June 1995
PILOT-SCALE INCINERATION TESTING OF
FLUFF WASTE AND CONTAMINATED SOIL
    FROM THE M. W. MANUFACTURING
             SUPERFUND SITE

        Volume I  Technical Results
                     by
   J. W. Lee, W. W. Vestal, S. Venkatesh, C. G. Goldman,
               and L. R. Waterland
          Acurex Environmental Corporation
           Incineration Research Facility
             Jefferson, Arkansas 72079
             EPA Contract 68-C9-0038
           Work Assignments 3-3 and 4-3
           Project Officer: R. C. Thurnau
       Technical Project Manager: M. K. Richards
          Sustainable Technology Division
     National Risk Management Research Laboratory
              Cincinnati, Ohio 45268
NATIONAL RISK MANAGEMENT RESEARCH LABORATORY
      OFFICE OF RESEARCH AND DEVELOPMENT
     U.S. ENVIRONMENTAL PROTECTION AGENCY
            CINCINNATI, OHIO 45268

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                                        DISCLAIMER
          The information in this document has been funded wholly by the U.S. Environmental Protection
Agency under Contract No. 68-C9-0038 to Acurex Environmental 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.

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                                          FOREWORD
        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. To meet this mandate, EPA's research program is providing data and technical
support for solving environmental problems today and building a science knowledge base necessary to manage
our ecological resources wisely, understand how pollutants affect our health, and prevent or reduce environmental
risks in the future.

        The National Risk Management Research Laboratory is the Agency's center for investigation of
technological arid management approaches for reducing risks from threats to human health and the environment.
The focus of the Laboratory's research program is on methods for the prevention and control of pollution to air,
land, water  and subsurface resources; protection of water quality in public water systems ; remediation of
contaminated sites and ground water; and prevention and control of indoor air pollution. The goal of this research
effort is to catalyze development and implementation of innovative, cost-effective environmental technologies;
develop scientific and engineering information needed by EPA to support regulatory and policy decisions!; and
provide  technical support and information transfer to ensure effective implementation  of environmental
regulations and strategies.

        This publication has been produced as part of the Laboratory's strategic long-term research plan. It is
published and made available by EPA's Office of Research and Development to assist the user community and
to link researchers with their clients.

                                             E. Timothy Oppelt, Director
                                             National Risk Management  Research Laboratory
                                                 ill

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                                           ABSTRACT
          At the request of EPA Region III and U.S. Army Corps of Engineers, a series of six tests was
conducted at the U.S. EPA Incineration Research Facility (IRF) to evaluate the incinerability of the fluff waste
and contaminated soil from the M. W. Manufacturing Corporation Superfund site in Danville, Pennsylvania.
Both materials are contaminated with volatile organic compounds (VOCs), semivolatile organic compounds
(SVOCs), chlorinated dioxins and furans, and several trace metals, including antimony, arsenic, barium,
cadmium, chromium, copper, lead, nickel, silver, and zinc.  Copper and lead, in particular, are at very high
concentrations in both the fluff and waste and contaminated soil.  The fluff was incinerated at two kiln exit gas
temperatures: nominally 871  and 760C (1,600 and 1,400F). The soil was incinerated only at the higher kiln
exit gas temperature of 871 C (1,600F). Each test was run in duplicate (i.e., two tests were performed for each
incinerator feed/kiln temperature combination). The afterburner exit gas temperature for all tests was nominally
at 1,090C (2,000F). The primary air pollution control system consisted of a venturi/packed column scrubber
system followed by a flue gas reheater and baghouse.

          Test results showed that greater than 99.99 percent DRE of the VOC and SVOC contaminants was
uniformly achieved.  HC1 emissions were well below  1.8 kg/hr and system HC1 control efficiencies well above
99 percent. Particulate emissions at the baghouse exit were well below 34 mg/dscm (0.015 gr/dscf) corrected
to 7 percent Oj, a guideline level announced in the draft waste combustion strategy in May 1993. Baghouise exit
flue gas total chlorinated dioxin/furan levels were well below 30 ng/dscm corrected to 7 percent O2, another draft
combustion strategy guideline.  Incineration effectively decontaminated both the fluff waste and soil of their VOC
and SVOC contaminants. However, the kiln ash discharge from the incineration of contaminated site soil at a
kiln gas temperature of 871C (1,600F) contained total chlorinated dioxin/furan concentrations of 2.4 to
3.6 ug/kg.  Levels in the kiln ash from fluff incineration at the same temperature were 65 to 89 ug/kg, and
significantly increased, at 830 to 2,700 ug/kg, for incineration at a kiln gas temperature of 760C (1,400F).
In addition, the flue gas particulate collected as baghouse ash for all tests was a cadmium- and lead-contaminated
toxicity characteristic (TC) hazardous waste.

          This report was submitted in fulfillment  of Contract No. 68-C9-0038 by Acurex Environmental
Corporation under the sponsorship of the U. S. Environmental Protection Agency.  This report covers a period
from October to December 1993, and the work was completed as of December 7, 1993.
                                                IV

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                                 CONTENTS                              _


Section                                                                   Page

         DISCLAIMER .  ................... ..... . . . . .........                   ii
         FOREWORD ............... . . .............................  ..............  jii
         ABSTRACT ............. . .................................... ............  iv
         FIGURES [[[ ............  vii
         TABLES                                              '   ''"'""'
    1     INTRODUCTION
    2    FACILITY DESCRIPTION, WASTE CHARACTERISTICS, AND TEST
         CONDITIONS ...... [[[ 2-1

         2.1   ROTARY KILN INCINERATION SYSTEM DESCRIPTION ................. 2-1

         2.1.1  Incinerator Characteristics .............................................. 2-4
         2. 1.2  Air Pollution Control System ............................................ 2-5

         2.2   TEST WASTE CHARACTERISTICS  ...............                   2-6
         2.3   TEST CONDITIONS ................................... '...'.'.'.'.'.'.'.'.'.'.'.' 2-11

    3    SAMPLING AND ANALYSIS PROCEDURES ..... .......................... 3.!

         3.1   SAMPLING PROCEDURES ....... ' ................                   3_1
         3.2   ANALYSIS METHODS ......................................... ]\\\[ '3_15

    4    TEST RESULTS  ........................... . ......... . ......... ............ 4-1

         4.1   PROXIMATE AND ULTIMATE ANALYSIS RESULTS ........            4-1
         4.2   SVOC ANALYSIS RESULTS ........ . .........................    "" 4.4
         4.3   VOC ANALYSIS RESULTS ................................... [". ...... 4.12
         4.4   PCDD/PCDF ANALYSIS RESULTS ............................ '.'.'.'.':'.'.' 4-18
         4.5   TRACE METAL AND TCLP ANALYSIS RESULTS  ...............       4-31

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                            CONTENTS (continued)


Section
         QUALITY ASSURANCE
         6.1   VOC ANALYSES ........................                         62
         6.2   SVOC ANALYSES ............. ; . . . . ........ '.'.'.'.'.'.'. ...............   6-13
         6.3   TRACE METAL ANALYSES ............  ........................... 6~26
         6.4   CHLORIDE ANALYSES .............. .... ........................... 6~42
         6.5   PCDD/PCDF ANALYSES ............................ "!"!!!.'" ...... 6-42

         REFERENCES .................................................           R.j

         APPENDICES
         (Volumes 2 and 3 can be obtained from Marta Richards.)

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                                           FIGURES





Number                                                                                  D
	                                                                                  Page


 2-1       Schematic of the rotary kiln incineration system	                 2-2



 3-1       Test sampling locations	                 3_2



 3-2       Generalized CEM gas flow schematic	                 3.7



 4-1       Afterburner exit particle size distributions	                4.39
                                             Vll

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                                            TABLES


Number                                                                                    Page


 2-1       Design characteristics of the IRF rotary kiln incineration system  ...  	  2-3

 2-2       M. W. Manufacturing site waste contaminants from the ROD  	             2-7

 2-3       M. W. Manufacturing site characterization sample analysis results	  2-8

 2-4       M. W. Manufacturing site characterization sample hazardous waste characteristics
           analysis results	                          2-9

 2-5       Test matrix	;	                  2-12

 2-6       APCS operating conditions	                                      2-13

 2-7       Kiln operating conditions	                                     2-14

 2-8       Afterburner operating conditions	             2-15

 2-9       Air pollution control system operating conditions 	  2-16

 2-10      Continuous emission monitor data 	                    2-17

 3-1       Continuous emission monitors used and locations monitored  	  3-6

 3-2       Analysis procedures	                                3_g

 3-3       Test program sample analysis summary	  3_10

 3-4       Sample analysis aliquot schedule for each test	  3_12

 3-5       Sample containers, preservation methods, and hold times	  3-14

 3-6       Semivolatile organic TCL constituents	       3_17

 3-7       Volatile organic TCL constituents	            3_lg

 4-1       Proximate and elemental analysis results for composite fluff and soil feed samples	  4-2
                                              vm

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                                  TABLES (continued)
                                                                                      Page
 4-2     Weights of test material fed and kiln ash collected ...........................        4.3




 4-3     Semivolatile organic contaminant analysis results ........................           4.5




 4-4     SVOCPOHCDREs ..................................                         4.8




 4-5     BEHP concentrations in replicate fluff waste samples ____  .......................    4_10




 4-6     SVOC contaminant concentrations in replicate soil samples ____ ..........            4-1 1




 4-7     Volatile organic contaminant analysis results ................                       4. J3




 4-8     Tetrachloroethene DREs .......... . ......................                      4_16




 4-9     Flue gas VOC concentrations  ...........  . ..............................        4_17




 4-10     PCDDs and PCDFs in test feed samples  ................. . .                       4_2Q




 4-11     PCDDs and PCDFs in kiln ash samples .  ......................................  4_2i




 4-12     PCDDs and PCDFs in scrubber liquor samples . ...............................    4_22




 4-13     PCDDs and PCDFs in baghouse ash samples ...................................  4.23




 4-14     PCDDs and PCDFs in baghouse exit flue gas ................ ...................  4_24




 4-15     2,3,7,8-TCDD toxicity equivalent factors  .......................................  4.25




 4-16     Total dioxins and TEQs in test program samples ..... . .  .......................    4-26




 4-17     Ratio of discharged dioxins and furans to fed amounts ..........................    4-28




4-18     Trace metal analysis results .........................................           4.32




4-19     TCLP leachate analysis results ........................................          4.35




4-20     Particulate and HC1 emissions  .........................................         4.33
                                          IX

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                                   TABLES (continued)






Number                                                                             page




   6-1     Sample hold times for the VOC analyses of solid and liquid samples by GC/FID	 6-3




   6-2     Sample hold times for the VOC analyses of Method 0030 samples by GC/MS	 6-5




   6-3     VOC measurement QAOs	..."	     6-6




   6-4     VOC measurement MDLs: objectives and achieved levels	 6-7




   6-5     VOC recoveries from MS samples analyzed by GC/FID	          6-8




   6-6     VOC recoveries from MS samples analyzed by GC/MS	       6-9




   6-7     Duplicate sample VOC analysis results 	  6-10




   6-8     VOC surrogate recoveries in the GC/FID analysis of test samples	  6-11




   6-9     VOC surrogate recoveries in the GC/MS analysis of Method 0030 samples 	  6-12




   6-10    Sample hold times for the SVOC analyses by GC/MS	  6-14




   6-1T    SVOC measurement QAOs	              6-18




   6-12    SVOC measurement MDLs: objectives and achieved levels	  6-19




   6-13    SVOC recoveries from solid and liquid MS samples analyzed by GC/MS	  6-20




   6-14    SVOC recoveries from the Method 0010 MS samples analyzed by GC/MS  	  6-21




   6-15    SVOC surrogate recoveries in the GC/MS analysis of solid and liquid samples 	...	  6-23

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                                    TABLES (continued)






Number                                                                               Page




   6-16    SVOC surrogate recoveries in the GC/MS analysis of Method 0010 flue gas samples  ...  6-25




   6-17    Sample hold times for trace metal analyses by ICAP	  6-28




   6-18    Trace metal measurement QAOs	  6-32




   6-19    Trace metal measurement MDLS: objectives and achieved levels 	  6-32




   6-20    Trace metal analyses of method blank samples  	  6-33




   6-21    Replicate trace metal sample analysis results	  6-34




   6-22    Trace metal recoveries from MS samples analyzed by ICAP	  6-39




   6-23    Sample hold times for chloride analyses by ion chromatography  	  6-43




   6-24    Flue gas chloride measurements QAOs 	  6-43




   6-25    Chloride recoveries from MS  samples analyzed by ion chromatography 	  6-44




   6-26    Duplicate sample chloride analysis results	  6-44




   6-27    Sample hold times for the PCDD/PCDF analyses by GC/MS	  6-45




   6-28    PCDD/PCDF measurement QAOs	;	 6-47




   6-29    Duplicate sample PCDD/PCDF analysis results 	 6-48




   6-30    Internal standards recoveries in the PCDD/PCDF analyses	 6-49




   6-31    Surrogate recoveries in the PCDD/PCDF analyses	 6-51




   6-32    PCDD/PCDF measurement MDLs: objectives and achieved levels	 6-53
                                            XI

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                                      SECTION 1




                                   INTRODUCTION








        One of the primary missions of the Environmental Protection Agency's (EPA's)




Incineration Research Facility  (IRF) is  to support Regional Offices in evaluations of the




potential of incineration as a treatment option for wastes and other contaminated materials at




Superfund sites. One priority site is the M. W. Manufacturing site in Danville, Pennsylvania.




EPA Region m and the U.S. Army Corps of Engineers (USAGE) requested that a pilot-scale



test program be conducted at the IRF to support evaluations of the suitability of incineration as



a treatment technology for wastes and contaminated soil at the site.




        The M. W. Manufacturing site  began operation in 1966.  M. W. Manufacturing



Corporation reclaimed copper from scrap wire using both mechanical and chemical processes.



Reclamation activities began in 1969 and continued until 1972 when M. W. Manufacturing filed




for bankruptcy. The  chemical recovery processes used by M. W. Manufacturing led to site




contamination with volatile organic solvents. Warehouse 81, Inc., acquired the site in 1976 and



began mechanical recovery  operations from the existing waste piles onsite.  The mechanical




recovery operations generated large volumes of waste material, termed fluff.




        The fluff waste produced  by the mechanical  stripping process consists  of fibrous



insulation material  mixed with plastic.   Phthalate esters, copper, and lead are  the major



contaminants in this material. The chemical recovery process used by M. W. Manufacturing was



a two-step process.  The first step involved the use of a hot oil bath to melt the plastic insulation






                                         1-1

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away from the metal in the scrap wire.  Residual oils were removed from the separated copper



in the second step through  the  use of chlorinated solvents, including trichloroethene and



tetrachloroethene. Thus, these solvents are waste and soil contaminants at the site.




        The June 1990 record of decision (ROD) document for the site identified five wastes



and contaminated materials for remedial treatment:



            Fluff waste piles




            Organic- and trace-metals-contaminated surface soils




            Organic- and trace-metals-contaminated subsurface soils



            Lagoon water




            Contents of drums and tanks




Onsite incineration was identified as the selected treatment  for the fluff and the soil, with




possible stabilization of the incineration ash prior to landfill disposal.  Other, non-incineration




remedies were selected for treating the lagoon water and the drum/tank contents.




        Region HI requested the pilot-scale test program at the IRF to support the further



progress of the remediation of the site, and specifically to supply data on optimum incineration




conditions for both fluff waste and contaminated  soil to the remediation design effort. The



specific objectives of the IRF test program were defined as follows:




            Verify that the fluff waste and the contaminated soil at the site can be incinerated




             in compliance with the hazardous waste incinerator performance standards and



             permit requirements of:




                 99.99 percent principal organic hazardous constituent (POHC) destruction



                  and removal efficiency (DRE)




                 HC1 emissions less than 1 percent of the air pollution control system (APCS)




                  inlet flowrate  or 1.8 kg/hr (4 Ib/hr), whichever is greater






                                          1-2

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                 CO emissions of less than 100 ppm at 7 percent O2, 1-hour rolling average



              and the performance guidance announced in 1993 of:




                 Particulate emissions of less than 34  mg/dscm (0.015 gr/dscf) corrected to



                  7 percent O2




                 Total tetra-  through octa- polychlorinated  dibenzo-p-dioxin  and  poly-




                  chlorinated dibenzofuran (PCDD/PCDF) emissions of less than 30 ng/dscm



                  corrected to 7 percent O2




             Measure the effectiveness of incineration treatment in decontaminating fluff and




              soil of their organic contaminants and evaluate whether incineration temperature



              affects the effectiveness of fluff decontamination




             Measure  the  distribution  of the contaminant metals in the fluff  and the



              contaminated soil among the incineration system discharge streams




             Determine whether the bottom ash residue and the APCS discharges from the




              incineration of fluff and contaminated soil will be toxicity  characteristic  (TC)



              hazardous wastes




             Determine whether the bottom ash residue from the incineration of contaminated



              soil meets the  cleanup levels for soil given  in the ROD




        To address these objectives, a series  of seven tests was performed in the rotary kiln



incineration system (RKS) at the IRF. Results of this test program are discussed in this report.




Section 2 of the report describes the IRF's RKS in which the tests were performed.  Section 2




also discusses the composition of the fluff waste  and contaminated soil incinerated in the tests,



and the test incinerator system operating conditions.  The sampling and analysis procedures



employed  during the tests are discussed in Section 3.  Section 4  presents the test results.



Section 5 summarizes the test program conclusions.  Section 6 discusses the quality assurance






                                         1-3

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(QA) aspects of the test program.  The Appendices provide a complete data set from which




information of interest can be extracted for further study.
                                          1-4

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                                     SECTION 2

                              FACILITY DESCRIPTION,
                WASTE CHARACTERISTICS, AND TEST CONDITIONS
        A description  of  the  RKS  is presented in  Section 2.1.  Section 2.2 describes the

composition and characteristics  of the fluff waste and contaminated soil as reported in earlier

site remedial investigation reports.  The test matrix and incinerator operating conditions are

discussed in Section 2.3.

2.1     ROTARY KILN INCINERATION SYSTEM DESCRIPTION

        A  process schematic of the RKS is  shown in Figure 2-1  and the system design

characteristics are listed in Table 2-1. The RKS consists of a rotary kiln primary combustion

chamber, a transition section, a fired afterburner chamber, and an afterburner extension for flue

gas flow conditioning to allow isokinetic sampling of afterburner exit flue gas. After exiting the

afterburner extension, flue gas flows through a quench section followed by a primary air pollution

control system (APCS). The initial element of the primary APCS for these tests consisted of a

venturi/packed column scrubber system which removes most of the coarse particulate and acid

gas such as HC1 in the flue gas. Downstream  of the scrubber system, a 100-kW electric

resistance heater reheats the flue gas to about 120C (250F) which is about 22C (40F) above

the saturation temperature. A fabric-filter baghouse downstream of the reheater removes most

of the remaining flue gas particulate. Reheating the flue gas prevents moisture condensation, in

the baghouse, which if allowed to occur, would adversely affect baghouse operation.  The flue
                                        2-1

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to
N)
       NATURAL
       GAS,
       LIQUID
       FEED
TRANSFER
DUCT
                                                            PACKED
                                                            COLUMN
                                                            SCRUBBER
              SECONDARY
              BURNER
                                           VENTURI
                                           SCRUBBER
                       AFTERBURNER
                       EXTENSION
                                            SCRUBBER
                                            LIQUOR
                                            RECIRCULATION
            AFTERBURNER
SOLIDS
FEEDER
                                                    FLUE GAS
                                                    REHEATER
                                NATURAL
                                GAS,
                                LIQUID FEED
                                              PRIMARY AIR POLLUTION
                                                 CONTROL SYSTEM
CARBON BED HEPA
ADSORBER   FILTER
                                                                        BA HOUSE
           ROTARY KILN
           INCINERATOR
                                             REDUNDANT AIR
                                           POLLUTION CONTROL
                                                 SYSTEM
                                                                                                             o
                                                                                           ATMOSPHERE


                                                                                                 STACK
                                                                                                      psr
                                                                        ID FAN
                                  Figure 2-1. Schematic of the rotary kiln incineration system.

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TABLE 2-1.  DESIGN CHARACTERISTICS OF THE IRF ROTARY KILN INCINERATION
               SYSTEM

Characteristics of the Kiln Main Chamber
Length                  2.26 m (7 ft-5 in)
Diameter, outside         137 m (4 ft-6 in)
Diameter, inside          Nominal 1.04 m (3 ft-4.75 in)
Chamber volume         1.90 m3 (613. ft3)
Construction             0.95 cm (0375 in) thick cold-rolled steel
Refractory               18.7 cm (7375 in) thick high, alumina castable refractory, variable depth to produce a
                         frustroconical effect for moving solids
Rotation                 Clockwise or counterclockwise, 0.2 to 1.5 rpm
Solids retention time      1 hr (at 0.2 rpm)
Burner                  North American burner rated  at 590 kW (2.0 MMBtu/hr) with liquid feed capability
Primary fuel              Natural gas
Feed system:
  Liquids                 Positive displacement pump via water-cooled lance
  Sludges                 Moyno pump via front face, water-cooled lance
  Solids                  Metered screw feeders or fiberpack ram feeder
Temperature (max)	I.OIO'C (1,850F)	

Characteristics of the Afterburner Chamber
Length                  3.05 m (10 ft)
Diameter, outside         1.22 m (4 ft)
Diameter, inside          0.91 m (3 ft)
Chamber volume         1.80 m3 (63.6 ft3)
Construction             0.63 cm (0.25 in) thick cold-rolled steel
Refractory               15.2 cm (6 in) thick high alumina castable refractory
Gas residence time        0.8 to 1.5 s depending on temperature and excess air
Burner                  North American Burner rated at 590 kW (2.0 MMBtu/hr) with liquid feed capability
Primary fuel              Natural gas
Temperature (max)	1,200C (2,200''F)	

Characteristics of the Afterburner Extension
Length, with transition     4.43 m (14 ft-6.5 in)
sections
Diameter, outside         0.915 m (3 ft)
Diameter, inside          0.61 m (2 ft)
Chamber volume       .  1.19 m3 (41.9 ft3)
Construction             0.63 cm (0.25 in) thick cold-rolled steel
Refractory               15.2 cm (6 in) thick high alumina castable refractory
Temperature (max)	1,200C (2,200F)	

Characteristics of the Venturi/Packed-column Scrubber APCS
System capacity, inlet gas   107 m3/min (3,773 acfm) at l,200eC (2,2000F) and 101 kPa (14.7 psia)
flow
Pressure Drop
  Venturi scrubber        75 kPa (30 in WC)
  Packed column          1.0 kPa (4 in WC)
Liquid flow
  Venturi scrubber        77.2 L/min (20.4 gpm) at 60 kPa (10 psig)
  Packed column          116 L/min (30.6 gpm) at 69 kPa (10 psig)
pH control               Feedback control by NaOH solution addition
                                                                                         '       (continued)
                                                  2-3

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                                  TABLE 2-1.  (continued)
  Characteristics of the Baghouse Collector
  System capacity, inlet gas 70 m3/min (2,500 acfm) at 120eC (250'F)
  flow
  Operating temperature   200C (400eF)
  Operating pressure      12.4 kPa (50 in WC)
  Diameter             1.8 m (6 ft)
  Overall height          42 m (13 ft, 8375 in)
  Filter elements (bags)
   Material             16 oz. Nomex
   Length              1.8m (6 ft)
   Number             69
 Total filter area        45 m2 (488 ft2)
 Material of construction
   Collector internals     304 SS
   Airlock              316 SS
   Venturi nozzles        Aluminum
  Insulation             Heat loss less than 8.8 kW
                      (30,000 Btu/hr) at 200C (400F)
gas reheat/baghouse system was installed just prior to the initiation of these tests, in large part

to satisfy a Region III request.

        Downstream of the baghouse, a backup secondary APCS, comprised of an activated-

carbon adsorber and a high-efficiency particulate air (HEPA) filter, is in place for further control

of organic compound and particulate emissions. The main components of the RKS and its APCS

are discussed in more detail in the following subsections.

2.1.1   Incinerator Characteristics

        The rotary kiln combustion chamber has an inside diameter of 1.04-m (40.75-in) and is

2.26-m (7-ft 5-in) long. The chamber is lined with refractory formed into a frustroconical shape

to an average thickness of 18.7 cm (7.375 in). The refractory is encased in a 0.95-cm (0.375-in)

thick steel shell. Total volume of the kiln chamber; including the transition section, is 1.90 m3

(67.2 ft3).  Four steel rollers support the kiln barrel. A variable-speed DC-motor coupled to a

reducing gear transmission turns the kiln. Rotation speeds can be varied from 0.2 to 1.5  rpm.

For these tests the kiln rotational speed was 0.2 rpm.
                                            2-4

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        The afterburner chamber has a 0.91-m (3-ft) inside diameter, and is 3.05 m (10 ft) long.



The afterburner wall is constructed of a 15.2-cm (6-in) thick layer of refractory encased in a




0.63 cm (0.25 in) thick carbon steel shell. The volume of the afterburner chamber is 1.80 m3



(63.6ft3).



2.1.2    Air Pollution Control System




        For this test program, the RKS primary APCS consisted of the venturi scrubber/packed-



column scrubber combination, followed by a flue gas reheater and a baghouse.  The flue gas




exiting the afterburner passes through the refractory-lined transfer section and enters the quench




section, where the flue gas temperature is reduced to approximately  82C (180F) by direct




injection of aqueous caustic scrubber liquor.  The  cooled flue gas then enters the venturi




scrubber, which is fitted with an automatically adjustable-area throat. The scrubber is designed




to operate at 6.2 kPa (25 in WC) differential pressure, with a maximum liquor flowrate of




77.2 L/min (20.4 gpm). The scrubber liquor, again an aqueous caustic solution, enters at the top




of the scrubber and contacts the flue gas to remove entrained particles and, to some degree, acid




gases.




        Downstream of the venturi scrubber, the flue gas enters the packed-column scrubber,



where additional acid gas and particulate cleanup occurs. The scrubber column is packed with



5.1 cm (2 in) diameter polypropylene ballast saddles to a depth of 2.1 m (82 in).  It is designed




to operate at  1.0 kPa (4 in WC) differential pressure, with a maximum liquor flowrate of



116 L/min (30.6 gpm).




        The quench, venturi scrubber, and packed-column scrubbers receive their scrubber liquor



from the same recirculation system. This liquor is a dilute aqueous NaOH solution, the pH of




which is monitored continuously by a pH sensor. An integral pH controller automatically meters




the amount of NaOH needed to maintain the setpoint pH for proper acid gas removal.
                                          2-5

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        Following the quench, venturi scrubber, and packed-column scrubber systems, the flue



gas is reheated to  about 120 C (250 F) by a 100-kW electric duct heater, and then passed




through the baghouse.  The baghouse removes most of the remaining flue gas participate.



Reheating the flue gas ensures that no moisture condenses in the baghouse, which can adversely



affect its operation.




        In  a typical commercial incinerator system,  the  flue gas would  be vented to  the



atmosphere downstream of the baghouse.  However, at the IRF, a backup APCS is in place to




further clean up the flue gas.  The flue gas exiting the baghouse is passed through a bed of




activated carbon to allow the vapor-phase organic compounds to be adsorbed.  A set of HEPA




filters designed to  remove any remaining suspended paniculate from the flue gas is located




downstream of the carbon bed. An induced-draft (ID) fan draws and vents the treated flue gas



to the atmosphere.




22     TEST WASTE CHARACTERISTICS




        Data on the  contaminant concentrations in the fluff waste and the  surface and




subsurface  soil  at  the site, taken from  the site record of decision (ROD) document,  are



summarized in Table 2-2. Only contaminants present at an average concentration of 1 mg/kg



or greater in one or more contaminated site matrix are listed in the table.  The data in Table 2-2




show that the major site contaminants are the two phthalate esters, bis(2-ethylhexyl)phthalate




(BEHP) and  di-n-octylphthalate (DNOP).  Thus, these compounds would be considered the




POHCs in the  site wastes.   In  addition, Region ffl was interested in establishing that



tetrachloroethene is effectively destroyed by incineration, so tetrachloroethene was also defined




to be a POHC.  Site wastes are also highly contaminated with copper and lead, with lesser,




though still significant, amounts of antimony, barium, chromium, nickel, and zinc.
                                         2-6

-------
        TABLE 2-2. M. W. MANUFACTURING SITE WASTE CONTAMINANTS FROM THE ROD
Concentration, mg/kg
Fluff
Contaminant
Volatile Organic Constituents
2-Butanone
Tetrachloroethene
Trichloroethene
1,1,2-Trichloroethane
1,2-Dichloroethene
Methylene chloride
Semivolatile Organic Constituents
Bis(2-ethylhexyl)phthalate
Di-n-octyl phthalate
Di-n-butyl phthalate
PCB-1254
Trace Metals
Antimony
Barium
Cadmium
Chromium
Copper
Lead
Nickel
Silver
Zinc
Range over
17 samples

2.8-6.4
0.72-18.0



up to 7.7

72,000-230,000
1.800-13,000

0.90-18.1

80-143
20-232
0.65-4.4
24-59
5,910-130,000
1,600-3,600
4.1-15
1.6-5.7
135-2,580
Average

1.6
4.4



0.45

149,000
4,400

9.4

65
93
2.4
40
50,000
2,400
4.6
1.8
620
Surface soil
Range over
21 samples

_
0.023-67
0.002-21
0.003-2.8
0.002-10
up to 0.83

3.9-3,000
0.2-140
0.48
0.061-3.7

62-118
22-107
1.2-12
7.1-59
742-171,000
32-9,770
8.5-40
8.6
55-787
Average


10
1.0
0.28
0.49
0.04

836
37
0.02
0.21

16
74
2.0
27
21,600
1,450
22
0.4
240
Maximum average
subsurface soil
Range

up to 3.9
0.001-l,600b
0.002-2.6
up to 5.4
0.004-0.58
-

OJO-30,OOOb
0.038-150
0.036-130
0.077-1.0

, ,
47-218
1-13
14-70
24-38,900
7-741
42-50
.
56-319
Average

0.78
56
2.7
1.1
0.04


1,480 '
7,850
3.9
0.043

1 	 T
107
1
20
1,850
160
46
__
144
Depth

16-18
4-6
12-14
16-18
8-10


12-14
0-2
0-2
0-2

v
0-2
0-2
0-14
12-14
16-18
6-8
_
6-8
* = Not reported.
bMaximum value in range represents an estimated value above minimum detection limit but below lowest calibration standard  ("J" flag).

