford Harbor Superfund site treatability tests.  Section 6 discusses the Calvert scrubber
trace metal tests. Section 7 discusses the Chemical Insecticide Corporation (CIC) Superfund site
treatability tests.  Section 8 describes various facility improvement and capability enhancement
activities completed during FY91.  Section  9  discusses environmental compliance  and permit
administration activities.  Section 10 outlines  third-party test solicitation efforts.  Section  11

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discusses  external communication  activities associated with  the  facility and its operation.
Section 12, the final section, presents an outline of plans for activities to be completed in FY92.

        In addition, FY91 saw the completion of a brief series of scoping tests for EPA Region 2
to evaluate low-temperature thermal desorption as a treatment approach for contaminated soil
from the Caldwell Trucking Superfund site in Fairfield, New Jersey.  Results from these tests are
not discussed in this report. Because this series of .tests was scoping in nature and performed
only to supply qualitative data to Region 2, no formal test report was prepared.

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                                      SECTION 2

                         PARAMETRIC TESTING TO EVALUATE
                  THE PROPOSED POHC INCINERABILITY RANKING
         One of the primary functions of the IRF is to conduct research activities for OSW in
 support of regulation development and implementation.  One major regulatory issue of high
 priority during 1990 concerned the evaluation of an incinerability ranking system for POHCs.
 Such a system was developed over the past several years by the University of Dayton Research
 Institute (UDRI) under contract to EPA's Risk Reduction Engineering Laboratory (RREL).

         The 1981 hazardous waste incinerator regulations require that an incinerator undergo
 a trial burn  performance test in order to become permitted to operate.  This trial burn is
 required to show that the incinerator is capable of achieving the mandated 99.99 percent POHC
 ORE-  In trial burn planning, the incinerator operator is required to select POHCs using two
 criteria: concentration in the waste and difficulty to thermally destroy, or "incinerability." The
 incinerability ranking  included in the  1981 regulations was  based on compound  heat of
 combustion.

        The  heat of combustion ranking has several acknowledged deficiencies, however. Thus,
 EPA initiated studies to define  or develop alternate, more  suitable incinerability ranking
 approaches.  One such approach is the thermal-stability-based POHC ranking, developed by
 UDRI. This  ranking is based on the temperature required to achieve 99 percent destruction at
 2 s residence time under oxygen-starved conditions as measured in laboratory experiments.  As
 of early 1990, the fundamental basis supporting the ranking approach had been documented and
 sufficient information to rank the organic hazardous constituents had been collected.  Since it
 is based only on laboratory-scale data, evaluation of the thermal stability POHC incinerability
 ranking under actual incineration conditions became a high-priority research need during 1990.

        The test program described in this section was designed to develop the data to evaluate
 the POHC incinerability ranking at the pilot scale.  The specific objective of the test program
 was to measure the ORE of a number of POHCs under each of several  modes of incinerator
 operation, and compare relative POHC DREs as a function of incineration conditions and feed
 characteristics. The comparison would facilitate a determination of how relative POHC DREs
 compared with expectations based on the thermal stability ranking.

        In the tests, a mixture of 12 POHCs with predicted incinerabilities spanning the range
from the most-difficult-to-incinerate class to the least-difficult-to-incinerate class was tested. This
"POHC soup" mixture was combined with a clay-based sorbent solid matrix and packaged into
fiberpack drums for incineration testing in the rotary kiln incineration system (RKS) at the IRF.

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The drums containing the soup/clay mixture were batch fed to the RKS via a fiberpack drum
ram feeder.

        A series of five incineration tests was performed during which incinerator operating
conditions and test mixture composition were varied.  Specific test program variables were:

        •    Kiln temperature

        •    Feed batch charge mass

        •    Feed composition, specifically H/C1 ratio

One test was performed under typical operating conditions with a baseline mixture composition.
The other tests varied the above in an attempt to simulate various modes of incineration failure:
thermal failure, mixing failure, feed matrix effects, and a worst-case combination of these.

2.1     TEST PROGRAM

        The IRF's RKS was used  for this test program.  A process schematic of the RKS is
shown in Figure 1.  The IRF RKS  consists of a primary combustion chamber, a transition
section, and a fired afterburner chamber. After exiting the afterburner, flue gas flows through
a quench section followed by a primary air pollution control system (APCS). The primary APCS
for  these  tests consisted of a venturi scrubber followed  by  a packed-column scrubber.
Downstream of the  primary APCS,  a backup secondary APCS, comprised of a demister, an
activated-carbon adsorber, and a high-efficiency particulate (HEPA) filter, is in place.

2.1.1   Synthetic Waste Mixture

        Twelve POHCs were selected for inclusion in the synthetic waste mixture employed in
 the test program. The incinerabiHty ranking groups 333 POHCs into 7 stability classes from most
 stable (class 1) to least stable (class 7). UDRI recommended that two compounds from each
 class be included in the test mixture and provided a list of candidates for selection. The selection
 of compounds from this candidate list was guided by  sampling.and analysis, compound
 compatibility, compound availability, and safety considerations.

        The compounds selected for the test mixture  are listed in Table 1.  The table also notes
 the composition of two test mixtures containing the POHCs.  Test mixture 1 was the baseline
 test mixture.  The POHC concentrations in  test mixture 2 represent adjustments to relative
 POHC concentrations to yield a mixture with decreased H/C1 ratio.

        The mixtures incinerated in the test program were prepared using commercially-available
 pure chemicals and materials. Test material formulation consisted of adding weighed quantities
 (1.3 kg, 3 Ib total) of the mixture of the twelve organic constituents to a weighed quantity (2.3 kg,
 5 Ib) of an absorbent clay.  The clay/organic mixtures were packaged into 1.5-gal fiberpack
 drums lined with polypropylene bags, the mouths of which were closed with wire ties.

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              TABLE 1.  SYNTHETIC WASTE MIXTURE COMPOSITION
Concentration (wt %)
Mixture 1 Mixture 2
Component high H/C1 low H/C1
Benzene
Chlorobenzene
Tetrachloroethene
1,2,2-Trichloro-
1,1,2-trifluoroethane
(Freon 113)
Benzenethiol
Nitrobenzene
Hexachlorocyclohexane
(Lindane)
Hexachloroethane
1,1,1-Trichloroethane
p-Dimethylaminoazobenzene
(methyl yellow)
Nicotine
N-nitroso-di-n-butyl amine
H/C1 (molar)
8
8
8
8
8
8
10
10
10
10
10
2
3.6
4
4
33
4
4
4
5
25
5
5
5
2
1.2
T99(2), "C"
1,150
990
890
780
725
655
645
585
545
-400
<320
<320

Stability
Rankb class
3
22
43
92
122
150/151
159
213
233
268
286 to 289
316 to 331

1
1
2
3
3
4
4
5
5
6
7
7

    "Temperature required to achieve 99 percent destruction in 2 s.
    blncinerability rank in list range from most refractory (No. 1) to most labile
     (No. 333).
2.12    Test Conditions

        The variables for the test program were the H/C1 ratio in the synthetic waste feed, kiln
temperature, and synthetic waste feed charge mass. Five tests, specified to be conducted with
various combinations of these parameters, were selected to evaluate the relative incinerability
of the POHCs.  The target test matrix is shown in Table 2.  Test  1  represented a baseline, or
normal, set of incinerator operating conditions.  Test 2 attempted thermal failure by decreasing
the kiln exit temperature to a target of 649° C (1,200°F). To further promote thermal.failure,
0.9 kg (2 lb) of water was added to each waste feed charge for Test 2.  In Test 3, mixing failure
was attempted by doubling the drum charge mass from 3.6 to 7.3 kg  (8 to 16 lb).  This doubled
charge mass was introduced at half the baseline frequency, so as to  maintain the overall waste
feedrate equal to that for the other test conditions. Test 4 was designed to investigate the effects
of reducing the H/C1 ratio (matrix failure) in the waste feed.  Test 5 combined the three failure-
promoting conditions to  produce  a "worst-case" condition by operating with the  kiln  exit
temperature at a target of 649° C (1,200° F), introducing the waste at  double the baseline charge
mass, and by using a low H/C1 ratio waste mixture.

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                        TABLE 2.  TARGET TEST CONDITIONS


Test
1
2
3
4
5


Klin H/CI,
molar
22.8
22.8
22.8
15.7
10.3

Kiln exit

Kiln
Afterburner
exit
temperature, exit O2, temperature,
°C(°F) % °C(°F)
871 (1,600)
649 (1,200)
871 (1,600)
871 (1,600)
649 (1,200)
10.4
12.6
10.4
10.4
13.2
982 (1,800)
982 (1,800)
982 (1,800)
982 (1,800)
982 (1,800)

Afterburner
exit O2,
%
9.0
9.1
9.0
9.2
9.2

Organic/clay
per fiberpack,
kg(lb)
3.6 (8)
4.5 (10)"
3.6 (8)
3.6 (8)
3.6 (8)
Feed
regimen
drums/
charge
1
1
2
1
2


Charge/
hr
12
12
6
12
6
 "0.9 kg (2 Ib) water added per fiberpack.
        For all tests, the average kiln exit temperatures were within  14° C (26° F) of the
respective target temperatures. However, actual O2 levels in the kiln exit flue gas were generally
higher than the target concentrations.  The higher O2 levels were generally the result of higher
than expected air in-leakage into the kiln chamber.

2.13    Sampling and Analysis Procedures

        The scope of the sampling effort undertaken during this test program is illustrated in
Figure 2, in which the sampling locations and the corresponding sample collection methods are
identified.  Specifically, the sampling effort during each test consisted of:

        •    Obtaining a sample of the POHC/clay feed mixture by compositing the contents
             of three waste fiberpack drums randomly selected during the test

        •    Obtaining a sample  of  the scrubber  blowdown liquor composited from  grab
             samples taken  at hourly intervals over the test period

        •    Obtaining a composite sample of the kiln  ash from the ash collection bin at the
             end of the test

        •    Continuously measuring O2, CO, CO2, and unheated total unburned hydrocarbon
             (TUHC) concentrations in the flue gas at  the kiln exit; O2 concentrations at the
             afterburner exit; O2, NOX, unheated TUHC, and heated TUHC concentrations at
             the scrubber exit; and O2, CO, CO2, and heated TUHC concentrations in the stack

        •   Sampling flue gas at the kiln exit, scrubber exit, and stack for the semivolatile and
            volatile POHCs using Method 0010  and Method 0030,  respectively

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         The laboratory analysis procedures used to characterize the samples collected over the
 test program included:

         •    Analyzing the composite feed, kiln ash, and scrubber blowdown samples from each
              test for volatile and semivolatile organic constituents

         •    Analyzing Method 0010 train samples from each test for semivolatile organic
              hazardous constituents

         •    Analyzing Method  0030 train  samples from each  test for volatile organic
              hazardous constituents

         Semivolatile organic analyses were performed by Method 8270. Solid samples, including
 waste feed and kiln ash, and Method 0010 samples were Soxhlet-extracted  by Method 3540 in
 preparation  for  analysis.   Liquid  samples  were liquid-liquid extracted  by Method 3510.
 Method 0030 (VOST) sample  analysis was by thermal desorption  purge and trap GC/MS
 (Method 5040) analysis with ah ion trap detector.

 22      TEST RESULTS

         The POHC measurements at the kiln  exit are the most  relevant with respect  to
 evaluating the incinerability ranking in that the incineration failure conditions tested involved
 varying kiln operation.  Thus, incineration failures achieved would be most evident and best
 measured at the kiln exit.

         Figures 3 through 7 show kiln exit POHC DREs  measured in bar chart form.  The
 POHCs are ordered along the horizontal axis by their thermal stability index ranking from
 predicted most stable (benzene) to least stable (N-nitroso-di-n-butyl amine). The vertical axis
 is the quantity [-log (l-DRE/100)]  for each POHC, which represents the  "number of 9's"  of
 POHC  destruction.  A value of 1 signifies 90 percent DRE, a value of 2 signifies 99 percent
 DRE, and so on.  Each bar represents the measured DRE for the corresponding POHC. Where
 flue gas analysis indicated that the particular POHC was below its detection limit, a stacked bar
 format is used to  convey this information. The height of the bottom bar of the stack represents
 the DRE calculated using the practical quantitation limit (PQL).  The combined stacked bar is
 extended to the top  of the chart (six "9's" DRE) as a visual reminder that the POHC was not
 detected and that the measured DRE was greater than that computed using the PQL.

        The bar graphs shown in Figures 3 through 7 show DREs based on the feed formulation
 data.  As noted in Section 2.1.3, feed samples were collected and analyzed for  the POHCs. Thus,
 DREs could be calculated based on feed POHC analysis results.  However, analyzed POHC
 concentrations in  feed samples were substantially lower  than the  concentrations corresponding
 to the POHC quantity used to  form the POHC mixtures.  On average, only between 12 and
 29 percent of the volatile organic constituents and between 27 and 82 percent of the semivolatile
 organic constituents in the prepared mixtures could be accounted  for in the feed analyses. One
 POHC,  nicotine, was not detected in the Test 3 feed.  Fiberpack weights measured during the
 tests rule out mass evaporative loss as the explanation  for differences between prepared and
 analyzed concentrations.  Thus, it is believed that what was prepared indeed was fed.  One
possible explanation is that the organic liquid constituents were so tightly adsorbed to the porous

                                          10

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    5 -
uJ
cc
9
3 -
    2 -
    1  -
                            4455
                              STABILITY CLASS
           DENOTES POHC NOT DETECTED
               Figure 3.  Kiln exit POHC DREs for Test 1.
o
o
s
tr
    5 -
    4 -
    3 -
              1     234455
                              STABILITY CLASS
            DENOTES POHC NOT DETECTED
               Figure 4. Kiln exit POHC DREs for Test 2.
                                 11

-------
ft
DC

-------
                      1     234455
                                        STABILITY CLASS
                   DENOTES POHC NOT DETECTED
                       Figure 7.  Kiln exit POHC DREs for Test 5.
clay that the sample preparation procedures associated with Methods 8240 and 8270 analyses
could not quantitatively free the organic constituents for detection in the analyses.  The validity
of this hypothesis was not examined, however. Nevertheless, test conclusions were supported by
DRE calculations  using  both the prepared  formulation and test  feed sample analysis
concentrations.  For clarity, only the feed formulation  evaluations are shown in Figures 3
through 7, and discussed in the following.

        In addition, Table 1 noted that benzenethiol was selected as one of the class 3 POHCs
in the POHC mixture.  However, while performing tests to verify that stable  synthetic waste
organic feed mixtures could be prepared, it was discovered that benzenethiol quite rapidly and
completely reacts,  in the presence of the other organics and the clay matrix, to form diphenyl
disulfide, a class 6 compound.  As a result, diphenyl disulfide, not benzenethiol, was actually fed
to  the  incinerator.   Thus,  the  DRE  for diphenyl disulfide is  shown in  the  Figure 3
through Figure 7 bar charts, and its bar location corresponds to its class 6 incinerability order.
        The following discusses relative POHC DREs measured for each test in turn.
                                           13

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 2.2.1    Test 1—Baseline Incineration Conditions

         The incinerator operating conditions for Test 1 represented baseline  incineration
 operation, which, from past experience would result in acceptable POHC destruction. As shown
 in Figures, kiln  exit DREs were 99.99 percent or greater for all  POHCs.   Benzene,
 chlorobenzene, tetrachloroethene, Freon  113 and  1,1,1-trichloroethane  were quantitatively
 measured at the kiln exit and their corresponding DREs are shown by the single bars.  The
 remaining POHCs were not detected at the kiln exit and their respective DREs are represented
 by the two-segment stacked bars, the significance of which was discussed above.

         The high POHC DREs confirmed that this baseline incinerator operating condition was
 indeed capable of satisfactorily destroying even the predicted most difficult to incinerate POHC,
 benzene. A weak correlation might exist between DRE and the POHC incinerability ranking'
 in that,  except for 1,1,1-trichloroethane which had a DRE of about 99.99 percent, DREs for
 POHCs ranked in  class 4 and above were higher  than the class 3 and below POHCs. It bears
 emphasis, however, that  the measured POHC DREs  only varied by a small degree (from
 99.994 percent to 99.9997+ percent). This, coupled with the lack of gross incineration failure
 to broaden the incinerability response, could explain the inability to establish a clear correlation
 between DRE and the incinerability ranking index from the baseline test data.

         It is interesting to note that  1,1,1-trichloroethane,  a POHC  ranked in class 5  and
 believed to be relatively  easy to  incinerate, had a measured DRE substantially lower than
 similarly ranked POHCs.  One possible explanation is that 1,1,1-trichloroethane is a common
 product  of incomplete combustion (PIC), and can be formed during the incineration process,
 most directly from  hexachloroethane, another component of the POHC mixture.

 222    Test 2—Thermal Failure (Quenching)

         Test 2 was  intended to simulate a thermal failure condition through incineration quench.
 This was accomplished by lowering the kiln temperature from nominally 871° C (1,600° F) to
 649° C (1,200° F) via two means. A measured amount of water contained in a polyethylene bag
 was added to each waste feed fiberpack drum and the kiln was fired at very high air/fuel ratio.
 These two actions  in combination would be expected to create conditions conducive to the
 formation of cold POHC-containing pockets of gas which would escape the kiln prior to being
 destroyed.

        Figure 4 presents the kiln exit POHC DREs for this test. The data clearly indicate that
 this test condition resulted in significantly different POHC DREs compared to the baseline test.
A wide range of POHC DREs was observed, from less than 99 percent for Freon 113 to greater
than about 99.999 percent for diphenyl disulfide, methyl yellow, nicotine, and N-nitroso-di-n-butyl
amine. The low DREs for several POHCs confirmed that incineration failure did occur during
this test.

        With the exception of a few anomalies (discussed below), a general correlation between
DRE and incinerability ranking seems apparent for this test. The observed DREs for the class 3
to 7 POHCs appeared to follow the incinerability ranking predicted behavior. Some POHC-to-
POHC variability existed within this sub-group of POHCs.  Lindane exhibited a higher DRE than
the neighboring ranked POHCs.
                                          14

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        A considerably more significant  deviation from incinerability ranking expectation
involved the DREs of the four most-stable ranked POHCs within classes 1,2 and 3. The relative
DREs measured for these four POHCs were in an order opposite to the ranking predictions.
The relative extent of incineration failure  for these four POHCs was not in accordance with
expectations from the thermal stability ranking.

223    Test 3—Mixing Failure

        One of the modes by which POHCs can escape an incinerator undestroyed results from
the lack of adequate mixing between POHC and oxidizer.  For Test 3, the weight of each waste
charge  to the kiln was doubled, while the hourly waste feedrate was  maintained at a level
consistent with the other four tests.  The doubled waste charge was thought to increase the
likelihood of creating oxygen-deficient pockets of POHCs in the kiln chamber. The expectation
was that if the oxygen-deficient conditions persisted through the kiln, undestroyed POHCs could
escape the kiln chamber.

        However,  as the data in Figure 5 show, no clear failure was apparent during this test.
All POHC DREs were greater than 99.99 percent and exhibited trends similar to those observed
for the baseline condition test (Test 1). DREs for nitrobenzene and the group of POHCs ranked
easier to incinerate were high. Within this  group, only 1,1,1-trichloroethane was detected in the
kiln exit flue gas sample at a level above its  PQL. The other less-stable ranked POHCs were not
detected in the kiln exit flue gas.

        The four most difficult to incinerate POHCs, benzene, chlorobenzene, tetrachloroethene
and Freon 113 were present in the kiln exit flue gas sample at levels  corresponding to between
99.99 and 99.999 percent DRE.

        No correlation between POHC DREs and POHC incinerability ranking was apparent
for this test.  DREs for the volatile POHCs (detected in the flue gas) were  comparable to the
DREs associated with  the PQLs for the semivolatile POHCs (not detected in the flue gas).

2.2.4   Test 4—Matrix Failure

        This test (Test 4) attempted to cause incineration failure by decreasing the H/C1 ratio
in the organic feed to the kiln. The H/C1 ratio in the feed waste for Test 4 was 1.2, as compared
to a H/C1 ratio of 3.6  for the baseline Test 1.

        The kiln exit POHC DREs for this test are shown in Figure 6. These were uniformly
high: all  exceeded 99.99  percent.  As  in Test 3, no correlation between  POHC DRE and
incinerability ranking was apparent because the POHC DREs were uniformly, high.

        One possible explanation for the inability to achieve POHC DRE failure in this test is
 that the actual H/C1 ratio in the kiln environment as a whole was quite different from  that in
 the waste feed itself.  This was so because the auxiliary fuel for the burner, in this case natural
 gas, was a significant additional source of hydrogen. If this source of hydrogen is included, the
 H/C1 ratio in the total kiln environment for this test would be 15.7, which may be considerably
 higher than the H/C1 ratio required to cause DRE failure.
                                           15

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 2.2.5    Test 5—Worst-Case Combination

         This last test was conducted to present the most  challenging combination of the
 mechanisms tested in terms of POHC destruction failure.  The kiln was operated at the reduced
 temperature of 640° C (1,184°F) to induce thermal failure;  the  waste  feed charge size was
 doubled to promote mixing failure; and the chlorine content in the feed waste was elevated to
 promote matrix failure. It should be noted that, in a departure from Test 2 procedures, no water
 was added to the feed waste fiber drums, because  doing so would introduce  a quantity of
 hydrogen that might nullify any potential elevated chlorine (matrix failure) effect.

         Figure 7 shows the POHC DREs for this test condition.  In this test, eight of the twelve
 POHCs were detected in the kiln exit flue gas.  This was in contrast to only five POHCs being
 found at concentrations above their PQLs during baseline Test 1.  The four predicted most easily
 incinerated POHCs, namely, diphenyl disulfide, methyl yellow, nicotine, and N-nitroso-di-n-butyl
 amine were not found above their PQLs.  Assuming that these POHCs  were present at their
 respective PQLs would lead to computed POHC DREs greater than 99.998 percent for these
 four POHCs. These DREs, being higher than those measured for the remaining POHCs, were
 consistent with their incinerability ranking indices.

        The DREs for the eight quantifiable POHCs ranged from over 99 to almost 99.999
 percent. Lindane had the highest DRE at 99.9989 percent. Freon 113 and 1,1,1-trichloroethane
 exhibited the lowest DRE at about 99.8 percent.  While no monotonic correlation between
 POHC DREs and incinerability ranking order existed for this test, a weak relationship may have
 existed for the class 3 through class 7 POHCs.  As observed in Test 1, 1,1,1-trichloroethane
 exhibited a DRE significantly below that of its neighboring ranked POHCs.

        It is interesting to note  how well the relative POHC DREs  of this "worst-case" test
 compared to those observed for Test 2.  Recall that Test 2 simulated only quench failure.  The
 relative DREs for these two tests exhibited quite similar patterns although two differences could
 be noted. One difference is the absolute DRE levels, which for this test were generally higher
 than those observed for Test 2. The other difference relates to the DREs for benzene and 1,1,1-
 trichloroethane. The DREs for benzene and 1,1,1-trichloroethane were nearly two "9's" higher
 for Test 2 than for Test 5.

23     CONCLUSIONS

        Conclusions from the tests include the following:

        •    The baseline operation condition  resulted in effective POHC destruction.  Kiln
             exit POHC DREs were in the 99.99 percent range for the volatile POHCs in the
             test mixture. Semivolatile POHCs were not  detected in the kiln exit flue gas;
             corresponding lower bound DREs were generally greater than 99.999 percent.

        «    Neither the mixing failure nor matrix failure attempts resulted in incineration
             failure.   Kiln exit  POHC DREs  were comparable  to  those measured  in  the
             baseline test for all POHCs.
                                          16

-------
        •    The thermal failure and worst-case tests resulted in kiln POHC destruction failure.
             For both tests, kiln exit POHC DRE ranged from 99 percent or less for Freon 113
             to greater than 99.999 percent for the highest ranked (least stable) semivolatile
             POHCs.
                                                           ?•"       -   ; -  .
        •    For the incineration failure tests, there was general agreement between observed
             relative kiln exit  POHC  DRE  and thermal  stability  incinerability ranking
             expectations. However, two deviations occurred for both  tests.

             •—   The  class 1 compounds  (benzene  and chlorobenzene)  and  the class 2
                  compound (tetrachloroethene) were less stable (had greater kiln exit DRE)
                  than the class 3 compound Freon 113.

             —   1,1,1-trichloroethane was apparently more stable in the baseline and worst-
                  case tests than its class 5 ranking would suggest, when compared to the other
                  class 5 and the class 4 compounds; production of 1,1,1-trichloroethane as a
                  PIC could account for this observation.

        Test results were documented in  the test report:

        •    Lee, J. W., W. E. Whitworth, and L. R. Waterland, "Pilot-Scale Evaluation of the
          *  Thermal Stability POHC Incinerability Ranking," draft June 1991.

Test results were also presented in a poster presentation:

        •    Carroll, G. J., "Pilot-Scale  Evaluation of an Incinerability Ranking System for
             Hazardous Organic Compounds," presented at the 17th Annual Hazardous Waste
             Research Symposium, Cincinnati, Ohio, April 1991

and in a technical paper:

        •    Lee, J. W., L. R. Waterland, and G. J. Carroll,  "Evaluation of the Thermal
             Stability POHC Incinerability Ranking in a Pilot-Scale Rotary Kiln Incinerator,"
             paper  91-343, presented at the 84th Annual  Meeting  of the Air  & Waste
             Management Association, Vancouver, British Columbia, June 1991.
                                           17

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                                      SECTION 3

                    INCINERATION TESTS OF SPENT POTLINERS
               FROM THE PRIMARY REDUCTION OF ALUMINUM (K088)
        OSW is under Congressional mandate to ban the landfill disposal of specific, listed
 hazardous wastes that can be treated to reduce their volume and/or hazardous characteristics.
 Because incineration is an appropriate treatment technology for  many such wastes, OSW
 (J. Labiosa, L. Rosengrant, coordinators) has requested that the incinerability of these wastes
 be evaluated, and the  characteristics of  the  incineration  residues be  determined.   The
 incineration residues of interest are the kiln bottom ash and the scrubber system blowdown
 discharge.

        This test  program  at  the  IRF evaluated the incinerability and characterized  the
 incineration residuals of spent potUners from the primary reduction of aluminum, listed waste
 K088. Specific objectives of the test program were to:

        •    Determine whether incineration of K088 can be accomplished while complying
             with the hazardous waste incinerator regulations

        •    Characterize the waste  feed and  incineration  residuals in terms of their
             concentrations of the hazardous constituents found  on the best demonstrated
             available technology (BDAT) list

The incineration tests were completed on January 15, 16, and  17, 1991.  Results  of the test
program are discussed in this section.
3.1
TEST PROGRAM
        In the electrolytic reduction process for the production of aluminum, alumina (A12O3)
contained in bauxite ore is dissolved in molten cryolite (3NaF • A1F3).  An electric current is
passed through this molten bath, reducing the alumina to aluminum and evolving oxygen (O2).
The electrodes for passing the current are carbon. Thus, the electrolytic cells are large carbon-
lined steel boxes, the carbon lining being the cathode, with carbon anodes suspended in  the bath.
The O2 released in the reduction combines with the carbon at the electrodes to form CO2. Thus,
the ^electrodes (the cathode potliner and the anodes) are consumed during the process and are
periodically replaced (the anodes much more frequently than the cathode potliner).  The spent
cathode potliner comprises the subject waste for these tests.
                                          18

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        This potliner waste consists of the remaining carbon cathode being replaced, along with
residual ore and cryolite material left in the cell when the spent potliner is removed.  Thus, its
major constituents are carbon, aluminum, alumina, silicon and iron oxides (from the bauxite ore),
and sodium and aluminum fluoride (from the cryolite). In addition, other ore and steel cell
elements, including trace quantities of several hazardous constituent trace metals, are present.
The potential presence of high cyanide levels is the basis for listing this waste as toxic.  Thus, for
these tests, cyanide was considered the POHC requiring 99.99 percent DRE in the incineration
treatment of the waste.

3.1.1    Test Conditions

        The tests for this test program were performed in the RKS at the IRF. Like the POHC
incinerability ranking tests, the waste was packaged into 1.5-gal fiberpack drums and fed to the
kiln via the fiberpack drum ram feed system. For these tests, each fiberpack contained nominally
5.7 kg (12.5 Ib) of waste.  The single-stage ionizing wet scrubber system shown in Figure 1 was
used in place of the venturi/packed-column scrubber system for the K088 tests. Three tests were
conducted, each under the same set of incinerator operating conditions.

        The planned incinerator operating conditions for each test are summarized in Table 3.
These conditions were chosen to maximize the opportunity for waste carbon burnout. However,
past experience with K088 has shown that the waste can  agglomerate and form slag at
temperatures in the range of the target kiln temperature for these tests shown in Table 3.  Slag
formation was to be avoided as an operational consideration for these tests.

        Table 4 summarizes the actual incinerator exit  temperatures  and flue gas  levels,
including their ranges and averages for each test during flue gas sampling.  These are compared
with the respective target conditions.  The average kiln exit temperature for Test 1 was observed
at 17° C (30° F) higher than target and allowed because there was no evidence of slagging.  The
average kiln exit temperature for Test 2 was within 2°C (3°F) of target temperature.  The kiln
exit temperatures for Test 3 were held to an average of 11° C (19° F) below target because there
was evidence of slagging at target conditions.  The average afterburner exit temperatures were
within 3°C (5°F) of the target temperatures for all tests. The average kiln O2 levels were within
1.6 percent of the target O2 levels for all tests.  The afterburner exit O2 levels were somewhat
higher than targeted levels, although average afterburner exit O2 levels were within 2.6 percent
of target O2 levels.

        Table 5 summarizes the total amount of waste fed to the RKS during each test, and the
cumulative amount of kiln ash discharged over each test's duration.  As shown in the upper
portion of Table 5, the amount of ash discharged from the kiln varied from  60 percent of the
amount  of waste fed during Test 1 to 48 percent for Test 3.  During  Test 1, there was no
evidence of waste slagging. During Test 2, there was some visual evidence of waste slagging late
in the test. The waste fed for Test 2 was of slightly smaller average size than for Test 1. In
Test 3, which fed a waste of even smaller average size, there was evidence of slagging essentially
throughout the test.  The relative amounts of ash collected as a fraction of the waste weight fed
in each test agrees with the relative degree of slagging observed. The largest  amount of ash, as
a fraction of waste weight fed, was discharged in Test 1 with no observed slag formation.  The
least amount of ash was discharged in Test 3, with observed slagging throughout the test.
                                           19

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                      TABLE 3. TARGET TEST CONDITIONS
                 Total waste feedrate
                 Kiln temperature
                 Kiln exit flue gas O2
                 Afterburner  temperature
                 Afterburner  exit flue gas O2
                 Scrubber blowdown flowrate   0 L/min (total recycle)
                 Scrubber liquor flowrate      230 L/min (60 gpm)
                 Scrubber pressure drop       1.5 kPa (6 in WC)
                 Scrubber liquor pH          7.5 to 8.0
68 kg/hr (150 Ib/hr)
980°C (1,800°F)
10 percent
1,090° C (2,000° F)
7 percent
TABLE 4.  ACTUAL VERSUS TARGET OPERATING CONDITIONS FOR THE K088 TESTS
Temperature, °C (°F)
Test
Date
Target
Minimum
Maximum
Average
Flue
gas O2, %
Target Range
Average
Kiln exit
1
2
3
1/15/91
1/16/91
1/17/91
982 (1,800)
982 (1,800)
982 (1,800)
962 (1,764)
954 (1,749)
922 (1,692)
1,062
1,016
1,012
(1,944)
(1,861)
(1,853)
999 (1,830)
984 (1,803)
972 (1,781)
10
10
10
9.6
9.9
9.7
to
to
to
12.3
12.8
12.9
11.0
11.6
11.4
Afterburner exit
1
2
3
1/15/91
1/16/91
1/17/91
1,093 (2,000)
1,093 (2,000)
1,093 (2,000)
1,088 (1,990)
1,091 (1,995)
1,088 (1,990)
1,102
1,103
1,102
(2,016)
(2,017)
(2,015)
1,096 (2,005)
1,096 (2,005)
1,096 (2,005)
7
7
7
8.2
7.9
8.4
to
to
to
10.0
9.9
10.4
9.0
9.2
9.6
                                       20

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                   TABLE 5. WASTE FEED AND ASH COLLECTED
Test
1 (1/15/91)
2 (1/16/91)
3 (1/17/91)
Total
Slag recovered15
Total ashc
Total waste
fed, kg
(Ib)
282 (621)
233 (513)
267 (587)
782 (1,721)


Ash collected8
Weight, kg Fraction of feed,
(Ib) %
168 (370)
125 (275)
129 (284)
422 (929)
121 (266)
543 (1,195)
60
54
48
54

69
             aAsh collected in collection drum during test.
             bSlag removed from kiln walls after test program completion.
             cSum of total ash collected during test program and slag
              removed from kiln walls after test program completion.
        The consequence of the slag formation experienced is greater ash holdup in the kiln,
with formed slag adhering to the kiln wall.  After the test program was completed, a buildup of
slag on the kiln walls was clearly evident.  The slag layer covered the entire length of the kiln
with an average thickness of 1.3 cm (0.5 in). The slag buildup was manually removed (chipped
off) after test program completion. A total of 121 kg (266 Ib) of slag was removed, as indicated
in Table 5. When this quantity is added to the ash collected in the ash collection drums during
the test, the total ash plus slag collected accounted for an increased 69 percent of the total waste
fed over the test program.  The relationship between this total recovered kiln ash and the ash
content in the waste is discussed in Section 3.2.1.

3.1.2    Sampling and Analysis Procedures

        The scope of the sampling effort undertaken during this test program is illustrated in
Figure 8, in which the sampling locations and the corresponding sample collection methods are
identified.  Specifically, the sampling during each test consisted of:

        •     Obtaining grab/composite samples of the waste feed from each drum as the waste
              was packaged into fiberpack containers

        •     Obtaining samples of the kiln ash generated  from each test

        •     Obtaining samples of the recirculating scrubber  liquor for each test

        •     Continuously measuring O2 levels in flue gas at the kiln exit and at the afterburner
              exit; O2, CO, CO2, NOX and TUHC levels at the scrubber exit;- and O2, CO, and
              CO2 levels in the stack gas
                                           21

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                                                 22

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        •    Sampling flue gas downstream of the scrubber for cyanide using a Method 5
             variation of a NIOSH Method 7904 sampling train, for fluoride using an EPA
             Method 13B train, and for paniculate and trace metals using an EPA Method 5
             train

        •    Sampling the stack  gas for cyanide using a  Method  5  variation of a NIOSH
             Method 7904 sampling train and for particulate and HC1 using an EPA Method
             5 train

        For each test, 48  fiberpack drums of waste wers packaged the day before the test.
During packaging, a nominal lOOg aliquot of the contents of each of the first 36 fiberpacks was
taken.  Each of these aliquots was ground to a nominal size of 1 mm or less. These ground
aliquots were then combined in groups of 12, so that three composite waste feed samples per test
day (nine total) resulted, each corresponding to a set of 12 fiberpacks of feed packaged for a test
day. Throughout each test, kiln ash discharged to the ash pit was continuously removed by an
auger system and conveyed to a series of  initially clean  55-gal drums.   Two ash samples
corresponding to two of the three feed samples were collected each day.

        Throughout the three-test program, the scrubber system was operated at total recycle
(zero blowdown). This mode allowed any combustion gas contaminants to build up to maximum
(worst-case) concentrations in the  scrubber liquor over the three-test program. Two samples of
the recirculating scrubber liquor were collected for cyanide analyses each test day. These two
samples were collected to correspond to two of the three feed sample sets incinerated each test
day. After all tests were completed, the scrubber system was drained to a storage tank. A final,
full test program composite scrubber liquor  sample was collected while the system was being
drained. This composite sample was analyzed for the other test program constituents of interest.

        The sample collection procedures resulted in two waste samples, with corresponding kiln
ash and scrubber liquor samples,  each test day, to provide six waste/kiln ash/scrubber liquor
combinations over the three tests. A third waste feed sample (the initial set of waste fiberpack
drums fed) was also analyzed to provide a further measure of the degree of waste composition
variability. One set of flue gas characterization samples was collected  for each test. One total
test scrubber liquor sample was collected as well.

        The test program composite scrubber liquor  sample was filtered using the  TCLP
filtration procedure for solids-containing liquid waste. An aliquot of the kiln ash was subjected
to the TCLP leaching procedure. Waste feed samples, kiln ash samples, kiln ash TCLP leachate
samples, and both the filterable solids and filtrate fractions of the scrubber liquor were analyzed
separately for:

         •    The BDAT semivolatile organic constituents

         •    The BDAT trace metals listed in Table 6

         •    The nonhazardous constituent metals listed in Table 6

         •    Fluoride

         •    Cyanides (total and amenable)

                                          23

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                       TABLE 6. TRACE METALS DETERMINED
                             BOAT List
                            trace metals
  Nonhazardous
constituent metals
                             Antimony
                             Arsenic
                             Barium
                             Beryllium
                             Cadmium
                             Chromium
                             Copper
                             Lead
                             Mercury
                             Nickel
                             Selenium
                             Silver
                             Thallium
                             Vanadium
                             Zinc
   Aluminum
   Calcium
   Cobalt  .
   Iron
   Lithium
   Magnesium
   Manganese
   Molybdenum
   Phosphorus
   Potassium
   Sodium
   Strontium
   Tin
Exceptions to this  were that kiln ash TCLP leachates were  not  analyzed  for the BDAT
semivolatile organic constituents, and the scrubber liquor solids were not analyzed for fluoride.
Waste feed, kiln ash, and scrubber liquor filtrate samples were  also analyzed  for sulfide; and
waste feed and kiln ash samples were subjected to proximate (ash, moisture, fixed carbon, and
volatile carbon), ultimate (C, H, O, N, S, Cl), and silica (SiO2) analyses.

32     TEST RESULTS

        Test results are presented in this section. In many of the data tables that follow, sample
analysis results are grouped by test day (Test 1, 2, and 3), with separate results grouped for each
of the two waste feed/kiln ash pairs within each test day (with scrubber liquor added for cyanide
analysis).  These two pairs are denoted the "a" pair and  the "b" pair in the tables. Results for
the third waste feed sample  (not paired with a kiln ash residue sample),  denoted as waste
sample "c," are also given.

3.2.1    Proximate, Ultimate,  and Silica Analysis Results

        Table 7 summarizes the proximate and silica results for the waste feed and kiln ash
samples. These data can be used to calculate the average proximate composition for the waste
feed and kiln ash for each test day.  Further, weighted averages can be calculated by weighting
each test day's average composition by the amount of waste feed/kiln ash  collected that day,
shown  in Table 5.

        Using these total test program weighted average concentrations, proximate component
distributions for  the incineration tests performed can be calculated.  These distributions are
summarized in Table 8.  The data in Table 8  show that roughly half  the carbon content (both
                                         24

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             TABLE 7. PROXIMATE AND SILICA ANALYSIS RESULTS
                                        Concentration, wt %
            Sample
 Fixed   Volatile   Total fixed
carbon  matter   plus volatile  Moisture  Ash  Silica
Test 1 (1/15/91):
Waste la
Kiln ash la
Waste Ib
Kiln ash Ib
Waste Ic
33.0
21.5
34.7
25.4
31.3
2.4
2.1
2.5
1.3
3.1
35.4
23.6
37.2
26.7
34.4
0.1
0.1
0.02
0.1
0.2
64.6
76.3
62.7
73.2
65.4
3.4
7.3
3.3
4.0
3.7
       Test 2 (1/16/91):
        Waste 2a         34.2     3.5
        Kiln ash 2a       27.7     4.0
        Waste 2b         34.8     4.8
        Kiln ash 2b       26.1     3.7
        Waste 2c         33.8     3.6
       Test 3 (1/17/91):
                     37.7
                     31.7
                     39.6
                     29.8
                     37.4
0.2
0.1
0.2
0.1
0.2
62.1
68.2
60.2
70.1
62.4
5.6
5.5
5.3
5.4
5.7
Waste 3a
Kiln ash 3a
Waste 3b
Kiln ash 3b
Waste 3c
37.4
28.9
36.4
20.3
38.8
5.4
2.3
5.4
3.6
4.0
42.8
31.2
41.8
23.9
42.8
0.1
0,1 .
0.2
0.1
0.2
. 57.1
. 68.7
58;0
76.0
57.6
5.9
5.6
5.5
5.7
6.3
TABLE 8. TEST PROGRAM COMPOSITE PROXIMATE COMPONENT DISTRIBUTIONS
Parameter
Waste feed:
Composite concentration1", %
Amount fed, kg (Ib)
Kiln ash:
Composite concentration13, %
Amount discharged0, kg (Ib)
Fraction of amount fed, %
Total

99.9
781 (1,719)

99.9
543 (1,194)
69
Fixed
carbon

34.9
273 (601)

24.8
135 (297)
49
Volatile
matter

3.8
30 (66)

2.7
15 (32)
48
Ash

61.2
478 (1,052)

72.4
393 (865)
82
Silica"

5.0
39 (86)

5.6
30 (67)
78
 aSilica is a component of the ash fraction.
 bMoisture excluded.
 Includes 121 kg (266 Ib) of slag removed after the test program; assumes slag has same
  composition as composite ash collected during the test program.
                                        25

-------
fixed and volatile fractions) of the waste was destroyed (oxidized) during the incineration of the
waste.  Roughly 80 percent of the ash content of the waste was discharged as kiln ash; the
remaining 20 percent of the ash was either volatilized out of the kiln or entrained as particulate
in kiln exit flue gas.  Roughly 80 percent of the waste silica (a component of the ash fraction of
the waste) remained with this kiln ash as well.  This distribution (80 percent kiln ash, 20 percent
entrainment/volatilization escaping the kiln) is in line with past IRF testing experience.

322   Cyanide and Semivolatile Organic Analysis Results

        Table 9 summarizes the cyanide concentrations in all test program samples analyzed.
The waste  incinerated during the first test day (Test 1) contained an average of 5,200 mg/kg
total cyanide, roughly 97 percent of which was amenable to chlorination.  The waste fed during
the second and third test days (Tests  2 and 3)  contained less cyanide, an average of about
3,500 mg/kg. In addition, less (about 85 percent) of the cyanide in the Test 2 and 3 waste feeds
was amenable to chlorination.

        Kiln ash cyanide content varied from test to test, and from sample to sample within a
test day. Measured levels were in the 60 to 330 mg/kg range. Interestingly, the kiln ash cyanide
levels were generally higher for  the lower-cyanide-content Tests 2 and 3 wastes than for the
higher-cyanide-content Test 1 waste.  The fraction  of kiln ash amenable to chlorination also
varied from test to  test, and from  sample to sample within a test day. Amenable cyanide
fractions ranged from 22 to 73 percent.

        Kiln ash TCLP leachates contained measurable cyanide levels  ranging from  0.5 to
0.6 mg/L for the Test 1 ash, to 3 to 4 mg/L  for the Tests 2 and 3 ash. Amenable cyanide
fractions ranged from <0.2 percent (no amenable cyanide in the TCLP leachate) to > 100 per-
cent (more amenable cyanide measured in the leachate than total cyanide). No cyanide was
detected in the scrubber liquor filtrate or solids from any test.  Cyanide was also not detected
in any scrubber exit flue gas or stack gas sampling train sample.

        In an approach similar to that followed in Table 8 for the distribution of the proximate
components from the incineration of K088, Table 10 summarizes the composite test program
cyanide distributions. As shown  in Table 10, the composite test program kiln ash is estimated
to have accounted for 2.7 percent of the waste total cyanide fed, and 1.6 percent of the amenable
cyanide fed. Alternatively, 97.3 percent of the waste total cyanide and 98.4 percent of the waste
amenable cyanide was removed by the incineration process and destroyed. (Table 9 shows that
cyanide was not detected in either scrubber exit flue gas or stack gas, nor was cyanide detected
in any test scrubber liquor filtrate or solids.)