-------
       Samples of the fluff waste and surface and subsurface soil were sent to the IRF for

characterization analyses. Results of the analyses are summarized in Table 2-3. As shown, the

soil characterization samples had contaminant concentrations in the range reported in the ROD.

Contaminant concentrations in the fluff waste characterization samples were also in the range

reported  in the ROD for most contaminants.  However,  the fluff characterization sample
TABLE 2-3.  M. W. MANUFACTURING SITE CHARACTERIZATION SAMPLE ANALYSIS
            RESULTS
Sample
Parameter
Characterization
Moisture, %
Ash, %
at 550C
at 900C
Heating value, MJ/kg
(Btu/lb)
Volatile Organic Constituents, mg/kg
Tetrachloroethene
1, 1,2-Trichloroethane
Semivolatile Organic Constituents, mg/kg
BEHP
DNOP
Trace Metals, mg/kg
Antimony
Barium
Cadmium
Chromium
Copper
Lead
Nickel
Silver
Zinc
Fluff

7.7

41
14
6.50
(2,800)

146
4.8

124,000
17,800

230
64
3.5
57
31,000
2,700
6.1
4.0
890
Surface soil

18

77
76
0.07
(30)

69
1.5

47.6
1.95

51
60
<0.2
30
8,300
1,800
15
<0.4
76
Subsurface soil

9.8

89
90
Will not burn

18
NDa

4.62
ND

<5
78
0.93
21
160
180
31
<0.4
62
    aND = Not detected.
                                        2-8

-------
contained substantially more tetrachloroethene, 1,1,2-trichloroethane, DNOP, and antimony that

did fluff samples reported in the ROD.

       Characterization  samples  received  were  also  analyzed  for  hazardous  waste

characteristics, including the preparation and analysis of toxicity characteristic leaching procedure

(TCLP) leachates of the samples. Results are summarized in Table 2-4.

       The two semivolatile POHCs in site materials, BEHP and DNOP, are poor candidates

for testing the incineration  process with regard to  destroying other site,  waste organic

contaminants because they are ranked as relatively easy to thermally destroy compounds in the
      TABLE 2-4. M. W. MANUFACTURING SITE CHARACTERIZATION SAMPLE
                 HAZARDOUS WASTE CHARACTERISTICS ANALYSIS RESULTS
Characteristic
Reactivity -S, mg/kg
Reactivity -CN, mg/kg
Corrosivity, pH
Ignitability, F
TCLP leachate,. mg/L
Arsenic
Barium
Cadmium
Chromium
Copper
Lead
Mercury
Nickel
Selenium
Silver
Zinc
Pesticides and other organics
Fluff
waste
<0.01
<0.01
6.85
>200

<0.10
0.10
0.11
0.11
199
3.1
< 0.002
<0.01
<0.10
<0.01
5.1
NDb
Surface
soU
<0.01
<0.01
8.15
>200

<0.10
0.37
0.07
0.09
158
3.2
< 0.002
<0.01
<0.10
<0.01
0.49
ND
Subsurface
soil
<0.01
<0.01
6.37
>200

<0.10
0.21
0.07
0.09 
1.88
0.20
< 0.002
<0.01
<0.10
<0.01
0.12
ND
Regulatory
level
Contains
and reacts
<2, >12
<140

5.0
100
1.0
5.0
__a
5.0
0.2
1.0
5.0

     a = No regulatory level.
     bND = Not detected at detection limits ranging from 0.004 to 0.01 mg/L.
                                        2-9

-------
 thermal stability based incinerability ranking (Reference  1).  This ranking groups the 333




 compounds ranked into seven stability classes from most stable, or most difficult to destroy



 (Class 1), to least stable or easiest to destroy (Class 7). Both BEHP and DNOP are ranked in




 Class 6, or relatively easy to destroy.  To present a challenge to the incineration process and




 develop data that suggest incineration is capable of achieving sufficient DREs for other site



 organic contaminants, the test waste materials were spiked with naphthalene, a Class 1 (most




 difficult to destroy) POHC, at 2 percent by weight.  This spiking level allows DREs of over



 99.999 percent to be quantitated at easily achieved flue gas sampling and analysis method




 quantitation limits.  In addition, it was decided to spike the volatile POHC, tetrachloroethene,




 into test materials at a level of 3,100 mg/kg by weight. Tetrachloroethene is a Class 2 POHC.




 Spiking was needed because site material concentrations of tetrachloroethene were too low to




 allow establishing 99.99 percent DRE  at achievable flue gas concentration quantitation limits.




        Prior to initiating the test program, all  test feed material was packaged into 1.5-gal




 (5.7-L) polyethylene (PE)-bag-lined  cubical cardboard containers for feeding to the RKS. For




 fluff packaging, the contents of three 55-gal (208-L) shipment drums (of the 14 fluff-containing




 drums received at the IRF for testing)  were emptied into a 250-gal (946-L) mixing trough. The




 trough contents were manually mixed  with hoes until visually homogeneous.  Trough contents



 were then used to fill feed containers. Each container was filled with about 1.8 kg (4 Ib) of




 mixed fluff.  A mixed trough would fill 150 containers, with a small quantity left over.  This small




 quantity would be combined with the next three drums added to the trough for mixing.




        This mixing process resulted in four full-trough fluff batches, with  each batch used to



package  150 feed containers. All containers from a given batch were placed on a pallet for




short-term storage, resulting in four 150-container pallets. A fifth partial-trough batch was used




to package a final 120 feed containers, which were placed on a fifth pallet.  The containers on
                                          2-10

-------
 the fifth pallet were used during scoping tests to verify the ability to feed the test material and




 maintain target RKS operating conditions. For each of the actual four fluff incineration tests



 performed, essentially equal numbers of Containers were randomly selected from each of the first



 four pallets to constitute the feed materials for the test.




        Naphthalene was  added  to  each fluff-filled box as a  preweighed count  of solid



 naphthalene crystals (36.4 g) contained in a 60-mL high-density polyethylene (HDPE) bottle with




 a polypropylene screw cap closure, weighing about 14.4  g. The tetrachloroethene (5.6 g) was




 added in a 4-mL HDPE bottle, with a polypropylene screw cap closure, weighing 2.6 g. Feed




 boxes were spiked the day before a given test by imbedding the HDPE bottles in the feed box




 contents. The box polyethylene liner was then closed with a plastic tie, and the box itself dosed



 and sealed with paper packaging tape.




        Contaminated soil for testing was similarly mixed, except that all five of the drums of




 soil received at the IRF for testing (whether surface, subsurface, or mixed not specified) were




 mixed in one trough mixing exercise. Mixed soil was packaged into the 120 feed containers, each




 containing about 4.5-kg (10-lb) of soil.  The naphthalene  spike added the day before a soil test



 was 90.9 g in a 125-mL HDPE bottle, and the tetrachloroethene spike was 14.5 g in an 8-rnL



 bottle.




23      TEST CONDITIONS




        The test program  completed consisted of seven tests.  Of these seven, two sets  of



 duplicate tests feeding fluff waste alone and one set of duplicate tests feeding contaminated soil




alone were performed.  The  two sets of fluff feed tests were conducted at different kfln




combustion gas temperatures.  Soil and fluff were separately tested because the eventual site




remediation may treat each material separately for logistical reasons. In addition, Region in
                                         2-11

-------
 requested data to determine whether the ash from incinerated soil alone would meet the cleanup



 levels given in the ROD.  The target test operating conditions were as given in Table 2-5.




        A seventh test, denoted Test 0 in Table 2-5, was performed as a blank burn. Only feed



 packaging materials - the cardboard box, PE bag liner, HDPE spike bottles (no POHC spike)



 with closures, plastic tie, and paper tape  were fed to the RKS for the blank burn.




        For all tests, the target afterburner exit gas temperature was 1,090 C (2,000 F). The




 venturi/packed-column scrubber and baghouse APCS units were operated at their normal design



 settings. Kiln rotation rate was set to give a 30-minute kiln solids residence time.




        The target average test material feedrate was 54.5 kg/hr (120 Ib/hr) for all tests except




 the blank burn.   Test materials were fed to the RKS via the fiberboard container ram feed




 system. A total of 30 containers per hour (one container every 2 minutes) was fed to achieve



 the target feedrate for the fluff tests;  12 containers per hour (one container every 5 minutes)




were fed to achieve the target feedrate for the soil tests.  The blank burn was conducted feeding



30 containers (no waste or soil) per hour.




        For all tests, the scrubber system was operated at its design settings, listed in Table 2-6,



and at as close to total recirculation  (zero to  minimum  blowdown) as possible.  Given the
                              TABLE 2-5.  TEST MATRIX
Test
0
1
2
3
4
5
6
Feed
Packaging container material
Fluff
Duplicate of Test 1
Soil
Duplicate of Test 3
Fluff
Duplicate of Test 5
Target kiln exit gas temperature,
O^t /O'K*\
** V. '/
870 (1,600)
870 (1,600)

870(1,600)

760 (1,400)

                                         2-12

-------
                     TABLE 2-6.  APCS OPERATING CONDITIONS
          Venturi liquor flowrate        76 L/min (20 gpm)
          Venturi pressure drop         6.2 kPa (25 in WC)
          Packed tower liquor flowrate,  115 L/min (30 gpm)
          Scrubber liquor temperature   49 C (120 F)
          Scrubber blowdown rate       0 L/min (0 gpm) or minimum operable
relatively short (nominally 4 to 5 hours) duration of a test, no operational problems due to solids
buildup in the scrubber liquor occurred even at total recirculation. For the fluff waste and blank
burn tests, kiln ash was continuously deposited in initially clean 20-gal (76-L) drums placed in
the RKS ash pit. For the soil tests, kiln ash was continuously removed from the kiln ash hopper
via an ash auger transfer system and deposited into 55-gal (208-L) drums.
        The  actual kiln and  afterburner operating conditions achieved  for each  test are
summarized in Tables 2-7 and 2-8, respectively.  Table 2-9 provides a similar summary of the
APCS operating conditions for each test.  Continuous  emission monitor (CEM) data are
summarized in Table 2-10. The ranges and averages of the temperature, CEM, and scrubber pH
data presented in Tables 2-7  through 2-10 were developed  for the periods of the  flue gas
sampling, using the data automatically recorded by a personal computer-based data acquisition
system.  The values given for the remaining parameters were derived from the control room
logbook data.
        Transcribed data from  the control room logs of the operating parameters, recorded at
15-minute intervals, are given in Appendix A. Appendix B contains graphic presentations of the
flue gas  temperature  and  continuous emission  monitor data for the kiln and afterburner.
Appendix B also contains graphic presentations of the scrubber exit and stack flue gas continuous
emissions monitor data. These data plots were based on incinerator system conditions recorded
                                        2-13

-------
                                    TABLE 2=7.  KILN OPERATING CONDITIONS
to
Parameter
Average natural gas
feedrate,

Average combustion air
flowrate,
Average total air flowrate
(includes inleakage),
Average draft,

Exit gas temperature,



Exit gas O2

Average waste feedrate,

Average waste heat input,

Total heat input,

=====
scm/hr
(scfh)
kW
(kBtu/hr)
scm/hr
(scfh)
scm/hr
(scfh)
Pa
(inWC)
Range, "C
(F)
Average, "C
(F)
Range, %
Average, %
kg/hr
(Ib/hr)
kW
(kBtu/hr)'
kW
(kBtu/hr)
TestO
(10/27/93)
33
(1,156)
339
(1,156)
226
(7,970)
679
(23,980)
7
0.03
842-898
(1,548-1,648)
871
(1,599)
8.4-13.4
11.6
5
(12) .
10
(34)
349
(1,190)
Testl
(11/9/93)
22
(778)
228
(778)
214
(7,560)
1,054
(37,200)
7
0.03
827-921
(1,520-1,689)
883
(1,622)
7.7-14.0
10.9
60
(132)
224
(765)
452
(1,543)
Test 2
(11/16/93)
23
(820)
240
(820)
205
(7,250)
1,067
(37,670)
7
0.03
814-918
(1,498-1,685)
876
(1,608)
8.2-14.6
11.0
59
(130)
218
(743)
458
(1,563)
======
TestS
(11/18/93)
13
(475)
139
(475)
191
(6,760)
1,000
(35^00)
5
0.02
716-804
(1321-1,479)
762
(1,403)
8.7-14.2
11.8
61
(134)
227
(774)
366
(1,249)
Test 6
(11/23/93)
14
(507)
149
(507)
174
(6,140)
1,008
(35,610)
7
0.03
724-807
(1336-1,484)
767
(1,412)
9.0-14.0
11.8
61
(134)
224
(765)
373
(1,272)
Test 3
(12/1/93)
JQ
J\t
(1,065)
312
(1,065)
200
(7,070)
675
(23,840)
5
0.02
853-912
(1,568-1,674)
876
(1,609)
8.0-13.5
11.1
59
(130)
30
(104)
342
(1,169)
.
Test 4
(12/2/93)
31
(1,085)
318
(1,085)
19ft
ixO
(6,990)
673
(23,750)

0.02
862-894
(1,583-1,642)
874
(1,606)
7.7-13.1
10.9
59
(130)
31 "
(104)
348
J*tO
(1,189)
     Calculated combustion gas
     residence time,
seconds

-------
TABLE 2-8. AFTERBURNER OPERATING CONDITIONS
Parameter
Average natural gas
feedrate,


Average combustion air
flowrate,
Exit gas temperature,



Exit gas O2


scm/hr
(scfh)
kW
(kBtu/hr)
scm/hr
(scfh)
Range, "C
(F)
Average, C
(F)
Range, %
Average, %
TestO
(10/27/93)
29
(1,025)
300
(1,025)
194
(6,840)
1,090-1,107
(1,994-2,025)
1,098
(2,008)
8.8-12.0
10.7
Testl
(11/9/93)
27
(948)
278
(948)
165
(5,830)
1,089-1,152
(1,992-2,106)
1,103
(2,017)
4.2-11.7
7.6
Test 2
(11/16/93)
26
(903)
265
(903)
156
(5,520)
1,087-1,105
(1,989-2,021)
1,097
(2,007)
5.7-10.8
8.2.
Test 5
(11/18/93)
24
(861)
252
(861)
129
(4,550)
1,091-1,105
(1,996-2,021)
1,097
(2,007)
5.1-10.8
8.0
Test 6
(11/23/93)
25
(876)
257
(876)
118
(4,180)
1,091-1,102
(1,995-2,016)
1,097
(2,007)
5.1-9.1
7.9
Test 3
(12/1/93)
27
(943)
276
(943)
157
(5,540)
1,091-1,115
(1,196-2,039)
1,098
(2,008)
8.7-14.2
11.8
Test 4
(12/2/93)
33
(1,166)
342
(1,166)
161
(5,700)
1,090-1,106
(1,994-2,023)
1,097
(2,007)
9.0-14.0
11.8

-------
TABLE 2-9. AIR POLLUTION CONTROL SYSTEM OPERATING CONDITIONS
ii =^^^s^aa
Parameter
Average quench chamber
liquid flowrate,
Average venturi scrubber
liquid flowrate
Average packed-column
scrubber liquid flowrate,
Scrubber liquor, pH

Average scrubber- makeup
flowrate,
Average scrubber liquor
temperature,
Average scrubber inlet gas
temperature,
Average scrubber exit gas
temperature,
===========.

L/min
(gpm)
L/min
(gpm)
L/min
(gpm)
Range
Average
L/min
(gpm)
c
(F)
c
(.F)
c
(F)
TestO
(10/27/93)
76
(20)
76
(20)
114
(30)
6.9-7.1
7.0
1,098
(290)
67
(152)
76
(169)
59
(138)
i3SS355BS2KHH
=====
Test 1
(H/9/93)
76
(20)
79
(21)
110
(29)
5.9-8.2
6.9
57
(15)
69
(156)
78
(173)
64.
(147)
=====
========
Test 2
(11/16/93)
75
(20)
76
(20)
114
(30)
6.0-83
7.1
0
(0)
69
(156)'
78
(173)
64
(147)
=====
==
Test 5
(11/18/93)
76
(20)
79
(21)
114
(30)
6.8-8.2
7.3
193
(51)
67
(152)
77
(171)
60
(140)
  
Test 6
(11/23/93)
If.
/U
(20)
79
(21)
114
(30)
6.4-8.2
7.2
o
(0)
68
(155)
77
(171)
62
UA>
(143)
 ^^ -^ .
Test 3
(12/1/93)
72
(19)
QO
OJ
(22)
110
(29)
6.7-75
7.2

(3)
f.Q
oy
(156)
7/
/O
(169)
1
Ol
(141)
Test 4
(12/2/93)
1C.
76
(20)
*TiT
76
(20)
114
(30)
6.6-7.5
7.2

(0)
sn
by
(156)
*7
76
(169)
*
61
.("I)

-------
TABLE 240. CONTINUOUS EMISSION MONITOR DATA
Parameter
Kiln Exit
02
Afterburner Exit
02
C02
NOX
Baghouse Exit
02
CO
C02
TUHC
NOX
Stack
02
CO


Range, %
Average, %
Target, %

Range, %
Average, %
Target, %
Range, %
Average, %
Range, ppm
Average, ppm

Range, %
Average, %
Range, ppm
Average, ppm
Range, %
Average, %
Range, ppm
Average, ppm
Range, ppm
Average, ppm

Range, %
Average, %
Range, ppm
Average, ppm
TestO
(10/27/93)

8.4-13.4
11.6
10.0

8.8-12.0
10.7
8.0
53-8.1
6.2
45-82
66

12.0-15.1
12.9
<1-10
2
2.5-5.2
4.3

-------
at about 35-second intervals on the RKS data acquisition system. In addition, durations of flue
gas sampling periods, major events, cumulative amounts of waste fed into the incinerator, and
cumulative amounts of ash removed from the incinerator are included in some plots. These data
provide the basis for  assembling a complete picture of the actual incinerator operating
conditions.
                                        2-18

-------
                                     SECTION 3




                      SAMPLING AND ANALYSIS PROCEDURES








        The scope of the sampling efforts performed in the test program is illustrated in




Figure 3-1. The sampling effort performed is discussed in Section 3.1, followed by a discussion



of the sample analysis procedures in Section 3.2.




3.1     SAMPLING PROCEDURES




        For all tests, the sampling matrix included:




            Obtaining a composite sample of the test feed material




            Obtaining a composite sample of the kiln ash discharge




            Obtaining a composite sample of the pre-test and post-test scrubber system liquor



            Obtaining a composite sample of the baghouse ash




            Continuously measuring O2 concentrations in the kiln exit flue gas; O2, CO2, and




             NOX in the afterburner exit flue gas; O2,  CO, CO2, NOX, and total unhurried




             hydrocarbon (TUHC) concentrations in the baghouse exit flue gas; and O2 and



             CO concentrations in the stack gas




            Sampling the flue gas at the baghouse exit for trace metals using the EPA multiple



             metals train (Reference 2)




            Sampling the flue gas at the baghouse exit for the waste and spiked semivolatile



             POHCs and other semivolatile target compound list (TCL) constituents using an



             EPA Method 0010 train (Reference 3)






                                        3-1

-------

KILN
1


AFTER-
BURNER



FLUE GAS
QUENCH

        2     3
VENTURI
SCRUBBER
1


PACKED
COLUMN
SCRUBBER
1
5


FLUE GAS
REHEAT


RAftMni IQP

1
6

7
CARBON
BED



HEPA
FILTER



u>
                                                                Continuous monitors
                Test feed  Kiln  Scrubber  Baghouse                     Healed
Sampling point    material  ash    liquor     ash    O2  CO  CO2  NO, TUHC
                                                                                                          Flue gas
                                                                                          EPA multiple
                                                                                          metals train,                                       Method 5,
                                                                                            test trace   Method 0010,  Method 0030,   Method 23,  participate
                                                                                             metals       SVOCs        VOCs     PCDD/PCDF  and HCI
1. Feed X
2. Kiln ash discharge X
3. Kiln exit flue gas
4. Afterburner exit
flue gas


X
XXX
        5. Scrubber liquor

        6. Baghouse hopper

        7. Baghouse exit flue
                                                  X   X   X    X
X
        8. Stack gas
                                                  X   X
                                                          Figure 3-1.  Test sampling locations.

-------
             Sampling the flue gas at the baghouse  exit for the waste and spiked volatile



              organic contaminants and other volatile fCL constituents using EPA Method 0030



              (Reference 3), the volatile organic sampling train (VOST)




             Sampling the flue gas at the baghouse exit for  PCDDs/PCDFs  using EPA



              Method 23  (Reference 2)




             Sampling the baghouse exit and the stack for particulate and HC1 using EPA




              MethodS;  the stack sample  was needed  to comply with the IRF's permit



              requirements




         Composite feed material samples were collected from each mixing trough after feed




 material was mixed in the trough, as discussed in Section 2.2, but before packaging into  the




 cardboard containers.  Samples were collected from six different locations in the  trough and




 combined to form the composite sample representing the trough's contents.  Four fluff feed




 samples resulted, each representing one full trough mixture. Two soil feed samples resulted, the




 first taken before the packaging of the first soil feed container, the second after-the filling of 60



 soil feed containers.




        The feed sample for Test 0, the blank burn test, consisted of proportionate samples of



 the cardboard box material, the polyethylene liner bag, the bag plastic tie, the HDPE bottle with



 screw cap, and the paper packaging tape used to prepare feed boxes.




        On  a given test day, the incinerator was brought to nominally steady operation at test




 conditions while firing auxiliary fuel (natural gas) alone.  Test material feed was then initiated.




 Flue gas sampling was started about 1 hour after test material feed initiation. At the conclusion



 of each test day, the  incinerator was operated  on natural gas for 2 hours after waste feed



cessation while ash material in the kiln continued to discharge until the kiln was empty.
                                         3-3

-------
          During the fluff waste tests, kiln ash was continuously deposited in an initially dean



  20-gal (76-L) drum placed in the RKS ash pit. The amount of collected ash was insufficient to



  allow representative thief sampling, therefore grab samples consisting of a large fraction of the



  collected ash were taken.




         During the soil feed tests, kiln ash was continuously removed from the kiln ash pit via



  a transfer auger and deposited into a 55-gal (208-L) 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. The three ash samples were combined to form one



  composite sample.




         No kiln ash resulted from the blank burn test.




         Each test was run with the scrubber liquor loop operating at as close to total recycle (no




 blowdown) as possible. At the end of each test day, a scrubber liquor sample was collected from




 a tap  in the recirculation loop. The scrubber liquor was then drained to a collection tank. In




 addition, a sample was  taken  from the  scrubber liquor loop from the same tap just  before



 initiating test material feed on a test day. The baghouse ash sample consisted of the entire



 amount of baghouse ash collected in the baghouse ash hopper for each test.




        The  Method 5  trains  for participate  and HC1 collection had dilute caustic-filled



 impingers  (0.1 N NaOH).  Admittedly, both HC1 and C12 in the flue gas are collected caustic



 impingers. However, this conservative estimate of HC1 concentrations (HC1 plus C12) satisfied



 test  program objectives.  A nominal 1.4 m3 (50 ft3)  sample was collected at the two locations




 sampled over  about a 1-hour time period.  The Method 0010, Method 23, and multiple metals




 trains sampled nominally 2.8 m3 (100 ft3) of flue gas over a 3-hour period. Because mercury was




not a trace metal of interest in this program, the permanganate impingers for mercury collection




were not used in the multiple metals train, and sample recovery steps specified for eventual
                                          3-4

-------
 mercury analysis were not performed.  Four Method 0030 trap pairs each sampled 20 L of flue



 gas. Four trap pairs were taken as insurance against trap breakage.




        The CEMs available at the IRF and the locations that they monitored during all tests



 are summarized in Table 3-1.  This  monitoring arrangement was  employed in  all tests.



 Figure 3-2 illustrates the generalized flue gas conditioning and flow distribution system at the




 IRF. Four independent systems, such as the one illustrated in Figure 3-2, were in place so that




 the appropriately conditioned sample  gas from four separate locations was routed to the




 respective monitors in Table 3-1. The CEM setup described in Table 3-1, with appropriate gas




 conditioning per Figure 3-2, was  employed throughout  this test program.  CEM data was




 recorded continuously on strip charts and also by an automatic data acquisition system.




        Test program samples were analyzed for matrix-specific combinations of SVOCs, VOCs,



 PCDDs/PCDFs, contaminant  trace metals, and chloride.   Sample analysis procedures are




 outlined in Table 3-2. The number of test program samples analyzed is summarized in Table 3-3.




 The numbers of method blank, split sample, and matrix spike/matrix spike duplicate QA analyses




 are also given in Table 3-3. The large numbers of fluff and soil feed split sample analyses for



 SVOC and trace metals, and kiln ash split sample analyses for trace metals, were at the request




 of Region HI.  The Region HI Remediation Project Manager (RPM) requested  that the



 precision of the feed and ash trace metal and feed SVOC concentration measurements be well



 characterized.




        Table 3-4 summarizes the sample aliquoting schedule for dividing samples taken for each



 test among the various analytical procedures.   Each sample was divided among the various



 analytical  procedures according to  Table 3-4.  Aliquots analyzed as noted in  Table 3-4



corresponded to respective method-recommended sample sizes.
                                         3-5

-------
TABLE 3-1. CONTINUOUS EMISSIONMONITORS USED AND LOCATIONS MONITORED
Monitor
Location
Kiln exit


Afterburner
exit






Baghouse
exit











Stack




Constituent Manufacturer
O2 Beckman


O2 Rosemount


CO2 Horiba

NOX Thermo
Electron

O2 Beckman


CO Horiba

CO2 Horiba

TUHC Beckman


NOX Thermo
Electron

O2 Teledyne


CO Horiba

Model
755


755


PIR 2000

10 AR


755


VIA 500

PIR 2000

402


10 AR


326A


VIA 500

Principle
Paramagnetic


Paramagnetic


NDIR

Chemiluminescent


Paramagnetic


NDIR

NDIR

FID


Chemiluminescent


Fuel cell


NDIR

Range
0-10 percent
0-25 percent
0-100 percent
0-10 percent
0-25 percent
0-100 percent
0-20 percent
0-80 percent
0-75 ppm to
0-10,000 ppm in
multiples of 2
0-10 percent
0-25 percent
0-100 percent
0-50 ppm
0-500 ppm
0-20 percent
0^80 percent
0-10 ppm
0-100 ppm
0-1,000 ppm
0-75 ppm to
0-10,000 ppm in
multiples of 2
0-5 percent
0-10 percent
0-25 percent
0-50 ppm
0-500 ppm
                                  3-6

-------
                           FILTER
HIGH
BAY
CONTROL
ROOM
                                       PUMP
                                                 FILTER
                            CHILLED WATER
                            MPINGER
                                   HEATED
                                   FLTERS'
                           CONDENSATE
                           REMOVALE
                r
                  r
]__/Ot5frU_ SAMPLE
                                                                                SAMPLE
                                                                                PORT
                                                      r
                                                                            -.STORE ROOM
                                    PUMP
                         AIR COOLED
                         COIL
                                                                  PORT
-H
                                               CALIBRATION
                                               GAS
           VENT
                 H
-MX!-
VENT
        HEATED
        SAMPLE LINE
                 HEATED
                 TUHC
                 MONITOR
                               PERMA PURE
                               DRYER
                                              CO       CO2      NO.       
-------
                           TABLE 3-2.  ANALYSIS PROCEDURES
Sample
Test feed
material


Parameter
Proximate analysis
(moisture, volatile matter,
fixed carbon, ash)
Elemental analysis
C, H, 0, N, S
a
Heating value
Analysis method
ASTM D-5142
ASTM D-3176
ASTME-442
ASTM D-3286
Frequency
1 composite for
each test material
1 composite for
each test material
1 composite for
               Test semivolatile POHCs

               Test volatile organic
               contaminants
Soxhlet extraction by Method 3540A, GC/MS
analysis by Method 8270A*
Purge and trap GC/FID of methanol extract by
Method 8015A*
each test material
I/test

I/test

Test feed TCLP
leachate
Feed packaging
material





Kiln ash



Kiln ash TCLP
leachate
PCDDs/PCDFs
Trace metalsb
TCLP extraction
Trace metals"
Proximate analysis
(moisture, volatile matter,
fixed carbon, ash)
Elemental analysis
C, H, 0, N, S
Cl
Heating value
Test semivolatile POHCs
Test volatile organic
contaminants
PCDDs/PCDFs
Trace metalsb
Test semivolatile POHCs
Test volatile organic
contaminants
PCDDs/PCDFs
Trace metalsb
TCLP extraction
Trace metals"
GC/MS by Method 8290"
Digestion by the multiple metals filter method0,
ICAP analysis by Method 6010A"
Method 1311*
Digestion by Method 3010A, ICAP analysis by
Method 6010A*
ASTM D-S142
ASTM D-3176
ASTME-442
ASTM D-3286
Soxhlet extraction by Method 3540A, GC/MS
analysis by Method 8270A*
Purge and trap GC/FID of methanol extract by
Method 8015A*
GC/MS by Method 8290*
Digestion by the multiple metals filter method6,
ICAP analysis by Method 6010A*
Soxhlet extraction by Method 3540A, GC/MS
analysis by Method 8270A*
Purge and trap GC/FID of methanol extract by
Method 8015A*
GC/MS by Method 8290*
Digestion by the multiple metals filter method0,
ICAP analysis by Method 6010A*
Method 1311"
Digestion by Method 3010A, ICAP analysis by
Method 6010A*
1 composite for
each test material
I/fluff test,
1 composite soil
I/fluff test,
1 composite soil
I/fluff test,
1 composite soil
1 composite
1 composite
1 composite
1 composite
1 composite
1 composite
1 composite
I/test
I/test
I/test
I/test
I/test
I/test
'Reference 3, SW-846.
bAs, Sb, Ba, Cd, Cr, Cu, Pb, Ni, Ag, and Zn.
Reference 2, 40 CFR 266, App. IX.
                                                (continued)
                                             3-8