        To assess the degree of  cyanide destruction, the cyanide DREs were calculated using
the regulatory definition:


                     DUE = 100 x (1  - flue gas emission ratelfeedrate)
Table 11 presents the data required to calculate cyanide DREs corresponding to the detection
limits noted in Table 9 for combustion  flue gas.  As shown in Table 11, cyanide DREs were

                                          26

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TABLE 9. CYANIDE ANALYSIS RESULTS

Sample
Test 1 (1/15/91):
Waste la, mg/kg
Kiln ash la, mg/kg
Kiln ash la TCLP leachate, mg/L
Scrubber liquor filtrate la, mg/L
Scrubber liquor solids la, mg/kg
Waste Ib, mg/kg
Kiln ash Ib, mg/kg
Kiln ash Ib TCLP leachate, mg/L
Scrubber liquor filtrate Ib, mg/L
Scrubber liquor solids Ib, mg/kg
Waste Ic, mg/kg
Scrubber exit flue gas, ftg/dscm
Stack gas, pg/dscm
Test 2 (1/16/91):
Waste 2a, mg/kg
Kiln ash 2a, mg/kg
Kiln ash 2a TCLP leachate, mg/L
Scrubber liquor filtrate 2a, mg/L
Scrubber liquor solids 2a, mg/kg
Waste 2b, mg/kg
Kiln ash 2b, mg/kg
Kiln ash 2b TCLP leachate, mg/L
Scrubber liquor filtrate 2b, mg/L •
Scrubber liquor solids 2b, mg/kg
Waste 2c, mg/kg
Scrubber exit flue gas, /ig/dscm
Stack gas, ng/dscm
Test 3 (1/17/91):
Waste 3a, mg/kg
Kiln ash 3a, mg/kg
Kiln ash 3a TCLP leachate, mg/L
Scrubber liquor filtrate 3a, mg/L
Scrubber liquor solids 3a, mg/kg
Waste 3b, mg/kg
Kiln ash 3b, mg/kg
Kiln ash 3b TCLP leachate, mg/L
Scrubber liquor filtrate 3b, mg/L
Scrubber liquor solids 3b, mg/kg
Waste 3c, mg/kg
Scrubber exit flue gas, /tg/dscm
Stack gas, /ig/dscm
"NA = Not analyzed. If total CN not

Total CN

5,290
60
0.51
< 0.005
<5
4,550
130
0.58
< 0.005
<5 .
5,880
<0.16
<0.14

3,200
90
3.1
< 0.005
<5
3,500
330
3.2
< 0.005
<5
3,500
<0.15
<0.14

3,390
260
4.0
< 0.005
<5
3,500
130
3.3
< 0.005
<5
3,800
<0.16
<0.15
detected, amenable CN ane
Amenable
CN '

5,120
36
0.21
NAa
NA
4,430
40
1;17
NA
NA
5,780
NA
NA

2,700
20
< 0.005
NA
NA
2,970
170
< 0.005
NA
NA
3,000
NA
NA

2,930
190
1.6
NA
NA
2,900
90
< 0.005
NA
NA
3,100
NA
NA
ilysis not perfor
Fraction
amenable, %

96.8
60.0
41.2


97.4
30.8
>100


98.3



84.4
22.2
<0.2


84.9
51.5
<0.2


85.7



86.4
73.1
40.0


82.9
56.3
<0.2


81.6


med.
               27

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TABLE 10.  TEST PROGRAM COMPOSITE CYANIDE DISTRIBUTIONS
                Parameter
Total CN Amenable CN
    Waste feed:
      Composite concentration, mg/kg       4,120       3,720
      Amount fed, kg                     3.22        2.91
    Kiln ash:
      Composite concentration, mg/kg       160        86
      Amount discharged8, g                87         47
      Fraction of amount fed, %	2/7	1.6
    "Includes 121 kg (266 Ib) of slag removed after test program;
     assumes slag has the same composition as the composite ash
     collected during the test program.
                    TABLE 11. CYANIDE DREs
Parameter
Waste feed:
Waste feedrate, kg/hr
Average CN concentration, mg/kg
CN feedrate, g/hr
Scrubber exit flue gas:
CN concentration, [ig/dscm
Flue gas flowrate, dscm/min
Flue gas CN emission rate, ng/hr
CN DRE, %
Stack gas:
CN concentration, iig/dscm
Flue gas flowrate, dscm/min
Flue gas CN emission rate, ng/hr
CN DRE, %
Test 1
(1/15/91)

72
5,240
377

<0.16
29.5
<280
> 99.99993

<0.14
33.0
<280
> 99.99993
Test 2
(1/16/91)

68
3,400
231

<0.15
34.6
<310
> 99.99987

<0.14
35.5
<300
> 99.99987
Test 3
(1/17/91)

72
3,560
256

<0.16 •
35.2
<340
> 99.99987

<0.15
36:6
<330
> 99.99987
                               28

-------
greater than 99.99993 percent at both the scrubber exit and at the stack for Test 1 and greater
than 99.99987 percent for Tests 2 and 3.

        As noted in Section 3.1.2, all nine waste feed, six kiln ash, and the one test program
composite scrubber liquor and solids filtrate samples, were analyzed for the semivolatile organic
BDAT list compounds.  None  of these  compounds was found in  any kiln ash sample  at
compound-specific practical quantitation limits (PQLs) of 0.4 to 4 mg/kg, in the scrubber liquor
filtrate sample at compound-specific PQLs of 20 to 200 |ig/L, and in the scrubber liquor solids
sample at compound-specific PQLs of 130 to 1,300 mg/kg. No waste feed sample contained any
semivolatile organic constituent at compound-specific PQLs of 0.8 to 8 mg/kg, with the exception
of waste feed 3c which contained benzo(b)fluoranthene at 4.0 mg/kg and benzo(a)pyrene at
3.6 mg/kg. The PQLs of the scrubber liquor solids were high because the solids content of the
scrubber liquor was very low (0.154 g/L), so very little sample was available for extraction.

323    Trace Metal Analysis Results

        Table 12 summarizes the BDAT list trace metal analysis results for all samples analyzed.
Table 13 presents a similar summary for the nonhazardous constituent  metals analyzed. In both
tables, scrubber exit flue gas concentrations are shown as ranges in many cases. Two sampling
train samples were analyzed to give the total flue gas concentration: the  probe wash and  filter
catch sample, and the combined impinger solutions sample. In many cases, one or both samples
contained no detectable metal.   In these instances, the flue gas concentration is shown as a
range; the lower bound corresponds to assuming a zero metal concentration in the sample or
samples having the not-detected metal, and the upper bound corresponds to assuming the metal
was present at the detection limit in the sample or samples having the not-detected metal.

        The data in Table 13 show that the major elemental constituents  of both the waste and
resulting kiln ashes were aluminum, calcium, and sodium. These were  present in waste and kiln
ash samples at levels greater than 1 percent.  Sodium alone accounted for about 20 to 30 percent
of individual waste and kiln ash samples.

        The data in Table 12 show that major BDAT trace metals present were barium, nickel,
and thallium.  These were present in waste and kiln ash  samples at levels in roughly the 100 to
200 mg/kg range. No antimony, lead, mercury,  selenium, or silver  was found in any waste
sample, nor, with the exception of lead, in any kiln ash, scrubber exit flue gas, or scrubber liquor
sample.  No data are shown for lead in the la and Ib kiln ash samples, the three test flue gas
samples, and the  three test composite scrubber liquor filtrate sample.  No lead was detected in
any waste feed sample.  The measurable levels  found  in the kiln ash  samples, the flue gas
samples, and the  composite scrubber liquor sample are attributed to contamination.

        Table  12 also notes the TCLP regulatory level established to define toxicity characteristic
hazardous waste per  the TCLP for those metals  having  a regulatory level  tabulated in
40 CFR 261, Appendix II.  Comparing kiln ash  TCLP leachate  and scrubber liquor filtrate
concentrations to the  regulatory levels shows that neither the kiln ash from any test nor the
program composite scrubber liquor would be a toxicity characteristic hazardous waste due to
their leachable hazardous constituent trace  metal content.
                                          29

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                 TABLE 12.  BOAT TRACE METAL ANALYSIS RESULTS
Sample
Test 1 (1/15/91):
Waste la, mg/fcg
Kiln ash la, mg/kg
Kiln ash TCLP leachate la, mg/L
Waste Ib, mg/kg
Kiln ash Ib, mg/kg
Kfln ash TCLP leachate Ib, mg/L
Waste Ic, mg/kg
Scrubber exit flue gas, Mg/dscm
Test 2 (1/16/91):
Waste 2a, mg/kg
Kiln ash 2a, mg/kg
Kiln ash TCLP leachate 2a, mg/L
Waste 2b, mg/kg
Kfln ash 2b, mg/kg
Kiln ash TCLP leachate 2b, mg/L
Waste 2c, mg/kg
Scrubber exit flue gas, Mg/dscm
Test 3 (1/17/91):
Waste 3a, mg/kg
Kiln ash 3a, mg/kg
Kiln ash TCLP leachate 3a, mg/L
Waste 3b, mg/kg
Kiln ash 3b, mg/kg
Kiln ash TCLP leachate 3b, mg/L
Waste 3c, mg/kg
Scrubber exit flue gas, Mg/dscm
3 test scrubber liquor:
Solids, mg/kg
Filtrate, mg/L
TCLP regulatory level, mg/L
Sb As

<10 11.0
<10 11.4
<0.2 0.016
<10 9.8
<10 8.6
<0.2 0.034
<10 8.8
<96 7.1-11.6"

<10 7.4
<10 10.0
<0.2 0.033
< 10 9.0
< 10 7.7
<0.2 0.020
<10 8.2
<93 2.5-6.9

< 10 13.4
<10 15.9
<0.2 < 0.010
<10 12.9
<10 9.7
<0.2 0.096
<10 11.2
<78 3.9-7.5

<40 <2.0
<0.5 <0.03
5.0
Ba

199
216
31.8
191
227
31.2
195
12.9-17.4

190
221
29.4
176
209
10.5
180
26.2-30.6

205
238
19.1
221
235
23.9
193
12.2-15.8

9,740
17.8
100
Be

26
28
0.020
24
26
0.026
25
3.7-8.2

20
25
0.015
22
26
0.013
21
1.0-5.5

19
25
0.015
17
29
0.025
17
1.1-4.7

2.1
<0.03

Cd

2.6
<3.9
<0.03
2.3
<3.6
<0.03
2.6
4.5-17.9

2.4
3.3
<0.03
2.2
3.3
<0.03
2.4
3.8-17.0

2.2
3.3
<0.03
2.2
3.7
<0.03
2.3
4.6-15.2

<7
<0.1
1.0
Cr

19
27
0.16
23
<20
<0.06
23
13.6-35.9

26
15
0.15
23
13
<0.05
22
13.6-35.7

27
15
<0.05
23
16
<0.05
26
12.5-30.2

<10
<0.2
5.0
Cu

25
33
0.05
22
23
0.14
22
10.3-19.2

24
22
0.36
23
19
0.41
30
7.4-16.3

40
31
0.45
41
35
0.73
36
6.2-13.2

6.5
1.1

Pb

<5
a
<5
<5
—

<5
<5
<5
<5
<5
—

<5
<5
<5
<5
<5
—

<20
—
5.0
*— Denotes sample contaminated, analytical result compromised.                               (continued)
bRange corresponds to assuming zero metal concentration in a sample having nondetectable metal to
 assuming metal concentration at the detection limit in a sample having nondetectable metal.
                                            30

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                                 TABLE 12.  (continued)
Sample
Test 1 (1/15/91):
Waste la, mg/kg
Kiln ash la, mg/kg
Kiln ash TCLP leachate la, mg/L
Waste Ib, mg/kg
Kiln ash Ib, mg/kg
Kiln ash TCLP leachate Ib, mg/L
Hg

<0.1
<0.1
< 0.002
<0.1
<0.1
< 0.002
Ni

94
142
<0.05
71
85
<0.05
Se Ag

<10 <1.0
<10 1.0
<0.2 <0.02
< 10 < 1.0
< 10 < 1.0
<0.2 <0.02
Tl

133
194
1.0
123
197
1.2
V

42
66
0.24
44
57
0.44
Zn

43
38
9.5
49
35
8.2
 Waste Ic, mg/kg
 Scrubber exit flue gas, Mg/dscm
Test 2 (1/16/91):
 Waste 2a, mg/kg
 Kiln ash 2a, mg/kg
 Kite ash TCLP leachate 2a, mg/L
 Waste 2b, mg/kg
 Kiln ash 2b, mg/kg
 Kiln ash TCLP leachate 2b, mg/L
 Waste 2c, mg/kg
 Scrubber exit flue gas, fig/dscm
Test 3 (1/17/91):
 Waste 3a, mg/kg
 Kiln ash 3a, mg/kg
 Kiln ash TCLP leachate 3a, mg/L
 Waste 3b, mg/kg
 Kiln ash 3b, mg/kg
 Kiln ash TCLP leachate 3b, mg/L
 Waste 3c, mg/kg
 Scrubber exit flue gas, jtg/dscm
3 test scrubber liquor:
 Solids, mg/kg
 Filtrate, mg/L
TCLP regulatory level, mg/L
                                            91
                                   NAC      2.6-24.8  <96
                                  121      83      41
                                  6.7-95.7  3.5-25.7  97.2
<0.1      55
<0.1      88
<0.002    <0.05   <0.2    <0.02

< 0.002    <0.05   <0.2    <0.02

NA       2.4-24.5  <96
108
169
1.2
101
174
1.2
33
32
0.32
37
34
0.56
48
37
8.7
44
50
5.7
                                                                     110
                                           22
                 46
                                                                     5.4-93.7  2.9-25.0  320
<0.1
<0.1
< 0.002
<0.1
<0.1
< 0.002
115
142
<0.05
93
159
<0.05
< 10 < 1.0 92
< 10 < 1.0 158
<0.2 <0.02 1.0
<10 , <1.0 102
< 10 < 1.0 181
<0.2 <0.02 1.8
36
37
0.50
35
40
0.68
42
40
7.0
59
23
5.6
<0.1      83
NA       2.2-19.9  <78    <8.0

<0.1      <10     <40,   <5.0
< 0.002    <0.2    <0.5    <0.05
0.2               1.0     5.0
                                                                     100      36      45
                                                                     7.0-78.0  2.9-20.6  262
<40
<0.5
                                                                              <0.2
                                                   7,250
                                                   5.9
°NA = not analyzed.
                                             31

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     TABLE 13. NONHAZARDOUS CONSTITUENT METAL ANALYSIS RESULTS
Sample
Test 1 (1/15/91):
Waste la, mg/kg
Kiln ash la, mg/kg
Kiln ash TCLP leachate la, mg/L
Waste Ib, mg/kg
Kiln ash Ib, mg/kg
Kiln ash TCLP leachate Ib, mg/L
Waste Ic, mg/kg
Scrubber exit flue gas, /ig/dscm
Test 2 (1/16/91):
Waste 2a, mg/kg
Kiln ash 2a, mg/kg
Kiln ash TCLP leachate 2a, mg/L
Waste 2b, mg/kg
Kiln ash 2b, mg/kg
Kiln ash TCLP leachate 2b, mg/L
Waste 2c, mg/kg
Scrubber exit flue gas, ng/dscm
Test 3 (1/17/91):
Waste 3a, mg/kg
Kiln ash 3a, mg/kg
Kiln ash TCLP leachate 3a, mg/L
Waste 3b, mg/kg
Kiln ash 3b, mg/kg
Kiln ash TCLP leachate 3b, mg/L
Waste 3c, mg/kg
Scrubber exit flue gas, /ig/dscm
3 test scrubber liquor:
Solids, mg/kg
Filtrate, mg/L
"Range corresponds to assuming zero
AI

86,500
62,500
672
80,700
123,000
642
75,600
4,910-5,000

73,200
104,000
664
71,400
106,000
693
76,400
4,230-4,320

54,200
96,900
570
68,700
112,000
1,070
57,600
3,800-3,880

5,450
25
Ca

14,700
13,600
8.6
14,300
16,100
9.6
18,600
6,950

15,300
15,900
8.4
15,100
13,200
6.4
16,200
7,390

16,800
14,200
8.1
13,200
15,200
6.9
12,400
6,690

2,550
640
metal concentration in a
Co

16
16
0.09
18
14
0.13
12
<15

10
14
0.24
11
12
0.23
13
<15

16
17
0.30
17
17
0.28
15
<11

8.3
<0.1
Fe

2,630
4,300
0.9
2,560
3,400
1.4
2,950
148-166

2,770
3,820
0.9
2,770
3,620
1.1
2,810
101-119

3,020
4,120
1.6
2,300
4,370
1.3
3,050
80.9-95.1

123
0.74
Li

5,620
6,500
18
5,710
5,700
22
5,530
1,290-1,310

8,250
7,180
30
8,520
5,940
22
7,810
1,560-1,610

7,390
6,640
23
6,470
8,030
23
7,610
1,190-1,230

<20
4.0
Mg

557
769
3.7
472
585
3.6
• 573
509-531

537
659
3.6
556
646
2.1
539
448-470

528
645
3.3
499
743
2.8
508
420-438

455
4.5
sample having nondetectable
Mn

19
37
0.30
18
27
0.32
27
2.5-11.4a

24
29
0.27
21
29
0.20
23
2.1-11.0

22
31
0.23
23
27
0.27
22
2.1-9.2

<4
<0.17
(continued)
metal to assuming metal concentration at the detection limit in a sample having nondetectable metal.
                                       32

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TABLE 13.  (continued)
Sample
Test 1 (1/15/91):
Waste la, mg/kg
Kiln ash la, mg/kg
Kiln ash TCLP leachate la, mg/L
Waste Ib, mg/kg
Kiln ash Ib, mg/kg
Kiln ash TCLP leachate Ib, mg/L
Waste Ic, mg/kg
Scrubber exit flue gas, /tg/dscm
Test 2 (1/16/91):
Waste 2a, mg/kg
Kiln ash 2a, mg/kg
Kiln ash TCLP leachate 2a, mg/L
Waste 2b, mg/kg
Kiln ash 2b, mg/kg
Kite ash TCLP leachate 2b, mg/L
Waste 2c, mg/kg
Scrubber exit flue gas, #g/dscm
Test 3 (1/17/91):
Waste 3a, mg/kg
Kiln ash 3a, mg/kg
Kiln ash TCLP leachate 3a, mg/L
Waste 3b, mg/kg
Kiln ash 3b, mg/kg
Kiln ash TCLP leachate 3b, mg/L
Waste 3c, mg/kg
Scrubber exit flue gas, iig/dscm
3 test scrubber liquor:
Solids, mg/kg
Filtrate, mg/L
Mo

<3
<3
0.10
<3
<3
0.09
<3
<29

<3
<3
0.06
<3
<3
0.07
<3
<29

<3
<3
0.10
<3
<3
0.11
<3
<23

<12
<0.2
P

170
<0.5
0.71
262
148
<0.5
94
148-370

231
151
<0.5
228
193
<0.5
234
85-306

250
148
4.4
275
238
<0.5
240
77-255

857
25
K

728
1,560
19
566
110
21
717
1,100-1,110

728
1,200
46
857
1,150
46
839
3,500

1,000
1,290
45
795
1,520
54
855
1,060-1,070

4,460
19
Na

176,000
287,000
6,420
196,000
207,000
6,850
210,000
91,100

199,000
215,000
8,660
203,000
243,000
9,660
208,000
108,500

186,000
183,000
7,770
61,300
209,000
9,000
176,000
30,100

19,600
2,950
Sr

137
148
0.42
138
144
0.44
133
77-86

156
144
0.38
148
143
0.29
149
70-79

144
153
0.39
147
178
0.33
144
66-73

196
0.42
Sn

<10
12
<0.2
<10
<10
<0.2
<1Q
<96

<10
<10
<0.2
<10
<10
<0.2
<10
<96

<10
<10
<0.2
<10
<10
<0.2
<10
<78

<40
<0.5
         33

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        The data from Table 12 are combined with appropriate waste and discharge stream
 flowrate data to give the distributions of the BDAT list trace metals among the three incinerator
 discharges (kiln ash, scrubber liquor, and flue gas) shown in Table  14. The distributions shown
 in Table 14 are in percentages of the amount of each metal introduced in the waste feed, and,
 thus, represent trace metal mass balances. The mass balances have been calculated over the
 entire three-test program for two reasons:

        •    A significant quantity  of slag was removed from the kiln after test program
              completion; arbitrarily allocating slag quantities among the three tests would be
              subject to challenge (the mass balances in Table 14 assume the slag removed had
              the test program composite trace metal composition)

        •    A single test program composite scrubber liquor sample was analyzed; again,
              arbitrarily allocating the scrubber liquor metal quantities to individual tests would
              be subject to challenge

 Table 15 represents the mass balance summary, analogous to Table 14, for  the nonhazardous
 constituent metals.

        In both Tables 14 and 15, fractional distributions are shown as ranges for the scrubber
 liquor and scrubber exit flue gas discharges of several metals. This is because scrubber liquor
 and flue gas contained nondetectable quantities of many metals, and flue gas concentrations for
 several metals were expressed as ranges as discussed  above.
                          t
        The data in Tables 14 and 15 show that, with the exception of phosphorus,  metal mass
 balance closures achieved for the test program ranged from 45 to 132 percent.  This level of
 closure is considered quite  good when compared  to past experience in  measuring metal
 distributions in discharges from combustion sources.  This past experience shows that closures
 in the 50 to 200 percent range represent about the best achievable.  Phosphorus closures would
 not be expected to be near 100 percent, as phosphorus is most likely oxidized to  P2O5.  The
 oxidizing acid impingers in the metals train supplying the flue gas phosphorus concentrations
would not be expected to be very efficient at collecting P2O5.

        Most of each metal fed was overwhelmingly accounted for by the kiln ash discharge for
all metals except barium and zinc (phosphorus, discussed above, is not a metal).  A substantial
fraction of these two metals was found in the scrubber liquor, and, for zinc, in the scrubber exit
flue gas.  The scrubber liquor also contained  moderate fractions  of calcium, potassium, and
copper. The scrubber exit flue gas contained moderate fractions of potassium and  cadmium.