-------
                                    TABLE 3-2. (continued)
     Sample	Parameter	Analysis method	Frequency
 Pre-test       Test semivolatile     Extraction by Method 3520A, GC/MS analysis by Method      I/test
 scrubber liquor POHCs            8270A*
               Test volatile organic  Purge and trap by Method 5030A, GC/FID by Method 8015A*  I/test
               contaminants
               Trace metalsb       Digestion by Method 3010A, ICAP analysis by Method 6010A*  I/test
               PCDDs/PCDFs      GC/MS by Method 8290*                                  1 sample
                                                                                         before the
	                 first test
 Post-test       Test semivolatile    Extraction by Method 3520A, GC/MS analysis by             I/test
 scrubber liquor POHCs            Method 8270A*
               Test volatile organic Purge and trap by Method 5030A, GC/FID by Method 8015A* I/test
               contaminants
               PCDDs/PCDFs     GC/MS by Method 8290*                                 I/test
      -        Trace metalsb       Digestion by Method 3010A, ICAP analysis by Method 6010A* I/test
	TCLP extraction    Method 1311*	         I/test
 Scrubber liquor Trace metalsb       Digestion by Method 3010A, ICAP analysis by Method 6010A* I/test
 TCLPleachate
 Baghouse ash   Test semivolatile    Soxhlet extraction by Method 3540A, GC/MS analysis by      I/test
               POHCs            Method 8270A*
               Test volatile organic Purge and trap GC/FID of methanol extract by              I/test
               contaminants       Method 8015A*
               PCDDs/PCDFs     GC/MS by Method 8290*                                 I/test
               Trace metalsb       Digestion by the multiple metals filter method0, ICAP analysis  I/test
                                 by Method 6010A"
               TCLP extraction    Method 1311*   	      I/test
Baghouse ash
TCLP leachate
Baghouse exit
flue gas





Stack gas

Trace metalsb
Semivolatile TCL
constituents
Volatile TCL
constituents
PCDDs/PCDFs
Trace metalsb
Paniculate
HC1
Paniculate
HC1
Digestion by Method 3010A, ICAP analysis by Method 6010A*
Soxhlet extraction of Method 0010A samples by
Method 3540A, GC/MS analysis by Method 8270A*
Purge and trap of Method 0030 samples by Method 5040,
GC/MS analysis by Method 8240A
GC/MS of Method 23 samples by Method 23
Digestion of multiple metals train samples by multiple metals
procedure6, ICAP analysis by Method 6010A*
Method 5"1
ICAP analysis of combined impinger solution by Method 9057
Method 3d
1C analysis of combined impinger solution by Method 9057
I/test
I/test
3 trap
pairs/test
I/test
I/test
I/test
I/test
I/test
J/test
"Reference 3, SW-846.
bAs, Sb, Ba, Cd, Cr, Cu, Pb, Ni, Ag, and Zn.
Reference 2, 40 CFR 266, App. IX.
Reference 4, 40 CFR 60, App. A.
                                               3-9

-------
            TABLE 3-3.  TEST PROGRAM SAMPLE ANALYSIS SUMMARY


Sample matrix
Fluff Waste Feed
Test sample
Split sample
Matrix spike
Spike duplicate
Soil Feed
Test sample
Split sample
Matrix spike
Spike duplicate


SVOCs

4
16
1
1

2
8
1
1
Number of analyses

VOCs PCDDs/PCDFs

4 1
1
1
1

2 1
1
1
1

Trace
metals Chloride

4
16
1
1

1
4
1
1
 Packaging Container Material

  Cardboard + packaging tape +
  HDPE bottle + bottle cap +
  polyethylene liner + plastic tie

 Kiln Ash

  Test sample*
  Split sample
  Matrix spike
  Spike duplicate

 Pre-test Scrubber Liquor

  Test sample

 Post-test Scrubber Liquor

  Test sample
  Split sample
  Matrix spike
  Spike duplicate

 Baghouse Ash

  Test sample
  Split sample
  Matrix spike
  Spike duplicate
7
1
1
1
7
1
1
1
              6
              1
              1
              1
7
1
1
1
7
1
1
1
               6
               1
7
1
            6
           22
            1
            1
7
1
1
1
           7
           1
           1
           1
*No kiln ash resulted from the blank burn test.
                                                                                  (continued)
                                           3-10

-------
                                      TABLE 3-3.  (continued)
               Sample matrix
                                          Trace
SVOCs	VOCs       PCDDs/PCDFs  metals  Chloride
  TCLP Leachate
   Fluff feed
   Soil feed
   Kiln ash
   Scrubber liquor
   Baghouse ash
   Method blank
   Split sample
   Matrix spike
   Spike duplicate
  Method 0010 Train
   Test sample
   Method blank
   Matrix spike
   Spike duplicate
 Method 0030
   Test sample trap paii*
   Field blank
   Trip blank
   Matrix spike
 Method 23 Train
  Test sample
  Method blank
 Multiple Metals Train
                21
                7
                1
                9
                                            4
                                            1
                                            6
                                            7
                                            7
                                            2
                                            2
                                            2
                                            2
Front half
Test sample
Method blank
Matrix spike
Spike duplicate
Back half
Test sample
Method blank
Matrix spike
Spike duplicate
Method 5 Train Impingers
Test sample
Matrix spike
Spike duplicate

7
/
1


i
i
1
1















4 A
14
1
1
                                             81            S?             35         140
"Tour trap pairs sampled per test, three trap pairs analyzed; fourth trap pair for breakage contingency.
                                               3-11

-------
TABLE 3-4. SAMPLE ANALYSIS ALIQUOT SCHEDULE FOR EACH TEST
Total quantity
of each sample Analyte/
Sample collected
Fluff waste feed 1 kg




Soil feed 1 kg



Packaging 50 g
container
material


Kiln ash 1 kg

'


Pre-test scrubber 4 L
liquor





Post-test scrubber 8 L
liquor





procedure
SVOCs
VOCs
PCDDs/PCDFs
Trace metals
TCLP extraction
SVOCs
VOCs
Trace metals
TCLP extraction
SVOCs
VOCs
PCDDs/PCDFs
Trace metals
SVOCs
VOCs
PCDDs/PCDFs
Trace metals
TCLP extraction
SVOCs

VOCs


PCDDs/PCDFs
Trace metals
SVOCs
VOCs


PCDDs/PCDFs
Trace metals
TCLP extraction
Aliquot size
10 g
4g
10 g
lg
100 g
10 g

-------
                                   TABLE 3-4.  (continued)
          Sample
 Total quantity
 of each sample
   collected
   Analyte/
   procedure
Aliquot
 size
                                                                   Number of aliquots needed
  Baghouse ash
As collected
SVOCs         10 g
VOCs          4 g
PCDDs/PCDFs   10 g
Trace metals     1 g
                                                              1 each test + 1 split + 1 MS + 1 MSD
                                                              1 each test + 1 split + 1 MS + 1 MSD
                                                              1 each test + 1 split
                                                              1 each test + 1 split + 1 MS + 1 MSD
                                        TCLP extraction  100 g    1 each test
TCLP leachate
Method 0010 train
Method 0030 train
Method 23 train
2L
As collected
As collected
As collected
Trace metals
SVOCs
VOCs
PCDDs/PCDFs
100 mL
Total
Total
Total
25 test samples + 2 method blank +
2 split + 2 MS + 2 MSD
1 each test + 1 method blank + 1 MS
+ 1MSD
4* each test + 7 field blanks + 1 trip
blank + 9 MS
1 each test + 1 method blank
 Multiple metals train
   Front half
   Back half
As collected    Trace metals    Total    1 each test + 1 method blank + 1 MS
                                    + 1 MSD
As collected    Trace metals    Total    1 each test + 1 method blank + 1 MS
                                    + 1MSD
 Method S train impinger     As collected    Cl             100 mL  2 each test + 1 MS + 1 MSD
 "Three of four analyzed; fourth represents breakage contingency.
        Table 3-5 summarizes the containers used for sample aliquot storage until analysis,
preservation methods used, and analysis hold times required.  Only new containers were used
for sample storage. They were purchased, precleaned to meet EPA standards, from a laboratory
supply vendor and are certified by the vendor as appropriate for use in storing samples for the
respective analyte class. No containers or preservation is shown in Table 3-5 for Method 0010
train samples. The procedure at the IRF is to transfer samples recovered from Method 0010
trains directly into the extraction apparatus  immediately after a  test and begin overnight
extractions the day of each test.
        Filters and other sampling train components for Method 0010, Method 23, the multiple
metals method train, and the Method 5 trains were cleaned  according to the procedures
                                            3-13

-------
 TABLE 3-5.  SAMPLE CONTAINERS, PRESERVATION METHODS, AND HOLD TIMES
Sample
Solid samples (fluff
waste, soil, packaging
container material, kiln
ash, baghouse ash)


Aqueous liquid samples
(scrubber liquor, TCLP
leachates)


Method 0010 train
Method 0030 traps
Method 23 train filter
Filter
Rinses and impinger
solutions
Analyte
SVOCs
VOCs
PCDDs/PCDFs
Trace metals
SVOCs
VOCs
PCDDs/PCDFs
Trace metals
SVOCs
VOCs
PCDDs/PCDFs

Sample
container*
G.T
G, T, zero
headspace
G, T
GorP
G,T
G, T VGA vial
G, T .
GorP
None
Sealed glass
traps
Glass petri dish
G, T
Sample
preservation
method
Cool to 4C
Cool to 4C
Cool to 4C
None
Cool to 4C
Cool to 4C
Cool to 4C
HNO3 to pH <2
None
Cool to 4C
Cool to 4C
Cool to 4C
Analysis hold time
Extraction: 14 days
Analysis'": 40 days
14 days
Extraction: 30 days
Analysis": 45 days
6 months
Extraction: 7 days
Analysis": 40 days
14 days
Extraction: 30 days
Analysis": 45 days
6 months
40 days
42 days
Extraction: 30 days
Analysis": 45 days

Multiple metals train

  Filter

  Rinses and impinger
  solutions
Trace metals
                 Glass petri dish   None

                 G or P           None
                                  6 months
Method 5 train
impinger solution
Chloride
GorP
None
28 days
*G = glass, P = polyethylene, T = Teflon-lined cap.
"After extraction.
                                          3-14

-------
documented in the respective methods. Sorbent resin for use in Method 0010 and Method 0030



trains was cleaned prior  to  use according  to  the procedures  in  the  respective methods.



Method 23 sorbent resin cartridges were cleaned and charged with clean sorbent, spiked with




method surrogates, by the analytical laboratory that performed the PCDD/PCDF analyses.




        A single container was used to store each sample collected for each analysis. Aliquots




were taken from this container as needed. MS and MSD samples were prepared from aliquots




from this container as well.  After preparation, however, MS and MSD samples were stored in



separate containers until analyzed.




        Unused sample collected  was stored in appropriate containers with appropriate




preservation until the expiration of method hold times. After method hold time expired, unused



samples were archived.




32     ANALYSIS METHODS




        Table 3-2 summarizes the analytes determined in each test program sample, and the




analysis procedures used.  As indicated in the table, the fluff feed samples for each fluff test, a




composite soil feed sample, the packaging container material, and the kiln ash, pre-test and




post-test scrubber liquor,  and baghouse ash samples for each  test  analyzed  for  the site



contaminant trace metals. Trace metal analyses were by ICAP spectroscopy in accordance with




Method 6010A.  Solid samples (feed material,  packaging container material, kiln ash, and



baghouse  ash) were digested  using the HNO3/HF procedure specified for use  with filter




particulate in the EPA multiple metals  method (Reference 2). Liquid samples (pre-test and



post-test scrubber liquor) were digested  using a minor variation of Method 3010A. This minor



variation consists of using concentrated HNO3 instead of 1:1 HC1 in the last step of Section 7.2



of Method 3010A. The 10 site contaminant metals measured in the test samples were antimony,
                                         3-15

-------
 arsenic, barium, cadmium, chromium, copper, lead, nickel, silver, and zinc. Omission of the HCI



 in the last Method 3010A step allows analysis for silver.




        Each fluff test's fluff feed, a composite soil feed sample,  and each test's kfln ash,




 baghouse ash, and post-test scrubber liquor samples were subjected to TCLP  extraction by




 Method 1311. The TCLP leachates were analyzed for the  10 site contaminant trace metals by



 Method 6010A.  The minor variation of Method 3010A, noted above, was used for leachate



 digestion.




        In addition, each fluff test's fluff feed, each soil test's soil feed, the packaging container




 material, and the kiln ash, baghouse ash, and pre-test and post-test scrubber liquor samples for




 each test were analyzed for the test semivolatile POHCs (BEHP, DNOP, and naphthalene).




 Semivolatile POHC  analyses were by gas chromatography/mass spectrometry  (GC/MS) in




 accordance with Method 8270A.  Solid samples (feed, packaging container material, baghouse




 ash, and kiln ash) were Soxhlet-extracted by Method 3540A.  Pre-test and post-test scrubber



 liquor samples were extracted via continuous liquid-liquid extraction by Method 3520A.




        One composite fluff feed sample, a composite soil feed sample, the packaging container




 material, the pre-test scrubber liquor sample taken before the first test program test, and the kiln



 ash, post-test scrubber liquor, and baghouse ash samples for each test were also analyzed for



 PCDDs/PCDFs by the high-resolution GC/MS method,  Method 8290.  The single composite




 fluff feed sample was prepared by combining aliquots of the four test feed samples collected.




       Each test's fluff feed or soil feed, the packaging container material, and each test's kiln




ash, baghouse ash, and pre-test and post-test scrubber liquor samples were also analyzed for the




test volatile organic contaminants by GC/FTD in accordance with Method 8015A.  Sample



introduction was by Method 5030A.
                                        3-16

-------
        The Method 0010 samples for each test were analyzed for the semivolatile organic TCL

constituents listed in Table 3-6. The target analytes were the semivolatile test POHCs, BEHP,

DNOP, and naphthalene. However, the other TCL constituents were also quantitated. Sample

preparation was  performed  according to  Method 0010, with  final  GC/MS analysis by

Method 8270A. The Method 23 samples for each test were analyzed for PCDDs/PCDFs by the

method.
            TABLE 3-6. SEMIVOLATILE ORGANIC TCL CONSTITUENTS
             Acenaphthene
             Acenaphthylene
             Anthracene
             Benz(a)anthracene
             Benzo(b)fluoranthene
             Benzo(k)fluoranthene
             Benzo(a)pyrene
             Benzo(ghi)perylene
             Benzyl butyl phthalate
             Bis(2-chloroethyl) ether
             Bis(2-chloroethoxy) methane
             Bis(2-chloroisopropyl) ether
             Bis(2-ethylhexyl) phthalate
             4-Bromophenyl phenyl ether
             2-Chloronaphthalene
             4-Chlorophenyl phenyl ether
             Chrysene
             Dibenzo(a,h)anthracene
             Di-n-butyl phthalate
             1,2-Dichlorobenzene
             1,3-Dichlorobenzene
             1,4-Dichlorobenzene
             3,3'-Dichlorobenzidine
             Diethyl phthalate
             Dimethyl phthalate
             2,4-Dinitrotoluene
 2,6-Dinitrotoluene
 Di-n-ocryl phthalate
 Fluoranthene
 Fluorene
 Hexachlorobenzene
 Hexachlorobutadiene
 Hexachloroethane
 Indeno(l,2,3-cd)pyrene
 Isophorone
 Naphthalene
 Nitrobenzene
 N-Nitrosodi-n-propylamine
 Phenanthrene
 Pyrene
 1,2,4-Trichlorobenzene
 4-Chloro-3-methylphenol
 2-Chlorophenol
 2,4-Dichlorophenol
 2,4-Dimethylphenol
 2,4-Dinitrophenol
 2-Methyl-4,6-dinitrophenol
 2-Nitrophenol
 4-Nitrophenol
 Pentachlorophenol
Phenol
2,4,6-Trichlprophenol
                                       3-17

-------
        As noted in Section 3.1, four Method 0030 trap pair samples were collected for each

 test.  Three trap pair samples for each test were analyzed for the test volatile organic TCL

 constituents listed in Table 3-7 by purge and trap GC/MS via Methods 5040 and 8240A. The

 fourth trap pair was collected for breakage contingency, so that the probability that three trap

 pair analyses could be done for each test was increased, given the inevitability of trap breakage.

 The target analytes were  the volatile site material organic contaminants, tetrachloroethene,

 trichloroethene, and 1,1,2-trichloroethane.  However, the other TCL constituents were .also

 quantitated.

        Multiple metals train samples were analyzed for the 10 site contaminant trace metals.

 Sample preparation was performed according to the method, with  final ICAP analysis by

 Method 6010A. Flue gas HC1 levels were determined by analyzing the combined Method 5 train

 impinger solutions for chloride via 1C according to Method 9057.

        One composite fluff feed sample, the composite soil feed sample, and the packaging

container material sample were, also subjected to proximate, elemental, and heating value

analyses by the ASTM procedures noted in Table 3-2.
               TABLE 3-7.  VOLATILE ORGANIC TCL CONSTITUENTS

              Acetone                       trans-l,2-Dichlorothene
              Benzene                       1,2-Dichloropropane
              Bromodichloromethane         cis-l,3-Dichloropropene
              Carbon disulfide                trans-l,3-Dichloropropene
              Carbon tetrachloride            Methylene chloride
              Chlorobenzene                 Tetrachloroethene
              Chlorodibromomethane         Toluene
              Chloroform                    1,1,1-Trichloroethane
              1,1-Dichloroethane              1,1,2-Trichloroethane
              1,2-Dichloroethane              Trichloroethene
              1,1-Dichloroethene              Trichlorofluoromethane
                                        3-18

-------
       Proximate and  elemental analyses were performed by Galbraith  Laboratories in



Knoxville, Tennessee. SVOC (Method 8270A), VOC (Method 8015A), HC1 (Method 9057), and




TCLP (Method 1311) procedures were performed in the IRF analytical laboratories. Trace




metal analyses (Method 6010A) were performed by the American Interplex Laboratories in



Little Rock, Arkansas. Method 0030 sample and PCDD/PCDF (Methods 8290 and 23) analyses



were performed by Triangle Laboratories in Research Triangle Park, North Carolina.
                                      3-19

-------
                                       SECTION 4



                                    TEST RESULTS








        The results of the test program are discussed in this section.  Test results are grouped



 by analyte class. Thus, Section 4.1 presents the fluff waste and soil feed proximate and elemental




 analysis results. Section 4.2 discusses the SVOC measurements. Section 4.3 discusses the VOC




 measurements. Section 4.4 discusses the PCDD/PCDF measurements. Each of the sections, 4.2,



 4.3, and 4.4, includes discussion on the effectiveness of incineration in removing the contaminants




 of interest in the fluff waste and contaminated soil. Where appropriate, contaminant destruction




 removal efficiencies (DREs) are presented and discussed. The concentrations of contaminants



 of interest in the RKS discharge streams, kiln ash, baghouse ash, and scrubber liquor, are also




 discussed. Section 4.5 discusses the trace metals measurements. Section 4.6 discusses the results




 of the flue gas paniculate and HC1 measurements,  as  well as the flue gas paniculate size



 distribution results. For the reader who is interested in studying the analytical results in more



 detail, the analytical laboratory reports are given in Appendix C of this report.




4.1     PROXIMATE AND ULTIMATE ANALYSIS RESULTS



        The proximate and elemental analysis results for the fluff waste, soil, and packaging



container material samples analyzed are presented in Table 4-1. As shown in the table, the fluff



waste was distinctly organic in nature as evidenced  by the high level of volatile matter at



39.1 percent and its higher heating value of 12.4 MJ/kg (5,330 Btu/lb). The fluff was also quite




moist, with 46.8 percent moisture.  The high moisture content was consistent with the fact that






                                          4-1

-------
         TABLE 4-1. PROXIMATE AND ELEMENTAL ANALYSIS RESULTS FOR
                    COMPOSITE FLUFF AND SOIL FEED SAMPLES

Proximate Analysis (as received)
Moisture, %
Ash, %
Fixed carbon, %
Volatile matter, %
Higher heating value, MJ/kg
(Btu/lb)
Elemental Analysis, % (dry
basis)
C
H
O
N
S
Cl
Ash
Fluff waste

46.8
5.2
8.9
39.1
12.4
(5,330)

44.2
6.2
7.4
<0.5
0.2
32.2
9.8
Contaminated
soil

23.0
64.4
2.6
10.0
0.58
(250)

7.3
1.1
5.8
<0.5
<0.04
2.3
83.6
Packaging
container
material

4.8
1.4
13.3
80.5
__a

46.4
7.0
45.0
<0.5
0.2
<0.5
1.4
    .  a - Not measured.


the fluff had been accumulated and stored in large piles outdoors, thereby being exposed to

precipitation. The fluff waste contained 32.2 percent chlorine (dry basis), a level suggesting the

presence of chlorinated plastics (e.g., polyvinyl chloride) and possibly other chloro-organic

solvents, both of which were present or used at the site.

        The character of the contaminated soil was distinctly different from the fluff, although

a small amount of fluff-like material was found to have commingled into the soiL  The heating

value of the soil was low, as expected at 0.58 MJ/kg (250 Btu/lb).  Its moisture content, at


                                        4-2

-------
23 percent, and ash content, at 64.4 percent are typical of soils.  The soil chlorine content, at


2.3 percent (dry), could have been due to the presence of a small amount of fluff or other


chlorine containing organic contaminants.


       Table 4-2 summarizes the cumulative weights of the fluff waste and contaminated soil
                                                    

fed for each test and the total amount of corresponding kiln ash collected. As indicated in (the


table, for Tests 1 and 2 (average kiln exit gas temperature at 875 to 883C [1,608 and 1,622F],


respectively), the collected ash weights were equal to about 5 percent of the amount of fluff fed.


The collected ash amounts accounted for 98 to 101 percent of the theoretical ash amount that


could be expected. For Tests 5 and 6, during which the average kiln exit temperatures were at


762 and 767C (1,403 and 1,412F), respectively, the collected ash amounts were equal to 5.7


and 6.7 percent of the amount of fluff fed.  These amounts of collected ash were greater than


the theoretical  ash  quantity in  the fluff fed.  The amounts  of. ash collected were 128 and


109 percent of the theoretical ash amount.  The greater-than-100-percent ash collected for these
    TABLE 4-2. WEIGHTS OF TEST MATERIAL FED AND KILN ASH COLLECTED
Total fed
Test
Fluff Waste Tests
1
2
5
6
Soil Feed Tests
3
4
Date

11/9/93
11/16/93
11/18/93
11/23/93

12/1/93
12/2/93
kg

303
304
307
305

288
290
Ob)

(666)
(669)
(675)
(671)

(634)
(638)

Kiln
Weight
kg

15
16
20
17

150
145
Ob)

(34)
(35)
(45)
(38)

(329)
(320)
ash collected
Fraction Fraction of
of feed expected ash

5.1
5.2
6.7
5.7

52
50

98
101
128
109

81
78
                                         4-3

-------
 tests would be consistent with incomplete fluff oxidation for these lower kiln exit gas temperature



 tests.




        For the soil tests (Tests 3 and 4), the kiln ash weights were about 50 percent of the fed




 soil weights, which corresponds to about 80 percent of the theoretical ash amounts. Evidently,




 about 20 percent of the theoretical ash in the soil tests was entrained in the kiln exit combustion



 gas and carried out of the kiln.




 4.2     SVOC ANALYSIS RESULTS




        Table 4-3 summarizes the measured concentrations of the target SVOC analytes in test



 program samples collected.  For the entries in the table noted as less than values, the value




 represents the  MDL of the analysis procedure.   Laboratory analysis  reports are given in




 Appendix C-3.  For  each test  performed, Table 4-3 also indicates  the average kiln exit gas




 temperature measured over the flue gas sampling period corresponding to each test.




        The data in Table 4-3 show that the BEHP concentrations in the actual fluff waste fed



 for each fluff waste test, at 48,300 to 53,300 mg/kg, were about half the level measured in the




 pretest characterization sample as reported in Table 2-3, as well as being below the lowest




 concentration reported in the ROD.  Similarly, the DNOP levels in actual test fluff waste, at




 1,850 to 2,870 mg/kg, were also substantially lower than the 17,800 mg/kg level measured in the



 pretest characterization sample, and were at the low end of the range of concentrations reported




 in the ROD. Nevertheless, contamination levels of these two  constituents in the test fluff waste




were still significant. The 20,200 mg/kg naphthalene concentration noted in incinerator feed




 samples in the table represents  the quantity of naphthalene spike added to feed containers. No



fluff waste or soil sample contained naphthalene at an MDL  of 25 mg/kg before spiking.




        The data in Table 4-3 show that the contaminated  soil tested contained 9,440 to




9,810 mg/kg of BEHP and 550 to 580 mg/kg DNOP. These levels are substantially greater than






                                         4-4

-------
    TABLE 4-3. SEMIVOLATILE ORGANIC CONTAMINANT ANALYSIS RESULTS
Concentration
Sample
Test 0 (10/27/93), kiln temperature:
871C (1,599F)
Packaging container material, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /ig/dscm
Fluff Waste Tests
Test 1 (11/9/93), kiln temperature:
883 C (1,622F)
Fluff feed, mg/kg
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, jig/dscm
Test 2 (11/16/93), kiln temperature:
876C (1,608F)
Fluff feed, mg/kg
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /zg/dscm
Test 5 (11/18/93), kiln temperature:
762C (1,403 F)
Fluff feed, mg/kg
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /*g/dscm
Test 6 (11/23/93), kiln temperature:
767C (1,412F)
Fluff feed, mg/kg
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /zg/dscm
BEHP


<1.3
< 0.013
6.6
8.4



48,800
<1.3
< 0.013
14.3
7.0


53,300
<1.3
<0.013
4.5
9.9


48,300
<1.3
< 0.013
21.1
9.8


49,000
<13
< 0.013
18.7
6.2
DNOP


<0.4
< 0.004
4.1
<0.9



1,850
<0.4
< 0.004
9.9
<1.2


2,610
<0.4
< 0.004
2.2
<1.3


2,870
<0.4
< 0.004
13.4
<1.1


2,810
<0.4
<0.004
12.1
<1.2
Naphthalene


<0.3
< 0.003
<0.3
<0.8



20,200a
<0.3
< 0.003
<0.3
<0.9


20,200a
<0.3
< 0.003
<0.3
<1.1


20,200a
<0.2
< 0.003
<0.3
<0.9


20,200a
<0.3
<0.003
<0.3
<1.0
aSpiked concentration.
(continued)
                                  4-5

-------
                                TABLE 4-3. (continued)
Concentration
Sample
Soil Feed Tests
Test 3 (12/1/93), kiln temperature:
876C (1,609F)
Soil feed, mg/kg
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /zg/dscm
Test 4 (12/2/93), kiln temperature:
874C (1,606F)
Soil feed, mg/kg
Kiln ash, mg/kg ^
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /tg/dscm
BEHP


9,810
< 0.013
23.5
7.8

9,440
< 0.013
14.2
7.0
DNOP


580
<0.4
< 0.004
17.0

547
<0.4
< 0.004
9.7
Naphthalene


20,200*
<03
< 0.003
<03

20,200a
<0.003
<03
Spiked concentration.
those measured in the pretest soil characterization samples analyzed, although they fall within



the concentration ranges reported in the ROD for these contaminants. Again, the naphthalene




concentrations in test soil feed samples correspond to spiked amounts.




        The data in Table 4-3 also show that the native and spiked SVOC contaminants were




essentially completely removed from the fluff waste by incineration at both kiln temperatures



tested, as evidenced by their absence in the kiln ash discharge for all fluff waste tests at method




detection limits (MDLs) of 0.3 to 1.3 mg/kg.  Similarly these contaminants were removed from




the contaminated soil for both soil tests at the single kiln temperature tested for this matrix. No




kiln ash concentration data are given for the blank burn test, Test 0, in Table 4-3 because no kiln



ash was discharged for this test.
                                          4-6

-------
         None of the three SVOC contaminants was found in the post-test scrubber liquor for



 any test at MDLs of 0.003 to 0.013 mg/L.




         Naphthalene was absent from the baghouse ash for all tests at an MDL of 0.3 mg/kg.



 However,  low levels of both BEHP (6.6 to 23.5 mg/kg) and DNOP (2.2 to 17.0 mg/kg) were



 found in the baghouse ash for all tests, including the blank burn. No explanation as to why these



 site contaminants  are found at these levels in the baghouse ash is offered, other than the  fact




 that phthalates are commonly encountered laboratory contaminants. Neither naphthalene nor



 DNOP was present in  the baghouse exit flue gas for any test, at MDLs of about 1 /tg/dscm.




 BEHP was found in the baghouse exit flue gas for all tests, including the blank burn, at levels



 ranging from 6.2 to 9.8 /ig/dscm.