3.2.4    Sulfide and Fluoride Analysis Results

        Table 16 summarizes the sulfide and fluoride analysis results for all  samples analyzed
for  these  two analytes.  As  shown in the table, waste sulfide levels ranged from 0,006  to
0.080  percent. Kiln ash levels were comparable and ranged from 0.010 to 0.081 percent. Kiln
ash TCLP leachate levels were generally less than 10 mg/L.
                                          34

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                                     35

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TABLE 16. SULFIDE AND FLUORIDE ANALYSIS RESULTS
         FOR WASTE FEED AND KILN ASH SAMPLES
Sample
Test 1 (1/15/91):
Waste la, %
Kiln ash la, %
Kiln ash TCLP leachate la, mg/L
Waste Ib, %
Kiln ash Ib, %
Kiln ash TCLP leachate Ib, mg/L
Waste Ic, %
Scrubber exit flue gas, mg/dscm
Test 2 (1/16/91):
Waste 2a, %
Kiln ash 2a, %
Kiln ash TCLP leachate 2a, mg/L
Waste 2b, %
Kiln ash 2b, %
Kiln ash TCLP leachate 2b, mg/L
Waste 2c, %
Scrubber exit flue gas, mg/dscm
Test 3 (1/17/91):
Waste 3a, %
Kiln ash 3a, %
Kiln ash TCLP leachate 3a, mg/L
Waste 3b, %
Kiln ash 3b, %
Kiln ash TCLP leachate 3b, mg/L
Waste 3c, %
Scrubber exit flue gas, mg/dscm
3 test scrubber liquor:
Filtrate, mg/L
Suffide
concentration

0.014
0.081
9
0.014
0.003
7
0.014
a

0.022
0.022
4
0.006
0.025
<0.4
0.020
—

0.080
0.035
6
0.018
0.010
11
0.019
—

50
Fluoride
concentration

2.72
6.80
85
1.30
4.05
122
5.92
, 17.4

4.33
3.48
78
3.48
2.44
668
5.33
4.75

4.98
2.54
46
4.39
1.34
42
3.51
135

0.3
*— Denotes not measured.
                     36

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        Waste fluoride levels ranged from 1.3 to 5 percent. Kiln ash levels were also comparable
and ranged from 1.3 to 6.8 percent. Kiln ash TCLP leachate fluoride levels were generally less
than about 100 mg/L, although one leachate contained almost 670 mg/L of fluoride.

        Table 17 takes the calculated composite test program weighted average concentrations
to calculate the fraction of waste feed sulfide and  fluoride accounted for in  the  kiln ash
discharge.  As shown in Table 17, the kiln ash sulfide accounted for 94 percent of the amount
present in the waste feed.  Thus, apparently very little of the waste feed sulfide content was
destroyed by incineration. The kiln ash discharge accounted for about 64 percent of the waste
feed fluoride.  The scrubber liquor and scrubber exit flue gas concentrations noted in Table 16
correspond to less than 0.01 and 4.1 percent of the fluoride fed over the test program.  Mass
balance closure for fluoride (sum of the amounts accounted for in the kiln ash, scrubber liquor,
and scrubber exit flue gas relative to the amount fed) was 68 percent.

3.2.5    Flue Gas Particulate and HC1 Emissions

        Table 18 summarizes the flue gas particulate  levels at the two locations measured, the
scrubber exit flue gas and the stack. Stack particulate levels were uniformly lower  than scrubber
exit flue gas levels. All levels measured were below the hazardous waste incinerator performance
standard of 180 mg/dscm at 7 percent O2.

        Table 19 summarizes the stack HC1 levels and emission rates measured.  All emission
rates were significantly below the hazardous waste incinerator performance standard of 1.8 kg/hr
(41b/hr).

33     CONCLUSIONS

        Test results confirm that K088 can be incinerated in compliance with the hazardous
waste incinerator performance standards under the test conditions employed.  Test data show
that the DRE for cyanide, the POHC in the waste, present at an average level of 4,120 mg/kg,
was greater than 99.999 percent.  This exceeds the performance standard of  99.99 percent.
 Furthermore, particulate emissions in the scrubber system exit  flue gas were 110 to  130
 mg/dscm, corrected to 7 percent 62, which meets the performance standard of 180 mg/dscm at
 7 percent  O2.  HC1 emissions were very low, consistent with the low chlorine content of the
 waste.

        The kiln ash discharge still contained measurable cyanide, however, at  a test average
 level of 160 mg/kg.  The degree of cyanide decontamination of the waste achieved (100 [1 -
 amount discharged in kiln ash/amount fed]) was 97.3 percent.  The kiln  ash TCLP leachate
 contained between 0.5 and 4.0 mg/L total cyanide.  Cyanide was not detected in scrubber liquor.

         Care must be exercised in incinerating K088 due to relatively low slagging temperatures.
 The material tested in these tests formed  slag in the kiln at temperatures just  above  the test
 temperature  of 980° C (1,800° F).  Incinerator operation for  these tests was  to be at" kiln
 temperatures below  the slag formation threshold.  However, despite  attempts to avoid slag
 formation, this proved to be a problem. About 20 percent of the kiln ash collected for the test
 series was in the form of slag removed from the kiln walls after test program completion.
                                           37

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  TABLE 17.    TEST PROGRAM SULFIDE AND
               FLUORIDE DISTRIBUTIONS
         Parameter
Sulfide
Fluoride
Waste feed:
  Composite concentration, %   0.023         3.97
  Amount fed, kg (Ib)          0.180 (0.396)   31.0 (68.3)
Kiln ash:
  Composite concentration, %   0.031         3.63
  Amount discharged3, kg (Ib)   0.168 (0.370)   19.7 (43.4)
  Fraction of amount fed, %    94            64
'Includes 121 kg (266 Ib) of slag removed after test
program; assumes slag has the same composition as the
composite ash collected during the test program.
    TABLE 18. FLUE GAS PARTICULATE LEVELS
Flue gas participate, mg/dscm at 7% O2

Test 1 (1/15/91)
Test 2 (1/16/91)
Test 3 (1/17/91)
Scrubber exit
121
110
131
Stack
78
100
70
      TABLE 19.  STACK GAS HCI EMISSIONS

Test 1 (1/15/91)
Test 2 (1/16/91)
Test 3 (1/17/91)
Stack gas HCI
Concentration
mg/dscm ppm g/hr
1.27 0.84 2.50
0.44 0.29 0.95
0.04 0.03 0.10
                       38

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Other test conclusions include:

•    About a 30-percent reduction in waste weight occurs with incineration; the kiln
     ash discharge was about 70 percent of the amount of waste feed

•    The waste contained about 35 percent fked carbon, 4 percent volatile carbon,
     61 percent ash, and 5 percent silica (an ash component).  Roughly 50 percent of
     both  the fixed and volatile carbon content  of the waste was  destroyed during
     incineration.  Roughly 80 percent of the ash and silica introduced in the waste
     feed  was discharged as kiln ash;  the remaining 20 percent  was likely  either
     volatilized or entrained into kiln exit flue gas.

•    An average of 90 percent of the waste total cyanide was analyzed to be amenable
     cyanide; an  average of 54 percent of the kiln ash cyanide was analyzed  to be
     amenable cyanide

•    The waste was essentially free of semivolatile organic BDAT list constituents, as
     were the kiln ash and scrubber liquor

•     The  major metal constituents of both the waste and kiln ash were aluminum,
      calcium, and sodium; the major BDAT list trace metal contaminants of both the
      waste and kiln ash were barium, nickel, and thallium, which were present at levels
      in the 100 to 200 mg/kg range

 •    Hazardous constituent trace metal concentrations in TCLP leachates of waste feed
      and  resulting kiln ash  were sufficiently low that neither  the waste nor the
      incineration kiln ash would be toxicity characteristic hazardous wastes

 •    The kiln ash discharge accounted for the major proportion of the waste feed metal
      content for all metals except barium and zinc.  A substantial fraction of these two
      metals was found in the scrubber  liquor, and, for  zinc, in the scrubber exit flue gas.
      The scrubber liquor contained moderate fractions  of calcium, potassium, and
      copper. The scrubber exit flue gas contained moderate fractions of potassium and
      cadmium.  Overall metal mass balance closures achieved (sum of the discharge
      metal measured in the kiln  ash,  scrubber liquor, and scrubber exit flue gas as a
      percentage  of the amount  of  metal fed in  the  waste)  ranged  from  45 to
      132 percent.

 •    About 94 percent of the waste sulfide content was accounted  for by the kiln ash
      discharge; apparently very little  sulfide destruction occurred.  About 64 percent
      of the  fluoride  fed in the waste was accounted for by the kiln ash discharge.
      Roughly 4 percent of the fluoride fed was accounted for in the scrubber exit flue
      gas.  Overall fluoride mass balance closure was  68 percent.

 Test results were reported in the report:

 •   Whitworth, W. E., J. W. Lee, and L. R Waterland, "Pilot-Scale Incineration Tests
       of Spent Potliners from the Primary Reduction of Aluminum (K088)," draft
      August 1991.

                                     39

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                                      SECTION 4

                  INCINERATION OF CONTAMINATED SOILS FROM
                      THE DRAKE CHEMICAL SUPERFUND SITE
        Another of the primary missions of the IRF is to support Regional Offices in evaluations
 of the potential of incineration as a treatment option for contaminated soils and sediments at
 Superfund sites.  One priority site is the Drake Chemical site in Lock Haven, Pennsylvania.
 EPA Region 3  and  the U.S. Army Corps  of  Engineers  (USAGE)  (R.  Schrock,  Region 3;
 D. Johnson, USAGE) requested that test burns be conducted at the IRF to support evaluations
 of the suitability of incineration as a  treatment technology for the  contaminated soils and
 sediments at the site.

       ^According to site investigation data, the soils and sediments at  the Drake site are
 contaminated  to varying degrees with various  organic constituents  and several hazardous
 constituent metals.   With respect to incinerability evaluation, the primary objective was  to
 determine whether treating the soils and sediments  by incineration would generate a residue
 environmentally suitable for disposal (redeposit), without further treatment,  at the Drake site
 during full-scale remediation. Therefore, one primary concern was whether incineration could
 effectively destroy the organic contaminants in fhe soils and sediments. Equally important was
what the  fate of the trace metals in the soils  and sediments would be  when  subjected  to
incineration.

        This test program was designed to evaluate the effectiveness of  varying incinerator
operating conditions  on organic contaminant  destruction and the effects of these varied
conditions on the distributions of the trace metals in the discharge streams. Particulate and HC1
emission measurements were taken  to establish the required flue  gas cleanup performance
necessary to safely treat the  soils and  sediments.  Analysis of the kiln bottom  ash (treated
soil/sediment) indicated whether the ash would be suitable for redeposit without further
treatment, or what additional treatment would be required before its  final disposal.  Specific
questions  answered in this test program were:

        •    Can rotary kiln incineration effectively destroy the organic contaminants in the
             site soils and sediments?

        •    Will the kiln  ash  from  incineration  of  the site soils and  sediments have
             characteristics  that will  allow  it  to be redeposited onsite,  without further
             treatment?
                                          40

-------
       «     Can the incineration treatment of the site soils and sediments be performed in
             compliance with the hazardous waste incinerator performance standards?

       *     What is the fate of the contaminant trace metals in the incineration of the site
             soils and sediments?

       •     What are the effects of incineration temperature on contaminant metal fate and
             kiln ash characteristics?

       As originally conceived, this test program was to have consisted of an initial phase of
nine tests  and an optional phase of four additional tests.  The results from the initial-phase
testing specifically'the toxicity characteristics exhibited by the incinerator residuals, guided the
decision as to whether the optional testing would be needed.  The initial-phase  incineration
testing, modified to consist of five, not nine, tests (see Section 4.1.1), was conducted at the IRF
in January and  February 1991.   The IRF RKS,  equipped with the venturi/packed-column
scrubber primary APCS (see Figure 1), was used for these tests. The toxicity characteristics of
all test program samples were demonstrated  to be below regulatory threshold levels.  These
results led to the conclusion that the optional testing would not be necessary to meet the stated
program objectives.

        Results  of the test program are discussed in the subsections that follow.

4.1     TEST PROGRAM

        The Phase III record of decision (ROD) document for the Drake Chemical site indicates
that about 252,000 yd3 of contaminated soils and sediments will be excavated and decontaminated
onsite by a transportable rotary kiln incinerator. The ROD further indicates that these materials
are contaminated with varying levels of organic compounds and several hazardous constituent
trace metals, including arsenic, barium, cadmium, chromium, lead, and mercury.

        For the test program, 17 55-gal drums of the contaminated site soils were excavated and
shipped to the IRF for  testing. These 17 drums consisted of:

        •    Two drums  of soil, one from  each of two "organic contamination  hot spots,"
              denoted as locations O-l and O-2

        •    Two drums of lagoon sediment from locations denoted as L-l and L-2

        •    Seven drums of soil from the "inorganic contamination, hot spots" (one from each
              of three locations denoted as M-l, M-2, and M-3; and two from locations denoted
              as M-4 and M-5)

         •    Six drums of composite soil representing general site characteristics from locations
              denoted  as G-l, G-2, G-3, G-4, G-5, and G-6
                                            41

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 4.1.1   Test Conditions

       ..As "ot?d above» the objective  of the  proposed test  program was to evaluate  the
 suitability of incineration as a treatment technology for the contaminated soils and sediments at
 the  Drake Chemical  Superfund  site.   Table 20 outlines the  nine originally planned test
 conditions.

         Analyses of samples of the soils actually excavated, however, revealed that several soils
 contained very low concentrations of contaminants, and that conducting incineration testing with
 these would therefore likely produce data of limited usefulness.  As a result of these analyses,
 the scope  of the test program was modified to  more adequately meet the original program
 objectives.   The modified test conditions are included in Table 20.  The specific changes
 included:

         •    Deleting the original test conditions 4, 5, 8, and 9

         •    Conducting Tests 3b and 7 with a  kiln temperature of 538° C (1,000° F)  instead
              of the originally planned 982°C (1,800°F)  and 816°C (1,500°F), respectively

         •    Reassigning the soil selection for each test, as shown in Table 20

         •    Spiking  each  soil  from  locations  L-2  and  O-2  with   naphthalene and
              1,4-dichlorobenzene to 3,000 and 130  ppm, respectively, and using these spiked
              soils for Tests 6 and 7; and designating naphthalene and 1,4-dichlorobenzene as
              the surrogate POHCs

         Of the five retained conditions, Tests 1, 2, 3a, and 3b were designed to study the fate
 of the inorganic contaminants (trace metals). Tests 1 and 2 studied the distribution of the trace
 metal contaminants throughout the incinerator system. These tests also provided information
 on the concentrations of trace metals in the kiln and flue gas flyash TCLP leachates. These data
 are important as they may affect whether additional  treatment of the incinerator solid residual
 streams is needed.  Tests 3a and 3b investigated  the effects of kiln temperature on the trace
 metal concentrations in the kiln ash and scrubber liquor streams. All these tests were conducted
 with the soils in their original, as-received, form. Tests 6 and 7 were designed to study the
 destruction  of the organic contaminants.  The destruction of the spiked POHCs became the
 principal indicator of the effectiveness of incineration under these tests conditions.

        Tests 1, 2, 3a, and 3b were performed with the high-inorganic-contaminant soils from
 locations M-2, M-5D, and O-l, respectively.  Tests 6  and  7 followed,  using the spiked location
 L-2 lagoon sediments and the location O-2 high-organic-contaminant soil.

        The five tests were conducted from January  30, 1991 through February 7, 1991.  Each
 test consisted of incinerating one 55-gal drum of the contaminated soils over a 4- to 5-hr period.
Tests 3a and 3b were performed in one day, with sufficient time allowed in between subtests to
achieve steady-state operation at the target kiln temperature of 816° C (1,500° F) for Test 3a and
538°C (1,000°F) for Test 3b.  Test soils were fed to the kiln via the fiberpack drum ram feeder
system. Each fiberpack contained 4.5 kg (10 Ib) of soil. One fiberpack was charged into the kiln
every 5 min, resulting in soil feedrates of nominally 55 kg/hr (120 Ib/hr).

                                           42

-------
                    TABLE 20. TARGET TEST CONDITIONS
                              =========
                                                   Revised
X-
Test
no.
1
2
,3a
3b
4a
4b
5a
5b
6
7
8
9
r a *^UKM**J
Test
material
M-5
M-4
M-l
M-l
M-2
M-2
M-3
M-3
O-l
O-2
L-l
L-2
Kiln
temperature,
°C (°F)
816(1,500)
816 (1,500)
816 (1,500)
982 (1,800)
816 (1,500)
982 (1,800)
816 (1,500)
982 (1,800)
816 (1,500)
816(1,500)
816 (1,500)
816(1,500)
Kiln Solids
Test Test temperature, residence
no. material °C (°F) time, hr
1
. 2
3a
3b
Deleted
Deleted
Deleted
Deleted
6
7
Deleted
Deleted
• •-—
M-2 816 (1,500) 0.5
M-5D 816 (1,500) 0.5
0-1 816 (1,500) 0.5
0-1 538(1,000) 0.5




L-2 816(1,500) 0.5
O-2 538 (1,000) 0.75

•
Organic
spiked
No
No
No
No




Yes
Yes

=====
For all tests:
 Total waste/soil feedrate
 Afterburner temperature
 Kiln exit flue gas O2
 Afterburner exit flue gas O2
 Scrubber blowdown rate
 Venturi liquor flowrate
 Venturi pressure drop
 Packed tower liquor flowrate
 Scrubber liquor temperature
55 kg/hr (120 Ib/hr)
1,093° C (2,000° F)
11 percent
7 percent
0 L/min (0 gpm) or minimum operable
76 L/min (20 gpm)
6.2 kPa (25 in WC)
115 L/min (30 gpm)
49° C (120°F)
                                        43

-------
        Table 21 compares the actual test operating conditions to the respective targets for the
 tests performed. As shown in the table, the average kiln temperatures were within about 15° C
 (25° F) of the  target temperatures for  all  of the tests.   Afterburner  temperatures were
 maintained within 3°C (5°F)  of the 1,093°C  (2,000°F) target for all tests. Both kiln exit and
 afterburner exit flue gas O2 levels were somewhat higher than target levels for all tests, however,
 because of excessive air inleakage into the kiln resulting from an inability to tightly secure the
 rotating kiln  seals.

        Table 22 summarizes  the total amount of soil fed to the  RKS for each test, and the
 cumulative amount of kiln ash discharged over each test's duration.  As shown, except for Test 7,
 the weight of ash discharged was generally about 70 percent of the weight of soil fed to the kiln.

 4.1.2   Sampling and Analysis Procedures

        Because the objectives of Tests 1, 2,  3a, and 3b were different from those of Tests 6
 and 7, different sampling and analysis procedures were employed for each test group. However,
 several procedures were performed for all tests, including:

        •     Obtaining a composite sample for the soil feed from each drum before the soil
              was packaged into fiberpack containers

        •     Collecting a composite kiln ash  sample

        •     Collecting a composite scrubber liquor sample

        •     Continuously measuring O2 concentrations at  the kiln  exit;  O2, CO, CO2, and
              TUHC at the afterburner exit; O2, CO2, and NOX at the scrubber exit; and CO and
              TUHC at the stack

        •     Sampling the flue gas at the stack  for HC1 and particulate using a Method 5
              sampling train

        The  above  were the only  sampling procedures employed for  Tests 3a and  3b.  In
addition to the above, the following were performed for Tests 1 and 2:

        •    Sampling the flue gas at the afterburner exit (i.e., upstream of the scrubber) for
             particulate  load  and  for  trace metals (excluding  mercury)  using a  Method 17
             sampling train, modified with multiple metals train impingers

        •    Determining the particle size  distribution of the  afterburner  exit flue gas
             particulating using an Anderson cascade impactor train

        •    Sampling the flue gas upstream and downstream of the scrubber for mercury using
             a Method 101A train at each location

       •    Sampling the flue gas downstream of the scrubber system for particulate and trace
             metals (excluding mercury) using a Method 5 sampling train modified for multiple
             metals capture
                                          44

-------
TABLE 21. TARGET VERSUS ACTUAL OPERATING CONDITIONS FOR THE DRAKE
         CHEMICAL SOIL TESTS
Test
no.
1
2
3a
3b
6
7

Kiln
Afterburner
Target Actual average Actual Actual
temperature, temperature, Target O2, average O2, Target O2, average O2,
° f* (° ¥T"^ * f1 (^ \^\ tffi tyf) ^7o ' /o~
816 (1,500) 826
816 (1,500) 823
816 (1,500) 829
538 (1,000) 546
816(1,500) 822
538 (1,000) 553
(1,519)
(1,513)
(1,524)
(1,015)
(1,512)
(1,027)
TABLE 22. SOIL
Test Test soil






1 (1/30/91)
2 (2/5/91)
3a (1/31/91)
3b (1/31/91)
6 (2/6/91)
7 (2/7/91)
M-2
M-5D
O-l
O-l
L-2
0-2 «
11.0
11.0
11.0
11.0
11.0
11.0
FEED AND
Total soil
fed, kg (Ib)
240 (529)
232 (512)
112(246)
113 (249)
240 (529)
209(460)
13.3 7.0
13.1 7.0
13.8 7.0
17.0 7.0
12.7 7.0
15.4 7.0 .',
ASH COLLECTED
Total ash collected
Weight, Fraction of
kg (Ib) soil fed, %
173 (381) 72
177 (390) 76
74 (163) 66
83 (183) 73
187 (411) 78
183 (404) 88
. 8.7
9.2
9.2
11.8
9.3
9.9






                               45

-------
         In addition to the sampling performed for a}l tests noted above,  the following was
 performed for Tests 6 and 7:

         •    Sampling the flue gas downstream of the scrubber system for semivolatile POHCs
              using a Method 0010 sampling train

         Figure 9 shows the system sampling locations sampled and identifies  the sampling
 procedures used.

         During each test, kiln ash was continuously removed from the ash hopper, via an ash
 auger system, and deposited in a 55-gal drum. Scrubber liquor was completely recycled (zero
 blowdown) for the duration of each test. After flue gas sampling was completed for each test
 (no flue gas sampling was performed for Test 3), soil feed  to the kiln was suspended.  The
 incinerator was operated, firing natural gas auxiliary fuel for a period of 2 hr, or until the kiln
 was visually clear of ash, whichever was longer. After this period, the ash collection drum was
 removed and kiln ash samples taken.  In addition, the entire volume of scrubber system liquor
 was transferred to a storage tank.  During this transfer, a scrubber liquor sample was collected
 from a tap in the transfer line. The scrubber system was then recharged with fresh makeup and
 restarted in preparation for the next test.

         In addition to  analyzing flue gas sampling trains for their sampled analyte set, the
 following were performed for Tests 1, 2, 3a, and 3b.