        Feed  SVOC contaminant  concentration, feedrate, baghouse  exit  flue gas  SVOC



 contaminant concentration, and flue gas flowrate  data can be combined to calculate SVOC




 contaminants DREs for each of the tests. Calculated DREs are summarized in Table 4-4.  As




 shown in the table, the measured levels of BEHP in the baghouse exit flue gas corresponded to




 BEHP DREs ranging from 99.99932 to 99.99962 percent for the fluff waste tests and 99.9974 to



 99.9980 percent for the soil feed tests. Kiln temperature had no apparent affect on BEHP DRE




 from fluff waste.  Neither the spiked naphthalene nor the native DNOP contaminants were




 detected in the baghouse exit flue gas for any test.  The DREs corresponding to baghouse exit



 flue gas MDLs, and noted with the ">" sign in Table 4-4, were 99.99982 to 99.99987 percent for



 naphthalene for all tests, 99.9982 to 99.9987 percent for DNOP  in the fluff waste tests, and



 99.9933 to  99.9940 percent for DNOP in the soil feed tests. All DREs demonstrated were




greater than the 99.99 percent level required by  the current hazardous waste incinerator



performance standard.
                                         4-7

-------
      TABLE 4-4. SVOC POHC DREs
Parameter
                                        BEHP
                                                                                 DNOP      Naphthalene
  Fluff Waste Tests
   Test 1 (11/9/93), kiln temperature: 883C (1,622F)
     Feed concentration, mg/kg
     Feedrate, kg/hr
     Baghouse exit flue gas:
      Concentration, /tg/dscm
      Emission rate, mg/hr
     DRE, %
   Test 2 (11/16/93), kfln temperature:  876C (1,608F)
     Feed concentration, mg/kg
     Feedrate, kg/hr
     Baghouse exit flue gas:
      Concentration, /tg/dscm
      Emission rate, mg/hr
    DRE, %

   Test 5 (11/18/93), kiln temperature:  762C (1,403F)
    Feed concentration, mg/kg
    Feedrate, kg/hr
    Baghouse exit flue gas:
     Concentration, /tg/dscm
     Emission rate, mg/hr
    DRE, %

  Test 6 (11/23/93), kiln temperature: 767C (1,412'F)
    Feed concentration, mg/kg
    Feedrate, kg/hr
    Baghouse exit flue gas
     Concentration, /zg/dscm
     Emission rate, mg/hr
    DRE, %
Soil Feed Tests
>  Test 3 (12/1/93), kiln temperature:  876eC (l,6d9F)
   Feed concentration, mg/kg
   Feedrate, kg/hr
   Baghouse exit flue gas:
     Concentration, pg/dscm
     Emission rate, mg/hr
   DRE, %
  Test 4 (12/2/93), Icfln temperature:  874C (1,606F)
   Feed concentration, mg/kg
   Feedrate, kg/hr
   Baghouse exit flue gas:
     Concentration, /jg/dscm
     Emission rate, mg/hr
   DRE, %
  48,800
  2.93

  7.0
  11.9
  99.99959
                                      53300
                                      3.15

                                      9.9
                                      19.4
1,850
0.11
                                                               20^00
                                     48300
                                     2.94

                                     9.8
                                     20.1
                                     99.99932
                                     49,000
                                     2.98

                                     6.2
                                     113
                                     99.99962
                                     9,810
                                     0.58

                                     7.8
                                     15.0
                                     99.9974
9,440
0.56

7.0
113
99.9980
                                                  <2.0
                                                  >99.9982
             2,610
             0.15

             <13
             <2.5
             20,200
             1.19
                                      99.99939    > 99.9984
             2,870
             0.18
             <23
             > 99.9987
            2,810
            0.17
             > 9959982


             20,200
              9939985


            20,200
            <2.2
            > 99.9987
            580
            0.034

             99.9933
                                                547
                                                0.032
                                                              > 99^9985
            20,200
            1.19
                                                              >99J9984
            20^00
            1.19
                                                >99.9940
                                                                                          > 99.99986
                     4-8

-------
        As noted in Section 3.2, the flue gas Method 0010 train samples were analyzed for the



full list of SVOC TCL compounds given in Table 3-6.  None were found at compound-specific



MDLs ranging from 0.4 to 8 /zg/dscm, with the exception of dimethylphthalate, which was found



in the flue gas for all tests (including the blank test, Test 0) at concentrations ranging from 1.1 to




2.1 /zg/dscm.



        Also recall from the discussion in Section 3 that the five replicates of each fluff waste



and soil feed samples collected were to be analyzed for the SVOC POHCs in the test program.




This was done for the soil feed samples collected.  However, only BEHP was quantitated in all




fluff waste replicate samples. In order to accurately quantitate the DNOP levels measured in




fluff waste  samples, the analysis of undiluted sample extracts was required.  However,,  the




concentration of BEHP in undiluted extracts was so high that the instrument cleanup times




required after an undiluted extract analysis were quite lengthy. For this reason, it was decided




to quantitate DNOP and naphthalene in a composite undiluted extract, formed by combining




aliquots of each replicate fluff waste  SVOC extract, to give a test composite analysis result for




these two analytes. Each replicate sample extract was then diluted and analyzed for BEHP.  The



DNOP concentrations for fluff waste samples given in Table 4-3 represent these test-specific



composite extract analysis results. Naphthalene was not  detected in any fluff waste composite




extract sample at an MDL of 130 mg/kg.



        Table 4-5 summarizes the BEHP replicate sample  analysis results for the fluff waste




samples. The average concentration noted for each test is the fluff waste concentration reported




in Table 4-3. The data in the table show that the percent relative standard deviation (% RSD)



of the BEHP concentration measured in the five replicate fluff waste samples analyzed for each



test ranged from 5.8 to 24.6. All are well within the precision data quality objective (DQO) for




this measurement of 50% RSD. The four test average fluff waste BEHP concentration, from
                                         4-9

-------
TABLE 4-5. BEHP CONCENTRATIONS IN REPLICATE FLUFF WASTE SAMPLES
BEHP concentration, mg/kg
Test
1 (11/9/93)
2 (11/16/93)
5 (11/18/93)
6 (11/23/93)
4 test total (20 samples)
f"
o
Sample
27,800
55,400
51,300
54,000



Replicate 1
52,800
51,200
53,300
43,300



Replicate 2
57,200
49,000
43,200
51,900



Replicate 3
50,700
56,100
47,300
54,000



Replicate 4
55,600
54,900
46,200
42,000



Average
concentration,
mg/kg
48,800
53,300
48,300
49,000
49,900


%RSD
24.6
5.8
8.4
12.1
13.8



-------
the analysis of 20 separate fluff samples, was 49,900 mg/kg, with the 20-sample % RSD at

13.8 percent.

       Table 4-6 summarizes the results of the replicate soil feed SVOC analyses. Again, the

average concentrations of BEHP and DNOP from the five samples analyzed for each test are

those given in Table 4-3. As shown in Table 4-6, naphthalene was not detected in any soil feed

sample at an MDL of 25 mg/kg. The data in Table 4-6 show that the % RSDs for the individual

test replicate soil feed analyses were 32.8 and 27.9  percent for BEHP and 48.7 and 30.2 percent

for DNOP. The two test average SVOC contaminant concentrations representing 10 separate
        TABLE 4-6. SVOC CONTAMINANT CONCENTRATIONS IN REPLICATE
                   SOIL SAMPLES
Concentration, mg/kg
Soil sample
Test 3
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
Average
%RSD
Test 4
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
Average
% RSD
2 test total (10 samples)
Average
%RSD
BEHP

10,700
14,900
6,450
8,530
8,470
9,810
32.8

11,000
8,270 .
9,450
5,780
12,700
9,440
27.9

9,630
28.9
DNOP

508
614
296
440
1,040
580
48.7

728
598
417
335
655
547
30.2

563
38.8
Naphthalene

<25
<25
<25
<25
<25
<25

<25
<25
<25
<25
<25
<25

<25
                                       4-11

-------
 analyses were  9,630 mg/kg for BEHP with 28.9 % RSD,  and 563 mg/kg for DNOP with


 38.8% RSD.    All  % RSD variances achieved  were within the  precision DQO for this


 measurement of 50% RSD.


 43     VOC ANALYSIS RESULTS


        Table 4-7 summarizes the measured concentrations of the target VOC analytes in test


 program samples collected.  As for the SVOC analysis data reported in Table 4-3, entries in


 Table 4-7 noted as less than values were not detected at the MDLs noted with the "<" sign.


 Complete analytical laboratory reports on the VOC  analyses  are given  in Appendices CM


 and C-2.


        As shown in Table 4-7, no fluff waste sample contained 1,1,2-trichloroethane at an MDL


 of 1 mg/kg. This contaminant was absent from one test soil sample, but found at 28 mg/kg in


 the other test soil.  Trichloroethene was not found in three of four fluff feeds at an MDL of


 1 mg/kg.  It was present in the fourth fluff feed at 2.4 mg/kg, and in the soil test feeds at 2.7 to


 3.9 mg/kg. Tetrachloroethene was not detected in two tests' fluff feed (before spiking) at an


 MDL of 4 mg/kg, though it was present at 4.9 and 17 mg/kg in the other two tests' fluff feed.
                              *'

 These  levels  are substantially lower than the 146 mg/kg  found in the pretest  fluff feed


 characterization sample indicated in Table 2-3, although they are comparable to levels reported


 in the ROD, indicated in Table 2-2. The contaminated soil tested contained 50 to 93 mg/kg of


 native  (before spiking) tetrachloroethene, in the range of the levels measured in pretest soil


 characterization samples,  as well as within the range of concentrations reported in  the ROD.


The addition of the tetrachloroethene spike to all test feed samples raised spiked fluff feed


concentrations to 3,100 mg/kg and spiked soil feed concentrations to the 3,200 to 3,300 mg/kg


range, as indicated in Table 4-7.
                                         4-12

-------
TABLE 4-7. VOLATILE ORGANIC CONTAMINANT ANALYSIS RESULTS
Sample
Test 0 (10/27/93), kiln temperature: 870C (1,599F)
Packaging container material, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, fig/dscm
Fluff Waste Tests
Test 1 (11/9/94), kiln temperature: 883C (1,622F)
Fluff feed, mg/kg, native
Fluff feed, mg/kg, spiked
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /tg/dscm
Test 2 (11/16/93), kiln temperature: 876C (1,608F)
Fluff feed, mg/kg, native
Fluff feed, mg/kg, spiked
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /ig/dscm
Test 5 (11/18/93), kiln temperature: 762C (1,403F)
Fluff feed, mg/kg, native
Fluff feed, mg/kg, spiked
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /tg/dscm
Test 6 (11/23/93), kiln temperature: 767C (1,412F)
Fluff feed, mg/kg, native
Fluff feed, mg/kg, spiked
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /tg/dscm .

. Tetrachloro-
ethene

<4
< 0.015
<4
0.66


4.9
3,100
<4
< 0.015
<4
0.27

<4
3,100
<4
<0.015
<4
0.71

<4
3,100
<4
<0.015
<4
0.68

17
3,100
5.6
< 0.015
<4
0.61
Concentration
1,1,2-Trichloro-
ethane

<0.004
<0.09


<0.004
<0.14

<0.004
<0.09

<0.004
<0.09

<0.004
0.23

Trichloiro-
ethene

<0.004
0.15


2.4
<0.004
0.16

< 0.004
0.14

<0.004
0.23

< 0.004
0.09
(continued)
                          4-13

-------
                                TABLE 4-7.  (continued)
Sample
Soil Feed Tests
Test 3 (12/1/93), kiln temperature: 876C (1,609F)
Soil feed, mg/kg, native
Soil feed, mg/kg, spiked
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, pg/dscm
Test 4 (12/2/93), kiln temperature: 874C (1,606F)
Soil feed, mg/kg, native
Soil feed, mg/kg, spiked
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /xg/dscm

Tetrachloro-
ethene


50
3,200
<4
<0.015
<4
1.57

93
3,300
<4
<0.015
<4
0.14
Concentration
1,1,2-Trichloro-
ethane


<1

<1
<0.004
<1
1.27

2.8

<1
<0.004
<1
<0.05

Trichloro-
ethene


2.7

<1
< 0.004
<1
0.73

3.9

<1
<0.004.
<1
0.17
        As was the case for the SVOC contaminants, incineration treatment of the fluff waste



at both temperatures tested and of the contaminated soil at the one temperature tested was




essentially completely effective in decontaminating the feed materials of their native and spiked



VOC contaminants.   The  kiln ash discharge for all tests  contained no detectable VOC




contaminants at MDLs ranging from 1 to 4 mg/kg with  the single exception of a 5.6 mg/kg




concentration of tetrachloroethene in the kiln ash from one low temperature fluff waste test.



This detected level is just above the MDL of 4 mg/kg. In addition, neither the post-test scrubber




liquor nor the baghouse ash from any test contained detectable VOC contaminants at MDLs, of




0.004 to 0.15  mg/L in scrubber liquor and 1 to 4 mg/kg in baghouse ash. Pretest scrubber liquor



samples similarly contained no detectable VOC contaminants at the same MDLs.




        The  baghouse exit flue gas for all tests,  including the blank burn test, contained low



levels of  both  trichloroethene, at 0.09 to 0.73 jig/dscm, and tetrachloroethene,  at 0.14 to
                                         4-14

-------
 1.57 /ig/dscm. No 1,1,2-trichloroethane was found in the baghouse exit flue gas at MDLs of 0.05



 to 0.14 ng/dscm for the blank burn test, either fluff test at the higher incinerator temperature,



 one of the two fluff tests at the lower incineration temperature, and one of the two soil feed



 tests. This contaminant was found in the baghouse exit flue gas from the two tests detected at



 0.23 to 1.27 /xg/dscm.  The baghouse exit flue gas concentration data noted represent averages



 for the three Method 0030 trap pairs analyzed for each test.   >




        Feed contaminant  concentration, feedrate,  baghouse exit flue  gas  contaminant




 concentration, and flue gas flowrate data can be combined to calculate spike tetrachloroethene




 DREs for each of the tests.  Calculated DREs are summarized in Table 4-8.  As shown in the




 table, the measured baghouse  exit flue gas tetrachloroethene concentrations corresponded  to




 tetrachloroethene  DREs  of  99.9984  to  99.99988 percent over  all  tests.   Comparable




 tetrachloroethene DREs were  measured for both fluff and soil, and for fluff treated  at both




 incineration temperatures.   All measured DREs were greater  than the 99.99 percent level




 required by the current hazardous waste incinerator performance standard.




        As noted in Section 3,  the Method 0030 train samples taken at the baghouse exit were



 also analyzed for the extended list of VOCs given in Table 3-7. The results of these analyses are



 summarized in Table 4-9 for those VOCs not given in Table 4-7. Concentrations in Table 4-9




 noted as less than values were either not detected at the MDL of the procedure used to measure



flue gas VOC concentration, or had a measured concentration not significantly different from



the method blank concentration. In these latter cases, the method blank concentration is noted



with the" <" sign.




        The data in Table 4-9 show that acetone, bromodichloromethane, carbon tetrachloride,




and chloroform were found in  the baghouse exit flue gas for all tests, including the blank test



(Test 0). Flue gas acetone concentrations were the highest for the blank test and the two fluff






                                         4-15

-------
          TABLE 4-8. TETRACHLOROETHENE DREs
                      Parameter
                                                        Tetrachloroethene
 Fluff Waste Tests
  Test 1 (11/9/93), kiln temperature: 883 C (lj622F)
   Feed concentration, mg/kg                                3,100
   Feedrate, kg/hr                                           0.19
   Baghouse exit flue gas:
     Concentration, pg/dscm
     Emission rate, mg/hr
   DRE,'%
  Test 2 (11/16/93), kiln temperature:  876C (1,608F)
   Feed concentration, mg/kg
   Feedrate, kg/hr
   Baghouse exit flue gas:
     Concentration, pg/dscm
     Emission rate, mg/hr
   DRE, %
  Test 5 (11/18/93), kiln temperature:  762C (1,403F)
   Feed concentration, mg/kg
   Feedrate, kg/hr
   Baghouse exit flue gas:
     Concentration, jjg/dscm
     Emission rate, mg/hr
   DRE, %
  Test 6 (11/23/93), kiln temperature:  767C (1,412F)
   Feed concentration, mg/kg
   Feedrate, kg/hr
   Baghouse exit flue gas
     Concentration, /ig/dscm
     Emission rate, mg/hr
   DRE, %
Soil Feed Tests
  Test 3 (12/1/93), kiln temperature:  876C (l,609eF)
   Feed concentration, mg/kg
   Feedrate, kg/hr
   Baghouse exit flue gas:
     Concentration, fig/dscm
     Emission rate, mg/hr
   DRE, %
  Test 4 (12/2/93), kiln temperature: 874eC (l,606eF)
   Feed concentration, mg/kg
   Feedrate, kg/hr
   Baghouse exit flue gas:
    Concentration, ;tg/dscm
    Emission rate, mg/hr
   DRE, %
 0.27
 0.46
 99.99975
 3,100
 0.18

 0.71
 1.4
 99.99924
3,100
0.19

0.68
1.4

99.99926
3,100
0.19

0.61
1.1
99.99941
3,200
0.19

1.57
3.0
99.9984
3,300
0.19

0.14
0.23
99.99988
                                 4-16

-------
TABLE 4-9. FLUE GAS VOC CONCENTRATIONS
Baghouse exit flue gas concentration, (ig/dscm
Compound
Acetone
Benzene
Bromodichloromethane
Carbon disulfide
Carbon tetrachloride
Chlorobenzene
Chloroform
Dibromochloromethane
1, 1-Dichloroethene
c- 1,3-Dichlof opropene
Methylene chloride
Toluene
1,1,1-Trichloroethane
Trichlorofluoromethane
Blank test
TestO
10/27/93
130
63
0.48
<0.5
0.25
<0.19
1.1
<0.09
<0.09
<0.05
<2.5
39
<0.09
<1,0
Fluff waste tests
Testl
11/9/93
420
32
0.17
<18
0.83
<0.05
3.6
1.3
<0.09
<0.05
18
11
<0.09
<2.3
Test 2
11/6/93
460
300
0.15
<73
0.44
1-1
2.4
1.3
<0.09
<0.05
97
210
0.39
<2.4
Tests
11/18/93
23
8.3
1.2
<17
0.19
<0.04
2.3
0.94
<0.09
<0.04
15
<2.0
0.16
<2.6
Test 6
11/23/93
2.5
<6.4
1.9
<64
0.41
<0.05
3.8
1.2
<0.09
0.21
34
<2.1
0.39
<0.8
Soil
Tests
12/1/93
1.4
14
4.4
<23
1.1
0.60
12
1.9
<0.09
<0.05
100
9.2
6.1
<1.5
tests
Test 4
12/2/93
1.2
<5.2
1.6
<22
0.36
<0.05
4.2
0.74
<0.10
<0.05
72
<2.1
<0.10
<0.39

-------
  waste tests at the higher incineration temperature tested; levels for the fluff waste tests at the




  lower incineration temperature and for the soils tests were substantially lower. No explanation



  for this observation is offered.  Flue gas carbon tetrachloride concentrations were comparable




  from test to test, including the blank test, and ranged from a few to several tenths of a /zg/dscm.




  Hue gas chloroform concentrations were also comparable from test to test, but were higher, in




  the 1 to 12 ng/dscm range. Methylene chloride was measured in the baghouse exit flue gas for



 all tests except the blank test; concentratiqns ranged from 18 to 100 /ig/dscm.




         The presence of bromodichloromethane, seen  in  the flue  gas  for  all tests,  and



 dibromochloromethane, seen in the flue gas for all tests except the blank test, arises from the




 trihalomethane (THM) compounds present in the recirculating scrubber liquor. The plant water




 used for scrubber makeup is local well water subjected to a water treatment process that includes




 disinfection.  The disinfection process leaves low levels of THM compounds in the water. The




 observation that dibromochloromethane was not detected in the Test 0 flue gas, but was at




 concentrations substantially above the MDL for the fluff waste and soil tests suggests that EtCl




 or organochlorine compounds, such as methylene chloride, need to be present in the flue gas



 being scrubbed in order to form dibromochloromethane.




 4.4     PCDD/PCDF ANALYSIS RESULTS




        As noted in Section 3, incinerator feed, kiln ash, post-test scrubber liquor, and baghouise



 ash samples for all tests were analyzed for PCDDs and PCDFs.  In addition, the baghouse exit



 flue gas was sampled, and collected samples correspondingly analyzed. Analyses were performed



for the total concentration of each homologue grouping of total tetra-, penta-, hexa-, hepta-, and



octa-chlorinated  dibenzo-p-dioxins  (TCDD,  PeCDD, HxCDD, HpCDD, and OCDD) and




dibenzofurans (TCDF, PeCDF, HxCDF, HpCDF, and OCDF) as well as the concentration of
                                        4-18

-------
 each congener chlorinated in the 2, 3, 7, and 8 positions within each group. Analysis results are



 given, by sample matrix, in Tables 4-10 through 4-14.




        Two summary measures of dioxin/furan concentrations are commonly cited.  The first



 measure, total PCDD/PCDF, represents the sum of the homologue group total concentrations



 analyzed. The second measure, 2,3,7,8-TCDD toxicity equivalent (TEQ), is a weighted sum of




 each 2,3,7,8-chlorinated  congener's concentration.   In  calculating  TEQs,  the measured




 concentration of each specific 2,3,7,8-chlorinated congener is weighted by a toxicity equivalent




 factor (TEF).  The TEF is a measure of the congener's toxicity relative to 2,3,7,8-TCDD, which




 has a TEF  of 1.  The TEFs used to calculate the TEQs here are those specified by EPA



 (Reference 2) and given in  Table 4-15.




        Table 4-16 summarizes the chlorinated dioxin  and furan concentrations in test program




 samples in terms of the two summary measures. In many cases, concentrations in Table 4-16 are




 reported as ranges. This arises out of the fact that analyzed concentrations for both homologue




 group totals and specific congeners are often reported as being less than an MDL, as indicated




 by the less than values in Tables 4-10 through 4-14.  Thus, in cases where  a concentration is



 listed as a range in Table 4-16, the maximum value in the range corresponds to the assumption



 that constituents not detected were present at the MDL,  and the minimum value in the range



 corresponds to the assumption that they were not present, i.e., at zero concentration.




       The data in Table 4-16 show that the fluff feed  contained 56 fig/kg of total  PCE'D/




 PCDF or 0.73 fig/kg on a TEQ basis (1 ng/kg, often reported as parts per billion, or ppb, equals



 1,000 ng/kg, the unit used for solid samples in Table 4-16;  1 ng/kg is often reported as parts per



 trillion, or ppt). Levels in the kiln ash discharge from the higher temperature incineration tests



were somewhat higher at 65 to 89 ng/kg total, or 1.2 to 2.0 /tg/kg TEQ. Levels in the kiln ash



 discharge from the lower temperature incineration tests were substantially higher, at 8301 to






                                        4-19

-------
           TABLE 4-10. PCDDs AND PCDFs IN TEST FEED SAMPLES

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
Test
Composite fluff
140
7.1a
180
31
1,360
45
110
150
3,160
1,590
10,700
2,660
110
2,740
250
220
4,660
1,580
470
530
180
9,360
4,180
2,240
22,100
feed concentration, i
Composite soil
170
2.8
310
18
680
28
54
77
790
430
2,290
1,360
34
1,220
51
100
1,260
420
100
150
7.2a
1,000
cen
120
920
ng/kg
Packaging container
material
1.6
0.20a
0.41
0.15a
3.2
<0.5
0.37
0.30a
20.2
10.0
126
6.3
0.50a
3.0
0.44
0.37
1.9
0.79
0.27
0.74a
<0.4
2.9
1 *3
2.6
<0.7
15.7
Estimated maximum possible concentration; see Appendix C-6.
                                  4-20

-------
                               TABLE 4-11. PCDDs AND PCDFs IN KILN ASH SAMPLES
to
Kiln ash concentration, ng/kg
Fluff waste tests


Kiln exit gas temperature, C
(F)
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
Testl
(H/9/93)
883
(1,622)

320
12
310
31
910
51
71
210
3,830
1,810
11,600
3,330
82
5,730
160
270
10,800
2,770
610
2310
25
15,800
6,180
1,360
12,200
Test 2
(11/16/93)
876
(1,608)

38
1.0
290
19
2,050
120
160
570
8,790
4,480
14,100
2,820
28
9,550
120
470
15,200
4,540
1,220
4,110
83
21,200
6,210
3,810
15,400
TestS
(11/18/93)
762
(1,403)

3,190
230
10,500
990
40,400
1,850
3,100
8,300
117,000
56,100
109,000
64,300
760
110,000
3,450
9,520
101,000
54,800*
18,800
46,900
5,840
164,000
51,600
233,000
,114,000
Test 6
(11/23/93)
767
(1,412)

450
23"
7,120
400
53,900
2,080
3,650
9,770
107,000
107,000
739,000
72,200
500
179,000
2,370
15,500
448,000
325,000"
25,800
287,000
1,210
360,000
106,000
14,800
728,000
Soil tests
Test 3
(12/1/93)
876
(1,609)

3.4
0.09"
14
1.2*
47
31
3.6
14
110
57
230
ISO
3.2
300
7.2
24
430
120
29
80
1.7
610
320
47
510
Test 4
(12/2/93)
874
(1,606)

6.6
0.18
19
2.2"
96
6.5
7.4
36
160
88
180
310
3.6
600
11
44
830
230
54
140
4.6
910
120
95
500
         Estimated maximum possible concentration; see Appendix C-6.

-------
                      TABLE 4-12. PCDDs AND PCDFs IN SCRUBBER LIQUOR SAMPLES
Post-test scrubber concentration, pg/L


Kiln exit gas temperature, *C
("F)
Analyte
Total TCDD
23,7,8-TCDD
Total PeCDD
1,2,3,7,8-PeCDD
Total HxCDD
1,23,4,7,8-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
1,23,7,8-PeCDF
23,4,7,8-PeCDF
Total HxCDF
1,2,3,4,7,8-HxCDF
1,23,6,7,8-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
Blank test
Test 0 .
(10/27/93)
870
(1,599)


-------
                       TABLE 4-13.  PCDDs AND PDCFs IN BAGHOUSE ASH SAMPLES
Baghouse ash concentration, ng/kg


Kiln exit gas temperature, C
("*) .
Analyte
Total TCDD
23,7,8-TCDD
Total PeCDD
1,23,7,8-PeCDD
Total HxCDD
1,23,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,23,7,8,9-HxCDD
Total HpCDD
1,23,4,6,7,8-HpCDD
OCDD
Total TCDF
23,7,8-TCDF
Total PeCDF
1,23,7,8-PeCDF
2,3,4,7,8-PeCDF
Total HxCDF
1,23,4,7,8-HxCDF
1,23,6,7,8-HxCDF
23,4,6,7,8-HxCDF
1,23,7,8,9-HxCDF
Total HpCDF
1,23,4,6,7,8-HpCDF
1,23,4,7,8,9-HpCDF
OCDF
Blank test
TestO
(10/27/93)
870
(1,559)

0.17
0.08*
0.19
<0.1
13
<0.2
<0.1
036
10
53
38
1.1
0.70
2.5
0.28
0.55
4.0
1.0
0.41
1.0
<0.2
3.4
2.4
0.56
3.6
Fluff waste tests
Testl
(11/9/93)
883
(1,622)

0.90
<03
 1.5
0.47
6.4
<0.4
0.69*
1.5
39
21
180
15
1.1
27
1.5
3.2
40
11
3.9*
9.1
<03
83
40
8.1
120
Test 2
(11/16/93)
876
(1,608)

<0.2
<0.2
0.62
<0.2
6.2
<0.2
0.85
1.7
40
21
180
12.
0.69
26 .
1.1
23
65
18
5.2
17
<0.2
120
79
15"
380
TestS
(11/18/93)
762
(1,403)

4.6
036
5.3
1.1
6.0
0.53
0.76*
1.6
20
11
51
39
1.9
50
3.4
4.7
46
10
4.7
8.9
1.9*
59
29
7.0
56
Test 6
(11/23/93)
767
(1,412)

0.6*
<0.6
3.9
<1.0
19
<0.9
1.8*
5.0
72
37
200
15
3.0
86
5.1
11
150
39
11
37
2.9*
250
110
34
230
Soil tests
Test 3
(12/1/93)
876
(1,609)

0.48
0.23
4.6
0.58
21
1.2
1.9*
1.6*
90
44
250
46
2.8
130
6.9
11
320
80
24
67
1.4
740
41
52
990
Test 4
(12/2/93)
874
(1,606)

03*

0.85*
<0.2
33
03*
0.68
1.4*
27
14
67
8.5
1.2
26
1.5*
3.5
61
15
5.5
15
038*
110
54
11
85
'Estimated maximum possible concentration; see Appendix C-6.

-------
                  TABLE 444. PCDDs AND PCDFs IN BAGHOUSE EXIT FLUE GAS
Baghouse exit flue gas concentration, ng/dscm



Kiln exit gas temperature, C
CF)
Analyte
Total TCDD
2,3,7,8-TCDD
Total PeCDD
1,2,3,7,8-PeCDD
Total HxCDD
lA3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2^,7,8,9-HxCDD
Total HpCDD
1,2,3,4,6,7,8-HpCDD
OCDD
Total TCDF
23,7,8-TCDF
Total PeCDF
1,2,3,7,8-PeCDF
23,4,7,8-PeCDF
Total HxCDF
1,2,3,4,7,8-HxCDF
lA3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
lA3,7,8,9-HxCDF
Total HpCDF
1,2,3,4,6,7,8-HpCDF
1^,4,7,8,9-HpCDF
OCDF
Blank test
TestO
(10/27/93)
870
(1399)

< 0.002
< 0.002
<0.002
< 0.002
< 0.005
<0.005
<0.002
<0.005
0.005
0.005
0.017
0.017
0.002
0.012*
<0.002
<0.002
0.022
0.010
0.005
0.002"
<0.002
0.024*
0.012'
< 0.005
0.017
Fluff waste tests
Testl
(H/9/93)
883
(1,622)

0.006*
<0.002
0.006"
< 0.002
0.021
< 0.002
0.002
0.003
0.024
0.012
0.021
0.175
0.015
0.275
0.021
0.024
0.206
0.057
0.021
0.024
<0.002
0.067
0.051
0.006"
0.039
Test 2
(11/16/93)
876
(1,608)

0.002
< 0.002
0.006
< 0.003
0.006
< 0.002
0.002
0.002
0.021 '
0.009
0.027
0.246
0.012
0.249
0.024
0.021
0.224
0.058
0.024
0.024
<0.002
0.061
0.048
0.009
0.058
Tests
(11/18/93)
762
(1,403)

< 0.003
< 0.003
<0.006
< 0.006
< 0.003
<0.006
< 0.003
< 0.003
0.009"
0.006"
0.024
0.065
0.006
0.065
0.009
0.009
0.059
0.018
0.006
0.012
< 0.003
0.042
0.027
< 0.006
0.027
Test 6
(11/23/93)
767
(1,412)

0.003
<0.003
<0.006
<0.006
0.003
<0.006
<0.003
< 0.003
0.009"
0.006"
0.016
0.169
0.019
0.228
0.019
0.022
0.169
0.047
0.016
0.022
<0.003
0.056
0.047
<0.006
0.031
Soil tests
Test3
(12/1/93)
876
(1,609)

<0.002
< 0.002
<0.003
<0.003
0.013
<0.003
<0.002
<0.002
0.013
0.013
0.066
0.078
0.009
0.097
0.009
0.013
0.085
0.031
0.009
0.016*
<0.002
0.066
0.035
0.006
0.035
Test 4
(12/2/93)
874
(1,606)

0.001
<0.001
< 0.001
< 0.001
0.003
<0.001
0.002
0.001"
0.019
0.009
0.044
0.078
0.006
0.062
0.006
0.009
0.056
0.019
0.006"
0.012
0.001
0.044
0.025
0.006
0.025
"Estimated maximum possible concentration; see Appendix C-6.

-------
TABLE 4-15.  2,3,7,8-TCDD TOXICITY EQUIVALENT FACTORS
            (Reference 2)

       .  Compound          Toxicity equivalent factor

   2,3,7,8-TCDD                       1
   Other TCDDs                      0

   2,3,7,8-PeCDD                      0.5
   Other PeCDDs                      0

   2,3,7,8-HxCDD                      0.1
   Other HxCDDs                     0

   2,3,7,8-HpCDD                      0.01
   Other HpCDDs                     0

   OCDD                            0.001

   2,3,7,8-TCDF                       0.1
   Other TCDFs                       0

   1,2,3,7,8-PeCDF                     0.05
   2,3,4,7,8-PeCDF                     0.5
   Other PeCDFs                      0

   2,3,7,8-HxCDFs                     0.1
   Other HxCDFs                      0

   2,3,7,8-HpCDFs                     0.01
   Other HpCDFs                     0

   OCDF                             0.001
                         4-25

-------
TABLE 4-16. TOTAL DIOXINS AND TEQs IN TEST PROGRAM SAMPLES
Sample
Test 0 (10/27/93), kiln temperature:
870C (1,599F)
Packaging container material, mg/kg
Scrubber liquor, pg/L
Baghouse ash, ng/kg
Baghouse exit flue gas ng/dscm at 7% O2
Fluff Waste Tests
Fluff feed, ng/kg
Test 1 (11/9/93), kiln temperature:
883 C (1,622F)
Kiln ash, ng/kg
Scrubber liquor, pg/L
Baghouse ash, ng/kg
Baghouse exit flue gas, ng/dscm at 7% O2
Test 2 (11/16/93), kiln temperature:
876C (1,608F)
Kiln ash, ng/kg
Scrubber liquor, pg/L
Baghouse ash, ng/kg
Baghpuse exit flue gas, ng/dscm at 7% O2
Test 5 (11/18/93), kiln temperature:
762 C (1,403 F)
Kiln ash, ng/kg
Scrubber liquor, pg/L
Baghouse ash, ng/kg
Baghouse exit flue gas, ng/dscm at 7% O2
Test 6 (11/23/93), kiln temperature:
767C (1,412F)
Kiln ash, ng/kg
Scrubber liquor, pg/L
Baghouse ash, ng/kg
Baghouse exit flue gas, ng/dscm at 7% O2
Total PCDD/PCDF

180
68-170
64
0.21

56,000

65,000
370-380
520
1.3

89,000
730-750
740
1.3

830,000
290
340
0.44

2,700,000
520-540 '
1,000
0.96
TEQ

1.2-1.3
9.7-25
0.94-1.0
0.005-0.017

730

1,200
4.6-12
6.8-7.0
0.048-0.052

2,000
7.0-23
8.9-9.2
0.044-0.049

29,000
17-18
81
0.016-0.027

110,000
6.7-23
22-23
0.038-0.049
                                                     (continued)
                          4-26

-------
                                TABLE 4-16.  (continued)
Sample
SoU Feed Tests
Soil feed, ng/kg
Test 3 (12/1/93), kiln temperature:
876 C (1,609 F)
Kiln ash, ng/kg
Scrubber liquor, pg/L
Baghouse ash, ng/kg
Baghouse exit flue gas, ng/dscm at 7% O2
Test 4 (12/2/93), kiln temperature:
874C (1,606F)
Kiln ash, ng/kg
Scrubber liquor, pg/L
Baghouse ash, ng/kg
Baghouse exit flue gas, ng/dscm at 7% O2
Total PCDD/PCDF

10,000

2,400
2,300-2,400
2,600
0.68

3,600
260-280
390
0.48
TEQ

210

55
46-54
39
0.025-0.032

98
1.3-15
8.2-8.4
0.018-0.020
2,700 /ig/kg total, or 29 to 110 /zg/kg TEQ. These data indicate that, not only was incineration




treatment ineffective in destroying contaminant dioxins and furans in the fluff waste, in fact




conditions experienced by the noncombustible fraction of the fluff waste during incineration



likely led to PCDD/PCDF formation at the lower temperature.




        That PCDD/PCDF formation in the kiln ash discharge occurred,  at least for the fluff



waste tests at  the lower incineration temperatures, is further substantiated by the data in




Table 4-17. The total weight of fluff waste or soil fed and the total weight of kiln ash collected




for each test are combined with respective PCDD/PCDF concentrations  from Table 4-16 to



ultimately give the ratios of the amounts of dioxins and furans discharged in the kiln ash to the



amounts introduced in the incinerator feed for each test. The data show that, for the fluff waste




tests at the target 870C (1,600F) kiln exit gas temperature, the amount of total PCDD/PCDF




discharged was 5.9 to 8.3 percent of the amount introduced to the incinerator in the fluff feed.






                                        4-27

-------
TABLE 4-17. RATIO OF DISCHARGED DIOXINS AND FURANS TO FED AMOUNTS
Waste feed


Test
Fluff Waste Tests
Test 1 (11/9/93)
Kiln temperature:
883C (1,622F)
Test 2 (11/16/93)
Kiln temperature:
876C (1,608F)
Test 5 (11/18/93)
Kiln temperature:
762C (1,403F)
Test 6 (11/23/93)

Total weight
fed, kg

303

304

307

305
PCDD/PCDF fed, ng
Total
PCDD/PCDF TEQ

17,000 220

17,000 220

17,200 220

17,100 220
s=s::======:======s=======s=====================^^
Ratio of PCDD/PCDF
discharged to amount fed,
Kiln ash discharge %

Total weight
discharged, kg

15.4

15.9

20.4

17.3
PCDD/PCDF
discharged, jig
Total
PCDD/PCDF TEQ Total PCDD/PCDF TEQ

1,000 18 5.9 8.4

1,420 32 8.3 14.3

16,900 590 98.5 264

46,700 1,900 273 855
  767C
Soil Feed Tests

 Test 3 (12/1/93)
  Kiln temperature:
  876C (1,609'F)

 Test 4 (12/2/93)
  Kiln temperature:
  874C (1,606F)
     288
     290
2.900
60
          61
                                        101
                                        145
                          240
                                    520
                                                               5.6
                                                              14.2
                                                             8.5
                                                             18.0
                                                                                         9.2
                                                                                         23.4

-------
 This would correspond to an effectiveness of dioxin/furan decontamination by incineration at



 this higher tested temperature of 91.7 to 94.1 percent. On a TEQ basis, the ratio of discharged-



 to-fed dioxins/furans was 8.4 to 14.3 percent, corresponding to incineration decontamination




 effectiveness or a TEQ basis of 85.7 to 91.6 percent at the higher incineration temperature.




        However,  for  the  fluff waste tests at the 760C (1,400F) target  kiln  exit gas




 temperature, the amount of total PCDD/PCDF discharged was 98.5 to 273 percent of the




 amount fed. In other words, the quantity of total PCDD/PCDF discharged for the lower kiln




 temperature fluff tests was roughly the same to 2.7 times the amount fed to the incinerator. On




 a TEQ basis the ratios of discharged to feed dioxins/furans were even larger, at 264 to




 855 percent. Clearly, at the lower incineration temperatures, dioxins/furans were beingproduced



 in the noncombustible fraction of the fluff waste feed ultimately discharged as kiln ash.




        This should not be surprising, however. It has become recognized over the past few




years that dioxins and furans arising out of combustion processes result from the formation of




 these compounds from precursor organic constituents and a chlorine source, such as HC1, at




 relatively low temperatures (Reference 5).  The presence of metal-containing solids, such as



 particulate, appears to catalyze  the process.  Copper has specifically been shown to  catalyze




 reactions leading to dioxin/furan formation.  The rate of dioxin/furan formation is highest at



temperatures near  300 C (570 F), and  this rate  decreases as the temperature at which



precursors, a chlorine source, and metal-bearing solids are held is either increased or decreased.




        Evidently, the right combination of conditions were in place in the kiln solids bed before,




or shortly after, discharge from the kiln into the ash collection  pit  of the RKS during the



incineration of the fluff waste at the 760C (1,400F) target kiln  temperature.  Dioxin/furan



precursors were likely present in the near-bed combustion gas, and chlorine, likely in the form




of HC1 from the chloroorganic components of the fluff, was likely in abundance. The fluff waste






                                          4-29

-------
 tested contained 17 percent by weight chlorine. As discussed below, a major contaminant metal




 in the fluff waste was copper, so this likely dioxin-formation catalyst was present. Apparently



 kiln solids bed temperatures were sufficiently close to the peak reaction temperature of 300C




 (570 F) to be within a "dioxin formation" window. The data clearly show that dioxin formation



 occurred at the lower incineration temperature tested.




        All other dioxin formation conditions would have been in effect for the fluff incineration



 tests, at the 870C  (1,600F) target kiln exit gas  temperature.   However, at this higher




 incineration  temperature, kiln solids bed temperatures were apparently above the window




 associated with more rapid dioxin formation.  Similar results were seen in the soil feed tests, also




 performed at the higher, 870C (1,600F), target kiln exit gas temperature. Ratios of discharged




 to feed PCDD/PCDFs noted in Table 4-17 for the soil tests are comparable to those experienced



 for the fluff waste tests at the higher incineration temperature.




        Returning to the data  in Table 4-16, the scrubber liquor for the fluff waste tests




 contained total PCDD/PCDF concentrations in the 290 to 750 pg/L (1 pg/L is often reported




 as parts per  quadrillion, or ppq). Scrubber  liquor concentrations were in the 4.6 to 23  pg/L




 ranges on  a  TEQ basis.  No apparent difference in the scrubber liquor concentrations with



 incineration temperature was seen.   The scrubber liquor concentration measured during the



 blank burn test was comparable to those for  the fluff waste tests on a TEQ basis, though total




 PCDD/PCDF concentrations were slightly lower. Scrubber liquor dioxin/furan concentrations



 for one of  the two soil feed  tests were also comparable to those measured for the fluff waste




 tests, although levels measured for the other  soil feed test were substantially higher.




        Baghouse ash total PCDD/PCDF concentrations ranged from 340 to 1,000 ng/kg (ppt)



for the  fluff waste tests, with no  apparent change associated with  changing incineration



temperature.  On a TEQ basis, the measured range was 6.8 to 23 ng/kg. Baghouse ash dioxin






                                         4-30

-------
 levels were lower for the blank burn test on both bases.  As for the scrubber liquor, baghoese



 ash dioxin levels for one of the two soil feed tests were comparable to those measured for the



 fluff waste tests; they were higher for the other soil feed  test.




        Baghouse exit flue gas total PCDD/PCDF levels were 0.021 ng/dscm  corrected to



 7 percent O2 for the blank burn  test.  Measured levels were  increased,  at 1.3 ng/dscm at




 7 percent O2, for the fluff waste tests at the 870C (1,600F) target kiln exit gas temperature.




 Levels for the fluff waste test at the 760C (1,400F) target kiln exit gas temperature, at 0.44 to




 0.96 ng/dscm at 7 percent O2, were slightly lower than for the higher temperature tests. Levels




 for the soil feed tests were comparable, at 0.48 to 0.68  ng/dscm.  All measured levels were




 significantly lower than the EPA guidance announced in 1993 of 30 ng/dscm at 7 percent O2.




        On a TEQ basis, baghouse exit flue gas dioxin/furan levels were 0.005 to 0.017 ng/dscm




 at 7 percent O2 for the blank burn test, increased, at 0.044 to 0.052 ng/dscm at 7 percent O2 for




 the fluff waste tests at the 870C (1,600F) target kiln exit gas temperature.  Compared to these




latter levels, comparable to slightly decreased emissions, at 0.016 to 0.049 ng/dscm at 7 percent




 O2, were measured for the fluff waste tests at the 760C (1,400F) target kiln exit gas




temperature.  Levels measured for the soil feed tests were also comparable,  at 0.018  to



0.032 ng/dscm at 7  percent O2.   The European suggested  dioxin emission  limit  for waste



incinerators is 0.1 ng/Nm3 TEQ corrected to 11 percent O2.  Thus, while the temperature



correction for son is slightly different than for Nm3, and the O2 correction for the  European



standard,  at  11 percent O2, differs from the 7 percent  O2  used in the Table 4-16 data, all




emission levels reported in Table 4-16 are lower than the suggested European  standard




4.5     TRACE METAL AND TCLP ANALYSIS RESULTS




        Trace metal concentrations measured in test program  samples are  summarized  in



Table 4-18.  The data in the table clearly show that the major metal contaminants in both the
                                         4-31

-------
                                           TABLE 4-18. TRACE METAL ANALYSIS RESULTS
                              Sample
         Test 0 (10/27/93), kiln temperature:  870C (1,599F)

          Packaging container material, mg/kg
          Scrubber liquor, mg/L
          Baghouse ash, mg/kg
         Fluff Waste Tests

          Test 1 (11/9/93), kiln temperature:  883C (1,622F)

           Fluff feed, mg/kg
           Kiln ash, mg/kg
           Scrubber liquor, mg/L
           Baghouse ash, mg/kg
^         Baghouse exit flue gas, /g/dscm

o        Test 2 (11/16/93), kiln temperature:  876C (1,608'F)

           Fluff feed, mg/kg
           Kiln ash, mg/kg
           Scrubber liquor, mg/L
           Baghouse ash, mg/kg
           Baghouse exit flue gas, pg/dscm

          Test 5 (11/18/93), kiln temperature:  762eC (1,403'F)

           Fluff feed, mg/kg
           Kiln ash, mg/kg
           Scrubber liquor, mg/L
           Baghouse ash, mg/kg
           Baghouse exit flue gas, /tg/dscm
Sb
                                                                                           Concentration
As
Ba     Cd
                                                                                         Cr
                                    Cu
                                      Pb
                                                                                                                   Ni
                                                              Ag
                                                                                                                                   Zn
<20
0.7
120
<20
<0.05
<20
6.7
8.5
18
<0.5
0.05
6.6
1.0
0.7
510
<2
0.6
58
<10
18
410
<4
030
150
<0.7
<0.007
<0.7
8.9
6.6
1,800
120
1,100
4.7
830
<21
180
940
3.7
400
<11
90
950
4.7
1,300
IJIIL1 "- '
<20
<20
0.12
24
<19
<20
30
0.08
<20
<22
<20
<20
0.20
<20
 Ml .!_  .
74
270
2.4
38
50
70
220
1.8
22
6
47
240
1.5
35
6
  *" i
1.4
<0.5
0.20
33
<50
1.5
<0.5
0.14
18

-------
                                                            TABLE 4-iS. (continued)
                                                                                             Concentration
                             Sample
Sb
As
Ba
Cd
                                Cr
                                                                                                     Cu
                                        Pb
                                        Ni
                                                                                                                              Ag
                                                                          Zn
fk
u>
         Fluff Waste Tests (concluded)

          Test 6 (11/23/93), kiln temperature: 767C (1,412F)

           Fluff feed, mg/kg
           Kiln ash, mg/kg
           Scrubber liquor, mg/L
           Baghouse ash, mg/kg
           Baghouse exit flue gas, pg/dscm

         Soil Feed Tests
100
950
4.9
1,900
<10
<20
46
0.10
<20
<14
81
250
1.4
19
5
1.0
<0.5
0.20
70
<1
24
530
1.4
510
<4
8,400
176,000
180
77,000
26
900
5,700
610
38,000
38
4.6
340
0.9
160
<4
13
3.0
0.08
1.0
<2
120
250
12
5,000
44
Average soil feed, mg/kg
Test 3 (12/1/93), kiln temperature: 876C (1,609F)
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, jtg/dscm
Test 4 (12/2/93), kiln temperature: 874C (1,606F)
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /tg/dscm
66

190
1.5
1,400
<10

190
13
950
<13
<20

<20
<0.05
<70
<15

<20
<0.05
<20
<29
72

120
13
29
10

91
1.3
19
6
13

<0.5
0.10
57
<1

<0.5
0.20
43
<2
85

73
0.8
540
<3

56
1.0
520
<3
14,000

53,000
iio
64,000
51

35,000
160
52,000
620
3,100

4,100
120
48,000
190

4,100
180
41,000
2,030
29

62
03
190
<9

51
0.4
200
<6
<2

1.5
0.02
<0.7
<2

1.9
0.02
<0.7
<2
190

320
3
4,200
20

290
4
2,900
42

-------
  fluff waste and the contaminated soil were copper and lead.  Both of these metals were also




  present in the kiln ash discharge for all tests. The presence of high concentrations of these



  metals, especially copper, in the kiln ash discharge substantiates that presumed catalysts for the




  relatively low temperature reactions in the dioxin formation pathway would be present in the kiln




  ash so that dioxin formation in this  matrix, especially as noticed for the lower incineration



  temperature fluff waste tests, can be understood.




         Fluff and soil feed, kiln ash, scrubber liquor, and baghouse ash samples from the test



 program were subjected to the TCLP, and resulting TCLP leachates were analyzed for the test




 program trace metals. Leachate analysis data are  summarized in Table 4-19 For the six TCLP




 metals with regulatory levels defined, the regulatory level is also given in the table. The data in




 the table show that the fluff waste from two of the four tests would be a lead-contaminated TC




 hazardous waste. Further, the lead concentrations in the leachates of the fluff for the other two




 tests were very close to the regulatory level for lead. Despite this, no resulting kiln ash discharge




 from the incineration of fluff waste would be a TC  hazardous waste due to its leachable lead, or



 any other metal analyzed, concentration. Similarly, the scrubber liquor from all fluff waste tests




 was not TC hazardous. However, the baghouse ash  for all fluff waste tests would be a lead-




 contaminated TC hazardous waste, and for three of the four tests a cadmium-contaminated TC



 hazardous waste.




        Although the contaminated soil tested was  not a TC hazardous waste, conclusions



regarding the TC status of the residual discharges from its incineration were the same as for the




fluff waste.  Namely, neither the kiln ash discharge nor the scrubber liquor resulting from its



incineration under the conditions tested would possess the TC,  and the baghouse  ash for both



tests performed would be considered both cadmium- and lead-contaminated TC hazardous waste.
                                         4-34

-------
                         TABLE 4-19. TCLP LEACHATE ANALYSIS RESULTS
Leachate concentration, mg/L
Sample leached
Regulatory Level
Test 0 (10/27/93), kiln temperature: 870C (1,599F)
Scrubber liquor
Baghouse ash
Fluff Waste Tests
Test 1 (11/9/93), kiln temperature: 883C (1,622F)
Fluff feed
Kiln ash
Scrubber liquor
Baghouse ash
Test 2 (11/16/93), kiln temperature: 876C (1,608F)
Fluff feed
Kiln ash
Scrubber liquor
Baghouse ash
Test 5 (11/18/93), kiln temperature: 762C (1,403F)
Fluff feed
Kiln ash
Scrubber liquor
Baghouse ash
Test 6 (11/23/93), kiln temperature: 767C (1,412F)
Fluff feed
Kiln ash
Scrubber liquor
Baghouse ash
Sb
__

<0.03
33


0.23
<0.03
0.55
0.85

0.26
0.05
0.42
0.43

0.26 
0.24
0.60
<0.2

0.26
0.28
0.71
<0.2

As
5

<0.05
0.34


<0.05
<0.05
<0.05
0.20

<0.05
<0.05
<0.05
0.08

<0.05
<0.2
<0.05
<0.2

<0.05
<0.2
<0.05
<0.2
Ba
100

0.17
0.25


0.25
1.2
0.93
0.23

0.26
13
0.76
0.05

0.19
2.2
0.60
0.4

0.55
1.2
0.6
0.6
Cd
1

< 0.004
030


0.03
< 0.004
0.03
1.4

0.04
< 0.004
0.03
0.9

0.03
< 0.005
0.03
1.8

0.03
<0.005
0.02
1.8
Cr
5

0.052
4.5


< 0.007
0.32
0.06
0.29

< 0.007
0.41
0.04
0.20

<0.007
0.05
0.04
0.13

< 0.007
0.01
0.05
0.2
Cu


0.05
1.4


120
0.14
0.91
720

130
0.05
0.09
340

130
<0.02
13
1,400

130
0.072
1.2
1,400
Pb
5

<0.04
0.07


3.6
0.42
0.52
3,800

5.4
0.09
0.40
1,900

3.7
<0.1
2.2
5,200

5.8
050
0.6
4,400
Ni
_

<0.01
1.7


0.02
<0.01
0.08
2.0

0.02
0.01
0.06
28

0.02
<0.01
0.05
23

0.02
<0.01
0.06
2.8

Ag
5

< 0.007
< 0.007


<0.007
< 0.007
0.08
< 0.007

< 0.007
<0.007
0.09
0.02

< 0.007
< 0.007
0.06
0.02

<0.007
< 0.007
0.08
0.02
r=^^==
Zn
_,

0.12
84


3.2
0.03
0.16
150

4.1
0.07
0.13
100

3.7
0.02
0.10
180

4.6
0.02
0.10
200
g"  
No regulatory level; not a TCLP metal.
                                                                                          (continued)

-------
                                                TABLE 4-19.  (continued)
O\
Leachate concentration, mg/L
Sample leached
Regulatory Level
Soli Feed Tests
Average soil feed
Test 3 (12/1/93), kiln temperature: '8760C (1,609F)
Kiln ash
Scrubber liquor
Baghouse ash
Test 4 (12/2/93), kiln temperature: 874C (1,606F)
Kiln ash
Scrubber liquor
Baghouse ash
 m Nrt rponfatArv l*nM1- tint o TV'T P Miafaf
Sb
a

0.09

<0.2
0.09
0.90

<0.2
0.08
0.80

As
5

<0.05

<0.2
<0.05
0.2

<0.2
<0.05
0.24

Ba
100

0.91

0.26
0.16
0.50

'0.70
0.09
0.2

Cd
1

0.02

< 0.005
<0.004
2.2

<0.005
.< 0.004
1.7

Cr
5

< 0.007

0.05
0.04
03

0.03
0.10
03

Cu


21

0.25
0.02
760

0.2
0.09
640

Pb
5

0.67

0.08
6,600

0.2
039
5,700

Ni
_

0.02

<0.01
<0.01
2.7

<0.01
0.24
3.2

Ag
5

< 0.007

< 0.007
< 0.007
0.03

< 0.007
< 0.007
0.03
===:
Zn
H

1.1

13
0.01
120

0.04
0.03
100
 ___

-------
        The scrubber liquor TCLP leachate metals content data given in Table 4-19 deserve



some discussion, especially when compared to the scrubber liquor metals content data given in




Table 4-18.  The scrubber liquor metals data in Table 4-18 correspond to complete scrubber




liquor samples, including the suspended solids in the liquor.  For liquid samples containing




suspended solids, the TCLP specifies filtering the sample. If the resulting filtered solids content



of the sample is less than 0.5 percent (the case for all scrubber liquor samples collected in this



test program), then the filtrate is defined to be the sample TCLP leachate.




        Comparing the scrubber liquor data in Table 4-19 to the data in Table 4-18 shows that




the metals concentrations in the scrubber liquor TCLP leachate are almost always less than, and




in many cases much less than, the corresponding concentrations in the complete scrubber liquor.




This suggests that  most of the scrubber  liquor's metals content was accounted  for in the



suspended solids fraction of the liquor.




        Special attention to the lead concentrations is warranted. Lead concentrations in bulk



scrubber liquor samples were in the 120 to 789 mg/L range for the fluff waste and soil feed tests.




These levels far exceed the regulatory level for lead of 5 mg/L. However, lead concentrations




in scrubber liquor TCLP leachates (scrubber liquor filtrate after removal of the suspended solids)




ranged from 0.08 to 2.2 mg/L over the fluff waste and soil feed tests, all below lead's regulatory



level.




4.6     PARTTCULATE AND HC1 EMISSIONS




        The baghouse  exit flue gas particulate and HC1 emission data developed in the test



program are  summarized in Table 4-20.   The  data show that baghouse exit particulate



concentrations were less  than 10 mg/dscm corrected to 7 percent O2 for all but one test for




which they were 14 mg/dscm at 7 percent O2.  All measured levels were well below the current
                                         4-37

-------
                                                        Baghouse exit
Test
Test 0 (10/27/93)
Fluff Waste Tests
Test 1 (11/9/93)
Test 2 (11/16/93)
Test 5 (11/18/93)
Test 6 (11/23/93)
Soil Feed Tests
Test 3 (12/1/93)
Test 4 (12/2/93)
Cl feedrate,
kg/hr
0.28

9.48
9.48
9.48
9.48

1.1
1.1
gJ"! 
Paniculate
concentration,
mg/dscm at 7%
2
7

7
4
6
14

5
9
HCI emission
rate, g/hr
<0.2

1.7
2.0
2.0
2.3

2.6
0.7
Apparent
system HCI
collection
efficiency, %
> 99.93

99.98
99.98
99.98
99.98

99.76
99.94
 hazardous waste incinerator performance standard of 180 mg/dscm at 7 percent O2, and even




 substantially below the EPA's announced 1993 guidance of 34 mg/dscm at 7 percent O2.




        Baghouse exit flue gas HCI emission rates were at most 2.6 g/hr.  Apparent system



 collection HCI efficiencies were greater than 99.9 percent for all except one soil feed test for



 which the apparent system HCI collection efficiency was 99.76 percent.




        Particle size distribution measurements were also performed for each test using an



 Andersen cascade impactor train in the afterburner extension.  The cascade impactor particle



 size distribution data analysis worksheets are presented in Appendix D-6. Figure 4-1 shows the




 size distribution data in the form of log-probability plot of cumulative mass percent less than




particle diameter (y-axis, probability scale) versus particle diameter (x-axis, log scale). A straight



line on such a plot corresponds to a log-normal size distribution.
                                          4-38

-------
              Cumulative percent less than size
          p
          en
                                     00

                                     (71
                                     CO
                                     09
                       CO
33

t
i
"
a
g'
a.
01
         ro
O.

CD

CO

N*
CD
         01
         ro
         o
to


0>
                               en
                                 CO
                 IV)
                                              tpl

-------
        The distribution data shown in Figure 4-1 indicate that the size distributions of the



afterburner exit particulate were comparable for 5 of the 6 tests, with the particulate for these



5 tests being relatively fine, with 50 percent less than 1 jim.  The distribution for Test 6 was



distinctly  shifted to much larger particle size, with over 90 percent greater than 1 ^m.  No



explanation for this shift is offered here.
                                           4-40

-------
                                     SECTION 5




                                   CONCLUSIONS








        Results of the test program conducted to evaluate the incineration treatment of fluff




waste  and contaminated soil from the M. W. Manufacturing Superfund site confirm that




incineration represents an effective treatment option, but several cautions regarding its use need




emphasis.  Indeed, incineration of  the fluff waste offers several benefits including substantial




waste volume reduction, and effective, near complete, decontamination and destruction of both




the VOC and SVOC contaminants in the waste. While  the volume reduction benefit is less




significant in the incineration treatment of the contaminated soil, the benefit of effective and




near complete decontamination and destruction of organic POHC contaminants remains.




        Both site materials can be incinerated in compliance with the current hazardous waste



incinerator performance standards in a rotary kiln incineration system of the type in place at the



IRF with an APCS consisting of a wet scrubber for acid gas control and a baghouse for final



particulate control. Specifically:




            Greater than 99.99 percent POHC DREs were uniformly measured




            HC1 emissions were well below 1.8 kg/hr and system HC1 control efficiencies well



             above 99 percent




In addition, compliance with the more recent incinerator emissions guidance announced in 1993



was demonstrated.  Specifically:
                                         5-1

-------
             Paniculate emissions measured were well below 34 mg/dscm corrected to



              7 percent O2




             Total PCDD/PCDF emissions measured were well below 30 ng/dscm corrected



              to 7 percent O2




 In fact, measured dioxin/furan emissions on a  TEQ basis  were well below the suggested



 European emission limit of 0.1 ng/Nm3 dry at 11  percent O2.




        However, the kiln ash discharge from the incineration of both site materials remains



 dioxin-contaminated. The kiln ash discharge from the incineration of contaminated site soil at




 a kiln temperature of nominally 870C (1,600F) contained total PCDD/PCDF concentrations




 of 2.4 to 3.6 /ig/kg.  Levels in the kiln ash discharge from the incineration of fluff waste at a




 nominal kiln temperature of 870C (1,600F) were higher, at 65 to 89 /ig/kg. Levels in the kiln



 ash  discharge from  the incineration of fluff waste at a nominal kiln temperature of 760C



 (1,400 F) were substantially higher, at 830 to 2,700 Mg/kg.




        Thus, with respect to  fluff waste, incineration  offers substantial volume  reduction,



 however the resulting treated waste discharge (kiln ash) may still need to be managed  as a




 dioxin-contaminated material. Dioxin contamination levels were decreased at higher incineration



 temperatures,  but  they remained significant nonetheless.  Perhaps even higher incineration



 temperatures,  with or without the use of an ash water quench system, would give a kiln ash




 discharge  relatively  free of dioxin  contamination.   However, further tests  are  needed  to



investigate this possibility.




        In addition, the flue gas particulate collected as baghouse ash in essentially all tests was



a cadmium- and lead-contaminated TC hazardous waste. Thus, this discharge would need to be



appropriately managed as a hazardous waste.
                                         5-2

-------
         All quality assurance (QA) objectives for the test program were met, with the exception
 of:
             The MDL objectives for:
                 Tetrachloroethene in solid residues
                 Trichloroethehe in aqueous liquids
                 2-nitrophenol in flue gas
                 Zinc in aqueous liquids
             The accuracy and precision objectives for antimony, barium, and silver as assessed
              by analyte recovery from MS samples and the RPD of MS/MSD analyses
             The accuracy objective for the other seven test trace metals as assessed by analyte
              recovery from MS samples
        The MDLs achieved for the above four analyte/sample matrix combinations were not
significantly greater than the respective objectives, so no measurable effects on test program
conclusions resulted.
        Failure  to meet the precision and accuracy objectives for the antimony, barium, and
silver analyses leads to the conclusion that test program results for these three  metals  are
compromised. The reported data for these three metals should be treated with caution, and test
program conclusions regarding these three metals must be viewed as tentative.
        The accuracy objective of 70 to 130 percent recovery from MS samples was not met for
the other seven test trace metals.  However, an objective of 60 to 140 percent recovery would
have been met.  This suggests that test program results and conclusions regarding these seven
analytes are valid and defensible, but are just not as certain as had been planned.
                                         5-3

-------
                                     SECTION 6

                                QUALITY ASSURANCE



        This test program was carried out as outlined in the Quality Assurance Project Plan

(QAPP) for Pilot-Scale Incineration Testing of Fluff Waste and Contaminated  Soil from the

M. W. Manufacturing Superfund Site. Thus, all QA aspects of the program were completed as

specified in the QAPP.   FJxcept  as noted, all tests were performed in accordance with the

procedures documented in the QAPP.