         •    Analyzing the soil feed  and kiln ash samples for trace metals (arsenic, barium,
             cadmium, chromium, copper, mercury, nickel, lead, selenium, silver, and zinc)

         •    Analyzing the soil and kiln ash TCLP leachates for trace metals

         •    Analyzing the scrubber liquor samples for trace metals

        In addition, for Tests 1 and 2  the following was performed:

        •    Subjecting an aliquot of  the afterburner exit particulate  collected with the
             Method 17 sampling train to the TCLP and analyzing the leachate for trace metals

        For Tests 6 and 7, the analysis protocol included:

        •    Analyzing the soil feed, kiln ash, and scrubber liquor samples for volatile and
             semivolatile organic contaminants

42     TEST RESULTS

        The test program was completed on February 7,  1991. Sample analysis, data reduction,
and test  results interpretation continued through September 1991.  Test report drafting was
nearing completion at the end of FY91.
                                          46

-------
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                               47

-------
Preliminary test conclusions include:

•    Organic contaminants in the test soils can  be destroyed  to  greater  than
      99.99 percent DRE. Naphthalene, spiked into test soils at 3,000 mg/kg for two
      tests (Tests 6 and 7) was destroyed at a  DRE of greater than 99.995 percent.
      1,4-dichlorobenzene, spiked into the test soils at 130 mg/kg for the same two tests,
      was not detected in incineration flue gas; detection limits corresponded to a DRE
      of greater than 99.89 percent.  No treated soil (kiln ash) contained detectable
      levels of organic contaminants.

•    Particulate levels in the flue gas at the exit of the venturi/packed-column scrubber
      APCS were  less than 20 mg/dscm at  7  percent  O2,  in compliance with the
      hazardous waste  incinerator performance  standard  of  180  mg/dscm  at
      7 percent O2

•    None of the soils tested, or the kiln ash resulting from their incineration, would
      be considered a toxicity characteristic (TC) hazardous waste due to its leachable
      trace metal contents

•    No test scrubber liquor (including suspended solids) would be considered a TC
      hazardous waste due to trace metal concentrations. However, lead concentrations
      in test scrubber liquors were at levels over 50 percent of the TC regulatory level
      in some cases.  This suggests that the scrubber liquor discharge from a wet
      scrubber APCS could become a TC hazardous waste in the incineration of "hot
      spot" lead-containing soils, or under scrubber operation at minimum  blowdown.

•     The flyash collected at the afterburner exit  (upstream of the wet scrubber APCS)
     would  be  a  TC  hazardous  waste due  to  leachable  chromium  and  lead
      concentrations.  This suggests that  the collected particulate  from a dry ACPS
      (such as a fabric filter) would be a TC hazardous waste.
                                  48

-------
                                     SECTION 5

            INCINERATION OF PCB-CONTAMINATED SEDIMENTS FROM
                  THE NEW BEDFORD HARBOR SUPERFUND SITE
        EPA Region 1 is conducting the remedial design (RD)  for the remediation of a
Superfund site located in New Bedford Harbor near New Bedford,  Massachusetts.  According
to the record of decision (ROD) document of 1990, the EPA has identified approximately
10,000 yd3 of contaminated sediment in the harbor. Incineration of the dredged sediment is the
selected treatment option. In support of the RD, incineration technologies will be examined to
determine the optimum equipment configuration and incinerator operating parameters for the
waste material. The EPA (M. Sanderson, Region 1;K. Howe, USAGE, coordinators) requested
that test burns be conducted at the IRF to support the RD for  this Superfund site.

        The sediment at the New Bedford Harbor site is contaminated with from 4,000 ppm to
more than 200,000 ppm of PCBs.  In addition to PCBs, other contaminants are present, including
polynuclear  aromatic hydrocarbons (PAHs), and trace metals (copper, chromium, lead, and
cadmium).  The primary objective of this test program was to  obtain data to support the RD
plans and specifications.   Therefore,  the test  conditions were  designed to evaluate the
effectiveness of varying incinerator operating conditions in the destruction of PCBs and other
pollutants. Specifically, the test program attempted to answer these questions:

        •    Can incineration effectively destroy PCBs to the required destruction and removal
             efficiency (DRE) of 99.9999 percent?

        •    What is the distribution of the contaminant trace  metals in the discharge streams
             during incineration of the sediment?

        •    What are the  effects of incineration excess  air and temperature on organic
             constituent destruction and metals distributions, including the leachability of the
             metals from the kiln ash?

        •    What is the effectiveness of the air pollution control system (APCS) in collecting
             particulate and trace metals?

        •    Can the treated sediment (i.e., kiln ash) from the incinerator be disposed of as
             non-hazardous solid waste?

        The test program consisted of a set of three incineration tests in the RKS at the IRF.
These tests were aimed at evaluating PCB destruction, and the fate of contaminant trace metals

                                         49

-------
in the sediment, as functions of kiln temperature and kiln excess air level. The tests were
performed in the RKS with the venturi/packed-column scrubber as the primary APCS. The
following subsections document the findings of the test program.
5.1
TEST PROGRAM
        Eight 30-gal drums of sediments were dredged from the Hot Spot area of New Bedford
Harbor for these tests. A characterization sample representing each drum dredged was shipped
to the IRF  for pretest analyses.   These samples were subjected  to  proximate, PCB,  and
hazardous constituent trace metals analyses.  The results of these analyses showed that the
average total PCB concentration of the eight drums was 5,300 ppm, as received.  The level
required in an RKS feed to  be able to just establish 99.9999 percent DRE at a typical RKS
feedrate of 68 kg/hr  (150 Ib/hr)  is  5,100 ppm,  just below  the average dredged drum
characterization sample level. Consequently, it was decided to spike the test sediment to higher
PCB concentrations to provide a margin in the ability to establish 99.9999 percent DRE.  The
material used to spike the sediments was an Askarel transformer fluid comprised of roughly
75 percent Aroclor 1242 and  25 percent Aroclor 1254.

        For the test program, all eight drums of sediment were shipped to the IRF, where they
were combined to form one test feed material.  Prior to testing, the combined sediments were
repackaged into 1.5-gal fiberpack containers for feeding to the RKS via the ram feeder system.
The PCB spike was added to the sediments during this packaging.   In addition  to spiked
sediments, a number of fiberpack drums were prepared without the PCB spike for testing using
only the native sediment.

5.1.1    Test Conditions

        The test series was designed to evaluate the effects of incinerator operating conditions
on PCB destruction and trace metal distributions in the incinerator discharge streams.  The
operating parameters to be varied were kiln exit temperature and kiln excess air (exit flue gas
O2). Three tests were to cover the range of target kiln exit flue gas temperatures of 816°  and
982°C (1,500° and 1,800°F) and target kiln exit O2 levels of 6 to 10 percent. For all tests, the
operating conditions noted in Table 23 were to be held at the nominal values noted in the table.
  TABLE 23.  INCINERATOR SYSTEM OPERATING CONDITIONS HELD CONSTANT
         Kiln solids residence time

         Total sediment feedrate

         Scrubber blowdown rate

         Venturi liquor flowrate

         Venturi pressure drop

         Packed tower liquor flowrate

         Scrubber liquor temperature
                                 0.5 hr

                                 68.2 kg/hr (150 Ib/hr)

                                 0 L/min (0 gpm) or minimum operable

                                 76 L/min (20 gpm)

                                 6.2 kPa (25 in WC)

                                 115 L/min (30 gpm)

                                 49°C (120°F)
                                         50

-------
        Table 24 summarizes the actual incinerator exit temperatures  and flue  gas levels,
including their ranges and averages for each test during flue gas sampling.  These are compared
with the respective target conditions. During Test 3, unspiked native sediment was fed to the
kiln for a period of time to collect kiln ash associated with native sediment feed only. Test 3a
represents the period of native sediment feed; Test 3b represents the period of spiked sediment
feed for the third test.

        For all tests, the average kiln exit temperature was within 8°C (16°F) of the respective
target temperature.  The actual O2 levels at the kiln exit were generally higher than the target
concentrations.  The higher  O2 levels experienced resulted from  higher than expected  air
inleakage into the kiln chamber due to the inability to tightly secure a rotating kiln seal. The
minimum O2 achievable was 9  percent at the kiln exit. The maximum O2 tested was 11.2 percent.
As a  practical  matter,  these two  levels  present comparable combustion  environments.
Consequently, it was not possible to test kiln excess air as a variable.

5.12    Sampling and Analysis Procedures

        The scope of the sampling effort undertaken during this test program is illustrated in
Figure 10, in which the sampling locations and the corresponding sample collection methods are
identified.  Specifically, the sampling effort during each test consisted of:

        •    Collecting a composite sample of the kiln ash

        •    Collecting a composite sample of the scrubber liquor

        •    Continuously measuring O2 levels in the kiln exit and afterburner exit flue gases;
             O2, CO, CO2, NOX, and TUHC levels at the venturi/packed-column scrubber exit;
             and O2, CO, and CO2 levels in the stack

        •    Sampling flue gas at the scrubber system exit for PAHs and PCBs

        •    Sampling flue gas at the scrubber system exit for polychlorinated dibenzo-p-dioxins
             (PCDDs) and dibenzofurans (PCDFs)

        •    Sampling flue gas at the scrubber system exit for volatile organics

        •    Sampling flue gas upstream of the scrubber system for particle size distribution

        •    Sampling flue gas upstream and downstream of the scrubber system for particulate
             and trace metals, using a variation of EPA Method 5 modified for multiple metals
             capture

        •    Sampling downstream of the scrubber system and at the stack downstream of the
             secondary APCS for particulate and HC1 using Method 5 to comply with permit
             requirements

In addition, grab/composite samples of the sediment feed from each drum were taken before
the sediments were mixed, and a grab/composite sample of the mixed sediment feed was taken.

                                          51

-------

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                               53

-------
        Each test was run with scrubber  system  operating at,  or  near, total recycle  (zero
 blowdown). At the conclusion of each test day, the  incinerator was operated on natural gas for
 2 hr after waste feed cessation. After the 2-hr cleanout time, the scrubber system was drained
 to a storage tank. A composite scrubber liquor sample was collected from the collection tank
 after draining was complete,  and a composite kiln ash sample was collected from the ash
 collection system drum.

        The sample collection procedures resulted in eight individual sediment samples and one
 composite sediment sample.  One sample of the PCB spike material was taken, resulting in a
 total of 10 feed samples for the test series. One set  of kUn ash samples was taken for each test.
 This  included the period of time with native sediment  only  as  the  feed.   No  flue gas
 characterization was done during the native sediment feed period; however, one set of flue gas
 characterization samples was collected during spiked sediment feed periods for all three tests.
 Scrubber liquor samples were collected for all tests.

        An aliquot of the composited sediment feed and each test's kiln  ash was subjected to
 the TCLP leaching procedure and analyzed for cadmium, chromium,  copper, and lead. Waste
 feed samples,  kiln ash samples, and scrubber liquor samples were analyzed separately for PCBs,
 PAHs, and cadmium, chromium, copper, and lead.  The composite sediment feed sample was
 also subjected to proximate (moisture, ash content, and heat content) analysis, and ultimate (C,
 H, O, N, S, Cl) analysis.
5.2
TEST RESULTS
        The results of the test program are discussed in the subsections that follow.  Test results
are grouped by analyte class.

52.1    Proximate and Ultimate Analysis Results

        The proximate and ultimate analysis results for the composite sediment sample analyzed
are presented in Table 25.  The high moisture content of the test sediments is consistent with
their marine origin. Table 26 summarizes the cumulative sediment weight fed for each test and
the total amount of kiln  ash collected. As indicated in the table, between 25 and 30 percent of
the sediment weight fed for a given test was collected as kiln ash. This fraction agrees quite well
with the ash content of the sediment obtained by proximate analysis shown in Table 25.

523,    PCB, Semivolatile and Volatile Organic, and Dioxin/Furan Analysis Results

        Table 27 summarizes the PCB contents of each incineration test sample.  As indicated,
the spiked sediment feed contained 3.48 percent Aroclor 1242 and 1.11 percent Aroclor 1254.
The kiln ash resulting from the  incineration of the sediments (both spiked and native) had
substantially reduced, though still significant, PCB contents. The kiln ash for the spiked sediment
feeds contained between 96 and 177 mg/kg of Aroclor 1242, and between 32 and 84 mg/kg of
Aroclor 1254.  Interestingly, within the  range of the variability of the  data, the  higher kiln
temperature tested for  Tests 2  and 3  did not  result in  significantly  lower kiln ash PCB
concentrations than the lower temperature tested in Test 1.  The kiln ash resulting from native
sediment feed also contained significant PCB levels.
                                          54

-------
TABLE 25. PROXIMATE AND ULTIMATE ANALYSIS RESULTS
          FOR THE COMPOSITE SEDIMENT FEED SAMPLE
        . Proximate Analyses
          Moisture, %                      63.9
          Ash,%                          28.5
          Volatile matter, %                  5.9
          Fixed carbon, %                   1.4
          Higher heating value, kJ/kg        2,200
                             (Btu/lb)      (948)
         Ultimate Analysis, %
          C                               11.1
          H                               1-2
          N                  '             0.4
          S                               0.6
          Cl                               0.9
     TABLE 26. SEDIMENT FEED AND ASH COLLECTED
Ash collected

1
2
3a
3b
Test
(3/15/91)
(3/19/91)
(3/21/91)
(3/22/91)
Total sediment fed,
kg(lb)
284 (625)
284 (625)
229 (504)
318(700)
Weight,
kg(lb)
85 (187)
76 (168)
62 (136)
80 (175)
Fraction of
feed,
%
30
27
27
25
                           55

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                         TABLE 27.  PCB ANALYSIS RESULTS
                                                   PCB concentration
                          Sample
Aroclor 1242  Aroclor 1254
              Spiked sediment feed, %                3.48
              Test 1:
               Kiln ash, mg/kg                       133
               Scrubber liquor, |ig/L                  < 1
               Scrubber exit flue gas, jig/dscm         0.76
              Test 2:
               Kiln ash, mg/kg                        96
               Scrubber liquor, ng/L                  < 1
               Scrubber exit flue gas, jig/dscm         0.54
              Test 3b:
               Kiln ash, mg/kg                       177
               Scrubber liquor, ng/L                  < 1
               Scrubber exit flue gas, ng/dscm       <0.26
              Composite native feed, mg/kg         4,850
              Test 3a:
               Kiln ash, mg/kg                        57
               Scrubber liquor, |ig/L                  < 1
                    1.11


                     84
                   <0.3
                    0.22


                     32
                   <0.3
                    0.21


                     68
                   <0.3
                  <0.09
                  1,300


                     44
                   <0.3
        No scrubber liquor sample contained detectable PCB at practical quantitation limits
(PQLs) of 1 (ig/L for Aroclor 1242, and 0.3 |ig/L for Aroclor 1254. The scrubber exit flue gas
contained low, though measurable, levels of both PCB formulations in Tests 1 and 2.

        Table 28 summarizes the degree of PCB decontamination achieved in each test, in terms
of the fraction of the amount of PCB introduced in the incinerator feed accounted for by the
resulting kiln ash. As shown in the table, about 0.1 percent of the Aroclor 1242 and about 0.1 to
0.2 percent of the Aroclor 1254 feed in spiked sediments was accounted for in the kiln  ash
produced.  The remaining 99.8 to 99.9 percent was removed and largely destroyed, as discussed
below. Higher fractions of feed PCBs were present in the kiln ash from the native sediment test:
0.3 percent for Aroclor 1242, and 0.9'percent for Aroclor 1254.

        The data shown in Tables 27 and 28 confirm that incineration under the conditions
tested was not  sufficient to completely decontaminate  the  sediments.   The incineration
temperatures tested, 820° to 980° C (1,500° to 1,800° F), were typical of those that have resulted
in successful decontamination, as was the kiln solids residence time (0.5 hr).  However, the New
Bedford Harbor  marine sediments contained substantial moisture, over 60 percent.  Evidently,
with such high moisture content, solids bed temperatures were not raised to levels needed for
more complete PCB destruction in the residence time available. It is suspected that longer solids
residence times, perhaps on the order of 1 hr, would allow essentially complete, or certainly more
complete, PCB decontamination.
                                          56

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TABLE 28. PCB DECONTAMINATION EFFECTIVENESS
Parameter
Test 1:
Sediment feed
Concentration, %
Amount fed, kg
Kiln ash
Concentration, mg/kg
Amount discharged, g
Fraction of amount fed, %
Test 2:
Sediment feed
Concentration, %
Amount fed, kg
Kiln ash
Concentration, mg/kg
Amount discharged, g
Fraction of amount fed, %
Test 3a:
Sediment feed
Concentration, %
Amount fed, kg
Kiln ash
Concentration, mg/kg
Amount discharged, g
Fraction of amount fed, %
Test 3b:
Sediment feed
Concentration, %
Amount fed, kg
Kiln ash
Concentration, mg/kg
Amount discharged, g
Fraction of amount fed, %
Aroclor 1242


3.48
9.87

133
11.3
0.11


3.48
9.87

96
7.3
0.07


0.485
1.11

57
3.5
0.32


3.48
11.05

177
14.1
0.13
Aroclor 1254


1.11
3.15,

84
7.1
0.22


1.11
3.15

32
2.5
0.08


0.130
0.30

44
2.7
0.91


1.11
3.52

68
5.3
0.15
                    57

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        Table 29 takes the scrubber exit flue gas PCB concentrations noted in Table 27, and
combines them with sediment feedrate and  flue  gas flowrate data to give  the PCB  DREs
achieved  for  the  tests.   As shown  in the table, greater than  the  regulation-required
99.9999 percent PCB ORE was achieved for all three tests.

        No PAH compounds analyzed for were detected in any sample at PQLs of 50 mg/kg in
sediment feed, 1.3 mg/kg in kiln ash, 20 ng/L in scrubber liquor, and 6 ng/dscm in scrubber exit
flue gas.

        Results of the scrubber exit flue gas PCDD/PCDF measurements are summarized in
Table 30.  As shown, total tetra-CDD (TCDD), penta-CDD (PeCDD), hexa-CDD  (HxCDD),
and hepta-CDD (HpCDD) levels were in the nominal 0.01 to 0.02 ng/dscm range for all three
tests, with octa-CDD (OCDD) levels in the 0.03 to 0.06 ng/dscm range.  Flue gas PCDF levels
were significantly greater, ranging up to about 2.8 ng/dscm for TCDF.  The  2,3,7,8-TCDD
toxicity equivalents corresponding to the isomer concentrations noted are also given in Table 30.
As shown, the scrubber exit flue gas PCDD/PCDF levels corresponded to 2,3,7,8-TCDD toxicity
equivalents ranging from nominally 0.05 to 0.10 ng/dscm.

5.23    Trace Metal Discharge Distributions

        Two primary objectives of the test program were to evaluate the fate of the contaminant
trace metals cadmium, chromium, copper, and lead in the incineration treatment of the New
Bedford Harbor sediments, and to investigate whether incineration  conditions affected the
distribution  of these metals in  the  incinerator discharges.  Table 31  summarizes  the
concentrations of the test metals in sediment samples and in each of the incinerator discharge
streams.
                               TABLE 29. PCB DREs
Parameter
Sediment feed:
Sediment feedrate, kg/hr
Aroclor 1242 feedrate, g/hr
Aroclor 1254 feedrate, g/hr
Scrubber exit flue gas:
Flue gas flowrate, dscm/min
Aroclor 1242 concentration, |ig/dscm
emission rate, ng/hr
DRE, %
Aroclor 1254 concentration, iig/dscm
emission rate, jig/hr
DRE, %
Test 1
(3/15/91)

69.5
2,420
773

33.9
0.76
1.6
99.999936
0.22
0.5
99.99994
Test 2
(3/19/91)

69.5
2,420
773

32.9
0.54
1.1
99.999956
0.21
0.5
99.99994
Test 3b
(3/21/91)

69.3
2,410
771

30.6
<0.26
<0.5
> 99.999980
<0.09
<0.2
> 99.99998
                                        58

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  TABLE 30. FLUE GAS PCDD/PCDF ANALYSIS RESULTS

Analyte
Total TCDD
2,3,7,8-TCDD
Total PeCDD
1,2,3,7,8-PeCDD
Total HxCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
Total HpCDD
1,2,3,4,6,7,8-HpCDD
OCDD
Total TCDF
2,3,7,8-TCDF
Total PeCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
Total HxCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
Total HpCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
2,3,7,8-TCDD equivalents
Scrubber exit
flue gas concentration,
ng/dscm
Test 1 Test 2
(3/15/91) (3/19/91)
0.016
0.003
0.005
0.002
0.011
0.001 '
0.001
0.002
0.008
0.0083
0.043
2.79
4.60
0.78
0.075
0.089
0.13
0.035
0.013
0.016
0.001a
0.005
0.0 lla
0.002
0.013
0.104
0.010
0.003
0.010
0.001a
0.008
0.0013
0.001
< 0.001
0.023
0.013
0.060
1.78
2.80
0.30 '
0.033
0.030
0.070
0,020
0.008
0.010
0.001
0.020
0.010
0.003
0.010
0.052
Test 3b
(3/21/91)
0.008
0.003
0.005
< 0.003
0.008
< 0.003
< 0.002
< 0.003
0.019
0.008
0.030
1.48
2.70
0.43
0.035
0.046
0.15
0.038
0.014
0.022
< 0.002
0.002
0.0223
0.005a
0.016
0.062
"Estimated maximum possible concentration.
                         59

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                   TABLE 31. TRACE METALS ANALYSIS RESULTS
                         Sample
        Sediment feed:

         Composite, mg/kg
         Composite TCLP leachate, mg/L

        Test 1 (3/15/91):

         Kiln ash, mg/kg
         Kiln ash TCLP leachate, mg/L
         Afterburner exit flue gas, fig/dscm
         Scrubber exit flue gas, jig/dscm
         Scrubber liquor, mg/L

        Test 2 (3/19/91):
         Kiln ash, mg/kg
         Kiln ash TCLP leachate, mg/L
         Afterburner exit flue gas, ug/dscm
         Scrubber exit flue gas, jig/dscm
         Scrubber liquor, mg/L

        Test 3a (3/21/91):

         Kiln ash, nig/kg1

        Test 3b (3/21/91):
         Kiln ash, mg/kg
         Kiln ash TCLP leachate, mg/L
         Afterburner  exit flue gas, ug/dscm
         Scrubber exit flue gas,  ug/dscm
         Scrubber liquor, mg/L

        TCLP regulatory level, mg/L
 Cd
 Cr
 Cu
7.4
0.11
 161
0.041
 308
0.066
2.3    367
        785
1.0
 5.0     -a
Pb
236
1.2
9.5
0.26
42.3
34.9
0.14
376
0.048
219
158
1.9
608
6.3
571
421,
4,5
277
0.71
1,030
903
8.8
2.7
0.046
77.6
55.3
0.27
434
0.030
136
73.2
1.4
828
3.01
768
436
2.6
75.6
0.17
1,814
1,273
5.4
        96
2.0
0.043
51.6
79.0
0.73
357
0.03
126
83.9
1.3
721
3.0
519
750
3.4
62
0.41
984
2,020
5.6
        5.0
             Not a TCLP metal.
        The concentrations of chromium and copper in resulting kiln ashes were higher than the
composite sediment feed sample for all tests, and were higher for cadmium and lead for the low-
kiln-temperature test (Test 1). This reflects the weight reduction in going from sediment to kiln
ash during incineration.  However, the cadmium and lead concentrations in kiln ash were
significantly lower in the high-kiln-temperature tests (Tests 2 and 3) when compared to the
Test 1 kiln ash concentrations; and were also lower than the corresponding sediment feed
concentrations.  Flue gas cadmium and lead concentrations, both in the afterburner exit flue gas
and the scrubber exit flue gas were generally higher  for Tests 2 and 3 than for Test 1  as well.
Both these trends are the result of the volatile  behavior of these two metals.  The extent of
volatilization of these metals was evidently higher in Tests 2 and 3 than in Test 1, giving rise to
                                         60

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lower kiln ash, and generally higher flue gas, concentrations of these metals for the higher
temperature tests.