        All samples analyzed to obtain data reported in this report were taken at the IRF by

members of the IRF operating staff. All samples were collected and/or recovered in accordance

with the methods appropriate to  their eventual analysis.  After appropriate preservation, the

samples were  relinquished to  the custody  of the onsite Sample Custodian.  The  Sample

Custodian subsequently directed  the splitting  of samples and the transport of these to the

appropriate laboratories for analysis. The sample chain-of-custody procedures described in the

QAPP for these tests were followed.  No compromise in sample integrity occurred, with one

exception as noted below.

        Numerous  QA procedures were  followed to assess the data quality of laboratory
    9
analytical measurements performed in this test program. These included blank sample analyses,

duplicate analyses, and matrix spike (MS) and matrix spike duplicate (MSD) sample analyses.

Method blank  samples were analyzed for all sample matrices for which logical matrix blanks
                                         6-1

-------
 could  be prepared.   Results of QA procedures performed for the  critical laboratory



 measurements are discussed, by analyte group, in the following subsections.



 6.1     VOC ANALYSES




         A total of 50 solid and aqueous samples was  analyzed for VOCs by GC/FID using




 Method 8015A. Included in this group were 5 MS/MSD sample sets and 5 duplicate analyses




 of test samples. Table 6-1 lists sample collection date, analysis date, and analysis hold time for




 these samples. The data in Table 6-1 show that 49 of the 50 samples were analyzed within the




 method hold time limit of 14 days. Table 6-2 provides an analogous listing for flue gas samples




 analyzed for volatile organic constituents by GC/MS using Method 5040.  The data in Table 6-2




 show that 35 out of 36 samples were analyzed, and that'all of those analyzed were analyzed




 within the method hold time limit of 42 days.  One sample, the Test 3 field blank, was lost in




 shipment (the compromise in sample integrity mentioned above). Still, analytical completeness



 was 97 percent (35 of 36).




      (  Table 6-3 summarizes the VOC analysis quality assurance objectives  (QAOs) for



 precision, accuracy, and completeness.  Table 6-4 shows the method detection limit (MDL)



 objectives and the achieved values for the VOC analyses. As can be seen in Table 6-4 the MDL




 objective was met for all primary target analytes except tetrachloroethene in solid residues and



 trichloroethene in aqueous liquids. In addition, all secondary target analyte MDLs in flue gas



 samples were met.




        VOC analysis precision and accuracy were assessed for GC/FID analyses by preparing



one MS/MSD sample set for each of the fluff waste, contaminated soil, scrubber liquor, kiln ash,



and baghouse ash sample matrices and measuring spike recovery.  One pair of VOST traps was




spiked with the primary target analytes for each test and analyzed by GC/MS. In addition, one
                                         6-2

-------
TABLE 6-1. SAMPLE HOLD TIMES FOR THE VOC ANALYSES OF SOLID AND LIQUID
          SAMPLES BY GC/FID
Sample
Test Feed
Test 0
Composite fluff
Composite fluff duplicate
Composite fluff MS
Composite fluff MSB
Testl
Test 2
TestS
Test 6
TestS
Test 3 duplicate
Test 3 MS
Test 3 MSD
Test 4
Scrubber Liquor
Test 0 pretest
Test 0 post-test
Test 0 post-test duplicate
Test 0 post-test MS
Test 0 post-test MSD
Test 1 pretest
Test 1 post-test
Test 2 pretest
Test 2 post-test
Test 3 pretest
Test 3 post-test
Test 4 pretest
Test 4 post-test
Test 5 pretest
Test 5 post-test
Test 6 pretest
Test 6 post-test
Method Requirement
Collection date

12/21/93 
10/14/93
10/14/93
10/14/93
10/14/93
10/14/93
10/14/93
10/18/93
10/18/93
10/20/93
10/20/93
10/20/93
10/20/93
10/20/93

10/27/93
10/27/93
10/27/93
10/27/93
10/27/93
11/09/93
11/09/93
11/16/93
11/16/93
12/01/93
12/01/93
12/02/93
12/02/93
11/18/93
11/18/93
11/23/93
11/23/93

Analysis date

01/10/94
10/25/93
10/25/93
10/27/93
10/27/93
10/25/93
10/26/93
10/26/93
10/29/93
10/28/93
10/28/93
10/29/93
10/29/93
10/29/93

11/03/93
11/03/93
11/04/93
11/03/93
11/03/93
11/11/93
11/11/93
11/23/93
11/23/93
12/07/93
12/07/83
12/07/93
12/07/93
11/29/93
11/29/93
12/06/93
12/06/93

Analysis hold time, days

20
11
11
13
13
11
12
8
11
8
8
9
9
9

7
7
8
7
7
2
2
7
7
6
6
5
5
11
11
13
13
14
                                                           (continued)
                                 6-3

-------
TABLE 6-1.  (continued)
Sample
Kiln Ash
Test 1
Test 2
Test 3
Test 3 duplicate
Test 3 MS
Test 3 MSB
Test 4
TestS
Test 6
Baghouse Ash
TestO
Test 1
Test 2
Test3
Test 3 duplicate
Test 3 MS
Test 3 MSD
Test 4
TestS
Test 6
Method Requirement
Collection date

11/09/93
11/16/93
12/01/93
12/01/93
12/01/93
12/01/93
12/02/93
11/18/93
11/23/93

10/28/93
11/09/93
11/16/93
12/01/93
12/01/93
12/01/93
12/01/93
12/02/93
11/18/93
11/23/93

Analysis date

11/11/93
11/23/93
12/08/93
12/08/93
12/08/93
12/08/93
12/10/93
11/29/93
12/06/93

11/04/93
11/11/93
11/23/93
12/09/93
12/09/93
12/09/93
12/09/93
12/10/93
11/29/93
12/06/93

Analysis hold time, day:

2
7
7
7
7
7
8
11
13

7
2
7
8
8
8
8
8
11
13
14
        6-4

-------
TABLE 6-2. SAMPLE HOLD TIMES FOR THE VOC ANALYSES OF METHOD 0030
          SAMPLES BY GC/MS
Sample
Test 0, Set 1
Test 0, Set 2
Test 0, Set 3
Test 0, Field blank
Test 0, MS
Test 1, Set 1
Test 1, Set 2
Test 1, Set 3
Test 1, Field blank
Test 1, MS
Test 2, Set 1
Test 2, Set 2
Test 2, Set 3
Test 2, Field blank
Test 2 MS
Test 3, Set 1
Test 3, Set 2
Test 3, Set 3
Test 3, Field blank
Test 3, MS
Test 4, Set 1
Test 4, Set 2
Test 4, Set 3
Test 4, Field blank
Test 4, MS
Test 5, Set 1
Test 5, Set 2
Test 5, Set 3
Test 5, Field blank
Test 5, MS
Test 6, Set 1
Test 6, Set 2
Test 6, Set 3
Test 6, Field blank
Test 6, MS
Trip blank
Method Requirement
Collection date
10/27/93
10/27/93
10/27/93
10/27/93
10/27/93
11/09/93
11/09/93
11/09/93
11/09/93
11/09/93
11/16/93
11/16/93
11/16/93
11/16/93
11/16/93
12/01/93-
12/01/93
12/01/93
12/01/93
12/01/93
12/02/93
12/02/93
12/02/93
12/02/93
12/02/93
11/18/93
11/18/93
11/18/93
11/18/93
11/18/93
11/23/93
11/23/93
11/23/93
11/23/93 .
11/23/93
12/07/93

Analysis date
11/09/93
11/09/93
11/09/93
11/09/93
11/09/93
11/22/93
11/22/93
11/22/93
11/22/93
11/22/93
12/03/93
12/03/93
12/03/93
12/03/93
12/03/93
12/16/93
12/16/93
12/16/93
lost
12/16/93
12/17/93
12/17/93
12/16/93
12/16/93
12/16/93
12/08/93
12/08/93
12/08/93
12/03/93
12/03/93
12/16/93
12/16/93
12/16/93
12/16/93
12/16/93
12/16/93

Analysis hold time, days
12
12
12
12
12
13
13
13
13
13
17
17
17
17
17
15
15
15

15
15
15
14
14
14
20
20
20
15
15
23
23
23
23
23
9
42
                              6-5

-------
                                     TABLE 6=3. VOC MEASUREMENT QAOs
Measurement parameter
Volatile organic contaminants
in feed, and residue samples
Volatile organic contaminants
in flue gas sampling trains
Measurement/
analytical method
Purge and trap
GC/FID
Method 0030 sampling,
GC/MS analysis
Reference Conditions %
SW-846 Methanol extract
Method 801SA of solid samples
SW-846 -
Methods 5040
and 8240A
Precision, Accuracy, Completeness,
USD or RPD % %
50 52 to 157* 70
70 52 to 157* 70
   'Compound-specific criteria taken from Table 6, Method 8240A.
\

-------
   TABLE 6-4.  VOC MEASUREMENT MDLs: OBJECTIVES AND ACHIEVED LEVELS




                                                MDL objective
                          Solid residues, mg/kg Aqueous liquids, ng/L,  Flue gas, ng/dscm
Compound objective / achieved
Primary Target Analytes
Tetrachloroethene
1,1,2-Trichloroethane
Trichloroethene
Secondary Analytes
Acetone
Benzene
Bromodichloromethane
Carbon disulfide
Carbon tetrachloride
Chlorobenzene
Chlorodibromomethane
Chloroform
1,1-Dichlo'roethane
1,2-Dichloroethane
1,1-Dichloroethene
trans,l,2-Dichloroethene
1,2-Dichloropropane
cis-l,3-Dichloropropene
trans-l,3-Dichloropropene
Methylene chloride
Toluene
1,1,1-Trichloroethane
Trichlorofluoromethane

2/3.9
1/1
1/1

NA*
NA
NA
NA
NA
NA
NA
NA
NA
NA .
NA
NA
NA
NA
NA
NA
NA
NA
NA
objective / achieved

20 / 4.1
10 / 3.9
10 / 15.4

NA.
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA '
NA
NA
NA
NA
NA
objective / achieven

2 / 0.05
1 / 0.14
1 / 0.05

2 / 0.05
2/0.23
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.09
2/0.23
2 / 0.05
2 / 0.05
   "NA = Not applicable; analyte not measured in this matrix.







MS/MSD  VOST sample set (two pairs of VOST traps) was spiked with the full set of VOC



analytes listed in Table 3-7.




        Table 6-5  summarizes VOC recoveries achieved from solid  and liquid MS samples



analyzed by GC/FEX The data in Table 6-5 show 29 out of 30 measurements, or 97 percent,




were within the compound-specific recovery range. As the completeness QAO was 70 percent
                                        6-7

-------
      TABLE 6-5. VOC RECOVERIES FROM MS SAMPLES ANALYZED BY GC/FID
                                        Spike recovery, %
Sample
Test Feed
Composite fluff MS
Composite fluff MSD
RPD, %
Test 3 soil MS
Test 3 soil MSD
RPD, %
Post-test Scrubber Liquor
Test 0 MS
Test 0 MSD
RPD, %
Kiln Ash
Test 3 MS
Test 3 MSD
RPD, %
Baghouse Ash
Test 3 MS
Test 3 MSD
RPD, %
Accuracy QAO
Tetrachloroethene

91.1
95.4
4.6
125
155
21.4

102
101
1.0

88.8
87.0
2.0

94.7
97.8
3.2
64-148
1,1,2-TrichIoroe thane

90.6
94.0
3.7
102
98.8
3.2

101
100
1.0

87.1
87,1
0

85.4
99.8
15.6
52-150
Trichloroethene

90.7
94.8
4.4
102
99.6
2.4

104
102
1.9

90.7
91.1
0.4

100
102
2.0
71-157
Precision
QAO, RPD

50
50

50

50

50

for this measurement,  the accuracy QAO, as measured by spike recovery from MS/MSD



samples, was met.




       The data in Table 6-5 also show that all 15 duplicate measurements were within the




precision QAO of 50 percent RPD.  Thus, the VOC measurement precision QAO for the



GC/FID analyses, as measured by MS/MSD sample analyses, was met.




       Table 6-6 summarizes the VOC spike recoveries from the VOST trap MS/MSD sample



analyses by GC/MS. The data in Table 6-6 show that 53 out of 61 measurements, or 87 percent,




were within the  compound-specific  recovery ranges.   The  completeness QAO for this




                                      6-8

-------
TABLE 6-6. VOC RECOVERIES FROM MS SAMPLES


analytes Test 0
Trichloroethene 97
1,1,2-trichloroethane 51
Tetrachloroethene 85

Secondary analytes
Trichlorofluoromethane
1,1-Dichloroethene
Methylene chloride
trans- 1,2-Dichloroethene
1,1-Dichloroethane
Chloroform
1,2-Dichloroethane
1,1,1-Trichloroethane
Carbon tetrachloride
Benzene
Trichloroethene
1,2-Dichloropropane
Bromodichloromethane
cis-l,3-Dichloropropene
trans- 1,3-Dichloropropene
1,1,2-Trichloroethane
Dibromobhloromethane
Toluene
Tetrachloroethene
Chlorobenzene
Precision QAO, RPD


Testl
99
68
94

MS
82.6
922
97.6
882
75.0
71.8
87.8
66.8
72.6
97.4
762
80.4
84.6
78.2
812
72.6
78.6
87.6
71.0
77.2

^n tie A rpcfvv&'rv
W^IUW * VVUTCl. J]
Test 2 Test 3 Test
102 50 62
74 48 63
91 58 74
Spike recovery, %
MSD
69.4
88.8
1082
85.4
82.6
832
80.8
71.0
76.2
76.2
702
742
762
612
37.6
64.6
68.8
127
64.8
68.0

ANALYZED BY GC/MS

w
4 Test 6
66
52
51

QAO*
17-181
59-155
D-221
54-156
59-155
51-138
49-155
52-162
70-140
37.151
71-157
D-210
35-155
D-227
17-183
52-150
53-149
47-150
64-148
37-160



Test 6 QAO*
73 71-157
64 52-150
86 64-148

RPD, %
17.4
3.8
103
32
9.6
14.7 .
83
6.1
4.8
24.4
8.2
8.0
10.4
24.4
73.4
11.7
133
37.0
9.1
12.7
70
     'Compound-specific criteria taken from Table 6, Method 8240A; D denotes detected.







measurement was 70 percent; therefore, the accuracy QAO, as measured by spike recovery, was




met. The data in Table 6-6 also show that 19 out of 20 RPD measurements, or 95 percent, were



within the precision QAO of 70 percent RPD. Therefore, the VOC measurement precision



QAO for the GC/MS analyses, as measured by MS/MSD sample analyses, was met.
                                        6-9

-------
        One sample from each of the fluff feed, soil feed, kiln ash, baghouse ash, and post-test



scrubber liquor matrices was analyzed in duplicate as a further check on measurement precision.




Neither of the kiln ash,  baghouse ash,  or  scrubber liquor duplicate samples contained any




detectable volatile organic target analytes, so no precision information was obtained from these




analyses.  Table 6-7 summarizes the duplicate sample analysis results for the two test feed




matrices. All precision measurements shown met the precision QAO of 50 percent RPD.




        Table 6-8 summarizes the method surrogate recoveries achieved in the GC/FED analyses



of test samples. Table 6-9 presents an analogous summary for the GC/MS analyses. The data




in Table 6-8 show that 95 out of 100, or 95 percent, of the surrogate recoveries were within the




surrogate-specific accuracy QAO range.  The data in Table 6-9 show that 105 out of 140, or




75 percent, of the surrogate recoveries were within the surrogate-specific accuracy QAO range.




Because the completeness QAO was 70 percent for this measurement, the accuracy QAO, as




measured by surrogate recovery, was met for both the GC/FID and the GC/MS analyses.








             TABLE 6-7. DUPLICATE SAMPLE VOC ANALYSIS RESULTS
Concentration
Sample
Test Feed, mg/kg
Composite fluff
Tetrachloroethene
1, 1,2-Trichloroethane
Trichloroethene
Test 3 soil
Tetrachloroethene
1, 1,2-Trichloroethane
Trichloroethene
Precision QAO, RPD
Analysis


4.8
1.2

50
2.7

Duplicate analysis


<4

50
2.7

RPD,%


18
0
18

0
0
0
50
                                         6-10

-------
TABLE 6-8. VOC SURROGATE RECOVERIES IN THE GC/FID ANALYSIS OF TEST
         SAMPLES
Sample
Test Feed
TestO
Composite fluff
Composite fluff duplicate
Composite fluff MS
Composite fluff MSD
Testl
Test 2
TestS
Test 6
Test 3
Test 3 duplicate
Test 3 MS
Test 3 MSD
Test 4

Scrubber Liquor

Test 0 pretest
Test 0 post-test
Test 0 post-test duplicate
Test 0 post-test MS
Test 0 post-test MSD
 Test 1 pretest
Test 1 post-test
Test 2 pretest
Test 2 post-test
Test 3 pretest
Test 3 post-test
Test 4 pretest
Test 4 post-test
Test 5 pretest
Test 5 post-test
Test 6 pretest
Test 6 post-test
Recovery QAO
Surrogate
1,1,1-
Trichloro-
ethane

97.5
93.6
672
81.9
82.1
86.4'
134
118
140
703
72.9
77.7
73.5
71.0



91.6
84.6
893
89.9
91.6
94.1
92.5
90.4
92.4
89.1
87.4
833
87.9
87.7
863
88.5
88.4
52-162
recovery, %
4-Bromo-
fluorobenzene

113
972
115
125
120
82.1
141
123,
150
85.2
85.7
87.0
90.7
94.5



105
96.7
101
103
106
104
106
103
109
102
100
93.0
100
101
97.9
103
100
74-121
Sample
Kiln Ash
Testl
Test 2
Test3
Test 3 duplicate
Test 3 MS
Test 3 MSD
Test 4
Test5
Test 6


Baghouse Ash

TestO
Testl
Test 2
Test3
Test 3 duplicate
Test 3 MS
Test 3 MSD
Test 4
TestS
Test 6











Recovery QAO
Surrogate
1,1,1-
Trichloro-
ethane

87.7
94.4
702
793
76.4
73.0
80.2
925
90.0




93.7
93.8
86.7
78.1
812
76.4
78.7
90.4
92.1
90.4











52-162
recovery, %
4-Bromo-
fluorobenzene

98.4
99.6
83.4
88.9
86.7
83.4
92.9
73.0
93.6




105
104
106
103
105
96.9
102
105
107
107











74-121
                             6-11

-------
TABLE 6-9. VOC SURROGATE RECOVERIES IN THE GC/MS ANALYSIS OF
         METHOD 0030 SAMPLES
Surrogate recovery, %
Sample l,2-Dichloroethane-d4 Toluene-d8 Benzene-d
TestO
Setl
Set 2
SetS
Field blank
MS
Testl
Set 1
Set 2
SetS
Field blank
MS
Test 2
Setl
Set 2
SetS
Field blank
MS
Tests
Setl
Set 2
SetS
Field blank
MS
Test 4
Setl
Set 2
SetS
Field blank
MS
Test 5
Setl
Set 2
SetS
Field blank
MS
Test 6
Setl
Set 2
SetS
Field blank
MS
Trip blank
Recovery QAO

98
98
99
96
101

128
128
115
111
119

20
104
100
108
104

175
256
134


126

128
127
131
131
128

118
126
108
98
111

128
122
123
131
121
135
70-121

90
88
89
98
97

84
88
93
104
98

80
121
105
98
106

90
90
98


102

97
97
98
101
103

88
85
97
97
105

98
100
100
100
105
103
81-117

84
89
64
65
57

96
96
98
100
99

96
107
130
116
119

118
127
108
Lo"t

107

109
109
108
108
108

91
94
88
110
132

110
106
105
108
113
105
74-121
4-Bromofl uorobenzene

92
61
61
62
45

90
65
85
84
76

152
94
93
80
109

168
204
86


75

72
83
56
94
82

49
48
53
76
68

101
57
62
64
94
46
74-121
                           6-12

-------
 6.2    SVOC ANALYSES




        A total of 101 samples was analyzed for SVOCs. Included in this group were 17 method



 blanks, 1 field blank, 7 MS/MSD sample sets, 3 sets of duplicate  test samples, and 6 sets of




 replicate feed samples. Table 6-10 lists the sample collection date, extraction date, analysis date,




 and analysis hold time for these samples.  As shown in Table 6-10, 89  of 101 samples, or



 88 percent were extracted within the specified method extraction hold time.  The data also show



 that all sample extracts were analyzed within the analysis hold time specified by the method.




        Table 6-11 summarizes the SVOC measurement  QAOs for  precision, accuracy, and




 completeness.  Table 6-12 lists the MDL objectives and the levels achieved. As can be seen in




 Table 6-12, the MDL objective was achieved for all of the analytes except 2-nitrophenol in flue




 gas, a secondary analyte.   SVOC  measurement precision and accuracy were assessed by




 preparing two  MS/MSD sample sets for the test feed (one set for each feed type) and kiln ash




 matrices, and one MS/MSD sample set for the baghouse ash, scrubber liquor, and Method 0010




 train matrices.  Table 6-13 summarizes the spike recovery data obtained for solid  and  liquid




 samples.  Table 6-14 presents an analogous summary for Method 0010 train samples.




        The data in Table 6-13  show that all achieved spike recoveries were within  the




 compound-specific recovery objective ranges.  Thus, the measurement accuracy QAO, as



 measured by spike recovery from solid and liquid samples, was met.  Table 6-13 also shows that




 all 12 RPD measurements for MS/MSD analyses were within the precision QAO of 50 percent



 RPD. Thus, the SVOC measurement precision QAO, as measured by solid and liquid MS/MSD



 sample analyses, was also met.




       The data in Table  6-14 show that all 112 spike recovery measurements from Method




0010 train samples were within the compound-specific recovery objective  ranges!  Thus, the




measurement accuracy QAO, as measured by spike recovery, was met. Table 6-14 also shows
                                        6-13

-------
TABLE 6-10. SAMPLE HOLD TIMES FOR THE SVOC ANALYSES BY GC/MS


Sample
Test 1 Feed
Extract 1
Extract 2
Extract 3
Extract 4
Extract 5
MS
MSD
Test 2 Feed
Extract 1
Extract 2
Extract 3
Extract 4
Extract 5
Test 3 Feed
Extract 1
Extract 2
Extracts
Extract 4
Extracts
MS
MSD
Test 4 Feed
Extract 1
Extract 2
Extracts
Extract 4
Extract 5
Test 5 Feed
Extract 1
Extract 2
Extract 3
Extract 4
Extract 5
Method Requirement

Collection
date

10/14/93
10/14/93
10/14/93
10/14/93
10/14/93
10/15/93
10/15/93

10/15/93
10/15/93
10/15/93
10/15/93
10/15/93

10/20/93^
10/20/93
10/20/93
10/20/93
10/20/93
10/20/93
10/20/93

10/20/93
10/20/93
10/20/93
10/20/93
10/20/93

10/18/93
10/18/93
10/18/93
10/18/93
10/18/93


Extraction
date

10/26/93
10/26/93
10/26/93
10/26/93
10/26/93
11/05/93
11/05/93

10/27/93
10/27/93
10/27/93
10/27/93
10/27/93

11/04/93
11/04/93
11/04/93
11/04/93
11/04/93
11/05/93
11/05/93

11/03/93
11/03/93
11/03/93
11/03/93
11/03/93

10/28/93
10/28/93
10/28/93
10/28/93
10/28/93

Extraction
hold time,
days

12
12
12
12
12
21
21

12
12
12
12
12

15
15
15
15
15
16
16

14
14
14
14
14

10
10
10
10
10
14

Analysis
date

11/19/93
11/19/93
11/19/93
11/19/93
11/19/93
12/10/93
12/10/93

11/21/93
11/21/93
11/21/93
11/21/93
11/21/93

12/06/93
12/06/93
12/06/93
12/07/93
12/07/93
12/10/93
12/10/93

12/07/93
12/07/93
12/07/93
12/07/93
12/07/93

11/21/93
11/21/93
11/21/93
11/22/93
11/22/93

Analysis
hold time,
days

24
24
24
24
24
35
35

25
25
25
26
26

32
32
32
33
33
35
35

34
34
34
34
34

24
24
24
25
25
40
(continued)
                             6-14

-------
TABLE 6-10.  (continued)


Sample
Test 6 Feed
Extract 1
Extract 2
Extract 3
Extract 4
Extract 5
Feed Packaging Container
Material (Test 0)
Sample 1
Sample 2
Feed Method Blanks
Blank 1
Blank 2
Blank3
Kiln Ash
Test 1
Test 2
Test 3
Test 3 duplicate
Test 3 MS
Test 3 MSD
Test 4
TestS
Test 6
Test 6 MS
Test 6 MSD
Baghouse Ash
TestO
Test 1
Test 2
Test 3
Test 3 duplicate
Test 4
TestS
Test 6
Test 6 MS
Test 6 MSD
Method Requirement

Collection
date

10/18/93
10/18/93
10/18/93
10/18/93
10/18/93


12/21/93
12/31/93

10/21/93
11/02/93
11/03/93

11/09/93
11/16/93
12/01/93
12/01/93
12/01/93
12/01/93
12/02/93
11/18/93
11/23/93
11/23/93
11/23/93

10/28/93
11/10/93
11/16/93
12/01/93
12/01/93
12/02/93
11/18/93
11/23/93
11/23/93
11/23/93


Extraction
date

10/29/93
10/29/93
10/29/93
10/29/93
10/29/93


01/05/94
01/05/94

10/22/93
11/03/93
11/04/93

11/16/93
11/18/93
12/03/93
12/08/93
12/07/93
12/07/93
12/08/93
11/24/93
12/01/93
12/09/93
12/09/93

11/09/93
11/16/93
11/18/93
12/03/93
12/08/93
12/08/93
11/24/93
12/01/93
12/07/93
12/07/93

Extraction
hold time,
days

11
11
11
11
11


15
5

1
1
1

7
2
2
7
6
6
6
6
8
15
15

12
6
2
2
7
6
6
8
14
14
14

Analysis
date

11/21/93
11/22/93
11/22/93
11/22/93
11/23/93


01/13/94
01/13/94

11/21/93
12/09/93
12/10/93

12/17/93
12/21/93
01/07/94
01/10/94
01/07/94
01/07/94
01/10/94
12/23/93
01/06/94
01/10/04
01/10/94

12/16/93
12/17/93
12/21/93
01/07/94
01/10/94
01/10/94
12/23/93
01/06/94
01/07/94
01/07/94

Analysis
hold time,
days

23
24
24
24
25


8
8

30
36
36

31
33
35
33
31
31
33
29
36
32
32

37
31
33
35
33
33
29
36
31
31 .
40
(continued)
          6-15

-------
TABLE 6-10.  (continued)


Sample
Ash Method Blanks
Blank 1
Blank 2
Blank 3
Blank 4
Blanks
Blank 6
Blank?
Blanks
Scrubber Liquor
Test 0 pretest
Test 0 post-test
Test 1 pretest
Test 1 post-test
Test 2 pretest
Test 2 post-test
Test 3 pretest
Test 3 post-test
Test 3 post-test duplicate
Test 4 pretest
Test 4 post-test
Test 4 MS
Test4MSD
Test 5 pretest
Test 5 post-test
Test 6 pretest
Test 6 post-test
Scrubber Liquor Method Blanks
Blank 1
Blank 2
Blank 3
Blank 4
Blanks
Method Requirement

Collection
date

11/08/93
11/15/93
11/17/93
11/23/93
11/30/93
12/02/93
12/07/93
12/08/93

10/27/93
10/27/93
11/09/93
11/09/93
11/16/93
11/16/93
12/01/93
12/01/93
12/01/93
12/02/93
12/02/93
12/02/93
12/02/93
11/18/93
11/18/93
11/23/93
11/23/93

11/01/93
11/15/93
11/22/93
11/29/93
12/09/93


Extraction
date

11/09/93
11/16/93
11/18/93
11/24/93
12/01/93
12/03/93
12/08/93
12/09/93

11/02/93
11/02/93
11/16/93
11/16/93
11/22/93
11/22/93
12/09/93
12/09/93
12/09/93
12/09/93
12/09/93
12/10/93
12/10/93
11/22/93
11/22/93
11/30/93
11/30/93

11/02/93
11/16/93
11/22/93
11/30/93
12/10/93

Extraction
hold time,
days

1
1
1
1
1
1
1
1

6
6
7
7
6
6
8
8
8
7
7
8
8
4
4
7
7

1
1
0
1
1
14

Analysis
date

12/10/93
12/21/93
12/21/93
12/23/93
01/06/94
01/07/94
01/10/94
01/10/94

12/09/93
12/09/93
12/17/93
12/17/93
12/21/93
12/21/93
01/11/94
01/11/94
01/11/94
01/11/94
01/11/94
01/11/94
01/11/94
12/23/93
12/23/93
12/23/93
12/23/93

12/09/93
12/21/93
12/23/93
12/23/93
01/11/94

Analysis
hold time,
days

31
35
33
29
36
34
32
31

37
37
31
31
29
29
33
33
33
33
33
32
32
31
31
23
23

37
35
31
23
31
40
(continued)
        6-16

-------
TABLE 6-10.  (continued)
Sample
Method 0010 Train
TestO
Test 1
Test 2
Test 3
Test 4
TestS
Test 6
Method blank
Held blank
Blank spike
Blank spike duplicate
Method Requirement
Collection
date

10/27/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
11/02/93
12/01/93
12/08/93
12/08/93

Extraction
date

10/28/93
11/10/93
11/17/93
12/02/93
12/03/93
11/19/93
11/24/93
11/03/93
12/02/93
12/09/93
12/09/93

Extraction
hold time,
days

1
1
1
1
1
1
1
1
1
1
1
14
Analysis
date

11/24/93
11/24/93
12/20/93
12/20/93
01/07/94
12/21/93
12/23/93
12/10/93
01/07/94
01/10/94
01/10/94

Analysis
hold time,
days

27
14
33
35
35
32
29
37
35
31
31
40
        6-17

-------
o\
>-
00
                                          TABLE 6-ii. SVOC MEASUREMENT QAOs
                                   Measurement/                                     Precision,     Accuracy,  Completeness,
         Measurement parameter    analytical method	Reference	Conditions  % RSD or RPD     %          %

       Semivolatile organic           Extraction,              SW-846         Methylene        50         D-262'        70
       contaminants in feed, residue,   concentration,      Methods 0010, 3520A,   chloride
       and flue gas samples          GC/MS             3540A, and 8270A    extraction      	

       'Compound-specific criteria taken from Table 6, Method 8270A.