        Table 31 also notes the TCLP regulatory limit for the three TCLP metals determined.
Comparing composite feed and kiln ash TCLP leachate and scrubber liquor metal concentrations
to the TCLP regulatory levels shows that neither the composite sediment feed nor any test's kiln
ash would  be a toxicity characteristic (TC) hazardous waste based on leachable cadmium,
chromium, or lead concentrations.

        The scrubber liquor cadmium and chromium concentrations noted in Table 31 are below
the TCLP regulatory level for all three tests.  In contrast, the scrubber liquor lead concentrations
exceed the regulatory level for all three tests. However, the scrubber liquor metal concentrations
noted in the  table are for the total scrubber liquor, which contains suspended solids.  A true
TCLP leachate was prepared from the three-test composite scrubber liquor which was held in
a storage tank until all analyses were completed. In accordance with the procedure,  a sample
of the scrubber liquor was filtered and the percent solids  content was measured.  If the solids
content is less than 0.5 percent, the procedure specifies  discarding the solids and using the
filtrate as the TCLP leachate. As this was the case, the filtrate was analyzed for lead and found
to contain 4.2 mg/L, less than the TCLP regulatory level.  Thus, the scrubber liquor for these
tests was also not a TC hazardous waste.

        The  metal concentrations shown in Table 31 can be  combined with feed  soil  and
discharge stream mass flowrate information to better show how the metals distribute among the
discharge streams as a function of incineration condition.  These distributions are summarized
in Table 32.  The distribution fractions in Table 32 have been normalized to the total amount
of each metal measured in all the discharge streams analyzed.  Thus, these normalized values
represent fractions that would have resulted had mass balance closure in each case been 100
percent.  Note  that the sum of the normalized values (the totals) for  each metal  is indeed
 100 percent in Table 32. Use of distribution fractions normalized in this manner allows clearer
data interpretation, because they remove variable mass balance closure as a source of test-to-test
data variability.

         Actual  mass balance closures achieved around the conventional incineration system
portion of the RKS ranged from 52 to 103 percent for cadmium, 72 to 79 percent for chromium,
 71 to 86 percent for copper, and 38 to 66 percent for lead. These levels of mass balance closure
 are considered excellent when viewed in light of past experience on achieving trace metal mass
 balance closures from a variety of combustion sources,  incinerators included.  Typical  mass
 balance closure results from this past  experience have been, at best, in the 30 to 200 percent
 range.

         Several interesting observations emerge from the data in Table 32. The first is that, in
 these tests,  chromium and copper  exhibited relatively  nonvolatile behavior.  The kiln ash
 discharge represented the predominant fraction of metal discharged for these two metals.  The
 kiln ash accounted for 88 to 92 percent of the chromium discharged and 82  to 89 percent of the
 copper discharged.  Further, these distributions were not affected by kiln temperature in the
 range varied (i.e., 824° to 985°C [1,516° to 1,805°F]).
                                           61

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              TABLE 32. NORMALIZED TRACE METAL DISTRIBUTIONS
Test

Kiln exit temperature, °C
(°F)
Kiln exit O2, %
1
(3/15/91)
824
(1,516)
11.2
2
(3/19/91)
984
(1,803)
9.0
3b
(3/21/91)
985
(1,805)
10.0
                                          Distribution, % of metal measured
             Cadmium
              Kiln ash
              Scrubber exit flue gas
              Scrubber liquor
               Total
             Chromium
              Kiln ash
              Scrubber exit flue gas
              Scrubber liquor
               Total
             Copper
              Kiln ash
              Scrubber exit flue gas
              Scrubber liquor
               Total
             Lead
              Kiln ash
              Scrubber exit flue gas
              Scrubber liquor
               Total
 61
 23
 16
100


 88
  4
  8
100


 83
  6
 11
100


 53
 17
 30
100
 19
 42
 39
100


 92
  2
  6
100


 89
  5
  6
100


 23
 42
 35
100
  8
 36
 56
100


 92
  2
  6
100


 82
 10
  8
100


 19
 55
 26
100
        In contrast, cadmium and lead exhibited relatively volatile behavior.  At the low-kiln-
temperature test (Test 1) conditions, the kiln ash accounted for 53 (lead) to 61 (cadmium)
percent of the metals discharged.  Even at this relatively  low incineration temperature, a
significant amount of each metal evidently vaporized in  the kiln  and was carried into the
afterburner and downstream to augment the amount entrained in flyash carried out of the kiln.

        The extent of evident vaporization was enhanced at the high-temperature-test (Tests 2
and 3) condition. For these tests, the kiln ash accounted for significantly decreased fractions of
cadmium and  lead discharged, 8 to 19 percent for cadmium and 19 to  23 percent for lead.
Scrubber exit flue gas and scrubber liquor fractions were higher than the kiln ash fractions at this
high-temperature condition.  Indeed, 36 to 42 percent of the cadmium discharged and 42 to
55 percent of  the lead discharged escaped the incineration  system and  the  venturi/packed-
column scrubber.
                                         62

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        Table 33 summarizes the apparent scrubber collection efficiencies calculated for each
metal measured in the test program.  In calculating apparent collection efficiency, it is assumed
that the flowrate of metals at the scrubber inlet can be obtained by summing the flows in the two
scrubber discharge streams:  the scrubber exit flue gas and the scrubber liquor. In other words,
apparent scrubber collection efficiency is defined to be (scrubber liquor fraction)/(scrubber
liquor fraction plus scrubber exit flue gas fraction). The data in Table 33 show that, at the low-
kiln-temperature test condition, apparent collection efficiencies for chromium, copper, and lead
were comparable, and in the nominal 65 to 70 percent range.  Collection efficiency for cadmium
was lower at 41 percent.  At the high-kiln-temperature test condition, cadmium and chromium
efficiencies were relatively unchanged.  Copper and lead collection efficiencies decreased.

52.4    Participate and HC1 Emissions Data

        Table 34 gives the particulate levels measured at the  scrubber exit. For the three tests,
flue gas particulate levels at the scrubber exit ranged  from 70 to 101 mg/dscm (corrected to
7 percent O2).  These levels were below the 180 mg/dscm (at  7 percent O2) hazardous waste
incinerator performance standard.

        The sediments incinerated  during this test program contained 0.85 percent chlorine.
Table 35 summarizes the levels of HC1 measured at the scrubber. Measured HC1 concentrations
at the scrubber exit ranged from 0.2 to 2.4 ppm, with corresponding emission rates ranging from
0.7 to 7.2 g/hr.  These emission  rates were  less than  the hazardous waste incinerator
performance standard floor of 2 kg/hr.  The scrubber system  HC1 collection efficiencies ranged
from  98.8 to 99.9 percent of the chlorine fed.

        Figure 11  illustrates  the results of the  particle size measurements performed  at the
afterburner exit.  In performing the particle size sampling,  it  was observed that the cascade
impactor sampling nozzle collected  noticeable amounts of particulate on  its inside wall. This
particulate adhered to the probe wall, and could not be recovered and weighed accurately. Thus,
it is  believed that a significant  amount of the flue  gas particulate  could have  been left
unaccounted for in the afterburner exit particle sizing measurements.

        The data in Figure 11 show that the afterburner exit size distributions were comparable
for Tests 2 and 3b, which were performed  at comparable incineration conditions.  The size
distribution for the low-temperature test (Test 1) was coarser.  Nonetheless, even for Test 1,
more than 50 percent of the measured particulate matter at the afterburner exit was smaller than
0.6 \im.  For Tests  2 and 3,  more than 70 and 80 percent, respectively, of the captured
particulate was smaller than 0.6 jim.  One explanation for the finer particles in Tests 2 and 3
could be the higher kiln temperature during these two tests,  985° C (1,805° F), compared to
824° C (1,516° F) during Test 1. This observation is consistent with the expectation that high
combustion temperature can favor the formation of fine particles via the vaporization and
condensation mechanism.
                                           63

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    TABLE 33. APPARENT SCRUBBER COLLECTION EFFICIENCIES
Test

Kiln exit temperature, °C
(°F)
Kiln exit O2, %
1
(3/15/91)
824
(1,516)
11.2
2 3b
(3/19/91) (3/21/91)
984 985
(1,803) (1,805)
9.0 10.0
Apparent scrubber collection

Cadmium
Chromium
Copper
Lead

41
69
66
64
efficiency, %
48 50
79 62
53 33
45 23
            TABLE 34.  FLUE GAS PARTICULATE LEVELS
                      Test
Scrubber exit flue
 gas participate,
mg/dscm at 7% O2
                Test 1 (3/15/91)
                Test 2 (3/19/91)

                Test 3b (3/21/91)
       70
       82

      101
                 TABLE 35. FLUE GAS HC1 LEVELS
             Parameter
     Test 1
   (3/15/91)
 Test 2
(3/19/91)
 Test 3b
(3/21/91)
Cl feedrate, g/hr
Scrubber exit
 Flue gas HC1 concentration,
      591
   591
   589
mg/dscm
ppm
Flue gas emission rate, g/hr
System collection efficiency, %
0.31
0.2
0.68
99.9
3.60
2.4
7.24
98.8
1.14
0.8
2.10
99.6
                               64

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  99.98
 g  93
 CD
 °-84

 I
 JO  70
 3


 O  5°

     30
       0.5
1.0
                2.0               5.0
              Particle size (microns)
Figure 11. Afterburner exit particle size distributions
                                                                 10.0
                                                          20.0
53      CONCLUSIONS

        Test conclusions are as follows:

        •    Greater than 99.9999 percent DRE of the PCBs in the site sediments can be
             achieved at incineration temperatures  of both 824° C (1,516° F)  and 984° C
             (1,803° F) in a rotary kiln with an afterburner operated at 1,208° C (2,206° F).
             However, with a kiln solids residence time of 0.5 hr, the treated sediments (kiln
             ash) are still PCB-contaminated.  In tests with a PCB-spiked sediment feed, the
             kiln ash discharge accounted for between 0.07 and 0.22 percent of the PCB fed in
             the spiked feed regardless of kiln temperature. For a native (unspiked) sediment
             feed, the kiln ash accounted for 0.32 to 0.91 percent of the PCBs introduced in the
             sediment feed.

        •    The APCS discharge flue gas from the incineration of the sediments contained low
             levels of PCDDs and higher levels of PCDFs, chiefly total TCDF, total PeCDF,
             and total HxCDF.  The 2,3,7,8-TCDD  toxicity equivalent levels were in the
             nominal 0.05 to 0.10 ng/dscm range. PCDD/PCDF emissions were not affected
             by kiln temperature.
                                          65

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         •    Of the contaminant trace metals, chromium and  copper  were  relatively
              nonvolatile.  The kiln ash discharge accounted for nominally 80 to 90 percent of
              the discharged amounts of these metals. These fractions were not affected by the
              range of kiln temperatures tested.

         •    Of the contaminant trace metals, cadmium and lead exhibited relatively volatile
              behavior, and  increasingly so at the high kiln  temperature (984° C [1,803° FJ).
              The kiln ash discharge accounted for 53 percent of the lead and 61 percaftt of the
              cadmium discharged at  the low kiln temperature (824° C  [1,516° F]).   These
              fractions decreased to the nominal 10 to 20 percent range for cadmium and the
              20 percent range for lead, at the high kiln temperature.  Scrubber exit flue gas
              fractions (cadmium and lead) and scrubber liquor fractions (cadmium) increased
              accordingly.

         •    Apparent scrubber collection efficiencies were in the nominal 65 to 70 percent
              range for chromium, copper, and lead at the low kiln temperature, and lower, at
              41 percent, for cadmium. Cadmium and chromium collection efficiencies were
              apparently unaffected by increased kiln temperature, although copper and lead
              collection efficiency decreased to the 33 to 53 percent range for  copper, and the
              23 to 45 percent range for lead.

        •    Neither treated sediments nor the scrubber liquor discharges would exhibit the TC
              based on their cadmium,  chromium, or lead concentrations.

        No conclusions regarding the effects of variations in kiln excess air levels on organic
constituent destruction and metals distributions were possible, as little variation in kiln excess
air level could be operationally achieved.

       ^The test results suggest that incineration would be an effective treatment option for the
site sediments. However, sediment dewatering prior to incineration, or incinerating at higher
kiln solids residence times (perhaps up  to 1 hr), might be required to yield a treated sediment
not contaminated by PCBs.

        Test results were reported in the following  report:

        •    Whitworth, W. E., and  L.  R.  Waterland, "Pilot-Scale Incineration of  PCB-
             Contaminated Sediments from the New Bedford Harbor Superfund Site," draft
             September 1991.
                                          66

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                                     SECTION 6

         FATE OF TRACE METALS IN THE ROTARY KILN SYSTEM WITH A
                CALVERT FLUX/FORCE CONDENSATION SCRUBBER
        Risk assessments have suggested that trace metal emissions from some incinerators
treating waste streams with high levels of metals could pose unacceptable risks to human health
and the environment. Despite their importance, available field data on the fate of trace metals
from hazardous waste incinerators are limited.  Data describing the effects of incinerator
operation and waste composition on trace metal fate are particularly lacking.  Data to evaluate
the effectiveness of typical APCSs for collecting flue gas metals are also needed.

        In response to these data needs, two extensive test programs were completed using the
RKS at the IRF in FY88 and FY89. Both test programs were performed to support regulations
development by EPA's OSW (S. Garg, R. Holloway, coordinators). These tests quantified the
distribution of metals among the discharge streams of the RKS, and identified the  effects of kiln
temperature,  afterburner temperature, and waste feed chlorine  content on* these discharge
distributions.

        For both test programs, kiln temperature was varied from nominally 816 to 927° C (1,500
to 1,700°F); afterburner temperature was varied  from  nominally 982 to 1,204°C (1,800 to
2,200° F); and waste feed chlorine content was varied from 0 to nominally 8 percent.  The main
difference between the two programs was the primary APCS used.  A venturi/packed-column
scrubber was used in the first test program (FY88); a single-stage ionizing wet scrubber was used
in the second test program (FY89).

        The feed for both test programs consisted of a synthetic waste containing organics
premixed with a clay absorbent material. Toluene, tetrachloroethylene, and chlorobenzene were
used as the organic compounds, and the waste feed chlorine content was altered by adjusting
their ratio in the mixture. The synthetic waste was continuously fed to the kiln by a screw
feeder.  The test metals were combined  in an aqueous solution and spiked onto the  solid
material as it was fed to the kiln. Five hazardous constituent metals were used: arsenic, barium,
cadmium, chromium, and lead.  In addition, the nonhazardous constituent trace elements
bismuth, copper, magnesium,  and strontium were also incorporated into the  test feed for
comparison and to provide data to evaluate a  predictive numerical model under development
in another effort within  RREL.

        The results of the two completed test programs have shown the following:
                                          67

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         •    Cadmium and  bismuth are relatively volatile, averaging less than 40 percent
               discharged to the kiln ash. The other metals are relatively nonvolatile, averaging
               greater than 75 percent discharged to the kiln ash.  Lead was the only exception,
               exhibiting volatile behavior in the first test program and relatively nonvolatile
               behavior in the second.

         •    Increased kiln temperature in the presence of feed chlorine caused  increased
               volatility of bismuth, cadmium, and lead. Data were not obtained to evaluate the
               effects of kiln temperature in the absence of feed chlorine.

         •    Afterburner temperature did not affect metal partitioning among the scrubber exit
               flue gas and scrubber liquor discharge streams. There was no conclusive evidence
               indicating an effect on scrubber collection efficiency for metals.

         •    The effect of the waste feed chlorine content on the partitioning of metals was not
               consistent between the two test programs.  Data  from the first test program
               indicated increased volatility with increased chlorine for copper and lead.  Data
               from the second test program showed that waste feed chlorine content did not
               affect metal discharge distributions within limits of data variability established by
               replicate test conditions.

         •     Further sample analysis has shown that Method 3050  may not  be sufficiently
               aggressive to fully liberate the metals from the clay feed  and kiln ash.  Metal
               recoveries achieved with sample preparation by fusion methods were about twice
               the recoveries achieved  by Method 3050.

         •     Relative  metal volatilities agreed  with expectations based on metal  volatility
              temperatures with the exception of arsenic, which  was much  less volatile than
              expected for  feeding arsenic as As2O3.  Dissolving  As2O3 in solution  results in
              AsO3" anion, which could be much less volatile than As2O3 or perhaps adsorbed
              onto the clay matrix. The other spiked metals were  added to the feed as soluble
              nitrates dissolved as soluble cations.

         •     The four nonhazardous constituent metals behaved similarly to the hazardous
              constituent metals; no unique information was obtained.

         •     Flue gas sampling using a Method 0030 volatile organic sampling train (VOST)
              provided  no significant information on PIC formation.

        The IRF trace metal research program continued in FY91 with the completion of a third
parametric test program. For the FY91 program, a Calvert Flux Force/Condensation Scrubber
pilot plant  was installed as the primary APCS. Mercury was added for a total of 10 test metals.
In addition, the particulate load and particle  size distribution were measured after the quench
and at the scrubber exit  in an attempt to determine fractional particulate collection efficiencies.
Scrubber pressure drop  was also added as a test variable to investigate its effect on fractional
particulate collection efficiencies by particle size range.
                                           68

-------
        As in the past trace metal test programs, the synthetic waste was a toluene-based organic
liquid mixture added to a clay absorbent material. The chlorine content of the synthetic waste
was varied by changing the relative amounts of toluene, chlorobenzene, and tetrachloroethylene.
The test metals were premixed in an aqueous solution and spiked onto this solid material during
feeding to the kiln.

        The test variables for the FY91 tests were kiln temperature, waste feed chlorine content,
and scrubber pressure drop. Afterburner temperature (a test variable in past programs) was not
a test variable for these tests and was held constant. The concern over metal emissions from
incinerators has  created an interest in determining whether operating the primary combustion
chamber at reduced temperature can cause greater metal  retention in the kiln  ash by reducing
metal  volatilization and entrainment.  To study  this mode of operation,  three  low-kiln-
temperature tests were specified. Unlike the two previous trace metals test programs, three tests
were performed with the kiln temperature varied with no chlorine in the waste feed.  These tests
were designed to provide data on the effects of kiln temperature in the absence of chlorine.

        Test data collected included feed  material composition, incinerator process variables,
and discharge stream analysis results. The  sampling and analysis protocol was specified to track
the distributions of metals among the RKS discharge streams (incinerator ash,  scrubber liquor,
and flue gas).  Sampling and analysis for volatile organics in the flue gas was also performed to
demonstrate that the RKS is operated at conditions suitable for organic waste destruction.

        In summary, a 6-week test program was performed, aimed at identifying:

        •    The distribution of metals among kiln ash, scrubber liquor, and flue gas discharge
             streams

        •    The effects of kiln temperature and waste feed chlorine content on metal fate

        •    The efficiency of the Calvert  scrubber for collecting flue gas metals and particulate
             by particle size range

        •    The  effects  of scrubber  pressure drop on metal collection efficiencies  and
             particulate collection efficiencies by particle size range
 6.1
TEST PROGRAM
        This test program was also conducted in the IRF RKS.  For the program, the RKS
 APCS was modified by installing a Calvert Flux Force/Condensation Scrubber pilot plant as the
 primary APCS. The skid-mounted components of the system supplied by Calvert were the
 condenser/absorber,  Calvert  Collision  Scrubber, entrainment separator, wet electrostatic
 precipitator, caustic tank and injection pump, and induced draft  (ID) fan, as shown  in the
 scrubber process schematic in Figure 12. The flue gas quench, heat exchanger, and secondary
 APCS currently in place at the IRF were used.

        The RKS quench at the IRF was modified to create a two-stage quench. Provision for
 injecting fresh water in the first  stage and recirculated water in the second stage was installed.
 This arrangement was designed minimize the addition of fine particles to the flue gas by reducing

                                           69

-------
                                           I
                                           I
                                           3
                                           I
70

-------
the spray dryer effect, which occurs when recirculated quench liquor containing dissolved solids
is used to quench hot flue gas. In the normal RKS quench configuration, makeup water is added
to the recirculating liquor storage tank for the quench and scrubber systems.  For these  tests,
however, the quench system plumbing was modified so that most of the makeup water could be
added as the fresh water supply to the first stage of the quench.

        After quenching, the flue gas was directed to the Calvert scrubber.  Flue gas exiting the
Calvert scrubber ID fan was directed  to the secondary APCS before being discharged to the
atmosphere.

6.1.1    Synthetic Waste Mixture

        These tests were conducted with the same base feed material used in the previous trace
metal test programs. The clay absorbent was combined with an organic POHC mixture in the
ratio of 0.4 kg organic liquid to 1 kg clay absorbent. This ratio produced  a free flowing solid,
similar  to the unspiked clay absorbent.   For these  tests,  the chlorine concentrations were
nominally 0,1, and 4 percent of the combined feed. Desired feed chlorine content was achieved
by adding chlorobenzene and tetrachloroethylene to toluene. The organic liquids were combined
as noted in Table 36, then mixed with the clay absorbent in a portable cement mixer.  The feed
mixture was stored in a  55-gal drum with lid until needed.  A twin-auger screw feeder was used
to continuously feed the mixture to the kiln during testing.

        As in the previous test programs, the trace metals were fed in an aqueous solution. The
test metals  were arsenic,  barium, bismuth, cadmium, chromium, copper, lead,  magnesium,
mercury, and strontium. Previous analyses showed that chromium and magnesium were present
in the clay matrix at approximately 53  ppm and 2.4 percent, respectively. These concentrations
were high enough to provide sufficient  feed quantities  of these metals that they were not
included in the aqueous metals spike solution.  Table 37 notes the  specific  metal compound
chosen for spiking and the  aqueous spike solution concentrations used.

        The aqueous trace metals solution was prepared  in 5-gal glass containers, from which
it was continuously metered into the solid matrix at the screw feeder. The spike solution was
added at a nominal flowrate of 2 L/hr using a separately controlled gear pump.  Inputs of the
solid matrices and the metals solution were carefully monitored and  recorded using scales.

        Previous analyses  showed that barium,  cadmium, copper, and strontium were present
in the clay absorbent at  the concentrations given in Table 37. These background concentrations
were included in the calculations to determine the total metal concentrations in the integrated
waste feed, shown in the last-column of Table 37. Chromium and magnesium concentrations in
 the integrated feed mixture were approximately 38 ppm and 1.7 percent, respectively.

 6.1.2    Test Conditions

         As noted above, the test variables were the kiln exit temperature, the waste feed chlorine
 content, and the scrubber pressure drop. Each was varied over three target levels, as specified
 in Table 38. The test program consisted of 11 test points.  Kiln  temperatures were nominally
 538°,  816° and 927°C (1,000°, 1,500° and 1,700°F).   Waste feed chlorine  content was
 nominally 0, 1, and 4 percent.  The scrubber pressure drop for Tests 1 through 9  was held

                                           71

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-------
                       TABLE 38.  TARGET TEST CONDITIONS
Test No.
1
2
3
4
5
6
7
8"
9
10
11
Kiln exit
temperature,
°C (°F)
538 (1,000)
816 (1,500)
927 (1,700)
538 (1,000)
816 (1,500)
927 (1,700)
538 (1,000)
816 (1,500)
927 (1,700)
816 (1,500)
816 (1,500)
Feed mixture
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%
0
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1
1
1
4
4
4
4
4
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in WC
50
50
50
50
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50
50
35
70
         "Two baseline tests were performed at test condition 8 with the clay/
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constant at nominally 50 in WC. Test points 10 and 11 were at the same conditions as test
point 8, but with scrubber pressure drops of nominally 35 and 70 in WC, respectively.

        Two baseline tests were also performed. These tests were  designed to clarify if there
was a hysteresis effect caused by test-to-test carryover of metals. The clay/organic liquid mixture
was used, but the aqueous metals spike  solution was not included. One test was conducted
before the test series began to establish baseline conditions for metals present in the incinerator
system. The second baseline test was performed after the test series was completed.  The two
baseline tests were performed at test condition 8.

        Table 39 summarizes the RKS operating conditions that were held constant.  All tests
were performed at the same nominal afterburner exit flue gas O2 (7.5 percent), afterburner exit
temperature  (1,093°C [2,000° F]), and synthetic waste feedrate (63.5 kg/hr [140 Ib/hr] of which
18 kg/hr [40  Ib/hr] was the organic liquid matrix). For all tests, the kiln rotation rate was held
constant to provide a solids residence time of nominally 1 hr.
                                          74

-------
                  TABLE 39. TEST CONDITIONS HELD CONSTANT
             Clay/organic liquid feedrate
             Afterburner temperature
             Afterburner exit flue gas O2
             Kiln solids residence time
             Quench blowdown rate
63.5 kg/hr (140 Ib/hr)
1,093° C (2,000° F)
7.5 percent
Ihr
Minimum operable
6.1 J    Sampling and Analysis
        Figure 13 identifies the sampling point locations. For the 11 tests and the two baseline
tests, the sampling effort included the following:
        •    Obtaining a composite sample of the clay/organic liquid mixture
        •    Obtaining two composite samples of the aqueous metals spike solution (except
             baseline tests)
        •    Obtaining two composite samples of the kiln ash
        •    Obtaining a scrubber liquor composite sample
        •    Sampling the flue gas at the quench and scrubber system exits for particulate, HC1,
             and trace metals (excluding mercury), using a Method 5 train modified for
             multiple metals capture
        •    Sampling the  flue gas  at the quench and scrubber exits for mercury using  a
             Method 101A train
        •    Determining the particle size distribution of flue gas particulate in the quench and
             scrubber exits using an  Anderson cascade impactor train
        •    Obtaining samples of the flue gas at the scrubber  exit using a  Method 0030
             sampling train
        •    Sampling the flue gas at the stack for HC1 and particulate using a Method 5 train
        •    Continuously measuring  O2 concentrations at the kiln exit; O2,  CO, CO2, and
             TUHC (unheated) at the afterburner exit; O2, CO2, and NOX at the scrubber exit;
             and O2, CO, and TUHC (unheated) at the stack
                                          75

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In addition, three composite samples of the feed clay absorbent material were collected for
metals analysis to  confirm earlier data on background metal concentrations.  Sampling for
volatile organics by Method 0030 (VOST) was performed at the stack during Test 8 and the two
baseline tests to meet trial burn requirements.

        Flue gas sampling train samples were analyzed for their method specific analytes, e.g.,
metals train samples for the test program trace metals, and Method 0030 samples for the test
program volatile POHCs. Synthetic waste feed mixtures and kiln ash samples were analyzed for
test program volatile POHCs. Feed clay absorbent, aqueous metal spike solution, kiln ash, and
scrubber liquor samples were analyzed for the ten test program trace metals. The ASTM lithium
tetraborate fusion method was used to digest solid samples for analysis.  In addition, kiln ash
TCLP leachates were prepared and analyzed for the test program trace metals.
6.2
TEST RESULTS
        The 13-test program was conducted from late May through mid-July 1991. Table 40
summarizes the actual kiln temperatures achieved for each test and compares them to test target
levels. In general, average achieved kiln exit gas temperatures were within about 17° C (30° F)
of test target temperatures for the tests.  Table 41 shows the cumulative amount of synthetic
waste fed for each test and the  amount of kiln ash collected.  As shown, between 72 and
88 percent of the synthetic waste clay (ash) fraction was collected as kiln ash.  The remaining
12 to 28 percent of the synthetic waste clay fraction was ostensibly carried out of the kiln as
entrained particulate in the combustion flue gas.  These fractions are comparable to past IRF
experience in feeding this synthetic waste mixture.

        Sample analyses and test data reduction were underway at the close of FY91 and are
continuing. Test results will be assembled and reported in FY92.
                                          77

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TABLE 40.   ACTUAL VERSUS TARGET OPERATING CONDITIONS FOR THE CALVERT
             SCRUBBER TRACE METAL TESTS
                                        Kiln temperature, °C (°F)
              Test
              Target
              Minimum    Maximum
                            Average
      Baseline  (5/29/91)
      1
      2
      3
      4
      5
      6
      7
      8
      9
      10
      11
      Repeat
      baseline
(6/5/91)
(6/6/91)
(6/13/91)
(6/18/91)
(6/19/91)
(6/21/91)
(6/25/91)
(6/28/91)
(7/9/91)
(7/11/91)
(7/16/91)
(7/18/91)
816 (1,500)
538 (1,000)
816 (1,500)
927 (1,700)
538 (1,000)
816 (1,500)
927 (1,700)
538 (1,000)
816 (1,500)
927 (1,700)
816 (1,500)
816 (1,500)
816 (1,500)
751 (1,384)
469 (876)
741 (1,366)
811 (1,491)
501 (934)
780 (1,436)
887 (1,629)
441 (825)
803 (1,477)
912 (1,673)
806 (1,483)
751 (1,383)
781 (1,437)
912 (1,673)
594 (1,102)
856 (1,573)
954 (1,750)
581 (1,077)
902 (1,656)
968 (1,775)
568 (1,055)
834 (1,533)
981 (1,798)
842 (1,547)
844 (1,552)
917 (1,682)
831 (1,528)
541 (1,006)
819 (1,507)
909 (1,669)
555 (1,031)
842 (1,547)
919 (1,686)
543 (1,010)
817 (1,502)
944 (1,731)
829 (1,524)
827 (1,521)
834 (1,534)
                                         78

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TABLE 41. SYNTHETIC WASTE FED AND ASH COLLECTED
Synthetic waste fed, kg (Ib)
Test
Baseline
1
2
3
4
5
6
7
8
9
10
11
Repeat
baseline
(5/29/91)
(6/5/91)
(6/6/91)
(6/13/91)
(6/18/91)
(6/19/91)
(6/21/91)
(6/25/91)
(6/28/91)
(7/9/91)
(7/11/91)
(7/16/91)
(7/18/91)
Clay/organic
liquid
313 (691)
279 (614)
271 (597)
331 (730)
299 (660)
255 (563)
305 (674)
269 (593)
281 (619)
264 (582)
284 (627)
298 (657)
343 (756)
Clay fraction
247 (545)
221 (487)
216 (475)
266 (587)
249 (550)
206 (453)
240 (528)
203 (448)
214 (471)
210 (463)
236(519)
230 (507)
265 (585)
Kiln ash collected
Weight, Fraction of
kg (Ib) clay fed, %
219 (482)
176 (388)
166 (365)
202 (446)
179 (396)
153 (338)
186 (409)
169 (373)
166 (367)
154 (340)
178 (392)
181 (398)
204 (450)
88
80
77
76
72
75
77
83
78
73
75
78
77
                      79

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                                     SECTION 7

                INCINERATION OF ARSENIC-CONTAMINATED SOILS
      FROM THE CHEMICAL INSECTICIDE CORPORATION SUPERFUND SITE
        The Chemical Insecticide Corporation (CIC) site in Edison Township, New Jersey, was
formerly used to manufacture and formulate pesticide products.  The results of the remedial
investigation and feasibility study (RI/FS) show that the soils at the site are highly contaminated
by organic pesticides and arsenic. Dioxin (i.e., 2,3,7,8-tetrachlorodibenzo-p-dioxin) has also been
found in some soil samples collected during the RI/FS at concentrations up to 1.8 ng/kg (ppb).
Thermal treatment has previously been demonstrated to be an effective means of destroying
organic pesticides, dioxin, and other organic compounds.  The finding of high concentrations of
arsenic in the soils at the CIC site has raised the question of whether a thermal treatment unit
treating soil from the site, and operating under conditions capable of attaining a 99.9999-percent
DRE for dioxin and other organic contaminants, can also reduce arsenic concentrations to
acceptable levels in the stack emissions.  To address this question, EPA Region 2  (J. Josephs,
coordinator) requested that incineration testing be performed at the IRF.
7.1
TEST PROGRAM
        The objective of the test program performed was to obtain data to support feasibility
study (FS) efforts in evaluating incineration as a possible remedial alternative.  To attain this
objective, the test program was designed to:

        •    Maintain critical operation parameters in the effective range, ensuring a dioxin
             DRE of 99.9999 percent and minimizing arsenic air emissions

        •    Determine whether the incinerator can attain a 99.96-percent removal efficiency
             (RE) for arsenic, where RE is defined as:

             RE = 100 (1 - [flue gas arsenic emission rate]/[arsenic in soil feedrate])

        •    Determine the characteristics and arsenic content (at a minimum) of all effluent
             streams resulting from the thermal treatment process based on the test equipment
             employed

        •    Serve as a model for determining important operating parameters to be used for
             projecting comparable full-scale performance and operational costs

All tests in this program were performed in the RKS at the IRF.

                                         80

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        The  high-efficiency  scrubber  system for  this  program was  the  Calvert  Flux
Force/Condensation Scrubber System used in the trace metal fate test program described in
Section 6.

7.1.1    Test Waste Description

        The CIC site is located in Edison Township, Middlesex County, New Jersey.  From 1958
through 1970, a variety of pesticides was formulated and distributed for both commercial and
military applications by CIC.  The CIC product list included a wide range of insecticides,
fungicides, rodenticides, and herbicides.  One specific product was 2,4,5-trichlorophenoxyacetic
acid (2,4,5-T),  which  might  have  contained tetrachlorodibenzo-p-dioxin (TCDD)  as  a
contaminant.

        Pesticide manufacturing activities, combined with process-water storage lagoons and
poor housekeeping, led  to the widespread chemical contamination of this site. As  part of the
RI/FS, approximately 170 surface/shallow subsurface and 200 soil boring samples were collected
and analyzed.   Analytical results  of these samples indicate that the major contamination
constituents at the CIC site are organochlorine pesticides, chlorinated herbicides, and hazardous
constituent trace metals.

        Four drums of soil were excavated from the site in February 1991 for use in this test
program.  Characterization samples from each drum were forwarded to the IRF  for pretest
analyses.  Each sample was analyzed for the eight TCLP trace metals, antimony, beryllium, and
thallium; and for the organochlorine  pesticides and chlorinated herbicides known to be site
contaminants.  In addition, TCLP leachates of each sample were prepared and analyzed for trace
metals and organochlorine pesticides.

        Soil sample analysis results are summarized in Table 42. TCLP leachate analysis results
are summarized in Table 43.  The data in Table 42 show that soil with an average arsenic
content of about 900 mg/kg was excavated for testing. This soil was also contaminated with an
average of 2 mg/kg of p,p'-DDD, 3 mg/kg of p,p'-DDE, 26 mg/kg  of p,p'-DDT, and 9 mg/kg
of chlordane.  Despite  having arsenic, barium, chromium, and lead contamination levels of
several tens to over 1,000 mg/kg, the soils were not toxicity characteristic (TC) hazardous wastes
based on the TCLP leachate analysis results summarized in Table 43.

        A composite of the four-characterization samples received was  also subjected  to
proximate (ash, moisture,  and heating value) analysis, with the following results:
        •    Ash content:

        •    Moisture content:

        •    Heating value:

        •    pH:
87 percent

13 percent

Will not burn

6.1
                                          81

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TABLE 42. SOIL CHARACTERIZATION SAMPLE ANALYSIS RESULTS
Concentration, mg/kg
Constituent
Trace metals:
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Lead
Mercury
Selenium
Silver
Thallium
Drum 1

12
1,260
63
0.25
2.3
17
55
7.8
<4.4
<0.33
164
Drum 2

10
771
52
0.25
1.5
17
80
8.9
<4.7
<0.35
185
DrumS

24
875
59
0.35
2.1
18
104
10.5
<4.5
<0.34
145
Drum 4

33
784
60
0.35
1.9
18
103
8.6
<6.6
<0.45
156
Average

20
922
59
0.33
2.0
18
86
9.0
<6
<0.5
163
Organochlorine pesticides:
«-BHC
y-BHC
p,p'-DDD
p.p'-DDE
p.p'-DDT
Chlordane
<0.8
<0.8
3.0
4.3
33
11
<0.8
<0.8
1.9
2.8
32
<8
<0.8
<0.8
1.5
2.3
21
<8
<0.8
<0.8
1.8
3.1
19
<8
<0.8
<0.8
2.1
3.1
26
9
Chlorinated herbicides:
2,4-D
2,4,5-T
Silvex
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
                          82

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TABLE 43. SOIL CHARACTERIZATION SAMPLE TCLP LEACHATE ANALYSIS RESULTS
Concentration, mg/L
Constituent
Trace metals:
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Lead
Mercury
Selenium
Silver
Thallium
Drum 1

0.175
3.0
0.92
0.002
0.015'
0.051
0.062
< 0.002
<0.08
<0.01
0.116
Drum 2

0.058
2.1
0.48
0.002
0.014
0.078
0.052
< 0.002
<0.08
<0.01
0.018
Drum 3

0.077
1.5
0.03
<0.001
0.012
0.072
0.051
< 0.002
<0.08
<0.01
0.076
Drum 4

0.113
1.2
0.08
< 0.001
0.014
0.216
0.051
< 0.002
<0.08
<0.01
0.029
TC
regulatory
level,
mg/L

—
5.0
100
—
1.0
5.0
5.0
0.2
<1.0
^<5.0
—
Organochlorine pesticides:
«-BHC
Y-BHC
p,p'-DDD
p,p'-DDE
p,p'-DDT
Chlordane
< 0.001
< 0.001
< 0.001
< 0.001
< 0.001
< 0.010
<0.001
< 0.001
< 0.001
< 0.001
< 0.001
< 0.0 10
<0.001
< 0.001
< 0.001
< 0.001
< 0.0025
<0.010
<0.001
< 0.001
< 0.001
< 0.001
< 0.001

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7.1.2    Test Conditions

        The test program performed to address the objectives of the project consisted of four
tests. Each test entailed incinerating one 55-gal drum of contaminated soil over a 4- to 5-hr time
period. As noted above, a primary test objective was to confirm the ability of a rotary kiln
incineration system equipped with a high-efficiency APCS to achieve 99.96 percent arsenic RE.
Preliminary results from the first test showed that arsenic RE was just less than 99.96  percent,
so a fourth test was performed in which the soil was mixed with lime, at a blend ratio  of 0.5 Ib
lime/10 Ib soil.

        For each test, the soil was fed to the kiln via the fiberpack drum ram feed system at a
rate of 12 fiberpack drums/hr  (1 fiberpack drum every 5 min).  Each  fiberpack drum held
approximately 4.6 kg (10 Ib) of soil.   Therefore, the  soil  feedrate was nominally 55 kg/hr
(120 Ib/hr).

        All tests were performed at a kiln gas  temperature of nominally  980° C (1,800°F) and
an  afterburner gas  temperature of  nominally  1,200° C (2,200° F).  These conditions  are
comparable to those that have resulted in 99.9999 percent dioxin and PCB DRE in past tests.
Thus, these conditions are anticipated to meet or exceed the requirements for destroying dioxin
to levels greater than 99.9999 percent.  In addition, these conditions are typical of full-scale
incinerator operation.

        For all tests, the kiln rotation rate was at a value corresponding to a kiln solids residence
time of 0.5 hr.  The Calvert scrubber system pressure drop was nominally 12 kPa (50  in WC),
and scrubber system blowdown was held to the minimum operable level.

7.13    Sampling and Analysis

        The sampling and analysis procedures employed for all tests are outlined in  Figure 14.
For all tests, the sampling protocol entailed:

        •    Obtaining a composite sample of the soil samples from each drum before the soil
             was packaged into the fiberpack containers

        •    Collecting a composite sample of the kiln ash

        •    Collecting a composite sample of the scrubber liquor

        •    Continuously measuring O2 levels in the kiln exit and afterburner exit flue gases;
             O2, CO, CO2, NOX, and TUHC levels at the scrubber exit; and O2, CO, and CO2
             levels at the stack

        •    Sampling flue gas at the scrubber system exit for semivolatile organics,  arsenic,
             and particulate and HC1

        •    Sampling  at the  stack downstream of  the secondary APCS for arsenic and
             particulate and HC1
                                          84

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                                85

-------
        The composite soil sample for each test was obtained by taking thief samples from each
shipment drum at three locations in the drum cross section just prior to packaging the soil into
the fiberpack drums.  These three samples were combined to form one composite waste feed
sample per test.

        During each test, kiln ash was continuously removed from the kiln ash pit via a transfer
auger, and deposited into an initially clean 55-gal drum. After all test ash was deposited in this
drum, representative kiln ash samples were taken  by thief sampling in at least three locations
across the collection drum cross section.  These three ash samples were then combined to form
one composite sample.

        As noted above, each test was run with the scrubber liquor loop operating at minimum
blowdown. At the end of each test, the incinerator was operated (firing natural gas) for at least
12 hr after stoppage of soil feed, or until the kiln was visually clear of ash, whichever was longer.
After this period of time, the scrubber system was drained to the blowdown collection  tank.
During the entire period the system was being drained, a sample was continuously taken from
a tap.

        The soil composite sample for each test, and  each of the kiln ash and scrubber liquor
samples, were subjected to analysis (still in progress) for the TCLP trace metals (arsenic, barium,
cadmium, lead, mercury, selenium, and silver).  The soil and kiln ash from each test  were
subjected to TCLP extraction. The resulting extracts were subjected to analysis (still in progress)
for the eight TCLP trace metals. In addition, the soil leachates were subjected to  analysis (still
in progress) for the  organochlorine pesticides. Flue gas sampling train samples were subjected
to analysis (still in progress) for these procedure-specific analytes, as  noted in Figure 14.
7.2
TEST RESULTS
        This test program was completed in early August 1991. Sample analysis and test data
reduction were  underway at the close of FY91 and are  currently in progress.  Test data
evaluation and reporting will be completed in FY92.
                                          86

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                                    SECTION 8

                   FACILITY PHYSICAL PLANT IMPROVEMENTS
       Several modifications and improvements to the IRF physical plant were completed
during FY91. These are briefly outlined in the following subsections.
8.1
OFFICE SPACE
        Since FY85, the IRF operating staff has worked in some combination of single- and
double-width office trailers adjacent to the main facility building. After the completion of the
new, 15,200 ft2 main facility building in FY891, and completion of the major RKS reconfiguration
and upgrade effort in FY902, efforts focused on providing for more appropriate office space for
the IRF staff.

        Plans to procure 5,040 ft2 of modular office space were finalized in late FY90. Approval
to purchase the planned complex was received in early FY91. The complex was subsequently
installed, and completed and occupied in March 1991.

8.2     INCINERATION SYSTEM IMPROVEMENTS

        Most aspects  of a major RKS reconfiguration and system upgrade were completed
during FY902.  However,  a few efforts extended into FY91, as discussed  in the following
paragraphs.

        The first effort involved replacing the kiln support and drive mechanism of the RKS.
It had been acknowledged for some time that the former performance of the rotary kiln drive
mechanism was not optimal.  To improve system performance, the design of a mechanically
sturdy trunion and roller system with an improved drive mechanism was completed in early
FY91. The retrofitting of this system to the RKS took place from late December 1990 through
early January 1991, and  was completed in time for the K088 waste incinerability test program
discussed in Section 3.