-------
 TABLE 6-12.  SVOC MEASUREMENT MDLs: OBJECTIVES AND ACHIEVED LEVELS
MDL objective
Solid residues, mg/kg
Compound
Primary Target Analytes
Naphthalene
Bis(2-ethylhexyl)phthalate
Di-n-octylphthalate
Objective

2
2
2
Achieved

03
13
0.4
Aqueous liquids, /ig//L
Objective Achieved

20 3.1
20 13
20 3.8
Flue gas, pg/dscm
Compound
Secondary Analytes1
Phenol
Bis(2-chloroethyl)ether
2-Chlorophenol
13-Dichlorobenzene
1,4-Dichlorobenzene
1,2-Dichlorobenzene
Bis(2-chloroisopropyl)ether
N-nitroso-di-n-propylamine
Hexachloroethane
Nitrobenzene
Isophorone
2-Nitrophenol
2,4-Dimethylphenol
Bis(2-chloroethoxy)methane
2,4-Dichlorophenol
1,2,4-Trichlorobenzene
Hexachlorobutadiene
4-Chloro-3-methylphenol
2-Methylnaphthalene
2,4,6-Trichlorophenol
2,4,5-Trichlorophenol
2-Chloronaphthalene
Dimethylphthalate
Acenaphthylene
2,6-Dinitrotoluene
Acenaphthene
Objective

10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
Achieved

4.5
13
7.1
1.5
. 1-8
13
1.0
1.6'
13
, 23
1.4
13.9
1.5
4.9
73
1.8
0.9
5.8
1.0
7.9
73
0.7
0.4
23
13
1.8
Compound
. Secondary Analytes"
2,4-Dinitrophenol
4-Nitrophenol
Dibenzofuran
2,4-Dinitrotoluene
Diethylphthalate
Huorene
4-Chlorophenylphenylether
4,6rDinitro-2-methylphenol
N-nitrosodiphenylamine
4-Bromophenylphenylether
Hexachlorobenzene
Pentachlorophenol
Phenanthrene
Anthracene
Di-n-butylphthalate
Ruoranthene
Pyrene
Butylbenzylphthalate
Benzo(a)anthracene
Chrysene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(a)pyrene
Indeno(l,23-cd)pyrene
Dibenz(a,h)anthracene
Benzo(ghi)perylene
Flue gas,
Objective

10
10
10
Flue gas,
Objective

10
10
10
10
10
' 10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
Hg/dscta
Achieved

OS
33
12
pg/dscm
Achieved

33
2.5
2.1
3.9
1.7
13
1.5
2.8
43
0.7
0.6
1.7
0.7
0.8
53
0.4
13
6.7
0.5
0.7
0.7
0.8
0.7
12
13
0.9
Measurement not performed on solid and liquid matrices.
                                   6-19

-------
     TABLE 6-13. SVOC RECOVERIES FROM SOLID AND LIQUID MS SAMPLES
                 ANALYZED BY GC/MS
Sample
Test 1 Feed8
MS
MSD
RPD, %
Test 3 Feed"
MS
MSD
RPD,%
Test 3 Kiln Ash
MS
MSD
RPD, %
Test 6 Kiln Ash
MS
MSD
RPD,%
Test 6 Baghouse Ashc
MS
MSD
RPD, %
Test 4 Scrubber Liquor
MS
MSD
RPD, %
Accuracy QAO
Spike
Naphthalene

88.0
83.5
5.2

86.9
88.7
2.1

88.1
93.9
6.4

78.8
90.3
13.6

91.6
85.3
7.1

85.7
86.2
0.6
21-133
recovery, %
BEHP

NSb
NS


NS
NS


81.8
90.3
9.9

71.0
83.5
16.2

ISd
IS


74.0
59.9
21.1
8-158

DNOP Precision QAO, RPD

NS
NS
- 50

NS
NS
- 50

81.3
87.2
7.0 50

79.3
91.0
13.7 50

IS
IS
 50

80.7
72.3
11.0 50
4-146
aThe amount of phthalates in the fluff and soil feed exceeded 1 percent therefore spiking
 was not required.
bNS = Not spiked.
cThe phthalate spiking levels were insignificant compared to the native amount found in
 the baghouse ash.
 IS = Insufficient spike.
                                     6-20

-------
TABLE 6-14. SVOC RECOVERIES FROM THE METHOD 0010 MS SAMPLES
           ANALYZED BY GC/MS
Spike recovery, %
Compound
Phenol
Bis(2-chloroethyl)ether
2-Chlorophenol
1,3-Dichlorobenzene
1,4-Dichlorobenzene
1,2-Dichlorobenzene
Bis(2-chloroisopropyl)ether
N-Nitroso-di-n-propylamine
Hexachloroethane
Nitrobenzene
Isophorone
2-Nitrophenol
2,4-Dimethylphenol
Bis(2-chloroethoxy)methane
2,4-Dichlorophenol
1,2,4-Trichlorobenzene
Naphthalene
Hexachlorobutadiene
4-Chloro-3-methylphenol
2-Methylnaphthalene
2,4,6-Trichlorophenol
2,4,5-Trichlorophenol
2-Chloronapthalene
Dimethylphthalate
Acenapthylene
2,6-Dinitrotoluene
Acenaphthene
2,4-Dinitrophenol
4-Nitrophenol
Dibenzofuran
2,4-Dinitrotoluene
Diethylphthalate
Fluorene
4-Chlorophenylphenylether
4,6-Dinitro-2-methylphenol
Precision QAO, RPD
MS
75.6
84.6
83.5
84.4
87.0
83.7
70.2
89.2
84.5
89.3
86.8
88.5
37.2
84.3
87.3
95.2
90.2
96.3
93.2
88.4
87.2
95.8
85.2
85.7
80.7
89.7
89.5
64.1
80.9
83.5
89.3
84.5
82.1
88.2
69.4

MSD
82.3
88.2
88.2
85.3
87.8
90.4
74.9
96.6
82.3
88.9
88.9
90.0
52.8
87.5
93.5
92.1
87.8
95.1
102
91.6
103
101
93.6
96.3
88.6
101
95.1
87.2
91.5
94.0
103
94.8
91.7
98.3
87.5

QAO
5-112
12-158
23-134
D-172
20-124
32-129
36-166
D-230
40-113
35-180
21-196
29-182
32-119
33-184
39-135
44-142
21-133
24-116
22-147
21-133
37-144
37-144
60-118
D-112
33-145
50-158
47-145
D-191
D-132
27-133
39-139
D-114
59-121
25-158
D-181

RPD
8.5
4.2
5.5
1.1
0.9
7.7
6.5
8.0
2.6
0.5
2.4
1.7
34.7
3.7
6.9
3.3
2.7
1.3
9.0
3.6
16.6
5.3
9.4
11.7
9.3
11.9
6.0
30.5
12.3
1.8
14.3
11.5
11.1
10.8
23.1
50
                            6-21
                                                    (continued)

-------
                                TABLE 6-14. (continued)
Spike recovery, %
Compound
N-Nitrosodiphenylamine
4-Bromophenylphenylether
Hexachlorobenzene
Pentachlorophenol
Phenanthrene
Anthracene
Di-n-butylphthalate
Fluoranthene
Pyrene
Butylbenzylphthalate
Benzo(a)anthracene
3,3-Dichlorobenzidine
Chrysene
Bis(2-ethylhexyl)phthalate
Di-n-octylphthalate
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(a)pyrene
Indeno(l,2,3-cd)pyrene
Dibenzo(a,h)anthracene
Benzo(g,h,i)perylene
Precision QAO, RPD
MS
86.0
97.0
103
104
91.2
89.4
89.7
92.2
82.2
76.9
86.3
79.6
87.0
86.8
82.6
85.5
80.4
79.4
49.6
82.2
83.4

MSD
93.8
106
109
114
97.5
96.4
95.4
96.7
90.6
82.6
94.9
94.6
96.2
93.0
91.7
94.5
87.6
84.8
83.8
80.9
82.7

QAO
D-230
53-127
D-152
14-176
54-120
27-133
1-118
26-137
52-115
D-152
33-143
D-262
17-168
8-158
4-146
24-159
11-162
17-163
D-171
D-227
D-219

RPD
8.7
8.9
5.7
9.2
6.7
7.5
6.2
4.8
9.7
7.2
9.5
17.2
10.0
6.9
10.4
10.0
8.6
6.8
51.3
1.6
0.8
50
that 55 of 56 RPD determinations from MS/MSD sample analyses, or 98 percent, were within



the precision QAO of 50 percent RPD. As the completeness QAO for this measurement was



70 percent, the precision QAO for the Method 0010 train SVOC analyses, as measured by the



RPD of MS/MSD sample analyses, was met.




       All samples extracted for SVOC analyses were spiked with method surrogates prior to



extraction, and surrogate recoveries were measured.  Table 6-15 summarizes the surrogate




recoveries achieved for solid and liquid samples. Table 6-16 provides an analogous summary for



flue  gas  samples.  The data in Table 6-15 show that 154  out of  159  surrogate recovery




                                        6-22

-------
TABLE 6-15. SVOC SURROGATE RECOVERIES IN THE GC/MS ANALYSIS OF SOLID
            AND LIQUID SAMPLES
Surrogate recovery, %
Sample
Feed Packaging Container Material
Sample 1
Sample 2
Kiln Ash
Testl
Test 2
TestS
Test 3 duplicate
Test 3 MS
Test 3 MSD
Test 4
TestS
Test 6
Test 6 MS
Test 6 MSD
Baghouse Ash
Test 0
Testl
Test 2
Test 3
Test 3 duplicate
Test 4
Test 5
Test 6
Test 6 MS
Test 6 MSD
Ash Method Blanks
Blank 1
Blank 2
Blank3
Blank 4
Blanks
Blank 6
Blank?
Blanks
Solid Sample Recovery QAO*
Nitrobenzene-dj

79
73

72
77
85
74
83
90
89
74
81
72
82

85
81
80
127
79
81
82
89
87
81

78
80
88
76
72
90
78
74
23-120
2-Fluorobiphenyl

71
67

77
83
80
76
79
84
92
75
83
77
79

85
82
85
112
78
80
87
84
79
73

82
85
91
78
73
85
83
67
30-115
4-Terphenyl-d14

100
116

82
94
84
79
77
86
92
76
86
75
84

95
88
91
120
81
81
94
86
93
77

86
95
98
95
84
89
82
78
18-137
   *Compound-specific criteria taken from Table 8 of Method 8270A.
                                     6-23
(continued)

-------
TABLE 6-15. (continued)
Sample
Scrubber Liquor
Test 0 pretest
Test 0 post-test
Test 1 pretest
Test 1 post-test
Test 2 pretest
Test 2 post-test
Test 3 pretest
Test 3 post-test
Test 3 post-test duplicate
Test 4 pretest
Test 4 post-test
Test 4 post-test MS
Test 4 post-test MSD
Test 5 pretest
Test 5 post-test
Test 6 pretest
Test 6 post-test
Scrubber Liquor Method Blanks
Blank 1
Blank 2
Blanks
Blank 4
Blanks
Liquid Sample Recovery QAO"

Nitrobenzene-dj

76
74
20
79
75
67
65
68
84
80
67
82
82
72
55
 84
74

79
77
79
84
82
35-114
Surrogate recovery, 9
2-Fluorobiphenyl

63
69
19
89
74
69
71
68
79
81
71
83
82
72
66
73
63

83
76
76
81
81
43-116
fe
4-Terphenyl-dM

82
84
25
108
97
89
84
83
86
82
83
83
82
89
92
95
86

85
96
93
91
79
33-141
"Compound-specific criteria taken from Table 8 of Method 8270A.
                                      6-24

-------
K
   TABLE 6-16. SVOC SURROGATE RECOVERIES IN THE GC/MS ANALYSIS OF METHOD 0010 FLUE GAS SAMPLES
                                                     Surrogate recovery, %
Sample
TestO
Testl
Test 2
Test3
Test 4
TestS
Test 6
Method blank
Field blank
Blank spike
Blank spike duplicate
Recovery QAO
2-Fluoro-
phenol
57
36
40
74
74
66
70
71
69
84
88
21-100
Phenol-d<
43
25
35
75
75
57
64
73
70
89
95
10-94
Nitro-
benzene-d$
76
72
81
90
90
86
76
69
86
120
121
35-114
2-Fluoro-
biphenyl
76
64
82
89
79
87
74
71
82
106
115
43-116
2,4,6-Tribromo-
phenol
80
61
78
85
78
83
84
92
84
119
' 125
10-123
4-Terphenyl-d,,
78
69
91
93
83
101
83
78
83
108
118
33-141
Octafluoro-
biphenyl
87
73
55
103
98
95
102
NS'
NS
NS
NS
30-115*
9-PhenyI-
anthracene
86
84
106
115
110
102
96
NS
NS
NS
NS
18-137*
-S=S=S==
      NS = Not spiked.
      "Recovery QAO the same as for 2-fluorobiphenyl.
      "Recovery QAO the same as for 4-terphenyl-d14.

-------
 measurements, or 97 percent, were within  the  surrogate-specific recovery objective range.



 Because the completeness QAO was 70 percent for this measurement, the accuracy QAO, as



 measured by surrogate recovery, was met.for solid and liquid samples.




        Table 6-16 summarizes surrogate recoveries achieved for flue gas samples. The data in



 Table 6-16 show that 76 out of 80 surrogate recovery measurements, or 95 percent, were within



 the surrogate-specific recovery objective range.  Again, because the completeness QAO for this




 measurement was 70 percent, the accuracy QAO, as measured by surrogate recovery from the



 flue gas samples, was met.




        One kiln ash, one baghouse ash, and one post-test scrubber liquor sample were analyzed




 in duplicate as a further measure of analysis precision.  The target SVOC analytes were not




 detected in either duplicate kiln ash or baghouse ash sample, so no precision information was




 obtained via this procedure. Both BEHP and DNOP were found in both duplicate baghouse ash




 samples. The RPDs from the duplicate analyses were 37 percent for BEHP and 47 percent for




 DNOP. Both measurements met the precision QAO of 50 percent RPD.




        As discussed in Section 4, five replicates of each fluff waste sample were analyzed for




 BEHP.  The percent RSDs of the five analyses ranged from 6 to 25 percent, all within the



 precision QAO of 50 percent RSD.  In addition, five replicates of each soil feed sample were



 analyzed for BEHP, DNOP, and naphthalene. Naphthalene was not detected in any soil feed



 replicate analysis at an MDL of 25 mg/kg. The percent RSDs of the replicate sample analyses




were 33 and 28 percent, for BEHP, and 49 and 30 percent, for DNOP. All met the precision



 QAO for the measurement of 50 percent RSD.



 63     TRACE METAL ANALYSES




       A total of 139 samples was analyzed by ICAP using Method 6010A. Included in this



number were 3 method blanks, 46 sample duplicates or replicates, and 9 MS/MSD sample sets.






                                       6-26

-------
 Table 6-17 summarizes the sample collection and analysis dates for these samples. As shown in



 Table 6-17, all trace metal analyses were completed within the method-required hold time of



 180 days.




         Table 6-18 summarizes trace metal measurement  QAOs for precision, accuracy, and



 completeness. Table 6-19 shows the MDL objectives and the achieved values for the trace metal



 analyses. As can be seen in Table 6-19, the MDL objective was met for all metals with the




 exception of zinc.  The zinc MDL was achieved for solid residues but not aqueous liquid or flue



 gas matrices.   ,   




         Three method blanks were analyzed for trace metals. Included in this group were one




 TCLP extraction fluid  blank and the front half  and back half of a multiple metals train field



 blank. Analysis results are shown in Table 6-20.




         Measurement  precision  was assessed by performing duplicate or replicate sample



 analyses. Table 6-21 summarizes the results of these analyses. The data in Table 6-21 show that




 103 out of 143 precision calculations performed,  or 72 percent, were within the precision QAO




 of 25 percent  RSD or RPD.  As the completeness QAO was 70 percent for this measurement,



 the precision QAO, as measured by duplicate or replicate sample analyses, was met.




        Trace metal measurement accuracy was assessed by preparing and analyzing MS/MSD



 samples. The MS/MSD sample analysis results are given in Table 6-22. The data in Table 6-22



 show that only 79 out of 168 measurements, or 47 percent, were within the accuracy QAO range




 of 70 to 130 percent recovery. Antimony, barium, and silver recoveries were particularly poor.



 The reason for poor antimony recoveries likely lay with the digestion method used. The method




 employed, heated HNO3/HF for solid samples and heated HNO3 for aqueous liquid samples,




may have caused evaporative loss of the relatively volatile antimony.  The poor silver recoveries



may have been caused  by the presence of chlorides in test program samples.  The data in






                                        6-27

-------
    TABLE 6-17.  SAMPLE HOLD TIMES FOR TRACE METAL ANALYSES BY ICAP
Collection/
Sample preparation date*
Test Feed
TestO
Test 1"
Test 2"
TestS"
Test 6"
Composite soil" (Tests 3 and 4)
Kiln Ash
Test 1"
Test 2b
Test 3C
Test4e
TestS"
Test6b
Baghouse Ash
Test 0
Test 1
Test 2d
Test 3
Test 4
TestS
Test 6
Scrubber Liquor
Test 0 pretest
Test 0 post-test
Test 1 pretest
Test 1 post-test"
Test 2 pretest
Test 2 post-test
Test 3 pretest
Test 3 post-test
Test 4 pretest
Test 4 post-test
Test 5 pretest
Test 5 post-test
Test 6 pretest
Test 6 post-test
Method Requirement
"Preparation date corresponds to TCLP leachates.

01/04/94
10/14/93
10/15/93
10/18/93
10/18/93
10/20/93

11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93

10/28/93
11/10/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93

10/27/93
10/27/93
11/09/93
11/09/93
11/16/93
11/16/93
12/01/93
12/01/93
12/02/93
12/02/93
11/18/93
11/18/93
11/23/93
11/23/93


Analysis hold time,
Analysis date days

01/18/94
12/09/93
12/09/93
12/09/93
12/09/93
12/09/93

12/09/93
12/14/93
01/03/94
01/03/94
12/14/93
12/14/93

12/09/93
12/09/93
12/17/93
12/23/93
12/23/93
12/17/93
12/17/93

12/09/93
12/09/93
12/09/93
12/09/93
12/14/93
12/14/93
12/23/93
12/23/93
12/23/93
12/23/93
12/14/93
12/14/93
12/14/93
12/14/93



14
56
55
52
52
50

30
28
33
32
26
21

42
29
31
22
21
29
24

43
43
30
30
28
28
22
- 22
21
21
28 ,
28
21
21
180
(continued)
     -             .  .          nalyzed.
Tour split samples were prepared and analyzed.
    i split samples were prepared and analyzed.
                                       6-28

-------
TABLE 6-17.  (continued)

Collection/
Sample preparation date*
Multiple Metals Train (front half)
Test 0
Test 1
Test 2
TestS
Test 4
TestS
Test 6
Multiple Metals Train (back half)
Test 0
Test 1
Test 2
TestS
Test 4
Test 5
Test 6
TCLP Leachates:
Test Feed
Test 1
Test 2
TestS
Test 6
Composite soil (Tests 3 and 4)
Kiln Ash
Test 1
t
Test 2
TestS"
Test 4
Test 5
Test 6
Method Requirement
"Preparation date corresponds to TCLP leachates.

10/27/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93

10/27/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93


10/14/93
10/15/93
10/18/93
10/18/93
10/20/93

11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93


Analysis hold time,
Analysis date

12/09/93
12/09/93
12/17/93
12/23/93
12/23/93
12/17/93
12/27/93

12/09/93
12/09/93
12/14/93
12/23/93
12/23/93
12/14/93
12/17/93


12/14/93
12/14/93
12/14/93
12/14/93
12/14/93

12/09/93
12/23/93
01/18/94
01/18/94
12/23/93
12/23/93


days

43
30
31
22
21
29
24 ,

43
30
28
22
21
26
24


61
60
57
57
55

30
39
48
47
35
30
180
(continued)
         6-29

-------
TABLE 6-17. (continued)
Collection/
Sample preparation date*
TCLP Leachates (continued):
Baghouse Ash
Test 0
Test 1
Test 2
TestS
Test 4d
TestS
Test 6
Post-test Scrubber Liquor
TestO
Test 1
Test 2
Test 3
Test 4
TestS
Test 6
Blanks
Multiple metals train field blank front half
Multiple metals train field blank back half
TCLP extraction fluid
Spikes:
Test Feed
Test 1 MS
Test 1 MSB
Composite soil MS
Composite soil MSD
Kiln Ash
Test 1 MS
Test 1 MSD
Baghouse Ash
Test 1 MS
Test 1 MSD
Method Requirement
'Preparation date corresponds to TCLP leachates.


10/28/93
11/10/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93

10/27/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93

12/07/93
12/07/93
12/30/93


10/14/93
10/14/93
10/20/93
10/20/93

11/09/93
11/09/93

11/10/93
11/10/93


Analysis hold time,
Analysis date days


12/09/93
12/09/93
12/23/93
01/18/94
01/18/94
12/23/93
12/23/93

12/14/93
12/14/93
12/23/93
01/18/94
01/18/94
12/23/93
12/23/93

01/18/94
01/18/94
01/18/94


01/26/94
01/26/94
01/18/94
01/18/94

01/18/94
01/18/94

01/18/93
01/18/93




42
29
37
48
47
35
30

48
35
37
48
47
35
30

42
42
19
c

104
104
98
98

70
70

69
69
180
(continued)
         6-30

-------
                                TABLE 6-17. (continued)
Sample
Spikes (continued):
Scrubber Liquor
Test 6 MS
Test6MSD
Multiple Metals Train (front half)
Blank spike MS
Blank spike MSD
Multiple Metals Train (back half)
Blank spike MS
Black spike MSD
TCLP Leachates:
Kiln Ash
Test 3 MS
Test 3 MSD
Baghouse Ash
Test 3 MS
Test 3 MSD
Method Requirement
Collection/ Analysis hold time,
preparation date* Analysis date days


11/23/93
11/23/93

01/11/94
01/11/94

01/11/94
01/11/94


12/01/93
12/01/93

12/01/93
12/01/93



01/18/94
01/18/94

01/18/94
01/18/94

01/18/94
01/18/94


01/18/94
01/18/94

01/18/94
01/18/94



56
56

7
7

7
7


48
48

48
48
180
Preparation date corresponds to TCLP leachates.
                                         6-31

-------
                        TABLE 6-18. TRACE METAL MEASUREMENT QAOs
Measurement
parameter
Trace metals in solid
samples
Trace metals in
Method Reference
ICAP BIF methods, SW-846
Method 6010A
ICAP BIF methods, SW-846
Conditions %
Microwave digestion
by BIF methods
Conventional digestion
Precision, Accuracy, Completeness,
iRSDorRPD % %
25
25
70-130 70
70-130 70
aqueous liquid samples
Method 6010A       by BIF methods
        TABLE 6-19. TRACE METAL MEASUREMENT MDLs; OBJECTIVES AND ACHIEVED LEVELS



                                              MDL objective
Measurement
parameter
Antimony
Arsenic
Barium
Cadmium
Chromium
Copper
Lead
Nickel
Silver
Zinc
Solid residues, mg/kg
objective / achieved
10 / 0.01
10 / 0.01
1 / 0.01
2 / 0.003
5 / 0.01
5 / 0.002
10 / 0.005
5 / 0.0049
5 / 0.0004
1 / 0.26
Aqueous liquids, ng/L
objective / achieved
100 / 30
100 / 50
10/3
20/4
50/7
50/23
100 / 77
50/10
50/7
10/25
Flue gas, /tg/dscm
objective / achieved
50 / 8.5
50 / 12.1
5/3.6
10 / 0.8
30/4.4
30 / 4.5
50 / 15.4
30 / 3.3
30 / 1.4
5 / 12.6

-------
                   TABLE 6-20. TRACE METAL ANALYSES OF METHOD BLANK SAMPLES
Concentration
Sample
TCLP extraction fluid, mg/L
Multiple metals tram field blank
Front half, mg
Back half, mg/L
Sb
<0.03

<0.01
<0.03
As
<0.05

<0.01
<0.05
Ba
0.56

0.010
0.0030
Cd
<0.004

< 0.0003
< 0.004
Cr
<0.007

0.010
<0.007
Cu
0.11

0.0023
0,023
Pb
0.87

<0.005
0.077
Ni
0.045

0.0049
<0.01
Ag
<0.007

< 0.0004
<0.007
Zn
98

0.026
0.025
o\

-------
                    TABLE 6-21.  REPLICATE TRACE METAL SAMPLE ANALYSIS RESULTS
o\
Concentration
Sample
Test Feed:
Testl
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
RSD, %
Test 2
Sample
Replicate 1
. Replicate 2
Replicate 3
Replicate 4
RSD, %
Test 5
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
RSD, %
- = RSD, RPD not calculated.
Sb


62
200
110
94
110
45

290
190
130
140
130
39

98
80
91
120
63
23

As


48
<20
<20
<20
<20
 *

<20
<20
<20
<20
<20
0

<20
<20
<20
<20
<20
0

Ba


43
87
120
75
47
42

76
44
72
70
90
24

52
50
48
37
48
12

Cd


 2.0
2.2
<0.5
0.9
1.2
53

1.3
1.4
1.5
2.2
1.1
28

1.5
1.3
1.4
<0.5
1.8
37

Cr


27
32
31
40
40
17

37
36
45
34
38
11

33
23
32
21
27
2Q

Cu


8,800
9,000
13,000
8,400
5,000
32

8,200 *
7,100
8,900
8,000
9,800
12

7,600
28,000
9,800
7,600
9,000
71

Pb


1,300
2,400
1,600
2,800
3,800
42

3,000
1,400
5,100
1,300
1,200
70

1,200
1,100
1,100
980
1,000
8

Ni


5.2
4.5
<3.0
5.1
<3.0
26

<3.0
3.7
<3.0
4.3
<3.0
17

<3
<3
<3
<3
<3
0

Ag


<0.7
1.2
<0.7
1.1
<0.7
28

1.3
<0.7
2.6
1.0
<0.7
63

<0.7
1.2
<0.7
1.4
2.1
48

Zn


95
120
100
100
96
10

110
130
310
240
120
49

150
140
150
110
140
12


Precision
QAO







25






25






25
(continued)

-------
TABLE 6-21. (continued)
Concentration
Sample
Test Feed (continued):
Test 6
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
RSD,%
Composite Soil (Tests 3 and 4)
Sample
Replicate 1
Replicate 2
ReplicateS
Replicate 4
RSD, %
Kiln Ash:
Testl
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
RSD, %
' = RSD, RPD not calculated.
Sb


66
86
75
92
200
53

75
66
87
52
48
25


1,100
1,100
1,200
1,100
1,200
5

As


<20
<20
<20
<20
<20
0

<20
<20
<20
<20
<20
0


42
<20
<20
<20
, <20


Ba


110
42
56
100
98
37

66
69
76
80
67
9


280
260
270
230
290
9

Cd


<0.5
<0.5
1.5
1.1
1.3
47

1.5
1.2
1.4
1.6
0.9
21


<0.5
<0.5
<0.5
<0.5
<0.5
0

Cr


21
23
23
27
26
10

70
73
130
83
68
31


360
390
400
350
440
9

Cu


8,300
7,900
7,700
9,500
15,000
32

12,000
14,000
26,000
11,000
7,400
50


130,000
200,000
240,000
210,000
150,000
24

Pb


980
800
900
970
840
9

4,200
2,300
3,800
2,500
2,900
26


3,000
2,600
3,100
3,100
3,000
7

Ni


<3.0
9.0
<3.0
<3.0
5.1
57

19
27
46
28
24
36
,

230
280
250
220
410
28

Ag


3.6
<0.7
<0.7
<0.7
<0.7
*

1.4
1.8
2.3
1.6
<0.7
38


1.9
1.3
1.6
1.7
2.0
16

Zn


130
120
150
120
89
!8

170
210
210
220
130
20


180
180
200
190
190
4


Precision
QAO







25






25







25'
(continued)

-------
TABLE 6-21. (continued)
Concentration
Sample
Kiln Ash (continued):
Test 2
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
RSD, %
Test 3
Sample
o\ _. ..
^ Replicate 1
<* Replicate 2
Replicate 3
RSD, %
Test 4
Sample
Replicate 1
Replicate 2
Replicate 3
RSD,%
Sb


880
870
1,000
930
1,000
7

180
200
180
190
5

190
190
190
200
3
As


<20
<20
<20
63
33
60

<20
<20
<20
<20
0

<20
<20
<20
<20
0
Ba


240
170
210
220
240
13

120
99
150
140
18

120
98
72
95
20
Cd


0.6
<0.5
<0.5
0.6
<0.5
10

<0.5
<0.5
<0.5
<0.5
0

<0.5
<0.5
<0.5
<0.5
0
Cr


370
430
600
410
600
23

67
66
79
70
8

41
60
56
50
16
Cu


83,000
190,000
150,000
99,000
190,000
35

46,000
69,000
32,000
67,000
33

18,000
21,000
67,000
50,000
60
Pb


3,600
3,300
3,800
3,600
4,500
12

4,000
4,300
4,400
3,800
7

4,000
4,000
3,700
4,000
4
Ni


320
750
1,300
450
1,400
58

65
59
66
70
7

42
60
56
48
16
Ag


3.0
4.8
3.9
3.5
7.0
35

2.1
15
1.7
13
21

1.7
1.8
2.3
2.2
15
Zn


220
270
290
270
260
10

320
350
340
310
6

290
300
300
300
2
W> "  
Precision
QAO







25





25





25
 (continued)