        The  second  effort involved expanding the operating functions attended to by the
automatic process control system installed in early FY90. The first phase in the implementation
of automatic process control included developing the controls for the burner management system
and implementing extensive data acquisition functions.  This phase was completed in June 1990,
and the controls were  used during the POHC incinerability ranking tests discussed in Section 2.
                                         87

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        The next phase of automatic control included bringing remaining process parameter
sensors online; implementing the required automatic waste feed cutoff interlock functions
mandated by the IRF's modified hazardous waste management permit; enhancing the system's
data gathering and recording features; and refining the burner controls for automatic gradual
startup and shutdown. This effort was initiated in early FY91 and completed, with the controls
largely functional, in April 1991.

83     FLAMMABLE CHEMICAL STORAGE BUILDING

        Following the recommendations that resulted from a facility environmental audit, an
adequate building for the IRF to store flammable chemicals in was procured and installed during
FY90. Several modifications to this building were required prior to its intended use. These were
completed, and the storage building commissioned for use in April 1991. With the addition of
the building, flammable liquids, previously stored  outdoors under a tent and inside containment
traps, can now be stored in an appropriate enclosed space.
8.4
BENCH-SCALE THERMAL TREATABILITY TEST UNIT
        The past two years have seen a significant amount of pilot-scale incinerability testing of
Superfund site wastes and contaminated soils conducted at the IRF.  In FY91, it became clear
that there was a need to supplement the pilot-scale testing capabilities at the IRF with smaller,
bench-scale capabilities that could offer screening information at less expense. The specific need
for such capabilities arose out of the Superfund Technical Assistance Response Team (START)
program recently initiated within RREL.

        The purpose of the START program is to assist EPA  Regional Offices in determining
the best methods for remediating Superfund sites. In a typical project, a Regional Office sends
an analysis of the site waste, and related data, to START.  Using this information, START
selects the possible remedial technologies applicable to  the site.  Once START identifies the
technologies, a screening process, called the Remedy Screen, is  undertaken to select those
treatment technologies likely to be the most effective.

        Remedy Screen testing, at present, is envisioned to be bench-scale, relatively inexpensive,
and capable of yielding proof-of-concept information.  In the  Remedy Screen process, the
Regional Office sends a quantity of the site waste material to the location designated to perform
the Remedy Screen testing.  Should the results of the testing suggest that a given treatment
technology is an appropriate and likely remedy for the site, larger scale pilot-scale testing may
be warranted.

        The IRF is the most logical location to conduct the thermal treatment  Remedy Screen
testing, as the waste management skills and the pilot-scale testing capabilities are already in place
at the facility.  Thus, in response to a START program request,  the conceptual design  of a
bench-scale thermal treatability test  unit (TTU) was initiated in  March 1991.  The conceptual
design of the unit focused on the unit's being capable of:

        •    Simulating an incinerator operation in terms of solids retention time  and  mixing

        •    Providing for continuous feed of the waste to the combustion zone

                                          88

-------
        •    Operating over a wide range of temperatures in order to simulate high- and low-
             temperature thermal treatment

             -    Temperature range of 260° to 980° C (500° to 1,800° F)

             —    Gas fired to expose waste to a flame

        •    Generating sufficient gas volume to allow for a variety of gas-phase analyses to be
             conducted, including analysis for volatile and semivolatile components and trace
             metal components

        •    Allowing for collection of the ash residue stream for analysis

        After examining several alternatives, modifying a small pathological incinerator  of
standard design was selected as the most  cost-effective approach to achieving the above
capabilities.  Figure 15 illustrates the TTU unit resulting from this approach.  The base
combustor system is a standard-design, National Incinerator, Inc., Model P-50 incinerator, with
the following modifications:

        •    The supplied burners were modified to accept modulating control valves and
             controllers to permit accurate temperature control without the undesirable side
             effects of on-off control

        •    Two load channels were attached to the sides of the main incineration chamber,
             as shown in Figure 16. The channels allow for the insertion of ceramic sample
             trays that are gradually fed through the combustion chamber by electrically driven
             rollers.  The feed rate (and the solids retention time in the combustion zone) is
             adjusted by variable speed control of the rollers. Sample trays can be inserted one
          "'  after the other in order to make continuous incinerator simulation possible.

        •    The stack was equipped with sampling ports

        Approval to proceed with procuring and installing the TTU was received in April.  The
incinerator unit was ordered in May, and delivered in late July.  Hookup and refractory curing
were completed in August. The material feed and removal system was installed in September.
Unit shakedown testing was underway at the end of FY91. Thus, the IRF will have bench-scale
TTU testing capability very early in FY92.
                                           89

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Figure 15. TTU: external configuration.




                 90

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                                            •a
                                            I
91

-------
                                    SECTION 9

              HEALTH AND SAFETY, ENVIRONMENTAL COMPLIANCE,
                          AND PERMIT ADMINISTRATION
        All aspects of the administration of the IRF's hazardous waste management permit were
 routinely accomplished throughout the year.  Special mention of the IRF's response to the new
 training  requirements  for workers  at hazardous  waste  management  facilities, under
 29 CFR 1910.120, is deserved.  In response to these new regulations, an IRF staff training plan
 was developed and implemented during FY91. All staff members were given the required level
 of training over the course of the year, and required refresher training is routinely scheduled.

        That all aspects of environmental compliance are properly administered is  evidenced by
 the results of the  facility's biannual environmental audit by  EPA's Safety,  Health, and
 Environmental Management Division (SHEMD). The results of this audit, which was conducted
 in August 1991, noted that the facility's environmental compliance program is of exemplary
 quality.

       Two  additional  areas  of environmental compliance and  permitting  that  deserve
 discussion are covered in the following subsections.

 9.1    TOXIC  SUBSTANCE  CONTROL ACT  RESEARCH AND   DEVELOPMENT
       PERMIT

       During the initial planning for the incineration tests of the PCB-contaminated sediments
 from the New Bedford Harbor Superfund site (discussed in Section 5) in early FY91, it became
 clear that some form  of PCB permit for the  facility would  be required under the Toxic
 Substances Control Act (TSCA) regulations before the tests could proceed.  After  investigating
 several approaches, it was decided that the most  appropriate and expedient approach would be
 to obtain a research and development (R&D) permit.

       Accordingly, a TSCA R&D permit application was prepared and submitted to EPA's
Office of Toxic Substances in November 1990.  The  permit, in the form  of an  Approval to
Conduct R&D Tests to Dispose of PCBs, was received in late February 1991. With this annually
renewable permit  in place, the IRF can now perform testing with both hazardous wastes
regulated under RCRA and PCB wastes regulated under TSCA.
                                        92

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92     RCRA FACILITY INVESTIGATION

       A modified hazardous waste management (RCRA Part B) permit for the facility, jointly
administered by the Arkansas Department of Pollution Control and Ecology (ADPCE) and EPA
Region 6, became effective in September 1990.  The corrective action module of the permit,
included  in  accordance  with regulations in response to the Hazardous  and Solid Waste
Amendments of 1984 (HSWA), requires a RCRA Facility Investigation (RFI) to determine the
nature and extent of releases  of hazardous wastes, including hazardous  constituents and
hazardous substances from identified solid waste management units (SWMUs).  The permit
outlines five Facility Investigation tasks.

        The first task requires the completion of a "Preliminary Report: Description of Current
Conditions." This report was completed and submitted in December 1990.  The second task
requires the completion of an RFI Work Plan describing the approach and procedures for the
initial phase of the RFI.  This document was completed and submitted in March 1991.
                                          93

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                                       SECTION 10

                                 THIRD-PARTY TESTING
     ^    The Federal Technology Transfer Act allows for the use of government facilities and
 equipment in joint projects with private-sector third parties. The IRF represents a unique facility
 with capabilities unavailable anywhere else in the United States.  Furthermore, the hazardous
 waste incineration research and  testing arena is quite active.  Thus, the potential demand for
 such third-party joint projects is  expected to become quite significant.

         The RREL policy established during FY89 was to encourage, and even solicit  third-
 party use of the IRF. In fact, the IRF operations and research contract specifically provides for
 this type of usage, and efforts to identify appropriate joint third-party projects have proceeded.
 •  CVnn        this 6nd> a facility caPabmties brochure was prepared, printed, and distributed
 in FY90. The purpose of the brochure is to outline the capabilities of the IRF and the type of
 testing that has, and can, be performed, and to solicit third-party inquiries.  This brochure was
 reissued in color in FY91. FY90 also saw the preparation and release of a videotape highlighting
 one of the test programs  completed during that year.  A solicitation-of-interest mailer was
 distributed during FY91, and preview copies of the videotape distributed to mailer respondents
 FY91:
        Three firm proposals to perform test programs for third-party users were prepared
in
        •    A proposal to evaluate the incinerability of contaminated soils via a parametric
              test program for a Department of Defense-administered Superfund site

        •    A proposal to  evaluate the incinerability of wastes from a petroleum refinery
              Superfund site being remediated by a private-sector potentially responsible party
              (PRP)

        •   A proposal to evaluate kiln particle carryover from the incineration of surrogate'
             mixed waste to support a Department of Energy incineration system design effort

All thee proposals were in active evaluation at the end of FY91, with the expectation that at least
one of the three will proceed.
                                          94

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                                    SECTION 11

                          EXTERNAL COMMUNICATIONS
        During FY91, six reports were prepared and submitted, and 11 technical papers were
presented. These are listed in Table 44. This level of external communication and technology
transfer is comparable to levels experienced over the preceding 4 years, and testifies to the high
level of important research being supported at the IRF.

        Table 45 lists some of the visitors to the IRF during FY91. The length of the list attests
to the visibility of the work being performed at the IRF to the incineration research community.
                                          95

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      Waterland, L. R., Operations and Research at the U.S. EPA Incineration Research
      Facility, Annual Report for FY90," draft January 1991, revised February 1991
      published as EPA/600/9-91/010, April 1991

      Fournier, Jr., D. J., and L. R. Waterland, "The Fate of Trace Metals in a Rotary Kiln
      incinerator with a Single-Stage Ionizing Wet Scrubber," revised February 1991, final
 •    Vocque, R. H., and L. R. Waterland, "Pilot-Scale Incineration of Contaminated Soil
      from the Purity Oil Sales and McColl Superfund Sites," revised February 1991  final
      May 1991                                                              '

 •    Lee, J. W., W. E. Whitworth, and L. R. Waterland, "Pilot-Scale Evaluation of the
      Thermal Stability POHC IncinerabiUty Ranking," draft June 1991  ,

 •    Whitworth, W. E., J. W. Lee, and L. R. Waterland, "Pilot-Scale Incineration Tests of
      Spent Potlmers from the Primary Reduction of Aluminum (K088)," draft August 1991

 •    Whitworth, W. E., and L. R. Waterland, "Pilot-Scale Incineration of
      PCB-Contaminated Sediments from the New Bedford Harbor Superfund Site "
      preliminary draft September 1991

Papers and Presentations:
            r, Jr., D. J., L. R. Waterland, and G. J. Carroll, "Size Distributions of Trace
     Metals in Flue Gas Particulate from a Pilot-Scale Rotary Kiln Incinerator," presented
     at the American Flame Research Committee 1990 Fall International Symposium on
     NO  Control, Waste Incineration, and Oxygen-Enriched Combustion, San Francisco
     California, October 1990

     Waterland, L. R., C. King,  R. C. Thurnau, and M. K. Richards, "Incinerability Testing
     of an Arsenic-Contaminated Superfund Site Soil," presented at the Pacific Northwest
     International Section of the Air & Waste Management Association 1990 Conference
     Portland, Oregon, November 1990                                              '

     Waterland, L. R., D. J. Fournier, Jr., J. W. Lee, and  G. J. Carroll, "Trace Metal Fate
     in a Rotary Kiln Incinerator with an Ionizing Wet Scrubber," Waste Management
     Vol. 11, p. 103, 1991                                        :	5	'

     Waterland, L. R., C. King, M. K. Richards, and R. C. Thurnau, "Incineration
     Treatment of Arsenic-Contaminated Soil," Remediation, p. 227, Spring 1991

     Waterland, L. R., D. J. Fournier, Jr., J. W. Lee, G. J. Carroll, and R. C. Thurnau
     ine Fate of Trace Metals in a  Rotary Kiln Incinerator-Tests  with Two Different
     Scrubber Systems," presented at the Second International Congress on Toxic
     Combustion Byproducts:  Formation and Control, Salt Lake City, Utah, March 1991
     submitted for publication to Combustion. Science, and Technology
                                                       ~~               =
                                                                        (continued)
                                       96

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                              TABLE 44. (continued)
Papers and Presentations (continued):
•    Wall, H. O., "The Incineration of Lead-Contaminated Soil Related to the
     Comprehensive Environmental Response, Compensation and Liability Act
     (CERCLA) (Superfund)," in Proceedings of the Seventeenth Annual RREL
     Hazardous Waste Research Symposium, EPA/600/9-91/002, April 1991

•    Fournier, D. J., Jr., L. R. Waterland, J. W. Lee, and G. J. Carroll, "The Behavior of
     Trace Metals in Rotary Kiln Incineration:  Results of Incineration Research Facility
     Studies," in Proceedings of the Seventeenth Annual RREL Hazardous Waste
     Research Symposium, EPA/600/9-91/002, April 1991

•    Carroll, G. J., W. E. Whitworth, J. W. Lee, and L. R. Waterland, "Pilot-Scale
     Evaluation of an Incinerability Ranking System for Hazardous Organic Compounds,"
     presented at the Seventeenth Annual RREL Hazardous Waste Research Symposium,
     Cincinnati, Ohio, April 1991
•    Lee, J. W., D. J. Fournier, Jr., and R. C. Thurnau, "U.S. EPA Incineration Research
     Facility Update," presented at the Seventeenth Annual RREL Hazardous Waste
     Research Symposium, Cincinnati, Ohio, April 1991

•    Waterland, L. R., C. King., R. H. Vocque, M. K.  Richards, and H. O. Wall,
     "Pilot-Scale Incinerability Evaluation of Arsenic-  and Lead-Contaminated Soils from
     Two Superfund Sites," presented at the 1991 Incineration Conference, Knoxville,
     Tennessee, May 1991
 •   Lee, J. W., L. R. Waterland, W. E.  Whitworth, and G. J. Carroll, "Evaluation of the
     Thermal Stability POHC Incinerability Ranking in a Pilot-Scale Rotary Kiln
     Incinerator," paper 91-34.3, presented at the 84th Annual Meeting of the Air &
      Waste Management Association, Vancouver, British Columbia, Canada, June 1991
                                         97

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TABLE 45. VISITORS TO THE IRF
Person
T. Bucci
T. Rice
G. Martin
D. Brown
A. Dorobati
G. McClure
R. Kennedy
J. Baudain
J. Calhoun
D. Pauley
B. Fontaine
P. Holland
R. McDuffee
J. Palmateer
F. Bales
R. Loftin
R. Wilkins
P. Murphy
A. Dorobati
H. Huppert
T. Wagner
R. Turner
J. Labrosa
C. Guffey
H. Hittner
D. Backfinch
A. Sykes
Affiliation
Pathology Associates, Inc.
ADPCE
ADPCE
ADPCE
ADPCE
University of Arkansas
Medical Sciences
Gentry & Associates
Clean Ventures
Pine Bluff Arsenal
Pine Bluff Fire
Department
Jefferson County Sheriffs
Department
White Hall Police
Department
ADPCE
Jefferson County Office
of Emergency Services
USAGE
USDA
Clean Ventures
ADPCE
ADPCE
SAIC
SAIC
EPA/RREL
EPA/OSW
Reynolds Metals
Alcoa
Noranda
Acurex
Date
10/15/90
10/31/90
11/9/90
11/16/90
11/27/90
12/6/90
12/6/90
12/13/90
12/19/90
1/3/91
1/11/91
1/15/91 '••'
through
1/18/91
1/15/91
1/16,17/91
1/18/91
1/23/91 .
through
1/25/91
Purpose of visit
Discuss incineration of
pathological waste
Facility familiarization tour
Facility familiarization tour
Facility tour
Facility tour
Facility tour
Permit-mandated facility
familiarization for emergency
planning
Witness Caldwell Trucking tests
Facility tour
Facility tour
Facility familiarization tour
Witness K088 tests
Witness K088 tests
Witness K088 tests
Witness K088 tests
Facility internal QA review
                                         (continued)
            98

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TABLE 45.  (continued)
^M^^^BS— -"^^••"^^— l^^^-" 1
Person
J. Claysori


H. Wong
R. Schrock
R. Wilson
M. Billedean
J. Sudnick
L. Tate
K. Bisgard
B. Heineman
G. McGill
R. DeCesare
E. Cole
S. Arnold
R. Schluite
J. Camara
T. Wesson

B. Laswell
D. McCormick
K. Yates
E. Fleming
E. Lagoutte
J. Camara
S.-C. Yung
J. Huff
C. Westerfield
G. Cathije
T. Ho
H. Lee
Affiliation
El Dorado Engineering


JMM Associates
EPA/Region 3
JMM Associates
NCTR
Four Nines
USAGE
USAGE
EPA/Region 6
Texas Water Commission
U.S. Bureau of Mines
U.S. Bureau of Mines
U.S. Bureau of Mines
U.S. Bureau of Mines
Calvert Environmental
Calvert Environmental

ICF Kaiser Engineers
IGF Kaiser Engineers
Acurex
ADPCE
Rhone Poulenc
Calvert Environmental
Calvert Environmental
Calvert Environmental
Mobay Chemical
3M
Lamar University
Lamar University
Date
1/29/91
, * i
through
2/7/91
1/30,31/91
1/31/91
2/7/91
3/18/91
3/21/91


4/10/91
4/18/91



4/29/91
through
5/3/91
5/1/91

5/9/91
5/15/91
5/17/91
5/20/91

5/30/91


6/4/91
- r
Purpose of visit
Witness Drake Chemical tests


Witness Drake Chemical tests
Witness Drake Chemical tests
Witness Drake Chemical tests
Facility tour
Facility tour, discuss potential
Superfund site test program
• . - " '
Facility tour, discuss potential
Superfund site test program
Facility tour



Install Calvert scrubber


Facility tour

Facility internal safety review
Facility familiarization tour
Facility tour
Witness Calvert scrubber
shakedown
Witness Calvert scrubber trace
metal tests

Facility tour, trace metal research
discussion 	 '
                                          (continued)
           99

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TABLE 45.  (continued)
Person
B. Russell
D. Banks
R. Fish
D. Brown
M. Greet
G. Thompson
D. Brown
K. Modearis
T. Yoder
P. Weggel
K. Crabtree
K. Roser

R. Shipmer
Affiliation
Calvert Environmental
Calvert Environmental
Garver and Garver
Garver and Garver
Pine Bluff Arsenal
Pine Bluff Arsenal
ADPCE
Booz, Allen, Hamilton
Booz, Allen, Hamilton
EPA/SHEMD
EPA/PMD
EG&G

CE O&MS
Date
6/27/91





6/28/91
8/19/91
through
8/21/91
9/3/91
through
9/5/91
9/30/91
Purpose of visit
Witness Calvert scrubber trace
metal tests




Annual hazardous waste inspection
Biennial facility environmental
audit

EPA property audit


Facility tour
        100

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                                     SECTION 12

                            PLANNED EFFORTS FOR FY92
        One test program was completed in the second quarter of FY91, the Drake Chemical
site tests discussed in Section 4, for which reporting efforts were underway at the end of FY91.
In addition, two major test programs were completed in the fourth quarter of FY91, the Calvert
scrubber trace metal tests discussed in Section 6 and the CIC site tests discussed in  Section 7,
for which sample analyses and data evaluation efforts were underway at the end of FY91.  All
remaining test sample analyses, test data reduction and interpretation, and test reporting efforts
for these three test programs will proceed through to  completion in FY92.

        With respect to test activities, three firm test  programs are  planned for FY92:

        •    Incinerability testing of contaminated sludges from the Bofors-Nobel Superfund
             site in Region 5 (D. H. Ellison, Region 5, L. Janis, USAGE, coordinators); testing
             is planned to begin in October 1991

        •    Incinerability testing of contaminated soils from the Scientific Chemical Processing
             Superfund site in Region 2 (P. Evangelista, Region 2, R. Koustas, RREL/Edison,
             coordinators); testing is tentatively planned to begin in November 1991

        •    Testing to evaluate incinerator emissions associated with repeated incinerator
             waste-feed-cutoff (WFCO) episodes  to support the Regional incinerator permit
             writers  (S. Sasseville, coordinator);  testing  is tentatively planned to begin in
             December 1991

        Other candidate test programs under discussion that could be conducted later in FY92
 (January 1992 on) include:

        •     One of the third-party test programs discussed in Section 10

        •     Testing of the fate of trace metals  in the RKS using a spray  dryer/baghouse
              combination for air pollution control. A test matrix similar to that employed in
              the Calvert scrubber tests discussed in Section 6 is contemplated if an appropriate
              spray dryer/baghouse system can be rented or fabricated at acceptable cost.

        •    A parametric test series to evaluate the effect of feed metal form on trace metal
              fate in  the RKS.  Alternative feed metal forms other than the aqueous solution
              co-fed  with a clay-based  hazardous waste  analog include  an aqueous metal

                                           101

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solution atomized into the kiln burner flame, and mixed metal oxide powders fed
with the clay-based hazardous waste analog.

A parametric field test series to evaluate a POHC surrogate soup for possible trial
burn applications.

Further evaluation testing of low-temperature thermal desorption as a Superfund
site remediation technology

Parametric testing of a synthetic Superfund soil matrix to support the Superfund
Program Office
                            102

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                                  REFERENCES
1.
2.
Waterland  L.  R, "Operations and Research at the U.S. EPA Incineration Research
Fac^ Annual Report for FY89," EPA/600/2-90/012, March 1990.

Waterland  L.  R., "Operations and Research at the U.S. EPA Incineration Research
    S£ Annual Report for FY90," EPA/600/9-91/010, April 1991.
       *U.S. GOVERNMENT PRINTING OFFICE: 1 9 9 2 .6-» 8 . 0 0 y. 0 7 9 9
                                          103

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