-------
TABLE 6-21. (continued)
Concentration
Sample
Kiln Ash (continued):
TestS
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
RSD,%
Test 6
Sample
o\ Replicate 1
53 Replicate 2
Replicate 3
Replicate 4
RSD%
Baghouse Ash
Test 2 sample
Duplicate
RPD, %
Post-test Scrubber Liquor
Test 1 sample
Duplicate
RPD,%
 = RSD, RPD not calculated.
Sb


1,000
980
790
1,000
1,000
10

1,100
820
940
890
1,000
13

400
340
16

0.47
0.65
32

As


<20
<20
<20
<20
<20
0

<20
<20
<20
120
48
95

<20
20


0.12
<0.05


Ba


270
290
140
240
240
24

270
210
270
220
270
12

-22
20
10

2.4
5.3
75

Cd


<0.5
0.8
<0.5
<0.5
0.6
22

1.0
<0.5
<0.5
<0.5
<0.5
 *

18
17
6

0.20
0.25
22

Cr


470
480
500
440
420
7

550
520
520
570
510
5

320
310
3

1.9
2.9
42

Cu


110,000
110,000
85,000
160,000
110,000
24

170,000
180,000
170,000
190,000
170,000
5

14,000
14,000
0

210
230
9

Pb


5,500
5,800
6,000
5,600
5,600
4

5,700
5,600
7,100
5,500
5,800
11

19,000
44,000
79

780
900
14

Ni


160
140
140
160
140
7

350
330
360
640
310
34

130
110
17

1.2
1.7
35

Ag


5.0
2.4
2.6
2.4
1.0
54

23
3.6
2.3
5.6
2.7
48

<0.7
1.0


0.072
0.094
25

Zn
=====

250
250
180
260
260
14

280
260
240
230
250
8

2,100
2,100
0

19
23
19

. , , asseg
n  *
Precision
QAO
===================






25





25


25



25
(continued1)

-------
TABLE 6-21. (continued)
Concentration
Sample
TCLP Leachate
Test 3 kiln ash sample
Duplicate
RPD, %
Test 4 sample
Duplicate
RPD, %
Sb

<0.2
<0.2
0
0.80
0.84
5
As

<0.2
<0.2
0
0.26
0.21
21
Ba

0.26
0.26
0
0.22
0.22
0
Cd

< 0.005
<0.005
o
1.7
1.8
6
Cr

0.046
0.044
4
0.27
0.30
11
Cu

0.28
0.22
24
640
650
2
Pb Ni

<0.1 <0.01
<0.1 <0.01
0 0
5,700 3.2
5,800 3.3
2 3
Ag

<0.007
<0.007
0
0.027
0.028
4
Zn

1.2
1.3
8
97
100
3
Precision
QAO


25

25
00

-------
             TABLE 6-22. TRACE METAL RECOVERIES FROM MS SAMPLES ANALYZED BY ICAP
% recovery
Sample
Test 1 Fluff Feed
MS
MSD
RPD, %
Test 3 and 4 Soil Feed
MS
MSD
RPD, %
Test 1 Kiln Ash
o\
 MS
* MSD
RPD, %
Test 1 Baghouse Ash
MS
MSD
RPD, %
Test 6 Scrubber Liquor
MS
MSD
RPD, %
Sb
=====

17
0
200

40
103
88


62
16
118

52
95
59

0
0
0
As

65
68
5

66
38
54


56
72
25

66
>134

79
79
0
Ba

63
27
80

910
4
198


0
0
0

17
37
74

46
54
16
Cd

195
81
83

76
61
22


75
90
18

60 
64
6

67
61
9

Cr

92
85
8

100
68
38


64
65
2

50
44
13

82
71
14
==
Cu
i in sza
NS'
NS
_b

NS
NS



NS
NS


NS
NS


112
112
0
5
Pb
.. . ,SS
30
57
62

87
63
32


19
4
130

NS
NS


99
63
44
X
Ni
5
9
8
12

61
63
3


84
80
5

44
42
5

75
69
8
=====
Ag

9
2
127

5
35
150


13
0
200

%
0

46
89
64
Zn Accuracy/precision QAO

108
94
14

63
50
23


95
70
30

53
44
19

71
234
107

70-130
70-130
25

70-130
70-130
25


70-130
70-130
25

70-130
70-130
25

70-130
70-130
25
NS = Not spiked.
b = RPD not calculated.
(continued)

-------
                                             TABLE 6-22.  (continued)
% recovery
Sample
Multiple Metals Train Blank Spike
Back half
MS
MSD
RPD, %
Front half
MS
MSD
RPD, %
 Test 3 Kiln Ash TCLP Leachate
o
MS
MSD
Sb As


117 85
100 90
15 6

<10 - 68
<10 71
0 4


<10 80
<10 85
Ba


88
85
3

17
0
200


73
77
Cd


84
84
0

97
77
23


85
85
Cr


91
91
0

12
8
40


75
73
Cu


102
102
0

108
85
24


119
94
Pb


109
101
8

85
70
19


120
109
Ni


80
79
1

100
36
94


69
66
Ag


72
46
44

90
160


45
43
Zn Accuracy/precision QAO


131
131
0

95
47
68


ISC
IS


70-130
70-130
25

70-130
70-130
25


70-130
70-130
 RPD, %

Test 3 Baghouse Ash TCLP
Leachate
23
10
5    -"
b = RPD not calculated.
IS = Spiked amount not significant compared to native sample amount.
25
MS
MSD
RPD, %
0
0
0
58
78
29
42
83
66
83
78
6
39
44
12
105
109
4
73
62
16
86
84
2
178
228
25
111
115
4
70-130
70-130
25

-------
 Section 4.1 show that both test feed material matrices contained significant amounts of chlorine.



 Thus, test program samples used to prepare the MS/MSD samples may have contained chlorine



 in the form of chlorides. The presence of chlorides will definitely interfere with the sample



 digestion method employed.  The reason for the poor barium recoveries is  not clear.



        If antimony, barium, and silver are removed from consideration, then 67 out of 114



 other metal spike recovery measurements, or 59 percent, fell within the accuracy QAO range of




 70 to 130 percent recovery.  This still fails the completeness objective of 70 percent. However,




 had the accuracy QAO range instead been a slightly relaxed 60 to 140 percent recovery, then 89




 of  114  other metal (antimony, barium, and silver excluded)  recovery  measurements, or




 78 percent, would have been acceptable,  a 70 percent  completeness  objective at this relaxes



 accuracy QAO range would have been met.




        Trace measurement precision was-also measured by calculating the RPD of each pair




 of MS/MSD measurements. The data in Table 6-22 show that 55 out of 84 RPDs, or 65 percent,




 met the  precision QAO  of 25 percent RPD.  However, again, the precision measures for




 antimony, barium, and silver were particularly poor. If these three metals are excluded, then 43




 of the remaining 57 RPD determinations, or 75 percent, met the precision QAO of 25 percent



 RPD. This would have satisfied the completeness objective of 70 percent.




       Based on both the precision and accuracy checks employing MS/MSD sample analyses,



test program results for antimony, barium, and silver appear to have been compromised, and the




reported  data should be treated with caution.   Test program conclusions regarding the




concentrations of these three metals in incinerator discharges, and their distributions among



these discharges, must be viewed as tentative at best.
                                        6-41

-------
 6.4     CHLORIDE ANALYSES




        A total of  17  samples was analyzed for chloride  ion  to  support  flue gas HC1



 concentration measurements.  Included in this number were 1 method blank and 1 MS/MSD




 sample set. Table 6-23 lists the sample collection and analysis dates and the analysis hold times




 for these  samples.  As the data in Table 6-23 show, all 17 samples were analyzed within the



 method required hold time limit of 28 days.




        Table 6-24 summarizes  the flue gas chloride measurement precision,  accuracy, and




 completeness QAOs.  The MDL objective for the measurement was 100 jzg/dscm. This objective



 was met with an achieved MDL of 49 /ig/dscm.




        Table 6-25 shows that the chloride recoveries for the MS/MSD sample set were both



 within the accuracy QAO range of 75 to 125 percent recovery.  Table 6-25 also shows that the




 RPD of the MS/MSD sample set was within the precision QAO of 30 percent RPD. Thus, both




 the accuracy and precision QAOs were met as measured by the MS/MSD sample analyses.




        Table 6-26  summarizes the chloride analysis results for the duplicate  test  samples



 analyzed.  As can be seen from the data in Table 6-26, 9 of the 11 RPDs, or 82 percent, met the



 precision QAO of 30 percent RPD.  As the completeness objective for the measurement was



 70 percent, the precision QAO, as measured by duplicate sample analyses, was met.



 6.5     PCDD/PCDF ANALYSES




       A total of 35  samples was analyzed for PCDDs and PCDFs by GC/MS using Method




 8290 or Method 23. Included in this number were one Method 23 sorbent resin method blank,




 one pretest scrubber liquor blank, and three duplicates of test samples.  Table 6-27 lists the




 sample collection, extraction, and analysis dates for these samples, and the corresponding analysis



hold  times. As shown in Table 6-27, all but five samples were extracted within the specified




method limit.  Three of the five samples not extracted within the method hold time were sample






                                       6-42

-------
         TABLE 6-23. SAMPLE HOLD TIMES FOR CHLORIDE ANALYSES BY ION CHROMATOGRAPHY
o\
4s






















Sample*
Stack Exit Flue Gas
TestO
Test 1
Test 1 MS
Test 1 MSD
Test 2
TestS
Test 4
TestS
Test 6
Method blank
Baghouse Exit Flue Gas
TestO
Test 1
Test 2
TestS
Test 4
Test 5
Test 6
Method Requirement
"All samples were analyzed
Collection/preparation date

10/27/93
11/09/93
11/09/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
12/07/93

10/27/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93

in duplicate.
TABLE 6-24. FLUE GAS CHLORIDE
Measurement
parameter Method
HClin

flue gas Ion chromatography

Reference
Analysis date Analysis

11/22/93
11/29/93
11/29/93
11/29/93
11/29/93
12/06/93
12/06/93
12/06/93
11/29/93
12/10/93

. 11/22/93
11/29/93
11/29/93
12/06/93
12/06/93
11/29/93
11/29/93


MEASUREMENT QAOs
Precision,
% RSD or RPD
40 CFR 60, Appendix A, Method 5; 30
BIF methods; Method 9057

hold time, days

26
20
20
'20
7
5
4
18
6
3

26
20
7
5
4
11
6
28


Accuracy, Completeness,
% %
75-125 70


-------
TABLE 6-25. CHLORIDE RECOVERIES FROM MS SAMPLES
            ANALYZED BY ION CHROMATOGRAPHY
       Sample
 Chloride recovery,
	   %         Precision QAO
  Stack Exit Flue Gas
   Test 1 MS
   Test 1 MSD
   RPD, %

  Recovery QAO
       105
       109
       3.7

     75-125
30
TABLE 6-26. DUPLICATE
SAMPLE CHLORIDE ANALYSIS RESULTS
Chloride concentration, mg/L
Sample
Stack Exit Flue Gas
Test 1
Test 2
Test3
Test 4
Test 5
Test 6
Baghouse Exit Flue Gas
Test 1
Test 2
Tests
Test 4
Test 6
QAO
Analyses Duplicate analyses RPD, %

0.40
0.88
0.52
<0.29
<0.29
<0.29

19.0
123
28.3
19.6
42.0


<0.29
0.78
0.64
0.60
<0.29
<0.29

18.8
12.0
28.4
20.0
42.7


>31.9
12.1
20.7
>69.7
0
0

1.1
2.5
0.4
2.0
1.7
30
                        6-44

-------
TABLE 6-27. SAMPLE HOLD TIMES FOR THE PCDD/PCDF ANALYSES BY GC/MS
Sample
Test Feed
Packaging container material
Composite fluff feed
Composite soil feed
Kiln Ash
Testl
Test 1 duplicate
Test 2
TestS
Test 4
TestS
Test 6
Baghouse Ash
TestO
Testl
Test 1 duplicate
Test 2
Test.3
Test 4
TestS
Test 6
Post-test Scrubber Liquor
TestO
Testl
Test 1 duplicate
Test 2
Test3
Test 4
TestS
Test 6
Pretest Scrubber Liquor
Testl
Baghouse Exit Flue Gas Method 23 Train
TestO
Testl
Test 2
TestS
Test 4
TestS
Test 6
Method blank
Method Requirement
Collection
date

12/21/93
10/20/93
10/20/93

11/09/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93

10/28/93
11/10/93
11/10/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93

10/27/93
11/09/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
12/23/93

10/09/93

10/27/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
12/07/93

Extraction Extraction hold Analysis Analysis hold
date time, days date time, days

01/12/94
11/08/93
12/02/93

11/19/93
01/21/93
12/02/93
12/10/93
12/10/93
12/02/93
12/07/93

11/08/93
12/02/93
01/12/94
12/02/93
12/10/93
12/10/93
12/02/93
12/07/93

11/10/93
12/10/93
01/14/94
12/03/93
12/16/93
12/16/93
12/10/93
12/06/93

12/03/93

11/10/93
11/19/93
12/02/93
12/09/93
12/09/93
12/02/93
12/02/93
12/09/93


22
13
43

10
73
16
9
8
14
14

11
22
63
16
9
8
14
14

14
31
66
17
15
14
22
13

14

'l4
10
16
8
7
14
9
2
30

,01/20/94
11/16/93
12/05/93

11/22/93
01/24/93
12/05/93
12/17/93
12/17/93
12/05/93
12/17/93

11/16/93.
12/05/93
01/20/94
12/05/93
12/18/93
12/18/93
12/05/93
12/17/93

11/15/93
12/14/93
01/21/94
12/07/93
12/19/93
12/19/93
12/15/93
12/15/93

12/07/93

11/15/93
11/24/93
12/06/93
12/13/93
12/13/93
12/06/93
12/06/93
12/13/93


8
8
3

3
3
3
7
7
3
10

8
3
8
3
8
8
3
10

5
4
7
4
3 
3
5
9

4

5
5
4
4 .
4
4
4
4
45
                              6-45

-------
  duplicates for analysis; one of the five missed extraction hold time by 1 day.




         Table 6-28 summarizes the PCDD/PCDF measurement QAOs for precision, accuracy,



  and completeness. Measurement precision was assessed by analyzing split samples in duplicate.



  Table  6-29  summarizes the  results  of these analyses and shows that 57 out of 75 RPD




  measurements, or 76 percent, were within the precision  QAO of 50 percent RPD.  As the




 completeness objective for the measurement was 70 percent, the precision QAO, as measured



 by duplicate sample analyses, was met.




         PCDD/PCDF measurement accuracy was assessed adding the method-specified internal



 standards and surrogates to all test samples and measuring their recovery.  Table 6-30 shows the




 internal standards recoveries achieved from the test samples.  As can be seen in Table 6-30,290




 out of 315 individual internal standard recovery measurements, or 92 percent, were within the




 compound-specific recovery ranges.  Since the completeness objective for this measurement was



 70 percent, the accuracy QAO, as measured by internal standards recovery, was met.




        Table 6-31 lists the surrogate recoveries achieved from test programs samples.  As



 shown,  149 out of 210 individual surrogate recovery measurements, or 71 percent, were within




 the method specified recovery ranges.  Again, with a completeness  objective of 70 percent, the



 accuracy QAO, as assessed by surrogate recoveries, was met.




        Table 6-32 shows the MDL objectives and the achieved values for the PCDD/PCDF




measurements.  As indicated, all MDL objectives were achieved.
                                        6-46

-------
                              TABLE 6-28.  PCDD/PCDF MEASUREMENT QAOs
  Measurement      Measurement/                                           Precision,   Accuracy,   Completeness,
    parameter      analytical method	Reference	Conditions	%	 %	%	

PCDDs/PCDFs in   Extraction,         40 CFR 266, Appendix IX,   Matrix-specific      50        25-130         70
feed, residual, and   concentration,      Method 23; SW-846        extraction
flue gas sampling    GC/MS           Method 8290
trains

-------
                    TABLE 6-29. DUPLICATE SAMPLE PCDD/PCDF ANALYSIS RESULTS
o\

Compound
23,7,8-TCDD
1,23,7,8-PeCDD
1,23,4,7,8-HxCDD
1,23,6,7,8-HxCDD
1,23,7,8,9-HxCDD
1,23,4,6,7,8-HpCDD
OCDD
23,7,8-TCDF
1,23,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,23,6,7,8-HxCDF
23,4,6,7,8-HxCDF
1,23,7,8,9-HxCDF
1,23,4,6,7,8-HpCDF
1,23,4,7,8,9-HpCDF
OCDF
Total TCDD
Total PeCDD
Total HxCDD
Total HpCDD
Total TCDF
Total PeCDF
Total HxCDF
Total HpCDF
Precision QAO
= m ===
Test 1 kiln ash, ng/kg
analysis / duplicate analysis
12.0 / 1.8
31.1 / 6.5
50.8 / 57.5
71.1 / 67.7
212/286
1,810 / 2340
11,590 / 24,580
496 / 281
155 / 49.1
273 / 215
2,770 / 3,160
614 / 676
2,130 / 2,560
25.2 / 35.8
6,180 / 15,220
1,360 / 2,070
12,160 / 44,810
232 / 2.4
305 / 76.6
914 / 905
3,830 / 4,660
3,330 / 1,430
5,730 / 4,630
10,780 / 11,190
15,810 / 28,870

~
RPD,
148
131
12
5
30
26
72
55
104
24
13
10
18
35
84
41
115
196
120
1
20
80
21
4
58
50
2-^^^^2E

Test 1 baghouse ash, ng/kg
analysis / duplicate analysis
0.3 / 1.0
0.47 / 030
0.40 / 0.46
0.69 / 0.74
1.5 / 1.4
213 / 18.1
179 / 110
3.6 / 3.1
1.5 / 1.2
3.2 / 3.7
10.7/9.4
3.9/3.3
9.1 / 9.7
03 / 1.1
39.8 / 25.9
8.1 / 63
123 / 603
0.9 / 0.88
1.5 / 0.42
6.4 / 6.8
38.6 / 32.6
15.4 / 3.1
26.8 / 10.1
40.2 / 41.5
833 / 57.3


RPD,
108
44
14
7
7
16
48
15
22
14
13
17
6
114
42
25
68
2
113
6
17
133
91
3
37
50
Test 1 post-test scrubber
liquor, pg/L
analysis / duplicate analysis
. 2.8 / 2.0
43 / 3.8
4.4 / 3.8
3.4 / 3.0
to t t 1
3.8 / 3.3
12.4 / 13.1
51.2 / 77.5
43 / 4.4
3.1 / 2.6
3.0 / 2.5
7.8 / 8.3
- 33 / 3.0
11.8 / 13.1
3.0 / 2.8
31.8 / 40.0
17.1 / 16.7
185 / 219
2.8 / 2.0
43 / 3.8
3.5 / 33
12.4 / 18.8
43 / 4.4
5.9 / 8.9
27.6 / 9.8
81.8 / 84.1


RPD,
33
12
15
13
1 A
14
5
41
2
18
18
6
10
10
7
23
2
17
33
12
6
41
2
41
95
3
50
===

-------
               TABLE 6-30. INTERNAL STANDARD RECOVERIES IN THE PCDD/PCDF ANALYSES
z
vo
% recovery
Sample
Test Feed
Packaging container material
Composite fluff feed
Composite soil feed
Kiln Ash
Test 1
Test 1 duplicate
Test 2
Test 3
Test 4
TestS
Test 6
Baghouse Ash
TestO
Testl
Test 1 duplicate
Test 2
TestS
Test 4
TestS
Test 6
Pretest Scrubber Liquor
Testl
Recovery QAO
13r
C12'
2,3,7,8.
TCDF

543
72.5
85.5

70.4
64.2
56.4
49.8
41.0
90.9
743

60.0
78.6
5.7
71.8
53.5
42.1
68.9
64.4

59.1
40-130
13r
L12-
23,7,8-
TCDD

53.6
79.7
97.0

75.8
62.3
55.5
48.4
42.0
81.2
84.9

63.0
76.5
6.5
71.5
52.0
45.1
68.1
63.0

57.2
40-130
13r
c,r
W.7,8-
PeCDF

58.2
82.2
94.4

83.2
69.4
65.9
47.7
48.9
99.4
773

69.6
86.6
17.5
80.9
58.0
46.6
75.7
64.4

63.3
40-130
13r
1-12"
W.7,8-
PeCDD

593
92.5
107

114
80.5
76.0
54.4
60.7
-90.7
77.2

883
103
33.9
97.4
68.0
63.8
93.0
67.6

66.7
40-130
13r
CI2'
1,23,6,7,8-
HxCDF

59.0
76.4
111

96.1
71.0
74.5
67.4
58.4
113
92.8

76.2
93.8
43.7
91.8
74.4
64.4
87.8
57.6

79.7
40-130
13r
C12'
1,23,6,7,8.
HxCDD

61.1
83.3
111

109
79.6
79.0
73.0
70.0
95.7
99.6

88.8
108
54.8
101
77.5
81.6
96.8
85.0

81.9
40-130
13r
c,2-
1,23,4,6,7,8-
HpCDF

47.2
77.7
117

107
82.2
86.1
612
62.2
164
392

70.9
110
57.5
95.4
69.6
61.2
95.2
66.0

76.7
25-130
13r
C,2.
1,23,4,6,7,8-
HpCDD

44.0
94.9
142

135
92.2
98.2
67.6
73.7
130
145

91.7
115
68.2
108
77.2
76.8
107
853

83.1
25-130
13CI2-OCDD

31.1
95.2
120

138
81.5
105
53.1
623
185
397

85.2
114
77.2
100
60.1
62.6
111
163

66.9
25-130
(continued)

-------
                                                TABLE 6-30. (continued)
o\

6,
o
% recovery
Sample
Post-test Scrubber Liquor
Test 0
Testl
Test 1 duplicate
Test 2
Test3
Test 4
TestS
Test 6
Baghouse Exit Method 23 Train
TestO
Testl
Test 2
Test3
Test 4
TestS
Test 6
Method blank
Recovery QAO
13r
C,2-
23,7,8-
TCDF

52.0
52.2
36.1
41.0
56.0
47.8
20.0
34.3

83.0
56.9
65.0
61.8
63.9
42.7
69.4
69.6
40-130
13r
t-12-
23,7,8-
TCDD

59.6
48.3
30.1
39.0
59.9
48.2
193
25.6

94.1
57.2
593
56.5
59.6
38.7
60.1
65.3
40-130
13r
c,r
1,23,7,8-
PeCDF

58.5
51.9
28.4
42.4
65.9
51.5
21.7
25.2

87.2
613
62.4
60.9
71.0
38.9
60.1
71.6
40-130
13r
C12-
W,7,8-
PeCDD

55.0
57.4
28.9
47.5
55.5
37.5
24.0
25.3

96.6
75.7
65.0
64.7
87.9
44.5
59.6
77.0
40-130
13r
C12'
1,2,3,6,7,8.
HxCDF

73.6
58.3
30.9
53.0
90.1
74.5
30.6
39.5

108
72.4
853
72.4
84.4
57.4
81.7
893
40-130
I3r
C,2-
1,23,6,7,8-
HxCDD

75.6
62.6
33.4
55.7
79.2
62.1
31.5
39.2

112
77.9
82.4
743
88.0
56.7
83.8
89.9
40-130
13r
C,2-
1,23,4,6,7,8.
HpCDF

62.8
53.1
29.1
45.8
76.1
53.4
28.2
33.2

89.1
69.7
79.9
66.0
83.1
513
76.8
88.0
25-130
13r
C12-
1,23,4,6,7,8.
HpCDD

63.2
57.4
36.7
50.8
78.2
59.9
30.5
37.2

90.7
813
83.7
69.9
89.0
56.1
81.7
973
25-130
13C,2-OCDD

413
50.4
263
39.7
663
54.2
26.2
30.6

71.8
68.2
74.5
58.2
78.5
50.8
70.4
92.4
25-130

-------
                  TABLE 6-31. SURROGATE RECOVERIES IN THE PCDD/PCDF ANALYSES
ON


Sample
Test Feed
Packaging container material
Composite fluff feed
Composite soil feed
Kiln Ash
Testl
Test 1 duplicate
Test 2
Test3
Test 4
TestS
Test 6
BaghouseAsh
TestO
Testl
Test 1 duplicate
Test 2
Test 3
Test 4
TestS
Test 6
Pretest Scrubber Liquor
Testl
Recovery QAO

37CI4-23,7,8-
TCDD

49.5
78.6
74.6

813
60.5
61.0
52.8
46.5
73.2
87.7

66.0
63.8
6.6
58.5
53.9
48.5
56.7
65.7

63.6
70-130

13C,2-2,3,4,7,8- 1;
PeCDF

573
81.2
74.5

86.5
723
77.5
543
58.2
863
81.5

802
79.1
273
75.5
59.9
63.7
70.5
66.7

75.4
70-130

3C,2-1^3,4,7^
HxCDF

63.9
81.7
92.5

92.9
71.5
87.7
78.9
69.1
114 .
144

87.1
79.5
49.4
79.6
75.6
823
70.9
695

81.2
70-130
% recovery
I- 13C12-1,23,4,7,8-
HxCDD

65.1
84.1
91.7

89.5
81.3
83.7
77.1
753
81.6
79.7

90.8
82.1
57.5
80.2
77.7
85.7
75.1
77.4

85.4
70-130

13C,2-1^3,4,7^,9- 
HpCDF

47.3
89.4
110

107
88.7
107
67.2
78.8
118
122

90.4
93.5
70.4
95.6
75.6
83.8
90.4
74.4

95.0
70-130

3C12-1^3,7^,9-
HxCDF

50.5
79.1
893

89.0
74.6
85.4
723
69.5
98.7
85.5

85.6
82.6
57.7
84.4
703
795
76.4
65.6

85.1
70-130
(continued)

-------
                                                TABLE 6-31.  (continued)
o\

^
to
Sample
Post-test Scrubber Liquor
TestO
Testl
Test 1 duplicate
Test 2
Test3
Test 4
TestS
Test 6
Baghouse Exit Method 23 Train
TestO
Test 1
Test 2
Test3
Test 4
TestS
Test 6
Method blank
Recovery QAO

TCDD

71.1
58.8
56.2
683
59.7
58.7
49.0
45.7

102
66.4
122 
119
114
124
. 115
113
70-130

13Cir23,4,7,8-
PeCDF

72.6
683
60.7
71.1
73.2
67.1
55.1
52.6

112
79.1
128
130
129
133
124
133
70-130

HxCDF

82.7
62.6
69.6
73.0
80.6
69.0
723
62.0

97.0 .
82.9
110
109
108
103
104
106
70-130
b recovery
HxCDI)'

86.1
74.4
88.4
77.0
90.8
73.9
76.8
66.4

107
88.2
121
110
108
107
103
117
70-130

13C12-1^3,4,7^,9-
HpCDF

75.0
80.0
86.6
833
93.8
81.0
73.5
81.1

97.1
96.1
137
139
131
138
129
138
70-130

HxCDF

75.4
75.9
71.8
81.5
913
80.8
71.1
68.8

79.6
74.0
84.4
64.1
71.8
54.6
723
75.6
70-130

-------
TABLE 6-32. PCDD/PCDF MEASUREMENT MDLs:  OBJECTIVES AND ACHIEVED
          LEVELS
Solid residues,
Measurement ng/kg
parameter objective / achieved
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
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
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Total TCDD
Total PeCDD
Total HxCDD
Total HpCDD
Total TCDF
Total PeCDF
Total HxCDF
Total HpCDF
20 / 0.6
20 / 0.9
20 / 1.0
20 / 0.8
20 / 0.9
20 / 1.0
20 / 1.1
20 / 0.6
20 / 0.7
20 / 0.7
20 / 0.7
20 / 0.5
20 / 0.7
20 / 0.8
20 / 0.6
20 / 1.0
20 / 0.9
30 / 0.6
30 / 0.9
30 / 0.9
30 / 1.0
30 / 0.6
30/0.7
30 / 0.7
30 / 0.8
Aqueous liquids,
Pg/L
objective / achieved
200 / 1.3
200 / 2.2
200 / 2.3
200 / 1.8
200 / 2.0
200 / 2.2
200 / 4.7
200 / 1.0
200 / 1.5
200 / 1.5
200 / 1.6
200 / 1.2
200 / 2.7
200/1.7
200 / 1.4
200/2.3
200 / 2.6
300 / 1.3
300 / 2.2
300 / 2.1
300 / 2.2
300 / 1.0
300/1.5
300 / 2.6
300 / 1.8 .
Flue gas, ng/dscm
objective / achieved
0.2 / 0.0009
0.2 / 0.0012
0.2 / 0.0015
0.2 / 0.0012
0.2 / 0.0015
0.2 / 0.0015
0.2/0.0061
0.2 / 0.0009
0.2 / 0.0009
0.2 / 0.0009
0.2 / 0.0012
0.2 / 0.0009
0.2 / 0.0025
0.2 / 0.0012
0.2 / 0.0009
0.2 / 0.0015
0.2 / 0.0018
0.5 / 0.0009
0.5 / 0.0012
0.5 / 0.0015
0.5 / 0.0015
0.5 / 0.0009
0.5 / 0.0009
0.5 / 0.0021
0.5 / 0.0012
                              6-53

-------
                                   REFERENCES
1.      "Guidance on Setting Permit Conditions and Reporting Trial Burn Results, Volume II
        of the Hazardous Waste Incineration Guidance Series," EPA/625/6-89-019  January
        1989.

2.      40 CFR Part 266, Appendix IX.

3.      "Test Methods for Evaluating Solid Waste: Physical/Chemical Methods," EPA SW-846,
        3rd edition, Revision 1, July 1992.

4.      40 CFR Part 60, Appendix A.

5.      Gullett, B., K. Bruce, and L.  Beach, "The Effect of Metal Catalysts on the Formation
        of Polychlorinated Dibenzo-p-dioxin and Polychlorinated Dibenzofuran Precursors,"
        presented at the 9th International Symposium  on Chlorinated Dioxins and Related
        Compounds (Dioxin 89), Toronto, Canada, 1989.
                                        R-l

-------